#------------------------------------------------------------------------------
#$Date: 2019-11-24 09:25:28 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237455 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/83/4088315.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4088315
loop_
_publ_author_name
'Hirasawa, Kengo'
'Tanaka, Shinya'
'Horiuchi, Takeru'
'Kobayashi, Takahiro'
'Sato, Takumi'
'Morohashi, Naoya'
'Hattori, Tetsutaro'
_publ_section_title
;
 Pd(II) Complexes Ligated by 1,3-Bis(diphenylphosphino)calix[4]arene:
 Preparation, X-ray Structures, and Catalyses
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              420
_journal_paper_doi               10.1021/acs.organomet.5b00999
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C73.5 H90 Cl5 O5 P2 Pd'
_chemical_formula_weight         1399.05
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.204(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.897(2)
_cell_length_b                   30.808(6)
_cell_length_c                   19.968(4)
_cell_measurement_reflns_used    5483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.17
_cell_volume                     7299(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40646
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6893
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.530
_refine_diff_density_min         -2.036
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         16389
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0637P)²+66.6791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.2232
_reflns_number_gt                10244
_reflns_number_total             16389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00999_si_006.cif
_cod_data_source_block           complex12
_cod_original_cell_volume        7299(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C73.50 H90 Cl5 O5 P2 Pd'
_cod_database_code               4088315
loop_
_symmetry_equiv_pos_as_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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7591(5) 0.2935(2) -0.1712(3) 0.0143(13) Uani 1 1 d . . .
H1 H 0.7496 0.2625 -0.1658 0.017 Uiso 1 1 calc R . .
H2 H 0.7382 0.3007 -0.2177 0.017 Uiso 1 1 calc R . .
C2 C 0.9582(5) 0.28263(19) -0.1079(3) 0.0126(12) Uani 1 1 d . . .
C3 C 1.0569(5) 0.3040(2) -0.0808(3) 0.0137(13) Uani 1 1 d . . .
C4 C 1.0899(5) 0.3420(2) -0.1119(3) 0.0163(13) Uani 1 1 d . . .
H3 H 1.1581 0.3547 -0.0969 0.020 Uiso 1 1 calc R . .
C5 C 1.0263(6) 0.3616(2) -0.1638(3) 0.0164(13) Uani 1 1 d . A .
C6 C 0.9218(5) 0.3432(2) -0.1825(3) 0.0158(13) Uani 1 1 d . . .
H4 H 0.8753 0.3570 -0.2153 0.019 Uiso 1 1 calc R . .
C7 C 0.8835(5) 0.3053(2) -0.1547(3) 0.0133(13) Uani 1 1 d . . .
C8 C 1.0660(6) 0.4024(2) -0.1998(3) 0.0197(14) Uani 1 1 d D . .
C9 C 1.1739(8) 0.4219(3) -0.1621(5) 0.052(3) Uani 1 1 d . A .
H5 H 1.2339 0.4010 -0.1614 0.077 Uiso 1 1 calc R . .
H6 H 1.1584 0.4289 -0.1168 0.077 Uiso 1 1 calc R . .
H7 H 1.1959 0.4477 -0.1847 0.077 Uiso 1 1 calc R . .
C10 C 1.0992(9) 0.3909(3) -0.2680(4) 0.048(3) Uani 1 1 d . A 1
H8 H 1.0353 0.3791 -0.2940 0.072 Uiso 1 1 calc R . .
H9 H 1.1585 0.3697 -0.2642 0.072 Uiso 1 1 calc R . .
H10 H 1.1251 0.4165 -0.2897 0.072 Uiso 1 1 calc R . .
C11 C 1.1253(5) 0.2905(2) -0.0159(3) 0.0166(13) Uani 1 1 d . . .
H11 H 1.1139 0.2598 -0.0079 0.020 Uiso 1 1 calc R . .
H12 H 1.2049 0.2951 -0.0211 0.020 Uiso 1 1 calc R . .
C12 C 1.0366(5) 0.2963(2) 0.0962(3) 0.0154(13) Uani 1 1 d . . .
C13 C 0.9807(5) 0.3211(2) 0.1431(3) 0.0141(13) Uani 1 1 d . . .
C14 C 0.9936(5) 0.3657(2) 0.1421(3) 0.0149(13) Uani 1 1 d . . .
H13 H 0.9580 0.3823 0.1732 0.018 Uiso 1 1 calc R . .
C15 C 1.0582(5) 0.3869(2) 0.0961(3) 0.0162(13) Uani 1 1 d . . .
C16 C 1.1047(5) 0.3612(2) 0.0466(3) 0.0162(13) Uani 1 1 d . . .
H14 H 1.1457 0.3745 0.0145 0.019 Uiso 1 1 calc R . .
C17 C 1.0907(5) 0.3165(2) 0.0447(3) 0.0154(13) Uani 1 1 d . . .
C18 C 1.0716(6) 0.4362(2) 0.0988(3) 0.0203(14) Uani 1 1 d . . .
C19 C 0.9559(7) 0.4574(2) 0.0855(6) 0.047(3) Uani 1 1 d . . .
H15 H 0.9235 0.4488 0.0421 0.071 Uiso 1 1 calc R . .
H16 H 0.9640 0.4884 0.0868 0.071 Uiso 1 1 calc R . .
H17 H 0.9075 0.4484 0.1193 0.071 Uiso 1 1 calc R . .
C20 C 1.1217(7) 0.4497(2) 0.1691(4) 0.0314(18) Uani 1 1 d . . .
H18 H 1.0711 0.4412 0.2021 0.047 Uiso 1 1 calc R . .
H19 H 1.1321 0.4806 0.1705 0.047 Uiso 1 1 calc R . .
H20 H 1.1931 0.4355 0.1785 0.047 Uiso 1 1 calc R . .
C21 C 1.1526(8) 0.4530(2) 0.0478(4) 0.039(2) Uani 1 1 d . . .
H21 H 1.2259 0.4406 0.0576 0.058 Uiso 1 1 calc R . .
H22 H 1.1577 0.4841 0.0508 0.058 Uiso 1 1 calc R . .
H23 H 1.1246 0.4449 0.0032 0.058 Uiso 1 1 calc R . .
C22 C 0.9027(5) 0.2998(2) 0.1909(3) 0.0166(13) Uani 1 1 d . . .
H24 H 0.9235 0.3094 0.2364 0.020 Uiso 1 1 calc R . .
H25 H 0.9119 0.2686 0.1894 0.020 Uiso 1 1 calc R . .
C23 C 0.7034(5) 0.28735(19) 0.1276(3) 0.0124(12) Uani 1 1 d . . .
C24 C 0.6056(5) 0.30802(19) 0.0986(3) 0.0135(13) Uani 1 1 d . . .
C25 C 0.5732(5) 0.34715(19) 0.1266(3) 0.0158(13) Uani 1 1 d . . .
H26 H 0.5057 0.3597 0.1100 0.019 Uiso 1 1 calc R . .
H27 H 0.5057 0.3597 0.1100 0.019 Uiso 1 1 d R . .
C26 C 0.6354(6) 0.36822(19) 0.1774(3) 0.0164(13) Uani 1 1 d . . .
C27 C 0.7409(5) 0.3503(2) 0.1975(3) 0.0164(13) Uani 1 1 d . . .
H90 H 0.7878 0.3651 0.2291 0.020 Uiso 1 1 calc R . .
C28 C 0.7779(5) 0.3115(2) 0.1721(3) 0.0135(12) Uani 1 1 d . . .
C29 C 0.5965(6) 0.4108(2) 0.2095(4) 0.0227(15) Uani 1 1 d . . .
C30 C 0.4810(6) 0.4257(2) 0.1797(4) 0.0264(16) Uani 1 1 d . . .
H28 H 0.4841 0.4307 0.1324 0.040 Uiso 1 1 calc R . .
H29 H 0.4601 0.4520 0.2012 0.040 Uiso 1 1 calc R . .
H30 H 0.4261 0.4036 0.1867 0.040 Uiso 1 1 calc R . .
C31 C 0.5867(8) 0.4027(3) 0.2849(4) 0.039(2) Uani 1 1 d . . .
H31 H 0.5637 0.4289 0.3059 0.059 Uiso 1 1 calc R . .
H32 H 0.6584 0.3936 0.3053 0.059 Uiso 1 1 calc R . .
H33 H 0.5318 0.3804 0.2906 0.059 Uiso 1 1 calc R . .
C32 C 0.6822(7) 0.4471(2) 0.1999(4) 0.0323(18) Uani 1 1 d . . .
H34 H 0.6883 0.4519 0.1528 0.048 Uiso 1 1 calc R . .
H35 H 0.7544 0.4388 0.2206 0.048 Uiso 1 1 calc R . .
H36 H 0.6575 0.4733 0.2203 0.048 Uiso 1 1 calc R . .
C33 C 0.5358(5) 0.2928(2) 0.0350(3) 0.0158(13) Uani 1 1 d . . .
H37 H 0.5461 0.2618 0.0293 0.019 Uiso 1 1 calc R . .
H38 H 0.4566 0.2981 0.0402 0.019 Uiso 1 1 calc R . .
C34 C 0.6244(5) 0.29480(19) -0.0776(3) 0.0138(13) Uani 1 1 d . . .
C35 C 0.6804(5) 0.3174(2) -0.1260(3) 0.0143(13) Uani 1 1 d . . .
C36 C 0.6706(5) 0.3622(2) -0.1283(3) 0.0145(13) Uani 1 1 d . . .
H39 H 0.7069 0.3777 -0.1604 0.017 Uiso 1 1 calc R . .
C37 C 0.6070(5) 0.38485(19) -0.0832(3) 0.0136(13) Uani 1 1 d . . .
C38 C 0.5601(5) 0.3616(2) -0.0327(3) 0.0140(13) Uani 1 1 d . . .
H40 H 0.5205 0.3764 -0.0015 0.017 Uiso 1 1 calc R . .
C39 C 0.5703(5) 0.3164(2) -0.0273(3) 0.0132(12) Uani 1 1 d . . .
C40 C 0.5915(6) 0.4346(2) -0.0865(3) 0.0179(14) Uani 1 1 d . . .
C41 C 0.6587(7) 0.4554(2) -0.1407(4) 0.0281(17) Uani 1 1 d . . .
H41 H 0.7367 0.4477 -0.1332 0.042 Uiso 1 1 calc R . .
H42 H 0.6510 0.4864 -0.1389 0.042 Uiso 1 1 calc R . .
H43 H 0.6302 0.4451 -0.1841 0.042 Uiso 1 1 calc R . .
C42 C 0.4671(6) 0.4451(2) -0.1027(4) 0.0308(18) Uani 1 1 d . . .
H44 H 0.4425 0.4329 -0.1455 0.046 Uiso 1 1 calc R . .
H45 H 0.4571 0.4760 -0.1041 0.046 Uiso 1 1 calc R . .
H46 H 0.4235 0.4330 -0.0687 0.046 Uiso 1 1 calc R . .
C43 C 0.6311(7) 0.4548(2) -0.0179(4) 0.0321(18) Uani 1 1 d . . .
H47 H 0.5840 0.4446 0.0158 0.048 Uiso 1 1 calc R . .
H48 H 0.6262 0.4859 -0.0209 0.048 Uiso 1 1 calc R . .
H49 H 0.7078 0.4465 -0.0061 0.048 Uiso 1 1 calc R . .
P1 P 0.73135(13) 0.23008(5) 0.10704(8) 0.0110(3) Uani 1 1 d . . .
C44 C 0.7977(5) 0.2066(2) 0.1845(3) 0.0145(13) Uani 1 1 d . . .
C45 C 0.8871(5) 0.1776(2) 0.1818(3) 0.0174(13) Uani 1 1 d . . .
H50 H 0.9135 0.1701 0.1407 0.021 Uiso 1 1 calc R . .
C46 C 0.9372(6) 0.1598(2) 0.2417(4) 0.0245(16) Uani 1 1 d . . .
H51 H 0.9961 0.1401 0.2400 0.029 Uiso 1 1 calc R . .
C47 C 0.8996(6) 0.1713(2) 0.3028(3) 0.0190(14) Uani 1 1 d . . .
H52 H 0.9340 0.1598 0.3422 0.023 Uiso 1 1 calc R . .
C48 C 0.8108(5) 0.2001(2) 0.3057(3) 0.0176(14) Uani 1 1 d . . .
H53 H 0.7853 0.2078 0.3470 0.021 Uiso 1 1 calc R . .
C49 C 0.7594(5) 0.2176(2) 0.2467(3) 0.0165(13) Uani 1 1 d . . .
H54 H 0.6993 0.2367 0.2488 0.020 Uiso 1 1 calc R . .
C50 C 0.5919(5) 0.2041(2) 0.1060(3) 0.0149(13) Uani 1 1 d . . .
C51 C 0.5647(5) 0.1702(2) 0.0620(3) 0.0184(14) Uani 1 1 d . . .
H55 H 0.6163 0.1608 0.0324 0.022 Uiso 1 1 calc R . .
C52 C 0.4603(6) 0.1504(2) 0.0627(4) 0.0268(17) Uani 1 1 d . . .
H56 H 0.4423 0.1276 0.0332 0.032 Uiso 1 1 calc R . .
C53 C 0.3829(6) 0.1638(2) 0.1058(4) 0.0269(17) Uani 1 1 d . . .
H57 H 0.3129 0.1504 0.1052 0.032 Uiso 1 1 calc R . .
C54 C 0.4091(6) 0.1974(2) 0.1503(3) 0.0204(14) Uani 1 1 d . . .
H58 H 0.3568 0.2065 0.1798 0.025 Uiso 1 1 calc R . .
C55 C 0.5137(5) 0.2176(2) 0.1509(3) 0.0160(13) Uani 1 1 d . . .
H59 H 0.5318 0.2400 0.1810 0.019 Uiso 1 1 calc R . .
P2 P 0.93061(13) 0.22612(5) -0.08352(8) 0.0115(3) Uani 1 1 d . . .
C56 C 1.0688(5) 0.1995(2) -0.0816(3) 0.0144(13) Uani 1 1 d . . .
C57 C 1.0938(6) 0.1654(2) -0.0380(4) 0.0208(14) Uani 1 1 d . . .
H60 H 1.0428 0.1573 -0.0071 0.025 Uiso 1 1 calc R . .
C58 C 1.1955(6) 0.1430(2) -0.0404(4) 0.0240(16) Uani 1 1 d . . .
H61 H 1.2113 0.1197 -0.0117 0.029 Uiso 1 1 calc R . .
C59 C 1.2733(6) 0.1554(2) -0.0854(4) 0.0245(16) Uani 1 1 d . . .
H62 H 1.3415 0.1407 -0.0862 0.029 Uiso 1 1 calc R . .
C60 C 1.2493(6) 0.1896(2) -0.1288(4) 0.0215(15) Uani 1 1 d . . .
H63 H 1.3010 0.1978 -0.1592 0.026 Uiso 1 1 calc R . .
C61 C 1.1479(5) 0.2114(2) -0.1270(3) 0.0182(14) Uani 1 1 d . . .
H64 H 1.1319 0.2344 -0.1563 0.022 Uiso 1 1 calc R . .
C62 C 0.8634(5) 0.20087(19) -0.1595(3) 0.0141(13) Uani 1 1 d . . .
C63 C 0.9026(6) 0.2095(2) -0.2228(3) 0.0184(14) Uani 1 1 d . . .
H65 H 0.9644 0.2277 -0.2261 0.022 Uiso 1 1 calc R . .
C64 C 0.8503(6) 0.1915(2) -0.2802(3) 0.0192(14) Uani 1 1 d . . .
H66 H 0.8768 0.1976 -0.3218 0.023 Uiso 1 1 calc R . .
C65 C 0.7577(6) 0.1641(2) -0.2760(4) 0.0233(15) Uani 1 1 d . . .
H67 H 0.7218 0.1522 -0.3146 0.028 Uiso 1 1 calc R . .
C66 C 0.7198(6) 0.1548(2) -0.2134(4) 0.0265(16) Uani 1 1 d . . .
H68 H 0.6586 0.1364 -0.2102 0.032 Uiso 1 1 calc R . .
C67 C 0.7723(6) 0.1729(2) -0.1555(4) 0.0218(15) Uani 1 1 d . . .
H69 H 0.7465 0.1662 -0.1138 0.026 Uiso 1 1 calc R . .
O1 O 0.6312(4) 0.24979(13) -0.0758(2) 0.0165(10) Uani 1 1 d . . .
C68 C 0.5319(6) 0.2293(2) -0.1062(4) 0.0229(15) Uani 1 1 d . . .
H70 H 0.5402 0.1983 -0.1031 0.034 Uiso 1 1 calc R . .
H71 H 0.5214 0.2376 -0.1525 0.034 Uiso 1 1 calc R . .
H72 H 0.4676 0.2381 -0.0832 0.034 Uiso 1 1 calc R . .
O2 O 1.0280(4) 0.25150(13) 0.0980(2) 0.0156(9) Uani 1 1 d . . .
C69 C 1.1268(6) 0.2317(2) 0.1295(4) 0.0242(16) Uani 1 1 d . . .
H73 H 1.1918 0.2415 0.1079 0.036 Uiso 1 1 calc R . .
H74 H 1.1206 0.2007 0.1256 0.036 Uiso 1 1 calc R . .
H75 H 1.1343 0.2397 0.1760 0.036 Uiso 1 1 calc R . .
Pd1 Pd 0.83083(4) 0.221632(14) 0.01202(2) 0.01158(12) Uani 1 1 d . . .
Cl1 Cl 0.83020(15) 0.14575(5) 0.01552(9) 0.0206(3) Uani 1 1 d . . .
Cl2 Cl 0.83087(13) 0.29545(4) 0.00909(8) 0.0131(3) Uani 1 1 d . . .
C70A C 0.9791(10) 0.4385(4) -0.1930(8) 0.015(3) Uani 0.50 1 d PDU A 1
H84 H 1.0074 0.4652 -0.2101 0.022 Uiso 0.50 1 calc PR A 1
H76 H 0.9654 0.4421 -0.1465 0.022 Uiso 0.70 1 calc PR A 1
H77 H 0.9100 0.4309 -0.2181 0.022 Uiso 0.70 1 calc PR A 1
C70B C 0.9689(17) 0.4329(8) -0.2233(15) 0.076(8) Uani 0.50 1 d PDU A 2
H86 H 0.9302 0.4421 -0.1853 0.114 Uiso 0.50 1 calc PR A 2
H79 H 0.9172 0.4178 -0.2543 0.114 Uiso 0.30 1 calc PR A 2
H81 H 0.9985 0.4577 -0.2451 0.114 Uiso 0.30 1 calc PR A 2
C71A C 0.3059(12) 0.5383(4) 0.3651(6) 0.089(4) Uani 0.50 1 d PDU B 2
H88 H 0.3729 0.5292 0.3930 0.107 Uiso 0.50 1 calc PR B 2
Cl3A Cl 0.2716(8) 0.4992(3) 0.3026(4) 0.111(3) Uani 0.50 1 d PDU B 2
Cl4A Cl 0.1909(7) 0.5446(3) 0.4147(4) 0.099(2) Uani 0.50 1 d PDU B 2
Cl5A Cl 0.3312(11) 0.5881(4) 0.3258(6) 0.116(4) Uani 0.50 1 d PDU B 2
C71B C 0.5023(10) 0.5727(4) 0.3835(4) 0.066(4) Uani 0.50 1 d PDU C 1
H89 H 0.5546 0.5968 0.3934 0.080 Uiso 0.50 1 calc PR C 1
Cl3B Cl 0.5550(7) 0.5398(3) 0.3207(4) 0.108(3) Uani 0.50 1 d PDU C 1
Cl4B Cl 0.3699(7) 0.5937(3) 0.3560(5) 0.081(2) Uani 0.50 1 d PDU C 1
Cl5B Cl 0.4824(8) 0.5446(3) 0.4579(4) 0.116(3) Uani 0.50 1 d PDU . 1
O3A O -0.066(2) 0.4444(8) 0.3428(13) 0.139(8) Uani 0.50 1 d PDU D 2
C72A C 0.017(3) 0.4178(12) 0.380(2) 0.137(10) Uani 0.50 1 d PDU D 2
C72B C 0.2083(13) 0.4292(8) 0.4186(13) 0.069(6) Uani 0.50 1 d PDU E 1
O3B O 0.0926(10) 0.4163(3) 0.4252(7) 0.047(3) Uani 0.50 1 d PDU E 1
C74A C -0.190(3) 0.5251(13) 0.4907(18) 0.130(10) Uani 0.50 1 d PDU . .
O5A O -0.100(2) 0.5399(8) 0.4523(14) 0.144(8) Uani 0.50 1 d PDU . .
O6 O 0.1253(16) 0.5310(6) 0.4714(10) 0.091(5) Uani 0.50 1 d PU F 1
O4 O 0.5098(17) 0.5184(6) 0.5636(11) 0.101(6) Uani 0.50 1 d PDU . .
C73 C 0.565(2) 0.5598(7) 0.5610(15) 0.088(7) Uani 0.50 1 d PDU . .
C74B C 0.674(2) 0.5013(8) 0.3806(14) 0.088(7) Uani 0.50 1 d PDU G 2
O5B O 0.7543(16) 0.4702(6) 0.4087(10) 0.096(6) Uani 0.50 1 d PDU G 2
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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_3
C7 C1 C35 112.4(5) .
C3 C2 C7 118.8(5) .
C3 C2 P2 119.8(5) .
C7 C2 P2 121.4(5) .
C4 C3 C2 118.2(6) .
C4 C3 C11 117.0(6) .
C2 C3 C11 124.6(6) .
C5 C4 C3 123.1(6) .
C4 C5 C6 117.0(6) .
C4 C5 C8 122.6(6) .
C6 C5 C8 120.4(6) .
C7 C6 C5 123.3(6) .
C6 C7 C2 117.9(6) .
C6 C7 C1 116.9(6) .
C2 C7 C1 124.8(5) .
C10 C8 C70A 118.7(8) .
C10 C8 C70B 96.3(13) .
C70A C8 C70B 23.9(12) .
C10 C8 C5 110.1(6) .
C70A C8 C5 108.7(7) .
C70B C8 C5 113.1(12) .
C10 C8 C9 105.6(7) .
C70A C8 C9 102.4(8) .
C70B C8 C9 119.2(13) .
C5 C8 C9 111.0(6) .
C17 C11 C3 111.6(5) .
O2 C12 C17 120.1(6) .
O2 C12 C13 118.9(6) .
C17 C12 C13 120.8(6) .
C14 C13 C12 118.0(6) .
C14 C13 C22 120.6(6) .
C12 C13 C22 121.3(6) .
C13 C14 C15 122.6(6) .
C14 C15 C16 117.4(6) .
C14 C15 C18 120.0(6) .
C16 C15 C18 122.6(6) .
C17 C16 C15 121.7(6) .
C16 C17 C12 118.8(6) .
C16 C17 C11 120.2(6) .
C12 C17 C11 120.9(6) .
C15 C18 C19 109.2(6) .
C15 C18 C21 112.3(6) .
C19 C18 C21 109.9(7) .
C15 C18 C20 109.4(5) .
C19 C18 C20 109.0(7) .
C21 C18 C20 107.0(6) .
C13 C22 C28 111.4(5) .
C24 C23 C28 118.6(5) .
C24 C23 P1 119.7(5) .
C28 C23 P1 121.7(5) .
C25 C24 C23 117.9(6) .
C25 C24 C33 116.5(5) .
C23 C24 C33 125.4(5) .
C26 C25 C24 123.7(6) .
C25 C26 C27 116.6(6) .
C25 C26 C29 123.1(6) .
C27 C26 C29 120.2(6) .
C28 C27 C26 122.5(6) .
C27 C28 C23 118.8(6) .
C27 C28 C22 115.9(5) .
C23 C28 C22 125.1(6) .
C30 C29 C32 108.7(6) .
C30 C29 C31 107.4(6) .
C32 C29 C31 109.9(7) .
C30 C29 C26 112.3(6) .
C32 C29 C26 110.2(6) .
C31 C29 C26 108.3(6) .
C39 C33 C24 111.6(5) .
O1 C34 C35 119.0(6) .
O1 C34 C39 119.0(6) .
C35 C34 C39 121.8(6) .
C36 C35 C34 118.4(6) .
C36 C35 C1 120.8(6) .
C34 C35 C1 120.5(6) .
C35 C36 C37 121.4(6) .
C38 C37 C36 118.3(6) .
C38 C37 C40 119.4(6) .
C36 C37 C40 122.2(6) .
C37 C38 C39 122.3(6) .
C34 C39 C38 117.2(6) .
C34 C39 C33 121.7(6) .
C38 C39 C33 120.7(6) .
C42 C40 C41 108.0(6) .
C42 C40 C37 109.3(5) .
C41 C40 C37 112.2(5) .
C42 C40 C43 109.3(6) .
C41 C40 C43 108.4(6) .
C37 C40 C43 109.6(5) .
C44 P1 C50 99.8(3) .
C44 P1 C23 105.3(3) .
C50 P1 C23 104.0(3) .
C44 P1 Pd1 115.5(2) .
C50 P1 Pd1 117.0(2) .
C23 P1 Pd1 113.6(2) .
C45 C44 C49 119.3(6) .
C45 C44 P1 120.3(5) .
C49 C44 P1 120.4(5) .
C44 C45 C46 119.6(6) .
C47 C46 C45 120.5(6) .
C46 C47 C48 120.1(6) .
C47 C48 C49 120.1(6) .
C48 C49 C44 120.4(6) .
C51 C50 C55 119.5(6) .
C51 C50 P1 120.2(5) .
C55 C50 P1 120.2(5) .
C52 C51 C50 119.6(7) .
C53 C52 C51 121.2(7) .
C52 C53 C54 120.0(6) .
C53 C54 C55 119.9(7) .
C54 C55 C50 119.8(6) .
C56 P2 C62 99.4(3) .
C56 P2 C2 104.5(3) .
C62 P2 C2 104.9(3) .
C56 P2 Pd1 117.9(2) .
C62 P2 Pd1 115.8(2) .
C2 P2 Pd1 112.6(2) .
C57 C56 C61 118.8(6) .
C57 C56 P2 120.2(5) .
C61 C56 P2 120.8(5) .
C56 C57 C58 120.0(7) .
C59 C58 C57 120.5(7) .
C60 C59 C58 120.0(6) .
C59 C60 C61 119.6(7) .
C60 C61 C56 121.2(6) .
C67 C62 C63 118.7(6) .
C67 C62 P2 120.6(5) .
C63 C62 P2 120.7(5) .
C64 C63 C62 120.8(6) .
C63 C64 C65 120.2(7) .
C66 C65 C64 119.2(6) .
C65 C66 C67 120.7(7) .
C66 C67 C62 120.3(7) .
C34 O1 C68 112.6(5) .
C12 O2 C69 112.1(5) .
Cl2 Pd1 P1 84.84(6) .
Cl2 Pd1 P2 85.32(6) .
P1 Pd1 P2 170.16(5) .
Cl2 Pd1 Cl1 179.69(7) .
P1 Pd1 Cl1 94.86(6) .
P2 Pd1 Cl1 94.99(6) .
Cl4A C71A Cl5A 108.7(9) .
Cl4A C71A Cl3A 109.0(8) .
Cl5A C71A Cl3A 108.6(9) .
Cl5B C71B Cl4B 105.9(7) .
Cl5B C71B Cl3B 113.4(8) .
Cl4B C71B Cl3B 110.4(7) .
C71B Cl5B O4 106.7(9) 3_666
C73 O4 Cl5B 146.1(18) 3_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C7 1.535(8) .
C1 C35 1.534(9) .
C2 C3 1.419(8) .
C2 C7 1.424(8) .
C2 P2 1.844(6) .
C3 C4 1.395(9) .
C3 C11 1.537(9) .
C4 C5 1.375(9) .
C5 C6 1.393(9) .
C5 C8 1.541(9) .
C6 C7 1.383(9) .
C8 C10 1.488(10) .
C8 C70A 1.532(7) .
C8 C70B 1.535(8) .
C8 C9 1.560(11) .
C11 C17 1.531(9) .
C12 O2 1.384(7) .
C12 C17 1.399(9) .
C12 C13 1.413(9) .
C13 C14 1.383(9) .
C13 C22 1.526(9) .
C14 C15 1.403(9) .
C15 C16 1.409(9) .
C15 C18 1.528(9) .
C16 C17 1.387(9) .
C18 C19 1.530(10) .
C18 C21 1.542(10) .
C18 C20 1.542(10) .
C22 C28 1.547(9) .
C23 C24 1.413(8) .
C23 C28 1.419(8) .
C23 P1 1.848(6) .
C24 C25 1.395(8) .
C24 C33 1.539(9) .
C25 C26 1.374(9) .
C26 C27 1.402(9) .
C26 C29 1.546(9) .
C27 C28 1.383(9) .
C29 C30 1.528(10) .
C29 C32 1.535(10) .
C29 C31 1.539(10) .
C33 C39 1.521(9) .
C34 O1 1.389(7) .
C34 C35 1.401(9) .
C34 C39 1.400(9) .
C35 C36 1.385(8) .
C36 C37 1.404(9) .
C37 C38 1.387(9) .
C37 C40 1.544(8) .
C38 C39 1.400(8) .
C40 C42 1.526(9) .
C40 C41 1.533(10) .
C40 C43 1.546(10) .
P1 C44 1.832(7) .
P1 C50 1.841(6) .
P1 Pd1 2.3234(17) .
C44 C45 1.392(9) .
C44 C49 1.396(9) .
C45 C46 1.409(9) .
C46 C47 1.377(10) .
C47 C48 1.383(9) .
C48 C49 1.394(9) .
C50 C51 1.388(9) .
C50 C55 1.402(9) .
C51 C52 1.384(9) .
C52 C53 1.370(11) .
C53 C54 1.384(10) .
C54 C55 1.390(9) .
P2 C56 1.835(6) .
P2 C62 1.835(6) .
P2 Pd1 2.3237(17) .
C56 C57 1.385(9) .
C56 C61 1.402(9) .
C57 C58 1.396(9) .
C58 C59 1.390(10) .
C59 C60 1.380(10) .
C60 C61 1.385(9) .
C62 C67 1.392(9) .
C62 C63 1.405(9) .
C63 C64 1.380(9) .
C64 C65 1.395(10) .
C65 C66 1.389(10) .
C66 C67 1.389(10) .
O1 C68 1.434(7) .
O2 C69 1.428(8) .
Pd1 Cl2 2.2750(15) .
Pd1 Cl1 2.3388(16) .
C71A Cl4A 1.758(6) .
C71A Cl5A 1.759(7) .
C71A Cl3A 1.760(6) .
C71B Cl5B 1.750(6) .
C71B Cl4B 1.753(6) .
C71B Cl3B 1.762(6) .
Cl5B O4 1.99(2) 3_666
O3A C72A 1.444(8) .
C72B O3B 1.448(8) .
C74A O5A 1.440(8) .
O4 C73 1.435(10) .
O4 Cl5B 1.99(2) 3_666
C74B O5B 1.438(8) .
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
_geom_torsion_site_symmetry_4
C7 C2 C3 C4 -14.4(9) .
P2 C2 C3 C4 164.4(5) .
C7 C2 C3 C11 160.3(6) .
P2 C2 C3 C11 -20.9(8) .
C2 C3 C4 C5 5.7(10) .
C11 C3 C4 C5 -169.4(6) .
C3 C4 C5 C6 3.6(10) .
C3 C4 C5 C8 -177.3(6) .
C4 C5 C6 C7 -4.4(10) .
C8 C5 C6 C7 176.6(6) .
C5 C6 C7 C2 -4.3(9) .
C5 C6 C7 C1 169.4(6) .
C3 C2 C7 C6 13.7(9) .
P2 C2 C7 C6 -165.0(5) .
C3 C2 C7 C1 -159.5(6) .
P2 C2 C7 C1 21.7(8) .
C35 C1 C7 C6 -82.4(7) .
C35 C1 C7 C2 90.9(7) .
C4 C5 C8 C10 107.0(8) .
C6 C5 C8 C10 -73.9(8) .
C4 C5 C8 C70A -121.4(9) .
C6 C5 C8 C70A 57.6(10) .
C4 C5 C8 C70B -146.5(14) .
C6 C5 C8 C70B 32.5(15) .
C4 C5 C8 C9 -9.5(9) .
C6 C5 C8 C9 169.5(7) .
C4 C3 C11 C17 79.3(7) .
C2 C3 C11 C17 -95.4(7) .
O2 C12 C13 C14 177.7(5) .
C17 C12 C13 C14 -8.5(9) .
O2 C12 C13 C22 -5.7(9) .
C17 C12 C13 C22 168.1(6) .
C12 C13 C14 C15 0.9(9) .
C22 C13 C14 C15 -175.6(6) .
C13 C14 C15 C16 4.3(9) .
C13 C14 C15 C18 -178.4(6) .
C14 C15 C16 C17 -2.2(9) .
C18 C15 C16 C17 -179.4(6) .
C15 C16 C17 C12 -5.0(9) .
C15 C16 C17 C11 170.0(6) .
O2 C12 C17 C16 -175.8(5) .
C13 C12 C17 C16 10.5(9) .
O2 C12 C17 C11 9.2(9) .
C13 C12 C17 C11 -164.5(6) .
C3 C11 C17 C16 -62.2(8) .
C3 C11 C17 C12 112.7(7) .
C14 C15 C18 C19 -62.1(8) .
C16 C15 C18 C19 115.0(8) .
C14 C15 C18 C21 175.7(6) .
C16 C15 C18 C21 -7.2(9) .
C14 C15 C18 C20 57.0(8) .
C16 C15 C18 C20 -125.8(7) .
C14 C13 C22 C28 66.9(7) .
C12 C13 C22 C28 -109.5(6) .
C28 C23 C24 C25 -14.8(9) .
P1 C23 C24 C25 165.2(5) .
C28 C23 C24 C33 160.3(6) .
P1 C23 C24 C33 -19.7(9) .
C23 C24 C25 C26 5.0(10) .
C33 C24 C25 C26 -170.5(6) .
C24 C25 C26 C27 5.1(10) .
C24 C25 C26 C29 -177.9(6) .
C25 C26 C27 C28 -5.4(10) .
C29 C26 C27 C28 177.6(6) .
C26 C27 C28 C23 -4.4(10) .
C26 C27 C28 C22 170.8(6) .
C24 C23 C28 C27 14.6(9) .
P1 C23 C28 C27 -165.4(5) .
C24 C23 C28 C22 -160.2(6) .
P1 C23 C28 C22 19.8(9) .
C13 C22 C28 C27 -84.7(7) .
C13 C22 C28 C23 90.3(7) .
C25 C26 C29 C30 1.5(9) .
C27 C26 C29 C30 178.4(6) .
C25 C26 C29 C32 -119.8(7) .
C27 C26 C29 C32 57.1(8) .
C25 C26 C29 C31 120.0(7) .
C27 C26 C29 C31 -63.1(8) .
C25 C24 C33 C39 79.6(7) .
C23 C24 C33 C39 -95.6(7) .
O1 C34 C35 C36 178.4(5) .
C39 C34 C35 C36 -7.3(9) .
O1 C34 C35 C1 -7.1(9) .
C39 C34 C35 C1 167.2(6) .
C7 C1 C35 C36 64.2(8) .
C7 C1 C35 C34 -110.2(7) .
C34 C35 C36 C37 0.4(9) .
C1 C35 C36 C37 -174.2(6) .
C35 C36 C37 C38 4.5(9) .
C35 C36 C37 C40 -177.8(6) .
C36 C37 C38 C39 -2.7(9) .
C40 C37 C38 C39 179.5(6) .
O1 C34 C39 C38 -176.7(5) .
C35 C34 C39 C38 9.0(9) .
O1 C34 C39 C33 10.1(9) .
C35 C34 C39 C33 -164.2(6) .
C37 C38 C39 C34 -3.8(9) .
C37 C38 C39 C33 169.4(6) .
C24 C33 C39 C34 111.9(6) .
C24 C33 C39 C38 -61.0(7) .
C38 C37 C40 C42 -66.1(8) .
C36 C37 C40 C42 116.2(7) .
C38 C37 C40 C41 174.2(6) .
C36 C37 C40 C41 -3.5(9) .
C38 C37 C40 C43 53.7(8) .
C36 C37 C40 C43 -124.0(7) .
C24 C23 P1 C44 -144.8(5) .
C28 C23 P1 C44 35.3(6) .
C24 C23 P1 C50 -40.4(6) .
C28 C23 P1 C50 139.7(5) .
C24 C23 P1 Pd1 87.9(5) .
C28 C23 P1 Pd1 -92.0(5) .
C50 P1 C44 C45 112.5(5) .
C23 P1 C44 C45 -140.0(5) .
Pd1 P1 C44 C45 -13.9(6) .
C50 P1 C44 C49 -67.7(6) .
C23 P1 C44 C49 39.8(6) .
Pd1 P1 C44 C49 165.9(4) .
C49 C44 C45 C46 0.2(10) .
P1 C44 C45 C46 -180.0(5) .
C44 C45 C46 C47 -1.1(10) .
C45 C46 C47 C48 1.1(10) .
C46 C47 C48 C49 -0.3(10) .
C47 C48 C49 C44 -0.6(10) .
C45 C44 C49 C48 0.6(9) .
P1 C44 C49 C48 -179.2(5) .
C44 P1 C50 C51 -104.7(5) .
C23 P1 C50 C51 146.7(5) .
Pd1 P1 C50 C51 20.6(6) .
C44 P1 C50 C55 73.4(5) .
C23 P1 C50 C55 -35.1(6) .
Pd1 P1 C50 C55 -161.2(4) .
C55 C50 C51 C52 0.7(9) .
P1 C50 C51 C52 178.9(5) .
C50 C51 C52 C53 0.2(11) .
C51 C52 C53 C54 -0.7(11) .
C52 C53 C54 C55 0.3(10) .
C53 C54 C55 C50 0.5(10) .
C51 C50 C55 C54 -1.0(9) .
P1 C50 C55 C54 -179.2(5) .
C3 C2 P2 C56 -40.4(6) .
C7 C2 P2 C56 138.3(5) .
C3 C2 P2 C62 -144.5(5) .
C7 C2 P2 C62 34.3(6) .
C3 C2 P2 Pd1 88.7(5) .
C7 C2 P2 Pd1 -92.6(5) .
C62 P2 C56 C57 -102.0(6) .
C2 P2 C56 C57 149.8(5) .
Pd1 P2 C56 C57 24.0(6) .
C62 P2 C56 C61 73.9(6) .
C2 P2 C56 C61 -34.2(6) .
Pd1 P2 C56 C61 -160.1(4) .
C61 C56 C57 C58 -1.0(10) .
P2 C56 C57 C58 175.0(5) .
C56 C57 C58 C59 1.5(11) .
C57 C58 C59 C60 -1.1(11) .
C58 C59 C60 C61 0.4(10) .
C59 C60 C61 C56 0.1(10) .
C57 C56 C61 C60 0.3(10) .
P2 C56 C61 C60 -175.7(5) .
C56 P2 C62 C67 113.5(6) .
C2 P2 C62 C67 -138.6(5) .
Pd1 P2 C62 C67 -13.8(6) .
C56 P2 C62 C63 -66.7(6) .
C2 P2 C62 C63 41.1(6) .
Pd1 P2 C62 C63 166.0(4) .
C67 C62 C63 C64 1.5(10) .
P2 C62 C63 C64 -178.3(5) .
C62 C63 C64 C65 -0.3(10) .
C63 C64 C65 C66 -0.7(10) .
C64 C65 C66 C67 0.6(11) .
C65 C66 C67 C62 0.5(11) .
C63 C62 C67 C66 -1.6(10) .
P2 C62 C67 C66 178.1(5) .
C35 C34 O1 C68 -101.4(7) .
C39 C34 O1 C68 84.1(7) .
C17 C12 O2 C69 84.1(7) .
C13 C12 O2 C69 -102.1(7) .
C44 P1 Pd1 Cl2 -120.4(2) .
C50 P1 Pd1 Cl2 122.6(2) .
C23 P1 Pd1 Cl2 1.4(2) .
C44 P1 Pd1 P2 -120.0(4) .
C50 P1 Pd1 P2 123.0(4) .
C23 P1 Pd1 P2 1.8(5) .
C44 P1 Pd1 Cl1 59.6(2) .
C50 P1 Pd1 Cl1 -57.4(2) .
C23 P1 Pd1 Cl1 -178.6(2) .
C56 P2 Pd1 Cl2 123.3(2) .
C62 P2 Pd1 Cl2 -119.3(2) .
C2 P2 Pd1 Cl2 1.5(2) .
C56 P2 Pd1 P1 122.9(4) .
C62 P2 Pd1 P1 -119.7(4) .
C2 P2 Pd1 P1 1.0(5) .
C56 P2 Pd1 Cl1 -56.7(2) .
C62 P2 Pd1 Cl1 60.7(2) .
C2 P2 Pd1 Cl1 -178.6(2) .
Cl4B C71B Cl5B O4 106.9(9) 3_666
Cl3B C71B Cl5B O4 -14.2(12) 3_666
