Protonation and Bromination of an Osmabenzyne: Reactions Leading to the Formation of New Metallabenzynes
Ting Bin Wen; Sze Ming Ng; Wai Yiu Hung; Zhong Yuan Zhou; Man Fung Lo; Lai-Yung Shek; Ian D. Williams; Zhenyang Lin; Guochen Jia; Journal of the American Chemical Society 125 (2003) 884–885; doi:10.1021/ja029110r

data_4113408
_publ_section_title
;
 Protonation and Bromination of an Osmabenzyne: Reactions Leading to the
 Formation of New Metallabenzynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              884
_journal_page_last               885
_journal_paper_doi               10.1021/ja029110r
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C42 H36 Cl2 Os P2, 1.5 (C H2 Cl2)'
_chemical_formula_sum            'C43.5 H39 Cl5 Os P2'
_chemical_formula_weight         991.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.246(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0243(9)
_cell_length_b                   22.590(2)
_cell_length_c                   17.5821(16)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      1
_cell_volume                     3970.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0728
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23906
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    3.661
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7125
_exptl_absorpt_correction_type   'empirical based on SADABS'
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1964
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.609
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9320
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1027
_reflns_number_gt                6322
_reflns_number_total             9320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029110r-2_s2_2.cif
_cod_data_source_block           Complex4
_cod_original_formula_sum        'C43.50 H39 Cl5 Os P2'
_cod_database_code               4113408