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_4111475
_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         'C52 H42 Cl2 Os P2, C7 H8'
_chemical_formula_sum            'C59 H50 Cl2 Os P2'
_chemical_formula_weight         1082.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.1540(10)
_cell_length_b                   24.671(3)
_cell_length_c                   35.434(6)
_cell_measurement_temperature    293(2)
_cell_volume                     9751(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.1110
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8712
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    2.829
_exptl_absorpt_correction_T_max  0.99340
_exptl_absorpt_correction_T_min  0.76915
_exptl_absorpt_correction_type   'empirical based on psi'
_exptl_absorpt_process_details   'PSI correction'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       plate
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         8417
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1430
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                4404
_reflns_number_total             8417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0429061si20050118_112343.cif
_cod_data_source_block           Compound2
_cod_database_code               4111475