#------------------------------------------------------------------------------
#$Date: 2025-02-05 05:03:59 +0200 (Wed, 05 Feb 2025) $
#$Revision: 297594 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023379.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_2023379
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 S2)2 [Pd2 Br6]'
_chemical_formula_moiety '2(C11 H25 Br P Se +), Pd2 Br6 2-'
_chemical_formula_sum 'C22 H50 Br8 P2 Pd2 Se2'
_chemical_formula_weight 1386.56
_chemical_name_systematic
;
(Bromoselanyl)di-tert-butylisopropylphosphanium
di-\m-bromido-bis[dibromidopalladium(II)]
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/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 125.957(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 19.3550(6)
_cell_length_b 14.8165(2)
_cell_length_c 16.3047(5)
_cell_measurement_reflns_used 7808
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.8018
_cell_measurement_theta_min 2.5948
_cell_volume 3784.8(3)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.35.11 (Rigaku OD, 2012)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.35.11 (Rigaku OD, 2012)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.35.11 (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 0.986
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0737
_diffrn_reflns_av_unetI/netI 0.0456
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 51432
_diffrn_reflns_theta_full 30.000
_diffrn_reflns_theta_max 30.871
_diffrn_reflns_theta_min 2.600
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 11.419
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.32647
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2012)
;
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 2.433
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 2608
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.02
_refine_diff_density_max 0.969
_refine_diff_density_min -1.020
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 172
_refine_ls_number_reflns 5622
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.037
_refine_ls_R_factor_all 0.0507
_refine_ls_R_factor_gt 0.0312
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0187P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0521
_refine_ls_wR_factor_ref 0.0565
_reflns_number_gt 4433
_reflns_number_total 5622
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2063.cif
_cod_data_source_block 8
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 2023379
_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 0.209
_shelx_estimated_absorpt_t_max 0.804
_shelx_hkl_file
;
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0 0 2 66404.8 1978.51
0 0 -2 64155.0 2031.99
0 0 -2 67197.2 1979.33
0 0 2 67090.5 1949.99
0 0 -2 64516.5 1966.36
0 0 2 69584.3 1988.64
0 0 -2 67011.5 1946.21
0 0 2 64218.7 2033.73
0 0 -2 64204.6 2029.57
0 0 -2 67709.9 1941.29
0 0 2 67328.2 2055.91
0 0 2 66885.8 1945.61
0 0 3 50.7525 106.444
0 0 -3 96.5670 79.9001
0 0 3 54.3966 74.9741
0 0 -3 237.266 128.021
0 0 3 47.2756 73.2541
0 0 -3 134.868 125.164
0 0 3-22.6320 70.5387
0 0 -3 44.8002 72.6802
0 0 3 288.224 123.656
0 0 -3 6.48956 62.9602
0 0 3 71.4168 91.0975
0 0 -3 18.8176 66.3468
0 0 3 50.5499 92.4184
0 0 3 98.0637 76.9344
0 0 -3-11.2688 72.3181
0 0 4 161262. 4922.77
0 0 -4 167685. 5001.88
0 0 -4 171549. 5132.42
0 0 -4 172466. 4920.24
0 0 -4 170316. 4991.09
0 0 4 174042. 4928.99
0 0 4 181692. 5036.53
0 0 4 178488. 5179.97
0 0 -4 166581. 5127.76
0 0 4 173538. 4958.48
0 0 -4 163123. 5108.77
0 0 4 175935. 5141.83
0 0 4 179381. 5031.19
0 0 -5 10.4061 105.512
0 0 5-29.8754 116.128
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0 0 5-88.9294 89.8672
0 0 -5-42.5451 94.3420
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0 0 6 71021.3 2424.11
0 0 -6 66274.7 2635.95
0 0 -6 73441.1 2253.29
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0 0 -6 72641.2 2509.68
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0 0 -7-65.8600 83.9790
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0 0 7 14.9199 89.8403
0 0 -7 307.573 188.652
0 0 7 21.7399 112.410
0 0 7-76.1788 66.8783
0 0 -7 193.865 194.932
0 0 8 286179. 8600.60
0 0 8 308566. 8139.84
0 0 8 290850. 8642.50
0 0 8 291426. 8498.54
0 0 -8 294278. 9037.63
0 0 -8 283168. 9042.53
0 0 -8 293635. 8783.07
0 0 -8 300947. 8349.80
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0 0 -9 158.637 181.936
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0 0 9 88.8295 105.385
0 0 -10 439.803 268.422
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0 0 10 285.373 226.120
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0 0 -11-39.5026 217.734
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0 0 12 37546.2 1769.96
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0 0 -12 35090.2 2162.26
0 0 -12 36873.4 2267.82
0 0 -12 35714.5 2004.50
0 0 12 36582.6 1896.63
0 0 -13 71.6755 244.599
0 0 13 17.1385 170.008
0 0 -13-87.6052 318.104
0 0 13 382.990 269.306
0 0 -13 163.960 242.540
0 0 -14 41156.8 2557.50
0 0 -14 41888.1 2377.39
0 0 -14 39311.7 2591.94
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-25 5 15 3163.21 753.874
25 5 -14 4677.84 1115.40
-25 5 14 4829.67 948.067
25 5 -14 6122.27 984.230
-25 -5 14 5027.10 885.046
25 -5 -14 5582.77 1141.41
-25 5 14 6309.58 1014.54
25 5 -13 3831.07 970.213
25 5 -13 6473.66 1029.05
-25 5 13 5865.88 995.418
-25 -5 13 4785.77 824.219
25 -5 -13 5163.29 1097.60
25 5 -13 3131.72 1054.95
-25 5 13 4346.80 866.296
25 5 -12-203.508 416.313
25 5 -12 319.644 477.682
-25 5 12 135.656 375.207
-25 -5 12-197.826 414.303
25 -5 -12 1058.22 506.386
25 5 -12 549.261 563.802
-25 5 12 195.667 420.376
25 -5 -12 403.557 489.410
25 5 -11 317.308 424.932
25 5 -11-127.241 450.479
-25 5 11 604.880 478.586
-25 -5 11 522.986 350.519
25 -5 -11 1088.56 799.826
25 5 -11-28.3357 537.176
-25 5 11-71.3661 430.592
25 -5 -11 391.260 336.713
25 5 -10 3079.65 977.283
-25 5 10 3911.62 831.286
-25 -5 10 2880.42 708.156
25 -5 -10 1823.04 701.394
-25 5 10 3238.23 823.131
25 -5 -10 3132.26 788.014
-25 5 9-39.4012 353.066
-25 -5 9 549.372 369.704
25 -5 -9 715.752 452.631
25 -5 -9 416.528 404.785
-25 -5 8-216.400 414.498
25 -5 -8-92.9851 381.844
25 -5 -8 469.284 438.997
25 -5 -7 3350.69 807.438
25 -5 -6 2613.97 817.588
25 7 -17 3081.67 712.440
25 7 -16 349.496 482.174
25 -7 -15-421.976 595.677
-25 7 15-62.7903 432.957
-25 7 14 167.874 462.920
-25 7 14 1964.71 636.731
-25 7 13 40.5094 421.839
25 -7 -13-804.133 660.575
-25 7 13-319.225 430.757
-25 7 12 153.291 429.951
-25 -7 12 242.253 345.362
25 -7 -12 63.6752 465.521
-25 7 12 69.6187 487.745
-25 7 11 2189.17 648.355
-25 -7 11 1568.96 512.587
25 -7 -11 2539.34 823.199
-25 7 11 3968.10 831.832
-25 -7 10 309.199 309.401
25 -7 -10 494.293 548.471
-25 -7 9 2220.45 632.881
25 -7 -9 740.215 548.891
-25 -7 8 1425.32 525.847
-25 9 13 216.253 440.831
-25 9 12-855.505 523.273
26 0 -14-455.588 597.522
-26 0 14-9.68476 408.001
26 0 -13-216.659 488.829
-26 0 13-462.421 461.282
26 0 -12 16768.7 1878.41
-26 0 12 15423.1 1536.08
-26 0 12 16287.7 1768.10
26 0 -11 268.654 497.169
26 0 -10 13044.0 1671.32
26 0 -9 923.981 591.430
26 0 -8 630.500 661.243
26 2 -17 855.527 476.406
-26 2 17 2008.13 627.924
26 2 -16 2636.85 858.615
26 2 -16 4371.02 818.537
-26 2 16 3777.45 871.080
26 2 -15 1500.52 660.763
26 2 -15 1292.62 527.067
26 -2 -15 3396.36 925.775
-26 2 15 2525.41 664.506
26 2 -14 1712.94 833.030
26 2 -14 2326.62 671.536
-26 2 14 2649.04 750.787
26 -2 -14 2387.32 798.506
-26 2 14 1581.18 630.396
26 2 -13 1756.20 660.660
26 2 -13 3648.22 793.369
-26 2 13 1870.54 675.936
-26 -2 13 2835.09 831.652
26 -2 -13 3027.67 1036.09
-26 2 13 2123.17 722.653
26 2 -12-15.5193 378.814
-26 2 12 456.754 377.372
-26 -2 12 1105.48 652.529
26 -2 -12 800.097 584.632
26 2 -11 971.928 536.285
-26 2 11 858.862 432.278
-26 -2 11 296.186 394.902
26 2 -10-609.676 520.769
26 -2 -9 3860.53 964.244
26 2 -9 3142.27 839.111
26 -2 -8 3862.09 906.936
26 -2 -7-226.661 504.259
-26 4 18-198.011 449.171
26 4 -17-196.459 413.169
26 4 -17 849.932 670.156
-26 4 17 639.195 506.811
26 4 -16 478.655 494.025
-26 4 16-151.366 368.066
26 4 -15 3423.16 778.193
26 4 -15 4383.63 1180.01
26 -4 -15 4473.66 1127.14
-26 4 15 2190.43 703.087
26 4 -14 10167.6 1286.56
26 4 -14 12416.1 1873.15
-26 4 14 12794.1 1514.35
-26 -4 14 10311.4 1367.00
26 -4 -14 12010.4 1709.62
-26 4 14 12858.4 1503.15
26 4 -13 765.296 871.708
-26 4 13-395.848 338.338
-26 -4 13-350.670 429.504
26 -4 -13 98.8750 578.140
26 4 -13 393.356 490.400
26 4 -12 7236.42 1403.35
-26 4 12 8472.15 1202.05
-26 -4 12 9463.17 1241.04
26 -4 -12 11383.9 1657.17
-26 4 11-617.099 443.495
-26 -4 11-2.32930 311.234
-26 4 10 2707.03 747.934
-26 -4 10 2429.19 609.297
-26 6 16 959.984 494.911
-26 -6 14 294.322 451.375
26 -6 -14-243.884 568.248
-26 -6 13 414.436 484.893
26 -6 -13-275.727 587.050
-26 6 12 250.963 354.704
-26 -6 12 360.857 427.738
-26 -6 11 1069.17 454.627
-26 -6 10-362.139 479.368
27 1 -16-246.030 328.243
27 1 -14 731.155 432.897
27 1 -13 91.3745 713.972
27 1 -12 740.153 435.890
27 1 -11 415.445 623.723
27 -1 -10 1796.44 776.952
;
_shelx_hkl_checksum 94815
_shelx_res_file
;
TITL Georg in C2/c
shelx.res
created by SHELXL-2019/3 at 11:15:47 on 26-Sep-2024
CELL 0.71073 19.355026 14.816505 16.304728 90.0000 125.9568 90.0000
ZERR 4.00 0.000607 0.000222 0.000504 0.0000 0.0046 0.0000
LATT 7
SYMM -x, y,-z+1/2
SFAC C H P Se Br Pd
UNIT 88.00 200.00 8.00 8.00 32.00 8.00
L.S. 6
FMAP 2
PLAN 10
SIZE 0.2 0.06 0.02
TEMP -173
OMIT 0 2 0
OMIT -2 4 1
ACTA 60
CONF 2.3
BOND $H
RTAB CONT Pd1 Pd2
BIND Br1 Br2
RTAB CONT Br1 Pd2
RTAB ANGL Se1 Br1 Pd2
EQIV $4 0.5-x, 1.5-y, -z
RTAB CONT Se1 Br4_$4
RTAB ANGL P1 Se1 Br4_$4
RTAB ANGL Se1 Br4_$4 Pd2_$4
RTAB CONT Se1 Br3_$4
RTAB ANGL P1 Se1 Br3_$4
RTAB ANGL Se1 Br3_$4 Pd1_$4
RTAB ANGL Se1 Br3_$4 Pd2_$4
REM Instructions for potential hydrogen bonds
HTAB C12 Se1
HTAB C13 Se1
HTAB C21 Br3
HTAB C21 Se1
HTAB C21 Br1
HTAB C31 Se1
HTAB C32 Se1
HTAB C32 Br1
EQIV $2 x-1/2, y-1/2, z
HTAB C12 Br2_$2
HTAB C12 Br3_$4
EQIV $1 -x+1, y, -z+1/2
HTAB C2 Br3_$1
EQIV $3 x, -y+2, z+1/2
HTAB C32 Br2_$3
WGHT 0.018700
FVAR 0.49716
P1 3 0.228485 0.778718 0.244382 11.00000 0.01037 0.00662 =
0.00937 0.00008 0.00622 0.00005
SE1 4 0.166733 0.879652 0.116976 11.00000 0.01218 0.00876 =
0.01024 0.00079 0.00600 -0.00039
BR1 5 0.282061 0.915647 0.113175 11.00000 0.01752 0.01363 =
0.01470 -0.00010 0.01135 -0.00296
C1 1 0.131644 0.721767 0.220250 11.00000 0.00939 0.00956 =
0.01472 0.00127 0.00676 -0.00029
C11 1 0.154031 0.669282 0.313672 11.00000 0.02232 0.01781 =
0.02098 0.00595 0.01419 0.00018
AFIX 137
H11A 2 0.171302 0.711590 0.368829 11.00000 -1.50000
H11B 2 0.201090 0.627609 0.334906 11.00000 -1.50000
H11C 2 0.104049 0.635007 0.297163 11.00000 -1.50000
AFIX 0
C12 1 0.095626 0.656494 0.130987 11.00000 0.01203 0.01170 =
0.01795 -0.00137 0.00772 -0.00194
AFIX 137
H12A 2 0.043484 0.628429 0.115900 11.00000 -1.50000
H12B 2 0.137963 0.609596 0.148605 11.00000 -1.50000
H12C 2 0.082397 0.689711 0.071368 11.00000 -1.50000
AFIX 0
C13 1 0.062863 0.791826 0.192012 11.00000 0.01359 0.01627 =
0.01545 -0.00002 0.00811 0.00016
AFIX 137
H13A 2 0.013385 0.761667 0.182044 11.00000 -1.50000
H13B 2 0.045404 0.822396 0.129251 11.00000 -1.50000
H13C 2 0.085754 0.836281 0.246658 11.00000 -1.50000
AFIX 0
C2 1 0.297494 0.701952 0.232583 11.00000 0.01152 0.01052 =
0.01475 -0.00287 0.00833 -0.00008
AFIX 13
H2 2 0.351708 0.735864 0.260464 11.00000 -1.20000
AFIX 0
C21 1 0.263154 0.676596 0.123157 11.00000 0.02050 0.01412 =
0.02139 -0.00311 0.01608 0.00180
AFIX 137
H21A 2 0.308543 0.647598 0.122918 11.00000 -1.50000
H21B 2 0.244019 0.731244 0.081387 11.00000 -1.50000
H21C 2 0.215056 0.634815 0.095559 11.00000 -1.50000
AFIX 0
C22 1 0.323242 0.616067 0.296738 11.00000 0.01814 0.01453 =
0.02215 0.00599 0.01234 0.00493
AFIX 137
H22A 2 0.273840 0.575778 0.266646 11.00000 -1.50000
H22B 2 0.343204 0.632082 0.365724 11.00000 -1.50000
H22C 2 0.369143 0.585433 0.298861 11.00000 -1.50000
AFIX 0
C3 1 0.295139 0.839895 0.368097 11.00000 0.01317 0.01235 =
0.01011 -0.00178 0.00640 -0.00186
C31 1 0.238715 0.896444 0.385343 11.00000 0.01752 0.01791 =
0.01611 -0.00568 0.01064 -0.00392
AFIX 137
H31A 2 0.205657 0.856415 0.398084 11.00000 -1.50000
H31B 2 0.199669 0.933141 0.325067 11.00000 -1.50000
H31C 2 0.274628 0.936049 0.443940 11.00000 -1.50000
AFIX 0
C32 1 0.355944 0.903622 0.363865 11.00000 0.01773 0.01599 =
0.01501 -0.00611 0.01006 -0.00595
AFIX 137
H32A 2 0.322466 0.947762 0.309403 11.00000 -1.50000
H32B 2 0.391368 0.868362 0.350777 11.00000 -1.50000
H32C 2 0.392649 0.935251 0.428725 11.00000 -1.50000
AFIX 0
C33 1 0.351345 0.775634 0.458198 11.00000 0.02000 0.02221 =
0.00984 0.00140 0.00421 0.00014
AFIX 137
H33A 2 0.381125 0.810013 0.521590 11.00000 -1.50000
H33B 2 0.393280 0.746527 0.451519 11.00000 -1.50000
H33C 2 0.315400 0.729465 0.458823 11.00000 -1.50000
AFIX 0
PD1 6 0.500000 0.860209 0.250000 10.50000 0.01055 0.00756 =
0.00919 0.00000 0.00583 0.00000
PD2 6 0.500000 0.617408 0.250000 10.50000 0.01087 0.00836 =
0.01348 0.00000 0.00661 0.00000
BR2 5 0.446772 0.973242 0.118584 11.00000 0.01631 0.01205 =
0.01485 0.00405 0.00962 0.00145
BR3 5 0.456420 0.739494 0.126716 11.00000 0.01799 0.01008 =
0.01034 -0.00139 0.00716 -0.00096
BR4 5 0.450061 0.504419 0.119764 11.00000 0.02289 0.01048 =
0.01998 -0.00316 0.00918 0.00065
HKLF 4
REM Georg in C2/c
REM wR2 = 0.0565, GooF = S = 1.037, Restrained GooF = 1.037 for all data
REM R1 = 0.0312 for 4433 Fo > 4sig(Fo) and 0.0507 for all 5622 data
REM 172 parameters refined using 0 restraints
END
WGHT 0.0187 0.0000
REM Highest difference peak 0.969, deepest hole -1.020, 1-sigma level 0.179
Q1 1 0.4969 0.9715 0.1727 11.00000 0.05 0.97
Q2 1 0.0996 0.7487 0.2038 11.00000 0.05 0.80
Q3 1 0.3899 0.5095 0.3378 11.00000 0.05 0.80
Q4 1 0.1057 0.8890 0.0667 11.00000 0.05 0.79
Q5 1 0.2331 0.9166 0.0604 11.00000 0.05 0.73
Q6 1 0.4582 0.6573 0.2459 11.00000 0.05 0.72
Q7 1 0.4420 0.6160 0.1992 11.00000 0.05 0.71
Q8 1 0.3835 0.9703 0.1504 11.00000 0.05 0.70
Q9 1 0.3367 0.9089 0.2628 11.00000 0.05 0.70
Q10 1 0.5000 0.5096 0.1688 11.00000 0.05 0.70
;
_shelx_res_checksum 92819
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
P P1 0.22849(5) 0.77872(5) 0.24438(6) 0.00853(16) Uani d 1 . .
Se Se1 0.16673(2) 0.87965(2) 0.11698(2) 0.01074(7) Uani d 1 . .
Br Br1 0.28206(2) 0.91565(2) 0.11317(2) 0.01416(8) Uani d 1 . .
C C1 0.13164(18) 0.7218(2) 0.2202(2) 0.0114(6) Uani d 1 . .
C C11 0.1540(2) 0.6693(2) 0.3137(2) 0.0195(7) Uani d 1 . .
H H11A 0.171302 0.711590 0.368829 0.029 Uiso calc 1 . .
H H11B 0.201090 0.627609 0.334906 0.029 Uiso calc 1 . .
H H11C 0.104049 0.635007 0.297163 0.029 Uiso calc 1 . .
C C12 0.09563(19) 0.6565(2) 0.1310(2) 0.0145(7) Uani d 1 . .
H H12A 0.043484 0.628429 0.115900 0.022 Uiso calc 1 . .
H H12B 0.137963 0.609596 0.148605 0.022 Uiso calc 1 . .
H H12C 0.082397 0.689711 0.071368 0.022 Uiso calc 1 . .
C C13 0.06286(19) 0.7918(2) 0.1920(2) 0.0154(7) Uani d 1 . .
H H13A 0.013385 0.761667 0.182044 0.023 Uiso calc 1 . .
H H13B 0.045404 0.822396 0.129251 0.023 Uiso calc 1 . .
H H13C 0.085754 0.836281 0.246658 0.023 Uiso calc 1 . .
C C2 0.29749(19) 0.7020(2) 0.2326(2) 0.0119(6) Uani d 1 . .
H H2 0.351708 0.735864 0.260464 0.014 Uiso calc 1 . .
C C21 0.2632(2) 0.6766(2) 0.1232(2) 0.0164(7) Uani d 1 . .
H H21A 0.308543 0.647598 0.122918 0.025 Uiso calc 1 . .
H H21B 0.244019 0.731244 0.081387 0.025 Uiso calc 1 . .
H H21C 0.215056 0.634815 0.095559 0.025 Uiso calc 1 . .
C C22 0.3232(2) 0.6161(2) 0.2967(2) 0.0180(7) Uani d 1 . .
H H22A 0.273840 0.575778 0.266646 0.027 Uiso calc 1 . .
H H22B 0.343204 0.632082 0.365724 0.027 Uiso calc 1 . .
H H22C 0.369143 0.585433 0.298861 0.027 Uiso calc 1 . .
C C3 0.29514(19) 0.8399(2) 0.3681(2) 0.0121(6) Uani d 1 . .
C C31 0.2387(2) 0.8964(2) 0.3853(2) 0.0167(7) Uani d 1 . .
H H31A 0.205657 0.856415 0.398084 0.025 Uiso calc 1 . .
H H31B 0.199669 0.933141 0.325067 0.025 Uiso calc 1 . .
H H31C 0.274628 0.936049 0.443940 0.025 Uiso calc 1 . .
C C32 0.3559(2) 0.9036(2) 0.3639(2) 0.0160(7) Uani d 1 . .
H H32A 0.322466 0.947762 0.309403 0.024 Uiso calc 1 . .
H H32B 0.391368 0.868362 0.350777 0.024 Uiso calc 1 . .
H H32C 0.392649 0.935251 0.428725 0.024 Uiso calc 1 . .
C C33 0.3513(2) 0.7756(2) 0.4582(2) 0.0201(8) Uani d 1 . .
H H33A 0.381125 0.810013 0.521590 0.030 Uiso calc 1 . .
H H33B 0.393280 0.746527 0.451519 0.030 Uiso calc 1 . .
H H33C 0.315400 0.729465 0.458823 0.030 Uiso calc 1 . .
Pd Pd1 0.500000 0.86021(2) 0.250000 0.00908(7) Uani d 1 . .
Pd Pd2 0.500000 0.61741(2) 0.250000 0.01122(8) Uani d 1 . .
Br Br2 0.44677(2) 0.97324(2) 0.11858(2) 0.01413(7) Uani d 1 . .
Br Br3 0.45642(2) 0.73949(2) 0.12672(2) 0.01349(7) Uani d 1 . .
Br Br4 0.45006(2) 0.50442(2) 0.11976(3) 0.01982(8) 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
P1 0.0104(4) 0.0066(4) 0.0094(4) 0.0001(3) 0.0062(3) 0.0001(3)
Se1 0.01218(15) 0.00876(16) 0.01024(15) -0.00039(12) 0.00600(13) 0.00079(12)
Br1 0.01752(16) 0.01363(17) 0.01470(16) -0.00296(13) 0.01135(14) -0.00010(13)
C1 0.0094(14) 0.0096(16) 0.0147(16) -0.0003(12) 0.0068(13) 0.0013(12)
C11 0.0223(18) 0.0178(19) 0.0210(18) 0.0002(14) 0.0142(16) 0.0059(14)
C12 0.0120(16) 0.0117(17) 0.0179(17) -0.0019(12) 0.0077(14) -0.0014(13)
C13 0.0136(16) 0.0163(18) 0.0155(17) 0.0002(13) 0.0081(14) 0.0000(13)
C2 0.0115(15) 0.0105(16) 0.0147(16) -0.0001(12) 0.0083(13) -0.0029(12)
C21 0.0205(17) 0.0141(18) 0.0214(18) 0.0018(13) 0.0161(15) -0.0031(14)
C22 0.0181(17) 0.0145(18) 0.0221(18) 0.0049(13) 0.0123(15) 0.0060(14)
C3 0.0132(16) 0.0124(17) 0.0101(15) -0.0019(12) 0.0064(13) -0.0018(12)
C31 0.0175(17) 0.0179(19) 0.0161(17) -0.0039(13) 0.0106(15) -0.0057(13)
C32 0.0177(17) 0.0160(18) 0.0150(17) -0.0059(13) 0.0101(14) -0.0061(13)
C33 0.0200(18) 0.022(2) 0.0098(16) 0.0001(14) 0.0042(14) 0.0014(14)
Pd1 0.01055(16) 0.00756(17) 0.00919(16) 0.000 0.00583(14) 0.000
Pd2 0.01087(16) 0.00836(17) 0.01348(17) 0.000 0.00661(14) 0.000
Br2 0.01631(16) 0.01205(17) 0.01485(16) 0.00145(12) 0.00962(13) 0.00405(12)
Br3 0.01799(16) 0.01008(16) 0.01034(15) -0.00096(12) 0.00716(13) -0.00139(12)
Br4 0.02289(18) 0.01048(17) 0.01998(18) 0.00065(13) 0.00918(15) -0.00316(13)
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'
Se Se -0.0929 2.2259 '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
C2 P1 C3 . . 109.11(14) ?
C2 P1 C1 . . 113.31(14) ?
C3 P1 C1 . . 114.58(14) ?
C2 P1 Se1 . . 109.72(10) y
C3 P1 Se1 . . 109.24(10) y
C1 P1 Se1 . . 100.47(10) y
P1 Se1 Br1 . . 100.30(2) y
Se1 Br1 Br2 . . 176.810(16) y
C11 C1 C13 . . 109.4(3) ?
C11 C1 C12 . . 109.3(3) ?
C13 C1 C12 . . 108.2(2) ?
C11 C1 P1 . . 110.9(2) ?
C13 C1 P1 . . 110.1(2) ?
C12 C1 P1 . . 108.9(2) ?
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 ?
C22 C2 C21 . . 109.5(3) ?
C22 C2 P1 . . 113.9(2) ?
C21 C2 P1 . . 115.1(2) ?
C22 C2 H2 . . 105.8 ?
C21 C2 H2 . . 105.8 ?
P1 C2 H2 . . 105.8 ?
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 ?
C31 C3 C33 . . 110.1(3) ?
C31 C3 C32 . . 108.6(3) ?
C33 C3 C32 . . 106.9(3) ?
C31 C3 P1 . . 110.4(2) ?
C33 C3 P1 . . 112.5(2) ?
C32 C3 P1 . . 108.0(2) ?
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 ?
Br2 Pd1 Br2 . 2_655 92.495(19) y
Br2 Pd1 Br3 . . 90.936(11) y
Br2 Pd1 Br3 2_655 . 175.531(13) ?
Br2 Pd1 Br3 . 2_655 175.531(13) y
Br2 Pd1 Br3 2_655 2_655 90.936(11) ?
Br3 Pd1 Br3 . 2_655 85.785(18) y
Br4 Pd2 Br4 2_655 . 92.26(2) y
Br4 Pd2 Br3 2_655 2_655 91.326(11) ?
Br4 Pd2 Br3 . 2_655 176.053(14) y
Br4 Pd2 Br3 2_655 . 176.054(14) ?
Br4 Pd2 Br3 . . 91.324(11) y
Br3 Pd2 Br3 2_655 . 85.139(18) y
Pd1 Br2 Br1 . . 75.133(10) y
Pd1 Br3 Pd2 . . 94.538(13) 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
P1 C2 . 1.848(3) ?
P1 C3 . 1.870(3) ?
P1 C1 . 1.875(3) ?
P1 Se1 . 2.2505(8) y
Se1 Br1 . 2.3310(4) y
Br1 Br2 . 3.2510(5) y
C1 C11 . 1.529(4) ?
C1 C13 . 1.530(4) ?
C1 C12 . 1.532(4) ?
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 ?
C2 C22 . 1.533(4) ?
C2 C21 . 1.541(4) ?
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 C31 . 1.528(4) ?
C3 C33 . 1.540(4) ?
C3 C32 . 1.542(4) ?
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 ?
Pd1 Br2 . 2.4218(4) y
Pd1 Br2 2_655 2.4218(4) ?
Pd1 Br3 . 2.4413(4) y
Pd1 Br3 2_655 2.4413(4) ?
Pd2 Br4 2_655 2.4157(4) ?
Pd2 Br4 . 2.4157(4) y
Pd2 Br3 2_655 2.4562(4) ?
Pd2 Br3 . 2.4562(4) 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
C12 H12C Se1 . 0.98 3.12 3.640(3) 114.9 yes
C13 H13B Se1 . 0.98 2.61 3.181(3) 117.1 yes
C21 H21A Br3 . 0.98 3.14 3.822(3) 128.3 yes
C21 H21B Se1 . 0.98 2.90 3.511(3) 121.0 yes
C21 H21B Br1 . 0.98 2.80 3.574(3) 136.6 yes
C31 H31B Se1 . 0.98 3.16 3.740(3) 119.2 yes
C32 H32A Se1 . 0.98 2.97 3.526(3) 116.8 yes
C32 H32A Br1 . 0.98 2.85 3.452(3) 120.3 yes
C12 H12A Br2 3_445 0.98 2.98 3.877(3) 152.4 yes
C12 H12C Br3 7_565 0.98 3.04 4.009(3) 169.9 yes
C2 H2 Br3 2_655 1.00 3.03 3.928(3) 150.6 yes
C32 H32C Br2 6_576 0.98 2.95 3.885(3) 159.6 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 Se1 Br1 . . . . -42.39(11) ?
C3 P1 Se1 Br1 . . . . 77.19(11) ?
C1 P1 Se1 Br1 . . . . -161.98(10) ?
C2 P1 C1 C11 . . . . 80.0(2) ?
C3 P1 C1 C11 . . . . -46.1(3) ?
Se1 P1 C1 C11 . . . . -163.1(2) ?
C2 P1 C1 C13 . . . . -158.8(2) ?
C3 P1 C1 C13 . . . . 75.1(2) ?
Se1 P1 C1 C13 . . . . -41.9(2) ?
C2 P1 C1 C12 . . . . -40.3(2) ?
C3 P1 C1 C12 . . . . -166.4(2) ?
Se1 P1 C1 C12 . . . . 76.6(2) ?
C3 P1 C2 C22 . . . . 76.0(3) ?
C1 P1 C2 C22 . . . . -52.9(3) ?
Se1 P1 C2 C22 . . . . -164.30(19) ?
C3 P1 C2 C21 . . . . -156.3(2) ?
C1 P1 C2 C21 . . . . 74.7(3) ?
Se1 P1 C2 C21 . . . . -36.6(2) ?
C2 P1 C3 C31 . . . . -174.0(2) ?
C1 P1 C3 C31 . . . . -45.8(3) ?
Se1 P1 C3 C31 . . . . 66.0(2) ?
C2 P1 C3 C33 . . . . -50.5(3) ?
C1 P1 C3 C33 . . . . 77.8(3) ?
Se1 P1 C3 C33 . . . . -170.4(2) ?
C2 P1 C3 C32 . . . . 67.3(2) ?
C1 P1 C3 C32 . . . . -164.4(2) ?
Se1 P1 C3 C32 . . . . -52.6(2) ?