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#$Date: 2019-11-28 14:23:56 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243941 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/26/7702668.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_7702668
loop_
_publ_author_name
'Liu, Hong-Ke'
'Hu, Jun'
'Wang, Tian-Wei'
'Yu, Xiao-Lan'
'Liu, Jun'
'Kang, Beisheng'
_publ_section_title
;
 Synthesis and crystal structures of silver(i), palladium(ii), zinc(ii)
 and cobalt(ii) complexes of the ditoptic ligand
 1,3-bis(imidazol-1-ylmethyl)-2,4,6-trimethylbenzene
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3534
_journal_paper_doi               10.1039/b104833n
_journal_year                    2001
_chemical_formula_sum            'C71 H100 Cl4 N17.5 O8 Pd2'
_chemical_formula_weight         1681.79
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        '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                96.710(2)
_cell_angle_beta                 113.302(2)
_cell_angle_gamma                94.745(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7708(15)
_cell_length_b                   14.3618(19)
_cell_length_c                   14.4184(19)
_cell_measurement_temperature    293(2)
_cell_volume                     2201.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15867
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         6.82
_exptl_absorpt_coefficient_mu    0.587
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             873
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         12124
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0948P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1791
_refine_ls_wR_factor_ref         0.2030
_reflns_number_gt                6036
_reflns_number_total             12124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104833n.txt
_cod_data_source_block           '[Pd2(bitmb)4]Cl4.cif'
_cod_original_formula_sum        'C71 H100 Cl4 N17.50 O8 Pd2'
_cod_database_code               7702668
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
Pd1 Pd 0.681173(15) 0.950269(11) 1.430666(12) 0.05159(5) Uani 1 1 d .
N1 N 0.65326(17) 0.88394(13) 1.29159(14) 0.0624(6) Uani 1 1 d .
N2 N 0.65749(19) 0.86101(16) 1.14058(15) 0.0731(7) Uani 1 1 d .
N3 N 0.70567(16) 0.82854(13) 1.48675(14) 0.0591(6) Uani 1 1 d .
N4 N 0.76601(17) 0.69190(13) 1.51828(16) 0.0685(6) Uani 1 1 d .
N5 N 0.70725(16) 1.01940(13) 1.56918(13) 0.0562(5) Uani 1 1 d .
N6 N 1.21651(17) 0.93756(16) 1.26548(15) 0.0727(7) Uani 1 1 d .
N7 N 0.64502(16) 1.07027(12) 1.37222(14) 0.0563(6) Uani 1 1 d .
N8 N 1.33859(17) 0.78200(13) 1.64908(16) 0.0662(6) Uani 1 1 d .
C1 C 0.5774(3) 0.79945(19) 1.2384(2) 0.0787(9) Uani 1 1 d .
H1A H 0.5318 0.7578 1.2632 0.080 Uiso 1 1 d R
C2 C 0.5779(3) 0.7869(2) 1.1450(2) 0.0974(12) Uani 1 1 d .
H2A H 0.5301 0.7362 1.0900 0.080 Uiso 1 1 d R
C3 C 0.6997(2) 0.91827(18) 1.22992(17) 0.0644(8) Uani 1 1 d .
H3A H 0.7562 0.9761 1.2477 0.080 Uiso 1 1 d R
C4 C 0.6832(3) 0.8774(3) 1.0510(2) 0.0952(12) Uani 1 1 d .
H4A H 0.6932 0.8181 1.0188 0.080 Uiso 1 1 d R
H4B H 0.6129 0.9002 1.0025 0.080 Uiso 1 1 d R
C5 C 0.7984(2) 0.9455(2) 1.07869(17) 0.0756(9) Uani 1 1 d .
C6 C 0.7938(3) 1.0415(2) 1.07464(19) 0.0895(11) Uani 1 1 d .
C7 C 0.9031(3) 1.1015(2) 1.1003(2) 0.0898(11) Uani 1 1 d .
H7A H 0.8995 1.1679 1.0995 0.080 Uiso 1 1 d R
C8 C 1.0167(3) 1.0705(3) 1.12805(19) 0.0892(11) Uani 1 1 d .
C9 C 1.0229(2) 0.9764(2) 1.13097(17) 0.0825(10) Uani 1 1 d .
C10 C 0.9156(3) 0.9121(2) 1.11098(18) 0.0825(9) Uani 1 1 d .
C11 C 0.6707(3) 1.0822(3) 1.0439(3) 0.1167(13) Uani 1 1 d .
H11A H 0.6864 1.1491 1.0456 0.080 Uiso 1 1 d R
H11B H 0.6342 1.0706 1.0911 0.080 Uiso 1 1 d R
H11C H 0.6142 1.0526 0.9759 0.080 Uiso 1 1 d R
C12 C 0.9210(3) 0.8068(3) 1.1196(3) 0.1119(14) Uani 1 1 d .
H12A H 1.0060 0.7948 1.1426 0.080 Uiso 1 1 d R
H12B H 0.8719 0.7686 1.0541 0.080 Uiso 1 1 d R
H12C H 0.8882 0.7913 1.1681 0.080 Uiso 1 1 d R
C13 C 1.1321(4) 1.1432(3) 1.1548(3) 0.1233(16) Uani 1 1 d .
H13A H 1.2043 1.1110 1.1722 0.080 Uiso 1 1 d R
H13B H 1.1427 1.1904 1.2116 0.080 Uiso 1 1 d R
H13C H 1.1222 1.1731 1.0964 0.080 Uiso 1 1 d R
C14 C 0.6484(2) 0.79137(19) 1.5433(2) 0.0748(8) Uani 1 1 d .
H14A H 0.5918 0.8217 1.5656 0.080 Uiso 1 1 d R
C15 C 0.6854(3) 0.7063(2) 1.5628(2) 0.0917(10) Uani 1 1 d .
H15A H 0.6589 0.6644 1.5999 0.080 Uiso 1 1 d R
C16 C 0.7777(2) 0.76617(15) 1.47457(19) 0.0632(7) Uani 1 1 d .
H16A H 0.8309 0.7741 1.4391 0.080 Uiso 1 1 d R
C17 C 0.8243(2) 0.60401(17) 1.5158(3) 0.0925(11) Uani 1 1 d .
H17A H 0.8469 0.5826 1.5806 0.080 Uiso 1 1 d R
H17B H 0.7638 0.5557 1.4641 0.080 Uiso 1 1 d R
C18 C 1.0545(2) 0.64954(15) 1.5710(2) 0.0682(8) Uani 1 1 d .
C19 C 1.1612(2) 0.65505(15) 1.5495(2) 0.0727(9) Uani 1 1 d .
C20 C 1.1492(2) 0.63364(17) 1.4505(2) 0.0783(9) Uani 1 1 d .
C21 C 1.0297(3) 0.60676(19) 1.3727(2) 0.0851(10) Uani 1 1 d .
H21A H 1.0210 0.5913 1.3034 0.080 Uiso 1 1 d R
C22 C 0.9245(3) 0.59837(17) 1.3915(2) 0.0796(10) Uani 1 1 d .
C23 C 0.9383(2) 0.61833(15) 1.4934(2) 0.0687(8) Uani 1 1 d .
C24 C 0.7991(3) 0.5686(2) 1.3046(3) 0.1213(17) Uani 1 1 d .
H24A H 0.7352 0.5668 1.3303 0.080 Uiso 1 1 d R
H24B H 0.7965 0.5069 1.2695 0.080 Uiso 1 1 d R
H24C H 0.7851 0.6134 1.2581 0.080 Uiso 1 1 d R
C25 C 1.2581(3) 0.6420(3) 1.4176(3) 0.1116(14) Uani 1 1 d .
H25A H 1.3345 0.6625 1.4774 0.080 Uiso 1 1 d R
H25B H 1.2463 0.6874 1.3718 0.080 Uiso 1 1 d R
H25C H 1.2624 0.5816 1.3838 0.080 Uiso 1 1 d R
C26 C 1.0661(3) 0.6772(2) 1.6777(2) 0.0993(12) Uani 1 1 d .
H26A H 0.9847 0.6688 1.6785 0.080 Uiso 1 1 d R
H26B H 1.1015 0.7427 1.7001 0.080 Uiso 1 1 d R
H26C H 1.1190 0.6395 1.7229 0.080 Uiso 1 1 d R
C27 C 1.1451(3) 0.9342(3) 1.1552(2) 0.1011(12) Uani 1 1 d .
H27A H 1.1278 0.8704 1.1195 0.080 Uiso 1 1 d R
H27B H 1.1955 0.9711 1.1303 0.080 Uiso 1 1 d R
C28 C 1.3136(2) 0.8882(2) 1.3067(2) 0.0763(9) Uani 1 1 d .
H28A H 1.3424 0.8433 1.2692 0.080 Uiso 1 1 d R
C29 C 0.6405(2) 1.08513(18) 1.59078(19) 0.0677(8) Uani 1 1 d .
H29A H 0.5722 1.1092 1.5415 0.080 Uiso 1 1 d R
C30 C 0.7922(2) 1.00748(19) 1.65756(17) 0.0679(7) Uani 1 1 d .
H30A H 0.8528 0.9648 1.6657 0.080 Uiso 1 1 d R
C31 C 1.2897(3) 0.68129(17) 1.6357(3) 0.0877(11) Uani 1 1 d .
H31A H 1.2844 0.6694 1.6982 0.080 Uiso 1 1 d R
H31B H 1.3462 0.6422 1.6233 0.080 Uiso 1 1 d R
C32 C 1.4545(3) 0.82435(19) 1.7168(2) 0.0818(10) Uani 1 1 d .
H32A H 1.5181 0.7945 1.7636 0.080 Uiso 1 1 d R
C33 C 0.5365(2) 1.08314(18) 1.29557(19) 0.0724(9) Uani 1 1 d .
H33A H 0.4663 1.0352 1.2561 0.080 Uiso 1 1 d R
C34 C 0.7192(2) 1.15255(16) 1.40486(19) 0.0655(8) Uani 1 1 d .
H34A H 0.8019 1.1635 1.4586 0.080 Uiso 1 1 d R
Cl1 Cl 1.0378(3) 0.9303(2) 0.6283(2) 0.1790(11) Uiso 0.50 1 d P
Cl1' Cl 1.0222(2) 0.9571(2) 0.5653(2) 0.1499(8) Uiso 0.50 1 d P
Cl2 Cl 1.5065(2) 0.51808(19) 0.61759(19) 0.2526(9) Uiso 1 1 d .
O1W O 1.2266(5) 0.7005(4) 1.1189(4) 0.243(2) Uiso 1 1 d .
O2W O 1.6320(6) 0.6678(5) 0.8498(5) 0.278(3) Uiso 1 1 d .
O3W O 1.4084(8) 0.5994(6) 1.2267(6) 0.195(3) Uiso 0.50 1 d P
O3W' O 1.8459(8) 0.5695(7) 0.7846(7) 0.206(3) Uiso 0.50 1 d P
O4W O 1.0025(4) 1.1560(3) 1.6052(3) 0.1005(13) Uiso 0.50 1 d P
O4W' O 1.0121(10) 1.0842(9) 1.5621(8) 0.233(4) Uiso 0.50 1 d P
N1W N 1.4912(4) 0.6555(7) 0.8964(6) 0.263(4) Uiso 0.75 1 d PD
C1W C 1.2874(5) 0.6424(11) 0.9259(6) 0.300 Uiso 0.75 1 d PD
C2W C 1.3927(3) 0.6540(4) 0.9005(3) 0.134(2) Uani 0.75 1 d PDU
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'
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_1
_geom_angle_site_symmetry_3
N1 Pd1 N3 90.88(8) . .
N1 Pd1 N7 89.09(8) . .
N3 Pd1 N7 176.37(8) . .
N1 Pd1 N5 178.70(8) . .
N3 Pd1 N5 90.33(8) . .
N7 Pd1 N5 89.68(8) . .
C3 N1 C1 107.1(2) . .
C3 N1 Pd1 124.82(15) . .
C1 N1 Pd1 127.9(2) . .
C3 N2 C2 106.9(2) . .
C3 N2 C4 126.3(2) . .
C2 N2 C4 126.7(2) . .
C16 N3 C14 105.8(2) . .
C16 N3 Pd1 127.25(18) . .
C14 N3 Pd1 126.93(17) . .
C16 N4 C15 108.5(2) . .
C16 N4 C17 127.1(3) . .
C15 N4 C17 124.3(2) . .
C30 N5 C29 106.3(2) . .
C30 N5 Pd1 125.84(17) . .
C29 N5 Pd1 127.85(14) . .
C30 N6 C28 107.3(2) 2_778 .
C30 N6 C27 128.2(2) 2_778 .
C28 N6 C27 124.3(2) . .
C34 N7 C33 107.54(19) . .
C34 N7 Pd1 126.33(14) . .
C33 N7 Pd1 126.03(15) . .
C34 N8 C32 107.7(2) 2_778 .
C34 N8 C31 127.06(19) 2_778 .
C32 N8 C31 125.2(2) . .
C2 C1 N1 107.3(3) . .
C1 C2 N2 108.2(2) . .
N2 C3 N1 110.5(2) . .
N2 C4 C5 112.9(2) . .
C6 C5 C10 119.1(3) . .
C6 C5 C4 121.6(3) . .
C10 C5 C4 119.3(3) . .
C7 C6 C5 119.3(3) . .
C7 C6 C11 119.2(3) . .
C5 C6 C11 121.5(3) . .
C8 C7 C6 122.7(3) . .
C9 C8 C7 118.9(3) . .
C9 C8 C13 122.7(3) . .
C7 C8 C13 118.4(3) . .
C8 C9 C10 121.2(3) . .
C8 C9 C27 122.6(3) . .
C10 C9 C27 116.2(3) . .
C9 C10 C5 118.6(3) . .
C9 C10 C12 122.4(3) . .
C5 C10 C12 119.0(3) . .
C15 C14 N3 109.1(3) . .
C14 C15 N4 106.1(3) . .
N4 C16 N3 110.5(2) . .
N4 C17 C23 112.6(2) . .
C23 C18 C19 120.0(3) . .
C23 C18 C26 119.5(3) . .
C19 C18 C26 120.5(2) . .
C20 C19 C18 120.1(2) . .
C20 C19 C31 119.8(3) . .
C18 C19 C31 120.0(3) . .
C19 C20 C21 118.6(3) . .
C19 C20 C25 124.6(2) . .
C21 C20 C25 116.7(3) . .
C22 C21 C20 122.7(3) . .
C21 C22 C23 118.2(2) . .
C21 C22 C24 120.0(3) . .
C23 C22 C24 121.8(3) . .
C18 C23 C22 120.2(3) . .
C18 C23 C17 121.0(3) . .
C22 C23 C17 118.8(2) . .
N6 C27 C9 112.4(2) . .
C29 C28 N6 106.4(2) 2_778 .
C28 C29 N5 108.9(2) 2_778 .
N5 C30 N6 111.1(2) . 2_778
N8 C31 C19 112.1(2) . .
N8 C32 C33 106.9(2) . 2_778
C32 C33 N7 108.1(2) 2_778 .
N7 C34 N8 109.67(18) . 2_778
Cl1 Cl1' O4W' 137.6(5) . 2_777
Cl1 Cl1' O4W' 121.5(5) . 1_554
O4W' Cl1' O4W' 100.8(5) 2_777 1_554
Cl1 Cl1' Cl1' 169.3(4) . 2_776
O4W' Cl1' Cl1' 52.5(4) 2_777 2_776
O4W' Cl1' Cl1' 48.3(4) 1_554 2_776
O4W O4W' Cl1' 133.2(9) . 2_777
O4W O4W' Cl1' 145.7(10) . 1_556
Cl1' O4W' Cl1' 79.2(5) 2_777 1_556
N1W C2W C1W 166.7(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N1 2.004(2) .
Pd1 N3 2.0056(19) .
Pd1 N7 2.0096(18) .
Pd1 N5 2.0174(19) .
N1 C3 1.333(4) .
N1 C1 1.386(3) .
N2 C3 1.327(3) .
N2 C2 1.383(4) .
N2 C4 1.478(4) .
N3 C16 1.326(3) .
N3 C14 1.372(4) .
N4 C16 1.325(3) .
N4 C15 1.355(4) .
N4 C17 1.489(3) .
N5 C30 1.313(3) .
N5 C29 1.361(3) .
N6 C30 1.328(3) 2_778
N6 C28 1.362(3) .
N6 C27 1.468(3) .
N7 C34 1.325(3) .
N7 C33 1.363(3) .
N8 C34 1.345(3) 2_778
N8 C32 1.362(3) .
N8 C31 1.473(3) .
C1 C2 1.340(5) .
C4 C5 1.488(4) .
C5 C6 1.391(4) .
C5 C10 1.416(4) .
C6 C7 1.379(4) .
C6 C11 1.527(5) .
C7 C8 1.365(5) .
C8 C9 1.364(5) .
C8 C13 1.530(5) .
C9 C10 1.410(4) .
C9 C27 1.535(4) .
C10 C12 1.537(5) .
C14 C15 1.355(4) .
C17 C23 1.503(4) .
C18 C23 1.376(3) .
C18 C19 1.407(4) .
C18 C26 1.492(4) .
C19 C20 1.371(4) .
C19 C31 1.512(3) .
C20 C21 1.395(4) .
C20 C25 1.534(5) .
C21 C22 1.367(5) .
C22 C23 1.405(4) .
C22 C24 1.496(4) .
C28 C29 1.351(4) 2_778
C29 C28 1.351(4) 2_778
C30 N6 1.328(3) 2_778
C32 C33 1.362(4) 2_778
C33 C32 1.362(4) 2_778
C34 N8 1.345(3) 2_778
Cl1 Cl1' 0.985(4) .
Cl1' O4W' 1.733(12) 2_777
Cl1' O4W' 1.843(13) 1_554
Cl1' Cl1' 2.282(6) 2_776
O4W O4W' 1.179(13) .
O4W' Cl1' 1.733(12) 2_777
O4W' Cl1' 1.843(13) 1_556
N1W C2W 1.183(6) .
C1W C2W 1.426(7) .
