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#$Date: 2022-06-29 12:27:40 +0300 (Wed, 29 Jun 2022) $
#$Revision: 276394 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/55/8105563.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_8105563
loop_
_publ_author_name
'Pang, Haixia'
'Zou, Xiaoqing'
'Tao, Defu'
'Li, Jun'
'Zhang, Jiahui'
'Zhang, Hong'
_publ_section_title
;
 Crystal structure of
 catena-poly[dichlorido-(μ2-1,5-dimethyl-2-phenyl-4-((pyridin-4-ylmethylene)amino)-1,2-dihydro-3H-pyrazol-3-one-κ2
 N:O)cobalt(II)] -- methanol (1/1), C18H20Cl2CoN4O2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              125
_journal_page_last               126
_journal_paper_doi               10.1515/ncrs-2018-0222
_journal_volume                  234
_journal_year                    2018
_chemical_formula_sum            'C18 H20 Cl2 Co N4 O2'
_chemical_formula_weight         454.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 94.196(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4744(18)
_cell_length_b                   18.084(3)
_cell_length_c                   12.290(2)
_cell_measurement_reflns_used    1710
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.96
_cell_measurement_theta_min      2.43
_cell_volume                     2100.1(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2 [2]'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014) [4]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008) [3]'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0932
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18542
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.934
_diffrn_reflns_theta_min         2.007
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5019
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1393
_refine_ls_R_factor_gt           0.0559
_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)+(0.0736P)²+0.2706P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2399
_reflns_number_total             5019
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2018-0222_suppl.cif
_cod_data_source_block           mo
_cod_original_cell_volume        2100.1(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8105563
_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   0.899
_shelx_estimated_absorpt_t_max   0.947
loop_
_space_group_symop_operation_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_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 0.24525(6) 0.20112(3) 0.35000(5) 0.0502(2) Uani 1 1 d . . . . .
C1 C 0.2319(5) -0.1399(3) 0.1901(4) 0.0663(14) Uani 1 1 d . . . . .
H1 H 0.1469 -0.1464 0.1484 0.080 Uiso 1 1 calc R U . . .
C2 C 0.2706(5) -0.0703(3) 0.2224(4) 0.0681(14) Uani 1 1 d . . . . .
H2 H 0.2113 -0.0307 0.2032 0.082 Uiso 1 1 calc R U . . .
C3 C 0.3973(5) -0.0577(2) 0.2835(4) 0.0500(11) Uani 1 1 d . . . . .
C4 C 0.4764(4) -0.1196(2) 0.3127(4) 0.0515(11) Uani 1 1 d . . . . .
H4 H 0.5599 -0.1145 0.3568 0.062 Uiso 1 1 calc R U . . .
C5 C 0.4335(5) -0.1879(2) 0.2775(4) 0.0529(11) Uani 1 1 d . . . . .
H5 H 0.4905 -0.2284 0.2966 0.063 Uiso 1 1 calc R U . . .
C6 C 0.4433(5) 0.0166(2) 0.3147(4) 0.0536(11) Uani 1 1 d . . . . .
H6 H 0.3857 0.0568 0.2952 0.064 Uiso 1 1 calc R U . . .
C7 C 0.6091(4) 0.0975(2) 0.3945(3) 0.0442(10) Uani 1 1 d . . . . .
C8 C 0.7370(4) 0.1094(2) 0.4516(4) 0.0483(10) Uani 1 1 d . . . . .
C9 C 0.5498(4) 0.1678(2) 0.3672(4) 0.0473(10) Uani 1 1 d . . . . .
C10 C 0.8421(5) 0.0535(3) 0.4948(4) 0.0654(13) Uani 1 1 d . . . . .
H10A H 0.9292 0.0601 0.4607 0.098 Uiso 1 1 calc R U . . .
H10B H 0.8060 0.0047 0.4791 0.098 Uiso 1 1 calc R U . . .
H10C H 0.8588 0.0595 0.5722 0.098 Uiso 1 1 calc R U . . .
C11 C 0.8778(5) 0.2222(3) 0.5135(5) 0.0768(16) Uani 1 1 d . . . . .
H11A H 0.8475 0.2516 0.5725 0.115 Uiso 1 1 calc R U . . .
H11B H 0.9162 0.2538 0.4603 0.115 Uiso 1 1 calc R U . . .
H11C H 0.9491 0.1879 0.5410 0.115 Uiso 1 1 calc R U . . .
C12 C 0.6394(4) 0.2969(2) 0.3981(4) 0.0490(10) Uani 1 1 d . . . . .
C13 C 0.6162(5) 0.3428(3) 0.4830(4) 0.0661(14) Uani 1 1 d . . . . .
H13 H 0.6028 0.3238 0.5518 0.079 Uiso 1 1 calc R U . . .
C14 C 0.6130(7) 0.4179(3) 0.4648(6) 0.092(2) Uani 1 1 d . . . . .
H14 H 0.5973 0.4498 0.5220 0.110 Uiso 1 1 calc R U . . .
C15 C 0.6324(7) 0.4463(3) 0.3642(8) 0.102(2) Uani 1 1 d . . . . .
H15 H 0.6304 0.4971 0.3530 0.122 Uiso 1 1 calc R U . . .
C16 C 0.6548(7) 0.3998(4) 0.2810(6) 0.097(2) Uani 1 1 d . . . . .
H16 H 0.6669 0.4190 0.2121 0.116 Uiso 1 1 calc R U . . .
C17 C 0.6596(5) 0.3254(3) 0.2968(5) 0.0712(15) Uani 1 1 d . . . . .
H17 H 0.6765 0.2940 0.2393 0.085 Uiso 1 1 calc R U . . .
Cl1 Cl 0.26123(16) 0.21811(11) 0.53018(11) 0.0994(6) Uani 1 1 d . . . . .
Cl2 Cl 0.08905(13) 0.11800(7) 0.28153(12) 0.0747(4) Uani 1 1 d . . . . .
N1 N 0.3118(4) -0.19910(18) 0.2163(3) 0.0490(9) Uani 1 1 d . . . . .
N2 N 0.5605(4) 0.02693(18) 0.3679(3) 0.0485(9) Uani 1 1 d . . . . .
N3 N 0.7590(3) 0.1822(2) 0.4636(3) 0.0517(9) Uani 1 1 d . . . . .
N4 N 0.6432(3) 0.21862(18) 0.4131(3) 0.0486(9) Uani 1 1 d . . . . .
C18 C 0.542(2) 0.0874(10) 0.0512(15) 0.251(8) Uani 0.877(14) 1 d D U P A 1
H18A H 0.4662 0.1026 0.0939 0.377 Uiso 0.877(14) 1 d R U P A 1
H18B H 0.5380 0.0349 0.0405 0.377 Uiso 0.877(14) 1 d R U P A 1
H18C H 0.5331 0.1119 -0.0183 0.377 Uiso 0.877(14) 1 d R U P A 1
O2 O 0.679(3) 0.1050(11) 0.0933(16) 0.359(11) Uani 0.877(14) 1 d D U P A 1
H2A H 0.6842 0.1494 0.1065 0.538 Uiso 0.877(14) 1 calc R U P A 1
C18' C 0.778(18) 0.115(8) 0.065(10) 0.251(8) Uani 0.123(14) 1 d D U P A 2
H18D H 0.8109 0.1263 -0.0050 0.377 Uiso 0.123(14) 1 d R U P A 2
H18E H 0.6788 0.1255 0.0647 0.377 Uiso 0.123(14) 1 d R U P A 2
H18F H 0.7939 0.0634 0.0808 0.377 Uiso 0.123(14) 1 d R U P A 2
O2' O 0.814(13) 0.154(6) 0.163(10) 0.359(11) Uani 0.123(14) 1 d D U P A 2
H2' H 0.8999 0.1515 0.1784 0.538 Uiso 0.123(14) 1 calc R U P A 2
O1 O 0.4388(3) 0.18744(15) 0.3108(2) 0.0519(8) 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'
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 N1 103.95(14) . 2
O1 Co1 Cl1 105.47(10) . .
N1 Co1 Cl1 105.79(12) 2 .
O1 Co1 Cl2 115.61(10) . .
N1 Co1 Cl2 107.25(10) 2 .
Cl1 Co1 Cl2 117.54(7) . .
N1 C1 C2 122.3(4) . .
N1 C1 H1 118.9 . .
C2 C1 H1 118.9 . .
C1 C2 C3 120.9(4) . .
C1 C2 H2 119.6 . .
C3 C2 H2 119.6 . .
C4 C3 C2 116.1(4) . .
C4 C3 C6 122.3(4) . .
C2 C3 C6 121.7(4) . .
C5 C4 C3 120.7(4) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
N1 C5 C4 122.5(4) . .
N1 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
N2 C6 C3 120.6(4) . .
N2 C6 H6 119.7 . .
C3 C6 H6 119.7 . .
C8 C7 N2 122.0(4) . .
C8 C7 C9 107.5(4) . .
N2 C7 C9 130.4(4) . .
N3 C8 C7 109.5(4) . .
N3 C8 C10 122.3(4) . .
C7 C8 C10 128.2(4) . .
O1 C9 N4 121.6(4) . .
O1 C9 C7 132.7(4) . .
N4 C9 C7 105.7(4) . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
N3 C11 H11A 109.5 . .
N3 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N3 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C13 C12 C17 120.4(4) . .
C13 C12 N4 120.6(4) . .
C17 C12 N4 119.0(4) . .
C12 C13 C14 118.6(5) . .
C12 C13 H13 120.7 . .
C14 C13 H13 120.7 . .
C15 C14 C13 121.1(6) . .
C15 C14 H14 119.4 . .
C13 C14 H14 119.4 . .
C16 C15 C14 119.4(6) . .
C16 C15 H15 120.3 . .
C14 C15 H15 120.3 . .
C15 C16 C17 120.8(6) . .
C15 C16 H16 119.6 . .
C17 C16 H16 119.6 . .
C16 C17 C12 119.7(6) . .
C16 C17 H17 120.2 . .
C12 C17 H17 120.2 . .
C1 N1 C5 117.5(4) . .
C1 N1 Co1 118.9(3) . 2_545
C5 N1 Co1 123.3(3) . 2_545
C6 N2 C7 121.6(4) . .
C8 N3 N4 107.9(3) . .
C8 N3 C11 130.7(4) . .
N4 N3 C11 121.4(4) . .
C9 N4 N3 109.4(3) . .
C9 N4 C12 127.0(4) . .
N3 N4 C12 122.7(3) . .
O2 C18 H18A 116.5 . .
O2 C18 H18B 107.6 . .
H18A C18 H18B 109.5 . .
O2 C18 H18C 104.1 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C18 O2 H2A 109.5 . .
O2' C18' H18D 125.4 . .
O2' C18' H18E 94.6 . .
H18D C18' H18E 109.5 . .
O2' C18' H18F 107.0 . .
H18D C18' H18F 109.5 . .
H18E C18' H18F 109.5 . .
C18' O2' H2' 109.5 . .
C9 O1 Co1 131.3(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 1.946(3) .
Co1 N1 2.037(3) 2
Co1 Cl1 2.2298(16) .
Co1 Cl2 2.2306(14) .
C1 N1 1.338(6) .
C1 C2 1.361(6) .
C1 H1 0.9300 .
C2 C3 1.388(6) .
C2 H2 0.9300 .
C3 C4 1.379(6) .
C3 C6 1.455(6) .
C4 C5 1.362(6) .
C4 H4 0.9300 .
C5 N1 1.345(5) .
C5 H5 0.9300 .
C6 N2 1.260(5) .
C6 H6 0.9300 .
C7 C8 1.372(6) .
C7 N2 1.388(5) .
C7 C9 1.421(6) .
C8 N3 1.339(5) .
C8 C10 1.489(6) .
C9 O1 1.266(5) .
C9 N4 1.369(5) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 N3 1.437(6) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 C13 1.363(6) .
C12 C17 1.374(7) .
C12 N4 1.428(5) .
C13 C14 1.376(7) .
C13 H13 0.9300 .
C14 C15 1.363(9) .
C14 H14 0.9300 .
C15 C16 1.353(9) .
C15 H15 0.9300 .
C16 C17 1.359(8) .
C16 H16 0.9300 .
C17 H17 0.9300 .
N1 Co1 2.037(3) 2_545
N3 N4 1.387(4) .
C18 O2 1.399(10) .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
O2 H2A 0.8200 .
C18' O2' 1.423(10) .
C18' H18D 0.9600 .
C18' H18E 0.9600 .
C18' H18F 0.9600 .
O2' H2' 0.8200 .
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
O2' H2' Cl2 0.82 2.20 2.96(12) 153.8 1_655
C17 H17 Cl1 0.93 2.76 3.570(6) 146.6 4_665
C10 H10A Cl2 0.96 2.95 3.821(5) 150.8 1_655
C6 H6 O1 0.93 2.42 3.091(5) 128.9 .
C4 H4 Cl1 0.93 2.82 3.519(4) 132.6 3_656
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
N1 C1 C2 C3 0.9(9) . . . .
C1 C2 C3 C4 -2.8(8) . . . .
C1 C2 C3 C6 177.3(5) . . . .
C2 C3 C4 C5 3.3(7) . . . .
C6 C3 C4 C5 -176.7(4) . . . .
C3 C4 C5 N1 -2.0(7) . . . .
C4 C3 C6 N2 1.8(7) . . . .
C2 C3 C6 N2 -178.2(5) . . . .
N2 C7 C8 N3 178.4(4) . . . .
C9 C7 C8 N3 1.5(5) . . . .
N2 C7 C8 C10 -0.7(7) . . . .
C9 C7 C8 C10 -177.6(4) . . . .
C8 C7 C9 O1 175.6(5) . . . .
N2 C7 C9 O1 -0.9(8) . . . .
C8 C7 C9 N4 -2.3(5) . . . .
N2 C7 C9 N4 -178.8(4) . . . .
C17 C12 C13 C14 0.2(7) . . . .
N4 C12 C13 C14 -179.8(5) . . . .
C12 C13 C14 C15 0.0(9) . . . .
C13 C14 C15 C16 0.2(10) . . . .
C14 C15 C16 C17 -0.8(11) . . . .
C15 C16 C17 C12 1.0(9) . . . .
C13 C12 C17 C16 -0.7(8) . . . .
N4 C12 C17 C16 179.3(5) . . . .
C2 C1 N1 C5 0.6(8) . . . .
C2 C1 N1 Co1 -173.4(4) . . . 2_545
C4 C5 N1 C1 0.0(7) . . . .
C4 C5 N1 Co1 173.6(4) . . . 2_545
C3 C6 N2 C7 177.3(4) . . . .
C8 C7 N2 C6 -179.5(4) . . . .
C9 C7 N2 C6 -3.3(7) . . . .
C7 C8 N3 N4 -0.1(5) . . . .
C10 C8 N3 N4 179.0(4) . . . .
C7 C8 N3 C11 -177.7(5) . . . .
C10 C8 N3 C11 1.5(8) . . . .
O1 C9 N4 N3 -175.9(4) . . . .
C7 C9 N4 N3 2.2(5) . . . .
O1 C9 N4 C12 -6.0(7) . . . .
C7 C9 N4 C12 172.1(4) . . . .
C8 N3 N4 C9 -1.4(5) . . . .
C11 N3 N4 C9 176.5(4) . . . .
C8 N3 N4 C12 -171.8(4) . . . .
C11 N3 N4 C12 6.1(6) . . . .
C13 C12 N4 C9 114.2(5) . . . .
C17 C12 N4 C9 -65.8(6) . . . .
C13 C12 N4 N3 -77.1(6) . . . .
C17 C12 N4 N3 102.8(5) . . . .
N4 C9 O1 Co1 -95.4(5) . . . .
C7 C9 O1 Co1 87.0(6) . . . .
