Synthesis, Characterization, and Structure Determination of the Heterobimetallic Polyhydride Complexes (C5Me5)Ru(μ-H)3MH3(C5Me5) (M = Mo, W) Containing Group VI and Group VIII Metals
Shima, Takanori; Ito, Jun-ichi; Suzuki, Hiroharu; Organometallics 20 (2001) 10–; doi:10.1021/om000769k

data_4077217
_publ_contact_author
;
    Hiroharu Suzuki
    Department of Applied Chemistry 
    Graduate School of Science and Engineering
    Tokyo Institute of Technology and CREST
    O-okayama Meguro-ku Tokyo
    152-8552 Japan
;
_publ_section_title
;
 Synthesis, Characterization, and Structure Determination of the
 Heterobimetallic Polyhydride Complexes (C5Me5)Ru(\m-H)3MH3(C5Me5) (M =
 Mo, W) Containing Group VI and Group VIII Metals
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              10
_journal_paper_doi               10.1021/om000769k
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         'C20 H36 Ru W '
_chemical_formula_sum            'C20 H36 Ru W'
_chemical_formula_weight         561.42
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Wed Sep  7 11:52:45 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 101.14(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.070(3)
_cell_length_b                   19.196(5)
_cell_length_c                   14.320(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     2176.5(12)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.08067
_diffrn_orient_matrix_UB_12      0.00806
_diffrn_orient_matrix_UB_13      0.04385
_diffrn_orient_matrix_UB_21      -0.05065
_diffrn_orient_matrix_UB_22      -0.04704
_diffrn_orient_matrix_UB_23      -0.01630
_diffrn_orient_matrix_UB_31      0.08293
_diffrn_orient_matrix_UB_32      -0.02088
_diffrn_orient_matrix_UB_33      0.05364
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.054
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5514
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        -6.20
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.978
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1096.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.96
_refine_diff_density_min         -1.78
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.339
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     0
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0391
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00005|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0472
_reflns_number_observed          3595
_reflns_number_total             5162
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            om000769k.cif
_cod_data_source_block           RUWH6
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00005|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00005|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2176(1)
_cod_original_sg_symbol_H-M      'P 21/n       '
_cod_original_formula_sum        'C20 H36 Ru W '
_cod_database_code               4077217