A double salt of iodobismuthate: <i>cis</i>-aquaiodidobis(1,10-phenanthroline)cobalt(II) tris(1,10-phenanthroline)cobalt(II) <i>trans</i>-hexa-μ~2~-iodido-hexaiodidotribismuthate(III)
Chen, Jiongke; Chai, Wenxiang; Song, Li; Yang, Yunyun; Niu, Feng; Acta Crystallographica Section E 67 (2011) m1284–m1285; doi:10.1107/S1600536811033460

data_2231654
_publ_section_title
;
 A double salt of iodobismuthate:
 <i>cis</i>-aquaiodidobis(1,10-phenanthroline)cobalt(II)
 tris(1,10-phenanthroline)cobalt(II)
 <i>trans</i>-hexa-\m~2~-iodido-hexaiodidotribismuthate(III)
;
_journal_coeditor_code           OM2460
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1284
_journal_page_last               m1285
_journal_paper_doi               10.1107/S1600536811033460
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'[Co (C12 H8 N2)3] [Co I (C12 H8 N2)2 (H2 O)] [Bi3 I12]'
_chemical_formula_moiety
'C36 H24 Co N6 2+, C24 H18 Co I N4 O +, Bi3 I12 3-'
_chemical_formula_sum            'C60 H42 Bi3 Co2 I13 N10 O'
_chemical_formula_weight         3313.6
_chemical_name_systematic
;
<i>cis</i>-aquaiodidobis(1,10-phenanthroline)cobalt(II)
tris(1,10-phenanthroline)cobalt(II)
<i>trans</i>-hexa-\m~2~-iodido-hexaiodidotribismuthate(III)
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.188(8)
_cell_length_b                   17.641(4)
_cell_length_c                   12.793(3)
_cell_measurement_reflns_used    3822
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.0844
_cell_volume                     7941(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 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      293(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            58697
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    12.132
_exptl_absorpt_correction_T_max  0.088
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5880
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.286
_refine_diff_density_min         -2.132
_refine_ls_abs_structure_details 'Flack (1983), 8549 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         18072
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                16129
_reflns_number_total             18072
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2460.cif
_cod_data_source_block           I
_cod_database_code               2231654
_cod_database_fobs_code          2231654