Oxidative Addition of Diphenyldichalcogenides PhEEPh (E = S, Se, Te) to Low-Valent CN- and NCN-Chelated Organoantimony and Organobismuth Compounds
Šimon, Petr; Jambor, Roman; Růžička, Aleš; Dostál, Libor; Organometallics 32 (2013) 239–; doi:10.1021/om3010383

data_4079903
_publ_section_title
;
 Oxidative Addition of Diphenyldichalcogenides PhEEPh (E = S, Se, Te) to
 Low-Valent CN- and NCN-Chelated Organoantimony and Organobismuth
 Compounds
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              239
_journal_paper_doi               10.1021/om3010383
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C38 H44 Bi2 Cl4 N2, C H2 Cl2'
_chemical_formula_sum            'C39 H46 Bi2 Cl6 N2'
_chemical_formula_weight         1173.44
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 108.194(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0140(12)
_cell_length_b                   13.9370(13)
_cell_length_c                   23.325(2)
_cell_measurement_reflns_used    66274
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     4327.9(7)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution
;SUPERFLIP (Palatinus & Chapuis, 2007)
Palatinus L., Chapuis G. (2007):  J. Appl. Cryst. 40, 786-790
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_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  0.0952
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            62674
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         4.125
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.520
_exptl_absorpt_correction_T_max  0.521
_exptl_absorpt_correction_T_min  0.159
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_description       plate
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.110
_refine_diff_density_max         2.253
_refine_diff_density_min         -1.799
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         8762
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0033P)^2^+54.2650P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0919
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7020
_reflns_number_total             8762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om3010383_si_002.cif
_cod_data_source_block           5
_cod_database_code               4079903
_diffrn_reflns_sigmai/neti       0.0487