Syntheses of Metallabenzynes from an Allenylcarbene Complex
Ting Bin Wen; Wai Yiu Hung; Herman H. Y. Sung; Ian D. Williams; Guochen Jia; Journal of the American Chemical Society 127 (2005) 2856–2857; doi:10.1021/ja0429061

data_4111476
_publ_section_title
;
 Syntheses of Metallabenzynes from an Allenylcarbene Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2856
_journal_page_last               2857
_journal_paper_doi               10.1021/ja0429061
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C60 H48 Cl2 Os P2, C H2 Cl2'
_chemical_formula_sum            'C61 H50 Cl4 Os P2'
_chemical_formula_weight         1176.95
_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                77.178(2)
_cell_angle_beta                 70.503(2)
_cell_angle_gamma                78.564(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7467(11)
_cell_length_b                   14.0114(12)
_cell_length_c                   17.2587(15)
_cell_measurement_temperature    293(2)
_cell_volume                     2807.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.2431
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19390
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    2.555
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8353
_exptl_absorpt_correction_type   'empirical based on SADABS'
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       needle
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.379
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         13363
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.1903
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0719P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1887
_reflns_number_gt                5271
_reflns_number_total             13363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0429061si20050118_112412.cif
_cod_data_source_block           Compound3
_cod_database_code               4111476