Stable Osmium Hydrido−Carbene Complexes with CH2and Secondary Carbenes CHR as Ligands
Werner, Helmut; Stüer, Wolfram; Laubender, Matthias; Lehmann, Christopher; Herbst-Irmer, Regine; Organometallics 16 (1997) 2236–; doi:10.1021/om970139r

data_4078371
_publ_contact_author
;
        Prof. Dr. Helmut Werner
        Institut f\"ur Anorganische Chemie
        Universit\"at W\"urzburg
        Am Hubland
        D-97074 W\"urzburg
        Deutschland
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_publ_section_title
;
 Stable Osmium Hydrido&#x2212;Carbene Complexes with CH2and Secondary
 Carbenes CHR as Ligands
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2236
_journal_paper_doi               10.1021/om970139r
_journal_volume                  16
_journal_year                    1997
_chemical_formula_sum            'C23 H53 Cl O Os P2 Si'
_chemical_formula_weight         661.33
_chemical_melting_point          405.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_symmetry_Int_Tables_number      14
_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     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.74(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.101(2)
_cell_length_b                   16.847(3)
_cell_length_c                   20.226(3)
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_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.02
_cell_volume                     3094.5(10)
_computing_cell_refinement       'Siemens SAINT (V. 4. 050, Siemens 1996)'
_computing_data_collection       'Siemens SMART (V. 4. 050, Siemens 1996)'
_computing_data_reduction        'Siemens SAINT (V. 4. 050, Siemens 1996)'
_computing_molecular_graphics    'Siemens SHELXTL (V. 5.05)'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Stoe-Siemens-Huber 4 circle diffractometer'
_diffrn_measurement_method       'phi scan'
_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  0.0568
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_min         2.35
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_exptl_absorpt_correction_T_min  0.5798
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_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       blocks
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_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    refxyz
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_refine_ls_number_reflns         5297
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_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_obs          0.0283
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0592
_refine_ls_wR_factor_obs         0.0577
_reflns_number_observed          3788
_reflns_number_total             5297
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om970139r.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '132_C' was changed to '405.15' - it
was converted from degrees Celsius(C) to
Kelvins(K).

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

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4078371