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_4083488
_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 H23 Bi Br2 O6'
_chemical_formula_sum            'C32 H23 Bi Br2 O6'
_chemical_formula_weight         872.30
_chemical_melting_point          461.6(15)
_chemical_name_systematic
;
 triphenylbismuth bis(5-bromosalicylate)
;
_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                87.118(6)
_cell_angle_beta                 84.411(6)
_cell_angle_gamma                67.603(5)
_cell_formula_units_Z            2
_cell_length_a                   9.0651(6)
_cell_length_b                   10.7285(7)
_cell_length_c                   16.4782(12)
_cell_measurement_temperature    173(2)
_cell_volume                     1474.50(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  RigakuSCXminidiffractometer
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15173
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.390
_diffrn_reflns_theta_min         3.201
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.732
_exptl_absorpt_correction_T_max  0.489
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 5.1,1997'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       thinneedles
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.040
_refine_diff_density_min         -2.152
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       0.0360(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0348
_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^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6226
_reflns_number_total             6682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500337z_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '187-190 degrees C' was changed to
'461.6(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               4083488
_shelx_estimated_absorpt_t_min   0.186
_shelx_estimated_absorpt_t_max   0.535
_shelxl_version_number           2013-2
_shelx_res_checksum              94831