Stereoselective Oxidative Additions of Iodoalkanes and Activated Alkynes to a Sulfido-Bridged Heterotrinuclear Early-Late (TiIr2) Complex
Miguel A. Casado; Jesús J. Pérez-Torrente; Miguel A. Ciriano; Isabel T. Dobrinovitch; Fernando J. Lahoz; Luis A. Oro; Inorganic Chemistry 42 (2003) 3956–3964; doi:10.1021/ic034278e

data_4313785
_publ_contact_author_address
;
  Dr. Fernando J. Lahoz
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       lahoz@posta.unizar.es
_publ_contact_author_fax         '+34 976 761187'
_publ_contact_author_name        'Dr. Fernando J. Lahoz'
_publ_contact_author_phone       '+34 976 761147'
_publ_section_title
;
 Stereoselective Oxidative Additions of Iodoalkanes and Activated Alkynes
 to a Sulfido-Bridged Heterotrinuclear Early-Late (TiIr2) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3956
_journal_page_last               3964
_journal_paper_doi               10.1021/ic034278e
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C15 H13 I3 Ir2 O6 S2 Ti, 0.5(H2 O)'
_chemical_formula_sum            'C15 H14 I3 Ir2 O6.5 S2 Ti'
_chemical_formula_weight         1175.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.4930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4230(8)
_cell_length_b                   16.7818(12)
_cell_length_c                   13.6965(10)
_cell_measurement_reflns_used    6304
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.16
_cell_measurement_theta_min      2.25
_cell_volume                     2475.1(3)
_computing_cell_refinement       'SAINT+ v. 6.22 (Bruker AXS, 2001)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.22 (Bruker AXS, 2001)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2001'
_computing_publication_material  'XCIF program, SHELXTL v6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14305
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    14.982
_exptl_absorpt_correction_T_max  0.056
_exptl_absorpt_correction_T_min  0.019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 The crystal showed an irregular shape and it was not possible
 to establish a model to apply a numerical absorption correction.
 A multi-scan correction was applied with SADABS program.
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.22.               
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.892
_refine_diff_density_min         -2.816
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4839
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+39.7243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0756
_reflns_number_gt                4421
_reflns_number_total             4839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034278esi20030416_101940_2.cif
_cod_data_source_block           compound3
_cod_original_formula_sum        'C15 H14 I3 Ir2 O6.50 S2 Ti'
_cod_database_code               4313785