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_4323269
_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            'C48 H72 Li N4 S2 Sm'
_chemical_formula_weight         926.58
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             'Wed Sep 30 09:52:04 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 96.98(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.077(4)
_cell_length_b                   13.904(4)
_cell_length_c                   20.516(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     5118(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    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02542
_diffrn_orient_matrix_UB_12      -0.05742
_diffrn_orient_matrix_UB_13      -0.02189
_diffrn_orient_matrix_UB_21      0.04936
_diffrn_orient_matrix_UB_22      -0.02618
_diffrn_orient_matrix_UB_23      -0.00878
_diffrn_orient_matrix_UB_31      0.00486
_diffrn_orient_matrix_UB_32      -0.03451
_diffrn_orient_matrix_UB_33      0.04307
_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  0.024
_diffrn_reflns_av_sigmaI/netI    0.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12625
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         0.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        -4.67
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1940.00
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.40
_refine_ls_abs_structure_Flack   1.00000
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.800
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     759
_refine_ls_number_reflns         6798
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0000
_refine_ls_R_factor_gt           0.0000
_refine_ls_shift/su_max          0.4980
_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          0.0000
_refine_ls_wR_factor_ref         0.0420
_reflns_number_gt                0
_reflns_number_total             12249
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic980901x_4.cif
_cod_data_source_block           '[Li(tmeda)2][Cp*2Sm(SCCPh)]'
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C48 H72 Li N4 S2 Sm '
_cod_database_code               4323269