#------------------------------------------------------------------------------
#$Date: 2022-04-04 10:34:54 +0300 (Mon, 04 Apr 2022) $
#$Revision: 274300 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/50/8105000.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_8105000
loop_
_publ_author_name
'Du, Zhong-Xiang'
'Li, Jun-Xia'
'Bai, Ruo-Fei'
_publ_section_title
;
 Crystal structure of
 catena-poly[μ2-4,4′-bipyridine-κ2N:N′)-tetrakis(μ2-2-((3,5,6-trichloropyridin-2-yl)oxy)acetato-κ2O:O′)dicobalt(II)],
 C19H10Cl6CoN3O6
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              15
_journal_page_last               17
_journal_paper_doi               10.1515/ncrs-2019-0434
_journal_volume                  235
_journal_year                    2019
_chemical_formula_moiety         '0.5(C38 H20 Cl12 Co2 N6 O12)'
_chemical_formula_sum            'C19 H10 Cl6 Co N3 O6'
_chemical_formula_weight         647.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1152(4)
_cell_length_b                   13.1152(4)
_cell_length_c                   14.2497(6)
_cell_measurement_reflns_used    1403
_cell_measurement_temperature    293.2(3)
_cell_measurement_theta_max      26.6720
_cell_measurement_theta_min      4.2170
_cell_volume                     2451.07(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -20.00  22.00   1.00    8.50    --  -13.80 -99.00  90.00   42
  2  ω    -51.00  17.00   1.00    8.50    --   14.82 -57.00-150.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0478113000
_diffrn_orient_matrix_UB_12      0.0199366000
_diffrn_orient_matrix_UB_13      0.0143532000
_diffrn_orient_matrix_UB_21      -0.0096861000
_diffrn_orient_matrix_UB_22      -0.0164008000
_diffrn_orient_matrix_UB_23      0.0465756000
_diffrn_orient_matrix_UB_31      0.0233857000
_diffrn_orient_matrix_UB_32      -0.0475240000
_diffrn_orient_matrix_UB_33      -0.0100429000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2720
_diffrn_reflns_point_group_measured_fraction_full 0.814
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.485
_diffrn_reflns_theta_min         3.606
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.087(17)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1844
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0417P)²+0.9515P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.552
_reflns_Friedel_fraction_full    0.613
_reflns_Friedel_fraction_max     0.603
_reflns_number_gt                1710
_reflns_number_total             1844
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0434_suppl.cif
_cod_data_source_block           ljx190512-2
_cod_original_cell_volume        2451.07(18)
_cod_database_code               8105000
_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_max   0.768
_shelx_estimated_absorpt_t_min   0.704
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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_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
Co1 Co 0.5000 0.0000 0.65336(5) 0.0227(2) Uani 1 2 d S T P . .
Cl1 Cl 0.65160(15) 0.44725(13) 0.74168(17) 0.0810(6) Uani 1 1 d . . . . .
Cl2 Cl 0.69339(19) 0.52911(17) 0.53514(19) 0.1002(8) Uani 1 1 d . . . . .
Cl3 Cl 0.8892(2) 0.1772(2) 0.46649(16) 0.1107(9) Uani 1 1 d . . . . .
O1 O 0.8284(3) 0.1313(3) 0.6567(3) 0.0463(10) Uani 1 1 d . . . . .
O2 O 0.6397(3) 0.0498(3) 0.6623(3) 0.0423(9) Uani 1 1 d . . . . .
O3 O 0.6414(3) 0.0479(3) 0.8200(2) 0.0416(10) Uani 1 1 d . . . . .
N1 N 0.7449(4) 0.2823(4) 0.6883(3) 0.0422(12) Uani 1 1 d . . . . .
N2 N 0.5000 0.0000 0.4994(3) 0.0346(12) Uani 1 2 d S T P . .
C1 C 0.7158(5) 0.3736(5) 0.6601(5) 0.0526(15) Uani 1 1 d . . . . .
C2 C 0.7345(5) 0.4103(5) 0.5709(5) 0.0572(18) Uani 1 1 d . . . . .
C3 C 0.7882(6) 0.3494(6) 0.5101(5) 0.066(2) Uani 1 1 d . . . . .
H3 H 0.8028 0.3720 0.4498 0.080 Uiso 1 1 calc R . . . .
C4 C 0.8201(5) 0.2550(5) 0.5391(5) 0.0548(17) Uani 1 1 d . . . . .
C5 C 0.7959(4) 0.2244(5) 0.6300(4) 0.0435(15) Uani 1 1 d . . . . .
C6 C 0.7909(4) 0.0955(4) 0.7452(5) 0.0443(12) Uani 1 1 d . . . . .
H6A H 0.7981 0.1492 0.7915 0.053 Uiso 1 1 calc R . . . .
H6B H 0.8320 0.0381 0.7656 0.053 Uiso 1 1 calc R . . . .
C7 C 0.6806(4) 0.0632(4) 0.7403(4) 0.0337(11) Uani 1 1 d . . . . .
C8 C 0.4241(5) -0.0394(5) 0.4503(4) 0.0500(16) Uani 1 1 d . . . . .
H8 H 0.3691 -0.0669 0.4828 0.060 Uiso 1 1 calc R . . . .
C9 C 0.4219(5) -0.0420(6) 0.3530(4) 0.0565(17) Uani 1 1 d . . . . .
H9 H 0.3672 -0.0724 0.3223 0.068 Uiso 1 1 calc R . . . .
C10 C 0.5000 0.0000 0.3016(4) 0.0401(15) Uani 1 2 d S T P . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
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
O2 Co1 Co1 86.25(12) 2_655 7_556
O2 Co1 Co1 86.25(12) . 7_556
O2 Co1 O2 172.5(2) . 2_655
O2 Co1 O3 90.2(2) . 7_556
O2 Co1 O3 90.2(2) 2_655 8_546
O2 Co1 O3 88.4(2) . 8_546
O2 Co1 O3 88.4(2) 2_655 7_556
O2 Co1 N2 93.75(12) 2_655 .
O2 Co1 N2 93.75(12) . .
O3 Co1 Co1 79.03(10) 8_546 7_556
O3 Co1 Co1 79.03(10) 7_556 7_556
O3 Co1 O3 158.1(2) 8_546 7_556
O3 Co1 N2 100.97(10) 8_546 .
O3 Co1 N2 100.97(10) 7_556 .
N2 Co1 Co1 180.0 . 7_556
C5 O1 C6 115.9(4) . .
C7 O2 Co1 120.7(3) . .
C7 O3 Co1 126.8(3) . 7_556
C5 N1 C1 118.7(5) . .
C8 N2 Co1 122.0(3) 2_655 .
C8 N2 Co1 122.0(3) . .
C8 N2 C8 116.1(6) 2_655 .
N1 C1 Cl1 116.3(5) . .
N1 C1 C2 123.0(6) . .
C2 C1 Cl1 120.7(5) . .
C1 C2 Cl2 122.0(6) . .
C3 C2 Cl2 120.0(5) . .
C3 C2 C1 118.0(6) . .
C2 C3 H3 120.2 . .
C4 C3 C2 119.5(6) . .
C4 C3 H3 120.2 . .
C3 C4 Cl3 121.2(5) . .
C3 C4 C5 118.0(7) . .
C5 C4 Cl3 120.8(5) . .
O1 C5 C4 116.8(6) . .
N1 C5 O1 120.5(5) . .
N1 C5 C4 122.7(6) . .
O1 C6 H6A 109.1 . .
O1 C6 H6B 109.1 . .
O1 C6 C7 112.3(5) . .
H6A C6 H6B 107.9 . .
C7 C6 H6A 109.1 . .
C7 C6 H6B 109.1 . .
O2 C7 O3 127.2(4) . .
O2 C7 C6 119.6(5) . .
O3 C7 C6 113.1(5) . .
N2 C8 H8 118.1 . .
N2 C8 C9 123.7(6) . .
C9 C8 H8 118.1 . .
C8 C9 H9 119.8 . .
C10 C9 C8 120.4(5) . .
C10 C9 H9 119.8 . .
C9 C10 C9 115.6(6) . 2_655
C9 C10 C10 122.2(3) 2_655 7
C9 C10 C10 122.2(3) . 7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Co1 2.7541(14) 7_556
Co1 O2 1.950(4) 2_655
Co1 O2 1.950(4) .
Co1 O3 1.995(4) 8_546
Co1 O3 1.995(4) 7_556
Co1 N2 2.194(5) .
Cl1 C1 1.730(7) .
Cl2 C2 1.725(7) .
Cl3 C4 1.712(7) .
O1 C5 1.348(7) .
O1 C6 1.433(8) .
O2 C7 1.246(7) .
O3 Co1 1.995(4) 7_556
O3 C7 1.263(6) .
N1 C1 1.321(8) .
N1 C5 1.309(7) .
N2 C8 1.322(6) 2_655
N2 C8 1.322(6) .
C1 C2 1.381(9) .
C2 C3 1.372(10) .
C3 H3 0.9300 .
C3 C4 1.371(10) .
C4 C5 1.393(8) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C6 C7 1.509(7) .
C8 H8 0.9300 .
C8 C9 1.387(8) .
C9 H9 0.9300 .
C9 C10 1.374(7) .
C10 C9 1.374(7) 2_655
C10 C10 1.471(12) 7
