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_2108077
_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
_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'
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_atom_sites_solution_hydrogens   geom
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_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.688(3)
_cell_length_b                   20.688(3)
_cell_length_c                   9.0563(15)
_cell_measurement_reflns_used    28207
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.56
_cell_measurement_theta_min      0.90
_cell_volume                     3356.7(9)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.1350
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
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_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.565
_diffrn_reflns_theta_min         0.897
_exptl_absorpt_coefficient_mu    2.134
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS, 2008'
_exptl_crystal_colour            blue
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_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         0.697
_refine_diff_density_min         -0.830
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0745
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0998P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2271
_reflns_number_gt                2101
_reflns_number_total             4605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ps5056sup1.cif
_cod_data_source_block           1S_296K
_cod_original_cell_volume        3356.6(12)
_cod_database_code               2108077
_cod_database_fobs_code          2108077
_shelx_estimated_absorpt_t_min   0.618
_shelx_estimated_absorpt_t_max   0.726
_shelx_hkl_checksum              20141
_shelx_res_checksum              58593
_shelxl_version_number           201.4