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#$Date: 2022-01-18 12:37:07 +0200 (Tue, 18 Jan 2022) $
#$Revision: 272102 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/60/1566021.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_1566021
loop_
_publ_author_name
'Mitsuhashi, Ryoji'
'Hosoya, Satoshi'
'Sunatsuki, Yukinari'
'Suzuki, Takayoshi'
'Mikuriya, Masahiro'
_publ_section_title
;
 Field-induced single-ion magnet behaviors in 1-dimensionally assembled
 tetrahedral cobalt(II) complexes with halide donors
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120667
_journal_paper_doi               10.1016/j.ica.2021.120667
_journal_volume                  529
_journal_year                    2022
_chemical_formula_moiety         'C20 H24 Br2 Co N4 O2'
_chemical_formula_sum            'C20 H24 Br2 Co N4 O2'
_chemical_formula_weight         571.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 112.930(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.659(2)
_cell_length_b                   9.0379(15)
_cell_length_c                   8.4520(14)
_cell_measurement_reflns_used    1348
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      2.62
_cell_volume                     1031.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1226
_diffrn_reflns_point_group_measured_fraction_full 0.529
_diffrn_reflns_point_group_measured_fraction_max 0.522
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         3.131
_exptl_absorpt_coefficient_mu    4.732
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Twinabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_description       platelet
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.140
_refine_diff_density_max         3.283
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   -0.005(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1226
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0466
_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)+(0.0689P)²+1.8815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                1155
_reflns_number_total             1226
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2022-529-120667.cif
_cod_data_source_block           twin4_c
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               1566021
_shelx_shelxl_version_number     2014/7
_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   0.396
_shelx_estimated_absorpt_t_max   0.557
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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
Br1 Br 0.64218(5) 0.21170(12) 0.69836(10) 0.0236(2) Uani 1 1 d . . . A 1
Co1 Co 0.5000 0.34144(16) 0.5000 0.0185(4) Uani 1 2 d S T P . .
O1 O 0.5725(4) 0.4687(7) 0.4032(8) 0.0215(12) Uani 1 1 d . . . . .
C1 C 0.5413(6) 0.6007(11) 0.3323(12) 0.0206(18) Uani 1 1 d . . . . .
C2 C 0.4561(6) 0.6085(10) 0.1787(11) 0.0223(19) Uani 1 1 d . . . . .
H2 H 0.4220 0.5199 0.1292 0.027 Uiso 1 1 calc R U . . .
C3 C 0.4214(5) 0.7403(9) 0.0997(9) 0.0131(16) Uani 1 1 d . . . . .
H3 H 0.3680 0.7417 -0.0096 0.016 Uiso 1 1 calc R U . . .
C4 C 0.4640(6) 0.8732(10) 0.1783(11) 0.0194(18) Uani 1 1 d . . . . .
H4 H 0.4368 0.9653 0.1274 0.023 Uiso 1 1 calc R U . . .
C5 C 0.5473(6) 0.8688(10) 0.3332(11) 0.0177(17) Uani 1 1 d . . . . .
H5 H 0.5772 0.9585 0.3872 0.021 Uiso 1 1 calc R U . . .
C6 C 0.5872(5) 0.7316(12) 0.4101(10) 0.0158(18) Uani 1 1 d . . . . .
C7 C 0.6748(5) 0.7344(9) 0.5746(10) 0.0143(15) Uani 1 1 d . . . . .
N1 N 0.7125(5) 0.8612(9) 0.6522(9) 0.0171(15) Uani 1 1 d D . . . .
H1 H 0.676(6) 0.938(7) 0.618(12) 0.021 Uiso 1 1 d D U . . .
C8 C 0.7967(6) 0.8703(9) 0.8176(11) 0.0194(17) Uani 1 1 d . . . . .
H8 H 0.7725 0.8776 0.9116 0.023 Uiso 1 1 calc R U . . .
H8A H 0.8363 0.9599 0.8208 0.023 Uiso 1 1 calc R U . . .
C9 C 0.8611(5) 0.7327(13) 0.8425(10) 0.021(2) Uani 1 1 d . . . . .
H9 H 0.8946 0.7343 0.7610 0.026 Uiso 1 1 calc R U . . .
H9A H 0.9125 0.7308 0.9608 0.026 Uiso 1 1 calc R U . . .
C10 C 0.7965(6) 0.5967(11) 0.8116(10) 0.0173(16) Uani 1 1 d . . . . .
H10 H 0.8365 0.5069 0.8184 0.021 Uiso 1 1 calc R U . . .
H10A H 0.7686 0.5894 0.9009 0.021 Uiso 1 1 calc R U . . .
N2 N 0.7153(5) 0.6066(8) 0.6399(9) 0.0129(14) Uani 1 1 d . . . . .
H2A H 0.6935 0.5253 0.5798 0.016 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'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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 O1 107.7(4) . 2_656
O1 Co1 Br1 96.55(18) . .
O1 Co1 Br1 117.41(18) 2_656 .
O1 Co1 Br1 117.41(18) . 2_656
O1 Co1 Br1 96.55(18) 2_656 2_656
Br1 Co1 Br1 121.76(8) . 2_656
C1 O1 Co1 124.7(5) . .
O1 C1 C6 122.0(8) . .
O1 C1 C2 118.9(8) . .
C6 C1 C2 119.0(8) . .
C3 C2 C1 121.5(8) . .
C3 C2 H2 119.3 . .
C1 C2 H2 119.3 . .
C2 C3 C4 120.4(7) . .
C2 C3 H3 119.8 . .
C4 C3 H3 119.8 . .
C3 C4 C5 119.0(7) . .
C3 C4 H4 120.5 . .
C5 C4 H4 120.5 . .
C4 C5 C6 120.5(8) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C1 C6 C5 119.3(7) . .
C1 C6 C7 122.7(9) . .
C5 C6 C7 117.9(8) . .
N2 C7 N1 121.1(7) . .
N2 C7 C6 117.6(8) . .
N1 C7 C6 121.3(8) . .
C7 N1 C8 123.6(7) . .
C7 N1 H1 117(7) . .
C8 N1 H1 117(7) . .
N1 C8 C9 109.4(7) . .
N1 C8 H8 109.8 . .
C9 C8 H8 109.8 . .
N1 C8 H8A 109.8 . .
C9 C8 H8A 109.8 . .
H8 C8 H8A 108.2 . .
C10 C9 C8 109.1(6) . .
C10 C9 H9 109.9 . .
C8 C9 H9 109.9 . .
C10 C9 H9A 109.9 . .
C8 C9 H9A 109.9 . .
H9 C9 H9A 108.3 . .
N2 C10 C9 109.3(7) . .
N2 C10 H10 109.8 . .
C9 C10 H10 109.8 . .
N2 C10 H10A 109.8 . .
C9 C10 H10A 109.8 . .
H10 C10 H10A 108.3 . .
C7 N2 C10 121.6(7) . .
C7 N2 H2A 119.2 . .
C10 N2 H2A 119.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Co1 2.4098(11) .
Co1 O1 1.949(6) .
Co1 O1 1.949(6) 2_656
Co1 Br1 2.4098(11) 2_656
O1 C1 1.333(11) .
C1 C6 1.393(14) .
C1 C2 1.410(12) .
C2 C3 1.364(12) .
C2 H2 0.9500 .
C3 C4 1.397(12) .
C3 H3 0.9500 .
C4 C5 1.401(11) .
C4 H4 0.9500 .
C5 C6 1.416(13) .
C5 H5 0.9500 .
C6 C7 1.481(10) .
C7 N2 1.317(10) .
C7 N1 1.329(11) .
N1 C8 1.463(11) .
N1 H1 0.86(2) .
C8 C9 1.526(13) .
C8 H8 0.9900 .
C8 H8A 0.9900 .
C9 C10 1.511(14) .
C9 H9 0.9900 .
C9 H9A 0.9900 .
C10 N2 1.479(10) .
C10 H10 0.9900 .
C10 H10A 0.9900 .
N2 H2A 0.8800 .
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
N1 H1 Br1 0.86(2) 2.66(6) 3.401(8) 146(8) 1_565
N2 H2A O1 0.88 1.89 2.583(9) 134.4 .
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
Co1 O1 C1 C6 110.4(8) . . . .
Co1 O1 C1 C2 -66.0(10) . . . .
O1 C1 C2 C3 -179.4(8) . . . .
C6 C1 C2 C3 4.1(12) . . . .
C1 C2 C3 C4 -6.5(12) . . . .
C2 C3 C4 C5 4.7(11) . . . .
C3 C4 C5 C6 -0.7(12) . . . .
O1 C1 C6 C5 -176.5(8) . . . .
C2 C1 C6 C5 -0.1(11) . . . .
O1 C1 C6 C7 1.4(12) . . . .
C2 C1 C6 C7 177.8(7) . . . .
C4 C5 C6 C1 -1.6(11) . . . .
C4 C5 C6 C7 -179.5(6) . . . .
C1 C6 C7 N2 6.2(11) . . . .
C5 C6 C7 N2 -175.9(7) . . . .
C1 C6 C7 N1 -174.9(7) . . . .
C5 C6 C7 N1 2.9(11) . . . .
N2 C7 N1 C8 -3.5(12) . . . .
C6 C7 N1 C8 177.7(6) . . . .
C7 N1 C8 C9 26.5(11) . . . .
N1 C8 C9 C10 -51.3(8) . . . .
C8 C9 C10 N2 55.0(8) . . . .
N1 C7 N2 C10 7.5(10) . . . .
C6 C7 N2 C10 -173.7(6) . . . .
C9 C10 N2 C7 -34.3(10) . . . .
