#------------------------------------------------------------------------------
#$Date: 2019-11-23 07:15:36 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232404 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/76/4347610.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_4347610
loop_
_publ_author_name
'Panja, Anangamohan'
'Jana, Narayan Ch'
'Bauzá, Antonio'
'Frontera, Antonio'
'Mathonière, Corine'
_publ_section_title
;
 Solvent-Triggered Cis/Trans Isomerism in Cobalt Dioxolene Chemistry:
 Distinguishing Effects of Packing on Valence Tautomerism.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8331
_journal_page_last               8340
_journal_paper_doi               10.1021/acs.inorgchem.6b00402
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C32 H32 Br8 Co N4 O8'
_chemical_formula_weight         1298.83
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 105.698(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   11.955(3)
_cell_length_b                   15.880(5)
_cell_length_c                   11.351(4)
_cell_measurement_reflns_used    10499
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.0
_cell_volume                     2074.6(11)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'Platon (Spek, 2008)and Mercury (CCDC)'
_computing_publication_material  'SHELXL-2013 (Sheldrick,2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick,2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick,2013)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi 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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4599
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    8.169
_exptl_absorpt_correction_T_max  0.5610
_exptl_absorpt_correction_T_min  0.2919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Red-Brown
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1246
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2445
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0424
_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)+(0.0612P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                1639
_reflns_number_total             2445
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00402_si_002.cif
_cod_data_source_block           complex-2
_cod_original_cell_volume        2074.6(12)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               4347610
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O1 O 0.0747(2) 0.41779(17) 0.4274(3) 0.0343(7) Uani 1 1 d .
C1 C 0.1408(3) 0.4553(3) 0.3640(4) 0.0308(9) Uani 1 1 d .
C2 C 0.2092(3) 0.4133(3) 0.3041(4) 0.0356(10) Uani 1 1 d .
C3 C 0.2784(3) 0.4563(3) 0.2412(4) 0.0390(11) Uani 1 1 d .
N1 N 0.1332(4) 0.5000 0.6453(5) 0.0330(11) Uani 1 2 d S
C5 C 0.3242(6) 0.5000 0.8466(6) 0.0460(17) Uani 1 2 d SD
C4 C 0.1800(4) 0.4276(3) 0.6967(4) 0.0401(11) Uani 1 1 d .
H4 H 0.1442(19) 0.373(3) 0.6607(19) 0.048 Uiso 1 1 calc R
C6 C 0.2753(4) 0.4260(3) 0.7969(5) 0.0473(13) Uani 1 1 d .
H6 H 0.3053(19) 0.376(3) 0.829(2) 0.057 Uiso 1 1 calc R
O2 O 0.5000 0.2958(4) 0.0000 0.0801(19) Uani 1 2 d S
O3 O 0.0000 0.2648(4) 0.5000 0.093(2) Uani 1 2 d SD
C8 C 0.5000 0.2206(6) 0.0000 0.056(2) Uani 1 2 d S
C9 C 0.4292(5) 0.1713(5) 0.0638(8) 0.090(2) Uani 1 1 d .
H9A H 0.4027 0.2081 0.1201 0.135 Uiso 1 1 calc R
H9B H 0.4763 0.1255 0.1101 0.135 Uiso 1 1 calc R
H9C H 0.3618 0.1476 0.0036 0.135 Uiso 1 1 calc R
N2 N 0.0000 0.0877(8) 0.5000 0.111(4) Uani 1 2 d S
H2 H 0.0000 0.145(9) 0.5000 0.133 Uiso 1 2 calc SR
C7 C 0.0749(5) 0.0434(6) 0.4513(6) 0.108(4) Uani 1 1 d .
H7 H 0.130(5) 0.074(3) 0.416(3) 0.130 Uiso 1 1 calc R
H5 H 0.382(4) 0.5000 0.914(4) 0.050 Uiso 1 2 d SD
Co1 Co 0.0000 0.5000 0.5000 0.0292(3) Uani 1 4 d S
Br1 Br 0.20862(5) 0.29420(3) 0.31360(5) 0.0539(2) Uani 1 1 d .
Br2 Br 0.37151(4) 0.39525(4) 0.16000(5) 0.0530(2) Uani 1 1 d .
H3 H -0.054(3) 0.300(3) 0.517(5) 0.050 Uiso 1 1 d 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'
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 O1 Co1 110.1(2) . .
O1 C1 C2 124.5(4) . .
O1 C1 C1 116.3(2) . 6_565
C2 C1 C1 119.1(3) . 6_565
C1 C2 C3 121.8(4) . .
C1 C2 Br1 116.5(3) . .
C3 C2 Br1 121.7(3) . .
C3 C3 C2 119.0(3) 6_565 .
C3 C3 Br2 120.79(15) 6_565 .
C2 C3 Br2 120.2(4) . .
C4 N1 C4 117.9(5) . 6_565
C4 N1 Co1 121.0(3) . .
C4 N1 Co1 121.0(3) 6_565 .
C6 C5 C6 118.9(6) . 6_565
N1 C4 C6 122.1(4) . .
C5 C6 C4 119.4(5) . .
O2 C8 C9 122.0(5) . 2_655
O2 C8 C9 122.0(5) . .
C9 C8 C9 116.1(9) 2_655 .
C7 N2 C7 118.2(12) 2_556 .
N2 C7 C7 120.9(6) . 6
O1 Co1 O1 92.75(18) 2_556 .
O1 Co1 O1 180.00(12) 2_556 6_565
O1 Co1 O1 87.25(18) . 6_565
O1 Co1 O1 87.25(18) 2_556 5_566
O1 Co1 O1 180.00(16) . 5_566
O1 Co1 O1 92.75(18) 6_565 5_566
O1 Co1 N1 89.70(14) 2_556 5_566
O1 Co1 N1 90.30(14) . 5_566
O1 Co1 N1 90.30(14) 6_565 5_566
O1 Co1 N1 89.70(14) 5_566 5_566
O1 Co1 N1 90.30(14) 2_556 .
O1 Co1 N1 89.70(14) . .
O1 Co1 N1 89.70(14) 6_565 .
O1 Co1 N1 90.30(14) 5_566 .
N1 Co1 N1 180.000(1) 5_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.344(5) .
O1 Co1 1.892(3) .
C1 C2 1.369(6) .
C1 C1 1.420(8) 6_565
C2 C3 1.407(7) .
C2 Br1 1.895(5) .
C3 C3 1.389(9) 6_565
C3 Br2 1.893(5) .
N1 C4 1.341(5) .
N1 C4 1.341(5) 6_565
N1 Co1 1.958(5) .
C5 C6 1.365(6) .
C5 C6 1.365(6) 6_565
C4 C6 1.375(6) .
O2 C8 1.195(9) .
C8 C9 1.478(8) 2_655
C8 C9 1.478(8) .
N2 C7 1.366(10) 2_556
N2 C7 1.366(10) .
C7 C7 1.38(2) 6
Co1 O1 1.892(3) 2_556
Co1 O1 1.892(3) 6_565
Co1 O1 1.892(3) 5_566
Co1 N1 1.958(5) 5_566
