Neutral and anionic aryloxy halides of bismuth(III)
Hodge, Philip; James, Siân C.; Norman, Nicholas C.; Orpen, A. Guy; Journal of the Chemical Society, Dalton Transactions  (1998) 4049–; doi:10.1039/a806647g

data_7027094
_publ_section_title
;
 Neutral and anionic aryloxy halides of bismuth(III)
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4049
_journal_paper_doi               10.1039/a806647g
_journal_year                    1998
_chemical_formula_structural     '[P Ph4]2 [Bi Br3 (O -2,4,6-Me3 C6 H2)2]'
_chemical_formula_sum            'C66 H62 Bi Br3 O2 P2'
_chemical_formula_weight         1397.81
_chemical_name_systematic
; 
 Bis tetraphenylphosphonium Tribromo Bis trimethylphenoxy bismuthate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.7700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5964(5)
_cell_length_b                   13.1136(6)
_cell_length_c                   38.747(2)
_cell_measurement_reflns_used    267
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.550
_cell_measurement_theta_min      14.450
_cell_volume                     5862.4(5)
_computing_cell_refinement       'SAINT (Siemens, 1995b)'
_computing_data_collection       'SMART (Siemens, 1995b)'
_computing_data_reduction        'SAINT (Siemens, 1995b)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995a)'
_computing_publication_material  'SHELXTL (Siemens, 1995a)'
_computing_structure_refinement  'SHELXTL (Siemens, 1995a)'
_computing_structure_solution    'SHELXTL (Siemens, 1995a)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Area Detector'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.1043
_diffrn_reflns_av_sigmaI/netI    0.1449
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            36656
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    5.150
_exptl_absorpt_correction_T_max  0.491535
_exptl_absorpt_correction_T_min  0.445101
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.169
_refine_diff_density_min         -2.228
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       0.00084(8)
_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_all   1.009
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         13385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.1477
_refine_ls_R_factor_obs          0.0659
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+39.5212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1716
_refine_ls_wR_factor_obs         0.1326
_reflns_number_observed          7431
_reflns_number_total             13388
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806647Gsup1.cif
_cod_data_source_block           5
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+39.5212P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+39.5212P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5862.5(4)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027094