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_4115552
_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            'C71 H34 Cl2 F20 N4 O2 Os'
_chemical_formula_weight         1616.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.515(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7755(15)
_cell_length_b                   15.3103(13)
_cell_length_c                   25.012(2)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     6394.3(9)
_computing_cell_refinement       'bruker smart '
_computing_data_collection       'bruker smart '
_computing_data_reduction        shelxtl
_computing_molecular_graphics    shelxtl
_computing_publication_material  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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker CCD Area Detector '
_diffrn_measurement_method       'phi and omega scan '
_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  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41733
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    2.187
_exptl_absorpt_correction_T_max  0.6942
_exptl_absorpt_correction_T_min  0.5598
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       0.00000(4)
_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   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         14601
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.004
_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          0.1264
_refine_ls_wR_factor_ref         0.1415
_reflns_number_gt                10458
_reflns_number_total             14601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja003184q_2.cif
_cod_data_source_block           complex_3.2H2O.CH2Cl2
_cod_original_cell_volume        6394.2(10)
_cod_database_code               4115552