Synthesis of Alkynechalcogenolato Complexes of Titanocene(IV) and Samarocene(III) and Formation of a Ti2Ni Trinuclear Cluster [Cp2Ti(μ-SC\τbCPh)2]2Ni
Hiroyasu Sugiyama; Yuji Hayashi; Hiroyuki Kawaguchi; Kazuyuki Tatsumi; Inorganic Chemistry 37 (1998) 6773–6779; doi:10.1021/ic980901x

data_4323268
_publ_section_title
;
 Synthesis of Alkynechalcogenolato Complexes of Titanocene(IV) and
 Samarocene(III) and Formation of a Ti2Ni Trinuclear Cluster
 [Cp2Ti(\m-SC\\tbCPh)2]2Ni
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6773
_journal_page_last               6779
_journal_paper_doi               10.1021/ic980901x
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C66 H56 Ni S4 Ti2'
_chemical_formula_weight         1131.91
_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             'Wed Sep 30 09:53:29 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 93.19(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.203(2)
_cell_length_b                   16.596(9)
_cell_length_c                   25.794(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      3.4
_cell_volume                     5643(3)
_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_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.06412
_diffrn_orient_matrix_UB_12      -0.00391
_diffrn_orient_matrix_UB_13      0.01875
_diffrn_orient_matrix_UB_21      -0.04049
_diffrn_orient_matrix_UB_22      0.00313
_diffrn_orient_matrix_UB_23      -0.03388
_diffrn_orient_matrix_UB_31      0.00193
_diffrn_orient_matrix_UB_32      -0.06005
_diffrn_orient_matrix_UB_33      -0.00295
_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  0.017
_diffrn_reflns_av_sigmaI/netI    0.057
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8100
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        -0.41
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2352.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.203
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     588
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.0020
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                4478
_reflns_number_total             7708
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic980901x_3.cif
_cod_data_source_block           '[Cp2Ti(SCCPh)2]2Ni.2(toluene)'
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C66 H56 Ni S4 Ti2 '
_cod_database_code               4323268