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#$Date: 2022-05-02 11:58:01 +0300 (Mon, 02 May 2022) $
#$Revision: 274790 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/51/8105100.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_8105100
loop_
_publ_author_name
'Tan, Yee Seng'
'Tiekink, Edward R.T.'
_publ_section_title
;
 Crystal structure of catena-[(bis(O,O′-diethyl
 dithiophosphato-S,S′)-μ2-1,2-bis(4-pyridylmethylene)hydrazine-N,N′)cadmium(II)],
 {C20H30CdN4O4P2S4}n
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              335
_journal_page_last               337
_journal_paper_doi               10.1515/ncrs-2019-0653
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C20 H30 Cd N4 O4 P2 S4'
_chemical_formula_sum            'C20 H30 Cd N4 O4 P2 S4'
_chemical_formula_weight         693.06
_space_group_crystal_system      triclinic
_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-2018/3
_cell_angle_alpha                63.153(2)
_cell_angle_beta                 64.193(2)
_cell_angle_gamma                62.710(2)
_cell_formula_units_Z            1
_cell_length_a                   9.3353(2)
_cell_length_b                   9.7725(2)
_cell_length_c                   10.6884(2)
_cell_measurement_reflns_used    15116
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2600
_cell_measurement_theta_min      4.8150
_cell_volume                     740.43(3)
_computing_cell_refinement       'CrysAlisPro [1]'
_computing_data_collection       'CrysAlisPro [1]'
_computing_data_reduction        'CrysAlisPro [1]'
_computing_molecular_graphics    'ORTEP-3 for Windows [4]'
_computing_publication_material  'SHELXL-2018/3 [3]'
_computing_structure_refinement  'SHELXL-2018/3 [3]'
_computing_structure_solution    'SHELXS-97 [2]'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.2558
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17287
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.028
_diffrn_reflns_theta_max         67.028
_diffrn_reflns_theta_min         4.842
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.841
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.301
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'CrysAlisPro [1]'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       prism
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         2640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0295P)²+0.4035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0465
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2640
_reflns_number_total             2640
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0653_suppl.cif
_cod_data_source_block           shelx
_cod_database_code               8105100
_shelx_shelxl_version_number     2018/3
_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   0.265
_shelx_estimated_absorpt_t_max   0.481
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
Cd Cd 0.500000 0.500000 1.000000 0.01659(6) Uani 1 2 d S . P . .
S1 S 0.43784(5) 0.73691(5) 0.75644(4) 0.01992(10) Uani 1 1 d . . . . .
S2 S 0.78190(5) 0.40747(5) 0.79299(4) 0.01703(9) Uani 1 1 d . . . . .
P1 P 0.66908(5) 0.61525(5) 0.66070(4) 0.01563(10) Uani 1 1 d . . . . .
O1 O 0.65337(14) 0.59094(15) 0.53066(13) 0.0214(3) Uani 1 1 d . . . . .
O2 O 0.79503(15) 0.71679(14) 0.58518(13) 0.0214(3) Uani 1 1 d . . . . .
N1 N 0.37474(18) 0.34397(17) 0.97217(16) 0.0200(3) Uani 1 1 d . . . . .
N2 N 0.01926(19) 0.05402(17) 1.01210(16) 0.0211(3) Uani 1 1 d . . . . .
C1 C 0.8052(2) 0.5068(2) 0.4358(2) 0.0272(4) Uani 1 1 d . . . . .
H1A H 0.893396 0.438216 0.486862 0.033 Uiso 1 1 calc R U . . .
H1B H 0.849115 0.586777 0.345291 0.033 Uiso 1 1 calc R U . . .
C2 C 0.7606(3) 0.4041(3) 0.3987(3) 0.0435(6) Uani 1 1 d . . . . .
H2A H 0.859683 0.350611 0.331630 0.065 Uiso 1 1 calc R U . . .
H2B H 0.670229 0.472448 0.351581 0.065 Uiso 1 1 calc R U . . .
H2C H 0.722602 0.321908 0.488372 0.065 Uiso 1 1 calc R U . . .
C3 C 0.7498(3) 0.8799(2) 0.4819(2) 0.0328(4) Uani 1 1 d . . . . .
H3A H 0.652187 0.954195 0.533556 0.039 Uiso 1 1 calc R U . . .
H3B H 0.718928 0.877899 0.405200 0.039 Uiso 1 1 calc R U . . .
C4 C 0.8977(3) 0.9366(2) 0.4146(3) 0.0391(5) Uani 1 1 d . . . . .
H4A H 0.870227 1.045995 0.344756 0.059 Uiso 1 1 calc R U . . .
H4B H 0.993353 0.862601 0.363273 0.059 Uiso 1 1 calc R U . . .
H4C H 0.926936 0.938490 0.491230 0.059 Uiso 1 1 calc R U . . .
C5 C 0.2169(3) 0.3459(3) 1.0460(2) 0.0361(5) Uani 1 1 d . . . . .
H5 H 0.150836 0.412889 1.107210 0.043 Uiso 1 1 calc R U . . .
C6 C 0.1434(3) 0.2556(3) 1.0385(2) 0.0330(5) Uani 1 1 d . . . . .
H6 H 0.030023 0.261564 1.093482 0.040 Uiso 1 1 calc R U . . .
C7 C 0.2358(2) 0.1576(2) 0.95107(19) 0.0206(3) Uani 1 1 d . . . . .
C8 C 0.3986(3) 0.1568(3) 0.8726(3) 0.0456(6) Uani 1 1 d . . . . .
H8 H 0.466819 0.091970 0.809652 0.055 Uiso 1 1 calc R U . . .
C9 C 0.4625(3) 0.2513(3) 0.8861(3) 0.0394(5) Uani 1 1 d . . . . .
H9 H 0.574927 0.249402 0.830795 0.047 Uiso 1 1 calc R U . . .
C10 C 0.1685(2) 0.0547(2) 0.9409(2) 0.0239(4) Uani 1 1 d . . . . .
H10 H 0.238062 -0.012362 0.879892 0.029 Uiso 1 1 calc R U . . .
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd 0.1185 4.6533 '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 Cd N1 180.0 . 2_667
N1 Cd S1 90.27(3) . .
N1 Cd S1 89.73(3) 2_667 .
N1 Cd S1 89.73(3) . 2_667
N1 Cd S1 90.27(3) 2_667 2_667
S1 Cd S1 180.0 . 2_667
N1 Cd S2 89.70(3) . .
N1 Cd S2 90.30(3) 2_667 .
S1 Cd S2 77.898(12) . .
S1 Cd S2 102.102(12) 2_667 .
N1 Cd S2 90.30(3) . 2_667
N1 Cd S2 89.69(3) 2_667 2_667
S1 Cd S2 102.102(12) . 2_667
S1 Cd S2 77.897(12) 2_667 2_667
S2 Cd S2 180.0 . 2_667
P1 S1 Cd 83.564(18) . .
P1 S2 Cd 83.024(17) . .
O1 P1 O2 105.54(7) . .
O1 P1 S1 105.62(5) . .
O2 P1 S1 112.64(5) . .
O1 P1 S2 112.69(5) . .
O2 P1 S2 104.70(5) . .
S1 P1 S2 115.37(3) . .
C1 O1 P1 119.08(10) . .
C3 O2 P1 119.62(11) . .
C9 N1 C5 116.67(16) . .
C9 N1 Cd 121.75(12) . .
C5 N1 Cd 121.55(12) . .
C10 N2 N2 111.79(18) . 2_557
O1 C1 C2 108.35(15) . .
O1 C1 H1A 110.0 . .
C2 C1 H1A 110.0 . .
O1 C1 H1B 110.0 . .
C2 C1 H1B 110.0 . .
H1A C1 H1B 108.4 . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
O2 C3 C4 107.99(15) . .
O2 C3 H3A 110.1 . .
C4 C3 H3A 110.1 . .
O2 C3 H3B 110.1 . .
C4 C3 H3B 110.1 . .
H3A C3 H3B 108.4 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N1 C5 C6 123.65(18) . .
N1 C5 H5 118.2 . .
C6 C5 H5 118.2 . .
C7 C6 C5 119.48(18) . .
C7 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
C6 C7 C8 117.19(17) . .
C6 C7 C10 122.67(16) . .
C8 C7 C10 120.13(16) . .
C7 C8 C9 119.67(19) . .
C7 C8 H8 120.2 . .
C9 C8 H8 120.2 . .
N1 C9 C8 123.31(18) . .
N1 C9 H9 118.3 . .
C8 C9 H9 118.3 . .
N2 C10 C7 120.95(16) . .
N2 C10 H10 119.5 . .
C7 C10 H10 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cd N1 2.4755(13) .
Cd N1 2.4756(13) 2_667
Cd S1 2.6671(4) .
Cd S1 2.6671(4) 2_667
Cd S2 2.6821(4) .
Cd S2 2.6822(4) 2_667
S1 P1 1.9856(6) .
S2 P1 1.9934(6) .
P1 O1 1.5867(12) .
P1 O2 1.5933(12) .
O1 C1 1.465(2) .
O2 C3 1.462(2) .
N1 C9 1.324(3) .
N1 C5 1.330(2) .
N2 C10 1.266(2) .
N2 N2 1.409(3) 2_557
C1 C2 1.491(3) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.485(3) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.386(3) .
C5 H5 0.9500 .
C6 C7 1.373(3) .
C6 H6 0.9500 .
C7 C8 1.378(3) .
C7 C10 1.469(2) .
C8 C9 1.390(3) .
C8 H8 0.9500 .
C9 H9 0.9500 .
C10 H10 0.9500 .
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
O2 P1 O1 C1 59.32(14) . . . .
S1 P1 O1 C1 178.83(12) . . . .
S2 P1 O1 C1 -54.37(13) . . . .
O1 P1 O2 C3 62.14(15) . . . .
S1 P1 O2 C3 -52.61(15) . . . .
S2 P1 O2 C3 -178.72(13) . . . .
P1 O1 C1 C2 142.22(15) . . . .
P1 O2 C3 C4 -172.70(15) . . . .
C9 N1 C5 C6 1.0(3) . . . .
Cd N1 C5 C6 -177.33(18) . . . .
N1 C5 C6 C7 0.1(4) . . . .
C5 C6 C7 C8 -1.0(3) . . . .
C5 C6 C7 C10 178.1(2) . . . .
C6 C7 C8 C9 0.9(4) . . . .
C10 C7 C8 C9 -178.3(2) . . . .
C5 N1 C9 C8 -1.2(4) . . . .
Cd N1 C9 C8 177.2(2) . . . .
C7 C8 C9 N1 0.2(4) . . . .
N2 N2 C10 C7 -179.40(17) 2_557 . . .
C6 C7 C10 N2 1.0(3) . . . .
C8 C7 C10 N2 -180.0(2) . . . .
