Structural Diversity in Supramolecular Complexes of MCl3 (M = As, Sb, Bi) with Constrained Thio- and Seleno-Ether Ligands
William Levason; Seema Maheshwari; Raju Ratnani; Gillian Reid; Michael Webster; Wenjian Zhang; Inorganic Chemistry 49 (2010) 9036–9048; doi:10.1021/ic101296e

data_4316636
_publ_contact_author_address
;   School of Chemistry
    University of Southampton
    Southampton SO17 1BJ, UK
;
_publ_contact_author_email       gr@soton.ac.uk
_publ_contact_author_fax         '023 8059 3781'
_publ_contact_author_name        'Professor Gillian Reid'
_publ_contact_author_phone       '023 8059 3609'
_publ_section_title
;
 Structural Diversity in Supramolecular Complexes of MCl3 (M = As, Sb, Bi)
 with Constrained Thio- and Seleno-Ether Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9036
_journal_page_last               9048
_journal_paper_doi               10.1021/ic101296e
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H42 Bi4 Cl12 Se6'
_chemical_formula_structural     '3(C10 H14 Se2) (Bi4 Cl12)'
_chemical_formula_sum            'C30 H42 Bi4 Cl12 Se6'
_chemical_formula_weight         2137.72
_chemical_name_systematic
; 
 tris(1,2-bis(methylselenomethyl)benzene)tetrakis(trichlorobismuth(III)) 
;
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Webster, M.'
_audit_creation_date             2010-04-22
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   18.184(3)
_cell_length_b                   18.184(3)
_cell_length_c                   15.147(3)
_cell_measurement_reflns_used    6399
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4337.5(13)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1369
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37383
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.487
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2886
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.314
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.260
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.422(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         5680
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0248P)^2^+77.4498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                4549
_reflns_number_total             5680
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic101296e_si_002_07.cif
_cod_data_source_block           10sm327b
_cod_original_cell_volume        4337.4(13)
_cod_database_code               4316636