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_2108084
_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 H44 Br6 Co N2 O4'
_chemical_formula_weight         1131.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
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_cell_angle_gamma                93.903(6)
_cell_formula_units_Z            1
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_cell_length_b                   10.6922(8)
_cell_length_c                   11.4658(13)
_cell_measurement_reflns_used    10578
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      1.34
_cell_volume                     1074.69(16)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      20(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku kappa'
_diffrn_radiation_source         SPring-8,BL02B1
_diffrn_radiation_type           Synchrotron,monochromatic
_diffrn_radiation_wavelength     0.4997
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10578
_diffrn_reflns_theta_full        17.447
_diffrn_reflns_theta_max         18.198
_diffrn_reflns_theta_min         1.343
_exptl_absorpt_coefficient_mu    2.370
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             555
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.809
_refine_diff_density_min         -2.091
_refine_ls_extinction_coef       0.020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1006P)^2^+1.3323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                3504
_reflns_number_total             4320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ps5056sup1.cif
_cod_data_source_block           3_20K
_cod_database_code               2108084
_shelx_hkl_checksum              44297
_shelx_res_checksum              79666
_shelxl_version_number           201.4
_cod_database_fobs_code 2108084