Insertion of CO2 and COS into Bi-C Bonds: Reactivity of a Bismuth NCN Pincer Complex of an Oxyaryl Dianionic Ligand, [2,6-(Me2NCH2)2C6H3]Bi(C6H2tBu2O)
Douglas R. Kindra; Ian J. Casely; Megan E. Fieser; Joseph W. Ziller; Filipp Furche; William J. Evans; Journal of the American Chemical Society 135 (2013) 7777–7787; doi:10.1021/ja403133f

data_4119793
_publ_section_title
;
 Insertion of CO2 and COS into Bi-C Bonds: Reactivity of a Bismuth NCN
 Pincer Complex of an Oxyaryl Dianionic Ligand,
 [2,6-(Me2NCH2)2C6H3]Bi(C6H2tBu2O)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7777
_journal_page_last               7787
_journal_paper_doi               10.1021/ja403133f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C32 H51 Bi F3 N3 O4 S Si'
_chemical_formula_weight         867.88
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0702(7)
_cell_length_b                   16.4669(9)
_cell_length_c                   37.181(2)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.16
_cell_volume                     7390.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker 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  0.0320
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            80299
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.012
_exptl_absorpt_coefficient_mu    4.913
_exptl_absorpt_correction_T_max  0.4873
_exptl_absorpt_correction_T_min  0.3537
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         8154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0177
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+5.9399P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0384
_refine_ls_wR_factor_ref         0.0401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7120
_reflns_number_total             8154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403133f_si_003.cif
_cod_data_source_block           dk17
_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 
;
_cod_original_cell_volume        7390.0(7)
_cod_database_code               4119793
_shelx_estimated_absorpt_t_min   0.298
_shelx_estimated_absorpt_t_max   0.403
_shelxl_version_number           2012-6
_shelx_res_checksum              93034