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_4111477
_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         'C61 H50 Cl2 Os P2, C H2 Cl2'
_chemical_formula_sum            'C62 H52 Cl4 Os P2'
_chemical_formula_weight         1190.98
_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                95.8400(10)
_cell_angle_beta                 100.0340(10)
_cell_angle_gamma                116.6070(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5348(8)
_cell_length_b                   13.5531(8)
_cell_length_c                   17.7530(11)
_cell_measurement_reflns_used    2200
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.72
_cell_measurement_theta_min      2.28
_cell_volume                     2599.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15281
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.761302
_exptl_absorpt_correction_type   'empirical based on SADABS'
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       plate
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10011
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0260P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                8363
_reflns_number_total             10011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0429061si20050118_112431.cif
_cod_data_source_block           Compound4
_cod_database_code               4111477