#------------------------------------------------------------------------------
#$Date: 2022-05-03 10:05:03 +0200 (mar 03 de may de 2022) $
#$Revision: 274836 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/51/8105106.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_8105106
loop_
_publ_author_name
'Huang, Junjie'
'Lu, Yang'
'Lu, Hui'
'Sun, Jianhua'
_publ_section_title
;
 Crystal structure of bis(hydroxydi(pyridin-2-yl)methanolato-κ3
 N,N′O)cobalt(III) 7,7,8,8-tetracyanoquinodimethane, C34H22CoN8O4
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              357
_journal_page_last               358
_journal_paper_doi               10.1515/ncrs-2019-0668
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C22 H18 Co N4 O4, C12 H4 N4 '
_chemical_formula_sum            'C34 H22 Co N8 O4'
_chemical_formula_weight         665.52
_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
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                104.743(2)
_cell_angle_beta                 94.606(2)
_cell_angle_gamma                90.934(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8423(10)
_cell_length_b                   8.8919(13)
_cell_length_c                   12.6319(18)
_cell_measurement_reflns_used    4580
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.37
_cell_volume                     740.30(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0217
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6587
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.489
_diffrn_reflns_theta_min         1.673
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       block
_exptl_crystal_F_000             341
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0369
_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)+(0.0720P)²+0.4195P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2505
_reflns_number_total             2720
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0668_suppl.cif
_cod_data_source_block           mo_20151222D_0m
_cod_database_code               8105106
_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   0.922
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2014-3
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
C1 C 0.0628(4) 0.5909(4) 0.1667(2) 0.0495(7) Uani 1 1 d . . . . .
C2 C 0.1446(4) 0.4646(4) 0.0934(2) 0.0422(6) Uani 1 1 d . . . . .
C3 C 0.0359(4) 0.3213(4) 0.0691(2) 0.0479(7) Uani 1 1 d . . . . .
C4 C 0.3219(4) 0.4808(3) 0.0465(2) 0.0357(5) Uani 1 1 d . . . . .
C5 C 0.4295(4) 0.6258(3) 0.0739(2) 0.0396(6) Uani 1 1 d . . . . .
H5 H 0.3821 0.7103 0.1237 0.047 Uiso 1 1 calc R U . . .
C6 C 0.4006(4) 0.3560(3) -0.0292(2) 0.0392(6) Uani 1 1 d . . . . .
H6 H 0.3346 0.2593 -0.0489 0.047 Uiso 1 1 calc R U . . .
C7 C 0.4188(4) 0.3133(3) 0.6338(2) 0.0361(5) Uani 1 1 d . . . . .
H7 H 0.3060 0.2724 0.6541 0.043 Uiso 1 1 calc R U . . .
C8 C 0.4700(5) 0.4696(3) 0.6750(2) 0.0470(7) Uani 1 1 d . . . . .
H8 H 0.3932 0.5339 0.7237 0.056 Uiso 1 1 calc R U . . .
C9 C 0.6358(5) 0.5287(3) 0.6430(2) 0.0490(7) Uani 1 1 d . . . . .
H9 H 0.6708 0.6339 0.6699 0.059 Uiso 1 1 calc R U . . .
C10 C 0.7505(4) 0.4338(3) 0.5715(2) 0.0419(6) Uani 1 1 d . . . . .
H10 H 0.8623 0.4734 0.5492 0.050 Uiso 1 1 calc R U . . .
C11 C 0.6948(3) 0.2768(3) 0.53321(19) 0.0309(5) Uani 1 1 d . . . . .
C12 C 0.7934(3) 0.1464(3) 0.4539(2) 0.0318(5) Uani 1 1 d . . . . .
C13 C 0.6633(3) 0.1120(3) 0.34610(19) 0.0307(5) Uani 1 1 d . . . . .
C14 C 0.7017(4) 0.1423(3) 0.2482(2) 0.0405(6) Uani 1 1 d . . . . .
H14 H 0.8222 0.1860 0.2400 0.049 Uiso 1 1 calc R U . . .
C15 C 0.5549(5) 0.1056(3) 0.1613(2) 0.0473(7) Uani 1 1 d . . . . .
H15 H 0.5766 0.1251 0.0942 0.057 Uiso 1 1 calc R U . . .
C16 C 0.3782(5) 0.0406(3) 0.1752(2) 0.0448(6) Uani 1 1 d . . . . .
H16 H 0.2788 0.0182 0.1182 0.054 Uiso 1 1 calc R U . . .
C17 C 0.3495(4) 0.0087(3) 0.2749(2) 0.0341(5) Uani 1 1 d . . . . .
H17 H 0.2311 -0.0370 0.2843 0.041 Uiso 1 1 calc R U . . .
Co1 Co 0.5000 0.0000 0.5000 0.02453(16) Uani 1 2 d S . P . .
N1 N -0.0021(4) 0.6945(4) 0.2267(2) 0.0663(8) Uani 1 1 d . . . . .
N2 N -0.0519(4) 0.2043(4) 0.0481(3) 0.0669(8) Uani 1 1 d . . . . .
N3 N 0.5314(3) 0.2203(2) 0.56445(15) 0.0281(4) Uani 1 1 d . . . . .
N4 N 0.4917(3) 0.0437(2) 0.35808(15) 0.0280(4) Uani 1 1 d . . . . .
O1 O 0.7733(2) 0.01420(18) 0.49409(14) 0.0308(4) Uani 1 1 d . . . . .
O2 O 0.9850(2) 0.1865(2) 0.44204(18) 0.0446(5) Uani 1 1 d . . . . .
H2 H 1.0591 0.1256 0.4621 0.067 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 0.0033 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'
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
N1 C1 C2 179.3(3) . .
C4 C2 C3 122.1(3) . .
C4 C2 C1 122.3(3) . .
C3 C2 C1 115.6(2) . .
N2 C3 C2 179.2(3) . .
C2 C4 C6 122.3(2) . .
C2 C4 C5 120.8(2) . .
C6 C4 C5 116.9(2) . .
C6 C5 C4 121.7(2) 2_665 .
C6 C5 H5 119.1 2_665 .
C4 C5 H5 119.1 . .
C5 C6 C4 121.4(3) 2_665 .
C5 C6 H6 119.3 2_665 .
C4 C6 H6 119.3 . .
N3 C7 C8 120.3(2) . .
N3 C7 H7 119.9 . .
C8 C7 H7 119.9 . .
C9 C8 C7 119.1(3) . .
C9 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
C10 C9 C8 120.6(3) . .
C10 C9 H9 119.7 . .
C8 C9 H9 119.7 . .
C9 C10 C11 118.3(2) . .
C9 C10 H10 120.9 . .
C11 C10 H10 120.9 . .
N3 C11 C10 120.7(2) . .
N3 C11 C12 110.02(19) . .
C10 C11 C12 129.3(2) . .
O2 C12 O1 114.23(18) . .
O2 C12 C13 112.77(19) . .
O1 C12 C13 105.57(19) . .
O2 C12 C11 112.3(2) . .
O1 C12 C11 105.76(18) . .
C13 C12 C11 105.55(18) . .
N4 C13 C14 121.6(2) . .
N4 C13 C12 109.70(19) . .
C14 C13 C12 128.7(2) . .
C13 C14 C15 118.2(2) . .
C13 C14 H14 120.9 . .
C15 C14 H14 120.9 . .
C16 C15 C14 119.9(2) . .
C16 C15 H15 120.1 . .
C14 C15 H15 120.1 . .
C15 C16 C17 119.5(3) . .
C15 C16 H16 120.3 . .
C17 C16 H16 120.3 . .
N4 C17 C16 120.4(2) . .
N4 C17 H17 119.8 . .
C16 C17 H17 119.8 . .
O1 Co1 O1 180.0 2_656 .
O1 Co1 N3 83.36(7) 2_656 2_656
O1 Co1 N3 96.64(7) . 2_656
O1 Co1 N3 96.64(7) 2_656 .
O1 Co1 N3 83.36(7) . .
N3 Co1 N3 180.0 2_656 .
O1 Co1 N4 96.33(7) 2_656 .
O1 Co1 N4 83.67(7) . .
N3 Co1 N4 92.13(8) 2_656 .
N3 Co1 N4 87.87(8) . .
O1 Co1 N4 83.67(7) 2_656 2_656
O1 Co1 N4 96.33(7) . 2_656
N3 Co1 N4 87.87(8) 2_656 2_656
N3 Co1 N4 92.13(8) . 2_656
N4 Co1 N4 180.0 . 2_656
C7 N3 C11 121.0(2) . .
C7 N3 Co1 128.77(17) . .
C11 N3 Co1 110.16(15) . .
C17 N4 C13 120.4(2) . .
C17 N4 Co1 129.35(16) . .
C13 N4 Co1 110.14(15) . .
C12 O1 Co1 101.44(12) . .
C12 O2 H2 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.154(4) .
C1 C2 1.416(4) .
C2 C4 1.412(3) .
C2 C3 1.416(4) .
C3 N2 1.152(4) .
C4 C6 1.414(4) .
C4 C5 1.423(4) .
C5 C6 1.357(4) 2_665
C5 H5 0.9300 .
C6 C5 1.357(4) 2_665
C6 H6 0.9300 .
C7 N3 1.343(3) .
C7 C8 1.383(4) .
C7 H7 0.9300 .
C8 C9 1.375(4) .
C8 H8 0.9300 .
C9 C10 1.375(4) .
C9 H9 0.9300 .
C10 C11 1.392(4) .
C10 H10 0.9300 .
C11 N3 1.346(3) .
C11 C12 1.532(3) .
C12 O2 1.383(3) .
C12 O1 1.402(3) .
C12 C13 1.525(3) .
C13 N4 1.350(3) .
C13 C14 1.375(3) .
C14 C15 1.396(4) .
C14 H14 0.9300 .
C15 C16 1.374(4) .
C15 H15 0.9300 .
C16 C17 1.388(4) .
C16 H16 0.9300 .
C17 N4 1.345(3) .
C17 H17 0.9300 .
Co1 O1 1.8809(15) 2_656
Co1 O1 1.8810(15) .
Co1 N3 1.9219(19) 2_656
Co1 N3 1.9219(19) .
Co1 N4 1.9253(19) .
Co1 N4 1.9253(19) 2_656
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 O1 0.82 1.86 2.680(2) 179.3 2_756
