Solid-State Structures of Trialkylbismuthines BiR3(R = Me,i-Pr)
Schulz, Stephan; Kuczkowski, Andreas; Bläser, Dieter; Wölper, Christoph; Jansen, Georg; Haack, Rebekka; Organometallics 32 (2013) 5445–; doi:10.1021/om400730r

data_4081634
_publ_contact_author
;
         Prof. Dr. Schulz, Stephan
         Fachbereich Chemie der
         Universit\"at Duisburg-Essen
         Campus Essen, Universit\"atsstr. 7
         D-45141 Essen, Germany
;
_publ_section_title
;
 Solid-State Structures of Trialkylbismuthines BiR3(R = Me,i-Pr)
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5445
_journal_paper_doi               10.1021/om400730r
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C9 H21 Bi'
_chemical_formula_sum            'C9 H21 Bi'
_chemical_formula_weight         338.24
_chemical_melting_point          191.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_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                 109.833(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.7023(3)
_cell_length_b                   10.0311(4)
_cell_length_c                   7.8506(3)
_cell_measurement_reflns_used    9062
_cell_measurement_temperature    141(2)
_cell_measurement_theta_max      30.7
_cell_measurement_theta_min      3.2
_cell_volume                     570.58(4)
_computing_cell_refinement       'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_data_collection       'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_data_reduction        'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_solution    'BRUKER AXS SMART APEX 2 Vers. 3.0-2009'
_diffrn_ambient_temperature      141(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.677
_diffrn_measured_fraction_theta_max 0.677
_diffrn_measurement_device_type
; 
 Siemens SMART three axis goniometer with APEX II area detector system
;
_diffrn_measurement_method       '\w-scans with chi = 0'
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10969
_diffrn_reflns_theta_full        30.66
_diffrn_reflns_theta_max         30.66
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    15.394
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cylindric
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.058
_refine_diff_density_min         -2.533
_refine_diff_density_rms         0.215
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.083(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2331
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+0.0475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0627
_reflns_number_gt                2246
_reflns_number_total             2331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400730r_si_002.cif
_cod_data_source_block           chw_ipr3bi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '-82' was changed to '191.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4081634