Electron-Deficient Early-Late Heterobimetallic Sulfido Clusters. Unusual Reactivities of Ti2Ru2S4 Cubane-Type Clusters with Four Cyclopentadienyl Coligands
Shin-ichiro Kabashima; Shigeki Kuwata; Masanobu Hidai; Journal of the American Chemical Society 121 (1999) 7837–7845; doi:10.1021/ja990034a

data_4116499
_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       ' hidai@chembio.t.u-tokyo.ac.jp '
_publ_contact_author_fax         ' +81-3-5800-6945 '
_publ_contact_author_name        ' Masanobu Hidai'
_publ_contact_author_phone       ' +81-3-3812-2111 '
_publ_section_title
;
 Electron-Deficient Early-Late Heterobimetallic Sulfido Clusters. Unusual
 Reactivities of Ti2Ru2S4 Cubane-Type Clusters with Four Cyclopentadienyl
 Coligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7837
_journal_page_last               7845
_journal_paper_doi               10.1021/ja990034a
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C36 H54 F12 N2 O2 P2 Ru2 S4 Ti2'
_chemical_formula_weight         1262.94
_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             'Fri Oct 30 23:01:58 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 105.36(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.284(4)
_cell_length_b                   11.094(4)
_cell_length_c                   21.909(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.3
_cell_volume                     4754(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
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.04586
_diffrn_orient_matrix_UB_12      0.03985
_diffrn_orient_matrix_UB_13      0.01130
_diffrn_orient_matrix_UB_21      0.00950
_diffrn_orient_matrix_UB_22      -0.03419
_diffrn_orient_matrix_UB_23      0.04370
_diffrn_orient_matrix_UB_31      0.02051
_diffrn_orient_matrix_UB_32      -0.07327
_diffrn_orient_matrix_UB_33      -0.01425
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.099
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11211
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        3.11
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2536.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.60
_refine_ls_extinction_coef       0.00033(6)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.855
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6494
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.1890
_refine_ls_shift/su_mean         0.0070
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0355
_refine_ls_wR_factor_ref         0.0355
_reflns_number_gt                6494
_reflns_number_total             10911
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja990034a_3.cif
_cod_data_source_block           '[(CpTi)2(Cp*Ru)2S4][PF6]2.2DMF(5.2DMF)'
_cod_original_cell_volume        4753(2)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C36 H54 F12 N2 O2 P2 S4 Ru2 Ti2 '
_cod_database_code               4116499