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_4077515
_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         'C42 H41 Cl3 Os P2.1/2CH2Cl2'
_chemical_formula_sum            'C42.5 H42 Cl4 Os P2'
_chemical_formula_weight         946.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.406(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9208(13)
_cell_length_b                   20.381(2)
_cell_length_c                   16.6709(16)
_cell_measurement_reflns_used    CCD
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     4252.1(7)
_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      294(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27942
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    3.353
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.347
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9696
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                7146
_reflns_number_total             9696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000306e.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        4252.0(7)
_cod_original_sg_symbol_H-M      'P2(1)/c (No.14)'
_cod_original_formula_sum        'C42.50 H42 Cl4 Os P2'
_cod_database_code               4077515