Synthesis of Group 8-Group 6 Heterotrimetallic Polyhydrido Complexes Having Only a C~5~Me~5~ Group as Auxiliary Ligand
Ito, Jun-ichi; Shima, Takanori; Suzuki, Hiroharu; Organometallics 25 (2006) 1333–1336; doi:10.1021/om050963c

data_4074866
_publ_section_title
;
 Synthesis of Group 8-Group 6 Heterotrimetallic Polyhydrido Complexes
 Having Only a C~5~Me~5~ Group as Auxiliary Ligand
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_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1333
_journal_page_last               1336
_journal_paper_doi               10.1021/om050963c
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C32 H54 Mo Ru2'
_chemical_formula_weight         736.83
_chemical_name_systematic
;
 penta(m2-hydrido)-tris(h5-pentamethylcyclopentadienyl)- molybdenum-diruthenium
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 101.95(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.088(6)
_cell_length_b                   12.012(4)
_cell_length_c                   12.627(5)
_cell_measurement_temperature    153(2)
_cell_volume                     1645.3(13)
_computing_cell_refinement       'Rigaku Raxis Rapid Diffractometer Control'
_computing_data_collection       'Rigaku Raxis Rapid Diffractometer Control'
_computing_data_reduction        'Process Auto'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku RAXIS Rapid'
_diffrn_radiation_monochromator  'Imaging Plate'
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3827
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5293
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_preparation       pentane
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.429
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         3827
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.686
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+5.2480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                3426
_reflns_number_total             3827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050963csi20051109_115911.cif
_cod_data_source_block           Ru2MoH5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        1645.3(12)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4074866