C‒H Bond Activation in a Molybdenumoxo-Bismuth Compound
Knispel, Christina; Limberg, Christian; Organometallics 30 (2011) 3701–; doi:10.1021/om2004223

data_4064914
_publ_section_title
;
 C--H Bond Activation in a Molybdenumoxo-Bismuth Compound
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3701
_journal_paper_doi               10.1021/om2004223
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C28 H37 Bi Mo N2 O Si2, 0.5(C7 H8)'
_chemical_formula_sum            'C31.5 H41 Bi Mo N2 O Si2'
_chemical_formula_weight         824.76
_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           SHELXL-97
_cell_angle_alpha                105.113(6)
_cell_angle_beta                 95.320(6)
_cell_angle_gamma                92.209(6)
_cell_formula_units_Z            2
_cell_length_a                   9.0300(7)
_cell_length_b                   10.6630(8)
_cell_length_c                   16.9402(13)
_cell_measurement_reflns_used    46540
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      2.27
_cell_volume                     1564.6(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        XPREP
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS 2T diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,316 exposures'
_diffrn_radiation_collimation    '0.5 mm diameter monocapillary'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'long fine focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22967
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    6.120
_exptl_absorpt_correction_T_max  0.68093
_exptl_absorpt_correction_T_min  0.21998
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The crystal faces were indexed by microscope on the diffractometer. After 
that a numerical absorption correction basing on a Gaussian algorithsm 
was applied, which is implemented in the X-RED program (Stoe, 2002).
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.852
_refine_diff_density_min         -2.452
_refine_diff_density_rms         0.167
_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     351
_refine_ls_number_reflns         7704
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                7145
_reflns_number_total             7704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2004223_si_002.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C31.50 H41 Bi Mo N2 O Si2'
_cod_database_code               4064914