A Ti2Ru2Pd2 Oxo-Sulfido Cluster Synthesized by Linking Two Rationally Preorganized TiRuPdS2 Heterotrimetallic Units with an Oxo Ligand: Its Reaction with an Alkyne
Shigeki Kuwata; Shin-ichiro Kabashima; Youichi Ishii; Masanobu Hidai; Journal of the American Chemical Society 123 (2001) 3826–3827; doi:10.1021/ja0040666

data_4115476
_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       ' skuwata@chembio.t.u-tokyo.ac.jp '
_publ_contact_author_fax         ' +81-3-5841-7265 '
_publ_contact_author_name        ' Shigeki KUWATA'
_publ_contact_author_phone       ' +81-3-5841-7264 '
_publ_section_title
;
 A Ti2Ru2Pd2 Oxo-Sulfido Cluster Synthesized by Linking Two Rationally
 Preorganized TiRuPdS2 Heterotrimetallic Units with an Oxo Ligand: Its
 Reaction with an Alkyne
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3826
_journal_page_last               3827
_journal_paper_doi               10.1021/ja0040666
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C53 H69 O3 P Pd2 Ru2 S4 Ti2'
_chemical_formula_weight         1424.08
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_audit_creation_date             'Tue Feb  8 11:53:43 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 116.47(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.873(5)
_cell_length_b                   11.955(4)
_cell_length_c                   22.234(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      19.8
_cell_volume                     5680(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    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.01567
_diffrn_orient_matrix_UB_12      -0.07094
_diffrn_orient_matrix_UB_13      -0.01097
_diffrn_orient_matrix_UB_21      -0.02744
_diffrn_orient_matrix_UB_22      -0.04422
_diffrn_orient_matrix_UB_23      0.01447
_diffrn_orient_matrix_UB_31      -0.03451
_diffrn_orient_matrix_UB_32      0.00295
_diffrn_orient_matrix_UB_33      -0.04684
_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  0.033
_diffrn_reflns_av_sigmaI/netI    0.066
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6688
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        -8.10
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.621
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.910
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2856.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.75
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.539
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     509
_refine_ls_number_reflns         4804
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.3657
_refine_ls_shift/su_mean         0.0099
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0471
_refine_ls_wR_factor_ref         0.0471
_reflns_number_gt                4804
_reflns_number_total             6536
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja0040666_1.cif
_cod_data_source_block
JA0040666-19-269_[(CpTi)2(Cp*Ru)2Pd2(PPh3)S4OH2].THF.MeOH(3.THF.MeOH)
_cod_original_cell_volume        5680(2)
_cod_original_sg_symbol_H-M      'C c '
_cod_original_formula_sum        'C53 H69 O3 P Pd2 S4 Ru2 Ti2 '
_cod_database_code               4115476