#------------------------------------------------------------------------------
#$Date: 2025-02-05 05:03:59 +0200 (Wed, 05 Feb 2025) $
#$Revision: 297594 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/33/2023380.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_2023380
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 '[Pd (C6 H14 O1 P1)2 (C6 H15 O1 P1)2]'
_chemical_formula_moiety 'C24 H58 O4 P4 Pd Se4'
_chemical_formula_sum 'C24 H58 O4 P4 Pd Se4'
_chemical_formula_weight 956.82
_chemical_name_systematic
;
Bis[dimethyl(sulfanylidene)phosphinito-\kSe]\
bis(hydroxydiisopropylphosphine selenide-\kSe)palladium(II)
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL2019/3
_cell_angle_alpha 90
_cell_angle_beta 92.7641(8)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.56435(6)
_cell_length_b 10.09140(9)
_cell_length_c 24.13960(19)
_cell_measurement_reflns_used 28620
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 30.8226
_cell_measurement_theta_min 2.1834
_cell_volume 1840.55(3)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.35.15 (Rigaku OD, 2012)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.35.15 (Rigaku OD, 2012)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.35.15 (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 0.996
_diffrn_measured_fraction_theta_max 0.959
_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 0.0470
_diffrn_reflns_av_unetI/netI 0.0230
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_limit_l_min -34
_diffrn_reflns_number 86102
_diffrn_reflns_theta_full 30.000
_diffrn_reflns_theta_max 30.892
_diffrn_reflns_theta_min 2.188
_exptl_absorpt_coefficient_mu 4.660
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.64953
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2012)
;
_exptl_crystal_colour 'dichroic orange yellow'
_exptl_crystal_density_diffrn 1.726
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 952
_exptl_crystal_size_max 0.10
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.469
_refine_diff_density_min -0.543
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 185
_refine_ls_number_reflns 5558
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.066
_refine_ls_R_factor_all 0.0292
_refine_ls_R_factor_gt 0.0219
_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^)+(0.0132P)^2^+1.1714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0392
_refine_ls_wR_factor_ref 0.0409
_reflns_number_gt 4939
_reflns_number_total 5558
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yz2063.cif
_cod_data_source_block 9
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2023380
_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 0.653
_shelx_estimated_absorpt_t_max 0.836
_shelx_hkl_file
;
0 0 -3 34.5177 51.0337
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0 0 -3 19.3079 61.6511
0 0 -3-27.8904 58.6431
0 0 -3 31.6682 51.7100
0 0 3 106.837 67.8992
0 0 -3 61.4148 52.8735
0 0 -3-8.34820 63.0507
0 0 -3 24.5453 55.7180
0 0 -3 85.0612 50.2478
0 0 -3 107.824 56.9191
0 0 3-3.82725 62.4006
0 0 4 242.517 96.4112
0 0 4 165.035 100.316
0 0 4 102.396 56.0847
0 0 4 248.879 80.8633
0 0 4 2.15781 88.9699
0 0 -4 160.602 97.6446
0 0 4 6.64119 110.863
0 0 -4 68.6370 76.3812
0 0 4 130.615 97.8847
0 0 -4 107.025 106.187
0 0 -4 165.955 92.5144
0 0 -4 117.402 64.6111
0 0 4 19.4848 54.8702
0 0 -4-9.82593 79.0212
0 0 4 123.190 82.9907
0 0 4 79.2270 102.385
0 0 -4 194.109 111.589
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0 0 4 109.119 75.1061
0 0 -4 230.489 102.547
0 0 -4 0.60655 80.5570
0 0 -4 395.093 121.597
0 0 -4 94.1451 93.9544
0 0 5 126.959 119.863
0 0 5-55.6326 108.006
0 0 5 57.9533 125.552
0 0 5-39.4502 110.422
0 0 -5-13.8221 113.934
0 0 -5 158.773 139.182
0 0 -5 181.415 113.499
0 0 -5 84.2284 139.864
0 0 5-29.4847 128.905
0 0 5 95.0957 119.867
0 0 5 51.0043 95.2472
0 0 5 79.9543 84.9177
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0 0 -5 127.357 130.336
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0 0 -5 64.2032 109.883
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0 0 -6 10217.5 583.904
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0 0 -7 413.385 213.450
0 0 -7 99.9460 179.003
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0 0 7-29.9594 103.094
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0 0 -7 147.801 125.333
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0 0 7 53.2482 117.907
0 0 -7 83.3478 82.1650
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0 0 -8 13364.3 710.602
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10 2 5 786.540 522.451
10 -2 5 1070.63 637.963
-10 -2 -5-121.485 459.023
-10 2 -5 388.544 451.501
-10 -2 -6 3700.58 1002.48
-10 2 -6 2378.81 841.176
10 -2 6 2067.18 717.895
10 2 6 1432.49 587.876
10 -2 6 3388.65 832.803
-10 -2 -6 1686.62 646.183
-10 -2 -6 2657.00 668.512
10 2 6 2686.14 778.407
10 -2 6 2332.77 804.079
-10 -2 -6 2090.87 705.871
-10 -2 -7 1912.78 716.587
-10 2 -7 385.817 523.005
10 -2 7 950.431 622.470
10 2 7 1049.27 589.834
10 2 7 725.668 505.796
-10 -2 -7 368.033 494.216
-10 -2 -7 2625.91 775.491
10 2 7-137.894 540.418
10 -2 7 684.041 552.010
-10 -2 -7 1105.29 575.788
-10 2 -8 6901.10 1243.42
10 -2 8 5551.05 1100.51
10 2 8 6305.75 1087.32
10 2 8 6884.38 1102.66
-10 2 -9 107.530 611.044
10 2 9 328.561 516.804
10 2 9-262.319 468.703
10 2 10 25090.5 2009.73
10 2 11 2411.47 852.299
-10 -3 12 6607.85 1132.35
-10 -3 11 1544.59 686.079
-10 -3 10 21444.8 1969.76
-10 -3 9 1894.92 778.998
-10 -3 8 3153.64 820.253
-10 -3 7 770.364 595.420
-10 -3 7 140.035 502.286
-10 -3 7 14.2865 452.314
-10 -3 7 379.546 489.413
-10 -3 6 2788.36 817.933
-10 -3 6 1826.53 712.573
-10 -3 6 348.105 483.164
-10 -3 6 2520.20 817.867
-10 -3 5 272.409 472.127
-10 -3 5 178.614 535.141
-10 -3 5-839.182 535.132
-10 -3 5 308.724 506.772
10 3 -4 1269.77 632.939
-10 -3 4 2298.17 672.802
-10 -3 4 2428.64 860.631
-10 -3 4 899.042 531.877
-10 -3 4 2191.46 688.575
10 3 -3 1014.14 504.926
-10 -3 3 1635.93 613.635
-10 -3 3 1079.50 678.975
-10 3 3 448.593 519.137
-10 -3 3 1023.04 572.736
-10 -3 3 399.668 375.269
-10 -3 2 659.938 431.837
10 -3 -2 2761.15 840.766
10 3 -2 1753.56 702.709
-10 -3 2 592.934 441.920
-10 -3 2 2167.62 753.228
-10 3 2 1616.82 658.134
-10 -3 2 1401.11 622.852
-10 -3 2 1713.77 653.644
-10 -3 1-106.091 537.409
10 -3 -1-311.836 468.617
-10 -3 1 829.687 578.168
-10 -3 1 293.851 597.585
-10 3 1 230.550 444.268
-10 -3 1 641.363 536.881
-10 -3 1 102.472 473.855
-10 -3 0 525.089 641.459
10 -3 0-184.822 396.707
-10 -3 0 1017.35 585.182
-10 3 0-273.436 565.224
-10 -3 0-666.471 622.425
-10 -3 0-621.175 554.836
-10 -3 -1 336.262 560.955
10 -3 1 192.635 480.710
10 -3 1 315.657 506.325
-10 -3 -1 490.123 505.870
-10 3 -1 189.904 465.198
-10 -3 -1 209.767 490.799
10 3 1 190.125 389.557
10 -3 1-332.715 466.363
-10 -3 -1-688.331 653.419
-10 -3 -2-249.771 553.673
10 -3 2-159.187 444.229
10 3 2 489.335 616.090
10 -3 2 99.7800 464.854
-10 -3 -2-250.213 372.773
-10 3 -2 647.558 669.656
-10 -3 -2 401.877 423.836
10 3 2 65.7002 399.327
10 -3 2 138.890 483.486
-10 -3 -2-176.950 447.251
-10 -3 -3 2234.99 650.107
10 -3 3 1641.78 643.757
10 3 3 900.805 517.139
10 -3 3 1806.82 675.471
-10 -3 -3 2497.46 629.829
-10 3 -3 2135.43 779.394
-10 -3 -3 1665.42 686.799
10 3 3 2230.39 739.223
10 -3 3 1247.44 588.702
-10 -3 -3 3056.12 745.794
-10 -3 -4 5013.78 1045.89
10 -3 4 2557.98 758.258
10 3 4 2554.62 776.139
10 -3 4 2934.95 783.539
-10 -3 -4 2379.31 701.627
-10 3 -4 4380.23 1077.83
-10 -3 -4 2365.94 651.110
10 3 4 4476.20 957.898
10 -3 4 2917.49 807.446
-10 -3 -4 2569.82 676.455
-10 -3 -5 3729.87 880.505
10 -3 5 4366.65 973.901
10 3 5 4185.12 923.969
10 -3 5 3272.87 836.023
10 3 5 4234.56 935.558
10 -3 5 4428.38 984.011
-10 3 -6 11108.3 1459.90
10 -3 6 9545.76 1360.47
10 3 6 8018.53 1226.26
10 3 6 11693.4 1492.19
10 -3 6 11279.6 1500.63
-10 3 -7 12845.8 1624.56
10 -3 7 9692.43 1370.48
10 3 7 10859.0 1417.57
-10 3 -8 3321.07 841.749
-10 3 -8 2183.35 791.498
10 3 8 1927.22 771.217
10 3 9 15624.1 1685.86
-10 -4 6 2519.99 743.391
-10 -4 6 3157.04 807.790
-10 -4 6 1421.54 612.197
-10 -4 5 935.169 587.494
-10 -4 5 378.917 545.181
-10 -4 4 9957.56 1336.62
-10 -4 4 7531.60 1201.57
-10 -4 4 11184.9 1416.21
-10 -4 4 10752.2 1386.36
-10 -4 3-500.192 576.111
-10 -4 3 589.558 550.186
-10 -4 3 906.496 592.032
-10 -4 3 43.7736 465.643
-10 -4 2 24531.1 2026.29
-10 4 2 28689.6 2244.06
-10 -4 2 23794.6 1996.83
-10 -4 2 27272.0 2128.22
-10 -4 2 25826.0 2121.16
-10 -4 1 1577.17 647.474
-10 -4 1 1270.05 622.396
-10 4 1 688.647 629.602
-10 -4 1 1409.02 648.734
-10 -4 1 2071.30 698.680
-10 -4 0 2746.41 732.397
-10 -4 0 2175.47 671.991
-10 4 0 2306.02 805.271
-10 -4 0 1724.86 623.568
-10 -4 0 2480.73 712.519
-10 -4 -1 3360.34 847.233
-10 -4 -1 2076.06 640.266
-10 4 -1 1549.18 745.460
10 4 1 2421.27 718.252
-10 -4 -1 3210.11 809.824
10 -4 1 3661.32 872.657
-10 -4 -1 1807.88 675.764
-10 -4 -2-476.180 507.763
10 -4 2 664.431 577.432
10 -4 2-443.843 438.832
-10 4 -2-3.01021 559.494
10 4 2-127.817 378.351
10 -4 2 135.505 440.649
-10 -4 -3 5782.53 1152.12
10 -4 3 4656.50 1021.60
10 -4 3 4659.90 973.321
-10 4 -3 5253.69 1053.03
10 4 3 5520.26 1043.14
10 -4 3 3862.62 877.560
10 -4 4 653.563 656.643
10 -4 4 55.8847 434.725
10 4 4 301.795 510.214
10 -4 4-256.098 450.867
-10 4 -5 8621.25 1188.58
10 -4 5 7096.54 1205.44
-10 4 -6 546.656 460.821
-10 4 -7 1265.81 609.506
-10 -5 5 5176.08 1004.05
-10 -5 5 6462.47 1113.67
-10 -5 4 57.7455 470.318
-10 -5 4 166.846 375.472
-10 -5 4 1214.21 639.331
-10 -5 3 35031.4 2446.46
-10 -5 3 35419.6 2458.47
-10 -5 3 32998.9 2354.09
-10 -5 3 38091.4 2616.54
-10 -5 2 1662.12 774.825
-10 5 0 219.063 601.530
-10 5 -1 2605.29 907.254
10 5 1 4517.66 940.711
-10 5 -2 1478.11 733.751
10 5 2 1906.25 695.630
10 -5 2 1282.26 648.919
-10 5 -3-215.258 452.215
10 -5 3 204.649 569.199
-10 5 -4 528.813 457.662
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 7723
_shelx_res_file
;
TITL Millie in P2(1)/n
shelx.res
created by SHELXL-2019/3 at 10:56:00 on 30-Sep-2024
CELL 0.71073 7.564349 10.091398 24.139595 90.0000 92.7641 90.0000
ZERR 2.00 0.000060 0.000085 0.000192 0.0000 0.0008 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H P Se Pd O
UNIT 48.00 116.00 8.00 8.00 2.00 8.00
L.S. 6
BOND $H
FMAP 2
PLAN 10
SIZE 0.1 0.08 0.04
TEMP -173
ACTA 60
CONF 2.5
DFIX 0.8 0.02 O2 H02 O1 H01
REM Instructions for potential hydrogen bonds
HTAB O1 O2
HTAB O2 O1
HTAB C11 Se1
EQIV $2 x-1, y, z
HTAB C21 O2_$2
EQIV $3 x+1, y, z
HTAB C32 Se2_$3
HTAB C41 Se2
EQIV $4 x, y+1, z
HTAB C42 Se1_$4
WGHT 0.013200 1.171400
FVAR 2.19018
PD1 5 0.500000 0.500000 0.000000 10.50000 0.01300 0.01194 =
0.00948 0.00009 -0.00123 -0.00030
SE1 4 0.570001 0.388612 0.089218 11.00000 0.01935 0.01597 =
0.01067 0.00170 0.00021 0.00335
SE2 4 0.415800 0.717441 0.037201 11.00000 0.01356 0.01384 =
0.01338 -0.00140 -0.00162 0.00039
P1 3 0.437978 0.475239 0.159383 11.00000 0.01670 0.01496 =
0.01200 0.00122 0.00040 0.00073
P2 3 0.657062 0.799396 0.077273 11.00000 0.01415 0.01285 =
0.01223 -0.00012 -0.00065 -0.00036
O1 6 0.495251 0.614133 0.178829 11.00000 0.03185 0.01812 =
0.01548 -0.00097 0.00569 -0.00430
H01 2 0.569214 0.652805 0.164031 10.50000 0.01219
O2 6 0.721568 0.730094 0.130814 11.00000 0.01923 0.01592 =
0.01637 0.00318 -0.00349 -0.00121
H02 2 0.651058 0.686486 0.144550 10.50000 0.02574
C1 1 0.489768 0.364460 0.217773 11.00000 0.02226 0.01983 =
0.01342 0.00349 0.00179 0.00029
AFIX 13
H1 2 0.444759 0.273758 0.208155 11.00000 -1.20000
AFIX 0
C2 1 0.199770 0.476688 0.142746 11.00000 0.01844 0.02960 =
0.02164 -0.00010 -0.00115 0.00587
AFIX 13
H2 2 0.184451 0.507699 0.103463 11.00000 -1.20000
AFIX 0
C3 1 0.844349 0.801810 0.032615 11.00000 0.01443 0.02219 =
0.01827 -0.00245 -0.00034 -0.00258
AFIX 13
H3 2 0.944534 0.845492 0.054113 11.00000 -1.20000
AFIX 0
C4 1 0.601134 0.970347 0.093516 11.00000 0.02095 0.01267 =
0.01568 0.00056 0.00017 0.00058
AFIX 13
H4 2 0.560610 1.016268 0.058455 11.00000 -1.20000
AFIX 0
C11 1 0.690195 0.357394 0.229364 11.00000 0.02566 0.04154 =
0.01546 0.00584 -0.00168 0.00673
AFIX 137
H11A 2 0.736533 0.446633 0.236850 11.00000 -1.50000
H11B 2 0.746032 0.320366 0.196994 11.00000 -1.50000
H11C 2 0.716396 0.300656 0.261670 11.00000 -1.50000
AFIX 0
C12 1 0.397809 0.413969 0.269236 11.00000 0.02820 0.03243 =
0.01494 0.00301 0.00483 -0.00116
AFIX 137
H12A 2 0.444268 0.365769 0.302042 11.00000 -1.50000
H12B 2 0.270059 0.398763 0.264315 11.00000 -1.50000
H12C 2 0.420437 0.508956 0.274180 11.00000 -1.50000
AFIX 0
C21 1 0.100762 0.575894 0.177524 11.00000 0.02832 0.04008 =
0.05255 -0.01021 0.00135 0.01603
AFIX 137
H21A 2 -0.020928 0.585362 0.162203 11.00000 -1.50000
H21B 2 0.160572 0.661983 0.176856 11.00000 -1.50000
H21C 2 0.099058 0.544047 0.215846 11.00000 -1.50000
AFIX 0
C22 1 0.119360 0.338297 0.144095 11.00000 0.01853 0.03868 =
0.02897 -0.00673 0.00223 -0.00513
AFIX 137
H22A 2 0.116893 0.307857 0.182601 11.00000 -1.50000
H22B 2 0.191026 0.277268 0.122951 11.00000 -1.50000
H22C 2 -0.001539 0.340790 0.127601 11.00000 -1.50000
AFIX 0
C31 1 0.806207 0.885566 -0.019327 11.00000 0.02491 0.02505 =
0.02027 0.00106 0.00582 -0.00378
AFIX 137
H31A 2 0.911658 0.888141 -0.041347 11.00000 -1.50000
H31B 2 0.774974 0.975846 -0.008477 11.00000 -1.50000
H31C 2 0.707527 0.846427 -0.041469 11.00000 -1.50000
AFIX 0
C32 1 0.906219 0.661916 0.018418 11.00000 0.01529 0.02649 =
0.02548 -0.00608 0.00050 0.00273
AFIX 137
H32A 2 0.817095 0.619247 -0.006420 11.00000 -1.50000
H32B 2 0.922430 0.609846 0.052553 11.00000 -1.50000
H32C 2 1.018726 0.667126 0.000034 11.00000 -1.50000
AFIX 0
C41 1 0.451414 0.973683 0.133726 11.00000 0.02704 0.02121 =
0.02148 -0.00357 0.00553 0.00322
AFIX 137
H41A 2 0.488956 0.927620 0.168046 11.00000 -1.50000
H41B 2 0.346770 0.929646 0.116767 11.00000 -1.50000
H41C 2 0.422435 1.065926 0.142169 11.00000 -1.50000
AFIX 0
C42 1 0.764062 1.043028 0.118689 11.00000 0.02778 0.01636 =
0.02987 -0.00421 -0.00303 -0.00405
AFIX 137
H42A 2 0.731021 1.133533 0.128663 11.00000 -1.50000
H42B 2 0.856172 1.046052 0.091527 11.00000 -1.50000
H42C 2 0.809062 0.995924 0.151958 11.00000 -1.50000
AFIX 0
HKLF 4
REM Millie in P2(1)/n
REM wR2 = 0.0409, GooF = S = 1.066, Restrained GooF = 1.066 for all data
REM R1 = 0.0219 for 4939 Fo > 4sig(Fo) and 0.0292 for all 5558 data
REM 185 parameters refined using 2 restraints
END
WGHT 0.0132 1.1714
REM Highest difference peak 0.469, deepest hole -0.543, 1-sigma level 0.092
Q1 1 0.4754 0.4418 0.1191 11.00000 0.05 0.47
Q2 1 0.6906 0.7641 0.1008 11.00000 0.05 0.45
Q3 1 0.3792 0.7609 0.0089 11.00000 0.05 0.45
Q4 1 0.4566 0.7463 0.0716 11.00000 0.05 0.45
Q5 1 0.8729 0.7204 0.0354 11.00000 0.05 0.44
Q6 1 0.8145 0.8472 0.0053 11.00000 0.05 0.44
Q7 1 0.7429 0.8093 0.0547 11.00000 0.05 0.43
Q8 1 0.6378 0.4629 0.0787 11.00000 0.05 0.43
Q9 1 0.3640 0.6891 0.0710 11.00000 0.05 0.42
Q10 1 0.5062 0.9510 0.1044 11.00000 0.05 0.41
;
_shelx_res_checksum 86566
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Pd Pd1 0.500000 0.500000 0.000000 0.01153(4) Uani d 1 . .
Se Se1 0.57000(2) 0.38861(2) 0.08922(2) 0.01535(4) Uani d 1 . .
Se Se2 0.41580(2) 0.71744(2) 0.03720(2) 0.01366(4) Uani d 1 . .
P P1 0.43798(6) 0.47524(4) 0.15938(2) 0.01456(8) Uani d 1 . .
P P2 0.65706(5) 0.79940(4) 0.07727(2) 0.01312(8) Uani d 1 . .
O O1 0.49525(18) 0.61413(12) 0.17883(5) 0.0217(3) Uani d 1 . .
H H01 0.569(4) 0.653(3) 0.1640(15) 0.012(10) Uiso d 0.5 . .
O O2 0.72157(16) 0.73009(12) 0.13081(5) 0.0173(2) Uani d 1 . .
H H02 0.651(5) 0.686(4) 0.1445(17) 0.026(12) Uiso d 0.5 . .
C C1 0.4898(2) 0.36446(17) 0.21777(7) 0.0185(3) Uani d 1 . .
H H1 0.444759 0.273758 0.208155 0.022 Uiso calc 1 . .
C C2 0.1998(2) 0.47669(19) 0.14275(8) 0.0233(4) Uani d 1 . .
H H2 0.184451 0.507699 0.103463 0.028 Uiso calc 1 . .
C C3 0.8443(2) 0.80181(17) 0.03261(7) 0.0183(3) Uani d 1 . .
H H3 0.944534 0.845492 0.054113 0.022 Uiso calc 1 . .
C C4 0.6011(2) 0.97035(16) 0.09352(7) 0.0165(3) Uani d 1 . .
H H4 0.560610 1.016268 0.058455 0.020 Uiso calc 1 . .
C C11 0.6902(2) 0.3574(2) 0.22936(8) 0.0276(4) Uani d 1 . .
H H11A 0.736533 0.446633 0.236850 0.041 Uiso calc 1 . .
H H11B 0.746032 0.320366 0.196994 0.041 Uiso calc 1 . .
H H11C 0.716396 0.300656 0.261670 0.041 Uiso calc 1 . .
C C12 0.3978(3) 0.4140(2) 0.26924(7) 0.0251(4) Uani d 1 . .
H H12A 0.444268 0.365769 0.302042 0.038 Uiso calc 1 . .
H H12B 0.270059 0.398763 0.264315 0.038 Uiso calc 1 . .
H H12C 0.420437 0.508956 0.274180 0.038 Uiso calc 1 . .
C C21 0.1008(3) 0.5759(2) 0.17752(10) 0.0403(5) Uani d 1 . .
H H21A -0.020928 0.585362 0.162203 0.061 Uiso calc 1 . .
H H21B 0.160572 0.661983 0.176856 0.061 Uiso calc 1 . .
H H21C 0.099058 0.544047 0.215846 0.061 Uiso calc 1 . .
C C22 0.1194(2) 0.3383(2) 0.14410(8) 0.0287(4) Uani d 1 . .
H H22A 0.116893 0.307857 0.182601 0.043 Uiso calc 1 . .
H H22B 0.191026 0.277268 0.122951 0.043 Uiso calc 1 . .
H H22C -0.001539 0.340790 0.127601 0.043 Uiso calc 1 . .
C C31 0.8062(2) 0.88557(19) -0.01933(7) 0.0233(4) Uani d 1 . .
H H31A 0.911658 0.888141 -0.041347 0.035 Uiso calc 1 . .
H H31B 0.774974 0.975846 -0.008477 0.035 Uiso calc 1 . .
H H31C 0.707527 0.846427 -0.041469 0.035 Uiso calc 1 . .
C C32 0.9062(2) 0.66192(19) 0.01842(8) 0.0224(4) Uani d 1 . .
H H32A 0.817095 0.619247 -0.006420 0.034 Uiso calc 1 . .
H H32B 0.922430 0.609846 0.052553 0.034 Uiso calc 1 . .
H H32C 1.018726 0.667126 0.000034 0.034 Uiso calc 1 . .
C C41 0.4514(2) 0.97368(18) 0.13373(8) 0.0231(4) Uani d 1 . .
H H41A 0.488956 0.927620 0.168046 0.035 Uiso calc 1 . .
H H41B 0.346770 0.929646 0.116767 0.035 Uiso calc 1 . .
H H41C 0.422435 1.065926 0.142169 0.035 Uiso calc 1 . .
C C42 0.7641(2) 1.04303(18) 0.11869(8) 0.0248(4) Uani d 1 . .
H H42A 0.731021 1.133533 0.128663 0.037 Uiso calc 1 . .
H H42B 0.856172 1.046052 0.091527 0.037 Uiso calc 1 . .
H H42C 0.809062 0.995924 0.151958 0.037 Uiso calc 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
Pd1 0.01300(8) 0.01194(8) 0.00948(8) -0.00030(6) -0.00123(6) 0.00009(6)
Se1 0.01935(8) 0.01597(8) 0.01067(8) 0.00335(6) 0.00021(6) 0.00170(6)
Se2 0.01356(7) 0.01384(8) 0.01338(8) 0.00039(6) -0.00162(6) -0.00140(6)
P1 0.01670(19) 0.0150(2) 0.01200(19) 0.00073(16) 0.00040(15) 0.00122(16)
P2 0.01415(19) 0.01285(19) 0.01223(19) -0.00036(15) -0.00065(15) -0.00012(15)
O1 0.0318(7) 0.0181(6) 0.0155(6) -0.0043(5) 0.0057(5) -0.0010(5)
O2 0.0192(6) 0.0159(6) 0.0164(6) -0.0012(5) -0.0035(5) 0.0032(5)
C1 0.0223(8) 0.0198(8) 0.0134(8) 0.0003(7) 0.0018(6) 0.0035(6)
C2 0.0184(8) 0.0296(10) 0.0216(9) 0.0059(7) -0.0011(7) -0.0001(8)
C3 0.0144(7) 0.0222(9) 0.0183(8) -0.0026(6) -0.0003(6) -0.0024(7)
C4 0.0209(8) 0.0127(8) 0.0157(8) 0.0006(6) 0.0002(6) 0.0006(6)
C11 0.0257(9) 0.0415(12) 0.0155(9) 0.0067(8) -0.0017(7) 0.0058(8)
C12 0.0282(9) 0.0324(11) 0.0149(8) -0.0012(8) 0.0048(7) 0.0030(8)
C21 0.0283(11) 0.0401(13) 0.0526(14) 0.0160(10) 0.0014(10) -0.0102(11)
C22 0.0185(9) 0.0387(11) 0.0290(10) -0.0051(8) 0.0022(7) -0.0067(9)
C31 0.0249(9) 0.0251(9) 0.0203(9) -0.0038(7) 0.0058(7) 0.0011(7)
C32 0.0153(8) 0.0265(9) 0.0255(9) 0.0027(7) 0.0005(7) -0.0061(8)
C41 0.0270(9) 0.0212(9) 0.0215(9) 0.0032(7) 0.0055(7) -0.0036(7)
C42 0.0278(9) 0.0164(9) 0.0299(10) -0.0041(7) -0.0030(8) -0.0042(7)
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
Se1 Pd1 Se1 . 3_665 180.0 y
Se1 Pd1 Se2 . 3_665 82.184(5) y
Se1 Pd1 Se2 3_665 3_665 97.816(5) ?
Se1 Pd1 Se2 . . 97.817(5) y
Se1 Pd1 Se2 3_665 . 82.183(5) ?
Se2 Pd1 Se2 3_665 . 180.0 y
P1 Se1 Pd1 . . 114.028(13) y
P2 Se2 Pd1 . . 105.840(13) y
O1 P1 C1 . . 106.03(8) ?
O1 P1 C2 . . 108.72(8) ?
C1 P1 C2 . . 110.31(8) ?
O1 P1 Se1 . . 117.97(5) ?
C1 P1 Se1 . . 105.29(6) ?
C2 P1 Se1 . . 108.36(6) ?
O2 P2 C3 . . 106.31(7) ?
O2 P2 C4 . . 108.60(7) ?
C3 P2 C4 . . 108.05(8) ?
O2 P2 Se2 . . 115.25(5) ?
C3 P2 Se2 . . 113.56(6) ?
C4 P2 Se2 . . 104.81(6) ?
P1 O1 H01 . . 121(3) ?
P2 O2 H02 . . 115(3) ?
C11 C1 C12 . . 110.52(15) ?
C11 C1 P1 . . 110.08(12) ?
C12 C1 P1 . . 109.65(12) ?
C11 C1 H1 . . 108.8 ?
C12 C1 H1 . . 108.8 ?
P1 C1 H1 . . 108.8 ?
C22 C2 C21 . . 112.48(17) ?
C22 C2 P1 . . 112.23(13) ?
C21 C2 P1 . . 112.91(14) ?
C22 C2 H2 . . 106.2 ?
C21 C2 H2 . . 106.2 ?
P1 C2 H2 . . 106.2 ?
C31 C3 C32 . . 111.96(15) ?
C31 C3 P2 . . 111.82(12) ?
C32 C3 P2 . . 112.02(12) ?
C31 C3 H3 . . 106.9 ?
C32 C3 H3 . . 106.9 ?
P2 C3 H3 . . 106.9 ?
C41 C4 C42 . . 110.11(15) ?
C41 C4 P2 . . 110.15(12) ?
C42 C4 P2 . . 110.32(12) ?
C41 C4 H4 . . 108.7 ?
C42 C4 H4 . . 108.7 ?
P2 C4 H4 . . 108.7 ?
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 ?
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 ?
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 ?
C4 C41 H41A . . 109.5 ?
C4 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
C4 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
C4 C42 H42A . . 109.5 ?
C4 C42 H42B . . 109.5 ?
H42A C42 H42B . . 109.5 ?
C4 C42 H42C . . 109.5 ?
H42A C42 H42C . . 109.5 ?
H42B C42 H42C . . 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
Pd1 Se1 . 2.46419(16) y
Pd1 Se1 3_665 2.46419(16) ?
Pd1 Se2 3_665 2.46617(16) ?
Pd1 Se2 . 2.46620(16) y
Se1 P1 . 2.1894(5) y
Se2 P2 . 2.1863(4) y
P1 O1 . 1.5340(13) y
P1 C1 . 1.8267(17) ?
P1 C2 . 1.8272(18) ?
P2 O2 . 1.5287(12) y
P2 C3 . 1.8213(17) ?
P2 C4 . 1.8234(17) ?
O1 H01 . 0.782(18) ?
O2 H02 . 0.778(19) ?
C1 C11 . 1.530(2) ?
C1 C12 . 1.536(2) ?
C1 H1 . 1.0000 ?
C2 C22 . 1.524(3) ?
C2 C21 . 1.526(3) ?
C2 H2 . 1.0000 ?
C3 C31 . 1.528(2) ?
C3 C32 . 1.531(2) ?
C3 H3 . 1.0000 ?
C4 C41 . 1.527(2) ?
C4 C42 . 1.534(2) ?
C4 H4 . 1.0000 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 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 ?
C31 H31A . 0.9800 ?
C31 H31B . 0.9800 ?
C31 H31C . 0.9800 ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
C32 H32C . 0.9800 ?
C41 H41A . 0.9800 ?
C41 H41B . 0.9800 ?
C41 H41C . 0.9800 ?
C42 H42A . 0.9800 ?
C42 H42B . 0.9800 ?
C42 H42C . 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
O1 H01 O2 . 0.782(18) 1.634(19) 2.4156(17) 178(4) yes
O2 H02 O1 . 0.778(19) 1.64(2) 2.4156(17) 172(5) yes
C11 H11B Se1 . 0.98 2.95 3.4748(18) 114.9 yes
C21 H21A O2 1_455 0.98 2.52 3.407(2) 150.2 yes
C32 H32C Se2 1_655 0.98 3.13 3.8999(17) 136.1 yes
C41 H41B Se2 . 0.98 2.94 3.4825(18) 116.0 yes
C42 H42A Se1 1_565 0.98 2.98 3.8370(19) 146.2 yes
C32 H32A Pd1 . 0.98 2.69 3.4897(18) 138.5 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
Se2 Pd1 Se1 P1 3_665 . . . -156.179(15) ?
Se2 Pd1 Se1 P1 . . . . 23.820(15) ?
Se1 Pd1 Se2 P2 . . . . 65.789(13) ?
Se1 Pd1 Se2 P2 3_665 . . . -114.210(13) ?
Pd1 Se1 P1 O1 . . . . -68.57(6) ?
Pd1 Se1 P1 C1 . . . . 173.44(6) ?
Pd1 Se1 P1 C2 . . . . 55.41(7) ?
Pd1 Se2 P2 O2 . . . . -70.31(6) ?
Pd1 Se2 P2 C3 . . . . 52.68(6) ?
Pd1 Se2 P2 C4 . . . . 170.38(6) ?
O1 P1 C1 C11 . . . . -65.74(14) ?
C2 P1 C1 C11 . . . . 176.72(13) ?
Se1 P1 C1 C11 . . . . 60.02(13) ?
O1 P1 C1 C12 . . . . 56.06(14) ?
C2 P1 C1 C12 . . . . -61.48(15) ?
Se1 P1 C1 C12 . . . . -178.17(11) ?
O1 P1 C2 C22 . . . . -158.62(13) ?
C1 P1 C2 C22 . . . . -42.75(16) ?
Se1 P1 C2 C22 . . . . 72.03(14) ?
O1 P1 C2 C21 . . . . -30.21(17) ?
C1 P1 C2 C21 . . . . 85.66(17) ?
Se1 P1 C2 C21 . . . . -159.57(14) ?
O2 P2 C3 C31 . . . . -172.02(12) ?
C4 P2 C3 C31 . . . . -55.61(14) ?
Se2 P2 C3 C31 . . . . 60.20(13) ?
O2 P2 C3 C32 . . . . 61.36(13) ?
C4 P2 C3 C32 . . . . 177.78(12) ?
Se2 P2 C3 C32 . . . . -66.41(13) ?
O2 P2 C4 C41 . . . . -61.77(13) ?
C3 P2 C4 C41 . . . . -176.69(12) ?
Se2 P2 C4 C41 . . . . 61.91(12) ?
O2 P2 C4 C42 . . . . 60.00(14) ?
C3 P2 C4 C42 . . . . -54.92(14) ?
Se2 P2 C4 C42 . . . . -176.32(11) ?