#------------------------------------------------------------------------------
#$Date: 2019-11-17 05:51:47 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228230 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/19/7121990.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_7121990
loop_
_publ_author_name
'Mitsuhashi, Ryoji'
'Pedersen, Kasper S.'
'Ueda, Takaaki'
'Suzuki, Takayoshi'
'Bendix, Jesper'
'Mikuriya, Masahiro'
_publ_section_title
;
 Field-induced single-molecule magnet behavior in ideal trigonal
 antiprismatic cobalt(ii) complexes: precise geometrical control by a
 hydrogen-bonded rigid metalloligand.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8869
_journal_page_last               8872
_journal_paper_doi               10.1039/c8cc04756a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C54 H54 Co3 N12 O6, 2(Br), 2(C H4 O)'
_chemical_formula_sum            'C56 H62 Br2 Co3 N12 O8'
_chemical_formula_weight         1367.78
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-09 deposited with the CCDC.
2018-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.0654(11)
_cell_length_b                   11.0654(11)
_cell_length_c                   87.132(9)
_cell_measurement_reflns_used    2235
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      2.18
_cell_volume                     9239.4(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.990
_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_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       104
_diffrn_reflns_limit_l_min       -116
_diffrn_reflns_number            18737
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.484
_diffrn_reflns_theta_min         2.831
_exptl_absorpt_coefficient_mu    2.157
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4182
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0370P)²+106.5615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1459
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1878
_reflns_number_total             2589
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc04756a2.cif
_cod_data_source_block           0721171m_0m_sq
_cod_depositor_comments
'Adding full bibliography for 7121989--7121991.cif.'
_cod_original_cell_volume        9239(2)
_cod_database_code               7121990
_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   0.626
_shelx_estimated_absorpt_t_max   0.938
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
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 1.0000 1.0000 0.53157(2) 0.0161(2) Uani 1 3 d S T P . .
Co2 Co 1.0000 1.0000 0.5000 0.0146(3) Uani 1 6 d S T P . .
Br1 Br 0.3333 0.6667 0.57207(2) 0.0235(2) Uani 1 3 d S T P . .
O1 O 0.8992(3) 1.0466(3) 0.51722(3) 0.0142(7) Uani 1 1 d . . . . .
C1 C 0.7754(5) 1.0359(4) 0.51937(5) 0.0159(9) Uani 1 1 d . . . . .
C2 C 0.7381(5) 1.1133(5) 0.50987(6) 0.0195(10) Uani 1 1 d . . . . .
H2 H 0.7999 1.1688 0.5019 0.023 Uiso 1 1 calc R U . . .
C3 C 0.6129(5) 1.1109(5) 0.51177(6) 0.0244(11) Uani 1 1 d . . . . .
H3 H 0.5896 1.1651 0.5052 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5211(6) 1.0292(5) 0.52323(6) 0.0283(11) Uani 1 1 d . . . . .
H4 H 0.4356 1.0285 0.5246 0.034 Uiso 1 1 calc R U . . .
C5 C 0.5532(5) 0.9502(5) 0.53249(6) 0.0237(11) Uani 1 1 d . . . . .
H5 H 0.4885 0.8933 0.5401 0.028 Uiso 1 1 calc R U . . .
C6 C 0.6805(5) 0.9512(5) 0.53097(5) 0.0191(10) Uani 1 1 d . . . . .
C7 C 0.7136(5) 0.8698(5) 0.54135(5) 0.0181(9) Uani 1 1 d . . . . .
N1 N 0.6167(5) 0.7671(4) 0.55025(5) 0.0231(9) Uani 1 1 d . . . . .
C8 C 0.6840(6) 0.7242(6) 0.56163(6) 0.0317(13) Uani 1 1 d . . . . .
H8 H 0.6362 0.6214 0.5626 0.038 Uiso 1 1 calc R U . . .
H8A H 0.6868 0.7652 0.5718 0.038 Uiso 1 1 calc R U . . .
C9 C 0.8290(5) 0.7825(5) 0.55498(6) 0.0219(10) Uani 1 1 d . . . . .
H9 H 0.9011 0.8285 0.5630 0.026 Uiso 1 1 calc R U . . .
H9A H 0.8404 0.7079 0.5501 0.026 Uiso 1 1 calc R U . . .
N2 N 0.8384(4) 0.8852(4) 0.54337(4) 0.0174(8) Uani 1 1 d . . . . .
O2 O 0.6678(13) 0.3959(13) 0.60467(15) 0.043(3) Uani 0.3333 1 d . . P A -1
H2A H 0.7506 0.4526 0.6022 0.064 Uiso 0.3333 1 calc R U P A -1
C10 C 0.6667 0.3333 0.61775(13) 0.063(4) Uani 1 3 d S T P . .
H10 H 0.7431 0.3127 0.6177 0.095 Uiso 0.3333 1 calc R U P A .
H10A H 0.5775 0.2462 0.6188 0.095 Uiso 0.3333 1 calc R U P . .
H10B H 0.6786 0.3950 0.6264 0.095 Uiso 0.3333 1 calc R U P . .
H10C H 0.551(5) 0.765(5) 0.5530(5) 0.008(12) Uiso 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'
Br Br -0.2901 2.4595 '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
N2 Co1 N2 93.41(17) 3_675 2_765
N2 Co1 N2 93.41(17) 3_675 .
N2 Co1 N2 93.41(17) 2_765 .
N2 Co1 O1 91.22(14) 3_675 .
N2 Co1 O1 171.82(15) 2_765 .
N2 Co1 O1 93.04(14) . .
N2 Co1 O1 171.82(15) 3_675 2_765
N2 Co1 O1 93.04(14) 2_765 2_765
N2 Co1 O1 91.22(15) . 2_765
O1 Co1 O1 81.80(14) . 2_765
N2 Co1 O1 93.04(15) 3_675 3_675
N2 Co1 O1 91.22(15) 2_765 3_675
N2 Co1 O1 171.82(16) . 3_675
O1 Co1 O1 81.80(14) . 3_675
O1 Co1 O1 81.80(14) 2_765 3_675
N2 Co1 Co2 122.81(12) 3_675 .
N2 Co1 Co2 122.81(12) 2_765 .
N2 Co1 Co2 122.81(12) . .
O1 Co1 Co2 49.12(9) . .
O1 Co1 Co2 49.11(9) 2_765 .
O1 Co1 Co2 49.11(9) 3_675 .
O1 Co2 O1 180.00(11) 20_566 2_765
O1 Co2 O1 73.83(13) 20_566 21_656
O1 Co2 O1 106.17(13) 2_765 21_656
O1 Co2 O1 106.17(13) 20_566 3_675
O1 Co2 O1 73.83(13) 2_765 3_675
O1 Co2 O1 180.00(11) 21_656 3_675
O1 Co2 O1 73.83(13) 20_566 19_776
O1 Co2 O1 106.17(13) 2_765 19_776
O1 Co2 O1 73.83(13) 21_656 19_776
O1 Co2 O1 106.17(13) 3_675 19_776
O1 Co2 O1 106.18(13) 20_566 .
O1 Co2 O1 73.82(13) 2_765 .
O1 Co2 O1 106.18(13) 21_656 .
O1 Co2 O1 73.82(13) 3_675 .
O1 Co2 O1 180.0 19_776 .
O1 Co2 Co1 43.91(8) 20_566 19_776
O1 Co2 Co1 136.09(8) 2_765 19_776
O1 Co2 Co1 43.91(9) 21_656 19_776
O1 Co2 Co1 136.09(9) 3_675 19_776
O1 Co2 Co1 43.91(8) 19_776 19_776
O1 Co2 Co1 136.09(8) . 19_776
O1 Co2 Co1 136.09(8) 20_566 .
O1 Co2 Co1 43.91(8) 2_765 .
O1 Co2 Co1 136.09(9) 21_656 .
O1 Co2 Co1 43.91(9) 3_675 .
O1 Co2 Co1 136.09(8) 19_776 .
O1 Co2 Co1 43.91(8) . .
Co1 Co2 Co1 180.0 19_776 .
C1 O1 Co1 126.8(3) . .
C1 O1 Co2 137.4(3) . .
Co1 O1 Co2 86.98(12) . .
O1 C1 C2 118.1(4) . .
O1 C1 C6 123.3(4) . .
C2 C1 C6 118.6(4) . .
C3 C2 C1 121.3(5) . .
C3 C2 H2 119.4 . .
C1 C2 H2 119.4 . .
C2 C3 C4 119.9(5) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C5 C4 C3 120.3(5) . .
C5 C4 H4 119.9 . .
C3 C4 H4 119.9 . .
C4 C5 C6 121.3(5) . .
C4 C5 H5 119.3 . .
C6 C5 H5 119.3 . .
C5 C6 C1 118.6(4) . .
C5 C6 C7 120.0(4) . .
C1 C6 C7 121.4(4) . .
N2 C7 N1 111.9(4) . .
N2 C7 C6 125.4(4) . .
N1 C7 C6 122.7(4) . .
C7 N1 C8 110.2(4) . .
C7 N1 H10C 124(4) . .
C8 N1 H10C 115(4) . .
N1 C8 C9 101.9(4) . .
N1 C8 H8 111.4 . .
C9 C8 H8 111.4 . .
N1 C8 H8A 111.4 . .
C9 C8 H8A 111.4 . .
H8 C8 H8A 109.2 . .
N2 C9 C8 103.9(4) . .
N2 C9 H9 111.0 . .
C8 C9 H9 111.0 . .
N2 C9 H9A 111.0 . .
C8 C9 H9A 111.0 . .
H9 C9 H9A 109.0 . .
C7 N2 C9 108.9(4) . .
C7 N2 Co1 126.3(3) . .
C9 N2 Co1 124.3(3) . .
C10 O2 H2A 109.5 . .
O2 C10 H10 109.5 . .
O2 C10 H10A 109.5 . .
H10 C10 H10A 109.5 . .
O2 C10 H10B 109.5 . .
H10 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 1.896(4) 3_675
Co1 N2 1.896(4) 2_765
Co1 N2 1.896(4) .
Co1 O1 1.910(3) .
Co1 O1 1.910(3) 2_765
Co1 O1 1.910(3) 3_675
Co1 Co2 2.7509(10) .
Co2 O1 2.083(3) 20_566
Co2 O1 2.083(3) 2_765
Co2 O1 2.083(3) 21_656
Co2 O1 2.083(3) 3_675
Co2 O1 2.083(3) 19_776
Co2 O1 2.083(3) .
Co2 Co1 2.7508(10) 19_776
O1 C1 1.328(5) .
C1 C2 1.394(6) .
C1 C6 1.420(6) .
C2 C3 1.382(7) .
C2 H2 0.9500 .
C3 C4 1.388(7) .
C3 H3 0.9500 .
C4 C5 1.361(7) .
C4 H4 0.9500 .
C5 C6 1.409(7) .
C5 H5 0.9500 .
C6 C7 1.448(7) .
C7 N2 1.315(6) .
C7 N1 1.350(6) .
N1 C8 1.455(7) .
N1 H10C 0.76(5) .
C8 C9 1.513(7) .
C8 H8 0.9900 .
C8 H8A 0.9900 .
C9 N2 1.486(6) .
C9 H9 0.9900 .
C9 H9A 0.9900 .
O2 C10 1.330(14) .
O2 H2A 0.8400 .
C10 H10 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
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
N1 H10C Br1 0.76(5) 2.67(5) 3.346(4) 150(5)
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
Co1 O1 C1 C2 160.3(3) .
Co2 O1 C1 C2 -64.0(6) .
Co1 O1 C1 C6 -18.8(6) .
Co2 O1 C1 C6 116.9(5) .
O1 C1 C2 C3 -177.8(4) .
C6 C1 C2 C3 1.3(7) .
C1 C2 C3 C4 -0.6(8) .
C2 C3 C4 C5 -0.8(8) .
C3 C4 C5 C6 1.4(8) .
C4 C5 C6 C1 -0.7(8) .
C4 C5 C6 C7 177.8(5) .
O1 C1 C6 C5 178.4(4) .
C2 C1 C6 C5 -0.7(7) .
O1 C1 C6 C7 -0.1(7) .
C2 C1 C6 C7 -179.2(4) .
C5 C6 C7 N2 -164.0(5) .
C1 C6 C7 N2 14.4(7) .
C5 C6 C7 N1 15.8(7) .
C1 C6 C7 N1 -165.7(4) .
N2 C7 N1 C8 11.7(6) .
C6 C7 N1 C8 -168.2(4) .
C7 N1 C8 C9 -17.4(5) .
N1 C8 C9 N2 16.3(5) .
N1 C7 N2 C9 -0.1(5) .
C6 C7 N2 C9 179.8(4) .
N1 C7 N2 Co1 171.8(3) .
C6 C7 N2 Co1 -8.4(7) .
C8 C9 N2 C7 -10.8(5) .
C8 C9 N2 Co1 177.2(3) .
N2 Co1 N2 C7 85.3(5) 3_675
N2 Co1 N2 C7 178.9(4) 2_765
O1 Co1 N2 C7 -6.1(4) .
O1 Co1 N2 C7 -87.9(4) 2_765
Co2 Co1 N2 C7 -47.9(4) .
N2 Co1 N2 C9 -104.1(3) 3_675
N2 Co1 N2 C9 -10.4(4) 2_765
O1 Co1 N2 C9 164.5(4) .
O1 Co1 N2 C9 82.7(4) 2_765
Co2 Co1 N2 C9 122.7(3) .
