Buy article online - an online subscription or single-article purchase is required to access this article.
Structure analysis using single-crystal diffraction was carried out as a contribution to the dispute about the nature of the water channel structure of bassanite (CaSO4·0.5H2O). A recent result of Weiss & Bräu (2009) for the crystal structure of bassanite (monoclinic, space group C2) at ambient conditions of air humidity was confirmed. In the presence of high relative air humidity the crystal structure of bassanite transformed due to the incorporation of additional water of hydration. The crystal structure of CaSO4·0.625H2O was solved by single-crystal diffraction at 298 K and 75% relative air humidity. The experimental results provided an insight into both crystal structures. A model explaining the phase transition from CaSO4·0.625H2O to CaSO4·0.5H2O was derived. The monoclinic cell setting of CaSO4·0.5H2O and the trigonal cell setting of CaSO4·0.625H2O were confirmed by powder diffraction.
Supporting information
(type here to add preparation details)
(type here to add refinement 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.
Crystal data top
CaH1.25O4.625S | Dx = 2.773 Mg m−3 |
Mr = 147.40 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3221 | Cell parameters from 943 reflections |
Hall symbol: P 32 2" | θ = 1–27.5° |
a = 13.8690 (4) Å | µ = 2.24 mm−1 |
c = 12.7189 (1) Å | T = 296 K |
V = 2118.70 (9) Å3 | Needle, colourless |
Z = 24 | 0.4 × 0.08 × 0.07 mm |
F(000) = 1782 | |
Data collection top
Bruker X8 Kappa. Apex2 diffractometer | 3252 independent reflections |
Radiation source: fine-focus sealed tube | 2578 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.043 |
ω and phi scans | θmax = 27.5°, θmin = 1.6° |
Absorption correction: numerical ? | h = −17→17 |
Tmin = 0.641, Tmax = 0.896 | k = −17→17 |
38925 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.039 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.108 | w = 1/[σ2(Fo2) + (0.0478P)2 + 2.072P] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.027 |
3252 reflections | Δρmax = 0.53 e Å−3 |
260 parameters | Δρmin = −0.45 e Å−3 |
5 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
0 constraints | Absolute structure parameter: 0.00 |
Primary atom site location: structure-invariant direct methods | |
Crystal data top
CaH1.25O4.625S | Z = 24 |
Mr = 147.40 | Mo Kα radiation |
Trigonal, P3221 | µ = 2.24 mm−1 |
a = 13.8690 (4) Å | T = 296 K |
c = 12.7189 (1) Å | 0.4 × 0.08 × 0.07 mm |
V = 2118.70 (9) Å3 | |
Data collection top
Bruker X8 Kappa. Apex2 diffractometer | 3252 independent reflections |
Absorption correction: numerical ? | 2578 reflections with I > 2σ(I) |
Tmin = 0.641, Tmax = 0.896 | Rint = 0.043 |
38925 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.039 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.108 | Δρmax = 0.53 e Å−3 |
S = 1.03 | Δρmin = −0.45 e Å−3 |
3252 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
260 parameters | Absolute structure parameter: 0.00 |
5 restraints | |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | |
S1 | 0.50186 (8) | 0.77388 (9) | 0.08244 (7) | 0.0099 (3) | |
S2 | 0.77410 (9) | 0.99600 (8) | 0.41478 (8) | 0.0103 (2) | |
S3 | 0.72701 (9) | 0.72106 (9) | −0.24660 (7) | 0.0096 (2) | |
S4 | 0.21741 (9) | 0.72177 (9) | 0.24212 (7) | 0.0100 (2) | |
Ca1 | 0.76903 (10) | 1.0000 | 0.1667 | 0.0126 (4) | |
Ca2 | 0.49029 (7) | 0.77610 (8) | 0.33088 (6) | 0.0142 (2) | |
Ca3 | 0.74268 (9) | 0.74268 (9) | 0.0000 | 0.0122 (3) | |
Ca4 | 0.71424 (9) | 0.71424 (9) | −0.5000 | 0.0148 (3) | |
Ca5 | 0.50256 (6) | 0.77197 (8) | −0.16455 (6) | 0.0135 (2) | |
Ca6 | 0.78358 (10) | 1.0000 | 0.6667 | 0.0123 (3) | |
O1 | 0.6334 (2) | 0.6938 (2) | −0.1736 (2) | 0.0160 (6) | |
O2 | 0.1951 (2) | 0.6233 (2) | 0.1778 (2) | 0.0166 (6) | |
O3 | 0.4352 (3) | 0.7974 (2) | 0.0072 (2) | 0.0169 (6) | |
O4 | 0.7339 (3) | 0.7999 (2) | −0.3272 (2) | 0.0169 (7) | |
O5 | 0.5663 (2) | 0.7355 (3) | 0.0209 (2) | 0.0206 (7) | |
O6 | 0.8680 (3) | 1.0603 (2) | 0.3412 (2) | 0.0164 (6) | |
O7 | 0.8289 (2) | 0.7705 (3) | −0.1815 (2) | 0.0175 (7) | |
O8 | 0.7927 (2) | 0.9169 (2) | 0.4753 (2) | 0.0180 (7) | |
O9 | 0.4298 (2) | 0.6907 (2) | 0.1594 (2) | 0.0151 (7) | |
O10 | 0.2966 (2) | 0.7407 (3) | 0.3266 (2) | 0.0167 (7) | |
O11 | 0.7664 (3) | 1.0720 (2) | 0.4902 (2) | 0.0163 (7) | |
O12 | 0.6738 (2) | 0.9397 (3) | 0.3496 (2) | 0.0178 (7) | |
O13 | 0.5778 (3) | 0.8753 (2) | 0.1423 (2) | 0.0187 (7) | |
O14 | 0.1128 (3) | 0.7027 (3) | 0.2901 (2) | 0.0200 (7) | |
O15 | 0.2623 (3) | 0.8162 (2) | 0.1692 (2) | 0.0171 (7) | |
O16 | 0.5018 (3) | 0.9431 (3) | −0.1888 (3) | 0.0336 (9) | |
O17 | 0.9508 (4) | 1.0000 | 0.6667 | 0.0560 (18) | |
O18 | 0.7094 (3) | 0.6206 (2) | −0.3009 (2) | 0.0199 (7) | |
O19 | 0.4803 (4) | 0.9522 (4) | 0.2989 (5) | 0.0663 (15) | |
H1 | 0.453 (7) | 0.985 (7) | 0.258 (5) | 0.099* | |
H2 | 0.545 (3) | 0.982 (6) | 0.277 (6) | 0.099* | |
H3 | 0.564 (3) | 0.993 (5) | −0.205 (6) | 0.099* | |
H4 | 0.457 (6) | 0.966 (7) | −0.181 (6) | 0.099* | |
H5 | 1.005 (4) | 1.060 (3) | 0.678 (7) | 0.099* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
S1 | 0.0110 (6) | 0.0113 (5) | 0.0065 (5) | 0.0050 (4) | −0.0002 (4) | −0.0002 (4) |
S2 | 0.0128 (5) | 0.0122 (6) | 0.0063 (5) | 0.0066 (5) | 0.0001 (4) | 0.0002 (4) |
S3 | 0.0118 (5) | 0.0128 (5) | 0.0061 (5) | 0.0074 (5) | 0.0005 (3) | −0.0007 (3) |
S4 | 0.0119 (5) | 0.0120 (5) | 0.0067 (5) | 0.0066 (4) | 0.0004 (4) | −0.0006 (4) |
Ca1 | 0.0162 (7) | 0.0130 (7) | 0.0076 (6) | 0.0065 (4) | −0.0002 (2) | −0.0004 (5) |
Ca2 | 0.0138 (5) | 0.0189 (6) | 0.0082 (4) | 0.0071 (5) | −0.0005 (4) | −0.0012 (3) |
Ca3 | 0.0154 (4) | 0.0154 (4) | 0.0074 (5) | 0.0088 (5) | −0.0001 (2) | 0.0001 (2) |
Ca4 | 0.0187 (5) | 0.0187 (5) | 0.0115 (6) | 0.0129 (6) | 0.0008 (2) | −0.0008 (2) |
Ca5 | 0.0134 (5) | 0.0148 (7) | 0.0102 (4) | 0.0054 (5) | −0.0003 (3) | −0.0013 (3) |
Ca6 | 0.0139 (5) | 0.0130 (8) | 0.0097 (6) | 0.0065 (4) | 0.0001 (2) | 0.0003 (5) |
O1 | 0.0150 (14) | 0.0203 (16) | 0.0126 (15) | 0.0087 (13) | 0.0053 (12) | 0.0009 (13) |
O2 | 0.0187 (16) | 0.0169 (15) | 0.0154 (14) | 0.0097 (13) | 0.0007 (13) | −0.0063 (13) |
O3 | 0.0199 (17) | 0.0231 (16) | 0.0073 (13) | 0.0104 (14) | −0.0038 (12) | −0.0006 (12) |
O4 | 0.0250 (18) | 0.0208 (17) | 0.0063 (14) | 0.0125 (15) | −0.0013 (12) | 0.0032 (12) |
O5 | 0.0184 (17) | 0.035 (2) | 0.0128 (15) | 0.0163 (16) | 0.0010 (13) | −0.0057 (13) |
O6 | 0.0167 (16) | 0.0199 (16) | 0.0113 (14) | 0.0083 (13) | 0.0039 (12) | 0.0015 (12) |
O7 | 0.0160 (15) | 0.0281 (18) | 0.0111 (14) | 0.0130 (14) | −0.0037 (11) | −0.0029 (13) |
O8 | 0.0185 (16) | 0.0187 (16) | 0.0192 (15) | 0.0112 (14) | 0.0018 (13) | 0.0058 (13) |
O9 | 0.0158 (16) | 0.0171 (16) | 0.0052 (13) | 0.0028 (13) | 0.0040 (12) | 0.0046 (11) |
O10 | 0.0214 (16) | 0.0265 (19) | 0.0056 (14) | 0.0145 (15) | −0.0035 (11) | −0.0002 (13) |
O11 | 0.0229 (18) | 0.0194 (17) | 0.0103 (14) | 0.0133 (15) | 0.0005 (12) | −0.0021 (12) |
O12 | 0.0155 (15) | 0.0173 (17) | 0.0165 (15) | 0.0051 (14) | −0.0072 (12) | −0.0016 (13) |
O13 | 0.0207 (17) | 0.0133 (16) | 0.0174 (16) | 0.0050 (15) | −0.0063 (12) | −0.0069 (13) |
O14 | 0.0131 (16) | 0.0230 (18) | 0.0239 (17) | 0.0091 (14) | 0.0101 (13) | 0.0043 (14) |
O15 | 0.0277 (18) | 0.0183 (16) | 0.0108 (15) | 0.0156 (15) | 0.0035 (12) | 0.0054 (12) |
O16 | 0.022 (2) | 0.026 (2) | 0.051 (2) | 0.0103 (18) | 0.0043 (18) | 0.0107 (17) |
O17 | 0.023 (2) | 0.022 (3) | 0.123 (6) | 0.0108 (16) | −0.005 (2) | −0.011 (4) |
O18 | 0.0257 (18) | 0.0156 (16) | 0.0200 (16) | 0.0116 (14) | 0.0021 (14) | −0.0047 (12) |
O19 | 0.039 (3) | 0.047 (3) | 0.093 (4) | 0.006 (2) | 0.017 (3) | −0.015 (3) |
Geometric parameters (Å, º) top
S1—O9 | 1.461 (3) | Ca3—O1 | 2.570 (3) |
S1—O5 | 1.473 (3) | Ca3—O1v | 2.570 (3) |
S1—O3 | 1.476 (3) | Ca3—S3v | 3.1479 (9) |
S1—O13 | 1.478 (3) | Ca3—Ca1vii | 4.0074 (7) |
S1—Ca5 | 3.1416 (11) | Ca4—O15viii | 2.403 (3) |
S1—Ca2 | 3.1649 (12) | Ca4—O15ix | 2.403 (3) |
S2—O8 | 1.465 (3) | Ca4—O4 | 2.448 (3) |
S2—O12 | 1.465 (3) | Ca4—O4x | 2.448 (3) |
S2—O11 | 1.467 (3) | Ca4—O8xi | 2.475 (3) |
S2—O6 | 1.484 (3) | Ca4—O8v | 2.475 (3) |
S2—Ca1 | 3.1576 (10) | Ca4—O18x | 2.831 (3) |
S2—Ca6 | 3.2058 (10) | Ca4—O18 | 2.831 (3) |
S3—O18 | 1.461 (3) | Ca4—S3x | 3.2267 (9) |
S3—O4 | 1.467 (3) | Ca4—Ca6xi | 4.1610 (8) |
S3—O7 | 1.478 (3) | Ca4—Ca6xii | 4.1611 (8) |
S3—O1 | 1.483 (3) | Ca5—O16 | 2.398 (4) |
S3—Ca3 | 3.1479 (9) | Ca5—O10viii | 2.403 (3) |
S3—Ca4 | 3.2267 (9) | Ca5—O2i | 2.433 (3) |
S4—O10 | 1.463 (3) | Ca5—O11iii | 2.453 (3) |
S4—O15 | 1.466 (3) | Ca5—O3 | 2.469 (3) |
S4—O14 | 1.471 (3) | Ca5—O9i | 2.486 (3) |
S4—O2 | 1.487 (3) | Ca5—O1 | 2.539 (3) |
S4—Ca2i | 3.1154 (12) | Ca5—O5 | 2.654 (3) |
S4—Ca5ii | 3.3097 (12) | Ca5—O14viii | 3.059 (3) |
Ca1—O13iii | 2.353 (3) | Ca5—S4viii | 3.3097 (12) |
Ca1—O13 | 2.353 (3) | Ca5—Ca2viii | 4.0094 (12) |
Ca1—O7iv | 2.390 (3) | Ca6—O17 | 2.319 (6) |
Ca1—O7v | 2.390 (3) | Ca6—O14vi | 2.400 (3) |
Ca1—O6 | 2.523 (3) | Ca6—O14xiii | 2.400 (3) |
Ca1—O6iii | 2.523 (3) | Ca6—O4iii | 2.504 (3) |
Ca1—O12 | 2.598 (3) | Ca6—O4xiv | 2.504 (3) |
Ca1—O12iii | 2.598 (3) | Ca6—O11xv | 2.516 (3) |
Ca1—S2iii | 3.1576 (10) | Ca6—O11 | 2.516 (3) |
Ca1—Ca3iv | 4.0074 (7) | Ca6—O8xv | 2.723 (3) |
Ca1—Ca3 | 4.0074 (7) | Ca6—O8 | 2.723 (3) |
Ca2—O9 | 2.423 (3) | Ca6—S2xv | 3.2058 (10) |
Ca2—O12 | 2.431 (3) | Ca6—Ca4xvi | 4.1611 (8) |
Ca2—O18v | 2.438 (3) | O2—Ca5vi | 2.433 (3) |
Ca2—O10 | 2.479 (3) | O2—Ca2i | 2.549 (3) |
Ca2—O15vi | 2.510 (3) | O3—Ca2i | 2.560 (3) |
Ca2—O19 | 2.548 (6) | O4—Ca6xi | 2.504 (3) |
Ca2—O2vi | 2.549 (3) | O6—Ca3iv | 2.414 (3) |
Ca2—O3vi | 2.560 (3) | O7—Ca1vii | 2.390 (3) |
Ca2—O13 | 2.730 (3) | O8—Ca4xiv | 2.475 (3) |
Ca2—S4vi | 3.1154 (12) | O9—Ca5vi | 2.486 (3) |
Ca2—Ca5ii | 4.0094 (12) | O10—Ca5ii | 2.403 (3) |
Ca3—O5 | 2.413 (3) | O11—Ca5iii | 2.453 (3) |
Ca3—O5v | 2.413 (3) | O14—Ca6i | 2.400 (3) |
Ca3—O6iii | 2.414 (3) | O14—Ca5ii | 3.059 (3) |
Ca3—O6vii | 2.414 (3) | O15—Ca4ii | 2.403 (3) |
Ca3—O7v | 2.539 (3) | O15—Ca2i | 2.510 (3) |
Ca3—O7 | 2.539 (3) | O18—Ca2v | 2.438 (3) |
| | | |
O9—S1—O5 | 111.69 (19) | O7—Ca3—Ca1 | 121.30 (7) |
O9—S1—O3 | 110.64 (18) | O1—Ca3—Ca1 | 117.93 (7) |
O5—S1—O3 | 107.13 (17) | O1v—Ca3—Ca1 | 87.16 (6) |
O9—S1—O13 | 106.69 (18) | S3—Ca3—Ca1 | 125.67 (3) |
O5—S1—O13 | 110.20 (18) | S3v—Ca3—Ca1 | 59.839 (19) |
O3—S1—O13 | 110.53 (19) | Ca1vii—Ca3—Ca1 | 121.20 (5) |
O9—S1—Ca5 | 131.83 (12) | O15viii—Ca4—O15ix | 133.50 (16) |
O5—S1—Ca5 | 57.34 (12) | O15viii—Ca4—O4 | 78.96 (10) |
O3—S1—Ca5 | 50.06 (12) | O15ix—Ca4—O4 | 115.28 (9) |
O13—S1—Ca5 | 121.27 (13) | O15viii—Ca4—O4x | 115.28 (9) |
O9—S1—Ca2 | 47.23 (11) | O15ix—Ca4—O4x | 78.96 (10) |
O5—S1—Ca2 | 125.26 (13) | O4—Ca4—O4x | 145.27 (15) |
O3—S1—Ca2 | 127.24 (13) | O15viii—Ca4—O8xi | 76.05 (10) |
O13—S1—Ca2 | 59.48 (13) | O15ix—Ca4—O8xi | 149.65 (11) |
Ca5—S1—Ca2 | 177.23 (4) | O4—Ca4—O8xi | 71.57 (10) |
O8—S2—O12 | 111.95 (18) | O4x—Ca4—O8xi | 81.13 (10) |
O8—S2—O11 | 107.33 (17) | O15viii—Ca4—O8v | 149.65 (11) |
O12—S2—O11 | 111.24 (19) | O15ix—Ca4—O8v | 76.05 (10) |
O8—S2—O6 | 110.52 (18) | O4—Ca4—O8v | 81.13 (10) |
O12—S2—O6 | 106.10 (17) | O4x—Ca4—O8v | 71.57 (10) |
O11—S2—O6 | 109.72 (17) | O8xi—Ca4—O8v | 76.04 (14) |
O8—S2—Ca1 | 123.50 (13) | O15viii—Ca4—O18x | 64.58 (9) |
O12—S2—Ca1 | 54.55 (12) | O15ix—Ca4—O18x | 103.82 (9) |
O11—S2—Ca1 | 129.07 (12) | O4—Ca4—O18x | 138.87 (9) |
O6—S2—Ca1 | 51.71 (12) | O4x—Ca4—O18x | 52.46 (9) |
O8—S2—Ca6 | 57.79 (12) | O8xi—Ca4—O18x | 81.33 (9) |
O12—S2—Ca6 | 126.50 (13) | O8v—Ca4—O18x | 122.04 (9) |
O11—S2—Ca6 | 49.58 (12) | O15viii—Ca4—O18 | 103.82 (9) |
O6—S2—Ca6 | 127.10 (13) | O15ix—Ca4—O18 | 64.58 (9) |
Ca1—S2—Ca6 | 178.27 (3) | O4—Ca4—O18 | 52.46 (9) |
O18—S3—O4 | 107.32 (18) | O4x—Ca4—O18 | 138.87 (9) |
O18—S3—O7 | 111.83 (18) | O8xi—Ca4—O18 | 122.04 (9) |
O4—S3—O7 | 110.80 (19) | O8v—Ca4—O18 | 81.33 (9) |
O18—S3—O1 | 110.19 (19) | O18x—Ca4—O18 | 152.10 (13) |
O4—S3—O1 | 110.49 (18) | O15viii—Ca4—S3 | 91.36 (7) |
O7—S3—O1 | 106.25 (16) | O15ix—Ca4—S3 | 90.54 (7) |
O18—S3—Ca3 | 122.15 (13) | O4—Ca4—S3 | 25.55 (7) |
O4—S3—Ca3 | 130.52 (12) | O4x—Ca4—S3 | 151.30 (7) |
O7—S3—Ca3 | 52.62 (11) | O8xi—Ca4—S3 | 96.15 (7) |
O1—S3—Ca3 | 53.89 (12) | O8v—Ca4—S3 | 80.01 (7) |
O18—S3—Ca4 | 61.29 (13) | O18x—Ca4—S3 | 155.78 (6) |
O4—S3—Ca4 | 46.04 (12) | O18—Ca4—S3 | 26.92 (6) |
O7—S3—Ca4 | 126.81 (12) | O15viii—Ca4—S3x | 90.54 (7) |
O1—S3—Ca4 | 126.11 (12) | O15ix—Ca4—S3x | 91.36 (7) |
Ca3—S3—Ca4 | 176.55 (4) | O4—Ca4—S3x | 151.30 (7) |
O10—S4—O15 | 111.06 (19) | O4x—Ca4—S3x | 25.55 (7) |
O10—S4—O14 | 108.16 (18) | O8xi—Ca4—S3x | 80.01 (7) |
O15—S4—O14 | 111.27 (18) | O8v—Ca4—S3x | 96.15 (7) |
O10—S4—O2 | 111.22 (18) | O18x—Ca4—S3x | 26.92 (6) |
O15—S4—O2 | 105.85 (17) | O18—Ca4—S3x | 155.78 (6) |
O14—S4—O2 | 109.29 (19) | S3—Ca4—S3x | 175.18 (6) |
O10—S4—Ca2i | 135.05 (13) | O15viii—Ca4—Ca6xi | 69.69 (7) |
O15—S4—Ca2i | 52.53 (12) | O15ix—Ca4—Ca6xi | 144.51 (7) |
O14—S4—Ca2i | 116.80 (14) | O4—Ca4—Ca6xi | 33.26 (7) |
O2—S4—Ca2i | 54.22 (12) | O4x—Ca4—Ca6xi | 118.88 (8) |
O10—S4—Ca5ii | 40.89 (12) | O8xi—Ca4—Ca6xi | 38.93 (7) |
O15—S4—Ca5ii | 127.46 (12) | O8v—Ca4—Ca6xi | 81.12 (8) |
O14—S4—Ca5ii | 67.28 (13) | O18x—Ca4—Ca6xi | 111.29 (6) |
O2—S4—Ca5ii | 124.69 (12) | O18—Ca4—Ca6xi | 85.54 (6) |
Ca2i—S4—Ca5ii | 175.88 (4) | S3—Ca4—Ca6xi | 58.67 (2) |
O13iii—Ca1—O13 | 81.10 (16) | S3x—Ca4—Ca6xi | 118.04 (3) |
O13iii—Ca1—O7iv | 81.17 (11) | O15viii—Ca4—Ca6xii | 144.52 (7) |
O13—Ca1—O7iv | 156.98 (11) | O15ix—Ca4—Ca6xii | 69.69 (7) |
O13iii—Ca1—O7v | 156.98 (12) | O4—Ca4—Ca6xii | 118.88 (8) |
O13—Ca1—O7v | 81.17 (11) | O4x—Ca4—Ca6xii | 33.26 (7) |
O7iv—Ca1—O7v | 119.39 (17) | O8xi—Ca4—Ca6xii | 81.12 (8) |
O13iii—Ca1—O6 | 89.35 (10) | O8v—Ca4—Ca6xii | 38.93 (7) |
O13—Ca1—O6 | 125.89 (10) | O18x—Ca4—Ca6xii | 85.54 (6) |
O7iv—Ca1—O6 | 68.39 (9) | O18—Ca4—Ca6xii | 111.29 (6) |
O7v—Ca1—O6 | 89.23 (10) | S3—Ca4—Ca6xii | 118.04 (3) |
O13iii—Ca1—O6iii | 125.89 (10) | S3x—Ca4—Ca6xii | 58.67 (2) |
O13—Ca1—O6iii | 89.35 (10) | Ca6xi—Ca4—Ca6xii | 107.43 (5) |
O7iv—Ca1—O6iii | 89.23 (10) | O16—Ca5—O10viii | 96.00 (13) |
O7v—Ca1—O6iii | 68.39 (9) | O16—Ca5—O2i | 141.21 (11) |
O6—Ca1—O6iii | 135.55 (14) | O10viii—Ca5—O2i | 71.62 (10) |
O13iii—Ca1—O12 | 78.20 (10) | O16—Ca5—O11iii | 70.83 (11) |
O13—Ca1—O12 | 71.14 (10) | O10viii—Ca5—O11iii | 112.87 (10) |
O7iv—Ca1—O12 | 119.04 (9) | O2i—Ca5—O11iii | 147.97 (11) |
O7v—Ca1—O12 | 82.24 (10) | O16—Ca5—O3 | 77.50 (12) |
O6—Ca1—O12 | 54.78 (9) | O10viii—Ca5—O3 | 143.29 (10) |
O6iii—Ca1—O12 | 147.07 (9) | O2i—Ca5—O3 | 90.83 (10) |
O13iii—Ca1—O12iii | 71.14 (10) | O11iii—Ca5—O3 | 99.18 (10) |
O13—Ca1—O12iii | 78.20 (10) | O16—Ca5—O9i | 68.74 (11) |
O7iv—Ca1—O12iii | 82.24 (10) | O10viii—Ca5—O9i | 76.34 (10) |
O7v—Ca1—O12iii | 119.04 (9) | O2i—Ca5—O9i | 72.59 (11) |
O6—Ca1—O12iii | 147.07 (9) | O11iii—Ca5—O9i | 139.28 (12) |
O6iii—Ca1—O12iii | 54.78 (9) | O3—Ca5—O9i | 67.58 (9) |
O12—Ca1—O12iii | 139.36 (14) | O16—Ca5—O1 | 140.73 (11) |
O13iii—Ca1—S2 | 84.34 (8) | O10viii—Ca5—O1 | 87.73 (11) |
O13—Ca1—S2 | 98.38 (8) | O2i—Ca5—O1 | 76.89 (10) |
O7iv—Ca1—S2 | 94.36 (7) | O11iii—Ca5—O1 | 71.76 (10) |
O7v—Ca1—S2 | 83.83 (7) | O3—Ca5—O1 | 120.20 (9) |
O6—Ca1—S2 | 27.50 (7) | O9i—Ca5—O1 | 148.70 (11) |
O6iii—Ca1—S2 | 149.71 (8) | O16—Ca5—O5 | 117.98 (13) |
O12—Ca1—S2 | 27.34 (6) | O10viii—Ca5—O5 | 145.97 (12) |
O12iii—Ca1—S2 | 155.48 (7) | O2i—Ca5—O5 | 81.86 (10) |
O13iii—Ca1—S2iii | 98.38 (8) | O11iii—Ca5—O5 | 79.32 (10) |
O13—Ca1—S2iii | 84.34 (8) | O3—Ca5—O5 | 55.02 (9) |
O7iv—Ca1—S2iii | 83.83 (7) | O9i—Ca5—O5 | 116.02 (9) |
O7v—Ca1—S2iii | 94.36 (7) | O1—Ca5—O5 | 65.30 (9) |
O6—Ca1—S2iii | 149.71 (8) | O16—Ca5—O14viii | 64.30 (12) |
O6iii—Ca1—S2iii | 27.50 (7) | O10viii—Ca5—O14viii | 49.82 (9) |
O12—Ca1—S2iii | 155.48 (7) | O2i—Ca5—O14viii | 120.55 (9) |
O12iii—Ca1—S2iii | 27.34 (6) | O11iii—Ca5—O14viii | 66.59 (9) |
S2—Ca1—S2iii | 176.44 (6) | O3—Ca5—O14viii | 141.69 (10) |
O13iii—Ca1—Ca3iv | 73.04 (8) | O9i—Ca5—O14viii | 99.36 (9) |
O13—Ca1—Ca3iv | 146.08 (8) | O1—Ca5—O14viii | 90.11 (9) |
O7iv—Ca1—Ca3iv | 36.86 (6) | O5—Ca5—O14viii | 143.14 (9) |
O7v—Ca1—Ca3iv | 116.28 (9) | O16—Ca5—S1 | 96.82 (11) |
O6—Ca1—Ca3iv | 34.84 (7) | O10viii—Ca5—S1 | 158.52 (8) |
O6iii—Ca1—Ca3iv | 123.57 (7) | O2i—Ca5—S1 | 87.66 (7) |
O12—Ca1—Ca3iv | 82.21 (6) | O11iii—Ca5—S1 | 87.65 (7) |
O12iii—Ca1—Ca3iv | 112.43 (7) | O3—Ca5—S1 | 27.28 (7) |
S2—Ca1—Ca3iv | 58.134 (19) | O9i—Ca5—S1 | 92.40 (7) |
S2iii—Ca1—Ca3iv | 120.39 (2) | O1—Ca5—S1 | 93.15 (7) |
O13iii—Ca1—Ca3 | 146.08 (8) | O5—Ca5—S1 | 27.84 (6) |
O13—Ca1—Ca3 | 73.04 (8) | O14viii—Ca5—S1 | 151.54 (7) |
O7iv—Ca1—Ca3 | 116.28 (9) | O16—Ca5—S4viii | 80.28 (11) |
O7v—Ca1—Ca3 | 36.86 (6) | O10viii—Ca5—S4viii | 23.48 (7) |
O6—Ca1—Ca3 | 123.57 (7) | O2i—Ca5—S4viii | 94.75 (7) |
O6iii—Ca1—Ca3 | 34.84 (7) | O11iii—Ca5—S4viii | 91.15 (7) |
O12—Ca1—Ca3 | 112.43 (7) | O3—Ca5—S4viii | 150.76 (8) |
O12iii—Ca1—Ca3 | 82.21 (6) | O9i—Ca5—S4viii | 86.77 (7) |
S2—Ca1—Ca3 | 120.39 (2) | O1—Ca5—S4viii | 88.99 (7) |
S2iii—Ca1—Ca3 | 58.134 (19) | O5—Ca5—S4viii | 154.22 (7) |
Ca3iv—Ca1—Ca3 | 138.53 (5) | O14viii—Ca5—S4viii | 26.34 (5) |
O9—Ca2—O12 | 119.30 (10) | S1—Ca5—S4viii | 177.09 (4) |
O9—Ca2—O18v | 79.31 (11) | O16—Ca5—Ca2viii | 117.10 (10) |
O12—Ca2—O18v | 74.95 (11) | O10viii—Ca5—Ca2viii | 35.41 (7) |
O9—Ca2—O10 | 78.91 (11) | O2i—Ca5—Ca2viii | 37.42 (7) |
O12—Ca2—O10 | 135.44 (12) | O11iii—Ca5—Ca2viii | 144.37 (7) |
O18v—Ca2—O10 | 149.05 (11) | O3—Ca5—Ca2viii | 116.39 (7) |
O9—Ca2—O15vi | 138.73 (12) | O9i—Ca5—Ca2viii | 63.73 (8) |
O12—Ca2—O15vi | 78.32 (10) | O1—Ca5—Ca2viii | 87.69 (7) |
O18v—Ca2—O15vi | 69.47 (10) | O5—Ca5—Ca2viii | 118.68 (7) |
O10—Ca2—O15vi | 116.02 (9) | O14viii—Ca5—Ca2viii | 85.22 (6) |
O9—Ca2—O19 | 98.84 (16) | S1—Ca5—Ca2viii | 123.14 (3) |
O12—Ca2—O19 | 69.78 (14) | S4viii—Ca5—Ca2viii | 58.88 (2) |
O18v—Ca2—O19 | 138.16 (13) | O17—Ca6—O14vi | 142.47 (8) |
O10—Ca2—O19 | 67.24 (13) | O17—Ca6—O14xiii | 142.47 (8) |
O15vi—Ca2—O19 | 122.41 (15) | O14vi—Ca6—O14xiii | 75.06 (15) |
O9—Ca2—O2vi | 145.53 (10) | O17—Ca6—O4iii | 73.79 (8) |
O12—Ca2—O2vi | 92.53 (10) | O14vi—Ca6—O4iii | 139.11 (11) |
O18v—Ca2—O2vi | 124.96 (10) | O14xiii—Ca6—O4iii | 71.75 (11) |
O10—Ca2—O2vi | 68.46 (9) | O17—Ca6—O4xiv | 73.79 (8) |
O15vi—Ca2—O2vi | 55.50 (9) | O14vi—Ca6—O4xiv | 71.75 (11) |
O19—Ca2—O2vi | 78.99 (14) | O14xiii—Ca6—O4xiv | 139.11 (12) |
O9—Ca2—O3vi | 67.08 (9) | O4iii—Ca6—O4xiv | 147.58 (16) |
O12—Ca2—O3vi | 150.16 (11) | O17—Ca6—O11xv | 107.03 (7) |
O18v—Ca2—O3vi | 78.18 (10) | O14vi—Ca6—O11xv | 77.19 (10) |
O10—Ca2—O3vi | 73.21 (11) | O14xiii—Ca6—O11xv | 75.95 (11) |
O15vi—Ca2—O3vi | 80.34 (10) | O4iii—Ca6—O11xv | 116.05 (9) |
O19—Ca2—O3vi | 139.98 (13) | O4xiv—Ca6—O11xv | 74.00 (10) |
O2vi—Ca2—O3vi | 92.33 (10) | O17—Ca6—O11 | 107.03 (7) |
O9—Ca2—O13 | 54.08 (9) | O14vi—Ca6—O11 | 75.95 (11) |
O12—Ca2—O13 | 67.76 (9) | O14xiii—Ca6—O11 | 77.19 (10) |
O18v—Ca2—O13 | 80.02 (11) | O4iii—Ca6—O11 | 74.00 (10) |
O10—Ca2—O13 | 104.18 (10) | O4xiv—Ca6—O11 | 116.05 (9) |
O15vi—Ca2—O13 | 139.16 (9) | O11xv—Ca6—O11 | 145.94 (15) |
O19—Ca2—O13 | 66.41 (14) | O17—Ca6—O8xv | 75.04 (7) |
O2vi—Ca2—O13 | 144.21 (11) | O14vi—Ca6—O8xv | 128.05 (10) |
O3vi—Ca2—O13 | 119.88 (9) | O14xiii—Ca6—O8xv | 78.06 (10) |
O9—Ca2—S4vi | 156.10 (8) | O4iii—Ca6—O8xv | 66.67 (9) |
O12—Ca2—S4vi | 81.61 (8) | O4xiv—Ca6—O8xv | 104.59 (9) |
O18v—Ca2—S4vi | 96.87 (8) | O11xv—Ca6—O8xv | 53.41 (9) |
O10—Ca2—S4vi | 94.23 (7) | O11—Ca6—O8xv | 138.36 (9) |
O15vi—Ca2—S4vi | 27.62 (7) | O17—Ca6—O8 | 75.04 (7) |
O19—Ca2—S4vi | 99.48 (13) | O14vi—Ca6—O8 | 78.06 (10) |
O2vi—Ca2—S4vi | 28.24 (7) | O14xiii—Ca6—O8 | 128.05 (10) |
O3vi—Ca2—S4vi | 89.02 (7) | O4iii—Ca6—O8 | 104.59 (9) |
O13—Ca2—S4vi | 149.03 (7) | O4xiv—Ca6—O8 | 66.67 (9) |
O9—Ca2—S1 | 26.28 (7) | O11xv—Ca6—O8 | 138.36 (9) |
O12—Ca2—S1 | 94.14 (7) | O11—Ca6—O8 | 53.41 (9) |
O18v—Ca2—S1 | 77.83 (8) | O8xv—Ca6—O8 | 150.08 (13) |
O10—Ca2—S1 | 91.80 (7) | O17—Ca6—S2xv | 91.85 (3) |
O15vi—Ca2—S1 | 147.29 (7) | O14vi—Ca6—S2xv | 102.22 (8) |
O19—Ca2—S1 | 82.94 (13) | O14xiii—Ca6—S2xv | 74.75 (8) |
O2vi—Ca2—S1 | 157.21 (7) | O4iii—Ca6—S2xv | 91.48 (7) |
O3vi—Ca2—S1 | 92.64 (7) | O4xiv—Ca6—S2xv | 89.56 (7) |
O13—Ca2—S1 | 27.80 (6) | O11xv—Ca6—S2xv | 26.35 (7) |
S4vi—Ca2—S1 | 173.97 (4) | O11—Ca6—S2xv | 151.30 (7) |
O9—Ca2—Ca5ii | 110.31 (8) | O8xv—Ca6—S2xv | 27.07 (6) |
O12—Ca2—Ca5ii | 122.55 (8) | O8—Ca6—S2xv | 155.11 (7) |
O18v—Ca2—Ca5ii | 144.27 (8) | O17—Ca6—S2 | 91.85 (3) |
O10—Ca2—Ca5ii | 34.17 (6) | O14vi—Ca6—S2 | 74.75 (8) |
O15vi—Ca2—Ca5ii | 83.22 (6) | O14xiii—Ca6—S2 | 102.22 (8) |
O19—Ca2—Ca5ii | 75.99 (11) | O4iii—Ca6—S2 | 89.56 (7) |
O2vi—Ca2—Ca5ii | 35.43 (7) | O4xiv—Ca6—S2 | 91.48 (7) |
O3vi—Ca2—Ca5ii | 74.81 (7) | O11xv—Ca6—S2 | 151.30 (7) |
O13—Ca2—Ca5ii | 134.14 (8) | O11—Ca6—S2 | 26.35 (7) |
S4vi—Ca2—Ca5ii | 60.06 (2) | O8xv—Ca6—S2 | 155.11 (7) |
S1—Ca2—Ca5ii | 125.96 (3) | O8—Ca6—S2 | 27.07 (6) |
O5—Ca3—O5v | 116.35 (16) | S2xv—Ca6—S2 | 176.29 (6) |
O5—Ca3—O6iii | 81.27 (10) | O17—Ca6—Ca4xvi | 75.81 (2) |
O5v—Ca3—O6iii | 161.06 (11) | O14vi—Ca6—Ca4xvi | 140.96 (8) |
O5—Ca3—O6vii | 161.06 (11) | O14xiii—Ca6—Ca4xvi | 67.18 (8) |
O5v—Ca3—O6vii | 81.27 (10) | O4iii—Ca6—Ca4xvi | 32.41 (6) |
O6iii—Ca3—O6vii | 82.33 (14) | O4xiv—Ca6—Ca4xvi | 135.02 (8) |
O5—Ca3—O7v | 80.28 (10) | O11xv—Ca6—Ca4xvi | 84.29 (7) |
O5v—Ca3—O7v | 119.82 (9) | O11—Ca6—Ca4xvi | 104.07 (7) |
O6iii—Ca3—O7v | 67.78 (9) | O8xv—Ca6—Ca4xvi | 34.81 (6) |
O6vii—Ca3—O7v | 84.80 (10) | O8—Ca6—Ca4xvi | 133.98 (7) |
O5—Ca3—O7 | 119.82 (9) | S2xv—Ca6—Ca4xvi | 59.099 (19) |
O5v—Ca3—O7 | 80.28 (10) | S2—Ca6—Ca4xvi | 121.97 (2) |
O6iii—Ca3—O7 | 84.80 (10) | S3—O1—Ca5 | 129.88 (17) |
O6vii—Ca3—O7 | 67.78 (9) | S3—O1—Ca3 | 98.32 (14) |
O7v—Ca3—O7 | 143.71 (14) | Ca5—O1—Ca3 | 107.55 (10) |
O5—Ca3—O1 | 68.38 (9) | S4—O2—Ca5vi | 135.82 (18) |
O5v—Ca3—O1 | 85.32 (10) | S4—O2—Ca2i | 97.54 (15) |
O6iii—Ca3—O1 | 95.73 (9) | Ca5vi—O2—Ca2i | 107.15 (10) |
O6vii—Ca3—O1 | 122.86 (9) | S1—O3—Ca5 | 102.66 (15) |
O7v—Ca3—O1 | 146.71 (9) | S1—O3—Ca2i | 129.33 (17) |
O7—Ca3—O1 | 55.24 (9) | Ca5—O3—Ca2i | 108.84 (11) |
O5—Ca3—O1v | 85.32 (10) | S3—O4—Ca4 | 108.42 (16) |
O5v—Ca3—O1v | 68.38 (9) | S3—O4—Ca6xi | 136.66 (17) |
O6iii—Ca3—O1v | 122.86 (9) | Ca4—O4—Ca6xi | 114.33 (11) |
O6vii—Ca3—O1v | 95.73 (9) | S1—O5—Ca3 | 146.02 (19) |
O7v—Ca3—O1v | 55.24 (9) | S1—O5—Ca5 | 94.82 (14) |
O7—Ca3—O1v | 146.71 (9) | Ca3—O5—Ca5 | 108.76 (11) |
O1—Ca3—O1v | 129.48 (13) | S2—O6—Ca3iv | 130.32 (16) |
O5—Ca3—S3 | 94.90 (7) | S2—O6—Ca1 | 100.79 (15) |
O5v—Ca3—S3 | 80.09 (7) | Ca3iv—O6—Ca1 | 108.51 (10) |
O6iii—Ca3—S3 | 92.02 (7) | S3—O7—Ca1vii | 139.76 (18) |
O6vii—Ca3—S3 | 95.08 (7) | S3—O7—Ca3 | 99.82 (14) |
O7v—Ca3—S3 | 159.67 (7) | Ca1vii—O7—Ca3 | 108.75 (10) |
O7—Ca3—S3 | 27.56 (6) | S2—O8—Ca4xiv | 140.84 (18) |
O1—Ca3—S3 | 27.79 (6) | S2—O8—Ca6 | 95.14 (15) |
O1v—Ca3—S3 | 144.55 (7) | Ca4xiv—O8—Ca6 | 106.26 (10) |
O5—Ca3—S3v | 80.09 (7) | S1—O9—Ca2 | 106.49 (15) |
O5v—Ca3—S3v | 94.90 (7) | S1—O9—Ca5vi | 140.65 (17) |
O6iii—Ca3—S3v | 95.08 (7) | Ca2—O9—Ca5vi | 112.85 (11) |
O6vii—Ca3—S3v | 92.02 (7) | S4—O10—Ca5ii | 115.63 (17) |
O7v—Ca3—S3v | 27.56 (6) | S4—O10—Ca2 | 133.90 (17) |
O7—Ca3—S3v | 159.67 (7) | Ca5ii—O10—Ca2 | 110.43 (11) |
O1—Ca3—S3v | 144.54 (7) | S2—O11—Ca5iii | 141.19 (17) |
O1v—Ca3—S3v | 27.79 (6) | S2—O11—Ca6 | 104.07 (15) |
S3—Ca3—S3v | 170.57 (6) | Ca5iii—O11—Ca6 | 114.53 (11) |
O5—Ca3—Ca1vii | 154.20 (7) | S2—O12—Ca2 | 145.59 (19) |
O5v—Ca3—Ca1vii | 67.51 (7) | S2—O12—Ca1 | 98.11 (15) |
O6iii—Ca3—Ca1vii | 93.62 (8) | Ca2—O12—Ca1 | 109.84 (11) |
O6vii—Ca3—Ca1vii | 36.66 (7) | S1—O13—Ca1 | 140.5 (2) |
O7v—Ca3—Ca1vii | 121.30 (8) | S1—O13—Ca2 | 92.71 (15) |
O7—Ca3—Ca1vii | 34.39 (6) | Ca1—O13—Ca2 | 107.94 (11) |
O1—Ca3—Ca1vii | 87.16 (6) | S4—O14—Ca6i | 145.68 (19) |
O1v—Ca3—Ca1vii | 117.93 (7) | S4—O14—Ca5ii | 86.38 (14) |
S3—Ca3—Ca1vii | 59.84 (2) | Ca6i—O14—Ca5ii | 99.24 (10) |
S3v—Ca3—Ca1vii | 125.67 (3) | S4—O15—Ca4ii | 136.74 (17) |
O5—Ca3—Ca1 | 67.51 (7) | S4—O15—Ca2i | 99.85 (14) |
O5v—Ca3—Ca1 | 154.20 (7) | Ca4ii—O15—Ca2i | 117.70 (11) |
O6iii—Ca3—Ca1 | 36.66 (7) | S3—O18—Ca2v | 146.74 (19) |
O6vii—Ca3—Ca1 | 93.62 (8) | S3—O18—Ca4 | 91.80 (14) |
O7v—Ca3—Ca1 | 34.39 (6) | Ca2v—O18—Ca4 | 105.62 (11) |
Symmetry codes: (i) −y+1, x−y+1, z−1/3; (ii) −y+1, x−y+1, z+2/3; (iii) x−y+1, −y+2, −z+1/3; (iv) −x+y+1, −x+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) y, x, −z−1; (xi) x, y, 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. |
Crystal data top
CaO4.5SH | F(000) = 924 |
Mr = 145.16 | Dx = 2.887 Mg m−3 |
Monoclinic, C2 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C 2y | Cell parameters from 100 reflections |
a = 17.5180 (8) Å | θ = 1–27.5° |
b = 6.9291 (1) Å | µ = 2.25 mm−1 |
c = 12.0344 (2) Å | T = 293 K |
β = 133.655 (4)° | Needle, colourless |
V = 1056.88 (4) Å3 | 0.4 × 0.08 × 0.07 mm |
Z = 12 | |
Data collection top
Bruker X8 Kappa. Apex2 diffractometer | 12774 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.000 |
Graphite monochromator | θmax = 27.5°, θmin = 2.3° |
ω and phi scans | h = −22→22 |
15532 measured reflections | k = −9→9 |
15543 independent reflections | l = −15→15 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0301P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.042 | (Δ/σ)max = 0.006 |
wR(F2) = 0.096 | Δρmax = 0.58 e Å−3 |
S = 0.97 | Δρmin = −0.49 e Å−3 |
15543 reflections | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
193 parameters | Extinction coefficient: 0.00034 (10) |
1 restraint | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.06 (3) |
Crystal data top
CaO4.5SH | V = 1056.88 (4) Å3 |
Mr = 145.16 | Z = 12 |
Monoclinic, C2 | Mo Kα radiation |
a = 17.5180 (8) Å | µ = 2.25 mm−1 |
b = 6.9291 (1) Å | T = 293 K |
c = 12.0344 (2) Å | 0.4 × 0.08 × 0.07 mm |
β = 133.655 (4)° | |
Data collection top
Bruker X8 Kappa. Apex2 diffractometer | 12774 reflections with I > 2σ(I) |
15532 measured reflections | Rint = 0.000 |
15543 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.042 | 1 restraint |
wR(F2) = 0.096 | Δρmax = 0.58 e Å−3 |
S = 0.97 | Δρmin = −0.49 e Å−3 |
15543 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
193 parameters | Absolute structure parameter: 0.06 (3) |
Special details top
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 (Å2) top | x | y | z | Uiso*/Ueq | |
Ca1 | 0.33496 (10) | 0.29588 (13) | 0.57126 (16) | 0.0128 (2) | |
Ca2 | −0.16388 (10) | 0.34101 (14) | 0.05509 (15) | 0.01086 (19) | |
Ca3 | 0.0000 | 0.5050 (3) | 0.5000 | 0.0118 (3) | |
Ca4 | 0.0000 | 0.0014 (3) | 0.0000 | 0.0118 (3) | |
S1 | 0.08626 (12) | 0.3120 (2) | 0.31005 (19) | 0.0102 (3) | |
S2 | 0.24834 (5) | 0.0029 (3) | 0.24705 (7) | 0.0084 (3) | |
S3 | 0.57935 (13) | 0.3338 (2) | 0.80377 (19) | 0.0096 (2) | |
O1 | 0.0134 (3) | 0.3877 (4) | 0.3186 (4) | 0.0125 (7) | |
O2 | 0.0272 (2) | 0.2603 (5) | 0.1521 (4) | 0.0164 (8) | |
O3 | 0.1466 (2) | 0.1475 (4) | 0.4151 (4) | 0.0177 (7) | |
O4 | 0.1659 (2) | 0.4619 (4) | 0.3609 (3) | 0.0141 (6) | |
O5 | 0.1720 (3) | 0.1210 (5) | 0.1076 (4) | 0.0141 (8) | |
O6 | 0.1830 (2) | 0.3859 (6) | 0.7602 (4) | 0.0146 (8) | |
O7 | 0.3192 (3) | 0.1274 (5) | 0.3843 (4) | 0.0146 (8) | |
O8 | 0.6651 (2) | 0.1904 (4) | 0.9036 (4) | 0.0140 (7) | |
O9 | 0.6290 (2) | 0.5187 (4) | 0.8348 (3) | 0.0197 (7) | |
O10 | 0.5120 (3) | 0.3333 (4) | 0.8354 (4) | 0.0165 (8) | |
O11 | 0.5122 (2) | 0.2868 (5) | 0.6418 (4) | 0.0153 (8) | |
O12 | 0.3171 (2) | 0.3751 (6) | 0.7433 (4) | 0.0144 (7) | |
O13 | 0.0000 | 0.1599 (6) | 0.5000 | 0.0355 (12) | |
O14 | −0.1689 (4) | 0.5093 (5) | −0.1181 (5) | 0.0667 (12) | |
H1 | −0.185 (5) | 0.603 (7) | −0.151 (7) | 0.100* | |
H2 | −0.198 (5) | 0.472 (8) | −0.199 (6) | 0.100* | |
H3 | 0.017 (5) | 0.100 (6) | 0.550 (5) | 0.100* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca1 | 0.0062 (3) | 0.0164 (7) | 0.0127 (5) | −0.0001 (4) | 0.0053 (4) | −0.0024 (4) |
Ca2 | 0.0080 (3) | 0.0111 (6) | 0.0109 (4) | −0.0007 (4) | 0.0056 (3) | 0.0005 (3) |
Ca3 | 0.0070 (6) | 0.0190 (8) | 0.0077 (7) | 0.000 | 0.0044 (6) | 0.000 |
Ca4 | 0.0060 (5) | 0.0197 (8) | 0.0076 (7) | 0.000 | 0.0039 (6) | 0.000 |
S1 | 0.0064 (4) | 0.0134 (7) | 0.0092 (6) | −0.0003 (4) | 0.0048 (4) | 0.0005 (4) |
S2 | 0.0032 (6) | 0.0177 (8) | 0.0050 (8) | 0.0009 (2) | 0.0031 (6) | 0.0011 (2) |
S3 | 0.0063 (4) | 0.0130 (7) | 0.0084 (6) | 0.0013 (5) | 0.0045 (4) | 0.0028 (5) |
O1 | 0.0132 (13) | 0.0142 (16) | 0.0117 (13) | −0.0004 (10) | 0.0092 (11) | −0.0024 (10) |
O2 | 0.0094 (15) | 0.0205 (17) | 0.0148 (16) | −0.0002 (11) | 0.0066 (14) | −0.0023 (12) |
O3 | 0.0103 (14) | 0.0188 (15) | 0.0150 (14) | 0.0090 (11) | 0.0053 (12) | 0.0083 (11) |
O4 | 0.0116 (15) | 0.0064 (13) | 0.0208 (14) | −0.0030 (10) | 0.0099 (14) | −0.0024 (10) |
O5 | 0.0088 (14) | 0.0163 (15) | 0.0125 (16) | 0.0044 (11) | 0.0055 (13) | 0.0063 (12) |
O6 | 0.0078 (15) | 0.0190 (18) | 0.0183 (16) | −0.0057 (12) | 0.0095 (14) | −0.0018 (12) |
O7 | 0.0130 (15) | 0.0145 (16) | 0.0137 (16) | −0.0025 (12) | 0.0083 (13) | −0.0062 (12) |
O8 | 0.0011 (12) | 0.0146 (14) | 0.0145 (14) | 0.0028 (10) | 0.0010 (11) | 0.0029 (10) |
O9 | 0.0172 (16) | 0.0176 (14) | 0.0212 (16) | −0.0073 (11) | 0.0120 (14) | −0.0043 (12) |
O10 | 0.0122 (15) | 0.019 (2) | 0.0133 (13) | 0.0029 (10) | 0.0069 (12) | −0.0037 (10) |
O11 | 0.0146 (16) | 0.0134 (16) | 0.0132 (15) | −0.0033 (12) | 0.0078 (14) | −0.0030 (12) |
O12 | 0.0048 (14) | 0.0167 (16) | 0.0171 (15) | 0.0036 (12) | 0.0058 (13) | −0.0011 (13) |
O13 | 0.058 (3) | 0.019 (3) | 0.033 (3) | 0.000 | 0.033 (3) | 0.000 |
O14 | 0.161 (4) | 0.0177 (18) | 0.084 (3) | 0.017 (2) | 0.109 (3) | 0.0137 (16) |
Geometric parameters (Å, º) top
Ca1—O12 | 2.362 (4) | Ca4—O10ii | 2.429 (4) |
Ca1—O7 | 2.375 (4) | Ca4—O10ix | 2.429 (4) |
Ca1—O3i | 2.449 (3) | Ca4—O5v | 2.462 (3) |
Ca1—O4ii | 2.458 (3) | Ca4—O5 | 2.462 (3) |
Ca1—O4 | 2.480 (3) | Ca4—O12ix | 2.629 (3) |
Ca1—O10 | 2.486 (4) | Ca4—O12ii | 2.629 (3) |
Ca1—O11 | 2.594 (3) | Ca4—S2v | 3.1477 (7) |
Ca1—O3 | 2.630 (3) | Ca4—S2 | 3.1477 (7) |
Ca1—S3 | 3.1125 (14) | Ca4—Ca1ix | 4.0514 (19) |
Ca1—S1 | 3.1571 (14) | Ca4—Ca1ii | 4.0514 (19) |
Ca1—Ca4iii | 4.0514 (19) | S1—O1 | 1.447 (4) |
Ca1—Ca3iv | 4.072 (2) | S1—O2 | 1.448 (4) |
Ca2—O14 | 2.336 (3) | S1—O3 | 1.473 (3) |
Ca2—O5v | 2.406 (4) | S1—O4 | 1.491 (3) |
Ca2—O8vi | 2.417 (3) | S2—O5 | 1.475 (4) |
Ca2—O9ii | 2.450 (3) | S2—O7 | 1.477 (4) |
Ca2—O8i | 2.475 (3) | S2—O6ii | 1.502 (4) |
Ca2—O6vii | 2.486 (4) | S2—O12ii | 1.515 (4) |
Ca2—O1 | 2.492 (4) | S2—Ca3iv | 3.1897 (7) |
Ca2—O2 | 2.736 (3) | S3—O9 | 1.446 (4) |
Ca2—O9vi | 2.903 (3) | S3—O11 | 1.457 (4) |
Ca2—S1 | 3.1770 (14) | S3—O10 | 1.468 (4) |
Ca2—S3vi | 3.2558 (15) | S3—O8 | 1.482 (3) |
Ca2—Ca4 | 4.104 (2) | S3—Ca2x | 3.2558 (15) |
Ca3—O13 | 2.392 (5) | O3—Ca1ii | 2.449 (3) |
Ca3—O1vii | 2.488 (3) | O4—Ca1i | 2.458 (3) |
Ca3—O1 | 2.488 (3) | O5—Ca2v | 2.406 (4) |
Ca3—O11viii | 2.503 (4) | O6—S2i | 1.502 (4) |
Ca3—O11i | 2.503 (4) | O6—Ca2vii | 2.486 (4) |
Ca3—O7viii | 2.570 (3) | O7—Ca3iv | 2.570 (3) |
Ca3—O7i | 2.570 (3) | O8—Ca2x | 2.417 (3) |
Ca3—O6vii | 2.628 (3) | O8—Ca2ii | 2.475 (3) |
Ca3—O6 | 2.628 (3) | O9—Ca2i | 2.450 (3) |
Ca3—S2viii | 3.1897 (7) | O9—Ca2x | 2.903 (3) |
Ca3—S2i | 3.1897 (7) | O10—Ca4iii | 2.429 (4) |
Ca3—Ca1i | 4.072 (2) | O11—Ca3iv | 2.503 (4) |
Ca4—O2 | 2.365 (4) | O12—S2i | 1.515 (4) |
Ca4—O2v | 2.365 (4) | O12—Ca4iii | 2.629 (3) |
| | | |
O12—Ca1—O7 | 160.93 (16) | O7viii—Ca3—S2viii | 27.08 (9) |
O12—Ca1—O3i | 78.52 (14) | O7i—Ca3—S2viii | 153.30 (9) |
O7—Ca1—O3i | 118.45 (11) | O6vii—Ca3—S2viii | 27.84 (8) |
O12—Ca1—O4ii | 83.83 (12) | O6—Ca3—S2viii | 151.81 (8) |
O7—Ca1—O4ii | 80.13 (12) | O13—Ca3—S2i | 89.74 (4) |
O3i—Ca1—O4ii | 161.00 (14) | O1vii—Ca3—S2i | 93.82 (8) |
O12—Ca1—O4 | 90.00 (11) | O1—Ca3—S2i | 86.00 (8) |
O7—Ca1—O4 | 89.11 (11) | O11viii—Ca3—S2i | 86.66 (7) |
O3i—Ca1—O4 | 67.43 (10) | O11i—Ca3—S2i | 93.76 (8) |
O4ii—Ca1—O4 | 119.93 (8) | O7viii—Ca3—S2i | 153.30 (9) |
O12—Ca1—O10 | 70.02 (11) | O7i—Ca3—S2i | 27.08 (9) |
O7—Ca1—O10 | 119.28 (13) | O6vii—Ca3—S2i | 151.81 (8) |
O3i—Ca1—O10 | 79.63 (10) | O6—Ca3—S2i | 27.84 (8) |
O4ii—Ca1—O10 | 87.81 (10) | S2viii—Ca3—S2i | 179.47 (7) |
O4—Ca1—O10 | 144.45 (11) | O13—Ca3—Ca1i | 119.67 (2) |
O12—Ca1—O11 | 124.87 (13) | O1vii—Ca3—Ca1i | 149.03 (8) |
O7—Ca1—O11 | 68.19 (12) | O1—Ca3—Ca1i | 57.72 (8) |
O3i—Ca1—O11 | 85.95 (11) | O11viii—Ca3—Ca1i | 91.06 (10) |
O4ii—Ca1—O11 | 98.59 (11) | O11i—Ca3—Ca1i | 37.75 (8) |
O4—Ca1—O11 | 131.39 (10) | O7viii—Ca3—Ca1i | 120.77 (10) |
O10—Ca1—O11 | 55.18 (12) | O7i—Ca3—Ca1i | 33.05 (8) |
O12—Ca1—O3 | 81.79 (12) | O6vii—Ca3—Ca1i | 111.36 (9) |
O7—Ca1—O3 | 82.11 (11) | O6—Ca3—Ca1i | 86.95 (8) |
O3i—Ca1—O3 | 118.64 (9) | S2viii—Ca3—Ca1i | 121.05 (3) |
O4ii—Ca1—O3 | 64.96 (9) | S2i—Ca3—Ca1i | 59.25 (3) |
O4—Ca1—O3 | 55.03 (8) | O2—Ca4—O2v | 81.3 (2) |
O10—Ca1—O3 | 142.86 (9) | O2—Ca4—O10ii | 79.47 (11) |
O11—Ca1—O3 | 148.49 (12) | O2v—Ca4—O10ii | 155.56 (14) |
O12—Ca1—S3 | 97.16 (9) | O2—Ca4—O10ix | 155.56 (14) |
O7—Ca1—S3 | 94.68 (10) | O2v—Ca4—O10ix | 79.47 (11) |
O3i—Ca1—S3 | 79.62 (9) | O10ii—Ca4—O10ix | 122.69 (16) |
O4ii—Ca1—S3 | 95.80 (7) | O2—Ca4—O5v | 70.80 (11) |
O4—Ca1—S3 | 144.15 (8) | O2v—Ca4—O5v | 79.52 (13) |
O10—Ca1—S3 | 27.61 (9) | O10ii—Ca4—O5v | 80.00 (11) |
O11—Ca1—S3 | 27.73 (9) | O10ix—Ca4—O5v | 119.77 (12) |
O3—Ca1—S3 | 160.76 (7) | O2—Ca4—O5 | 79.52 (13) |
O12—Ca1—S1 | 86.44 (9) | O2v—Ca4—O5 | 70.80 (11) |
O7—Ca1—S1 | 84.02 (9) | O10ii—Ca4—O5 | 119.77 (12) |
O3i—Ca1—S1 | 93.39 (8) | O10ix—Ca4—O5 | 80.00 (11) |
O4ii—Ca1—S1 | 92.47 (7) | O5v—Ca4—O5 | 140.65 (18) |
O4—Ca1—S1 | 27.46 (7) | O2—Ca4—O12ix | 126.39 (12) |
O10—Ca1—S1 | 156.30 (9) | O2v—Ca4—O12ix | 84.95 (11) |
O11—Ca1—S1 | 147.58 (10) | O10ii—Ca4—O12ix | 94.43 (12) |
O3—Ca1—S1 | 27.61 (7) | O10ix—Ca4—O12ix | 66.64 (11) |
S3—Ca1—S1 | 171.28 (5) | O5v—Ca4—O12ix | 55.77 (12) |
O12—Ca1—Ca4iii | 37.99 (8) | O5—Ca4—O12ix | 141.87 (11) |
O7—Ca1—Ca4iii | 153.28 (10) | O2—Ca4—O12ii | 84.95 (11) |
O3i—Ca1—Ca4iii | 67.64 (10) | O2v—Ca4—O12ii | 126.39 (12) |
O4ii—Ca1—Ca4iii | 94.04 (8) | O10ii—Ca4—O12ii | 66.64 (11) |
O4—Ca1—Ca4iii | 115.89 (9) | O10ix—Ca4—O12ii | 94.43 (12) |
O10—Ca1—Ca4iii | 34.04 (8) | O5v—Ca4—O12ii | 141.87 (11) |
O11—Ca1—Ca4iii | 87.20 (9) | O5—Ca4—O12ii | 55.77 (12) |
O3—Ca1—Ca4iii | 119.20 (8) | O12ix—Ca4—O12ii | 141.1 (2) |
S3—Ca1—Ca4iii | 59.73 (4) | O2—Ca4—S2v | 97.89 (8) |
S1—Ca1—Ca4iii | 122.46 (4) | O2v—Ca4—S2v | 81.82 (8) |
O12—Ca1—Ca3iv | 147.41 (10) | O10ii—Ca4—S2v | 86.01 (8) |
O7—Ca1—Ca3iv | 36.16 (8) | O10ix—Ca4—S2v | 94.17 (8) |
O3i—Ca1—Ca3iv | 115.26 (8) | O5v—Ca4—S2v | 27.14 (9) |
O4ii—Ca1—Ca3iv | 76.84 (8) | O5—Ca4—S2v | 152.59 (9) |
O4—Ca1—Ca3iv | 122.37 (8) | O12ix—Ca4—S2v | 28.65 (8) |
O10—Ca1—Ca3iv | 83.12 (8) | O12ii—Ca4—S2v | 151.61 (9) |
O11—Ca1—Ca3iv | 36.22 (8) | O2—Ca4—S2 | 81.82 (8) |
O3—Ca1—Ca3iv | 112.28 (9) | O2v—Ca4—S2 | 97.89 (8) |
S3—Ca1—Ca3iv | 59.68 (4) | O10ii—Ca4—S2 | 94.17 (8) |
S1—Ca1—Ca3iv | 120.02 (4) | O10ix—Ca4—S2 | 86.01 (8) |
Ca4iii—Ca1—Ca3iv | 117.13 (3) | O5v—Ca4—S2 | 152.59 (9) |
O14—Ca2—O5v | 69.27 (14) | O5—Ca4—S2 | 27.14 (9) |
O14—Ca2—O8vi | 106.17 (16) | O12ix—Ca4—S2 | 151.61 (9) |
O5v—Ca2—O8vi | 76.47 (11) | O12ii—Ca4—S2 | 28.65 (8) |
O14—Ca2—O9ii | 141.24 (14) | S2v—Ca4—S2 | 179.62 (7) |
O5v—Ca2—O9ii | 73.46 (12) | O2—Ca4—Ca1ix | 146.92 (10) |
O8vi—Ca2—O9ii | 74.38 (10) | O2v—Ca4—Ca1ix | 72.27 (10) |
O14—Ca2—O8i | 71.99 (12) | O10ii—Ca4—Ca1ix | 118.85 (9) |
O5v—Ca2—O8i | 141.22 (10) | O10ix—Ca4—Ca1ix | 34.95 (8) |
O8vi—Ca2—O8i | 113.30 (9) | O5v—Ca4—Ca1ix | 84.86 (8) |
O9ii—Ca2—O8i | 144.75 (13) | O5—Ca4—Ca1ix | 109.05 (9) |
O14—Ca2—O6vii | 142.18 (14) | O12ix—Ca4—Ca1ix | 33.58 (8) |
O5v—Ca2—O6vii | 146.91 (17) | O12ii—Ca4—Ca1ix | 126.80 (11) |
O8vi—Ca2—O6vii | 82.34 (12) | S2v—Ca4—Ca1ix | 59.49 (3) |
O9ii—Ca2—O6vii | 76.54 (12) | S2—Ca4—Ca1ix | 120.66 (3) |
O8i—Ca2—O6vii | 70.88 (13) | O2—Ca4—Ca1ii | 72.27 (10) |
O14—Ca2—O1 | 108.46 (16) | O2v—Ca4—Ca1ii | 146.92 (10) |
O5v—Ca2—O1 | 116.07 (13) | O10ii—Ca4—Ca1ii | 34.95 (8) |
O8vi—Ca2—O1 | 145.37 (9) | O10ix—Ca4—Ca1ii | 118.85 (9) |
O9ii—Ca2—O1 | 78.68 (10) | O5v—Ca4—Ca1ii | 109.05 (9) |
O8i—Ca2—O1 | 78.07 (11) | O5—Ca4—Ca1ii | 84.86 (8) |
O6vii—Ca2—O1 | 70.42 (10) | O12ix—Ca4—Ca1ii | 126.80 (11) |
O14—Ca2—O2 | 76.36 (15) | O12ii—Ca4—Ca1ii | 33.58 (8) |
O5v—Ca2—O2 | 65.53 (11) | S2v—Ca4—Ca1ii | 120.66 (3) |
O8vi—Ca2—O2 | 138.38 (12) | S2—Ca4—Ca1ii | 59.49 (3) |
O9ii—Ca2—O2 | 78.95 (11) | Ca1ix—Ca4—Ca1ii | 138.84 (5) |
O8i—Ca2—O2 | 106.99 (11) | O1—S1—O2 | 108.49 (19) |
O6vii—Ca2—O2 | 121.64 (13) | O1—S1—O3 | 111.41 (18) |
O1—Ca2—O2 | 53.16 (11) | O2—S1—O3 | 112.0 (3) |
O14—Ca2—O9vi | 73.72 (14) | O1—S1—O4 | 109.9 (2) |
O5v—Ca2—O9vi | 100.99 (11) | O2—S1—O4 | 109.19 (19) |
O8vi—Ca2—O9vi | 51.51 (8) | O3—S1—O4 | 105.84 (16) |
O9ii—Ca2—O9vi | 124.64 (9) | O1—S1—Ca1 | 128.33 (17) |
O8i—Ca2—O9vi | 65.78 (10) | O2—S1—Ca1 | 122.85 (16) |
O6vii—Ca2—O9vi | 84.76 (10) | O3—S1—Ca1 | 55.84 (12) |
O1—Ca2—O9vi | 141.37 (12) | O4—S1—Ca1 | 50.09 (10) |
O2—Ca2—O9vi | 149.98 (9) | O1—S1—Ca2 | 49.46 (15) |
O14—Ca2—S1 | 94.05 (13) | O2—S1—Ca2 | 59.25 (14) |
O5v—Ca2—S1 | 90.77 (10) | O3—S1—Ca2 | 124.90 (14) |
O8vi—Ca2—S1 | 149.98 (8) | O4—S1—Ca2 | 128.96 (13) |
O9ii—Ca2—S1 | 75.96 (8) | Ca1—S1—Ca2 | 177.68 (7) |
O8i—Ca2—S1 | 93.76 (9) | O5—S2—O7 | 110.5 (3) |
O6vii—Ca2—S1 | 95.27 (8) | O5—S2—O6ii | 111.48 (18) |
O1—Ca2—S1 | 26.19 (9) | O7—S2—O6ii | 106.99 (17) |
O2—Ca2—S1 | 27.05 (9) | O5—S2—O12ii | 105.81 (18) |
O9vi—Ca2—S1 | 158.41 (7) | O7—S2—O12ii | 110.57 (18) |
O14—Ca2—S3vi | 90.11 (13) | O6ii—S2—O12ii | 111.6 (4) |
O5v—Ca2—S3vi | 88.08 (10) | O5—S2—Ca4 | 49.56 (14) |
O8vi—Ca2—S3vi | 25.16 (8) | O7—S2—Ca4 | 127.19 (15) |
O9ii—Ca2—S3vi | 99.03 (8) | O6ii—S2—Ca4 | 125.67 (13) |
O8i—Ca2—S3vi | 90.20 (8) | O12ii—S2—Ca4 | 56.29 (13) |
O6vii—Ca2—S3vi | 83.10 (8) | O5—S2—Ca3iv | 130.77 (16) |
O1—Ca2—S3vi | 153.28 (9) | O7—S2—Ca3iv | 52.38 (14) |
O2—Ca2—S3vi | 153.13 (9) | O6ii—S2—Ca3iv | 54.79 (13) |
O9vi—Ca2—S3vi | 26.36 (7) | O12ii—S2—Ca3iv | 123.37 (13) |
S1—Ca2—S3vi | 174.98 (6) | Ca4—S2—Ca3iv | 179.43 (2) |
O14—Ca2—Ca4 | 75.04 (10) | O9—S3—O11 | 109.22 (18) |
O5v—Ca2—Ca4 | 32.94 (9) | O9—S3—O10 | 112.6 (2) |
O8vi—Ca2—Ca4 | 105.74 (9) | O11—S3—O10 | 107.2 (2) |
O9ii—Ca2—Ca4 | 67.91 (8) | O9—S3—O8 | 107.0 (2) |
O8i—Ca2—Ca4 | 134.23 (7) | O11—S3—O8 | 111.4 (3) |
O6vii—Ca2—Ca4 | 139.23 (10) | O10—S3—O8 | 109.57 (15) |
O1—Ca2—Ca4 | 83.32 (8) | O9—S3—Ca1 | 121.09 (14) |
O2—Ca2—Ca4 | 33.45 (8) | O11—S3—Ca1 | 55.91 (14) |
O9vi—Ca2—Ca4 | 131.92 (7) | O10—S3—Ca1 | 51.71 (14) |
S1—Ca2—Ca4 | 57.83 (4) | O8—S3—Ca1 | 131.92 (16) |
S3vi—Ca2—Ca4 | 120.86 (4) | O9—S3—Ca2x | 63.06 (13) |
O13—Ca3—O1vii | 70.93 (8) | O11—S3—Ca2x | 124.60 (16) |
O13—Ca3—O1 | 70.93 (8) | O10—S3—Ca2x | 126.94 (16) |
O1vii—Ca3—O1 | 141.86 (16) | O8—S3—Ca2x | 43.90 (13) |
O13—Ca3—O11viii | 141.26 (10) | Ca1—S3—Ca2x | 175.77 (6) |
O1vii—Ca3—O11viii | 70.86 (11) | S1—O1—Ca3 | 143.4 (2) |
O1—Ca3—O11viii | 146.89 (14) | S1—O1—Ca2 | 104.4 (2) |
O13—Ca3—O11i | 141.26 (10) | Ca3—O1—Ca2 | 111.67 (13) |
O1vii—Ca3—O11i | 146.89 (14) | S1—O2—Ca4 | 141.6 (2) |
O1—Ca3—O11i | 70.86 (11) | S1—O2—Ca2 | 93.69 (18) |
O11viii—Ca3—O11i | 77.5 (2) | Ca4—O2—Ca2 | 106.93 (12) |
O13—Ca3—O7viii | 109.26 (9) | S1—O3—Ca1ii | 144.2 (2) |
O1vii—Ca3—O7viii | 75.83 (11) | S1—O3—Ca1 | 96.55 (15) |
O1—Ca3—O7viii | 117.41 (12) | Ca1ii—O3—Ca1 | 107.37 (11) |
O11viii—Ca3—O7viii | 66.75 (10) | S1—O4—Ca1i | 124.97 (16) |
O11i—Ca3—O7viii | 83.12 (13) | S1—O4—Ca1 | 102.46 (14) |
O13—Ca3—O7i | 109.26 (9) | Ca1i—O4—Ca1 | 111.99 (11) |
O1vii—Ca3—O7i | 117.41 (12) | S2—O5—Ca2v | 140.9 (2) |
O1—Ca3—O7i | 75.83 (11) | S2—O5—Ca4 | 103.31 (19) |
O11viii—Ca3—O7i | 83.12 (13) | Ca2v—O5—Ca4 | 114.95 (14) |
O11i—Ca3—O7i | 66.75 (10) | S2i—O6—Ca2vii | 136.6 (2) |
O7viii—Ca3—O7i | 141.48 (19) | S2i—O6—Ca3 | 97.37 (17) |
O13—Ca3—O6vii | 71.69 (11) | Ca2vii—O6—Ca3 | 107.34 (12) |
O1vii—Ca3—O6vii | 99.57 (12) | S2—O7—Ca1 | 143.6 (2) |
O1—Ca3—O6vii | 68.19 (11) | S2—O7—Ca3iv | 100.54 (18) |
O11viii—Ca3—O6vii | 121.14 (12) | Ca1—O7—Ca3iv | 110.79 (14) |
O11i—Ca3—O6vii | 88.45 (11) | S3—O8—Ca2x | 110.94 (17) |
O7viii—Ca3—O6vii | 54.85 (11) | S3—O8—Ca2ii | 132.37 (18) |
O7i—Ca3—O6vii | 141.53 (10) | Ca2x—O8—Ca2ii | 116.67 (12) |
O13—Ca3—O6 | 71.69 (10) | S3—O9—Ca2i | 145.9 (2) |
O1vii—Ca3—O6 | 68.19 (11) | S3—O9—Ca2x | 90.58 (15) |
O1—Ca3—O6 | 99.57 (12) | Ca2i—O9—Ca2x | 101.83 (10) |
O11viii—Ca3—O6 | 88.45 (11) | S3—O10—Ca4iii | 138.4 (2) |
O11i—Ca3—O6 | 121.14 (12) | S3—O10—Ca1 | 100.67 (19) |
O7viii—Ca3—O6 | 141.53 (10) | Ca4iii—O10—Ca1 | 111.01 (13) |
O7i—Ca3—O6 | 54.85 (11) | S3—O11—Ca3iv | 134.1 (2) |
O6vii—Ca3—O6 | 143.4 (2) | S3—O11—Ca1 | 96.36 (19) |
O13—Ca3—S2viii | 89.74 (4) | Ca3iv—O11—Ca1 | 106.03 (12) |
O1vii—Ca3—S2viii | 86.00 (8) | S2i—O12—Ca1 | 140.2 (2) |
O1—Ca3—S2viii | 93.82 (8) | S2i—O12—Ca4iii | 95.06 (17) |
O11viii—Ca3—S2viii | 93.76 (8) | Ca1—O12—Ca4iii | 108.43 (13) |
O11i—Ca3—S2viii | 86.66 (7) | | |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1; (ii) −x+1/2, y−1/2, −z+1; (iii) x+1/2, y+1/2, z+1; (iv) x+1/2, y−1/2, z; (v) −x, y, −z; (vi) x−1, y, z−1; (vii) −x, y, −z+1; (viii) x−1/2, y+1/2, z; (ix) x−1/2, y−1/2, z−1; (x) x+1, y, z+1. |
Experimental details
| (caso40625) | (caso4_05) |
Crystal data |
Chemical formula | CaH1.25O4.625S | CaO4.5SH |
Mr | 147.40 | 145.16 |
Crystal system, space group | Trigonal, P3221 | Monoclinic, C2 |
Temperature (K) | 296 | 293 |
a, b, c (Å) | 13.8690 (4), 13.8690 (4), 12.7189 (1) | 17.5180 (8), 6.9291 (1), 12.0344 (2) |
α, β, γ (°) | 90, 90, 120 | 90, 133.655 (4), 90 |
V (Å3) | 2118.70 (9) | 1056.88 (4) |
Z | 24 | 12 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 2.24 | 2.25 |
Crystal size (mm) | 0.4 × 0.08 × 0.07 | 0.4 × 0.08 × 0.07 |
|
Data collection |
Diffractometer | Bruker X8 Kappa. Apex2 diffractometer | Bruker X8 Kappa. Apex2 diffractometer |
Absorption correction | Numerical | – |
Tmin, Tmax | 0.641, 0.896 | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 38925, 3252, 2578 | 15532, 15543, 12774 |
Rint | 0.043 | 0.000 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.108, 1.03 | 0.042, 0.096, 0.97 |
No. of reflections | 3252 | 15543 |
No. of parameters | 260 | 193 |
No. of restraints | 5 | 1 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | – |
Δρmax, Δρmin (e Å−3) | 0.53, −0.45 | 0.58, −0.49 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 |
Absolute structure parameter | 0.00 | 0.06 (3) |
Subscribe to Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.
The stucture of the title compound, (I), is shown below. Dimensions are available in the archived CIF.
For related literature, see [type here to add references to related literature].