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_4111478
_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         'C58 H52 Cl2 Os P2, 2 (C H2 Cl2)'
_chemical_formula_sum            'C60 H56 Cl6 Os P2'
_chemical_formula_weight         1241.89
_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                76.9980(10)
_cell_angle_beta                 73.8680(10)
_cell_angle_gamma                78.6610(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6117(7)
_cell_length_b                   13.9967(8)
_cell_length_c                   16.4390(9)
_cell_measurement_reflns_used    5317
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.19
_cell_volume                     2688.1(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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27916
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_T_max  0.7692
_exptl_absorpt_correction_T_min  0.6073
_exptl_absorpt_correction_type   'empirical based on SADABS'
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10477
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0473P)^2^+3.2031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0824
_reflns_number_gt                9558
_reflns_number_total             10477
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0429061si20050118_112500.cif
_cod_data_source_block           Compound5
_cod_database_code               4111478