#------------------------------------------------------------------------------
#$Date: 2018-07-24 08:09:47 +0200 (mar 24 de jul de 2018) $
#$Revision: 209230 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/12/7231231.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_7231231
loop_
_publ_author_name
'Chiu, Chien-Cheng'
'Chiu, Hui-Tzu'
'Lee, Dong-Sheng'
'Lu, Ta-Jung'
_publ_section_title
;
 An efficient class of bis-NHC salts: applications in Pd-catalyzed
 reactions under mild reaction conditions
;
_journal_issue                   46
_journal_name_full               'RSC Advances'
_journal_page_first              26407
_journal_paper_doi               10.1039/C8RA04094J
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C66 H64 Cl3 N8 O4 Pd2, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C68 H68 Cl7 F6 N8 O4 P Pd2'
_chemical_formula_weight         1667.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-19 deposited with the CCDC.
2018-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                87.943(3)
_cell_angle_beta                 84.738(3)
_cell_angle_gamma                76.841(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6608(10)
_cell_length_b                   17.1920(14)
_cell_length_c                   18.8963(15)
_cell_measurement_reflns_used    9042
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.409
_cell_measurement_theta_min      2.951
_cell_volume                     3987.7(6)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            84054
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.838
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.413
_refine_diff_density_min         -2.193
_refine_diff_density_rms         0.181
_refine_ls_extinction_coef       0.0066(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     870
_refine_ls_number_reflns         16416
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.1096
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1009P)²+76.2741P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2830
_refine_ls_wR_factor_ref         0.3036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12337
_reflns_number_total             16416
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ra04094j2.cif
_cod_data_source_block           l1pd
_cod_database_code               7231231
_shelx_shelxl_version_number     2014/7
_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   0.831
_shelx_estimated_absorpt_t_max   0.977
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.79125(6) 0.82985(4) 0.86362(4) 0.0304(2) Uani 1 1 d . . . . .
Pd2 Pd 0.82737(6) 0.83276(6) 0.62768(4) 0.0457(3) Uani 1 1 d . . . . .
Cl1 Cl 0.7887(2) 0.87044(16) 0.74551(13) 0.0454(6) Uani 1 1 d . . . . .
Cl2 Cl 0.7767(3) 0.80722(19) 0.98370(13) 0.0597(9) Uani 1 1 d . . . . .
Cl3 Cl 0.8639(3) 0.8115(2) 0.50883(13) 0.0740(12) Uani 1 1 d . . . . .
O1 O 1.2143(6) 0.5570(4) 0.9069(4) 0.0427(17) Uani 1 1 d . . . . .
O2 O 0.6156(9) 0.5270(6) 0.5864(6) 0.076(3) Uani 1 1 d D . . . .
O3 O 0.3462(8) 1.0846(5) 0.7925(5) 0.062(3) Uani 1 1 d . . . . .
O4 O 1.0491(9) 1.1386(6) 0.6637(5) 0.084(4) Uani 1 1 d . . . . .
N1 N 0.9987(7) 0.8757(4) 0.8968(4) 0.0312(17) Uani 1 1 d . . . . .
N2 N 0.8761(7) 0.9830(4) 0.8733(4) 0.0340(18) Uani 1 1 d . . . . .
N3 N 0.6292(7) 0.9702(6) 0.6156(4) 0.043(2) Uani 1 1 d . . . . .
N4 N 0.5948(7) 0.8540(6) 0.5930(4) 0.045(2) Uani 1 1 d . . . . .
N5 N 0.5822(7) 0.7763(5) 0.8419(4) 0.040(2) Uani 1 1 d . . . . .
N6 N 0.7161(7) 0.6753(4) 0.8643(4) 0.0309(17) Uani 1 1 d . . . . .
N7 N 1.0264(8) 0.6974(8) 0.6338(5) 0.063(4) Uani 1 1 d . . . . .
N8 N 1.0665(7) 0.8115(8) 0.6547(5) 0.057(3) Uani 1 1 d . . . . .
C1 C 0.8943(8) 0.8999(6) 0.8762(5) 0.035(2) Uani 1 1 d . . . . .
C2 C 1.0420(8) 0.9413(6) 0.9051(5) 0.034(2) Uani 1 1 d . . . . .
C3 C 1.1454(9) 0.9469(7) 0.9236(5) 0.042(2) Uani 1 1 d . . . . .
H3A H 1.2008 0.9009 0.9323 0.051 Uiso 1 1 calc R U . . .
C4 C 1.1608(10) 1.0230(7) 0.9282(5) 0.043(2) Uani 1 1 d . . . . .
H4A H 1.2288 1.0296 0.9415 0.052 Uiso 1 1 calc R U . . .
C5 C 1.0818(10) 1.0905(6) 0.9143(5) 0.041(2) Uani 1 1 d . . . . .
H5A H 1.0961 1.1417 0.9199 0.049 Uiso 1 1 calc R U . . .
C6 C 0.9830(9) 1.0850(6) 0.8926(5) 0.041(2) Uani 1 1 d . . . . .
H6A H 0.9304 1.1308 0.8795 0.049 Uiso 1 1 calc R U . . .
C7 C 0.9655(9) 1.0105(6) 0.8910(5) 0.036(2) Uani 1 1 d . . . . .
C8 C 0.7791(9) 1.0342(6) 0.8480(5) 0.041(2) Uani 1 1 d . . . . .
H8A H 0.7506 1.0783 0.8818 0.049 Uiso 1 1 calc R U . . .
H8B H 0.7225 1.0030 0.8464 0.049 Uiso 1 1 calc R U . . .
C9 C 0.8017(9) 1.0696(6) 0.7732(6) 0.044(3) Uani 1 1 d . . . . .
H9A H 0.8389 1.0259 0.7408 0.053 Uiso 1 1 calc R U . . .
H9B H 0.8508 1.1065 0.7760 0.053 Uiso 1 1 calc R U . . .
C10 C 0.6962(10) 1.1146(7) 0.7432(6) 0.052(3) Uani 1 1 d . . . . .
H10A H 0.7142 1.1524 0.7058 0.063 Uiso 1 1 calc R U . . .
H10B H 0.6494 1.1464 0.7817 0.063 Uiso 1 1 calc R U . . .
C11 C 0.6317(9) 1.0611(8) 0.7118(6) 0.053(3) Uani 1 1 d . . . . .
H11A H 0.6284 1.0154 0.7447 0.064 Uiso 1 1 calc R U . . .
H11B H 0.5562 1.0919 0.7075 0.064 Uiso 1 1 calc R U . . .
C12 C 0.6815(9) 1.0295(7) 0.6391(5) 0.047(3) Uani 1 1 d . . . . .
H12A H 0.6743 1.0743 0.6042 0.057 Uiso 1 1 calc R U . . .
H12B H 0.7601 1.0058 0.6415 0.057 Uiso 1 1 calc R U . . .
C13 C 0.5196(8) 0.9851(8) 0.5990(5) 0.047(3) Uani 1 1 d . . . . .
C14 C 0.4402(9) 1.0556(8) 0.5950(5) 0.053(3) Uani 1 1 d . . . . .
H14A H 0.4538 1.1062 0.6041 0.064 Uiso 1 1 calc R U . . .
C15 C 0.3371(8) 1.0466(9) 0.5764(6) 0.054(4) Uani 1 1 d . . . . .
H15A H 0.2799 1.0929 0.5737 0.065 Uiso 1 1 calc R U . . .
C16 C 0.3173(9) 0.9742(9) 0.5623(6) 0.057(4) Uani 1 1 d . . . . .
H16A H 0.2471 0.9719 0.5498 0.068 Uiso 1 1 calc R U . . .
C17 C 0.3966(9) 0.9035(8) 0.5657(5) 0.052(3) Uani 1 1 d . . . . .
H17A H 0.3828 0.8529 0.5567 0.063 Uiso 1 1 calc R U . . .
C18 C 0.4984(9) 0.9126(8) 0.5834(5) 0.050(3) Uani 1 1 d . . . . .
C19 C 0.6717(8) 0.8907(7) 0.6119(5) 0.046(3) Uani 1 1 d . . . . .
C20 C 1.0520(8) 0.7927(5) 0.9000(5) 0.0307(19) Uani 1 1 d . . . . .
C21 C 1.0629(9) 0.7458(6) 0.8418(5) 0.038(2) Uani 1 1 d . . . . .
H21A H 1.0336 0.7676 0.7989 0.046 Uiso 1 1 calc R U . . .
C22 C 1.1168(8) 0.6662(6) 0.8454(5) 0.034(2) Uani 1 1 d . . . . .
H22A H 1.1232 0.6329 0.8054 0.041 Uiso 1 1 calc R U . . .
C23 C 1.1612(8) 0.6352(5) 0.9073(5) 0.035(2) Uani 1 1 d . . . . .
C24 C 1.1533(9) 0.6842(6) 0.9664(5) 0.040(2) Uani 1 1 d . . . . .
H24A H 1.1843 0.6633 1.0090 0.049 Uiso 1 1 calc R U . . .
C25 C 1.1001(8) 0.7625(6) 0.9615(5) 0.034(2) Uani 1 1 d . . . . .
H25A H 1.0959 0.7968 1.0005 0.041 Uiso 1 1 calc R U . . .
C26 C 1.2649(9) 0.5246(6) 0.9684(7) 0.049(3) Uani 1 1 d . . . . .
H26A H 1.2999 0.4682 0.9609 0.073 Uiso 1 1 calc R U . . .
H26B H 1.3199 0.5540 0.9779 0.073 Uiso 1 1 calc R U . . .
H26C H 1.2100 0.5293 1.0090 0.073 Uiso 1 1 calc R U . . .
C27 C 0.6048(8) 0.7715(8) 0.5901(6) 0.050(3) Uani 1 1 d . . . . .
C28 C 0.5776(11) 0.7374(8) 0.5299(6) 0.058(4) Uani 1 1 d . . . . .
H28A H 0.5545 0.7701 0.4902 0.069 Uiso 1 1 calc R U . . .
C29 C 0.5845(14) 0.6557(9) 0.5286(9) 0.079(5) Uani 1 1 d . . . . .
H29A H 0.5693 0.6329 0.4867 0.095 Uiso 1 1 calc R U . . .
C30 C 0.6128(12) 0.6070(9) 0.5862(8) 0.073(5) Uani 1 1 d . . . . .
C31 C 0.6426(10) 0.6394(10) 0.6448(9) 0.079(6) Uani 1 1 d . . . . .
H31A H 0.6674 0.6055 0.6835 0.095 Uiso 1 1 calc R U . . .
C32 C 0.6370(9) 0.7220(9) 0.6482(6) 0.060(4) Uani 1 1 d . . . . .
H32A H 0.6550 0.7440 0.6897 0.072 Uiso 1 1 calc R U . . .
C33 C 0.6592(17) 0.4872(13) 0.6465(16) 0.077(7) Uani 0.56(2) 1 d . . P A 1
H33A H 0.6594 0.4303 0.6441 0.115 Uiso 0.56(2) 1 calc R U P A 1
H33B H 0.7339 0.4935 0.6482 0.115 Uiso 0.56(2) 1 calc R U P A 1
H33C H 0.6149 0.5099 0.6892 0.115 Uiso 0.56(2) 1 calc R U P A 1
C33' C 0.5757(18) 0.4929(16) 0.5346(11) 0.077(7) Uani 0.44(2) 1 d D . P A 2
H33D H 0.5854 0.4354 0.5445 0.115 Uiso 0.44(2) 1 calc R U P A 2
H33E H 0.4980 0.5172 0.5329 0.115 Uiso 0.44(2) 1 calc R U P A 2
H33F H 0.6148 0.5012 0.4887 0.115 Uiso 0.44(2) 1 calc R U P A 2
C34 C 0.6886(9) 0.7560(5) 0.8556(5) 0.035(2) Uani 1 1 d . . . . .
C35 C 0.5415(9) 0.7053(6) 0.8420(5) 0.037(2) Uani 1 1 d . . . . .
C36 C 0.4388(9) 0.6943(7) 0.8309(6) 0.045(3) Uani 1 1 d . . . . .
H36A H 0.3796 0.7377 0.8225 0.054 Uiso 1 1 calc R U . . .
C37 C 0.4288(10) 0.6145(7) 0.8329(6) 0.051(3) Uani 1 1 d . . . . .
H37A H 0.3609 0.6033 0.8246 0.061 Uiso 1 1 calc R U . . .
C38 C 0.5154(11) 0.5516(7) 0.8468(5) 0.047(3) Uani 1 1 d . . . . .
H38A H 0.5053 0.4986 0.8466 0.056 Uiso 1 1 calc R U . . .
C39 C 0.6153(10) 0.5636(6) 0.8606(6) 0.049(3) Uani 1 1 d . . . . .
H39A H 0.6727 0.5208 0.8733 0.059 Uiso 1 1 calc R U . . .
C40 C 0.6274(9) 0.6431(6) 0.8548(5) 0.036(2) Uani 1 1 d . . . . .
C41 C 0.8253(9) 0.6282(6) 0.8771(5) 0.040(2) Uani 1 1 d . . . . .
H41A H 0.8193 0.5917 0.9182 0.048 Uiso 1 1 calc R U . . .
H41B H 0.8708 0.6648 0.8893 0.048 Uiso 1 1 calc R U . . .
C42 C 0.8803(10) 0.5802(6) 0.8140(6) 0.047(3) Uani 1 1 d . . . . .
H42A H 0.8377 0.5408 0.8041 0.056 Uiso 1 1 calc R U . . .
H42B H 0.9534 0.5504 0.8254 0.056 Uiso 1 1 calc R U . . .
C43 C 0.8920(9) 0.6315(6) 0.7477(5) 0.045(3) Uani 1 1 d . . . . .
H43A H 0.9310 0.6729 0.7585 0.053 Uiso 1 1 calc R U . . .
H43B H 0.8186 0.6591 0.7348 0.053 Uiso 1 1 calc R U . . .
C44 C 0.9537(11) 0.5834(9) 0.6839(6) 0.067(4) Uani 1 1 d . . . . .
H44A H 0.9130 0.5439 0.6710 0.081 Uiso 1 1 calc R U . . .
H44B H 1.0261 0.5539 0.6969 0.081 Uiso 1 1 calc R U . . .
C45 C 0.9677(11) 0.6383(10) 0.6202(6) 0.067(4) Uani 1 1 d . . . . .
H45A H 1.0066 0.6055 0.5798 0.080 Uiso 1 1 calc R U . . .
H45B H 0.8949 0.6655 0.6060 0.080 Uiso 1 1 calc R U . . .
C46 C 1.1394(9) 0.6837(11) 0.6449(6) 0.067(5) Uani 1 1 d . . . . .
C47 C 1.2190(11) 0.6107(10) 0.6408(6) 0.076(5) Uani 1 1 d . . . . .
H47A H 1.2029 0.5608 0.6319 0.091 Uiso 1 1 calc R U . . .
C48 C 1.3241(12) 0.6196(13) 0.6512(7) 0.088(7) Uani 1 1 d . . . . .
H48A H 1.3816 0.5731 0.6504 0.106 Uiso 1 1 calc R U . . .
C49 C 1.3484(10) 0.6917(12) 0.6626(7) 0.074(5) Uani 1 1 d . . . . .
H49A H 1.4217 0.6936 0.6677 0.089 Uiso 1 1 calc R U . . .
C50 C 1.2686(9) 0.7617(10) 0.6667(6) 0.067(4) Uani 1 1 d . . . . .
H50A H 1.2857 0.8114 0.6752 0.080 Uiso 1 1 calc R U . . .
C51 C 1.1635(9) 0.7569(9) 0.6582(6) 0.057(4) Uani 1 1 d . . . . .
C52 C 0.9841(10) 0.7752(8) 0.6400(5) 0.057(4) Uani 1 1 d . . . . .
C53 C 0.5229(8) 0.8554(6) 0.8315(5) 0.042(3) Uani 1 1 d . . . . .
C54 C 0.5253(9) 0.9144(6) 0.8787(5) 0.044(3) Uani 1 1 d . . . . .
H54A H 0.5662 0.9017 0.9189 0.053 Uiso 1 1 calc R U . . .
C55 C 0.4676(10) 0.9927(7) 0.8673(6) 0.053(3) Uani 1 1 d . . . . .
H55A H 0.4707 1.0340 0.8987 0.064 Uiso 1 1 calc R U . . .
C56 C 0.4050(10) 1.0092(6) 0.8087(6) 0.047(3) Uani 1 1 d . . . . .
C57 C 0.4002(9) 0.9513(7) 0.7639(6) 0.045(3) Uani 1 1 d . . . . .
H57A H 0.3568 0.9641 0.7249 0.054 Uiso 1 1 calc R U . . .
C58 C 0.4590(9) 0.8716(6) 0.7739(5) 0.037(2) Uani 1 1 d . . . . .
H58A H 0.4551 0.8306 0.7425 0.044 Uiso 1 1 calc R U . . .
C59 C 0.3533(12) 1.1476(7) 0.8334(7) 0.061(4) Uani 1 1 d . . . . .
H59A H 0.3075 1.1970 0.8157 0.092 Uiso 1 1 calc R U . . .
H59B H 0.3284 1.1379 0.8829 0.092 Uiso 1 1 calc R U . . .
H59C H 0.4291 1.1527 0.8308 0.092 Uiso 1 1 calc R U . . .
C60 C 1.0565(9) 0.8958(8) 0.6598(6) 0.056(4) Uani 1 1 d . . . . .
C61 C 1.1006(9) 0.9265(9) 0.7168(6) 0.061(4) Uani 1 1 d . . . . .
H61A H 1.1306 0.8919 0.7538 0.073 Uiso 1 1 calc R U . . .
C62 C 1.0993(9) 1.0063(8) 0.7175(6) 0.059(4) Uani 1 1 d . . . . .
H62A H 1.1311 1.0260 0.7548 0.070 Uiso 1 1 calc R U . . .
C63 C 1.0532(10) 1.0598(9) 0.6658(6) 0.066(4) Uani 1 1 d . . . . .
C64 C 1.0079(10) 1.0273(9) 0.6095(6) 0.066(4) Uani 1 1 d . . . . .
H64A H 0.9736 1.0619 0.5739 0.079 Uiso 1 1 calc R U . . .
C65 C 1.0138(9) 0.9495(10) 0.6069(6) 0.066(4) Uani 1 1 d . . . . .
H65A H 0.9878 0.9293 0.5673 0.079 Uiso 1 1 calc R U . . .
C66 C 1.0981(13) 1.1691(10) 0.7175(8) 0.079(5) Uani 1 1 d . . . . .
H66A H 1.0899 1.2268 0.7102 0.118 Uiso 1 1 calc R U . . .
H66B H 1.0628 1.1586 0.7640 0.118 Uiso 1 1 calc R U . . .
H66C H 1.1757 1.1431 0.7154 0.118 Uiso 1 1 calc R U . . .
Cl4 Cl 0.7985(4) 0.1954(3) 0.5236(3) 0.0877(12) Uani 1 1 d . . . . .
Cl6 Cl 0.3955(5) 0.8111(3) 1.0105(3) 0.1058(18) Uani 1 1 d . . . . .
Cl5 Cl 0.8320(5) 0.3541(3) 0.5476(3) 0.1041(16) Uani 1 1 d . . . . .
Cl7 Cl 0.5647(6) 0.6896(4) 1.0593(5) 0.162(3) Uani 1 1 d . . . . .
C67 C 0.8608(11) 0.2557(9) 0.5739(7) 0.061(4) Uani 1 1 d . . . . .
H67A H 0.9407 0.2348 0.5689 0.073 Uiso 1 1 calc R U . . .
H67B H 0.8355 0.2516 0.6247 0.073 Uiso 1 1 calc R U . . .
C68 C 0.4409(15) 0.7067(12) 1.0295(9) 0.094(6) Uani 1 1 d . . . . .
H68A H 0.3892 0.6894 1.0659 0.113 Uiso 1 1 calc R U . . .
H68B H 0.4437 0.6758 0.9859 0.113 Uiso 1 1 calc R U . . .
P P 0.8014(4) 0.3289(2) 0.80598(17) 0.0694(12) Uani 1 1 d . . . . .
F1 F 0.8275(13) 0.2723(6) 0.7416(5) 0.126(5) Uani 1 1 d . . . . .
F2 F 0.8880(13) 0.2727(7) 0.8450(9) 0.162(7) Uani 1 1 d . U . . .
F3 F 0.7869(17) 0.3864(7) 0.8701(6) 0.194(9) Uani 1 1 d . . . . .
F4 F 0.725(3) 0.381(2) 0.7627(16) 0.39(3) Uani 1 1 d . . . . .
F5 F 0.868(3) 0.3812(12) 0.7719(9) 0.317(18) Uani 1 1 d . U . . .
F6 F 0.7244(18) 0.282(2) 0.8394(10) 0.293(16) Uani 1 1 d . . . . .
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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 '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
C1 Pd1 C34 177.1(4) .
C1 Pd1 Cl2 89.7(3) .
C34 Pd1 Cl2 87.7(3) .
C1 Pd1 Cl1 88.7(3) .
C34 Pd1 Cl1 94.1(3) .
Cl2 Pd1 Cl1 171.67(12) .
C19 Pd2 C52 178.2(4) .
C19 Pd2 Cl3 90.3(3) .
C52 Pd2 Cl3 88.0(3) .
C19 Pd2 Cl1 87.2(3) .
C52 Pd2 Cl1 94.5(3) .
Cl3 Pd2 Cl1 173.16(13) .
Pd1 Cl1 Pd2 146.70(13) .
C23 O1 C26 118.1(8) .
C30 O2 C33 112.6(16) .
C30 O2 C33' 122.1(16) .
C56 O3 C59 118.7(11) .
C63 O4 C66 117.2(11) .
C2 N1 C1 110.1(8) .
C2 N1 C20 128.3(8) .
C1 N1 C20 121.2(8) .
C1 N2 C7 112.5(8) .
C1 N2 C8 123.4(9) .
C7 N2 C8 123.9(8) .
C13 N3 C12 124.9(9) .
C13 N3 C19 108.4(11) .
C12 N3 C19 126.5(9) .
C19 N4 C27 125.8(9) .
C19 N4 C18 108.8(11) .
C27 N4 C18 125.1(11) .
C34 N5 C35 108.8(8) .
C34 N5 C53 124.5(9) .
C35 N5 C53 126.7(9) .
C34 N6 C40 109.9(9) .
C34 N6 C41 125.3(9) .
C40 N6 C41 124.7(8) .
C52 N7 C46 107.8(14) .
C52 N7 C45 125.6(11) .
C46 N7 C45 126.7(12) .
C52 N8 C51 111.5(13) .
C52 N8 C60 125.4(9) .
C51 N8 C60 123.0(12) .
N1 C1 N2 103.9(9) .
N1 C1 Pd1 126.6(7) .
N2 C1 Pd1 129.3(7) .
N1 C2 C7 109.5(9) .
N1 C2 C3 131.0(9) .
C7 C2 C3 119.5(9) .
C4 C3 C2 115.6(10) .
C5 C4 C3 122.9(11) .
C4 C5 C6 121.5(10) .
C7 C6 C5 115.8(10) .
C6 C7 C2 124.4(11) .
C6 C7 N2 131.5(10) .
C2 C7 N2 104.0(8) .
N2 C8 C9 112.0(8) .
C8 C9 C10 111.3(9) .
C9 C10 C11 114.5(9) .
C12 C11 C10 112.6(10) .
N3 C12 C11 111.3(10) .
N3 C13 C14 131.7(14) .
N3 C13 C18 107.3(9) .
C14 C13 C18 121.0(12) .
C13 C14 C15 115.4(13) .
C16 C15 C14 122.7(10) .
C15 C16 C17 122.2(13) .
C18 C17 C16 115.1(14) .
C17 C18 N4 129.8(13) .
C17 C18 C13 123.6(10) .
N4 C18 C13 106.5(11) .
N4 C19 N3 109.0(9) .
N4 C19 Pd2 124.0(8) .
N3 C19 Pd2 126.9(10) .
C21 C20 N1 120.6(8) .
C21 C20 C25 120.6(8) .
N1 C20 C25 118.7(8) .
C20 C21 C22 119.7(9) .
C23 C22 C21 119.9(8) .
O1 C23 C22 116.8(9) .
O1 C23 C24 122.8(9) .
C22 C23 C24 120.4(8) .
C25 C24 C23 118.7(9) .
C24 C25 C20 120.7(9) .
C32 C27 N4 120.7(12) .
C32 C27 C28 118.8(13) .
N4 C27 C28 120.4(9) .
C29 C28 C27 119.9(12) .
C28 C29 C30 121.7(17) .
C31 C30 O2 119.0(12) .
C31 C30 C29 118.8(16) .
O2 C30 C29 122.2(17) .
C30 C31 C32 121.1(12) .
C27 C32 C31 119.6(14) .
O2 C33' C33' 143(2) 2_666
N6 C34 N5 107.6(9) .
N6 C34 Pd1 124.6(8) .
N5 C34 Pd1 127.8(7) .
C40 C35 N5 106.2(9) .
C40 C35 C36 122.8(10) .
N5 C35 C36 131.0(10) .
C35 C36 C37 115.3(10) .
C36 C37 C38 121.8(11) .
C39 C38 C37 122.3(10) .
C38 C39 C40 116.0(11) .
C35 C40 N6 107.6(9) .
C35 C40 C39 121.6(11) .
N6 C40 C39 130.7(10) .
N6 C41 C42 112.6(8) .
C41 C42 C43 112.8(8) .
C42 C43 C44 113.2(9) .
C43 C44 C45 110.9(11) .
N7 C45 C44 113.5(11) .
N7 C46 C47 128.4(18) .
N7 C46 C51 108.4(11) .
C47 C46 C51 123.1(14) .
C48 C47 C46 113.3(17) .
C47 C48 C49 123.7(13) .
C50 C49 C48 121.6(15) .
C49 C50 C51 117.7(17) .
N8 C51 C50 134.6(16) .
N8 C51 C46 104.5(12) .
C50 C51 C46 120.7(12) .
N8 C52 N7 107.8(10) .
N8 C52 Pd2 125.4(9) .
N7 C52 Pd2 126.7(12) .
C58 C53 N5 118.3(10) .
C58 C53 C54 121.1(9) .
N5 C53 C54 120.5(10) .
C55 C54 C53 120.1(11) .
C54 C55 C56 118.7(12) .
O3 C56 C57 115.7(11) .
O3 C56 C55 123.1(11) .
C57 C56 C55 121.2(10) .
C56 C57 C58 121.1(11) .
C53 C58 C57 117.7(10) .
C65 C60 N8 122.1(13) .
C65 C60 C61 117.8(14) .
N8 C60 C61 119.9(9) .
C62 C61 C60 119.2(11) .
C61 C62 C63 122.5(14) .
O4 C63 C62 125.3(15) .
O4 C63 C64 117.7(11) .
C62 C63 C64 117.0(14) .
C65 C64 C63 120.5(11) .
C64 C65 C60 122.8(15) .
Cl4 C67 Cl5 112.8(7) .
Cl7 C68 Cl6 109.4(12) .
F6 P F4 97(2) .
F6 P F2 86.4(14) .
F4 P F2 174.7(18) .
F6 P F3 94.1(12) .
F4 P F3 96.8(12) .
F2 P F3 87.1(7) .
F6 P F1 90.3(11) .
F4 P F1 86.0(12) .
F2 P F1 89.8(8) .
F3 P F1 174.5(11) .
F6 P F5 174.4(19) .
F4 P F5 78(2) .
F2 P F5 98.9(17) .
F3 P F5 84.3(10) .
F1 P F5 91.6(8) .
P F2 F5 39.7(10) .
P F5 F2 41.4(8) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C1 2.000(11) .
Pd1 C34 2.031(11) .
Pd1 Cl2 2.286(3) .
Pd1 Cl1 2.315(2) .
Pd2 C19 2.039(10) .
Pd2 C52 2.036(10) .
Pd2 Cl3 2.277(3) .
Pd2 Cl1 2.318(3) .
O1 C23 1.359(11) .
O1 C26 1.414(13) .
O2 C30 1.368(19) .
O2 C33 1.40(3) .
O2 C33' 1.351(2) .
O3 C56 1.379(12) .
O3 C59 1.377(15) .
O4 C63 1.344(19) .
O4 C66 1.41(2) .
N1 C2 1.382(12) .
N1 C1 1.380(13) .
N1 C20 1.434(11) .
N2 C1 1.395(12) .
N2 C7 1.393(14) .
N2 C8 1.448(13) .
N3 C13 1.416(14) .
N3 C12 1.438(16) .
N3 C19 1.352(15) .
N4 C19 1.354(16) .
N4 C27 1.398(16) .
N4 C18 1.415(12) .
N5 C34 1.358(14) .
N5 C35 1.429(14) .
N5 C53 1.412(13) .
N6 C34 1.359(12) .
N6 C40 1.390(13) .
N6 C41 1.470(13) .
N7 C52 1.328(17) .
N7 C46 1.429(16) .
N7 C45 1.43(2) .
N8 C52 1.384(19) .
N8 C51 1.371(13) .
N8 C60 1.432(19) .
C2 C7 1.386(14) .
C2 C3 1.410(15) .
C3 C4 1.373(15) .
C4 C5 1.384(16) .
C5 C6 1.375(16) .
C6 C7 1.352(14) .
C8 C9 1.547(13) .
C9 C10 1.530(16) .
C10 C11 1.529(19) .
C11 C12 1.524(14) .
C13 C14 1.392(14) .
C13 C18 1.380(19) .
C14 C15 1.425(18) .
C15 C16 1.36(2) .
C16 C17 1.392(16) .
C17 C18 1.405(18) .
C20 C21 1.366(13) .
C20 C25 1.390(13) .
C21 C22 1.386(13) .
C22 C23 1.380(14) .
C23 C24 1.406(14) .
C24 C25 1.365(14) .
C27 C32 1.397(14) .
C27 C28 1.402(19) .
C28 C29 1.39(2) .
C29 C30 1.373(19) .
C30 C31 1.38(2) .
C31 C32 1.41(2) .
C33' C33' 2.38(4) 2_666
C35 C40 1.373(14) .
C35 C36 1.391(16) .
C36 C37 1.405(17) .
C37 C38 1.390(17) .
C38 C39 1.376(17) .
C39 C40 1.408(15) .
C41 C42 1.498(14) .
C42 C43 1.520(15) .
C43 C44 1.534(15) .
C44 C45 1.53(2) .
C46 C47 1.419(18) .
C46 C51 1.40(2) .
C47 C48 1.41(2) .
C48 C49 1.37(3) .
C49 C50 1.383(19) .
C50 C51 1.377(19) .
C53 C58 1.398(15) .
C53 C54 1.382(16) .
C54 C55 1.397(15) .
C55 C56 1.405(18) .
C56 C57 1.344(17) .
C57 C58 1.418(14) .
C60 C65 1.397(14) .
C60 C61 1.43(2) .
C61 C62 1.37(2) .
C62 C63 1.391(16) .
C63 C64 1.44(2) .
C64 C65 1.33(2) .
Cl4 C67 1.782(15) .
Cl6 C68 1.79(2) .
Cl5 C67 1.713(15) .
Cl7 C68 1.67(2) .
P F6 1.483(19) .
P F4 1.450(17) .
P F2 1.515(11) .
P F3 1.562(11) .
P F1 1.550(9) .
P F5 1.463(17) .
F2 F5 2.26(2) .
