Crystal structure of tris(1,3-dimesityl-4,5-dihydro-1<i>H</i>-imidazol-3-ium) tetrabromidocobaltate(II) bromide chloroform hexasolvate
Rais, Eduard; Flörke, Ulrich; Wilhelm, René; Acta Crystallographica Section E 71 (2015) m177–m178; doi:10.1107/S2056989015016254

data_2241098
_publ_section_title
;
 Crystal structure of
 tris(1,3-dimesityl-4,5-dihydro-1<i>H</i>-imidazol-3-ium)
 tetrabromidocobaltate(II) bromide chloroform hexasolvate
;
_journal_coeditor_code           NR2061
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m177
_journal_page_last               m178
_journal_paper_doi               10.1107/S2056989015016254
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C21 H27 N2)3 [Co Br4] Br, 6C H Cl3'
_chemical_formula_moiety
'3(C21 H27 N2 +), Br4 Co 2-, Br -, 6(C H Cl3)'
_chemical_formula_sum            'C69 H87 Br5 Cl18 Co N6'
_chemical_formula_weight         2097.02
_chemical_name_systematic
;
Tris(1,3-dimesityl-4,5-dihydro-1<i>H</i>-imidazol-3-ium)
tetrabromidocobaltate(II)
bromide chloroform hexasolvate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.0535(14)
_cell_length_b                   16.0535(14)
_cell_length_c                   61.790(12)
_cell_measurement_reflns_used    4234
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      19.70
_cell_measurement_theta_min      2.53
_cell_volume                     13791(3)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       81
_diffrn_reflns_limit_l_min       -81
_diffrn_reflns_number            41734
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         1.606
_exptl_absorpt_coefficient_mu    2.923
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2004)
;
_exptl_crystal_colour            pale-green
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       prism
_exptl_crystal_F_000             6306
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.645
_refine_ls_abs_structure_details
;
Flack (1983), 1821 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.020(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.789
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         7309
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.789
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                4427
_reflns_number_total             7309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nr2061sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        13791(4)
_cod_database_code               2241098
_shelx_estimated_absorpt_t_min   0.566
_shelx_estimated_absorpt_t_max   0.593
_shelx_hkl_checksum              77823
_shelx_res_checksum              89421
_shelxl_version_number           .2013
_cod_database_fobs_code 2241098