#------------------------------------------------------------------------------
#$Date: 2024-10-01 04:15:35 +0200 (Tue, 01 Oct 2024) $
#$Revision: 294951 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/32/2023269.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2023269
loop_
_publ_author_name
'Upmann, Daniel'
'Bockfeld, Dirk'
'Jones, Peter G.'
'T\^arcoveanu, Eliza'
_publ_section_title
;
Crystal structures of seven mixed-valence gold compounds of the form [(R
1 R 2 R 3PE)2AuI]+[AuIII X 4]− (R = tert-butyl or isopropyl, E = S
or Se, and X = Cl or Br)
;
_journal_coeditor_code WM5733
_journal_issue 10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 1087
_journal_page_last 1096
_journal_paper_doi 10.1107/S2056989024009095
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Au (C12 H27 P1 S1)2] [Au Br4]'
_chemical_formula_moiety 'C24 H54 Au P2 S2 +, Au Br4 -'
_chemical_formula_sum 'C24 H54 Au2 Br4 P2 S2'
_chemical_formula_weight 1182.30
_chemical_name_common
;
Bis(tri-tert-butylphosphane sulfide)gold(I) tetrabromidoaurate(III)
;
_chemical_name_systematic
;
Bis(tri-tert-butylphosphane sulfide)gold(I) tetrabromidoaurate(III)
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 105.533(4)
_cell_angle_beta 97.476(4)
_cell_angle_gamma 99.318(4)
_cell_formula_units_Z 1
_cell_length_a 8.4858(4)
_cell_length_b 9.3738(4)
_cell_length_c 11.9910(5)
_cell_measurement_reflns_used 18685
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.6703
_cell_measurement_theta_min 2.2998
_cell_volume 891.63(7)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
XP (Bruker, 1998)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scan'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0345
_diffrn_reflns_av_unetI/netI 0.0192
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 47038
_diffrn_reflns_theta_full 30.000
_diffrn_reflns_theta_max 30.739
_diffrn_reflns_theta_min 2.304
_diffrn_source 'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu 12.919
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.76446
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour 'dichroic red / orange'
_exptl_crystal_density_diffrn 2.202
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 558
_exptl_crystal_size_max 0.120
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.080
_refine_diff_density_max 0.734
_refine_diff_density_min -0.707
_refine_ls_extinction_coef 0.00106(8)
_refine_ls_extinction_expression
;F~c~^*^ =
kF~c~[1+0.001\\timesF~c~^2^\l^3^/sin(2\q)]^-1/4^
;
_refine_ls_extinction_method
;
SHELXL2019/3 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 167
_refine_ls_number_reflns 5273
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.060
_refine_ls_R_factor_all 0.0212
_refine_ls_R_factor_gt 0.0165
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0116P)^2^+0.5840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0314
_refine_ls_wR_factor_ref 0.0325
_reflns_number_gt 4754
_reflns_number_total 5273
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm5733.cif
_cod_data_source_block 5a
_cod_database_code 2023269
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.306
_shelx_estimated_absorpt_t_max 0.425
_shelx_hkl_file
;
-12 1 3 16105.5 1555.23 9
-12 1 3 15808.2 1609.10 11
-12 1 3 17318.0 1639.38 23
-12 2 2 14858.0 1513.58 2
-12 3 1 6390.50 1031.29 2
-12 3 2 444.808 532.741 2
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-11 -3 3 21100.6 1777.41 13
-11 -3 4 5366.30 1019.80 8
-11 -3 4 6109.86 1053.33 13
-11 -3 5 27042.5 2215.30 8
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-11 -2 1 6003.48 971.072 13
-11 -2 2 10870.2 1276.86 13
-11 -2 3 1874.82 727.057 13
-11 -2 4 41359.7 2516.11 13
-11 -2 4 44950.9 2738.79 8
-11 -2 5 7591.89 1155.64 13
-11 -2 5 7702.05 1221.42 8
-11 -2 6 18435.2 1878.82 8
-11 -1 -2 1439.85 584.931 18
-11 -1 -1 53104.9 2749.87 13
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-11 -1 1 23021.5 1817.36 13
-11 -1 2 3056.44 912.853 2
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-11 -1 4 5784.93 1048.17 8
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-11 -1 5 33829.2 2381.12 22
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-11 -1 6 97.8730 575.394 11
-11 -1 6 271.722 567.287 25
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-11 0 7 600.152 601.949 11
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10 1 -8 332.247 709.293 19
10 1 -8 21.1163 677.977 12
10 1 -8 1155.36 788.902 3
10 1 -8 418.589 538.665 20
10 1 -7 10971.8 1524.59 19
10 1 -7 12209.6 1632.06 12
10 1 -7 14015.4 1627.89 3
10 1 -7 14356.9 1518.02 20
10 1 -6-340.511 769.514 19
10 1 -6 337.843 733.492 12
10 1 -6-403.776 734.920 3
10 1 -6 1109.97 664.177 20
10 1 -5 4263.69 899.786 19
10 1 -5 3848.23 1108.93 12
10 1 -5 3979.18 1036.08 3
10 1 -5 4257.14 989.870 20
10 1 -4 2155.82 781.337 19
10 1 -4 3137.14 952.196 12
10 1 -4 2174.51 832.679 3
10 1 -4 1288.03 705.848 20
10 1 -3 37625.0 2405.11 19
10 1 -3 41736.5 2549.91 3
10 1 -3 42298.5 2734.47 12
10 1 -3 39694.4 2562.49 20
10 1 -2-105.086 608.343 20
10 1 -2 55.2114 507.750 19
10 1 -2-203.532 715.943 12
10 1 -2-171.294 568.114 3
10 1 -1 5499.22 1032.97 20
10 1 -1 5440.77 1065.15 12
10 1 -1 5116.50 1004.73 3
10 1 -1 5610.74 1029.05 5
10 1 0 2407.01 730.376 20
10 1 0 2127.55 808.233 12
10 1 0 4170.48 947.413 5
10 1 1 28877.1 2236.10 15
10 1 1 29955.0 2174.53 12
10 1 1 32859.1 2199.21 5
10 1 1 28523.3 2193.39 20
10 1 2 1466.22 746.387 20
10 1 2 1843.53 924.012 15
10 1 2 563.904 623.358 5
10 1 3 19568.7 1854.92 15
10 1 3 17515.5 1690.47 5
10 1 3 18746.0 1777.96 20
10 1 4-22.5756 704.484 15
10 1 4 1552.03 673.101 5
10 1 4 575.082 619.081 20
10 1 5 16642.9 1651.55 5
10 1 5 13909.7 1571.13 20
10 2 -10 2885.07 724.039 20
10 2 -9 1599.62 873.003 19
10 2 -9 3966.48 1154.76 3
10 2 -9 2844.76 773.090 20
10 2 -8 19193.4 1999.08 19
10 2 -8 19711.1 2075.27 12
10 2 -8 19436.2 2056.27 3
10 2 -8 20615.4 1828.79 20
10 2 -7 426.650 610.470 19
10 2 -7 296.537 754.603 12
10 2 -7 2245.43 995.701 3
10 2 -7 332.001 504.088 20
10 2 -6 1414.05 721.239 19
10 2 -6 3641.51 1085.80 12
10 2 -6 2416.38 970.688 3
10 2 -6 2496.30 833.045 20
10 2 -5 895.136 641.972 19
10 2 -5 533.632 691.073 12
10 2 -5 2646.10 917.172 3
10 2 -5 568.448 563.275 20
10 2 -4 20987.1 1860.42 19
10 2 -4 24701.3 2075.12 3
10 2 -4 21481.5 2036.75 12
10 2 -4 21530.1 1905.78 20
10 2 -3 559.552 500.130 19
10 2 -3 266.400 580.075 12
10 2 -3 655.514 759.757 3
10 2 -3 650.598 638.922 20
10 2 -2 7440.72 1229.31 12
10 2 -2 10168.5 1351.88 3
10 2 -2 9075.60 1294.49 20
10 2 -1 741.797 703.648 12
10 2 -1 668.655 657.046 3
10 2 -1 933.321 773.385 5
10 2 -1 1113.71 687.197 20
10 2 0 17298.9 1783.94 15
10 2 0 14069.0 1560.61 12
10 2 0 18569.1 1694.76 5
10 2 0 16660.2 1719.04 20
10 2 1 8159.57 1242.28 15
10 2 1 6883.09 1142.82 12
10 2 1 5754.80 1015.68 5
10 2 1 5226.63 1028.63 20
10 2 2 16429.3 1734.91 15
10 2 2 14027.3 1493.06 5
10 2 2 16239.7 1717.86 20
10 2 3 1502.04 757.914 15
10 2 3 784.469 636.635 5
10 2 3 1945.30 830.082 20
10 2 4 12658.4 1412.08 5
10 2 4 9857.64 1347.96 20
10 3 -10 158.582 499.570 20
10 3 -9 16419.8 1641.03 20
10 3 -8 137.503 665.312 19
10 3 -8 1310.44 942.001 3
10 3 -8 715.359 557.543 20
10 3 -7 2862.67 896.355 19
10 3 -7 4715.87 1191.60 12
10 3 -7 3532.74 1070.29 3
10 3 -7 3381.06 936.222 20
10 3 -6 238.121 640.732 19
10 3 -6-1192.74 811.624 12
10 3 -6-1779.13 1002.80 3
10 3 -6 329.769 529.986 20
10 3 -5 22072.9 1999.88 19
10 3 -5 26947.1 2314.24 3
10 3 -5 21412.0 2096.49 12
10 3 -5 23810.8 2033.70 20
10 3 -4 897.807 584.368 19
10 3 -4 413.654 681.909 12
10 3 -4 1542.00 888.791 3
10 3 -4-77.3163 522.795 20
10 3 -3 4618.75 885.907 19
10 3 -3 4112.82 1032.19 12
10 3 -3 5937.53 1193.21 3
10 3 -3 2895.73 878.805 20
10 3 -2 4689.96 1123.73 12
10 3 -2 4842.73 995.512 5
10 3 -2 3466.77 891.023 3
10 3 -2 3745.00 942.791 20
10 3 -1 18809.1 1679.84 4
10 3 -1 16399.7 1777.68 12
10 3 -1 22996.2 1872.21 5
10 3 -1 21098.0 1850.02 3
10 3 -1 18187.8 1806.78 20
10 3 0 1320.43 684.681 4
10 3 0 991.020 774.868 12
10 3 0 2316.37 777.013 5
10 3 0 921.602 662.858 20
10 3 1 11865.9 1479.15 15
10 3 1 14390.2 1490.47 5
10 3 1 9341.46 1335.44 20
10 3 2 239.955 643.012 15
10 3 2 758.038 596.643 5
10 4 -7 1985.32 802.701 19
10 4 -6 24190.4 2181.87 19
10 4 -6 22969.0 2205.19 3
10 4 -6 22471.0 2025.37 20
10 4 -5-509.501 555.687 19
10 4 -5-88.4054 751.641 12
10 4 -5-654.424 837.848 3
10 4 -5-360.023 652.135 20
10 4 -4 7337.34 1189.07 19
10 4 -4 9207.04 1491.07 12
10 4 -4 8985.55 1416.88 3
10 4 -4 9840.65 1369.98 20
10 4 -3 810.310 600.162 19
10 4 -3 874.622 690.262 12
10 4 -3-115.019 653.007 3
10 4 -2 8970.06 1397.47 12
10 4 -2 9052.22 1295.22 3
10 4 -2 9823.92 1263.69 5
10 4 -1 823.055 701.893 15
10 4 -1 1539.38 748.576 4
10 4 -1-504.433 663.706 3
10 4 -1 1013.20 714.042 5
10 4 0 25804.8 2020.08 4
10 4 0 26982.0 2136.47 15
10 4 0 27949.0 2029.97 5
10 4 1 204.737 634.093 15
10 4 2 2338.00 819.674 15
10 5 -6 687.528 739.976 19
10 5 -5 22251.2 2024.54 19
10 5 -4 1918.18 768.362 19
10 5 -3 1243.24 829.714 3
10 5 -2-1164.88 840.102 3
11 -7 -2-16.8865 660.506 19
11 -7 -2 147.048 612.031 12
11 -7 -1 8256.78 1243.60 12
11 -6 -4 38029.7 2528.21 5
11 -6 -3 160.826 532.754 19
11 -6 -3 780.366 633.989 12
11 -6 -3 73.9615 593.290 5
11 -6 -2 7671.55 1218.08 19
11 -6 -2 7881.90 1249.95 12
11 -6 -2 8234.75 1246.87 5
11 -6 -1 467.440 590.828 12
11 -6 -1 286.247 666.507 5
11 -6 0 30400.0 2257.26 5
11 -5 -6 4951.85 1062.01 3
11 -5 -5 16248.2 1780.10 19
11 -5 -5 19276.0 1806.26 3
11 -5 -4-349.945 583.696 19
11 -5 -4 63.1761 669.525 12
11 -5 -4 587.234 679.779 5
11 -5 -3 13805.0 1569.41 19
11 -5 -3 17521.2 1804.16 12
11 -5 -3 16628.4 1699.57 5
11 -5 -2-295.091 600.021 19
11 -5 -2 618.110 606.947 12
11 -5 -2 377.162 637.276 5
11 -5 -1 17037.8 1732.14 12
11 -5 -1 17478.5 1758.78 5
11 -5 0 3638.87 945.941 5
11 -5 1 23978.8 2040.15 5
11 -4 -7 1876.33 826.815 3
11 -4 -6 22085.6 2007.46 3
11 -4 -5 8698.03 1306.96 19
11 -4 -5 10192.4 1497.97 12
11 -4 -5 9097.09 1316.76 3
11 -4 -4 16701.8 1751.77 19
11 -4 -4 18580.9 1907.42 12
11 -4 -3-1149.53 663.070 19
11 -4 -3-999.690 731.169 12
11 -4 -3 378.247 653.511 5
11 -4 -2 25150.5 1987.00 19
11 -4 -2 25925.4 2141.72 12
11 -4 -2 27927.9 2153.84 5
11 -4 -1 3948.26 899.717 12
11 -4 -1 6704.19 1193.21 5
11 -4 0 14057.3 1537.79 12
11 -4 0 17994.5 1755.48 5
11 -4 1 1936.80 817.230 5
11 -3 -7 26184.1 2238.80 3
11 -3 -6 5009.89 1093.35 19
11 -3 -6 7317.23 1200.44 3
11 -3 -5 22094.7 2003.71 19
11 -3 -5 26543.4 2117.82 3
11 -3 -5 21536.9 2069.96 12
11 -3 -4 2534.78 881.110 19
11 -3 -4 1931.99 913.644 12
11 -3 -4 1667.64 775.700 3
11 -3 -3 10041.1 1309.73 19
11 -3 -3 11217.6 1395.29 5
11 -3 -3 12363.9 1548.23 12
11 -3 -2 2797.55 798.089 19
11 -3 -2 3361.04 952.551 12
11 -3 -2 3709.51 1021.80 5
11 -3 -1 65048.5 3365.27 12
11 -3 -1 64117.7 3295.84 5
11 -3 0 2961.65 853.695 12
11 -3 0 1132.72 643.375 5
11 -3 1 3819.36 1021.17 5
11 -2 -7 5430.20 1163.28 19
11 -2 -7 5013.46 1120.35 3
11 -2 -6 37753.5 2672.49 19
11 -2 -6 37476.0 2620.58 3
11 -2 -6 39707.1 2815.34 12
11 -2 -5-83.6351 611.943 19
11 -2 -5-1010.54 742.428 12
11 -2 -5-1043.04 711.490 3
11 -2 -4 13421.9 1535.79 19
11 -2 -4 14688.4 1697.92 12
11 -2 -4 13985.1 1530.09 3
11 -2 -3 10546.5 1319.61 19
11 -2 -3 11733.1 1575.99 12
11 -2 -2 42237.1 2760.67 12
11 -2 -2 50495.5 2881.27 5
11 -2 -1-79.0491 616.606 12
11 -2 -1 1547.02 831.972 5
11 -2 0 30113.5 2239.88 12
11 -2 0 33969.2 2372.33 5
11 -2 1 457.428 592.940 5
11 -1 -8 2530.97 807.082 20
11 -1 -7 43022.8 2942.50 19
11 -1 -7 44952.7 2967.65 3
11 -1 -7 45777.2 2788.56 20
11 -1 -6-201.765 714.815 19
11 -1 -6-147.779 659.924 12
11 -1 -6-442.710 722.630 3
11 -1 -5 29637.7 2319.01 19
11 -1 -5 27207.0 2221.43 3
11 -1 -5 29248.0 2420.69 12
11 -1 -4 417.174 562.476 19
11 -1 -4 41.2091 727.204 12
11 -1 -4 1016.24 732.262 3
11 -1 -3 35865.0 2410.03 19
11 -1 -3 39467.7 2699.80 12
11 -1 -2 3946.48 1002.94 12
11 -1 -2 6457.49 1150.16 5
11 -1 -1 37967.6 2586.21 12
11 -1 -1 36999.4 2517.96 5
11 -1 0-439.018 613.881 12
11 -1 0 576.128 639.444 5
11 -1 1 36031.0 2616.81 15
11 -1 1 35879.0 2412.93 5
11 0 -9 3404.05 815.911 20
11 0 -8 37784.9 2523.59 20
11 0 -7 3038.05 906.924 19
11 0 -7 1562.57 885.763 3
11 0 -7 1644.62 798.633 20
11 0 -6 27457.2 2267.95 19
11 0 -6 26512.7 2261.08 3
11 0 -6 26659.1 2348.22 12
11 0 -6 26922.4 2181.13 20
11 0 -5-436.724 641.068 20
11 0 -5 80.2025 568.775 19
11 0 -5-147.078 733.872 12
11 0 -5 1085.40 804.715 3
11 0 -4 45947.5 2814.80 19
11 0 -4 49815.9 2963.12 3
11 0 -4 47934.6 3082.23 12
11 0 -4 44439.1 2804.18 20
11 0 -3 8172.57 1162.94 19
11 0 -3 12330.3 1612.11 12
11 0 -3 9732.54 1336.30 3
11 0 -2 37685.7 2660.06 12
11 0 -2 41348.4 2616.41 5
11 0 -1-658.124 651.843 12
11 0 -1-714.380 561.659 5
11 0 0 41432.4 2665.06 12
11 0 0 39361.0 2551.53 5
11 0 1 3999.53 954.659 5
11 1 -7 15635.2 1827.85 19
11 1 -7 17637.8 1941.66 3
11 1 -7 16782.4 1709.82 20
11 1 -6 1429.20 796.032 19
11 1 -6 947.587 872.557 3
11 1 -6 1321.62 705.824 20
11 1 -5 27542.6 2246.94 19
11 1 -5 34756.3 2573.44 3
11 1 -5 30666.0 2498.19 12
11 1 -5 28527.7 2275.22 20
11 1 -4 4027.51 987.463 19
11 1 -4 2925.82 939.615 12
11 1 -4 5303.13 1113.80 3
11 1 -4 4873.36 1017.26 20
11 1 -3 36721.6 2508.69 3
11 1 -3 41644.6 2878.40 12
11 1 -3 36717.1 2565.44 20
11 1 -2 2456.53 904.627 12
11 1 -2 4061.62 1034.97 5
11 1 -1 22382.2 2051.86 12
11 1 -1 25135.2 2064.99 5
11 1 0 1414.14 758.163 12
11 1 0 3896.09 987.758 5
11 2 -6 10881.3 1517.89 19
11 2 -6 13168.9 1715.49 3
11 2 -5 9531.94 1387.03 19
11 2 -5 7133.56 1279.94 3
11 2 -4 37498.3 2575.19 19
11 2 -4 40002.2 2759.34 3
11 2 -3-800.651 798.645 12
11 2 -3 449.462 616.216 3
11 2 -2 9603.24 1442.67 12
11 2 -2 10073.0 1363.13 5
11 2 -1 5087.76 1067.96 12
11 2 0 32122.0 2450.57 12
11 3 -5 20635.5 1984.58 19
11 3 -4 5997.93 1180.93 3
11 3 -3 18934.6 1885.48 3
12 -4 -2 4089.27 1021.28 12
12 -3 -4 1380.50 749.746 19
12 -3 -2 129.798 611.452 12
12 -2 -4 2028.96 754.803 19
12 -2 -2 16978.0 1839.88 12
12 -2 -1 411.974 710.218 12
12 -1 -1 5247.80 1112.00 12
;
_shelx_hkl_checksum 66123
_shelx_res_file
;
TITL Kea in P-1
shelx.res
created by SHELXL-2019/3 at 09:26:43 on 26-Jul-2024
CELL 0.71073 8.485805 9.373796 11.990966 105.5329 97.4756 99.3178
ZERR 1.00 0.0004 0.0004 0.0005 0.0036 0.0036 0.004
LATT 1
SFAC C H P S Br Au
UNIT 24.00 54.00 2.00 2.00 4.00 2.00
TEMP -173
SIZE 0.12 0.12 0.08
ACTA 60
CONF 2.3
FMAP 2
PLAN 10
BOND $H
L.S. 6
OMIT 0 1 2
OMIT 2 1 1
EQIV $1 -x, 1-y, 1-z
EQIV $2 1-x, 2-y, 1-z
HTAB C33 Au1
HTAB C23 Au1
HTAB C22 Br1_$1
HTAB C12 Br1_$2
HTAB C32 S1
HTAB C23 S1
HTAB C13 S1
RTAB CONT Br1 S1
RTAB ANGL Au2 Br1 S1
EQIV $3 2-x,2-y,2-z
RTAB CONT BR2 BR2_$3
WGHT 0.011600 0.584000
EXTI 0.001056
FVAR 3.14264
AU1 6 0.500000 0.500000 0.500000 10.50000 0.01701 0.02443 =
0.01215 0.00762 -0.00136 0.00535
P1 3 0.235193 0.625697 0.318230 11.00000 0.01152 0.01449 =
0.00997 0.00408 0.00132 0.00275
S1 4 0.321468 0.657245 0.491720 11.00000 0.02140 0.02571 =
0.00996 0.00408 0.00031 0.00850
C1 1 0.119341 0.784623 0.326733 11.00000 0.01786 0.01970 =
0.01749 0.00502 0.00357 0.00859
C2 1 0.094669 0.433954 0.252006 11.00000 0.01574 0.01681 =
0.01418 0.00607 -0.00017 -0.00098
C3 1 0.408588 0.647592 0.234409 11.00000 0.01470 0.01636 =
0.01506 0.00588 0.00557 0.00367
C11 1 0.004131 0.765102 0.210744 11.00000 0.02083 0.02941 =
0.02330 0.01241 0.00263 0.01174
AFIX 137
H11A 2 -0.046051 0.853518 0.218391 11.00000 -1.50000
H11B 2 -0.080684 0.673822 0.193650 11.00000 -1.50000
H11C 2 0.065876 0.755553 0.146441 11.00000 -1.50000
AFIX 0
C12 1 0.239095 0.937845 0.358913 11.00000 0.02790 0.01607 =
0.02918 0.00527 0.00595 0.00802
AFIX 137
H12A 2 0.294987 0.942582 0.293034 11.00000 -1.50000
H12B 2 0.319085 0.948369 0.428893 11.00000 -1.50000
H12C 2 0.179396 1.020062 0.375282 11.00000 -1.50000
AFIX 0
C13 1 0.018980 0.795636 0.426402 11.00000 0.02594 0.03156 =
0.02332 0.00692 0.01135 0.01482
AFIX 137
H13A 2 0.092498 0.822098 0.502309 11.00000 -1.50000
H13B 2 -0.054057 0.697986 0.413248 11.00000 -1.50000
H13C 2 -0.045101 0.873804 0.426810 11.00000 -1.50000
AFIX 0
C21 1 0.049040 0.392592 0.117103 11.00000 0.02354 0.02100 =
0.01530 0.00461 -0.00470 -0.00028
AFIX 137
H21A 2 -0.032059 0.297666 0.087433 11.00000 -1.50000
H21B 2 0.146181 0.380317 0.082385 11.00000 -1.50000
H21C 2 0.003949 0.473460 0.095605 11.00000 -1.50000
AFIX 0
C22 1 -0.062069 0.432067 0.303160 11.00000 0.01746 0.02929 =
0.02686 0.01028 0.00502 -0.00247
AFIX 137
H22A 2 -0.124008 0.499729 0.275828 11.00000 -1.50000
H22B 2 -0.034697 0.466349 0.389330 11.00000 -1.50000
H22C 2 -0.127572 0.328918 0.276980 11.00000 -1.50000
AFIX 0
C23 1 0.170805 0.308819 0.284682 11.00000 0.02497 0.01697 =
0.02199 0.00866 0.00110 0.00090
AFIX 137
H23A 2 0.189478 0.328889 0.370358 11.00000 -1.50000
H23B 2 0.274437 0.307373 0.257067 11.00000 -1.50000
H23C 2 0.096941 0.210579 0.247410 11.00000 -1.50000
AFIX 0
C31 1 0.355819 0.687667 0.120544 11.00000 0.02218 0.02345 =
0.01968 0.01111 0.00821 0.00657
AFIX 137
H31A 2 0.446562 0.692699 0.077889 11.00000 -1.50000
H31B 2 0.323728 0.785957 0.140472 11.00000 -1.50000
H31C 2 0.263619 0.609826 0.070876 11.00000 -1.50000
AFIX 0
C32 1 0.551308 0.771680 0.313739 11.00000 0.01374 0.02373 =
0.02648 0.00861 0.00267 0.00135
AFIX 137
H32A 2 0.588570 0.743513 0.384194 11.00000 -1.50000
H32B 2 0.515439 0.867910 0.337020 11.00000 -1.50000
H32C 2 0.640651 0.782509 0.270440 11.00000 -1.50000
AFIX 0
C33 1 0.473853 0.500816 0.200839 11.00000 0.01900 0.02337 =
0.01816 0.00698 0.00603 0.00890
AFIX 137
H33A 2 0.567617 0.516960 0.162526 11.00000 -1.50000
H33B 2 0.388545 0.419573 0.146635 11.00000 -1.50000
H33C 2 0.506945 0.472478 0.271985 11.00000 -1.50000
AFIX 0
AU2 6 0.500000 1.000000 1.000000 10.50000 0.01409 0.00987 =
0.01663 0.00460 0.00114 0.00063
BR1 5 0.439745 0.873578 0.789980 11.00000 0.02326 0.01784 =
0.01773 0.00270 0.00122 -0.00018
BR2 5 0.777797 0.964875 1.007514 11.00000 0.01682 0.02703 =
0.03089 0.00063 0.00045 0.00700
HKLF 4
REM Kea in P-1
REM wR2 = 0.0325, GooF = S = 1.060, Restrained GooF = 1.060 for all data
REM R1 = 0.0165 for 4754 Fo > 4sig(Fo) and 0.0212 for all 5273 data
REM 167 parameters refined using 0 restraints
END
WGHT 0.0116 0.5840
REM Highest difference peak 0.734, deepest hole -0.707, 1-sigma level 0.105
Q1 1 0.7421 0.9008 1.0205 11.00000 0.05 0.73
Q2 1 0.3889 0.4825 0.4821 11.00000 0.05 0.65
Q3 1 0.5035 0.4380 0.4183 11.00000 0.05 0.61
Q4 1 0.4847 1.0574 1.0838 11.00000 0.05 0.61
Q5 1 0.3746 1.0067 0.9808 11.00000 0.05 0.60
Q6 1 0.5600 0.8768 0.7860 11.00000 0.05 0.55
Q7 1 0.7079 0.9832 0.9684 11.00000 0.05 0.54
Q8 1 1.0000 1.0000 1.0000 10.50000 0.05 0.50
Q9 1 0.3146 0.8645 0.7760 11.00000 0.05 0.50
Q10 1 0.4523 0.5653 0.4328 11.00000 0.05 0.49
;
_shelx_res_checksum 60032
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au Au1 0.500000 0.500000 0.500000 0.01767(3) Uani d 1 . .
P P1 0.23519(6) 0.62570(6) 0.31823(4) 0.01195(9) Uani d 1 . .
S S1 0.32147(7) 0.65725(6) 0.49172(4) 0.01907(11) Uani d 1 . .
C C1 0.1193(3) 0.7846(2) 0.32673(19) 0.0179(4) Uani d 1 . .
C C2 0.0947(2) 0.4340(2) 0.25201(18) 0.0161(4) Uani d 1 . .
C C3 0.4086(2) 0.6476(2) 0.23441(18) 0.0148(4) Uani d 1 . .
C C11 0.0041(3) 0.7651(3) 0.2107(2) 0.0229(5) Uani d 1 . .
H H11A -0.046051 0.853518 0.218391 0.034 Uiso calc 1 . .
H H11B -0.080684 0.673822 0.193650 0.034 Uiso calc 1 . .
H H11C 0.065876 0.755553 0.146441 0.034 Uiso calc 1 . .
C C12 0.2391(3) 0.9378(2) 0.3589(2) 0.0242(5) Uani d 1 . .
H H12A 0.294987 0.942582 0.293034 0.036 Uiso calc 1 . .
H H12B 0.319085 0.948369 0.428893 0.036 Uiso calc 1 . .
H H12C 0.179396 1.020062 0.375282 0.036 Uiso calc 1 . .
C C13 0.0190(3) 0.7956(3) 0.4264(2) 0.0255(5) Uani d 1 . .
H H13A 0.092498 0.822098 0.502309 0.038 Uiso calc 1 . .
H H13B -0.054057 0.697986 0.413248 0.038 Uiso calc 1 . .
H H13C -0.045101 0.873804 0.426810 0.038 Uiso calc 1 . .
C C21 0.0490(3) 0.3926(3) 0.11710(18) 0.0214(4) Uani d 1 . .
H H21A -0.032059 0.297666 0.087433 0.032 Uiso calc 1 . .
H H21B 0.146181 0.380317 0.082385 0.032 Uiso calc 1 . .
H H21C 0.003949 0.473460 0.095605 0.032 Uiso calc 1 . .
C C22 -0.0621(3) 0.4321(3) 0.3032(2) 0.0249(5) Uani d 1 . .
H H22A -0.124008 0.499729 0.275828 0.037 Uiso calc 1 . .
H H22B -0.034697 0.466349 0.389330 0.037 Uiso calc 1 . .
H H22C -0.127572 0.328918 0.276980 0.037 Uiso calc 1 . .
C C23 0.1708(3) 0.3088(2) 0.2847(2) 0.0214(4) Uani d 1 . .
H H23A 0.189478 0.328889 0.370358 0.032 Uiso calc 1 . .
H H23B 0.274437 0.307373 0.257067 0.032 Uiso calc 1 . .
H H23C 0.096941 0.210579 0.247410 0.032 Uiso calc 1 . .
C C31 0.3558(3) 0.6877(3) 0.12054(19) 0.0202(4) Uani d 1 . .
H H31A 0.446562 0.692699 0.077889 0.030 Uiso calc 1 . .
H H31B 0.323728 0.785957 0.140472 0.030 Uiso calc 1 . .
H H31C 0.263619 0.609826 0.070876 0.030 Uiso calc 1 . .
C C32 0.5513(3) 0.7717(3) 0.3137(2) 0.0215(4) Uani d 1 . .
H H32A 0.588570 0.743513 0.384194 0.032 Uiso calc 1 . .
H H32B 0.515439 0.867910 0.337020 0.032 Uiso calc 1 . .
H H32C 0.640651 0.782509 0.270440 0.032 Uiso calc 1 . .
C C33 0.4739(3) 0.5008(2) 0.20084(19) 0.0192(4) Uani d 1 . .
H H33A 0.567617 0.516960 0.162526 0.029 Uiso calc 1 . .
H H33B 0.388545 0.419573 0.146635 0.029 Uiso calc 1 . .
H H33C 0.506945 0.472478 0.271985 0.029 Uiso calc 1 . .
Au Au2 0.500000 1.000000 1.000000 0.01376(3) Uani d 1 . .
Br Br1 0.43975(3) 0.87358(2) 0.78998(2) 0.02087(5) Uani d 1 . .
Br Br2 0.77780(3) 0.96487(3) 1.00751(2) 0.02657(5) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Au1 0.01701(6) 0.02443(6) 0.01215(6) 0.00535(4) -0.00136(4) 0.00762(4)
P1 0.0115(2) 0.0145(2) 0.0100(2) 0.00275(18) 0.00132(18) 0.00408(19)
S1 0.0214(3) 0.0257(3) 0.0100(2) 0.0085(2) 0.00031(19) 0.0041(2)
C1 0.0179(10) 0.0197(10) 0.0175(10) 0.0086(8) 0.0036(8) 0.0050(8)
C2 0.0157(10) 0.0168(10) 0.0142(10) -0.0010(8) -0.0002(8) 0.0061(8)
C3 0.0147(9) 0.0164(9) 0.0151(10) 0.0037(7) 0.0056(8) 0.0059(8)
C11 0.0208(11) 0.0294(12) 0.0233(11) 0.0117(9) 0.0026(9) 0.0124(10)
C12 0.0279(12) 0.0161(10) 0.0292(13) 0.0080(9) 0.0060(10) 0.0053(9)
C13 0.0259(12) 0.0316(12) 0.0233(12) 0.0148(10) 0.0114(10) 0.0069(10)
C21 0.0235(11) 0.0210(11) 0.0153(11) -0.0003(9) -0.0047(8) 0.0046(9)
C22 0.0175(11) 0.0293(12) 0.0269(12) -0.0025(9) 0.0050(9) 0.0103(10)
C23 0.0250(11) 0.0170(10) 0.0220(11) 0.0009(8) 0.0011(9) 0.0087(9)
C31 0.0222(11) 0.0235(11) 0.0197(11) 0.0066(9) 0.0082(9) 0.0111(9)
C32 0.0137(10) 0.0237(11) 0.0265(12) 0.0013(8) 0.0027(9) 0.0086(9)
C33 0.0190(10) 0.0234(11) 0.0182(11) 0.0089(8) 0.0060(8) 0.0070(9)
Au2 0.01409(5) 0.00987(5) 0.01663(6) 0.00063(4) 0.00114(4) 0.00460(4)
Br1 0.02326(11) 0.01784(10) 0.01773(11) -0.00018(8) 0.00122(8) 0.00270(8)
Br2 0.01682(10) 0.02703(12) 0.03089(13) 0.00700(9) 0.00045(9) 0.00063(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 Au1 S1 2_666 . 180.0 y
C2 P1 C3 . . 111.22(9) ?
C2 P1 C1 . . 111.27(10) ?
C3 P1 C1 . . 111.39(9) ?
C2 P1 S1 . . 110.08(7) ?
C3 P1 S1 . . 110.94(7) ?
C1 P1 S1 . . 101.58(7) y
P1 S1 Au1 . . 107.15(3) y
C12 C1 C11 . . 108.38(18) ?
C12 C1 C13 . . 106.10(18) ?
C11 C1 C13 . . 108.66(18) ?
C12 C1 P1 . . 110.09(14) ?
C11 C1 P1 . . 113.07(15) ?
C13 C1 P1 . . 110.28(14) ?
C22 C2 C21 . . 108.46(18) ?
C22 C2 C23 . . 105.66(17) ?
C21 C2 C23 . . 109.05(17) ?
C22 C2 P1 . . 109.93(15) ?
C21 C2 P1 . . 112.27(14) ?
C23 C2 P1 . . 111.23(14) ?
C33 C3 C31 . . 108.08(17) ?
C33 C3 C32 . . 106.56(17) ?
C31 C3 C32 . . 109.51(16) ?
C33 C3 P1 . . 110.98(14) ?
C31 C3 P1 . . 111.94(14) ?
C32 C3 P1 . . 109.63(14) ?
C1 C11 H11A . . 109.5 ?
C1 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C1 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C1 C12 H12A . . 109.5 ?
C1 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C1 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C1 C13 H13A . . 109.5 ?
C1 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C1 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C2 C21 H21A . . 109.5 ?
C2 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C2 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C2 C22 H22A . . 109.5 ?
C2 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C2 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
C2 C23 H23A . . 109.5 ?
C2 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C2 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C3 C31 H31A . . 109.5 ?
C3 C31 H31B . . 109.5 ?
H31A C31 H31B . . 109.5 ?
C3 C31 H31C . . 109.5 ?
H31A C31 H31C . . 109.5 ?
H31B C31 H31C . . 109.5 ?
C3 C32 H32A . . 109.5 ?
C3 C32 H32B . . 109.5 ?
H32A C32 H32B . . 109.5 ?
C3 C32 H32C . . 109.5 ?
H32A C32 H32C . . 109.5 ?
H32B C32 H32C . . 109.5 ?
C3 C33 H33A . . 109.5 ?
C3 C33 H33B . . 109.5 ?
H33A C33 H33B . . 109.5 ?
C3 C33 H33C . . 109.5 ?
H33A C33 H33C . . 109.5 ?
H33B C33 H33C . . 109.5 ?
Br1 Au2 Br1 . 2_677 180.0 y
Br1 Au2 Br2 . 2_677 89.687(9) y
Br1 Au2 Br2 2_677 2_677 90.313(9) ?
Br1 Au2 Br2 . . 90.312(9) y
Br1 Au2 Br2 2_677 . 89.687(9) ?
Br2 Au2 Br2 2_677 . 180.0 y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Au1 S1 2_666 2.2891(5) ?
Au1 S1 . 2.2891(5) y
P1 C2 . 1.892(2) ?
P1 C3 . 1.901(2) ?
P1 C1 . 1.901(2) ?
P1 S1 . 2.0384(7) y
C1 C12 . 1.540(3) ?
C1 C11 . 1.541(3) ?
C1 C13 . 1.546(3) ?
C2 C22 . 1.535(3) ?
C2 C21 . 1.539(3) ?
C2 C23 . 1.540(3) ?
C3 C33 . 1.539(3) ?
C3 C31 . 1.541(3) ?
C3 C32 . 1.541(3) ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C13 H13C . 0.9800 ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 0.9800 ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C31 H31A . 0.9800 ?
C31 H31B . 0.9800 ?
C31 H31C . 0.9800 ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
C32 H32C . 0.9800 ?
C33 H33A . 0.9800 ?
C33 H33B . 0.9800 ?
C33 H33C . 0.9800 ?
Au2 Br1 . 2.4245(2) y
Au2 Br1 2_677 2.4245(2) ?
Au2 Br2 2_677 2.4260(2) ?
Au2 Br2 . 2.4260(2) y
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C33 H33C Au1 . 0.98 2.69 3.567(2) 149.8 yes
C23 H23A Au1 . 0.98 2.86 3.421(2) 117.5 yes
C22 H22C Br1 2_566 0.98 2.88 3.756(2) 150.0 yes
C12 H12A Br1 2_676 0.98 3.05 3.890(2) 145.2 yes
C32 H32A S1 . 0.98 2.86 3.338(2) 110.9 yes
C23 H23A S1 . 0.98 2.98 3.456(2) 110.8 yes
C13 H13A S1 . 0.98 2.67 3.160(2) 111.5 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 P1 S1 Au1 . . . . 71.01(7) ?
C3 P1 S1 Au1 . . . . -52.53(7) ?
C1 P1 S1 Au1 . . . . -171.01(7) y
C2 P1 C1 C12 . . . . -169.51(14) ?
C3 P1 C1 C12 . . . . -44.79(17) ?
S1 P1 C1 C12 . . . . 73.37(15) ?
C2 P1 C1 C11 . . . . -48.13(18) ?
C3 P1 C1 C11 . . . . 76.59(17) ?
S1 P1 C1 C11 . . . . -165.24(14) ?
C2 P1 C1 C13 . . . . 73.75(17) ?
C3 P1 C1 C13 . . . . -161.53(15) ?
S1 P1 C1 C13 . . . . -43.37(16) ?
C3 P1 C2 C22 . . . . -167.67(14) ?
C1 P1 C2 C22 . . . . -42.86(17) ?
S1 P1 C2 C22 . . . . 68.96(15) ?
C3 P1 C2 C21 . . . . -46.85(17) ?
C1 P1 C2 C21 . . . . 77.96(17) ?
S1 P1 C2 C21 . . . . -170.22(13) ?
C3 P1 C2 C23 . . . . 75.67(16) ?
C1 P1 C2 C23 . . . . -159.52(14) ?
S1 P1 C2 C23 . . . . -47.70(16) ?
C2 P1 C3 C33 . . . . -40.99(17) ?
C1 P1 C3 C33 . . . . -165.73(14) ?
S1 P1 C3 C33 . . . . 81.89(15) ?
C2 P1 C3 C31 . . . . 79.86(16) ?
C1 P1 C3 C31 . . . . -44.89(17) ?
S1 P1 C3 C31 . . . . -157.27(13) ?
C2 P1 C3 C32 . . . . -158.42(13) ?
C1 P1 C3 C32 . . . . 76.83(15) ?
S1 P1 C3 C32 . . . . -35.55(15) ?