Synthesis and Structure of Bis- and Tris-Benzyl Bismuth Complexes
Kindra, Douglas R.; Peterson, Jeffrey K.; Ziller, Joseph W.; Evans, William J.; Organometallics 34 (2015) 395–; doi:10.1021/om5010786

data_4085128
_publ_section_title
;
 Synthesis and Structure of Bis- and Tris-Benzyl Bismuth Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              395
_journal_paper_doi               10.1021/om5010786
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C26 H33 Bi N2'
_chemical_formula_weight         582.52
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           169
_space_group_name_Hall           'P 61'
_space_group_name_H-M_alt        'P 61'
_symmetry_space_group_name_Hall  'P 61'
_symmetry_space_group_name_H-M   'P 61'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.7269(5)
_cell_length_b                   9.7269(5)
_cell_length_c                   43.282(2)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.68
_cell_measurement_theta_min      2.46
_cell_volume                     3546.4(3)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2013/1'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            42189
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.684
_diffrn_reflns_theta_min         2.418
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    7.471
_exptl_absorpt_correction_T_max  0.3941
_exptl_absorpt_correction_T_min  0.2097
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2014/2'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.217
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
; 
 Flack x determined using 2646 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.030(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5814
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0182
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+4.1435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0361
_refine_ls_wR_factor_ref         0.0364
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                5611
_reflns_number_total             5814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5010786_si_002.cif
_cod_data_source_block           dk34
_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 

 Adding full bibliography for 4085128--4085129.cif.
;
_cod_original_cell_volume        3546.4(4)
_cod_database_code               4085128
_shelx_estimated_absorpt_t_min   0.183
_shelx_estimated_absorpt_t_max   0.294
_shelxl_version_number           2014-3
_shelx_res_checksum              47747
_shelx_hkl_checksum              4594