Oxidation of Tertiary Silanes by Osmium Tetroxide
Karine Valliant-Saunders; Erica Gunn; G. Robert Shelton; David A. Hrovat; Weston Thatcher Borden; James M. Mayer; Inorganic Chemistry 46 (2007) 5212–5219; doi:10.1021/ic062468u

data_4308012
_publ_contact_author_address
;
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195
USA
;
_publ_contact_author_email       wernerka@u.washington.edu
_publ_contact_author_name        'Werner Kaminsky'
_publ_section_title
;
Oxidation of Tertiary Silanes by Osmium Tetroxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5212
_journal_page_last               5219
_journal_paper_doi               10.1021/ic062468u
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C36 H52 N4 O6 Os2, 6(C H2 Cl2)'
_chemical_formula_sum            'C42 H64 Cl12 N4 O6 Os2'
_chemical_formula_weight         1526.77
_chemical_name_common            Os2O6(tbupy)4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 114.251(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2650(13)
_cell_length_b                   23.736(3)
_cell_length_c                   21.737(3)
_cell_measurement_reflns_used    343
_cell_measurement_temperature    130(2)
_cell_volume                     5769.7(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.819
_diffrn_measured_fraction_theta_max 0.752
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \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  0.1176
_diffrn_reflns_av_sigmaI/netI    0.2929
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15030
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    5.001
_exptl_absorpt_correction_T_max  0.7794
_exptl_absorpt_correction_T_min  0.3724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.775
_refine_diff_density_min         -2.516
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         10865
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.2753
_refine_ls_R_factor_gt           0.0874
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.2159
_reflns_number_gt                3518
_reflns_number_total             10865
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic062468u-file004.cif
_cod_data_source_block           shelxl
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5769.7(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4308012