Synthesis of Heterometallic Trinuclear Polyhydrido Clusters Containing Ruthenium and Osmium and Their Electronic and Structural Deviation from Homometallic Systems
Kameo, Hajime; Shima, Takanori; Nakajima, Yumiko; Suzuki, Hiroharu; Organometallics 28 (2009) 2535–; doi:10.1021/om801222h

data_4069052
_publ_section_title
;
 Synthesis of Heterometallic Trinuclear Polyhydrido Clusters Containing
 Ruthenium and Osmium and Their Electronic and Structural Deviation from
 Homometallic Systems
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2535
_journal_paper_doi               10.1021/om801222h
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C59 H81 B O Os Ru2'
_chemical_formula_weight         1209.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.0110(10)
_cell_angle_beta                 87.9720(13)
_cell_angle_gamma                88.6270(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5832(3)
_cell_length_b                   14.6209(4)
_cell_length_c                   17.4584(6)
_cell_measurement_reflns_used    26706
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.08
_cell_volume                     2692.58(14)
_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      183(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26706
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    2.945
_exptl_absorpt_correction_T_max  0.7634
_exptl_absorpt_correction_T_min  0.4809
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.445
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    ref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         12260
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+1.7826P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                10558
_reflns_number_total             12270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801222h_si_002.cif
_cod_data_source_block           7'-BPh4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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      P-1
_cod_database_code               4069052