An Osmabenzofuran from Reaction between Os(PhC⋮CPh)(CS)(PPh3)2and Methyl Propiolate and the C-Protonation of this Compound to Form a Tethered Osmabenzene
Clark, George R.; Johns, Paul M.; Roper, Warren R.; Wright, L. James; Organometallics 25 (2006) 1771–; doi:10.1021/om0510371

data_4074948
_publ_section_title
;
 An Osmabenzofuran from Reaction between Os(PhC&#x22EE;CPh)(CS)(PPh3)2and
 Methyl Propiolate and the C-Protonation of this Compound to Form a
 Tethered Osmabenzene
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1771
_journal_paper_doi               10.1021/om0510371
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C59 H48 O4 Os P2 S'
_chemical_formula_sum            'C59 H48 O4 Os P2 S'
_chemical_formula_weight         1105.17
_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                91.612(1)
_cell_angle_beta                 99.010(1)
_cell_angle_gamma                114.221(1)
_cell_formula_units_Z            2
_cell_length_a                   11.6740(1)
_cell_length_b                   11.8790(1)
_cell_length_c                   19.4041(1)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    84(2)
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      1.89
_cell_volume                     2410.93(4)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'Ortep-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      84(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       'Area detector \w scans'
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18206
_diffrn_reflns_theta_full        26.56
_diffrn_reflns_theta_max         26.56
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        <2%
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.803
_exptl_absorpt_correction_T_max  0.7669
_exptl_absorpt_correction_T_min  0.4674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1997'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.663
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0058P)^2^+3.0647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0503
_refine_ls_wR_factor_ref         0.0527
_reflns_number_gt                9100
_reflns_number_total             9923
_reflns_threshold_expression     I>2\s(I))
_cod_data_source_file            om0510371si20051204_030917.cif
_cod_data_source_block           pmj212
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2410.89(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074948