Low-temperature phase transition and magnetic properties of K₃YbSi₂O₇

The new ambient-temperature hexagonal (space group P6₃/mmc) polymorph of tripotassium ytterbium(III) disilicate (β-K₃YbSi₂O₇) has been synthesized by the high-temperature flux method and subsequently structurally characterized. In the course of the temperature-dependent single-crystal diffraction experiments, a phase transformation of β-K₃YbSi₂O₇ to a novel low-temperature orthorhombic phase (β′-K₃YbSi₂O₇, space group Cmcm) has been observed at about 210 K. β-K₃YbSi₂O₇ is isostructural with K₃ErSi₂O₇, whereas β′-K₃YbSi₂O₇ adopts a new type of structure. Both compounds can be built up from a regular alternation of layers of two types, which are parallel to the (001) plane. In the octahedral layer, YbO₆ octahedra are isolated and linked by K1O₆₊₃ polyhedra. The second, slightly thicker sorosilicate layer is formed by a combination of Si₂O₇ dimers and K2O₆₊₃ polyhedra. The boundary between the layers is a pseudo-kagome oxide sheet based on 3.6.3.6 meshes. The phase transition is due to a tilt of the two SiO₄ tetrahedra forming a single dimer which induces a decrease of the Si—O—Si angle between bridging Si—O bonds from 180° (dictated by symmetry in space group P6₃/mmc) to ≃164°. Magnetic characterization indicates that K₃YbSi₂O₇ remains paramagnetic down to 2 K, showing no apparent influence of the phase transformation on its magnetic properties. Analysis of the magnetization data revealed the positions of the three lowest crystal field levels of the Yb³⁺ cations, as well as the corresponding projections of their angular momentum on the direction of the magnetic field.

Computing details

Data collection: CrysAlis PRO 1.171.38.43 (Rigaku Oxford Diffraction, 2014) for beta-K3YbSi2O7, beta_prime-K3YbSi2O7. Cell refinement: CrysAlis PRO 1.171.38.43 (Rigaku Oxford Diffraction, 2014) for beta-K3YbSi2O7, beta_prime-K3YbSi2O7. Data reduction: CrysAlis PRO 1.171.38.43 (Rigaku Oxford Diffraction, 2014) for beta-K3YbSi2O7, beta_prime-K3YbSi2O7. Program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007) for beta_prime-K3YbSi2O7. Program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015) for beta-K3YbSi2O7; Jana2006 (Petricek et al., 2014) for beta_prime-K3YbSi2O7; SHELXL2018/3 (Sheldrick, 2018) for 93_K, 103_K, 113_K, 123_K, 133_K, 143_K, 153_K, 163_K, 173_K, 183_K, 193_K, 203_K, 213_K, 223_K, 233_K, 243_K, 253_K, 263_K, 273_K, 283_K, RT_after. Molecular graphics: VESTA (Momma & Izumi, 2011) for beta-K3YbSi2O7, beta_prime-K3YbSi2O7. Software used to prepare material for publication: SHELXL2018/3 (Sheldrick, 2015) for beta-K3YbSi2O7; Jana2006 (Petricek et al., 2014) for beta_prime-K3YbSi2O7.

(beta-K3YbSi2O7)

Crystal data

K3O7Si2Yb	Dx = 3.847 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1141 reflections
a = 5.7274 (5) Å	θ = 4.3–29.7°
c = 13.9339 (15) Å	µ = 13.69 mm^−1
V = 395.84 (8) Å^3	T = 298 K
Z = 2	Prismatic, colourless
F(000) = 422	0.28 × 0.09 × 0.08 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	187 reflections with I > 2σ(I)
ω scans	Rint = 0.040
Absorption correction: analytical CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 4.1°
Tmin = 0.110, Tmax = 0.450	h = −7→5
2409 measured reflections	k = −5→7
208 independent reflections	l = −14→17

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0168P)^2 + 0.3684P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.013	(Δ/σ)max < 0.001
wR(F^2) = 0.035	Δρmax = 1.02 e Å^−3
S = 1.17	Δρmin = −0.44 e Å^−3
208 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0129 (10)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09178 (11)	0.0113 (3)
K2	0.000000	0.000000	0.250000	0.0161 (5)
Yb1	0.000000	0.000000	0.000000	0.00325 (19)
Si1	0.666667	0.333333	0.13222 (12)	0.0033 (3)
O1	0.3575 (5)	0.1788 (2)	0.09590 (18)	0.0115 (6)
O2	0.666667	0.333333	0.250000	0.0203 (16)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0093 (4)	0.0093 (4)	0.0153 (7)	0.0047 (2)	0.000	0.000
K2	0.0208 (8)	0.0208 (8)	0.0065 (10)	0.0104 (4)	0.000	0.000
Yb1	0.0024 (2)	0.0024 (2)	0.0049 (3)	0.00121 (10)	0.000	0.000
Si1	0.0033 (5)	0.0033 (5)	0.0033 (8)	0.0016 (2)	0.000	0.000
O1	0.0073 (12)	0.0111 (10)	0.0148 (13)	0.0036 (6)	−0.0030 (12)	−0.0015 (6)
O2	0.030 (2)	0.030 (2)	0.002 (3)	0.0148 (12)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8668 (3)	K2—O1^xii	2.785 (3)
K1—O1^ii	2.8668 (3)	K2—O2^xiii	3.3067 (3)
K1—O1	2.8668 (3)	K2—O2	3.3067 (3)
K1—O1^iii	2.8668 (3)	K2—O2^xiv	3.3067 (3)
K1—O1^iv	2.8668 (3)	K2—Yb1	3.4835 (4)
K1—O1^v	2.8668 (3)	K2—Yb1^xv	3.4835 (4)
K1—O1^vi	3.032 (3)	K2—Si1^xiii	3.6915 (8)
K1—O1^vii	3.032 (3)	Yb1—O1^xvi	2.220 (2)
K1—O1^viii	3.032 (3)	Yb1—O1^xvii	2.220 (2)
K1—Si1^viii	3.121 (2)	Yb1—O1^iv	2.220 (2)
K1—Si1	3.3544 (5)	Yb1—O1^vii	2.220 (2)
K1—Si1^iii	3.3544 (5)	Yb1—O1^x	2.220 (2)
K2—O1	2.785 (3)	Yb1—O1	2.221 (2)
K2—O1^ix	2.785 (3)	Si1—O1^xviii	1.615 (2)
K2—O1^x	2.785 (3)	Si1—O1	1.615 (2)
K2—O1^xi	2.785 (3)	Si1—O1^v	1.615 (2)
K2—O1^iv	2.785 (3)	Si1—O2	1.6411 (17)
O1^i—K1—O1^ii	119.960 (4)	O1^xvii—Yb1—O1^x	92.48 (9)
O1^i—K1—O1	119.960 (5)	O1^iv—Yb1—O1^x	87.52 (9)
O1^ii—K1—O1	119.960 (5)	O1^vii—Yb1—O1^x	180.00 (15)
O1^i—K1—O1^iii	64.79 (10)	O1^xvi—Yb1—O1	180.0
O1^ii—K1—O1^iii	55.19 (10)	O1^xvii—Yb1—O1	92.48 (9)
O1—K1—O1^iii	174.68 (10)	O1^iv—Yb1—O1	87.52 (9)
O1^i—K1—O1^iv	55.19 (10)	O1^vii—Yb1—O1	92.48 (9)
O1^ii—K1—O1^iv	174.68 (10)	O1^x—Yb1—O1	87.52 (9)
O1—K1—O1^iv	64.79 (10)	O1^xvi—Yb1—K2	127.00 (7)
O1^iii—K1—O1^iv	119.960 (5)	O1^xvii—Yb1—K2	127.00 (7)
O1^i—K1—O1^v	174.68 (10)	O1^iv—Yb1—K2	53.00 (7)
O1^ii—K1—O1^v	64.79 (10)	O1^vii—Yb1—K2	127.00 (7)
O1—K1—O1^v	55.19 (10)	O1^x—Yb1—K2	53.00 (7)
O1^iii—K1—O1^v	119.960 (5)	O1—Yb1—K2	53.00 (7)
O1^iv—K1—O1^v	119.960 (4)	O1^xvi—Yb1—K2^xvi	53.00 (7)
O1^i—K1—O1^vi	65.81 (8)	O1^xvii—Yb1—K2^xvi	53.00 (7)
O1^ii—K1—O1^vi	89.78 (6)	O1^iv—Yb1—K2^xvi	127.00 (7)
O1—K1—O1^vi	117.74 (6)	O1^vii—Yb1—K2^xvi	53.00 (7)
O1^iii—K1—O1^vi	65.81 (8)	O1^x—Yb1—K2^xvi	127.00 (7)
O1^iv—K1—O1^vi	89.78 (6)	O1—Yb1—K2^xvi	127.00 (7)
O1^v—K1—O1^vi	117.74 (6)	K2—Yb1—K2^xvi	180.0
O1^i—K1—O1^vii	89.78 (6)	O1^xvi—Yb1—K1^xvi	53.876 (12)
O1^ii—K1—O1^vii	117.74 (6)	O1^xvii—Yb1—K1^xvi	53.878 (12)
O1—K1—O1^vii	65.82 (8)	O1^iv—Yb1—K1^xvi	126.122 (12)
O1^iii—K1—O1^vii	117.74 (6)	O1^vii—Yb1—K1^xvi	121.86 (7)
O1^iv—K1—O1^vii	65.81 (8)	O1^x—Yb1—K1^xvi	58.14 (7)
O1^v—K1—O1^vii	89.78 (6)	O1—Yb1—K1^xvi	126.123 (12)
O1^vi—K1—O1^vii	51.96 (8)	K2—Yb1—K1^xvi	111.14 (2)
O1^i—K1—O1^viii	117.74 (6)	K2^xvi—Yb1—K1^xvi	68.86 (2)
O1^ii—K1—O1^viii	65.81 (9)	O1^xvi—Yb1—K1^xiii	58.14 (7)
O1—K1—O1^viii	89.78 (6)	O1^xvii—Yb1—K1^xiii	126.123 (12)
O1^iii—K1—O1^viii	89.78 (6)	O1^iv—Yb1—K1^xiii	53.877 (12)
O1^iv—K1—O1^viii	117.74 (6)	O1^vii—Yb1—K1^xiii	126.123 (12)
O1^v—K1—O1^viii	65.81 (8)	O1^x—Yb1—K1^xiii	53.877 (12)
O1^vi—K1—O1^viii	51.96 (8)	O1—Yb1—K1^xiii	121.86 (7)
O1^vii—K1—O1^viii	51.96 (8)	K2—Yb1—K1^xiii	68.86 (2)
O1^i—K1—Si1^viii	91.15 (6)	K2^xvi—Yb1—K1^xiii	111.14 (2)
O1^ii—K1—Si1^viii	91.15 (6)	K1^xvi—Yb1—K1^xiii	72.25 (3)
O1—K1—Si1^viii	91.15 (6)	O1^xvi—Yb1—K1^viii	121.86 (7)
O1^iii—K1—Si1^viii	91.15 (6)	O1^xvii—Yb1—K1^viii	53.877 (12)
O1^iv—K1—Si1^viii	91.15 (6)	O1^iv—Yb1—K1^viii	126.123 (12)
O1^v—K1—Si1^viii	91.15 (6)	O1^vii—Yb1—K1^viii	53.877 (12)
O1^vi—K1—Si1^viii	30.38 (5)	O1^x—Yb1—K1^viii	126.123 (12)
O1^vii—K1—Si1^viii	30.38 (5)	O1—Yb1—K1^viii	58.14 (7)
O1^viii—K1—Si1^viii	30.38 (5)	K2—Yb1—K1^viii	111.14 (2)
O1^i—K1—Si1	145.98 (5)	K2^xvi—Yb1—K1^viii	68.86 (2)
O1^ii—K1—Si1	92.17 (5)	K1^xvi—Yb1—K1^viii	107.75 (3)
O1—K1—Si1	28.74 (5)	K1^xiii—Yb1—K1^viii	180.0
O1^iii—K1—Si1	145.98 (5)	O1^xvi—Yb1—K1	126.123 (12)
O1^iv—K1—Si1	92.17 (5)	O1^xvii—Yb1—K1	126.122 (12)
O1^v—K1—Si1	28.74 (5)	O1^iv—Yb1—K1	53.878 (12)
O1^vi—K1—Si1	130.05 (7)	O1^vii—Yb1—K1	58.14 (7)
O1^vii—K1—Si1	84.01 (4)	O1^x—Yb1—K1	121.86 (7)
O1^viii—K1—Si1	84.01 (4)	O1—Yb1—K1	53.877 (12)
Si1^viii—K1—Si1	99.67 (4)	K2—Yb1—K1	68.86 (2)
O1^i—K1—Si1^iii	92.17 (5)	K2^xvi—Yb1—K1	111.14 (2)
O1^ii—K1—Si1^iii	28.74 (5)	K1^xvi—Yb1—K1	180.0
O1—K1—Si1^iii	145.98 (5)	K1^xiii—Yb1—K1	107.75 (3)
O1^iii—K1—Si1^iii	28.74 (5)	K1^viii—Yb1—K1	72.25 (3)
O1^iv—K1—Si1^iii	145.97 (5)	O1^xviii—Si1—O1	110.65 (11)
O1^v—K1—Si1^iii	92.17 (5)	O1^xviii—Si1—O1^v	110.65 (11)
O1^vi—K1—Si1^iii	84.01 (4)	O1—Si1—O1^v	110.65 (11)
O1^vii—K1—Si1^iii	130.06 (7)	O1^xviii—Si1—O2	108.27 (11)
O1^viii—K1—Si1^iii	84.01 (4)	O1—Si1—O2	108.27 (11)
Si1^viii—K1—Si1^iii	99.67 (4)	O1^v—Si1—O2	108.27 (11)
Si1—K1—Si1^iii	117.24 (2)	O1^xviii—Si1—K1^viii	71.73 (11)
O1—K2—O1^ix	100.89 (10)	O1—Si1—K1^viii	71.73 (11)
O1—K2—O1^x	66.94 (8)	O1^v—Si1—K1^viii	71.73 (11)
O1^ix—K2—O1^x	142.87 (4)	O2—Si1—K1^viii	180.0
O1—K2—O1^xi	142.87 (4)	O1^xviii—Si1—K1	152.06 (13)
O1^ix—K2—O1^xi	66.94 (8)	O1—Si1—K1	58.620 (11)
O1^x—K2—O1^xi	142.87 (4)	O1^v—Si1—K1	58.621 (11)
O1—K2—O1^iv	66.94 (8)	O2—Si1—K1	99.67 (4)
O1^ix—K2—O1^iv	142.87 (4)	K1^viii—Si1—K1	80.33 (4)
O1^x—K2—O1^iv	66.94 (8)	O1^xviii—Si1—K1^xix	58.619 (11)
O1^xi—K2—O1^iv	100.89 (10)	O1—Si1—K1^xix	58.620 (11)
O1—K2—O1^xii	142.87 (4)	O1^v—Si1—K1^xix	152.06 (13)
O1^ix—K2—O1^xii	66.94 (8)	O2—Si1—K1^xix	99.67 (4)
O1^x—K2—O1^xii	100.89 (10)	K1^viii—Si1—K1^xix	80.33 (4)
O1^xi—K2—O1^xii	66.94 (8)	K1—Si1—K1^xix	117.24 (2)
O1^iv—K2—O1^xii	142.87 (4)	O1^xviii—Si1—K1^xx	58.620 (11)
O1—K2—O2^xiii	108.57 (2)	O1—Si1—K1^xx	152.06 (13)
O1^ix—K2—O2^xiii	108.57 (2)	O1^v—Si1—K1^xx	58.620 (11)
O1^x—K2—O2^xiii	50.45 (5)	O2—Si1—K1^xx	99.67 (4)
O1^xi—K2—O2^xiii	108.57 (2)	K1^viii—Si1—K1^xx	80.33 (4)
O1^iv—K2—O2^xiii	108.57 (2)	K1—Si1—K1^xx	117.24 (2)
O1^xii—K2—O2^xiii	50.45 (5)	K1^xix—Si1—K1^xx	117.24 (2)
O1—K2—O2	50.45 (5)	O1^xviii—Si1—K2^xx	44.66 (10)
O1^ix—K2—O2	50.45 (5)	O1—Si1—K2^xx	124.38 (4)
O1^x—K2—O2	108.57 (2)	O1^v—Si1—K2^xx	124.38 (4)
O1^xi—K2—O2	108.57 (2)	O2—Si1—K2^xx	63.61 (2)
O1^iv—K2—O2	108.57 (2)	K1^viii—Si1—K2^xx	116.40 (2)
O1^xii—K2—O2	108.57 (2)	K1—Si1—K2^xx	163.28 (6)
O2^xiii—K2—O2	120.0	K1^xix—Si1—K2^xx	68.479 (16)
O1—K2—O2^xiv	108.57 (2)	K1^xx—Si1—K2^xx	68.479 (16)
O1^ix—K2—O2^xiv	108.57 (2)	O1^xviii—Si1—K2^xxi	124.38 (4)
O1^x—K2—O2^xiv	108.57 (2)	O1—Si1—K2^xxi	124.38 (4)
O1^xi—K2—O2^xiv	50.45 (5)	O1^v—Si1—K2^xxi	44.66 (10)
O1^iv—K2—O2^xiv	50.45 (5)	O2—Si1—K2^xxi	63.61 (2)
O1^xii—K2—O2^xiv	108.57 (2)	K1^viii—Si1—K2^xxi	116.39 (2)
O2^xiii—K2—O2^xiv	120.0	K1—Si1—K2^xxi	68.480 (16)
O2—K2—O2^xiv	120.0	K1^xix—Si1—K2^xxi	163.28 (6)
O1—K2—Yb1	39.55 (5)	K1^xx—Si1—K2^xxi	68.480 (16)
O1^ix—K2—Yb1	140.45 (5)	K2^xx—Si1—K2^xxi	101.75 (3)
O1^x—K2—Yb1	39.55 (5)	O1^xviii—Si1—K2	124.38 (4)
O1^xi—K2—Yb1	140.45 (5)	O1—Si1—K2	44.66 (10)
O1^iv—K2—Yb1	39.55 (5)	O1^v—Si1—K2	124.38 (4)
O1^xii—K2—Yb1	140.45 (5)	O2—Si1—K2	63.61 (2)
O2^xiii—K2—Yb1	90.0	K1^viii—Si1—K2	116.39 (2)
O2—K2—Yb1	90.0	K1—Si1—K2	68.480 (16)
O2^xiv—K2—Yb1	90.0	K1^xix—Si1—K2	68.480 (16)
O1—K2—Yb1^xv	140.45 (5)	K1^xx—Si1—K2	163.28 (6)
O1^ix—K2—Yb1^xv	39.55 (5)	K2^xx—Si1—K2	101.75 (3)
O1^x—K2—Yb1^xv	140.45 (5)	K2^xxi—Si1—K2	101.75 (3)
O1^xi—K2—Yb1^xv	39.55 (5)	Si1—O1—Yb1	161.27 (17)
O1^iv—K2—Yb1^xv	140.45 (5)	Si1—O1—K2	111.29 (14)
O1^xii—K2—Yb1^xv	39.55 (5)	Yb1—O1—K2	87.44 (8)
O2^xiii—K2—Yb1^xv	90.0	Si1—O1—K1	92.64 (5)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.39 (5)
O2^xiv—K2—Yb1^xv	90.0	K2—O1—K1	89.36 (6)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.64 (5)
O1—K2—Si1^xiii	86.70 (4)	Yb1—O1—K1^xix	87.39 (5)
O1^ix—K2—Si1^xiii	128.901 (17)	K2—O1—K1^xix	89.36 (6)
O1^x—K2—Si1^xiii	24.05 (6)	K1—O1—K1^xix	174.68 (10)
O1^xi—K2—Si1^xiii	128.900 (17)	Si1—O1—K1^viii	77.88 (12)
O1^iv—K2—Si1^xiii	86.70 (4)	Yb1—O1—K1^viii	83.38 (8)
O1^xii—K2—Si1^xiii	76.84 (6)	K2—O1—K1^viii	170.83 (10)
O2^xiii—K2—Si1^xiii	26.39 (2)	K1—O1—K1^viii	90.22 (6)
O2—K2—Si1^xiii	116.608 (6)	K1^xix—O1—K1^viii	90.22 (6)
O2^xiv—K2—Si1^xiii	116.607 (6)	Si1^ix—O2—Si1	180.0
Yb1—K2—Si1^xiii	63.61 (2)	Si1^ix—O2—K2^xx	90.0
Yb1^xv—K2—Si1^xiii	116.39 (2)	Si1—O2—K2^xx	90.0
O1^xvi—Yb1—O1^xvii	87.52 (10)	Si1^ix—O2—K2	90.0
O1^xvi—Yb1—O1^iv	92.48 (10)	Si1—O2—K2	90.0
O1^xvii—Yb1—O1^iv	180.00 (10)	K2^xx—O2—K2	120.0
O1^xvi—Yb1—O1^vii	87.52 (10)	Si1^ix—O2—K2^xxi	90.0
O1^xvii—Yb1—O1^vii	87.52 (9)	Si1—O2—K2^xxi	90.0
O1^iv—Yb1—O1^vii	92.48 (9)	K2^xx—O2—K2^xxi	120.0
O1^xvi—Yb1—O1^x	92.48 (9)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) −x+y, −x+1, z; (ii) −y+1, x−y+1, z; (iii) x, y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) y, −x+y+1, −z; (vii) x−y, x, −z; (viii) −x+1, −y+1, −z; (ix) x, y, −z+1/2; (x) −x+y, −x, z; (xi) −y, x−y, −z+1/2; (xii) −x+y, −x, −z+1/2; (xiii) x−1, y−1, z; (xiv) x−1, y, z; (xv) −x, −y, z+1/2; (xvi) −x, −y, −z; (xvii) y, −x+y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(beta_prime-K3YbSi2O7)

Crystal data

O7Si2K3Yb	F(000) = 844
Mr = 458.5	Dx = 3.884 Mg m^−3
Orthorhombic, Cmcm	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C -2x;-2yc;-2zc	Cell parameters from 1193 reflections
a = 5.7099 (5) Å	θ = 4.1–29.0°
b = 9.8898 (9) Å	µ = 13.82 mm^−1
c = 13.8867 (14) Å	T = 100 K
V = 784.18 (13) Å^3	Prismatic, colourless
Z = 4	0.28 × 0.09 × 0.08 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	840 reflections with I > 2σ(I)
Radiation source: X-ray tube	Rint = 0.045
ω scans	θmax = 30.0°, θmin = 4.1°
Absorption correction: analytical CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	h = −7→7
Tmin = 0.107, Tmax = 0.444	k = −13→9
2644 measured reflections	l = −14→18
922 independent reflections

Refinement

Refinement on F^2	8 constraints
R[F^2 > 2σ(F^2)] = 0.027	Weighting scheme based on measured s.u.'s w = 1/(σ^2(I) + 0.0004I^2)
wR(F^2) = 0.064	(Δ/σ)max = 0.045
S = 1.14	Δρmax = 1.40 e Å^−3
922 reflections	Δρmin = −0.77 e Å^−3
26 parameters	Extinction correction: B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)
0 restraints	Extinction coefficient: 620 (50)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0	0	0.5	0.00140 (12)
K1	0.5	0.1739 (2)	0.40753 (11)	0.0047 (3)
K2	0	0.0185 (3)	0.25	0.0064 (5)
Si1	0	−0.3385 (3)	0.63224 (13)	0.0017 (4)
O1	0.2658 (8)	−0.0794 (4)	0.3989 (3)	0.0080 (10)*
O2	0	−0.1889 (6)	0.5866 (5)	0.0032 (15)*
O3	0	−0.3156 (9)	0.75	0.0081 (15)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00079 (9)	0.0008 (3)	0.0026 (2)	0	0	0
K1	0.0045 (2)	0.0045 (6)	0.0052 (7)	0	0	0
K2	0.0073 (3)	0.0073 (9)	0.0048 (10)	0	0	0
Si1	0.0016 (3)	0.0016 (8)	0.0019 (8)	0	0	0

Geometric parameters (Å, º)

Yb1—K1^i	3.5716 (13)	K1—O1	2.842 (5)
Yb1—K1	3.5716 (13)	K1—O1^xii	2.876 (5)
Yb1—K1^ii	3.472 (2)	K1—O1^iv	3.144 (4)
Yb1—K1^iii	3.5716 (13)	K1—O1^xv	3.144 (4)
Yb1—K1^iv	3.5716 (13)	K1—O1^xvi	2.842 (5)
Yb1—K1^v	3.472 (2)	K1—O1^xvii	2.876 (5)
Yb1—K2	3.4765 (7)	K1—O2^xii	2.833 (7)
Yb1—K2^vi	3.4765 (7)	K1—O2^iv	2.8600 (6)
Yb1—O1	2.212 (4)	K1—O2^xiii	2.8600 (6)
Yb1—O1^iv	2.212 (4)	K2—Si1^xviii	3.562 (3)
Yb1—O1^vii	2.212 (4)	K2—Si1^iv	3.562 (3)
Yb1—O1^viii	2.212 (4)	K2—O1	2.742 (4)
Yb1—O2	2.222 (6)	K2—O1^xix	2.742 (4)
Yb1—O2^iv	2.222 (6)	K2—O1^xx	2.742 (4)
K1—K1^ix	4.375 (2)	K2—O1^viii	2.742 (4)
K1—K1^iv	4.292 (3)	K2—O2^xviii	2.827 (7)
K1—K1^v	4.1249 (18)	K2—O2^iv	2.827 (7)
K1—K1^x	4.1249 (18)	K2—O3^xviii	2.938 (10)
K1—K2	3.9110 (16)	K2—O3^xxi	3.489 (6)
K1—K2^xi	3.9110 (16)	K2—O3^xxii	3.489 (6)
K1—K2^xii	4.050 (3)	Si1—O1^xxiii	1.623 (5)
K1—Si1^xii	3.123 (2)	Si1—O1^xxiv	1.623 (5)
K1—Si1^iv	3.3326 (18)	Si1—O2	1.609 (7)
K1—Si1^xiii	3.3326 (18)	Si1—O3	1.651 (2)
K1—Si1^xiv	3.363 (3)
K1^i—Yb1—K1	106.14 (4)	K2^xii—K1—O1^xvii	42.56 (9)
K1^i—Yb1—K1^ii	108.32 (3)	K2^xii—K1—O2^xii	94.07 (14)
K1^i—Yb1—K1^iii	73.86 (4)	K2^xii—K1—O2^iv	88.37 (13)
K1^i—Yb1—K1^iv	180	K2^xii—K1—O2^xiii	88.37 (13)
K1^i—Yb1—K1^v	71.68 (3)	Si1^xii—K1—Si1^iv	100.64 (5)
K1^i—Yb1—K2	67.39 (3)	Si1^xii—K1—Si1^xiii	100.64 (5)
K1^i—Yb1—K2^vi	112.61 (3)	Si1^xii—K1—Si1^xiv	97.22 (8)
K1^i—Yb1—O1	119.42 (11)	Si1^xii—K1—O1	90.45 (10)
K1^i—Yb1—O1^iv	127.29 (12)	Si1^xii—K1—O1^xii	94.29 (10)
K1^i—Yb1—O1^vii	60.58 (11)	Si1^xii—K1—O1^xvi	90.45 (10)
K1^i—Yb1—O1^viii	52.71 (12)	Si1^xii—K1—O1^xvii	94.29 (10)
K1^i—Yb1—O2	126.83 (3)	Si1^xii—K1—O2^xii	30.86 (14)
K1^i—Yb1—O2^iv	53.17 (3)	Si1^xii—K1—O2^iv	88.48 (14)
K1—Yb1—K1^ii	108.32 (3)	Si1^xii—K1—O2^xiii	88.48 (14)
K1—Yb1—K1^iii	180	Si1^iv—K1—Si1^xiii	117.89 (8)
K1—Yb1—K1^iv	73.86 (4)	Si1^iv—K1—Si1^xiv	117.04 (5)
K1—Yb1—K1^v	71.68 (3)	Si1^iv—K1—O1	91.17 (10)
K1—Yb1—K2	67.39 (3)	Si1^iv—K1—O1^xii	91.76 (11)
K1—Yb1—K2^vi	112.61 (3)	Si1^iv—K1—O1^xvi	145.75 (11)
K1—Yb1—O1	52.71 (12)	Si1^iv—K1—O1^xvii	29.14 (10)
K1—Yb1—O1^iv	60.58 (11)	Si1^iv—K1—O2^xii	84.92 (8)
K1—Yb1—O1^vii	127.29 (12)	Si1^iv—K1—O2^iv	28.85 (13)
K1—Yb1—O1^viii	119.42 (11)	Si1^iv—K1—O2^xiii	146.56 (15)
K1—Yb1—O2	126.83 (3)	Si1^xiii—K1—Si1^xiv	117.04 (5)
K1—Yb1—O2^iv	53.17 (3)	Si1^xiii—K1—O1	145.75 (11)
K1^ii—Yb1—K1^iii	71.68 (3)	Si1^xiii—K1—O1^xii	29.14 (10)
K1^ii—Yb1—K1^iv	71.68 (3)	Si1^xiii—K1—O1^xvi	91.17 (10)
K1^ii—Yb1—K1^v	180	Si1^xiii—K1—O1^xvii	91.76 (11)
K1^ii—Yb1—K2	71.31 (5)	Si1^xiii—K1—O2^xii	84.92 (8)
K1^ii—Yb1—K2^vi	108.69 (5)	Si1^xiii—K1—O2^iv	146.56 (15)
K1^ii—Yb1—O1	55.61 (12)	Si1^xiii—K1—O2^xiii	28.85 (13)
K1^ii—Yb1—O1^iv	124.39 (12)	Si1^xiv—K1—O1	28.79 (10)
K1^ii—Yb1—O1^vii	124.39 (12)	Si1^xiv—K1—O1^xii	146.10 (10)
K1^ii—Yb1—O1^viii	55.61 (12)	Si1^xiv—K1—O1^xvi	28.79 (10)
K1^ii—Yb1—O2	54.47 (18)	Si1^xiv—K1—O1^xvii	146.10 (10)
K1^ii—Yb1—O2^iv	125.53 (18)	Si1^xiv—K1—O2^xii	128.08 (14)
K1^iii—Yb1—K1^iv	106.14 (4)	Si1^xiv—K1—O2^iv	93.22 (13)
K1^iii—Yb1—K1^v	108.32 (3)	Si1^xiv—K1—O2^xiii	93.22 (13)
K1^iii—Yb1—K2	112.61 (3)	O1—K1—O1^xii	173.87 (13)
K1^iii—Yb1—K2^vi	67.39 (3)	O1—K1—O1^xvi	56.13 (14)
K1^iii—Yb1—O1	127.29 (12)	O1—K1—O1^xvii	119.85 (13)
K1^iii—Yb1—O1^iv	119.42 (11)	O1—K1—O2^xii	117.34 (14)
K1^iii—Yb1—O1^vii	52.71 (12)	O1—K1—O2^iv	65.01 (15)
K1^iii—Yb1—O1^viii	60.58 (11)	O1—K1—O2^xiii	121.12 (17)
K1^iii—Yb1—O2	53.17 (3)	O1^xii—K1—O1^xvi	119.85 (13)
K1^iii—Yb1—O2^iv	126.83 (3)	O1^xii—K1—O1^xvii	63.70 (14)
K1^iv—Yb1—K1^v	108.32 (3)	O1^xii—K1—O2^xii	68.30 (14)
K1^iv—Yb1—K2	112.61 (3)	O1^xii—K1—O2^iv	118.93 (17)
K1^iv—Yb1—K2^vi	67.39 (3)	O1^xii—K1—O2^xiii	55.26 (15)
K1^iv—Yb1—O1	60.58 (11)	O1^xvi—K1—O1^xvii	173.87 (13)
K1^iv—Yb1—O1^iv	52.71 (12)	O1^xvi—K1—O2^xii	117.34 (14)
K1^iv—Yb1—O1^vii	119.42 (11)	O1^xvi—K1—O2^iv	121.12 (17)
K1^iv—Yb1—O1^viii	127.29 (12)	O1^xvi—K1—O2^xiii	65.01 (15)
K1^iv—Yb1—O2	53.17 (3)	O1^xvii—K1—O2^xii	68.30 (14)
K1^iv—Yb1—O2^iv	126.83 (3)	O1^xvii—K1—O2^iv	55.26 (15)
K1^v—Yb1—K2	108.69 (5)	O1^xvii—K1—O2^xiii	118.93 (17)
K1^v—Yb1—K2^vi	71.31 (5)	O2^xii—K1—O2^iv	87.13 (14)
K1^v—Yb1—O1	124.39 (12)	O2^xii—K1—O2^xiii	87.13 (14)
K1^v—Yb1—O1^iv	55.61 (12)	O2^iv—K1—O2^xiii	173.2 (2)
K1^v—Yb1—O1^vii	55.61 (12)	Yb1—K2—Yb1^xviii	173.96 (8)
K1^v—Yb1—O1^viii	124.39 (12)	Yb1—K2—K1^i	57.46 (2)
K1^v—Yb1—O2	125.53 (18)	Yb1—K2—K1	57.46 (2)
K1^v—Yb1—O2^iv	54.47 (18)	Yb1—K2—K1^ii	54.29 (3)
K2—Yb1—K2^vi	180	Yb1—K2—K1^xix	125.40 (3)
K2—Yb1—O1	52.03 (11)	Yb1—K2—K1^ix	125.40 (3)
K2—Yb1—O1^iv	127.97 (11)	Yb1—K2—K1^xxv	119.67 (7)
K2—Yb1—O1^vii	127.97 (11)	Yb1—K2—Si1^xviii	120.35 (7)
K2—Yb1—O1^viii	52.03 (11)	Yb1—K2—Si1^iv	65.69 (4)
K2—Yb1—O2	125.78 (18)	Yb1—K2—O1	39.50 (9)
K2—Yb1—O2^iv	54.22 (18)	Yb1—K2—O1^xix	137.26 (10)
K2^vi—Yb1—O1	127.97 (11)	Yb1—K2—O1^xx	137.26 (10)
K2^vi—Yb1—O1^iv	52.03 (11)	Yb1—K2—O1^viii	39.50 (9)
K2^vi—Yb1—O1^vii	52.03 (11)	Yb1—K2—O2^xviii	146.42 (15)
K2^vi—Yb1—O1^viii	127.97 (11)	Yb1—K2—O2^iv	39.62 (13)
K2^vi—Yb1—O2	54.22 (18)	Yb1^xviii—K2—K1^i	125.40 (3)
K2^vi—Yb1—O2^iv	125.78 (18)	Yb1^xviii—K2—K1	125.40 (3)
O1—Yb1—O1^iv	93.34 (16)	Yb1^xviii—K2—K1^ii	119.67 (7)
O1—Yb1—O1^vii	180	Yb1^xviii—K2—K1^xix	57.46 (2)
O1—Yb1—O1^viii	86.66 (16)	Yb1^xviii—K2—K1^ix	57.46 (2)
O1—Yb1—O2	92.58 (17)	Yb1^xviii—K2—K1^xxv	54.29 (3)
O1—Yb1—O2^iv	87.42 (17)	Yb1^xviii—K2—Si1^xviii	65.69 (4)
O1^iv—Yb1—O1^vii	86.66 (16)	Yb1^xviii—K2—Si1^iv	120.35 (7)
O1^iv—Yb1—O1^viii	180	Yb1^xviii—K2—O1	137.26 (10)
O1^iv—Yb1—O2	87.42 (17)	Yb1^xviii—K2—O1^xix	39.50 (9)
O1^iv—Yb1—O2^iv	92.58 (17)	Yb1^xviii—K2—O1^xx	39.50 (9)
O1^vii—Yb1—O1^viii	93.34 (16)	Yb1^xviii—K2—O1^viii	137.26 (10)
O1^vii—Yb1—O2	87.42 (17)	Yb1^xviii—K2—O2^xviii	39.62 (13)
O1^vii—Yb1—O2^iv	92.58 (17)	Yb1^xviii—K2—O2^iv	146.42 (15)
O1^viii—Yb1—O2	92.58 (17)	K1^i—K2—K1	93.77 (4)
O1^viii—Yb1—O2^iv	87.42 (17)	K1^i—K2—K1^ii	91.63 (4)
O2—Yb1—O2^iv	180	K1^i—K2—K1^xix	68.02 (4)
Yb1—K1—Yb1^xi	106.14 (5)	K1^i—K2—K1^ix	133.74 (8)
Yb1—K1—Yb1^xii	108.32 (3)	K1^i—K2—K1^xxv	129.25 (4)
Yb1—K1—K1^ix	111.07 (3)	K1^i—K2—Si1^xviii	84.71 (6)
Yb1—K1—K1^iv	53.07 (3)	K1^i—K2—Si1^iv	52.72 (4)
Yb1—K1—K1^v	53.03 (3)	K1^i—K2—O1	96.96 (9)
Yb1—K1—K1^x	120.34 (4)	K1^i—K2—O1^xix	99.00 (10)
Yb1—K1—K2	55.14 (2)	K1^i—K2—O1^xx	164.73 (10)
Yb1—K1—K2^xi	126.55 (7)	K1^i—K2—O1^viii	46.60 (10)
Yb1—K1—K2^xii	126.82 (3)	K1^i—K2—O2^xviii	102.41 (11)
Yb1—K1—Si1^xii	67.79 (4)	K1^i—K2—O2^iv	46.90 (3)
Yb1—K1—Si1^iv	67.04 (4)	K1—K2—K1^ii	91.63 (4)
Yb1—K1—Si1^xiii	168.39 (6)	K1—K2—K1^xix	133.74 (8)
Yb1—K1—Si1^xiv	65.43 (4)	K1—K2—K1^ix	68.02 (4)
Yb1—K1—O1	38.26 (9)	K1—K2—K1^xxv	129.25 (4)
Yb1—K1—O1^xii	147.70 (10)	K1—K2—Si1^xviii	84.71 (6)
Yb1—K1—O1^xvi	88.11 (11)	K1—K2—Si1^iv	52.72 (4)
Yb1—K1—O1^xvii	90.09 (9)	K1—K2—O1	46.60 (10)
Yb1—K1—O2^xii	85.13 (8)	K1—K2—O1^xix	164.73 (10)
Yb1—K1—O2^iv	38.45 (13)	K1—K2—O1^xx	99.00 (10)
Yb1—K1—O2^xiii	144.37 (14)	K1—K2—O1^viii	96.96 (9)
Yb1^xi—K1—Yb1^xii	108.32 (3)	K1—K2—O2^xviii	102.41 (11)
Yb1^xi—K1—K1^ix	111.07 (3)	K1—K2—O2^iv	46.90 (3)
Yb1^xi—K1—K1^iv	53.07 (3)	K1^ii—K2—K1^xix	129.25 (4)
Yb1^xi—K1—K1^v	120.34 (4)	K1^ii—K2—K1^ix	129.25 (4)
Yb1^xi—K1—K1^x	53.03 (3)	K1^ii—K2—K1^xxv	65.38 (5)
Yb1^xi—K1—K2	126.55 (7)	K1^ii—K2—Si1^xviii	174.64 (6)
Yb1^xi—K1—K2^xi	55.14 (2)	K1^ii—K2—Si1^iv	119.98 (4)
Yb1^xi—K1—K2^xii	126.82 (3)	K1^ii—K2—O1	45.20 (10)
Yb1^xi—K1—Si1^xii	67.79 (4)	K1^ii—K2—O1^xix	96.31 (11)
Yb1^xi—K1—Si1^iv	168.39 (6)	K1^ii—K2—O1^xx	96.31 (11)
Yb1^xi—K1—Si1^xiii	67.04 (4)	K1^ii—K2—O1^viii	45.20 (10)
Yb1^xi—K1—Si1^xiv	65.43 (4)	K1^ii—K2—O2^xviii	159.29 (15)
Yb1^xi—K1—O1	88.11 (11)	K1^ii—K2—O2^iv	93.91 (13)
Yb1^xi—K1—O1^xii	90.09 (9)	K1^xix—K2—K1^ix	93.77 (4)
Yb1^xi—K1—O1^xvi	38.26 (9)	K1^xix—K2—K1^xxv	91.63 (4)
Yb1^xi—K1—O1^xvii	147.70 (10)	K1^xix—K2—Si1^xviii	52.72 (4)
Yb1^xi—K1—O2^xii	85.13 (8)	K1^xix—K2—Si1^iv	84.71 (6)
Yb1^xi—K1—O2^iv	144.37 (14)	K1^xix—K2—O1	164.73 (10)
Yb1^xi—K1—O2^xiii	38.45 (13)	K1^xix—K2—O1^xix	46.60 (10)
Yb1^xii—K1—K1^ix	111.71 (6)	K1^xix—K2—O1^xx	96.96 (9)
Yb1^xii—K1—K1^iv	121.54 (5)	K1^xix—K2—O1^viii	99.00 (10)
Yb1^xii—K1—K1^v	55.28 (4)	K1^xix—K2—O2^xviii	46.90 (3)
Yb1^xii—K1—K1^x	55.28 (4)	K1^xix—K2—O2^iv	102.41 (11)
Yb1^xii—K1—K2	124.88 (5)	K1^ix—K2—K1^xxv	91.63 (4)
Yb1^xii—K1—K2^xi	124.88 (5)	K1^ix—K2—Si1^xviii	52.72 (4)
Yb1^xii—K1—K2^xii	54.40 (4)	K1^ix—K2—Si1^iv	84.71 (6)
Yb1^xii—K1—Si1^xii	70.53 (6)	K1^ix—K2—O1	99.00 (10)
Yb1^xii—K1—Si1^iv	66.89 (5)	K1^ix—K2—O1^xix	96.96 (9)
Yb1^xii—K1—Si1^xiii	66.89 (5)	K1^ix—K2—O1^xx	46.60 (10)
Yb1^xii—K1—Si1^xiv	167.74 (6)	K1^ix—K2—O1^viii	164.73 (10)
Yb1^xii—K1—O1	146.57 (10)	K1^ix—K2—O2^xviii	46.90 (3)
Yb1^xii—K1—O1^xii	39.40 (9)	K1^ix—K2—O2^iv	102.41 (11)
Yb1^xii—K1—O1^xvi	146.57 (10)	K1^xxv—K2—Si1^xviii	119.98 (4)
Yb1^xii—K1—O1^xvii	39.40 (9)	K1^xxv—K2—Si1^iv	174.64 (6)
Yb1^xii—K1—O2^xii	39.67 (13)	K1^xxv—K2—O1	96.31 (11)
Yb1^xii—K1—O2^iv	86.62 (13)	K1^xxv—K2—O1^xix	45.20 (10)
Yb1^xii—K1—O2^xiii	86.62 (13)	K1^xxv—K2—O1^xx	45.20 (10)
K1^ix—K1—K1^iv	126.75 (6)	K1^xxv—K2—O1^viii	96.31 (11)
K1^ix—K1—K1^v	128.51 (4)	K1^xxv—K2—O2^xviii	93.91 (13)
K1^ix—K1—K1^x	128.51 (4)	K1^xxv—K2—O2^iv	159.29 (15)
K1^ix—K1—K2	55.99 (3)	Si1^xviii—K2—Si1^iv	54.66 (6)
K1^ix—K1—K2^xi	55.99 (3)	Si1^xviii—K2—O1	131.31 (11)
K1^ix—K1—K2^xii	57.31 (4)	Si1^xviii—K2—O1^xix	88.15 (10)
K1^ix—K1—Si1^xii	177.76 (9)	Si1^xviii—K2—O1^xx	88.15 (10)
K1^ix—K1—Si1^iv	80.46 (4)	Si1^xviii—K2—O1^viii	131.31 (11)
K1^ix—K1—Si1^xiii	80.46 (4)	Si1^xviii—K2—O2^xviii	26.07 (14)
K1^ix—K1—Si1^xiv	80.55 (5)	Si1^xviii—K2—O2^iv	80.73 (15)
K1^ix—K1—O1	87.58 (9)	Si1^iv—K2—O1	88.15 (10)
K1^ix—K1—O1^xii	87.61 (9)	Si1^iv—K2—O1^xix	131.31 (11)
K1^ix—K1—O1^xvi	87.58 (9)	Si1^iv—K2—O1^xx	131.31 (11)
K1^ix—K1—O1^xvii	87.61 (9)	Si1^iv—K2—O1^viii	88.15 (10)
K1^ix—K1—O2^xii	151.38 (15)	Si1^iv—K2—O2^xviii	80.73 (15)
K1^ix—K1—O2^iv	91.64 (14)	Si1^iv—K2—O2^iv	26.07 (14)
K1^ix—K1—O2^xiii	91.64 (14)	O1—K2—O1^xix	138.62 (16)
K1^iv—K1—K1^v	85.41 (4)	O1—K2—O1^xx	97.89 (14)
K1^iv—K1—K1^x	85.41 (4)	O1—K2—O1^viii	67.23 (14)
K1^iv—K1—K2	91.15 (5)	O1—K2—O2^xviii	144.69 (11)
K1^iv—K1—K2^xi	91.15 (5)	O1—K2—O2^iv	66.75 (14)
K1^iv—K1—K2^xii	175.94 (6)	O1^xix—K2—O1^xx	67.23 (14)
K1^iv—K1—Si1^xii	51.01 (6)	O1^xix—K2—O1^viii	97.89 (14)
K1^iv—K1—Si1^iv	119.38 (4)	O1^xix—K2—O2^xviii	66.75 (14)
K1^iv—K1—Si1^xiii	119.38 (4)	O1^xix—K2—O2^iv	144.69 (11)
K1^iv—K1—Si1^xiv	46.21 (5)	O1^xx—K2—O1^viii	138.62 (16)
K1^iv—K1—O1	47.09 (9)	O1^xx—K2—O2^xviii	66.75 (14)
K1^iv—K1—O1^xii	134.81 (9)	O1^xx—K2—O2^iv	144.69 (11)
K1^iv—K1—O1^xvi	47.09 (9)	O1^viii—K2—O2^xviii	144.69 (11)
K1^iv—K1—O1^xvii	134.81 (9)	O1^viii—K2—O2^iv	66.75 (14)
K1^iv—K1—O2^xii	81.87 (13)	O2^xviii—K2—O2^iv	106.8 (2)
K1^iv—K1—O2^iv	91.41 (13)	K1^ii—Si1—K1^iii	79.36 (5)
K1^iv—K1—O2^xiii	91.41 (13)	K1^ii—Si1—K1^iv	79.36 (5)
K1^v—K1—K1^x	87.60 (4)	K1^ii—Si1—K1^xxiii	82.78 (7)
K1^v—K1—K2	89.22 (2)	K1^ii—Si1—K2^vi	115.09 (8)
K1^v—K1—K2^xi	175.49 (5)	K1^ii—Si1—O1^xxiii	75.73 (16)
K1^v—K1—K2^xii	91.66 (5)	K1^ii—Si1—O1^xxiv	75.73 (16)
K1^v—K1—Si1^xii	52.56 (4)	K1^ii—Si1—O2	64.6 (3)
K1^v—K1—Si1^iv	48.08 (4)	K1^ii—Si1—O3	169.9 (4)
K1^v—K1—Si1^xiii	121.18 (7)	K1^iii—Si1—K1^iv	117.89 (9)
K1^v—K1—Si1^xiv	117.54 (5)	K1^iii—Si1—K1^xxiii	117.04 (5)
K1^v—K1—O1	91.29 (10)	K1^iii—Si1—K2^vi	69.03 (5)
K1^v—K1—O1^xii	94.67 (10)	K1^iii—Si1—O1^xxiii	59.63 (16)
K1^v—K1—O1^xvi	132.36 (10)	K1^iii—Si1—O1^xxiv	154.97 (17)
K1^v—K1—O1^xvii	49.53 (9)	K1^iii—Si1—O2	59.05 (5)
K1^v—K1—O2^xii	43.83 (2)	K1^iii—Si1—O3	95.59 (18)
K1^v—K1—O2^iv	43.31 (14)	K1^iv—Si1—K1^xxiii	117.04 (5)
K1^v—K1—O2^xiii	130.85 (15)	K1^iv—Si1—K2^vi	69.03 (5)
K1^x—K1—K2	175.49 (5)	K1^iv—Si1—O1^xxiii	154.97 (17)
K1^x—K1—K2^xi	89.22 (2)	K1^iv—Si1—O1^xxiv	59.63 (16)
K1^x—K1—K2^xii	91.66 (5)	K1^iv—Si1—O2	59.05 (5)
K1^x—K1—Si1^xii	52.56 (4)	K1^iv—Si1—O3	95.59 (18)
K1^x—K1—Si1^iv	121.18 (7)	K1^xxiii—Si1—K2^vi	162.12 (7)
K1^x—K1—Si1^xiii	48.08 (4)	K1^xxiii—Si1—O1^xxiii	57.50 (17)
K1^x—K1—Si1^xiv	117.54 (5)	K1^xxiii—Si1—O1^xxiv	57.50 (17)
K1^x—K1—O1	132.36 (10)	K1^xxiii—Si1—O2	147.3 (3)
K1^x—K1—O1^xii	49.53 (9)	K1^xxiii—Si1—O3	107.3 (3)
K1^x—K1—O1^xvi	91.29 (10)	K2^vi—Si1—O1^xxiii	124.52 (17)
K1^x—K1—O1^xvii	94.67 (10)	K2^vi—Si1—O1^xxiv	124.52 (17)
K1^x—K1—O2^xii	43.83 (2)	K2^vi—Si1—O2	50.5 (3)
K1^x—K1—O2^iv	130.85 (15)	K2^vi—Si1—O3	54.8 (3)
K1^x—K1—O2^xiii	43.31 (14)	O1^xxiii—Si1—O1^xxiv	111.0 (3)
K2—K1—K2^xi	93.77 (4)	O1^xxiii—Si1—O2	110.8 (2)
K2—K1—K2^xii	91.63 (4)	O1^xxiii—Si1—O3	109.4 (2)
K2—K1—Si1^xii	122.93 (4)	O1^xxiv—Si1—O2	110.8 (2)
K2—K1—Si1^iv	58.25 (5)	O1^xxiv—Si1—O3	109.4 (2)
K2—K1—Si1^xiii	136.43 (6)	O2—Si1—O3	105.3 (4)
K2—K1—Si1^xiv	61.36 (5)	Yb1—O1—K1	89.03 (14)
K2—K1—O1	44.50 (9)	Yb1—O1—K1^ii	84.99 (15)
K2—K1—O1^xii	134.04 (10)	Yb1—O1—K2	88.48 (15)
K2—K1—O1^xvi	88.49 (11)	Yb1—O1—Si1^xiv	155.8 (3)
K2—K1—O1^xvii	85.68 (10)	K1—O1—K1^ii	173.87 (18)
K2—K1—O2^xii	132.78 (2)	K1—O1—K2	88.91 (13)
K2—K1—O2^iv	46.19 (14)	K1—O1—Si1^xiv	93.7 (2)
K2—K1—O2^xiii	139.92 (15)	K1^ii—O1—K2	92.24 (14)
K2^xi—K1—K2^xii	91.63 (4)	K1^ii—O1—Si1^xiv	91.23 (19)
K2^xi—K1—Si1^xii	122.93 (4)	K2—O1—Si1^xiv	115.6 (2)
K2^xi—K1—Si1^iv	136.43 (6)	Yb1—O2—K1^ii	85.9 (2)
K2^xi—K1—Si1^xiii	58.25 (5)	Yb1—O2—K1^iii	88.37 (13)
K2^xi—K1—Si1^xiv	61.36 (5)	Yb1—O2—K1^iv	88.37 (13)
K2^xi—K1—O1	88.49 (11)	Yb1—O2—K2^vi	86.2 (2)
K2^xi—K1—O1^xii	85.68 (10)	Yb1—O2—Si1	170.4 (4)
K2^xi—K1—O1^xvi	44.50 (9)	K1^ii—O2—K1^iii	92.87 (14)
K2^xi—K1—O1^xvii	134.04 (10)	K1^ii—O2—K1^iv	92.87 (14)
K2^xi—K1—O2^xii	132.78 (2)	K1^ii—O2—K2^vi	172.0 (3)
K2^xi—K1—O2^iv	139.92 (15)	K1^ii—O2—Si1	84.6 (3)
K2^xi—K1—O2^xiii	46.19 (14)	K1^iii—O2—K1^iv	173.2 (3)
K2^xii—K1—Si1^xii	124.93 (8)	K1^iii—O2—K2^vi	86.90 (14)
K2^xii—K1—Si1^iv	59.96 (5)	K1^iii—O2—Si1	92.10 (13)
K2^xii—K1—Si1^xiii	59.96 (5)	K1^iv—O2—K2^vi	86.90 (14)
K2^xii—K1—Si1^xiv	137.86 (6)	K1^iv—O2—Si1	92.10 (13)
K2^xii—K1—O1	135.97 (9)	K2^vi—O2—Si1	103.4 (3)
K2^xii—K1—O1^xii	42.56 (9)	Si1—O3—Si1^xxvi	164.3 (7)
K2^xii—K1—O1^xvi	135.97 (9)

Symmetry codes: (i) x−1, y, z; (ii) x−1/2, y−1/2, z; (iii) x−1, −y, −z+1; (iv) x, −y, −z+1; (v) x−1/2, −y+1/2, −z+1; (vi) −x, −y, z+1/2; (vii) −x, −y, −z+1; (viii) −x, y, z; (ix) −x+1, y, −z+1/2; (x) x+1/2, −y+1/2, −z+1; (xi) x+1, y, z; (xii) x+1/2, y+1/2, z; (xiii) x+1, −y, −z+1; (xiv) x+1/2, −y−1/2, −z+1; (xv) −x+1, −y, −z+1; (xvi) −x+1, y, z; (xvii) −x+1/2, y+1/2, z; (xviii) −x, −y, z−1/2; (xix) −x, y, −z+1/2; (xx) x, y, −z+1/2; (xxi) −x−1/2, −y−1/2, z−1/2; (xxii) −x+1/2, −y−1/2, z−1/2; (xxiii) x−1/2, −y−1/2, −z+1; (xxiv) −x+1/2, −y−1/2, −z+1; (xxv) −x+1/2, y−1/2, −z+1/2; (xxvi) −x, y, −z+3/2.

(93_K)

Crystal data

K3O7Si2Yb	Dx = 3.896 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1225 reflections
a = 5.7059 (5) Å	θ = 4.4–29.2°
b = 9.8800 (8) Å	µ = 13.87 mm^−1
c = 13.8658 (11) Å	T = 95 K
V = 781.67 (11) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	479 reflections with I > 2σ(I)
ω scans	Rint = 0.040
Absorption correction: analytical CrysAlisPro 1.171.40.76a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 4.1°
Tmin = 0.306, Tmax = 0.398	h = −5→7
2641 measured reflections	k = −12→12
538 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + 7.4861P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.022	(Δ/σ)max < 0.001
wR(F^2) = 0.043	Δρmax = 1.10 e Å^−3
S = 1.12	Δρmin = −1.14 e Å^−3
538 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
29 parameters	Extinction coefficient: 0.00251 (13)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00124 (16)
K1	0.500000	0.1737 (3)	0.40748 (12)	0.0047 (3)
K2	0.000000	0.0187 (3)	0.250000	0.0056 (6)
Si1	0.000000	−0.3388 (4)	0.63220 (15)	0.0012 (4)
O1	0.2659 (12)	−0.0797 (6)	0.3986 (4)	0.0084 (13)
O2	0.000000	−0.1889 (8)	0.5865 (7)	0.001 (2)
O3	0.000000	−0.3169 (14)	0.750000	0.009 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00094 (17)	0.00094 (17)	0.0018 (2)	0.000	0.000	0.000
K1	0.0047 (5)	0.0047 (5)	0.0048 (7)	0.000	0.000	0.000
K2	0.0069 (8)	0.0069 (8)	0.0030 (9)	0.000	0.000	0.000
Si1	0.0007 (6)	0.0007 (6)	0.0021 (8)	0.000	0.000	0.000
O1	0.006 (4)	0.003 (3)	0.017 (3)	0.000	0.000	0.000
O2	0.001 (2)	0.001 (2)	0.001 (2)	0.000	0.000	0.000
O3	0.012 (3)	0.012 (3)	0.003 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O1	2.213 (5)	K1—Si1^vii	3.118 (3)
Yb1—O1^i	2.213 (5)	K1—O1^ix	3.143 (6)
Yb1—O1^ii	2.213 (5)	K1—O1^ii	3.143 (6)
Yb1—O1^iii	2.213 (5)	K1—Si1^ix	3.332 (3)
Yb1—O2	2.218 (8)	K1—Si1^iii	3.332 (3)
Yb1—O2^iii	2.218 (8)	K2—O1	2.737 (5)
Yb1—K1^iv	3.470 (3)	K2—O1^xi	2.737 (5)
Yb1—K1^v	3.470 (3)	K2—O1^xii	2.737 (5)
Yb1—K2	3.4714 (3)	K2—O1^i	2.737 (5)
Yb1—K2^iii	3.4714 (3)	K2—O2^iii	2.822 (10)
Yb1—K1^iii	3.5677 (18)	K2—O2^xiii	2.822 (10)
Yb1—K1^vi	3.5677 (18)	K2—O3^iii	2.946 (15)
K1—O2^vii	2.830 (9)	K2—Si1^iii	3.559 (5)
K1—O1	2.840 (9)	K2—Si1^xiii	3.559 (5)
K1—O1^viii	2.840 (9)	K2—Si1^xiv	3.737 (3)
K1—O2^ix	2.8581 (6)	Si1—O2	1.611 (9)
K1—O2^iii	2.8581 (6)	Si1—O1^xv	1.617 (6)
K1—O1^vii	2.873 (9)	Si1—O1^xvi	1.617 (6)
K1—O1^x	2.873 (9)	Si1—O3	1.648 (3)
O1—Yb1—O1^i	86.5 (4)	O1^xi—K2—O2^xiii	66.86 (14)
O1—Yb1—O1^ii	93.5 (4)	O1^xii—K2—O2^xiii	66.86 (14)
O1^i—Yb1—O1^ii	180.0	O1^i—K2—O2^xiii	144.72 (16)
O1—Yb1—O1^iii	180.0 (2)	O2^iii—K2—O2^xiii	106.9 (4)
O1^i—Yb1—O1^iii	93.5 (4)	O1—K2—O3^iii	110.82 (14)
O1^ii—Yb1—O1^iii	86.5 (4)	O1^xi—K2—O3^iii	110.82 (14)
O1—Yb1—O2	92.5 (2)	O1^xii—K2—O3^iii	110.82 (14)
O1^i—Yb1—O2	92.5 (2)	O1^i—K2—O3^iii	110.82 (14)
O1^ii—Yb1—O2	87.5 (2)	O2^iii—K2—O3^iii	53.45 (18)
O1^iii—Yb1—O2	87.5 (2)	O2^xiii—K2—O3^iii	53.45 (18)
O1—Yb1—O2^iii	87.5 (2)	O1—K2—Yb1^xiii	137.11 (12)
O1^i—Yb1—O2^iii	87.5 (2)	O1^xi—K2—Yb1^xiii	39.59 (11)
O1^ii—Yb1—O2^iii	92.5 (2)	O1^xii—K2—Yb1^xiii	39.59 (11)
O1^iii—Yb1—O2^iii	92.5 (2)	O1^i—K2—Yb1^xiii	137.11 (12)
O2—Yb1—O2^iii	180.0	O2^iii—K2—Yb1^xiii	146.5 (2)
O1—Yb1—K1^iv	55.56 (19)	O2^xiii—K2—Yb1^xiii	39.61 (17)
O1^i—Yb1—K1^iv	55.56 (19)	O3^iii—K2—Yb1^xiii	93.06 (6)
O1^ii—Yb1—K1^iv	124.44 (19)	O1—K2—Yb1	39.59 (11)
O1^iii—Yb1—K1^iv	124.4 (2)	O1^xi—K2—Yb1	137.11 (12)
O2—Yb1—K1^iv	54.4 (2)	O1^xii—K2—Yb1	137.11 (12)
O2^iii—Yb1—K1^iv	125.6 (2)	O1^i—K2—Yb1	39.59 (11)
O1—Yb1—K1^v	124.44 (19)	O2^iii—K2—Yb1	39.61 (17)
O1^i—Yb1—K1^v	124.44 (19)	O2^xiii—K2—Yb1	146.5 (2)
O1^ii—Yb1—K1^v	55.56 (19)	O3^iii—K2—Yb1	93.06 (6)
O1^iii—Yb1—K1^v	55.56 (19)	Yb1^xiii—K2—Yb1	173.88 (11)
O2—Yb1—K1^v	125.6 (2)	O1—K2—Si1^iii	88.30 (13)
O2^iii—Yb1—K1^v	54.4 (2)	O1^xi—K2—Si1^iii	131.39 (17)
K1^iv—Yb1—K1^v	180.00 (5)	O1^xii—K2—Si1^iii	131.39 (17)
O1—Yb1—K2	52.02 (14)	O1^i—K2—Si1^iii	88.30 (13)
O1^i—Yb1—K2	52.02 (14)	O2^iii—K2—Si1^iii	26.13 (18)
O1^ii—Yb1—K2	127.98 (14)	O2^xiii—K2—Si1^iii	80.77 (19)
O1^iii—Yb1—K2	127.98 (14)	O3^iii—K2—Si1^iii	27.32 (5)
O2—Yb1—K2	125.8 (3)	Yb1^xiii—K2—Si1^iii	120.38 (10)
O2^iii—Yb1—K2	54.2 (3)	Yb1—K2—Si1^iii	65.74 (5)
K1^iv—Yb1—K2	71.36 (7)	O1—K2—Si1^xiii	131.39 (17)
K1^v—Yb1—K2	108.64 (7)	O1^xi—K2—Si1^xiii	88.30 (13)
O1—Yb1—K2^iii	127.98 (14)	O1^xii—K2—Si1^xiii	88.30 (13)
O1^i—Yb1—K2^iii	127.98 (14)	O1^i—K2—Si1^xiii	131.39 (17)
O1^ii—Yb1—K2^iii	52.02 (14)	O2^iii—K2—Si1^xiii	80.77 (19)
O1^iii—Yb1—K2^iii	52.02 (14)	O2^xiii—K2—Si1^xiii	26.13 (18)
O2—Yb1—K2^iii	54.2 (3)	O3^iii—K2—Si1^xiii	27.32 (5)
O2^iii—Yb1—K2^iii	125.8 (3)	Yb1^xiii—K2—Si1^xiii	65.74 (5)
K1^iv—Yb1—K2^iii	108.64 (7)	Yb1—K2—Si1^xiii	120.38 (10)
K1^v—Yb1—K2^iii	71.36 (7)	Si1^iii—K2—Si1^xiii	54.64 (10)
K2—Yb1—K2^iii	180.0	O1—K2—Si1^xiv	125.66 (19)
O1—Yb1—K1^iii	127.3 (2)	O1^xi—K2—Si1^xiv	22.92 (11)
O1^i—Yb1—K1^iii	60.61 (14)	O1^xii—K2—Si1^xiv	85.70 (16)
O1^ii—Yb1—K1^iii	119.39 (14)	O1^i—K2—Si1^xiv	74.74 (12)
O1^iii—Yb1—K1^iii	52.7 (2)	O2^iii—K2—Si1^xiv	129.37 (5)
O2—Yb1—K1^iii	53.20 (4)	O2^xiii—K2—Si1^xiv	86.11 (12)
O2^iii—Yb1—K1^iii	126.80 (4)	O3^iii—K2—Si1^xiv	118.40 (8)
K1^iv—Yb1—K1^iii	71.70 (4)	Yb1^xiii—K2—Si1^xiv	62.50 (4)
K1^v—Yb1—K1^iii	108.30 (4)	Yb1—K2—Si1^xiv	114.27 (6)
K2—Yb1—K1^iii	112.62 (4)	Si1^iii—K2—Si1^xiv	128.55 (8)
K2^iii—Yb1—K1^iii	67.38 (4)	Si1^xiii—K2—Si1^xiv	102.83 (6)
O1—Yb1—K1^vi	119.39 (14)	O2—Si1—O1^xv	110.7 (3)
O1^i—Yb1—K1^vi	52.7 (2)	O2—Si1—O1^xvi	110.7 (3)
O1^ii—Yb1—K1^vi	127.3 (2)	O1^xv—Si1—O1^xvi	111.4 (6)
O1^iii—Yb1—K1^vi	60.61 (14)	O2—Si1—O3	105.6 (7)
O2—Yb1—K1^vi	126.80 (4)	O1^xv—Si1—O3	109.1 (3)
O2^iii—Yb1—K1^vi	53.20 (4)	O1^xvi—Si1—O3	109.1 (3)
K1^iv—Yb1—K1^vi	108.30 (4)	O2—Si1—K1^iv	64.6 (4)
K1^v—Yb1—K1^vi	71.70 (4)	O1^xv—Si1—K1^iv	75.9 (2)
K2—Yb1—K1^vi	67.38 (4)	O1^xvi—Si1—K1^iv	75.9 (2)
K2^iii—Yb1—K1^vi	112.62 (4)	O3—Si1—K1^iv	170.2 (5)
K1^iii—Yb1—K1^vi	73.81 (8)	O2—Si1—K1^ix	59.00 (9)
O2^vii—K1—O1	117.5 (2)	O1^xv—Si1—K1^ix	155.2 (2)
O2^vii—K1—O1^viii	117.5 (2)	O1^xvi—Si1—K1^ix	59.5 (3)
O1—K1—O1^viii	56.1 (2)	O3—Si1—K1^ix	95.7 (3)
O2^vii—K1—O2^ix	87.08 (19)	K1^iv—Si1—K1^ix	79.38 (5)
O1—K1—O2^ix	121.1 (2)	O2—Si1—K1^iii	59.00 (9)
O1^viii—K1—O2^ix	65.04 (16)	O1^xv—Si1—K1^iii	59.5 (3)
O2^vii—K1—O2^iii	87.08 (19)	O1^xvi—Si1—K1^iii	155.2 (2)
O1—K1—O2^iii	65.04 (16)	O3—Si1—K1^iii	95.7 (3)
O1^viii—K1—O2^iii	121.1 (2)	K1^iv—Si1—K1^iii	79.38 (5)
O2^ix—K1—O2^iii	173.1 (4)	K1^ix—Si1—K1^iii	117.78 (18)
O2^vii—K1—O1^vii	68.32 (14)	O2—Si1—K1^xvi	147.4 (3)
O1—K1—O1^vii	173.7 (2)	O1^xv—Si1—K1^xvi	57.7 (3)
O1^viii—K1—O1^vii	119.82 (2)	O1^xvi—Si1—K1^xvi	57.7 (3)
O2^ix—K1—O1^vii	55.22 (16)	O3—Si1—K1^xvi	107.0 (5)
O2^iii—K1—O1^vii	118.9 (2)	K1^iv—Si1—K1^xvi	82.82 (8)
O2^vii—K1—O1^x	68.32 (14)	K1^ix—Si1—K1^xvi	117.12 (9)
O1—K1—O1^x	119.82 (2)	K1^iii—Si1—K1^xvi	117.12 (9)
O1^viii—K1—O1^x	173.7 (2)	O2—Si1—K2^iii	50.5 (3)
O2^ix—K1—O1^x	118.9 (2)	O1^xv—Si1—K2^iii	124.3 (3)
O2^iii—K1—O1^x	55.22 (16)	O1^xvi—Si1—K2^iii	124.3 (3)
O1^vii—K1—O1^x	63.7 (2)	O3—Si1—K2^iii	55.1 (5)
O2^vii—K1—Si1^vii	30.95 (18)	K1^iv—Si1—K2^iii	115.06 (11)
O1—K1—Si1^vii	90.49 (13)	K1^ix—Si1—K2^iii	68.95 (9)
O1^viii—K1—Si1^vii	90.49 (13)	K1^iii—Si1—K2^iii	68.95 (10)
O2^ix—K1—Si1^vii	88.45 (19)	K1^xvi—Si1—K2^iii	162.12 (8)
O2^iii—K1—Si1^vii	88.45 (19)	O2—Si1—K2^xvii	127.54 (11)
O1^vii—K1—Si1^vii	94.38 (13)	O1^xv—Si1—K2^xvii	41.23 (19)
O1^x—K1—Si1^vii	94.38 (13)	O1^xvi—Si1—K2^xvii	120.6 (3)
O2^vii—K1—O1^ix	52.50 (14)	O3—Si1—K2^xvii	68.2 (3)
O1—K1—O1^ix	88.67 (19)	K1^iv—Si1—K2^xvii	117.10 (6)
O1^viii—K1—O1^ix	64.97 (17)	K1^ix—Si1—K2^xvii	163.46 (6)
O2^ix—K1—O1^ix	64.3 (2)	K1^iii—Si1—K2^xvii	69.61 (6)
O2^iii—K1—O1^ix	114.5 (2)	K1^xvi—Si1—K2^xvii	66.57 (8)
O1^vii—K1—O1^ix	93.60 (15)	K2^iii—Si1—K2^xvii	102.83 (6)
O1^x—K1—O1^ix	120.77 (11)	O2—Si1—K2^xvi	127.54 (11)
Si1^vii—K1—O1^ix	29.93 (10)	O1^xv—Si1—K2^xvi	120.6 (3)
O2^vii—K1—O1^ii	52.50 (14)	O1^xvi—Si1—K2^xvi	41.23 (19)
O1—K1—O1^ii	64.97 (17)	O3—Si1—K2^xvi	68.2 (3)
O1^viii—K1—O1^ii	88.67 (18)	K1^iv—Si1—K2^xvi	117.10 (6)
O2^ix—K1—O1^ii	114.5 (2)	K1^ix—Si1—K2^xvi	69.61 (6)
O2^iii—K1—O1^ii	64.3 (2)	K1^iii—Si1—K2^xvi	163.46 (6)
O1^vii—K1—O1^ii	120.77 (11)	K1^xvi—Si1—K2^xvi	66.57 (8)
O1^x—K1—O1^ii	93.60 (15)	K2^iii—Si1—K2^xvi	102.83 (6)
Si1^vii—K1—O1^ii	29.93 (10)	K2^xvii—Si1—K2^xvi	99.52 (10)
O1^ix—K1—O1^ii	50.3 (3)	Si1^xvi—O1—Yb1	155.7 (3)
O2^vii—K1—Si1^ix	84.83 (12)	Si1^xvi—O1—K2	115.9 (3)
O1—K1—Si1^ix	145.80 (16)	Yb1—O1—K2	88.39 (17)
O1^viii—K1—Si1^ix	91.24 (13)	Si1^xvi—O1—K1	93.5 (3)
O2^ix—K1—Si1^ix	28.90 (18)	Yb1—O1—K1	88.92 (19)
O2^iii—K1—Si1^ix	146.5 (2)	K2—O1—K1	88.86 (17)
O1^vii—K1—Si1^ix	29.02 (12)	Si1^xvi—O1—K1^iv	91.5 (3)
O1^x—K1—Si1^ix	91.70 (15)	Yb1—O1—K1^iv	85.0 (2)
Si1^vii—K1—Si1^ix	100.62 (5)	K2—O1—K1^iv	92.4 (2)
O1^ix—K1—Si1^ix	85.52 (14)	K1—O1—K1^iv	173.7 (2)
O1^ii—K1—Si1^ix	130.53 (11)	Si1^xvi—O1—K1^ix	74.2 (2)
O2^vii—K1—Si1^iii	84.83 (12)	Yb1—O1—K1^ix	81.54 (16)
O1—K1—Si1^iii	91.24 (13)	K2—O1—K1^ix	169.9 (2)
O1^viii—K1—Si1^iii	145.80 (16)	K1—O1—K1^ix	91.33 (18)
O2^ix—K1—Si1^iii	146.5 (2)	K1^iv—O1—K1^ix	86.40 (15)
O2^iii—K1—Si1^iii	28.90 (18)	Si1—O2—Yb1	170.4 (6)
O1^vii—K1—Si1^iii	91.70 (15)	Si1—O2—K2^iii	103.4 (4)
O1^x—K1—Si1^iii	29.02 (12)	Yb1—O2—K2^iii	86.2 (3)
Si1^vii—K1—Si1^iii	100.62 (5)	Si1—O2—K1^iv	84.5 (4)
O1^ix—K1—Si1^iii	130.53 (11)	Yb1—O2—K1^iv	86.0 (3)
O1^ii—K1—Si1^iii	85.52 (14)	K2^iii—O2—K1^iv	172.1 (3)
Si1^ix—K1—Si1^iii	117.77 (18)	Si1—O2—K1^ix	92.11 (19)
O1—K2—O1^xi	138.4 (3)	Yb1—O2—K1^ix	88.37 (18)
O1—K2—O1^xii	97.6 (2)	K2^iii—O2—K1^ix	86.86 (19)
O1^xi—K2—O1^xii	67.3 (3)	K1^iv—O2—K1^ix	92.91 (19)
O1—K2—O1^i	67.3 (3)	Si1—O2—K1^iii	92.11 (19)
O1^xi—K2—O1^i	97.6 (2)	Yb1—O2—K1^iii	88.37 (18)
O1^xii—K2—O1^i	138.4 (3)	K2^iii—O2—K1^iii	86.86 (19)
O1—K2—O2^iii	66.86 (14)	K1^iv—O2—K1^iii	92.91 (19)
O1^xi—K2—O2^iii	144.72 (16)	K1^ix—O2—K1^iii	173.1 (4)
O1^xii—K2—O2^iii	144.72 (16)	Si1^xviii—O3—Si1	164.9 (10)
O1^i—K2—O2^iii	66.86 (14)	Si1^xviii—O3—K2^iii	97.5 (5)
O1—K2—O2^xiii	144.72 (16)	Si1—O3—K2^iii	97.5 (5)

Symmetry codes: (i) −x, y, z; (ii) x, −y, −z+1; (iii) −x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) x−1, y, z; (vii) x+1/2, y+1/2, z; (viii) −x+1, y, z; (ix) −x+1, −y, −z+1; (x) −x+1/2, y+1/2, z; (xi) −x, y, −z+1/2; (xii) x, y, −z+1/2; (xiii) −x, −y, z−1/2; (xiv) −x−1/2, −y−1/2, z−1/2; (xv) x−1/2, −y−1/2, −z+1; (xvi) −x+1/2, −y−1/2, −z+1; (xvii) −x−1/2, −y−1/2, −z+1; (xviii) x, y, −z+3/2.

(103_K)

Crystal data

K3O7Si2Yb	Dx = 3.871 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1218 reflections
a = 5.7112 (7) Å	θ = 7.1–29.3°
b = 9.9118 (14) Å	µ = 13.78 mm^−1
c = 13.8975 (17) Å	T = 103 K
V = 786.72 (17) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	486 reflections with I > 2σ(I)
ω scans	Rint = 0.040
Absorption correction: analytical CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −7→5
2685 measured reflections	k = −12→12
542 independent reflections	l = −16→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0089P)^2 + 2.0136P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.021	(Δ/σ)max < 0.001
wR(F^2) = 0.042	Δρmax = 0.89 e Å^−3
S = 1.16	Δρmin = −1.14 e Å^−3
542 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
30 parameters	Extinction coefficient: 0.00253 (13)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00161 (16)
K1	0.500000	0.1739 (3)	0.40749 (12)	0.0046 (3)
K2	0.000000	0.0182 (3)	0.250000	0.0065 (5)
Si1	0.000000	−0.3387 (4)	0.63250 (15)	0.0017 (4)
O1	0.2677 (11)	−0.0792 (5)	0.3989 (4)	0.0093 (13)
O2	0.000000	−0.1877 (8)	0.5869 (6)	0.001 (2)
O3	0.000000	−0.3166 (13)	0.750000	0.0090 (19)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00137 (17)	0.00137 (17)	0.0021 (2)	0.000	0.000	0.000
K1	0.0040 (5)	0.0040 (5)	0.0059 (7)	0.000	0.000	0.000
K2	0.0082 (8)	0.0082 (8)	0.0030 (9)	0.000	0.000	0.000
Si1	0.0016 (6)	0.0016 (6)	0.0017 (8)	0.000	0.000	0.000
O1	0.009 (4)	0.002 (3)	0.017 (3)	0.000	0.000	0.000
O2	0.002 (3)	0.001 (4)	0.002 (3)	0.000	0.000	0.000
O3	0.012 (3)	0.012 (3)	0.003 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O2	2.218 (8)	K1—Si1^viii	3.130 (3)
Yb1—O2^i	2.218 (8)	K1—O1^vi	3.143 (6)
Yb1—O1^ii	2.220 (5)	K1—O1^iii	3.143 (6)
Yb1—O1^iii	2.220 (5)	K1—Si1^vi	3.336 (3)
Yb1—O1^i	2.220 (5)	K1—Si1^i	3.336 (3)
Yb1—O1	2.220 (5)	K2—O1	2.748 (5)
Yb1—K1^iv	3.478 (3)	K2—O1^x	2.748 (5)
Yb1—K1^v	3.478 (3)	K2—O1^xi	2.748 (5)
Yb1—K2	3.4791 (4)	K2—O1^ii	2.748 (5)
Yb1—K2^i	3.4791 (4)	K2—O2^i	2.822 (9)
Yb1—K1^i	3.5748 (17)	K2—O2^xii	2.822 (9)
Yb1—K1^vi	3.5748 (17)	K2—O3^i	2.957 (14)
K1—O1	2.841 (8)	K2—Si1^i	3.572 (5)
K1—O1^vii	2.841 (8)	K2—Si1^xii	3.572 (5)
K1—O2^viii	2.845 (9)	K2—Si1^xiii	3.740 (3)
K1—O2^vi	2.8600 (6)	Si1—O1^xiv	1.616 (5)
K1—O2^i	2.8600 (6)	Si1—O1^xv	1.616 (5)
K1—O1^viii	2.888 (8)	Si1—O2	1.625 (9)
K1—O1^ix	2.888 (8)	Si1—O3	1.648 (3)
O2—Yb1—O2^i	180.0	O1^x—K2—O2^xii	66.68 (13)
O2—Yb1—O1^ii	92.7 (2)	O1^xi—K2—O2^xii	66.68 (13)
O2^i—Yb1—O1^ii	87.3 (2)	O1^ii—K2—O2^xii	144.51 (15)
O2—Yb1—O1^iii	87.3 (2)	O2^i—K2—O2^xii	106.9 (3)
O2^i—Yb1—O1^iii	92.7 (2)	O1—K2—O3^i	110.57 (13)
O1^ii—Yb1—O1^iii	180.0	O1^x—K2—O3^i	110.57 (13)
O2—Yb1—O1^i	87.3 (2)	O1^xi—K2—O3^i	110.57 (13)
O2^i—Yb1—O1^i	92.7 (2)	O1^ii—K2—O3^i	110.57 (13)
O1^ii—Yb1—O1^i	92.9 (3)	O2^i—K2—O3^i	53.46 (16)
O1^iii—Yb1—O1^i	87.1 (3)	O2^xii—K2—O3^i	53.46 (16)
O2—Yb1—O1	92.7 (2)	O1—K2—Yb1^xii	137.20 (11)
O2^i—Yb1—O1	87.3 (2)	O1^x—K2—Yb1^xii	39.62 (11)
O1^ii—Yb1—O1	87.1 (3)	O1^xi—K2—Yb1^xii	39.62 (11)
O1^iii—Yb1—O1	92.9 (3)	O1^ii—K2—Yb1^xii	137.20 (11)
O1^i—Yb1—O1	180.0	O2^i—K2—Yb1^xii	146.44 (19)
O2—Yb1—K1^iv	54.7 (2)	O2^xii—K2—Yb1^xii	39.52 (16)
O2^i—Yb1—K1^iv	125.3 (2)	O3^i—K2—Yb1^xii	92.98 (5)
O1^ii—Yb1—K1^iv	55.77 (18)	O1—K2—Yb1	39.62 (11)
O1^iii—Yb1—K1^iv	124.23 (18)	O1^x—K2—Yb1	137.20 (11)
O1^i—Yb1—K1^iv	124.23 (18)	O1^xi—K2—Yb1	137.20 (11)
O1—Yb1—K1^iv	55.77 (18)	O1^ii—K2—Yb1	39.62 (11)
O2—Yb1—K1^v	125.3 (2)	O2^i—K2—Yb1	39.52 (16)
O2^i—Yb1—K1^v	54.7 (2)	O2^xii—K2—Yb1	146.44 (19)
O1^ii—Yb1—K1^v	124.23 (18)	O3^i—K2—Yb1	92.98 (5)
O1^iii—Yb1—K1^v	55.77 (18)	Yb1^xii—K2—Yb1	174.04 (11)
O1^i—Yb1—K1^v	55.77 (18)	O1—K2—Si1^i	88.18 (12)
O1—Yb1—K1^v	124.23 (18)	O1^x—K2—Si1^i	131.06 (16)
K1^iv—Yb1—K1^v	180.00 (5)	O1^xi—K2—Si1^i	131.06 (16)
O2—Yb1—K2	125.9 (2)	O1^ii—K2—Si1^i	88.18 (12)
O2^i—Yb1—K2	54.1 (2)	O2^i—K2—Si1^i	26.25 (17)
O1^ii—Yb1—K2	52.15 (14)	O2^xii—K2—Si1^i	80.67 (18)
O1^iii—Yb1—K2	127.85 (14)	O3^i—K2—Si1^i	27.21 (5)
O1^i—Yb1—K2	127.85 (14)	Yb1^xii—K2—Si1^i	120.19 (9)
O1—Yb1—K2	52.15 (14)	Yb1—K2—Si1^i	65.77 (5)
K1^iv—Yb1—K2	71.29 (7)	O1—K2—Si1^xii	131.06 (16)
K1^v—Yb1—K2	108.71 (7)	O1^x—K2—Si1^xii	88.18 (12)
O2—Yb1—K2^i	54.1 (2)	O1^xi—K2—Si1^xii	88.18 (12)
O2^i—Yb1—K2^i	126.0 (2)	O1^ii—K2—Si1^xii	131.06 (16)
O1^ii—Yb1—K2^i	127.85 (14)	O2^i—K2—Si1^xii	80.67 (18)
O1^iii—Yb1—K2^i	52.15 (14)	O2^xii—K2—Si1^xii	26.25 (17)
O1^i—Yb1—K2^i	52.15 (14)	O3^i—K2—Si1^xii	27.21 (5)
O1—Yb1—K2^i	127.85 (14)	Yb1^xii—K2—Si1^xii	65.77 (5)
K1^iv—Yb1—K2^i	108.71 (7)	Yb1—K2—Si1^xii	120.19 (9)
K1^v—Yb1—K2^i	71.29 (7)	Si1^i—K2—Si1^xii	54.41 (10)
K2—Yb1—K2^i	180.00 (11)	O1—K2—Si1^xiii	125.90 (17)
O2—Yb1—K1^i	53.11 (4)	O1^x—K2—Si1^xiii	22.97 (11)
O2^i—Yb1—K1^i	126.89 (4)	O1^xi—K2—Si1^xiii	85.91 (16)
O1^ii—Yb1—K1^i	60.45 (13)	O1^ii—K2—Si1^xiii	74.74 (11)
O1^iii—Yb1—K1^i	119.55 (13)	O2^i—K2—Si1^xiii	129.35 (4)
O1^i—Yb1—K1^i	52.61 (19)	O2^xii—K2—Si1^xiii	86.13 (11)
O1—Yb1—K1^i	127.39 (19)	O3^i—K2—Si1^xiii	118.41 (7)
K1^iv—Yb1—K1^i	71.63 (4)	Yb1^xii—K2—Si1^xiii	62.56 (4)
K1^v—Yb1—K1^i	108.37 (4)	Yb1—K2—Si1^xiii	114.29 (5)
K2—Yb1—K1^i	112.59 (4)	Si1^i—K2—Si1^xiii	128.52 (7)
K2^i—Yb1—K1^i	67.41 (4)	Si1^xii—K2—Si1^xiii	102.92 (5)
O2—Yb1—K1^vi	53.11 (4)	O1^xiv—Si1—O1^xv	110.3 (5)
O2^i—Yb1—K1^vi	126.89 (4)	O1^xiv—Si1—O2	111.0 (3)
O1^ii—Yb1—K1^vi	127.39 (19)	O1^xv—Si1—O2	111.0 (3)
O1^iii—Yb1—K1^vi	52.61 (19)	O1^xiv—Si1—O3	109.6 (3)
O1^i—Yb1—K1^vi	119.55 (13)	O1^xv—Si1—O3	109.6 (3)
O1—Yb1—K1^vi	60.45 (13)	O2—Si1—O3	105.3 (6)
K1^iv—Yb1—K1^vi	71.63 (4)	O1^xiv—Si1—K1^iv	75.5 (2)
K1^v—Yb1—K1^vi	108.37 (4)	O1^xv—Si1—K1^iv	75.5 (2)
K2—Yb1—K1^vi	112.59 (4)	O2—Si1—K1^iv	64.7 (3)
K2^i—Yb1—K1^vi	67.41 (4)	O3—Si1—K1^iv	170.1 (5)
K1^i—Yb1—K1^vi	106.03 (7)	O1^xiv—Si1—K1^vi	154.7 (2)
O1—K1—O1^vii	55.7 (2)	O1^xv—Si1—K1^vi	59.9 (3)
O1—K1—O2^viii	117.5 (2)	O2—Si1—K1^vi	58.95 (8)
O1^vii—K1—O2^viii	117.5 (2)	O3—Si1—K1^vi	95.7 (2)
O1—K1—O2^vi	120.6 (2)	K1^iv—Si1—K1^vi	79.28 (5)
O1^vii—K1—O2^vi	64.98 (15)	O1^xiv—Si1—K1^i	59.9 (3)
O2^viii—K1—O2^vi	87.30 (18)	O1^xv—Si1—K1^i	154.7 (2)
O1—K1—O2^i	64.98 (15)	O2—Si1—K1^i	58.95 (8)
O1^vii—K1—O2^i	120.6 (2)	O3—Si1—K1^i	95.7 (2)
O2^viii—K1—O2^i	87.30 (18)	K1^iv—Si1—K1^i	79.28 (5)
O2^vi—K1—O2^i	173.7 (3)	K1^vi—Si1—K1^i	117.72 (16)
O1—K1—O1^viii	173.7 (2)	O1^xiv—Si1—K1^xv	57.2 (3)
O1^vii—K1—O1^viii	119.96 (2)	O1^xv—Si1—K1^xv	57.2 (3)
O2^viii—K1—O1^viii	68.15 (13)	O2—Si1—K1^xv	147.5 (3)
O2^vi—K1—O1^viii	55.38 (15)	O3—Si1—K1^xv	107.1 (5)
O2^i—K1—O1^viii	119.3 (2)	K1^iv—Si1—K1^xv	82.80 (8)
O1—K1—O1^ix	119.96 (2)	K1^vi—Si1—K1^xv	117.09 (8)
O1^vii—K1—O1^ix	173.7 (2)	K1^i—Si1—K1^xv	117.09 (8)
O2^viii—K1—O1^ix	68.15 (13)	O1^xiv—Si1—K2^i	124.8 (3)
O2^vi—K1—O1^ix	119.3 (2)	O1^xv—Si1—K2^i	124.8 (3)
O2^i—K1—O1^ix	55.38 (15)	O2—Si1—K2^i	50.2 (3)
O1^viii—K1—O1^ix	63.94 (19)	O3—Si1—K2^i	55.1 (5)
O1—K1—Si1^viii	90.37 (12)	K1^iv—Si1—K2^i	114.91 (10)
O1^vii—K1—Si1^viii	90.37 (12)	K1^vi—Si1—K2^i	68.95 (9)
O2^viii—K1—Si1^viii	31.11 (17)	K1^i—Si1—K2^i	68.95 (9)
O2^vi—K1—Si1^viii	88.54 (18)	K1^xv—Si1—K2^i	162.29 (8)
O2^i—K1—Si1^viii	88.54 (18)	O1^xiv—Si1—K2^xvi	41.57 (19)
O1^viii—K1—Si1^viii	94.31 (13)	O1^xv—Si1—K2^xvi	120.3 (3)
O1^ix—K1—Si1^viii	94.31 (13)	O2—Si1—K2^xvi	127.48 (10)
O1—K1—O1^vi	88.23 (17)	O3—Si1—K2^xvi	68.3 (3)
O1^vii—K1—O1^vi	64.84 (17)	K1^iv—Si1—K2^xvi	117.09 (6)
O2^viii—K1—O1^vi	52.70 (13)	K1^vi—Si1—K2^xvi	163.57 (6)
O2^vi—K1—O1^vi	64.5 (2)	K1^i—Si1—K2^xvi	69.64 (6)
O2^i—K1—O1^vi	114.3 (2)	K1^xv—Si1—K2^xvi	66.59 (8)
O1^viii—K1—O1^vi	93.72 (15)	K2^i—Si1—K2^xvi	102.92 (5)
O1^ix—K1—O1^vi	120.79 (11)	O1^xiv—Si1—K2^xv	120.3 (3)
Si1^viii—K1—O1^vi	29.86 (10)	O1^xv—Si1—K2^xv	41.57 (19)
O1—K1—O1^iii	64.84 (17)	O2—Si1—K2^xv	127.48 (10)
O1^vii—K1—O1^iii	88.23 (17)	O3—Si1—K2^xv	68.3 (3)
O2^viii—K1—O1^iii	52.70 (13)	K1^iv—Si1—K2^xv	117.09 (6)
O2^vi—K1—O1^iii	114.3 (2)	K1^vi—Si1—K2^xv	69.64 (6)
O2^i—K1—O1^iii	64.5 (2)	K1^i—Si1—K2^xv	163.57 (6)
O1^viii—K1—O1^iii	120.79 (11)	K1^xv—Si1—K2^xv	66.59 (8)
O1^ix—K1—O1^iii	93.72 (15)	K2^i—Si1—K2^xv	102.92 (5)
Si1^viii—K1—O1^iii	29.86 (10)	K2^xvi—Si1—K2^xv	99.55 (10)
O1^vi—K1—O1^iii	49.9 (2)	Si1^xv—O1—Yb1	156.1 (3)
O1—K1—Si1^vi	145.60 (14)	Si1^xv—O1—K2	115.5 (3)
O1^vii—K1—Si1^vi	91.47 (12)	Yb1—O1—K2	88.23 (16)
O2^viii—K1—Si1^vi	84.84 (11)	Si1^xv—O1—K1	94.2 (3)
O2^vi—K1—Si1^vi	29.14 (16)	Yb1—O1—K1	89.01 (18)
O2^i—K1—Si1^vi	146.7 (2)	K2—O1—K1	88.91 (17)
O1^viii—K1—Si1^vi	28.97 (11)	Si1^xv—O1—K1^iv	91.1 (3)
O1^ix—K1—Si1^vi	91.80 (14)	Yb1—O1—K1^iv	84.8 (2)
Si1^viii—K1—Si1^vi	100.72 (5)	K2—O1—K1^iv	92.0 (2)
O1^vi—K1—Si1^vi	85.85 (13)	K1—O1—K1^iv	173.7 (2)
O1^iii—K1—Si1^vi	130.55 (11)	Si1^xv—O1—K1^vi	74.6 (2)
O1—K1—Si1^i	91.47 (12)	Yb1—O1—K1^vi	81.65 (15)
O1^vii—K1—Si1^i	145.60 (14)	K2—O1—K1^vi	169.8 (2)
O2^viii—K1—Si1^i	84.84 (11)	K1—O1—K1^vi	91.77 (17)
O2^vi—K1—Si1^i	146.7 (2)	K1^iv—O1—K1^vi	86.28 (15)
O2^i—K1—Si1^i	29.14 (16)	Si1—O2—Yb1	170.0 (5)
O1^viii—K1—Si1^i	91.80 (14)	Si1—O2—K2^i	103.6 (4)
O1^ix—K1—Si1^i	28.97 (11)	Yb1—O2—K2^i	86.4 (3)
Si1^viii—K1—Si1^i	100.72 (5)	Si1—O2—K1^iv	84.2 (3)
O1^vi—K1—Si1^i	130.55 (11)	Yb1—O2—K1^iv	85.8 (3)
O1^iii—K1—Si1^i	85.85 (13)	K2^i—O2—K1^iv	172.3 (3)
Si1^vi—K1—Si1^i	117.72 (16)	Si1—O2—K1^vi	91.91 (17)
O1—K2—O1^x	138.9 (3)	Yb1—O2—K1^vi	88.56 (17)
O1—K2—O1^xi	97.7 (2)	K2^i—O2—K1^vi	87.10 (17)
O1^x—K2—O1^xi	67.6 (3)	K1^iv—O2—K1^vi	92.70 (18)
O1—K2—O1^ii	67.6 (3)	Si1—O2—K1^i	91.91 (17)
O1^x—K2—O1^ii	97.7 (2)	Yb1—O2—K1^i	88.56 (17)
O1^xi—K2—O1^ii	138.9 (3)	K2^i—O2—K1^i	87.10 (17)
O1—K2—O2^i	66.68 (13)	K1^iv—O2—K1^i	92.70 (18)
O1^x—K2—O2^i	144.51 (15)	K1^vi—O2—K1^i	173.7 (3)
O1^xi—K2—O2^i	144.51 (15)	Si1^xvii—O3—Si1	164.7 (9)
O1^ii—K2—O2^i	66.68 (13)	Si1^xvii—O3—K2^i	97.6 (5)
O1—K2—O2^xii	144.51 (15)	Si1—O3—K2^i	97.6 (5)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, y, z; (iii) x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1, −y, −z+1; (vii) −x+1, y, z; (viii) x+1/2, y+1/2, z; (ix) −x+1/2, y+1/2, z; (x) −x, y, −z+1/2; (xi) x, y, −z+1/2; (xii) −x, −y, z−1/2; (xiii) −x−1/2, −y−1/2, z−1/2; (xiv) x−1/2, −y−1/2, −z+1; (xv) −x+1/2, −y−1/2, −z+1; (xvi) −x−1/2, −y−1/2, −z+1; (xvii) x, y, −z+3/2.

(113_K)

Crystal data

K3O7Si2Yb	Dx = 3.887 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1196 reflections
a = 5.7071 (6) Å	θ = 4.3–29.2°
b = 9.8905 (9) Å	µ = 13.83 mm^−1
c = 13.8818 (12) Å	T = 113 K
V = 783.57 (13) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	475 reflections with I > 2σ(I)
ω scans	Rint = 0.037
Absorption correction: analytical CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.4°, θmin = 2.9°
Tmin = 0.303, Tmax = 0.396	h = −6→7
2683 measured reflections	k = −12→10
539 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0082P)^2 + 2.143P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.020	(Δ/σ)max < 0.001
wR(F^2) = 0.038	Δρmax = 0.97 e Å^−3
S = 1.13	Δρmin = −1.20 e Å^−3
539 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
28 parameters	Extinction coefficient: 0.00260 (12)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00159 (15)
K1	0.500000	0.1730 (3)	0.40752 (11)	0.0050 (3)
K2	0.000000	0.0178 (3)	0.250000	0.0070 (5)
Si1	0.000000	−0.3390 (4)	0.63238 (14)	0.0019 (4)
O1	0.2669 (10)	−0.0793 (5)	0.3988 (3)	0.0080 (11)
O2	0.000000	−0.1887 (7)	0.5866 (6)	0.0012 (17)
O3	0.000000	−0.3172 (12)	0.750000	0.0086 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00127 (16)	0.00127 (16)	0.0022 (2)	0.000	0.000	0.000
K1	0.0044 (4)	0.0044 (4)	0.0064 (6)	0.000	0.000	0.000
K2	0.0089 (7)	0.0089 (7)	0.0032 (9)	0.000	0.000	0.000
Si1	0.0017 (5)	0.0017 (5)	0.0024 (7)	0.000	0.000	0.000
O1	0.0042 (14)	0.0042 (14)	0.016 (2)	0.000	0.000	0.000
O2	0.0012 (17)	0.0012 (17)	0.0012 (17)	0.000	0.000	0.000
O3	0.011 (3)	0.011 (3)	0.004 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O1	2.215 (4)	K1—Si1^viii	3.124 (3)
Yb1—O1^i	2.215 (4)	K1—O1^ix	3.139 (5)
Yb1—O1^ii	2.215 (4)	K1—O1^ii	3.139 (5)
Yb1—O1^iii	2.215 (4)	K1—Si1^ix	3.338 (3)
Yb1—O2^iii	2.219 (7)	K1—Si1^iii	3.338 (3)
Yb1—O2	2.219 (7)	K2—O1	2.741 (5)
Yb1—K2	3.4749 (4)	K2—O1^xi	2.741 (5)
Yb1—K2^iii	3.4749 (3)	K2—O1^xii	2.741 (5)
Yb1—K1^iv	3.480 (3)	K2—O1^i	2.741 (5)
Yb1—K1^v	3.480 (3)	K2—O2^iii	2.829 (8)
Yb1—K1^iii	3.5663 (16)	K2—O2^xiii	2.829 (8)
Yb1—K1^vi	3.5663 (15)	K2—O3^iii	2.961 (13)
K1—O1	2.831 (8)	K2—Si1^iii	3.571 (5)
K1—O1^vii	2.831 (8)	K2—Si1^xiii	3.571 (5)
K1—O2^viii	2.837 (8)	K2—Si1^xiv	3.733 (3)
K1—O2^ix	2.8589 (6)	Si1—O1^xv	1.616 (5)
K1—O2^iii	2.8589 (6)	Si1—O1^xvi	1.616 (5)
K1—O1^viii	2.887 (8)	Si1—O2	1.617 (8)
K1—O1^x	2.887 (8)	Si1—O3	1.647 (3)
O1—Yb1—O1^i	86.9 (3)	O1^xi—K2—O2^xiii	66.72 (12)
O1—Yb1—O1^ii	93.1 (3)	O1^xii—K2—O2^xiii	66.72 (12)
O1^i—Yb1—O1^ii	180.0	O1^i—K2—O2^xiii	144.49 (14)
O1—Yb1—O1^iii	180.0 (2)	O2^iii—K2—O2^xiii	106.6 (3)
O1^i—Yb1—O1^iii	93.1 (3)	O1—K2—O3^iii	110.52 (13)
O1^ii—Yb1—O1^iii	86.9 (3)	O1^xi—K2—O3^iii	110.52 (13)
O1—Yb1—O2^iii	87.40 (19)	O1^xii—K2—O3^iii	110.52 (13)
O1^i—Yb1—O2^iii	87.40 (18)	O1^i—K2—O3^iii	110.52 (13)
O1^ii—Yb1—O2^iii	92.60 (19)	O2^iii—K2—O3^iii	53.32 (15)
O1^iii—Yb1—O2^iii	92.60 (18)	O2^xiii—K2—O3^iii	53.32 (15)
O1—Yb1—O2	92.60 (18)	O1—K2—Yb1^xiii	137.32 (10)
O1^i—Yb1—O2	92.60 (19)	O1^xi—K2—Yb1^xiii	39.59 (9)
O1^ii—Yb1—O2	87.40 (18)	O1^xii—K2—Yb1^xiii	39.59 (9)
O1^iii—Yb1—O2	87.40 (19)	O1^i—K2—Yb1^xiii	137.32 (10)
O2^iii—Yb1—O2	180.0	O2^iii—K2—Yb1^xiii	146.22 (17)
O1—Yb1—K2	52.04 (12)	O2^xiii—K2—Yb1^xiii	39.59 (15)
O1^i—Yb1—K2	52.04 (12)	O3^iii—K2—Yb1^xiii	92.90 (5)
O1^ii—Yb1—K2	127.96 (12)	O1—K2—Yb1	39.59 (9)
O1^iii—Yb1—K2	127.96 (12)	O1^xi—K2—Yb1	137.32 (10)
O2^iii—Yb1—K2	54.3 (2)	O1^xii—K2—Yb1	137.32 (10)
O2—Yb1—K2	125.7 (2)	O1^i—K2—Yb1	39.59 (9)
O1—Yb1—K2^iii	127.96 (12)	O2^iii—K2—Yb1	39.59 (15)
O1^i—Yb1—K2^iii	127.96 (12)	O2^xiii—K2—Yb1	146.22 (17)
O1^ii—Yb1—K2^iii	52.04 (12)	O3^iii—K2—Yb1	92.90 (5)
O1^iii—Yb1—K2^iii	52.04 (12)	Yb1^xiii—K2—Yb1	174.19 (10)
O2^iii—Yb1—K2^iii	125.7 (2)	O1—K2—Si1^iii	88.12 (11)
O2—Yb1—K2^iii	54.3 (2)	O1^xi—K2—Si1^iii	131.03 (15)
K2—Yb1—K2^iii	180.0	O1^xii—K2—Si1^iii	131.03 (15)
O1—Yb1—K1^iv	55.73 (17)	O1^i—K2—Si1^iii	88.12 (11)
O1^i—Yb1—K1^iv	55.73 (17)	O2^iii—K2—Si1^iii	26.12 (15)
O1^ii—Yb1—K1^iv	124.27 (17)	O2^xiii—K2—Si1^iii	80.52 (17)
O1^iii—Yb1—K1^iv	124.27 (17)	O3^iii—K2—Si1^iii	27.20 (5)
O2^iii—Yb1—K1^iv	125.6 (2)	Yb1^xiii—K2—Si1^iii	120.11 (9)
O2—Yb1—K1^iv	54.4 (2)	Yb1—K2—Si1^iii	65.70 (4)
K2—Yb1—K1^iv	71.25 (6)	O1—K2—Si1^xiii	131.03 (15)
K2^iii—Yb1—K1^iv	108.75 (6)	O1^xi—K2—Si1^xiii	88.12 (11)
O1—Yb1—K1^v	124.27 (17)	O1^xii—K2—Si1^xiii	88.12 (11)
O1^i—Yb1—K1^v	124.27 (17)	O1^i—K2—Si1^xiii	131.03 (15)
O1^ii—Yb1—K1^v	55.73 (17)	O2^iii—K2—Si1^xiii	80.52 (17)
O1^iii—Yb1—K1^v	55.73 (17)	O2^xiii—K2—Si1^xiii	26.12 (15)
O2^iii—Yb1—K1^v	54.4 (2)	O3^iii—K2—Si1^xiii	27.20 (5)
O2—Yb1—K1^v	125.6 (2)	Yb1^xiii—K2—Si1^xiii	65.70 (4)
K2—Yb1—K1^v	108.75 (6)	Yb1—K2—Si1^xiii	120.11 (9)
K2^iii—Yb1—K1^v	71.25 (6)	Si1^iii—K2—Si1^xiii	54.41 (10)
K1^iv—Yb1—K1^v	180.0	O1—K2—Si1^xiv	126.04 (17)
O1—Yb1—K1^iii	127.47 (18)	O1^xi—K2—Si1^xiv	23.00 (9)
O1^i—Yb1—K1^iii	60.53 (12)	O1^xii—K2—Si1^xiv	85.93 (14)
O1^ii—Yb1—K1^iii	119.47 (12)	O1^i—K2—Si1^xiv	74.86 (10)
O1^iii—Yb1—K1^iii	52.53 (18)	O2^iii—K2—Si1^xiv	129.33 (4)
O2^iii—Yb1—K1^iii	126.75 (4)	O2^xiii—K2—Si1^xiv	86.12 (10)
O2—Yb1—K1^iii	53.25 (4)	O3^iii—K2—Si1^xiv	118.28 (7)
K2—Yb1—K1^iii	112.57 (4)	Yb1^xiii—K2—Si1^xiv	62.56 (3)
K2^iii—Yb1—K1^iii	67.43 (4)	Yb1—K2—Si1^xiv	114.38 (5)
K1^iv—Yb1—K1^iii	71.75 (4)	Si1^iii—K2—Si1^xiv	128.41 (7)
K1^v—Yb1—K1^iii	108.25 (4)	Si1^xiii—K2—Si1^xiv	102.79 (5)
O1—Yb1—K1^vi	119.47 (12)	O1^xv—Si1—O1^xvi	110.9 (5)
O1^i—Yb1—K1^vi	52.53 (18)	O1^xv—Si1—O2	110.7 (3)
O1^ii—Yb1—K1^vi	127.47 (18)	O1^xvi—Si1—O2	110.7 (3)
O1^iii—Yb1—K1^vi	60.53 (12)	O1^xv—Si1—O3	109.3 (3)
O2^iii—Yb1—K1^vi	53.25 (4)	O1^xvi—Si1—O3	109.3 (3)
O2—Yb1—K1^vi	126.75 (4)	O2—Si1—O3	105.7 (6)
K2—Yb1—K1^vi	67.43 (4)	O1^xv—Si1—K1^iv	75.57 (17)
K2^iii—Yb1—K1^vi	112.57 (4)	O1^xvi—Si1—K1^iv	75.57 (17)
K1^iv—Yb1—K1^vi	108.25 (4)	O2—Si1—K1^iv	64.7 (3)
K1^v—Yb1—K1^vi	71.75 (4)	O3—Si1—K1^iv	170.3 (5)
K1^iii—Yb1—K1^vi	73.71 (7)	O1^xv—Si1—K1^ix	154.85 (18)
O1—K1—O1^vii	56.07 (18)	O1^xvi—Si1—K1^ix	59.8 (2)
O1—K1—O2^viii	117.54 (18)	O2—Si1—K1^ix	58.85 (8)
O1^vii—K1—O2^viii	117.54 (18)	O3—Si1—K1^ix	95.8 (2)
O1—K1—O2^ix	121.2 (2)	K1^iv—Si1—K1^ix	79.37 (5)
O1^vii—K1—O2^ix	65.16 (14)	O1^xv—Si1—K1^iii	59.8 (2)
O2^viii—K1—O2^ix	87.06 (16)	O1^xvi—Si1—K1^iii	154.85 (18)
O1—K1—O2^iii	65.16 (14)	O2—Si1—K1^iii	58.85 (8)
O1^vii—K1—O2^iii	121.2 (2)	O3—Si1—K1^iii	95.8 (2)
O2^viii—K1—O2^iii	87.06 (16)	K1^iv—Si1—K1^iii	79.37 (5)
O2^ix—K1—O2^iii	173.0 (3)	K1^ix—Si1—K1^iii	117.47 (16)
O1—K1—O1^viii	173.85 (18)	O1^xv—Si1—K1^xvi	57.5 (3)
O1^vii—K1—O1^viii	119.889 (19)	O1^xvi—Si1—K1^xvi	57.5 (3)
O2^viii—K1—O1^viii	68.12 (12)	O2—Si1—K1^xvi	147.3 (3)
O2^ix—K1—O1^viii	55.15 (14)	O3—Si1—K1^xvi	107.0 (4)
O2^iii—K1—O1^viii	118.8 (2)	K1^iv—Si1—K1^xvi	82.65 (7)
O1—K1—O1^x	119.889 (19)	K1^ix—Si1—K1^xvi	117.23 (8)
O1^vii—K1—O1^x	173.85 (18)	K1^iii—Si1—K1^xvi	117.23 (8)
O2^viii—K1—O1^x	68.12 (12)	O1^xv—Si1—K2^iii	124.6 (3)
O2^ix—K1—O1^x	118.8 (2)	O1^xvi—Si1—K2^iii	124.6 (3)
O2^iii—K1—O1^x	55.15 (14)	O2—Si1—K2^iii	50.4 (3)
O1^viii—K1—O1^x	63.68 (18)	O3—Si1—K2^iii	55.3 (4)
O1—K1—Si1^viii	90.52 (11)	K1^iv—Si1—K2^iii	115.04 (10)
O1^vii—K1—Si1^viii	90.52 (11)	K1^ix—Si1—K2^iii	68.81 (8)
O2^viii—K1—Si1^viii	31.00 (16)	K1^iii—Si1—K2^iii	68.81 (9)
O2^ix—K1—Si1^viii	88.47 (17)	K1^xvi—Si1—K2^iii	162.31 (8)
O2^iii—K1—Si1^viii	88.47 (17)	O1^xv—Si1—K2^xvii	41.50 (17)
O1^viii—K1—Si1^viii	94.23 (11)	O1^xvi—Si1—K2^xvii	120.6 (3)
O1^x—K1—Si1^viii	94.23 (11)	O2—Si1—K2^xvii	127.42 (10)
O1—K1—O1^ix	88.60 (16)	O3—Si1—K2^xvii	68.2 (3)
O1^vii—K1—O1^ix	64.98 (14)	K1^iv—Si1—K2^xvii	117.06 (5)
O2^viii—K1—O1^ix	52.57 (12)	K1^ix—Si1—K2^xvii	163.52 (6)
O2^ix—K1—O1^ix	64.43 (18)	K1^iii—Si1—K2^xvii	69.65 (5)
O2^iii—K1—O1^ix	114.5 (2)	K1^xvi—Si1—K2^xvii	66.74 (8)
O1^viii—K1—O1^ix	93.58 (13)	K2^iii—Si1—K2^xvii	102.79 (5)
O1^x—K1—O1^ix	120.64 (9)	O1^xv—Si1—K2^xvi	120.6 (3)
Si1^viii—K1—O1^ix	29.90 (9)	O1^xvi—Si1—K2^xvi	41.50 (17)
O1—K1—O1^ii	64.98 (14)	O2—Si1—K2^xvi	127.42 (10)
O1^vii—K1—O1^ii	88.60 (16)	O3—Si1—K2^xvi	68.2 (2)
O2^viii—K1—O1^ii	52.57 (12)	K1^iv—Si1—K2^xvi	117.06 (5)
O2^ix—K1—O1^ii	114.5 (2)	K1^ix—Si1—K2^xvi	69.65 (5)
O2^iii—K1—O1^ii	64.43 (18)	K1^iii—Si1—K2^xvi	163.52 (6)
O1^viii—K1—O1^ii	120.64 (9)	K1^xvi—Si1—K2^xvi	66.74 (8)
O1^x—K1—O1^ii	93.58 (13)	K2^iii—Si1—K2^xvi	102.79 (5)
Si1^viii—K1—O1^ii	29.90 (9)	K2^xvii—Si1—K2^xvi	99.70 (10)
O1^ix—K1—O1^ii	50.2 (2)	Si1^xvi—O1—Yb1	156.0 (3)
O1—K1—Si1^ix	145.92 (14)	Si1^xvi—O1—K2	115.5 (2)
O1^vii—K1—Si1^ix	91.42 (11)	Yb1—O1—K2	88.37 (15)
O2^viii—K1—Si1^ix	84.73 (10)	Si1^xvi—O1—K1	93.7 (3)
O2^ix—K1—Si1^ix	28.95 (15)	Yb1—O1—K1	89.08 (17)
O2^iii—K1—Si1^ix	146.2 (2)	K2—O1—K1	89.09 (15)
O1^viii—K1—Si1^ix	28.94 (10)	Si1^xvi—O1—K1^iv	91.2 (2)
O1^x—K1—Si1^ix	91.54 (13)	Yb1—O1—K1^iv	84.92 (19)
Si1^viii—K1—Si1^ix	100.63 (5)	K2—O1—K1^iv	92.05 (18)
O1^ix—K1—Si1^ix	85.69 (12)	K1—O1—K1^iv	173.85 (18)
O1^ii—K1—Si1^ix	130.50 (10)	Si1^xvi—O1—K1^ix	74.53 (18)
O1—K1—Si1^iii	91.42 (11)	Yb1—O1—K1^ix	81.56 (13)
O1^vii—K1—Si1^iii	145.92 (14)	K2—O1—K1^ix	169.91 (18)
O2^viii—K1—Si1^iii	84.73 (10)	K1—O1—K1^ix	91.40 (16)
O2^ix—K1—Si1^iii	146.2 (2)	K1^iv—O1—K1^ix	86.42 (13)
O2^iii—K1—Si1^iii	28.95 (15)	Si1—O2—Yb1	170.4 (5)
O1^viii—K1—Si1^iii	91.54 (13)	Si1—O2—K2^iii	103.5 (4)
O1^x—K1—Si1^iii	28.94 (10)	Yb1—O2—K2^iii	86.1 (2)
Si1^viii—K1—Si1^iii	100.63 (5)	Si1—O2—K1^iv	84.3 (3)
O1^ix—K1—Si1^iii	130.50 (9)	Yb1—O2—K1^iv	86.1 (3)
O1^ii—K1—Si1^iii	85.69 (12)	K2^iii—O2—K1^iv	172.2 (3)
Si1^ix—K1—Si1^iii	117.47 (16)	Si1—O2—K1^ix	92.21 (16)
O1—K2—O1^xi	139.0 (3)	Yb1—O2—K1^ix	88.28 (16)
O1—K2—O1^xii	97.86 (18)	K2^iii—O2—K1^ix	86.82 (16)
O1^xi—K2—O1^xii	67.5 (2)	K1^iv—O2—K1^ix	92.94 (16)
O1—K2—O1^i	67.5 (2)	Si1—O2—K1^iii	92.21 (16)
O1^xi—K2—O1^i	97.86 (18)	Yb1—O2—K1^iii	88.28 (16)
O1^xii—K2—O1^i	139.0 (3)	K2^iii—O2—K1^iii	86.82 (16)
O1—K2—O2^iii	66.72 (12)	K1^iv—O2—K1^iii	92.94 (16)
O1^xi—K2—O2^iii	144.49 (14)	K1^ix—O2—K1^iii	173.0 (3)
O1^xii—K2—O2^iii	144.49 (14)	Si1^xviii—O3—Si1	165.0 (9)
O1^i—K2—O2^iii	66.72 (12)	Si1^xviii—O3—K2^iii	97.5 (4)
O1—K2—O2^xiii	144.49 (14)	Si1—O3—K2^iii	97.5 (4)

Symmetry codes: (i) −x, y, z; (ii) x, −y, −z+1; (iii) −x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) x−1, y, z; (vii) −x+1, y, z; (viii) x+1/2, y+1/2, z; (ix) −x+1, −y, −z+1; (x) −x+1/2, y+1/2, z; (xi) −x, y, −z+1/2; (xii) x, y, −z+1/2; (xiii) −x, −y, z−1/2; (xiv) −x−1/2, −y−1/2, z−1/2; (xv) x−1/2, −y−1/2, −z+1; (xvi) −x+1/2, −y−1/2, −z+1; (xvii) −x−1/2, −y−1/2, −z+1; (xviii) x, y, −z+3/2.

(123_K)

Crystal data

K3O7Si2Yb	Dx = 3.868 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1208 reflections
a = 5.7161 (6) Å	θ = 4.1–29.3°
b = 9.9090 (12) Å	µ = 13.77 mm^−1
c = 13.9021 (15) Å	T = 123 K
V = 787.42 (15) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	470 reflections with I > 2σ(I)
ω scans	Rint = 0.039
Absorption correction: analytical CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.303, Tmax = 0.397	h = −5→7
2687 measured reflections	k = −12→12
542 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0082P)^2 + 1.5863P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.019	(Δ/σ)max < 0.001
wR(F^2) = 0.037	Δρmax = 1.11 e Å^−3
S = 1.11	Δρmin = −1.52 e Å^−3
542 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
29 parameters	Extinction coefficient: 0.00307 (13)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00218 (15)
K1	0.500000	0.1731 (3)	0.40754 (11)	0.0057 (3)
K2	0.000000	0.0171 (3)	0.250000	0.0084 (5)
Si1	0.000000	−0.3390 (4)	0.63246 (14)	0.0021 (4)
O1	0.2670 (11)	−0.0799 (5)	0.3989 (3)	0.0095 (13)
O2	0.000000	−0.1878 (8)	0.5865 (6)	0.0030 (19)
O3	0.000000	−0.3172 (12)	0.750000	0.0086 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00191 (16)	0.00191 (16)	0.0027 (2)	0.000	0.000	0.000
K1	0.0050 (5)	0.0050 (5)	0.0071 (6)	0.000	0.000	0.000
K2	0.0107 (8)	0.0107 (8)	0.0039 (9)	0.000	0.000	0.000
Si1	0.0018 (6)	0.0018 (6)	0.0027 (7)	0.000	0.000	0.000
O1	0.008 (4)	0.004 (3)	0.017 (2)	0.000	0.000	0.000
O2	0.0030 (19)	0.0030 (19)	0.0030 (19)	0.000	0.000	0.000
O3	0.011 (3)	0.004 (5)	0.011 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O2	2.216 (8)	K1—Si1^viii	3.129 (3)
Yb1—O2^i	2.216 (8)	K1—O1^vi	3.142 (5)
Yb1—O1	2.221 (5)	K1—O1^iii	3.142 (5)
Yb1—O1^ii	2.221 (5)	K1—Si1^vi	3.344 (3)
Yb1—O1^iii	2.221 (5)	K1—Si1^i	3.344 (3)
Yb1—O1^i	2.221 (5)	K2—O1	2.745 (5)
Yb1—K2^i	3.4797 (4)	K2—O1^x	2.745 (5)
Yb1—K2	3.4797 (4)	K2—O1^xi	2.745 (5)
Yb1—K1^iv	3.485 (3)	K2—O1^ii	2.745 (5)
Yb1—K1^v	3.485 (3)	K2—O2^i	2.834 (9)
Yb1—K1^i	3.5725 (17)	K2—O2^xii	2.834 (9)
Yb1—K1^vi	3.5725 (17)	K2—O3^i	2.974 (13)
K1—O1	2.841 (8)	K2—Si1^i	3.584 (5)
K1—O1^vii	2.841 (8)	K2—Si1^xii	3.584 (5)
K1—O2^viii	2.844 (9)	K2—Si1^xiii	3.735 (3)
K1—O2^vi	2.8629 (6)	Si1—O1^xiv	1.615 (5)
K1—O2^i	2.8629 (6)	Si1—O1^xv	1.615 (5)
K1—O1^viii	2.887 (8)	Si1—O2	1.629 (9)
K1—O1^ix	2.887 (8)	Si1—O3	1.648 (3)
O2—Yb1—O2^i	180.0	O1^x—K2—O2^xii	66.69 (13)
O2—Yb1—O1	92.5 (2)	O1^xi—K2—O2^xii	66.69 (13)
O2^i—Yb1—O1	87.5 (2)	O1^ii—K2—O2^xii	144.46 (14)
O2—Yb1—O1^ii	92.5 (2)	O2^i—K2—O2^xii	106.7 (3)
O2^i—Yb1—O1^ii	87.5 (2)	O1—K2—O3^i	110.49 (13)
O1—Yb1—O1^ii	86.8 (3)	O1^x—K2—O3^i	110.49 (13)
O2—Yb1—O1^iii	87.5 (2)	O1^xi—K2—O3^i	110.49 (13)
O2^i—Yb1—O1^iii	92.5 (2)	O1^ii—K2—O3^i	110.49 (13)
O1—Yb1—O1^iii	93.2 (3)	O2^i—K2—O3^i	53.34 (17)
O1^ii—Yb1—O1^iii	180.00 (19)	O2^xii—K2—O3^i	53.34 (17)
O2—Yb1—O1^i	87.5 (2)	O1—K2—Yb1^xii	137.39 (11)
O2^i—Yb1—O1^i	92.5 (2)	O1^x—K2—Yb1^xii	39.65 (10)
O1—Yb1—O1^i	180.0 (2)	O1^xi—K2—Yb1^xii	39.65 (10)
O1^ii—Yb1—O1^i	93.2 (3)	O1^ii—K2—Yb1^xii	137.39 (11)
O1^iii—Yb1—O1^i	86.8 (3)	O2^i—K2—Yb1^xii	146.13 (19)
O2—Yb1—K2^i	54.4 (2)	O2^xii—K2—Yb1^xii	39.45 (16)
O2^i—Yb1—K2^i	125.7 (2)	O3^i—K2—Yb1^xii	92.79 (6)
O1—Yb1—K2^i	127.95 (13)	O1—K2—Yb1	39.65 (10)
O1^ii—Yb1—K2^i	127.95 (13)	O1^x—K2—Yb1	137.39 (11)
O1^iii—Yb1—K2^i	52.05 (13)	O1^xi—K2—Yb1	137.39 (11)
O1^i—Yb1—K2^i	52.05 (13)	O1^ii—K2—Yb1	39.65 (10)
O2—Yb1—K2	125.7 (2)	O2^i—K2—Yb1	39.45 (16)
O2^i—Yb1—K2	54.3 (2)	O2^xii—K2—Yb1	146.13 (19)
O1—Yb1—K2	52.05 (13)	O3^i—K2—Yb1	92.79 (6)
O1^ii—Yb1—K2	52.05 (13)	Yb1^xii—K2—Yb1	174.42 (11)
O1^iii—Yb1—K2	127.95 (13)	O1—K2—Si1^i	88.16 (11)
O1^i—Yb1—K2	127.95 (13)	O1^x—K2—Si1^i	130.94 (16)
K2^i—Yb1—K2	180.0	O1^xi—K2—Si1^i	130.94 (16)
O2—Yb1—K1^iv	54.5 (2)	O1^ii—K2—Si1^i	88.16 (11)
O2^i—Yb1—K1^iv	125.5 (2)	O2^i—K2—Si1^i	26.22 (17)
O1—Yb1—K1^iv	55.61 (18)	O2^xii—K2—Si1^i	80.46 (18)
O1^ii—Yb1—K1^iv	55.61 (18)	O3^i—K2—Si1^i	27.12 (5)
O1^iii—Yb1—K1^iv	124.39 (18)	Yb1^xii—K2—Si1^i	119.91 (10)
O1^i—Yb1—K1^iv	124.39 (18)	Yb1—K2—Si1^i	65.67 (5)
K2^i—Yb1—K1^iv	108.86 (7)	O1—K2—Si1^xii	130.94 (16)
K2—Yb1—K1^iv	71.14 (7)	O1^x—K2—Si1^xii	88.16 (11)
O2—Yb1—K1^v	125.5 (2)	O1^xi—K2—Si1^xii	88.16 (11)
O2^i—Yb1—K1^v	54.5 (2)	O1^ii—K2—Si1^xii	130.94 (16)
O1—Yb1—K1^v	124.39 (18)	O2^i—K2—Si1^xii	80.46 (18)
O1^ii—Yb1—K1^v	124.39 (18)	O2^xii—K2—Si1^xii	26.22 (17)
O1^iii—Yb1—K1^v	55.61 (18)	O3^i—K2—Si1^xii	27.12 (5)
O1^i—Yb1—K1^v	55.61 (18)	Yb1^xii—K2—Si1^xii	65.67 (5)
K2^i—Yb1—K1^v	71.14 (7)	Yb1—K2—Si1^xii	119.91 (10)
K2—Yb1—K1^v	108.86 (7)	Si1^i—K2—Si1^xii	54.25 (10)
K1^iv—Yb1—K1^v	180.00 (5)	O1—K2—Si1^xiii	126.15 (18)
O2—Yb1—K1^i	53.23 (4)	O1^x—K2—Si1^xiii	22.99 (10)
O2^i—Yb1—K1^i	126.77 (4)	O1^xi—K2—Si1^xiii	86.00 (15)
O1—Yb1—K1^i	127.32 (19)	O1^ii—K2—Si1^xiii	74.87 (11)
O1^ii—Yb1—K1^i	60.45 (12)	O2^i—K2—Si1^xiii	129.27 (4)
O1^iii—Yb1—K1^i	119.55 (12)	O2^xii—K2—Si1^xiii	86.05 (11)
O1^i—Yb1—K1^i	52.68 (19)	O3^i—K2—Si1^xiii	118.19 (8)
K2^i—Yb1—K1^i	67.50 (4)	Yb1^xii—K2—Si1^xiii	62.62 (4)
K2—Yb1—K1^i	112.50 (4)	Yb1—K2—Si1^xiii	114.45 (5)
K1^iv—Yb1—K1^i	71.72 (4)	Si1^i—K2—Si1^xiii	128.31 (8)
K1^v—Yb1—K1^i	108.28 (4)	Si1^xii—K2—Si1^xiii	102.77 (6)
O2—Yb1—K1^vi	53.23 (4)	O1^xiv—Si1—O1^xv	111.1 (5)
O2^i—Yb1—K1^vi	126.77 (4)	O1^xiv—Si1—O2	110.6 (3)
O1—Yb1—K1^vi	60.45 (12)	O1^xv—Si1—O2	110.6 (3)
O1^ii—Yb1—K1^vi	127.32 (19)	O1^xiv—Si1—O3	109.4 (3)
O1^iii—Yb1—K1^vi	52.68 (19)	O1^xv—Si1—O3	109.4 (3)
O1^i—Yb1—K1^vi	119.55 (12)	O2—Si1—O3	105.6 (6)
K2^i—Yb1—K1^vi	67.50 (4)	O1^xiv—Si1—K1^iv	75.51 (18)
K2—Yb1—K1^vi	112.50 (4)	O1^xv—Si1—K1^iv	75.51 (18)
K1^iv—Yb1—K1^vi	71.72 (4)	O2—Si1—K1^iv	64.7 (3)
K1^v—Yb1—K1^vi	108.28 (4)	O3—Si1—K1^iv	170.3 (5)
K1^i—Yb1—K1^vi	106.26 (7)	O1^xiv—Si1—K1^vi	154.76 (19)
O1—K1—O1^vii	55.9 (2)	O1^xv—Si1—K1^vi	59.7 (3)
O1—K1—O2^viii	117.7 (2)	O2—Si1—K1^vi	58.84 (9)
O1^vii—K1—O2^viii	117.7 (2)	O3—Si1—K1^vi	95.8 (2)
O1—K1—O2^vi	120.9 (2)	K1^iv—Si1—K1^vi	79.33 (5)
O1^vii—K1—O2^vi	65.06 (15)	O1^xiv—Si1—K1^i	59.7 (3)
O2^viii—K1—O2^vi	87.13 (17)	O1^xv—Si1—K1^i	154.76 (19)
O1—K1—O2^i	65.06 (15)	O2—Si1—K1^i	58.84 (9)
O1^vii—K1—O2^i	120.9 (2)	O3—Si1—K1^i	95.8 (2)
O2^viii—K1—O2^i	87.13 (17)	K1^iv—Si1—K1^i	79.33 (5)
O2^vi—K1—O2^i	173.3 (3)	K1^vi—Si1—K1^i	117.47 (18)
O1—K1—O1^viii	173.7 (2)	O1^xiv—Si1—K1^xv	57.6 (3)
O1^vii—K1—O1^viii	119.90 (2)	O1^xv—Si1—K1^xv	57.6 (3)
O2^viii—K1—O1^viii	68.03 (13)	O2—Si1—K1^xv	147.4 (3)
O2^vi—K1—O1^viii	55.27 (15)	O3—Si1—K1^xv	107.1 (5)
O2^i—K1—O1^viii	119.1 (2)	K1^iv—Si1—K1^xv	82.67 (8)
O1—K1—O1^ix	119.90 (2)	K1^vi—Si1—K1^xv	117.21 (9)
O1^vii—K1—O1^ix	173.7 (2)	K1^i—Si1—K1^xv	117.21 (9)
O2^viii—K1—O1^ix	68.03 (13)	O1^xiv—Si1—K2^i	124.4 (3)
O2^vi—K1—O1^ix	119.1 (2)	O1^xv—Si1—K2^i	124.4 (3)
O2^i—K1—O1^ix	55.27 (15)	O2—Si1—K2^i	50.2 (3)
O1^viii—K1—O1^ix	63.84 (19)	O3—Si1—K2^i	55.3 (4)
O1—K1—Si1^viii	90.49 (12)	K1^iv—Si1—K2^i	114.92 (11)
O1^vii—K1—Si1^viii	90.49 (12)	K1^vi—Si1—K2^i	68.79 (10)
O2^viii—K1—Si1^viii	31.18 (18)	K1^i—Si1—K2^i	68.79 (10)
O2^vi—K1—Si1^viii	88.45 (18)	K1^xv—Si1—K2^i	162.41 (8)
O2^i—K1—Si1^viii	88.45 (18)	O1^xiv—Si1—K2^xvi	41.58 (18)
O1^viii—K1—Si1^viii	94.27 (12)	O1^xv—Si1—K2^xvi	120.9 (3)
O1^ix—K1—Si1^viii	94.27 (12)	O2—Si1—K2^xvi	127.31 (11)
O1—K1—O1^vi	88.60 (17)	O3—Si1—K2^xvi	68.2 (3)
O1^vii—K1—O1^vi	65.06 (15)	K1^iv—Si1—K2^xvi	117.08 (6)
O2^viii—K1—O1^vi	52.63 (13)	K1^vi—Si1—K2^xvi	163.54 (6)
O2^vi—K1—O1^vi	64.34 (19)	K1^i—Si1—K2^xvi	69.57 (6)
O2^i—K1—O1^vi	114.4 (2)	K1^xv—Si1—K2^xvi	66.83 (9)
O1^viii—K1—O1^vi	93.50 (13)	K2^i—Si1—K2^xvi	102.77 (6)
O1^ix—K1—O1^vi	120.61 (10)	O1^xiv—Si1—K2^xv	120.9 (3)
Si1^viii—K1—O1^vi	29.85 (9)	O1^xv—Si1—K2^xv	41.58 (18)
O1—K1—O1^iii	65.06 (15)	O2—Si1—K2^xv	127.31 (11)
O1^vii—K1—O1^iii	88.60 (17)	O3—Si1—K2^xv	68.2 (3)
O2^viii—K1—O1^iii	52.63 (13)	K1^iv—Si1—K2^xv	117.08 (6)
O2^vi—K1—O1^iii	114.4 (2)	K1^vi—Si1—K2^xv	69.57 (6)
O2^i—K1—O1^iii	64.34 (19)	K1^i—Si1—K2^xv	163.54 (6)
O1^viii—K1—O1^iii	120.61 (10)	K1^xv—Si1—K2^xv	66.83 (9)
O1^ix—K1—O1^iii	93.50 (13)	K2^i—Si1—K2^xv	102.77 (6)
Si1^viii—K1—O1^iii	29.85 (9)	K2^xvi—Si1—K2^xv	99.84 (11)
O1^vi—K1—O1^iii	50.2 (2)	Si1^xv—O1—Yb1	156.1 (3)
O1—K1—Si1^vi	145.82 (15)	Si1^xv—O1—K2	115.4 (2)
O1^vii—K1—Si1^vi	91.50 (13)	Yb1—O1—K2	88.30 (16)
O2^viii—K1—Si1^vi	84.68 (11)	Si1^xv—O1—K1	93.7 (3)
O2^vi—K1—Si1^vi	29.13 (17)	Yb1—O1—K1	88.89 (17)
O2^i—K1—Si1^vi	146.4 (2)	K2—O1—K1	89.07 (16)
O1^viii—K1—Si1^vi	28.87 (12)	Si1^xv—O1—K1^iv	91.5 (3)
O1^ix—K1—Si1^vi	91.62 (15)	Yb1—O1—K1^iv	85.0 (2)
Si1^viii—K1—Si1^vi	100.67 (5)	K2—O1—K1^iv	92.0 (2)
O1^vi—K1—Si1^vi	85.68 (13)	K1—O1—K1^iv	173.7 (2)
O1^iii—K1—Si1^vi	130.49 (10)	Si1^xv—O1—K1^vi	74.64 (19)
O1—K1—Si1^i	91.50 (13)	Yb1—O1—K1^vi	81.59 (14)
O1^vii—K1—Si1^i	145.82 (15)	K2—O1—K1^vi	169.87 (19)
O2^viii—K1—Si1^i	84.68 (11)	K1—O1—K1^vi	91.40 (17)
O2^vi—K1—Si1^i	146.4 (2)	K1^iv—O1—K1^vi	86.50 (13)
O2^i—K1—Si1^i	29.13 (17)	Si1—O2—Yb1	170.2 (5)
O1^viii—K1—Si1^i	91.62 (15)	Si1—O2—K2^i	103.6 (4)
O1^ix—K1—Si1^i	28.87 (12)	Yb1—O2—K2^i	86.2 (3)
Si1^viii—K1—Si1^i	100.67 (5)	Si1—O2—K1^iv	84.1 (3)
O1^vi—K1—Si1^i	130.49 (10)	Yb1—O2—K1^iv	86.1 (3)
O1^iii—K1—Si1^i	85.68 (13)	K2^i—O2—K1^iv	172.3 (3)
Si1^vi—K1—Si1^i	117.47 (18)	Si1—O2—K1^vi	92.03 (18)
O1—K2—O1^x	139.0 (3)	Yb1—O2—K1^vi	88.45 (17)
O1—K2—O1^xi	97.85 (19)	K2^i—O2—K1^vi	86.92 (17)
O1^x—K2—O1^xi	67.6 (3)	K1^iv—O2—K1^vi	92.87 (17)
O1—K2—O1^ii	67.6 (3)	Si1—O2—K1^i	92.03 (18)
O1^x—K2—O1^ii	97.8 (2)	Yb1—O2—K1^i	88.45 (17)
O1^xi—K2—O1^ii	139.0 (3)	K2^i—O2—K1^i	86.92 (17)
O1—K2—O2^i	66.69 (13)	K1^iv—O2—K1^i	92.87 (17)
O1^x—K2—O2^i	144.46 (14)	K1^vi—O2—K1^i	173.3 (3)
O1^xi—K2—O2^i	144.46 (14)	Si1^xvii—O3—Si1	164.9 (9)
O1^ii—K2—O2^i	66.69 (13)	Si1^xvii—O3—K2^i	97.5 (5)
O1—K2—O2^xii	144.46 (14)	Si1—O3—K2^i	97.5 (5)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, y, z; (iii) x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1, −y, −z+1; (vii) −x+1, y, z; (viii) x+1/2, y+1/2, z; (ix) −x+1/2, y+1/2, z; (x) −x, y, −z+1/2; (xi) x, y, −z+1/2; (xii) −x, −y, z−1/2; (xiii) −x−1/2, −y−1/2, z−1/2; (xiv) x−1/2, −y−1/2, −z+1; (xv) −x+1/2, −y−1/2, −z+1; (xvi) −x−1/2, −y−1/2, −z+1; (xvii) x, y, −z+3/2.

(133_K)

Crystal data

K3O7Si2Yb	Dx = 3.879 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1204 reflections
a = 5.7090 (6) Å	θ = 7.1–29.2°
b = 9.9018 (10) Å	µ = 13.81 mm^−1
c = 13.8876 (13) Å	T = 133 K
V = 785.06 (14) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	474 reflections with I > 2σ(I)
ω scans	Rint = 0.041
Absorption correction: analytical CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −7→6
2682 measured reflections	k = −10→12
540 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + 0.4229P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.019	(Δ/σ)max < 0.001
wR(F^2) = 0.035	Δρmax = 0.99 e Å^−3
S = 1.12	Δρmin = −1.16 e Å^−3
540 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
29 parameters	Extinction coefficient: 0.00302 (13)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00215 (14)
K1	0.500000	0.1729 (3)	0.40752 (10)	0.0062 (3)
K2	0.000000	0.0165 (3)	0.250000	0.0078 (5)
Si1	0.000000	−0.3384 (4)	0.63242 (13)	0.0022 (3)
O1	0.2682 (11)	−0.0798 (5)	0.3992 (3)	0.0095 (12)
O2	0.000000	−0.1879 (7)	0.5874 (6)	0.0037 (19)
O3	0.000000	−0.3174 (12)	0.750000	0.0083 (16)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00194 (15)	0.00194 (15)	0.0026 (2)	0.000	0.000	0.000
K1	0.0056 (4)	0.0056 (4)	0.0075 (6)	0.000	0.000	0.000
K2	0.0096 (7)	0.0096 (7)	0.0042 (8)	0.000	0.000	0.000
Si1	0.0019 (5)	0.0019 (5)	0.0028 (7)	0.000	0.000	0.000
O1	0.0060 (14)	0.0060 (14)	0.017 (2)	0.000	0.000	0.000
O2	0.004 (3)	0.004 (3)	0.004 (3)	0.000	0.000	0.000
O3	0.011 (2)	0.011 (2)	0.002 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O1^i	2.220 (5)	K1—Si1^vii	3.125 (3)
Yb1—O1^ii	2.220 (5)	K1—O1^viii	3.132 (5)
Yb1—O1^iii	2.220 (5)	K1—O1^ii	3.132 (5)
Yb1—O1	2.220 (5)	K1—Si1^viii	3.338 (3)
Yb1—O2^iii	2.221 (7)	K1—Si1^iii	3.338 (3)
Yb1—O2	2.221 (7)	K2—O1	2.747 (5)
Yb1—K2	3.4757 (4)	K2—O1^x	2.747 (5)
Yb1—K2^iii	3.4757 (4)	K2—O1^xi	2.747 (5)
Yb1—K1^iv	3.484 (3)	K2—O1^i	2.747 (5)
Yb1—K1^v	3.484 (3)	K2—O2^iii	2.824 (8)
Yb1—K1	3.5676 (16)	K2—O2^xii	2.824 (8)
Yb1—K1^iii	3.5676 (16)	K2—O3^iii	2.980 (13)
K1—O1^vi	2.832 (8)	K2—Si1^iii	3.581 (5)
K1—O1	2.832 (8)	K2—Si1^xii	3.581 (5)
K1—O2^vii	2.854 (8)	K2—Si1^xiii	3.732 (3)
K1—O2^viii	2.8592 (6)	Si1—O1^xiv	1.613 (5)
K1—O2^iii	2.8592 (6)	Si1—O1^xv	1.613 (5)
K1—O1^vii	2.891 (8)	Si1—O2	1.616 (8)
K1—O1^ix	2.891 (8)	Si1—O3	1.646 (2)
O1^i—Yb1—O1^ii	180.0	O1^x—K2—O2^xii	66.76 (12)
O1^i—Yb1—O1^iii	92.8 (3)	O1^xi—K2—O2^xii	66.76 (12)
O1^ii—Yb1—O1^iii	87.2 (3)	O1^i—K2—O2^xii	144.23 (14)
O1^i—Yb1—O1	87.2 (3)	O2^iii—K2—O2^xii	106.1 (3)
O1^ii—Yb1—O1	92.8 (3)	O1—K2—O3^iii	110.30 (13)
O1^iii—Yb1—O1	180.0	O1^x—K2—O3^iii	110.30 (13)
O1^i—Yb1—O2^iii	87.31 (19)	O1^xi—K2—O3^iii	110.30 (13)
O1^ii—Yb1—O2^iii	92.69 (19)	O1^i—K2—O3^iii	110.30 (13)
O1^iii—Yb1—O2^iii	92.69 (19)	O2^iii—K2—O3^iii	53.07 (15)
O1—Yb1—O2^iii	87.31 (19)	O2^xii—K2—O3^iii	53.07 (15)
O1^i—Yb1—O2	92.69 (19)	O1—K2—Yb1^xii	137.49 (10)
O1^ii—Yb1—O2	87.31 (19)	O1^x—K2—Yb1^xii	39.67 (10)
O1^iii—Yb1—O2	87.31 (19)	O1^xi—K2—Yb1^xii	39.67 (10)
O1—Yb1—O2	92.69 (19)	O1^i—K2—Yb1^xii	137.49 (10)
O2^iii—Yb1—O2	180.0	O2^iii—K2—Yb1^xii	145.76 (17)
O1^i—Yb1—K2	52.18 (12)	O2^xii—K2—Yb1^xii	39.62 (15)
O1^ii—Yb1—K2	127.82 (12)	O3^iii—K2—Yb1^xii	92.69 (5)
O1^iii—Yb1—K2	127.82 (12)	O1—K2—Yb1	39.67 (10)
O1—Yb1—K2	52.18 (12)	O1^x—K2—Yb1	137.49 (10)
O2^iii—Yb1—K2	54.2 (2)	O1^xi—K2—Yb1	137.49 (10)
O2—Yb1—K2	125.8 (2)	O1^i—K2—Yb1	39.67 (10)
O1^i—Yb1—K2^iii	127.82 (12)	O2^iii—K2—Yb1	39.62 (15)
O1^ii—Yb1—K2^iii	52.18 (12)	O2^xii—K2—Yb1	145.76 (17)
O1^iii—Yb1—K2^iii	52.18 (12)	O3^iii—K2—Yb1	92.69 (5)
O1—Yb1—K2^iii	127.82 (12)	Yb1^xii—K2—Yb1	174.62 (10)
O2^iii—Yb1—K2^iii	125.8 (2)	O1—K2—Si1^iii	87.98 (11)
O2—Yb1—K2^iii	54.2 (2)	O1^x—K2—Si1^iii	130.74 (15)
K2—Yb1—K2^iii	180.0	O1^xi—K2—Si1^iii	130.74 (15)
O1^i—Yb1—K1^iv	55.73 (17)	O1^i—K2—Si1^iii	87.98 (11)
O1^ii—Yb1—K1^iv	124.27 (17)	O2^iii—K2—Si1^iii	25.94 (15)
O1^iii—Yb1—K1^iv	124.27 (17)	O2^xii—K2—Si1^iii	80.20 (17)
O1—Yb1—K1^iv	55.73 (17)	O3^iii—K2—Si1^iii	27.13 (5)
O2^iii—Yb1—K1^iv	125.2 (2)	Yb1^xii—K2—Si1^iii	119.82 (9)
O2—Yb1—K1^iv	54.8 (2)	Yb1—K2—Si1^iii	65.56 (4)
K2—Yb1—K1^iv	71.06 (6)	O1—K2—Si1^xii	130.74 (15)
K2^iii—Yb1—K1^iv	108.94 (6)	O1^x—K2—Si1^xii	87.98 (11)
O1^i—Yb1—K1^v	124.27 (17)	O1^xi—K2—Si1^xii	87.98 (11)
O1^ii—Yb1—K1^v	55.73 (17)	O1^i—K2—Si1^xii	130.74 (15)
O1^iii—Yb1—K1^v	55.73 (17)	O2^iii—K2—Si1^xii	80.20 (17)
O1—Yb1—K1^v	124.27 (17)	O2^xii—K2—Si1^xii	25.94 (15)
O2^iii—Yb1—K1^v	54.8 (2)	O3^iii—K2—Si1^xii	27.13 (5)
O2—Yb1—K1^v	125.2 (2)	Yb1^xii—K2—Si1^xii	65.56 (4)
K2—Yb1—K1^v	108.94 (6)	Yb1—K2—Si1^xii	119.82 (9)
K2^iii—Yb1—K1^v	71.06 (6)	Si1^iii—K2—Si1^xii	54.26 (9)
K1^iv—Yb1—K1^v	180.00 (4)	O1—K2—Si1^xiii	126.34 (17)
O1^i—Yb1—K1	119.71 (12)	O1^x—K2—Si1^xiii	23.01 (10)
O1^ii—Yb1—K1	60.29 (12)	O1^xi—K2—Si1^xiii	86.12 (15)
O1^iii—Yb1—K1	127.46 (18)	O1^i—K2—Si1^xiii	74.91 (10)
O1—Yb1—K1	52.54 (18)	O2^iii—K2—Si1^xiii	129.33 (4)
O2^iii—Yb1—K1	53.23 (4)	O2^xii—K2—Si1^xiii	86.23 (10)
O2—Yb1—K1	126.77 (4)	O3^iii—K2—Si1^xiii	118.20 (7)
K2—Yb1—K1	67.53 (3)	Yb1^xii—K2—Si1^xiii	62.66 (3)
K2^iii—Yb1—K1	112.47 (3)	Yb1—K2—Si1^xiii	114.52 (5)
K1^iv—Yb1—K1	108.26 (4)	Si1^iii—K2—Si1^xiii	128.33 (7)
K1^v—Yb1—K1	71.74 (4)	Si1^xii—K2—Si1^xiii	102.77 (5)
O1^i—Yb1—K1^iii	60.29 (12)	O1^xiv—Si1—O1^xv	110.3 (5)
O1^ii—Yb1—K1^iii	119.71 (12)	O1^xiv—Si1—O2	111.0 (3)
O1^iii—Yb1—K1^iii	52.54 (18)	O1^xv—Si1—O2	111.0 (3)
O1—Yb1—K1^iii	127.46 (18)	O1^xiv—Si1—O3	109.5 (3)
O2^iii—Yb1—K1^iii	126.77 (4)	O1^xv—Si1—O3	109.5 (3)
O2—Yb1—K1^iii	53.23 (4)	O2—Si1—O3	105.5 (6)
K2—Yb1—K1^iii	112.47 (3)	O1^xiv—Si1—K1^iv	75.28 (18)
K2^iii—Yb1—K1^iii	67.53 (3)	O1^xv—Si1—K1^iv	75.28 (18)
K1^iv—Yb1—K1^iii	71.74 (4)	O2—Si1—K1^iv	65.2 (3)
K1^v—Yb1—K1^iii	108.26 (4)	O3—Si1—K1^iv	170.7 (5)
K1—Yb1—K1^iii	180.0	O1^xiv—Si1—K1^viii	154.59 (19)
O1^vi—K1—O1	55.71 (19)	O1^xv—Si1—K1^viii	60.0 (3)
O1^vi—K1—O2^vii	117.55 (19)	O2—Si1—K1^viii	58.87 (8)
O1—K1—O2^vii	117.55 (19)	O3—Si1—K1^viii	95.9 (2)
O1^vi—K1—O2^viii	65.19 (13)	K1^iv—Si1—K1^viii	79.42 (5)
O1—K1—O2^viii	120.9 (2)	O1^xiv—Si1—K1^iii	60.0 (3)
O2^vii—K1—O2^viii	87.33 (16)	O1^xv—Si1—K1^iii	154.59 (19)
O1^vi—K1—O2^iii	120.9 (2)	O2—Si1—K1^iii	58.87 (8)
O1—K1—O2^iii	65.19 (13)	O3—Si1—K1^iii	95.9 (2)
O2^vii—K1—O2^iii	87.33 (16)	K1^iv—Si1—K1^iii	79.42 (5)
O2^viii—K1—O2^iii	173.4 (3)	K1^viii—Si1—K1^iii	117.57 (16)
O1^vi—K1—O1^vii	119.95 (2)	O1^xiv—Si1—K1^xv	57.3 (3)
O1—K1—O1^vii	173.79 (19)	O1^xv—Si1—K1^xv	57.3 (3)
O2^vii—K1—O1^vii	68.01 (12)	O2—Si1—K1^xv	147.8 (3)
O2^viii—K1—O1^vii	55.13 (13)	O3—Si1—K1^xv	106.7 (4)
O2^iii—K1—O1^vii	119.1 (2)	K1^iv—Si1—K1^xv	82.54 (7)
O1^vi—K1—O1^ix	173.79 (19)	K1^viii—Si1—K1^xv	117.18 (8)
O1—K1—O1^ix	119.948 (19)	K1^iii—Si1—K1^xv	117.18 (8)
O2^vii—K1—O1^ix	68.01 (12)	O1^xiv—Si1—K2^iii	124.9 (3)
O2^viii—K1—O1^ix	119.1 (2)	O1^xv—Si1—K2^iii	124.9 (3)
O2^iii—K1—O1^ix	55.13 (13)	O2—Si1—K2^iii	49.9 (3)
O1^vii—K1—O1^ix	63.97 (18)	O3—Si1—K2^iii	55.6 (4)
O1^vi—K1—Si1^vii	90.54 (11)	K1^iv—Si1—K2^iii	115.09 (10)
O1—K1—Si1^vii	90.54 (11)	K1^viii—Si1—K2^iii	68.83 (9)
O2^vii—K1—Si1^vii	30.93 (16)	K1^iii—Si1—K2^iii	68.83 (9)
O2^viii—K1—Si1^vii	88.70 (17)	K1^xv—Si1—K2^iii	162.38 (7)
O2^iii—K1—Si1^vii	88.70 (17)	O1^xiv—Si1—K2^xvi	41.75 (17)
O1^vii—K1—Si1^vii	94.02 (11)	O1^xv—Si1—K2^xvi	120.6 (3)
O1^ix—K1—Si1^vii	94.02 (11)	O2—Si1—K2^xvi	127.23 (10)
O1^vi—K1—O1^viii	65.01 (15)	O3—Si1—K2^xvi	68.0 (2)
O1—K1—O1^viii	88.42 (17)	K1^iv—Si1—K2^xvi	117.01 (5)
O2^vii—K1—O1^viii	52.54 (12)	K1^viii—Si1—K2^xvi	163.52 (5)
O2^viii—K1—O1^viii	64.69 (19)	K1^iii—Si1—K2^xvi	69.55 (5)
O2^iii—K1—O1^viii	114.6 (2)	K1^xv—Si1—K2^xvi	66.81 (8)
O1^vii—K1—O1^viii	93.43 (13)	K2^iii—Si1—K2^xvi	102.77 (5)
O1^ix—K1—O1^viii	120.50 (9)	O1^xiv—Si1—K2^xv	120.6 (3)
Si1^vii—K1—O1^viii	29.87 (9)	O1^xv—Si1—K2^xv	41.75 (17)
O1^vi—K1—O1^ii	88.42 (17)	O2—Si1—K2^xv	127.23 (10)
O1—K1—O1^ii	65.01 (15)	O3—Si1—K2^xv	68.0 (2)
O2^vii—K1—O1^ii	52.54 (12)	K1^iv—Si1—K2^xv	117.01 (5)
O2^viii—K1—O1^ii	114.6 (2)	K1^viii—Si1—K2^xv	69.55 (5)
O2^iii—K1—O1^ii	64.69 (19)	K1^iii—Si1—K2^xv	163.52 (5)
O1^vii—K1—O1^ii	120.50 (9)	K1^xv—Si1—K2^xv	66.81 (8)
O1^ix—K1—O1^ii	93.43 (13)	K2^iii—Si1—K2^xv	102.77 (5)
Si1^vii—K1—O1^ii	29.87 (9)	K2^xvi—Si1—K2^xv	99.81 (9)
O1^viii—K1—O1^ii	50.0 (2)	Si1^xv—O1—Yb1	156.4 (3)
O1^vi—K1—Si1^viii	91.56 (11)	Si1^xv—O1—K2	115.2 (2)
O1—K1—Si1^viii	145.73 (14)	Yb1—O1—K2	88.15 (15)
O2^vii—K1—Si1^viii	84.73 (10)	Si1^xv—O1—K1	94.1 (3)
O2^viii—K1—Si1^viii	28.93 (15)	Yb1—O1—K1	88.99 (17)
O2^iii—K1—Si1^viii	146.3 (2)	K2—O1—K1	89.13 (15)
O1^vii—K1—Si1^viii	28.89 (11)	Si1^xv—O1—K1^iv	91.1 (2)
O1^ix—K1—Si1^viii	91.74 (14)	Yb1—O1—K1^iv	84.9 (2)
Si1^vii—K1—Si1^viii	100.57 (5)	K2—O1—K1^iv	91.65 (19)
O1^viii—K1—Si1^viii	85.73 (13)	K1—O1—K1^iv	173.79 (19)
O1^ii—K1—Si1^viii	130.42 (10)	Si1^xv—O1—K1^viii	74.85 (18)
O1^vi—K1—Si1^iii	145.73 (14)	Yb1—O1—K1^viii	81.70 (14)
O1—K1—Si1^iii	91.56 (11)	K2—O1—K1^viii	169.81 (19)
O2^vii—K1—Si1^iii	84.73 (10)	K1—O1—K1^viii	91.58 (16)
O2^viii—K1—Si1^iii	146.3 (2)	K1^iv—O1—K1^viii	86.57 (13)
O2^iii—K1—Si1^iii	28.93 (15)	Si1—O2—Yb1	169.6 (5)
O1^vii—K1—Si1^iii	91.74 (14)	Si1—O2—K2^iii	104.2 (4)
O1^ix—K1—Si1^iii	28.89 (11)	Yb1—O2—K2^iii	86.2 (2)
Si1^vii—K1—Si1^iii	100.57 (5)	Si1—O2—K1^iv	83.8 (3)
O1^viii—K1—Si1^iii	130.42 (10)	Yb1—O2—K1^iv	85.8 (3)
O1^ii—K1—Si1^iii	85.73 (13)	K2^iii—O2—K1^iv	172.0 (3)
Si1^viii—K1—Si1^iii	117.56 (16)	Si1—O2—K1^viii	92.20 (16)
O1—K2—O1^x	139.4 (3)	Yb1—O2—K1^viii	88.28 (16)
O1—K2—O1^xi	97.92 (19)	K2^iii—O2—K1^viii	87.09 (16)
O1^x—K2—O1^xi	67.8 (3)	K1^iv—O2—K1^viii	92.67 (16)
O1—K2—O1^i	67.8 (3)	Si1—O2—K1^iii	92.20 (16)
O1^x—K2—O1^i	97.92 (19)	Yb1—O2—K1^iii	88.28 (16)
O1^xi—K2—O1^i	139.4 (3)	K2^iii—O2—K1^iii	87.09 (16)
O1—K2—O2^iii	66.77 (12)	K1^iv—O2—K1^iii	92.67 (16)
O1^x—K2—O2^iii	144.23 (14)	K1^viii—O2—K1^iii	173.4 (3)
O1^xi—K2—O2^iii	144.23 (14)	Si1—O3—Si1^xvii	165.5 (9)
O1^i—K2—O2^iii	66.76 (12)	Si1—O3—K2^iii	97.2 (4)
O1—K2—O2^xii	144.23 (14)	Si1^xvii—O3—K2^iii	97.2 (4)

Symmetry codes: (i) −x, y, z; (ii) x, −y, −z+1; (iii) −x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1, y, z; (vii) x+1/2, y+1/2, z; (viii) −x+1, −y, −z+1; (ix) −x+1/2, y+1/2, z; (x) −x, y, −z+1/2; (xi) x, y, −z+1/2; (xii) −x, −y, z−1/2; (xiii) −x−1/2, −y−1/2, z−1/2; (xiv) x−1/2, −y−1/2, −z+1; (xv) −x+1/2, −y−1/2, −z+1; (xvi) −x−1/2, −y−1/2, −z+1; (xvii) x, y, −z+3/2.

(143_K)

Crystal data

K3O7Si2Yb	Dx = 3.868 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1211 reflections
a = 5.7166 (6) Å	θ = 4.1–29.4°
b = 9.9059 (10) Å	µ = 13.77 mm^−1
c = 13.9043 (14) Å	T = 143 K
V = 787.38 (14) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	476 reflections with I > 2σ(I)
ω scans	Rint = 0.039
Absorption correction: analytical CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −7→7
2677 measured reflections	k = −10→12
539 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0068P)^2 + 2.2016P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.019	(Δ/σ)max < 0.001
wR(F^2) = 0.037	Δρmax = 0.99 e Å^−3
S = 1.08	Δρmin = −0.82 e Å^−3
539 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
29 parameters	Extinction coefficient: 0.00313 (14)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00227 (14)
K1	0.500000	0.1731 (3)	0.40764 (11)	0.0063 (3)
K2	0.000000	0.0162 (3)	0.250000	0.0080 (5)
Si1	0.000000	−0.3377 (4)	0.63232 (13)	0.0024 (3)
O1	0.2660 (11)	−0.0809 (5)	0.3992 (3)	0.0089 (11)
O2	0.000000	−0.1879 (7)	0.5867 (6)	0.0044 (19)
O3	0.000000	−0.3175 (13)	0.750000	0.0103 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00194 (15)	0.00194 (15)	0.0029 (2)	0.000	0.000	0.000
K1	0.0052 (4)	0.0052 (4)	0.0084 (6)	0.000	0.000	0.000
K2	0.0101 (7)	0.0101 (7)	0.0039 (8)	0.000	0.000	0.000
Si1	0.0027 (5)	0.0027 (5)	0.0017 (7)	0.000	0.000	0.000
O1	0.0077 (14)	0.0077 (14)	0.011 (2)	0.000	0.000	0.000
O2	0.006 (3)	0.002 (3)	0.006 (3)	0.000	0.000	0.000
O3	0.014 (3)	0.014 (3)	0.004 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O1^i	2.218 (5)	K1—Si1^vi	3.126 (3)
Yb1—O1^ii	2.218 (5)	K1—O1^viii	3.136 (5)
Yb1—O1^iii	2.218 (5)	K1—O1^ii	3.136 (5)
Yb1—O1	2.218 (5)	K1—Si1^viii	3.337 (3)
Yb1—O2^iii	2.218 (8)	K1—Si1^iii	3.337 (3)
Yb1—O2	2.218 (8)	K2—O1	2.746 (5)
Yb1—K2^iii	3.4798 (4)	K2—O1^x	2.746 (5)
Yb1—K2	3.4798 (4)	K2—O1^xi	2.746 (5)
Yb1—K1^iv	3.484 (3)	K2—O1^i	2.746 (5)
Yb1—K1^v	3.484 (3)	K2—O2^iii	2.837 (9)
Yb1—K1	3.5720 (17)	K2—O2^xii	2.837 (9)
Yb1—K1^iii	3.5720 (17)	K2—O3^iii	2.985 (14)
K1—O2^vi	2.845 (8)	K2—Si1^iii	3.581 (5)
K1—O1	2.852 (8)	K2—Si1^xii	3.581 (5)
K1—O1^vii	2.852 (8)	K2—Si1^xiii	3.738 (3)
K1—O2^viii	2.8632 (6)	Si1—O2	1.614 (8)
K1—O2^iii	2.8632 (6)	Si1—O1^xiv	1.622 (5)
K1—O1^vi	2.875 (8)	Si1—O1^xv	1.622 (5)
K1—O1^ix	2.875 (8)	Si1—O3	1.649 (3)
O1^i—Yb1—O1^ii	180.0	O1^x—K2—O2^xii	66.76 (12)
O1^i—Yb1—O1^iii	93.4 (3)	O1^xi—K2—O2^xii	66.76 (12)
O1^ii—Yb1—O1^iii	86.6 (3)	O1^i—K2—O2^xii	144.55 (15)
O1^i—Yb1—O1	86.6 (3)	O2^iii—K2—O2^xii	106.3 (3)
O1^ii—Yb1—O1	93.4 (3)	O1—K2—O3^iii	110.50 (13)
O1^iii—Yb1—O1	180.0 (2)	O1^x—K2—O3^iii	110.50 (13)
O1^i—Yb1—O2^iii	87.70 (19)	O1^xi—K2—O3^iii	110.50 (13)
O1^ii—Yb1—O2^iii	92.30 (19)	O1^i—K2—O3^iii	110.50 (13)
O1^iii—Yb1—O2^iii	92.30 (19)	O2^iii—K2—O3^iii	53.16 (16)
O1—Yb1—O2^iii	87.70 (19)	O2^xii—K2—O3^iii	53.16 (16)
O1^i—Yb1—O2	92.30 (19)	O1—K2—Yb1^xii	137.60 (10)
O1^ii—Yb1—O2	87.70 (19)	O1^x—K2—Yb1^xii	39.58 (10)
O1^iii—Yb1—O2	87.70 (19)	O1^xi—K2—Yb1^xii	39.58 (10)
O1—Yb1—O2	92.30 (19)	O1^i—K2—Yb1^xii	137.60 (10)
O2^iii—Yb1—O2	180.0	O2^iii—K2—Yb1^xii	145.80 (18)
O1^i—Yb1—K2^iii	127.92 (12)	O2^xii—K2—Yb1^xii	39.49 (16)
O1^ii—Yb1—K2^iii	52.08 (12)	O3^iii—K2—Yb1^xii	92.64 (5)
O1^iii—Yb1—K2^iii	52.08 (12)	O1—K2—Yb1	39.58 (10)
O1—Yb1—K2^iii	127.92 (12)	O1^x—K2—Yb1	137.60 (10)
O2^iii—Yb1—K2^iii	125.6 (2)	O1^xi—K2—Yb1	137.60 (10)
O2—Yb1—K2^iii	54.4 (2)	O1^i—K2—Yb1	39.58 (10)
O1^i—Yb1—K2	52.08 (12)	O2^iii—K2—Yb1	39.49 (16)
O1^ii—Yb1—K2	127.92 (12)	O2^xii—K2—Yb1	145.80 (18)
O1^iii—Yb1—K2	127.92 (12)	O3^iii—K2—Yb1	92.64 (5)
O1—Yb1—K2	52.08 (12)	Yb1^xii—K2—Yb1	174.71 (11)
O2^iii—Yb1—K2	54.4 (2)	O1—K2—Si1^iii	88.07 (11)
O2—Yb1—K2	125.6 (2)	O1^x—K2—Si1^iii	131.05 (16)
K2^iii—Yb1—K2	180.0	O1^xi—K2—Si1^iii	131.05 (16)
O1^i—Yb1—K1^iv	55.33 (18)	O1^i—K2—Si1^iii	88.07 (11)
O1^ii—Yb1—K1^iv	124.67 (17)	O2^iii—K2—Si1^iii	25.96 (16)
O1^iii—Yb1—K1^iv	124.67 (18)	O2^xii—K2—Si1^iii	80.35 (17)
O1—Yb1—K1^iv	55.33 (18)	O3^iii—K2—Si1^iii	27.19 (5)
O2^iii—Yb1—K1^iv	125.4 (2)	Yb1^xii—K2—Si1^iii	119.84 (9)
O2—Yb1—K1^iv	54.6 (2)	Yb1—K2—Si1^iii	65.45 (4)
K2^iii—Yb1—K1^iv	108.99 (6)	O1—K2—Si1^xii	131.05 (16)
K2—Yb1—K1^iv	71.01 (6)	O1^x—K2—Si1^xii	88.07 (11)
O1^i—Yb1—K1^v	124.67 (18)	O1^xi—K2—Si1^xii	88.07 (11)
O1^ii—Yb1—K1^v	55.33 (17)	O1^i—K2—Si1^xii	131.05 (16)
O1^iii—Yb1—K1^v	55.33 (18)	O2^iii—K2—Si1^xii	80.35 (17)
O1—Yb1—K1^v	124.67 (18)	O2^xii—K2—Si1^xii	25.96 (16)
O2^iii—Yb1—K1^v	54.6 (2)	O3^iii—K2—Si1^xii	27.19 (5)
O2—Yb1—K1^v	125.4 (2)	Yb1^xii—K2—Si1^xii	65.45 (4)
K2^iii—Yb1—K1^v	71.01 (6)	Yb1—K2—Si1^xii	119.84 (9)
K2—Yb1—K1^v	108.99 (6)	Si1^iii—K2—Si1^xii	54.38 (10)
K1^iv—Yb1—K1^v	180.0	O1—K2—Si1^xiii	126.05 (18)
O1^i—Yb1—K1	119.67 (12)	O1^x—K2—Si1^xiii	23.11 (10)
O1^ii—Yb1—K1	60.33 (12)	O1^xi—K2—Si1^xiii	85.82 (15)
O1^iii—Yb1—K1	127.04 (19)	O1^i—K2—Si1^xiii	75.03 (10)
O1—Yb1—K1	52.96 (19)	O2^iii—K2—Si1^xiii	129.34 (4)
O2^iii—Yb1—K1	53.25 (4)	O2^xii—K2—Si1^xiii	86.17 (11)
O2—Yb1—K1	126.75 (4)	O3^iii—K2—Si1^xiii	118.23 (8)
K2^iii—Yb1—K1	112.41 (4)	Yb1^xii—K2—Si1^xiii	62.67 (3)
K2—Yb1—K1	67.59 (4)	Yb1—K2—Si1^xiii	114.55 (5)
K1^iv—Yb1—K1	108.28 (4)	Si1^iii—K2—Si1^xiii	128.37 (8)
K1^v—Yb1—K1	71.72 (4)	Si1^xii—K2—Si1^xiii	102.75 (5)
O1^i—Yb1—K1^iii	60.33 (12)	O2—Si1—O1^xiv	110.5 (3)
O1^ii—Yb1—K1^iii	119.67 (12)	O2—Si1—O1^xv	110.5 (3)
O1^iii—Yb1—K1^iii	52.96 (19)	O1^xiv—Si1—O1^xv	111.1 (5)
O1—Yb1—K1^iii	127.04 (19)	O2—Si1—O3	106.2 (6)
O2^iii—Yb1—K1^iii	126.75 (4)	O1^xiv—Si1—O3	109.2 (3)
O2—Yb1—K1^iii	53.25 (4)	O1^xv—Si1—O3	109.2 (3)
K2^iii—Yb1—K1^iii	67.59 (4)	O2—Si1—K1^iv	64.9 (3)
K2—Yb1—K1^iii	112.41 (4)	O1^xiv—Si1—K1^iv	75.34 (17)
K1^iv—Yb1—K1^iii	71.72 (4)	O1^xv—Si1—K1^iv	75.34 (17)
K1^v—Yb1—K1^iii	108.28 (4)	O3—Si1—K1^iv	171.1 (5)
K1—Yb1—K1^iii	180.0	O2—Si1—K1^viii	59.02 (9)
O2^vi—K1—O1	117.57 (19)	O1^xiv—Si1—K1^viii	154.70 (18)
O2^vi—K1—O1^vii	117.57 (19)	O1^xv—Si1—K1^viii	59.4 (3)
O1—K1—O1^vii	55.9 (2)	O3—Si1—K1^viii	96.1 (3)
O2^vi—K1—O2^viii	87.20 (17)	K1^iv—Si1—K1^viii	79.45 (5)
O1—K1—O2^viii	121.0 (2)	O2—Si1—K1^iii	59.02 (9)
O1^vii—K1—O2^viii	65.05 (14)	O1^xiv—Si1—K1^iii	59.4 (3)
O2^vi—K1—O2^iii	87.20 (17)	O1^xv—Si1—K1^iii	154.70 (18)
O1—K1—O2^iii	65.05 (14)	O3—Si1—K1^iii	96.1 (3)
O1^vii—K1—O2^iii	121.0 (2)	K1^iv—Si1—K1^iii	79.45 (5)
O2^viii—K1—O2^iii	173.3 (3)	K1^viii—Si1—K1^iii	117.84 (18)
O2^vi—K1—O1^vi	68.01 (12)	O2—Si1—K1^xv	147.4 (3)
O1—K1—O1^vi	173.85 (19)	O1^xiv—Si1—K1^xv	57.7 (3)
O1^vii—K1—O1^vi	119.872 (19)	O1^xv—Si1—K1^xv	57.7 (3)
O2^viii—K1—O1^vi	55.21 (14)	O3—Si1—K1^xv	106.5 (5)
O2^iii—K1—O1^vi	119.1 (2)	K1^iv—Si1—K1^xv	82.47 (8)
O2^vi—K1—O1^ix	68.01 (12)	K1^viii—Si1—K1^xv	117.04 (9)
O1—K1—O1^ix	119.871 (19)	K1^iii—Si1—K1^xv	117.04 (9)
O1^vii—K1—O1^ix	173.86 (19)	O2—Si1—K2^iii	50.3 (3)
O2^viii—K1—O1^ix	119.1 (2)	O1^xiv—Si1—K2^iii	124.4 (3)
O2^iii—K1—O1^ix	55.21 (14)	O1^xv—Si1—K2^iii	124.4 (3)
O1^vi—K1—O1^ix	63.87 (19)	O3—Si1—K2^iii	55.8 (5)
O2^vi—K1—Si1^vi	30.90 (17)	K1^iv—Si1—K2^iii	115.23 (11)
O1—K1—Si1^vi	90.62 (11)	K1^viii—Si1—K2^iii	68.99 (10)
O1^vii—K1—Si1^vi	90.62 (11)	K1^iii—Si1—K2^iii	68.99 (10)
O2^viii—K1—Si1^vi	88.53 (18)	K1^xv—Si1—K2^iii	162.30 (8)
O2^iii—K1—Si1^vi	88.53 (18)	O2—Si1—K2^xvi	127.37 (11)
O1^vi—K1—Si1^vi	94.00 (11)	O1^xiv—Si1—K2^xvi	41.64 (17)
O1^ix—K1—Si1^vi	94.00 (11)	O1^xv—Si1—K2^xvi	120.9 (3)
O2^vi—K1—O1^viii	52.52 (12)	O3—Si1—K2^xvi	67.8 (3)
O1—K1—O1^viii	88.76 (17)	K1^iv—Si1—K2^xvi	116.98 (6)
O1^vii—K1—O1^viii	65.06 (15)	K1^viii—Si1—K2^xvi	163.51 (5)
O2^viii—K1—O1^viii	64.26 (19)	K1^iii—Si1—K2^xvi	69.46 (6)
O2^iii—K1—O1^viii	114.7 (2)	K1^xv—Si1—K2^xvi	66.78 (8)
O1^vi—K1—O1^viii	93.22 (14)	K2^iii—Si1—K2^xvi	102.75 (5)
O1^ix—K1—O1^viii	120.49 (10)	O2—Si1—K2^xv	127.37 (11)
Si1^vi—K1—O1^viii	30.02 (9)	O1^xiv—Si1—K2^xv	120.9 (3)
O2^vi—K1—O1^ii	52.52 (12)	O1^xv—Si1—K2^xv	41.64 (17)
O1—K1—O1^ii	65.06 (15)	O3—Si1—K2^xv	67.8 (3)
O1^vii—K1—O1^ii	88.76 (17)	K1^iv—Si1—K2^xv	116.98 (6)
O2^viii—K1—O1^ii	114.7 (2)	K1^viii—Si1—K2^xv	69.46 (6)
O2^iii—K1—O1^ii	64.26 (19)	K1^iii—Si1—K2^xv	163.51 (5)
O1^vi—K1—O1^ii	120.49 (10)	K1^xv—Si1—K2^xv	66.78 (8)
O1^ix—K1—O1^ii	93.22 (13)	K2^iii—Si1—K2^xv	102.75 (5)
Si1^vi—K1—O1^ii	30.02 (9)	K2^xvi—Si1—K2^xv	99.75 (10)
O1^viii—K1—O1^ii	50.5 (2)	Si1^xv—O1—Yb1	156.3 (3)
O2^vi—K1—Si1^viii	84.79 (11)	Si1^xv—O1—K2	115.2 (2)
O1—K1—Si1^viii	145.69 (15)	Yb1—O1—K2	88.34 (15)
O1^vii—K1—Si1^viii	91.30 (12)	Si1^xv—O1—K1	93.6 (3)
O2^viii—K1—Si1^viii	28.89 (16)	Yb1—O1—K1	88.67 (17)
O2^iii—K1—Si1^viii	146.6 (2)	K2—O1—K1	88.95 (16)
O1^vi—K1—Si1^viii	29.07 (11)	Si1^xv—O1—K1^iv	91.5 (3)
O1^ix—K1—Si1^viii	91.84 (15)	Yb1—O1—K1^iv	85.3 (2)
Si1^vi—K1—Si1^viii	100.55 (5)	K2—O1—K1^iv	91.99 (19)
O1^viii—K1—Si1^viii	85.39 (13)	K1—O1—K1^iv	173.86 (19)
O1^ii—K1—Si1^viii	130.55 (10)	Si1^xv—O1—K1^viii	74.63 (18)
O2^vi—K1—Si1^iii	84.79 (11)	Yb1—O1—K1^viii	81.75 (14)
O1—K1—Si1^iii	91.30 (12)	K2—O1—K1^viii	170.08 (19)
O1^vii—K1—Si1^iii	145.69 (15)	K1—O1—K1^viii	91.24 (17)
O2^viii—K1—Si1^iii	146.6 (2)	K1^iv—O1—K1^viii	86.78 (13)
O2^iii—K1—Si1^iii	28.89 (16)	Si1—O2—Yb1	170.2 (5)
O1^vi—K1—Si1^iii	91.84 (15)	Si1—O2—K2^iii	103.7 (4)
O1^ix—K1—Si1^iii	29.07 (11)	Yb1—O2—K2^iii	86.1 (2)
Si1^vi—K1—Si1^iii	100.55 (5)	Si1—O2—K1^iv	84.2 (3)
O1^viii—K1—Si1^iii	130.55 (10)	Yb1—O2—K1^iv	86.0 (3)
O1^ii—K1—Si1^iii	85.39 (13)	K2^iii—O2—K1^iv	172.1 (3)
Si1^viii—K1—Si1^iii	117.84 (18)	Si1—O2—K1^viii	92.09 (17)
O1—K2—O1^x	139.0 (3)	Yb1—O2—K1^viii	88.39 (17)
O1—K2—O1^xi	98.13 (19)	K2^iii—O2—K1^viii	86.97 (17)
O1^x—K2—O1^xi	67.2 (3)	K1^iv—O2—K1^viii	92.80 (17)
O1—K2—O1^i	67.2 (3)	Si1—O2—K1^iii	92.09 (17)
O1^x—K2—O1^i	98.13 (19)	Yb1—O2—K1^iii	88.39 (17)
O1^xi—K2—O1^i	139.0 (3)	K2^iii—O2—K1^iii	86.97 (17)
O1—K2—O2^iii	66.76 (12)	K1^iv—O2—K1^iii	92.80 (17)
O1^x—K2—O2^iii	144.55 (15)	K1^viii—O2—K1^iii	173.3 (3)
O1^xi—K2—O2^iii	144.55 (15)	Si1—O3—Si1^xvii	166.1 (10)
O1^i—K2—O2^iii	66.76 (12)	Si1—O3—K2^iii	97.0 (5)
O1—K2—O2^xii	144.55 (15)	Si1^xvii—O3—K2^iii	97.0 (5)

Symmetry codes: (i) −x, y, z; (ii) x, −y, −z+1; (iii) −x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) x+1/2, y+1/2, z; (vii) −x+1, y, z; (viii) −x+1, −y, −z+1; (ix) −x+1/2, y+1/2, z; (x) −x, y, −z+1/2; (xi) x, y, −z+1/2; (xii) −x, −y, z−1/2; (xiii) −x−1/2, −y−1/2, z−1/2; (xiv) x−1/2, −y−1/2, −z+1; (xv) −x+1/2, −y−1/2, −z+1; (xvi) −x−1/2, −y−1/2, −z+1; (xvii) x, y, −z+3/2.

(153_K)

Crystal data

K3O7Si2Yb	Dx = 3.882 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1202 reflections
a = 5.7095 (5) Å	θ = 4.1–29.2°
b = 9.8960 (9) Å	µ = 13.81 mm^−1
c = 13.8868 (12) Å	T = 153 K
V = 784.61 (12) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	475 reflections with I > 2σ(I)
ω scans	Rint = 0.040
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.305, Tmax = 0.398	h = −7→7
2736 measured reflections	k = −12→10
537 independent reflections	l = −16→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0011P)^2 + 3.5301P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.020	(Δ/σ)max < 0.001
wR(F^2) = 0.037	Δρmax = 0.89 e Å^−3
S = 1.08	Δρmin = −0.91 e Å^−3
537 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
30 parameters	Extinction coefficient: 0.00322 (14)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00200 (14)
K1	0.500000	0.1729 (4)	0.40769 (11)	0.0062 (3)
K2	0.000000	0.0157 (4)	0.250000	0.0085 (5)
Si1	0.000000	−0.3378 (4)	0.63238 (13)	0.0021 (3)
O1	0.2664 (12)	−0.0815 (6)	0.3999 (4)	0.0084 (12)
O2	0.000000	−0.1872 (8)	0.5877 (7)	0.006 (2)
O3	0.000000	−0.3201 (14)	0.750000	0.0132 (19)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00169 (15)	0.00169 (15)	0.0026 (2)	0.000	0.000	0.000
K1	0.0056 (5)	0.0056 (5)	0.0075 (6)	0.000	0.000	0.000
K2	0.0111 (8)	0.0111 (8)	0.0033 (8)	0.000	0.000	0.000
Si1	0.0022 (5)	0.0022 (5)	0.0018 (7)	0.000	0.000	0.000
O1	0.0057 (15)	0.0057 (15)	0.014 (2)	0.000	0.000	0.000
O2	0.007 (3)	0.004 (3)	0.007 (3)	0.000	0.000	0.000
O3	0.034 (8)	0.002 (6)	0.004 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O1^i	2.213 (5)	K1—O1^ix	3.121 (5)
Yb1—O1^ii	2.213 (5)	K1—O1^ii	3.121 (5)
Yb1—O1^iii	2.213 (5)	K1—Si1^viii	3.122 (3)
Yb1—O1	2.213 (5)	K1—Si1^ix	3.335 (3)
Yb1—O2^iii	2.217 (9)	K1—Si1^iii	3.335 (3)
Yb1—O2	2.217 (9)	K2—O1	2.752 (5)
Yb1—K2	3.4752 (3)	K2—O1^xi	2.752 (5)
Yb1—K2^iii	3.4752 (3)	K2—O1^xii	2.752 (5)
Yb1—K1^iv	3.481 (4)	K2—O1^i	2.752 (5)
Yb1—K1^v	3.481 (4)	K2—O2^iii	2.821 (10)
Yb1—K1^iii	3.5666 (19)	K2—O2^xiii	2.821 (10)
Yb1—K1^vi	3.5666 (19)	K2—O3^iii	3.012 (15)
K1—O1^vii	2.851 (9)	K2—Si1^iii	3.581 (6)
K1—O1	2.851 (9)	K2—Si1^xiii	3.581 (6)
K1—O2^viii	2.858 (10)	K2—Si1^xiv	3.731 (3)
K1—O2^ix	2.8590 (6)	Si1—O2	1.614 (9)
K1—O2^iii	2.8590 (6)	Si1—O1^xv	1.617 (5)
K1—O1^viii	2.869 (9)	Si1—O1^xvi	1.617 (5)
K1—O1^x	2.869 (9)	Si1—O3	1.643 (3)
O1^i—Yb1—O1^ii	180.0	O1^xi—K2—O2^xiii	66.81 (14)
O1^i—Yb1—O1^iii	93.2 (4)	O1^xii—K2—O2^xiii	66.81 (14)
O1^ii—Yb1—O1^iii	86.8 (4)	O1^i—K2—O2^xiii	144.55 (16)
O1^i—Yb1—O1	86.8 (4)	O2^iii—K2—O2^xiii	106.0 (4)
O1^ii—Yb1—O1	93.2 (4)	O1—K2—O3^iii	110.48 (14)
O1^iii—Yb1—O1	180.0	O1^xi—K2—O3^iii	110.48 (14)
O1^i—Yb1—O2^iii	87.7 (2)	O1^xii—K2—O3^iii	110.48 (14)
O1^ii—Yb1—O2^iii	92.3 (2)	O1^i—K2—O3^iii	110.48 (14)
O1^iii—Yb1—O2^iii	92.3 (2)	O2^iii—K2—O3^iii	53.02 (18)
O1—Yb1—O2^iii	87.7 (2)	O2^xiii—K2—O3^iii	53.02 (18)
O1^i—Yb1—O2	92.3 (2)	O1—K2—Yb1^xiii	137.72 (11)
O1^ii—Yb1—O2	87.7 (2)	O1^xi—K2—Yb1^xiii	39.54 (10)
O1^iii—Yb1—O2	87.7 (2)	O1^xii—K2—Yb1^xiii	39.54 (10)
O1—Yb1—O2	92.3 (2)	O1^i—K2—Yb1^xiii	137.72 (11)
O2^iii—Yb1—O2	180.0	O2^iii—K2—Yb1^xiii	145.6 (2)
O1^i—Yb1—K2	52.32 (13)	O2^xiii—K2—Yb1^xiii	39.55 (18)
O1^ii—Yb1—K2	127.68 (13)	O3^iii—K2—Yb1^xiii	92.57 (6)
O1^iii—Yb1—K2	127.68 (13)	O1—K2—Yb1	39.54 (10)
O1—Yb1—K2	52.32 (13)	O1^xi—K2—Yb1	137.72 (11)
O2^iii—Yb1—K2	54.1 (3)	O1^xii—K2—Yb1	137.72 (11)
O2—Yb1—K2	125.9 (3)	O1^i—K2—Yb1	39.54 (11)
O1^i—Yb1—K2^iii	127.68 (13)	O2^iii—K2—Yb1	39.55 (18)
O1^ii—Yb1—K2^iii	52.32 (13)	O2^xiii—K2—Yb1	145.6 (2)
O1^iii—Yb1—K2^iii	52.32 (13)	O3^iii—K2—Yb1	92.57 (6)
O1—Yb1—K2^iii	127.68 (13)	Yb1^xiii—K2—Yb1	174.87 (12)
O2^iii—Yb1—K2^iii	125.9 (3)	O1—K2—Si1^iii	88.07 (12)
O2—Yb1—K2^iii	54.1 (3)	O1^xi—K2—Si1^iii	131.02 (17)
K2—Yb1—K2^iii	180.0	O1^xii—K2—Si1^iii	131.02 (17)
O1^i—Yb1—K1^iv	55.23 (19)	O1^i—K2—Si1^iii	88.07 (12)
O1^ii—Yb1—K1^iv	124.77 (19)	O2^iii—K2—Si1^iii	25.88 (18)
O1^iii—Yb1—K1^iv	124.77 (19)	O2^xiii—K2—Si1^iii	80.2 (2)
O1—Yb1—K1^iv	55.23 (19)	O3^iii—K2—Si1^iii	27.14 (5)
O2^iii—Yb1—K1^iv	125.1 (2)	Yb1^xiii—K2—Si1^iii	119.70 (11)
O2—Yb1—K1^iv	54.9 (2)	Yb1—K2—Si1^iii	65.43 (5)
K2—Yb1—K1^iv	70.96 (7)	O1—K2—Si1^xiii	131.02 (17)
K2^iii—Yb1—K1^iv	109.04 (7)	O1^xi—K2—Si1^xiii	88.07 (12)
O1^i—Yb1—K1^v	124.77 (19)	O1^xii—K2—Si1^xiii	88.07 (12)
O1^ii—Yb1—K1^v	55.23 (19)	O1^i—K2—Si1^xiii	131.02 (17)
O1^iii—Yb1—K1^v	55.23 (19)	O2^iii—K2—Si1^xiii	80.2 (2)
O1—Yb1—K1^v	124.77 (19)	O2^xiii—K2—Si1^xiii	25.88 (18)
O2^iii—Yb1—K1^v	54.9 (2)	O3^iii—K2—Si1^xiii	27.14 (5)
O2—Yb1—K1^v	125.1 (2)	Yb1^xiii—K2—Si1^xiii	65.43 (5)
K2—Yb1—K1^v	109.04 (7)	Yb1—K2—Si1^xiii	119.70 (11)
K2^iii—Yb1—K1^v	70.96 (7)	Si1^iii—K2—Si1^xiii	54.27 (11)
K1^iv—Yb1—K1^v	180.00 (5)	O1—K2—Si1^xiv	126.1 (2)
O1^i—Yb1—K1^iii	60.05 (13)	O1^xi—K2—Si1^xiv	23.18 (10)
O1^ii—Yb1—K1^iii	119.95 (13)	O1^xii—K2—Si1^xiv	85.80 (17)
O1^iii—Yb1—K1^iii	53.1 (2)	O1^i—K2—Si1^xiv	75.11 (11)
O1—Yb1—K1^iii	126.9 (2)	O2^iii—K2—Si1^xiv	129.32 (5)
O2^iii—Yb1—K1^iii	126.75 (4)	O2^xiii—K2—Si1^xiv	86.23 (12)
O2—Yb1—K1^iii	53.25 (4)	O3^iii—K2—Si1^xiv	118.17 (8)
K2—Yb1—K1^iii	112.37 (4)	Yb1^xiii—K2—Si1^xiv	62.71 (4)
K2^iii—Yb1—K1^iii	67.63 (4)	Yb1—K2—Si1^xiv	114.60 (6)
K1^iv—Yb1—K1^iii	71.72 (5)	Si1^iii—K2—Si1^xiv	128.30 (8)
K1^v—Yb1—K1^iii	108.28 (4)	Si1^xiii—K2—Si1^xiv	102.73 (6)
O1^i—Yb1—K1^vi	53.1 (2)	O2—Si1—O1^xv	110.5 (3)
O1^ii—Yb1—K1^vi	126.9 (2)	O2—Si1—O1^xvi	110.5 (3)
O1^iii—Yb1—K1^vi	60.05 (13)	O1^xv—Si1—O1^xvi	111.1 (6)
O1—Yb1—K1^vi	119.95 (13)	O2—Si1—O3	106.5 (7)
O2^iii—Yb1—K1^vi	53.25 (4)	O1^xv—Si1—O3	109.1 (3)
O2—Yb1—K1^vi	126.75 (4)	O1^xvi—Si1—O3	109.1 (3)
K2—Yb1—K1^vi	67.63 (4)	O2—Si1—K1^iv	65.5 (4)
K2^iii—Yb1—K1^vi	112.37 (4)	O1^xv—Si1—K1^iv	74.93 (19)
K1^iv—Yb1—K1^vi	108.28 (5)	O1^xvi—Si1—K1^iv	74.93 (19)
K1^v—Yb1—K1^vi	71.72 (4)	O3—Si1—K1^iv	171.9 (6)
K1^iii—Yb1—K1^vi	73.66 (8)	O2—Si1—K1^ix	58.95 (10)
O1^vii—K1—O1	55.8 (2)	O1^xv—Si1—K1^ix	154.3 (2)
O1^vii—K1—O2^viii	117.5 (2)	O1^xvi—Si1—K1^ix	59.3 (3)
O1—K1—O2^viii	117.5 (2)	O3—Si1—K1^ix	96.5 (3)
O1^vii—K1—O2^ix	65.01 (15)	K1^iv—Si1—K1^ix	79.44 (5)
O1—K1—O2^ix	120.8 (3)	O2—Si1—K1^iii	58.95 (10)
O2^viii—K1—O2^ix	87.51 (19)	O1^xv—Si1—K1^iii	59.3 (3)
O1^vii—K1—O2^iii	120.8 (3)	O1^xvi—Si1—K1^iii	154.3 (2)
O1—K1—O2^iii	65.01 (15)	O3—Si1—K1^iii	96.5 (3)
O2^viii—K1—O2^iii	87.51 (19)	K1^iv—Si1—K1^iii	79.44 (5)
O2^ix—K1—O2^iii	173.8 (4)	K1^ix—Si1—K1^iii	117.75 (19)
O1^vii—K1—O1^viii	119.90 (2)	O2—Si1—K1^xvi	147.9 (4)
O1—K1—O1^viii	174.0 (2)	O1^xv—Si1—K1^xvi	57.8 (3)
O2^viii—K1—O1^viii	67.84 (14)	O1^xvi—Si1—K1^xvi	57.8 (3)
O2^ix—K1—O1^viii	55.21 (15)	O3—Si1—K1^xvi	105.6 (5)
O2^iii—K1—O1^viii	119.2 (3)	K1^iv—Si1—K1^xvi	82.41 (8)
O1^vii—K1—O1^x	174.0 (2)	K1^ix—Si1—K1^xvi	117.06 (10)
O1—K1—O1^x	119.90 (2)	K1^iii—Si1—K1^xvi	117.06 (10)
O2^viii—K1—O1^x	67.84 (14)	O2—Si1—K2^iii	49.7 (3)
O2^ix—K1—O1^x	119.2 (3)	O1^xv—Si1—K2^iii	124.4 (3)
O2^iii—K1—O1^x	55.21 (15)	O1^xvi—Si1—K2^iii	124.4 (3)
O1^viii—K1—O1^x	64.0 (2)	O3—Si1—K2^iii	56.8 (5)
O1^vii—K1—O1^ix	64.97 (16)	K1^iv—Si1—K2^iii	115.20 (11)
O1—K1—O1^ix	88.66 (18)	K1^ix—Si1—K2^iii	68.95 (10)
O2^viii—K1—O1^ix	52.49 (14)	K1^iii—Si1—K2^iii	68.95 (10)
O2^ix—K1—O1^ix	64.4 (2)	K1^xvi—Si1—K2^iii	162.39 (8)
O2^iii—K1—O1^ix	115.0 (3)	O2—Si1—K2^xvii	127.16 (12)
O1^viii—K1—O1^ix	92.94 (15)	O1^xv—Si1—K2^xvii	42.04 (18)
O1^x—K1—O1^ix	120.29 (11)	O1^xvi—Si1—K2^xvii	121.3 (3)
O1^vii—K1—O1^ii	88.66 (18)	O3—Si1—K2^xvii	67.4 (3)
O1—K1—O1^ii	64.97 (16)	K1^iv—Si1—K2^xvii	116.97 (6)
O2^viii—K1—O1^ii	52.49 (14)	K1^ix—Si1—K2^xvii	163.54 (5)
O2^ix—K1—O1^ii	115.0 (3)	K1^iii—Si1—K2^xvii	69.45 (7)
O2^iii—K1—O1^ii	64.4 (2)	K1^xvi—Si1—K2^xvii	66.85 (9)
O1^viii—K1—O1^ii	120.29 (11)	K2^iii—Si1—K2^xvii	102.73 (6)
O1^x—K1—O1^ii	92.94 (15)	O2—Si1—K2^xvi	127.16 (12)
O1^ix—K1—O1^ii	50.6 (3)	O1^xv—Si1—K2^xvi	121.3 (3)
O1^vii—K1—Si1^viii	90.47 (12)	O1^xvi—Si1—K2^xvi	42.04 (18)
O1—K1—Si1^viii	90.47 (12)	O3—Si1—K2^xvi	67.4 (3)
O2^viii—K1—Si1^viii	30.91 (19)	K1^iv—Si1—K2^xvi	116.97 (6)
O2^ix—K1—Si1^viii	88.8 (2)	K1^ix—Si1—K2^xvi	69.45 (7)
O2^iii—K1—Si1^viii	88.8 (2)	K1^iii—Si1—K2^xvi	163.54 (5)
O1^viii—K1—Si1^viii	93.81 (13)	K1^xvi—Si1—K2^xvi	66.85 (9)
O1^x—K1—Si1^viii	93.81 (13)	K2^iii—Si1—K2^xvi	102.73 (6)
O1^ix—K1—Si1^viii	30.03 (10)	K2^xvii—Si1—K2^xvi	99.85 (11)
O1^ii—K1—Si1^viii	30.03 (10)	Si1^xvi—O1—Yb1	157.0 (3)
O1^vii—K1—Si1^ix	91.45 (13)	Si1^xvi—O1—K2	114.8 (2)
O1—K1—Si1^ix	145.69 (16)	Yb1—O1—K2	88.15 (16)
O2^viii—K1—Si1^ix	84.78 (12)	Si1^xvi—O1—K1	93.5 (3)
O2^ix—K1—Si1^ix	28.92 (18)	Yb1—O1—K1	88.60 (19)
O2^iii—K1—Si1^ix	146.5 (2)	K2—O1—K1	88.76 (17)
O1^viii—K1—Si1^ix	29.00 (12)	Si1^xvi—O1—K1^iv	91.7 (3)
O1^x—K1—Si1^ix	91.90 (16)	Yb1—O1—K1^iv	85.4 (2)
O1^ix—K1—Si1^ix	85.34 (14)	K2—O1—K1^iv	91.8 (2)
O1^ii—K1—Si1^ix	130.57 (11)	K1—O1—K1^iv	174.0 (2)
Si1^viii—K1—Si1^ix	100.56 (5)	Si1^xvi—O1—K1^ix	75.03 (19)
O1^vii—K1—Si1^iii	145.69 (16)	Yb1—O1—K1^ix	82.03 (15)
O1—K1—Si1^iii	91.45 (13)	K2—O1—K1^ix	170.2 (2)
O2^viii—K1—Si1^iii	84.78 (12)	K1—O1—K1^ix	91.34 (18)
O2^ix—K1—Si1^iii	146.5 (2)	K1^iv—O1—K1^ix	87.06 (15)
O2^iii—K1—Si1^iii	28.92 (18)	Si1—O2—Yb1	169.3 (6)
O1^viii—K1—Si1^iii	91.90 (16)	Si1—O2—K2^iii	104.4 (4)
O1^x—K1—Si1^iii	29.00 (12)	Yb1—O2—K2^iii	86.4 (3)
O1^ix—K1—Si1^iii	130.57 (11)	Si1—O2—K1^iv	83.6 (4)
O1^ii—K1—Si1^iii	85.34 (14)	Yb1—O2—K1^iv	85.6 (3)
Si1^viii—K1—Si1^iii	100.56 (5)	K2^iii—O2—K1^iv	172.0 (3)
Si1^ix—K1—Si1^iii	117.75 (19)	Si1—O2—K1^ix	92.1 (2)
O1—K2—O1^xi	139.0 (3)	Yb1—O2—K1^ix	88.33 (19)
O1—K2—O1^xii	98.3 (2)	K2^iii—O2—K1^ix	87.28 (19)
O1^xi—K2—O1^xii	67.1 (3)	K1^iv—O2—K1^ix	92.49 (19)
O1—K2—O1^i	67.1 (3)	Si1—O2—K1^iii	92.1 (2)
O1^xi—K2—O1^i	98.3 (2)	Yb1—O2—K1^iii	88.33 (19)
O1^xii—K2—O1^i	139.0 (3)	K2^iii—O2—K1^iii	87.28 (19)
O1—K2—O2^iii	66.81 (14)	K1^iv—O2—K1^iii	92.49 (19)
O1^xi—K2—O2^iii	144.55 (16)	K1^ix—O2—K1^iii	173.8 (4)
O1^xii—K2—O2^iii	144.55 (16)	Si1—O3—Si1^xviii	167.8 (10)
O1^i—K2—O2^iii	66.81 (14)	Si1—O3—K2^iii	96.1 (5)
O1—K2—O2^xiii	144.55 (16)	Si1^xviii—O3—K2^iii	96.1 (5)

Symmetry codes: (i) −x, y, z; (ii) x, −y, −z+1; (iii) −x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) x−1, y, z; (vii) −x+1, y, z; (viii) x+1/2, y+1/2, z; (ix) −x+1, −y, −z+1; (x) −x+1/2, y+1/2, z; (xi) −x, y, −z+1/2; (xii) x, y, −z+1/2; (xiii) −x, −y, z−1/2; (xiv) −x−1/2, −y−1/2, z−1/2; (xv) x−1/2, −y−1/2, −z+1; (xvi) −x+1/2, −y−1/2, −z+1; (xvii) −x−1/2, −y−1/2, −z+1; (xviii) x, y, −z+3/2.

(163_K)

Crystal data

K3O7Si2Yb	Dx = 3.868 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1191 reflections
a = 5.7158 (6) Å	θ = 5.0–29.9°
b = 9.9012 (10) Å	µ = 13.77 mm^−1
c = 13.9112 (14) Å	T = 163 K
V = 787.28 (14) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	472 reflections with I > 2σ(I)
ω scans	Rint = 0.042
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.305, Tmax = 0.398	h = −7→7
2682 measured reflections	k = −12→10
539 independent reflections	l = −16→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0048P)^2 + 4.5201P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.021	(Δ/σ)max < 0.001
wR(F^2) = 0.042	Δρmax = 0.95 e Å^−3
S = 1.09	Δρmin = −0.87 e Å^−3
539 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
29 parameters	Extinction coefficient: 0.00358 (17)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00265 (16)
K1	0.500000	0.1712 (4)	0.40787 (12)	0.0077 (3)
K2	0.000000	0.0148 (4)	0.250000	0.0095 (5)
Si1	0.000000	−0.3380 (5)	0.63220 (14)	0.0028 (4)
O1	0.2675 (12)	−0.0807 (6)	0.3997 (4)	0.0088 (13)
O2	0.000000	−0.1871 (9)	0.5880 (7)	0.005 (2)
O3	0.000000	−0.3192 (15)	0.750000	0.0110 (19)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00237 (17)	0.00237 (17)	0.0032 (2)	0.000	0.000	0.000
K1	0.0069 (5)	0.0069 (5)	0.0093 (7)	0.000	0.000	0.000
K2	0.0120 (8)	0.0120 (8)	0.0043 (9)	0.000	0.000	0.000
Si1	0.0027 (6)	0.0027 (6)	0.0031 (8)	0.000	0.000	0.000
O1	0.0054 (16)	0.0054 (16)	0.015 (3)	0.000	0.000	0.000
O2	0.004 (3)	0.008 (4)	0.004 (3)	0.000	0.000	0.000
O3	0.005 (3)	0.023 (7)	0.005 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O1^i	2.219 (5)	K1—O1^vii	3.120 (6)
Yb1—O1^ii	2.219 (5)	K1—O1^ii	3.120 (6)
Yb1—O1^iii	2.219 (5)	K1—Si1^viii	3.122 (3)
Yb1—O1	2.219 (5)	K1—Si1^x	3.346 (7)
Yb1—O2^iii	2.220 (9)	K1—Si1^vii	3.347 (3)
Yb1—O2	2.220 (9)	K2—O1	2.751 (5)
Yb1—K2	3.4809 (4)	K2—O1^xi	2.751 (5)
Yb1—K2^iii	3.4809 (4)	K2—O1^xii	2.751 (5)
Yb1—K1^iv	3.498 (3)	K2—O1^i	2.751 (5)
Yb1—K1^v	3.498 (3)	K2—O2^iii	2.826 (10)
Yb1—K1	3.5616 (19)	K2—O2^xiii	2.826 (10)
Yb1—K1^iii	3.5616 (19)	K2—O3^iii	3.014 (17)
K1—O1^vi	2.829 (9)	K2—Si1^iii	3.595 (6)
K1—O1	2.829 (9)	K2—Si1^xiii	3.595 (6)
K1—O2^vii	2.8628 (7)	K2—Si1^xiv	3.730 (3)
K1—O2^iii	2.8628 (6)	Si1—O1^xv	1.616 (6)
K1—O2^viii	2.872 (10)	Si1—O1^x	1.616 (6)
K1—O1^viii	2.895 (9)	Si1—O2	1.616 (10)
K1—O1^ix	2.895 (9)	Si1—O3	1.649 (3)
O1^i—Yb1—O1^ii	180.0	O1^xi—K2—O2^xiii	66.66 (14)
O1^i—Yb1—O1^iii	92.9 (4)	O1^xii—K2—O2^xiii	66.66 (14)
O1^ii—Yb1—O1^iii	87.1 (4)	O1^i—K2—O2^xiii	144.19 (17)
O1^i—Yb1—O1	87.1 (4)	O2^iii—K2—O2^xiii	105.8 (4)
O1^ii—Yb1—O1	92.9 (4)	O1—K2—O3^iii	110.10 (15)
O1^iii—Yb1—O1	180.0 (3)	O1^xi—K2—O3^iii	110.10 (15)
O1^i—Yb1—O2^iii	87.3 (2)	O1^xii—K2—O3^iii	110.10 (15)
O1^ii—Yb1—O2^iii	92.7 (2)	O1^i—K2—O3^iii	110.10 (15)
O1^iii—Yb1—O2^iii	92.7 (2)	O2^iii—K2—O3^iii	52.88 (19)
O1—Yb1—O2^iii	87.3 (2)	O2^xiii—K2—O3^iii	52.88 (19)
O1^i—Yb1—O2	92.7 (2)	O1—K2—Yb1^xiii	137.89 (12)
O1^ii—Yb1—O2	87.3 (2)	O1^xi—K2—Yb1^xiii	39.57 (11)
O1^iii—Yb1—O2	87.3 (2)	O1^xii—K2—Yb1^xiii	39.57 (11)
O1—Yb1—O2	92.7 (2)	O1^i—K2—Yb1^xiii	137.89 (12)
O2^iii—Yb1—O2	180.0	O2^iii—K2—Yb1^xiii	145.3 (2)
O1^i—Yb1—K2	52.19 (14)	O2^xiii—K2—Yb1^xiii	39.54 (18)
O1^ii—Yb1—K2	127.81 (14)	O3^iii—K2—Yb1^xiii	92.42 (7)
O1^iii—Yb1—K2	127.81 (14)	O1—K2—Yb1	39.57 (11)
O1—Yb1—K2	52.19 (14)	O1^xi—K2—Yb1	137.89 (12)
O2^iii—Yb1—K2	54.1 (3)	O1^xii—K2—Yb1	137.89 (12)
O2—Yb1—K2	125.9 (3)	O1^i—K2—Yb1	39.57 (11)
O1^i—Yb1—K2^iii	127.81 (14)	O2^iii—K2—Yb1	39.54 (18)
O1^ii—Yb1—K2^iii	52.19 (14)	O2^xiii—K2—Yb1	145.3 (2)
O1^iii—Yb1—K2^iii	52.19 (14)	O3^iii—K2—Yb1	92.42 (7)
O1—Yb1—K2^iii	127.81 (14)	Yb1^xiii—K2—Yb1	175.17 (13)
O2^iii—Yb1—K2^iii	125.9 (3)	O1—K2—Si1^iii	87.76 (13)
O2—Yb1—K2^iii	54.1 (3)	O1^xi—K2—Si1^iii	130.61 (19)
K2—Yb1—K2^iii	180.00 (13)	O1^xii—K2—Si1^iii	130.61 (19)
O1^i—Yb1—K1^iv	55.6 (2)	O1^i—K2—Si1^iii	87.76 (13)
O1^ii—Yb1—K1^iv	124.4 (2)	O2^iii—K2—Si1^iii	25.76 (19)
O1^iii—Yb1—K1^iv	124.4 (2)	O2^xiii—K2—Si1^iii	80.0 (2)
O1—Yb1—K1^iv	55.6 (2)	O3^iii—K2—Si1^iii	27.11 (6)
O2^iii—Yb1—K1^iv	125.0 (2)	Yb1^xiii—K2—Si1^iii	119.53 (11)
O2—Yb1—K1^iv	55.0 (2)	Yb1—K2—Si1^iii	65.30 (5)
K2—Yb1—K1^iv	70.92 (8)	O1—K2—Si1^xiii	130.61 (19)
K2^iii—Yb1—K1^iv	109.08 (8)	O1^xi—K2—Si1^xiii	87.76 (13)
O1^i—Yb1—K1^v	124.4 (2)	O1^xii—K2—Si1^xiii	87.76 (13)
O1^ii—Yb1—K1^v	55.6 (2)	O1^i—K2—Si1^xiii	130.61 (19)
O1^iii—Yb1—K1^v	55.6 (2)	O2^iii—K2—Si1^xiii	80.0 (2)
O1—Yb1—K1^v	124.4 (2)	O2^xiii—K2—Si1^xiii	25.76 (19)
O2^iii—Yb1—K1^v	55.0 (2)	O3^iii—K2—Si1^xiii	27.11 (6)
O2—Yb1—K1^v	125.0 (2)	Yb1^xiii—K2—Si1^xiii	65.30 (5)
K2—Yb1—K1^v	109.08 (8)	Yb1—K2—Si1^xiii	119.53 (11)
K2^iii—Yb1—K1^v	70.92 (8)	Si1^iii—K2—Si1^xiii	54.23 (11)
K1^iv—Yb1—K1^v	180.00 (5)	O1—K2—Si1^xiv	126.7 (2)
O1^i—Yb1—K1	119.88 (14)	O1^xi—K2—Si1^xiv	23.14 (11)
O1^ii—Yb1—K1	60.12 (14)	O1^xii—K2—Si1^xiv	86.10 (18)
O1^iii—Yb1—K1	127.4 (2)	O1^i—K2—Si1^xiv	75.26 (12)
O1—Yb1—K1	52.6 (2)	O2^iii—K2—Si1^xiv	129.30 (5)
O2^iii—Yb1—K1	53.45 (4)	O2^xiii—K2—Si1^xiv	86.15 (13)
O2—Yb1—K1	126.55 (4)	O3^iii—K2—Si1^xiv	117.98 (9)
K2—Yb1—K1	67.69 (4)	Yb1^xiii—K2—Si1^xiv	62.70 (4)
K2^iii—Yb1—K1	112.31 (4)	Yb1—K2—Si1^xiv	114.78 (6)
K1^iv—Yb1—K1	108.13 (5)	Si1^iii—K2—Si1^xiv	128.16 (9)
K1^v—Yb1—K1	71.87 (5)	Si1^xiii—K2—Si1^xiv	102.56 (6)
O1^i—Yb1—K1^iii	60.12 (14)	O1^xv—Si1—O1^x	110.7 (6)
O1^ii—Yb1—K1^iii	119.88 (14)	O1^xv—Si1—O2	110.9 (3)
O1^iii—Yb1—K1^iii	52.6 (2)	O1^x—Si1—O2	110.9 (3)
O1—Yb1—K1^iii	127.4 (2)	O1^xv—Si1—O3	109.2 (4)
O2^iii—Yb1—K1^iii	126.55 (4)	O1^x—Si1—O3	109.2 (4)
O2—Yb1—K1^iii	53.45 (4)	O2—Si1—O3	105.9 (7)
K2—Yb1—K1^iii	112.31 (4)	O1^xv—Si1—K1^iv	74.9 (2)
K2^iii—Yb1—K1^iii	67.69 (4)	O1^x—Si1—K1^iv	74.9 (2)
K1^iv—Yb1—K1^iii	71.87 (5)	O2—Si1—K1^iv	66.0 (4)
K1^v—Yb1—K1^iii	108.13 (5)	O3—Si1—K1^iv	171.8 (6)
K1—Yb1—K1^iii	180.00 (10)	O1^xv—Si1—K1^x	57.5 (3)
O1^vi—K1—O1	56.0 (2)	O1^x—Si1—K1^x	57.5 (3)
O1^vi—K1—O2^vii	65.17 (16)	O2—Si1—K1^x	148.1 (4)
O1—K1—O2^vii	121.2 (3)	O3—Si1—K1^x	106.1 (6)
O1^vi—K1—O2^iii	121.2 (3)	K1^iv—Si1—K1^x	82.10 (9)
O1—K1—O2^iii	65.17 (16)	O1^xv—Si1—K1^vii	154.4 (2)
O2^vii—K1—O2^iii	173.3 (4)	O1^x—Si1—K1^vii	59.9 (3)
O1^vi—K1—O2^viii	117.8 (2)	O2—Si1—K1^vii	58.69 (10)
O1—K1—O2^viii	117.8 (2)	O3—Si1—K1^vii	96.3 (3)
O2^vii—K1—O2^viii	87.5 (2)	K1^iv—Si1—K1^vii	79.57 (5)
O2^iii—K1—O2^viii	87.5 (2)	K1^x—Si1—K1^vii	117.30 (10)
O1^vi—K1—O1^viii	119.90 (2)	O1^xv—Si1—K1^iii	59.9 (3)
O1—K1—O1^viii	174.0 (2)	O1^x—Si1—K1^iii	154.4 (2)
O2^vii—K1—O1^viii	55.05 (16)	O2—Si1—K1^iii	58.69 (10)
O2^iii—K1—O1^viii	118.8 (3)	O3—Si1—K1^iii	96.3 (3)
O2^viii—K1—O1^viii	67.66 (14)	K1^iv—Si1—K1^iii	79.57 (5)
O1^vi—K1—O1^ix	174.0 (2)	K1^x—Si1—K1^iii	117.30 (10)
O1—K1—O1^ix	119.90 (2)	K1^vii—Si1—K1^iii	117.24 (19)
O2^vii—K1—O1^ix	118.8 (3)	O1^xv—Si1—K2^iii	124.7 (3)
O2^iii—K1—O1^ix	55.05 (16)	O1^x—Si1—K2^iii	124.7 (3)
O2^viii—K1—O1^ix	67.66 (14)	O2—Si1—K2^iii	49.5 (4)
O1^viii—K1—O1^ix	63.8 (2)	O3—Si1—K2^iii	56.4 (6)
O1^vi—K1—O1^vii	65.22 (17)	K1^iv—Si1—K2^iii	115.43 (12)
O1—K1—O1^vii	88.91 (19)	K1^x—Si1—K2^iii	162.48 (9)
O2^vii—K1—O1^vii	64.7 (2)	K1^vii—Si1—K2^iii	68.70 (10)
O2^iii—K1—O1^vii	115.1 (3)	K1^iii—Si1—K2^iii	68.70 (11)
O2^viii—K1—O1^vii	52.54 (14)	O1^xv—Si1—K2^xvi	42.02 (19)
O1^viii—K1—O1^vii	93.01 (16)	O1^x—Si1—K2^xvi	121.1 (3)
O1^ix—K1—O1^vii	120.15 (11)	O2—Si1—K2^xvi	126.94 (13)
O1^vi—K1—O1^ii	88.91 (19)	O3—Si1—K2^xvi	67.5 (3)
O1—K1—O1^ii	65.22 (17)	K1^iv—Si1—K2^xvi	116.93 (6)
O2^vii—K1—O1^ii	115.1 (3)	K1^x—Si1—K2^xvi	67.08 (10)
O2^iii—K1—O1^ii	64.7 (2)	K1^vii—Si1—K2^xvi	163.47 (6)
O2^viii—K1—O1^ii	52.54 (14)	K1^iii—Si1—K2^xvi	69.55 (7)
O1^viii—K1—O1^ii	120.15 (11)	K2^iii—Si1—K2^xvi	102.56 (6)
O1^ix—K1—O1^ii	93.01 (16)	O1^xv—Si1—K2^x	121.1 (3)
O1^vii—K1—O1^ii	50.4 (3)	O1^x—Si1—K2^x	42.02 (19)
O1^vi—K1—Si1^viii	90.80 (13)	O2—Si1—K2^x	126.94 (13)
O1—K1—Si1^viii	90.80 (13)	O3—Si1—K2^x	67.5 (3)
O2^vii—K1—Si1^viii	88.9 (2)	K1^iv—Si1—K2^x	116.93 (6)
O2^iii—K1—Si1^viii	88.9 (2)	K1^x—Si1—K2^x	67.08 (10)
O2^viii—K1—Si1^viii	30.9 (2)	K1^vii—Si1—K2^x	69.55 (7)
O1^viii—K1—Si1^viii	93.67 (13)	K1^iii—Si1—K2^x	163.47 (6)
O1^ix—K1—Si1^viii	93.67 (13)	K2^iii—Si1—K2^x	102.56 (6)
O1^vii—K1—Si1^viii	30.00 (11)	K2^xvi—Si1—K2^x	100.01 (12)
O1^ii—K1—Si1^viii	30.00 (11)	Si1^x—O1—Yb1	156.8 (3)
O1^vi—K1—Si1^x	28.81 (11)	Si1^x—O1—K2	114.8 (3)
O1—K1—Si1^x	28.81 (11)	Yb1—O1—K2	88.24 (17)
O2^vii—K1—Si1^x	93.29 (19)	Si1^x—O1—K1	93.7 (4)
O2^iii—K1—Si1^x	93.29 (19)	Yb1—O1—K1	88.9 (2)
O2^viii—K1—Si1^x	128.83 (19)	K2—O1—K1	89.33 (19)
O1^viii—K1—Si1^x	146.09 (11)	Si1^x—O1—K1^iv	91.3 (3)
O1^ix—K1—Si1^x	146.09 (11)	Yb1—O1—K1^iv	85.2 (2)
O1^vii—K1—Si1^x	81.92 (13)	K2—O1—K1^iv	91.6 (2)
O1^ii—K1—Si1^x	81.92 (13)	K1—O1—K1^iv	174.0 (2)
Si1^viii—K1—Si1^x	97.90 (9)	Si1^x—O1—K1^vii	75.1 (2)
O1^vi—K1—Si1^vii	91.57 (13)	Yb1—O1—K1^vii	81.82 (16)
O1—K1—Si1^vii	146.05 (16)	K2—O1—K1^vii	170.0 (2)
O2^vii—K1—Si1^vii	28.84 (19)	K1—O1—K1^vii	91.09 (19)
O2^iii—K1—Si1^vii	146.0 (2)	K1^iv—O1—K1^vii	86.99 (16)
O2^viii—K1—Si1^vii	84.51 (12)	Si1—O2—Yb1	168.9 (6)
O1^viii—K1—Si1^vii	28.85 (13)	Si1—O2—K2^iii	104.8 (5)
O1^ix—K1—Si1^vii	91.48 (16)	Yb1—O2—K2^iii	86.3 (3)
O1^vii—K1—Si1^vii	85.47 (15)	Si1—O2—K1^vii	92.5 (2)
O1^ii—K1—Si1^vii	130.41 (11)	Yb1—O2—K1^vii	88.0 (2)
Si1^viii—K1—Si1^vii	100.43 (5)	K2^iii—O2—K1^vii	87.2 (2)
Si1^x—K1—Si1^vii	117.30 (10)	Si1—O2—K1^iii	92.5 (2)
O1—K2—O1^xi	139.8 (3)	Yb1—O2—K1^iii	88.0 (2)
O1—K2—O1^xii	98.4 (2)	K2^iii—O2—K1^iii	87.2 (2)
O1^xi—K2—O1^xii	67.5 (3)	K1^vii—O2—K1^iii	173.3 (4)
O1—K2—O1^i	67.5 (3)	Si1—O2—K1^iv	83.1 (4)
O1^xi—K2—O1^i	98.4 (2)	Yb1—O2—K1^iv	85.8 (3)
O1^xii—K2—O1^i	139.8 (3)	K2^iii—O2—K1^iv	172.1 (4)
O1—K2—O2^iii	66.66 (14)	K1^vii—O2—K1^iv	92.5 (2)
O1^xi—K2—O2^iii	144.19 (17)	K1^iii—O2—K1^iv	92.5 (2)
O1^xii—K2—O2^iii	144.19 (17)	Si1—O3—Si1^xvii	167.0 (11)
O1^i—K2—O2^iii	66.66 (14)	Si1—O3—K2^iii	96.5 (6)
O1—K2—O2^xiii	144.19 (17)	Si1^xvii—O3—K2^iii	96.5 (6)

Symmetry codes: (i) −x, y, z; (ii) x, −y, −z+1; (iii) −x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1, y, z; (vii) −x+1, −y, −z+1; (viii) x+1/2, y+1/2, z; (ix) −x+1/2, y+1/2, z; (x) −x+1/2, −y−1/2, −z+1; (xi) −x, y, −z+1/2; (xii) x, y, −z+1/2; (xiii) −x, −y, z−1/2; (xiv) −x−1/2, −y−1/2, z−1/2; (xv) x−1/2, −y−1/2, −z+1; (xvi) −x−1/2, −y−1/2, −z+1; (xvii) x, y, −z+3/2.

(173_K)

Crystal data

K3O7Si2Yb	Dx = 3.861 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1195 reflections
a = 5.7197 (6) Å	θ = 7.1–29.4°
b = 9.9102 (10) Å	µ = 13.74 mm^−1
c = 13.9165 (14) Å	T = 173 K
V = 788.83 (14) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	476 reflections with I > 2σ(I)
ω scans	Rint = 0.040
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.4°, θmin = 2.9°
Tmin = 0.304, Tmax = 0.398	h = −7→7
2683 measured reflections	k = −10→12
539 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0087P)^2 + 3.7066P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.020	(Δ/σ)max < 0.001
wR(F^2) = 0.041	Δρmax = 0.94 e Å^−3
S = 1.08	Δρmin = −0.80 e Å^−3
539 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
30 parameters	Extinction coefficient: 0.00355 (17)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00269 (15)
K1	0.500000	0.1720 (4)	0.40796 (11)	0.0076 (3)
K2	0.000000	0.0138 (4)	0.250000	0.0096 (5)
Si1	0.000000	−0.3374 (4)	0.63215 (14)	0.0029 (4)
O1	0.2667 (12)	−0.0815 (6)	0.3998 (4)	0.0092 (13)
O2	0.000000	−0.1861 (8)	0.5880 (7)	0.004 (2)
O3	0.000000	−0.3214 (15)	0.750000	0.0137 (19)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00242 (17)	0.00242 (17)	0.0032 (2)	0.000	0.000	0.000
K1	0.0062 (5)	0.0062 (5)	0.0103 (6)	0.000	0.000	0.000
K2	0.0121 (8)	0.0121 (8)	0.0047 (9)	0.000	0.000	0.000
Si1	0.0030 (5)	0.0030 (5)	0.0028 (7)	0.000	0.000	0.000
O1	0.0070 (15)	0.0070 (15)	0.014 (2)	0.000	0.000	0.000
O2	0.006 (3)	0.001 (3)	0.006 (3)	0.000	0.000	0.000
O3	0.029 (9)	0.006 (7)	0.006 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O2^i	2.214 (8)	K1—O1^vi	3.121 (6)
Yb1—O2	2.214 (8)	K1—O1^iii	3.121 (6)
Yb1—O1^ii	2.219 (5)	K1—Si1^viii	3.121 (3)
Yb1—O1^iii	2.219 (5)	K1—Si1^vi	3.343 (3)
Yb1—O1^i	2.219 (5)	K1—Si1^i	3.343 (3)
Yb1—O1	2.219 (5)	K2—O1	2.750 (5)
Yb1—K2	3.4818 (4)	K2—O1^x	2.750 (5)
Yb1—K2^i	3.4818 (4)	K2—O1^xi	2.750 (5)
Yb1—K1^iv	3.494 (4)	K2—O1^ii	2.750 (5)
Yb1—K1^v	3.494 (4)	K2—O2^i	2.828 (10)
Yb1—K1^i	3.5670 (19)	K2—O2^xii	2.828 (10)
Yb1—K1^vi	3.5670 (19)	K2—O3^i	3.048 (16)
K1—O1^vii	2.847 (9)	K2—Si1^i	3.602 (6)
K1—O1	2.847 (9)	K2—Si1^xii	3.602 (6)
K1—O2^vi	2.8638 (6)	K2—Si1^xiii	3.732 (3)
K1—O2^i	2.8638 (6)	Si1—O2	1.620 (9)
K1—O2^viii	2.873 (10)	Si1—O1^xiv	1.620 (5)
K1—O1^viii	2.882 (9)	Si1—O1^xv	1.620 (5)
K1—O1^ix	2.882 (9)	Si1—O3	1.648 (3)
O2^i—Yb1—O2	180.0	O1^x—K2—O2^xii	66.61 (13)
O2^i—Yb1—O1^ii	87.5 (2)	O1^xi—K2—O2^xii	66.61 (13)
O2—Yb1—O1^ii	92.5 (2)	O1^ii—K2—O2^xii	144.24 (16)
O2^i—Yb1—O1^iii	92.5 (2)	O2^i—K2—O2^xii	105.7 (4)
O2—Yb1—O1^iii	87.5 (2)	O1—K2—O3^i	110.08 (15)
O1^ii—Yb1—O1^iii	180.0 (2)	O1^x—K2—O3^i	110.08 (15)
O2^i—Yb1—O1^i	92.5 (2)	O1^xi—K2—O3^i	110.08 (15)
O2—Yb1—O1^i	87.5 (2)	O1^ii—K2—O3^i	110.08 (15)
O1^ii—Yb1—O1^i	93.1 (4)	O2^i—K2—O3^i	52.85 (18)
O1^iii—Yb1—O1^i	86.9 (4)	O2^xii—K2—O3^i	52.85 (18)
O2^i—Yb1—O1	87.5 (2)	O1—K2—Yb1^xii	138.07 (12)
O2—Yb1—O1	92.5 (2)	O1^x—K2—Yb1^xii	39.57 (11)
O1^ii—Yb1—O1	86.9 (4)	O1^xi—K2—Yb1^xii	39.57 (11)
O1^iii—Yb1—O1	93.1 (4)	O1^ii—K2—Yb1^xii	138.07 (12)
O1^i—Yb1—O1	180.0 (4)	O2^i—K2—Yb1^xii	145.1 (2)
O2^i—Yb1—K2	54.2 (3)	O2^xii—K2—Yb1^xii	39.39 (17)
O2—Yb1—K2	125.8 (3)	O3^i—K2—Yb1^xii	92.25 (7)
O1^ii—Yb1—K2	52.14 (14)	O1—K2—Yb1	39.57 (11)
O1^iii—Yb1—K2	127.86 (14)	O1^x—K2—Yb1	138.07 (12)
O1^i—Yb1—K2	127.86 (14)	O1^xi—K2—Yb1	138.07 (12)
O1—Yb1—K2	52.14 (14)	O1^ii—K2—Yb1	39.57 (11)
O2^i—Yb1—K2^i	125.8 (3)	O2^i—K2—Yb1	39.39 (17)
O2—Yb1—K2^i	54.2 (3)	O2^xii—K2—Yb1	145.1 (2)
O1^ii—Yb1—K2^i	127.86 (14)	O3^i—K2—Yb1	92.25 (6)
O1^iii—Yb1—K2^i	52.14 (14)	Yb1^xii—K2—Yb1	175.51 (13)
O1^i—Yb1—K2^i	52.14 (14)	O1—K2—Si1^i	87.74 (12)
O1—Yb1—K2^i	127.86 (14)	O1^x—K2—Si1^i	130.60 (18)
K2—Yb1—K2^i	180.0	O1^xi—K2—Si1^i	130.60 (18)
O2^i—Yb1—K1^iv	124.9 (2)	O1^ii—K2—Si1^i	87.74 (12)
O2—Yb1—K1^iv	55.1 (2)	O2^i—K2—Si1^i	25.77 (18)
O1^ii—Yb1—K1^iv	55.3 (2)	O2^xii—K2—Si1^i	79.94 (19)
O1^iii—Yb1—K1^iv	124.69 (19)	O3^i—K2—Si1^i	27.09 (5)
O1^i—Yb1—K1^iv	124.7 (2)	Yb1^xii—K2—Si1^i	119.33 (11)
O1—Yb1—K1^iv	55.3 (2)	Yb1—K2—Si1^i	65.16 (5)
K2—Yb1—K1^iv	70.74 (8)	O1—K2—Si1^xii	130.60 (18)
K2^i—Yb1—K1^iv	109.26 (8)	O1^x—K2—Si1^xii	87.74 (12)
O2^i—Yb1—K1^v	55.1 (2)	O1^xi—K2—Si1^xii	87.74 (12)
O2—Yb1—K1^v	124.9 (2)	O1^ii—K2—Si1^xii	130.60 (18)
O1^ii—Yb1—K1^v	124.7 (2)	O2^i—K2—Si1^xii	79.94 (19)
O1^iii—Yb1—K1^v	55.3 (2)	O2^xii—K2—Si1^xii	25.77 (18)
O1^i—Yb1—K1^v	55.3 (2)	O3^i—K2—Si1^xii	27.09 (5)
O1—Yb1—K1^v	124.7 (2)	Yb1^xii—K2—Si1^xii	65.16 (5)
K2—Yb1—K1^v	109.26 (8)	Yb1—K2—Si1^xii	119.33 (11)
K2^i—Yb1—K1^v	70.74 (8)	Si1^i—K2—Si1^xii	54.17 (11)
K1^iv—Yb1—K1^v	180.0	O1—K2—Si1^xiii	126.7 (2)
O2^i—Yb1—K1^i	126.63 (4)	O1^x—K2—Si1^xiii	23.22 (10)
O2—Yb1—K1^i	53.37 (4)	O1^xi—K2—Si1^xiii	86.05 (17)
O1^ii—Yb1—K1^i	60.04 (13)	O1^ii—K2—Si1^xiii	75.36 (11)
O1^iii—Yb1—K1^i	119.96 (14)	O2^i—K2—Si1^xiii	129.29 (5)
O1^i—Yb1—K1^i	52.9 (2)	O2^xii—K2—Si1^xiii	86.13 (12)
O1—Yb1—K1^i	127.1 (2)	O3^i—K2—Si1^xiii	117.94 (9)
K2—Yb1—K1^i	112.18 (4)	Yb1^xii—K2—Si1^xiii	62.77 (4)
K2^i—Yb1—K1^i	67.82 (4)	Yb1—K2—Si1^xiii	114.89 (6)
K1^iv—Yb1—K1^i	71.77 (5)	Si1^i—K2—Si1^xiii	128.11 (9)
K1^v—Yb1—K1^i	108.23 (5)	Si1^xii—K2—Si1^xiii	102.53 (6)
O2^i—Yb1—K1^vi	126.63 (4)	O2—Si1—O1^xiv	110.8 (3)
O2—Yb1—K1^vi	53.37 (4)	O2—Si1—O1^xv	110.8 (3)
O1^ii—Yb1—K1^vi	127.1 (2)	O1^xiv—Si1—O1^xv	110.9 (6)
O1^iii—Yb1—K1^vi	52.9 (2)	O2—Si1—O3	106.8 (7)
O1^i—Yb1—K1^vi	119.96 (13)	O1^xiv—Si1—O3	108.7 (3)
O1—Yb1—K1^vi	60.04 (13)	O1^xv—Si1—O3	108.7 (3)
K2—Yb1—K1^vi	112.18 (4)	O2—Si1—K1^iv	66.0 (4)
K2^i—Yb1—K1^vi	67.82 (4)	O1^xiv—Si1—K1^iv	74.95 (19)
K1^iv—Yb1—K1^vi	71.77 (5)	O1^xv—Si1—K1^iv	74.95 (19)
K1^v—Yb1—K1^vi	108.23 (5)	O3—Si1—K1^iv	172.8 (6)
K1^i—Yb1—K1^vi	106.59 (8)	O2—Si1—K1^vi	58.87 (10)
O1^vii—K1—O1	55.9 (2)	O1^xiv—Si1—K1^vi	154.4 (2)
O1^vii—K1—O2^vi	64.90 (15)	O1^xv—Si1—K1^vi	59.5 (3)
O1—K1—O2^vi	120.8 (3)	O3—Si1—K1^vi	96.8 (3)
O1^vii—K1—O2^i	120.8 (3)	K1^iv—Si1—K1^vi	79.55 (5)
O1—K1—O2^i	64.90 (15)	O2—Si1—K1^i	58.87 (10)
O2^vi—K1—O2^i	174.0 (4)	O1^xiv—Si1—K1^i	59.5 (3)
O1^vii—K1—O2^viii	117.8 (2)	O1^xv—Si1—K1^i	154.4 (2)
O1—K1—O2^viii	117.8 (2)	O3—Si1—K1^i	96.8 (3)
O2^vi—K1—O2^viii	87.6 (2)	K1^iv—Si1—K1^i	79.55 (5)
O2^i—K1—O2^viii	87.6 (2)	K1^vi—Si1—K1^i	117.61 (19)
O1^vii—K1—O1^viii	119.89 (2)	O2—Si1—K1^xv	148.2 (4)
O1—K1—O1^viii	174.0 (2)	O1^xiv—Si1—K1^xv	57.7 (3)
O2^vi—K1—O1^viii	55.31 (15)	O1^xv—Si1—K1^xv	57.7 (3)
O2^i—K1—O1^viii	119.2 (3)	O3—Si1—K1^xv	105.1 (5)
O2^viii—K1—O1^viii	67.63 (13)	K1^iv—Si1—K1^xv	82.14 (8)
O1^vii—K1—O1^ix	174.0 (2)	K1^vi—Si1—K1^xv	117.12 (10)
O1—K1—O1^ix	119.89 (2)	K1^i—Si1—K1^xv	117.12 (10)
O2^vi—K1—O1^ix	119.2 (3)	O2—Si1—K2^i	49.4 (3)
O2^i—K1—O1^ix	55.31 (15)	O1^xiv—Si1—K2^i	124.5 (3)
O2^viii—K1—O1^ix	67.63 (13)	O1^xv—Si1—K2^i	124.5 (3)
O1^viii—K1—O1^ix	63.9 (2)	O3—Si1—K2^i	57.4 (5)
O1^vii—K1—O1^vi	65.18 (16)	K1^iv—Si1—K2^i	115.39 (11)
O1—K1—O1^vi	88.92 (19)	K1^vi—Si1—K2^i	68.87 (11)
O2^vi—K1—O1^vi	64.5 (2)	K1^i—Si1—K2^i	68.87 (11)
O2^i—K1—O1^vi	115.1 (3)	K1^xv—Si1—K2^i	162.47 (8)
O2^viii—K1—O1^vi	52.64 (13)	O2—Si1—K2^xvi	126.88 (12)
O1^viii—K1—O1^vi	92.92 (15)	O1^xiv—Si1—K2^xvi	42.00 (19)
O1^ix—K1—O1^vi	120.23 (11)	O1^xv—Si1—K2^xvi	121.3 (3)
O1^vii—K1—O1^iii	88.92 (19)	O3—Si1—K2^xvi	66.9 (3)
O1—K1—O1^iii	65.18 (16)	K1^iv—Si1—K2^xvi	116.95 (6)
O2^vi—K1—O1^iii	115.1 (3)	K1^vi—Si1—K2^xvi	163.47 (6)
O2^i—K1—O1^iii	64.5 (2)	K1^i—Si1—K2^xvi	69.36 (7)
O2^viii—K1—O1^iii	52.64 (13)	K1^xv—Si1—K2^xvi	67.11 (9)
O1^viii—K1—O1^iii	120.23 (11)	K2^i—Si1—K2^xvi	102.53 (6)
O1^ix—K1—O1^iii	92.92 (15)	O2—Si1—K2^xv	126.88 (12)
O1^vi—K1—O1^iii	50.6 (3)	O1^xiv—Si1—K2^xv	121.3 (3)
O1^vii—K1—Si1^viii	90.78 (12)	O1^xv—Si1—K2^xv	42.00 (18)
O1—K1—Si1^viii	90.78 (12)	O3—Si1—K2^xv	66.9 (3)
O2^vi—K1—Si1^viii	89.0 (2)	K1^iv—Si1—K2^xv	116.95 (6)
O2^i—K1—Si1^viii	89.0 (2)	K1^vi—Si1—K2^xv	69.36 (7)
O2^viii—K1—Si1^viii	31.01 (18)	K1^i—Si1—K2^xv	163.47 (6)
O1^viii—K1—Si1^viii	93.70 (13)	K1^xv—Si1—K2^xv	67.11 (9)
O1^ix—K1—Si1^viii	93.70 (13)	K2^i—Si1—K2^xv	102.53 (6)
O1^vi—K1—Si1^viii	30.09 (10)	K2^xvi—Si1—K2^xv	100.06 (11)
O1^iii—K1—Si1^viii	30.09 (10)	Si1^xv—O1—Yb1	156.8 (3)
O1^vii—K1—Si1^vi	91.43 (13)	Si1^xv—O1—K2	114.8 (2)
O1—K1—Si1^vi	145.79 (17)	Yb1—O1—K2	88.29 (17)
O2^vi—K1—Si1^vi	28.96 (17)	Si1^xv—O1—K1	93.6 (4)
O2^i—K1—Si1^vi	146.5 (2)	Yb1—O1—K1	88.62 (19)
O2^viii—K1—Si1^vi	84.58 (12)	K2—O1—K1	89.27 (17)
O1^viii—K1—Si1^vi	28.98 (12)	Si1^xv—O1—K1^iv	91.5 (3)
O1^ix—K1—Si1^vi	91.75 (17)	Yb1—O1—K1^iv	85.4 (2)
O1^vi—K1—Si1^vi	85.31 (14)	K2—O1—K1^iv	91.6 (2)
O1^iii—K1—Si1^vi	130.52 (11)	K1—O1—K1^iv	174.0 (2)
Si1^viii—K1—Si1^vi	100.45 (5)	Si1^xv—O1—K1^vi	74.96 (19)
O1^vii—K1—Si1^i	145.79 (17)	Yb1—O1—K1^vi	81.94 (15)
O1—K1—Si1^i	91.43 (13)	K2—O1—K1^vi	170.2 (2)
O2^vi—K1—Si1^i	146.5 (2)	K1—O1—K1^vi	91.08 (19)
O2^i—K1—Si1^i	28.96 (17)	K1^iv—O1—K1^vi	87.08 (15)
O2^viii—K1—Si1^i	84.58 (12)	Si1—O2—Yb1	168.7 (6)
O1^viii—K1—Si1^i	91.75 (17)	Si1—O2—K2^i	104.9 (4)
O1^ix—K1—Si1^i	28.98 (12)	Yb1—O2—K2^i	86.4 (3)
O1^vi—K1—Si1^i	130.52 (11)	Si1—O2—K1^vi	92.17 (19)
O1^iii—K1—Si1^i	85.31 (14)	Yb1—O2—K1^vi	88.29 (19)
Si1^viii—K1—Si1^i	100.45 (5)	K2^i—O2—K1^vi	87.41 (19)
Si1^vi—K1—Si1^i	117.61 (19)	Si1—O2—K1^i	92.17 (19)
O1—K2—O1^x	139.8 (3)	Yb1—O2—K1^i	88.29 (19)
O1—K2—O1^xi	98.6 (2)	K2^i—O2—K1^i	87.41 (19)
O1^x—K2—O1^xi	67.4 (3)	K1^vi—O2—K1^i	174.0 (4)
O1—K2—O1^ii	67.4 (3)	Si1—O2—K1^iv	83.0 (4)
O1^x—K2—O1^ii	98.6 (2)	Yb1—O2—K1^iv	85.7 (3)
O1^xi—K2—O1^ii	139.8 (3)	K2^i—O2—K1^iv	172.2 (3)
O1—K2—O2^i	66.62 (13)	K1^vi—O2—K1^iv	92.4 (2)
O1^x—K2—O2^i	144.24 (16)	K1^i—O2—K1^iv	92.4 (2)
O1^xi—K2—O2^i	144.24 (16)	Si1^xvii—O3—Si1	168.9 (11)
O1^ii—K2—O2^i	66.61 (13)	Si1^xvii—O3—K2^i	95.5 (5)
O1—K2—O2^xii	144.24 (16)	Si1—O3—K2^i	95.5 (5)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, y, z; (iii) x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1, −y, −z+1; (vii) −x+1, y, z; (viii) x+1/2, y+1/2, z; (ix) −x+1/2, y+1/2, z; (x) −x, y, −z+1/2; (xi) x, y, −z+1/2; (xii) −x, −y, z−1/2; (xiii) −x−1/2, −y−1/2, z−1/2; (xiv) x−1/2, −y−1/2, −z+1; (xv) −x+1/2, −y−1/2, −z+1; (xvi) −x−1/2, −y−1/2, −z+1; (xvii) x, y, −z+3/2.

(183_K)

Crystal data

K3O7Si2Yb	Dx = 3.865 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1186 reflections
a = 5.7170 (6) Å	θ = 4.1–29.4°
b = 9.9025 (10) Å	µ = 13.76 mm^−1
c = 13.9173 (14) Å	T = 183 K
V = 787.89 (14) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	467 reflections with I > 2σ(I)
ω scans	Rint = 0.039
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.304, Tmax = 0.397	h = −7→7
2681 measured reflections	k = −12→10
539 independent reflections	l = −16→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0144P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.021	(Δ/σ)max < 0.001
wR(F^2) = 0.043	Δρmax = 1.03 e Å^−3
S = 1.12	Δρmin = −0.97 e Å^−3
539 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
29 parameters	Extinction coefficient: 0.00346 (17)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00276 (16)
K1	0.500000	0.1712 (4)	0.40795 (11)	0.0077 (3)
K2	0.000000	0.0119 (4)	0.250000	0.0113 (5)
Si1	0.000000	−0.3369 (5)	0.63239 (14)	0.0034 (4)
O1	0.2666 (12)	−0.0821 (6)	0.3998 (3)	0.0093 (13)
O2	0.000000	−0.1864 (8)	0.5881 (6)	0.004 (2)
O3	0.000000	−0.3223 (16)	0.750000	0.0121 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00260 (18)	0.00260 (18)	0.0031 (2)	0.000	0.000	0.000
K1	0.0060 (4)	0.0060 (4)	0.0110 (7)	0.000	0.000	0.000
K2	0.0144 (8)	0.0144 (8)	0.0053 (10)	0.000	0.000	0.000
Si1	0.0035 (5)	0.0035 (5)	0.0032 (8)	0.000	0.000	0.000
O1	0.0081 (17)	0.0081 (17)	0.012 (2)	0.000	0.000	0.000
O2	0.004 (2)	0.004 (2)	0.004 (2)	0.000	0.000	0.000
O3	0.024 (9)	0.010 (7)	0.003 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O2^i	2.216 (8)	K1—O1^vii	3.117 (5)
Yb1—O2	2.216 (8)	K1—O1^iii	3.117 (5)
Yb1—O1^ii	2.220 (5)	K1—Si1^viii	3.125 (3)
Yb1—O1^iii	2.220 (5)	K1—Si1^vii	3.343 (3)
Yb1—O1^i	2.220 (5)	K1—Si1^i	3.343 (3)
Yb1—O1	2.220 (5)	K2—O1	2.746 (5)
Yb1—K2^i	3.4813 (4)	K2—O1^x	2.746 (5)
Yb1—K2	3.4813 (4)	K2—O1^xi	2.746 (5)
Yb1—K1^iv	3.499 (4)	K2—O1^ii	2.746 (5)
Yb1—K1^v	3.499 (4)	K2—O2^i	2.839 (10)
Yb1—K1^i	3.5617 (19)	K2—O2^xii	2.839 (10)
Yb1—K1	3.5617 (19)	K2—O3^i	3.074 (18)
K1—O1	2.843 (9)	K2—O3^xiii	3.420 (10)
K1—O1^vi	2.843 (9)	K2—O3^xiv	3.420 (10)
K1—O2^vii	2.8630 (6)	K2—Si1^i	3.610 (6)
K1—O2^i	2.8630 (6)	Si1—O2	1.613 (9)
K1—O2^viii	2.877 (9)	Si1—O1^xv	1.620 (5)
K1—O1^viii	2.882 (9)	Si1—O1^xiv	1.620 (5)
K1—O1^ix	2.882 (9)	Si1—O3	1.643 (3)
O2^i—Yb1—O2	180.0	O1—K2—O3^i	109.83 (16)
O2^i—Yb1—O1^ii	87.6 (2)	O1^x—K2—O3^i	109.83 (16)
O2—Yb1—O1^ii	92.4 (2)	O1^xi—K2—O3^i	109.83 (16)
O2^i—Yb1—O1^iii	92.4 (2)	O1^ii—K2—O3^i	109.83 (16)
O2—Yb1—O1^iii	87.6 (2)	O2^i—K2—O3^i	52.52 (18)
O1^ii—Yb1—O1^iii	180.0	O2^xii—K2—O3^i	52.52 (18)
O2^i—Yb1—O1^i	92.4 (2)	O1—K2—O3^xiii	106.1 (3)
O2—Yb1—O1^i	87.6 (2)	O1^x—K2—O3^xiii	49.44 (10)
O1^ii—Yb1—O1^i	93.3 (4)	O1^xi—K2—O3^xiii	106.1 (3)
O1^iii—Yb1—O1^i	86.7 (4)	O1^ii—K2—O3^xiii	49.44 (10)
O2^i—Yb1—O1	87.6 (2)	O2^i—K2—O3^xiii	109.51 (14)
O2—Yb1—O1	92.4 (2)	O2^xii—K2—O3^xiii	109.51 (14)
O1^ii—Yb1—O1	86.7 (4)	O3^i—K2—O3^xiii	123.3 (2)
O1^iii—Yb1—O1	93.3 (4)	O1—K2—O3^xiv	49.44 (10)
O1^i—Yb1—O1	180.0	O1^x—K2—O3^xiv	106.1 (3)
O2^i—Yb1—K2^i	125.5 (3)	O1^xi—K2—O3^xiv	49.44 (10)
O2—Yb1—K2^i	54.5 (3)	O1^ii—K2—O3^xiv	106.1 (3)
O1^ii—Yb1—K2^i	127.97 (13)	O2^i—K2—O3^xiv	109.51 (14)
O1^iii—Yb1—K2^i	52.03 (14)	O2^xii—K2—O3^xiv	109.51 (14)
O1^i—Yb1—K2^i	52.03 (13)	O3^i—K2—O3^xiv	123.3 (2)
O1—Yb1—K2^i	127.97 (13)	O3^xiii—K2—O3^xiv	113.4 (5)
O2^i—Yb1—K2	54.5 (3)	O1—K2—Yb1^xii	138.37 (12)
O2—Yb1—K2	125.5 (3)	O1^x—K2—Yb1^xii	39.60 (10)
O1^ii—Yb1—K2	52.03 (13)	O1^xi—K2—Yb1^xii	39.60 (10)
O1^iii—Yb1—K2	127.97 (14)	O1^ii—K2—Yb1^xii	138.37 (12)
O1^i—Yb1—K2	127.97 (13)	O2^i—K2—Yb1^xii	144.5 (2)
O1—Yb1—K2	52.03 (13)	O2^xii—K2—Yb1^xii	39.42 (17)
K2^i—Yb1—K2	180.0	O3^i—K2—Yb1^xii	91.94 (7)
O2^i—Yb1—K1^iv	124.9 (2)	O3^xiii—K2—Yb1^xii	88.93 (4)
O2—Yb1—K1^iv	55.1 (2)	O3^xiv—K2—Yb1^xii	88.93 (4)
O1^ii—Yb1—K1^iv	55.2 (2)	O1—K2—Yb1	39.60 (10)
O1^iii—Yb1—K1^iv	124.8 (2)	O1^x—K2—Yb1	138.37 (12)
O1^i—Yb1—K1^iv	124.8 (2)	O1^xi—K2—Yb1	138.37 (12)
O1—Yb1—K1^iv	55.2 (2)	O1^ii—K2—Yb1	39.60 (10)
K2^i—Yb1—K1^iv	109.53 (8)	O2^i—K2—Yb1	39.42 (17)
K2—Yb1—K1^iv	70.47 (8)	O2^xii—K2—Yb1	144.5 (2)
O2^i—Yb1—K1^v	55.1 (2)	O3^i—K2—Yb1	91.94 (7)
O2—Yb1—K1^v	124.9 (2)	O3^xiii—K2—Yb1	88.93 (4)
O1^ii—Yb1—K1^v	124.8 (2)	O3^xiv—K2—Yb1	88.93 (4)
O1^iii—Yb1—K1^v	55.2 (2)	Yb1^xii—K2—Yb1	176.11 (14)
O1^i—Yb1—K1^v	55.2 (2)	O1—K2—Si1^i	87.59 (13)
O1—Yb1—K1^v	124.8 (2)	O1^x—K2—Si1^i	130.29 (19)
K2^i—Yb1—K1^v	70.47 (8)	O1^xi—K2—Si1^i	130.29 (19)
K2—Yb1—K1^v	109.53 (8)	O1^ii—K2—Si1^i	87.59 (13)
K1^iv—Yb1—K1^v	180.00 (5)	O2^i—K2—Si1^i	25.56 (18)
O2^i—Yb1—K1^i	126.55 (4)	O2^xii—K2—Si1^i	79.5 (2)
O2—Yb1—K1^i	53.45 (4)	O3^i—K2—Si1^i	26.96 (6)
O1^ii—Yb1—K1^i	60.03 (13)	O3^xiii—K2—Si1^i	119.3 (2)
O1^iii—Yb1—K1^i	119.97 (13)	O3^xiv—K2—Si1^i	119.3 (2)
O1^i—Yb1—K1^i	52.9 (2)	Yb1^xii—K2—Si1^i	118.90 (12)
O1—Yb1—K1^i	127.1 (2)	Yb1—K2—Si1^i	64.98 (5)
K2^i—Yb1—K1^i	67.94 (5)	O2—Si1—O1^xv	110.6 (3)
K2—Yb1—K1^i	112.06 (5)	O2—Si1—O1^xiv	110.6 (3)
K1^iv—Yb1—K1^i	71.87 (5)	O1^xv—Si1—O1^xiv	110.9 (6)
K1^v—Yb1—K1^i	108.13 (5)	O2—Si1—O3	107.4 (8)
O2^i—Yb1—K1	53.45 (4)	O1^xv—Si1—O3	108.6 (4)
O2—Yb1—K1	126.55 (4)	O1^xiv—Si1—O3	108.6 (4)
O1^ii—Yb1—K1	119.97 (13)	O2—Si1—K1^iv	66.1 (3)
O1^iii—Yb1—K1	60.03 (13)	O1^xv—Si1—K1^iv	74.69 (18)
O1^i—Yb1—K1	127.1 (2)	O1^xiv—Si1—K1^iv	74.69 (18)
O1—Yb1—K1	52.9 (2)	O3—Si1—K1^iv	173.5 (6)
K2^i—Yb1—K1	112.06 (5)	O2—Si1—K1^vii	58.82 (10)
K2—Yb1—K1	67.94 (5)	O1^xv—Si1—K1^vii	154.24 (19)
K1^iv—Yb1—K1	108.13 (5)	O1^xiv—Si1—K1^vii	59.5 (3)
K1^v—Yb1—K1	71.87 (5)	O3—Si1—K1^vii	97.1 (3)
K1^i—Yb1—K1	180.00 (11)	K1^iv—Si1—K1^vii	79.60 (5)
O1—K1—O1^vi	56.0 (2)	O2—Si1—K1^i	58.82 (10)
O1—K1—O2^vii	121.0 (3)	O1^xv—Si1—K1^i	59.5 (3)
O1^vi—K1—O2^vii	65.08 (15)	O1^xiv—Si1—K1^i	154.24 (19)
O1—K1—O2^i	65.08 (15)	O3—Si1—K1^i	97.1 (3)
O1^vi—K1—O2^i	121.0 (3)	K1^iv—Si1—K1^i	79.60 (5)
O2^vii—K1—O2^i	173.6 (4)	K1^vii—Si1—K1^i	117.51 (19)
O1—K1—O2^viii	117.9 (2)	O2—Si1—K1^xiv	147.9 (3)
O1^vi—K1—O2^viii	117.9 (2)	O1^xv—Si1—K1^xiv	57.7 (3)
O2^vii—K1—O2^viii	87.56 (18)	O1^xiv—Si1—K1^xiv	57.7 (3)
O2^i—K1—O2^viii	87.56 (19)	O3—Si1—K1^xiv	104.7 (6)
O1—K1—O1^viii	174.0 (2)	K1^iv—Si1—K1^xiv	81.84 (9)
O1^vi—K1—O1^viii	119.87 (2)	K1^vii—Si1—K1^xiv	117.12 (10)
O2^vii—K1—O1^viii	55.11 (15)	K1^i—Si1—K1^xiv	117.12 (10)
O2^i—K1—O1^viii	119.0 (3)	O2—Si1—K2^i	49.4 (3)
O2^viii—K1—O1^viii	67.58 (14)	O1^xv—Si1—K2^i	124.5 (3)
O1—K1—O1^ix	119.87 (2)	O1^xiv—Si1—K2^i	124.5 (3)
O1^vi—K1—O1^ix	174.0 (2)	O3—Si1—K2^i	58.0 (6)
O2^vii—K1—O1^ix	119.0 (3)	K1^iv—Si1—K2^i	115.49 (12)
O2^i—K1—O1^ix	55.11 (15)	K1^vii—Si1—K2^i	68.82 (11)
O2^viii—K1—O1^ix	67.58 (14)	K1^i—Si1—K2^i	68.82 (11)
O1^viii—K1—O1^ix	63.9 (2)	K1^xiv—Si1—K2^i	162.67 (9)
O1—K1—O1^vii	89.16 (19)	O2—Si1—K2^xiii	126.75 (12)
O1^vi—K1—O1^vii	65.40 (15)	O1^xv—Si1—K2^xiii	42.15 (17)
O2^vii—K1—O1^vii	64.6 (2)	O1^xiv—Si1—K2^xiii	121.6 (3)
O2^i—K1—O1^vii	115.2 (2)	O3—Si1—K2^xiii	66.6 (3)
O2^viii—K1—O1^vii	52.46 (13)	K1^iv—Si1—K2^xiii	116.84 (6)
O1^viii—K1—O1^vii	92.70 (14)	K1^vii—Si1—K2^xiii	163.53 (6)
O1^ix—K1—O1^vii	120.00 (10)	K1^i—Si1—K2^xiii	69.26 (7)
O1—K1—O1^iii	65.40 (15)	K1^xiv—Si1—K2^xiii	67.32 (10)
O1^vi—K1—O1^iii	89.16 (19)	K2^i—Si1—K2^xiii	102.46 (6)
O2^vii—K1—O1^iii	115.2 (2)	O2—Si1—K2^xiv	126.75 (12)
O2^i—K1—O1^iii	64.6 (2)	O1^xv—Si1—K2^xiv	121.6 (3)
O2^viii—K1—O1^iii	52.46 (13)	O1^xiv—Si1—K2^xiv	42.15 (17)
O1^viii—K1—O1^iii	120.00 (10)	O3—Si1—K2^xiv	66.6 (3)
O1^ix—K1—O1^iii	92.70 (14)	K1^iv—Si1—K2^xiv	116.84 (6)
O1^vii—K1—O1^iii	50.7 (3)	K1^vii—Si1—K2^xiv	69.26 (7)
O1—K1—Si1^viii	90.99 (12)	K1^i—Si1—K2^xiv	163.53 (6)
O1^vi—K1—Si1^viii	90.99 (12)	K1^xiv—Si1—K2^xiv	67.32 (10)
O2^vii—K1—Si1^viii	88.98 (19)	K2^i—Si1—K2^xiv	102.46 (6)
O2^i—K1—Si1^viii	88.98 (19)	K2^xiii—Si1—K2^xiv	100.35 (12)
O2^viii—K1—Si1^viii	30.83 (18)	Si1^xiv—O1—Yb1	157.0 (3)
O1^viii—K1—Si1^viii	93.49 (12)	Si1^xiv—O1—K2	114.5 (2)
O1^ix—K1—Si1^viii	93.49 (12)	Yb1—O1—K2	88.37 (17)
O1^vii—K1—Si1^viii	30.09 (10)	Si1^xiv—O1—K1	93.5 (4)
O1^iii—K1—Si1^viii	30.09 (10)	Yb1—O1—K1	88.51 (19)
O1—K1—Si1^vii	145.84 (16)	K2—O1—K1	89.52 (18)
O1^vi—K1—Si1^vii	91.44 (13)	Si1^xiv—O1—K1^iv	91.5 (3)
O2^vii—K1—Si1^vii	28.81 (18)	Yb1—O1—K1^iv	85.6 (2)
O2^i—K1—Si1^vii	146.2 (2)	K2—O1—K1^iv	91.4 (2)
O2^viii—K1—Si1^vii	84.59 (12)	K1—O1—K1^iv	174.0 (2)
O1^viii—K1—Si1^vii	28.97 (12)	Si1^xiv—O1—K1^vii	75.22 (19)
O1^ix—K1—Si1^vii	91.70 (17)	Yb1—O1—K1^vii	81.86 (14)
O1^vii—K1—Si1^vii	85.24 (15)	K2—O1—K1^vii	170.2 (2)
O1^iii—K1—Si1^vii	130.46 (11)	K1—O1—K1^vii	90.84 (19)
Si1^viii—K1—Si1^vii	100.39 (5)	K1^iv—O1—K1^vii	87.29 (14)
O1—K1—Si1^i	91.44 (13)	Si1—O2—Yb1	168.9 (6)
O1^vi—K1—Si1^i	145.84 (16)	Si1—O2—K2^i	105.0 (4)
O2^vii—K1—Si1^i	146.2 (2)	Yb1—O2—K2^i	86.1 (3)
O2^i—K1—Si1^i	28.81 (18)	Si1—O2—K1^vii	92.36 (19)
O2^viii—K1—Si1^i	84.59 (12)	Yb1—O2—K1^vii	88.10 (19)
O1^viii—K1—Si1^i	91.70 (16)	K2^i—O2—K1^vii	87.30 (18)
O1^ix—K1—Si1^i	28.97 (12)	Si1—O2—K1^i	92.36 (19)
O1^vii—K1—Si1^i	130.46 (11)	Yb1—O2—K1^i	88.10 (19)
O1^iii—K1—Si1^i	85.24 (15)	K2^i—O2—K1^i	87.30 (18)
Si1^viii—K1—Si1^i	100.39 (5)	K1^vii—O2—K1^i	173.6 (4)
Si1^vii—K1—Si1^i	117.51 (19)	Si1—O2—K1^iv	83.1 (4)
O1—K2—O1^x	140.3 (3)	Yb1—O2—K1^iv	85.8 (3)
O1—K2—O1^xi	98.8 (2)	K2^i—O2—K1^iv	171.9 (3)
O1^x—K2—O1^xi	67.4 (3)	K1^vii—O2—K1^iv	92.43 (18)
O1—K2—O1^ii	67.5 (3)	K1^i—O2—K1^iv	92.43 (18)
O1^x—K2—O1^ii	98.8 (2)	Si1—O3—Si1^xvi	169.9 (12)
O1^xi—K2—O1^ii	140.3 (3)	Si1—O3—K2^i	95.0 (6)
O1—K2—O2^i	66.65 (14)	Si1^xvi—O3—K2^i	95.0 (6)
O1^x—K2—O2^i	144.00 (17)	Si1—O3—K2^xiii	87.2 (3)
O1^xi—K2—O2^i	144.00 (17)	Si1^xvi—O3—K2^xiii	87.2 (3)
O1^ii—K2—O2^i	66.65 (14)	K2^i—O3—K2^xiii	123.3 (2)
O1—K2—O2^xii	144.00 (17)	Si1—O3—K2^xiv	87.2 (3)
O1^x—K2—O2^xii	66.65 (14)	Si1^xvi—O3—K2^xiv	87.2 (3)
O1^xi—K2—O2^xii	66.65 (14)	K2^i—O3—K2^xiv	123.3 (2)
O1^ii—K2—O2^xii	144.00 (17)	K2^xiii—O3—K2^xiv	113.4 (5)
O2^i—K2—O2^xii	105.0 (4)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, y, z; (iii) x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1, y, z; (vii) −x+1, −y, −z+1; (viii) x+1/2, y+1/2, z; (ix) −x+1/2, y+1/2, z; (x) −x, y, −z+1/2; (xi) x, y, −z+1/2; (xii) −x, −y, z−1/2; (xiii) −x−1/2, −y−1/2, −z+1; (xiv) −x+1/2, −y−1/2, −z+1; (xv) x−1/2, −y−1/2, −z+1; (xvi) x, y, −z+3/2.

(193_K)

Crystal data

K3O7Si2Yb	Dx = 3.857 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1180 reflections
a = 5.7205 (7) Å	θ = 5.8–29.4°
b = 9.9117 (11) Å	µ = 13.73 mm^−1
c = 13.9253 (15) Å	T = 193 K
V = 789.56 (15) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	462 reflections with I > 2σ(I)
ω scans	Rint = 0.040
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.4°, θmin = 2.9°
Tmin = 0.304, Tmax = 0.398	h = −7→7
2693 measured reflections	k = −12→10
539 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0064P)^2 + 2.6726P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.019	(Δ/σ)max < 0.001
wR(F^2) = 0.038	Δρmax = 0.83 e Å^−3
S = 1.06	Δρmin = −0.73 e Å^−3
539 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
30 parameters	Extinction coefficient: 0.00350 (15)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00290 (14)
K1	0.500000	0.1706 (4)	0.40806 (11)	0.0083 (3)
K2	0.000000	0.0110 (5)	0.250000	0.0111 (5)
Si1	0.000000	−0.3362 (5)	0.63224 (13)	0.0032 (3)
O1	0.2675 (13)	−0.0831 (7)	0.4001 (4)	0.0079 (13)
O2	0.000000	−0.1845 (9)	0.5885 (7)	0.006 (2)
O3	0.000000	−0.3221 (18)	0.750000	0.0139 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00250 (16)	0.00250 (16)	0.0037 (2)	0.000	0.000	0.000
K1	0.0069 (4)	0.0069 (4)	0.0111 (6)	0.000	0.000	0.000
K2	0.0142 (7)	0.0142 (7)	0.0050 (8)	0.000	0.000	0.000
Si1	0.0038 (5)	0.0038 (5)	0.0020 (7)	0.000	0.000	0.000
O1	0.0065 (16)	0.0065 (16)	0.011 (2)	0.000	0.000	0.000
O2	0.007 (3)	0.003 (3)	0.007 (3)	0.000	0.000	0.000
O3	0.020 (8)	0.018 (8)	0.004 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O2	2.206 (9)	K1—O1^vi	3.107 (6)
Yb1—O2^i	2.206 (9)	K1—O1^iii	3.107 (6)
Yb1—O1	2.226 (5)	K1—Si1^viii	3.122 (3)
Yb1—O1^ii	2.226 (5)	K1—Si1^vi	3.346 (4)
Yb1—O1^iii	2.226 (5)	K1—Si1^i	3.346 (4)
Yb1—O1^i	2.226 (5)	K2—O1^x	2.754 (5)
Yb1—K2	3.4830 (4)	K2—O1^xi	2.754 (5)
Yb1—K2^i	3.4830 (4)	K2—O1^ii	2.754 (5)
Yb1—K1^iv	3.507 (4)	K2—O1	2.754 (5)
Yb1—K1^v	3.507 (4)	K2—O2^i	2.831 (11)
Yb1—K1^i	3.561 (2)	K2—O2^xii	2.831 (11)
Yb1—K1^vi	3.561 (2)	K2—O3^i	3.084 (19)
K1—O1^vii	2.846 (10)	K2—O3^xiii	3.418 (11)
K1—O1	2.846 (10)	K2—O3^xiv	3.418 (11)
K1—O2^vi	2.8640 (6)	K2—Si1^i	3.617 (7)
K1—O2^i	2.8640 (6)	Si1—O1^xv	1.616 (6)
K1—O1^viii	2.884 (10)	Si1—O1^xiv	1.616 (6)
K1—O1^ix	2.884 (10)	Si1—O2	1.622 (10)
K1—O2^viii	2.895 (10)	Si1—O3	1.646 (3)
O2—Yb1—O2^i	180.0	O1^x—K2—O3^i	109.79 (17)
O2—Yb1—O1	92.4 (2)	O1^xi—K2—O3^i	109.79 (17)
O2^i—Yb1—O1	87.6 (2)	O1^ii—K2—O3^i	109.79 (17)
O2—Yb1—O1^ii	92.4 (2)	O1—K2—O3^i	109.79 (17)
O2^i—Yb1—O1^ii	87.6 (2)	O2^i—K2—O3^i	52.58 (19)
O1—Yb1—O1^ii	86.9 (4)	O2^xii—K2—O3^i	52.58 (19)
O2—Yb1—O1^iii	87.6 (2)	O1^x—K2—O3^xiii	49.42 (10)
O2^i—Yb1—O1^iii	92.4 (2)	O1^xi—K2—O3^xiii	106.2 (3)
O1—Yb1—O1^iii	93.1 (4)	O1^ii—K2—O3^xiii	49.42 (10)
O1^ii—Yb1—O1^iii	180.0	O1—K2—O3^xiii	106.2 (3)
O2—Yb1—O1^i	87.6 (2)	O2^i—K2—O3^xiii	109.43 (15)
O2^i—Yb1—O1^i	92.4 (2)	O2^xii—K2—O3^xiii	109.43 (15)
O1—Yb1—O1^i	180.0 (3)	O3^i—K2—O3^xiii	123.2 (3)
O1^ii—Yb1—O1^i	93.1 (4)	O1^x—K2—O3^xiv	106.2 (3)
O1^iii—Yb1—O1^i	86.9 (4)	O1^xi—K2—O3^xiv	49.42 (10)
O2—Yb1—K2	125.8 (3)	O1^ii—K2—O3^xiv	106.2 (3)
O2^i—Yb1—K2	54.2 (3)	O1—K2—O3^xiv	49.42 (10)
O1—Yb1—K2	52.20 (14)	O2^i—K2—O3^xiv	109.43 (15)
O1^ii—Yb1—K2	52.20 (14)	O2^xii—K2—O3^xiv	109.43 (15)
O1^iii—Yb1—K2	127.80 (14)	O3^i—K2—O3^xiv	123.2 (3)
O1^i—Yb1—K2	127.80 (14)	O3^xiii—K2—O3^xiv	113.6 (5)
O2—Yb1—K2^i	54.2 (3)	O1^x—K2—Yb1^xii	39.69 (11)
O2^i—Yb1—K2^i	125.8 (3)	O1^xi—K2—Yb1^xii	39.69 (11)
O1—Yb1—K2^i	127.80 (14)	O1^ii—K2—Yb1^xii	138.45 (12)
O1^ii—Yb1—K2^i	127.80 (14)	O1—K2—Yb1^xii	138.45 (12)
O1^iii—Yb1—K2^i	52.20 (14)	O2^i—K2—Yb1^xii	144.4 (2)
O1^i—Yb1—K2^i	52.20 (14)	O2^xii—K2—Yb1^xii	39.20 (19)
K2—Yb1—K2^i	180.0	O3^i—K2—Yb1^xii	91.79 (8)
O2—Yb1—K1^iv	55.4 (2)	O3^xiii—K2—Yb1^xii	89.02 (5)
O2^i—Yb1—K1^iv	124.6 (2)	O3^xiv—K2—Yb1^xii	89.02 (5)
O1—Yb1—K1^iv	55.1 (2)	O1^x—K2—Yb1	138.45 (12)
O1^ii—Yb1—K1^iv	55.1 (2)	O1^xi—K2—Yb1	138.45 (12)
O1^iii—Yb1—K1^iv	124.9 (2)	O1^ii—K2—Yb1	39.69 (11)
O1^i—Yb1—K1^iv	124.9 (2)	O1—K2—Yb1	39.69 (11)
K2—Yb1—K1^iv	70.38 (9)	O2^i—K2—Yb1	39.20 (19)
K2^i—Yb1—K1^iv	109.62 (9)	O2^xii—K2—Yb1	144.4 (2)
O2—Yb1—K1^v	124.6 (2)	O3^i—K2—Yb1	91.79 (8)
O2^i—Yb1—K1^v	55.4 (2)	O3^xiii—K2—Yb1	89.02 (5)
O1—Yb1—K1^v	124.9 (2)	O3^xiv—K2—Yb1	89.02 (5)
O1^ii—Yb1—K1^v	124.9 (2)	Yb1^xii—K2—Yb1	176.42 (15)
O1^iii—Yb1—K1^v	55.1 (2)	O1^x—K2—Si1^i	130.2 (2)
O1^i—Yb1—K1^v	55.1 (2)	O1^xi—K2—Si1^i	130.2 (2)
K2—Yb1—K1^v	109.62 (9)	O1^ii—K2—Si1^i	87.57 (14)
K2^i—Yb1—K1^v	70.38 (9)	O1—K2—Si1^i	87.57 (14)
K1^iv—Yb1—K1^v	180.0	O2^i—K2—Si1^i	25.62 (19)
O2—Yb1—K1^i	53.51 (5)	O2^xii—K2—Si1^i	79.5 (2)
O2^i—Yb1—K1^i	126.49 (5)	O3^i—K2—Si1^i	26.96 (6)
O1—Yb1—K1^i	127.0 (2)	O3^xiii—K2—Si1^i	119.2 (2)
O1^ii—Yb1—K1^i	59.78 (14)	O3^xiv—K2—Si1^i	119.2 (2)
O1^iii—Yb1—K1^i	120.22 (14)	Yb1^xii—K2—Si1^i	118.75 (13)
O1^i—Yb1—K1^i	53.0 (2)	Yb1—K2—Si1^i	64.83 (5)
K2—Yb1—K1^i	111.97 (5)	O1^xv—Si1—O1^xiv	110.8 (6)
K2^i—Yb1—K1^i	68.03 (5)	O1^xv—Si1—O2	110.7 (3)
K1^iv—Yb1—K1^i	71.89 (5)	O1^xiv—Si1—O2	110.7 (3)
K1^v—Yb1—K1^i	108.11 (5)	O1^xv—Si1—O3	108.7 (4)
O2—Yb1—K1^vi	53.51 (5)	O1^xiv—Si1—O3	108.7 (4)
O2^i—Yb1—K1^vi	126.49 (5)	O2—Si1—O3	107.2 (9)
O1—Yb1—K1^vi	59.78 (13)	O1^xv—Si1—K1^iv	74.44 (19)
O1^ii—Yb1—K1^vi	127.0 (2)	O1^xiv—Si1—K1^iv	74.44 (19)
O1^iii—Yb1—K1^vi	53.0 (2)	O2—Si1—K1^iv	66.7 (4)
O1^i—Yb1—K1^vi	120.22 (13)	O3—Si1—K1^iv	173.9 (7)
K2—Yb1—K1^vi	111.97 (5)	O1^xv—Si1—K1^vi	154.12 (19)
K2^i—Yb1—K1^vi	68.03 (5)	O1^xiv—Si1—K1^vi	59.5 (3)
K1^iv—Yb1—K1^vi	71.89 (5)	O2—Si1—K1^vi	58.81 (12)
K1^v—Yb1—K1^vi	108.11 (5)	O3—Si1—K1^vi	97.2 (4)
K1^i—Yb1—K1^vi	106.89 (9)	K1^iv—Si1—K1^vi	79.73 (5)
O1^vii—K1—O1	55.7 (2)	O1^xv—Si1—K1^i	59.5 (3)
O1^vii—K1—O2^vi	64.95 (15)	O1^xiv—Si1—K1^i	154.12 (19)
O1—K1—O2^vi	120.7 (3)	O2—Si1—K1^i	58.81 (11)
O1^vii—K1—O2^i	120.7 (3)	O3—Si1—K1^i	97.2 (4)
O1—K1—O2^i	64.95 (15)	K1^iv—Si1—K1^i	79.73 (5)
O2^vi—K1—O2^i	174.2 (4)	K1^vi—Si1—K1^i	117.5 (2)
O1^vii—K1—O1^viii	119.90 (2)	O1^xv—Si1—K1^xiv	57.7 (3)
O1—K1—O1^viii	173.9 (2)	O1^xiv—Si1—K1^xiv	57.7 (3)
O2^vi—K1—O1^viii	55.24 (15)	O2—Si1—K1^xiv	148.4 (4)
O2^i—K1—O1^viii	119.3 (3)	O3—Si1—K1^xiv	104.5 (7)
O1^vii—K1—O1^ix	173.9 (2)	K1^iv—Si1—K1^xiv	81.62 (9)
O1—K1—O1^ix	119.90 (2)	K1^vi—Si1—K1^xiv	117.13 (12)
O2^vi—K1—O1^ix	119.3 (3)	K1^i—Si1—K1^xiv	117.13 (12)
O2^i—K1—O1^ix	55.24 (15)	O1^xv—Si1—K2^i	124.6 (3)
O1^viii—K1—O1^ix	64.1 (2)	O1^xiv—Si1—K2^i	124.6 (3)
O1^vii—K1—O2^viii	118.2 (2)	O2—Si1—K2^i	49.0 (4)
O1—K1—O2^viii	118.2 (2)	O3—Si1—K2^i	58.2 (7)
O2^vi—K1—O2^viii	87.8 (2)	K1^iv—Si1—K2^i	115.72 (13)
O2^i—K1—O2^viii	87.8 (2)	K1^vi—Si1—K2^i	68.81 (12)
O1^viii—K1—O2^viii	67.23 (14)	K1^i—Si1—K2^i	68.81 (12)
O1^ix—K1—O2^viii	67.23 (14)	K1^xiv—Si1—K2^i	162.65 (9)
O1^vii—K1—O1^vi	65.60 (16)	O1^xv—Si1—K2^xiii	42.33 (19)
O1—K1—O1^vi	89.2 (2)	O1^xiv—Si1—K2^xiii	121.7 (4)
O2^vi—K1—O1^vi	64.6 (2)	O2—Si1—K2^xiii	126.60 (14)
O2^i—K1—O1^vi	115.3 (3)	O3—Si1—K2^xiii	66.5 (4)
O1^viii—K1—O1^vi	92.40 (16)	K1^iv—Si1—K2^xiii	116.76 (7)
O1^ix—K1—O1^vi	119.75 (11)	K1^vi—Si1—K2^xiii	163.48 (6)
O2^viii—K1—O1^vi	52.57 (14)	K1^i—Si1—K2^xiii	69.24 (8)
O1^vii—K1—O1^iii	89.2 (2)	K1^xiv—Si1—K2^xiii	67.36 (11)
O1—K1—O1^iii	65.60 (16)	K2^i—Si1—K2^xiii	102.41 (7)
O2^vi—K1—O1^iii	115.3 (3)	O1^xv—Si1—K2^xiv	121.7 (4)
O2^i—K1—O1^iii	64.6 (2)	O1^xiv—Si1—K2^xiv	42.33 (19)
O1^viii—K1—O1^iii	119.75 (11)	O2—Si1—K2^xiv	126.60 (14)
O1^ix—K1—O1^iii	92.40 (16)	O3—Si1—K2^xiv	66.5 (4)
O2^viii—K1—O1^iii	52.57 (14)	K1^iv—Si1—K2^xiv	116.76 (7)
O1^vi—K1—O1^iii	50.7 (3)	K1^vi—Si1—K2^xiv	69.24 (8)
O1^vii—K1—Si1^viii	91.13 (13)	K1^i—Si1—K2^xiv	163.48 (6)
O1—K1—Si1^viii	91.13 (13)	K1^xiv—Si1—K2^xiv	67.36 (11)
O2^vi—K1—Si1^viii	89.1 (2)	K2^i—Si1—K2^xiv	102.41 (7)
O2^i—K1—Si1^viii	89.1 (2)	K2^xiii—Si1—K2^xiv	100.35 (13)
O1^viii—K1—Si1^viii	93.24 (13)	Si1^xiv—O1—Yb1	157.4 (3)
O1^ix—K1—Si1^viii	93.24 (13)	Si1^xiv—O1—K2	114.4 (2)
O2^viii—K1—Si1^viii	31.0 (2)	Yb1—O1—K2	88.11 (17)
O1^vi—K1—Si1^viii	30.07 (11)	Si1^xiv—O1—K1	93.6 (4)
O1^iii—K1—Si1^viii	30.07 (11)	Yb1—O1—K1	88.3 (2)
O1^vii—K1—Si1^vi	91.58 (14)	K2—O1—K1	89.4 (2)
O1—K1—Si1^vi	145.74 (19)	Si1^xiv—O1—K1^iv	91.6 (3)
O2^vi—K1—Si1^vi	28.99 (19)	Yb1—O1—K1^iv	85.7 (3)
O2^i—K1—Si1^vi	146.4 (3)	K2—O1—K1^iv	91.2 (2)
O1^viii—K1—Si1^vi	28.87 (13)	K1—O1—K1^iv	173.9 (2)
O1^ix—K1—Si1^vi	91.81 (19)	Si1^xiv—O1—K1^vi	75.5 (2)
O2^viii—K1—Si1^vi	84.38 (13)	Yb1—O1—K1^vi	81.98 (15)
O1^vi—K1—Si1^vi	85.14 (16)	K2—O1—K1^vi	170.1 (2)
O1^iii—K1—Si1^vi	130.32 (11)	K1—O1—K1^vi	90.8 (2)
Si1^viii—K1—Si1^vi	100.27 (5)	K1^iv—O1—K1^vi	87.60 (16)
O1^vii—K1—Si1^i	145.74 (19)	Si1—O2—Yb1	168.0 (6)
O1—K1—Si1^i	91.58 (14)	Si1—O2—K2^i	105.4 (5)
O2^vi—K1—Si1^i	146.4 (3)	Yb1—O2—K2^i	86.6 (3)
O2^i—K1—Si1^i	28.99 (19)	Si1—O2—K1^vi	92.2 (2)
O1^viii—K1—Si1^i	91.81 (19)	Yb1—O2—K1^vi	88.2 (2)
O1^ix—K1—Si1^i	28.87 (13)	K2^i—O2—K1^vi	87.6 (2)
O2^viii—K1—Si1^i	84.38 (13)	Si1—O2—K1^i	92.2 (2)
O1^vi—K1—Si1^i	130.32 (11)	Yb1—O2—K1^i	88.2 (2)
O1^iii—K1—Si1^i	85.14 (16)	K2^i—O2—K1^i	87.6 (2)
Si1^viii—K1—Si1^i	100.27 (5)	K1^vi—O2—K1^i	174.2 (4)
Si1^vi—K1—Si1^i	117.5 (2)	Si1—O2—K1^iv	82.3 (4)
O1^x—K2—O1^xi	67.5 (3)	Yb1—O2—K1^iv	85.8 (3)
O1^x—K2—O1^ii	98.8 (2)	K2^i—O2—K1^iv	172.3 (4)
O1^xi—K2—O1^ii	140.4 (3)	K1^vi—O2—K1^iv	92.2 (2)
O1^x—K2—O1	140.4 (3)	K1^i—O2—K1^iv	92.2 (2)
O1^xi—K2—O1	98.8 (2)	Si1^xvi—O3—Si1	170.3 (13)
O1^ii—K2—O1	67.5 (3)	Si1^xvi—O3—K2^i	94.9 (7)
O1^x—K2—O2^i	143.98 (18)	Si1—O3—K2^i	94.9 (7)
O1^xi—K2—O2^i	143.98 (18)	Si1^xvi—O3—K2^xiii	87.3 (4)
O1^ii—K2—O2^i	66.59 (15)	Si1—O3—K2^xiii	87.3 (4)
O1—K2—O2^i	66.59 (15)	K2^i—O3—K2^xiii	123.2 (3)
O1^x—K2—O2^xii	66.59 (15)	Si1^xvi—O3—K2^xiv	87.3 (4)
O1^xi—K2—O2^xii	66.59 (15)	Si1—O3—K2^xiv	87.3 (4)
O1^ii—K2—O2^xii	143.98 (18)	K2^i—O3—K2^xiv	123.2 (3)
O1—K2—O2^xii	143.98 (18)	K2^xiii—O3—K2^xiv	113.6 (5)
O2^i—K2—O2^xii	105.2 (4)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, y, z; (iii) x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1, −y, −z+1; (vii) −x+1, y, z; (viii) x+1/2, y+1/2, z; (ix) −x+1/2, y+1/2, z; (x) −x, y, −z+1/2; (xi) x, y, −z+1/2; (xii) −x, −y, z−1/2; (xiii) −x−1/2, −y−1/2, −z+1; (xiv) −x+1/2, −y−1/2, −z+1; (xv) x−1/2, −y−1/2, −z+1; (xvi) x, y, −z+3/2.

(203_K)

Crystal data

K3O7Si2Yb	Dx = 3.857 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Cmcm	Cell parameters from 1177 reflections
a = 5.7202 (7) Å	θ = 7.1–29.2°
b = 9.9055 (11) Å	µ = 13.73 mm^−1
c = 13.9343 (15) Å	T = 203 K
V = 789.54 (15) Å^3	Prismatic, colourless
Z = 4	0.13 × 0.11 × 0.09 mm
F(000) = 844

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	442 reflections with I > 2σ(I)
ω scans	Rint = 0.038
Absorption correction: analytical CrysAlisPro 1.171.40.77a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −7→7
2693 measured reflections	k = −10→12
540 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0098P)^2 + 0.1039P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.017	(Δ/σ)max < 0.001
wR(F^2) = 0.037	Δρmax = 0.83 e Å^−3
S = 1.09	Δρmin = −0.78 e Å^−3
540 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
32 parameters	Extinction coefficient: 0.00309 (14)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 3-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Yb1	0.000000	0.000000	0.500000	0.00316 (14)
K1	0.500000	0.1686 (5)	0.40849 (10)	0.0088 (3)
K2	0.000000	0.0081 (6)	0.250000	0.0115 (5)
Si1	0.000000	−0.3350 (6)	0.63226 (12)	0.0034 (3)
O1	0.2682 (16)	−0.0848 (8)	0.4015 (5)	0.0090 (18)
O2	0.000000	−0.1831 (12)	0.5916 (10)	0.008 (3)
O3	0.000000	−0.329 (3)	0.750000	0.0187 (15)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Yb1	0.00279 (15)	0.00279 (15)	0.00389 (19)	0.000	0.000	0.000
K1	0.0075 (4)	0.0075 (4)	0.0114 (6)	0.000	0.000	0.000
K2	0.0142 (7)	0.0142 (7)	0.0063 (8)	0.000	0.000	0.000
Si1	0.0039 (5)	0.0039 (5)	0.0025 (6)	0.000	0.000	0.000
O1	0.007 (6)	0.004 (5)	0.016 (4)	0.000	0.000	0.000
O2	0.013 (7)	0.006 (6)	0.005 (7)	0.000	0.000	0.000
O3	0.026 (14)	0.023 (13)	0.007 (3)	0.000	0.000	0.000

Geometric parameters (Å, º)

Yb1—O2	2.218 (13)	K1—O1^vii	3.076 (8)
Yb1—O2^i	2.218 (13)	K1—O1^iii	3.076 (8)
Yb1—O1	2.224 (7)	K1—Si1^viii	3.118 (2)
Yb1—O1^ii	2.224 (7)	K1—Si1^vii	3.349 (5)
Yb1—O1^iii	2.224 (7)	K1—Si1^i	3.349 (5)
Yb1—O1^i	2.224 (7)	K2—O1	2.767 (8)
Yb1—K2	3.4845 (4)	K2—O1^x	2.767 (8)
Yb1—K2^i	3.4845 (4)	K2—O1^xi	2.767 (8)
Yb1—K1^iv	3.521 (5)	K2—O1^ii	2.767 (8)
Yb1—K1^v	3.521 (5)	K2—O2^i	2.806 (16)
Yb1—K1	3.549 (3)	K2—O2^xii	2.806 (16)
Yb1—K1^i	3.549 (3)	K2—O3^i	3.17 (3)
K1—O1	2.840 (12)	K2—O3^xiii	3.368 (15)
K1—O1^vi	2.840 (12)	K2—O3^xiv	3.368 (15)
K1—O2^vii	2.8637 (8)	K2—Si1^i	3.630 (8)
K1—O2^i	2.8637 (8)	Si1—O2	1.608 (14)
K1—O1^viii	2.886 (12)	Si1—O1^xv	1.616 (7)
K1—O1^ix	2.886 (12)	Si1—O1^xiv	1.616 (7)
K1—O2^viii	2.944 (14)	Si1—O3	1.642 (2)
O2—Yb1—O2^i	180.0	O1—K2—O3^i	109.4 (2)
O2—Yb1—O1	92.7 (3)	O1^x—K2—O3^i	109.4 (2)
O2^i—Yb1—O1	87.3 (3)	O1^xi—K2—O3^i	109.4 (2)
O2—Yb1—O1^ii	92.7 (3)	O1^ii—K2—O3^i	109.4 (2)
O2^i—Yb1—O1^ii	87.3 (3)	O2^i—K2—O3^i	51.9 (3)
O1—Yb1—O1^ii	87.3 (5)	O2^xii—K2—O3^i	51.9 (3)
O2—Yb1—O1^iii	87.3 (3)	O1—K2—O3^xiii	107.2 (4)
O2^i—Yb1—O1^iii	92.7 (3)	O1^x—K2—O3^xiii	49.72 (14)
O1—Yb1—O1^iii	92.7 (5)	O1^xi—K2—O3^xiii	107.2 (4)
O1^ii—Yb1—O1^iii	180.0	O1^ii—K2—O3^xiii	49.72 (14)
O2—Yb1—O1^i	87.3 (3)	O2^i—K2—O3^xiii	109.0 (2)
O2^i—Yb1—O1^i	92.7 (3)	O2^xii—K2—O3^xiii	109.0 (2)
O1—Yb1—O1^i	180.0	O3^i—K2—O3^xiii	121.9 (4)
O1^ii—Yb1—O1^i	92.7 (5)	O1—K2—O3^xiv	49.72 (14)
O1^iii—Yb1—O1^i	87.3 (5)	O1^x—K2—O3^xiv	107.2 (4)
O2—Yb1—K2	126.5 (4)	O1^xi—K2—O3^xiv	49.72 (14)
O2^i—Yb1—K2	53.5 (4)	O1^ii—K2—O3^xiv	107.2 (4)
O1—Yb1—K2	52.5 (2)	O2^i—K2—O3^xiv	109.0 (2)
O1^ii—Yb1—K2	52.5 (2)	O2^xii—K2—O3^xiv	109.0 (2)
O1^iii—Yb1—K2	127.5 (2)	O3^i—K2—O3^xiv	121.9 (4)
O1^i—Yb1—K2	127.5 (2)	O3^xiii—K2—O3^xiv	116.3 (8)
O2—Yb1—K2^i	53.5 (4)	O1—K2—Yb1^xii	139.02 (17)
O2^i—Yb1—K2^i	126.5 (4)	O1^x—K2—Yb1^xii	39.62 (14)
O1—Yb1—K2^i	127.5 (2)	O1^xi—K2—Yb1^xii	39.62 (14)
O1^ii—Yb1—K2^i	127.5 (2)	O1^ii—K2—Yb1^xii	139.02 (17)
O1^iii—Yb1—K2^i	52.5 (2)	O2^i—K2—Yb1^xii	143.2 (3)
O1^i—Yb1—K2^i	52.5 (2)	O2^xii—K2—Yb1^xii	39.5 (3)
K2—Yb1—K2^i	180.0 (2)	O3^i—K2—Yb1^xii	91.32 (10)
O2—Yb1—K1^iv	56.4 (4)	O3^xiii—K2—Yb1^xii	89.30 (6)
O2^i—Yb1—K1^iv	123.6 (4)	O3^xiv—K2—Yb1^xii	89.30 (6)
O1—Yb1—K1^iv	54.9 (3)	O1—K2—Yb1	39.62 (14)
O1^ii—Yb1—K1^iv	54.9 (3)	O1^x—K2—Yb1	139.02 (17)
O1^iii—Yb1—K1^iv	125.1 (3)	O1^xi—K2—Yb1	139.02 (17)
O1^i—Yb1—K1^iv	125.1 (3)	O1^ii—K2—Yb1	39.62 (14)
K2—Yb1—K1^iv	70.09 (11)	O2^i—K2—Yb1	39.5 (3)
K2^i—Yb1—K1^iv	109.91 (11)	O2^xii—K2—Yb1	143.2 (3)
O2—Yb1—K1^v	123.6 (4)	O3^i—K2—Yb1	91.32 (10)
O2^i—Yb1—K1^v	56.4 (4)	O3^xiii—K2—Yb1	89.30 (6)
O1—Yb1—K1^v	125.1 (3)	O3^xiv—K2—Yb1	89.30 (6)
O1^ii—Yb1—K1^v	125.1 (3)	Yb1^xii—K2—Yb1	177.4 (2)
O1^iii—Yb1—K1^v	54.9 (3)	O1—K2—Si1^i	87.24 (19)
O1^i—Yb1—K1^v	54.9 (3)	O1^x—K2—Si1^i	129.9 (3)
K2—Yb1—K1^v	109.91 (11)	O1^xi—K2—Si1^i	129.9 (3)
K2^i—Yb1—K1^v	70.09 (11)	O1^ii—K2—Si1^i	87.24 (19)
K1^iv—Yb1—K1^v	180.00 (4)	O2^i—K2—Si1^i	25.0 (3)
O2—Yb1—K1	126.27 (6)	O2^xii—K2—Si1^i	78.7 (3)
O2^i—Yb1—K1	53.73 (6)	O3^i—K2—Si1^i	26.87 (7)
O1—Yb1—K1	53.1 (3)	O3^xiii—K2—Si1^i	118.1 (3)
O1^ii—Yb1—K1	120.79 (18)	O3^xiv—K2—Si1^i	118.1 (3)
O1^iii—Yb1—K1	59.21 (18)	Yb1^xii—K2—Si1^i	118.19 (16)
O1^i—Yb1—K1	126.9 (3)	Yb1—K2—Si1^i	64.45 (7)
K2—Yb1—K1	68.28 (6)	O2—Si1—O1^xv	111.0 (4)
K2^i—Yb1—K1	111.72 (6)	O2—Si1—O1^xiv	111.0 (4)
K1^iv—Yb1—K1	107.97 (6)	O1^xv—Si1—O1^xiv	110.3 (8)
K1^v—Yb1—K1	72.03 (6)	O2—Si1—O3	108.4 (12)
O2—Yb1—K1^i	53.73 (6)	O1^xv—Si1—O3	108.0 (6)
O2^i—Yb1—K1^i	126.27 (6)	O1^xiv—Si1—O3	108.0 (6)
O1—Yb1—K1^i	126.9 (3)	O2—Si1—K1^iv	68.7 (5)
O1^ii—Yb1—K1^i	59.21 (18)	O1^xv—Si1—K1^iv	73.4 (3)
O1^iii—Yb1—K1^i	120.79 (18)	O1^xiv—Si1—K1^iv	73.4 (3)
O1^i—Yb1—K1^i	53.1 (3)	O3—Si1—K1^iv	177.1 (10)
K2—Yb1—K1^i	111.72 (6)	O2—Si1—K1^vii	58.65 (14)
K2^i—Yb1—K1^i	68.28 (6)	O1^xv—Si1—K1^vii	153.3 (3)
K1^iv—Yb1—K1^i	72.03 (6)	O1^xiv—Si1—K1^vii	59.5 (4)
K1^v—Yb1—K1^i	107.97 (6)	O3—Si1—K1^vii	98.7 (5)
K1—Yb1—K1^i	180.00 (15)	K1^iv—Si1—K1^vii	79.91 (6)
O1—K1—O1^vi	55.7 (3)	O2—Si1—K1^i	58.65 (14)
O1—K1—O2^vii	120.7 (4)	O1^xv—Si1—K1^i	59.5 (4)
O1^vi—K1—O2^vii	65.04 (17)	O1^xiv—Si1—K1^i	153.3 (3)
O1—K1—O2^i	65.04 (17)	O3—Si1—K1^i	98.7 (5)
O1^vi—K1—O2^i	120.7 (4)	K1^iv—Si1—K1^i	79.91 (6)
O2^vii—K1—O2^i	174.3 (5)	K1^vii—Si1—K1^i	117.3 (3)
O1—K1—O1^viii	174.2 (3)	O2—Si1—K1^xiv	149.6 (5)
O1^vi—K1—O1^viii	119.91 (3)	O1^xv—Si1—K1^xiv	57.7 (4)
O2^vii—K1—O1^viii	55.02 (17)	O1^xiv—Si1—K1^xiv	57.7 (4)
O2^i—K1—O1^viii	119.2 (4)	O3—Si1—K1^xiv	102.0 (9)
O1—K1—O1^ix	119.91 (3)	K1^iv—Si1—K1^xiv	80.91 (12)
O1^vi—K1—O1^ix	174.2 (3)	K1^vii—Si1—K1^xiv	117.14 (14)
O2^vii—K1—O1^ix	119.2 (4)	K1^i—Si1—K1^xiv	117.14 (14)
O2^i—K1—O1^ix	55.02 (17)	O2—Si1—K2^i	47.5 (5)
O1^viii—K1—O1^ix	64.2 (3)	O1^xv—Si1—K2^i	124.8 (4)
O1—K1—O2^viii	118.1 (3)	O1^xiv—Si1—K2^i	124.8 (4)
O1^vi—K1—O2^viii	118.1 (3)	O3—Si1—K2^i	60.9 (9)
O2^vii—K1—O2^viii	88.6 (3)	K1^iv—Si1—K2^i	116.21 (16)
O2^i—K1—O2^viii	88.6 (3)	K1^vii—Si1—K2^i	68.76 (15)
O1^viii—K1—O2^viii	66.87 (18)	K1^i—Si1—K2^i	68.76 (15)
O1^ix—K1—O2^viii	66.87 (18)	K1^xiv—Si1—K2^i	162.88 (10)
O1—K1—O1^vii	89.6 (3)	O2—Si1—K2^xiii	125.97 (19)
O1^vi—K1—O1^vii	65.8 (2)	O1^xv—Si1—K2^xiii	43.1 (3)
O2^vii—K1—O1^vii	65.4 (3)	O1^xiv—Si1—K2^xiii	122.2 (5)
O2^i—K1—O1^vii	116.4 (4)	O3—Si1—K2^xiii	65.0 (5)
O1^viii—K1—O1^vii	91.6 (2)	K1^iv—Si1—K2^xiii	116.53 (8)
O1^ix—K1—O1^vii	119.14 (15)	K1^vii—Si1—K2^xiii	163.54 (6)
O2^viii—K1—O1^vii	52.31 (19)	K1^i—Si1—K2^xiii	69.19 (10)
O1—K1—O1^iii	65.8 (2)	K1^xiv—Si1—K2^xiii	67.67 (14)
O1^vi—K1—O1^iii	89.6 (3)	K2^i—Si1—K2^xiii	102.24 (8)
O2^vii—K1—O1^iii	116.4 (4)	O2—Si1—K2^xiv	125.97 (19)
O2^i—K1—O1^iii	65.4 (3)	O1^xv—Si1—K2^xiv	122.2 (5)
O1^viii—K1—O1^iii	119.14 (15)	O1^xiv—Si1—K2^xiv	43.1 (3)
O1^ix—K1—O1^iii	91.6 (2)	O3—Si1—K2^xiv	65.0 (5)
O2^viii—K1—O1^iii	52.31 (19)	K1^iv—Si1—K2^xiv	116.53 (8)
O1^vii—K1—O1^iii	51.1 (4)	K1^vii—Si1—K2^xiv	69.19 (10)
O1—K1—Si1^viii	91.39 (17)	K1^i—Si1—K2^xiv	163.54 (6)
O1^vi—K1—Si1^viii	91.39 (17)	K1^xiv—Si1—K2^xiv	67.67 (14)
O2^vii—K1—Si1^viii	90.1 (3)	K2^i—Si1—K2^xiv	102.24 (8)
O2^i—K1—Si1^viii	90.1 (3)	K2^xiii—Si1—K2^xiv	100.63 (16)
O1^viii—K1—Si1^viii	92.50 (19)	Si1^xiv—O1—Yb1	158.7 (4)
O1^ix—K1—Si1^viii	92.50 (19)	Si1^xiv—O1—K2	113.4 (4)
O2^viii—K1—Si1^viii	30.6 (3)	Yb1—O1—K2	87.9 (2)
O1^vii—K1—Si1^viii	30.23 (14)	Si1^xiv—O1—K1	93.5 (5)
O1^iii—K1—Si1^viii	30.23 (14)	Yb1—O1—K1	88.1 (3)
O1—K1—Si1^vii	145.9 (2)	K2—O1—K1	89.5 (3)
O1^vi—K1—Si1^vii	91.74 (17)	Si1^xiv—O1—K1^iv	91.7 (4)
O2^vii—K1—Si1^vii	28.7 (3)	Yb1—O1—K1^iv	86.1 (3)
O2^i—K1—Si1^vii	145.9 (3)	K2—O1—K1^iv	90.7 (3)
O1^viii—K1—Si1^vii	28.83 (16)	K1—O1—K1^iv	174.2 (3)
O1^ix—K1—Si1^vii	91.8 (2)	Si1^xiv—O1—K1^vii	76.3 (2)
O2^viii—K1—Si1^vii	84.35 (17)	Yb1—O1—K1^vii	82.4 (2)
O1^vii—K1—Si1^vii	84.9 (2)	K2—O1—K1^vii	170.3 (3)
O1^iii—K1—Si1^vii	130.31 (14)	K1—O1—K1^vii	90.4 (3)
Si1^viii—K1—Si1^vii	100.09 (6)	K1^iv—O1—K1^vii	88.4 (2)
O1—K1—Si1^i	91.74 (17)	Si1—O2—Yb1	165.5 (9)
O1^vi—K1—Si1^i	145.8 (2)	Si1—O2—K2^i	107.5 (7)
O2^vii—K1—Si1^i	145.9 (3)	Yb1—O2—K2^i	87.0 (4)
O2^i—K1—Si1^i	28.7 (3)	Si1—O2—K1^vii	92.7 (3)
O1^viii—K1—Si1^i	91.8 (2)	Yb1—O2—K1^vii	87.6 (3)
O1^ix—K1—Si1^i	28.83 (16)	K2^i—O2—K1^vii	88.3 (3)
O2^viii—K1—Si1^i	84.35 (17)	Si1—O2—K1^i	92.7 (3)
O1^vii—K1—Si1^i	130.31 (14)	Yb1—O2—K1^i	87.6 (3)
O1^iii—K1—Si1^i	84.9 (2)	K2^i—O2—K1^i	88.3 (3)
Si1^viii—K1—Si1^i	100.09 (6)	K1^vii—O2—K1^i	174.3 (5)
Si1^vii—K1—Si1^i	117.3 (3)	Si1—O2—K1^iv	80.7 (5)
O1—K2—O1^x	141.2 (5)	Yb1—O2—K1^iv	84.8 (4)
O1—K2—O1^xi	99.4 (3)	K2^i—O2—K1^iv	171.8 (5)
O1^x—K2—O1^xi	67.4 (4)	K1^vii—O2—K1^iv	91.4 (3)
O1—K2—O1^ii	67.4 (4)	K1^i—O2—K1^iv	91.4 (3)
O1^x—K2—O1^ii	99.4 (3)	Si1^xvi—O3—Si1	175.6 (19)
O1^xi—K2—O1^ii	141.2 (5)	Si1^xvi—O3—K2^i	92.2 (9)
O1—K2—O2^i	66.8 (2)	Si1—O3—K2^i	92.2 (9)
O1^x—K2—O2^i	143.6 (2)	Si1^xvi—O3—K2^xiii	88.8 (5)
O1^xi—K2—O2^i	143.6 (2)	Si1—O3—K2^xiii	88.8 (5)
O1^ii—K2—O2^i	66.8 (2)	K2^i—O3—K2^xiii	121.9 (4)
O1—K2—O2^xii	143.6 (2)	Si1^xvi—O3—K2^xiv	88.8 (5)
O1^x—K2—O2^xii	66.8 (2)	Si1—O3—K2^xiv	88.8 (5)
O1^xi—K2—O2^xii	66.8 (2)	K2^i—O3—K2^xiv	121.9 (4)
O1^ii—K2—O2^xii	143.6 (2)	K2^xiii—O3—K2^xiv	116.3 (8)
O2^i—K2—O2^xii	103.7 (6)

Symmetry codes: (i) −x, −y, −z+1; (ii) −x, y, z; (iii) x, −y, −z+1; (iv) x−1/2, y−1/2, z; (v) −x+1/2, −y+1/2, −z+1; (vi) −x+1, y, z; (vii) −x+1, −y, −z+1; (viii) x+1/2, y+1/2, z; (ix) −x+1/2, y+1/2, z; (x) −x, y, −z+1/2; (xi) x, y, −z+1/2; (xii) −x, −y, z−1/2; (xiii) −x−1/2, −y−1/2, −z+1; (xiv) −x+1/2, −y−1/2, −z+1; (xv) x−1/2, −y−1/2, −z+1; (xvi) x, y, −z+3/2.

(213_K)

Crystal data

K3O7Si2Yb	Dx = 3.864 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1167 reflections
a = 5.7173 (5) Å	θ = 7.1–29.4°
c = 13.9228 (12) Å	µ = 13.75 mm^−1
V = 394.13 (8) Å^3	T = 213 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	189 reflections with I > 2σ(I)
ω scans	Rint = 0.045
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.305, Tmax = 0.398	h = −7→7
2483 measured reflections	k = −7→6
209 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0064P)^2 + 1.3339P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.015	(Δ/σ)max < 0.001
wR(F^2) = 0.035	Δρmax = 0.50 e Å^−3
S = 1.20	Δρmin = −0.52 e Å^−3
209 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0138 (8)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09125 (13)	0.0094 (4)
K2	0.000000	0.000000	0.250000	0.0125 (5)
Yb1	0.000000	0.000000	0.000000	0.0033 (2)
Si1	0.666667	0.333333	0.13235 (15)	0.0030 (4)
O1	0.3564 (7)	0.1782 (3)	0.0959 (2)	0.0093 (7)
O2	0.666667	0.333333	0.250000	0.019 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0086 (5)	0.0086 (5)	0.0109 (8)	0.0043 (3)	0.000	0.000
K2	0.0160 (8)	0.0160 (8)	0.0053 (11)	0.0080 (4)	0.000	0.000
Yb1	0.0030 (2)	0.0030 (2)	0.0037 (3)	0.00152 (11)	0.000	0.000
Si1	0.0032 (6)	0.0032 (6)	0.0026 (9)	0.0016 (3)	0.000	0.000
O1	0.0070 (16)	0.0091 (12)	0.0110 (15)	0.0035 (8)	−0.0037 (15)	−0.0018 (7)
O2	0.026 (3)	0.026 (3)	0.005 (4)	0.0129 (16)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8616 (3)	K2—O1^xiii	2.778 (3)
K1—O1^ii	2.8616 (3)	K2—O2^xiv	3.3009 (3)
K1—O1^iii	2.8616 (3)	K2—O2	3.3009 (3)
K1—O1^iv	2.8616 (3)	K2—O2^ix	3.3009 (3)
K1—O1	2.8616 (3)	K2—Yb1	3.4807 (3)
K1—O1^v	2.8616 (3)	K2—Yb1^xv	3.4807 (3)
K1—O1^vi	3.025 (3)	K2—Si1	3.6850 (10)
K1—O1^vii	3.025 (3)	Yb1—O1	2.213 (3)
K1—O1^viii	3.025 (3)	Yb1—O1^xvi	2.213 (3)
K1—Si1^viii	3.113 (3)	Yb1—O1^xvii	2.213 (3)
K1—Si1^ii	3.3501 (5)	Yb1—O1^iv	2.213 (3)
K1—Si1^ix	3.3501 (5)	Yb1—O1^vii	2.213 (3)
K2—O1	2.778 (3)	Yb1—O1^x	2.213 (3)
K2—O1^x	2.778 (3)	Si1—O1^xviii	1.618 (3)
K2—O1^xi	2.778 (3)	Si1—O1^v	1.618 (3)
K2—O1^xii	2.778 (3)	Si1—O1	1.618 (3)
K2—O1^iv	2.778 (3)	Si1—O2	1.638 (2)
O1^i—K1—O1^ii	64.55 (13)	O1^xvi—Yb1—O1^vii	87.36 (12)
O1^i—K1—O1^iii	119.950 (6)	O1^xvii—Yb1—O1^vii	87.36 (12)
O1^ii—K1—O1^iii	55.42 (13)	O1^iv—Yb1—O1^vii	92.64 (12)
O1^i—K1—O1^iv	55.42 (13)	O1—Yb1—O1^x	87.36 (12)
O1^ii—K1—O1^iv	119.950 (6)	O1^xvi—Yb1—O1^x	92.64 (12)
O1^iii—K1—O1^iv	174.75 (13)	O1^xvii—Yb1—O1^x	92.64 (12)
O1^i—K1—O1	119.949 (6)	O1^iv—Yb1—O1^x	87.36 (12)
O1^ii—K1—O1	174.75 (13)	O1^vii—Yb1—O1^x	180.00 (19)
O1^iii—K1—O1	119.950 (6)	O1—Yb1—K2	52.89 (8)
O1^iv—K1—O1	64.55 (13)	O1^xvi—Yb1—K2	127.11 (8)
O1^i—K1—O1^v	174.75 (13)	O1^xvii—Yb1—K2	127.11 (8)
O1^ii—K1—O1^v	119.950 (6)	O1^iv—Yb1—K2	52.89 (8)
O1^iii—K1—O1^v	64.55 (13)	O1^vii—Yb1—K2	127.11 (8)
O1^iv—K1—O1^v	119.950 (6)	O1^x—Yb1—K2	52.89 (8)
O1—K1—O1^v	55.42 (13)	O1—Yb1—K2^xvi	127.11 (8)
O1^i—K1—O1^vi	65.80 (10)	O1^xvi—Yb1—K2^xvi	52.89 (8)
O1^ii—K1—O1^vi	65.80 (10)	O1^xvii—Yb1—K2^xvi	52.89 (8)
O1^iii—K1—O1^vi	89.95 (7)	O1^iv—Yb1—K2^xvi	127.11 (8)
O1^iv—K1—O1^vi	89.95 (7)	O1^vii—Yb1—K2^xvi	52.89 (8)
O1—K1—O1^vi	117.97 (7)	O1^x—Yb1—K2^xvi	127.11 (8)
O1^v—K1—O1^vi	117.97 (7)	K2—Yb1—K2^xvi	180.0
O1^i—K1—O1^vii	89.95 (7)	O1—Yb1—K1^xvi	126.076 (14)
O1^ii—K1—O1^vii	117.97 (7)	O1^xvi—Yb1—K1^xvi	53.924 (14)
O1^iii—K1—O1^vii	117.97 (7)	O1^xvii—Yb1—K1^xvi	53.925 (14)
O1^iv—K1—O1^vii	65.80 (10)	O1^iv—Yb1—K1^xvi	126.075 (14)
O1—K1—O1^vii	65.80 (10)	O1^vii—Yb1—K1^xvi	121.84 (8)
O1^v—K1—O1^vii	89.95 (7)	O1^x—Yb1—K1^xvi	58.16 (8)
O1^vi—K1—O1^vii	52.20 (10)	K2—Yb1—K1^xvi	111.05 (3)
O1^i—K1—O1^viii	117.97 (7)	K2^xvi—Yb1—K1^xvi	68.95 (3)
O1^ii—K1—O1^viii	89.95 (7)	O1—Yb1—K1^viii	58.16 (8)
O1^iii—K1—O1^viii	65.80 (11)	O1^xvi—Yb1—K1^viii	121.84 (8)
O1^iv—K1—O1^viii	117.97 (7)	O1^xvii—Yb1—K1^viii	53.925 (14)
O1—K1—O1^viii	89.95 (7)	O1^iv—Yb1—K1^viii	126.075 (14)
O1^v—K1—O1^viii	65.80 (10)	O1^vii—Yb1—K1^viii	53.924 (14)
O1^vi—K1—O1^viii	52.20 (10)	O1^x—Yb1—K1^viii	126.075 (15)
O1^vii—K1—O1^viii	52.20 (10)	K2—Yb1—K1^viii	111.05 (3)
O1^i—K1—Si1^viii	91.29 (7)	K2^xvi—Yb1—K1^viii	68.95 (3)
O1^ii—K1—Si1^viii	91.29 (7)	K1^xvi—Yb1—K1^viii	107.85 (3)
O1^iii—K1—Si1^viii	91.29 (7)	O1—Yb1—K1^xiv	121.84 (8)
O1^iv—K1—Si1^viii	91.29 (7)	O1^xvi—Yb1—K1^xiv	58.16 (8)
O1—K1—Si1^viii	91.29 (7)	O1^xvii—Yb1—K1^xiv	126.075 (14)
O1^v—K1—Si1^viii	91.29 (7)	O1^iv—Yb1—K1^xiv	53.925 (14)
O1^vi—K1—Si1^viii	30.53 (6)	O1^vii—Yb1—K1^xiv	126.075 (15)
O1^vii—K1—Si1^viii	30.53 (6)	O1^x—Yb1—K1^xiv	53.924 (14)
O1^viii—K1—Si1^viii	30.53 (6)	K2—Yb1—K1^xiv	68.95 (3)
O1^i—K1—Si1^ii	92.03 (7)	K2^xvi—Yb1—K1^xiv	111.05 (3)
O1^ii—K1—Si1^ii	28.85 (7)	K1^xvi—Yb1—K1^xiv	72.15 (3)
O1^iii—K1—Si1^ii	28.85 (7)	K1^viii—Yb1—K1^xiv	180.0
O1^iv—K1—Si1^ii	145.99 (7)	O1—Yb1—K1	53.924 (14)
O1—K1—Si1^ii	145.99 (7)	O1^xvi—Yb1—K1	126.076 (14)
O1^v—K1—Si1^ii	92.03 (7)	O1^xvii—Yb1—K1	126.075 (14)
O1^vi—K1—Si1^ii	84.08 (5)	O1^iv—Yb1—K1	53.925 (14)
O1^vii—K1—Si1^ii	130.36 (8)	O1^vii—Yb1—K1	58.16 (8)
O1^viii—K1—Si1^ii	84.08 (5)	O1^x—Yb1—K1	121.84 (8)
Si1^viii—K1—Si1^ii	99.83 (4)	K2—Yb1—K1	68.95 (3)
O1^i—K1—Si1^ix	28.85 (6)	K2^xvi—Yb1—K1	111.05 (3)
O1^ii—K1—Si1^ix	92.03 (7)	K1^xvi—Yb1—K1	180.0
O1^iii—K1—Si1^ix	145.99 (7)	K1^viii—Yb1—K1	72.15 (3)
O1^iv—K1—Si1^ix	28.85 (6)	K1^xiv—Yb1—K1	107.85 (3)
O1—K1—Si1^ix	92.03 (7)	O1^xviii—Si1—O1^v	110.63 (13)
O1^v—K1—Si1^ix	145.99 (7)	O1^xviii—Si1—O1	110.63 (13)
O1^vi—K1—Si1^ix	84.08 (5)	O1^v—Si1—O1	110.63 (13)
O1^vii—K1—Si1^ix	84.08 (5)	O1^xviii—Si1—O2	108.28 (14)
O1^viii—K1—Si1^ix	130.36 (8)	O1^v—Si1—O2	108.28 (14)
Si1^viii—K1—Si1^ix	99.83 (4)	O1—Si1—O2	108.28 (14)
Si1^ii—K1—Si1^ix	117.14 (3)	O1^xviii—Si1—K1^viii	71.72 (14)
O1—K2—O1^x	66.74 (10)	O1^v—Si1—K1^viii	71.71 (14)
O1—K2—O1^xi	101.14 (13)	O1—Si1—K1^viii	71.72 (14)
O1^x—K2—O1^xi	142.97 (5)	O2—Si1—K1^viii	180.0
O1—K2—O1^xii	142.97 (5)	O1^xviii—Si1—K1	151.88 (16)
O1^x—K2—O1^xii	142.97 (5)	O1^v—Si1—K1	58.576 (12)
O1^xi—K2—O1^xii	66.74 (10)	O1—Si1—K1	58.576 (12)
O1—K2—O1^iv	66.74 (10)	O2—Si1—K1	99.83 (4)
O1^x—K2—O1^iv	66.74 (10)	K1^viii—Si1—K1	80.16 (4)
O1^xi—K2—O1^iv	142.97 (5)	O1^xviii—Si1—K1^xix	58.576 (12)
O1^xii—K2—O1^iv	101.14 (13)	O1^v—Si1—K1^xix	151.88 (16)
O1—K2—O1^xiii	142.97 (5)	O1—Si1—K1^xix	58.576 (12)
O1^x—K2—O1^xiii	101.14 (13)	O2—Si1—K1^xix	99.84 (4)
O1^xi—K2—O1^xiii	66.74 (10)	K1^viii—Si1—K1^xix	80.16 (4)
O1^xii—K2—O1^xiii	66.74 (10)	K1—Si1—K1^xix	117.14 (3)
O1^iv—K2—O1^xiii	142.97 (5)	O1^xviii—Si1—K1^xx	58.576 (12)
O1—K2—O2^xiv	108.52 (3)	O1^v—Si1—K1^xx	58.576 (12)
O1^x—K2—O2^xiv	50.57 (6)	O1—Si1—K1^xx	151.88 (16)
O1^xi—K2—O2^xiv	108.52 (3)	O2—Si1—K1^xx	99.84 (4)
O1^xii—K2—O2^xiv	108.52 (3)	K1^viii—Si1—K1^xx	80.16 (4)
O1^iv—K2—O2^xiv	108.52 (3)	K1—Si1—K1^xx	117.14 (3)
O1^xiii—K2—O2^xiv	50.57 (6)	K1^xix—Si1—K1^xx	117.14 (3)
O1—K2—O2	50.57 (6)	O1^xviii—Si1—K2^xx	44.68 (12)
O1^x—K2—O2	108.52 (3)	O1^v—Si1—K2^xx	124.38 (5)
O1^xi—K2—O2	50.57 (6)	O1—Si1—K2^xx	124.38 (5)
O1^xii—K2—O2	108.52 (3)	O2—Si1—K2^xx	63.61 (3)
O1^iv—K2—O2	108.52 (3)	K1^viii—Si1—K2^xx	116.39 (3)
O1^xiii—K2—O2	108.52 (3)	K1—Si1—K2^xx	163.44 (7)
O2^xiv—K2—O2	120.0	K1^xix—Si1—K2^xx	68.569 (18)
O1—K2—O2^ix	108.52 (3)	K1^xx—Si1—K2^xx	68.569 (18)
O1^x—K2—O2^ix	108.52 (3)	O1^xviii—Si1—K2^xxi	124.38 (5)
O1^xi—K2—O2^ix	108.52 (3)	O1^v—Si1—K2^xxi	44.68 (12)
O1^xii—K2—O2^ix	50.57 (6)	O1—Si1—K2^xxi	124.38 (5)
O1^iv—K2—O2^ix	50.57 (6)	O2—Si1—K2^xxi	63.61 (3)
O1^xiii—K2—O2^ix	108.52 (3)	K1^viii—Si1—K2^xxi	116.39 (3)
O2^xiv—K2—O2^ix	120.0	K1—Si1—K2^xxi	68.569 (18)
O2—K2—O2^ix	120.0	K1^xix—Si1—K2^xxi	163.44 (7)
O1—K2—Yb1	39.43 (6)	K1^xx—Si1—K2^xxi	68.570 (18)
O1^x—K2—Yb1	39.43 (6)	K2^xx—Si1—K2^xxi	101.75 (4)
O1^xi—K2—Yb1	140.57 (7)	O1^xviii—Si1—K2	124.38 (4)
O1^xii—K2—Yb1	140.57 (6)	O1^v—Si1—K2	124.38 (5)
O1^iv—K2—Yb1	39.43 (6)	O1—Si1—K2	44.68 (12)
O1^xiii—K2—Yb1	140.57 (6)	O2—Si1—K2	63.61 (3)
O2^xiv—K2—Yb1	90.0	K1^viii—Si1—K2	116.39 (3)
O2—K2—Yb1	90.0	K1—Si1—K2	68.569 (18)
O2^ix—K2—Yb1	90.0	K1^xix—Si1—K2	68.570 (18)
O1—K2—Yb1^xv	140.57 (6)	K1^xx—Si1—K2	163.44 (7)
O1^x—K2—Yb1^xv	140.57 (6)	K2^xx—Si1—K2	101.75 (4)
O1^xi—K2—Yb1^xv	39.43 (7)	K2^xxi—Si1—K2	101.75 (4)
O1^xii—K2—Yb1^xv	39.43 (6)	Si1—O1—Yb1	161.2 (2)
O1^iv—K2—Yb1^xv	140.57 (6)	Si1—O1—K2	111.15 (16)
O1^xiii—K2—Yb1^xv	39.43 (7)	Yb1—O1—K2	87.68 (11)
O2^xiv—K2—Yb1^xv	90.0	Si1—O1—K1	92.57 (7)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.40 (7)
O2^ix—K2—Yb1^xv	90.0	K2—O1—K1	89.55 (7)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.57 (7)
O1—K2—Si1	24.18 (7)	Yb1—O1—K1^xix	87.40 (7)
O1^x—K2—Si1	86.63 (5)	K2—O1—K1^xix	89.55 (7)
O1^xi—K2—Si1	76.96 (7)	K1—O1—K1^xix	174.75 (13)
O1^xii—K2—Si1	128.89 (2)	Si1—O1—K1^viii	77.76 (15)
O1^iv—K2—Si1	86.63 (5)	Yb1—O1—K1^viii	83.42 (9)
O1^xiii—K2—Si1	128.89 (2)	K2—O1—K1^viii	171.10 (12)
O2^xiv—K2—Si1	116.609 (7)	K1—O1—K1^viii	90.05 (7)
O2—K2—Si1	26.39 (3)	K1^xix—O1—K1^viii	90.05 (7)
O2^ix—K2—Si1	116.608 (7)	Si1—O2—Si1^xi	180.0
Yb1—K2—Si1	63.61 (3)	Si1—O2—K2^xx	90.0
Yb1^xv—K2—Si1	116.39 (3)	Si1^xi—O2—K2^xx	90.0
O1—Yb1—O1^xvi	180.0	Si1—O2—K2	90.0
O1—Yb1—O1^xvii	92.64 (12)	Si1^xi—O2—K2	90.0
O1^xvi—Yb1—O1^xvii	87.36 (12)	K2^xx—O2—K2	120.0
O1—Yb1—O1^iv	87.36 (12)	Si1—O2—K2^xxi	90.0
O1^xvi—Yb1—O1^iv	92.64 (12)	Si1^xi—O2—K2^xxi	90.0
O1^xvii—Yb1—O1^iv	180.00 (13)	K2^xx—O2—K2^xxi	120.0
O1—Yb1—O1^vii	92.64 (12)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) −x+y, −x+1, z; (ii) x, y+1, z; (iii) −y+1, x−y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) y, −x+y+1, −z; (vii) x−y, x, −z; (viii) −x+1, −y+1, −z; (ix) x−1, y, z; (x) −x+y, −x, z; (xi) x, y, −z+1/2; (xii) −y, x−y, −z+1/2; (xiii) −x+y, −x, −z+1/2; (xiv) x−1, y−1, z; (xv) −x, −y, z+1/2; (xvi) −x, −y, −z; (xvii) y, −x+y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(223_K)

Crystal data

K3O7Si2Yb	Dx = 3.865 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1160 reflections
a = 5.7156 (5) Å	θ = 7.1–29.4°
c = 13.9269 (12) Å	µ = 13.76 mm^−1
V = 394.01 (8) Å^3	T = 223 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	187 reflections with I > 2σ(I)
ω scans	Rint = 0.045
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −6→7
2481 measured reflections	k = −7→7
209 independent reflections	l = −16→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0087P)^2 + 0.3221P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.014	(Δ/σ)max < 0.001
wR(F^2) = 0.032	Δρmax = 0.46 e Å^−3
S = 1.23	Δρmin = −0.46 e Å^−3
209 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0140 (8)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09129 (12)	0.0097 (3)
K2	0.000000	0.000000	0.250000	0.0131 (5)
Yb1	0.000000	0.000000	0.000000	0.00340 (19)
Si1	0.666667	0.333333	0.13222 (14)	0.0034 (4)
O1	0.3569 (6)	0.1784 (3)	0.09582 (19)	0.0093 (6)
O2	0.666667	0.333333	0.250000	0.0174 (17)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0085 (5)	0.0085 (5)	0.0120 (8)	0.0043 (2)	0.000	0.000
K2	0.0171 (8)	0.0171 (8)	0.0052 (10)	0.0085 (4)	0.000	0.000
Yb1	0.0032 (2)	0.0032 (2)	0.0038 (3)	0.00159 (10)	0.000	0.000
Si1	0.0034 (6)	0.0034 (6)	0.0034 (8)	0.0017 (3)	0.000	0.000
O1	0.0061 (15)	0.0091 (11)	0.0117 (14)	0.0030 (7)	−0.0024 (13)	−0.0012 (7)
O2	0.024 (3)	0.024 (3)	0.005 (4)	0.0119 (14)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8609 (3)	K2—O1^xii	2.780 (3)
K1—O1^ii	2.8609 (3)	K2—O2^xiii	3.2999 (3)
K1—O1^iii	2.8609 (3)	K2—O2	3.2999 (3)
K1—O1^iv	2.8609 (3)	K2—O2^xiv	3.2999 (3)
K1—O1	2.8609 (3)	K2—Yb1	3.4817 (3)
K1—O1^v	2.8609 (3)	K2—Yb1^xv	3.4817 (3)
K1—O1^vi	3.024 (3)	K2—Si1^x	3.6851 (9)
K1—O1^vii	3.024 (3)	Yb1—O1	2.214 (3)
K1—O1^viii	3.024 (3)	Yb1—O1^xvi	2.214 (3)
K1—Si1^viii	3.113 (3)	Yb1—O1^xvii	2.214 (3)
K1—Si1	3.3488 (5)	Yb1—O1^iv	2.214 (3)
K1—Si1^i	3.3488 (5)	Yb1—O1^vii	2.214 (3)
K2—O1^ix	2.780 (3)	Yb1—O1^ix	2.214 (3)
K2—O1^x	2.780 (3)	Si1—O1^xviii	1.615 (3)
K2—O1^xi	2.780 (3)	Si1—O1^v	1.615 (3)
K2—O1^iv	2.780 (3)	Si1—O1	1.615 (3)
K2—O1	2.780 (3)	Si1—O2	1.640 (2)
O1^i—K1—O1^ii	64.65 (11)	O1^xvi—Yb1—O1^vii	87.42 (11)
O1^i—K1—O1^iii	55.32 (11)	O1^xvii—Yb1—O1^vii	87.42 (11)
O1^ii—K1—O1^iii	119.952 (5)	O1^iv—Yb1—O1^vii	92.58 (11)
O1^i—K1—O1^iv	119.952 (5)	O1—Yb1—O1^ix	87.42 (10)
O1^ii—K1—O1^iv	55.32 (11)	O1^xvi—Yb1—O1^ix	92.58 (11)
O1^iii—K1—O1^iv	174.69 (12)	O1^xvii—Yb1—O1^ix	92.58 (11)
O1^i—K1—O1	174.69 (12)	O1^iv—Yb1—O1^ix	87.42 (11)
O1^ii—K1—O1	119.951 (5)	O1^vii—Yb1—O1^ix	180.00 (16)
O1^iii—K1—O1	119.952 (5)	O1—Yb1—K2	52.93 (7)
O1^iv—K1—O1	64.65 (11)	O1^xvi—Yb1—K2	127.07 (7)
O1^i—K1—O1^v	119.952 (6)	O1^xvii—Yb1—K2	127.07 (7)
O1^ii—K1—O1^v	174.69 (12)	O1^iv—Yb1—K2	52.93 (7)
O1^iii—K1—O1^v	64.65 (12)	O1^vii—Yb1—K2	127.07 (7)
O1^iv—K1—O1^v	119.952 (5)	O1^ix—Yb1—K2	52.93 (7)
O1—K1—O1^v	55.32 (11)	O1—Yb1—K2^xvi	127.07 (7)
O1^i—K1—O1^vi	65.83 (9)	O1^xvi—Yb1—K2^xvi	52.93 (7)
O1^ii—K1—O1^vi	65.83 (9)	O1^xvii—Yb1—K2^xvi	52.93 (7)
O1^iii—K1—O1^vi	89.91 (7)	O1^iv—Yb1—K2^xvi	127.07 (7)
O1^iv—K1—O1^vi	89.91 (7)	O1^vii—Yb1—K2^xvi	52.93 (7)
O1—K1—O1^vi	117.91 (6)	O1^ix—Yb1—K2^xvi	127.07 (7)
O1^v—K1—O1^vi	117.91 (6)	K2—Yb1—K2^xvi	180.0
O1^i—K1—O1^vii	117.91 (6)	O1—Yb1—K1^xvi	126.086 (13)
O1^ii—K1—O1^vii	89.91 (7)	O1^xvi—Yb1—K1^xvi	53.914 (13)
O1^iii—K1—O1^vii	117.91 (6)	O1^xvii—Yb1—K1^xvi	53.915 (13)
O1^iv—K1—O1^vii	65.83 (9)	O1^iv—Yb1—K1^xvi	126.086 (13)
O1—K1—O1^vii	65.83 (9)	O1^vii—Yb1—K1^xvi	121.86 (7)
O1^v—K1—O1^vii	89.91 (7)	O1^ix—Yb1—K1^xvi	58.14 (7)
O1^vi—K1—O1^vii	52.11 (9)	K2—Yb1—K1^xvi	111.07 (3)
O1^i—K1—O1^viii	89.91 (7)	K2^xvi—Yb1—K1^xvi	68.93 (3)
O1^ii—K1—O1^viii	117.91 (6)	O1—Yb1—K1^viii	58.14 (7)
O1^iii—K1—O1^viii	65.83 (9)	O1^xvi—Yb1—K1^viii	121.86 (7)
O1^iv—K1—O1^viii	117.91 (6)	O1^xvii—Yb1—K1^viii	53.915 (13)
O1—K1—O1^viii	89.91 (7)	O1^iv—Yb1—K1^viii	126.085 (13)
O1^v—K1—O1^viii	65.83 (9)	O1^vii—Yb1—K1^viii	53.914 (13)
O1^vi—K1—O1^viii	52.11 (9)	O1^ix—Yb1—K1^viii	126.086 (13)
O1^vii—K1—O1^viii	52.11 (9)	K2—Yb1—K1^viii	111.07 (3)
O1^i—K1—Si1^viii	91.26 (7)	K2^xvi—Yb1—K1^viii	68.93 (3)
O1^ii—K1—Si1^viii	91.26 (7)	K1^xvi—Yb1—K1^viii	107.83 (3)
O1^iii—K1—Si1^viii	91.26 (7)	O1—Yb1—K1^xiii	121.86 (7)
O1^iv—K1—Si1^viii	91.26 (7)	O1^xvi—Yb1—K1^xiii	58.14 (7)
O1—K1—Si1^viii	91.26 (7)	O1^xvii—Yb1—K1^xiii	126.085 (13)
O1^v—K1—Si1^viii	91.26 (7)	O1^iv—Yb1—K1^xiii	53.915 (13)
O1^vi—K1—Si1^viii	30.47 (6)	O1^vii—Yb1—K1^xiii	126.086 (13)
O1^vii—K1—Si1^viii	30.47 (6)	O1^ix—Yb1—K1^xiii	53.914 (13)
O1^viii—K1—Si1^viii	30.47 (6)	K2—Yb1—K1^xiii	68.93 (3)
O1^i—K1—Si1	145.96 (6)	K2^xvi—Yb1—K1^xiii	111.07 (3)
O1^ii—K1—Si1	145.96 (6)	K1^xvi—Yb1—K1^xiii	72.17 (3)
O1^iii—K1—Si1	92.08 (6)	K1^viii—Yb1—K1^xiii	180.0
O1^iv—K1—Si1	92.08 (6)	O1—Yb1—K1	53.914 (13)
O1—K1—Si1	28.80 (6)	O1^xvi—Yb1—K1	126.086 (13)
O1^v—K1—Si1	28.80 (6)	O1^xvii—Yb1—K1	126.086 (13)
O1^vi—K1—Si1	130.27 (7)	O1^iv—Yb1—K1	53.914 (13)
O1^vii—K1—Si1	84.08 (4)	O1^vii—Yb1—K1	58.14 (7)
O1^viii—K1—Si1	84.08 (4)	O1^ix—Yb1—K1	121.86 (7)
Si1^viii—K1—Si1	99.80 (4)	K2—Yb1—K1	68.93 (3)
O1^i—K1—Si1^i	28.80 (6)	K2^xvi—Yb1—K1	111.07 (3)
O1^ii—K1—Si1^i	92.08 (6)	K1^xvi—Yb1—K1	180.0
O1^iii—K1—Si1^i	28.80 (6)	K1^viii—Yb1—K1	72.17 (3)
O1^iv—K1—Si1^i	145.96 (6)	K1^xiii—Yb1—K1	107.83 (3)
O1—K1—Si1^i	145.96 (6)	O1^xviii—Si1—O1^v	110.63 (12)
O1^v—K1—Si1^i	92.09 (6)	O1^xviii—Si1—O1	110.63 (12)
O1^vi—K1—Si1^i	84.08 (4)	O1^v—Si1—O1	110.63 (12)
O1^vii—K1—Si1^i	130.27 (7)	O1^xviii—Si1—O2	108.29 (12)
O1^viii—K1—Si1^i	84.08 (4)	O1^v—Si1—O2	108.29 (12)
Si1^viii—K1—Si1^i	99.80 (4)	O1—Si1—O2	108.29 (12)
Si1—K1—Si1^i	117.16 (2)	O1^xviii—Si1—K1^viii	71.71 (12)
O1^ix—K2—O1^x	142.96 (5)	O1^v—Si1—K1^viii	71.71 (12)
O1^ix—K2—O1^xi	142.96 (5)	O1—Si1—K1^viii	71.71 (12)
O1^x—K2—O1^xi	66.76 (9)	O2—Si1—K1^viii	180.0
O1^ix—K2—O1^iv	66.76 (9)	O1^xviii—Si1—K1	151.91 (14)
O1^x—K2—O1^iv	142.96 (5)	O1^v—Si1—K1	58.585 (11)
O1^xi—K2—O1^iv	101.11 (11)	O1—Si1—K1	58.585 (11)
O1^ix—K2—O1	66.76 (9)	O2—Si1—K1	99.80 (4)
O1^x—K2—O1	101.11 (11)	K1^viii—Si1—K1	80.20 (4)
O1^xi—K2—O1	142.96 (5)	O1^xviii—Si1—K1^xix	58.585 (11)
O1^iv—K2—O1	66.76 (9)	O1^v—Si1—K1^xix	151.91 (14)
O1^ix—K2—O1^xii	101.11 (11)	O1—Si1—K1^xix	58.586 (11)
O1^x—K2—O1^xii	66.76 (9)	O2—Si1—K1^xix	99.80 (4)
O1^xi—K2—O1^xii	66.76 (9)	K1^viii—Si1—K1^xix	80.20 (4)
O1^iv—K2—O1^xii	142.96 (5)	K1—Si1—K1^xix	117.16 (2)
O1—K2—O1^xii	142.96 (5)	O1^xviii—Si1—K1^xx	58.585 (11)
O1^ix—K2—O2^xiii	50.56 (6)	O1^v—Si1—K1^xx	58.586 (11)
O1^x—K2—O2^xiii	108.52 (2)	O1—Si1—K1^xx	151.91 (14)
O1^xi—K2—O2^xiii	108.52 (2)	O2—Si1—K1^xx	99.80 (4)
O1^iv—K2—O2^xiii	108.52 (2)	K1^viii—Si1—K1^xx	80.20 (4)
O1—K2—O2^xiii	108.52 (2)	K1—Si1—K1^xx	117.16 (2)
O1^xii—K2—O2^xiii	50.56 (6)	K1^xix—Si1—K1^xx	117.16 (2)
O1^ix—K2—O2	108.52 (2)	O1^xviii—Si1—K2^xx	44.72 (11)
O1^x—K2—O2	50.56 (6)	O1^v—Si1—K2^xx	124.39 (4)
O1^xi—K2—O2	108.52 (2)	O1—Si1—K2^xx	124.39 (4)
O1^iv—K2—O2	108.52 (2)	O2—Si1—K2^xx	63.57 (3)
O1—K2—O2	50.56 (6)	K1^viii—Si1—K2^xx	116.43 (3)
O1^xii—K2—O2	108.52 (2)	K1—Si1—K2^xx	163.37 (6)
O2^xiii—K2—O2	120.0	K1^xix—Si1—K2^xx	68.565 (17)
O1^ix—K2—O2^xiv	108.52 (2)	K1^xx—Si1—K2^xx	68.565 (17)
O1^x—K2—O2^xiv	108.52 (2)	O1^xviii—Si1—K2^xxi	124.39 (4)
O1^xi—K2—O2^xiv	50.56 (6)	O1^v—Si1—K2^xxi	44.72 (11)
O1^iv—K2—O2^xiv	50.56 (6)	O1—Si1—K2^xxi	124.39 (4)
O1—K2—O2^xiv	108.52 (2)	O2—Si1—K2^xxi	63.57 (3)
O1^xii—K2—O2^xiv	108.52 (2)	K1^viii—Si1—K2^xxi	116.43 (3)
O2^xiii—K2—O2^xiv	120.0	K1—Si1—K2^xxi	68.565 (17)
O2—K2—O2^xiv	120.0	K1^xix—Si1—K2^xxi	163.37 (6)
O1^ix—K2—Yb1	39.44 (6)	K1^xx—Si1—K2^xxi	68.566 (17)
O1^x—K2—Yb1	140.56 (6)	K2^xx—Si1—K2^xxi	101.70 (3)
O1^xi—K2—Yb1	140.56 (6)	O1^xviii—Si1—K2	124.39 (4)
O1^iv—K2—Yb1	39.44 (6)	O1^v—Si1—K2	124.39 (4)
O1—K2—Yb1	39.44 (6)	O1—Si1—K2	44.72 (11)
O1^xii—K2—Yb1	140.56 (6)	O2—Si1—K2	63.57 (3)
O2^xiii—K2—Yb1	90.0	K1^viii—Si1—K2	116.43 (3)
O2—K2—Yb1	90.0	K1—Si1—K2	68.565 (17)
O2^xiv—K2—Yb1	90.0	K1^xix—Si1—K2	68.566 (17)
O1^ix—K2—Yb1^xv	140.56 (6)	K1^xx—Si1—K2	163.37 (6)
O1^x—K2—Yb1^xv	39.44 (6)	K2^xx—Si1—K2	101.70 (3)
O1^xi—K2—Yb1^xv	39.44 (6)	K2^xxi—Si1—K2	101.70 (3)
O1^iv—K2—Yb1^xv	140.56 (6)	Si1—O1—Yb1	161.22 (19)
O1—K2—Yb1^xv	140.56 (6)	Si1—O1—K2	111.15 (15)
O1^xii—K2—Yb1^xv	39.44 (6)	Yb1—O1—K2	87.63 (9)
O2^xiii—K2—Yb1^xv	90.0	Si1—O1—K1	92.61 (6)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.38 (6)
O2^xiv—K2—Yb1^xv	90.0	K2—O1—K1	89.49 (6)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.61 (6)
O1^ix—K2—Si1^x	128.92 (2)	Yb1—O1—K1^xix	87.38 (6)
O1^x—K2—Si1^x	24.12 (6)	K2—O1—K1^xix	89.49 (6)
O1^xi—K2—Si1^x	86.60 (4)	K1—O1—K1^xix	174.69 (12)
O1^iv—K2—Si1^x	128.92 (2)	Si1—O1—K1^viii	77.82 (13)
O1—K2—Si1^x	76.99 (6)	Yb1—O1—K1^viii	83.40 (8)
O1^xii—K2—Si1^x	86.60 (4)	K2—O1—K1^viii	171.03 (11)
O2^xiii—K2—Si1^x	116.599 (7)	K1—O1—K1^viii	90.09 (7)
O2—K2—Si1^x	26.43 (3)	K1^xix—O1—K1^viii	90.09 (7)
O2^xiv—K2—Si1^x	116.598 (7)	Si1—O2—Si1^x	180.0
Yb1—K2—Si1^x	116.43 (3)	Si1—O2—K2^xx	90.0
Yb1^xv—K2—Si1^x	63.57 (3)	Si1^x—O2—K2^xx	90.0
O1—Yb1—O1^xvi	180.00 (16)	Si1—O2—K2	90.0
O1—Yb1—O1^xvii	92.58 (11)	Si1^x—O2—K2	90.0
O1^xvi—Yb1—O1^xvii	87.42 (11)	K2^xx—O2—K2	120.0
O1—Yb1—O1^iv	87.42 (11)	Si1—O2—K2^xxi	90.0
O1^xvi—Yb1—O1^iv	92.58 (11)	Si1^x—O2—K2^xxi	90.0
O1^xvii—Yb1—O1^iv	180.00 (11)	K2^xx—O2—K2^xxi	120.0
O1—Yb1—O1^vii	92.58 (10)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) x, y+1, z; (ii) −x+y, −x+1, z; (iii) −y+1, x−y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) y, −x+y+1, −z; (vii) x−y, x, −z; (viii) −x+1, −y+1, −z; (ix) −x+y, −x, z; (x) x, y, −z+1/2; (xi) −y, x−y, −z+1/2; (xii) −x+y, −x, −z+1/2; (xiii) x−1, y−1, z; (xiv) x−1, y, z; (xv) −x, −y, z+1/2; (xvi) −x, −y, −z; (xvii) y, −x+y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(233_K)

Crystal data

K3O7Si2Yb	Dx = 3.852 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1155 reflections
a = 5.7207 (6) Å	θ = 4.3–29.4°
c = 13.9476 (16) Å	µ = 13.71 mm^−1
V = 395.30 (9) Å^3	T = 233 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	191 reflections with I > 2σ(I)
ω scans	Rint = 0.046
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −6→7
2496 measured reflections	k = −7→5
211 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0107P)^2 + 0.7839P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.014	(Δ/σ)max < 0.001
wR(F^2) = 0.034	Δρmax = 0.46 e Å^−3
S = 1.17	Δρmin = −0.49 e Å^−3
211 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0143 (9)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09132 (12)	0.0102 (3)
K2	0.000000	0.000000	0.250000	0.0132 (5)
Yb1	0.000000	0.000000	0.000000	0.00361 (19)
Si1	0.666667	0.333333	0.13215 (14)	0.0036 (4)
O1	0.3571 (6)	0.1786 (3)	0.09585 (19)	0.0097 (6)
O2	0.666667	0.333333	0.250000	0.0186 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0091 (5)	0.0091 (5)	0.0123 (7)	0.0045 (2)	0.000	0.000
K2	0.0165 (8)	0.0165 (8)	0.0066 (10)	0.0082 (4)	0.000	0.000
Yb1	0.0033 (2)	0.0033 (2)	0.0042 (3)	0.00165 (10)	0.000	0.000
Si1	0.0038 (6)	0.0038 (6)	0.0031 (8)	0.0019 (3)	0.000	0.000
O1	0.0077 (15)	0.0090 (11)	0.0120 (13)	0.0039 (8)	−0.0038 (14)	−0.0019 (7)
O2	0.026 (3)	0.026 (3)	0.004 (3)	0.0129 (14)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8635 (3)	K2—O1	2.785 (3)
K1—O1^ii	2.8635 (3)	K2—O2^xiii	3.3028 (4)
K1—O1^iii	2.8635 (3)	K2—O2	3.3028 (4)
K1—O1^iv	2.8635 (3)	K2—O2^xiv	3.3029 (4)
K1—O1	2.8635 (3)	K2—Yb1	3.4869 (4)
K1—O1^v	2.8635 (3)	K2—Yb1^xv	3.4869 (4)
K1—O1^vi	3.028 (3)	K2—Si1^ix	3.6893 (9)
K1—O1^vii	3.028 (3)	Yb1—O1	2.218 (3)
K1—O1^viii	3.028 (3)	Yb1—O1^xvi	2.218 (3)
K1—Si1^viii	3.117 (3)	Yb1—O1^xvii	2.218 (3)
K1—Si1	3.3516 (5)	Yb1—O1^iv	2.218 (3)
K1—Si1^ii	3.3516 (5)	Yb1—O1^vii	2.218 (3)
K2—O1^ix	2.785 (3)	Yb1—O1^x	2.218 (3)
K2—O1^x	2.785 (3)	Si1—O1^xviii	1.615 (3)
K2—O1^xi	2.785 (3)	Si1—O1^v	1.615 (3)
K2—O1^iv	2.785 (3)	Si1—O1	1.615 (3)
K2—O1^xii	2.785 (3)	Si1—O2	1.6438 (19)
O1^i—K1—O1^ii	64.71 (12)	O1^xvi—Yb1—O1^vii	87.42 (11)
O1^i—K1—O1^iii	119.952 (5)	O1^xvii—Yb1—O1^vii	87.42 (11)
O1^ii—K1—O1^iii	55.26 (12)	O1^iv—Yb1—O1^vii	92.58 (11)
O1^i—K1—O1^iv	55.26 (12)	O1—Yb1—O1^x	87.42 (11)
O1^ii—K1—O1^iv	119.952 (5)	O1^xvi—Yb1—O1^x	92.58 (11)
O1^iii—K1—O1^iv	174.64 (12)	O1^xvii—Yb1—O1^x	92.58 (11)
O1^i—K1—O1	119.952 (5)	O1^iv—Yb1—O1^x	87.42 (11)
O1^ii—K1—O1	174.64 (12)	O1^vii—Yb1—O1^x	180.00 (17)
O1^iii—K1—O1	119.952 (5)	O1—Yb1—K2	52.93 (7)
O1^iv—K1—O1	64.71 (12)	O1^xvi—Yb1—K2	127.07 (7)
O1^i—K1—O1^v	174.64 (12)	O1^xvii—Yb1—K2	127.07 (7)
O1^ii—K1—O1^v	119.952 (6)	O1^iv—Yb1—K2	52.93 (7)
O1^iii—K1—O1^v	64.71 (12)	O1^vii—Yb1—K2	127.07 (7)
O1^iv—K1—O1^v	119.952 (5)	O1^x—Yb1—K2	52.93 (7)
O1—K1—O1^v	55.26 (12)	O1—Yb1—K2^xvi	127.07 (7)
O1^i—K1—O1^vi	65.88 (9)	O1^xvi—Yb1—K2^xvi	52.93 (7)
O1^ii—K1—O1^vi	65.88 (9)	O1^xvii—Yb1—K2^xvi	52.93 (7)
O1^iii—K1—O1^vi	89.90 (7)	O1^iv—Yb1—K2^xvi	127.07 (7)
O1^iv—K1—O1^vi	89.90 (7)	O1^vii—Yb1—K2^xvi	52.93 (7)
O1—K1—O1^vi	117.88 (7)	O1^x—Yb1—K2^xvi	127.07 (7)
O1^v—K1—O1^vi	117.88 (7)	K2—Yb1—K2^xvi	180.0
O1^i—K1—O1^vii	89.90 (7)	O1—Yb1—K1^xvi	126.095 (13)
O1^ii—K1—O1^vii	117.88 (7)	O1^xvi—Yb1—K1^xvi	53.905 (13)
O1^iii—K1—O1^vii	117.88 (7)	O1^xvii—Yb1—K1^xvi	53.906 (13)
O1^iv—K1—O1^vii	65.88 (9)	O1^iv—Yb1—K1^xvi	126.094 (13)
O1—K1—O1^vii	65.88 (9)	O1^vii—Yb1—K1^xvi	121.84 (8)
O1^v—K1—O1^vii	89.90 (7)	O1^x—Yb1—K1^xvi	58.16 (8)
O1^vi—K1—O1^vii	52.03 (9)	K2—Yb1—K1^xvi	111.09 (3)
O1^i—K1—O1^viii	117.88 (7)	K2^xvi—Yb1—K1^xvi	68.91 (3)
O1^ii—K1—O1^viii	89.90 (7)	O1—Yb1—K1^viii	58.16 (8)
O1^iii—K1—O1^viii	65.88 (9)	O1^xvi—Yb1—K1^viii	121.84 (8)
O1^iv—K1—O1^viii	117.88 (7)	O1^xvii—Yb1—K1^viii	53.906 (13)
O1—K1—O1^viii	89.89 (7)	O1^iv—Yb1—K1^viii	126.094 (13)
O1^v—K1—O1^viii	65.88 (9)	O1^vii—Yb1—K1^viii	53.905 (13)
O1^vi—K1—O1^viii	52.03 (9)	O1^x—Yb1—K1^viii	126.095 (13)
O1^vii—K1—O1^viii	52.03 (9)	K2—Yb1—K1^viii	111.09 (3)
O1^i—K1—Si1^viii	91.27 (7)	K2^xvi—Yb1—K1^viii	68.91 (3)
O1^ii—K1—Si1^viii	91.27 (7)	K1^xvi—Yb1—K1^viii	107.81 (3)
O1^iii—K1—Si1^viii	91.27 (7)	O1—Yb1—K1^xiii	121.84 (8)
O1^iv—K1—Si1^viii	91.27 (7)	O1^xvi—Yb1—K1^xiii	58.16 (8)
O1—K1—Si1^viii	91.26 (7)	O1^xvii—Yb1—K1^xiii	126.094 (13)
O1^v—K1—Si1^viii	91.26 (7)	O1^iv—Yb1—K1^xiii	53.906 (13)
O1^vi—K1—Si1^viii	30.43 (6)	O1^vii—Yb1—K1^xiii	126.095 (13)
O1^vii—K1—Si1^viii	30.43 (6)	O1^x—Yb1—K1^xiii	53.905 (13)
O1^viii—K1—Si1^viii	30.43 (6)	K2—Yb1—K1^xiii	68.91 (3)
O1^i—K1—Si1	145.94 (6)	K2^xvi—Yb1—K1^xiii	111.09 (3)
O1^ii—K1—Si1	145.94 (6)	K1^xvi—Yb1—K1^xiii	72.19 (3)
O1^iii—K1—Si1	92.11 (6)	K1^viii—Yb1—K1^xiii	180.00 (5)
O1^iv—K1—Si1	92.11 (6)	O1—Yb1—K1	53.906 (13)
O1—K1—Si1	28.77 (6)	O1^xvi—Yb1—K1	126.094 (13)
O1^v—K1—Si1	28.77 (6)	O1^xvii—Yb1—K1	126.094 (13)
O1^vi—K1—Si1	130.21 (7)	O1^iv—Yb1—K1	53.906 (13)
O1^vii—K1—Si1	84.08 (4)	O1^vii—Yb1—K1	58.16 (8)
O1^viii—K1—Si1	84.08 (4)	O1^x—Yb1—K1	121.84 (8)
Si1^viii—K1—Si1	99.78 (4)	K2—Yb1—K1	68.91 (3)
O1^i—K1—Si1^ii	92.11 (6)	K2^xvi—Yb1—K1	111.09 (3)
O1^ii—K1—Si1^ii	28.77 (6)	K1^xvi—Yb1—K1	180.0
O1^iii—K1—Si1^ii	28.77 (6)	K1^viii—Yb1—K1	72.19 (3)
O1^iv—K1—Si1^ii	145.94 (6)	K1^xiii—Yb1—K1	107.81 (3)
O1—K1—Si1^ii	145.94 (6)	O1^xviii—Si1—O1^v	110.64 (12)
O1^v—K1—Si1^ii	92.11 (6)	O1^xviii—Si1—O1	110.64 (12)
O1^vi—K1—Si1^ii	84.09 (4)	O1^v—Si1—O1	110.64 (12)
O1^vii—K1—Si1^ii	130.21 (7)	O1^xviii—Si1—O2	108.27 (12)
O1^viii—K1—Si1^ii	84.09 (4)	O1^v—Si1—O2	108.27 (12)
Si1^viii—K1—Si1^ii	99.78 (4)	O1—Si1—O2	108.27 (12)
Si1—K1—Si1^ii	117.17 (2)	O1^xviii—Si1—K1^viii	71.73 (12)
O1^ix—K2—O1^x	142.95 (5)	O1^v—Si1—K1^viii	71.73 (12)
O1^ix—K2—O1^xi	66.78 (9)	O1—Si1—K1^viii	71.73 (12)
O1^x—K2—O1^xi	142.95 (5)	O2—Si1—K1^viii	180.0
O1^ix—K2—O1^iv	142.95 (5)	O1^xviii—Si1—K1^xix	58.590 (11)
O1^x—K2—O1^iv	66.78 (9)	O1^v—Si1—K1^xix	151.95 (14)
O1^xi—K2—O1^iv	101.09 (12)	O1—Si1—K1^xix	58.590 (11)
O1^ix—K2—O1^xii	66.78 (9)	O2—Si1—K1^xix	99.78 (4)
O1^x—K2—O1^xii	101.09 (12)	K1^viii—Si1—K1^xix	80.22 (4)
O1^xi—K2—O1^xii	66.78 (9)	O1^xviii—Si1—K1^xx	58.590 (11)
O1^iv—K2—O1^xii	142.95 (5)	O1^v—Si1—K1^xx	58.590 (11)
O1^ix—K2—O1	101.09 (12)	O1—Si1—K1^xx	151.95 (14)
O1^x—K2—O1	66.78 (9)	O2—Si1—K1^xx	99.78 (4)
O1^xi—K2—O1	142.95 (5)	K1^viii—Si1—K1^xx	80.22 (4)
O1^iv—K2—O1	66.78 (9)	K1^xix—Si1—K1^xx	117.17 (2)
O1^xii—K2—O1	142.95 (5)	O1^xviii—Si1—K1	151.95 (14)
O1^ix—K2—O2^xiii	108.53 (2)	O1^v—Si1—K1	58.590 (11)
O1^x—K2—O2^xiii	50.55 (6)	O1—Si1—K1	58.590 (11)
O1^xi—K2—O2^xiii	108.53 (2)	O2—Si1—K1	99.78 (4)
O1^iv—K2—O2^xiii	108.52 (2)	K1^viii—Si1—K1	80.22 (4)
O1^xii—K2—O2^xiii	50.55 (6)	K1^xix—Si1—K1	117.17 (2)
O1—K2—O2^xiii	108.53 (2)	K1^xx—Si1—K1	117.17 (2)
O1^ix—K2—O2	50.55 (6)	O1^xviii—Si1—K2^xx	44.73 (11)
O1^x—K2—O2	108.53 (2)	O1^v—Si1—K2^xx	124.38 (4)
O1^xi—K2—O2	108.53 (2)	O1—Si1—K2^xx	124.39 (4)
O1^iv—K2—O2	108.53 (2)	O2—Si1—K2^xx	63.54 (3)
O1^xii—K2—O2	108.53 (2)	K1^viii—Si1—K2^xx	116.46 (3)
O1—K2—O2	50.55 (6)	K1^xix—Si1—K2^xx	68.567 (17)
O2^xiii—K2—O2	120.0	K1^xx—Si1—K2^xx	68.567 (17)
O1^ix—K2—O2^xiv	108.53 (2)	K1—Si1—K2^xx	163.32 (6)
O1^x—K2—O2^xiv	108.53 (2)	O1^xviii—Si1—K2^xxi	124.38 (4)
O1^xi—K2—O2^xiv	50.55 (6)	O1^v—Si1—K2^xxi	44.73 (11)
O1^iv—K2—O2^xiv	50.55 (6)	O1—Si1—K2^xxi	124.39 (4)
O1^xii—K2—O2^xiv	108.53 (2)	O2—Si1—K2^xxi	63.54 (3)
O1—K2—O2^xiv	108.53 (2)	K1^viii—Si1—K2^xxi	116.46 (3)
O2^xiii—K2—O2^xiv	120.0	K1^xix—Si1—K2^xxi	163.32 (6)
O2—K2—O2^xiv	120.0	K1^xx—Si1—K2^xxi	68.567 (17)
O1^ix—K2—Yb1	140.55 (6)	K1—Si1—K2^xxi	68.567 (17)
O1^x—K2—Yb1	39.45 (6)	K2^xx—Si1—K2^xxi	101.67 (3)
O1^xi—K2—Yb1	140.55 (6)	O1^xviii—Si1—K2	124.38 (4)
O1^iv—K2—Yb1	39.45 (6)	O1^v—Si1—K2	124.38 (4)
O1^xii—K2—Yb1	140.55 (6)	O1—Si1—K2	44.73 (11)
O1—K2—Yb1	39.45 (6)	O2—Si1—K2	63.54 (3)
O2^xiii—K2—Yb1	90.0	K1^viii—Si1—K2	116.46 (3)
O2—K2—Yb1	90.0	K1^xix—Si1—K2	68.567 (17)
O2^xiv—K2—Yb1	90.0	K1^xx—Si1—K2	163.32 (6)
O1^ix—K2—Yb1^xv	39.45 (6)	K1—Si1—K2	68.567 (17)
O1^x—K2—Yb1^xv	140.55 (6)	K2^xx—Si1—K2	101.67 (3)
O1^xi—K2—Yb1^xv	39.45 (6)	K2^xxi—Si1—K2	101.67 (3)
O1^iv—K2—Yb1^xv	140.55 (6)	Si1—O1—Yb1	161.20 (19)
O1^xii—K2—Yb1^xv	39.45 (6)	Si1—O1—K2	111.18 (15)
O1—K2—Yb1^xv	140.55 (6)	Yb1—O1—K2	87.62 (10)
O2^xiii—K2—Yb1^xv	90.0	Si1—O1—K1	92.64 (6)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.35 (6)
O2^xiv—K2—Yb1^xv	90.0	K2—O1—K1	89.48 (7)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.64 (6)
O1^ix—K2—Si1^ix	24.09 (6)	Yb1—O1—K1^xix	87.35 (6)
O1^x—K2—Si1^ix	128.94 (2)	K2—O1—K1^xix	89.48 (7)
O1^xi—K2—Si1^ix	86.58 (4)	K1—O1—K1^xix	174.64 (12)
O1^iv—K2—Si1^ix	128.94 (2)	Si1—O1—K1^viii	77.84 (13)
O1^xii—K2—Si1^ix	86.58 (4)	Yb1—O1—K1^viii	83.36 (8)
O1—K2—Si1^ix	77.01 (6)	K2—O1—K1^viii	170.98 (11)
O2^xiii—K2—Si1^ix	116.592 (7)	K1—O1—K1^viii	90.10 (7)
O2—K2—Si1^ix	26.46 (3)	K1^xix—O1—K1^viii	90.11 (7)
O2^xiv—K2—Si1^ix	116.591 (7)	Si1^ix—O2—Si1	180.0
Yb1—K2—Si1^ix	116.46 (3)	Si1^ix—O2—K2^xx	90.0
Yb1^xv—K2—Si1^ix	63.54 (3)	Si1—O2—K2^xx	90.0
O1—Yb1—O1^xvi	180.0	Si1^ix—O2—K2	90.0
O1—Yb1—O1^xvii	92.58 (11)	Si1—O2—K2	90.0
O1^xvi—Yb1—O1^xvii	87.42 (11)	K2^xx—O2—K2	120.0
O1—Yb1—O1^iv	87.42 (11)	Si1^ix—O2—K2^xxi	90.0
O1^xvi—Yb1—O1^iv	92.58 (11)	Si1—O2—K2^xxi	90.0
O1^xvii—Yb1—O1^iv	180.00 (13)	K2^xx—O2—K2^xxi	120.0
O1—Yb1—O1^vii	92.58 (11)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) −x+y, −x+1, z; (ii) x, y+1, z; (iii) −y+1, x−y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) y, −x+y+1, −z; (vii) x−y, x, −z; (viii) −x+1, −y+1, −z; (ix) x, y, −z+1/2; (x) −x+y, −x, z; (xi) −y, x−y, −z+1/2; (xii) −x+y, −x, −z+1/2; (xiii) x−1, y−1, z; (xiv) x−1, y, z; (xv) −x, −y, z+1/2; (xvi) −x, −y, −z; (xvii) y, −x+y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(243_K)

Crystal data

K3O7Si2Yb	Dx = 3.846 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1187 reflections
a = 5.7268 (7) Å	θ = 4.3–29.9°
c = 13.9407 (17) Å	µ = 13.69 mm^−1
V = 395.95 (11) Å^3	T = 243 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	187 reflections with I > 2σ(I)
ω scans	Rint = 0.046
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −7→7
2498 measured reflections	k = −5→7
211 independent reflections	l = −16→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0144P)^2 + 0.3601P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.015	(Δ/σ)max < 0.001
wR(F^2) = 0.035	Δρmax = 0.47 e Å^−3
S = 1.15	Δρmin = −0.44 e Å^−3
211 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0126 (9)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09128 (12)	0.0107 (4)
K2	0.000000	0.000000	0.250000	0.0142 (5)
Yb1	0.000000	0.000000	0.000000	0.0038 (2)
Si1	0.666667	0.333333	0.13226 (14)	0.0040 (4)
O1	0.3564 (6)	0.1782 (3)	0.09583 (19)	0.0103 (6)
O2	0.666667	0.333333	0.250000	0.0197 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0092 (5)	0.0092 (5)	0.0135 (8)	0.0046 (2)	0.000	0.000
K2	0.0185 (8)	0.0185 (8)	0.0056 (11)	0.0092 (4)	0.000	0.000
Yb1	0.0035 (2)	0.0035 (2)	0.0045 (3)	0.00175 (11)	0.000	0.000
Si1	0.0043 (6)	0.0043 (6)	0.0036 (8)	0.0021 (3)	0.000	0.000
O1	0.0088 (15)	0.0112 (11)	0.0101 (13)	0.0044 (8)	−0.0021 (14)	−0.0011 (7)
O2	0.029 (3)	0.029 (3)	0.002 (3)	0.0143 (14)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8664 (4)	K2—O1	2.783 (3)
K1—O1^ii	2.8664 (4)	K2—O2^xiii	3.3064 (4)
K1—O1^iii	2.8664 (4)	K2—O2	3.3064 (4)
K1—O1^iv	2.8664 (4)	K2—O2^xiv	3.3064 (4)
K1—O1	2.8664 (4)	K2—Yb1	3.4852 (4)
K1—O1^v	2.8664 (4)	K2—Yb1^xv	3.4852 (4)
K1—O1^vi	3.029 (3)	K2—Si1^xi	3.6913 (9)
K1—O1^vii	3.029 (3)	Yb1—O1^xvi	2.216 (3)
K1—O1^viii	3.029 (3)	Yb1—O1^iv	2.216 (3)
K1—Si1^vii	3.116 (3)	Yb1—O1	2.216 (3)
K1—Si1	3.3554 (6)	Yb1—O1^xvii	2.216 (3)
K1—Si1^ii	3.3554 (6)	Yb1—O1^vi	2.216 (3)
K2—O1^ix	2.783 (3)	Yb1—O1^x	2.216 (3)
K2—O1^iv	2.783 (3)	Si1—O1^v	1.620 (3)
K2—O1^x	2.783 (3)	Si1—O1	1.620 (3)
K2—O1^xi	2.783 (3)	Si1—O1^xviii	1.620 (3)
K2—O1^xii	2.783 (3)	Si1—O2	1.6414 (19)
O1^i—K1—O1^ii	64.56 (12)	O1^iv—Yb1—O1^vi	92.60 (10)
O1^i—K1—O1^iii	119.952 (5)	O1—Yb1—O1^vi	92.60 (10)
O1^ii—K1—O1^iii	55.41 (12)	O1^xvii—Yb1—O1^vi	87.40 (10)
O1^i—K1—O1^iv	55.41 (12)	O1^xvi—Yb1—O1^x	92.60 (10)
O1^ii—K1—O1^iv	119.952 (5)	O1^iv—Yb1—O1^x	87.40 (10)
O1^iii—K1—O1^iv	174.77 (12)	O1—Yb1—O1^x	87.40 (10)
O1^i—K1—O1	119.951 (5)	O1^xvii—Yb1—O1^x	92.60 (10)
O1^ii—K1—O1	174.77 (12)	O1^vi—Yb1—O1^x	180.00 (16)
O1^iii—K1—O1	119.951 (5)	O1^xvi—Yb1—K2	127.08 (7)
O1^iv—K1—O1	64.56 (12)	O1^iv—Yb1—K2	52.92 (7)
O1^i—K1—O1^v	174.77 (12)	O1—Yb1—K2	52.92 (7)
O1^ii—K1—O1^v	119.951 (5)	O1^xvii—Yb1—K2	127.08 (7)
O1^iii—K1—O1^v	64.56 (12)	O1^vi—Yb1—K2	127.08 (7)
O1^iv—K1—O1^v	119.951 (5)	O1^x—Yb1—K2	52.92 (7)
O1—K1—O1^v	55.41 (12)	O1^xvi—Yb1—K2^xvii	52.92 (7)
O1^i—K1—O1^vi	89.93 (7)	O1^iv—Yb1—K2^xvii	127.08 (7)
O1^ii—K1—O1^vi	117.96 (7)	O1—Yb1—K2^xvii	127.08 (7)
O1^iii—K1—O1^vi	117.96 (7)	O1^xvii—Yb1—K2^xvii	52.92 (7)
O1^iv—K1—O1^vi	65.77 (9)	O1^vi—Yb1—K2^xvii	52.92 (7)
O1—K1—O1^vi	65.77 (9)	O1^x—Yb1—K2^xvii	127.08 (7)
O1^v—K1—O1^vi	89.93 (7)	K2—Yb1—K2^xvii	180.0
O1^i—K1—O1^vii	117.96 (7)	O1^xvi—Yb1—K1^xvii	53.926 (14)
O1^ii—K1—O1^vii	89.93 (7)	O1^iv—Yb1—K1^xvii	126.074 (14)
O1^iii—K1—O1^vii	65.77 (9)	O1—Yb1—K1^xvii	126.075 (13)
O1^iv—K1—O1^vii	117.96 (7)	O1^xvii—Yb1—K1^xvii	53.926 (13)
O1—K1—O1^vii	89.93 (7)	O1^vi—Yb1—K1^xvii	121.87 (7)
O1^v—K1—O1^vii	65.77 (9)	O1^x—Yb1—K1^xvii	58.13 (7)
O1^vi—K1—O1^vii	52.21 (9)	K2—Yb1—K1^xvii	111.05 (3)
O1^i—K1—O1^viii	65.77 (9)	K2^xvii—Yb1—K1^xvii	68.95 (3)
O1^ii—K1—O1^viii	65.77 (9)	O1^xvi—Yb1—K1^vii	53.926 (14)
O1^iii—K1—O1^viii	89.93 (7)	O1^iv—Yb1—K1^vii	126.074 (14)
O1^iv—K1—O1^viii	89.93 (7)	O1—Yb1—K1^vii	58.13 (7)
O1—K1—O1^viii	117.96 (7)	O1^xvii—Yb1—K1^vii	121.87 (7)
O1^v—K1—O1^viii	117.96 (7)	O1^vi—Yb1—K1^vii	53.926 (14)
O1^vi—K1—O1^viii	52.21 (9)	O1^x—Yb1—K1^vii	126.074 (14)
O1^vii—K1—O1^viii	52.21 (9)	K2—Yb1—K1^vii	111.05 (3)
O1^i—K1—Si1^vii	91.27 (7)	K2^xvii—Yb1—K1^vii	68.95 (3)
O1^ii—K1—Si1^vii	91.27 (7)	K1^xvii—Yb1—K1^vii	107.85 (3)
O1^iii—K1—Si1^vii	91.27 (7)	O1^xvi—Yb1—K1^xiii	126.074 (14)
O1^iv—K1—Si1^vii	91.27 (7)	O1^iv—Yb1—K1^xiii	53.926 (14)
O1—K1—Si1^vii	91.27 (7)	O1—Yb1—K1^xiii	121.87 (7)
O1^v—K1—Si1^vii	91.27 (7)	O1^xvii—Yb1—K1^xiii	58.13 (7)
O1^vi—K1—Si1^vii	30.54 (6)	O1^vi—Yb1—K1^xiii	126.074 (14)
O1^vii—K1—Si1^vii	30.54 (6)	O1^x—Yb1—K1^xiii	53.926 (14)
O1^viii—K1—Si1^vii	30.54 (6)	K2—Yb1—K1^xiii	68.95 (3)
O1^i—K1—Si1	146.00 (6)	K2^xvii—Yb1—K1^xiii	111.05 (3)
O1^ii—K1—Si1	146.00 (6)	K1^xvii—Yb1—K1^xiii	72.15 (3)
O1^iii—K1—Si1	92.04 (6)	K1^vii—Yb1—K1^xiii	180.00 (5)
O1^iv—K1—Si1	92.04 (6)	O1^xvi—Yb1—K1	126.075 (13)
O1—K1—Si1	28.85 (6)	O1^iv—Yb1—K1	53.925 (13)
O1^v—K1—Si1	28.85 (6)	O1—Yb1—K1	53.925 (13)
O1^vi—K1—Si1	84.05 (4)	O1^xvii—Yb1—K1	126.074 (13)
O1^vii—K1—Si1	84.05 (4)	O1^vi—Yb1—K1	58.13 (7)
O1^viii—K1—Si1	130.34 (7)	O1^x—Yb1—K1	121.87 (7)
Si1^vii—K1—Si1	99.80 (4)	K2—Yb1—K1	68.95 (3)
O1^i—K1—Si1^ii	92.04 (6)	K2^xvii—Yb1—K1	111.05 (3)
O1^ii—K1—Si1^ii	28.85 (6)	K1^xvii—Yb1—K1	180.0
O1^iii—K1—Si1^ii	28.85 (6)	K1^vii—Yb1—K1	72.15 (3)
O1^iv—K1—Si1^ii	146.00 (6)	K1^xiii—Yb1—K1	107.85 (3)
O1—K1—Si1^ii	146.00 (6)	O1^v—Si1—O1	110.65 (11)
O1^v—K1—Si1^ii	92.04 (6)	O1^v—Si1—O1^xviii	110.65 (11)
O1^vi—K1—Si1^ii	130.34 (7)	O1—Si1—O1^xviii	110.65 (11)
O1^vii—K1—Si1^ii	84.05 (4)	O1^v—Si1—O2	108.26 (12)
O1^viii—K1—Si1^ii	84.05 (4)	O1—Si1—O2	108.26 (12)
Si1^vii—K1—Si1^ii	99.80 (4)	O1^xviii—Si1—O2	108.26 (12)
Si1—K1—Si1^ii	117.16 (2)	O1^v—Si1—K1^vii	71.74 (12)
O1^ix—K2—O1^iv	101.13 (11)	O1—Si1—K1^vii	71.74 (12)
O1^ix—K2—O1^x	142.97 (5)	O1^xviii—Si1—K1^vii	71.74 (12)
O1^iv—K2—O1^x	66.75 (9)	O2—Si1—K1^vii	180.0
O1^ix—K2—O1^xi	66.75 (9)	O1^v—Si1—K1	58.585 (12)
O1^iv—K2—O1^xi	142.97 (5)	O1—Si1—K1	58.585 (12)
O1^x—K2—O1^xi	142.96 (5)	O1^xviii—Si1—K1	151.93 (14)
O1^ix—K2—O1^xii	66.75 (9)	O2—Si1—K1	99.80 (4)
O1^iv—K2—O1^xii	142.97 (5)	K1^vii—Si1—K1	80.20 (4)
O1^x—K2—O1^xii	101.13 (11)	O1^v—Si1—K1^xix	151.93 (14)
O1^xi—K2—O1^xii	66.75 (9)	O1—Si1—K1^xix	58.585 (12)
O1^ix—K2—O1	142.96 (5)	O1^xviii—Si1—K1^xix	58.584 (12)
O1^iv—K2—O1	66.75 (9)	O2—Si1—K1^xix	99.80 (4)
O1^x—K2—O1	66.75 (9)	K1^vii—Si1—K1^xix	80.20 (4)
O1^xi—K2—O1	101.13 (12)	K1—Si1—K1^xix	117.16 (2)
O1^xii—K2—O1	142.96 (5)	O1^v—Si1—K1^xx	58.584 (12)
O1^ix—K2—O2^xiii	108.52 (2)	O1—Si1—K1^xx	151.93 (14)
O1^iv—K2—O2^xiii	108.52 (2)	O1^xviii—Si1—K1^xx	58.584 (12)
O1^x—K2—O2^xiii	50.57 (6)	O2—Si1—K1^xx	99.80 (4)
O1^xi—K2—O2^xiii	108.52 (2)	K1^vii—Si1—K1^xx	80.20 (4)
O1^xii—K2—O2^xiii	50.57 (6)	K1—Si1—K1^xx	117.16 (2)
O1—K2—O2^xiii	108.52 (2)	K1^xix—Si1—K1^xx	117.16 (2)
O1^ix—K2—O2	108.52 (2)	O1^v—Si1—K2^xx	124.38 (4)
O1^iv—K2—O2	108.52 (2)	O1—Si1—K2^xx	124.38 (4)
O1^x—K2—O2	108.52 (2)	O1^xviii—Si1—K2^xx	44.66 (10)
O1^xi—K2—O2	50.57 (6)	O2—Si1—K2^xx	63.60 (3)
O1^xii—K2—O2	108.52 (2)	K1^vii—Si1—K2^xx	116.40 (3)
O1—K2—O2	50.57 (6)	K1—Si1—K2^xx	163.40 (6)
O2^xiii—K2—O2	120.0	K1^xix—Si1—K2^xx	68.555 (17)
O1^ix—K2—O2^xiv	50.57 (6)	K1^xx—Si1—K2^xx	68.555 (17)
O1^iv—K2—O2^xiv	50.57 (6)	O1^v—Si1—K2^xxi	44.66 (10)
O1^x—K2—O2^xiv	108.52 (2)	O1—Si1—K2^xxi	124.38 (4)
O1^xi—K2—O2^xiv	108.52 (2)	O1^xviii—Si1—K2^xxi	124.38 (4)
O1^xii—K2—O2^xiv	108.52 (2)	O2—Si1—K2^xxi	63.60 (3)
O1—K2—O2^xiv	108.52 (2)	K1^vii—Si1—K2^xxi	116.40 (3)
O2^xiii—K2—O2^xiv	120.0	K1—Si1—K2^xxi	68.555 (17)
O2—K2—O2^xiv	120.0	K1^xix—Si1—K2^xxi	163.40 (6)
O1^ix—K2—Yb1	140.57 (6)	K1^xx—Si1—K2^xxi	68.556 (17)
O1^iv—K2—Yb1	39.43 (6)	K2^xx—Si1—K2^xxi	101.74 (3)
O1^x—K2—Yb1	39.43 (6)	O1^v—Si1—K2	124.38 (4)
O1^xi—K2—Yb1	140.57 (6)	O1—Si1—K2	44.66 (10)
O1^xii—K2—Yb1	140.57 (6)	O1^xviii—Si1—K2	124.38 (4)
O1—K2—Yb1	39.43 (6)	O2—Si1—K2	63.60 (3)
O2^xiii—K2—Yb1	90.0	K1^vii—Si1—K2	116.40 (3)
O2—K2—Yb1	90.0	K1—Si1—K2	68.555 (17)
O2^xiv—K2—Yb1	90.0	K1^xix—Si1—K2	68.556 (17)
O1^ix—K2—Yb1^xv	39.43 (6)	K1^xx—Si1—K2	163.40 (6)
O1^iv—K2—Yb1^xv	140.57 (6)	K2^xx—Si1—K2	101.74 (3)
O1^x—K2—Yb1^xv	140.57 (6)	K2^xxi—Si1—K2	101.74 (3)
O1^xi—K2—Yb1^xv	39.43 (6)	Si1—O1—Yb1	161.18 (18)
O1^xii—K2—Yb1^xv	39.43 (6)	Si1—O1—K2	111.17 (14)
O1—K2—Yb1^xv	140.57 (6)	Yb1—O1—K2	87.65 (10)
O2^xiii—K2—Yb1^xv	90.0	Si1—O1—K1	92.57 (6)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.41 (6)
O2^xiv—K2—Yb1^xv	90.0	K2—O1—K1	89.53 (7)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.57 (6)
O1^ix—K2—Si1^xi	86.62 (4)	Yb1—O1—K1^xix	87.41 (6)
O1^iv—K2—Si1^xi	128.89 (2)	K2—O1—K1^xix	89.53 (7)
O1^x—K2—Si1^xi	128.90 (2)	K1—O1—K1^xix	174.77 (12)
O1^xi—K2—Si1^xi	24.16 (6)	Si1—O1—K1^vii	77.73 (13)
O1^xii—K2—Si1^xi	86.62 (4)	Yb1—O1—K1^vii	83.45 (8)
O1—K2—Si1^xi	76.97 (6)	K2—O1—K1^vii	171.10 (11)
O2^xiii—K2—Si1^xi	116.607 (7)	K1—O1—K1^vii	90.07 (7)
O2—K2—Si1^xi	26.40 (3)	K1^xix—O1—K1^vii	90.07 (7)
O2^xiv—K2—Si1^xi	116.606 (7)	Si1^xi—O2—Si1	180.0
Yb1—K2—Si1^xi	116.40 (3)	Si1^xi—O2—K2^xx	90.0
Yb1^xv—K2—Si1^xi	63.60 (3)	Si1—O2—K2^xx	90.0
O1^xvi—Yb1—O1^iv	180.00 (11)	Si1^xi—O2—K2	90.0
O1^xvi—Yb1—O1	92.60 (10)	Si1—O2—K2	90.0
O1^iv—Yb1—O1	87.40 (10)	K2^xx—O2—K2	120.0
O1^xvi—Yb1—O1^xvii	87.40 (10)	Si1^xi—O2—K2^xxi	90.0
O1^iv—Yb1—O1^xvii	92.60 (10)	Si1—O2—K2^xxi	90.0
O1—Yb1—O1^xvii	180.00 (11)	K2^xx—O2—K2^xxi	120.0
O1^xvi—Yb1—O1^vi	87.40 (10)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) −x+y, −x+1, z; (ii) x, y+1, z; (iii) −y+1, x−y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) x−y, x, −z; (vii) −x+1, −y+1, −z; (viii) y, −x+y+1, −z; (ix) −y, x−y, −z+1/2; (x) −x+y, −x, z; (xi) x, y, −z+1/2; (xii) −x+y, −x, −z+1/2; (xiii) x−1, y−1, z; (xiv) x−1, y, z; (xv) −x, −y, z+1/2; (xvi) y, −x+y, −z; (xvii) −x, −y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(253_K)

Crystal data

K3O7Si2Yb	Dx = 3.863 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1139 reflections
a = 5.7173 (4) Å	θ = 4.1–29.9°
c = 13.9234 (12) Å	µ = 13.75 mm^−1
V = 394.15 (6) Å^3	T = 253 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	191 reflections with I > 2σ(I)
ω scans	Rint = 0.047
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 28.3°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −7→7
2550 measured reflections	k = −7→7
223 independent reflections	l = −16→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0096P)^2 + 0.918P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.016	(Δ/σ)max < 0.001
wR(F^2) = 0.035	Δρmax = 0.51 e Å^−3
S = 1.15	Δρmin = −0.57 e Å^−3
223 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0143 (9)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09162 (13)	0.0115 (4)
K2	0.000000	0.000000	0.250000	0.0148 (5)
Yb1	0.000000	0.000000	0.000000	0.00413 (19)
Si1	0.666667	0.333333	0.13206 (15)	0.0040 (4)
O1	0.3571 (6)	0.1785 (3)	0.0957 (2)	0.0106 (6)
O2	0.666667	0.333333	0.250000	0.0185 (19)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0104 (5)	0.0104 (5)	0.0135 (8)	0.0052 (3)	0.000	0.000
K2	0.0193 (8)	0.0193 (8)	0.0057 (10)	0.0097 (4)	0.000	0.000
Yb1	0.0039 (2)	0.0039 (2)	0.0046 (3)	0.00194 (10)	0.000	0.000
Si1	0.0042 (6)	0.0042 (6)	0.0038 (8)	0.0021 (3)	0.000	0.000
O1	0.0082 (16)	0.0102 (11)	0.0128 (14)	0.0041 (8)	−0.0030 (14)	−0.0015 (7)
O2	0.027 (3)	0.027 (3)	0.002 (3)	0.0135 (15)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8616 (2)	K2—O1	2.783 (3)
K1—O1^ii	2.8616 (2)	K2—O2^xiv	3.3009 (2)
K1—O1^iii	2.8616 (2)	K2—O2	3.3009 (2)
K1—O1^iv	2.8616 (2)	K2—O2^ix	3.3009 (2)
K1—O1	2.8616 (2)	K2—Yb1	3.4808 (3)
K1—O1^v	2.8616 (2)	K2—Yb1^xv	3.4808 (3)
K1—O1^vi	3.025 (3)	K2—Si1^xi	3.6868 (9)
K1—O1^vii	3.025 (3)	Yb1—O1	2.214 (3)
K1—O1^viii	3.025 (3)	Yb1—O1^xvi	2.214 (3)
K1—Si1^viii	3.114 (3)	Yb1—O1^xvii	2.214 (3)
K1—Si1^i	3.3486 (5)	Yb1—O1^iv	2.214 (3)
K1—Si1^ix	3.3486 (5)	Yb1—O1^vii	2.214 (3)
K2—O1^x	2.783 (3)	Yb1—O1^x	2.214 (3)
K2—O1^xi	2.783 (3)	Si1—O1^xviii	1.614 (3)
K2—O1^xii	2.783 (3)	Si1—O1^v	1.614 (3)
K2—O1^iv	2.783 (3)	Si1—O1	1.614 (3)
K2—O1^xiii	2.783 (3)	Si1—O2	1.642 (2)
O1^i—K1—O1^ii	64.70 (12)	O1^xvi—Yb1—O1^vii	87.53 (11)
O1^i—K1—O1^iii	55.28 (12)	O1^xvii—Yb1—O1^vii	87.53 (11)
O1^ii—K1—O1^iii	119.961 (5)	O1^iv—Yb1—O1^vii	92.47 (11)
O1^i—K1—O1^iv	119.961 (5)	O1—Yb1—O1^x	87.53 (11)
O1^ii—K1—O1^iv	55.28 (12)	O1^xvi—Yb1—O1^x	92.47 (11)
O1^iii—K1—O1^iv	174.77 (12)	O1^xvii—Yb1—O1^x	92.47 (11)
O1^i—K1—O1	174.77 (13)	O1^iv—Yb1—O1^x	87.53 (11)
O1^ii—K1—O1	119.961 (5)	O1^vii—Yb1—O1^x	180.00 (17)
O1^iii—K1—O1	119.962 (5)	O1—Yb1—K2	53.01 (8)
O1^iv—K1—O1	64.70 (12)	O1^xvi—Yb1—K2	127.00 (8)
O1^i—K1—O1^v	119.961 (5)	O1^xvii—Yb1—K2	127.00 (8)
O1^ii—K1—O1^v	174.77 (12)	O1^iv—Yb1—K2	53.00 (8)
O1^iii—K1—O1^v	64.70 (12)	O1^vii—Yb1—K2	127.00 (8)
O1^iv—K1—O1^v	119.961 (5)	O1^x—Yb1—K2	53.00 (8)
O1—K1—O1^v	55.28 (12)	O1—Yb1—K2^xvi	126.99 (8)
O1^i—K1—O1^vi	65.73 (10)	O1^xvi—Yb1—K2^xvi	53.00 (8)
O1^ii—K1—O1^vi	65.73 (10)	O1^xvii—Yb1—K2^xvi	53.00 (8)
O1^iii—K1—O1^vi	89.78 (7)	O1^iv—Yb1—K2^xvi	127.00 (8)
O1^iv—K1—O1^vi	89.78 (7)	O1^vii—Yb1—K2^xvi	53.00 (8)
O1—K1—O1^vi	117.76 (7)	O1^x—Yb1—K2^xvi	127.00 (8)
O1^v—K1—O1^vi	117.76 (7)	K2—Yb1—K2^xvi	180.0
O1^i—K1—O1^vii	117.76 (7)	O1—Yb1—K1^xvi	126.115 (14)
O1^ii—K1—O1^vii	89.78 (7)	O1^xvi—Yb1—K1^xvi	53.885 (14)
O1^iii—K1—O1^vii	117.76 (7)	O1^xvii—Yb1—K1^xvi	53.886 (14)
O1^iv—K1—O1^vii	65.73 (10)	O1^iv—Yb1—K1^xvi	126.114 (14)
O1—K1—O1^vii	65.73 (10)	O1^vii—Yb1—K1^xvi	121.88 (8)
O1^v—K1—O1^vii	89.78 (7)	O1^x—Yb1—K1^xvi	58.12 (8)
O1^vi—K1—O1^vii	52.06 (10)	K2—Yb1—K1^xvi	111.13 (3)
O1^i—K1—O1^viii	89.78 (7)	K2^xvi—Yb1—K1^xvi	68.87 (3)
O1^ii—K1—O1^viii	117.76 (7)	O1—Yb1—K1^viii	58.12 (8)
O1^iii—K1—O1^viii	65.73 (10)	O1^xvi—Yb1—K1^viii	121.88 (8)
O1^iv—K1—O1^viii	117.76 (7)	O1^xvii—Yb1—K1^viii	53.886 (14)
O1—K1—O1^viii	89.78 (7)	O1^iv—Yb1—K1^viii	126.114 (14)
O1^v—K1—O1^viii	65.73 (10)	O1^vii—Yb1—K1^viii	53.885 (14)
O1^vi—K1—O1^viii	52.06 (10)	O1^x—Yb1—K1^viii	126.115 (14)
O1^vii—K1—O1^viii	52.06 (10)	K2—Yb1—K1^viii	111.13 (3)
O1^i—K1—Si1^viii	91.13 (7)	K2^xvi—Yb1—K1^viii	68.87 (3)
O1^ii—K1—Si1^viii	91.13 (7)	K1^xvi—Yb1—K1^viii	107.77 (3)
O1^iii—K1—Si1^viii	91.13 (7)	O1—Yb1—K1^xiv	121.88 (8)
O1^iv—K1—Si1^viii	91.13 (7)	O1^xvi—Yb1—K1^xiv	58.12 (8)
O1—K1—Si1^viii	91.13 (7)	O1^xvii—Yb1—K1^xiv	126.114 (14)
O1^v—K1—Si1^viii	91.13 (7)	O1^iv—Yb1—K1^xiv	53.886 (14)
O1^vi—K1—Si1^viii	30.45 (6)	O1^vii—Yb1—K1^xiv	126.115 (14)
O1^vii—K1—Si1^viii	30.45 (6)	O1^x—Yb1—K1^xiv	53.885 (14)
O1^viii—K1—Si1^viii	30.45 (6)	K2—Yb1—K1^xiv	68.87 (3)
O1^i—K1—Si1^i	28.79 (6)	K2^xvi—Yb1—K1^xiv	111.13 (3)
O1^ii—K1—Si1^i	92.13 (6)	K1^xvi—Yb1—K1^xiv	72.23 (3)
O1^iii—K1—Si1^i	28.79 (6)	K1^viii—Yb1—K1^xiv	180.00 (5)
O1^iv—K1—Si1^i	146.02 (6)	O1—Yb1—K1	53.885 (14)
O1—K1—Si1^i	146.02 (6)	O1^xvi—Yb1—K1	126.115 (14)
O1^v—K1—Si1^i	92.13 (6)	O1^xvii—Yb1—K1	126.115 (14)
O1^vi—K1—Si1^i	83.98 (4)	O1^iv—Yb1—K1	53.885 (14)
O1^vii—K1—Si1^i	130.13 (8)	O1^vii—Yb1—K1	58.12 (8)
O1^viii—K1—Si1^i	83.98 (4)	O1^x—Yb1—K1	121.88 (8)
Si1^viii—K1—Si1^i	99.68 (4)	K2—Yb1—K1	68.87 (3)
O1^i—K1—Si1^ix	92.13 (6)	K2^xvi—Yb1—K1	111.13 (3)
O1^ii—K1—Si1^ix	28.79 (6)	K1^xvi—Yb1—K1	180.0
O1^iii—K1—Si1^ix	146.02 (6)	K1^viii—Yb1—K1	72.24 (3)
O1^iv—K1—Si1^ix	28.79 (6)	K1^xiv—Yb1—K1	107.76 (3)
O1—K1—Si1^ix	92.13 (6)	O1^xviii—Si1—O1^v	110.63 (12)
O1^v—K1—Si1^ix	146.02 (6)	O1^xviii—Si1—O1	110.63 (12)
O1^vi—K1—Si1^ix	83.98 (4)	O1^v—Si1—O1	110.63 (12)
O1^vii—K1—Si1^ix	83.98 (4)	O1^xviii—Si1—O2	108.29 (13)
O1^viii—K1—Si1^ix	130.13 (8)	O1^v—Si1—O2	108.29 (13)
Si1^viii—K1—Si1^ix	99.68 (4)	O1—Si1—O2	108.29 (13)
Si1^i—K1—Si1^ix	117.23 (2)	O1^xviii—Si1—K1^viii	71.71 (13)
O1^x—K2—O1^xi	142.95 (5)	O1^v—Si1—K1^viii	71.71 (13)
O1^x—K2—O1^xii	142.95 (5)	O1—Si1—K1^viii	71.71 (13)
O1^xi—K2—O1^xii	66.77 (10)	O2—Si1—K1^viii	180.0
O1^x—K2—O1^iv	66.77 (10)	O1^xviii—Si1—K1	152.03 (15)
O1^xi—K2—O1^iv	142.95 (5)	O1^v—Si1—K1	58.617 (12)
O1^xii—K2—O1^iv	101.10 (12)	O1—Si1—K1	58.617 (12)
O1^x—K2—O1^xiii	101.10 (12)	O2—Si1—K1	99.68 (4)
O1^xi—K2—O1^xiii	66.77 (10)	K1^viii—Si1—K1	80.32 (4)
O1^xii—K2—O1^xiii	66.77 (10)	O1^xviii—Si1—K1^xix	58.617 (12)
O1^iv—K2—O1^xiii	142.95 (5)	O1^v—Si1—K1^xix	152.03 (15)
O1^x—K2—O1	66.77 (10)	O1—Si1—K1^xix	58.617 (12)
O1^xi—K2—O1	101.10 (12)	O2—Si1—K1^xix	99.68 (4)
O1^xii—K2—O1	142.95 (5)	K1^viii—Si1—K1^xix	80.32 (4)
O1^iv—K2—O1	66.77 (10)	K1—Si1—K1^xix	117.23 (2)
O1^xiii—K2—O1	142.95 (5)	O1^xviii—Si1—K1^xx	58.617 (12)
O1^x—K2—O2^xiv	50.55 (6)	O1^v—Si1—K1^xx	58.617 (12)
O1^xi—K2—O2^xiv	108.52 (2)	O1—Si1—K1^xx	152.03 (15)
O1^xii—K2—O2^xiv	108.52 (2)	O2—Si1—K1^xx	99.68 (4)
O1^iv—K2—O2^xiv	108.52 (2)	K1^viii—Si1—K1^xx	80.32 (4)
O1^xiii—K2—O2^xiv	50.55 (6)	K1—Si1—K1^xx	117.23 (2)
O1—K2—O2^xiv	108.52 (2)	K1^xix—Si1—K1^xx	117.23 (2)
O1^x—K2—O2	108.52 (2)	O1^xviii—Si1—K2^xx	44.74 (11)
O1^xi—K2—O2	50.55 (6)	O1^v—Si1—K2^xx	124.39 (4)
O1^xii—K2—O2	108.52 (2)	O1—Si1—K2^xx	124.39 (4)
O1^iv—K2—O2	108.52 (2)	O2—Si1—K2^xx	63.55 (3)
O1^xiii—K2—O2	108.52 (2)	K1^viii—Si1—K2^xx	116.45 (3)
O1—K2—O2	50.55 (6)	K1—Si1—K2^xx	163.23 (6)
O2^xiv—K2—O2	120.0	K1^xix—Si1—K2^xx	68.507 (17)
O1^x—K2—O2^ix	108.52 (2)	K1^xx—Si1—K2^xx	68.507 (17)
O1^xi—K2—O2^ix	108.52 (2)	O1^xviii—Si1—K2^xxi	124.39 (4)
O1^xii—K2—O2^ix	50.55 (6)	O1^v—Si1—K2^xxi	44.74 (11)
O1^iv—K2—O2^ix	50.55 (6)	O1—Si1—K2^xxi	124.39 (4)
O1^xiii—K2—O2^ix	108.52 (2)	O2—Si1—K2^xxi	63.55 (3)
O1—K2—O2^ix	108.52 (2)	K1^viii—Si1—K2^xxi	116.45 (3)
O2^xiv—K2—O2^ix	120.0	K1—Si1—K2^xxi	68.507 (17)
O2—K2—O2^ix	120.0	K1^xix—Si1—K2^xxi	163.23 (6)
O1^x—K2—Yb1	39.45 (6)	K1^xx—Si1—K2^xxi	68.508 (17)
O1^xi—K2—Yb1	140.55 (6)	K2^xx—Si1—K2^xxi	101.68 (3)
O1^xii—K2—Yb1	140.55 (6)	O1^xviii—Si1—K2	124.39 (4)
O1^iv—K2—Yb1	39.45 (6)	O1^v—Si1—K2	124.39 (4)
O1^xiii—K2—Yb1	140.55 (6)	O1—Si1—K2	44.74 (11)
O1—K2—Yb1	39.45 (6)	O2—Si1—K2	63.55 (3)
O2^xiv—K2—Yb1	90.0	K1^viii—Si1—K2	116.45 (3)
O2—K2—Yb1	90.0	K1—Si1—K2	68.507 (17)
O2^ix—K2—Yb1	90.0	K1^xix—Si1—K2	68.508 (17)
O1^x—K2—Yb1^xv	140.55 (6)	K1^xx—Si1—K2	163.23 (6)
O1^xi—K2—Yb1^xv	39.45 (6)	K2^xx—Si1—K2	101.68 (3)
O1^xii—K2—Yb1^xv	39.45 (6)	K2^xxi—Si1—K2	101.68 (3)
O1^iv—K2—Yb1^xv	140.55 (6)	Si1—O1—Yb1	161.30 (19)
O1^xiii—K2—Yb1^xv	39.45 (6)	Si1—O1—K2	111.16 (15)
O1—K2—Yb1^xv	140.55 (6)	Yb1—O1—K2	87.55 (10)
O2^xiv—K2—Yb1^xv	90.0	Si1—O1—K1	92.59 (6)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.44 (6)
O2^ix—K2—Yb1^xv	90.0	K2—O1—K1	89.38 (7)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.59 (6)
O1^x—K2—Si1^xi	128.93 (2)	Yb1—O1—K1^xix	87.44 (6)
O1^xi—K2—Si1^xi	24.10 (7)	K2—O1—K1^xix	89.38 (7)
O1^xii—K2—Si1^xi	86.59 (5)	K1—O1—K1^xix	174.78 (12)
O1^iv—K2—Si1^xi	128.93 (2)	Si1—O1—K1^viii	77.84 (14)
O1^xiii—K2—Si1^xi	86.59 (5)	Yb1—O1—K1^viii	83.45 (8)
O1—K2—Si1^xi	77.00 (7)	K2—O1—K1^viii	171.00 (12)
O2^xiv—K2—Si1^xi	116.594 (7)	K1—O1—K1^viii	90.22 (7)
O2—K2—Si1^xi	26.45 (3)	K1^xix—O1—K1^viii	90.22 (7)
O2^ix—K2—Si1^xi	116.593 (7)	Si1—O2—Si1^xi	180.0
Yb1—K2—Si1^xi	116.45 (3)	Si1—O2—K2^xx	90.0
Yb1^xv—K2—Si1^xi	63.55 (3)	Si1^xi—O2—K2^xx	90.0
O1—Yb1—O1^xvi	180.0	Si1—O2—K2	90.0
O1—Yb1—O1^xvii	92.47 (11)	Si1^xi—O2—K2	90.0
O1^xvi—Yb1—O1^xvii	87.53 (11)	K2^xx—O2—K2	120.0
O1—Yb1—O1^iv	87.53 (11)	Si1—O2—K2^xxi	90.0
O1^xvi—Yb1—O1^iv	92.47 (11)	Si1^xi—O2—K2^xxi	90.0
O1^xvii—Yb1—O1^iv	180.00 (13)	K2^xx—O2—K2^xxi	120.0
O1—Yb1—O1^vii	92.47 (11)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) x, y+1, z; (ii) −x+y, −x+1, z; (iii) −y+1, x−y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) y, −x+y+1, −z; (vii) x−y, x, −z; (viii) −x+1, −y+1, −z; (ix) x−1, y, z; (x) −x+y, −x, z; (xi) x, y, −z+1/2; (xii) −y, x−y, −z+1/2; (xiii) −x+y, −x, −z+1/2; (xiv) x−1, y−1, z; (xv) −x, −y, z+1/2; (xvi) −x, −y, −z; (xvii) y, −x+y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(263_K)

Crystal data

K3O7Si2Yb	Dx = 3.848 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1127 reflections
a = 5.7236 (6) Å	θ = 4.3–29.6°
c = 13.9498 (16) Å	µ = 13.69 mm^−1
V = 395.76 (9) Å^3	T = 263 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	187 reflections with I > 2σ(I)
ω scans	Rint = 0.048
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −6→7
2517 measured reflections	k = −7→5
211 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0057P)^2 + 1.0462P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.015	(Δ/σ)max < 0.001
wR(F^2) = 0.032	Δρmax = 0.50 e Å^−3
S = 1.16	Δρmin = −0.45 e Å^−3
211 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0145 (8)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09150 (13)	0.0114 (4)
K2	0.000000	0.000000	0.250000	0.0147 (5)
Yb1	0.000000	0.000000	0.000000	0.00415 (19)
Si1	0.666667	0.333333	0.13215 (15)	0.0040 (4)
O1	0.3564 (6)	0.1782 (3)	0.0956 (2)	0.0113 (7)
O2	0.666667	0.333333	0.250000	0.0188 (19)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0099 (5)	0.0099 (5)	0.0146 (8)	0.0049 (3)	0.000	0.000
K2	0.0190 (8)	0.0190 (8)	0.0060 (11)	0.0095 (4)	0.000	0.000
Yb1	0.0038 (2)	0.0038 (2)	0.0049 (3)	0.00190 (10)	0.000	0.000
Si1	0.0036 (6)	0.0036 (6)	0.0048 (9)	0.0018 (3)	0.000	0.000
O1	0.0078 (16)	0.0114 (12)	0.0135 (14)	0.0039 (8)	−0.0025 (15)	−0.0013 (7)
O2	0.027 (3)	0.027 (3)	0.003 (4)	0.0133 (15)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8646 (3)	K2—O1	2.785 (3)
K1—O1^ii	2.8647 (3)	K2—O2^xiii	3.3045 (3)
K1—O1^iii	2.8647 (3)	K2—O2	3.3045 (4)
K1—O1	2.8647 (3)	K2—O2^xiv	3.3045 (4)
K1—O1^iv	2.8647 (3)	K2—Yb1	3.4874 (4)
K1—O1^v	2.8647 (3)	K2—Yb1^xv	3.4874 (4)
K1—O1^vi	3.030 (3)	K2—Si1^x	3.6908 (10)
K1—O1^vii	3.030 (3)	Yb1—O1	2.214 (3)
K1—O1^viii	3.030 (3)	Yb1—O1^xvi	2.214 (3)
K1—Si1^viii	3.120 (3)	Yb1—O1^vii	2.214 (3)
K1—Si1	3.3528 (5)	Yb1—O1^ix	2.214 (3)
K1—Si1^iv	3.3528 (5)	Yb1—O1^xvii	2.214 (3)
K2—O1^ix	2.785 (3)	Yb1—O1^iii	2.214 (3)
K2—O1^x	2.785 (3)	Si1—O1^xviii	1.620 (3)
K2—O1^xi	2.785 (3)	Si1—O1	1.620 (3)
K2—O1^xii	2.785 (3)	Si1—O1^i	1.620 (3)
K2—O1^iii	2.785 (3)	Si1—O2	1.644 (2)
O1^i—K1—O1^ii	64.56 (13)	O1^xvi—Yb1—O1^xvii	87.43 (11)
O1^i—K1—O1^iii	119.960 (5)	O1^vii—Yb1—O1^xvii	87.43 (11)
O1^ii—K1—O1^iii	174.88 (13)	O1^ix—Yb1—O1^xvii	92.57 (11)
O1^i—K1—O1	55.42 (13)	O1—Yb1—O1^iii	87.43 (11)
O1^ii—K1—O1	119.960 (5)	O1^xvi—Yb1—O1^iii	92.57 (11)
O1^iii—K1—O1	64.56 (13)	O1^vii—Yb1—O1^iii	92.57 (11)
O1^i—K1—O1^iv	119.960 (5)	O1^ix—Yb1—O1^iii	87.43 (11)
O1^ii—K1—O1^iv	55.42 (13)	O1^xvii—Yb1—O1^iii	180.00 (12)
O1^iii—K1—O1^iv	119.959 (5)	O1—Yb1—K2	52.94 (8)
O1—K1—O1^iv	174.88 (13)	O1^xvi—Yb1—K2	127.07 (8)
O1^i—K1—O1^v	174.88 (13)	O1^vii—Yb1—K2	127.07 (8)
O1^ii—K1—O1^v	119.959 (5)	O1^ix—Yb1—K2	52.93 (8)
O1^iii—K1—O1^v	55.42 (13)	O1^xvii—Yb1—K2	127.06 (8)
O1—K1—O1^v	119.960 (5)	O1^iii—Yb1—K2	52.94 (8)
O1^iv—K1—O1^v	64.56 (13)	O1—Yb1—K2^xvi	127.06 (8)
O1^i—K1—O1^vi	117.82 (7)	O1^xvi—Yb1—K2^xvi	52.93 (8)
O1^ii—K1—O1^vi	89.84 (7)	O1^vii—Yb1—K2^xvi	52.93 (8)
O1^iii—K1—O1^vi	89.84 (7)	O1^ix—Yb1—K2^xvi	127.07 (8)
O1—K1—O1^vi	117.82 (7)	O1^xvii—Yb1—K2^xvi	52.94 (8)
O1^iv—K1—O1^vi	65.69 (10)	O1^iii—Yb1—K2^xvi	127.06 (8)
O1^v—K1—O1^vi	65.69 (10)	K2—Yb1—K2^xvi	180.0
O1^i—K1—O1^vii	89.84 (7)	O1—Yb1—K1	53.889 (14)
O1^ii—K1—O1^vii	117.82 (7)	O1^xvi—Yb1—K1	126.112 (14)
O1^iii—K1—O1^vii	65.69 (10)	O1^vii—Yb1—K1	58.19 (8)
O1—K1—O1^vii	65.69 (10)	O1^ix—Yb1—K1	121.81 (8)
O1^iv—K1—O1^vii	117.82 (7)	O1^xvii—Yb1—K1	126.111 (14)
O1^v—K1—O1^vii	89.84 (7)	O1^iii—Yb1—K1	53.889 (14)
O1^vi—K1—O1^vii	52.15 (10)	K2—Yb1—K1	68.88 (3)
O1^i—K1—O1^viii	65.69 (10)	K2^xvi—Yb1—K1	111.12 (3)
O1^ii—K1—O1^viii	65.69 (10)	O1—Yb1—K1^xvi	126.112 (14)
O1^iii—K1—O1^viii	117.82 (7)	O1^xvi—Yb1—K1^xvi	53.888 (14)
O1—K1—O1^viii	89.84 (7)	O1^vii—Yb1—K1^xvi	121.81 (8)
O1^iv—K1—O1^viii	89.84 (7)	O1^ix—Yb1—K1^xvi	58.19 (8)
O1^v—K1—O1^viii	117.82 (7)	O1^xvii—Yb1—K1^xvi	53.889 (14)
O1^vi—K1—O1^viii	52.15 (10)	O1^iii—Yb1—K1^xvi	126.111 (14)
O1^vii—K1—O1^viii	52.15 (10)	K2—Yb1—K1^xvi	111.12 (3)
O1^i—K1—Si1^viii	91.16 (7)	K2^xvi—Yb1—K1^xvi	68.88 (3)
O1^ii—K1—Si1^viii	91.16 (7)	K1—Yb1—K1^xvi	180.0
O1^iii—K1—Si1^viii	91.16 (7)	O1—Yb1—K1^viii	58.19 (8)
O1—K1—Si1^viii	91.16 (7)	O1^xvi—Yb1—K1^viii	121.81 (8)
O1^iv—K1—Si1^viii	91.16 (7)	O1^vii—Yb1—K1^viii	53.888 (14)
O1^v—K1—Si1^viii	91.16 (7)	O1^ix—Yb1—K1^viii	126.112 (14)
O1^vi—K1—Si1^viii	30.50 (6)	O1^xvii—Yb1—K1^viii	53.889 (14)
O1^vii—K1—Si1^viii	30.50 (6)	O1^iii—Yb1—K1^viii	126.111 (14)
O1^viii—K1—Si1^viii	30.50 (6)	K2—Yb1—K1^viii	111.12 (3)
O1^i—K1—Si1	28.86 (6)	K2^xvi—Yb1—K1^viii	68.88 (3)
O1^ii—K1—Si1	92.06 (6)	K1—Yb1—K1^viii	72.23 (3)
O1^iii—K1—Si1	92.06 (6)	K1^xvi—Yb1—K1^viii	107.77 (3)
O1—K1—Si1	28.86 (6)	O1—Yb1—K1^xiii	121.81 (8)
O1^iv—K1—Si1	146.06 (7)	O1^xvi—Yb1—K1^xiii	58.19 (8)
O1^v—K1—Si1	146.06 (7)	O1^vii—Yb1—K1^xiii	126.112 (14)
O1^vi—K1—Si1	130.24 (8)	O1^ix—Yb1—K1^xiii	53.888 (14)
O1^vii—K1—Si1	84.01 (5)	O1^xvii—Yb1—K1^xiii	126.111 (14)
O1^viii—K1—Si1	84.01 (5)	O1^iii—Yb1—K1^xiii	53.889 (14)
Si1^viii—K1—Si1	99.74 (4)	K2—Yb1—K1^xiii	68.88 (3)
O1^i—K1—Si1^iv	92.06 (6)	K2^xvi—Yb1—K1^xiii	111.12 (3)
O1^ii—K1—Si1^iv	28.86 (6)	K1—Yb1—K1^xiii	107.77 (3)
O1^iii—K1—Si1^iv	146.06 (7)	K1^xvi—Yb1—K1^xiii	72.23 (3)
O1—K1—Si1^iv	146.06 (7)	K1^viii—Yb1—K1^xiii	180.0
O1^iv—K1—Si1^iv	28.86 (6)	O1^xviii—Si1—O1	110.60 (12)
O1^v—K1—Si1^iv	92.06 (6)	O1^xviii—Si1—O1^i	110.60 (12)
O1^vi—K1—Si1^iv	84.01 (5)	O1—Si1—O1^i	110.60 (12)
O1^vii—K1—Si1^iv	130.24 (8)	O1^xviii—Si1—O2	108.32 (13)
O1^viii—K1—Si1^iv	84.01 (5)	O1—Si1—O2	108.32 (13)
Si1^viii—K1—Si1^iv	99.74 (4)	O1^i—Si1—O2	108.32 (13)
Si1—K1—Si1^iv	117.20 (2)	O1^xviii—Si1—K1^viii	71.68 (13)
O1^ix—K2—O1^x	143.02 (5)	O1—Si1—K1^viii	71.68 (13)
O1^ix—K2—O1^xi	101.27 (12)	O1^i—Si1—K1^viii	71.68 (13)
O1^x—K2—O1^xi	66.64 (10)	O2—Si1—K1^viii	180.0
O1^ix—K2—O1^xii	143.02 (5)	O1^xviii—Si1—K1^xix	58.602 (12)
O1^x—K2—O1^xii	66.64 (10)	O1—Si1—K1^xix	58.602 (12)
O1^xi—K2—O1^xii	66.64 (10)	O1^i—Si1—K1^xix	151.94 (15)
O1^ix—K2—O1^iii	66.64 (10)	O2—Si1—K1^xix	99.74 (4)
O1^x—K2—O1^iii	143.02 (5)	K1^viii—Si1—K1^xix	80.26 (4)
O1^xi—K2—O1^iii	143.02 (5)	O1^xviii—Si1—K1^xx	58.602 (12)
O1^xii—K2—O1^iii	101.27 (12)	O1—Si1—K1^xx	151.94 (15)
O1^ix—K2—O1	66.64 (10)	O1^i—Si1—K1^xx	58.603 (12)
O1^x—K2—O1	101.27 (12)	O2—Si1—K1^xx	99.74 (4)
O1^xi—K2—O1	143.02 (5)	K1^viii—Si1—K1^xx	80.26 (4)
O1^xii—K2—O1	143.02 (5)	K1^xix—Si1—K1^xx	117.20 (2)
O1^iii—K2—O1	66.64 (10)	O1^xviii—Si1—K1	151.94 (15)
O1^ix—K2—O2^xiii	50.63 (6)	O1—Si1—K1	58.602 (12)
O1^x—K2—O2^xiii	108.49 (3)	O1^i—Si1—K1	58.601 (12)
O1^xi—K2—O2^xiii	50.63 (6)	O2—Si1—K1	99.74 (4)
O1^xii—K2—O2^xiii	108.49 (3)	K1^viii—Si1—K1	80.26 (4)
O1^iii—K2—O2^xiii	108.49 (3)	K1^xix—Si1—K1	117.20 (2)
O1—K2—O2^xiii	108.49 (2)	K1^xx—Si1—K1	117.20 (2)
O1^ix—K2—O2	108.49 (2)	O1^xviii—Si1—K2^xx	44.77 (11)
O1^x—K2—O2	50.63 (6)	O1—Si1—K2^xx	124.40 (4)
O1^xi—K2—O2	108.49 (3)	O1^i—Si1—K2^xx	124.40 (4)
O1^xii—K2—O2	108.49 (3)	O2—Si1—K2^xx	63.55 (3)
O1^iii—K2—O2	108.49 (3)	K1^viii—Si1—K2^xx	116.45 (3)
O1—K2—O2	50.63 (6)	K1^xix—Si1—K2^xx	68.537 (18)
O2^xiii—K2—O2	120.0	K1^xx—Si1—K2^xx	68.537 (18)
O1^ix—K2—O2^xiv	108.49 (3)	K1—Si1—K2^xx	163.29 (7)
O1^x—K2—O2^xiv	108.49 (3)	O1^xviii—Si1—K2^xxi	124.40 (4)
O1^xi—K2—O2^xiv	108.49 (3)	O1—Si1—K2^xxi	124.40 (4)
O1^xii—K2—O2^xiv	50.63 (6)	O1^i—Si1—K2^xxi	44.77 (11)
O1^iii—K2—O2^xiv	50.63 (6)	O2—Si1—K2^xxi	63.55 (3)
O1—K2—O2^xiv	108.49 (3)	K1^viii—Si1—K2^xxi	116.45 (3)
O2^xiii—K2—O2^xiv	120.0	K1^xix—Si1—K2^xxi	163.29 (7)
O2—K2—O2^xiv	120.0	K1^xx—Si1—K2^xxi	68.538 (18)
O1^ix—K2—Yb1	39.37 (6)	K1—Si1—K2^xxi	68.538 (18)
O1^x—K2—Yb1	140.63 (6)	K2^xx—Si1—K2^xxi	101.68 (4)
O1^xi—K2—Yb1	140.63 (6)	O1^xviii—Si1—K2	124.40 (4)
O1^xii—K2—Yb1	140.63 (6)	O1—Si1—K2	44.77 (11)
O1^iii—K2—Yb1	39.37 (6)	O1^i—Si1—K2	124.40 (4)
O1—K2—Yb1	39.37 (6)	O2—Si1—K2	63.55 (3)
O2^xiii—K2—Yb1	90.0	K1^viii—Si1—K2	116.45 (3)
O2—K2—Yb1	90.0	K1^xix—Si1—K2	68.538 (18)
O2^xiv—K2—Yb1	90.0	K1^xx—Si1—K2	163.29 (7)
O1^ix—K2—Yb1^xv	140.63 (6)	K1—Si1—K2	68.538 (18)
O1^x—K2—Yb1^xv	39.37 (6)	K2^xx—Si1—K2	101.68 (3)
O1^xi—K2—Yb1^xv	39.37 (6)	K2^xxi—Si1—K2	101.68 (3)
O1^xii—K2—Yb1^xv	39.37 (6)	Si1—O1—Yb1	161.3 (2)
O1^iii—K2—Yb1^xv	140.63 (6)	Si1—O1—K2	111.05 (15)
O1—K2—Yb1^xv	140.63 (6)	Yb1—O1—K2	87.70 (10)
O2^xiii—K2—Yb1^xv	90.0	Si1—O1—K1	92.53 (6)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.48 (6)
O2^xiv—K2—Yb1^xv	90.0	K2—O1—K1	89.44 (7)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.53 (6)
O1^ix—K2—Si1^x	128.92 (2)	Yb1—O1—K1^xix	87.48 (6)
O1^x—K2—Si1^x	24.18 (7)	K2—O1—K1^xix	89.44 (7)
O1^xi—K2—Si1^x	86.54 (5)	K1—O1—K1^xix	174.88 (13)
O1^xii—K2—Si1^x	86.54 (5)	Si1—O1—K1^viii	77.82 (14)
O1^iii—K2—Si1^x	128.92 (2)	Yb1—O1—K1^viii	83.44 (9)
O1—K2—Si1^x	77.08 (7)	K2—O1—K1^viii	171.14 (12)
O2^xiii—K2—Si1^x	116.595 (7)	K1—O1—K1^viii	90.16 (7)
O2—K2—Si1^x	26.45 (3)	K1^xix—O1—K1^viii	90.16 (7)
O2^xiv—K2—Si1^x	116.594 (7)	Si1^x—O2—Si1	180.0
Yb1—K2—Si1^x	116.45 (3)	Si1^x—O2—K2^xx	90.0
Yb1^xv—K2—Si1^x	63.55 (3)	Si1—O2—K2^xx	90.0
O1—Yb1—O1^xvi	180.0	Si1^x—O2—K2	90.0
O1—Yb1—O1^vii	92.57 (11)	Si1—O2—K2	90.0
O1^xvi—Yb1—O1^vii	87.43 (11)	K2^xx—O2—K2	120.0
O1—Yb1—O1^ix	87.43 (11)	Si1^x—O2—K2^xxi	90.0
O1^xvi—Yb1—O1^ix	92.57 (11)	Si1—O2—K2^xxi	90.0
O1^vii—Yb1—O1^ix	180.00 (18)	K2^xx—O2—K2^xxi	120.0
O1—Yb1—O1^xvii	92.57 (11)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) −x+y+1, −x+1, z; (ii) −y+1, x−y+1, z; (iii) −y, x−y, z; (iv) x, y+1, z; (v) −x+y, −x+1, z; (vi) y, −x+y+1, −z; (vii) x−y, x, −z; (viii) −x+1, −y+1, −z; (ix) −x+y, −x, z; (x) x, y, −z+1/2; (xi) −x+y, −x, −z+1/2; (xii) −y, x−y, −z+1/2; (xiii) x−1, y−1, z; (xiv) x−1, y, z; (xv) −x, −y, z+1/2; (xvi) −x, −y, −z; (xvii) y, −x+y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(273_K)

Crystal data

K3O7Si2Yb	Dx = 3.852 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1117 reflections
a = 5.7212 (6) Å	θ = 7.1–29.8°
c = 13.9445 (16) Å	µ = 13.71 mm^−1
V = 395.28 (9) Å^3	T = 273 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	186 reflections with I > 2σ(I)
ω scans	Rint = 0.049
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.306, Tmax = 0.399	h = −6→7
2517 measured reflections	k = −7→7
210 independent reflections	l = −16→18

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.009P)^2 + 0.593P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.015	(Δ/σ)max < 0.001
wR(F^2) = 0.035	Δρmax = 0.51 e Å^−3
S = 1.23	Δρmin = −0.54 e Å^−3
210 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0152 (9)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09166 (13)	0.0116 (4)
K2	0.000000	0.000000	0.250000	0.0154 (5)
Yb1	0.000000	0.000000	0.000000	0.0042 (2)
Si1	0.666667	0.333333	0.13238 (15)	0.0049 (4)
O1	0.3576 (6)	0.1788 (3)	0.0957 (2)	0.0108 (7)
O2	0.666667	0.333333	0.250000	0.0184 (19)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0097 (5)	0.0097 (5)	0.0153 (8)	0.0049 (3)	0.000	0.000
K2	0.0198 (8)	0.0198 (8)	0.0065 (11)	0.0099 (4)	0.000	0.000
Yb1	0.0039 (2)	0.0039 (2)	0.0048 (3)	0.00195 (11)	0.000	0.000
Si1	0.0053 (6)	0.0053 (6)	0.0041 (9)	0.0027 (3)	0.000	0.000
O1	0.0080 (16)	0.0109 (12)	0.0126 (14)	0.0040 (8)	−0.0037 (15)	−0.0018 (7)
O2	0.025 (3)	0.025 (3)	0.005 (4)	0.0126 (15)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8636 (3)	K2—O1^xii	2.788 (3)
K1—O1^ii	2.8636 (3)	K2—O2^xiii	3.3031 (3)
K1—O1^iii	2.8637 (3)	K2—O2	3.3031 (3)
K1—O1^iv	2.8637 (3)	K2—O2^xiv	3.3032 (3)
K1—O1	2.8637 (3)	K2—Yb1	3.4861 (4)
K1—O1^v	2.8637 (3)	K2—Yb1^xv	3.4861 (4)
K1—O1^vi	3.028 (3)	K2—Si1^xi	3.6879 (10)
K1—O1^vii	3.028 (3)	Yb1—O1^xvi	2.218 (3)
K1—O1^viii	3.028 (3)	Yb1—O1^iv	2.218 (3)
K1—Si1^vii	3.124 (3)	Yb1—O1^xvii	2.218 (3)
K1—Si1^ii	3.3516 (6)	Yb1—O1^vi	2.218 (3)
K1—Si1	3.3516 (6)	Yb1—O1^x	2.218 (3)
K2—O1	2.788 (3)	Yb1—O1	2.218 (3)
K2—O1^ix	2.788 (3)	Si1—O1	1.615 (3)
K2—O1^iv	2.788 (3)	Si1—O1^v	1.615 (3)
K2—O1^x	2.788 (3)	Si1—O1^xviii	1.615 (3)
K2—O1^xi	2.788 (3)	Si1—O2	1.640 (2)
O1^i—K1—O1^ii	64.80 (13)	O1^iv—Yb1—O1^x	87.56 (11)
O1^i—K1—O1^iii	119.963 (5)	O1^xvii—Yb1—O1^x	92.44 (11)
O1^ii—K1—O1^iii	55.18 (13)	O1^vi—Yb1—O1^x	180.00 (18)
O1^i—K1—O1^iv	55.18 (13)	O1^xvi—Yb1—O1	92.44 (11)
O1^ii—K1—O1^iv	119.963 (5)	O1^iv—Yb1—O1	87.56 (11)
O1^iii—K1—O1^iv	174.70 (13)	O1^xvii—Yb1—O1	180.0
O1^i—K1—O1	119.962 (5)	O1^vi—Yb1—O1	92.44 (11)
O1^ii—K1—O1	174.70 (13)	O1^x—Yb1—O1	87.56 (11)
O1^iii—K1—O1	119.962 (5)	O1^xvi—Yb1—K2	126.97 (8)
O1^iv—K1—O1	64.80 (13)	O1^iv—Yb1—K2	53.03 (8)
O1^i—K1—O1^v	174.70 (13)	O1^xvii—Yb1—K2	126.97 (8)
O1^ii—K1—O1^v	119.963 (5)	O1^vi—Yb1—K2	126.97 (8)
O1^iii—K1—O1^v	64.80 (13)	O1^x—Yb1—K2	53.03 (8)
O1^iv—K1—O1^v	119.962 (5)	O1—Yb1—K2	53.03 (8)
O1—K1—O1^v	55.18 (13)	O1^xvi—Yb1—K2^xvii	53.03 (8)
O1^i—K1—O1^vi	89.74 (7)	O1^iv—Yb1—K2^xvii	126.97 (8)
O1^ii—K1—O1^vi	117.70 (7)	O1^xvii—Yb1—K2^xvii	53.03 (8)
O1^iii—K1—O1^vi	117.71 (7)	O1^vi—Yb1—K2^xvii	53.03 (8)
O1^iv—K1—O1^vi	65.78 (10)	O1^x—Yb1—K2^xvii	126.97 (8)
O1—K1—O1^vi	65.79 (10)	O1—Yb1—K2^xvii	126.97 (8)
O1^v—K1—O1^vi	89.74 (7)	K2—Yb1—K2^xvii	180.0
O1^i—K1—O1^vii	117.70 (7)	O1^xvi—Yb1—K1^xvii	53.873 (15)
O1^ii—K1—O1^vii	89.74 (7)	O1^iv—Yb1—K1^xvii	126.127 (15)
O1^iii—K1—O1^vii	65.78 (10)	O1^xvii—Yb1—K1^xvii	53.873 (14)
O1^iv—K1—O1^vii	117.71 (7)	O1^vi—Yb1—K1^xvii	121.87 (8)
O1—K1—O1^vii	89.75 (7)	O1^x—Yb1—K1^xvii	58.13 (8)
O1^v—K1—O1^vii	65.79 (10)	O1—Yb1—K1^xvii	126.128 (15)
O1^vi—K1—O1^vii	51.95 (10)	K2—Yb1—K1^xvii	111.15 (3)
O1^i—K1—O1^viii	65.78 (10)	K2^xvii—Yb1—K1^xvii	68.85 (3)
O1^ii—K1—O1^viii	65.78 (10)	O1^xvi—Yb1—K1^xiii	126.127 (15)
O1^iii—K1—O1^viii	89.74 (7)	O1^iv—Yb1—K1^xiii	53.873 (15)
O1^iv—K1—O1^viii	89.74 (7)	O1^xvii—Yb1—K1^xiii	58.13 (8)
O1—K1—O1^viii	117.71 (7)	O1^vi—Yb1—K1^xiii	126.128 (15)
O1^v—K1—O1^viii	117.71 (7)	O1^x—Yb1—K1^xiii	53.872 (15)
O1^vi—K1—O1^viii	51.95 (10)	O1—Yb1—K1^xiii	121.87 (8)
O1^vii—K1—O1^viii	51.95 (10)	K2—Yb1—K1^xiii	68.85 (3)
O1^i—K1—Si1^vii	91.11 (7)	K2^xvii—Yb1—K1^xiii	111.15 (3)
O1^ii—K1—Si1^vii	91.11 (7)	K1^xvii—Yb1—K1^xiii	72.26 (3)
O1^iii—K1—Si1^vii	91.11 (7)	O1^xvi—Yb1—K1^vii	53.873 (15)
O1^iv—K1—Si1^vii	91.11 (7)	O1^iv—Yb1—K1^vii	126.127 (15)
O1—K1—Si1^vii	91.11 (7)	O1^xvii—Yb1—K1^vii	121.87 (8)
O1^v—K1—Si1^vii	91.11 (7)	O1^vi—Yb1—K1^vii	53.872 (15)
O1^vi—K1—Si1^vii	30.38 (6)	O1^x—Yb1—K1^vii	126.128 (15)
O1^vii—K1—Si1^vii	30.38 (6)	O1—Yb1—K1^vii	58.13 (8)
O1^viii—K1—Si1^vii	30.38 (6)	K2—Yb1—K1^vii	111.15 (3)
O1^i—K1—Si1^ii	92.18 (6)	K2^xvii—Yb1—K1^vii	68.85 (3)
O1^ii—K1—Si1^ii	28.77 (6)	K1^xvii—Yb1—K1^vii	107.74 (3)
O1^iii—K1—Si1^ii	28.77 (6)	K1^xiii—Yb1—K1^vii	180.00 (6)
O1^iv—K1—Si1^ii	145.96 (7)	O1^xvi—Yb1—K1	126.128 (15)
O1—K1—Si1^ii	145.96 (7)	O1^iv—Yb1—K1	53.872 (15)
O1^v—K1—Si1^ii	92.18 (6)	O1^xvii—Yb1—K1	126.127 (14)
O1^vi—K1—Si1^ii	130.14 (8)	O1^vi—Yb1—K1	58.13 (8)
O1^vii—K1—Si1^ii	84.08 (5)	O1^x—Yb1—K1	121.87 (8)
O1^viii—K1—Si1^ii	84.08 (5)	O1—Yb1—K1	53.872 (14)
Si1^vii—K1—Si1^ii	99.75 (4)	K2—Yb1—K1	68.85 (3)
O1^i—K1—Si1	145.96 (7)	K2^xvii—Yb1—K1	111.15 (3)
O1^ii—K1—Si1	145.96 (7)	K1^xvii—Yb1—K1	180.0
O1^iii—K1—Si1	92.18 (6)	K1^xiii—Yb1—K1	107.74 (3)
O1^iv—K1—Si1	92.18 (6)	K1^vii—Yb1—K1	72.26 (3)
O1—K1—Si1	28.77 (6)	O1—Si1—O1^v	110.43 (13)
O1^v—K1—Si1	28.77 (6)	O1—Si1—O1^xviii	110.43 (13)
O1^vi—K1—Si1	84.08 (5)	O1^v—Si1—O1^xviii	110.43 (13)
O1^vii—K1—Si1	84.08 (5)	O1—Si1—O2	108.49 (13)
O1^viii—K1—Si1	130.14 (8)	O1^v—Si1—O2	108.49 (13)
Si1^vii—K1—Si1	99.75 (4)	O1^xviii—Si1—O2	108.49 (13)
Si1^ii—K1—Si1	117.19 (3)	O1—Si1—K1^vii	71.51 (13)
O1—K2—O1^ix	142.94 (5)	O1^v—Si1—K1^vii	71.51 (13)
O1—K2—O1^iv	66.79 (10)	O1^xviii—Si1—K1^vii	71.51 (13)
O1^ix—K2—O1^iv	101.08 (12)	O2—Si1—K1^vii	180.0
O1—K2—O1^x	66.79 (10)	O1—Si1—K1	58.596 (12)
O1^ix—K2—O1^x	142.94 (5)	O1^v—Si1—K1	58.597 (12)
O1^iv—K2—O1^x	66.79 (10)	O1^xviii—Si1—K1	151.75 (15)
O1—K2—O1^xi	101.08 (12)	O2—Si1—K1	99.75 (4)
O1^ix—K2—O1^xi	66.79 (10)	K1^vii—Si1—K1	80.25 (4)
O1^iv—K2—O1^xi	142.94 (5)	O1—Si1—K1^xix	58.597 (12)
O1^x—K2—O1^xi	142.94 (5)	O1^v—Si1—K1^xix	151.75 (15)
O1—K2—O1^xii	142.94 (5)	O1^xviii—Si1—K1^xix	58.596 (12)
O1^ix—K2—O1^xii	66.79 (10)	O2—Si1—K1^xix	99.75 (4)
O1^iv—K2—O1^xii	142.94 (5)	K1^vii—Si1—K1^xix	80.25 (4)
O1^x—K2—O1^xii	101.08 (12)	K1—Si1—K1^xix	117.19 (3)
O1^xi—K2—O1^xii	66.79 (10)	O1—Si1—K1^xx	151.75 (15)
O1—K2—O2^xiii	108.53 (2)	O1^v—Si1—K1^xx	58.596 (12)
O1^ix—K2—O2^xiii	108.53 (2)	O1^xviii—Si1—K1^xx	58.596 (12)
O1^iv—K2—O2^xiii	108.53 (3)	O2—Si1—K1^xx	99.75 (4)
O1^x—K2—O2^xiii	50.54 (6)	K1^vii—Si1—K1^xx	80.25 (4)
O1^xi—K2—O2^xiii	108.53 (2)	K1—Si1—K1^xx	117.19 (3)
O1^xii—K2—O2^xiii	50.54 (6)	K1^xix—Si1—K1^xx	117.19 (3)
O1—K2—O2	50.54 (6)	O1—Si1—K2^xx	124.46 (4)
O1^ix—K2—O2	108.53 (2)	O1^v—Si1—K2^xx	124.46 (4)
O1^iv—K2—O2	108.53 (2)	O1^xviii—Si1—K2^xx	44.90 (12)
O1^x—K2—O2	108.53 (2)	O2—Si1—K2^xx	63.59 (3)
O1^xi—K2—O2	50.54 (6)	K1^vii—Si1—K2^xx	116.41 (3)
O1^xii—K2—O2	108.53 (2)	K1—Si1—K2^xx	163.35 (7)
O2^xiii—K2—O2	120.0	K1^xix—Si1—K2^xx	68.530 (18)
O1—K2—O2^xiv	108.53 (2)	K1^xx—Si1—K2^xx	68.530 (18)
O1^ix—K2—O2^xiv	50.54 (6)	O1—Si1—K2^xxi	124.46 (4)
O1^iv—K2—O2^xiv	50.54 (6)	O1^v—Si1—K2^xxi	44.90 (12)
O1^x—K2—O2^xiv	108.53 (2)	O1^xviii—Si1—K2^xxi	124.46 (4)
O1^xi—K2—O2^xiv	108.53 (3)	O2—Si1—K2^xxi	63.59 (3)
O1^xii—K2—O2^xiv	108.53 (2)	K1^vii—Si1—K2^xxi	116.41 (3)
O2^xiii—K2—O2^xiv	120.0	K1—Si1—K2^xxi	68.530 (18)
O2—K2—O2^xiv	120.0	K1^xix—Si1—K2^xxi	163.35 (7)
O1—K2—Yb1	39.46 (6)	K1^xx—Si1—K2^xxi	68.530 (18)
O1^ix—K2—Yb1	140.54 (6)	K2^xx—Si1—K2^xxi	101.73 (4)
O1^iv—K2—Yb1	39.46 (6)	O1—Si1—K2	44.90 (12)
O1^x—K2—Yb1	39.46 (6)	O1^v—Si1—K2	124.46 (4)
O1^xi—K2—Yb1	140.54 (6)	O1^xviii—Si1—K2	124.46 (4)
O1^xii—K2—Yb1	140.54 (6)	O2—Si1—K2	63.59 (3)
O2^xiii—K2—Yb1	90.0	K1^vii—Si1—K2	116.41 (3)
O2—K2—Yb1	90.0	K1—Si1—K2	68.530 (18)
O2^xiv—K2—Yb1	90.0	K1^xix—Si1—K2	68.531 (18)
O1—K2—Yb1^xv	140.54 (6)	K1^xx—Si1—K2	163.35 (7)
O1^ix—K2—Yb1^xv	39.46 (6)	K2^xx—Si1—K2	101.73 (4)
O1^iv—K2—Yb1^xv	140.54 (6)	K2^xxi—Si1—K2	101.73 (4)
O1^x—K2—Yb1^xv	140.54 (6)	Si1—O1—Yb1	161.5 (2)
O1^xi—K2—Yb1^xv	39.46 (6)	Si1—O1—K2	110.97 (16)
O1^xii—K2—Yb1^xv	39.46 (6)	Yb1—O1—K2	87.51 (10)
O2^xiii—K2—Yb1^xv	90.0	Si1—O1—K1	92.64 (6)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.41 (6)
O2^xiv—K2—Yb1^xv	90.0	K2—O1—K1	89.33 (7)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.64 (6)
O1—K2—Si1^xi	76.95 (7)	Yb1—O1—K1^xix	87.41 (6)
O1^ix—K2—Si1^xi	86.63 (5)	K2—O1—K1^xix	89.33 (7)
O1^iv—K2—Si1^xi	128.90 (2)	K1—O1—K1^xix	174.70 (13)
O1^x—K2—Si1^xi	128.90 (2)	Si1—O1—K1^vii	78.11 (14)
O1^xi—K2—Si1^xi	24.13 (7)	Yb1—O1—K1^vii	83.41 (9)
O1^xii—K2—Si1^xi	86.63 (5)	K2—O1—K1^vii	170.92 (12)
O2^xiii—K2—Si1^xi	116.605 (7)	K1—O1—K1^vii	90.25 (7)
O2—K2—Si1^xi	26.41 (3)	K1^xix—O1—K1^vii	90.26 (7)
O2^xiv—K2—Si1^xi	116.604 (7)	Si1—O2—Si1^xi	180.0
Yb1—K2—Si1^xi	116.41 (3)	Si1—O2—K2^xx	90.0
Yb1^xv—K2—Si1^xi	63.59 (3)	Si1^xi—O2—K2^xx	90.0
O1^xvi—Yb1—O1^iv	180.00 (12)	Si1—O2—K2	90.0
O1^xvi—Yb1—O1^xvii	87.56 (11)	Si1^xi—O2—K2	90.0
O1^iv—Yb1—O1^xvii	92.44 (11)	K2^xx—O2—K2	120.0
O1^xvi—Yb1—O1^vi	87.56 (11)	Si1—O2—K2^xxi	90.0
O1^iv—Yb1—O1^vi	92.44 (11)	Si1^xi—O2—K2^xxi	90.0
O1^xvii—Yb1—O1^vi	87.56 (11)	K2^xx—O2—K2^xxi	120.0
O1^xvi—Yb1—O1^x	92.44 (11)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) −x+y, −x+1, z; (ii) x, y+1, z; (iii) −y+1, x−y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) x−y, x, −z; (vii) −x+1, −y+1, −z; (viii) y, −x+y+1, −z; (ix) −y, x−y, −z+1/2; (x) −x+y, −x, z; (xi) x, y, −z+1/2; (xii) −x+y, −x, −z+1/2; (xiii) x−1, y−1, z; (xiv) x−1, y, z; (xv) −x, −y, z+1/2; (xvi) y, −x+y, −z; (xvii) −x, −y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(283_K)

Crystal data

K3O7Si2Yb	Dx = 3.848 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1097 reflections
a = 5.7238 (6) Å	θ = 5.0–29.8°
c = 13.9479 (17) Å	µ = 13.70 mm^−1
V = 395.74 (10) Å^3	T = 283 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	188 reflections with I > 2σ(I)
ω scans	Rint = 0.047
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.305, Tmax = 0.399	h = −6→7
2526 measured reflections	k = −7→5
211 independent reflections	l = −18→16

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0034P)^2 + 0.5483P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.014	(Δ/σ)max < 0.001
wR(F^2) = 0.031	Δρmax = 0.43 e Å^−3
S = 1.26	Δρmin = −0.54 e Å^−3
211 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0147 (8)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09159 (13)	0.0120 (4)
K2	0.000000	0.000000	0.250000	0.0157 (5)
Yb1	0.000000	0.000000	0.000000	0.00407 (19)
Si1	0.666667	0.333333	0.13223 (14)	0.0044 (4)
O1	0.3565 (6)	0.1782 (3)	0.0958 (2)	0.0110 (7)
O2	0.666667	0.333333	0.250000	0.0193 (18)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0104 (5)	0.0104 (5)	0.0151 (8)	0.0052 (3)	0.000	0.000
K2	0.0203 (8)	0.0203 (8)	0.0064 (11)	0.0102 (4)	0.000	0.000
Yb1	0.0037 (2)	0.0037 (2)	0.0048 (3)	0.00185 (10)	0.000	0.000
Si1	0.0045 (6)	0.0045 (6)	0.0040 (9)	0.0023 (3)	0.000	0.000
O1	0.0088 (16)	0.0104 (12)	0.0134 (14)	0.0044 (8)	−0.0021 (14)	−0.0010 (7)
O2	0.026 (3)	0.026 (3)	0.005 (4)	0.0132 (15)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8648 (3)	K2—O1^xiii	2.783 (3)
K1—O1^ii	2.8648 (3)	K2—O2^xiv	3.3046 (4)
K1—O1^iii	2.8648 (3)	K2—O2	3.3046 (4)
K1—O1^iv	2.8648 (3)	K2—O2^ix	3.3047 (4)
K1—O1^v	2.8648 (3)	K2—Yb1	3.4870 (4)
K1—O1	2.8648 (3)	K2—Yb1^xv	3.4870 (4)
K1—O1^vi	3.033 (3)	K2—Si1^xi	3.6904 (10)
K1—O1^vii	3.033 (3)	Yb1—O1^xvi	2.215 (3)
K1—O1^viii	3.033 (3)	Yb1—O1^xvii	2.215 (3)
K1—Si1^viii	3.122 (3)	Yb1—O1^iv	2.215 (3)
K1—Si1^ii	3.3529 (6)	Yb1—O1^vii	2.215 (3)
K1—Si1^ix	3.3529 (5)	Yb1—O1^x	2.215 (3)
K2—O1	2.783 (3)	Yb1—O1	2.215 (3)
K2—O1^x	2.783 (3)	Si1—O1	1.619 (3)
K2—O1^xi	2.783 (3)	Si1—O1^xviii	1.619 (3)
K2—O1^xii	2.783 (3)	Si1—O1^v	1.619 (3)
K2—O1^iv	2.783 (3)	Si1—O2	1.643 (2)
O1^i—K1—O1^ii	64.57 (12)	O1^xvii—Yb1—O1^x	92.62 (11)
O1^i—K1—O1^iii	119.958 (5)	O1^iv—Yb1—O1^x	87.38 (11)
O1^ii—K1—O1^iii	55.40 (12)	O1^vii—Yb1—O1^x	180.00 (17)
O1^i—K1—O1^iv	55.40 (12)	O1^xvi—Yb1—O1	180.0
O1^ii—K1—O1^iv	119.958 (5)	O1^xvii—Yb1—O1	92.63 (11)
O1^iii—K1—O1^iv	174.84 (12)	O1^iv—Yb1—O1	87.37 (11)
O1^i—K1—O1^v	174.84 (12)	O1^vii—Yb1—O1	92.63 (11)
O1^ii—K1—O1^v	119.958 (5)	O1^x—Yb1—O1	87.37 (11)
O1^iii—K1—O1^v	64.57 (12)	O1^xvi—Yb1—K2	127.10 (8)
O1^iv—K1—O1^v	119.958 (5)	O1^xvii—Yb1—K2	127.10 (8)
O1^i—K1—O1	119.958 (5)	O1^iv—Yb1—K2	52.90 (8)
O1^ii—K1—O1	174.84 (13)	O1^vii—Yb1—K2	127.10 (8)
O1^iii—K1—O1	119.958 (5)	O1^x—Yb1—K2	52.90 (8)
O1^iv—K1—O1	64.57 (12)	O1—Yb1—K2	52.90 (8)
O1^v—K1—O1	55.40 (12)	O1^xvi—Yb1—K2^xvi	52.90 (8)
O1^i—K1—O1^vi	65.74 (10)	O1^xvii—Yb1—K2^xvi	52.90 (8)
O1^ii—K1—O1^vi	65.74 (10)	O1^iv—Yb1—K2^xvi	127.10 (8)
O1^iii—K1—O1^vi	89.85 (7)	O1^vii—Yb1—K2^xvi	52.90 (8)
O1^iv—K1—O1^vi	89.85 (7)	O1^x—Yb1—K2^xvi	127.10 (8)
O1^v—K1—O1^vi	117.81 (7)	O1—Yb1—K2^xvi	127.10 (8)
O1—K1—O1^vi	117.81 (7)	K2—Yb1—K2^xvi	180.0
O1^i—K1—O1^vii	89.85 (7)	O1^xvi—Yb1—K1	126.120 (14)
O1^ii—K1—O1^vii	117.81 (7)	O1^xvii—Yb1—K1	126.120 (14)
O1^iii—K1—O1^vii	117.81 (7)	O1^iv—Yb1—K1	53.880 (14)
O1^iv—K1—O1^vii	65.74 (10)	O1^vii—Yb1—K1	58.24 (8)
O1^v—K1—O1^vii	89.85 (7)	O1^x—Yb1—K1	121.76 (8)
O1—K1—O1^vii	65.74 (10)	O1—Yb1—K1	53.880 (14)
O1^vi—K1—O1^vii	52.09 (10)	K2—Yb1—K1	68.86 (3)
O1^i—K1—O1^viii	117.81 (7)	K2^xvi—Yb1—K1	111.14 (3)
O1^ii—K1—O1^viii	89.85 (7)	O1^xvi—Yb1—K1^xvi	53.880 (14)
O1^iii—K1—O1^viii	65.74 (10)	O1^xvii—Yb1—K1^xvi	53.880 (14)
O1^iv—K1—O1^viii	117.81 (7)	O1^iv—Yb1—K1^xvi	126.120 (14)
O1^v—K1—O1^viii	65.74 (10)	O1^vii—Yb1—K1^xvi	121.76 (8)
O1—K1—O1^viii	89.85 (7)	O1^x—Yb1—K1^xvi	58.24 (8)
O1^vi—K1—O1^viii	52.09 (10)	O1—Yb1—K1^xvi	126.120 (14)
O1^vii—K1—O1^viii	52.09 (10)	K2—Yb1—K1^xvi	111.14 (3)
O1^i—K1—Si1^viii	91.18 (7)	K2^xvi—Yb1—K1^xvi	68.86 (3)
O1^ii—K1—Si1^viii	91.18 (7)	K1—Yb1—K1^xvi	180.0
O1^iii—K1—Si1^viii	91.18 (7)	O1^xvi—Yb1—K1^xiv	58.24 (8)
O1^iv—K1—Si1^viii	91.18 (7)	O1^xvii—Yb1—K1^xiv	126.120 (14)
O1^v—K1—Si1^viii	91.18 (7)	O1^iv—Yb1—K1^xiv	53.880 (14)
O1—K1—Si1^viii	91.18 (7)	O1^vii—Yb1—K1^xiv	126.120 (14)
O1^vi—K1—Si1^viii	30.47 (6)	O1^x—Yb1—K1^xiv	53.880 (14)
O1^vii—K1—Si1^viii	30.47 (6)	O1—Yb1—K1^xiv	121.76 (8)
O1^viii—K1—Si1^viii	30.47 (6)	K2—Yb1—K1^xiv	68.86 (3)
O1^i—K1—Si1^ii	92.06 (6)	K2^xvi—Yb1—K1^xiv	111.14 (3)
O1^ii—K1—Si1^ii	28.85 (6)	K1—Yb1—K1^xiv	107.76 (3)
O1^iii—K1—Si1^ii	28.85 (6)	K1^xvi—Yb1—K1^xiv	72.24 (3)
O1^iv—K1—Si1^ii	146.05 (6)	O1^xvi—Yb1—K1^viii	121.76 (8)
O1^v—K1—Si1^ii	92.06 (6)	O1^xvii—Yb1—K1^viii	53.880 (14)
O1—K1—Si1^ii	146.05 (6)	O1^iv—Yb1—K1^viii	126.120 (14)
O1^vi—K1—Si1^ii	84.02 (4)	O1^vii—Yb1—K1^viii	53.880 (14)
O1^vii—K1—Si1^ii	130.20 (8)	O1^x—Yb1—K1^viii	126.120 (14)
O1^viii—K1—Si1^ii	84.02 (4)	O1—Yb1—K1^viii	58.24 (8)
Si1^viii—K1—Si1^ii	99.73 (4)	K2—Yb1—K1^viii	111.14 (3)
O1^i—K1—Si1^ix	28.85 (6)	K2^xvi—Yb1—K1^viii	68.86 (3)
O1^ii—K1—Si1^ix	92.06 (6)	K1—Yb1—K1^viii	72.24 (3)
O1^iii—K1—Si1^ix	146.05 (6)	K1^xvi—Yb1—K1^viii	107.76 (3)
O1^iv—K1—Si1^ix	28.85 (6)	K1^xiv—Yb1—K1^viii	180.00 (5)
O1^v—K1—Si1^ix	146.05 (6)	O1—Si1—O1^xviii	110.64 (12)
O1—K1—Si1^ix	92.06 (6)	O1—Si1—O1^v	110.64 (12)
O1^vi—K1—Si1^ix	84.02 (4)	O1^xviii—Si1—O1^v	110.64 (12)
O1^vii—K1—Si1^ix	84.02 (4)	O1—Si1—O2	108.28 (13)
O1^viii—K1—Si1^ix	130.20 (8)	O1^xviii—Si1—O2	108.28 (13)
Si1^viii—K1—Si1^ix	99.73 (4)	O1^v—Si1—O2	108.28 (13)
Si1^ii—K1—Si1^ix	117.20 (2)	O1—Si1—K1^viii	71.72 (13)
O1—K2—O1^x	66.70 (10)	O1^xviii—Si1—K1^viii	71.72 (13)
O1—K2—O1^xi	101.19 (12)	O1^v—Si1—K1^viii	71.72 (13)
O1^x—K2—O1^xi	142.99 (5)	O2—Si1—K1^viii	180.0
O1—K2—O1^xii	142.99 (5)	O1—Si1—K1^xix	58.604 (12)
O1^x—K2—O1^xii	142.99 (5)	O1^xviii—Si1—K1^xix	58.604 (12)
O1^xi—K2—O1^xii	66.70 (10)	O1^v—Si1—K1^xix	151.99 (15)
O1—K2—O1^iv	66.70 (10)	O2—Si1—K1^xix	99.73 (4)
O1^x—K2—O1^iv	66.70 (10)	K1^viii—Si1—K1^xix	80.27 (4)
O1^xi—K2—O1^iv	142.99 (5)	O1—Si1—K1^xx	151.99 (15)
O1^xii—K2—O1^iv	101.19 (12)	O1^xviii—Si1—K1^xx	58.604 (12)
O1—K2—O1^xiii	142.99 (5)	O1^v—Si1—K1^xx	58.604 (12)
O1^x—K2—O1^xiii	101.19 (12)	O2—Si1—K1^xx	99.73 (4)
O1^xi—K2—O1^xiii	66.70 (10)	K1^viii—Si1—K1^xx	80.27 (4)
O1^xii—K2—O1^xiii	66.70 (10)	K1^xix—Si1—K1^xx	117.20 (2)
O1^iv—K2—O1^xiii	142.99 (5)	O1—Si1—K1	58.604 (12)
O1—K2—O2^xiv	108.51 (2)	O1^xviii—Si1—K1	151.99 (15)
O1^x—K2—O2^xiv	50.59 (6)	O1^v—Si1—K1	58.604 (12)
O1^xi—K2—O2^xiv	108.51 (2)	O2—Si1—K1	99.73 (4)
O1^xii—K2—O2^xiv	108.51 (2)	K1^viii—Si1—K1	80.27 (4)
O1^iv—K2—O2^xiv	108.51 (2)	K1^xix—Si1—K1	117.20 (2)
O1^xiii—K2—O2^xiv	50.59 (6)	K1^xx—Si1—K1	117.20 (2)
O1—K2—O2	50.59 (6)	O1—Si1—K2^xx	124.39 (4)
O1^x—K2—O2	108.51 (2)	O1^xviii—Si1—K2^xx	44.71 (11)
O1^xi—K2—O2	50.59 (6)	O1^v—Si1—K2^xx	124.39 (4)
O1^xii—K2—O2	108.51 (2)	O2—Si1—K2^xx	63.57 (3)
O1^iv—K2—O2	108.51 (2)	K1^viii—Si1—K2^xx	116.43 (3)
O1^xiii—K2—O2	108.51 (2)	K1^xix—Si1—K2^xx	68.527 (18)
O2^xiv—K2—O2	120.0	K1^xx—Si1—K2^xx	68.527 (18)
O1—K2—O2^ix	108.51 (2)	K1—Si1—K2^xx	163.30 (7)
O1^x—K2—O2^ix	108.51 (2)	O1—Si1—K2^xxi	124.39 (4)
O1^xi—K2—O2^ix	108.51 (2)	O1^xviii—Si1—K2^xxi	124.39 (4)
O1^xii—K2—O2^ix	50.59 (6)	O1^v—Si1—K2^xxi	44.71 (11)
O1^iv—K2—O2^ix	50.59 (6)	O2—Si1—K2^xxi	63.57 (3)
O1^xiii—K2—O2^ix	108.51 (2)	K1^viii—Si1—K2^xxi	116.43 (3)
O2^xiv—K2—O2^ix	120.0	K1^xix—Si1—K2^xxi	163.30 (7)
O2—K2—O2^ix	120.0	K1^xx—Si1—K2^xxi	68.527 (18)
O1—K2—Yb1	39.41 (6)	K1—Si1—K2^xxi	68.528 (18)
O1^x—K2—Yb1	39.41 (6)	K2^xx—Si1—K2^xxi	101.70 (3)
O1^xi—K2—Yb1	140.59 (6)	O1—Si1—K2	44.71 (11)
O1^xii—K2—Yb1	140.59 (6)	O1^xviii—Si1—K2	124.39 (4)
O1^iv—K2—Yb1	39.41 (6)	O1^v—Si1—K2	124.39 (4)
O1^xiii—K2—Yb1	140.59 (6)	O2—Si1—K2	63.57 (3)
O2^xiv—K2—Yb1	90.0	K1^viii—Si1—K2	116.43 (3)
O2—K2—Yb1	90.0	K1^xix—Si1—K2	68.527 (18)
O2^ix—K2—Yb1	90.0	K1^xx—Si1—K2	163.30 (7)
O1—K2—Yb1^xv	140.59 (6)	K1—Si1—K2	68.528 (18)
O1^x—K2—Yb1^xv	140.59 (6)	K2^xx—Si1—K2	101.70 (3)
O1^xi—K2—Yb1^xv	39.41 (6)	K2^xxi—Si1—K2	101.70 (3)
O1^xii—K2—Yb1^xv	39.41 (6)	Si1—O1—Yb1	161.18 (19)
O1^iv—K2—Yb1^xv	140.59 (6)	Si1—O1—K2	111.13 (15)
O1^xiii—K2—Yb1^xv	39.41 (6)	Yb1—O1—K2	87.69 (10)
O2^xiv—K2—Yb1^xv	90.0	Si1—O1—K1	92.55 (6)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.46 (6)
O2^ix—K2—Yb1^xv	90.0	K2—O1—K1	89.45 (7)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.55 (6)
O1—K2—Si1^xi	77.02 (7)	Yb1—O1—K1^xix	87.46 (6)
O1^x—K2—Si1^xi	128.92 (2)	K2—O1—K1^xix	89.45 (7)
O1^xi—K2—Si1^xi	24.16 (7)	K1—O1—K1^xix	174.84 (12)
O1^xii—K2—Si1^xi	86.58 (4)	Si1—O1—K1^viii	77.81 (14)
O1^iv—K2—Si1^xi	128.91 (2)	Yb1—O1—K1^viii	83.37 (8)
O1^xiii—K2—Si1^xi	86.58 (5)	K2—O1—K1^viii	171.06 (12)
O2^xiv—K2—Si1^xi	116.599 (7)	K1—O1—K1^viii	90.15 (7)
O2—K2—Si1^xi	26.43 (3)	K1^xix—O1—K1^viii	90.15 (7)
O2^ix—K2—Si1^xi	116.598 (7)	Si1—O2—Si1^xi	180.0
Yb1—K2—Si1^xi	116.43 (3)	Si1—O2—K2^xx	90.0
Yb1^xv—K2—Si1^xi	63.57 (3)	Si1^xi—O2—K2^xx	90.0
O1^xvi—Yb1—O1^xvii	87.38 (11)	Si1—O2—K2	90.0
O1^xvi—Yb1—O1^iv	92.62 (11)	Si1^xi—O2—K2	90.0
O1^xvii—Yb1—O1^iv	180.00 (11)	K2^xx—O2—K2	120.0
O1^xvi—Yb1—O1^vii	87.38 (11)	Si1—O2—K2^xxi	90.0
O1^xvii—Yb1—O1^vii	87.38 (11)	Si1^xi—O2—K2^xxi	90.0
O1^iv—Yb1—O1^vii	92.62 (11)	K2^xx—O2—K2^xxi	120.0
O1^xvi—Yb1—O1^x	92.62 (11)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) −x+y, −x+1, z; (ii) x, y+1, z; (iii) −y+1, x−y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) y, −x+y+1, −z; (vii) x−y, x, −z; (viii) −x+1, −y+1, −z; (ix) x−1, y, z; (x) −x+y, −x, z; (xi) x, y, −z+1/2; (xii) −y, x−y, −z+1/2; (xiii) −x+y, −x, −z+1/2; (xiv) x−1, y−1, z; (xv) −x, −y, z+1/2; (xvi) −x, −y, −z; (xvii) y, −x+y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.

(RT_after)

Crystal data

K3O7Si2Yb	Dx = 3.851 Mg m^−3
Mr = 458.52	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P63/mmc	Cell parameters from 1168 reflections
a = 5.7256 (5) Å	θ = 5.0–29.8°
c = 13.9295 (13) Å	µ = 13.70 mm^−1
V = 395.46 (8) Å^3	T = 295 K
Z = 2	Prismatic, colourless
F(000) = 422	0.13 × 0.11 × 0.09 mm

Data collection

Xcalibur, Ruby, Gemini ultra diffractometer	186 reflections with I > 2σ(I)
ω scans	Rint = 0.040
Absorption correction: analytical CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.	θmax = 27.5°, θmin = 2.9°
Tmin = 0.288, Tmax = 0.398	h = −7→4
2487 measured reflections	k = −5→7
209 independent reflections	l = −17→17

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0088P)^2 + 0.8419P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.012	(Δ/σ)max < 0.001
wR(F^2) = 0.030	Δρmax = 0.40 e Å^−3
S = 1.13	Δρmin = −0.37 e Å^−3
209 reflections	Extinction correction: SHELXL-2018/3 (Sheldrick 2018), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
20 parameters	Extinction coefficient: 0.0125 (7)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.333333	0.666667	0.09159 (12)	0.0117 (3)
K2	0.000000	0.000000	0.250000	0.0162 (5)
Yb1	0.000000	0.000000	0.000000	0.00362 (17)
Si1	0.666667	0.333333	0.13226 (13)	0.0035 (3)
O1	0.3575 (5)	0.1787 (3)	0.09573 (19)	0.0109 (6)
O2	0.666667	0.333333	0.250000	0.0213 (17)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0102 (4)	0.0102 (4)	0.0148 (7)	0.0051 (2)	0.000	0.000
K2	0.0211 (7)	0.0211 (7)	0.0066 (10)	0.0105 (4)	0.000	0.000
Yb1	0.00314 (18)	0.00314 (18)	0.0046 (2)	0.00157 (9)	0.000	0.000
Si1	0.0036 (5)	0.0036 (5)	0.0034 (8)	0.0018 (2)	0.000	0.000
O1	0.0055 (13)	0.0108 (10)	0.0148 (13)	0.0027 (7)	−0.0029 (12)	−0.0015 (6)
O2	0.030 (3)	0.030 (3)	0.004 (3)	0.0149 (14)	0.000	0.000

Geometric parameters (Å, º)

K1—O1^i	2.8659 (3)	K2—O1	2.786 (3)
K1—O1^ii	2.8659 (3)	K2—O2^xiii	3.3057 (3)
K1—O1^iii	2.8659 (3)	K2—O2	3.3057 (3)
K1—O1^iv	2.8659 (3)	K2—O2^xiv	3.3057 (3)
K1—O1^v	2.8659 (3)	K2—Yb1	3.4824 (3)
K1—O1	2.8659 (3)	K2—Yb1^xv	3.4824 (3)
K1—O1^vi	3.026 (3)	K2—Si1^xiii	3.6901 (9)
K1—O1^vii	3.026 (3)	Yb1—O1	2.218 (3)
K1—O1^viii	3.026 (3)	Yb1—O1^xvi	2.218 (3)
K1—Si1^viii	3.118 (3)	Yb1—O1^xvii	2.218 (3)
K1—Si1	3.3539 (5)	Yb1—O1^iv	2.218 (3)
K1—Si1^ii	3.3539 (5)	Yb1—O1^vii	2.218 (3)
K2—O1^ix	2.786 (3)	Yb1—O1^ix	2.218 (3)
K2—O1^x	2.786 (3)	Si1—O1^xviii	1.615 (3)
K2—O1^xi	2.786 (3)	Si1—O1^v	1.615 (3)
K2—O1^iv	2.786 (3)	Si1—O1	1.615 (3)
K2—O1^xii	2.786 (3)	Si1—O2	1.6401 (18)
O1^i—K1—O1^ii	64.78 (10)	O1^xvi—Yb1—O1^vii	87.59 (10)
O1^i—K1—O1^iii	119.960 (5)	O1^xvii—Yb1—O1^vii	87.59 (10)
O1^ii—K1—O1^iii	55.19 (10)	O1^iv—Yb1—O1^vii	92.41 (10)
O1^i—K1—O1^iv	55.19 (10)	O1—Yb1—O1^ix	87.59 (10)
O1^ii—K1—O1^iv	119.960 (5)	O1^xvi—Yb1—O1^ix	92.41 (10)
O1^iii—K1—O1^iv	174.68 (11)	O1^xvii—Yb1—O1^ix	92.41 (10)
O1^i—K1—O1^v	174.68 (11)	O1^iv—Yb1—O1^ix	87.59 (10)
O1^ii—K1—O1^v	119.960 (5)	O1^vii—Yb1—O1^ix	180.00 (15)
O1^iii—K1—O1^v	64.78 (10)	O1—Yb1—K2	53.05 (7)
O1^iv—K1—O1^v	119.960 (5)	O1^xvi—Yb1—K2	126.95 (7)
O1^i—K1—O1	119.960 (5)	O1^xvii—Yb1—K2	126.95 (7)
O1^ii—K1—O1	174.68 (11)	O1^iv—Yb1—K2	53.05 (7)
O1^iii—K1—O1	119.960 (5)	O1^vii—Yb1—K2	126.95 (7)
O1^iv—K1—O1	64.78 (10)	O1^ix—Yb1—K2	53.05 (7)
O1^v—K1—O1	55.19 (10)	O1—Yb1—K2^xvi	126.95 (7)
O1^i—K1—O1^vi	65.78 (9)	O1^xvi—Yb1—K2^xvi	53.05 (7)
O1^ii—K1—O1^vi	65.78 (9)	O1^xvii—Yb1—K2^xvi	53.05 (7)
O1^iii—K1—O1^vi	89.78 (6)	O1^iv—Yb1—K2^xvi	126.95 (7)
O1^iv—K1—O1^vi	89.78 (6)	O1^vii—Yb1—K2^xvi	53.05 (7)
O1^v—K1—O1^vi	117.79 (6)	O1^ix—Yb1—K2^xvi	126.95 (7)
O1—K1—O1^vi	117.79 (6)	K2—Yb1—K2^xvi	180.0
O1^i—K1—O1^vii	89.78 (6)	O1—Yb1—K1^xvi	126.101 (13)
O1^ii—K1—O1^vii	117.79 (6)	O1^xvi—Yb1—K1^xvi	53.899 (13)
O1^iii—K1—O1^vii	117.79 (6)	O1^xvii—Yb1—K1^xvi	53.900 (13)
O1^iv—K1—O1^vii	65.78 (9)	O1^iv—Yb1—K1^xvi	126.100 (13)
O1^v—K1—O1^vii	89.78 (6)	O1^vii—Yb1—K1^xvi	121.94 (7)
O1—K1—O1^vii	65.78 (9)	O1^ix—Yb1—K1^xvi	58.06 (7)
O1^vi—K1—O1^vii	52.04 (8)	K2—Yb1—K1^xvi	111.10 (2)
O1^i—K1—O1^viii	117.79 (6)	K2^xvi—Yb1—K1^xvi	68.90 (2)
O1^ii—K1—O1^viii	89.78 (6)	O1—Yb1—K1^viii	58.06 (7)
O1^iii—K1—O1^viii	65.78 (9)	O1^xvi—Yb1—K1^viii	121.94 (7)
O1^iv—K1—O1^viii	117.79 (6)	O1^xvii—Yb1—K1^viii	53.899 (13)
O1^v—K1—O1^viii	65.78 (9)	O1^iv—Yb1—K1^viii	126.101 (13)
O1—K1—O1^viii	89.78 (6)	O1^vii—Yb1—K1^viii	53.899 (13)
O1^vi—K1—O1^viii	52.04 (8)	O1^ix—Yb1—K1^viii	126.101 (13)
O1^vii—K1—O1^viii	52.04 (8)	K2—Yb1—K1^viii	111.10 (2)
O1^i—K1—Si1^viii	91.16 (7)	K2^xvi—Yb1—K1^viii	68.90 (2)
O1^ii—K1—Si1^viii	91.16 (7)	K1^xvi—Yb1—K1^viii	107.79 (3)
O1^iii—K1—Si1^viii	91.16 (7)	O1—Yb1—K1^xiii	121.94 (7)
O1^iv—K1—Si1^viii	91.16 (7)	O1^xvi—Yb1—K1^xiii	58.06 (7)
O1^v—K1—Si1^viii	91.15 (7)	O1^xvii—Yb1—K1^xiii	126.101 (13)
O1—K1—Si1^viii	91.15 (7)	O1^iv—Yb1—K1^xiii	53.899 (13)
O1^vi—K1—Si1^viii	30.44 (5)	O1^vii—Yb1—K1^xiii	126.101 (13)
O1^vii—K1—Si1^viii	30.44 (5)	O1^ix—Yb1—K1^xiii	53.899 (13)
O1^viii—K1—Si1^viii	30.44 (5)	K2—Yb1—K1^xiii	68.90 (2)
O1^i—K1—Si1	145.96 (6)	K2^xvi—Yb1—K1^xiii	111.10 (2)
O1^ii—K1—Si1	145.96 (6)	K1^xvi—Yb1—K1^xiii	72.21 (3)
O1^iii—K1—Si1	92.17 (5)	K1^viii—Yb1—K1^xiii	180.00 (5)
O1^iv—K1—Si1	92.17 (5)	O1—Yb1—K1	53.899 (13)
O1^v—K1—Si1	28.76 (5)	O1^xvi—Yb1—K1	126.101 (13)
O1—K1—Si1	28.76 (5)	O1^xvii—Yb1—K1	126.101 (13)
O1^vi—K1—Si1	130.16 (7)	O1^iv—Yb1—K1	53.899 (13)
O1^vii—K1—Si1	84.03 (4)	O1^vii—Yb1—K1	58.06 (7)
O1^viii—K1—Si1	84.03 (4)	O1^ix—Yb1—K1	121.94 (7)
Si1^viii—K1—Si1	99.73 (4)	K2—Yb1—K1	68.90 (2)
O1^i—K1—Si1^ii	92.17 (5)	K2^xvi—Yb1—K1	111.10 (2)
O1^ii—K1—Si1^ii	28.76 (5)	K1^xvi—Yb1—K1	180.0
O1^iii—K1—Si1^ii	28.76 (5)	K1^viii—Yb1—K1	72.21 (3)
O1^iv—K1—Si1^ii	145.96 (6)	K1^xiii—Yb1—K1	107.79 (3)
O1^v—K1—Si1^ii	92.17 (5)	O1^xviii—Si1—O1^v	110.56 (11)
O1—K1—Si1^ii	145.96 (6)	O1^xviii—Si1—O1	110.56 (11)
O1^vi—K1—Si1^ii	84.03 (4)	O1^v—Si1—O1	110.56 (11)
O1^vii—K1—Si1^ii	130.16 (7)	O1^xviii—Si1—O2	108.36 (12)
O1^viii—K1—Si1^ii	84.03 (4)	O1^v—Si1—O2	108.36 (12)
Si1^viii—K1—Si1^ii	99.73 (4)	O1—Si1—O2	108.36 (12)
Si1—K1—Si1^ii	117.21 (2)	O1^xviii—Si1—K1^viii	71.64 (12)
O1^ix—K2—O1^x	142.89 (4)	O1^v—Si1—K1^viii	71.64 (12)
O1^ix—K2—O1^xi	142.89 (4)	O1—Si1—K1^viii	71.64 (12)
O1^x—K2—O1^xi	66.88 (8)	O2—Si1—K1^viii	180.0
O1^ix—K2—O1^iv	66.88 (8)	O1^xviii—Si1—K1	151.91 (14)
O1^x—K2—O1^iv	142.89 (4)	O1^v—Si1—K1	58.605 (11)
O1^xi—K2—O1^iv	100.96 (11)	O1—Si1—K1	58.605 (11)
O1^ix—K2—O1^xii	100.96 (11)	O2—Si1—K1	99.73 (4)
O1^x—K2—O1^xii	66.88 (9)	K1^viii—Si1—K1	80.27 (4)
O1^xi—K2—O1^xii	66.88 (9)	O1^xviii—Si1—K1^xix	58.604 (11)
O1^iv—K2—O1^xii	142.89 (4)	O1^v—Si1—K1^xix	151.91 (14)
O1^ix—K2—O1	66.88 (8)	O1—Si1—K1^xix	58.605 (11)
O1^x—K2—O1	100.96 (11)	O2—Si1—K1^xix	99.73 (4)
O1^xi—K2—O1	142.89 (4)	K1^viii—Si1—K1^xix	80.27 (4)
O1^iv—K2—O1	66.88 (8)	K1—Si1—K1^xix	117.21 (2)
O1^xii—K2—O1	142.89 (4)	O1^xviii—Si1—K1^xx	58.604 (11)
O1^ix—K2—O2^xiii	50.48 (5)	O1^v—Si1—K1^xx	58.605 (11)
O1^x—K2—O2^xiii	108.55 (2)	O1—Si1—K1^xx	151.91 (14)
O1^xi—K2—O2^xiii	108.55 (2)	O2—Si1—K1^xx	99.73 (4)
O1^iv—K2—O2^xiii	108.55 (2)	K1^viii—Si1—K1^xx	80.27 (4)
O1^xii—K2—O2^xiii	50.48 (5)	K1—Si1—K1^xx	117.21 (2)
O1—K2—O2^xiii	108.55 (2)	K1^xix—Si1—K1^xx	117.21 (2)
O1^ix—K2—O2	108.55 (2)	O1^xviii—Si1—K2^xx	44.75 (11)
O1^x—K2—O2	50.48 (5)	O1^v—Si1—K2^xx	124.41 (4)
O1^xi—K2—O2	108.55 (2)	O1—Si1—K2^xx	124.41 (4)
O1^iv—K2—O2	108.55 (2)	O2—Si1—K2^xx	63.61 (3)
O1^xii—K2—O2	108.55 (2)	K1^viii—Si1—K2^xx	116.39 (3)
O1—K2—O2	50.48 (5)	K1—Si1—K2^xx	163.34 (6)
O2^xiii—K2—O2	120.0	K1^xix—Si1—K2^xx	68.507 (16)
O1^ix—K2—O2^xiv	108.55 (2)	K1^xx—Si1—K2^xx	68.507 (16)
O1^x—K2—O2^xiv	108.55 (2)	O1^xviii—Si1—K2^xxi	124.41 (4)
O1^xi—K2—O2^xiv	50.48 (5)	O1^v—Si1—K2^xxi	44.75 (11)
O1^iv—K2—O2^xiv	50.48 (5)	O1—Si1—K2^xxi	124.41 (4)
O1^xii—K2—O2^xiv	108.55 (2)	O2—Si1—K2^xxi	63.61 (3)
O1—K2—O2^xiv	108.55 (2)	K1^viii—Si1—K2^xxi	116.39 (3)
O2^xiii—K2—O2^xiv	120.0	K1—Si1—K2^xxi	68.507 (16)
O2—K2—O2^xiv	120.0	K1^xix—Si1—K2^xxi	163.34 (6)
O1^ix—K2—Yb1	39.52 (5)	K1^xx—Si1—K2^xxi	68.508 (16)
O1^x—K2—Yb1	140.48 (5)	K2^xx—Si1—K2^xxi	101.75 (3)
O1^xi—K2—Yb1	140.48 (5)	O1^xviii—Si1—K2	124.41 (4)
O1^iv—K2—Yb1	39.52 (5)	O1^v—Si1—K2	124.41 (4)
O1^xii—K2—Yb1	140.48 (5)	O1—Si1—K2	44.75 (11)
O1—K2—Yb1	39.52 (5)	O2—Si1—K2	63.61 (3)
O2^xiii—K2—Yb1	90.0	K1^viii—Si1—K2	116.39 (3)
O2—K2—Yb1	90.0	K1—Si1—K2	68.507 (16)
O2^xiv—K2—Yb1	90.0	K1^xix—Si1—K2	68.508 (16)
O1^ix—K2—Yb1^xv	140.48 (5)	K1^xx—Si1—K2	163.34 (6)
O1^x—K2—Yb1^xv	39.52 (5)	K2^xx—Si1—K2	101.75 (3)
O1^xi—K2—Yb1^xv	39.52 (5)	K2^xxi—Si1—K2	101.75 (3)
O1^iv—K2—Yb1^xv	140.48 (5)	Si1—O1—Yb1	161.41 (18)
O1^xii—K2—Yb1^xv	39.52 (5)	Si1—O1—K2	111.16 (14)
O1—K2—Yb1^xv	140.48 (5)	Yb1—O1—K2	87.43 (8)
O2^xiii—K2—Yb1^xv	90.0	Si1—O1—K1	92.64 (5)
O2—K2—Yb1^xv	90.0	Yb1—O1—K1	87.39 (6)
O2^xiv—K2—Yb1^xv	90.0	K2—O1—K1	89.37 (6)
Yb1—K2—Yb1^xv	180.0	Si1—O1—K1^xix	92.64 (5)
O1^ix—K2—Si1^xiii	24.09 (6)	Yb1—O1—K1^xix	87.39 (6)
O1^x—K2—Si1^xiii	128.893 (19)	K2—O1—K1^xix	89.37 (6)
O1^xi—K2—Si1^xiii	128.892 (19)	K1—O1—K1^xix	174.68 (11)
O1^iv—K2—Si1^xiii	86.69 (4)	Si1—O1—K1^viii	77.92 (12)
O1^xii—K2—Si1^xiii	76.87 (6)	Yb1—O1—K1^viii	83.48 (8)
O1—K2—Si1^xiii	86.69 (4)	K2—O1—K1^viii	170.92 (10)
O2^xiii—K2—Si1^xiii	26.39 (3)	K1—O1—K1^viii	90.22 (6)
O2—K2—Si1^xiii	116.610 (6)	K1^xix—O1—K1^viii	90.22 (6)
O2^xiv—K2—Si1^xiii	116.609 (6)	Si1^x—O2—Si1	180.0
Yb1—K2—Si1^xiii	63.61 (3)	Si1^x—O2—K2^xx	90.0
Yb1^xv—K2—Si1^xiii	116.39 (3)	Si1—O2—K2^xx	90.0
O1—Yb1—O1^xvi	180.00 (11)	Si1^x—O2—K2	90.0
O1—Yb1—O1^xvii	92.41 (10)	Si1—O2—K2	90.0
O1^xvi—Yb1—O1^xvii	87.59 (10)	K2^xx—O2—K2	120.0
O1—Yb1—O1^iv	87.59 (10)	Si1^x—O2—K2^xxi	90.0
O1^xvi—Yb1—O1^iv	92.41 (10)	Si1—O2—K2^xxi	90.0
O1^xvii—Yb1—O1^iv	180.00 (11)	K2^xx—O2—K2^xxi	120.0
O1—Yb1—O1^vii	92.41 (10)	K2—O2—K2^xxi	120.0

Symmetry codes: (i) −x+y, −x+1, z; (ii) x, y+1, z; (iii) −y+1, x−y+1, z; (iv) −y, x−y, z; (v) −x+y+1, −x+1, z; (vi) y, −x+y+1, −z; (vii) x−y, x, −z; (viii) −x+1, −y+1, −z; (ix) −x+y, −x, z; (x) x, y, −z+1/2; (xi) −y, x−y, −z+1/2; (xii) −x+y, −x, −z+1/2; (xiii) x−1, y−1, z; (xiv) x−1, y, z; (xv) −x, −y, z+1/2; (xvi) −x, −y, −z; (xvii) y, −x+y, −z; (xviii) −y+1, x−y, z; (xix) x, y−1, z; (xx) x+1, y, z; (xxi) x+1, y+1, z.