Synthesis of Trinuclear Osmium Polyhydrido Clusters [{(C5Me5)Os}3(μ-H)6]+and {(C5Me5)Os}3(μ-H)3(μ3-H)2and Comparison with the Ruthenium Analogues
Kameo, Hajime; Suzuki, Hiroharu; Organometallics 27 (2008) 4248–; doi:10.1021/om8003866

data_4071791
_publ_section_title
;
 Synthesis of Trinuclear Osmium Polyhydrido Clusters
 [{(C5Me5)Os}3(\m-H)6]+and {(C5Me5)Os}3(\m-H)3(\m3-H)2and Comparison with
 the Ruthenium Analogues
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4248
_journal_paper_doi               10.1021/om8003866
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C30 H50 Os3'
_chemical_formula_weight         981.30
_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                71.327(2)
_cell_angle_beta                 73.298(4)
_cell_angle_gamma                60.641(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0085(10)
_cell_length_b                   11.0311(6)
_cell_length_c                   15.1064(7)
_cell_measurement_reflns_used    17712
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.98
_cell_volume                     1495.67(18)
_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      153(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17712
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    12.727
_exptl_absorpt_correction_T_max  0.7226
_exptl_absorpt_correction_T_min  0.4020
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (T.Higashi, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         4.974
_refine_diff_density_min         -4.630
_refine_diff_density_rms         0.319
_refine_ls_extinction_coef       0.0017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    ref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         8598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.106
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.0659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                7871
_reflns_number_total             8613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8003866-file002.cif
_cod_data_source_block           7
_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 2.4.1 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      P-1
_cod_database_code               4071791