Osmabenzenes from the Reactions of HC\τbCCH(OH)C\τbCH with OsX2(PPh3)3 (X = Cl, Br)
Haiping Xia; Guomei He; Hong Zhang; Ting Bin Wen; Herman H. Y. Sung; Ian D. Williams; Guochen Jia; Journal of the American Chemical Society 126 (2004) 6862–6863; doi:10.1021/ja0486871

data_4112630
_publ_section_title
;
 Osmabenzenes from the Reactions of HC\\tbCCH(OH)C\\tbCH with OsX2(PPh3)3
 (X = Cl, Br)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6862
_journal_page_last               6863
_journal_paper_doi               10.1021/ja0486871
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C51 H68.5 Cl5 O3.25 Os P5'
_chemical_formula_weight         1255.86
_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                94.3350(10)
_cell_angle_beta                 95.0370(10)
_cell_angle_gamma                104.7610(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4923(7)
_cell_length_b                   14.1998(8)
_cell_length_c                   17.7994(10)
_cell_measurement_reflns_used    5070
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.5363
_cell_measurement_theta_min      2.2818
_cell_volume                     2783.4(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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0523
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            20145
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    2.714
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       bar
_exptl_crystal_F_000             1273
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9691
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                8489
_reflns_number_total             9691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0486871si20040308_082627.cif
_cod_data_source_block           xia2
_cod_original_formula_sum        'C51 H68.50 Cl5 O3.25 Os P5'
_cod_database_code               4112630