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#$Date: 2019-11-25 17:13:51 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241424 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/11/4131140.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_4131140
loop_
_publ_author_name
'Woods, Toby J.'
'Ballesteros-Rivas, María F'
'Gómez-Coca, Silvia'
'Ruiz, Eliseo'
'Dunbar, Kim R.'
_publ_section_title
;
 Relaxation Dynamics of Identical Trigonal Bipyramidal Cobalt Molecules
 with Different Local Symmetries and Packing Arrangements:
 Magnetostructural Correlations and ab inito Calculations.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16407
_journal_page_last               16416
_journal_paper_doi               10.1021/jacs.6b10154
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C18 H18 Br2 Co N4'
_chemical_formula_weight         509.11
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/5
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.626(4)
_cell_length_b                   12.626(4)
_cell_length_c                   12.626(4)
_cell_measurement_temperature    110(2)
_cell_volume                     2012.8(11)
_computing_cell_refinement       'Bruker APEX2 v2014.11-0'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'Bruker APEX2 v2014.11-0'
_computing_molecular_graphics    'Diamond v3.2i'
_computing_publication_material  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21852
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.831
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1, Bruker'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 517 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0323P)²+0.8057P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.764
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1262
_reflns_number_total             1388
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b10154_si_002.cif
_cod_data_source_block           autop213_a_CoTPMABr_cubic
_cod_original_cell_volume        2013(2)
_cod_database_code               4131140
_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   0.523
_shelx_estimated_absorpt_t_max   0.774
_shelxl_version_number           2014/5
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+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
Br1 Br 0.19838(4) 0.19838(4) 0.19838(4) 0.0203(2) Uani 1 3 d S T P
N1 N 0.4106(3) 0.4106(3) 0.4106(3) 0.0181(15) Uani 1 3 d S T P
C1 C 0.4738(4) 0.3388(4) 0.4769(4) 0.0198(12) Uani 1 1 d . . .
H1A H 0.5006 0.3775 0.5397 0.024 Uiso 1 1 calc R U .
H1B H 0.5354 0.3126 0.4362 0.024 Uiso 1 1 calc R U .
Co1 Co 0.30939(5) 0.30939(5) 0.30939(5) 0.0149(3) Uani 1 3 d S T P
N2 N 0.3319(3) 0.2164(3) 0.4423(3) 0.0162(10) Uani 1 1 d . . .
Br2 Br 0.58493(4) 0.58493(4) 0.58493(4) 0.0173(2) Uani 1 3 d S T P
C2 C 0.4072(4) 0.2471(4) 0.5120(4) 0.0177(10) Uani 1 1 d . . .
C4 C 0.3601(5) 0.1077(5) 0.6311(4) 0.0253(13) Uani 1 1 d . . .
H4 H 0.3689 0.0710 0.6962 0.030 Uiso 1 1 calc R U .
C3 C 0.4222(4) 0.1945(4) 0.6075(4) 0.0226(11) Uani 1 1 d . . .
H3 H 0.4748 0.2179 0.6560 0.027 Uiso 1 1 calc R U .
C5 C 0.2845(4) 0.0748(4) 0.5585(4) 0.0216(11) Uani 1 1 d . . .
H5 H 0.2416 0.0146 0.5726 0.026 Uiso 1 1 calc R U .
C6 C 0.2725(4) 0.1310(4) 0.4656(4) 0.0194(11) Uani 1 1 d . . .
H6 H 0.2204 0.1085 0.4161 0.023 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'
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
C1 N1 C1 112.2(3) 9 5
C1 N1 C1 112.2(3) 9 .
C1 N1 C1 112.2(3) 5 .
C1 N1 Co1 106.6(3) 9 .
C1 N1 Co1 106.6(3) 5 .
C1 N1 Co1 106.6(3) . .
N1 C1 C2 109.9(4) . .
N2 Co1 N2 115.30(8) . 9
N2 Co1 N2 115.30(8) . 5
N2 Co1 N2 115.30(8) 9 5
N2 Co1 N1 77.29(12) . .
N2 Co1 N1 77.29(12) 9 .
N2 Co1 N1 77.29(12) 5 .
N2 Co1 Br1 102.71(12) . .
N2 Co1 Br1 102.71(12) 9 .
N2 Co1 Br1 102.71(12) 5 .
N1 Co1 Br1 180.00(11) . .
C6 N2 C2 118.7(4) . .
C6 N2 Co1 123.8(3) . .
C2 N2 Co1 117.5(3) . .
N2 C2 C3 121.5(5) . .
N2 C2 C1 115.1(4) . .
C3 C2 C1 123.3(5) . .
C3 C4 C5 119.0(5) . .
C4 C3 C2 119.3(5) . .
C6 C5 C4 119.0(5) . .
N2 C6 C5 122.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Co1 2.4276(16) .
N1 C1 1.469(6) 9
N1 C1 1.469(6) 5
N1 C1 1.469(6) .
N1 Co1 2.214(7) .
C1 C2 1.497(7) .
Co1 N2 2.068(4) .
Co1 N2 2.068(4) 9
Co1 N2 2.068(4) 5
N2 C6 1.346(7) .
N2 C2 1.352(6) .
C2 C3 1.390(7) .
C4 C3 1.380(8) .
C4 C5 1.387(8) .
C5 C6 1.379(7) .
