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_4074868
_publ_section_title
;
 Synthesis of Group 8-Group 6 Heterotrimetallic Polyhydrido Complexes
 Having Only a C~5~Me~5~ Group as Auxiliary Ligand
;
_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            'C31 H54 Ru W2'
_chemical_formula_weight         895.51
_chemical_name_systematic
;
 penta(m2-hydrido)-tris(h5-pentamethylcyclopentadienyl)-dihydrido- ruthenium-ditungsten
;
_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                94.46(3)
_cell_angle_beta                 100.65(3)
_cell_angle_gamma                110.17(3)
_cell_formula_units_Z            2
_cell_length_a                   8.039(8)
_cell_length_b                   11.224(16)
_cell_length_c                   19.51(3)
_cell_measurement_temperature    223(2)
_cell_volume                     1605(4)
_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      223(2)
_diffrn_measured_fraction_theta_full 0.791
_diffrn_measured_fraction_theta_max 0.791
_diffrn_measurement_device_type  'Rigaku RAXIS CS'
_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    0.0453
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7430
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    7.630
_exptl_absorpt_correction_T_max  1.3167
_exptl_absorpt_correction_T_min  0.5659
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_preparation       pentane
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         4.257
_refine_diff_density_min         -3.187
_refine_diff_density_rms         0.253
_refine_ls_extinction_coef       0.0110(8)
_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   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         7430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0702
_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^)+(0.1142P)^2^+12.8667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2018
_reflns_number_gt                6519
_reflns_number_total             7430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050963csi20051109_115911.cif
_cod_data_source_block           RuW2H7
_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 

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.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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 
;
_cod_original_cell_volume        1605(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074868