Structure of the new iron(II) oxalate potassium salt K₂Fe[(C₂O₄)₂(H₂O)₂]·0.18H₂O

The discovery of a new Fe^II oxalate framework of composition K₂Fe[(C₂O₄)₂(H₂O)₂]·0.18H₂O is reported. Its crystal structure was solved by means of single crystal and powder X-ray diffraction. The new organic–inorganic hybrid compound crystallizes in the orthorhombic space group Pca2₁ with unit-cell parameters: a = 12.0351 (4) Å, b = 15.1265 (5) Å, c = 10.5562 (4) Å. This crystal structure, containing eight chemical formula, consists of a succession of FeO₄(H₂O)₂ octahedra and K⁺ cations growing along b direction. Magnetization measurements indicate that the title compound is paramagnetic over the investigated temperature range (2–300 K). Both magnetization and ⁵⁷Fe Mössbauer data indicate that Fe²⁺ is in a high-spin state.

Computing details

Program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2018).

(I)

Crystal data

K2Fe(C2O4)2(H2O)20.18(H2O)	Dx = 2.385 Mg m^−3
Mr = 344.95	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Pca21	Cell parameters from 11933 reflections
a = 12.0351 (4) Å	θ = 1.4–40.3°
b = 15.1265 (5) Å	µ = 2.48 mm^−1
c = 10.5562 (4) Å	T = 296 K
V = 1921.74 (12) Å^3	Plate, light green
Z = 8	0.27 × 0.19 × 0.18 mm
F(000) = 1355.5

Data collection

Bruker APEX-II QUAZAR CCD diffractometer	10385 reflections with I > 2σ(I)
Radiation source: ImuS	Rint = 0.026
f\ and ω scans	θmax = 40.3°, θmin = 1.4°
Absorption correction: multi-scan SADABS (Bruker, 2004)	h = −21→21
	k = −27→27
50068 measured reflections	l = −18→19
11933 independent reflections

Refinement

Refinement on F^2	H-atom parameters not defined
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0498P)^2 + 1.7589P] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.037	(Δ/σ)max = 0.001
wR(F^2) = 0.100	Δρmax = 2.28 e Å^−3
S = 1.08	Δρmin = −1.03 e Å^−3
11933 reflections	Absolute structure: Refined as an inversion twin.
318 parameters	Absolute structure parameter: 0.512 (13)
1 restraint

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 2-component inversion twin.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
Fe1	0.57527 (3)	0.37529 (2)	0.41806 (4)	0.00767 (8)
Fe2	0.57584 (3)	0.87864 (2)	0.39496 (3)	0.00642 (7)
K1	0.15296 (4)	1.00515 (3)	0.08100 (7)	0.01088 (9)
K2	0.84231 (4)	0.75030 (3)	0.61398 (6)	0.00981 (8)
K3	0.34061 (5)	0.75029 (4)	0.61061 (6)	0.01093 (8)
K4	0.15658 (5)	0.50195 (3)	0.12461 (7)	0.01279 (10)
C1A	0.34303 (19)	0.38627 (16)	0.3362 (2)	0.0087 (3)
C2A	0.4084 (2)	0.36038 (17)	0.2160 (2)	0.0099 (3)
O1A	0.39588 (16)	0.38205 (11)	0.43982 (17)	0.0091 (3)
O2A	0.24528 (18)	0.41121 (17)	0.3216 (2)	0.0196 (4)
O3A	0.35460 (18)	0.33417 (17)	0.1228 (2)	0.0202 (4)
O4A	0.51306 (17)	0.36704 (13)	0.22508 (19)	0.0129 (3)
C1B	0.6017 (2)	0.37194 (14)	0.6988 (2)	0.0077 (3)
C2B	0.67172 (19)	0.37729 (14)	0.8230 (2)	0.0068 (3)
O1B	0.77576 (16)	0.37112 (12)	0.80943 (19)	0.0108 (3)
O2B	0.61993 (16)	0.38686 (13)	0.92450 (18)	0.0116 (3)
O3B	0.65585 (16)	0.37712 (12)	0.59543 (17)	0.0104 (3)
O4B	0.49970 (17)	0.36274 (14)	0.70862 (19)	0.0135 (3)
C1C	0.3417 (2)	0.86090 (16)	0.3233 (2)	0.0089 (3)
C2C	0.40106 (19)	0.88501 (15)	0.1980 (2)	0.0075 (3)
O1C	0.40172 (16)	0.86431 (13)	0.42287 (18)	0.0105 (3)
O2C	0.24256 (18)	0.83954 (18)	0.3192 (2)	0.0219 (4)
O3C	0.34115 (17)	0.90514 (15)	0.10561 (19)	0.0144 (3)
O4C	0.50599 (15)	0.88356 (12)	0.20109 (17)	0.0089 (3)
C1D	0.89776 (19)	0.88001 (13)	0.1809 (2)	0.0064 (3)
C2D	0.82378 (19)	0.87185 (14)	0.3017 (2)	0.0071 (3)
O1D	0.72217 (16)	0.89200 (14)	0.28778 (19)	0.0129 (3)
O2D	0.86779 (17)	0.84462 (15)	0.40071 (19)	0.0152 (3)
O3D	0.84677 (16)	0.87663 (11)	0.07576 (18)	0.0093 (3)
O4D	1.00011 (16)	0.88804 (13)	0.19609 (18)	0.0115 (3)
OW1	0.56748 (15)	0.23819 (13)	0.4300 (2)	0.0133 (3)
OW2	0.57196 (15)	0.51244 (13)	0.4287 (2)	0.0144 (4)
OW3	0.55566 (18)	0.01555 (12)	0.41170 (18)	0.0129 (3)
OW4	0.58754 (18)	0.74056 (13)	0.3998 (2)	0.0148 (4)
OW5	0.5716 (10)	0.1224 (7)	0.4001 (19)	0.013 (3)*	0.177 (13)
OW6	0.5710 (8)	0.6262 (6)	0.4076 (15)	0.008 (3)*	0.182 (12)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Fe1	0.00613 (13)	0.00959 (13)	0.00728 (17)	−0.00021 (9)	−0.00041 (10)	0.00055 (10)
Fe2	0.00544 (12)	0.00828 (12)	0.00555 (15)	0.00019 (9)	−0.00011 (9)	−0.00004 (10)
K1	0.00853 (19)	0.01004 (18)	0.0141 (2)	−0.00090 (14)	0.00165 (15)	−0.00352 (16)
K2	0.01035 (18)	0.00986 (18)	0.00921 (16)	0.00103 (14)	0.00008 (15)	−0.00145 (14)
K3	0.01282 (19)	0.01081 (19)	0.00916 (17)	−0.00061 (15)	0.00134 (16)	0.00135 (14)
K4	0.0170 (2)	0.01024 (18)	0.0111 (2)	−0.00263 (16)	−0.00474 (17)	0.00023 (15)
C1A	0.0062 (8)	0.0108 (8)	0.0091 (8)	0.0013 (6)	0.0008 (6)	0.0009 (6)
C2A	0.0065 (8)	0.0128 (8)	0.0106 (8)	−0.0006 (7)	0.0001 (6)	−0.0015 (7)
O1A	0.0079 (6)	0.0125 (7)	0.0069 (7)	0.0002 (5)	−0.0010 (5)	0.0000 (5)
O2A	0.0102 (8)	0.0318 (11)	0.0169 (9)	0.0074 (8)	0.0007 (6)	0.0042 (8)
O3A	0.0167 (9)	0.0315 (11)	0.0123 (8)	−0.0062 (8)	−0.0009 (7)	−0.0075 (8)
O4A	0.0074 (7)	0.0202 (9)	0.0111 (7)	0.0006 (6)	0.0001 (6)	−0.0009 (6)
C1B	0.0077 (8)	0.0090 (8)	0.0066 (8)	−0.0003 (6)	−0.0011 (6)	−0.0004 (6)
C2B	0.0062 (7)	0.0076 (8)	0.0066 (7)	−0.0003 (6)	−0.0014 (6)	0.0013 (6)
O1B	0.0064 (7)	0.0180 (8)	0.0082 (6)	0.0006 (5)	−0.0011 (5)	0.0000 (5)
O2B	0.0103 (7)	0.0194 (8)	0.0051 (6)	0.0034 (6)	0.0003 (5)	−0.0010 (6)
O3B	0.0095 (7)	0.0159 (8)	0.0059 (6)	−0.0002 (5)	0.0001 (5)	0.0005 (5)
O4B	0.0074 (7)	0.0231 (9)	0.0099 (7)	−0.0025 (6)	−0.0009 (5)	0.0003 (6)
C1C	0.0078 (8)	0.0121 (8)	0.0068 (8)	−0.0016 (7)	0.0008 (6)	−0.0016 (6)
C2C	0.0065 (8)	0.0103 (8)	0.0056 (8)	−0.0004 (6)	−0.0013 (6)	0.0000 (6)
O1C	0.0100 (7)	0.0174 (7)	0.0041 (6)	−0.0017 (6)	0.0004 (5)	0.0006 (5)
O2C	0.0124 (8)	0.0401 (13)	0.0132 (8)	−0.0126 (9)	0.0014 (6)	−0.0046 (9)
O3C	0.0117 (8)	0.0221 (9)	0.0094 (7)	0.0018 (7)	−0.0017 (6)	0.0040 (6)
O4C	0.0061 (6)	0.0131 (7)	0.0076 (6)	−0.0013 (5)	0.0009 (5)	0.0002 (5)
C1D	0.0065 (8)	0.0076 (7)	0.0052 (7)	−0.0004 (6)	0.0012 (6)	0.0000 (5)
C2D	0.0065 (8)	0.0096 (8)	0.0054 (7)	0.0000 (6)	0.0018 (6)	−0.0004 (6)
O1D	0.0070 (7)	0.0217 (8)	0.0099 (7)	0.0017 (6)	0.0012 (5)	0.0014 (6)
O2D	0.0116 (7)	0.0247 (9)	0.0094 (7)	0.0036 (7)	0.0017 (6)	0.0052 (7)
O3D	0.0083 (7)	0.0138 (7)	0.0058 (6)	0.0007 (5)	0.0003 (5)	0.0004 (5)
O4D	0.0070 (7)	0.0183 (8)	0.0091 (7)	−0.0019 (6)	0.0011 (5)	−0.0010 (6)
OW1	0.0071 (7)	0.0132 (7)	0.0197 (9)	0.0025 (5)	−0.0015 (6)	−0.0071 (7)
OW2	0.0073 (7)	0.0112 (7)	0.0246 (10)	−0.0011 (5)	−0.0002 (7)	0.0064 (7)
OW3	0.0193 (8)	0.0119 (7)	0.0075 (7)	−0.0018 (6)	−0.0051 (6)	0.0004 (5)
OW4	0.0219 (9)	0.0097 (6)	0.0128 (8)	−0.0025 (6)	−0.0092 (7)	0.0023 (6)

Geometric parameters (Å, º)

Fe1—OW2	2.078 (2)	K3—O1B^iv	2.896 (2)
Fe1—OW1	2.080 (2)	K3—O2B^iii	2.896 (2)
Fe1—O3B	2.1087 (19)	K3—O3B^iv	2.947 (2)
Fe1—O1B^i	2.1292 (19)	K3—O4D^vi	2.972 (2)
Fe1—O4A	2.174 (2)	K3—O3C^viii	3.205 (2)
Fe1—O1A	2.1736 (19)	K3—C1C	3.464 (2)
Fe1—K4^ii	3.7419 (8)	K3—K4^viii	3.7595 (8)
Fe1—K3^iii	3.8944 (8)	K4—O2A	2.711 (2)
Fe1—K2^iv	3.9682 (7)	K4—O2B^xv	2.736 (2)
Fe2—OW3^v	2.0926 (19)	K4—O1A^x	2.7374 (19)
Fe2—OW4	2.094 (2)	K4—O4A^iv	2.835 (2)
Fe2—O1D	2.103 (2)	K4—O1B^iii	2.856 (2)
Fe2—O3D^vi	2.1240 (19)	K4—O3B^iii	2.922 (2)
Fe2—O1C	2.1272 (19)	K4—O4B^x	2.959 (2)
Fe2—O4C	2.2137 (19)	K4—OW2^iv	3.375 (3)
Fe2—K2^i	3.6793 (7)	K4—C2B^iii	3.463 (2)
Fe2—K1^vii	3.8645 (7)	K4—C1A^x	3.511 (3)
Fe2—K1^viii	3.8862 (7)	C1A—O2A	1.245 (3)
K1—O3C	2.736 (2)	C1A—O1A	1.267 (3)
K1—O4C^ix	2.7513 (18)	C1A—C2A	1.544 (3)
K1—O1C^x	2.785 (2)	C2A—O3A	1.243 (3)
K1—O1D^ix	2.807 (2)	C2A—O4A	1.267 (3)
K1—O4D^xi	2.828 (2)	C1B—O4B	1.240 (3)
K1—O3D^ix	2.9396 (19)	C1B—O3B	1.273 (3)
K1—O2D^xii	2.975 (2)	C1B—C2B	1.561 (3)
K1—OW3^xiii	3.086 (2)	C2B—O2B	1.248 (3)
K1—C1C^x	3.488 (2)	C2B—O1B	1.264 (3)
K1—C2D^xii	3.498 (2)	C1C—O2C	1.237 (3)
K1—K2^xii	3.7159 (7)	C1C—O1C	1.276 (3)
K2—O2D	2.683 (2)	C1C—C2C	1.547 (3)
K2—O3A^xiv	2.694 (2)	C2C—O3C	1.251 (3)
K2—O4B^ii	2.740 (2)	C2C—O4C	1.264 (3)
K2—O1A^ii	2.7935 (19)	C1D—O4D	1.248 (3)
K2—O4C^vi	2.8709 (19)	C1D—O3D	1.269 (3)
K2—O1D^vi	2.926 (2)	C1D—C2D	1.560 (3)
K2—O3D^vi	2.9989 (19)	C2D—O2D	1.242 (3)
K2—OW4^vi	3.137 (2)	C2D—O1D	1.269 (3)
K2—OW1^ii	3.339 (2)	OW1—OW5	1.781 (11)
K2—C2D^vi	3.362 (2)	OW2—OW6	1.736 (10)
K3—O1C	2.728 (2)	OW3—OW5	1.632 (11)
K3—O2C^viii	2.770 (2)	OW4—OW6	1.743 (10)
K3—O4A^xiv	2.777 (2)
OW2—Fe1—OW1	172.47 (10)	O3B^iv—K3—O3C^viii	87.83 (5)
OW2—Fe1—O3B	87.00 (8)	O4D^vi—K3—O3C^viii	86.15 (5)
OW1—Fe1—O3B	88.87 (8)	O1C—K3—C1C	19.54 (6)
OW2—Fe1—O1B^i	94.30 (8)	O2C^viii—K3—C1C	117.52 (7)
OW1—Fe1—O1B^i	92.35 (8)	O4A^xiv—K3—C1C	133.42 (6)
O3B—Fe1—O1B^i	95.24 (8)	O1B^iv—K3—C1C	160.37 (6)
OW2—Fe1—O4A	95.82 (9)	O2B^iii—K3—C1C	75.61 (6)
OW1—Fe1—O4A	89.07 (8)	O3B^iv—K3—C1C	105.73 (6)
O3B—Fe1—O4A	172.37 (8)	O4D^vi—K3—C1C	85.68 (6)
O1B^i—Fe1—O4A	77.50 (8)	O3C^viii—K3—C1C	68.60 (5)
OW2—Fe1—O1A	85.88 (7)	O1C—K3—K4^viii	131.13 (5)
OW1—Fe1—O1A	89.76 (7)	O2C^viii—K3—K4^viii	117.32 (6)
O3B—Fe1—O1A	111.24 (7)	O4A^xiv—K3—K4^viii	48.59 (4)
O1B^i—Fe1—O1A	153.47 (7)	O1B^iv—K3—K4^viii	48.72 (4)
O4A—Fe1—O1A	76.09 (7)	O2B^iii—K3—K4^viii	46.33 (4)
OW2—Fe1—K4^ii	63.54 (7)	O3B^iv—K3—K4^viii	49.87 (4)
OW1—Fe1—K4^ii	123.82 (7)	O4D^vi—K3—K4^viii	133.07 (4)
O3B—Fe1—K4^ii	127.46 (5)	O3C^viii—K3—K4^viii	137.47 (4)
O1B^i—Fe1—K4^ii	49.35 (5)	C1C—K3—K4^viii	121.13 (5)
O4A—Fe1—K4^ii	48.91 (5)	O1C—K3—K1^viii	46.05 (4)
O1A—Fe1—K4^ii	108.90 (5)	O2C^viii—K3—K1^viii	65.53 (6)
OW2—Fe1—K3^iii	122.49 (7)	O4A^xiv—K3—K1^viii	131.25 (5)
OW1—Fe1—K3^iii	64.89 (7)	O1B^iv—K3—K1^viii	134.10 (4)
O3B—Fe1—K3^iii	128.82 (5)	O2B^iii—K3—K1^viii	130.97 (4)
O1B^i—Fe1—K3^iii	46.99 (5)	O3B^iv—K3—K1^viii	131.48 (4)
O4A—Fe1—K3^iii	43.99 (5)	O4D^vi—K3—K1^viii	46.60 (4)
O1A—Fe1—K3^iii	111.67 (5)	O3C^viii—K3—K1^viii	44.28 (4)
K4^ii—Fe1—K3^iii	58.947 (15)	C1C—K3—K1^viii	56.48 (4)
OW2—Fe1—K2^iv	115.86 (6)	K4^viii—K3—K1^viii	177.10 (2)
OW1—Fe1—K2^iv	57.27 (6)	O1C—K3—Fe1^xiv	147.53 (4)
O3B—Fe1—K2^iv	82.44 (5)	O2C^viii—K3—Fe1^xiv	70.68 (5)
O1B^i—Fe1—K2^iv	149.48 (5)	O4A^xiv—K3—Fe1^xiv	32.94 (4)
O4A—Fe1—K2^iv	102.57 (6)	O1B^iv—K3—Fe1^xiv	32.52 (4)
O1A—Fe1—K2^iv	42.75 (5)	O2B^iii—K3—Fe1^xiv	99.98 (4)
K4^ii—Fe1—K2^iv	148.627 (16)	O3B^iv—K3—Fe1^xiv	85.55 (4)
K3^iii—Fe1—K2^iv	112.612 (14)	O4D^vi—K3—Fe1^xiv	85.48 (4)
OW3^v—Fe2—OW4	173.14 (9)	O3C^viii—K3—Fe1^xiv	123.20 (4)
OW3^v—Fe2—O1D	92.72 (8)	C1C—K3—Fe1^xiv	164.65 (4)
OW4—Fe2—O1D	93.02 (9)	K4^viii—K3—Fe1^xiv	58.503 (14)
OW3^v—Fe2—O3D^vi	89.38 (7)	K1^viii—K3—Fe1^xiv	123.24 (2)
OW4—Fe2—O3D^vi	86.22 (7)	O2A—K4—O2B^xv	165.25 (7)
O1D—Fe2—O3D^vi	96.75 (8)	O2A—K4—O1A^x	107.58 (7)
OW3^v—Fe2—O1C	88.56 (8)	O2B^xv—K4—O1A^x	79.62 (6)
OW4—Fe2—O1C	87.78 (8)	O2A—K4—O4A^iv	107.87 (7)
O1D—Fe2—O1C	155.41 (8)	O2B^xv—K4—O4A^iv	76.17 (6)
O3D^vi—Fe2—O1C	107.82 (7)	O1A^x—K4—O4A^iv	126.11 (6)
OW3^v—Fe2—O4C	90.04 (7)	O2A—K4—O1B^iii	72.78 (7)
OW4—Fe2—O4C	94.69 (7)	O2B^xv—K4—O1B^iii	99.22 (6)
O1D—Fe2—O4C	79.48 (7)	O1A^x—K4—O1B^iii	176.41 (6)
O3D^vi—Fe2—O4C	176.16 (7)	O4A^iv—K4—O1B^iii	56.51 (6)
O1C—Fe2—O4C	75.96 (7)	O2A—K4—O3B^iii	95.37 (7)
OW3^v—Fe2—K2^i	128.41 (6)	O2B^xv—K4—O3B^iii	70.02 (6)
OW4—Fe2—K2^i	58.36 (6)	O1A^x—K4—O3B^iii	121.19 (6)
O1D—Fe2—K2^i	52.61 (6)	O4A^iv—K4—O3B^iii	94.16 (6)
O3D^vi—Fe2—K2^i	126.83 (5)	O1B^iii—K4—O3B^iii	55.31 (5)
O1C—Fe2—K2^i	108.76 (5)	O2A—K4—O4B^x	70.13 (7)
O4C—Fe2—K2^i	51.25 (5)	O2B^xv—K4—O4B^x	124.49 (6)
OW3^v—Fe2—K1^vii	69.52 (6)	O1A^x—K4—O4B^x	66.14 (6)
OW4—Fe2—K1^vii	117.29 (7)	O4A^iv—K4—O4B^x	89.89 (6)
O1D—Fe2—K1^vii	45.07 (6)	O1B^iii—K4—O4B^x	117.06 (6)
O3D^vi—Fe2—K1^vii	132.21 (5)	O3B^iii—K4—O4B^x	165.48 (6)
O1C—Fe2—K1^vii	113.69 (5)	O2A—K4—OW2^iv	49.94 (6)
O4C—Fe2—K1^vii	44.20 (5)	O2B^xv—K4—OW2^iv	136.51 (6)
K2^i—Fe2—K1^vii	58.958 (15)	O1A^x—K4—OW2^iv	124.44 (5)
OW3^v—Fe2—K1^viii	52.25 (6)	O4A^iv—K4—OW2^iv	60.35 (5)
OW4—Fe2—K1^viii	121.77 (7)	O1B^iii—K4—OW2^iv	58.64 (5)
O1D—Fe2—K1^viii	144.88 (6)	O3B^iii—K4—OW2^iv	111.95 (5)
O3D^vi—Fe2—K1^viii	82.16 (5)	O4B^x—K4—OW2^iv	58.48 (5)
O1C—Fe2—K1^viii	44.12 (5)	O2A—K4—C2B^iii	64.41 (7)
O4C—Fe2—K1^viii	100.46 (5)	O2B^xv—K4—C2B^iii	103.82 (6)
K2^i—Fe2—K1^viii	148.977 (17)	O1A^x—K4—C2B^iii	156.64 (6)
K1^vii—Fe2—K1^viii	112.309 (11)	O4A^iv—K4—C2B^iii	76.62 (6)
O3C—K1—O4C^ix	145.77 (6)	O1B^iii—K4—C2B^iii	20.30 (5)
O3C—K1—O1C^x	80.19 (6)	O3B^iii—K4—C2B^iii	43.32 (5)
O4C^ix—K1—O1C^x	126.31 (6)	O4B^x—K4—C2B^iii	124.98 (6)
O3C—K1—O1D^ix	89.25 (6)	OW2^iv—K4—C2B^iii	68.83 (5)
O4C^ix—K1—O1D^ix	59.56 (6)	O2A—K4—C1A^x	114.35 (7)
O1C^x—K1—O1D^ix	163.76 (7)	O2B^xv—K4—C1A^x	68.72 (6)
O3C—K1—O4D^xi	98.70 (6)	O1A^x—K4—C1A^x	18.61 (5)
O4C^ix—K1—O4D^xi	76.54 (6)	O4A^iv—K4—C1A^x	132.34 (6)
O1C^x—K1—O4D^xi	67.95 (6)	O1B^iii—K4—C1A^x	157.96 (6)
O1D^ix—K1—O4D^xi	101.90 (6)	O3B^iii—K4—C1A^x	102.68 (6)
O3C—K1—O3D^ix	71.42 (6)	O4B^x—K4—C1A^x	84.61 (6)
O4C^ix—K1—O3D^ix	98.43 (5)	OW2^iv—K4—C1A^x	142.46 (5)
O1C^x—K1—O3D^ix	129.90 (6)	C2B^iii—K4—C1A^x	141.85 (6)
O1D^ix—K1—O3D^ix	56.08 (5)	O2A—K4—Fe1^iv	73.69 (5)
O4D^xi—K1—O3D^ix	154.86 (6)	O2B^xv—K4—Fe1^iv	106.98 (5)
O3C—K1—O2D^xii	123.55 (6)	O1A^x—K4—Fe1^iv	149.14 (4)
O4C^ix—K1—O2D^xii	76.90 (6)	O4A^iv—K4—Fe1^iv	35.31 (4)
O1C^x—K1—O2D^xii	100.43 (6)	O1B^iii—K4—Fe1^iv	34.45 (4)
O1D^ix—K1—O2D^xii	95.69 (6)	O3B^iii—K4—Fe1^iv	88.78 (4)
O4D^xi—K1—O2D^xii	134.33 (6)	O4B^x—K4—Fe1^iv	86.49 (4)
O3D^ix—K1—O2D^xii	65.79 (5)	OW2^iv—K4—Fe1^iv	33.45 (3)
O3C—K1—OW3^xiii	139.17 (6)	C2B^iii—K4—Fe1^iv	52.68 (4)
O4C^ix—K1—OW3^xiii	73.30 (5)	C1A^x—K4—Fe1^iv	164.88 (4)
O1C^x—K1—OW3^xiii	59.98 (5)	O2A—K4—K3^x	122.18 (6)
O1D^ix—K1—OW3^xiii	131.57 (6)	O2B^xv—K4—K3^x	49.98 (4)
O4D^xi—K1—OW3^xiii	75.61 (5)	O1A^x—K4—K3^x	129.50 (5)
O3D^ix—K1—OW3^xiii	127.14 (6)	O4A^iv—K4—K3^x	47.29 (4)
O2D^xii—K1—OW3^xiii	61.46 (5)	O1B^iii—K4—K3^x	49.65 (4)
O3C—K1—C1C^x	73.31 (6)	O3B^iii—K4—K3^x	50.46 (4)
O4C^ix—K1—C1C^x	138.94 (6)	O4B^x—K4—K3^x	136.76 (4)
O1C^x—K1—C1C^x	19.69 (6)	OW2^iv—K4—K3^x	96.00 (4)
O1D^ix—K1—C1C^x	161.40 (6)	C2B^iii—K4—K3^x	59.43 (4)
O4D^xi—K1—C1C^x	87.43 (6)	C1A^x—K4—K3^x	117.64 (4)
O3D^ix—K1—C1C^x	110.56 (6)	Fe1^iv—K4—K3^x	62.551 (15)
O2D^xii—K1—C1C^x	88.88 (6)	O2A—C1A—O1A	126.6 (2)
OW3^xiii—K1—C1C^x	66.12 (5)	O2A—C1A—C2A	117.2 (2)
O3C—K1—C2D^xii	107.93 (6)	O1A—C1A—C2A	116.2 (2)
O4C^ix—K1—C2D^xii	96.57 (6)	O2A—C1A—K4^viii	87.58 (16)
O1C^x—K1—C2D^xii	85.44 (6)	O1A—C1A—K4^viii	43.61 (12)
O1D^ix—K1—C2D^xii	109.69 (6)	C2A—C1A—K4^viii	146.98 (15)
O4D^xi—K1—C2D^xii	138.36 (6)	O3A—C2A—O4A	127.1 (2)
O3D^ix—K1—C2D^xii	66.24 (5)	O3A—C2A—C1A	117.8 (2)
O2D^xii—K1—C2D^xii	20.12 (5)	O4A—C2A—C1A	115.1 (2)
OW3^xiii—K1—C2D^xii	63.24 (5)	C1A—O1A—Fe1	114.20 (16)
C1C^x—K1—C2D^xii	70.96 (6)	C1A—O1A—K4^viii	117.78 (15)
O3C—K1—K2^xii	121.93 (5)	Fe1—O1A—K4^viii	109.61 (7)
O4C^ix—K1—K2^xii	50.03 (4)	C1A—O1A—K2^iv	119.24 (15)
O1C^x—K1—K2^xii	145.20 (5)	Fe1—O1A—K2^iv	105.37 (7)
O1D^ix—K1—K2^xii	51.02 (5)	K4^viii—O1A—K2^iv	87.29 (6)
O4D^xi—K1—K2^xii	126.39 (4)	C1A—O2A—K4	128.37 (18)
O3D^ix—K1—K2^xii	51.98 (4)	C2A—O3A—K2^iii	129.59 (18)
O2D^xii—K1—K2^xii	45.63 (4)	C2A—O4A—Fe1	114.72 (17)
OW3^xiii—K1—K2^xii	90.92 (4)	C2A—O4A—K3^iii	123.12 (16)
C1C^x—K1—K2^xii	134.07 (5)	Fe1—O4A—K3^iii	103.06 (8)
C2D^xii—K1—K2^xii	63.14 (4)	C2A—O4A—K4^ii	129.25 (17)
O3C—K1—Fe2^ix	111.65 (5)	Fe1—O4A—K4^ii	95.77 (7)
O4C^ix—K1—Fe2^ix	34.12 (4)	K3^iii—O4A—K4^ii	84.12 (6)
O1C^x—K1—Fe2^ix	143.62 (4)	O4B—C1B—O3B	125.8 (2)
O1D^ix—K1—Fe2^ix	32.03 (4)	O4B—C1B—C2B	118.0 (2)
O4D^xi—K1—Fe2^ix	76.13 (4)	O3B—C1B—C2B	116.1 (2)
O3D^ix—K1—Fe2^ix	85.99 (4)	O2B—C2B—O1B	126.9 (2)
O2D^xii—K1—Fe2^ix	100.43 (4)	O2B—C2B—C1B	117.2 (2)
OW3^xiii—K1—Fe2^ix	106.15 (4)	O1B—C2B—C1B	115.8 (2)
C1C^x—K1—Fe2^ix	163.30 (4)	O2B—C2B—K4^xiv	139.12 (16)
C2D^xii—K1—Fe2^ix	120.01 (4)	O1B—C2B—K4^xiv	51.63 (12)
K2^xii—K1—Fe2^ix	58.032 (13)	C1B—C2B—K4^xiv	80.88 (12)
O2D—K2—O3A^xiv	112.44 (7)	C2B—O1B—Fe1^vi	140.45 (17)
O2D—K2—O4B^ii	123.97 (6)	C2B—O1B—K4^xiv	108.07 (14)
O3A^xiv—K2—O4B^ii	107.43 (7)	Fe1^vi—O1B—K4^xiv	96.19 (7)
O2D—K2—O1A^ii	78.61 (6)	C2B—O1B—K3^ii	113.33 (15)
O3A^xiv—K2—O1A^ii	83.44 (7)	Fe1^vi—O1B—K3^ii	100.49 (7)
O4B^ii—K2—O1A^ii	68.48 (6)	K4^xiv—O1B—K3^ii	81.63 (5)
O2D—K2—O4C^vi	79.79 (6)	C2B—O2B—K4^xvii	130.82 (16)
O3A^xiv—K2—O4C^vi	151.81 (7)	C2B—O2B—K3^xiv	114.67 (14)
O4B^ii—K2—O4C^vi	83.21 (6)	K4^xvii—O2B—K3^xiv	83.69 (5)
O1A^ii—K2—O4C^vi	124.56 (6)	C1B—O3B—Fe1	121.64 (16)
O2D—K2—O1D^vi	99.61 (7)	C1B—O3B—K4^xiv	110.10 (14)
O3A^xiv—K2—O1D^vi	95.31 (7)	Fe1—O3B—K4^xiv	117.20 (8)
O4B^ii—K2—O1D^vi	114.32 (6)	C1B—O3B—K3^ii	107.42 (14)
O1A^ii—K2—O1D^vi	177.19 (6)	Fe1—O3B—K3^ii	112.75 (7)
O4C^vi—K2—O1D^vi	56.87 (5)	K4^xiv—O3B—K3^ii	79.67 (5)
O2D—K2—O3D^vi	68.59 (6)	C1B—O4B—K2^iv	136.38 (17)
O3A^xiv—K2—O3D^vi	68.86 (6)	C1B—O4B—K4^viii	121.62 (16)
O4B^ii—K2—O3D^vi	166.21 (6)	K2^iv—O4B—K4^viii	84.00 (6)
O1A^ii—K2—O3D^vi	122.91 (6)	O2C—C1C—O1C	125.8 (2)
O4C^vi—K2—O3D^vi	94.49 (5)	O2C—C1C—C2C	118.5 (2)
O1D^vi—K2—O3D^vi	54.29 (5)	O1C—C1C—C2C	115.7 (2)
O2D—K2—OW4^vi	143.27 (6)	O2C—C1C—K3	84.29 (16)
O3A^xiv—K2—OW4^vi	100.44 (6)	O1C—C1C—K3	45.63 (12)
O4B^ii—K2—OW4^vi	55.53 (6)	C2C—C1C—K3	149.80 (15)
O1A^ii—K2—OW4^vi	122.50 (5)	O2C—C1C—K1^viii	102.02 (16)
O4C^vi—K2—OW4^vi	63.49 (5)	O1C—C1C—K1^viii	47.32 (12)
O1D^vi—K2—OW4^vi	60.17 (5)	C2C—C1C—K1^viii	120.72 (14)
O3D^vi—K2—OW4^vi	111.32 (5)	K3—C1C—K1^viii	67.63 (5)
O2D—K2—OW1^ii	52.50 (5)	O3C—C2C—O4C	126.9 (2)
O3A^xiv—K2—OW1^ii	139.36 (7)	O3C—C2C—C1C	117.3 (2)
O4B^ii—K2—OW1^ii	71.56 (6)	O4C—C2C—C1C	115.8 (2)
O1A^ii—K2—OW1^ii	57.80 (6)	C1C—O1C—Fe2	116.59 (15)
O4C^vi—K2—OW1^ii	68.51 (6)	C1C—O1C—K3	114.83 (15)
O1D^vi—K2—OW1^ii	122.81 (6)	Fe2—O1C—K3	115.51 (8)
O3D^vi—K2—OW1^ii	120.29 (5)	C1C—O1C—K1^viii	113.00 (15)
OW4^vi—K2—OW1^ii	110.10 (6)	Fe2—O1C—K1^viii	103.76 (7)
O2D—K2—C2D^vi	105.76 (6)	K3—O1C—K1^viii	89.11 (6)
O3A^xiv—K2—C2D^vi	73.50 (7)	C1C—O2C—K3^x	120.23 (17)
O4B^ii—K2—C2D^vi	122.50 (6)	C2C—O3C—K1	133.31 (17)
O1A^ii—K2—C2D^vi	156.50 (6)	C2C—O3C—K3^x	101.69 (15)
O4C^vi—K2—C2D^vi	78.77 (5)	K1—O3C—K3^x	80.83 (5)
O1D^vi—K2—C2D^vi	21.90 (5)	C2C—O4C—Fe2	113.82 (15)
O3D^vi—K2—C2D^vi	43.91 (5)	C2C—O4C—K1^vii	128.33 (15)
OW4^vi—K2—C2D^vi	67.59 (5)	Fe2—O4C—K1^vii	101.68 (7)
OW1^ii—K2—C2D^vi	142.84 (6)	C2C—O4C—K2^i	129.76 (15)
O2D—K2—Fe2^vi	111.42 (5)	Fe2—O4C—K2^i	91.78 (6)
O3A^xiv—K2—Fe2^vi	117.26 (6)	K1^vii—O4C—K2^i	82.71 (5)
O4B^ii—K2—Fe2^vi	81.39 (5)	O4D—C1D—O3D	126.4 (2)
O1A^ii—K2—Fe2^vi	147.88 (4)	O4D—C1D—C2D	117.8 (2)
O4C^vi—K2—Fe2^vi	36.97 (4)	O3D—C1D—C2D	115.8 (2)
O1D^vi—K2—Fe2^vi	34.82 (4)	O2D—C2D—O1D	126.0 (2)
O3D^vi—K2—Fe2^vi	88.59 (4)	O2D—C2D—C1D	118.1 (2)
OW4^vi—K2—Fe2^vi	34.64 (4)	O1D—C2D—C1D	115.9 (2)
OW1^ii—K2—Fe2^vi	102.96 (4)	O2D—C2D—K2^i	124.63 (17)
C2D^vi—K2—Fe2^vi	52.81 (4)	O1D—C2D—K2^i	59.35 (13)
O2D—K2—K1^xvi	52.43 (5)	C1D—C2D—K2^i	84.31 (12)
O3A^xiv—K2—K1^xvi	119.26 (6)	O2D—C2D—K1^xvi	55.44 (13)
O4B^ii—K2—K1^xvi	130.15 (5)	O1D—C2D—K1^xvi	92.68 (14)
O1A^ii—K2—K1^xvi	130.41 (4)	C1D—C2D—K1^xvi	126.96 (13)
O4C^vi—K2—K1^xvi	47.26 (4)	K2^i—C2D—K1^xvi	146.65 (7)
O1D^vi—K2—K1^xvi	48.21 (4)	C2D—O1D—Fe2	136.20 (17)
O3D^vi—K2—K1^xvi	50.55 (4)	C2D—O1D—K1^vii	120.60 (15)
OW4^vi—K2—K1^xvi	97.63 (4)	Fe2—O1D—K1^vii	102.89 (7)
OW1^ii—K2—K1^xvi	83.17 (4)	C2D—O1D—K2^i	98.75 (15)
C2D^vi—K2—K1^xvi	61.31 (4)	Fe2—O1D—K2^i	92.57 (7)
Fe2^vi—K2—K1^xvi	63.008 (14)	K1^vii—O1D—K2^i	80.77 (6)
O1C—K3—O2C^viii	111.52 (7)	C2D—O2D—K2	146.49 (17)
O1C—K3—O4A^xiv	123.31 (6)	C2D—O2D—K1^xvi	104.44 (16)
O2C^viii—K3—O4A^xiv	101.22 (7)	K2—O2D—K1^xvi	81.94 (6)
O1C—K3—O1B^iv	179.85 (6)	C1D—O3D—Fe2^i	124.97 (16)
O2C^viii—K3—O1B^iv	68.62 (7)	C1D—O3D—K1^vii	110.04 (14)
O4A^xiv—K3—O1B^iv	56.65 (6)	Fe2^i—O3D—K1^vii	110.87 (7)
O1C—K3—O2B^iii	85.17 (6)	C1D—O3D—K2^i	105.96 (13)
O2C^viii—K3—O2B^iii	161.36 (7)	Fe2^i—O3D—K2^i	117.57 (7)
O4A^xiv—K3—O2B^iii	74.54 (6)	K1^vii—O3D—K2^i	77.47 (5)
O1B^iv—K3—O2B^iii	94.68 (6)	C1D—O4D—K1^xviii	130.36 (16)
O1C—K3—O3B^iv	125.26 (6)	C1D—O4D—K3^i	121.97 (15)
O2C^viii—K3—O3B^iv	95.12 (7)	K1^xviii—O4D—K3^i	83.64 (5)
O4A^xiv—K3—O3B^iv	94.83 (6)	OW5—OW1—Fe1	165.7 (6)
O1B^iv—K3—O3B^iv	54.64 (5)	OW5—OW1—K2^iv	100.2 (5)
O2B^iii—K3—O3B^iv	67.57 (6)	Fe1—OW1—K2^iv	91.13 (6)
O1C—K3—O4D^vi	66.63 (6)	OW6—OW2—Fe1	169.5 (5)
O2C^viii—K3—O4D^vi	69.51 (7)	OW6—OW2—K4^ii	86.8 (5)
O4A^xiv—K3—O4D^vi	84.66 (6)	Fe1—OW2—K4^ii	83.01 (8)
O1B^iv—K3—O4D^vi	113.48 (6)	OW5—OW3—Fe2^xix	163.7 (5)
O2B^iii—K3—O4D^vi	127.04 (6)	OW5—OW3—K1^xx	100.9 (5)
O3B^iv—K3—O4D^vi	164.12 (6)	Fe2^xix—OW3—K1^xx	95.33 (7)
O1C—K3—O3C^viii	73.14 (6)	OW6—OW4—Fe2	169.5 (4)
O2C^viii—K3—O3C^viii	53.87 (6)	OW6—OW4—K2^i	97.0 (5)
O4A^xiv—K3—O3C^viii	155.09 (6)	Fe2—OW4—K2^i	87.00 (7)
O1B^iv—K3—O3C^viii	106.94 (5)	OW3—OW5—OW1	163.3 (12)
O2B^iii—K3—O3C^viii	128.62 (6)	OW2—OW6—OW4	171.6 (8)

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