The first quaternary hafnium thiophosphate, tricaesium dihafnium pentaphosphorus octadecasulfide, Cs3Hf2P5S18 was synthesized by reacting HfS2 with an in situ formed melt of Cs2S3, P2S5 and S. The crystal structure is composed of a two-dimensional anionic [Hf2P5S18]3- layer and intervening Cs+ cations. Each of the two independent Hf4+ ions is surrounded by seven S atoms forming a distorted pentagonal bipyramid. The HfS7 polyhedra are connected by an unusual edge- and corner-sharing arrangement of [P2S7] groups and edge-sharing [PS4] tetrahedra into the final double-layered anion.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 180 K
- Mean (S-P) = 0.007 Å
- R factor = 0.041
- wR factor = 0.104
- Data-to-parameter ratio = 16.6
checkCIF/PLATON results
No syntax errors found
Alert level A
DIFF020_ALERT_1_A _diffrn_standards_interval_count and
_diffrn_standards_interval_time are missing. Number of measurements
between standards or time (min) between standards.
PLAT027_ALERT_3_A _diffrn_reflns_theta_full (too) Low ............ 23.12 Deg.
| Author Response: The data were measured on a IPDS-1 with a limited size of the
plate. Because of the extremely large c-axis and the width of the reflection
profiles it was not possible to measure the crystal to higher diffraction
angles. There is no other chance. However, the paper is submitted to Acta
crystallographica E. As far as we know for this journal it is not neccessary
to reach the value of 50 deg. in 2 theta.
|
Alert level B
THETM01_ALERT_3_B The value of sine(theta_max)/wavelength is less than 0.575
Calculated sin(theta_max)/wavelength = 0.5525
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96
Alert level G
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 23.12
From the CIF: _reflns_number_total 4211
Count of symmetry unique reflns 2224
Completeness (_total/calc) 189.34%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 1987
Fraction of Friedel pairs measured 0.893
Are heavy atom types Z>Si present yes
2 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
1 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: CIFTAB in SHELXTL (Bruker, 1998).
tricaesium dihafnium pentaphosphorus octadecasulfide
top
Crystal data top
Cs3Hf2(P2S7)2(PS4) | F(000) = 2688 |
Mr = 1487.64 | Dx = 3.152 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C -2yc | Cell parameters from 8000 reflections |
a = 9.3168 (4) Å | θ = 1.3–23.3° |
b = 9.8985 (6) Å | µ = 11.51 mm−1 |
c = 34.0830 (17) Å | T = 180 K |
β = 94.236 (6)° | Plate, yellow |
V = 3134.6 (3) Å3 | 0.2 × 0.2 × 0.1 mm |
Z = 4 | |
Data collection top
Stoe Image Plate Diffraction System diffractometer | 4211 independent reflections |
Radiation source: fine-focus sealed tube | 4119 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
φ scans | θmax = 23.1°, θmin = 2.4° |
Absorption correction: numerical (X-SHAPE and X-RED32; Stoe & Cie, 1998) | h = −10→10 |
Tmin = 0.120, Tmax = 0.312 | k = −10→10 |
9627 measured reflections | l = −37→37 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0238P)2 + 298.6042P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.041 | (Δ/σ)max = 0.001 |
wR(F2) = 0.104 | Δρmax = 1.82 e Å−3 |
S = 1.15 | Δρmin = −1.87 e Å−3 |
4211 reflections | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
254 parameters | Extinction coefficient: 0.00031 (3) |
2 restraints | Absolute structure: Flack (1983) |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.010 (13) |
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 | |
Hf1 | 0.56305 (8) | 0.41115 (8) | 0.34548 (3) | 0.0134 (2) | |
Hf2 | 0.66761 (7) | 0.29213 (8) | 0.53642 (3) | 0.0122 (2) | |
P1 | 0.5973 (6) | 0.2515 (6) | 0.26157 (16) | 0.0158 (12) | |
P2 | 0.8836 (6) | 0.1871 (5) | 0.32596 (15) | 0.0129 (11) | |
P3 | 0.5879 (5) | 0.3522 (5) | 0.44087 (15) | 0.0114 (11) | |
P4 | 0.9599 (6) | 0.4668 (5) | 0.55559 (15) | 0.0136 (11) | |
P5 | 1.0287 (6) | 0.7216 (5) | 0.62040 (15) | 0.0135 (11) | |
S1 | 0.5236 (7) | 0.1750 (6) | 0.21068 (16) | 0.0280 (14) | |
S2 | 0.5910 (6) | 0.4522 (5) | 0.27014 (16) | 0.0183 (12) | |
S3 | 0.5074 (6) | 0.1804 (5) | 0.31004 (14) | 0.0157 (11) | |
S4 | 0.8247 (6) | 0.2005 (5) | 0.26494 (15) | 0.0181 (11) | |
S5 | 1.1028 (5) | 0.1779 (5) | 0.33151 (16) | 0.0170 (11) | |
S6 | 0.8050 (5) | 0.0076 (5) | 0.34505 (15) | 0.0148 (11) | |
S7 | 0.8302 (6) | 0.3532 (5) | 0.35626 (15) | 0.0164 (11) | |
S8 | 0.4787 (6) | 0.2409 (5) | 0.39774 (14) | 0.0162 (11) | |
S9 | 0.6390 (6) | 0.5234 (5) | 0.41293 (15) | 0.0177 (11) | |
S10 | 0.7611 (5) | 0.2505 (5) | 0.46605 (15) | 0.0143 (11) | |
S11 | 0.4653 (6) | 0.3863 (5) | 0.48743 (15) | 0.0174 (11) | |
S12 | 0.9568 (5) | 0.2629 (5) | 0.54899 (16) | 0.0165 (11) | |
S13 | 0.7608 (5) | 0.5369 (5) | 0.53606 (15) | 0.0135 (11) | |
S14 | 1.1250 (6) | 0.5378 (5) | 0.52590 (16) | 0.0174 (12) | |
S15 | 0.9865 (6) | 0.5071 (5) | 0.61715 (14) | 0.0159 (11) | |
S16 | 0.9323 (5) | 0.8168 (5) | 0.57293 (15) | 0.0145 (11) | |
S17 | 1.2386 (6) | 0.7460 (6) | 0.61166 (15) | 0.0180 (12) | |
S18 | 0.9582 (6) | 0.7748 (6) | 0.67164 (15) | 0.0228 (12) | |
Cs1 | 0.20183 (16) | 0.35539 (15) | 0.24510 (5) | 0.0290 (4) | |
Cs2 | 0.11285 (15) | 0.39023 (14) | 0.43180 (4) | 0.0252 (4) | |
Cs3 | 0.61868 (14) | 0.59948 (14) | 0.63653 (4) | 0.0261 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Hf1 | 0.0144 (5) | 0.0126 (4) | 0.0128 (4) | 0.0030 (4) | −0.0004 (4) | 0.0022 (4) |
Hf2 | 0.0114 (4) | 0.0135 (4) | 0.0116 (4) | −0.0019 (3) | 0.0002 (3) | 0.0000 (3) |
P1 | 0.015 (3) | 0.023 (3) | 0.010 (3) | 0.006 (2) | −0.001 (2) | 0.000 (2) |
P2 | 0.016 (3) | 0.013 (3) | 0.009 (2) | −0.001 (2) | −0.003 (2) | −0.002 (2) |
P3 | 0.013 (3) | 0.012 (2) | 0.010 (2) | 0.003 (2) | 0.000 (2) | −0.002 (2) |
P4 | 0.013 (3) | 0.015 (3) | 0.013 (3) | −0.005 (2) | −0.003 (2) | 0.001 (2) |
P5 | 0.016 (3) | 0.019 (3) | 0.005 (2) | −0.004 (2) | 0.000 (2) | 0.000 (2) |
S1 | 0.035 (4) | 0.036 (3) | 0.012 (3) | 0.006 (3) | −0.005 (3) | 0.000 (2) |
S2 | 0.021 (3) | 0.015 (3) | 0.019 (3) | 0.009 (2) | 0.002 (2) | 0.006 (2) |
S3 | 0.023 (3) | 0.016 (3) | 0.009 (2) | −0.001 (2) | 0.001 (2) | −0.002 (2) |
S4 | 0.017 (3) | 0.026 (3) | 0.012 (3) | 0.006 (2) | 0.004 (2) | 0.001 (2) |
S5 | 0.011 (3) | 0.016 (3) | 0.024 (3) | −0.002 (2) | 0.004 (2) | 0.006 (2) |
S6 | 0.010 (3) | 0.011 (3) | 0.024 (3) | 0.000 (2) | 0.005 (2) | 0.002 (2) |
S7 | 0.011 (3) | 0.018 (3) | 0.020 (3) | 0.006 (2) | −0.003 (2) | −0.005 (2) |
S8 | 0.025 (3) | 0.013 (3) | 0.010 (2) | −0.004 (2) | −0.002 (2) | 0.004 (2) |
S9 | 0.027 (3) | 0.014 (3) | 0.013 (3) | 0.001 (2) | 0.003 (2) | 0.001 (2) |
S10 | 0.013 (3) | 0.018 (3) | 0.012 (2) | 0.004 (2) | 0.004 (2) | 0.002 (2) |
S11 | 0.013 (3) | 0.025 (3) | 0.014 (3) | 0.004 (2) | −0.002 (2) | −0.001 (2) |
S12 | 0.009 (2) | 0.013 (3) | 0.027 (3) | 0.0040 (19) | −0.004 (2) | 0.000 (2) |
S13 | 0.009 (3) | 0.012 (2) | 0.019 (3) | −0.006 (2) | 0.000 (2) | 0.001 (2) |
S14 | 0.018 (3) | 0.014 (3) | 0.021 (3) | −0.002 (2) | 0.008 (2) | 0.000 (2) |
S15 | 0.016 (3) | 0.021 (3) | 0.010 (3) | −0.007 (2) | −0.003 (2) | 0.005 (2) |
S16 | 0.014 (3) | 0.017 (3) | 0.013 (3) | 0.004 (2) | 0.002 (2) | 0.003 (2) |
S17 | 0.013 (3) | 0.028 (3) | 0.013 (3) | −0.011 (2) | 0.000 (2) | 0.000 (2) |
S18 | 0.031 (3) | 0.032 (3) | 0.005 (2) | −0.003 (3) | 0.002 (2) | −0.005 (2) |
Cs1 | 0.0263 (8) | 0.0294 (8) | 0.0302 (8) | −0.0045 (6) | −0.0049 (7) | 0.0040 (6) |
Cs2 | 0.0236 (8) | 0.0270 (8) | 0.0243 (8) | −0.0021 (6) | −0.0023 (6) | −0.0080 (6) |
Cs3 | 0.0238 (8) | 0.0247 (8) | 0.0297 (8) | 0.0031 (6) | 0.0006 (7) | −0.0046 (6) |
Geometric parameters (Å, º) top
Hf1—S7 | 2.554 (5) | S5—Cs1vi | 3.607 (5) |
Hf1—S6i | 2.586 (5) | S5—Cs2vi | 4.008 (6) |
Hf1—S9 | 2.604 (5) | S6—Hf1iii | 2.586 (5) |
Hf1—S8 | 2.615 (5) | S6—Cs2iii | 3.752 (5) |
Hf1—S3 | 2.618 (5) | S6—Cs1iii | 3.783 (5) |
Hf1—S2 | 2.632 (5) | S7—Cs2vi | 3.563 (5) |
Hf1—S5i | 2.713 (5) | S8—Cs2iii | 3.840 (5) |
Hf1—Cs1 | 4.6512 (17) | S8—Cs2 | 3.967 (6) |
Hf2—S14ii | 2.570 (5) | S9—Cs2iv | 3.699 (5) |
Hf2—S13 | 2.574 (5) | S10—Cs2vi | 3.818 (5) |
Hf2—S11 | 2.597 (5) | S10—Cs2iii | 3.969 (5) |
Hf2—S16ii | 2.611 (5) | S11—Cs2 | 3.669 (5) |
Hf2—S17ii | 2.640 (5) | S12—Cs3iii | 3.623 (5) |
Hf2—S10 | 2.644 (5) | S13—Cs3 | 3.812 (5) |
Hf2—S12 | 2.712 (5) | S14—Hf2iv | 2.570 (5) |
Hf2—Cs3 | 4.6190 (16) | S14—Cs2vi | 3.518 (6) |
P1—S1 | 1.969 (8) | S15—Cs3 | 3.654 (6) |
P1—S2 | 2.010 (7) | S16—Hf2iv | 2.611 (5) |
P1—S3 | 2.032 (8) | S16—Cs3iv | 3.872 (5) |
P1—S4 | 2.172 (8) | S17—Hf2iv | 2.640 (5) |
P1—Cs1 | 3.827 (5) | S17—Cs3iv | 3.788 (6) |
P1—Cs1iii | 4.088 (6) | S17—Cs3vi | 3.863 (6) |
P2—S7 | 2.023 (7) | S18—Cs1vii | 3.499 (6) |
P2—S5 | 2.039 (7) | S18—Cs3 | 3.727 (6) |
P2—S6 | 2.046 (7) | S18—Cs3iv | 3.776 (6) |
P2—S4 | 2.115 (7) | Cs1—S18viii | 3.499 (6) |
P3—S9 | 2.017 (7) | Cs1—S5ix | 3.607 (5) |
P3—S10 | 2.037 (7) | Cs1—S4i | 3.650 (6) |
P3—S8 | 2.047 (7) | Cs1—S1i | 3.722 (6) |
P3—S11 | 2.051 (7) | Cs1—S6i | 3.783 (5) |
P4—S14 | 2.028 (8) | Cs1—S4ix | 3.938 (6) |
P4—S12 | 2.031 (7) | Cs1—P1i | 4.088 (6) |
P4—S13 | 2.045 (7) | Cs2—S14ix | 3.518 (6) |
P4—S15 | 2.132 (7) | Cs2—S7ix | 3.563 (5) |
P5—S18 | 1.982 (8) | Cs2—S9ii | 3.699 (5) |
P5—S17 | 2.014 (8) | Cs2—S6i | 3.752 (5) |
P5—S16 | 2.024 (7) | Cs2—S10ix | 3.818 (6) |
P5—S15 | 2.160 (8) | Cs2—S8i | 3.840 (5) |
P5—Cs3iv | 3.864 (6) | Cs2—S10i | 3.969 (5) |
P5—Cs3 | 4.083 (6) | Cs2—S5ix | 4.008 (6) |
S1—Cs3v | 3.534 (6) | Cs3—S1x | 3.534 (6) |
S1—Cs1iii | 3.722 (6) | Cs3—S12i | 3.623 (5) |
S1—Cs1 | 3.751 (6) | Cs3—S18ii | 3.776 (6) |
S2—Cs1 | 3.787 (6) | Cs3—S17ii | 3.788 (6) |
S3—Cs1 | 3.882 (5) | Cs3—S17ix | 3.863 (6) |
S4—Cs1iii | 3.650 (6) | Cs3—P5ii | 3.864 (6) |
S4—Cs1vi | 3.938 (6) | Cs3—S16ii | 3.872 (5) |
S5—Hf1iii | 2.713 (5) | | |
| | | |
S7—Hf1—S6i | 168.37 (16) | S18viii—Cs1—S6i | 154.05 (13) |
S7—Hf1—S9 | 76.73 (17) | S5ix—Cs1—S6i | 61.45 (12) |
S6i—Hf1—S9 | 92.26 (17) | S4i—Cs1—S6i | 53.50 (11) |
S7—Hf1—S8 | 95.50 (18) | S1i—Cs1—S6i | 91.32 (12) |
S6i—Hf1—S8 | 85.17 (17) | S1—Cs1—S6i | 108.39 (12) |
S9—Hf1—S8 | 75.48 (16) | S18viii—Cs1—S2 | 144.52 (13) |
S7—Hf1—S3 | 91.62 (17) | S5ix—Cs1—S2 | 103.75 (12) |
S6i—Hf1—S3 | 99.61 (16) | S4i—Cs1—S2 | 55.90 (11) |
S9—Hf1—S3 | 144.23 (16) | S1i—Cs1—S2 | 104.68 (13) |
S8—Hf1—S3 | 72.10 (16) | S1—Cs1—S2 | 54.33 (12) |
S7—Hf1—S2 | 90.53 (17) | S6i—Cs1—S2 | 61.38 (11) |
S6i—Hf1—S2 | 95.54 (16) | S18viii—Cs1—S3 | 130.79 (12) |
S9—Hf1—S2 | 139.08 (17) | S5ix—Cs1—S3 | 62.50 (12) |
S8—Hf1—S2 | 145.15 (16) | S4i—Cs1—S3 | 96.04 (11) |
S3—Hf1—S2 | 73.44 (16) | S1i—Cs1—S3 | 148.23 (12) |
S7—Hf1—S5i | 95.72 (17) | S1—Cs1—S3 | 52.89 (11) |
S6i—Hf1—S5i | 77.21 (16) | S6i—Cs1—S3 | 62.45 (10) |
S9—Hf1—S5i | 73.02 (16) | S2—Cs1—S3 | 48.30 (11) |
S8—Hf1—S5i | 142.99 (17) | S18viii—Cs1—S4ix | 55.91 (12) |
S3—Hf1—S5i | 142.48 (16) | S5ix—Cs1—S4ix | 52.04 (11) |
S2—Hf1—S5i | 69.75 (16) | S4i—Cs1—S4ix | 127.17 (15) |
S7—Hf1—Cs1 | 136.35 (12) | S1i—Cs1—S4ix | 90.12 (13) |
S6i—Hf1—Cs1 | 54.39 (12) | S1—Cs1—S4ix | 127.75 (13) |
S9—Hf1—Cs1 | 146.59 (12) | S6i—Cs1—S4ix | 99.85 (11) |
S8—Hf1—Cs1 | 100.78 (11) | S2—Cs1—S4ix | 155.74 (12) |
S3—Hf1—Cs1 | 56.57 (11) | P1—Cs1—S4ix | 137.04 (12) |
S2—Hf1—Cs1 | 54.49 (12) | S3—Cs1—S4ix | 110.76 (11) |
S5i—Hf1—Cs1 | 95.00 (11) | S14ix—Cs2—S7ix | 132.34 (13) |
S14ii—Hf2—S13 | 165.98 (17) | S14ix—Cs2—S11 | 64.28 (12) |
S14ii—Hf2—S11 | 99.47 (17) | S7ix—Cs2—S11 | 163.31 (13) |
S13—Hf2—S11 | 83.57 (16) | S14ix—Cs2—S9ii | 124.61 (12) |
S14ii—Hf2—S16ii | 91.79 (17) | S7ix—Cs2—S9ii | 80.09 (12) |
S13—Hf2—S16ii | 102.11 (16) | S11—Cs2—S9ii | 90.66 (12) |
S11—Hf2—S16ii | 71.20 (16) | S14ix—Cs2—S6i | 127.21 (12) |
S14ii—Hf2—S17ii | 89.49 (17) | S7ix—Cs2—S6i | 80.37 (12) |
S13—Hf2—S17ii | 96.15 (16) | S11—Cs2—S6i | 87.11 (12) |
S11—Hf2—S17ii | 143.54 (18) | S9ii—Cs2—S6i | 97.21 (12) |
S16ii—Hf2—S17ii | 73.27 (16) | S14ix—Cs2—S10ix | 80.92 (12) |
S14ii—Hf2—S10 | 77.21 (17) | S7ix—Cs2—S10ix | 65.06 (12) |
S13—Hf2—S10 | 90.48 (16) | S11—Cs2—S10ix | 126.43 (12) |
S11—Hf2—S10 | 75.21 (16) | S9ii—Cs2—S10ix | 76.50 (12) |
S16ii—Hf2—S10 | 142.32 (16) | S6i—Cs2—S10ix | 145.41 (11) |
S17ii—Hf2—S10 | 141.12 (17) | S14ix—Cs2—S8i | 83.58 (12) |
S14ii—Hf2—S12 | 93.38 (16) | S7ix—Cs2—S8i | 70.60 (11) |
S13—Hf2—S12 | 76.69 (15) | S11—Cs2—S8i | 115.13 (12) |
S11—Hf2—S12 | 143.64 (17) | S9ii—Cs2—S8i | 149.21 (11) |
S16ii—Hf2—S12 | 142.56 (16) | S6i—Cs2—S8i | 69.23 (11) |
S17ii—Hf2—S12 | 69.72 (16) | S10ix—Cs2—S8i | 98.76 (12) |
S10—Hf2—S12 | 74.74 (16) | S14ix—Cs2—S8 | 116.81 (12) |
S14ii—Hf2—Cs3 | 136.52 (13) | S7ix—Cs2—S8 | 110.82 (12) |
S13—Hf2—Cs3 | 55.62 (12) | S11—Cs2—S8 | 52.53 (11) |
S11—Hf2—Cs3 | 97.58 (12) | S9ii—Cs2—S8 | 60.94 (12) |
S16ii—Hf2—Cs3 | 56.93 (11) | S6i—Cs2—S8 | 54.16 (10) |
S17ii—Hf2—Cs3 | 55.10 (13) | S10ix—Cs2—S8 | 136.88 (11) |
S10—Hf2—Cs3 | 146.09 (12) | S8i—Cs2—S8 | 121.06 (14) |
S12—Hf2—Cs3 | 96.01 (11) | S14ix—Cs2—S10i | 51.09 (11) |
S1—P1—S2 | 119.8 (3) | S7ix—Cs2—S10i | 121.84 (12) |
S1—P1—S3 | 116.4 (4) | S11—Cs2—S10i | 65.08 (11) |
S2—P1—S3 | 101.9 (3) | S9ii—Cs2—S10i | 155.14 (12) |
S1—P1—S4 | 103.4 (3) | S6i—Cs2—S10i | 77.15 (11) |
S2—P1—S4 | 105.1 (3) | S10ix—Cs2—S10i | 121.56 (14) |
S3—P1—S4 | 109.6 (3) | S8i—Cs2—S10i | 51.32 (10) |
S7—P2—S5 | 105.7 (3) | S8—Cs2—S10i | 97.64 (11) |
S7—P2—S6 | 115.8 (3) | S14ix—Cs2—S5ix | 172.89 (12) |
S5—P2—S6 | 108.2 (3) | S7ix—Cs2—S5ix | 50.23 (11) |
S7—P2—S4 | 113.3 (3) | S11—Cs2—S5ix | 113.51 (12) |
S5—P2—S4 | 106.2 (3) | S9ii—Cs2—S5ix | 48.29 (11) |
S6—P2—S4 | 107.1 (3) | S6i—Cs2—S5ix | 58.18 (11) |
S9—P3—S10 | 114.0 (3) | S10ix—Cs2—S5ix | 95.99 (11) |
S9—P3—S8 | 103.6 (3) | S8i—Cs2—S5ix | 103.27 (11) |
S10—P3—S8 | 111.9 (3) | S8—Cs2—S5ix | 61.41 (10) |
S9—P3—S11 | 113.0 (3) | S10i—Cs2—S5ix | 135.05 (11) |
S10—P3—S11 | 103.0 (3) | S1x—Cs3—S12i | 101.29 (13) |
S8—P3—S11 | 111.6 (3) | S1x—Cs3—S15 | 125.13 (13) |
S14—P4—S12 | 107.1 (3) | S12i—Cs3—S15 | 107.57 (12) |
S14—P4—S13 | 115.0 (3) | S1x—Cs3—S18 | 74.21 (14) |
S12—P4—S13 | 107.2 (3) | S12i—Cs3—S18 | 110.39 (13) |
S14—P4—S15 | 112.9 (3) | S15—Cs3—S18 | 52.37 (12) |
S12—P4—S15 | 107.1 (3) | S1x—Cs3—S18ii | 100.67 (14) |
S13—P4—S15 | 107.1 (3) | S12i—Cs3—S18ii | 119.36 (12) |
S18—P5—S17 | 119.1 (3) | S15—Cs3—S18ii | 104.06 (12) |
S18—P5—S16 | 115.1 (3) | S18—Cs3—S18ii | 129.87 (16) |
S17—P5—S16 | 101.8 (3) | S1x—Cs3—S17ii | 146.86 (13) |
S18—P5—S15 | 103.6 (3) | S12i—Cs3—S17ii | 109.86 (12) |
S17—P5—S15 | 106.6 (3) | S15—Cs3—S17ii | 55.42 (11) |
S16—P5—S15 | 110.4 (3) | S18—Cs3—S17ii | 104.16 (13) |
Cs3v—S1—Cs1iii | 129.26 (19) | S18ii—Cs3—S17ii | 54.20 (12) |
Cs3v—S1—Cs1 | 99.86 (15) | S1x—Cs3—S13 | 150.12 (13) |
Cs1iii—S1—Cs1 | 130.87 (18) | S12i—Cs3—S13 | 58.93 (12) |
P2—S4—P1 | 104.4 (3) | S15—Cs3—S13 | 53.44 (11) |
Cs1iii—S4—Cs1vi | 127.17 (15) | S18—Cs3—S13 | 91.21 (12) |
Cs1vi—S5—Cs2vi | 116.72 (13) | S18ii—Cs3—S13 | 108.56 (11) |
Cs2iii—S8—Cs2 | 121.06 (14) | S17ii—Cs3—S13 | 61.39 (11) |
Cs2vi—S10—Cs2iii | 121.56 (14) | S1x—Cs3—S17ix | 69.24 (13) |
P4—S15—P5 | 104.0 (3) | S12i—Cs3—S17ix | 48.12 (11) |
Cs3iv—S17—Cs3vi | 125.34 (14) | S15—Cs3—S17ix | 155.67 (12) |
Cs1vii—S18—Cs3 | 123.27 (16) | S18—Cs3—S17ix | 129.66 (13) |
Cs1vii—S18—Cs3iv | 106.81 (15) | S18ii—Cs3—S17ix | 90.63 (12) |
Cs3—S18—Cs3iv | 129.87 (16) | S17ii—Cs3—S17ix | 125.34 (14) |
S18viii—Cs1—S5ix | 102.32 (13) | S13—Cs3—S17ix | 103.74 (11) |
S18viii—Cs1—S4i | 130.94 (13) | S1x—Cs3—S16ii | 136.99 (14) |
S5ix—Cs1—S4i | 113.59 (12) | S12i—Cs3—S16ii | 73.70 (11) |
S18viii—Cs1—S1i | 80.60 (13) | S15—Cs3—S16ii | 96.07 (11) |
S5ix—Cs1—S1i | 122.42 (14) | S18—Cs3—S16ii | 148.36 (12) |
S4i—Cs1—S1i | 52.37 (13) | S18ii—Cs3—S16ii | 52.45 (11) |
S18viii—Cs1—S1 | 95.28 (13) | S17ii—Cs3—S16ii | 48.28 (11) |
S5ix—Cs1—S1 | 106.38 (13) | S13—Cs3—S16ii | 63.31 (11) |
S4i—Cs1—S1 | 104.87 (13) | S17ix—Cs3—S16ii | 77.43 (11) |
S1i—Cs1—S1 | 130.87 (18) | | |
Symmetry codes: (i) x−1/2, y+1/2, z; (ii) x−1/2, y−1/2, z; (iii) x+1/2, y−1/2, z; (iv) x+1/2, y+1/2, z; (v) x, −y+1, z−1/2; (vi) x+1, y, z; (vii) x+1, −y+1, z+1/2; (viii) x−1, −y+1, z−1/2; (ix) x−1, y, z; (x) x, −y+1, z+1/2. |