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_4112629
_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_moiety         'C77 H63 Cl2 P4 Os, O H, 1.5 C H2 CL2'
_chemical_formula_sum            'C78.5 H67 Cl5 O Os P4'
_chemical_formula_weight         1517.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.6820(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0416(3)
_cell_length_b                   24.7309(2)
_cell_length_c                   18.9007(3)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     7836.5(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens 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  0.1056
_diffrn_reflns_av_sigmaI/netI    0.1820
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29878
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  0.6975
_exptl_absorpt_correction_T_min  0.5323
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       'Habit, blocked'
_exptl_crystal_F_000             3068
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.043
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         13878
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1948
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.2255
_reflns_number_gt                6484
_reflns_number_total             13878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0486871si20040308_082604.cif
_cod_data_source_block           osc5
_cod_original_cell_volume        7836.55(19)
_cod_original_formula_sum        'C78.50 H67 Cl5 O Os P4'
_cod_database_code               4112629