Variable-temperature structural studies on valence tautomerism in cobalt bis(dioxolene) molecular complexes
Hathwar, Venkatesha R.; Stingaciu, Marian; Richter, Bo; Overgaard, Jacob; Iversen, Bo B.; Acta Crystallographica Section B 73 (2017) 304–312; doi:10.1107/S2052520616019235

data_2108073
_publ_section_title
;
 Variable-temperature structural studies on valence tautomerism in cobalt
 bis(dioxolene) molecular complexes
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              304
_journal_page_last               312
_journal_paper_doi               10.1107/S2052520616019235
_journal_volume                  73
_journal_year                    2017
_chemical_formula_sum            'C38 H46 Br4 Co N2 O4'
_chemical_formula_weight         973.34
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.1281(7)
_cell_length_b                   20.1281(7)
_cell_length_c                   8.9942(3)
_cell_measurement_reflns_used    23579
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      0.92
_cell_volume                     3155.72(19)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            23579
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.619
_diffrn_reflns_theta_min         0.922
_exptl_absorpt_coefficient_mu    2.270
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS, 2008'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             1461
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_platon_squeeze_details
;
;
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.982
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0572
_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/[\s^2^(Fo^2^)+(0.0657P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1520
_reflns_number_gt                3675
_reflns_number_total             6428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ps5056sup1.cif
_cod_data_source_block           1S_100K
_cod_original_cell_volume        3155.7(2)
_cod_database_code               2108073
_shelx_estimated_absorpt_t_min   0.601
_shelx_estimated_absorpt_t_max   0.713
_shelx_hkl_checksum              99933
_shelx_res_checksum              19302
_shelxl_version_number           201.4
_cod_database_fobs_code 2108073