Synthesis, Structure, and Reactivity of Organometallic Osmium(VI) Hydroxo Compounds
Kiefer, Adam M.; Giles, John A.; Shapley, Patricia A.; Organometallics 26 (2007) 1881–; doi:10.1021/om060918k

data_4072662
_publ_contact_author
; 
Patricia A. Shapley 
University of Illinois 
School of Chemical Sciences 
A404 Chemical and Life Sciences Building, MC-712 
601 S. Goodwin Ave 
Urbana, Illinois  61801 
USA 
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_publ_section_title
;
 Synthesis, Structure, and Reactivity of Organometallic Osmium(VI) Hydroxo
 Compounds
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1881
_journal_paper_doi               10.1021/om060918k
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C16 H36 N, C8 H24 N O2 Os Si2'
_chemical_formula_sum            'C24 H60 N2 O2 Os Si2'
_chemical_formula_weight         655.12
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2006-07-14  text and data added, amk 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.045(6)
_cell_length_b                   19.289(8)
_cell_length_c                   22.687(9)
_cell_measurement_reflns_used    958
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.15
_cell_measurement_theta_min      2.66
_cell_volume                     6584(5)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2001)'
_computing_publication_material  'XCIF (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  hydro5
_diffrn_reflns_av_R_equivalents  0.2908
_diffrn_reflns_av_sigmaI/netI    0.1667
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51024
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        5.8
_diffrn_standards_interval_time  304
_diffrn_standards_number         132
_exptl_absorpt_coefficient_mu    3.966
_exptl_absorpt_correction_T_max  0.8526
_exptl_absorpt_correction_T_min  0.3829
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             2704
_exptl_crystal_id                hydro5
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (3 2 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.783
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         6030
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1715
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1191
_reflns_number_gt                2962
_reflns_number_total             6030
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060918ksi20061006_033450.cif
_cod_data_source_block           hydro5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_sg_symbol_Hall     '-P 2ac 2ab '
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               4072662