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_4072661
_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 
;
_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         'C26 H52 N4 O2 Os2 Pd Si4, C4 H8 O'
_chemical_formula_sum            'C30 H60 N4 O3 Os2 Pd Si4'
_chemical_formula_weight         1123.98
_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
_audit_update_record
; 
2006-07-14   text and data added, jag 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.883(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3500(9)
_cell_length_b                   18.3598(13)
_cell_length_c                   19.9189(13)
_cell_measurement_reflns_used    6199
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      24.77
_cell_measurement_theta_min      2.22
_cell_volume                     4419.7(5)
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_collection       'APEX2 V1.0-27 (Bruker, 2004)'
_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      297(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \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_radiation_wavelength_id  ga43las
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47165
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    6.277
_exptl_absorpt_correction_T_max  0.7354
_exptl_absorpt_correction_T_min  0.2658
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             2184
_exptl_crystal_id                ga43las
_exptl_crystal_preparation
; 
The data crystal was mounted using epoxy to a 0.3 mm cryo-loop 
(Hampton Research) with the (1 0 -9) scattering planes roughly 
normal to the spindle axis. 
;
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.365
_refine_diff_density_min         -1.344
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         10317
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0241P)^2^+9.9778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                7244
_reflns_number_total             10317
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060918ksi20061006_033430.cif
_cod_data_source_block           ga43las
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c  '
_cod_database_code               4072661