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#$Date: 2022-09-16 12:14:05 +0300 (Fri, 16 Sep 2022) $
#$Revision: 277915 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/57/8105780.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_8105780
loop_
_publ_author_name
'Pang, Haixia'
'He, Xiong'
'Feng, Xiang'
'Yuan, Ximing'
_publ_section_title
;
 Crystal structure of
 diaqua-dichlorido-bis(μ2-2-(((1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)imino)methyl)phenolato-κ4
 O:O,N,O′)dicobalt(II), C36H36Cl2N6O6Co2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              563
_journal_page_last               565
_journal_paper_doi               10.1515/ncrs-2018-0560
_journal_volume                  234
_journal_year                    2019
_chemical_formula_sum            'C36 H36 Cl2 Co2 N6 O6'
_chemical_formula_weight         837.47
_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   mixed
_cell_angle_alpha                73.589(2)
_cell_angle_beta                 84.396(2)
_cell_angle_gamma                74.709(2)
_cell_formula_units_Z            1
_cell_length_a                   7.4399(9)
_cell_length_b                   9.5362(11)
_cell_length_c                   13.1754(15)
_cell_measurement_reflns_used    3925
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.88
_cell_measurement_theta_min      2.84
_cell_volume                     864.68(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2 [1]'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014) [3]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990) [2]'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7072
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.612
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       block
_exptl_crystal_F_000             430
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3723
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0306
_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)+(0.0558P)²+0.4876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3231
_reflns_number_total             3723
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2018-0560_suppl.cif
_cod_data_source_block           mo
_cod_database_code               8105780
_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   0.800
_shelx_estimated_absorpt_t_max   0.892
_publcif_funding_html
;
;
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
Co1 Co 0.57715(4) 0.90182(3) 0.91716(2) 0.02184(12) Uani 1 1 d . . . . .
C1 C 0.5425(3) 0.7457(3) 1.15178(18) 0.0224(5) Uani 1 1 d . . . . .
C2 C 0.6033(3) 0.5999(3) 1.13353(19) 0.0241(5) Uani 1 1 d . . . . .
C3 C 0.5969(4) 0.4720(3) 1.2189(2) 0.0310(5) Uani 1 1 d . . . . .
H3 H 0.6347 0.3769 1.2068 0.037 Uiso 1 1 calc R U . . .
C4 C 0.5372(4) 0.4830(3) 1.3189(2) 0.0343(6) Uani 1 1 d . . . . .
H4 H 0.5337 0.3972 1.3737 0.041 Uiso 1 1 calc R U . . .
C5 C 0.4821(4) 0.6252(3) 1.3360(2) 0.0374(6) Uani 1 1 d . . . . .
H5 H 0.4427 0.6342 1.4036 0.045 Uiso 1 1 calc R U . . .
C6 C 0.4842(4) 0.7529(3) 1.2557(2) 0.0325(6) Uani 1 1 d . . . . .
H6 H 0.4464 0.8465 1.2702 0.039 Uiso 1 1 calc R U . . .
C7 C 0.6767(3) 0.5685(3) 1.03451(19) 0.0264(5) Uani 1 1 d . . . . .
H7 H 0.7149 0.4678 1.0336 0.032 Uiso 1 1 calc R U . . .
C8 C 0.7702(3) 0.6335(3) 0.85369(18) 0.0235(5) Uani 1 1 d . . . . .
C9 C 0.8704(3) 0.5060(3) 0.82495(19) 0.0252(5) Uani 1 1 d . . . . .
C10 C 0.7474(3) 0.7572(3) 0.76184(19) 0.0255(5) Uani 1 1 d . . . . .
C11 C 0.9301(4) 0.3450(3) 0.8869(2) 0.0355(6) Uani 1 1 d . . . . .
H11A H 0.8403 0.2924 0.8799 0.053 Uiso 1 1 calc R U . . .
H11B H 0.9391 0.3398 0.9601 0.053 Uiso 1 1 calc R U . . .
H11C H 1.0495 0.2991 0.8605 0.053 Uiso 1 1 calc R U . . .
C12 C 0.9794(5) 0.4499(3) 0.6508(2) 0.0452(7) Uani 1 1 d . . . . .
H12A H 1.1023 0.4580 0.6247 0.068 Uiso 1 1 calc R U . . .
H12B H 0.8973 0.4802 0.5924 0.068 Uiso 1 1 calc R U . . .
H12C H 0.9834 0.3473 0.6891 0.068 Uiso 1 1 calc R U . . .
C13 C 0.8636(4) 0.7790(3) 0.57385(19) 0.0291(5) Uani 1 1 d . . . . .
C14 C 1.0445(4) 0.7862(3) 0.5394(2) 0.0391(6) Uani 1 1 d . . . . .
H14 H 1.1428 0.7398 0.5856 0.047 Uiso 1 1 calc R U . . .
C15 C 1.0775(5) 0.8623(4) 0.4367(3) 0.0499(8) Uani 1 1 d . . . . .
H15 H 1.1985 0.8672 0.4139 0.060 Uiso 1 1 calc R U . . .
C16 C 0.9341(6) 0.9312(4) 0.3674(2) 0.0551(9) Uani 1 1 d . . . . .
H16 H 0.9581 0.9812 0.2979 0.066 Uiso 1 1 calc R U . . .
C17 C 0.7524(6) 0.9255(4) 0.4020(3) 0.0567(9) Uani 1 1 d . . . . .
H17 H 0.6542 0.9736 0.3559 0.068 Uiso 1 1 calc R U . . .
C18 C 0.7183(5) 0.8482(4) 0.5050(2) 0.0431(7) Uani 1 1 d . . . . .
H18 H 0.5974 0.8430 0.5278 0.052 Uiso 1 1 calc R U . . .
Cl1 Cl 0.26885(9) 0.87593(8) 0.88696(5) 0.03302(16) Uani 1 1 d . . . . .
N3 N 0.6936(3) 0.6686(2) 0.94707(15) 0.0231(4) Uani 1 1 d . . . . .
N4 N 0.9118(3) 0.5467(2) 0.72054(17) 0.0315(5) Uani 1 1 d . . . . .
N5 N 0.8291(3) 0.7001(2) 0.68013(17) 0.0318(5) Uani 1 1 d . . . . .
O1 O 0.5404(2) 0.87214(18) 1.07690(13) 0.0239(3) Uani 1 1 d . . . . .
O2 O 0.6689(3) 0.89351(19) 0.75584(13) 0.0296(4) Uani 1 1 d . . . . .
O3 O 0.8275(3) 0.9675(2) 0.92313(18) 0.0390(5) Uani 1 1 d D . . . .
H3A H 0.947(3) 0.932(4) 0.913(3) 0.059 Uiso 1 1 d D U . . .
H3B H 0.822(5) 1.007(4) 0.972(2) 0.059 Uiso 1 1 d D U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Co Co 0.3494 0.9721 '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
O1 Co1 N3 88.25(7) . .
O1 Co1 O1 79.41(7) . 2_677
N3 Co1 O1 167.58(7) . 2_677
O1 Co1 O3 89.46(8) . .
N3 Co1 O3 97.69(8) . .
O1 Co1 O3 80.96(7) 2_677 .
O1 Co1 O2 167.74(7) . .
N3 Co1 O2 81.41(7) . .
O1 Co1 O2 110.68(6) 2_677 .
O3 Co1 O2 85.45(8) . .
O1 Co1 Cl1 96.03(5) . .
N3 Co1 Cl1 92.29(6) . .
O1 Co1 Cl1 90.39(5) 2_677 .
O3 Co1 Cl1 168.76(6) . .
O2 Co1 Cl1 90.97(5) . .
O1 C1 C6 119.3(2) . .
O1 C1 C2 123.3(2) . .
C6 C1 C2 117.4(2) . .
C3 C2 C1 118.7(2) . .
C3 C2 C7 115.5(2) . .
C1 C2 C7 125.8(2) . .
C4 C3 C2 122.4(2) . .
C4 C3 H3 118.8 . .
C2 C3 H3 118.8 . .
C3 C4 C5 118.2(2) . .
C3 C4 H4 120.9 . .
C5 C4 H4 120.9 . .
C6 C5 C4 121.6(2) . .
C6 C5 H5 119.2 . .
C4 C5 H5 119.2 . .
C5 C6 C1 121.5(2) . .
C5 C6 H6 119.2 . .
C1 C6 H6 119.2 . .
N3 C7 C2 125.4(2) . .
N3 C7 H7 117.3 . .
C2 C7 H7 117.3 . .
C9 C8 N3 136.5(2) . .
C9 C8 C10 108.1(2) . .
N3 C8 C10 115.3(2) . .
N4 C9 C8 108.0(2) . .
N4 C9 C11 120.2(2) . .
C8 C9 C11 131.8(2) . .
O2 C10 N5 126.1(2) . .
O2 C10 C8 127.5(2) . .
N5 C10 C8 106.4(2) . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N4 C12 H12A 109.5 . .
N4 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
N4 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C18 C13 C14 119.9(3) . .
C18 C13 N5 120.3(3) . .
C14 C13 N5 119.8(2) . .
C15 C14 C13 119.7(3) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C16 C15 C14 120.9(3) . .
C16 C15 H15 119.5 . .
C14 C15 H15 119.5 . .
C15 C16 C17 119.6(3) . .
C15 C16 H16 120.2 . .
C17 C16 H16 120.2 . .
C18 C17 C16 119.9(3) . .
C18 C17 H17 120.1 . .
C16 C17 H17 120.1 . .
C13 C18 C17 120.1(3) . .
C13 C18 H18 120.0 . .
C17 C18 H18 120.0 . .
C7 N3 C8 123.7(2) . .
C7 N3 Co1 125.81(16) . .
C8 N3 Co1 109.90(15) . .
C9 N4 N5 108.81(19) . .
C9 N4 C12 127.9(2) . .
N5 N4 C12 120.9(2) . .
C10 N5 N4 108.5(2) . .
C10 N5 C13 128.8(2) . .
N4 N5 C13 121.7(2) . .
C1 O1 Co1 128.46(15) . .
C1 O1 Co1 128.79(14) . 2_677
Co1 O1 Co1 100.59(7) . 2_677
C10 O2 Co1 105.82(15) . .
Co1 O3 H3A 137(2) . .
Co1 O3 H3B 111(2) . .
H3A O3 H3B 104(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.0436(16) .
Co1 N3 2.099(2) .
Co1 O1 2.1225(16) 2_677
Co1 O3 2.131(2) .
Co1 O2 2.1848(17) .
Co1 Cl1 2.4521(7) .
C1 O1 1.322(3) .
C1 C6 1.410(3) .
C1 C2 1.426(3) .
C2 C3 1.414(3) .
C2 C7 1.444(3) .
C3 C4 1.373(4) .
C3 H3 0.9300 .
C4 C5 1.385(4) .
C4 H4 0.9300 .
C5 C6 1.372(4) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 N3 1.292(3) .
C7 H7 0.9300 .
C8 C9 1.380(3) .
C8 N3 1.395(3) .
C8 C10 1.419(3) .
C9 N4 1.348(3) .
C9 C11 1.491(3) .
C10 O2 1.260(3) .
C10 N5 1.361(3) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 N4 1.447(3) .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C18 1.380(4) .
C13 C14 1.391(4) .
C13 N5 1.425(3) .
C14 C15 1.376(4) .
C14 H14 0.9300 .
C15 C16 1.373(5) .
C15 H15 0.9300 .
C16 C17 1.394(6) .
C16 H16 0.9300 .
C17 C18 1.384(5) .
C17 H17 0.9300 .
C18 H18 0.9300 .
N4 N5 1.397(3) .
O1 Co1 2.1225(16) 2_677
O3 H3A 0.877(18) .
O3 H3B 0.831(18) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3B Cl1 0.831(18) 2.379(19) 3.194(2) 167(3) 2_677
O3 H3A Cl1 0.877(18) 2.323(19) 3.192(2) 171(3) 1_655
C6 H6 O2 0.93 2.34 3.226(3) 160.2 2_677
C6 H6 O2 0.93 2.34 3.226(3) 160.2 2_677
O3 H3B Cl1 0.831(18) 2.379(19) 3.194(2) 167(3) 2_677
O3 H3A Cl1 0.877(18) 2.323(19) 3.192(2) 171(3) 1_655
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
O1 C1 C2 C3 -179.0(2) . . . .
C6 C1 C2 C3 1.8(3) . . . .
O1 C1 C2 C7 2.6(4) . . . .
C6 C1 C2 C7 -176.7(2) . . . .
C1 C2 C3 C4 -1.0(4) . . . .
C7 C2 C3 C4 177.6(2) . . . .
C2 C3 C4 C5 -0.3(4) . . . .
C3 C4 C5 C6 0.8(5) . . . .
C4 C5 C6 C1 0.0(5) . . . .
O1 C1 C6 C5 179.4(2) . . . .
C2 C1 C6 C5 -1.3(4) . . . .
C3 C2 C7 N3 179.6(2) . . . .
C1 C2 C7 N3 -1.8(4) . . . .
N3 C8 C9 N4 -177.3(3) . . . .
C10 C8 C9 N4 0.9(3) . . . .
N3 C8 C9 C11 3.9(5) . . . .
C10 C8 C9 C11 -177.9(3) . . . .
C9 C8 C10 O2 -177.6(3) . . . .
N3 C8 C10 O2 1.0(4) . . . .
C9 C8 C10 N5 1.9(3) . . . .
N3 C8 C10 N5 -179.5(2) . . . .
C18 C13 C14 C15 -0.1(4) . . . .
N5 C13 C14 C15 179.9(3) . . . .
C13 C14 C15 C16 -0.1(5) . . . .
C14 C15 C16 C17 0.8(5) . . . .
C15 C16 C17 C18 -1.3(5) . . . .
C14 C13 C18 C17 -0.4(4) . . . .
N5 C13 C18 C17 179.6(3) . . . .
C16 C17 C18 C13 1.1(5) . . . .
C2 C7 N3 C8 178.1(2) . . . .
C2 C7 N3 Co1 -11.7(4) . . . .
C9 C8 N3 C7 -12.5(5) . . . .
C10 C8 N3 C7 169.4(2) . . . .
C9 C8 N3 Co1 175.9(3) . . . .
C10 C8 N3 Co1 -2.2(3) . . . .
C8 C9 N4 N5 -3.2(3) . . . .
C11 C9 N4 N5 175.7(2) . . . .
C8 C9 N4 C12 -165.8(3) . . . .
C11 C9 N4 C12 13.1(4) . . . .
O2 C10 N5 N4 175.7(2) . . . .
C8 C10 N5 N4 -3.8(3) . . . .
O2 C10 N5 C13 7.5(5) . . . .
C8 C10 N5 C13 -172.0(3) . . . .
C9 N4 N5 C10 4.5(3) . . . .
C12 N4 N5 C10 168.5(3) . . . .
C9 N4 N5 C13 173.7(2) . . . .
C12 N4 N5 C13 -22.3(4) . . . .
C18 C13 N5 C10 -72.8(4) . . . .
C14 C13 N5 C10 107.2(3) . . . .
C18 C13 N5 N4 120.3(3) . . . .
C14 C13 N5 N4 -59.6(4) . . . .
C6 C1 O1 Co1 -169.76(18) . . . .
C2 C1 O1 Co1 11.0(3) . . . .
C6 C1 O1 Co1 -9.8(3) . . . 2_677
C2 C1 O1 Co1 170.96(16) . . . 2_677
N5 C10 O2 Co1 -178.6(2) . . . .
C8 C10 O2 Co1 0.7(3) . . . .
