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_4074950
_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 H49 I3 O4 Os1 P2 S1, 0.88(C1 H2 Cl2), 0.12(C1 H1 Cl3)
;
_chemical_formula_sum            'C60 H50.88 Cl2.12 I3 O4 Os P2 S'
_chemical_formula_weight         1576.11
_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                82.513(1)
_cell_angle_beta                 75.312(1)
_cell_angle_gamma                64.78
_cell_formula_units_Z            2
_cell_length_a                   12.7455(1)
_cell_length_b                   14.9228(2)
_cell_length_c                   17.4255(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    84(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      1.51
_cell_volume                     2899.46(6)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27934
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        <2%
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.031
_exptl_absorpt_correction_T_max  0.5648
_exptl_absorpt_correction_T_min  0.3982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1997'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.808
_refine_diff_density_min         -1.908
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         11733
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+26.4795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                10423
_reflns_number_total             11733
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om0510371si20051204_031024.cif
_cod_data_source_block           pmj235
_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        2899.53(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074950