Heterometallic Effects in Nitrogen‒Hydrogen Bond Cleavage by Trinuclear Mixed-Metal Polyhydrido Clusters Containing Ruthenium and Osmium
Kameo, Hajime; Nakajima, Yumiko; Namura, Kyo; Suzuki, Hiroharu; Organometallics 30 (2011) 6703–; doi:10.1021/om200901j

data_4065524
_publ_section_title
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 Heterometallic Effects in Nitrogen--Hydrogen Bond Cleavage by Trinuclear
 Mixed-Metal Polyhydrido Clusters Containing Ruthenium and Osmium
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6703
_journal_paper_doi               10.1021/om200901j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C30 H46 O2 Os3'
_chemical_formula_weight         1009.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
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_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.4828(7)
_cell_length_b                   18.4828(7)
_cell_length_c                   15.7459(4)
_cell_measurement_reflns_used    11791
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.61
_cell_volume                     4658.4(3)
_computing_cell_refinement       'PROCESS-AUTO (T.Higashi, 1998)'
_computing_data_collection       'PROCESS-AUTO (T.Higashi, 1998)'
_computing_data_reduction        'PROCESS-AUTO (T.Higashi, 1998)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method       'oscillation photograph'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku Rotating Anode ultraX18'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0510
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_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11791
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    12.267
_exptl_absorpt_correction_T_max  0.4518
_exptl_absorpt_correction_T_min  0.2478
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (T.Higashi, 1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2820
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.450
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     111
_refine_ls_number_reflns         2358
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_refine_ls_R_factor_all          0.0253
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_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+16.5882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                2237
_reflns_number_total             2373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200901j_si_001.cif
_cod_data_source_block           13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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 'not measured' 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_sg_symbol_H-M      R-3
_cod_database_code               4065524