Unexpected Formation of Osmium Carbyne and Vinylidene Complexes from the Reaction of OsCl2(PPh3)3with HC⋮CCMe3
Wen, Ting Bin; Yang, Sheng-Yong; Zhou, Zhong Yuan; Lin, Zhenyang; Lau, Chak-Po; Jia, Guochen; Organometallics 19 (2000) 3757–; doi:10.1021/om000306e

data_4077516
_publ_section_title
;
 Unexpected Formation of Osmium Carbyne and Vinylidene Complexes from the
 Reaction of OsCl2(PPh3)3with HC&#x22EE;CCMe3
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3757
_journal_paper_doi               10.1021/om000306e
_journal_volume                  19
_journal_year                    2000
_chemical_formula_moiety         'C54 H59 Cl Os P2'
_chemical_formula_sum            'C54 H59 Cl Os P2'
_chemical_formula_weight         995.60
_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                78.280(2)
_cell_angle_beta                 70.488(2)
_cell_angle_gamma                65.374(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3785(13)
_cell_length_b                   13.8032(14)
_cell_length_c                   17.2639(17)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2520.4(4)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16949
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    2.679
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'brownish red'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.528
_refine_diff_density_min         -2.146
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         11421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                8616
_reflns_number_total             11421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000306e.cif
_cod_data_source_block           Complex3
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077516