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#$Date: 2021-06-10 12:12:31 +0300 (Thu, 10 Jun 2021) $
#$Revision: 266357 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/32/1563293.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_1563293
loop_
_publ_author_name
'Jin, Juan'
'Wu, Di'
'Jia, Ming-Jun'
'Peng, Yu'
'Yu, Jie-Hui'
'Wang, Yu-Chang'
'Xu, Ji-Qing'
_publ_section_title
;
 New 4,5-dichlorophthalhydrazidate-bridged chained coordination polymers
;
_journal_issue                   3
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              667
_journal_page_last               674
_journal_paper_doi               10.1016/j.jssc.2011.01.034
_journal_volume                  184
_journal_year                    2011
_chemical_formula_sum            'C52 H24 Cd3 Cl8 N8 O12'
_chemical_formula_weight         1573.59
_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                 93.416(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.9126(3)
_cell_length_b                   25.7233(12)
_cell_length_c                   13.2669(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2695.5(2)
_computing_cell_refinement       'Bruker SMART '
_computing_data_collection       'Bruker SMART '
_computing_data_reduction        'Bruker SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'siements SMART CCD'
_diffrn_measurement_method       '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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19657
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.355
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0632
_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)+(0.0422P)²+16.9492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                4243
_reflns_number_total             6739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2011-184-667.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1563293
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
Cd1 Cd 0.72067(7) 0.03804(2) 0.25807(4) 0.02763(15) Uani 1 1 d . . .
Cd2 Cd 1.0000 0.0000 0.0000 0.02802(19) Uiso 1 2 d S . .
O1 O 0.8533(7) -0.0388(2) 0.1206(4) 0.0391(13) Uani 1 1 d . . .
O2 O 0.1913(7) -0.0633(2) 0.0407(5) 0.0510(17) Uani 1 1 d . . .
O3 O 0.6052(7) 0.1191(2) 0.2129(4) 0.0374(13) Uani 1 1 d . . .
O4 O 0.4122(7) 0.0622(2) 0.2584(4) 0.0354(13) Uani 1 1 d . . .
O5 O -0.0230(7) 0.0665(3) 0.2391(5) 0.0497(16) Uani 1 1 d . . .
O6 O 0.1360(7) 0.0595(2) 0.1062(4) 0.0363(13) Uani 1 1 d . . .
N1 N 0.5895(8) -0.0129(2) 0.1337(5) 0.0325(15) Uani 1 1 d . . .
N2 N 0.4154(8) -0.0200(3) 0.1131(5) 0.0349(16) Uani 1 1 d . . .
N3 N 0.6979(9) 0.0651(3) 0.4292(5) 0.0352(15) Uani 1 1 d . . .
N4 N 0.8024(8) -0.0301(2) 0.3716(5) 0.0327(15) Uani 1 1 d . . .
C1 C 0.7437(11) -0.1400(3) 0.0584(6) 0.038(2) Uani 1 1 d . . .
H1A H 0.8599 -0.1353 0.0689 0.046 Uiso 1 1 calc R . .
C2 C 0.6776(13) -0.1876(3) 0.0312(6) 0.042(2) Uani 1 1 d . . .
C3 C 0.5020(13) -0.1939(3) 0.0098(7) 0.045(2) Uani 1 1 d . . .
C4 C 0.3964(12) -0.1534(3) 0.0163(6) 0.041(2) Uani 1 1 d . . .
H4A H 0.2815 -0.1574 -0.0010 0.049 Uiso 1 1 calc R . .
C5 C 0.4599(10) -0.1054(3) 0.0491(6) 0.0310(17) Uani 1 1 d . . .
C6 C 0.6320(10) -0.0989(3) 0.0700(6) 0.0302(17) Uani 1 1 d . . .
C7 C 0.6946(10) -0.0482(3) 0.1074(5) 0.0298(17) Uani 1 1 d . . .
C8 C 0.3454(10) -0.0618(3) 0.0642(6) 0.0334(18) Uani 1 1 d . . .
C9 C 0.3693(11) 0.1994(3) 0.2419(6) 0.0367(19) Uani 1 1 d . . .
H9A H 0.4836 0.2071 0.2537 0.044 Uiso 1 1 calc R . .
C10 C 0.2532(11) 0.2386(3) 0.2444(6) 0.0360(19) Uani 1 1 d . . .
C11 C 0.0804(11) 0.2278(3) 0.2284(6) 0.0350(19) Uani 1 1 d . . .
C12 C 0.0307(10) 0.1765(3) 0.2080(6) 0.0360(19) Uani 1 1 d . . .
H12A H -0.0837 0.1688 0.1966 0.043 Uiso 1 1 calc R . .
C13 C 0.1494(9) 0.1368(3) 0.2045(6) 0.0290(16) Uani 1 1 d . . .
C14 C 0.3212(9) 0.1485(3) 0.2222(5) 0.0279(16) Uani 1 1 d . . .
C15 C 0.4560(10) 0.1073(3) 0.2296(5) 0.0300(17) Uani 1 1 d . . .
C16 C 0.0838(9) 0.0830(3) 0.1801(6) 0.0298(17) Uani 1 1 d . . .
C17 C 0.6476(13) 0.1122(3) 0.4550(7) 0.050(2) Uani 1 1 d . . .
H17A H 0.6401 0.1379 0.4056 0.060 Uiso 1 1 calc R . .
C18 C 0.6057(14) 0.1252(4) 0.5519(8) 0.058(3) Uani 1 1 d . . .
H18A H 0.5701 0.1586 0.5671 0.069 Uiso 1 1 calc R . .
C19 C 0.6184(13) 0.0877(4) 0.6238(7) 0.053(3) Uani 1 1 d . . .
H19A H 0.5904 0.0950 0.6894 0.064 Uiso 1 1 calc R . .
C20 C 0.6725(12) 0.0389(4) 0.5993(6) 0.047(2) Uani 1 1 d . . .
H20A H 0.6811 0.0129 0.6480 0.057 Uiso 1 1 calc R . .
C21 C 0.7142(10) 0.0288(3) 0.5015(6) 0.0305(17) Uani 1 1 d . . .
C22 C 0.7804(10) -0.0233(3) 0.4700(6) 0.0328(18) Uani 1 1 d . . .
C23 C 0.8167(12) -0.0615(4) 0.5408(6) 0.046(2) Uani 1 1 d . . .
H23A H 0.7955 -0.0564 0.6082 0.056 Uiso 1 1 calc R . .
C24 C 0.8847(14) -0.1073(4) 0.5093(8) 0.059(3) Uani 1 1 d . . .
H24A H 0.9114 -0.1335 0.5558 0.071 Uiso 1 1 calc R . .
C25 C 0.9138(14) -0.1145(4) 0.4087(8) 0.056(3) Uani 1 1 d . . .
H25A H 0.9617 -0.1451 0.3866 0.067 Uiso 1 1 calc R . .
C26 C 0.8698(13) -0.0750(3) 0.3419(7) 0.050(2) Uani 1 1 d . . .
H26A H 0.8875 -0.0797 0.2739 0.060 Uiso 1 1 calc R . .
Cl4 Cl -0.0719(3) 0.27562(10) 0.2291(2) 0.0575(7) Uani 1 1 d . . .
Cl1 Cl 0.8160(4) -0.24017(10) 0.0262(2) 0.0736(9) Uani 1 1 d . . .
Cl3 Cl 0.3175(4) 0.30224(9) 0.2696(2) 0.0602(7) Uani 1 1 d . . .
Cl2 Cl 0.4235(5) -0.25457(10) -0.0232(3) 0.0807(10) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
O5 Cd1 N1 119.3(2) 1_655 .
O5 Cd1 O3 91.3(2) 1_655 .
N1 Cd1 O3 99.9(2) . .
O5 Cd1 N4 95.8(2) 1_655 .
N1 Cd1 N4 97.4(2) . .
O3 Cd1 N4 155.1(2) . .
O5 Cd1 N3 97.7(2) 1_655 .
N1 Cd1 N3 142.1(2) . .
O3 Cd1 N3 86.2(2) . .
N4 Cd1 N3 69.3(2) . .
O5 Cd1 O4 145.4(2) 1_655 .
N1 Cd1 O4 75.3(2) . .
O3 Cd1 O4 54.35(18) . .
N4 Cd1 O4 114.1(2) . .
N3 Cd1 O4 78.4(2) . .
O5 Cd1 C15 118.0(2) 1_655 .
N1 Cd1 C15 87.9(2) . .
O3 Cd1 C15 26.86(19) . .
N4 Cd1 C15 137.6(2) . .
N3 Cd1 C15 80.9(2) . .
O4 Cd1 C15 27.49(19) . .
O1 Cd2 O1 180.0(3) . 3_755
O1 Cd2 O2 83.0(2) . 1_655
O1 Cd2 O2 97.0(2) 3_755 1_655
O1 Cd2 O2 97.0(2) . 3_655
O1 Cd2 O2 83.0(2) 3_755 3_655
O2 Cd2 O2 180.0(2) 1_655 3_655
O1 Cd2 O6 84.2(2) . 3_655
O1 Cd2 O6 95.8(2) 3_755 3_655
O2 Cd2 O6 87.1(2) 1_655 3_655
O2 Cd2 O6 92.9(2) 3_655 3_655
O1 Cd2 O6 95.8(2) . 1_655
O1 Cd2 O6 84.2(2) 3_755 1_655
O2 Cd2 O6 92.9(2) 1_655 1_655
O2 Cd2 O6 87.1(2) 3_655 1_655
O6 Cd2 O6 180.0(3) 3_655 1_655
C7 O1 Cd2 121.7(5) . .
C8 O2 Cd2 132.1(6) . 1_455
C15 O3 Cd1 95.5(5) . .
C15 O4 Cd1 86.8(5) . .
C16 O5 Cd1 147.8(6) . 1_455
C16 O6 Cd2 129.8(5) . 1_455
C7 N1 N2 119.9(6) . .
C7 N1 Cd1 108.9(5) . .
N2 N1 Cd1 127.5(5) . .
C8 N2 N1 124.4(6) . .
C17 N3 C21 118.0(7) . .
C17 N3 Cd1 123.5(6) . .
C21 N3 Cd1 117.9(5) . .
C22 N4 C26 118.4(7) . .
C22 N4 Cd1 118.4(5) . .
C26 N4 Cd1 123.2(5) . .
C2 C1 C6 118.2(8) . .
C1 C2 C3 120.7(8) . .
C1 C2 Cl1 118.2(8) . .
C3 C2 Cl1 121.1(7) . .
C4 C3 C2 120.5(8) . .
C4 C3 Cl2 120.1(8) . .
C2 C3 Cl2 119.4(7) . .
C3 C4 C5 119.6(8) . .
C6 C5 C4 120.2(8) . .
C6 C5 C8 119.3(7) . .
C4 C5 C8 120.5(7) . .
C5 C6 C1 120.6(7) . .
C5 C6 C7 118.9(7) . .
C1 C6 C7 120.5(7) . .
O1 C7 N1 118.1(7) . .
O1 C7 C6 121.5(7) . .
N1 C7 C6 120.3(7) . .
O2 C8 N2 120.7(7) . .
O2 C8 C5 123.3(7) . .
N2 C8 C5 115.8(7) . .
C10 C9 C14 121.7(8) . .
C9 C10 C11 120.1(7) . .
C9 C10 Cl3 120.7(7) . .
C11 C10 Cl3 119.2(6) . .
C10 C11 C12 118.6(7) . .
C10 C11 Cl4 122.4(6) . .
C12 C11 Cl4 119.1(7) . .
C13 C12 C11 121.1(8) . .
C12 C13 C14 119.3(7) . .
C12 C13 C16 117.2(7) . .
C14 C13 C16 123.5(7) . .
C9 C14 C13 119.2(7) . .
C9 C14 C15 117.9(7) . .
C13 C14 C15 122.6(7) . .
O3 C15 O4 123.4(7) . .
O3 C15 C14 119.4(7) . .
O4 C15 C14 117.2(7) . .
O3 C15 Cd1 57.6(4) . .
O4 C15 Cd1 65.8(4) . .
C14 C15 Cd1 174.1(5) . .
O6 C16 O5 126.4(8) . .
O6 C16 C13 119.3(7) . .
O5 C16 C13 114.2(7) . .
N3 C17 C18 123.5(9) . .
C19 C18 C17 117.9(9) . .
C18 C19 C20 119.8(9) . .
C19 C20 C21 119.3(8) . .
N3 C21 C20 121.6(8) . .
N3 C21 C22 116.2(7) . .
C20 C21 C22 122.3(7) . .
N4 C22 C23 122.5(7) . .
N4 C22 C21 117.0(7) . .
C23 C22 C21 120.5(7) . .
C24 C23 C22 118.4(8) . .
C23 C24 C25 120.1(9) . .
C26 C25 C24 118.2(9) . .
N4 C26 C25 122.4(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd1 O5 2.185(6) 1_655
Cd1 N1 2.306(6) .
Cd1 O3 2.340(5) .
Cd1 N4 2.376(6) .
Cd1 N3 2.391(6) .
Cd1 O4 2.519(5) .
Cd1 C15 2.758(8) .
Cd2 O1 2.264(5) .
Cd2 O1 2.264(5) 3_755
Cd2 O2 2.266(6) 1_655
Cd2 O2 2.266(6) 3_655
Cd2 O6 2.304(5) 3_655
Cd2 O6 2.304(5) 1_655
O1 C7 1.281(9) .
O2 C8 1.241(9) .
O2 Cd2 2.266(6) 1_455
O3 C15 1.252(9) .
O4 C15 1.275(9) .
O5 C16 1.259(9) .
O5 Cd1 2.185(6) 1_455
O6 C16 1.243(9) .
O6 Cd2 2.304(5) 1_455
N1 C7 1.293(10) .
N1 N2 1.400(8) .
N2 C8 1.357(10) .
N3 C17 1.327(11) .
N3 C21 1.339(10) .
N4 C22 1.339(10) .
N4 C26 1.342(10) .
C1 C2 1.372(12) .
C1 C6 1.393(11) .
C2 C3 1.411(13) .
C2 Cl1 1.744(8) .
C3 C4 1.342(12) .
C3 Cl2 1.726(8) .
C4 C5 1.393(11) .
C5 C6 1.383(11) .
C5 C8 1.464(11) .
C6 C7 1.470(11) .
C9 C10 1.366(11) .
C9 C14 1.385(11) .
C10 C11 1.399(11) .
C10 Cl3 1.740(8) .
C11 C12 1.400(11) .
C11 Cl4 1.722(8) .
C12 C13 1.390(10) .
C13 C14 1.398(10) .
C13 C16 1.507(11) .
C14 C15 1.503(11) .
C17 C18 1.388(13) .
C18 C19 1.357(14) .
C19 C20 1.371(13) .
C20 C21 1.382(11) .
C21 C22 1.507(11) .
C22 C23 1.378(11) .
C23 C24 1.369(13) .
C24 C25 1.381(13) .
C25 C26 1.378(12) .
