#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/37/4303724.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_4303724
loop_
_publ_author_name
'Arun Kumar Bar'
'Rajesh Chakrabarty'
'Partha Sarathi Mukherjee'
_publ_section_title
;
Self-Assembly of a Pd6-Molecular Double-Square and a
Cu3-Trigonalbipyramidal Cage via a New Tripodal Flexible Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10880
_journal_page_last               10882
_journal_paper_doi               10.1021/ic901633g
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C144 H240 N36 Pd6, 8(Cl O4), 4(N O3)'
_chemical_formula_sum            'C144 H240 Cl8 N40 O44 Pd6'
_chemical_formula_weight         4157.83
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.75(3)
_cell_angle_beta                 101.71(3)
_cell_angle_gamma                93.90(3)
_cell_formula_units_Z            6
_cell_length_a                   16.057(3)
_cell_length_b                   18.914(4)
_cell_length_c                   22.570(5)
_cell_measurement_temperature    150(2)
_cell_volume                     6405(3)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BR5UKER SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows(Farrugia, 1997)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.818
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15500
_diffrn_reflns_theta_full        23.51
_diffrn_reflns_theta_max         23.51
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.9313
_exptl_absorpt_correction_T_min  0.9066
_exptl_absorpt_correction_type   emperical
_exptl_absorpt_process_details
'SADABS: Blessing, R. (1995), Acta Cryst., A51, 33'
_exptl_crystal_colour            'color less'
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent
contributions.  Total electron count found = 472/unit cell.
Calculated for 15 nitromethane (the reaction solvent)
= 480/unit cell.  The intensive properties (density, F(000), etc.)
reflect these contributions
;
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.435
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1061
_refine_ls_number_reflns         15500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.435
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.391
_refine_ls_shift/su_mean         0.076
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3021
_refine_ls_wR_factor_ref         0.3147
_reflns_number_gt                12801
_reflns_number_total             9344
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic901633g_si_002.cif
_cod_data_source_block           complex-1
_cod_original_cell_volume        6404(2)
_cod_original_formula_sum        'C144 H240 N40 O44 Cl8 Pd6'
_cod_database_code               4303724
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
Pd1 Pd 1.02039(3) 0.38498(3) 1.21138(2) 0.0855(3) Uani 1 1 d . . .
Pd3 Pd 1.47553(3) 0.18016(3) 1.27503(2) 0.0916(3) Uani 1 1 d . . .
Pd2 Pd 0.98289(3) 0.02728(3) 0.67974(2) 0.0895(3) Uani 1 1 d . . .
N1 N 1.0961(4) 0.4407(4) 1.3007(3) 0.0997(17) Uani 1 1 d . . .
N2 N 0.9419(4) 0.3482(4) 1.2583(3) 0.1019(17) Uani 1 1 d . . .
N3 N 0.9415(4) 0.3344(4) 1.1256(3) 0.0949(16) Uani 1 1 d . . .
N4 N 0.8761(4) 0.3660(4) 1.1003(3) 0.1007(17) Uani 1 1 d . . .
H4 H 0.8636 0.4087 1.1188 0.121 Uiso 1 1 calc R . .
N5 N 0.9071(4) 0.1092(4) 0.6909(3) 0.0993(17) Uani 1 1 d . . .
N6 N 0.9313(5) 0.1748(4) 0.6826(3) 0.1060(18) Uani 1 1 d . . .
H6 H 0.9719 0.1816 0.6643 0.127 Uiso 1 1 calc R . .
N7 N 0.9064(4) -0.0308(4) 0.5925(3) 0.1018(18) Uani 1 1 d . . .
N8 N 1.0586(4) -0.0575(4) 0.6670(3) 0.1044(18) Uani 1 1 d . . .
N9 N 1.0629(5) 0.0855(4) 0.7613(3) 0.1034(18) Uani 1 1 d . . .
N10 N 1.1285(4) 0.1358(4) 0.7634(3) 0.0961(16) Uani 1 1 d . . .
H10 H 1.1423 0.1437 0.7306 0.115 Uiso 1 1 calc R . .
N11 N 1.4566(5) 0.1549(5) 1.3561(3) 0.117(2) Uani 1 1 d . . .
N12 N 1.5758(4) 0.0540(4) 1.2441(3) 0.1025(17) Uani 1 1 d . . .
H12 H 1.6213 0.0838 1.2659 0.123 Uiso 1 1 calc R . .
N13 N 1.0746(4) 0.4811(3) 1.1411(3) 0.0930(15) Uani 1 1 d . . .
H13 H 1.0354 0.5078 1.1511 0.112 Uiso 1 1 calc R . .
N14 N 1.0979(4) 0.4264(3) 1.1648(3) 0.0882(14) Uani 1 1 d . . .
N15 N 1.5762(4) 0.2367(4) 1.1986(3) 0.1014(18) Uani 1 1 d . . .
H15 H 1.6209 0.2426 1.2287 0.122 Uiso 1 1 calc R . .
N16 N 1.4967(4) 0.2099(3) 1.1986(3) 0.0899(15) Uani 1 1 d . . .
N17 N 1.4932(4) 0.0739(4) 1.2334(3) 0.0973(17) Uani 1 1 d . . .
N19 N 1.4578(4) 0.2871(4) 1.3207(3) 0.113(2) Uani 1 1 d . . .
N22 N 0.7443(2) 0.2211(3) 1.3315(3) 0.0720(13) Uani 1 1 d . . .
N23 N 1.1451(5) 0.1716(4) 0.6154(3) 0.108(2) Uani 1 1 d . . .
C1 C 1.5272(7) 0.1162(7) 1.3816(5) 0.144(4) Uani 1 1 d . . .
H1A H 1.5811 0.1470 1.3910 0.217 Uiso 1 1 calc R . .
H1B H 1.5283 0.0703 1.3506 0.217 Uiso 1 1 calc R . .
H1C H 1.5177 0.1066 1.4194 0.217 Uiso 1 1 calc R . .
C2 C 0.8901(5) 0.2480(5) 0.8772(4) 0.113(2) Uani 1 1 d . . .
H2A H 0.9235 0.2484 0.9177 0.169 Uiso 1 1 calc R . .
H2B H 0.8908 0.2977 0.8743 0.169 Uiso 1 1 calc R . .
H2C H 0.9140 0.2187 0.8444 0.169 Uiso 1 1 calc R . .
C3 C 1.4642(5) 0.2492(6) 1.0439(3) 0.107(2) Uani 1 1 d . . .
H3A H 1.4702 0.2044 1.0126 0.128 Uiso 1 1 calc R . .
H3B H 1.5029 0.2892 1.0411 0.128 Uiso 1 1 calc R . .
C4 C 1.4919(5) 0.2388(5) 1.1082(4) 0.098(2) Uani 1 1 d . . .
C5 C 0.8274(5) 0.1949(4) 0.7308(3) 0.0956(19) Uani 1 1 d . . .
C6 C 1.3520(5) 0.1808(6) 1.1303(4) 0.110(2) Uani 1 1 d . . .
H6A H 1.3401 0.1646 1.1649 0.165 Uiso 1 1 calc R . .
H6B H 1.3379 0.1398 1.0924 0.165 Uiso 1 1 calc R . .
H6C H 1.3182 0.2194 1.1245 0.165 Uiso 1 1 calc R . .
C7 C 0.8699(5) 0.2605(4) 1.0311(3) 0.0907(18) Uani 1 1 d . . .
C8 C 1.1525(5) 0.1626(4) 0.9340(3) 0.097(2) Uani 1 1 d . . .
H8A H 1.1004 0.1742 0.9479 0.116 Uiso 1 1 calc R . .
H8B H 1.1673 0.1178 0.9443 0.116 Uiso 1 1 calc R . .
C9 C 1.3706(5) 0.2670(5) 1.0267(4) 0.098(2) Uani 1 1 d . . .
C10 C 1.2440(5) 0.2350(5) 0.8360(4) 0.105(2) Uani 1 1 d . . .
H10A H 1.2531 0.2382 0.7960 0.158 Uiso 1 1 calc R . .
H10B H 1.2956 0.2244 0.8601 0.158 Uiso 1 1 calc R . .
H10C H 1.2292 0.2814 0.8588 0.158 Uiso 1 1 calc R . .
C11 C 1.2043(5) 0.3365(4) 1.1548(4) 0.0947(19) Uani 1 1 d . . .
H11A H 1.1783 0.3204 1.1844 0.142 Uiso 1 1 calc R . .
H11B H 1.2642 0.3530 1.1732 0.142 Uiso 1 1 calc R . .
H11C H 1.1978 0.2961 1.1170 0.142 Uiso 1 1 calc R . .
C12 C 1.2446(5) 0.4304(4) 1.0569(4) 0.099(2) Uani 1 1 d . . .
H12A H 1.2231 0.4467 1.0201 0.119 Uiso 1 1 calc R . .
H12B H 1.2967 0.4630 1.0810 0.119 Uiso 1 1 calc R . .
C13 C 0.8324(5) 0.3231(4) 1.0426(4) 0.097(2) Uani 1 1 d . . .
C14 C 1.3486(5) 0.3366(5) 1.0509(3) 0.096(2) Uani 1 1 d . . .
C15 C 0.7555(5) 0.3483(5) 1.0081(4) 0.106(2) Uani 1 1 d . . .
H15A H 0.7490 0.3973 1.0317 0.158 Uiso 1 1 calc R . .
H15B H 0.7051 0.3150 1.0034 0.158 Uiso 1 1 calc R . .
H15C H 0.7631 0.3488 0.9671 0.158 Uiso 1 1 calc R . .
C16 C 1.4445(4) 0.2094(4) 1.1443(3) 0.0895(18) Uani 1 1 d . . .
C17 C 0.8442(5) 0.1216(4) 0.7220(4) 0.097(2) Uani 1 1 d . . .
C18 C 0.8506(6) 0.1913(5) 0.9741(3) 0.104(2) Uani 1 1 d . . .
H18A H 0.8362 0.1491 0.9885 0.125 Uiso 1 1 calc R . .
H18B H 0.9027 0.1838 0.9591 0.125 Uiso 1 1 calc R . .
C19 C 1.1095(7) 0.5513(5) 1.0684(4) 0.117(3) Uani 1 1 d . . .
H19A H 1.0622 0.5759 1.0799 0.175 Uiso 1 1 calc R . .
H19B H 1.0979 0.5310 1.0233 0.175 Uiso 1 1 calc R . .
H19C H 1.1608 0.5862 1.0828 0.175 Uiso 1 1 calc R . .
C20 C 0.5849(6) 0.1636(5) 0.7471(4) 0.117(3) Uani 1 1 d . . .
H20A H 0.6104 0.1794 0.7171 0.175 Uiso 1 1 calc R . .
H20B H 0.5389 0.1918 0.7556 0.175 Uiso 1 1 calc R . .
H20C H 0.5629 0.1119 0.7301 0.175 Uiso 1 1 calc R . .
C21 C 1.3750(6) 0.1077(6) 1.3419(5) 0.127(3) Uani 1 1 d . . .
H21A H 1.3293 0.1320 1.3251 0.190 Uiso 1 1 calc R . .
H21B H 1.3655 0.0984 1.3799 0.190 Uiso 1 1 calc R . .
H21C H 1.3766 0.0615 1.3113 0.190 Uiso 1 1 calc R . .
C22 C 0.8041(5) 0.0638(5) 0.7417(4) 0.106(2) Uani 1 1 d . . .
H22A H 0.8294 0.0193 0.7288 0.160 Uiso 1 1 calc R . .
H22B H 0.7438 0.0547 0.7225 0.160 Uiso 1 1 calc R . .
H22C H 0.8124 0.0791 0.7869 0.160 Uiso 1 1 calc R . .
C23 C 1.6571(5) 0.2878(6) 1.1319(5) 0.120(3) Uani 1 1 d . . .
H23A H 1.7040 0.2901 1.1666 0.180 Uiso 1 1 calc R . .
H23B H 1.6505 0.3370 1.1291 0.180 Uiso 1 1 calc R . .
H23C H 1.6685 0.2582 1.0932 0.180 Uiso 1 1 calc R . .
C24 C 1.2229(4) 0.2244(4) 0.9712(3) 0.0846(17) Uani 1 1 d . . .
C25 C 1.0031(6) 0.0431(5) 0.8391(4) 0.109(2) Uani 1 1 d . . .
H25A H 0.9661 0.0110 0.8010 0.164 Uiso 1 1 calc R . .
H25B H 0.9695 0.0732 0.8640 0.164 Uiso 1 1 calc R . .
H25C H 1.0331 0.0138 0.8630 0.164 Uiso 1 1 calc R . .
C26 C 1.0729(8) -0.0891(6) 0.7231(5) 0.141(4) Uani 1 1 d . . .
H26A H 1.0185 -0.1057 0.7295 0.212 Uiso 1 1 calc R . .
H26B H 1.1040 -0.0514 0.7604 0.212 Uiso 1 1 calc R . .
H26C H 1.1052 -0.1301 0.7148 0.212 Uiso 1 1 calc R . .
C27 C 1.1334(4) 0.1466(4) 0.8631(3) 0.0863(18) Uani 1 1 d . . .
C28 C 1.3492(5) 0.0186(5) 1.1749(5) 0.115(3) Uani 1 1 d . . .
H28A H 1.3370 0.0681 1.1916 0.173 Uiso 1 1 calc R . .
H28B H 1.3161 -0.0150 1.1891 0.173 Uiso 1 1 calc R . .
H28C H 1.3345 0.0049 1.1295 0.173 Uiso 1 1 calc R . .
C29 C 0.6526(5) 0.1759(5) 0.8087(4) 0.099(2) Uani 1 1 d . . .
C30 C 0.9382(4) 0.2675(4) 1.0818(3) 0.0828(16) Uani 1 1 d . . .
C31 C 0.6706(7) 0.1452(6) 0.9701(4) 0.134(3) Uani 1 1 d . . .
H31A H 0.6106 0.1266 0.9592 0.200 Uiso 1 1 calc R . .
H31B H 0.6819 0.1889 1.0057 0.200 Uiso 1 1 calc R . .
H31C H 0.7036 0.1081 0.9809 0.200 Uiso 1 1 calc R . .
C32 C 1.1613(5) 0.3994(4) 1.1386(3) 0.0869(18) Uani 1 1 d . . .
C33 C 1.1121(5) 0.3134(5) 0.9719(3) 0.103(2) Uani 1 1 d . . .
H33A H 1.1100 0.3652 0.9902 0.154 Uiso 1 1 calc R . .
H33B H 1.0735 0.2847 0.9864 0.154 Uiso 1 1 calc R . .
H33C H 1.0956 0.3014 0.9266 0.154 Uiso 1 1 calc R . .
C34 C 1.0017(5) 0.2189(4) 1.0938(3) 0.098(2) Uani 1 1 d . . .
H34A H 1.0402 0.2416 1.1342 0.147 Uiso 1 1 calc R . .
H34B H 1.0334 0.2105 1.0613 0.147 Uiso 1 1 calc R . .
H34C H 0.9733 0.1725 1.0937 0.147 Uiso 1 1 calc R . .
C35 C 1.5750(5) 0.2533(5) 1.1424(4) 0.098(2) Uani 1 1 d . . .
C36 C 1.1212(6) 0.4890(4) 1.0992(4) 0.099(2) Uani 1 1 d . . .
C37 C 0.8010(5) 0.2157(4) 0.8695(4) 0.0951(19) Uani 1 1 d . . .
C38 C 1.3086(5) 0.2089(4) 0.9850(3) 0.0937(19) Uani 1 1 d . . .
C39 C 0.8863(6) 0.2277(5) 0.7054(4) 0.111(2) Uani 1 1 d . . .
C40 C 1.6535(5) -0.0537(5) 1.2207(4) 0.110(2) Uani 1 1 d . . .
H40A H 1.7015 -0.0176 1.2458 0.165 Uiso 1 1 calc R . .
H40B H 1.6629 -0.0746 1.1792 0.165 Uiso 1 1 calc R . .
H40C H 1.6474 -0.0922 1.2404 0.165 Uiso 1 1 calc R . .
C41 C 0.6951(5) 0.1637(5) 0.9147(4) 0.100(2) Uani 1 1 d . . .
C42 C 1.1701(5) 0.1725(4) 0.8249(3) 0.0907(18) Uani 1 1 d . . .
C43 C 1.3973(7) 0.3199(6) 1.2800(5) 0.134(3) Uani 1 1 d . . .
H43A H 1.3430 0.2889 1.2650 0.201 Uiso 1 1 calc R . .
H43B H 1.4201 0.3235 1.2446 0.201 Uiso 1 1 calc R . .
H43C H 1.3898 0.3684 1.3040 0.201 Uiso 1 1 calc R . .
C44 C 0.7613(5) 0.2336(5) 0.7605(4) 0.104(2) Uani 1 1 d . . .
H44A H 0.7090 0.2265 0.7280 0.125 Uiso 1 1 calc R . .
H44B H 0.7814 0.2863 0.7761 0.125 Uiso 1 1 calc R . .
C45 C 1.2673(5) 0.3535(4) 1.0344(3) 0.0913(19) Uani 1 1 d . . .
C46 C 1.5742(5) -0.0174(5) 1.2157(3) 0.096(2) Uani 1 1 d . . .
C47 C 0.8945(7) 0.0163(6) 0.5507(4) 0.130(3) Uani 1 1 d . . .
H47A H 0.9495 0.0364 0.5478 0.195 Uiso 1 1 calc R . .
H47B H 0.8638 0.0560 0.5674 0.195 Uiso 1 1 calc R . .
H47C H 0.8625 -0.0126 0.5094 0.195 Uiso 1 1 calc R . .
C48 C 1.1785(5) 0.4397(4) 1.0973(3) 0.0928(18) Uani 1 1 d . . .
C49 C 0.7396(5) 0.2083(5) 0.8146(4) 0.106(2) Uani 1 1 d . . .
C50 C 0.7778(5) 0.1909(5) 0.9172(4) 0.100(2) Uani 1 1 d . . .
C51 C 1.0648(5) 0.0904(5) 0.8231(3) 0.096(2) Uani 1 1 d . . .
C52 C 1.4895(5) -0.0481(5) 1.1840(4) 0.101(2) Uani 1 1 d . . .
C53 C 1.1044(6) 0.5200(5) 1.3095(4) 0.115(2) Uani 1 1 d . . .
H53A H 1.0484 0.5354 1.3029 0.173 Uiso 1 1 calc R . .
H53B H 1.1341 0.5314 1.2798 0.173 Uiso 1 1 calc R . .
H53C H 1.1361 0.5455 1.3518 0.173 Uiso 1 1 calc R . .
C54 C 0.6320(5) 0.1564(5) 0.8588(4) 0.102(2) Uani 1 1 d . . .
C55 C 0.9144(9) 0.2632(5) 1.2324(7) 0.167(5) Uani 1 1 d . . .
H55A H 0.9645 0.2382 1.2330 0.250 Uiso 1 1 calc R . .
H55B H 0.8808 0.2511 1.1898 0.250 Uiso 1 1 calc R . .
H55C H 0.8808 0.2476 1.2584 0.250 Uiso 1 1 calc R . .
C56 C 1.2034(5) 0.2959(5) 0.9917(3) 0.0921(19) Uani 1 1 d . . .
C57 C 0.8958(9) 0.3058(5) 0.7001(5) 0.148(4) Uani 1 1 d . . .
H57A H 0.9423 0.3123 0.6805 0.222 Uiso 1 1 calc R . .
H57B H 0.9074 0.3406 0.7416 0.222 Uiso 1 1 calc R . .
H57C H 0.8436 0.3141 0.6750 0.222 Uiso 1 1 calc R . .
C58 C 1.4209(8) 0.2806(7) 1.3742(4) 0.141(3) Uani 1 1 d . . .
H58A H 1.4319 0.3285 1.4060 0.170 Uiso 1 1 calc R . .
H58B H 1.3592 0.2679 1.3592 0.170 Uiso 1 1 calc R . .
C59 C 0.9576(7) -0.0904(6) 0.5666(4) 0.129(3) Uani 1 1 d . . .
H59A H 0.9185 -0.1312 0.5356 0.155 Uiso 1 1 calc R . .
H59B H 0.9956 -0.0709 0.5448 0.155 Uiso 1 1 calc R . .
C60 C 1.4427(5) 0.0150(5) 1.1973(4) 0.096(2) Uani 1 1 d . . .
C61 C 1.3287(7) 0.1338(5) 0.9588(4) 0.123(3) Uani 1 1 d . . .
H61A H 1.3889 0.1324 0.9728 0.185 Uiso 1 1 calc R . .
H61B H 1.3134 0.1205 0.9134 0.185 Uiso 1 1 calc R . .
H61C H 1.2968 0.0994 0.9730 0.185 Uiso 1 1 calc R . .
C62 C 1.0441(10) 0.4242(7) 1.3460(5) 0.160(5) Uani 1 1 d . . .
H62A H 1.0834 0.4257 1.3853 0.192 Uiso 1 1 calc R . .
H62B H 1.0084 0.4632 1.3557 0.192 Uiso 1 1 calc R . .
C63 C 0.9902(8) 0.3539(7) 1.3226(4) 0.139(3) Uani 1 1 d . . .
H63A H 0.9511 0.3511 1.3497 0.167 Uiso 1 1 calc R . .
H63B H 1.0249 0.3138 1.3216 0.167 Uiso 1 1 calc R . .
C64 C 1.4598(6) -0.1279(6) 1.1451(6) 0.127(3) Uani 1 1 d . . .
H64A H 1.4971 -0.1590 1.1628 0.152 Uiso 1 1 calc R . .
H64B H 1.4668 -0.1334 1.1025 0.152 Uiso 1 1 calc R . .
C65 C 0.8643(6) 0.3812(6) 1.2548(5) 0.133(3) Uani 1 1 d . . .
H65A H 0.8373 0.3745 1.2112 0.199 Uiso 1 1 calc R . .
H65B H 0.8772 0.4332 1.2768 0.199 Uiso 1 1 calc R . .
H65C H 0.8264 0.3580 1.2738 0.199 Uiso 1 1 calc R . .
C66 C 0.8221(6) -0.0615(7) 0.5958(4) 0.138(3) Uani 1 1 d . . .
H66A H 0.8288 -0.0933 0.6226 0.206 Uiso 1 1 calc R . .
H66B H 0.7905 -0.0895 0.5541 0.206 Uiso 1 1 calc R . .
H66C H 0.7914 -0.0219 0.6127 0.206 Uiso 1 1 calc R . .
C67 C 1.1419(7) -0.0312(6) 0.6590(7) 0.161(5) Uani 1 1 d . . .
H67A H 1.1701 0.0088 0.6956 0.242 Uiso 1 1 calc R . .
H67B H 1.1340 -0.0141 0.6221 0.242 Uiso 1 1 calc R . .
H67C H 1.1765 -0.0709 0.6540 0.242 Uiso 1 1 calc R . .
C68 C 1.4530(10) 0.2279(7) 1.4026(6) 0.163(4) Uani 1 1 d . . .
H68A H 1.4173 0.2197 1.4305 0.196 Uiso 1 1 calc R . .
H68B H 1.5104 0.2476 1.4282 0.196 Uiso 1 1 calc R . .
C69 C 1.1812(6) 0.4181(6) 1.3104(4) 0.134(3) Uani 1 1 d . . .
H69A H 1.1764 0.3655 1.3040 0.200 Uiso 1 1 calc R . .
H69B H 1.2129 0.4433 1.3527 0.200 Uiso 1 1 calc R . .
H69C H 1.2106 0.4304 1.2807 0.200 Uiso 1 1 calc R . .
C70 C 1.0084(8) -0.1190(6) 0.6131(6) 0.150(4) Uani 1 1 d . . .
H70A H 1.0470 -0.1502 0.5939 0.180 Uiso 1 1 calc R . .
H70B H 0.9710 -0.1491 0.6282 0.180 Uiso 1 1 calc R . .
C71 C 1.5421(6) 0.3337(6) 1.3434(6) 0.141(4) Uani 1 1 d . . .
H71A H 1.5809 0.3118 1.3693 0.211 Uiso 1 1 calc R . .
H71B H 1.5356 0.3823 1.3677 0.211 Uiso 1 1 calc R . .
H71C H 1.5644 0.3371 1.3078 0.211 Uiso 1 1 calc R . .
C72 C 1.4180(5) 0.3974(5) 1.1015(4) 0.109(2) Uani 1 1 d . . .
H72A H 1.4717 0.3780 1.1083 0.163 Uiso 1 1 calc R . .
H72B H 1.3998 0.4116 1.1406 0.163 Uiso 1 1 calc R . .
H72C H 1.4250 0.4400 1.0867 0.163 Uiso 1 1 calc R . .
Cl1 Cl 1.16627(12) 0.18021(12) 1.26382(11) 0.1100(6) Uani 1 1 d . . .
Cl2 Cl 0.6649(3) 0.4280(3) 0.7463(2) 0.1717(12) Uani 1 1 d . . .
Cl3 Cl 1.11353(19) 0.43153(15) 0.84503(12) 0.1316(8) Uani 1 1 d . . .
O2 O 1.0834(6) 0.4792(4) 0.8120(3) 0.153(3) Uani 1 1 d . . .
O3 O 0.7189(4) 0.2666(5) 1.3009(3) 0.140(2) Uani 1 1 d . . .
O4 O 0.8261(4) 0.2392(4) 1.3675(3) 0.1227(17) Uani 1 1 d . . .
O5 O 1.1496(6) 0.4687(4) 0.9093(3) 0.150(2) Uani 1 1 d . . .
O6 O 1.1707(8) 0.1812(8) 0.5734(4) 0.245(7) Uani 1 1 d . . .
O7 O 1.1570(8) 0.3796(6) 0.8204(6) 0.219(5) Uani 1 1 d . . .
O8 O 1.0345(7) 0.3904(7) 0.8444(6) 0.221(5) Uani 1 1 d . . .
O10 O 0.7021(7) 0.1641(6) 1.3296(5) 0.196(4) Uani 1 1 d . . .
O11 O 0.7207(12) 0.4177(6) 0.7910(9) 0.270(9) Uani 1 1 d . . .
O12 O 1.0893(10) 0.1307(11) 0.6130(6) 0.258(7) Uani 1 1 d . . .
O13 O 1.199(2) 0.1762(14) 0.6659(9) 0.416(15) Uani 1 1 d . . .
O15 O 0.5927(8) 0.3748(13) 0.7276(9) 0.335(10) Uani 1 1 d . . .
O16 O 0.7157(14) 0.4058(8) 0.7112(12) 0.318(11) Uani 1 1 d . . .
O17 O 0.6503(8) 0.4966(5) 0.7550(6) 0.202(4) Uani 1 1 d . . .
O19 O 1.2412(5) 0.1747(7) 1.2381(4) 0.179(3) Uani 1 1 d . . .
O20 O 1.1085(8) 0.2255(5) 1.2425(4) 0.198(4) Uani 1 1 d . . .
O21 O 1.1932(7) 0.2166(9) 1.3334(4) 0.226(5) Uani 1 1 d . . .
O22 O 1.1366(6) 0.1155(6) 1.2682(5) 0.181(3) Uiso 1 1 d . . .
Cl4 Cl 0.7999(3) 0.0702(3) 0.1055(3) 0.2084(16) Uiso 1 1 d . . .
O26 O 0.7813(5) 0.0272(5) 0.1431(4) 0.152(2) Uiso 1 1 d . . .
O25 O 0.7863(6) 0.1401(5) 0.1176(4) 0.170(3) Uiso 1 1 d . . .
O28 O 0.7858(14) 0.0286(12) 0.0427(10) 0.316(8) Uiso 1 1 d . . .
O27 O 0.9014(13) 0.0864(11) 0.1264(9) 0.314(8) Uiso 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'
Pd Pd -0.9988 1.0072 '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'
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
N2 Pd1 N14 177.6(2) . . ?
N2 Pd1 N3 93.5(3) . . ?
N14 Pd1 N3 87.0(2) . . ?
N2 Pd1 N1 85.2(3) . . ?
N14 Pd1 N1 94.2(3) . . ?
N3 Pd1 N1 176.8(2) . . ?
N17 Pd3 N16 90.2(2) . . ?
N17 Pd3 N19 177.7(2) . . ?
N16 Pd3 N19 92.1(3) . . ?
N17 Pd3 N11 92.2(3) . . ?
N16 Pd3 N11 177.2(3) . . ?
N19 Pd3 N11 85.5(3) . . ?
N9 Pd2 N5 88.5(3) . . ?
N9 Pd2 N7 176.1(2) . . ?
N5 Pd2 N7 92.5(3) . . ?
N9 Pd2 N8 92.5(3) . . ?
N5 Pd2 N8 179.0(3) . . ?
N7 Pd2 N8 86.5(3) . . ?
C69 N1 C53 108.8(8) . . ?
C69 N1 C62 113.7(8) . . ?
C53 N1 C62 107.9(7) . . ?
C69 N1 Pd1 112.3(5) . . ?
C53 N1 Pd1 109.9(5) . . ?
C62 N1 Pd1 104.1(6) . . ?
C65 N2 C63 115.5(8) . . ?
C65 N2 C55 106.1(8) . . ?
C63 N2 C55 100.2(9) . . ?
C65 N2 Pd1 112.6(5) . . ?
C63 N2 Pd1 109.4(6) . . ?
C55 N2 Pd1 112.5(5) . . ?
C30 N3 N4 105.0(6) . . ?
C30 N3 Pd1 132.8(4) . . ?
N4 N3 Pd1 122.2(5) . . ?
C13 N4 N3 112.5(6) . . ?
C17 N5 N6 105.2(6) . . ?
C17 N5 Pd2 131.6(5) . . ?
N6 N5 Pd2 120.6(5) . . ?
C39 N6 N5 113.4(7) . . ?
C66 N7 C47 108.5(8) . . ?
C66 N7 C59 111.8(8) . . ?
C47 N7 C59 108.2(7) . . ?
C66 N7 Pd2 113.4(5) . . ?
C47 N7 Pd2 110.6(5) . . ?
C59 N7 Pd2 104.1(5) . . ?
C67 N8 C70 114.6(9) . . ?
C67 N8 C26 108.6(9) . . ?
C70 N8 C26 104.8(8) . . ?
C67 N8 Pd2 110.7(6) . . ?
C70 N8 Pd2 106.6(5) . . ?
C26 N8 Pd2 111.4(5) . . ?
N10 N9 C51 105.1(6) . . ?
N10 N9 Pd2 121.9(5) . . ?
C51 N9 Pd2 132.9(6) . . ?
N9 N10 C42 110.9(6) . . ?
C21 N11 C1 109.0(8) . . ?
C21 N11 C68 109.3(9) . . ?
C1 N11 C68 111.6(9) . . ?
C21 N11 Pd3 110.1(5) . . ?
C1 N11 Pd3 111.3(6) . . ?
C68 N11 Pd3 105.6(6) . . ?
C46 N12 N17 110.2(7) . . ?
N14 N13 C36 110.4(6) . . ?
N13 N14 C32 106.9(6) . . ?
N13 N14 Pd1 118.9(5) . . ?
C32 N14 Pd1 132.2(4) . . ?
N16 N15 C35 109.1(6) . . ?
C16 N16 N15 108.3(6) . . ?
C16 N16 Pd3 132.3(5) . . ?
N15 N16 Pd3 119.4(4) . . ?
C60 N17 N12 106.8(6) . . ?
C60 N17 Pd3 134.4(5) . . ?
N12 N17 Pd3 118.7(6) . . ?
C43 N19 C71 110.0(8) . . ?
C43 N19 C58 108.7(8) . . ?
C71 N19 C58 111.2(8) . . ?
C43 N19 Pd3 113.1(6) . . ?
C71 N19 Pd3 108.5(5) . . ?
C58 N19 Pd3 105.3(6) . . ?
O10 N22 O3 125.3(7) . . ?
O10 N22 O4 119.5(6) . . ?
O3 N22 O4 115.3(5) . . ?
O12 N23 O6 127.3(10) . . ?
O12 N23 O13 106.2(12) . . ?
O6 N23 O13 118.0(13) . . ?
C4 C3 C9 115.5(6) . . ?
C35 C4 C16 105.7(6) . . ?
C35 C4 C3 123.8(7) . . ?
C16 C4 C3 130.4(7) . . ?
C17 C5 C39 105.7(7) . . ?
C17 C5 C44 129.6(7) . . ?
C39 C5 C44 124.7(7) . . ?
C13 C7 C30 108.2(7) . . ?
C13 C7 C18 131.3(7) . . ?
C30 C7 C18 120.5(6) . . ?
C24 C8 C27 116.3(6) . . ?
C14 C9 C38 121.0(7) . . ?
C14 C9 C3 121.7(8) . . ?
C38 C9 C3 117.3(7) . . ?
C45 C12 C48 116.2(6) . . ?
N4 C13 C7 105.9(6) . . ?
N4 C13 C15 119.9(7) . . ?
C7 C13 C15 134.1(8) . . ?
C45 C14 C9 122.3(8) . . ?
C45 C14 C72 118.6(7) . . ?
C9 C14 C72 119.0(7) . . ?
N16 C16 C4 109.2(6) . . ?
N16 C16 C6 120.4(6) . . ?
C4 C16 C6 130.4(6) . . ?
N5 C17 C5 109.9(7) . . ?
N5 C17 C22 121.3(7) . . ?
C5 C17 C22 128.9(7) . . ?
C7 C18 C50 117.0(6) . . ?
C56 C24 C38 120.8(7) . . ?
C56 C24 C8 119.6(6) . . ?
C38 C24 C8 119.6(6) . . ?
C42 C27 C51 106.1(6) . . ?
C42 C27 C8 133.0(7) . . ?
C51 C27 C8 120.8(6) . . ?
C54 C29 C49 119.2(7) . . ?
C54 C29 C20 120.6(8) . . ?
C49 C29 C20 120.2(7) . . ?
N3 C30 C7 108.5(6) . . ?
N3 C30 C34 119.6(6) . . ?
C7 C30 C34 131.9(6) . . ?
N14 C32 C48 109.2(6) . . ?
N14 C32 C11 121.9(6) . . ?
C48 C32 C11 129.0(7) . . ?
N15 C35 C4 107.6(6) . . ?
N15 C35 C23 119.5(7) . . ?
C4 C35 C23 132.7(7) . . ?
N13 C36 C48 108.4(6) . . ?
N13 C36 C19 120.0(7) . . ?
C48 C36 C19 131.3(8) . . ?
C49 C37 C50 118.9(8) . . ?
C49 C37 C2 121.0(7) . . ?
C50 C37 C2 120.1(7) . . ?
C24 C38 C9 117.2(7) . . ?
C24 C38 C61 119.8(8) . . ?
C9 C38 C61 122.9(7) . . ?
N6 C39 C5 105.8(7) . . ?
N6 C39 C57 125.4(9) . . ?
C5 C39 C57 128.7(9) . . ?
C50 C41 C54 117.9(7) . . ?
C50 C41 C31 121.8(7) . . ?
C54 C41 C31 120.3(8) . . ?
C27 C42 N10 108.9(7) . . ?
C27 C42 C10 133.4(7) . . ?
N10 C42 C10 117.6(6) . . ?
C5 C44 C49 115.4(6) . . ?
C14 C45 C56 117.9(7) . . ?
C14 C45 C12 122.5(7) . . ?
C56 C45 C12 119.5(7) . . ?
N12 C46 C52 109.1(7) . . ?
N12 C46 C40 121.3(7) . . ?
C52 C46 C40 129.5(8) . . ?
C36 C48 C32 105.1(6) . . ?
C36 C48 C12 125.9(7) . . ?
C32 C48 C12 129.0(6) . . ?
C37 C49 C29 119.4(8) . . ?
C37 C49 C44 121.4(8) . . ?
C29 C49 C44 119.2(7) . . ?
C37 C50 C41 123.3(7) . . ?
C37 C50 C18 117.2(7) . . ?
C41 C50 C18 119.4(8) . . ?
N9 C51 C27 109.0(6) . . ?
N9 C51 C25 120.5(8) . . ?
C27 C51 C25 130.5(7) . . ?
C46 C52 C60 102.7(7) . . ?
C46 C52 C64 126.1(7) . . ?
C60 C52 C64 131.2(7) . . ?
C29 C54 C41 121.1(7) . . ?
C29 C54 C64 119.7(8) . 2_757 ?
C41 C54 C64 119.2(8) . 2_757 ?
C24 C56 C45 120.4(6) . . ?
C24 C56 C33 120.5(7) . . ?
C45 C56 C33 119.1(7) . . ?
C68 C58 N19 114.5(10) . . ?
C70 C59 N7 115.0(8) . . ?
N17 C60 C52 111.2(7) . . ?
N17 C60 C28 120.2(8) . . ?
C52 C60 C28 128.6(9) . . ?
C63 C62 N1 114.7(9) . . ?
C62 C63 N2 107.3(9) . . ?
C52 C64 C54 115.6(7) . 2_757 ?
C58 C68 N11 113.7(9) . . ?
C59 C70 N8 110.4(9) . . ?
O22 Cl1 O20 119.5(7) . . ?
O22 Cl1 O19 110.9(7) . . ?
O20 Cl1 O19 115.7(6) . . ?
O22 Cl1 O21 95.5(7) . . ?
O20 Cl1 O21 103.4(6) . . ?
O19 Cl1 O21 109.0(6) . . ?
O11 Cl2 O16 86.4(13) . . ?
O11 Cl2 O17 114.1(9) . . ?
O16 Cl2 O17 116.7(10) . . ?
O11 Cl2 O15 111.5(13) . . ?
O16 Cl2 O15 108.1(12) . . ?
O17 Cl2 O15 116.2(11) . . ?
O7 Cl3 O2 120.0(6) . . ?
O7 Cl3 O5 113.5(6) . . ?
O2 Cl3 O5 112.0(4) . . ?
O7 Cl3 O8 103.0(8) . . ?
O2 Cl3 O8 100.9(7) . . ?
O5 Cl3 O8 105.0(7) . . ?
Cl2 O11 O16 46.5(8) . . ?
Cl2 O16 O11 47.0(8) . . ?
O25 Cl4 O26 121.6(7) . . ?
O25 Cl4 O28 117.9(11) . . ?
O26 Cl4 O28 111.5(11) . . ?
O25 Cl4 O27 96.2(9) . . ?
O26 Cl4 O27 102.0(9) . . ?
O28 Cl4 O27 102.5(12) . . ?
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
Pd1 N2 2.004(7) . ?
Pd1 N14 2.027(6) . ?
Pd1 N3 2.026(6) . ?
Pd1 N1 2.081(7) . ?
Pd3 N17 2.039(7) . ?
Pd3 N16 2.038(6) . ?
Pd3 N19 2.074(7) . ?
Pd3 N11 2.085(7) . ?
Pd2 N9 1.999(7) . ?
Pd2 N5 2.028(7) . ?
Pd2 N7 2.062(6) . ?
Pd2 N8 2.072(7) . ?
N1 C69 1.451(11) . ?
N1 C53 1.452(11) . ?
N1 C62 1.525(13) . ?
N2 C65 1.428(12) . ?
N2 C63 1.470(11) . ?
N2 C55 1.554(12) . ?
N3 C30 1.368(9) . ?
N3 N4 1.346(8) . ?
N4 C13 1.349(10) . ?
N5 C17 1.341(10) . ?
N5 N6 1.346(9) . ?
N6 C39 1.326(11) . ?
N7 C66 1.460(11) . ?
N7 C47 1.458(11) . ?
N7 C59 1.502(11) . ?
N8 C67 1.458(12) . ?
N8 C70 1.480(13) . ?
N8 C26 1.525(10) . ?
N9 N10 1.355(9) . ?
N9 C51 1.367(9) . ?
N10 C42 1.377(10) . ?
N11 C21 1.461(12) . ?
N11 C1 1.493(12) . ?
N11 C68 1.503(14) . ?
N12 C46 1.325(10) . ?
N12 N17 1.396(9) . ?
N13 N14 1.331(7) . ?
N13 C36 1.352(10) . ?
N14 C32 1.341(9) . ?
N15 N16 1.341(8) . ?
N15 C35 1.384(9) . ?
N16 C16 1.334(9) . ?
N17 C60 1.295(10) . ?
N19 C43 1.483(11) . ?
N19 C71 1.477(12) . ?
N19 C58 1.477(12) . ?
N22 O10 1.220(10) . ?
N22 O3 1.281(8) . ?
N22 O4 1.362(7) . ?
N23 O12 1.126(15) . ?
N23 O6 1.160(10) . ?
N23 O13 1.26(3) . ?
C2 C37 1.474(11) . ?
C3 C4 1.499(10) . ?
C3 C9 1.558(10) . ?
C4 C35 1.367(11) . ?
C4 C16 1.411(10) . ?
C5 C17 1.398(11) . ?
C5 C39 1.393(12) . ?
C5 C44 1.498(11) . ?
C6 C16 1.485(11) . ?
C7 C13 1.353(10) . ?
C7 C30 1.386(10) . ?
C7 C18 1.526(11) . ?
C8 C24 1.501(10) . ?
C8 C27 1.506(10) . ?
C9 C14 1.380(11) . ?
C9 C38 1.412(12) . ?
C10 C42 1.549(11) . ?
C11 C32 1.506(10) . ?
C12 C45 1.500(11) . ?
C12 C48 1.523(10) . ?
C13 C15 1.500(11) . ?
C14 C45 1.367(10) . ?
C14 C72 1.571(12) . ?
C17 C22 1.447(11) . ?
C18 C50 1.550(10) . ?
C19 C36 1.526(10) . ?
C20 C29 1.530(11) . ?
C23 C35 1.522(11) . ?
C24 C56 1.385(10) . ?
C24 C38 1.416(10) . ?
C25 C51 1.455(11) . ?
C27 C42 1.314(10) . ?
C27 C51 1.440(11) . ?
C28 C60 1.496(11) . ?
C29 C54 1.373(11) . ?
C29 C49 1.452(12) . ?
C30 C34 1.450(10) . ?
C31 C41 1.505(12) . ?
C32 C48 1.411(9) . ?
C33 C56 1.529(10) . ?
C36 C48 1.351(10) . ?
C37 C49 1.384(11) . ?
C37 C50 1.390(11) . ?
C38 C61 1.468(11) . ?
C39 C57 1.514(12) . ?
C40 C46 1.486(11) . ?
C41 C50 1.375(11) . ?
C41 C54 1.416(11) . ?
C44 C49 1.519(11) . ?
C45 C56 1.430(11) . ?
C46 C52 1.404(11) . ?
C52 C60 1.450(11) . ?
C52 C64 1.512(13) . ?
C54 C64 1.511(12) 2_757 ?
C58 C68 1.396(16) . ?
C59 C70 1.442(14) . ?
C62 C63 1.440(15) . ?
C64 C54 1.511(12) 2_757 ?
Cl1 O22 1.319(10) . ?
Cl1 O20 1.405(8) . ?
Cl1 O19 1.436(7) . ?
Cl1 O21 1.492(10) . ?
Cl2 O11 1.275(13) . ?
Cl2 O16 1.264(13) . ?
Cl2 O17 1.304(9) . ?
Cl2 O15 1.395(17) . ?
Cl3 O7 1.309(9) . ?
Cl3 O2 1.371(7) . ?
Cl3 O5 1.408(7) . ?
Cl3 O8 1.437(11) . ?
O11 O16 1.74(2) . ?
Cl4 O25 1.319(9) . ?
Cl4 O26 1.385(8) . ?
Cl4 O28 1.39(2) . ?
Cl4 O27 1.59(2) . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 165 43 ' '
2 -0.034 0.327 0.533 2106 398 ' '
3 0.500 1.000 1.000 121 31 ' '
