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_4313784
_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         'C14 H12 I2 Ir2 O6 S2 Ti, C H2 Cl2'
_chemical_formula_sum            'C15 H14 Cl2 I2 Ir2 O6 S2 Ti'
_chemical_formula_weight         1111.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4291(9)
_cell_length_b                   9.9988(6)
_cell_length_c                   18.2839(12)
_cell_measurement_reflns_used    6643
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.32
_cell_volume                     2637.9(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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.941
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16328
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    13.089
_exptl_absorpt_correction_T_max  0.181
_exptl_absorpt_correction_T_min  0.054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.22.                  
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.382
_refine_diff_density_min         -4.316
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3300
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+131.0070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                3059
_reflns_number_total             3300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034278esi20030416_101940_1.cif
_cod_data_source_block           compound2a
_cod_database_code               4313784