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_4113407
_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         'C48 H54 Cl O Os P2 Si2, B F4, 2(CH2 Cl2)'
_chemical_formula_sum            'C50 H58 B Cl5 F4 O Os P2 Si2'
_chemical_formula_weight         1247.34
_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                80.135(3)
_cell_angle_beta                 78.298(2)
_cell_angle_gamma                88.082(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1352(15)
_cell_length_b                   13.9997(16)
_cell_length_c                   17.118(2)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2805.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Smart CCD Area Detector'
_diffrn_measurement_method       \w
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19130
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.658
_exptl_absorpt_correction_T_max  0.935674
_exptl_absorpt_correction_T_min  0.757176
_exptl_absorpt_correction_type   'empirical based on SADABS'
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Purplish-red
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         12719
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                10448
_reflns_number_total             12719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029110r-2_s2_1.cif
_cod_data_source_block           complex2
_cod_original_cell_volume        2805.5(6)
_cod_database_code               4113407