Synthesis of TiRu2 Heterobimetallic and TiRuM (M = Rh, Ir, Pd, Pt) Heterotrimetallic Sulfido Clusters from a Hydrosulfido-Bridged Titanium-Ruthenium Complex
Shigeki Kuwata; Shin-ichiro Kabashima; Nobuyuki Sugiyama; Youichi Ishii; Masanobu Hidai; Inorganic Chemistry 40 (2001) 2034–2040; doi:10.1021/ic0009324

data_4319537
_publ_contact_author_address
;
    Department of Chemistry and Biotechnology, Graduate School of Engineering,
The University of Tokyo, Hongo, Bunkyo-ku, Tokyo 113-8656, Japan
;
_publ_contact_author_email       ' ishii@chembio.t.u-tokyo.ac.jp '
_publ_contact_author_fax         ' +81-3-5841-7265 '
_publ_contact_author_name        ' Youichi ISHII'
_publ_contact_author_phone       ' +81-3-5841-7264 '
_publ_section_title
;
 Synthesis of TiRu2 Heterobimetallic and TiRuM (M = Rh, Ir, Pd, Pt)
 Heterotrimetallic Sulfido Clusters from a Hydrosulfido-Bridged
 Titanium-Ruthenium Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2034
_journal_page_last               2040
_journal_paper_doi               10.1021/ic0009324
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C51 H51 Cl P2 Pd S2 Ru Ti '
_chemical_formula_sum            'C51 H51 Cl P2 Pd Ru S2 Ti'
_chemical_formula_weight         1080.85
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             'Fri Jun  9 19:45:48 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 102.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.259(4)
_cell_length_b                   16.438(4)
_cell_length_c                   26.092(5)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.9
_cell_volume                     4719(2)
_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
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.01658
_diffrn_orient_matrix_UB_12      -0.03745
_diffrn_orient_matrix_UB_13      0.03090
_diffrn_orient_matrix_UB_21      0.01074
_diffrn_orient_matrix_UB_22      0.04793
_diffrn_orient_matrix_UB_23      0.02415
_diffrn_orient_matrix_UB_31      -0.08871
_diffrn_orient_matrix_UB_32      -0.00120
_diffrn_orient_matrix_UB_33      0.00019
_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  0.023
_diffrn_reflns_av_sigmaI/netI    0.059
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11067
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        -0.55
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            darkbrown
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2192.00
_exptl_crystal_size_max          0.900
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.99
_refine_diff_density_min         -0.57
_refine_ls_extinction_coef       0.0003(1)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   2.170
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7954
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.0400
_refine_ls_shift/su_mean         0.0060
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0461
_reflns_number_gt                7954
_reflns_number_total             10832
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic0009324_4.cif
_cod_data_source_block           '[(CpTiCl)(Cp*Ru){Pd(PPh3)2}S2H](5a)'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_reflns_observed_expression' tag replaced with
'_reflns_threshold_expression' tag as specified in the replacement
file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_site_calc_flags'
tag replaced with '_atom_site_calc_flag' tag as specified in the
replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_type_scat_imag'
tag replaced with '_atom_type_scat_dispersion_imag' tag as specified
in the replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 3137 2015-03-23 15:08:43Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C51 H51 Cl P2 Pd S2 Ru Ti '
_cod_database_code               4319537