Facile Bismuth-Oxygen Bond Cleavage, C-H Activation, and Formation of a Monodentate Carbon-Bound Oxyaryl Dianion, (C6H2tBu2-3,5-O-4)2-
Ian J. Casely; Joseph W. Ziller; Ming Fang; Filipp Furche; William J. Evans; Journal of the American Chemical Society 133 (2011) 5244–5247; doi:10.1021/ja201128d

data_4105921
_publ_section_title
;
 Facile Bismuth-Oxygen Bond Cleavage, C-H Activation, and Formation of a
 Monodentate Carbon-Bound Oxyaryl Dianion, (C6H2tBu2-3,5-O-4)2-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5244
_journal_page_last               5247
_journal_paper_doi               10.1021/ja201128d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C27 H40.5 Bi N2.5 O'
_chemical_formula_weight         625.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                98.9882(6)
_cell_angle_beta                 96.4784(6)
_cell_angle_gamma                90.1828(6)
_cell_formula_units_Z            4
_cell_length_a                   10.1403(6)
_cell_length_b                   14.3990(8)
_cell_length_c                   18.6374(10)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.19
_cell_volume                     2670.1(3)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0178
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30775
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    6.624
_exptl_absorpt_correction_T_max  0.2249
_exptl_absorpt_correction_T_min  0.1954
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.843
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         12168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0165
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.6522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0399
_reflns_number_gt                11387
_reflns_number_total             12168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja201128d_si_003.cif
_cod_data_source_block           ijc29
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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_formula_sum        'C27 H40.50 Bi N2.50 O'
_cod_database_code               4105921