Two polymorphs of tris(ethylenediamine)cobalt(III) tetrathioantimonate(V)
Wang, Ming-Feng; Yue, Cheng-Yang; Yuan, Zhuang-Dong; Lei, Xiao-Wu; Acta Crystallographica Section C 69 (2013) 855–858; doi:10.1107/S0108270113017277

data_2019080
_publ_section_title
;
 Two polymorphs of tris(ethylenediamine)cobalt(III) tetrathioantimonate(V)
;
_journal_coeditor_code           FG3290
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              855
_journal_page_last               858
_journal_paper_doi               10.1107/S0108270113017277
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Co (C2 H8 N2)3] [Sb S4]'
_chemical_formula_moiety         'C6 H24 Co N6 3+, S4 Sb 3-'
_chemical_formula_sum            'C6 H24 Co N6 S4 Sb'
_chemical_formula_weight         489.23
_chemical_name_systematic
;
Tris(ethylenediamine)cobalt(III) tetrathioantimonate(V)
;
_space_group_IT_number           106
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4c -2ab'
_symmetry_space_group_name_H-M   'P 42 b c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.4909(11)
_cell_length_b                   15.4909(11)
_cell_length_c                   13.6285(9)
_cell_measurement_temperature    296(2)
_cell_volume                     3270.4(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            35970
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    3.170
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.311
_refine_ls_abs_structure_details 'Flack (1983), with 1808 Friedel pairs'
_refine_ls_abs_structure_Flack   0.328(17)
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0130P)^2^+3.5797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                3449
_reflns_number_total             3783
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3290.cif
_cod_data_source_block           II
_cod_original_sg_symbol_Hall     'p 4c -2ab'
_cod_original_sg_symbol_H-M      'P 4 2 bc'
_cod_original_formula_sum        'C6 H24 Co1 N6 S4 Sb1'
_cod_database_code               2019080
_cod_database_fobs_code          2019080