#------------------------------------------------------------------------------
#$Date: 2023-02-06 11:57:42 +0200 (Mon, 06 Feb 2023) $
#$Revision: 280796 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/66/8106697.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_8106697
loop_
_publ_author_name
'Liu, Feng'
'Li, Weihua'
'Lu, Hui'
'Sun, Jianhua'
_publ_section_title
;
 Crystal structure of bis(hydroxydi(pyridin-2-yl)methanolato-κ3
 N,N′,O)cobalt(III) perchlorate dihydrate, C22H22ClCoN4O10
;
_journal_issue                   5
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              843
_journal_page_last               844
_journal_paper_doi               10.1515/ncrs-2017-0090
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C22 H18 Co N4 O4, Cl O4, 2(H2 O)'
_chemical_formula_sum            'C22 H22 Cl Co N4 O10'
_chemical_formula_weight         596.82
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                99.7700(10)
_cell_angle_beta                 103.4900(10)
_cell_angle_gamma                90.2900(10)
_cell_formula_units_Z            2
_cell_length_a                   8.4566(7)
_cell_length_b                   11.9163(7)
_cell_length_c                   12.4333(9)
_cell_measurement_reflns_used    4716
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      1.71
_cell_volume                     1199.38(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12848
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0351P)²+1.0858P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                4180
_reflns_number_total             4716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0090_suppl.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '-P 1   '
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               8106697
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3518(2) 0.43507(16) 0.14215(17) 0.0159(4) Uani 1 1 d . . .
H1 H 0.4135 0.4914 0.1972 0.019 Uiso 1 1 calc R . .
C2 C 0.2622(3) 0.46329(18) 0.04288(18) 0.0218(4) Uani 1 1 d . . .
H2 H 0.2637 0.5382 0.0309 0.026 Uiso 1 1 calc R . .
C3 C 0.1704(3) 0.37881(19) -0.03834(17) 0.0220(4) Uani 1 1 d . . .
H3 H 0.1104 0.3967 -0.1056 0.026 Uiso 1 1 calc R . .
C4 C 0.1678(2) 0.26707(18) -0.01933(16) 0.0176(4) Uani 1 1 d . . .
H4 H 0.1056 0.2095 -0.0726 0.021 Uiso 1 1 calc R . .
C5 C 0.2604(2) 0.24436(16) 0.08103(15) 0.0127(4) Uani 1 1 d . . .
C6 C 0.2801(2) 0.13023(16) 0.12329(15) 0.0125(4) Uani 1 1 d . . .
C7 C 0.1886(2) 0.13771(15) 0.21638(15) 0.0121(4) Uani 1 1 d . . .
C8 C 0.0448(2) 0.08184(16) 0.21354(16) 0.0145(4) Uani 1 1 d . . .
H8 H -0.0106 0.0328 0.1492 0.017 Uiso 1 1 calc R . .
C9 C -0.0159(2) 0.10076(17) 0.30997(17) 0.0160(4) Uani 1 1 d . . .
H9 H -0.1123 0.0637 0.3112 0.019 Uiso 1 1 calc R . .
C10 C 0.0694(2) 0.17556(16) 0.40409(16) 0.0149(4) Uani 1 1 d . . .
H10 H 0.0304 0.1889 0.4690 0.018 Uiso 1 1 calc R . .
C11 C 0.2128(2) 0.23023(15) 0.40077(16) 0.0123(4) Uani 1 1 d . . .
H11 H 0.2690 0.2812 0.4634 0.015 Uiso 1 1 calc R . .
C12 C 0.6099(2) 0.09871(16) 0.42911(16) 0.0140(4) Uani 1 1 d . . .
H12 H 0.5503 0.0400 0.3758 0.017 Uiso 1 1 calc R . .
C13 C 0.7068(2) 0.07459(17) 0.52777(17) 0.0172(4) Uani 1 1 d . . .
H13 H 0.7134 -0.0001 0.5404 0.021 Uiso 1 1 calc R . .
C14 C 0.7943(2) 0.16238(18) 0.60783(17) 0.0183(4) Uani 1 1 d . . .
H14 H 0.8574 0.1474 0.6754 0.022 Uiso 1 1 calc R . .
C15 C 0.7863(2) 0.27306(17) 0.58572(16) 0.0146(4) Uani 1 1 d . . .
H15 H 0.8451 0.3332 0.6374 0.018 Uiso 1 1 calc R . .
C16 C 0.6890(2) 0.29130(16) 0.48532(15) 0.0111(4) Uani 1 1 d . . .
C17 C 0.6666(2) 0.40385(15) 0.44040(15) 0.0114(4) Uani 1 1 d . . .
C18 C 0.7554(2) 0.39252(15) 0.34524(15) 0.0114(4) Uani 1 1 d . . .
C19 C 0.8993(2) 0.44627(16) 0.34361(16) 0.0144(4) Uani 1 1 d . . .
H19 H 0.9545 0.4994 0.4048 0.017 Uiso 1 1 calc R . .
C20 C 0.9597(2) 0.41895(17) 0.24793(17) 0.0161(4) Uani 1 1 d . . .
H20 H 1.0577 0.4528 0.2451 0.019 Uiso 1 1 calc R . .
C21 C 0.8737(2) 0.34116(17) 0.15676(16) 0.0160(4) Uani 1 1 d . . .
H21 H 0.9127 0.3228 0.0922 0.019 Uiso 1 1 calc R . .
C22 C 0.7287(2) 0.29126(16) 0.16338(16) 0.0137(4) Uani 1 1 d . . .
H22 H 0.6697 0.2394 0.1026 0.016 Uiso 1 1 calc R . .
Cl1 Cl 0.35462(6) 0.25888(4) 0.71162(4) 0.01958(12) Uani 1 1 d . . .
Co1 Co 0.47303(3) 0.26503(2) 0.283712(19) 0.00877(8) Uani 1 1 d . . .
N1 N 0.35016(18) 0.32694(13) 0.15925(13) 0.0114(3) Uani 1 1 d . . .
N2 N 0.27125(18) 0.21052(12) 0.30839(13) 0.0100(3) Uani 1 1 d . . .
N3 N 0.60113(18) 0.20618(13) 0.40965(13) 0.0109(3) Uani 1 1 d . . .
N4 N 0.67287(18) 0.31691(13) 0.25644(13) 0.0109(3) Uani 1 1 d . . .
O1 O 0.22439(16) 0.03552(11) 0.04157(11) 0.0157(3) Uani 1 1 d . . .
H1A H 0.2703 0.0346 -0.0098 0.024 Uiso 1 1 calc R . .
O2 O 0.44622(15) 0.12907(11) 0.17721(10) 0.0117(3) Uani 1 1 d . . .
O3 O 0.49996(15) 0.40353(10) 0.38741(10) 0.0109(3) Uani 1 1 d . . .
O4 O 0.72561(15) 0.49792(11) 0.52127(11) 0.0133(3) Uani 1 1 d . . .
H4A H 0.6522 0.5235 0.5498 0.020 Uiso 1 1 calc R . .
O5 O 0.4120(3) 0.35758(16) 0.67894(18) 0.0600(7) Uani 1 1 d . . .
O6 O 0.3879(3) 0.16244(16) 0.63732(15) 0.0524(6) Uani 1 1 d . . .
O7 O 0.1861(2) 0.2647(3) 0.70504(17) 0.0722(8) Uani 1 1 d . . .
O8 O 0.44206(19) 0.25270(15) 0.82571(13) 0.0303(4) Uani 1 1 d . . .
O1W O 0.21733(19) 0.81053(14) 0.10506(13) 0.0291(4) Uani 1 1 d . . .
H1WA H 0.2183 0.8759 0.0863 0.035 Uiso 1 1 d R . .
H1WB H 0.3152 0.7916 0.1251 0.035 Uiso 1 1 d R . .
O2W O 0.34963(17) 0.03274(12) 0.86945(12) 0.0210(3) Uani 1 1 d . . .
H2WA H 0.3798 0.0960 0.8559 0.025 Uiso 1 1 d R . .
H2WB H 0.4165 -0.0169 0.8539 0.025 Uiso 1 1 d R . .
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
N1 C1 C2 120.34(18) . .
N1 C1 H1 119.8 . .
C2 C1 H1 119.8 . .
C1 C2 C3 119.30(19) . .
C1 C2 H2 120.4 . .
C3 C2 H2 120.4 . .
C2 C3 C4 119.97(19) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C5 C4 C3 117.92(19) . .
C5 C4 H4 121.0 . .
C3 C4 H4 121.0 . .
N1 C5 C4 121.70(18) . .
N1 C5 C6 109.51(15) . .
C4 C5 C6 128.79(17) . .
O1 C6 O2 113.82(15) . .
O1 C6 C7 110.39(15) . .
O2 C6 C7 105.60(14) . .
O1 C6 C5 114.60(15) . .
O2 C6 C5 105.34(14) . .
C7 C6 C5 106.40(15) . .
N2 C7 C8 122.34(17) . .
N2 C7 C6 109.61(15) . .
C8 C7 C6 128.04(17) . .
C7 C8 C9 118.12(18) . .
C7 C8 H8 120.9 . .
C9 C8 H8 120.9 . .
C10 C9 C8 119.28(18) . .
C10 C9 H9 120.4 . .
C8 C9 H9 120.4 . .
C11 C10 C9 119.62(17) . .
C11 C10 H10 120.2 . .
C9 C10 H10 120.2 . .
N2 C11 C10 120.75(17) . .
N2 C11 H11 119.6 . .
C10 C11 H11 119.6 . .
N3 C12 C13 120.49(17) . .
N3 C12 H12 119.8 . .
C13 C12 H12 119.8 . .
C12 C13 C14 119.74(18) . .
C12 C13 H13 120.1 . .
C14 C13 H13 120.1 . .
C13 C14 C15 119.14(18) . .
C13 C14 H14 120.4 . .
C15 C14 H14 120.4 . .
C16 C15 C14 118.30(18) . .
C16 C15 H15 120.9 . .
C14 C15 H15 120.9 . .
N3 C16 C15 122.12(17) . .
N3 C16 C17 110.14(15) . .
C15 C16 C17 127.72(17) . .
O4 C17 O3 115.28(14) . .
O4 C17 C18 111.17(15) . .
O3 C17 C18 105.28(14) . .
O4 C17 C16 113.20(15) . .
O3 C17 C16 105.46(14) . .
C18 C17 C16 105.67(14) . .
N4 C18 C19 121.46(17) . .
N4 C18 C17 109.90(15) . .
C19 C18 C17 128.63(17) . .
C18 C19 C20 118.21(18) . .
C18 C19 H19 120.9 . .
C20 C19 H19 120.9 . .
C21 C20 C19 119.92(18) . .
C21 C20 H20 120.0 . .
C19 C20 H20 120.0 . .
C22 C21 C20 118.93(18) . .
C22 C21 H21 120.5 . .
C20 C21 H21 120.5 . .
N4 C22 C21 120.66(18) . .
N4 C22 H22 119.7 . .
C21 C22 H22 119.7 . .
O7 Cl1 O6 111.05(15) . .
O7 Cl1 O5 109.57(16) . .
O6 Cl1 O5 107.30(14) . .
O7 Cl1 O8 110.20(11) . .
O6 Cl1 O8 109.30(11) . .
O5 Cl1 O8 109.37(11) . .
O2 Co1 O3 178.49(6) . .
O2 Co1 N1 83.33(6) . .
O3 Co1 N1 95.38(6) . .
O2 Co1 N4 95.89(6) . .
O3 Co1 N4 83.31(6) . .
N1 Co1 N4 90.71(6) . .
O2 Co1 N3 97.67(6) . .
O3 Co1 N3 83.60(6) . .
N1 Co1 N3 178.40(6) . .
N4 Co1 N3 87.94(6) . .
O2 Co1 N2 82.97(6) . .
O3 Co1 N2 97.82(6) . .
N1 Co1 N2 88.89(6) . .
N4 Co1 N2 178.83(6) . .
N3 Co1 N2 92.47(6) . .
C1 N1 C5 120.76(16) . .
C1 N1 Co1 128.26(13) . .
C5 N1 Co1 110.88(12) . .
C11 N2 C7 119.88(16) . .
C11 N2 Co1 129.69(13) . .
C7 N2 Co1 110.34(12) . .
C12 N3 C16 120.17(16) . .
C12 N3 Co1 129.54(13) . .
C16 N3 Co1 110.28(12) . .
C22 N4 C18 120.81(16) . .
C22 N4 Co1 128.54(13) . .
C18 N4 Co1 110.56(12) . .
C6 O1 H1A 109.5 . .
C6 O2 Co1 101.31(10) . .
C17 O3 Co1 101.26(10) . .
C17 O4 H4A 109.5 . .
H1WA O1W H1WB 108.4 . .
H2WA O2W H2WB 108.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.342(2) .
C1 C2 1.385(3) .
C1 H1 0.9300 .
C2 C3 1.385(3) .
C2 H2 0.9300 .
C3 C4 1.392(3) .
C3 H3 0.9300 .
C4 C5 1.380(3) .
C4 H4 0.9300 .
C5 N1 1.347(2) .
C5 C6 1.535(3) .
C6 O1 1.382(2) .
C6 O2 1.409(2) .
C6 C7 1.526(3) .
C7 N2 1.354(2) .
C7 C8 1.374(3) .
C8 C9 1.396(3) .
C8 H8 0.9300 .
C9 C10 1.389(3) .
C9 H9 0.9300 .
C10 C11 1.386(3) .
C10 H10 0.9300 .
C11 N2 1.339(2) .
C11 H11 0.9300 .
C12 N3 1.342(2) .
C12 C13 1.383(3) .
C12 H12 0.9300 .
C13 C14 1.388(3) .
C13 H13 0.9300 .
C14 C15 1.391(3) .
C14 H14 0.9300 .
C15 C16 1.377(3) .
C15 H15 0.9300 .
C16 N3 1.345(2) .
C16 C17 1.534(3) .
C17 O4 1.376(2) .
C17 O3 1.409(2) .
C17 C18 1.530(3) .
C18 N4 1.347(2) .
C18 C19 1.378(3) .
C19 C20 1.392(3) .
C19 H19 0.9300 .
C20 C21 1.387(3) .
C20 H20 0.9300 .
C21 C22 1.386(3) .
C21 H21 0.9300 .
C22 N4 1.339(2) .
C22 H22 0.9300 .
Cl1 O7 1.411(2) .
Cl1 O6 1.4205(18) .
Cl1 O5 1.426(2) .
Cl1 O8 1.4529(16) .
Co1 O2 1.8862(12) .
Co1 O3 1.8908(12) .
Co1 N1 1.9141(16) .
Co1 N4 1.9186(16) .
Co1 N3 1.9252(16) .
Co1 N2 1.9309(15) .
O1 H1A 0.8200 .
O4 H4A 0.8200 .
O1W H1WA 0.8501 .
O1W H1WB 0.8500 .
O2W H2WA 0.8500 .
O2W H2WB 0.8501 .
