#------------------------------------------------------------------------------
#$Date: 2025-02-05 05:03:59 +0200 (Wed, 05 Feb 2025) $
#$Revision: 297594 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023378.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_2023378
loop_
_publ_author_name
'Upmann, Daniel'
'Jones, Peter G.'
_publ_section_title
;
Crystal structures of six complexes of phosphane chalcogenides R 1 R 2 R
3PE (R = tert-butyl or isopropyl, E = S or Se) with the metal halides MX
2 (M = Pd or Pt, X = Cl or Br), two halochalcogenylphosphonium
derivatives ( t Bu2 iPrPEBr)2[Pd2Br6] and one hydrolysis product
;
_journal_coeditor_code YZ2063
_journal_issue 3
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989025000805
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '(C11 H25 Br P S)2 [Pd2 Br6]'
_chemical_formula_moiety '2(C11 H25 Br P S +), Pd2 Br6 2-'
_chemical_formula_sum 'C22 H50 Br8 P2 Pd2 S2'
_chemical_formula_weight 1292.76
_chemical_name_systematic
;
(Bromosulfanyl)di-tert-butylisopropylphosphanium
di-\m-bromido-bis[dibromidopalladium(II)]
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL2019/3
_cell_angle_alpha 90
_cell_angle_beta 98.386(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.8691(4)
_cell_length_b 22.7255(8)
_cell_length_c 10.5879(3)
_cell_measurement_reflns_used 8375
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 29.1954
_cell_measurement_theta_min 2.1366
_cell_volume 1873.18(13)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2012)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2012)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2012)
;
_computing_molecular_graphics
;
Bruker XP; Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0824
_diffrn_reflns_av_unetI/netI 0.0483
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 30
_diffrn_reflns_limit_k_min -30
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 52903
_diffrn_reflns_theta_full 28.000
_diffrn_reflns_theta_max 28.281
_diffrn_reflns_theta_min 2.141
_exptl_absorpt_coefficient_mu 9.704
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.49462
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2012)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 2.292
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1232
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.713
_refine_diff_density_min -0.954
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.105
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 196
_refine_ls_number_reflns 4622
_refine_ls_number_restraints 87
_refine_ls_restrained_S_all 1.100
_refine_ls_R_factor_all 0.0622
_refine_ls_R_factor_gt 0.0421
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+6.2080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0668
_refine_ls_wR_factor_ref 0.0716
_reflns_number_gt 3740
_reflns_number_total 4622
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2063.cif
_cod_data_source_block 7
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 2023378
_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 0.247
_shelx_estimated_absorpt_t_max 0.909
_shelx_hkl_file
;
0 0 2 405.028 64.8448 6
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0 0 -2 328.109 65.3344 6
0 0 2 319.688 74.9925 12
0 0 -2 332.498 87.1756 12
0 0 2 293.148 80.1111 7
0 0 2 351.488 82.8139 1
0 0 -2 296.320 76.5159 7
0 0 3 1.41716 81.2397 1
0 0 -3 18.0520 108.885 7
0 0 3 156.804 102.284 7
0 0 -3 76.5699 77.3035 1
0 0 3-12.2371 54.7667 6
0 0 -3-89.7792 97.6992 12
0 0 3 59.2641 101.340 12
0 0 4 14485.3 613.057 1
0 0 4 15443.7 684.683 12
0 0 -4 14852.7 600.417 1
0 0 4 14170.1 527.873 6
0 0 -4 14369.2 667.843 7
0 0 -4 14117.8 660.889 12
0 0 4 15002.8 677.873 7
0 0 -5 54.3701 132.247 7
0 0 -5 179.654 110.142 1
0 0 5 85.1668 77.8623 6
0 0 5 164.596 127.832 1
0 0 -5-99.5795 120.696 12
0 0 -6 14202.5 788.418 12
0 0 6 13550.5 706.061 1
0 0 -6 13421.3 772.144 7
0 0 6 13609.3 592.681 6
0 0 7 73.0735 79.6393 6
0 0 7 152.850 153.379 1
0 0 -7 110.943 197.705 7
0 0 -7 305.093 193.855 12
0 0 -8 2120.00 351.373 12
0 0 8 2540.51 408.512 17
0 0 -8 2161.95 367.920 7
0 0 8 2085.05 339.981 1
0 0 8 2016.84 287.217 8
0 0 9 24.1187 124.208 8
0 0 9-66.4867 179.240 1
0 0 -9 150.378 181.680 12
0 0 -9 217.232 237.342 7
0 0 9 260.467 220.507 17
0 0 -10 5153.48 620.104 16
0 0 -10 4547.65 571.861 7
0 0 10 5141.48 578.558 1
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0 0 -10 5394.70 638.368 12
0 0 10 5327.21 470.355 8
0 0 11-11.1465 266.757 17
0 0 11-29.3916 197.570 1
0 0 -11 211.903 254.862 2
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0 0 -12 8419.83 856.993 16
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0 0 -12 8503.86 920.122 2
0 0 12 9780.09 893.783 1
0 0 -13 278.314 254.122 16
0 0 -13-159.122 280.145 2
0 0 13 756.102 418.977 10
0 0 13 56.1621 253.258 17
0 1 1 45583.1 1009.09 17
0 1 1 41229.8 994.382 12
0 1 1 41334.7 994.596 7
0 1 -1 47942.1 1023.50 1
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0 -1 2 19933.8 539.517 19
0 1 -2 18736.6 622.466 12
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0 -1 -2 19781.0 554.610 1
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0 -1 2 18847.4 601.110 1
0 -1 -2 18946.8 609.273 7
0 -1 2 19428.1 628.863 7
0 -1 -2 18912.0 617.631 14
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0 1 2 19385.0 617.434 7
0 1 -2 19428.6 628.268 7
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0 -1 3 550.803 94.3387 6
0 -1 3 755.544 118.439 19
0 -1 3 769.222 145.223 12
0 1 3 698.688 115.064 1
0 -1 -3 613.128 108.073 1
0 -1 -3 779.941 143.646 7
0 -1 -3 743.606 99.0099 6
0 1 3 733.391 104.560 6
0 1 -3 684.611 149.379 7
0 1 3 884.221 149.298 12
0 1 -3 749.740 132.233 1
0 -1 3 565.757 129.353 1
0 -1 -3 776.530 149.507 12
0 -1 3 663.645 134.622 7
0 1 3 723.251 141.741 7
0 1 -3 422.514 126.561 12
0 -1 -4 7523.69 347.994 6
0 1 4 6909.20 442.448 12
0 -1 -4 7509.04 452.305 7
0 -1 4 7056.04 424.407 1
0 1 4 7583.49 408.357 1
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0 -1 -4 7009.68 439.958 14
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0 -1 -4 7657.09 462.326 12
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0 -1 -5 44978.1 1514.50 7
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0 1 5 48684.6 1292.33 6
0 -1 5 50409.2 1304.94 6
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0 1 8 730.079 183.025 8
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0 1 -8 660.933 275.157 12
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0 -2 -3 5607.37 282.977 6
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0 3 -1 117.653 52.5253 3
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0 -3 1 130.191 54.1859 2
0 3 1 114.007 47.2215 12
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0 -3 -1 57.1370 47.7481 6
0 -3 -1-5.64373 43.6648 11
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0 3 1 132.191 65.8367 6
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0 -3 1 95.3812 59.1987 1
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0 -3 -2 6080.35 288.453 6
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0 -3 -2 6043.87 310.973 7
0 -3 2 6290.52 335.685 7
0 3 2 6556.47 351.602 14
0 3 2 6218.28 318.191 17
0 -3 2 6560.33 341.093 12
0 -3 2 5975.61 328.226 1
0 -3 -2 6318.84 314.400 17
0 3 -2 6481.92 236.440 16
0 3 -2 6172.97 335.509 2
0 -3 -3 1864.86 207.110 7
0 -3 3 2066.20 222.700 1
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0 -3 -3 2047.89 173.936 6
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0 -3 -3 1739.88 212.712 3
0 -3 -3 2133.02 238.001 14
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0 3 3 2079.14 211.859 12
0 3 3 2067.54 213.329 17
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-10 2 2-277.835 279.018 18
-10 -2 1-130.491 241.667 19
-10 -2 1 254.356 263.299 18
-10 2 1 375.741 401.364 18
10 2 -1 639.360 400.998 10
-10 -2 0-15.9224 230.873 18
-10 2 0 65.0233 271.867 18
10 2 0 321.346 350.232 10
10 -2 0 405.945 336.043 10
-10 2 -1 658.784 366.129 18
10 2 1 1315.82 483.895 10
-10 2 -2 159.451 325.364 3
-10 2 -2 848.470 475.424 18
10 2 2 20.6612 317.221 10
-10 -3 6 213.464 284.424 1
-10 3 5 1471.53 466.370 1
-10 -3 5 1345.40 392.632 1
-10 -3 4 1431.07 396.370 1
-10 -3 4 1733.53 507.336 18
-10 3 4 1617.12 440.468 1
-10 3 3 1349.73 415.096 1
-10 -3 3 1667.61 469.621 18
-10 3 3 1025.10 410.090 18
-10 -3 2 626.870 346.190 19
-10 3 2 504.110 296.066 1
-10 -3 2 131.257 268.682 18
-10 3 2 772.951 375.074 18
-10 -3 1-592.385 333.104 19
-10 -3 1 95.7705 222.970 18
-10 3 1-65.8181 272.830 18
10 3 -1-19.6783 242.942 10
-10 -3 0 316.122 297.494 19
-10 -3 0 71.0527 235.601 18
-10 3 0-96.3735 249.831 18
10 3 0 164.656 271.548 10
-10 3 -1-272.261 270.786 18
10 3 1-324.514 365.013 17
-10 -3 -1 236.774 242.434 7
-10 -3 -1-92.5856 216.936 12
-10 3 -2 4241.18 697.375 3
-10 3 -2 3590.99 692.374 18
10 3 2 3302.99 745.182 17
-10 -3 -2 3507.69 612.149 7
-10 -3 -2 3042.82 557.339 12
10 3 3 141.953 353.518 17
-10 -3 -3 154.520 284.938 7
-10 -3 -3-7.90442 292.030 12
-10 -4 6 567.171 407.188 1
-10 4 5-215.883 344.442 1
-10 -4 5 143.434 270.192 1
-10 4 4 918.630 322.532 1
-10 -4 4 1103.07 413.863 18
-10 -4 3 4430.06 655.583 19
-10 4 3 4030.15 625.086 1
-10 -4 3 3333.21 613.199 18
-10 -4 2 1442.00 403.853 19
-10 -4 2 1311.62 433.079 18
-10 4 2 1264.49 404.031 18
-10 4 2 1329.47 360.144 1
-10 -4 1 1.57121 251.045 19
-10 -4 1 50.2596 218.061 18
-10 4 1 232.496 259.951 18
10 4 -1 83.0553 281.341 10
-10 -4 1 189.400 288.114 7
-10 -4 1-519.016 331.619 12
-10 -4 0 43.7850 272.784 19
-10 4 0-602.183 391.893 18
10 4 0-67.4732 272.502 10
-10 -4 0 128.644 269.414 7
-10 -4 0 53.0548 254.304 12
-10 4 -1 1382.07 432.020 3
-10 4 -1 927.802 391.312 18
10 4 1 766.035 429.984 10
10 4 1 581.951 413.887 17
-10 -4 -1 573.311 338.730 7
-10 -4 -1 518.939 291.264 12
-10 4 -2 1274.13 441.600 3
-10 4 -2 1102.26 425.445 18
10 4 2 1285.05 544.549 17
-10 -4 -2 1379.10 450.582 7
-10 -4 -2 892.443 349.868 12
-10 -5 6 204.421 260.390 1
-10 -5 5 738.292 343.944 1
-10 5 4-178.307 277.624 1
-10 -5 4 63.4828 280.374 19
-10 -5 3 693.076 361.120 12
-10 -5 3 227.643 257.629 19
-10 -5 3 605.051 380.328 18
-10 5 3-378.878 286.062 1
-10 -5 3-35.9556 284.855 7
-10 -5 2 2761.07 565.900 19
-10 -5 2 2953.75 587.846 18
-10 -5 2 2213.51 544.309 7
-10 5 2 2037.18 494.889 1
-10 -5 2 2690.26 551.488 12
-10 -5 1 1450.15 416.467 19
-10 -5 1 1973.54 486.075 18
-10 5 1 1047.63 433.954 18
10 5 -1 949.788 419.342 10
-10 -5 1 1406.29 423.197 7
-10 -5 1 663.127 351.400 12
-10 -5 0-78.4933 296.775 19
-10 5 0 142.077 275.707 18
10 5 0 246.449 334.861 10
-10 -5 0-29.0767 242.004 7
-10 -5 0-474.129 267.981 12
-10 5 -1 1822.89 509.191 3
-10 5 -1 1116.73 439.517 18
10 5 1 479.467 408.005 17
-10 -5 -1 959.999 362.812 7
-10 -5 -1 1246.09 392.715 12
-10 5 -2 5048.81 769.353 3
-10 5 -2 3184.28 676.851 18
10 5 2 4083.15 851.082 17
-10 -5 -2 3340.60 622.990 7
-10 -5 -2 2709.83 566.011 12
-10 5 -3 289.669 331.385 18
10 6 -6-411.079 449.138 2
-10 -6 6 467.738 323.626 1
-10 -6 4 1519.52 480.562 12
-10 6 4 2094.72 493.047 1
-10 -6 4 2095.91 558.541 7
-10 -6 3 821.545 378.895 12
-10 -6 3 1310.57 401.430 19
-10 -6 3 171.336 243.924 18
-10 6 3 1269.32 428.053 1
-10 -6 3 751.971 352.025 7
-10 -6 2 324.721 354.471 12
-10 6 2 1114.89 368.576 1
-10 -6 2 934.877 364.650 19
-10 -6 2 1087.63 356.499 18
-10 -6 2 790.834 356.262 7
-10 -6 1 144.676 266.221 19
-10 -6 1-192.706 267.592 7
-10 6 1-409.269 284.760 1
-10 -6 1 34.3285 238.560 12
-10 -6 0 1012.87 463.361 7
-10 -6 0 1137.17 392.139 12
-10 6 -1 120.944 272.108 3
10 6 1 513.278 369.824 17
-10 -6 -1 545.313 322.741 7
-10 -6 -1 328.278 286.441 12
-10 6 -2 14.2293 272.709 3
10 7 -6-148.858 362.090 2
-10 -7 6 82.6699 341.666 1
-10 -7 5 1066.30 453.313 12
-10 -7 4 1303.67 483.802 12
-10 -7 4 599.330 374.577 7
-10 -7 3 314.270 331.088 12
-10 7 3 403.534 281.233 1
-10 -7 3 417.995 243.830 19
-10 -7 3 671.097 388.934 18
-10 -7 3 1124.27 460.442 7
-10 -7 2 281.081 254.384 12
-10 -7 2-236.911 297.048 19
-10 -7 2 54.1627 239.819 18
-10 7 2 181.976 276.218 1
-10 -7 2-343.451 352.388 7
-10 -7 1 292.508 269.520 19
-10 7 1 188.429 216.448 1
-10 -7 1 444.218 292.426 7
-10 -7 1 853.881 420.142 12
-10 7 0 690.825 382.355 3
-10 -7 0 1200.02 455.027 7
-10 -7 0 1026.76 386.711 12
-10 7 -1 1301.21 438.400 3
-10 -7 -1 1206.46 437.134 7
-10 -7 -1 349.241 327.452 12
-10 -8 5 1871.17 517.197 12
-10 -8 4 2309.62 644.715 12
-10 -8 3-48.6797 293.193 12
-10 -8 3-11.8329 220.577 19
-10 8 3-314.844 341.310 1
-10 -8 3-263.527 284.422 7
-10 -8 2-443.153 339.783 12
-10 8 2-123.575 232.935 1
-10 -8 2 170.786 245.832 19
-10 -8 2 168.282 238.455 18
-10 -8 2-730.890 468.445 7
10 -8 -1 309.698 275.112 11
-10 -8 1 331.701 315.502 19
-10 8 1-400.298 313.609 1
-10 -8 1 113.646 301.478 7
-10 -8 1 253.359 300.551 12
-10 8 0-221.710 283.319 3
-10 -8 0 93.6116 340.498 7
-10 -8 0 457.008 323.609 12
-10 8 -1 808.849 369.098 3
-10 -9 5 1839.10 529.151 4
-10 -9 4 1695.73 563.956 12
-10 -9 3 1114.97 442.986 12
-10 -9 3-72.6553 325.173 7
-10 -9 2 93.9528 292.778 12
10 -9 -2 1084.60 428.157 11
-10 9 2 236.182 254.984 1
-10 -9 2 967.534 361.767 19
-10 -9 2 1296.98 462.484 7
10 -9 -1-92.7541 255.690 11
-10 -9 1 375.241 278.646 19
-10 9 0 399.145 299.915 3
-10 -10 2 454.850 291.934 19
10 -10 -1-174.667 232.134 11
-10 -10 1-439.845 319.164 19
-10 10 0-53.6873 290.774 3
-10 11 1-56.3954 369.224 3
-10 -11 1 181.098 235.108 19
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 52511
_shelx_res_file
;
TITL Alina in P2(1)/c
shelx.res
created by SHELXL-2019/3 at 11:13:19 on 27-Sep-2024
CELL 0.71073 7.869080 22.725520 10.587903 90.0000 98.3861 90.0000
ZERR 2.00 0.0004 0.0008 0.0003 0.0000 0.003 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H P S Br Pd
UNIT 44.00 100.00 4.00 4.00 16.00 4.00
MERG 2
FMAP 2
PLAN 10
L.S. 8
SIZE 0.2 0.1 0.01
TEMP -173
SHEL 999 0.75
ACTA 56
BOND $H
CONF 2.5
BIND Br1 Br2
EQIV $2 1-x, 1-y, 1-z
RTAB CONT S1 Br3_$2
RTAB ANGL P1 S1 Br3_$2
EQIV $3 1+x, y, z
RTAB CONT S1 Br4_$3
RTAB ANGL P1 S1 Br4_$3
REM Instructions for potential hydrogen bonds
EQIV $4 x+1, y, z+1
HTAB C11 Br4_$4
HTAB C12 S1
EQIV $5 x+1, -y+3/2, z+1/2
HTAB C12 Br4_$5
HTAB C13 S1
HTAB C2 Br1
EQIV $1 -x, -y+1, -z+1
HTAB C2 Br3_$1
HTAB C21 Br1
HTAB C21 S1
HTAB C21 Br3_$2
HTAB C31 Br1
HTAB C33 S1
WGHT 0.017700 6.208000
FVAR 0.79634 0.80635 0.80496
BR1 5 0.395927 0.617504 0.468995 11.00000 0.03073 0.02693 =
0.01117 -0.00014 0.00170 -0.00029
P1 3 0.435994 0.635741 0.788362 11.00000 0.02030 0.01526 =
0.01016 0.00048 0.00278 -0.00043
S1 4 0.574144 0.648274 0.635777 11.00000 0.02694 0.02105 =
0.01290 -0.00074 0.00485 -0.00547
PD1 6 -0.001820 0.561590 0.392192 11.00000 0.01969 0.01357 =
0.00967 -0.00032 0.00232 0.00020
BR2 5 0.143305 0.582186 0.210706 11.00000 0.02873 0.02366 =
0.01326 0.00260 0.00672 -0.00171
BR3 5 0.136643 0.464947 0.421821 11.00000 0.02514 0.01705 =
0.01537 0.00110 0.00877 0.00447
BR4 5 -0.146365 0.655497 0.371748 11.00000 0.02966 0.01635 =
0.02103 0.00144 0.00196 0.00486
SAME C1 C11' C12' C13'
SADI C1 C11 C1 C12 C1 C13
SADI C11 C12 C12 C13 C13 C11
RIGU C1 > C33'
C1 1 0.614470 0.637332 0.927161 11.00000 0.02595 0.02084 =
0.01137 -0.00039 0.00119 -0.00593
Part 1 21
C11 1 0.546099 0.614895 1.048031 21.00000 0.02886 0.04175 =
0.01540 0.00267 -0.00094 -0.00877
AFIX 137
H11A 2 0.516541 0.573107 1.037742 21.00000 -1.50000
H11B 2 0.443594 0.637366 1.060595 21.00000 -1.50000
H11C 2 0.634802 0.619982 1.122408 21.00000 -1.50000
AFIX 0
C12 1 0.680131 0.700831 0.952909 21.00000 0.03726 0.02768 =
0.02490 -0.00267 -0.00030 -0.01011
AFIX 137
H12A 2 0.784684 0.700238 1.015776 21.00000 -1.50000
H12B 2 0.591760 0.724207 0.986083 21.00000 -1.50000
H12C 2 0.705636 0.718364 0.873216 21.00000 -1.50000
AFIX 0
C13 1 0.763174 0.598733 0.901503 21.00000 0.02190 0.04386 =
0.01585 -0.00359 -0.00343 0.00523
AFIX 137
H13A 2 0.849008 0.596782 0.978382 21.00000 -1.50000
H13B 2 0.815668 0.615459 0.831111 21.00000 -1.50000
H13C 2 0.720826 0.559044 0.878454 21.00000 -1.50000
AFIX 0
Part 2 -21
C11' 1 0.748771 0.683636 0.901947 -21.00000 0.02634
AFIX 33
H11D 2 0.782645 0.676778 0.817698 -21.00000 -1.50000
H11E 2 0.699108 0.723087 0.904523 -21.00000 -1.50000
H11F 2 0.849914 0.680470 0.967595 -21.00000 -1.50000
AFIX 0
C12' 1 0.708320 0.576666 0.930816 -21.00000 0.01865
AFIX 33
H12D 2 0.748162 0.569631 0.848642 -21.00000 -1.50000
H12E 2 0.806985 0.576953 0.998990 -21.00000 -1.50000
H12F 2 0.628702 0.545347 0.947110 -21.00000 -1.50000
AFIX 0
C13' 1 0.556176 0.645503 1.056887 -21.00000 0.02184
AFIX 33
H13D 2 0.471188 0.615273 1.068942 -21.00000 -1.50000
H13E 2 0.655300 0.641940 1.124171 -21.00000 -1.50000
H13F 2 0.504494 0.684557 1.061098 -21.00000 -1.50000
AFIX 0
Part 0
C2 1 0.325033 0.564481 0.764014 11.00000 0.02180 0.02110 =
0.01292 -0.00027 -0.00080 -0.00586
AFIX 13
H2 2 0.240842 0.569285 0.684305 11.00000 -1.20000
AFIX 0
C21 1 0.440864 0.513593 0.736924 11.00000 0.03426 0.01635 =
0.03944 0.00156 0.00035 0.00043
AFIX 137
H21A 2 0.518108 0.503466 0.815075 11.00000 -1.50000
H21B 2 0.508807 0.525260 0.670503 11.00000 -1.50000
H21C 2 0.370096 0.479360 0.707790 11.00000 -1.50000
AFIX 0
C22 1 0.217108 0.547970 0.867942 11.00000 0.05371 0.04081 =
0.03081 -0.01081 0.01607 -0.02439
AFIX 137
H22A 2 0.155513 0.511174 0.844575 11.00000 -1.50000
H22B 2 0.134199 0.579387 0.876382 11.00000 -1.50000
H22C 2 0.292551 0.542783 0.949374 11.00000 -1.50000
AFIX 0
SAME C3 C31' C32' C33'
SADI C3 C31 C3 C32 C3 C33
SADI C31 C32 C32 C33 C33 C31
C3 1 0.274237 0.696680 0.788678 11.00000 0.02795 0.02449 =
0.02260 -0.00138 0.00438 0.00974
Part 1 31
C31 1 0.115541 0.683461 0.687059 31.00000 0.03623 0.03240 =
0.02089 -0.00719 0.00383 0.01318
AFIX 137
H31A 2 0.029423 0.714453 0.689240 31.00000 -1.50000
H31B 2 0.066127 0.645410 0.705724 31.00000 -1.50000
H31C 2 0.151004 0.682183 0.602136 31.00000 -1.50000
AFIX 0
C32 1 0.214061 0.705883 0.918032 31.00000 0.04520 0.04889 =
0.02323 -0.00952 0.00304 0.01945
AFIX 137
H32A 2 0.309512 0.720990 0.979274 31.00000 -1.50000
H32B 2 0.174793 0.668312 0.948854 31.00000 -1.50000
H32C 2 0.119269 0.734253 0.908965 31.00000 -1.50000
AFIX 0
C33 1 0.354787 0.754796 0.748848 31.00000 0.07073 0.01655 =
0.04560 -0.00280 0.01351 0.00658
AFIX 137
H33A 2 0.267982 0.786020 0.740752 31.00000 -1.50000
H33B 2 0.396150 0.749228 0.666732 31.00000 -1.50000
H33C 2 0.451165 0.765887 0.813872 31.00000 -1.50000
AFIX 0
Part 2 -31
C31' 1 0.166971 0.683858 0.897192 -31.00000 10.02000
AFIX 33
H31D 2 0.110910 0.645445 0.882746 -31.00000 -1.50000
H31E 2 0.242663 0.683535 0.979350 -31.00000 -1.50000
H31F 2 0.079489 0.714485 0.898118 -31.00000 -1.50000
AFIX 0
C32' 1 0.362997 0.756001 0.808189 -31.00000 0.02935
AFIX 33
H32D 2 0.441494 0.755791 0.889056 -31.00000 -1.50000
H32E 2 0.428090 0.763569 0.737704 -31.00000 -1.50000
H32F 2 0.276691 0.786928 0.810399 -31.00000 -1.50000
AFIX 0
C33' 1 0.148295 0.693120 0.663641 -31.00000 0.02184
AFIX 33
H33D 2 0.094962 0.654067 0.656033 -31.00000 -1.50000
H33E 2 0.059080 0.723190 0.663899 -31.00000 -1.50000
H33F 2 0.210480 0.699831 0.591204 -31.00000 -1.50000
Part 0
AFIX 0
HKLF 4
REM Alina in P2(1)/c
REM wR2 = 0.0716, GooF = S = 1.105, Restrained GooF = 1.100 for all data
REM R1 = 0.0421 for 3740 Fo > 4sig(Fo) and 0.0622 for all 4622 data
REM 196 parameters refined using 87 restraints
END
WGHT 0.0177 6.2080
REM Highest difference peak 0.713, deepest hole -0.954, 1-sigma level 0.176
Q1 1 -0.2009 0.6081 0.2615 11.00000 0.05 0.71
Q2 1 0.9467 0.5608 0.9528 11.00000 0.05 0.71
Q3 1 -0.0839 0.5230 0.3266 11.00000 0.05 0.70
Q4 1 0.0866 0.6163 0.2545 11.00000 0.05 0.70
Q5 1 0.2280 0.5269 0.2183 11.00000 0.05 0.70
Q6 1 0.0865 0.6205 0.1801 11.00000 0.05 0.64
Q7 1 0.0843 0.6106 0.0857 11.00000 0.05 0.64
Q8 1 0.8006 0.7489 1.0780 11.00000 0.05 0.64
Q9 1 0.2537 0.5584 0.8242 11.00000 0.05 0.63
Q10 1 0.0575 0.5036 0.3751 11.00000 0.05 0.63
;
_shelx_res_checksum 99091
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Br Br1 0.39593(7) 0.61750(2) 0.46899(5) 0.02308(12) Uani d 1 . .
P P1 0.43599(16) 0.63574(5) 0.78836(12) 0.0152(3) Uani d 1 . .
S S1 0.57414(17) 0.64827(6) 0.63578(12) 0.0201(3) Uani d 1 . .
Pd Pd1 -0.00182(5) 0.56159(2) 0.39219(3) 0.01429(9) Uani d 1 . .
Br Br2 0.14330(7) 0.58219(2) 0.21071(5) 0.02152(12) Uani d 1 . .
Br Br3 0.13664(6) 0.46495(2) 0.42182(5) 0.01861(12) Uani d 1 . .
Br Br4 -0.14636(7) 0.65550(2) 0.37175(5) 0.02252(12) Uani d 1 . .
C C1 0.6145(6) 0.6373(2) 0.9272(4) 0.0195(10) Uani d 1 . .
C C11 0.5461(9) 0.6149(4) 1.0480(6) 0.0291(19) Uani d 0.806(14) A 1
H H11A 0.516541 0.573107 1.037742 0.044 Uiso calc 0.806(14) A 1
H H11B 0.443594 0.637366 1.060595 0.044 Uiso calc 0.806(14) A 1
H H11C 0.634802 0.619982 1.122408 0.044 Uiso calc 0.806(14) A 1
C C12 0.6801(10) 0.7008(3) 0.9529(7) 0.030(2) Uani d 0.806(14) A 1
H H12A 0.784684 0.700238 1.015776 0.046 Uiso calc 0.806(14) A 1
H H12B 0.591760 0.724207 0.986083 0.046 Uiso calc 0.806(14) A 1
H H12C 0.705636 0.718364 0.873216 0.046 Uiso calc 0.806(14) A 1
C C13 0.7632(9) 0.5987(4) 0.9015(7) 0.028(2) Uani d 0.806(14) A 1
H H13A 0.849008 0.596782 0.978382 0.042 Uiso calc 0.806(14) A 1
H H13B 0.815668 0.615459 0.831111 0.042 Uiso calc 0.806(14) A 1
H H13C 0.720826 0.559044 0.878454 0.042 Uiso calc 0.806(14) A 1
C C11' 0.749(3) 0.6836(11) 0.902(3) 0.026(8) Uiso d 0.194(14) A 2
H H11D 0.782645 0.676778 0.817698 0.040 Uiso calc 0.194(14) A 2
H H11E 0.699108 0.723087 0.904523 0.040 Uiso calc 0.194(14) A 2
H H11F 0.849914 0.680470 0.967595 0.040 Uiso calc 0.194(14) A 2
C C12' 0.708(4) 0.5767(8) 0.931(3) 0.019(7) Uiso d 0.194(14) A 2
H H12D 0.748162 0.569631 0.848642 0.028 Uiso calc 0.194(14) A 2
H H12E 0.806985 0.576953 0.998990 0.028 Uiso calc 0.194(14) A 2
H H12F 0.628702 0.545347 0.947110 0.028 Uiso calc 0.194(14) A 2
C C13' 0.556(4) 0.6455(14) 1.0569(19) 0.022(8) Uiso d 0.194(14) A 2
H H13D 0.471188 0.615273 1.068942 0.033 Uiso calc 0.194(14) A 2
H H13E 0.655300 0.641940 1.124171 0.033 Uiso calc 0.194(14) A 2
H H13F 0.504494 0.684557 1.061098 0.033 Uiso calc 0.194(14) A 2
C C2 0.3250(6) 0.5645(2) 0.7640(5) 0.0189(10) Uani d 1 . .
H H2 0.240842 0.569285 0.684305 0.023 Uiso calc 1 . .
C C21 0.4409(7) 0.5136(2) 0.7369(6) 0.0305(13) Uani d 1 . .
H H21A 0.518108 0.503466 0.815075 0.046 Uiso calc 1 . .
H H21B 0.508807 0.525260 0.670503 0.046 Uiso calc 1 . .
H H21C 0.370096 0.479360 0.707790 0.046 Uiso calc 1 . .
C C22 0.2171(9) 0.5480(3) 0.8679(6) 0.0408(16) Uani d 1 . .
H H22A 0.155513 0.511174 0.844575 0.061 Uiso calc 1 . .
H H22B 0.134199 0.579387 0.876382 0.061 Uiso calc 1 . .
H H22C 0.292551 0.542783 0.949374 0.061 Uiso calc 1 . .
C C3 0.2742(7) 0.6967(2) 0.7887(5) 0.0249(12) Uani d 1 . .
C C31 0.1155(13) 0.6835(5) 0.6871(9) 0.030(2) Uani d 0.80(3) B 1
H H31A 0.029423 0.714453 0.689240 0.045 Uiso calc 0.80(3) B 1
H H31B 0.066127 0.645410 0.705724 0.045 Uiso calc 0.80(3) B 1
H H31C 0.151004 0.682183 0.602136 0.045 Uiso calc 0.80(3) B 1
C C32 0.2141(15) 0.7059(6) 0.9180(7) 0.039(3) Uani d 0.80(3) B 1
H H32A 0.309512 0.720990 0.979274 0.059 Uiso calc 0.80(3) B 1
H H32B 0.174793 0.668312 0.948854 0.059 Uiso calc 0.80(3) B 1
H H32C 0.119269 0.734253 0.908965 0.059 Uiso calc 0.80(3) B 1
C C33 0.3548(12) 0.7548(3) 0.7488(14) 0.044(3) Uani d 0.80(3) B 1
H H33A 0.267982 0.786020 0.740752 0.066 Uiso calc 0.80(3) B 1
H H33B 0.396150 0.749228 0.666732 0.066 Uiso calc 0.80(3) B 1
H H33C 0.451165 0.765887 0.813872 0.066 Uiso calc 0.80(3) B 1
C C31' 0.167(4) 0.6839(16) 0.897(3) 0.020 Uiso d 0.20(3) B 2
H H31D 0.110910 0.645445 0.882746 0.030 Uiso calc 0.20(3) B 2
H H31E 0.242663 0.683535 0.979350 0.030 Uiso calc 0.20(3) B 2
H H31F 0.079489 0.714485 0.898118 0.030 Uiso calc 0.20(3) B 2
C C32' 0.363(4) 0.7560(10) 0.808(4) 0.029(10) Uiso d 0.20(3) B 2
H H32D 0.441494 0.755791 0.889056 0.044 Uiso calc 0.20(3) B 2
H H32E 0.428090 0.763569 0.737704 0.044 Uiso calc 0.20(3) B 2
H H32F 0.276691 0.786928 0.810399 0.044 Uiso calc 0.20(3) B 2
C C33' 0.148(5) 0.693(2) 0.664(2) 0.022(10) Uiso d 0.20(3) B 2
H H33D 0.094962 0.654067 0.656033 0.033 Uiso calc 0.20(3) B 2
H H33E 0.059080 0.723190 0.663899 0.033 Uiso calc 0.20(3) B 2
H H33F 0.210480 0.699831 0.591204 0.033 Uiso calc 0.20(3) B 2
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
Br1 0.0307(3) 0.0269(3) 0.0112(2) -0.0003(2) 0.0017(2) -0.0001(2)
P1 0.0203(6) 0.0153(6) 0.0102(6) -0.0004(5) 0.0028(5) 0.0005(5)
S1 0.0269(7) 0.0211(7) 0.0129(6) -0.0055(5) 0.0049(5) -0.0007(5)
Pd1 0.01969(19) 0.01357(18) 0.00967(18) 0.00020(14) 0.00232(14) -0.00032(14)
Br2 0.0287(3) 0.0237(3) 0.0133(2) -0.0017(2) 0.0067(2) 0.0026(2)
Br3 0.0251(3) 0.0171(2) 0.0154(2) 0.0045(2) 0.0088(2) 0.00110(19)
Br4 0.0297(3) 0.0163(3) 0.0210(3) 0.0049(2) 0.0020(2) 0.0014(2)
C1 0.026(3) 0.021(3) 0.011(2) -0.006(2) 0.001(2) -0.0004(19)
C11 0.029(4) 0.042(5) 0.015(3) -0.009(4) -0.001(3) 0.003(3)
C12 0.037(4) 0.028(4) 0.025(4) -0.010(3) 0.000(3) -0.003(3)
C13 0.022(4) 0.044(5) 0.016(4) 0.005(3) -0.003(3) -0.004(3)
C2 0.022(3) 0.021(3) 0.013(2) -0.006(2) -0.001(2) 0.000(2)
C21 0.034(3) 0.016(3) 0.039(4) 0.000(2) 0.000(3) 0.002(2)
C22 0.054(4) 0.041(4) 0.031(3) -0.024(3) 0.016(3) -0.011(3)
C3 0.028(3) 0.024(3) 0.023(3) 0.010(2) 0.004(2) -0.001(2)
C31 0.036(5) 0.032(5) 0.021(4) 0.013(4) 0.004(4) -0.007(4)
C32 0.045(6) 0.049(7) 0.023(4) 0.019(5) 0.003(4) -0.010(4)
C33 0.071(6) 0.017(4) 0.046(7) 0.007(3) 0.014(5) -0.003(4)
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'
Pd Pd -0.9988 1.0072 '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 Br1 Br2 . . 175.04(4) y
C2 P1 C1 . . 114.3(2) ?
C2 P1 C3 . . 109.9(2) ?
C1 P1 C3 . . 114.4(2) ?
C2 P1 S1 . . 107.50(17) y
C1 P1 S1 . . 100.83(16) y
C3 P1 S1 . . 109.19(17) y
P1 S1 Br1 . . 103.52(7) y
Br4 Pd1 Br2 . . 91.64(2) y
Br4 Pd1 Br3 . 3_566 92.07(2) y
Br2 Pd1 Br3 . 3_566 176.25(2) y
Br4 Pd1 Br3 . . 177.07(2) y
Br2 Pd1 Br3 . . 91.29(2) y
Br3 Pd1 Br3 3_566 . 85.00(2) y
Pd1 Br2 Br1 . . 71.340(18) y
Pd1 Br3 Pd1 3_566 . 95.00(2) y
C13' C1 C11' . . 112.2(14) ?
C13 C1 C12 . . 109.0(5) ?
C13 C1 C11 . . 109.1(5) ?
C12 C1 C11 . . 108.1(5) ?
C13' C1 C12' . . 106.8(14) ?
C11' C1 C12' . . 105.9(13) ?
C13 C1 P1 . . 110.9(4) ?
C13' C1 P1 . . 114.8(12) ?
C11' C1 P1 . . 109.3(11) ?
C12 C1 P1 . . 110.4(4) ?
C11 C1 P1 . . 109.3(4) ?
C12' C1 P1 . . 107.4(11) ?
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 ?
C1 C11' H11D . . 109.5 ?
C1 C11' H11E . . 109.5 ?
H11D C11' H11E . . 109.5 ?
C1 C11' H11F . . 109.5 ?
H11D C11' H11F . . 109.5 ?
H11E C11' H11F . . 109.5 ?
C1 C12' H12D . . 109.5 ?
C1 C12' H12E . . 109.5 ?
H12D C12' H12E . . 109.5 ?
C1 C12' H12F . . 109.5 ?
H12D C12' H12F . . 109.5 ?
H12E C12' H12F . . 109.5 ?
C1 C13' H13D . . 109.5 ?
C1 C13' H13E . . 109.5 ?
H13D C13' H13E . . 109.5 ?
C1 C13' H13F . . 109.5 ?
H13D C13' H13F . . 109.5 ?
H13E C13' H13F . . 109.5 ?
C21 C2 C22 . . 111.0(5) ?
C21 C2 P1 . . 114.2(4) ?
C22 C2 P1 . . 114.6(4) ?
C21 C2 H2 . . 105.3 ?
C22 C2 H2 . . 105.3 ?
P1 C2 H2 . . 105.3 ?
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 ?
C32' C3 C33' . . 113.0(18) ?
C32' C3 C31' . . 110.8(15) ?
C33' C3 C31' . . 106.1(16) ?
C32 C3 C33 . . 108.7(5) ?
C32 C3 C31 . . 108.9(6) ?
C33 C3 C31 . . 107.2(6) ?
C32' C3 P1 . . 110.8(15) ?
C32 C3 P1 . . 113.6(4) ?
C33' C3 P1 . . 108.1(19) ?
C31' C3 P1 . . 107.7(12) ?
C33 C3 P1 . . 108.9(4) ?
C31 C3 P1 . . 109.4(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 ?
C3 C31' H31D . . 109.5 ?
C3 C31' H31E . . 109.5 ?
H31D C31' H31E . . 109.5 ?
C3 C31' H31F . . 109.5 ?
H31D C31' H31F . . 109.5 ?
H31E C31' H31F . . 109.5 ?
C3 C32' H32D . . 109.5 ?
C3 C32' H32E . . 109.5 ?
H32D C32' H32E . . 109.5 ?
C3 C32' H32F . . 109.5 ?
H32D C32' H32F . . 109.5 ?
H32E C32' H32F . . 109.5 ?
C3 C33' H33D . . 109.5 ?
C3 C33' H33E . . 109.5 ?
H33D C33' H33E . . 109.5 ?
C3 C33' H33F . . 109.5 ?
H33D C33' H33F . . 109.5 ?
H33E C33' H33F . . 109.5 ?
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
Br1 S1 . 2.2027(14) y
Br1 Br2 . 3.2387(7) y
P1 C2 . 1.840(5) ?
P1 C1 . 1.879(5) ?
P1 C3 . 1.881(5) ?
P1 S1 . 2.0941(18) y
Pd1 Br4 . 2.4131(6) y
Pd1 Br2 . 2.4199(6) y
Pd1 Br3 3_566 2.4447(6) y
Pd1 Br3 . 2.4514(6) y
C1 C13 . 1.518(7) ?
C1 C13' . 1.522(14) ?
C1 C11' . 1.542(14) ?
C1 C12 . 1.544(7) ?
C1 C11 . 1.545(7) ?
C1 C12' . 1.562(13) ?
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 ?
C11' H11D . 0.9800 ?
C11' H11E . 0.9800 ?
C11' H11F . 0.9800 ?
C12' H12D . 0.9800 ?
C12' H12E . 0.9800 ?
C12' H12F . 0.9800 ?
C13' H13D . 0.9800 ?
C13' H13E . 0.9800 ?
C13' H13F . 0.9800 ?
C2 C21 . 1.525(7) ?
C2 C22 . 1.531(7) ?
C2 H2 . 1.0000 ?
C21 H21A . 0.9800 ?
C21 H21B . 0.9800 ?
C21 H21C . 0.9800 ?
C22 H22A . 0.9800 ?
C22 H22B . 0.9800 ?
C22 H22C . 0.9800 ?
C3 C32' . 1.518(14) ?
C3 C32 . 1.527(8) ?
C3 C33' . 1.536(14) ?
C3 C31' . 1.549(14) ?
C3 C33 . 1.550(8) ?
C3 C31 . 1.554(8) ?
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 ?
C31' H31D . 0.9800 ?
C31' H31E . 0.9800 ?
C31' H31F . 0.9800 ?
C32' H32D . 0.9800 ?
C32' H32E . 0.9800 ?
C32' H32F . 0.9800 ?
C33' H33D . 0.9800 ?
C33' H33E . 0.9800 ?
C33' H33F . 0.9800 ?
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
C11 H11C Br4 1_656 0.98 3.04 4.005(7) 167.2 yes
C12 H12C S1 . 0.98 3.03 3.547(7) 114.4 yes
C12 H12C Br4 4_676 0.98 3.10 3.689(6) 120.4 yes
C13 H13B S1 . 0.98 2.70 3.190(7) 111.2 yes
C2 H2 Br1 . 1.00 2.95 3.468(5) 113.3 yes
C2 H2 Br3 3_566 1.00 3.12 3.928(5) 139.1 yes
C21 H21B Br1 . 0.98 3.03 3.668(6) 123.9 yes
C21 H21B S1 . 0.98 2.88 3.456(6) 118.8 yes
C21 H21B Br3 3_666 0.98 3.10 3.968(6) 149.0 yes
C31 H31C Br1 . 0.98 2.94 3.732(11) 138.5 yes
C33 H33B S1 . 0.98 2.73 3.298(10) 117.2 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 Br1 . . . . 41.39(18) ?
C1 P1 S1 Br1 . . . . 161.38(15) ?
C3 P1 S1 Br1 . . . . -77.83(18) ?
Br4 Pd1 Br2 Br1 . . . . 95.390(19) ?
Br3 Pd1 Br2 Br1 . . . . -84.823(19) ?
Br2 Pd1 Br3 Pd1 . . . 3_566 179.44(2) ?
Br3 Pd1 Br3 Pd1 3_566 . . 3_566 0.0 ?
C2 P1 C1 C13 . . . . 68.1(5) ?
C3 P1 C1 C13 . . . . -163.9(5) ?
S1 P1 C1 C13 . . . . -46.9(5) ?
C2 P1 C1 C13' . . . . -80.4(14) ?
C3 P1 C1 C13' . . . . 47.6(14) ?
S1 P1 C1 C13' . . . . 164.6(14) ?
C2 P1 C1 C11' . . . . 152.6(14) ?
C3 P1 C1 C11' . . . . -79.4(14) ?
S1 P1 C1 C11' . . . . 37.6(14) ?
C2 P1 C1 C12 . . . . -171.1(4) ?
C3 P1 C1 C12 . . . . -43.1(5) ?
S1 P1 C1 C12 . . . . 74.0(4) ?
C2 P1 C1 C11 . . . . -52.3(5) ?
C3 P1 C1 C11 . . . . 75.7(5) ?
S1 P1 C1 C11 . . . . -167.3(4) ?
C2 P1 C1 C12' . . . . 38.2(13) ?
C3 P1 C1 C12' . . . . 166.2(13) ?
S1 P1 C1 C12' . . . . -76.8(13) ?
C1 P1 C2 C21 . . . . -60.8(4) ?
C3 P1 C2 C21 . . . . 169.0(4) ?
S1 P1 C2 C21 . . . . 50.2(4) ?
C1 P1 C2 C22 . . . . 68.8(5) ?
C3 P1 C2 C22 . . . . -61.4(5) ?
S1 P1 C2 C22 . . . . 179.8(4) ?
C2 P1 C3 C32' . . . . -179.8(19) ?
C1 P1 C3 C32' . . . . 50.0(19) ?
S1 P1 C3 C32' . . . . -62.1(19) ?
C2 P1 C3 C32 . . . . 83.8(8) ?
C1 P1 C3 C32 . . . . -46.4(8) ?
S1 P1 C3 C32 . . . . -158.5(7) ?
C2 P1 C3 C33' . . . . -55.5(17) ?
C1 P1 C3 C33' . . . . 174.4(17) ?
S1 P1 C3 C33' . . . . 62.2(17) ?
C2 P1 C3 C31' . . . . 58.8(17) ?
C1 P1 C3 C31' . . . . -71.4(17) ?
S1 P1 C3 C31' . . . . 176.5(16) ?
C2 P1 C3 C33 . . . . -155.0(6) ?
C1 P1 C3 C33 . . . . 74.8(7) ?
S1 P1 C3 C33 . . . . -37.3(7) ?
C2 P1 C3 C31 . . . . -38.2(7) ?
C1 P1 C3 C31 . . . . -168.4(6) ?
S1 P1 C3 C31 . . . . 79.5(6) ?