CaSeO₄·0.625H₂O - water channel occupation in a bassanite related structure

Calcium selenate subhydrate, CaSeO₄·0.625H₂O, was prepared by hydrothermal conversion of CaSeO₄·2H₂O at 463 K. From the single crystals obtained in the shape of hexagonal needles, 50-300 µm in length, the crystal structure could be solved in a trigonal unit cell with space group P3₂21. The cell was confirmed and refined by high-resolution synchrotron powder diffraction. The subhydrate was characterized by thermal analysis and Raman spectroscopy.

Computing details

For both compounds, data collection: Apex2; cell refinement: Apex2; data reduction: Apex2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Diamond 3.

(296K)

Crystal data

CaH1.25O4.625Se	Dx = 3.318 Mg m^−3
Mr = 194.30	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3221	Cell parameters from 100 reflections
Hall symbol: P 32 2"	θ = 1–55°
a = 14.1681 (2) Å	µ = 10.85 mm^−1
c = 13.4241 (2) Å	T = 296 K
V = 2333.68 (6) Å^3	Needle, colourless
Z = 24	0.1 × 0.04 × 0.01 mm
F(000) = 2214

Data collection

Bruker X8 Kappa. Apex2 diffractometer	3584 independent reflections
Radiation source: fine-focus sealed tube	2801 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.054
ω and phi scans	θmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan Sortav (Blessing 1995)	h = −18→18
Tmin = 0.695, Tmax = 0.748	k = −18→18
25493 measured reflections	l = −17→17

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.074	w = 1/[σ^2(Fo^2) + (0.0052P)^2 + 3.955P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.007
3584 reflections	Δρmax = 0.57 e Å^−3
258 parameters	Δρmin = −0.59 e Å^−3
5 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 constraints	Absolute structure parameter: 0.551 (14)
Primary atom site location: structure-invariant direct methods

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	Uiso*/Ueq
Se1	0.50317 (4)	0.77604 (5)	0.08460 (4)	0.00955 (15)
Se2	0.77513 (5)	0.99674 (5)	0.41646 (4)	0.01115 (17)
Se3	0.72331 (5)	0.71792 (4)	−0.24550 (4)	0.00990 (16)
Se4	0.21455 (5)	0.72243 (5)	0.24137 (4)	0.00972 (14)
Ca1	0.77406 (12)	1.0000	0.1667	0.0137 (4)
Ca2	0.48576 (9)	0.77327 (10)	0.33499 (8)	0.0143 (2)
Ca3	0.74341 (13)	0.74341 (13)	0.0000	0.0130 (4)
Ca4	0.71821 (13)	0.71821 (13)	−0.5000	0.0189 (5)
Ca5	0.49836 (9)	0.76787 (9)	−0.16074 (8)	0.0133 (2)
Ca6	0.78786 (13)	1.0000	0.6667	0.0137 (4)
O1	0.6241 (3)	0.6878 (3)	−0.1665 (3)	0.0190 (9)
O2	0.1934 (3)	0.6194 (3)	0.1706 (3)	0.0159 (8)
O3	0.4324 (3)	0.7983 (3)	0.0007 (3)	0.0175 (8)
O4	0.7298 (3)	0.8004 (3)	−0.3338 (3)	0.0191 (9)
O5	0.5689 (3)	0.7286 (4)	0.0217 (3)	0.0232 (10)
O6	0.8727 (3)	1.0630 (3)	0.3342 (3)	0.0201 (9)
O7	0.8332 (3)	0.7748 (3)	−0.1755 (3)	0.0200 (10)
O8	0.7976 (4)	0.9139 (3)	0.4823 (3)	0.0244 (10)
O9	0.4232 (3)	0.6936 (3)	0.1708 (3)	0.0171 (9)
O10	0.2926 (3)	0.7366 (3)	0.3367 (2)	0.0168 (9)
O11	0.7736 (4)	1.0834 (3)	0.4954 (3)	0.0201 (9)
O12	0.6657 (4)	0.9336 (4)	0.3495 (3)	0.0281 (11)
O13	0.5867 (3)	0.8885 (3)	0.1427 (3)	0.0226 (9)
O14	0.0976 (3)	0.7001 (3)	0.2832 (3)	0.0191 (9)
O15	0.2699 (3)	0.8257 (3)	0.1647 (3)	0.0187 (10)
O16	0.5014 (4)	0.9341 (4)	−0.1942 (4)	0.0268 (11)
O17	0.9505 (6)	1.0000	0.6667	0.084 (4)
O18	0.7054 (4)	0.6090 (3)	−0.3013 (3)	0.0303 (11)
O19	0.4810 (5)	0.9447 (5)	0.3018 (5)	0.0516 (16)
H1	0.468 (8)	0.985 (7)	0.266 (6)	0.077*
H2	0.545 (3)	0.992 (6)	0.296 (7)	0.077*
H3	0.557 (4)	0.987 (5)	−0.212 (6)	0.077*
H4	0.461 (7)	0.957 (8)	−0.180 (7)	0.077*
H5	1.003 (4)	1.051 (5)	0.692 (6)	0.077*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Se1	0.0089 (3)	0.0106 (3)	0.0074 (3)	0.0036 (3)	−0.0007 (2)	−0.0008 (2)
Se2	0.0143 (3)	0.0105 (4)	0.0080 (3)	0.0058 (3)	0.0004 (2)	0.0009 (2)
Se3	0.0108 (3)	0.0117 (3)	0.0085 (3)	0.0066 (2)	−0.0002 (2)	−0.0008 (2)
Se4	0.0104 (3)	0.0116 (3)	0.0080 (3)	0.0061 (2)	0.0002 (2)	−0.0004 (2)
Ca1	0.0146 (8)	0.0098 (10)	0.0152 (8)	0.0049 (5)	−0.0012 (3)	−0.0024 (7)
Ca2	0.0115 (6)	0.0192 (7)	0.0110 (5)	0.0069 (6)	−0.0007 (5)	−0.0033 (5)
Ca3	0.0135 (6)	0.0135 (6)	0.0125 (8)	0.0072 (8)	0.0004 (3)	−0.0004 (3)
Ca4	0.0237 (8)	0.0237 (8)	0.0167 (9)	0.0174 (8)	0.0013 (3)	−0.0013 (3)
Ca5	0.0129 (6)	0.0133 (7)	0.0125 (5)	0.0057 (6)	0.0006 (5)	−0.0010 (5)
Ca6	0.0137 (6)	0.0135 (11)	0.0138 (7)	0.0067 (5)	0.0001 (3)	0.0002 (7)
O1	0.022 (2)	0.021 (2)	0.017 (2)	0.0128 (19)	0.0081 (17)	0.0021 (17)
O2	0.019 (2)	0.016 (2)	0.0158 (18)	0.0111 (17)	−0.0028 (16)	−0.0076 (17)
O3	0.016 (2)	0.027 (2)	0.0098 (17)	0.0100 (18)	−0.0050 (16)	0.0036 (16)
O4	0.028 (3)	0.021 (2)	0.0095 (19)	0.014 (2)	−0.0031 (17)	0.0044 (16)
O5	0.020 (2)	0.032 (3)	0.021 (2)	0.016 (2)	0.0004 (18)	−0.0075 (19)
O6	0.023 (2)	0.021 (2)	0.0146 (19)	0.0095 (19)	0.0103 (17)	0.0050 (17)
O7	0.015 (2)	0.028 (3)	0.015 (2)	0.010 (2)	−0.0087 (16)	−0.0056 (17)
O8	0.027 (2)	0.025 (2)	0.028 (2)	0.018 (2)	0.0038 (19)	0.0127 (19)
O9	0.021 (2)	0.017 (2)	0.0086 (18)	0.0057 (18)	0.0050 (16)	0.0017 (16)
O10	0.022 (2)	0.023 (2)	0.0089 (18)	0.014 (2)	−0.0037 (15)	−0.0022 (17)
O11	0.029 (3)	0.015 (2)	0.019 (2)	0.013 (2)	0.0055 (18)	−0.0026 (17)
O12	0.027 (2)	0.018 (2)	0.024 (2)	0.001 (2)	−0.0145 (19)	−0.0024 (19)
O13	0.018 (2)	0.015 (2)	0.027 (2)	0.002 (2)	−0.0053 (17)	−0.0125 (18)
O14	0.013 (2)	0.021 (2)	0.024 (2)	0.0091 (18)	0.0066 (17)	−0.0002 (18)
O15	0.027 (3)	0.019 (2)	0.013 (2)	0.0133 (19)	0.0036 (17)	0.0065 (16)
O16	0.017 (3)	0.018 (2)	0.044 (3)	0.008 (2)	0.011 (2)	0.007 (2)
O17	0.016 (3)	0.022 (5)	0.216 (12)	0.011 (3)	−0.007 (3)	−0.014 (6)
O18	0.029 (3)	0.023 (2)	0.042 (3)	0.016 (2)	−0.002 (2)	−0.016 (2)
O19	0.031 (3)	0.031 (3)	0.083 (5)	0.008 (3)	−0.001 (3)	−0.009 (3)

Geometric parameters (Å, º)

Se1—O5	1.632 (4)	Ca3—O1	2.673 (4)
Se1—O13	1.632 (4)	Ca3—O1^v	2.673 (4)
Se1—O9	1.632 (4)	Ca3—Se3^v	3.3120 (6)
Se1—O3	1.639 (3)	Ca3—Se2^vii	3.6360 (11)
Se1—Ca5	3.2951 (11)	Ca3—Se2^iv	3.6360 (11)
Se1—Ca2	3.3690 (12)	Ca4—O15^viii	2.390 (4)
Se2—O12	1.620 (4)	Ca4—O15^ix	2.390 (4)
Se2—O8	1.623 (4)	Ca4—O8^v	2.427 (4)
Se2—O11	1.630 (4)	Ca4—O8^x	2.427 (4)
Se2—O6	1.647 (4)	Ca4—O4	2.483 (4)
Se2—Ca1	3.3537 (5)	Ca4—O4^xi	2.483 (4)
Se2—Ca6	3.3627 (5)	Ca4—O18^xi	3.043 (5)
Se2—Ca3^i	3.6360 (11)	Ca4—O18	3.043 (5)
Se3—O18	1.618 (4)	Ca4—Se3^xi	3.4173 (5)
Se3—O4	1.635 (4)	Ca4—Ca6^x	4.2402 (12)
Se3—O1	1.637 (4)	Ca4—Ca6^xii	4.2402 (12)
Se3—O7	1.644 (4)	Ca5—O16	2.377 (5)
Se3—Ca3	3.3120 (6)	Ca5—O2^ii	2.397 (4)
Se3—Ca4	3.4173 (5)	Ca5—O10^viii	2.414 (4)
Se4—O14	1.623 (4)	Ca5—O11^iv	2.470 (4)
Se4—O15	1.634 (4)	Ca5—O3	2.481 (4)
Se4—O2	1.639 (3)	Ca5—O9^ii	2.493 (4)
Se4—O10	1.637 (3)	Ca5—O1	2.547 (4)
Se4—Ca2^ii	3.2295 (12)	Ca5—O5	2.804 (4)
Se4—Ca5^iii	3.5579 (12)	Ca5—Se4^viii	3.5579 (12)
Ca1—O13^iv	2.335 (4)	Ca5—Ca2^viii	4.0457 (16)
Ca1—O13	2.335 (4)	Ca5—Ca2^ii	4.1424 (17)
Ca1—O7^i	2.371 (4)	Ca6—O17	2.304 (9)
Ca1—O7^v	2.371 (4)	Ca6—O14^xiii	2.374 (4)
Ca1—O6	2.561 (4)	Ca6—O14^vi	2.374 (4)
Ca1—O6^iv	2.561 (4)	Ca6—O4^xiv	2.519 (4)
Ca1—O12	2.796 (4)	Ca6—O4^iv	2.519 (4)
Ca1—O12^iv	2.796 (4)	Ca6—O11^xv	2.638 (4)
Ca1—Se2^iv	3.3537 (5)	Ca6—O11	2.638 (4)
Ca1—Ca3^i	4.1026 (10)	Ca6—O8^xv	2.794 (4)
Ca1—Ca3	4.1026 (10)	Ca6—O8	2.794 (4)
Ca2—O18^v	2.419 (4)	Ca6—Se2^xv	3.3627 (5)
Ca2—O12	2.431 (4)	Ca6—Ca4^xvi	4.2402 (12)
Ca2—O9	2.432 (4)	O2—Ca5^vi	2.397 (4)
Ca2—O19	2.503 (7)	O2—Ca2^ii	2.546 (4)
Ca2—O10	2.517 (4)	O3—Ca2^ii	2.536 (4)
Ca2—O3^vi	2.536 (4)	O4—Ca6^x	2.519 (4)
Ca2—O2^vi	2.546 (4)	O6—Ca3^i	2.415 (4)
Ca2—O15^vi	2.599 (4)	O7—Ca1^vii	2.371 (4)
Ca2—O13	3.006 (4)	O8—Ca4^xiv	2.427 (4)
Ca2—Se4^vi	3.2295 (12)	O9—Ca5^vi	2.493 (4)
Ca2—Ca5^iii	4.0457 (16)	O10—Ca5^iii	2.414 (4)
Ca3—O5^v	2.391 (4)	O11—Ca5^iv	2.470 (4)
Ca3—O5	2.391 (4)	O14—Ca6^ii	2.374 (4)
Ca3—O6^vii	2.415 (4)	O15—Ca4^iii	2.390 (4)
Ca3—O6^iv	2.415 (4)	O15—Ca2^ii	2.599 (4)
Ca3—O7^v	2.608 (4)	O18—Ca2^v	2.419 (4)
Ca3—O7	2.608 (4)
O5—Se1—O13	111.4 (2)	O5—Ca3—Se2^iv	74.81 (11)
O5—Se1—O9	114.0 (2)	O6^vii—Ca3—Se2^iv	93.12 (11)
O13—Se1—O9	105.4 (2)	O6^iv—Ca3—Se2^iv	21.50 (8)
O5—Se1—O3	104.7 (2)	O7^v—Ca3—Se2^iv	83.08 (9)
O13—Se1—O3	110.8 (2)	O7—Ca3—Se2^iv	75.07 (10)
O9—Se1—O3	110.6 (2)	O1—Ca3—Se2^iv	77.73 (9)
O5—Se1—Ca5	58.26 (14)	O1^v—Ca3—Se2^iv	138.15 (8)
O13—Se1—Ca5	120.30 (15)	Se3—Ca3—Se2^iv	76.457 (17)
O9—Se1—Ca5	133.54 (14)	Se3^v—Ca3—Se2^iv	110.26 (2)
O3—Se1—Ca5	46.85 (14)	Se2^vii—Ca3—Se2^iv	109.88 (5)
O5—Se1—Ca2	124.44 (15)	O15^viii—Ca4—O15^ix	127.0 (2)
O13—Se1—Ca2	63.09 (14)	O15^viii—Ca4—O8^v	152.29 (16)
O9—Se1—Ca2	42.58 (14)	O15^ix—Ca4—O8^v	80.27 (14)
O3—Se1—Ca2	129.75 (14)	O15^viii—Ca4—O8^x	80.27 (14)
Ca5—Se1—Ca2	175.34 (3)	O15^ix—Ca4—O8^x	152.29 (16)
O12—Se2—O8	112.5 (2)	O8^v—Ca4—O8^x	73.2 (2)
O12—Se2—O11	114.0 (2)	O15^viii—Ca4—O4	79.47 (13)
O8—Se2—O11	105.8 (2)	O15^ix—Ca4—O4	114.93 (12)
O12—Se2—O6	103.9 (2)	O8^v—Ca4—O4	84.37 (15)
O8—Se2—O6	111.4 (2)	O8^x—Ca4—O4	70.61 (13)
O11—Se2—O6	109.3 (2)	O15^viii—Ca4—O4^xi	114.93 (12)
O12—Se2—Ca1	56.16 (16)	O15^ix—Ca4—O4^xi	79.47 (13)
O8—Se2—Ca1	123.92 (15)	O8^v—Ca4—O4^xi	70.61 (13)
O11—Se2—Ca1	129.65 (14)	O8^x—Ca4—O4^xi	84.37 (15)
O6—Se2—Ca1	47.94 (14)	O4—Ca4—O4^xi	148.9 (2)
O12—Se2—Ca6	126.29 (16)	O15^viii—Ca4—O18^xi	61.01 (11)
O8—Se2—Ca6	55.79 (15)	O15^ix—Ca4—O18^xi	103.37 (12)
O11—Se2—Ca6	50.27 (14)	O8^v—Ca4—O18^xi	122.87 (12)
O6—Se2—Ca6	129.64 (14)	O8^x—Ca4—O18^xi	85.04 (13)
Ca1—Se2—Ca6	177.56 (4)	O4—Ca4—O18^xi	136.68 (12)
O12—Se2—Ca3^i	120.05 (15)	O4^xi—Ca4—O18^xi	54.88 (12)
O8—Se2—Ca3^i	120.66 (16)	O15^viii—Ca4—O18	103.37 (12)
O11—Se2—Ca3^i	76.81 (15)	O15^ix—Ca4—O18	61.01 (11)
O6—Se2—Ca3^i	32.50 (14)	O8^v—Ca4—O18	85.04 (13)
Ca1—Se2—Ca3^i	71.753 (16)	O8^x—Ca4—O18	122.87 (12)
Ca6—Se2—Ca3^i	106.189 (18)	O4—Ca4—O18	54.88 (12)
O18—Se3—O4	105.8 (2)	O4^xi—Ca4—O18	136.68 (12)
O18—Se3—O1	110.3 (2)	O18^xi—Ca4—O18	146.99 (18)
O4—Se3—O1	112.9 (2)	O15^viii—Ca4—Se3	91.89 (8)
O18—Se3—O7	113.0 (2)	O15^ix—Ca4—Se3	88.62 (8)
O4—Se3—O7	111.3 (2)	O8^v—Ca4—Se3	83.25 (10)
O1—Se3—O7	103.7 (2)	O8^x—Ca4—Se3	95.82 (10)
O18—Se3—Ca3	121.93 (17)	O4—Ca4—Se3	26.64 (9)
O4—Se3—Ca3	132.27 (14)	O4^xi—Ca4—Se3	152.68 (10)
O1—Se3—Ca3	53.14 (14)	O18^xi—Ca4—Se3	152.44 (8)
O7—Se3—Ca3	50.89 (14)	O18—Ca4—Se3	28.25 (8)
O18—Se3—Ca4	62.91 (17)	O15^viii—Ca4—Se3^xi	88.62 (8)
O4—Se3—Ca4	42.92 (14)	O15^ix—Ca4—Se3^xi	91.89 (8)
O1—Se3—Ca4	129.16 (14)	O8^v—Ca4—Se3^xi	95.82 (10)
O7—Se3—Ca4	125.89 (14)	O8^x—Ca4—Se3^xi	83.25 (10)
Ca3—Se3—Ca4	174.49 (4)	O4—Ca4—Se3^xi	152.68 (10)
O14—Se4—O15	112.2 (2)	O4^xi—Ca4—Se3^xi	26.64 (9)
O14—Se4—O2	108.2 (2)	O18^xi—Ca4—Se3^xi	28.25 (8)
O15—Se4—O2	102.98 (19)	O18—Ca4—Se3^xi	152.44 (8)
O14—Se4—O10	108.3 (2)	Se3—Ca4—Se3^xi	178.86 (7)
O15—Se4—O10	113.0 (2)	O15^viii—Ca4—Ca6^x	73.64 (10)
O2—Se4—O10	111.9 (2)	O15^ix—Ca4—Ca6^x	143.64 (9)
O14—Se4—Ca2^ii	114.05 (14)	O8^v—Ca4—Ca6^x	80.65 (11)
O15—Se4—Ca2^ii	53.04 (14)	O8^x—Ca4—Ca6^x	38.69 (9)
O2—Se4—Ca2^ii	51.21 (13)	O4—Ca4—Ca6^x	32.30 (9)
O10—Se4—Ca2^ii	137.46 (13)	O4^xi—Ca4—Ca6^x	122.06 (12)
O14—Se4—Ca5^iii	73.11 (14)	O18^xi—Ca4—Ca6^x	112.99 (8)
O15—Se4—Ca5^iii	127.29 (14)	O18—Ca4—Ca6^x	86.74 (8)
O2—Se4—Ca5^iii	125.86 (14)	Se3—Ca4—Ca6^x	58.568 (15)
O10—Se4—Ca5^iii	35.26 (13)	Se3^xi—Ca4—Ca6^x	120.65 (3)
Ca2^ii—Se4—Ca5^iii	172.57 (3)	O15^viii—Ca4—Ca6^xii	143.64 (9)
O13^iv—Ca1—O13	74.0 (2)	O15^ix—Ca4—Ca6^xii	73.64 (10)
O13^iv—Ca1—O7^i	84.40 (15)	O8^v—Ca4—Ca6^xii	38.69 (9)
O13—Ca1—O7^i	154.19 (16)	O8^x—Ca4—Ca6^xii	80.65 (11)
O13^iv—Ca1—O7^v	154.19 (16)	O4—Ca4—Ca6^xii	122.06 (12)
O13—Ca1—O7^v	84.40 (15)	O4^xi—Ca4—Ca6^xii	32.30 (9)
O7^i—Ca1—O7^v	119.7 (2)	O18^xi—Ca4—Ca6^xii	86.74 (8)
O13^iv—Ca1—O6	89.94 (14)	O18—Ca4—Ca6^xii	112.99 (8)
O13—Ca1—O6	126.45 (13)	Se3—Ca4—Ca6^xii	120.65 (3)
O7^i—Ca1—O6	66.23 (12)	Se3^xi—Ca4—Ca6^xii	58.568 (15)
O7^v—Ca1—O6	91.70 (14)	Ca6^x—Ca4—Ca6^xii	108.09 (6)
O13^iv—Ca1—O6^iv	126.45 (13)	O16—Ca5—O2^ii	142.24 (15)
O13—Ca1—O6^iv	89.94 (14)	O16—Ca5—O10^viii	91.05 (16)
O7^i—Ca1—O6^iv	91.70 (14)	O2^ii—Ca5—O10^viii	70.55 (13)
O7^v—Ca1—O6^iv	66.23 (12)	O16—Ca5—O11^iv	71.73 (15)
O6—Ca1—O6^iv	136.40 (19)	O2^ii—Ca5—O11^iv	144.68 (14)
O13^iv—Ca1—O12	75.28 (15)	O10^viii—Ca5—O11^iv	108.40 (13)
O13—Ca1—O12	69.27 (13)	O16—Ca5—O3	79.33 (15)
O7^i—Ca1—O12	119.12 (12)	O2^ii—Ca5—O3	95.84 (13)
O7^v—Ca1—O12	84.03 (13)	O10^viii—Ca5—O3	143.36 (14)
O6—Ca1—O12	57.21 (12)	O11^iv—Ca5—O3	101.98 (13)
O6^iv—Ca1—O12	145.51 (12)	O16—Ca5—O9^ii	71.98 (14)
O13^iv—Ca1—O12^iv	69.27 (13)	O2^ii—Ca5—O9^ii	72.08 (13)
O13—Ca1—O12^iv	75.28 (15)	O10^viii—Ca5—O9^ii	78.11 (13)
O7^i—Ca1—O12^iv	84.03 (13)	O11^iv—Ca5—O9^ii	143.20 (15)
O7^v—Ca1—O12^iv	119.12 (12)	O3—Ca5—O9^ii	65.28 (12)
O6—Ca1—O12^iv	145.51 (12)	O16—Ca5—O1	139.94 (15)
O6^iv—Ca1—O12^iv	57.21 (12)	O2^ii—Ca5—O1	74.37 (13)
O12—Ca1—O12^iv	135.2 (2)	O10^viii—Ca5—O1	89.05 (14)
O13^iv—Ca1—Se2	83.02 (10)	O11^iv—Ca5—O1	70.31 (14)
O13—Ca1—Se2	98.03 (10)	O3—Ca5—O1	120.78 (12)
O7^i—Ca1—Se2	93.13 (9)	O9^ii—Ca5—O1	146.39 (14)
O7^v—Ca1—Se2	86.21 (9)	O16—Ca5—O5	122.03 (15)
O6—Ca1—Se2	28.52 (8)	O2^ii—Ca5—O5	83.97 (13)
O6^iv—Ca1—Se2	150.48 (10)	O10^viii—Ca5—O5	146.45 (14)
O12—Ca1—Se2	28.76 (8)	O11^iv—Ca5—O5	80.00 (13)
O12^iv—Ca1—Se2	152.29 (9)	O3—Ca5—O5	58.29 (12)
O13^iv—Ca1—Se2^iv	98.03 (10)	O9^ii—Ca5—O5	115.08 (12)
O13—Ca1—Se2^iv	83.02 (10)	O1—Ca5—O5	62.60 (12)
O7^i—Ca1—Se2^iv	86.21 (9)	O16—Ca5—Se1	99.46 (12)
O7^v—Ca1—Se2^iv	93.13 (9)	O2^ii—Ca5—Se1	92.38 (9)
O6—Ca1—Se2^iv	150.48 (10)	O10^viii—Ca5—Se1	161.86 (10)
O6^iv—Ca1—Se2^iv	28.52 (8)	O11^iv—Ca5—Se1	89.02 (9)
O12—Ca1—Se2^iv	152.29 (9)	O3—Ca5—Se1	28.82 (8)
O12^iv—Ca1—Se2^iv	28.76 (8)	O9^ii—Ca5—Se1	91.05 (9)
Se2—Ca1—Se2^iv	178.69 (6)	O1—Ca5—Se1	92.26 (9)
O13^iv—Ca1—Ca3^i	75.20 (10)	O5—Ca5—Se1	29.66 (8)
O13—Ca1—Ca3^i	142.56 (11)	O16—Ca5—Se4^viii	76.16 (12)
O7^i—Ca1—Ca3^i	36.44 (9)	O2^ii—Ca5—Se4^viii	92.84 (9)
O7^v—Ca1—Ca3^i	117.74 (12)	O10^viii—Ca5—Se4^viii	23.05 (9)
O6—Ca1—Ca3^i	33.33 (9)	O11^iv—Ca5—Se4^viii	86.89 (9)
O6^iv—Ca1—Ca3^i	125.81 (10)	O3—Ca5—Se4^viii	149.77 (10)
O12—Ca1—Ca3^i	82.72 (8)	O9^ii—Ca5—Se4^viii	90.27 (8)
O12^iv—Ca1—Ca3^i	112.55 (10)	O1—Ca5—Se4^viii	89.44 (9)
Se2—Ca1—Ca3^i	57.319 (14)	O5—Ca5—Se4^viii	151.73 (9)
Se2^iv—Ca1—Ca3^i	122.16 (2)	Se1—Ca5—Se4^viii	174.77 (4)
O13^iv—Ca1—Ca3	142.56 (11)	O16—Ca5—Ca2^viii	114.35 (13)
O13—Ca1—Ca3	75.20 (10)	O2^ii—Ca5—Ca2^viii	36.31 (9)
O7^i—Ca1—Ca3	117.74 (12)	O10^viii—Ca5—Ca2^viii	35.71 (9)
O7^v—Ca1—Ca3	36.44 (9)	O11^iv—Ca5—Ca2^viii	139.67 (10)
O6—Ca1—Ca3	125.81 (10)	O3—Ca5—Ca2^viii	118.34 (10)
O6^iv—Ca1—Ca3	33.33 (9)	O9^ii—Ca5—Ca2^viii	63.95 (10)
O12—Ca1—Ca3	112.55 (10)	O1—Ca5—Ca2^viii	87.56 (10)
O12^iv—Ca1—Ca3	82.72 (8)	O5—Ca5—Ca2^viii	119.81 (9)
Se2—Ca1—Ca3	122.16 (2)	Se1—Ca5—Ca2^viii	126.24 (4)
Se2^iv—Ca1—Ca3	57.319 (14)	Se4^viii—Ca5—Ca2^viii	58.76 (3)
Ca3^i—Ca1—Ca3	140.59 (6)	O16—Ca5—Ca2^ii	80.90 (11)
O18^v—Ca2—O12	76.01 (16)	O2^ii—Ca5—Ca2^ii	74.95 (9)
O18^v—Ca2—O9	79.28 (16)	O10^viii—Ca5—Ca2^ii	109.05 (10)
O12—Ca2—O9	118.35 (14)	O11^iv—Ca5—Ca2^ii	133.43 (10)
O18^v—Ca2—O19	136.64 (19)	O3—Ca5—Ca2^ii	34.77 (9)
O12—Ca2—O19	68.39 (19)	O9^ii—Ca5—Ca2^ii	32.31 (8)
O9—Ca2—O19	96.26 (18)	O1—Ca5—Ca2^ii	136.24 (9)
O18^v—Ca2—O10	147.72 (15)	O5—Ca5—Ca2^ii	83.84 (9)
O12—Ca2—O10	135.75 (16)	Se1—Ca5—Ca2^ii	58.77 (3)
O9—Ca2—O10	78.85 (13)	Se4^viii—Ca5—Ca2^ii	122.53 (3)
O19—Ca2—O10	69.41 (17)	Ca2^viii—Ca5—Ca2^ii	85.80 (2)
O18^v—Ca2—O3^vi	75.18 (14)	O17—Ca6—O14^xiii	144.62 (10)
O12—Ca2—O3^vi	149.50 (17)	O17—Ca6—O14^vi	144.62 (10)
O9—Ca2—O3^vi	65.33 (13)	O14^xiii—Ca6—O14^vi	70.8 (2)
O19—Ca2—O3^vi	141.89 (17)	O17—Ca6—O4^xiv	76.42 (10)
O10—Ca2—O3^vi	74.23 (13)	O14^xiii—Ca6—O4^xiv	133.06 (15)
O18^v—Ca2—O2^vi	127.79 (15)	O14^vi—Ca6—O4^xiv	72.55 (14)
O12—Ca2—O2^vi	92.63 (14)	O17—Ca6—O4^iv	76.42 (10)
O9—Ca2—O2^vi	144.63 (13)	O14^xiii—Ca6—O4^iv	72.55 (14)
O19—Ca2—O2^vi	78.80 (17)	O14^vi—Ca6—O4^iv	133.06 (15)
O10—Ca2—O2^vi	66.56 (11)	O4^xiv—Ca6—O4^iv	152.8 (2)
O3^vi—Ca2—O2^vi	97.11 (13)	O17—Ca6—O11^xv	107.48 (10)
O18^v—Ca2—O15^vi	68.13 (14)	O14^xiii—Ca6—O11^xv	72.76 (13)
O12—Ca2—O15^vi	78.86 (14)	O14^vi—Ca6—O11^xv	78.84 (13)
O9—Ca2—O15^vi	138.34 (14)	O4^xiv—Ca6—O11^xv	72.29 (12)
O19—Ca2—O15^vi	125.21 (18)	O4^iv—Ca6—O11^xv	116.44 (11)
O10—Ca2—O15^vi	116.57 (12)	O17—Ca6—O11	107.48 (10)
O3^vi—Ca2—O15^vi	81.33 (13)	O14^xiii—Ca6—O11	78.84 (13)
O2^vi—Ca2—O15^vi	59.68 (12)	O14^vi—Ca6—O11	72.76 (13)
O18^v—Ca2—O13	79.25 (14)	O4^xiv—Ca6—O11	116.44 (11)
O12—Ca2—O13	64.49 (12)	O4^iv—Ca6—O11	72.29 (12)
O9—Ca2—O13	55.81 (12)	O11^xv—Ca6—O11	145.0 (2)
O19—Ca2—O13	63.68 (17)	O17—Ca6—O8^xv	74.46 (9)
O10—Ca2—O13	107.04 (12)	O14^xiii—Ca6—O8^xv	77.06 (13)
O3^vi—Ca2—O13	118.90 (11)	O14^vi—Ca6—O8^xv	131.36 (13)
O2^vi—Ca2—O13	140.90 (13)	O4^xiv—Ca6—O8^xv	107.89 (12)
O15^vi—Ca2—O13	135.77 (12)	O4^iv—Ca6—O8^xv	64.34 (12)
O18^v—Ca2—Se4^vi	97.89 (12)	O11^xv—Ca6—O8^xv	56.98 (12)
O12—Ca2—Se4^vi	80.90 (10)	O11—Ca6—O8^xv	134.90 (12)
O9—Ca2—Se4^vi	158.55 (10)	O17—Ca6—O8	74.46 (9)
O19—Ca2—Se4^vi	100.04 (15)	O14^xiii—Ca6—O8	131.36 (13)
O10—Ca2—Se4^vi	93.91 (8)	O14^vi—Ca6—O8	77.06 (13)
O3^vi—Ca2—Se4^vi	93.32 (9)	O4^xiv—Ca6—O8	64.34 (12)
O2^vi—Ca2—Se4^vi	30.10 (8)	O4^iv—Ca6—O8	107.89 (12)
O15^vi—Ca2—Se4^vi	30.15 (8)	O11^xv—Ca6—O8	134.90 (12)
O13—Ca2—Se4^vi	145.02 (8)	O11—Ca6—O8	56.98 (11)
O18^v—Ca2—Se1	75.83 (12)	O8^xv—Ca6—O8	148.92 (19)
O12—Ca2—Se1	91.87 (10)	O17—Ca6—Se2^xv	92.68 (3)
O9—Ca2—Se1	27.00 (9)	O14^xiii—Ca6—Se2^xv	70.88 (10)
O19—Ca2—Se1	81.29 (15)	O14^vi—Ca6—Se2^xv	104.55 (10)
O10—Ca2—Se1	94.44 (8)	O4^xiv—Ca6—Se2^xv	91.45 (8)
O3^vi—Ca2—Se1	90.65 (9)	O4^iv—Ca6—Se2^xv	89.81 (8)
O2^vi—Ca2—Se1	156.31 (9)	O11^xv—Ca6—Se2^xv	28.38 (8)
O15^vi—Ca2—Se1	143.94 (9)	O11—Ca6—Se2^xv	148.40 (9)
O13—Ca2—Se1	28.95 (7)	O8^xv—Ca6—Se2^xv	28.72 (8)
Se4^vi—Ca2—Se1	171.46 (4)	O8—Ca6—Se2^xv	154.43 (9)
O18^v—Ca2—Ca5^iii	144.06 (12)	O17—Ca6—Se2	92.68 (3)
O12—Ca2—Ca5^iii	122.19 (12)	O14^xiii—Ca6—Se2	104.55 (10)
O9—Ca2—Ca5^iii	110.75 (10)	O14^vi—Ca6—Se2	70.88 (10)
O19—Ca2—Ca5^iii	78.09 (15)	O4^xiv—Ca6—Se2	89.81 (8)
O10—Ca2—Ca5^iii	34.04 (8)	O4^iv—Ca6—Se2	91.45 (8)
O3^vi—Ca2—Ca5^iii	78.24 (9)	O11^xv—Ca6—Se2	148.40 (9)
O2^vi—Ca2—Ca5^iii	33.88 (9)	O11—Ca6—Se2	28.38 (8)
O15^vi—Ca2—Ca5^iii	84.40 (9)	O8^xv—Ca6—Se2	154.43 (9)
O13—Ca2—Ca5^iii	135.57 (10)	O8—Ca6—Se2	28.72 (8)
Se4^vi—Ca2—Ca5^iii	59.87 (3)	Se2^xv—Ca6—Se2	174.64 (6)
Se1—Ca2—Ca5^iii	128.46 (4)	O17—Ca6—Ca4^xvi	76.23 (3)
O5^v—Ca3—O5	111.8 (2)	O14^xiii—Ca6—Ca4^xvi	68.46 (10)
O5^v—Ca3—O6^vii	84.17 (14)	O14^vi—Ca6—Ca4^xvi	139.05 (11)
O5—Ca3—O6^vii	163.12 (16)	O4^xiv—Ca6—Ca4^xvi	137.58 (10)
O5^v—Ca3—O6^iv	163.12 (16)	O4^iv—Ca6—Ca4^xvi	31.79 (8)
O5—Ca3—O6^iv	84.17 (14)	O11^xv—Ca6—Ca4^xvi	85.87 (8)
O6^vii—Ca3—O6^iv	80.6 (2)	O11—Ca6—Ca4^xvi	102.41 (9)
O5^v—Ca3—O7^v	121.31 (13)	O8^xv—Ca6—Ca4^xvi	32.88 (8)
O5—Ca3—O7^v	81.35 (14)	O8—Ca6—Ca4^xvi	135.42 (10)
O6^vii—Ca3—O7^v	85.56 (13)	Se2^xv—Ca6—Ca4^xvi	58.290 (15)
O6^iv—Ca3—O7^v	64.87 (12)	Se2—Ca6—Ca4^xvi	123.221 (17)
O5^v—Ca3—O7	81.35 (14)	Se3—O1—Ca5	127.2 (2)
O5—Ca3—O7	121.31 (13)	Se3—O1—Ca3	97.51 (18)
O6^vii—Ca3—O7	64.87 (12)	Ca5—O1—Ca3	108.87 (14)
O6^iv—Ca3—O7	85.56 (13)	Se4—O2—Ca5^vi	131.9 (2)
O7^v—Ca3—O7	141.56 (19)	Se4—O2—Ca2^ii	98.69 (17)
O5^v—Ca3—O1	82.99 (14)	Ca5^vi—O2—Ca2^ii	109.80 (14)
O5—Ca3—O1	66.56 (13)	Se1—O3—Ca5	104.33 (19)
O6^vii—Ca3—O1	123.14 (11)	Se1—O3—Ca2^ii	124.8 (2)
O6^iv—Ca3—O1	99.22 (12)	Ca5—O3—Ca2^ii	111.31 (14)
O7^v—Ca3—O1	145.87 (12)	Se3—O4—Ca4	110.4 (2)
O7—Ca3—O1	58.50 (11)	Se3—O4—Ca6^x	132.1 (2)
O5^v—Ca3—O1^v	66.56 (13)	Ca4—O4—Ca6^x	115.91 (14)
O5—Ca3—O1^v	82.99 (14)	Se1—O5—Ca3	143.6 (2)
O6^vii—Ca3—O1^v	99.22 (12)	Se1—O5—Ca5	92.09 (17)
O6^iv—Ca3—O1^v	123.14 (11)	Ca3—O5—Ca5	109.39 (14)
O7^v—Ca3—O1^v	58.50 (11)	Se2—O6—Ca3^i	126.0 (2)
O7—Ca3—O1^v	145.87 (12)	Se2—O6—Ca1	103.54 (19)
O1—Ca3—O1^v	124.78 (18)	Ca3^i—O6—Ca1	111.04 (14)
O5^v—Ca3—Se3	78.93 (10)	Se3—O7—Ca1^vii	136.8 (2)
O5—Ca3—Se3	94.74 (9)	Se3—O7—Ca3	99.83 (18)
O6^vii—Ca3—Se3	93.79 (9)	Ca1^vii—O7—Ca3	110.88 (14)
O6^iv—Ca3—Se3	94.73 (9)	Se2—O8—Ca4^xiv	137.1 (2)
O7^v—Ca3—Se3	159.46 (9)	Se2—O8—Ca6	95.50 (18)
O7—Ca3—Se3	29.28 (8)	Ca4^xiv—O8—Ca6	108.43 (14)
O1—Ca3—Se3	29.35 (8)	Se1—O9—Ca2	110.4 (2)
O1^v—Ca3—Se3	141.37 (10)	Se1—O9—Ca5^vi	134.6 (2)
O5^v—Ca3—Se3^v	94.74 (9)	Ca2—O9—Ca5^vi	114.48 (14)
O5—Ca3—Se3^v	78.93 (10)	Se4—O10—Ca5^iii	121.7 (2)
O6^vii—Ca3—Se3^v	94.73 (9)	Se4—O10—Ca2	128.03 (19)
O6^iv—Ca3—Se3^v	93.79 (9)	Ca5^iii—O10—Ca2	110.25 (13)
O7^v—Ca3—Se3^v	29.28 (8)	Se2—O11—Ca5^iv	137.7 (2)
O7—Ca3—Se3^v	159.46 (9)	Se2—O11—Ca6	101.34 (18)
O1—Ca3—Se3^v	141.37 (10)	Ca5^iv—O11—Ca6	119.70 (15)
O1^v—Ca3—Se3^v	29.35 (8)	Se2—O12—Ca2	145.8 (2)
Se3—Ca3—Se3^v	168.81 (6)	Se2—O12—Ca1	95.09 (19)
O5^v—Ca3—Se2^vii	74.81 (11)	Ca2—O12—Ca1	112.76 (15)
O5—Ca3—Se2^vii	155.00 (9)	Se1—O13—Ca1	138.7 (2)
O6^vii—Ca3—Se2^vii	21.50 (8)	Se1—O13—Ca2	87.97 (16)
O6^iv—Ca3—Se2^vii	93.12 (11)	Ca1—O13—Ca2	108.70 (14)
O7^v—Ca3—Se2^vii	75.07 (10)	Se4—O14—Ca6^ii	143.2 (2)
O7—Ca3—Se2^vii	83.08 (9)	Se4—O15—Ca4^iii	132.3 (2)
O1—Ca3—Se2^vii	138.15 (8)	Se4—O15—Ca2^ii	96.81 (18)
O1^v—Ca3—Se2^vii	77.73 (9)	Ca4^iii—O15—Ca2^ii	121.37 (14)
Se3—Ca3—Se2^vii	110.26 (2)	Se3—O18—Ca2^v	147.7 (3)
Se3^v—Ca3—Se2^vii	76.456 (17)	Se3—O18—Ca4	88.84 (19)
O5^v—Ca3—Se2^iv	155.00 (9)	Ca2^v—O18—Ca4	105.02 (15)

Symmetry codes: (i) −x+y+1, −x+2, z+1/3; (ii) −y+1, x−y+1, z−1/3; (iii) −y+1, x−y+1, z+2/3; (iv) x−y+1, −y+2, −z+1/3; (v) y, x, −z; (vi) −x+y, −x+1, z+1/3; (vii) −y+2, x−y+1, z−1/3; (viii) −x+y, −x+1, z−2/3; (ix) −x+1, −x+y, −z−1/3; (x) x, y, z−1; (xi) y, x, −z−1; (xii) −y+2, x−y+1, z−4/3; (xiii) y, x+1, −z+1; (xiv) x, y, z+1; (xv) x−y+1, −y+2, −z+4/3; (xvi) −x+y+1, −x+2, z+4/3.

(100K)

Crystal data

CaH1.25O4.625Se	Dx = 3.318 Mg m^−3
Mr = 194.30	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3221	Cell parameters from 100 reflections
Hall symbol: P 32 2"	θ = 1–55°
a = 14.1035 (7) Å	µ = 10.85 mm^−1
c = 13.3622 (10) Å	T = 100 K
V = 2301.8 (2) Å^3	Needle, colourless
Z = 24	0.1 × 0.04 × 0.01 mm
F(000) = 2214

Data collection

Bruker X8 Kappa. Apex2 diffractometer	3531 independent reflections
Radiation source: fine-focus sealed tube	3005 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.044
ω and phi scans	θmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan Sortav (Blessing 1995)	h = −18→18
Tmin = 0.695, Tmax = 0.748	k = −16→18
31621 measured reflections	l = −17→17

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.033	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.082	w = 1/[σ^2(Fo^2) + (0.0171P)^2 + 9.5385P] where P = (Fo^2 + 2Fc^2)/3
S = 1.18	(Δ/σ)max = 0.002
3531 reflections	Δρmax = 0.81 e Å^−3
258 parameters	Δρmin = −1.13 e Å^−3
5 restraints	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
0 constraints	Absolute structure parameter: 0.426 (15)
Primary atom site location: structure-invariant direct methods

Special details

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	Uiso*/Ueq
Se1	0.50223 (4)	0.77603 (5)	0.08497 (4)	0.00504 (16)
Se2	0.77547 (5)	0.99645 (5)	0.41641 (4)	0.00632 (17)
Se3	0.72271 (5)	0.71739 (5)	−0.24537 (4)	0.00531 (16)
Se4	0.21423 (5)	0.72213 (5)	0.24185 (4)	0.00522 (15)
Ca1	0.77386 (13)	1.0000	0.1667	0.0085 (4)
Ca2	0.48519 (10)	0.77339 (10)	0.33583 (10)	0.0083 (2)
Ca3	0.74321 (13)	0.74321 (13)	0.0000	0.0066 (4)
Ca4	0.71697 (13)	0.71697 (13)	−0.5000	0.0102 (4)
Ca5	0.49903 (9)	0.76799 (10)	−0.15966 (9)	0.0071 (2)
Ca6	0.78906 (13)	1.0000	0.6667	0.0070 (4)
O1	0.6235 (3)	0.6874 (3)	−0.1653 (3)	0.0103 (8)
O2	0.1928 (3)	0.6187 (3)	0.1705 (3)	0.0107 (8)
O3	0.4305 (3)	0.7973 (3)	0.0008 (3)	0.0103 (8)
O4	0.7282 (3)	0.7998 (3)	−0.3339 (3)	0.0119 (9)
O5	0.5685 (3)	0.7282 (4)	0.0211 (3)	0.0115 (9)
O6	0.8733 (3)	1.0624 (3)	0.3339 (3)	0.0129 (9)
O7	0.8336 (3)	0.7754 (3)	−0.1753 (3)	0.0101 (9)
O8	0.7980 (4)	0.9133 (3)	0.4821 (3)	0.0165 (10)
O9	0.4225 (3)	0.6929 (4)	0.1713 (3)	0.0109 (9)
O10	0.2923 (3)	0.7363 (4)	0.3376 (3)	0.0107 (9)
O11	0.7748 (4)	1.0838 (3)	0.4963 (3)	0.0126 (9)
O12	0.6652 (4)	0.9325 (4)	0.3486 (3)	0.0203 (11)
O13	0.5861 (3)	0.8897 (3)	0.1435 (3)	0.0146 (9)
O14	0.0961 (3)	0.6996 (3)	0.2831 (3)	0.0118 (9)
O15	0.2706 (3)	0.8262 (3)	0.1645 (3)	0.0087 (9)
O16	0.5025 (4)	0.9346 (4)	−0.1929 (4)	0.0140 (10)
O17	0.9506 (6)	1.0000	0.6667	0.079 (5)
O18	0.7049 (4)	0.6078 (4)	−0.3017 (4)	0.0180 (10)
O19	0.4823 (4)	0.9445 (5)	0.3012 (5)	0.0329 (14)
H1	0.462 (8)	0.986 (6)	0.281 (7)	0.049*
H2	0.548 (2)	0.971 (7)	0.290 (7)	0.049*
H3	0.558 (5)	0.983 (5)	−0.218 (6)	0.049*
H4	0.464 (7)	0.956 (8)	−0.173 (7)	0.049*
H5	0.995 (6)	1.042 (7)	0.706 (6)	0.049*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Se1	0.0044 (3)	0.0052 (3)	0.0050 (3)	0.0021 (3)	−0.0004 (2)	−0.0006 (2)
Se2	0.0088 (3)	0.0043 (4)	0.0053 (3)	0.0029 (3)	0.0007 (2)	0.0007 (2)
Se3	0.0048 (3)	0.0056 (3)	0.0062 (3)	0.0030 (2)	−0.0002 (2)	−0.0005 (2)
Se4	0.0048 (3)	0.0052 (3)	0.0058 (3)	0.0026 (2)	0.0005 (2)	−0.0001 (2)
Ca1	0.0095 (7)	0.0061 (10)	0.0089 (8)	0.0031 (5)	−0.0002 (4)	−0.0005 (7)
Ca2	0.0054 (6)	0.0101 (7)	0.0070 (5)	0.0021 (6)	−0.0008 (5)	−0.0021 (5)
Ca3	0.0052 (6)	0.0052 (6)	0.0089 (9)	0.0021 (7)	0.0000 (3)	0.0000 (3)
Ca4	0.0134 (7)	0.0134 (7)	0.0092 (9)	0.0109 (8)	0.0005 (3)	−0.0005 (3)
Ca5	0.0058 (6)	0.0067 (7)	0.0072 (6)	0.0019 (6)	−0.0002 (5)	−0.0003 (5)
Ca6	0.0064 (6)	0.0071 (10)	0.0078 (8)	0.0035 (5)	0.0000 (4)	−0.0001 (7)
O1	0.011 (2)	0.011 (2)	0.008 (2)	0.0051 (17)	0.0042 (17)	0.0002 (17)
O2	0.012 (2)	0.012 (2)	0.010 (2)	0.0066 (18)	−0.0021 (17)	−0.0061 (17)
O3	0.009 (2)	0.013 (2)	0.010 (2)	0.0060 (18)	−0.0046 (17)	0.0005 (17)
O4	0.010 (2)	0.013 (2)	0.010 (2)	0.0033 (19)	−0.0029 (17)	0.0008 (17)
O5	0.010 (2)	0.015 (2)	0.012 (2)	0.0076 (19)	0.0012 (17)	−0.0071 (18)
O6	0.015 (2)	0.009 (2)	0.010 (2)	0.0018 (18)	0.0075 (17)	0.0010 (17)
O7	0.0077 (19)	0.010 (2)	0.010 (2)	0.0028 (18)	−0.0030 (16)	−0.0013 (17)
O8	0.016 (2)	0.012 (2)	0.025 (3)	0.009 (2)	0.004 (2)	0.0105 (19)
O9	0.012 (2)	0.012 (2)	0.008 (2)	0.0050 (18)	0.0013 (17)	0.0008 (17)
O10	0.013 (2)	0.014 (2)	0.006 (2)	0.0063 (19)	−0.0044 (16)	−0.0033 (17)
O11	0.013 (2)	0.010 (2)	0.014 (2)	0.0046 (19)	−0.0001 (18)	−0.0042 (18)
O12	0.021 (2)	0.011 (2)	0.017 (2)	0.000 (2)	−0.008 (2)	0.001 (2)
O13	0.012 (2)	0.009 (2)	0.023 (2)	0.0050 (19)	−0.0068 (18)	−0.0081 (18)
O14	0.005 (2)	0.011 (2)	0.017 (2)	0.0030 (18)	0.0042 (17)	−0.0021 (18)
O15	0.014 (2)	0.0078 (19)	0.005 (2)	0.0062 (18)	0.0039 (17)	0.0050 (16)
O16	0.010 (2)	0.006 (2)	0.027 (3)	0.0054 (19)	0.002 (2)	0.0002 (19)
O17	0.009 (3)	0.011 (5)	0.217 (16)	0.006 (2)	0.001 (3)	0.003 (7)
O18	0.020 (3)	0.012 (2)	0.025 (3)	0.011 (2)	0.000 (2)	−0.011 (2)
O19	0.021 (3)	0.020 (3)	0.057 (4)	0.010 (2)	−0.001 (3)	−0.005 (3)

Geometric parameters (Å, º)

Se1—O9	1.628 (4)	Ca3—O1	2.650 (4)
Se1—O3	1.637 (4)	Ca3—O1^v	2.650 (4)
Se1—O13	1.638 (4)	Ca3—Se3^v	3.2955 (7)
Se1—O5	1.639 (4)	Ca3—Se2^iv	3.6213 (11)
Se1—Ca5	3.2703 (13)	Ca3—Se2^vii	3.6213 (11)
Se1—Ca2	3.3594 (14)	Ca4—O15^viii	2.369 (4)
Se2—O8	1.618 (4)	Ca4—O15^ix	2.369 (4)
Se2—O12	1.628 (5)	Ca4—O8^v	2.422 (4)
Se2—O11	1.634 (4)	Ca4—O8^x	2.422 (4)
Se2—O6	1.644 (4)	Ca4—O4	2.476 (4)
Se2—Ca1	3.3378 (6)	Ca4—O4^xi	2.476 (4)
Se2—Ca6	3.3484 (6)	Ca4—O18^xi	3.026 (5)
Se2—Ca3^i	3.6213 (12)	Ca4—O18	3.026 (5)
Se3—O18	1.621 (4)	Ca4—Se3^xi	3.4033 (6)
Se3—O4	1.633 (4)	Ca4—Ca6^xii	4.2271 (12)
Se3—O1	1.639 (4)	Ca4—Ca6^x	4.2271 (12)
Se3—O7	1.647 (4)	Ca5—O16	2.368 (5)
Se3—Ca3	3.2955 (7)	Ca5—O2^ii	2.387 (4)
Se3—Ca4	3.4033 (6)	Ca5—O10^viii	2.406 (4)
Se4—O14	1.628 (4)	Ca5—O11^iv	2.459 (4)
Se4—O10	1.634 (4)	Ca5—O3	2.470 (4)
Se4—O2	1.639 (4)	Ca5—O9^ii	2.481 (4)
Se4—O15	1.640 (4)	Ca5—O1	2.526 (4)
Se4—Ca2^ii	3.2103 (14)	Ca5—O5	2.767 (5)
Se4—Ca5^iii	3.5498 (14)	Ca5—Se4^viii	3.5498 (14)
Ca1—O13	2.326 (4)	Ca5—Ca2^viii	4.0257 (17)
Ca1—O13^iv	2.326 (4)	Ca5—Ca2^ii	4.1278 (18)
Ca1—O7^i	2.361 (4)	Ca6—O17	2.278 (9)
Ca1—O7^v	2.361 (4)	Ca6—O14^xiii	2.364 (4)
Ca1—O6	2.550 (4)	Ca6—O14^vi	2.364 (4)
Ca1—O6^iv	2.550 (4)	Ca6—O4^iv	2.508 (4)
Ca1—O12	2.775 (5)	Ca6—O4^xiv	2.508 (4)
Ca1—O12^iv	2.775 (5)	Ca6—O11^xv	2.618 (5)
Ca1—Se2^iv	3.3378 (6)	Ca6—O11	2.618 (5)
Ca1—Ca3^i	4.0862 (11)	Ca6—O8^xv	2.784 (5)
Ca1—Ca3	4.0862 (11)	Ca6—O8	2.784 (5)
Ca2—O18^v	2.409 (4)	Ca6—Se2^xv	3.3484 (6)
Ca2—O12	2.411 (5)	Ca6—Ca4^xvi	4.2271 (12)
Ca2—O9	2.429 (4)	O2—Ca5^vi	2.387 (4)
Ca2—O19	2.477 (6)	O2—Ca2^ii	2.523 (4)
Ca2—O10	2.501 (4)	O3—Ca2^ii	2.502 (4)
Ca2—O3^vi	2.502 (4)	O4—Ca6^x	2.508 (4)
Ca2—O2^vi	2.523 (4)	O6—Ca3^i	2.410 (4)
Ca2—O15^vi	2.583 (4)	O7—Ca1^vii	2.361 (4)
Ca2—O13	2.998 (5)	O8—Ca4^xiv	2.422 (4)
Ca2—Se4^vi	3.2103 (14)	O9—Ca5^vi	2.481 (4)
Ca2—Ca5^iii	4.0257 (17)	O10—Ca5^iii	2.406 (4)
Ca3—O5^v	2.383 (4)	O11—Ca5^iv	2.459 (4)
Ca3—O5	2.383 (4)	O14—Ca6^ii	2.364 (4)
Ca3—O6^iv	2.410 (4)	O15—Ca4^iii	2.369 (4)
Ca3—O6^vii	2.410 (4)	O15—Ca2^ii	2.583 (4)
Ca3—O7^v	2.595 (4)	O18—Ca2^v	2.409 (4)
Ca3—O7	2.595 (4)
O9—Se1—O3	110.5 (2)	O5—Ca3—Se2^vii	155.20 (10)
O9—Se1—O13	105.5 (2)	O6^iv—Ca3—Se2^vii	92.57 (11)
O3—Se1—O13	111.0 (2)	O6^vii—Ca3—Se2^vii	21.68 (10)
O9—Se1—O5	113.8 (2)	O7^v—Ca3—Se2^vii	74.84 (10)
O3—Se1—O5	104.4 (2)	O7—Ca3—Se2^vii	82.96 (10)
O13—Se1—O5	111.7 (2)	O1—Ca3—Se2^vii	138.39 (9)
O9—Se1—Ca5	133.66 (15)	O1^v—Ca3—Se2^vii	77.94 (9)
O3—Se1—Ca5	47.21 (15)	Se3—Ca3—Se2^vii	110.32 (2)
O13—Se1—Ca5	120.11 (17)	Se3^v—Ca3—Se2^vii	76.534 (18)
O5—Se1—Ca5	57.72 (15)	Se2^iv—Ca3—Se2^vii	109.56 (5)
O9—Se1—Ca2	42.73 (15)	O15^viii—Ca4—O15^ix	127.4 (2)
O3—Se1—Ca2	129.80 (15)	O15^viii—Ca4—O8^v	151.70 (17)
O13—Se1—Ca2	63.08 (16)	O15^ix—Ca4—O8^v	80.54 (14)
O5—Se1—Ca2	124.57 (16)	O15^viii—Ca4—O8^x	80.54 (14)
Ca5—Se1—Ca2	175.76 (3)	O15^ix—Ca4—O8^x	151.70 (17)
O8—Se2—O12	112.3 (2)	O8^v—Ca4—O8^x	72.3 (2)
O8—Se2—O11	105.6 (2)	O15^viii—Ca4—O4	79.25 (13)
O12—Se2—O11	114.7 (2)	O15^ix—Ca4—O4	115.09 (13)
O8—Se2—O6	111.1 (2)	O8^v—Ca4—O4	84.27 (15)
O12—Se2—O6	103.8 (2)	O8^x—Ca4—O4	70.56 (15)
O11—Se2—O6	109.4 (2)	O15^viii—Ca4—O4^xi	115.09 (13)
O8—Se2—Ca1	123.93 (17)	O15^ix—Ca4—O4^xi	79.25 (13)
O12—Se2—Ca1	55.93 (17)	O8^v—Ca4—O4^xi	70.56 (15)
O11—Se2—Ca1	129.77 (16)	O8^x—Ca4—O4^xi	84.27 (15)
O6—Se2—Ca1	48.01 (15)	O4—Ca4—O4^xi	148.9 (2)
O8—Se2—Ca6	55.87 (16)	O15^viii—Ca4—O18^xi	60.84 (12)
O12—Se2—Ca6	126.58 (17)	O15^ix—Ca4—O18^xi	103.69 (13)
O11—Se2—Ca6	50.04 (16)	O8^v—Ca4—O18^xi	122.86 (14)
O6—Se2—Ca6	129.48 (15)	O8^x—Ca4—O18^xi	85.05 (14)
Ca1—Se2—Ca6	177.48 (4)	O4—Ca4—O18^xi	136.25 (13)
O8—Se2—Ca3^i	120.80 (16)	O4^xi—Ca4—O18^xi	55.18 (12)
O12—Se2—Ca3^i	119.99 (17)	O15^viii—Ca4—O18	103.69 (13)
O11—Se2—Ca3^i	76.58 (16)	O15^ix—Ca4—O18	60.84 (12)
O6—Se2—Ca3^i	32.80 (14)	O8^v—Ca4—O18	85.05 (14)
Ca1—Se2—Ca3^i	71.782 (17)	O8^x—Ca4—O18	122.86 (14)
Ca6—Se2—Ca3^i	106.051 (18)	O4—Ca4—O18	55.18 (12)
O18—Se3—O4	105.8 (2)	O4^xi—Ca4—O18	136.25 (13)
O18—Se3—O1	110.5 (2)	O18^xi—Ca4—O18	147.18 (18)
O4—Se3—O1	112.8 (2)	O15^viii—Ca4—Se3	92.01 (9)
O18—Se3—O7	113.2 (2)	O15^ix—Ca4—Se3	88.63 (9)
O4—Se3—O7	111.3 (2)	O8^v—Ca4—Se3	83.09 (11)
O1—Se3—O7	103.5 (2)	O8^x—Ca4—Se3	95.72 (11)
O18—Se3—Ca3	122.02 (18)	O4—Ca4—Se3	26.76 (10)
O4—Se3—Ca3	132.22 (15)	O4^xi—Ca4—Se3	152.38 (11)
O1—Se3—Ca3	52.83 (15)	O18^xi—Ca4—Se3	152.43 (9)
O7—Se3—Ca3	50.96 (14)	O18—Ca4—Se3	28.44 (8)
O18—Se3—Ca4	62.76 (18)	O15^viii—Ca4—Se3^xi	88.63 (9)
O4—Se3—Ca4	43.06 (15)	O15^ix—Ca4—Se3^xi	92.01 (9)
O1—Se3—Ca4	129.44 (15)	O8^v—Ca4—Se3^xi	95.72 (11)
O7—Se3—Ca4	125.83 (15)	O8^x—Ca4—Se3^xi	83.09 (11)
Ca3—Se3—Ca4	174.56 (4)	O4—Ca4—Se3^xi	152.38 (11)
O14—Se4—O10	108.7 (2)	O4^xi—Ca4—Se3^xi	26.76 (10)
O14—Se4—O2	107.9 (2)	O18^xi—Ca4—Se3^xi	28.44 (8)
O10—Se4—O2	112.2 (2)	O18—Ca4—Se3^xi	152.43 (9)
O14—Se4—O15	112.3 (2)	Se3—Ca4—Se3^xi	178.54 (7)
O10—Se4—O15	112.9 (2)	O15^viii—Ca4—Ca6^xii	143.36 (10)
O2—Se4—O15	102.8 (2)	O15^ix—Ca4—Ca6^xii	73.91 (10)
O14—Se4—Ca2^ii	113.69 (16)	O8^v—Ca4—Ca6^xii	38.68 (11)
O10—Se4—Ca2^ii	137.51 (15)	O8^x—Ca4—Ca6^xii	79.86 (12)
O2—Se4—Ca2^ii	50.99 (15)	O4—Ca4—Ca6^xii	121.92 (11)
O15—Se4—Ca2^ii	53.08 (14)	O4^xi—Ca4—Ca6^xii	32.21 (10)
O14—Se4—Ca5^iii	73.53 (16)	O18^xi—Ca4—Ca6^xii	86.84 (8)
O10—Se4—Ca5^iii	35.16 (15)	O18—Ca4—Ca6^xii	112.95 (9)
O2—Se4—Ca5^iii	126.16 (15)	Se3—Ca4—Ca6^xii	120.50 (3)
O15—Se4—Ca5^iii	127.13 (14)	Se3^xi—Ca4—Ca6^xii	58.492 (16)
Ca2^ii—Se4—Ca5^iii	172.53 (3)	O15^viii—Ca4—Ca6^x	73.91 (10)
O13—Ca1—O13^iv	73.0 (2)	O15^ix—Ca4—Ca6^x	143.36 (10)
O13—Ca1—O7^i	154.10 (16)	O8^v—Ca4—Ca6^x	79.86 (12)
O13^iv—Ca1—O7^i	85.12 (15)	O8^x—Ca4—Ca6^x	38.68 (11)
O13—Ca1—O7^v	85.12 (15)	O4—Ca4—Ca6^x	32.21 (10)
O13^iv—Ca1—O7^v	154.10 (16)	O4^xi—Ca4—Ca6^x	121.92 (11)
O7^i—Ca1—O7^v	119.1 (2)	O18^xi—Ca4—Ca6^x	112.95 (9)
O13—Ca1—O6	126.41 (14)	O18—Ca4—Ca6^x	86.84 (8)
O13^iv—Ca1—O6	90.78 (15)	Se3—Ca4—Ca6^x	58.492 (16)
O7^i—Ca1—O6	66.05 (14)	Se3^xi—Ca4—Ca6^x	120.50 (3)
O7^v—Ca1—O6	91.34 (14)	Ca6^xii—Ca4—Ca6^x	107.34 (6)
O13—Ca1—O6^iv	90.78 (15)	O16—Ca5—O2^ii	142.30 (15)
O13^iv—Ca1—O6^iv	126.41 (14)	O16—Ca5—O10^viii	90.97 (16)
O7^i—Ca1—O6^iv	91.34 (14)	O2^ii—Ca5—O10^viii	70.25 (14)
O7^v—Ca1—O6^iv	66.05 (14)	O16—Ca5—O11^iv	71.65 (15)
O6—Ca1—O6^iv	135.6 (2)	O2^ii—Ca5—O11^iv	144.44 (15)
O13—Ca1—O12	68.81 (15)	O10^viii—Ca5—O11^iv	107.87 (15)
O13^iv—Ca1—O12	75.49 (16)	O16—Ca5—O3	79.18 (15)
O7^i—Ca1—O12	119.43 (13)	O2^ii—Ca5—O3	95.80 (14)
O7^v—Ca1—O12	83.93 (15)	O10^viii—Ca5—O3	142.35 (15)
O6—Ca1—O12	57.67 (13)	O11^iv—Ca5—O3	103.29 (14)
O6^iv—Ca1—O12	145.32 (13)	O16—Ca5—O9^ii	72.13 (14)
O13—Ca1—O12^iv	75.49 (16)	O2^ii—Ca5—O9^ii	72.04 (14)
O13^iv—Ca1—O12^iv	68.81 (15)	O10^viii—Ca5—O9^ii	77.68 (15)
O7^i—Ca1—O12^iv	83.93 (15)	O11^iv—Ca5—O9^ii	143.41 (15)
O7^v—Ca1—O12^iv	119.43 (13)	O3—Ca5—O9^ii	64.69 (14)
O6—Ca1—O12^iv	145.32 (13)	O16—Ca5—O1	140.10 (15)
O6^iv—Ca1—O12^iv	57.67 (13)	O2^ii—Ca5—O1	74.07 (14)
O12—Ca1—O12^iv	135.3 (2)	O10^viii—Ca5—O1	89.25 (15)
O13—Ca1—Se2	97.89 (11)	O11^iv—Ca5—O1	70.38 (14)
O13^iv—Ca1—Se2	83.44 (11)	O3—Ca5—O1	121.31 (14)
O7^i—Ca1—Se2	93.02 (10)	O9^ii—Ca5—O1	146.06 (14)
O7^v—Ca1—Se2	86.15 (10)	O16—Ca5—O5	122.09 (15)
O6—Ca1—Se2	28.63 (9)	O2^ii—Ca5—O5	84.08 (13)
O6^iv—Ca1—Se2	150.10 (10)	O10^viii—Ca5—O5	146.50 (15)
O12—Ca1—Se2	29.08 (9)	O11^iv—Ca5—O5	80.64 (14)
O12^iv—Ca1—Se2	152.23 (10)	O3—Ca5—O5	58.94 (13)
O13—Ca1—Se2^iv	83.44 (11)	O9^ii—Ca5—O5	115.16 (14)
O13^iv—Ca1—Se2^iv	97.89 (11)	O1—Ca5—O5	62.53 (13)
O7^i—Ca1—Se2^iv	86.15 (10)	O16—Ca5—Se1	99.21 (12)
O7^v—Ca1—Se2^iv	93.02 (10)	O2^ii—Ca5—Se1	92.69 (10)
O6—Ca1—Se2^iv	150.10 (10)	O10^viii—Ca5—Se1	161.63 (11)
O6^iv—Ca1—Se2^iv	28.63 (9)	O11^iv—Ca5—Se1	89.91 (11)
O12—Ca1—Se2^iv	152.23 (10)	O3—Ca5—Se1	29.11 (9)
O12^iv—Ca1—Se2^iv	29.08 (9)	O9^ii—Ca5—Se1	90.87 (10)
Se2—Ca1—Se2^iv	178.36 (6)	O1—Ca5—Se1	92.58 (10)
O13—Ca1—Ca3^i	142.06 (12)	O5—Ca5—Se1	30.06 (8)
O13^iv—Ca1—Ca3^i	75.75 (11)	O16—Ca5—Se4^viii	76.12 (12)
O7^i—Ca1—Ca3^i	36.38 (10)	O2^ii—Ca5—Se4^viii	92.48 (10)
O7^v—Ca1—Ca3^i	117.61 (12)	O10^viii—Ca5—Se4^viii	23.02 (10)
O6—Ca1—Ca3^i	33.44 (9)	O11^iv—Ca5—Se4^viii	86.38 (11)
O6^iv—Ca1—Ca3^i	125.43 (11)	O3—Ca5—Se4^viii	149.04 (10)
O12—Ca1—Ca3^i	83.07 (9)	O9^ii—Ca5—Se4^viii	89.91 (10)
O12^iv—Ca1—Ca3^i	112.18 (10)	O1—Ca5—Se4^viii	89.65 (10)
Se2—Ca1—Ca3^i	57.332 (14)	O5—Ca5—Se4^viii	151.88 (9)
Se2^iv—Ca1—Ca3^i	122.01 (2)	Se1—Ca5—Se4^viii	174.77 (4)
O13—Ca1—Ca3	75.75 (11)	O16—Ca5—Ca2^viii	114.41 (12)
O13^iv—Ca1—Ca3	142.06 (12)	O2^ii—Ca5—Ca2^viii	36.06 (10)
O7^i—Ca1—Ca3	117.61 (12)	O10^viii—Ca5—Ca2^viii	35.65 (10)
O7^v—Ca1—Ca3	36.38 (10)	O11^iv—Ca5—Ca2^viii	139.03 (11)
O6—Ca1—Ca3	125.43 (11)	O3—Ca5—Ca2^viii	117.68 (10)
O6^iv—Ca1—Ca3	33.44 (9)	O9^ii—Ca5—Ca2^viii	63.74 (10)
O12—Ca1—Ca3	112.18 (10)	O1—Ca5—Ca2^viii	87.42 (10)
O12^iv—Ca1—Ca3	83.07 (9)	O5—Ca5—Ca2^viii	119.69 (9)
Se2—Ca1—Ca3	122.01 (2)	Se1—Ca5—Ca2^viii	126.15 (4)
Se2^iv—Ca1—Ca3	57.332 (14)	Se4^viii—Ca5—Ca2^viii	58.66 (3)
Ca3^i—Ca1—Ca3	140.57 (6)	O16—Ca5—Ca2^ii	81.05 (12)
O18^v—Ca2—O12	75.73 (17)	O2^ii—Ca5—Ca2^ii	75.04 (10)
O18^v—Ca2—O9	78.92 (16)	O10^viii—Ca5—Ca2^ii	108.73 (11)
O12—Ca2—O9	117.81 (16)	O11^iv—Ca5—Ca2^ii	134.14 (11)
O18^v—Ca2—O19	136.05 (18)	O3—Ca5—Ca2^ii	34.12 (10)
O12—Ca2—O19	68.23 (19)	O9^ii—Ca5—Ca2^ii	32.41 (10)
O9—Ca2—O19	96.12 (19)	O1—Ca5—Ca2^ii	135.99 (10)
O18^v—Ca2—O10	147.35 (16)	O5—Ca5—Ca2^ii	83.84 (9)
O12—Ca2—O10	136.34 (17)	Se1—Ca5—Ca2^ii	58.49 (3)
O9—Ca2—O10	78.88 (14)	Se4^viii—Ca5—Ca2^ii	122.28 (4)
O19—Ca2—O10	70.11 (17)	Ca2^viii—Ca5—Ca2^ii	85.65 (2)
O18^v—Ca2—O3^vi	74.79 (15)	O17—Ca6—O14^xiii	145.10 (11)
O12—Ca2—O3^vi	149.04 (17)	O17—Ca6—O14^vi	145.10 (10)
O9—Ca2—O3^vi	64.97 (14)	O14^xiii—Ca6—O14^vi	69.8 (2)
O19—Ca2—O3^vi	142.34 (17)	O17—Ca6—O4^iv	77.24 (11)
O10—Ca2—O3^vi	74.24 (14)	O14^xiii—Ca6—O4^iv	72.30 (14)
O18^v—Ca2—O2^vi	128.07 (16)	O14^vi—Ca6—O4^iv	131.79 (15)
O12—Ca2—O2^vi	93.19 (16)	O17—Ca6—O4^xiv	77.24 (11)
O9—Ca2—O2^vi	144.70 (15)	O14^xiii—Ca6—O4^xiv	131.79 (15)
O19—Ca2—O2^vi	79.26 (18)	O14^vi—Ca6—O4^xiv	72.30 (14)
O10—Ca2—O2^vi	66.56 (13)	O4^iv—Ca6—O4^xiv	154.5 (2)
O3^vi—Ca2—O2^vi	97.56 (14)	O17—Ca6—O11^xv	107.60 (10)
O18^v—Ca2—O15^vi	67.86 (15)	O14^xiii—Ca6—O11^xv	72.48 (14)
O12—Ca2—O15^vi	79.16 (15)	O14^vi—Ca6—O11^xv	78.75 (15)
O9—Ca2—O15^vi	137.75 (15)	O4^iv—Ca6—O11^xv	116.44 (13)
O19—Ca2—O15^vi	125.86 (18)	O4^xiv—Ca6—O11^xv	71.84 (14)
O10—Ca2—O15^vi	116.76 (13)	O17—Ca6—O11	107.60 (10)
O3^vi—Ca2—O15^vi	81.21 (13)	O14^xiii—Ca6—O11	78.75 (15)
O2^vi—Ca2—O15^vi	60.22 (13)	O14^vi—Ca6—O11	72.48 (14)
O18^v—Ca2—O13	79.48 (15)	O4^iv—Ca6—O11	71.84 (14)
O12—Ca2—O13	63.92 (14)	O4^xiv—Ca6—O11	116.44 (13)
O9—Ca2—O13	56.07 (13)	O11^xv—Ca6—O11	144.8 (2)
O19—Ca2—O13	62.71 (17)	O17—Ca6—O8^xv	74.64 (10)
O10—Ca2—O13	106.98 (13)	O14^xiii—Ca6—O8^xv	77.09 (14)
O3^vi—Ca2—O13	118.86 (13)	O14^vi—Ca6—O8^xv	131.14 (14)
O2^vi—Ca2—O13	140.45 (14)	O4^iv—Ca6—O8^xv	64.39 (13)
O15^vi—Ca2—O13	135.68 (13)	O4^xiv—Ca6—O8^xv	108.37 (13)
O18^v—Ca2—Se4^vi	97.96 (12)	O11^xv—Ca6—O8^xv	57.21 (13)
O12—Ca2—Se4^vi	81.32 (12)	O11—Ca6—O8^xv	134.57 (13)
O9—Ca2—Se4^vi	158.48 (11)	O17—Ca6—O8	74.64 (10)
O19—Ca2—Se4^vi	100.53 (15)	O14^xiii—Ca6—O8	131.14 (14)
O10—Ca2—Se4^vi	94.03 (10)	O14^vi—Ca6—O8	77.09 (14)
O3^vi—Ca2—Se4^vi	93.59 (10)	O4^iv—Ca6—O8	108.37 (13)
O2^vi—Ca2—Se4^vi	30.31 (9)	O4^xiv—Ca6—O8	64.39 (13)
O15^vi—Ca2—Se4^vi	30.50 (9)	O11^xv—Ca6—O8	134.57 (13)
O13—Ca2—Se4^vi	144.81 (9)	O11—Ca6—O8	57.21 (13)
O18^v—Ca2—Se1	75.74 (12)	O8^xv—Ca6—O8	149.3 (2)
O12—Ca2—Se1	91.37 (12)	O17—Ca6—Se2^xv	92.85 (3)
O9—Ca2—Se1	27.04 (10)	O14^xiii—Ca6—Se2^xv	70.67 (11)
O19—Ca2—Se1	80.72 (15)	O14^vi—Ca6—Se2^xv	104.44 (11)
O10—Ca2—Se1	94.37 (10)	O4^iv—Ca6—Se2^xv	89.73 (10)
O3^vi—Ca2—Se1	90.38 (10)	O4^xiv—Ca6—Se2^xv	91.53 (10)
O2^vi—Ca2—Se1	156.12 (10)	O11^xv—Ca6—Se2^xv	28.57 (9)
O15^vi—Ca2—Se1	143.60 (10)	O11—Ca6—Se2^xv	148.01 (10)
O13—Ca2—Se1	29.16 (8)	O8^xv—Ca6—Se2^xv	28.76 (9)
Se4^vi—Ca2—Se1	171.42 (4)	O8—Ca6—Se2^xv	154.55 (9)
O18^v—Ca2—Ca5^iii	144.05 (12)	O17—Ca6—Se2	92.85 (3)
O12—Ca2—Ca5^iii	122.77 (13)	O14^xiii—Ca6—Se2	104.44 (11)
O9—Ca2—Ca5^iii	110.87 (11)	O14^vi—Ca6—Se2	70.67 (11)
O19—Ca2—Ca5^iii	78.78 (14)	O4^iv—Ca6—Se2	91.53 (10)
O10—Ca2—Ca5^iii	34.10 (9)	O4^xiv—Ca6—Se2	89.73 (10)
O3^vi—Ca2—Ca5^iii	78.57 (10)	O11^xv—Ca6—Se2	148.01 (10)
O2^vi—Ca2—Ca5^iii	33.83 (10)	O11—Ca6—Se2	28.57 (9)
O15^vi—Ca2—Ca5^iii	84.67 (9)	O8^xv—Ca6—Se2	154.55 (9)
O13—Ca2—Ca5^iii	135.36 (10)	O8—Ca6—Se2	28.76 (9)
Se4^vi—Ca2—Ca5^iii	59.93 (3)	Se2^xv—Ca6—Se2	174.30 (6)
Se1—Ca2—Ca5^iii	128.45 (4)	O17—Ca6—Ca4^xvi	76.61 (3)
O5^v—Ca3—O5	111.7 (2)	O14^xiii—Ca6—Ca4^xvi	68.54 (10)
O5^v—Ca3—O6^iv	162.92 (16)	O14^vi—Ca6—Ca4^xvi	138.23 (11)
O5—Ca3—O6^iv	84.58 (15)	O4^iv—Ca6—Ca4^xvi	31.75 (10)
O5^v—Ca3—O6^vii	84.58 (15)	O4^xiv—Ca6—Ca4^xvi	138.42 (11)
O5—Ca3—O6^vii	162.92 (16)	O11^xv—Ca6—Ca4^xvi	86.08 (9)
O6^iv—Ca3—O6^vii	79.9 (2)	O11—Ca6—Ca4^xvi	102.04 (9)
O5^v—Ca3—O7^v	121.18 (14)	O8^xv—Ca6—Ca4^xvi	32.93 (9)
O5—Ca3—O7^v	81.74 (14)	O8—Ca6—Ca4^xvi	135.77 (10)
O6^iv—Ca3—O7^v	64.66 (13)	Se2^xv—Ca6—Ca4^xvi	58.318 (15)
O6^vii—Ca3—O7^v	85.26 (14)	Se2—Ca6—Ca4^xvi	123.247 (17)
O5^v—Ca3—O7	81.74 (14)	Se3—O1—Ca5	126.8 (2)
O5—Ca3—O7	121.18 (14)	Se3—O1—Ca3	97.63 (18)
O6^iv—Ca3—O7	85.26 (14)	Ca5—O1—Ca3	108.90 (15)
O6^vii—Ca3—O7	64.66 (13)	Se4—O2—Ca5^vi	131.5 (2)
O7^v—Ca3—O7	141.10 (19)	Se4—O2—Ca2^ii	98.70 (19)
O5^v—Ca3—O1	83.10 (15)	Ca5^vi—O2—Ca2^ii	110.12 (16)
O5—Ca3—O1	66.13 (14)	Se1—O3—Ca5	103.68 (19)
O6^iv—Ca3—O1	99.60 (13)	Se1—O3—Ca2^ii	124.9 (2)
O6^vii—Ca3—O1	123.34 (12)	Ca5—O3—Ca2^ii	112.25 (16)
O7^v—Ca3—O1	145.85 (13)	Se3—O4—Ca4	110.2 (2)
O7—Ca3—O1	58.91 (12)	Se3—O4—Ca6^x	131.8 (2)
O5^v—Ca3—O1^v	66.13 (14)	Ca4—O4—Ca6^x	116.04 (16)
O5—Ca3—O1^v	83.10 (15)	Se1—O5—Ca3	143.3 (2)
O6^iv—Ca3—O1^v	123.34 (12)	Se1—O5—Ca5	92.22 (18)
O6^vii—Ca3—O1^v	99.60 (13)	Ca3—O5—Ca5	109.51 (15)
O7^v—Ca3—O1^v	58.91 (12)	Se2—O6—Ca3^i	125.5 (2)
O7—Ca3—O1^v	145.85 (13)	Se2—O6—Ca1	103.4 (2)
O1—Ca3—O1^v	124.30 (19)	Ca3^i—O6—Ca1	110.90 (15)
O5^v—Ca3—Se3	79.08 (10)	Se3—O7—Ca1^vii	136.4 (2)
O5—Ca3—Se3	94.48 (10)	Se3—O7—Ca3	99.52 (18)
O6^iv—Ca3—Se3	94.90 (10)	Ca1^vii—O7—Ca3	110.96 (16)
O6^vii—Ca3—Se3	93.82 (10)	Se2—O8—Ca4^xiv	137.0 (3)
O7^v—Ca3—Se3	159.42 (10)	Se2—O8—Ca6	95.37 (19)
O7—Ca3—Se3	29.52 (9)	Ca4^xiv—O8—Ca6	108.39 (15)
O1—Ca3—Se3	29.53 (8)	Se1—O9—Ca2	110.2 (2)
O1^v—Ca3—Se3	141.03 (10)	Se1—O9—Ca5^vi	135.0 (2)
O5^v—Ca3—Se3^v	94.48 (10)	Ca2—O9—Ca5^vi	114.40 (17)
O5—Ca3—Se3^v	79.08 (10)	Se4—O10—Ca5^iii	121.8 (2)
O6^iv—Ca3—Se3^v	93.82 (10)	Se4—O10—Ca2	127.9 (2)
O6^vii—Ca3—Se3^v	94.90 (10)	Ca5^iii—O10—Ca2	110.25 (15)
O7^v—Ca3—Se3^v	29.52 (9)	Se2—O11—Ca5^iv	136.7 (2)
O7—Ca3—Se3^v	159.42 (10)	Se2—O11—Ca6	101.4 (2)
O1—Ca3—Se3^v	141.03 (10)	Ca5^iv—O11—Ca6	120.54 (17)
O1^v—Ca3—Se3^v	29.53 (8)	Se2—O12—Ca2	145.5 (3)
Se3—Ca3—Se3^v	168.62 (6)	Se2—O12—Ca1	95.0 (2)
O5^v—Ca3—Se2^iv	155.20 (10)	Ca2—O12—Ca1	113.67 (17)
O5—Ca3—Se2^iv	74.93 (11)	Se1—O13—Ca1	137.9 (2)
O6^iv—Ca3—Se2^iv	21.68 (10)	Se1—O13—Ca2	87.76 (18)
O6^vii—Ca3—Se2^iv	92.57 (11)	Ca1—O13—Ca2	108.78 (16)
O7^v—Ca3—Se2^iv	82.96 (10)	Se4—O14—Ca6^ii	142.7 (2)
O7—Ca3—Se2^iv	74.84 (10)	Se4—O15—Ca4^iii	132.1 (2)
O1—Ca3—Se2^iv	77.94 (9)	Se4—O15—Ca2^ii	96.42 (18)
O1^v—Ca3—Se2^iv	138.39 (9)	Ca4^iii—O15—Ca2^ii	121.81 (16)
Se3—Ca3—Se2^iv	76.534 (18)	Se3—O18—Ca2^v	147.7 (3)
Se3^v—Ca3—Se2^iv	110.32 (2)	Se3—O18—Ca4	88.80 (19)
O5^v—Ca3—Se2^vii	74.93 (11)	Ca2^v—O18—Ca4	104.98 (16)

Symmetry codes: (i) −x+y+1, −x+2, z+1/3; (ii) −y+1, x−y+1, z−1/3; (iii) −y+1, x−y+1, z+2/3; (iv) x−y+1, −y+2, −z+1/3; (v) y, x, −z; (vi) −x+y, −x+1, z+1/3; (vii) −y+2, x−y+1, z−1/3; (viii) −x+y, −x+1, z−2/3; (ix) −x+1, −x+y, −z−1/3; (x) x, y, z−1; (xi) y, x, −z−1; (xii) −y+2, x−y+1, z−4/3; (xiii) y, x+1, −z+1; (xiv) x, y, z+1; (xv) x−y+1, −y+2, −z+4/3; (xvi) −x+y+1, −x+2, z+4/3.