Isolation and X-ray Crystal Structure of an Unusual Biscarbene Metal Complex and Its Reactivity toward Cyclopropanation and Allylic C-H Insertion of Unfunctionalized Alkenes
Yan Li; Jie-Sheng Huang; Zhong-Yuan Zhou; Chi-Ming Che; Journal of the American Chemical Society 123 (2001) 4843–4844; doi:10.1021/ja003184q

data_4115554
_publ_section_title
;
 Isolation and X-ray Crystal Structure of an Unusual Biscarbene Metal
 Complex and Its Reactivity toward Cyclopropanation and Allylic C-H
 Insertion of Unfunctionalized Alkenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4843
_journal_page_last               4844
_journal_paper_doi               10.1021/ja003184q
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C45 H12 F20 N4 O3 Os'
_chemical_formula_weight         1226.79
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.013(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.507(3)
_cell_length_b                   13.088(2)
_cell_length_c                   12.321(3)
_cell_measurement_reflns_used    'Bruker CCD'
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2136.9(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13782
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    3.12
_exptl_absorpt_correction_T_max  0.7882
_exptl_absorpt_correction_T_min  0.5739
_exptl_absorpt_correction_type   SADABS(semi-empirical)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       plate
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.17
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.00000(16)
_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_ref   0.748
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4837
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.750
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                3143
_reflns_number_total             4837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja003184q_4.cif
_cod_data_source_block           complex_5.MeOH
_cod_original_cell_volume        2137.0(7)
_cod_database_code               4115554