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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/18/4321845.cif $
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#
# 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_4321845
loop_
_publ_author_name
'Tianle Zhang'
'Marc Drouin'
'Pierre D. Harvey'
_publ_contact_author
;
Pierre D. Harvey
Department de chimie
Universite de Sherbrooke
2500 boul. Universite, Sherbrooke
Que., J1K 2R1
CANADA
;
_publ_contact_author_email       pharvey@courrier.usherb.ca
_publ_contact_author_fax         819-821-8017
_publ_contact_author_phone       819-821-7092
_publ_section_title
;
 Preparation, Spectroscopic Characterization, and Theoretical Study of the
 [Pd4(dmb)4(PPh3)2]Cl2 Complex (dmb = 1,8-Diisocyano-p-menthane) and Its
 Organometallic Polymer {[Pd4(dmb)5](CH3CO2)2}n: The First Examples of
 58-Electron Linear Pd4 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1305
_journal_page_last               1315
_journal_paper_doi               10.1021/ic9811594
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C48 H44 Cl0.5 N12 Pd'
_chemical_formula_weight         913.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                108.267(10)
_cell_angle_beta                 104.834(10)
_cell_angle_gamma                101.221(10)
_cell_formula_units_Z            2
_cell_length_a                   13.314(2)
_cell_length_b                   13.490(2)
_cell_length_c                   14.645(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2303.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     1.54060
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8739
_diffrn_reflns_theta_full        69.87
_diffrn_reflns_theta_max         69.87
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    0.845
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             941
_refine_diff_density_max         1.626
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8739
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1524P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2241
_reflns_number_gt                5313
_reflns_number_total             8739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9811594_2.cif
_cod_data_source_block           3
_cod_original_formula_sum        'C48 H44 Cl0.50 N12 Pd'
_cod_database_code               4321845
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.05558(4) 0.35597(3) 0.35996(3) 0.0744(2) Uani 1 1 d . . .
Cl Cl 0.0000 0.5000 0.5000 0.1297(11) Uani 1 2 d S . .
N1 N 0.0684(5) 0.5669(5) 0.8005(4) 0.0873(15) Uani 1 1 d . . .
N2 N 0.1589(5) 0.2943(4) 0.5420(4) 0.0856(15) Uani 1 1 d . . .
N3 N 0.1646(6) 0.8028(5) 0.6750(4) 0.0832(15) Uani 1 1 d . . .
N4 N 0.2580(5) 0.5463(5) 0.4078(4) 0.0875(15) Uani 1 1 d . . .
N5 N 0.4560(7) -0.1683(6) 0.2277(6) 0.126(3) Uani 1 1 d . . .
N6 N 0.3778(8) 0.0343(7) 0.4776(6) 0.137(3) Uani 1 1 d . . .
N7 N 0.2147(7) 0.1849(6) -0.1220(5) 0.115(2) Uani 1 1 d . . .
N8 N 0.1514(7) 0.3847(6) 0.1335(6) 0.117(2) Uani 1 1 d . . .
N9 N 0.1442(6) 0.7877(6) 1.1776(6) 0.120(2) Uani 1 1 d . . .
N10 N 0.0311(7) 1.0503(6) 1.3395(5) 0.112(2) Uani 1 1 d . . .
N11 N 0.4762(8) 0.8386(6) 0.9902(6) 0.127(3) Uani 1 1 d . . .
N12 N 0.5329(7) 0.6079(6) 0.7335(6) 0.116(2) Uani 1 1 d . . .
C1 C 0.0209(6) 0.6002(5) 0.7478(5) 0.0827(17) Uani 1 1 d . . .
C2 C 0.1312(13) 0.5240(11) 0.8689(13) 0.1022(10) Uani 0.644(5) 1 d PD A 1
C3 C 0.2437(10) 0.5370(9) 0.8566(8) 0.1022(10) Uani 0.644(5) 1 d PD A 1
H3A H 0.2765 0.6129 0.8689 0.123 Uiso 0.64 1 calc P A 1
H3B H 0.2902 0.5187 0.9076 0.123 Uiso 0.64 1 calc P A 1
C4 C 0.2379(14) 0.4642(10) 0.7497(14) 0.1022(10) Uani 0.644(5) 1 d PD A 1
H4A H 0.3107 0.4737 0.7460 0.123 Uiso 0.64 1 calc P A 1
H4B H 0.1956 0.4852 0.6985 0.123 Uiso 0.64 1 calc P A 1
C5 C 0.1841(9) 0.3425(8) 0.7284(8) 0.1022(10) Uani 0.644(5) 1 d PD A 1
H5 H 0.2237 0.3274 0.7864 0.123 Uiso 0.64 1 calc P A 1
C6 C 0.0673(10) 0.3323(11) 0.7302(9) 0.1022(10) Uani 0.644(5) 1 d PD A 1
H6A H 0.0276 0.3534 0.6776 0.123 Uiso 0.64 1 calc P A 1
H6B H 0.0302 0.2566 0.7150 0.123 Uiso 0.64 1 calc P A 1
C7 C 0.0671(10) 0.4049(9) 0.8348(8) 0.1022(10) Uani 0.644(5) 1 d PD A 1
H7A H -0.0076 0.4003 0.8312 0.123 Uiso 0.64 1 calc P A 1
H7B H 0.0977 0.3771 0.8856 0.123 Uiso 0.64 1 calc P A 1
C8 C 0.1923(12) 0.2628(10) 0.6328(13) 0.1022(10) Uani 0.644(5) 1 d PD A 1
C9 C 0.1257(6) 0.3123(5) 0.4719(5) 0.0800(17) Uani 1 1 d . A .
C10 C 0.1439(11) 0.5938(9) 0.9809(8) 0.1022(10) Uani 0.644(5) 1 d PD A 1
H10A H 0.1856 0.6680 0.9989 0.153 Uiso 0.64 1 calc P A 1
H10B H 0.1807 0.5643 1.0265 0.153 Uiso 0.64 1 calc P A 1
H10C H 0.0732 0.5923 0.9861 0.153 Uiso 0.64 1 calc P A 1
C11 C 0.3119(10) 0.2633(10) 0.6455(9) 0.1022(10) Uani 0.644(5) 1 d PD A 1
H11A H 0.3140 0.2110 0.5845 0.153 Uiso 0.64 1 calc P A 1
H11B H 0.3407 0.2442 0.7027 0.153 Uiso 0.64 1 calc P A 1
H11C H 0.3550 0.3349 0.6573 0.153 Uiso 0.64 1 calc P A 1
C12 C 0.1220(11) 0.1456(9) 0.6000(9) 0.1022(10) Uani 0.644(5) 1 d PD A 1
H12A H 0.1303 0.0998 0.5390 0.153 Uiso 0.64 1 calc P A 1
H12B H 0.0471 0.1435 0.5868 0.153 Uiso 0.64 1 calc P A 1
H12C H 0.1445 0.1195 0.6535 0.153 Uiso 0.64 1 calc P A 1
C13 C 0.0827(6) 0.7518(5) 0.6672(5) 0.0784(17) Uani 1 1 d . . .
C14 C 0.2668(18) 0.8731(14) 0.6851(10) 0.0966(9) Uani 0.602(5) 1 d PD B 1
C20 C 0.3491(15) 0.6486(16) 0.4382(9) 0.0966(9) Uani 0.602(5) 1 d PD B 1
C15 C 0.2507(11) 0.8869(9) 0.5830(8) 0.0966(9) Uani 0.602(5) 1 d PD B 1
H15A H 0.3120 0.9449 0.5907 0.116 Uiso 0.60 1 calc P B 1
H15B H 0.1855 0.9089 0.5651 0.116 Uiso 0.60 1 calc P B 1
C16 C 0.2402(15) 0.7817(15) 0.4956(9) 0.0966(9) Uani 0.602(5) 1 d PD B 1
H16A H 0.1741 0.7257 0.4819 0.116 Uiso 0.60 1 calc P B 1
H16B H 0.2352 0.7961 0.4339 0.116 Uiso 0.60 1 calc P B 1
C17 C 0.3387(10) 0.7410(9) 0.5241(8) 0.0966(9) Uani 0.602(5) 1 d PD B 1
H17 H 0.4035 0.8033 0.5463 0.116 Uiso 0.60 1 calc P B 1
C18 C 0.3400(13) 0.7122(10) 0.6186(9) 0.0966(9) Uani 0.602(5) 1 d PD B 1
H18A H 0.3995 0.6824 0.6363 0.116 Uiso 0.60 1 calc P B 1
H18B H 0.2722 0.6577 0.6037 0.116 Uiso 0.60 1 calc P B 1
C19 C 0.3545(10) 0.8187(9) 0.7090(8) 0.0966(9) Uani 0.602(5) 1 d PD B 1
H19A H 0.3534 0.8013 0.7683 0.116 Uiso 0.60 1 calc P B 1
H19B H 0.4251 0.8700 0.7264 0.116 Uiso 0.60 1 calc P B 1
C21 C 0.1899(6) 0.4711(5) 0.3875(5) 0.0794(16) Uani 1 1 d . B .
C22 C 0.2883(11) 0.9846(9) 0.7712(9) 0.0966(9) Uani 0.602(5) 1 d PD B 1
H22A H 0.2309 1.0155 0.7525 0.145 Uiso 0.60 1 calc P B 1
H22B H 0.3566 1.0333 0.7809 0.145 Uiso 0.60 1 calc P B 1
H22C H 0.2908 0.9742 0.8335 0.145 Uiso 0.60 1 calc P B 1
C23 C 0.3353(11) 0.6688(10) 0.3387(9) 0.0966(9) Uani 0.602(5) 1 d PD B 1
H23A H 0.3420 0.6075 0.2879 0.145 Uiso 0.60 1 calc P B 1
H23B H 0.3906 0.7338 0.3514 0.145 Uiso 0.60 1 calc P B 1
H23C H 0.2648 0.6777 0.3145 0.145 Uiso 0.60 1 calc P B 1
C24 C 0.4565(10) 0.6226(10) 0.4718(10) 0.0966(9) Uani 0.602(5) 1 d PD B 1
H24A H 0.4607 0.5649 0.4157 0.145 Uiso 0.60 1 calc P B 1
H24B H 0.4595 0.5997 0.5280 0.145 Uiso 0.60 1 calc P B 1
H24C H 0.5166 0.6867 0.4927 0.145 Uiso 0.60 1 calc P B 1
C25 C 0.3340(5) 0.0430(5) 0.2363(5) 0.0750(15) Uani 1 1 d . . .
C26 C 0.2919(6) 0.1300(5) 0.2754(5) 0.0790(16) Uani 1 1 d . . .
H26 H 0.2903 0.1484 0.3416 0.095 Uiso 1 1 calc . . .
C27 C 0.2541(6) 0.1872(5) 0.2203(5) 0.0794(16) Uani 1 1 d . . .
H27 H 0.2284 0.2443 0.2495 0.095 Uiso 1 1 calc . . .
C28 C 0.2534(5) 0.1605(5) 0.1180(5) 0.0764(16) Uani 1 1 d . . .
C29 C 0.2961(6) 0.0723(5) 0.0778(5) 0.0814(17) Uani 1 1 d . . .
H29 H 0.2969 0.0534 0.0112 0.098 Uiso 1 1 calc . . .
C30 C 0.3350(6) 0.0166(5) 0.1332(5) 0.0854(18) Uani 1 1 d . . .
H30 H 0.3626 -0.0392 0.1049 0.103 Uiso 1 1 calc . . .
C31 C 0.3741(6) -0.0139(5) 0.2937(5) 0.0845(17) Uani 1 1 d . . .
C32 C 0.4190(7) -0.0998(6) 0.2563(6) 0.096(2) Uani 1 1 d . . .
C33 C 0.3762(7) 0.0117(6) 0.3948(7) 0.096(2) Uani 1 1 d . . .
C34 C 0.2179(5) 0.2207(5) 0.0606(5) 0.0797(16) Uani 1 1 d . . .
C35 C 0.1805(6) 0.3120(6) 0.1023(5) 0.091(2) Uani 1 1 d . . .
C36 C 0.2173(6) 0.1991(6) -0.0407(6) 0.090(2) Uani 1 1 d . . .
C37 C 0.0307(6) 0.9700(5) 1.0862(5) 0.0820(17) Uani 1 1 d . . .
C38 C 0.0431(6) 0.9139(5) 0.9938(5) 0.0850(18) Uani 1 1 d . . .
H38 H 0.0718 0.8555 0.9886 0.102 Uiso 1 1 calc . . .
C39 C 0.0149(6) 0.9415(5) 0.9118(5) 0.0832(17) Uani 1 1 d . . .
H39 H 0.0254 0.9021 0.8522 0.100 Uiso 1 1 calc . . .
C40 C 0.0597(6) 0.9419(5) 1.1716(5) 0.0822(17) Uani 1 1 d . . .
C41 C 0.1051(6) 0.8560(6) 1.1724(6) 0.093(2) Uani 1 1 d . . .
C42 C 0.0441(6) 1.0017(6) 1.2651(6) 0.093(2) Uani 1 1 d . . .
C43 C 0.5105(6) 0.5803(6) 0.9567(5) 0.0851(18) Uani 1 1 d . . .
C44 C 0.5203(6) 0.4749(6) 0.9086(5) 0.0859(18) Uani 1 1 d . . .
H44 H 0.5350 0.4583 0.8477 0.103 Uiso 1 1 calc . . .
C45 C 0.4913(6) 0.6020(6) 1.0497(5) 0.0847(18) Uani 1 1 d . . .
H45 H 0.4864 0.6708 1.0840 0.102 Uiso 1 1 calc . . .
C46 C 0.5134(6) 0.6577(6) 0.9100(5) 0.0903(19) Uani 1 1 d . . .
C47 C 0.5238(6) 0.6319(6) 0.8127(7) 0.095(2) Uani 1 1 d . . .
C48 C 0.4942(7) 0.7582(7) 0.9532(6) 0.102(2) 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 0.0181 0.0091 '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'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd C13 88.9(3) 2_566 2_566 ?
C1 Pd C21 88.8(3) 2_566 . ?
C13 Pd C21 176.5(2) 2_566 . ?
C1 Pd C9 176.7(3) 2_566 . ?
C13 Pd C9 88.8(3) 2_566 . ?
C21 Pd C9 93.4(3) . . ?
C1 N1 C2 179.4(9) . . ?
C9 N2 C8 174.4(8) . . ?
C13 N3 C14 176.8(8) . . ?
C21 N4 C20 178.3(8) . . ?
N1 C1 Pd 171.4(6) . 2_566 ?
N1 C2 C7 106.1(11) . . ?
N1 C2 C3 107.4(12) . . ?
C7 C2 C3 112.3(11) . . ?
N1 C2 C10 108.1(11) . . ?
C7 C2 C10 112.7(12) . . ?
C3 C2 C10 109.9(11) . . ?
C4 C3 C2 112.6(10) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 109.6(11) . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C8 C5 C4 113.4(9) . . ?
C8 C5 C6 115.0(9) . . ?
C4 C5 C6 106.9(9) . . ?
C8 C5 H5 107.0 . . ?
C4 C5 H5 107.0 . . ?
C6 C5 H5 107.0 . . ?
C7 C6 C5 111.6(9) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C2 C7 C6 113.1(10) . . ?
C2 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C2 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C5 C8 C12 113.7(11) . . ?
C5 C8 N2 112.4(11) . . ?
C12 C8 N2 106.3(11) . . ?
C5 C8 C11 111.6(11) . . ?
C12 C8 C11 108.8(11) . . ?
N2 C8 C11 103.4(10) . . ?
N2 C9 Pd 171.7(6) . . ?
C2 C10 H10A 109.5 . . ?
C2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 Pd 171.4(6) . 2_566 ?
N3 C14 C19 108.3(12) . . ?
N3 C14 C15 106.3(12) . . ?
C19 C14 C15 112.3(12) . . ?
N3 C14 C22 107.1(11) . . ?
C19 C14 C22 112.7(12) . . ?
C15 C14 C22 109.8(11) . . ?
N4 C20 C17 109.4(12) . . ?
N4 C20 C24 107.3(12) . . ?
C17 C20 C24 111.8(11) . . ?
N4 C20 C23 103.9(11) . . ?
C17 C20 C23 113.8(11) . . ?
C24 C20 C23 110.1(12) . . ?
C14 C15 C16 112.8(10) . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C15 110.4(10) . . ?
C17 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
C17 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
C20 C17 C16 116.1(9) . . ?
C20 C17 C18 112.3(9) . . ?
C16 C17 C18 108.2(10) . . ?
C20 C17 H17 106.6 . . ?
C16 C17 H17 106.6 . . ?
C18 C17 H17 106.6 . . ?
C17 C18 C19 108.2(9) . . ?
C17 C18 H18A 110.1 . . ?
C19 C18 H18A 110.1 . . ?
C17 C18 H18B 110.1 . . ?
C19 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
C14 C19 C18 113.1(10) . . ?
C14 C19 H19A 109.0 . . ?
C18 C19 H19A 108.9 . . ?
C14 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.8 . . ?
N4 C21 Pd 170.0(6) . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C24 H24A 109.5 . . ?
C20 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C20 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C31 C25 C26 122.4(6) . . ?
C31 C25 C30 120.6(6) . . ?
C26 C25 C30 117.0(6) . . ?
C27 C26 C25 122.8(6) . . ?
C27 C26 H26 118.6 . . ?
C25 C26 H26 118.6 . . ?
C26 C27 C28 120.5(6) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C34 C28 C27 121.5(6) . . ?
C34 C28 C29 121.3(6) . . ?
C27 C28 C29 117.1(5) . . ?
C30 C29 C28 122.3(6) . . ?
C30 C29 H29 118.9 . . ?
C28 C29 H29 118.9 . . ?
C29 C30 C25 120.4(6) . . ?
C29 C30 H30 119.8 . . ?
C25 C30 H30 119.8 . . ?
C25 C31 C33 121.7(6) . . ?
C25 C31 C32 123.1(7) . . ?
C33 C31 C32 115.2(6) . . ?
N5 C32 C31 179.0(9) . . ?
N6 C33 C31 178.9(8) . . ?
C28 C34 C36 123.9(6) . . ?
C28 C34 C35 121.5(6) . . ?
C36 C34 C35 114.6(6) . . ?
N8 C35 C34 178.6(8) . . ?
N7 C36 C34 177.2(8) . . ?
C38 C37 C40 122.6(6) . . ?
C38 C37 C39 115.8(6) . 2_577 ?
C40 C37 C39 121.7(6) . 2_577 ?
C39 C38 C37 122.2(6) . . ?
C39 C38 H38 118.9 . . ?
C37 C38 H38 118.9 . . ?
C38 C39 C37 122.0(6) . 2_577 ?
C38 C39 H39 119.0 . . ?
C37 C39 H39 119.0 2_577 . ?
C37 C40 C41 123.2(7) . . ?
C37 C40 C42 120.5(6) . . ?
C41 C40 C42 116.4(6) . . ?
N9 C41 C40 177.0(9) . . ?
N10 C42 C40 179.3(8) . . ?
C45 C43 C46 121.2(6) . . ?
C45 C43 C44 117.0(6) . . ?
C46 C43 C44 121.7(7) . . ?
C45 C44 C43 121.2(7) 2_667 . ?
C45 C44 H44 119.4 2_667 . ?
C43 C44 H44 119.4 . . ?
C44 C45 C43 121.8(6) 2_667 . ?
C44 C45 H45 119.1 2_667 . ?
C43 C45 H45 119.1 . . ?
C47 C46 C48 117.1(7) . . ?
C47 C46 C43 120.9(7) . . ?
C48 C46 C43 121.7(7) . . ?
N12 C47 C46 177.8(9) . . ?
N11 C48 C46 177.5(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd C1 1.968(7) 2_566 ?
Pd C13 1.970(8) 2_566 ?
Pd C21 1.982(8) . ?
Pd C9 1.985(6) . ?
N1 C1 1.130(8) . ?
N1 C2 1.47(2) . ?
N2 C9 1.129(8) . ?
N2 C8 1.51(2) . ?
N3 C13 1.128(9) . ?
N3 C14 1.44(3) . ?
N4 C21 1.121(9) . ?
N4 C20 1.50(2) . ?
N5 C32 1.146(9) . ?
N6 C33 1.148(10) . ?
N7 C36 1.135(9) . ?
N8 C35 1.131(9) . ?
N9 C41 1.155(9) . ?
N10 C42 1.157(10) . ?
N11 C48 1.152(10) . ?
N12 C47 1.148(10) . ?
C1 Pd 1.968(7) 2_566 ?
C2 C7 1.518(14) . ?
C2 C3 1.538(15) . ?
C2 C10 1.559(13) . ?
C3 C4 1.538(14) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.553(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9699 . ?
C5 C8 1.519(13) . ?
C5 C6 1.543(13) . ?
C5 H5 0.9800 . ?
C6 C7 1.539(12) . ?
C6 H6A 0.9701 . ?
C6 H6B 0.9699 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C12 1.525(14) . ?
C8 C11 1.554(15) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 Pd 1.970(8) 2_566 ?
C14 C19 1.519(15) . ?
C14 C15 1.531(14) . ?
C14 C22 1.547(14) . ?
C20 C17 1.526(13) . ?
C20 C24 1.535(14) . ?
C20 C23 1.538(14) . ?
C15 C16 1.538(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.530(13) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.547(13) . ?
C17 H17 0.9800 . ?
C18 C19 1.558(13) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C31 1.384(9) . ?
C25 C26 1.420(9) . ?
C25 C30 1.442(9) . ?
C26 C27 1.355(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.423(9) . ?
C27 H27 0.9300 . ?
C28 C34 1.401(8) . ?
C28 C29 1.443(9) . ?
C29 C30 1.346(9) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 C33 1.403(11) . ?
C31 C32 1.428(10) . ?
C34 C36 1.418(10) . ?
C34 C35 1.434(10) . ?
C37 C38 1.397(10) . ?
C37 C40 1.402(9) . ?
C37 C39 1.436(9) 2_577 ?
C38 C39 1.353(9) . ?
C38 H38 0.9300 . ?
C39 C37 1.436(9) 2_577 ?
C39 H39 0.9300 . ?
C40 C41 1.409(9) . ?
C40 C42 1.445(11) . ?
C43 C45 1.401(10) . ?
C43 C46 1.416(10) . ?
C43 C44 1.424(10) . ?
C44 C45 1.362(10) 2_667 ?
C44 H44 0.9300 . ?
C45 C44 1.362(10) 2_667 ?
C45 H45 0.9300 . ?
C46 C47 1.407(12) . ?
C46 C48 1.409(11) . ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 Pd 63(87) . . . 2_566 ?
C1 N1 C2 C7 -133(85) . . . . ?
C1 N1 C2 C3 -12(86) . . . . ?
C1 N1 C2 C10 106(85) . . . . ?
N1 C2 C3 C4 -66.5(13) . . . . ?
C7 C2 C3 C4 49.8(18) . . . . ?
C10 C2 C3 C4 176.1(13) . . . . ?
C2 C3 C4 C5 -58.0(17) . . . . ?
C3 C4 C5 C8 -170.1(12) . . . . ?
C3 C4 C5 C6 62.1(15) . . . . ?
C8 C5 C6 C7 172.5(11) . . . . ?
C4 C5 C6 C7 -60.7(13) . . . . ?
N1 C2 C7 C6 69.7(12) . . . . ?
C3 C2 C7 C6 -47.4(18) . . . . ?
C10 C2 C7 C6 -172.2(12) . . . . ?
C5 C6 C7 C2 54.5(16) . . . . ?
C4 C5 C8 C12 -169.1(14) . . . . ?
C6 C5 C8 C12 -45.7(18) . . . . ?
C4 C5 C8 N2 -48.3(15) . . . . ?
C6 C5 C8 N2 75.1(13) . . . . ?
C4 C5 C8 C11 67.3(17) . . . . ?
C6 C5 C8 C11 -169.2(11) . . . . ?
C9 N2 C8 C5 -94(7) . . . . ?
C9 N2 C8 C12 31(8) . . . . ?
C9 N2 C8 C11 146(7) . . . . ?
C8 N2 C9 Pd 71(9) . . . . ?
C1 Pd C9 N2 -26(8) 2_566 . . . ?
C13 Pd C9 N2 -74(4) 2_566 . . . ?
C21 Pd C9 N2 104(4) . . . . ?
C14 N3 C13 Pd 144(12) . . . 2_566 ?
C13 N3 C14 C19 168(14) . . . . ?
C13 N3 C14 C15 -71(14) . . . . ?
C13 N3 C14 C22 46(15) . . . . ?
C21 N4 C20 C17 -24(28) . . . . ?
C21 N4 C20 C24 97(27) . . . . ?
C21 N4 C20 C23 -146(27) . . . . ?
N3 C14 C15 C16 -70.2(14) . . . . ?
C19 C14 C15 C16 48(2) . . . . ?
C22 C14 C15 C16 174.3(14) . . . . ?
C14 C15 C16 C17 -55(2) . . . . ?
N4 C20 C17 C16 -67.4(15) . . . . ?
C24 C20 C17 C16 173.8(15) . . . . ?
C23 C20 C17 C16 48(2) . . . . ?
N4 C20 C17 C18 57.8(13) . . . . ?
C24 C20 C17 C18 -61.0(18) . . . . ?
C23 C20 C17 C18 173.5(13) . . . . ?
C15 C16 C17 C20 -170.1(14) . . . . ?
C15 C16 C17 C18 62.7(17) . . . . ?
C20 C17 C18 C19 167.9(12) . . . . ?
C16 C17 C18 C19 -62.7(14) . . . . ?
N3 C14 C19 C18 67.4(13) . . . . ?
C15 C14 C19 C18 -49.6(19) . . . . ?
C22 C14 C19 C18 -174.3(13) . . . . ?
C17 C18 C19 C14 57.1(16) . . . . ?
C20 N4 C21 Pd 52(29) . . . . ?
C1 Pd C21 N4 67(4) 2_566 . . . ?
C13 Pd C21 N4 19(7) 2_566 . . . ?
C9 Pd C21 N4 -110(4) . . . . ?
C31 C25 C26 C27 179.0(7) . . . . ?
C30 C25 C26 C27 -0.2(10) . . . . ?
C25 C26 C27 C28 1.1(11) . . . . ?
C26 C27 C28 C34 -177.9(7) . . . . ?
C26 C27 C28 C29 -1.1(10) . . . . ?
C34 C28 C29 C30 177.1(7) . . . . ?
C27 C28 C29 C30 0.2(10) . . . . ?
C28 C29 C30 C25 0.7(11) . . . . ?
C31 C25 C30 C29 -179.9(7) . . . . ?
C26 C25 C30 C29 -0.7(10) . . . . ?
C26 C25 C31 C33 -0.5(11) . . . . ?
C30 C25 C31 C33 178.6(7) . . . . ?
C26 C25 C31 C32 -178.5(7) . . . . ?
C30 C25 C31 C32 0.6(11) . . . . ?
C25 C31 C32 N5 148(60) . . . . ?
C33 C31 C32 N5 -30(61) . . . . ?
C25 C31 C33 N6 -19(58) . . . . ?
C32 C31 C33 N6 159(57) . . . . ?
C27 C28 C34 C36 178.8(7) . . . . ?
C29 C28 C34 C36 2.1(11) . . . . ?
C27 C28 C34 C35 -0.1(10) . . . . ?
C29 C28 C34 C35 -176.8(7) . . . . ?
C28 C34 C35 N8 162(38) . . . . ?
C36 C34 C35 N8 -17(38) . . . . ?
C28 C34 C36 N7 173(20) . . . . ?
C35 C34 C36 N7 -8(20) . . . . ?
C40 C37 C38 C39 -180.0(7) . . . . ?
C39 C37 C38 C39 0.5(12) 2_577 . . . ?
C37 C38 C39 C37 -0.6(12) . . . 2_577 ?
C38 C37 C40 C41 0.8(11) . . . . ?
C39 C37 C40 C41 -179.7(7) 2_577 . . . ?
C38 C37 C40 C42 -179.3(7) . . . . ?
C39 C37 C40 C42 0.2(11) 2_577 . . . ?
C37 C40 C41 N9 157(17) . . . . ?
C42 C40 C41 N9 -23(18) . . . . ?
C37 C40 C42 N10 -2(87) . . . . ?
C41 C40 C42 N10 178(100) . . . . ?
C45 C43 C44 C45 1.7(11) . . . 2_667 ?
C46 C43 C44 C45 -174.7(7) . . . 2_667 ?
C46 C43 C45 C44 174.7(7) . . . 2_667 ?
C44 C43 C45 C44 -1.7(12) . . . 2_667 ?
C45 C43 C46 C47 -174.7(7) . . . . ?
C44 C43 C46 C47 1.5(11) . . . . ?
C45 C43 C46 C48 -1.8(11) . . . . ?
C44 C43 C46 C48 174.4(7) . . . . ?
C48 C46 C47 N12 177(100) . . . . ?
C43 C46 C47 N12 -9(25) . . . . ?
C47 C46 C48 N11 146(22) . . . . ?
C43 C46 C48 N11 -27(23) . . . . ?
