Synthesis and Characterization of Osmium-Containing Silsesquioxanes: High-Yield Routes to {Os3(CO)10(μ-H)[(μ-O)Si7O10(c-C6H11)7]} and the New Clusters {Os3(CO)10(μ-H)[(μ-O)Si7O9(OH)2(c-C6H11)7]}, {[Os3(CO)10(μ-H)]2(μ-O)2Si7O9(OH)(c-C6H11)7}, {Os3(CO)10(μ-H)[(μ-O)Si8O11(OH)(c-C6H11)8]}, and {[Os3(CO)10(μ-H)]2(μ-O)2Si8O11(c-C6H11)8}
Lucenti, Elena; Feher, Frank J.; Ziller, Joseph W.; Organometallics 26 (2007) 75–; doi:10.1021/om060844c

data_4072580
_publ_section_title
;
 Synthesis and Characterization of Osmium-Containing
 Silsesquioxanes:&#x00A0; High-Yield Routes to
 {Os3(CO)10(\m-H)[(\m-O)Si7O10(c-C6H11)7]} and the New Clusters
 {Os3(CO)10(\m-H)[(\m-O)Si7O9(OH)2(c-C6H11)7]},
 {[Os3(CO)10(\m-H)]2(\m-O)2Si7O9(OH)(c-C6H11)7},
 {Os3(CO)10(\m-H)[(\m-O)Si8O11(OH)(c-C6H11)8]}, and
 {[Os3(CO)10(\m-H)]2(\m-O)2Si8O11(c-C6H11)8}
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              75
_journal_paper_doi               10.1021/om060844c
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C116 H180 O46 Os6 Si16'
_chemical_formula_weight         3901.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.8740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   51.535(2)
_cell_length_b                   12.9064(5)
_cell_length_c                   24.7552(10)
_cell_measurement_temperature    163(2)
_cell_volume                     15670.7(11)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1351
_diffrn_reflns_av_sigmaI/netI    0.1389
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            83561
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         0.83
_diffrn_standards_decay_%        '< 1.0'
_exptl_absorpt_coefficient_mu    5.041
_exptl_absorpt_correction_T_max  0.7867
_exptl_absorpt_correction_T_min  0.3655
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             7696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.956
_refine_diff_density_min         -2.183
_refine_diff_density_rms         0.432
_refine_ls_extinction_coef       0.00030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         19118
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.0943
_refine_ls_shift/su_max          0.379
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1792P)^2^+82.9626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2741
_refine_ls_wR_factor_ref         0.3557
_reflns_number_gt                7750
_reflns_number_total             19118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060844csi20060914_012913.cif
_cod_data_source_block           fjf41
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        15670.8(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4072580