Facile One-Pot Synthesis of Triphenylbismuth(V) Bis(carboxylate) Complexes
Kumar, Ish; Bhattacharya, Prateek; Whitmire, Kenton H.; Organometallics 33 (2014) 2906–; doi:10.1021/om500337z

data_4083492
_publ_section_title
;
 Facile One-Pot Synthesis of Triphenylbismuth(V) Bis(carboxylate)
 Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2906
_journal_paper_doi               10.1021/om500337z
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C32 H25 Bi O4'
_chemical_formula_sum            'C32 H25 Bi O4'
_chemical_formula_weight         682.50
_chemical_melting_point          444.6(15)
_chemical_name_systematic
;
 triphenylbismuth bis(benzoate)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                87.535(17)
_cell_angle_beta                 76.790(9)
_cell_angle_gamma                81.595(12)
_cell_formula_units_Z            4
_cell_length_a                   10.566(5)
_cell_length_b                   15.509(8)
_cell_length_c                   16.743(8)
_cell_measurement_temperature    173(2)
_cell_volume                     2642(2)
_computing_molecular_graphics    'DIAMOND 3.2i(Brandenburg, 1997-2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  RigakuSCXminidiffractometer
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13809
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.325
_diffrn_reflns_theta_min         2.499
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.709
_exptl_absorpt_correction_T_max  0.134
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 5.1,1997'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       thinneedles
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         2.926
_refine_diff_density_min         -2.798
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         11531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0468P)^2^+1.2988P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9924
_reflns_number_total             11531
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500337z_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '170-173 degrees C' was changed to
'444.6(15)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083488--4083492.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4083492
_shelx_estimated_absorpt_t_min   0.174
_shelx_estimated_absorpt_t_max   0.238
_shelxl_version_number           2013-2
_shelx_res_checksum              6294