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#$Date: 2016-03-23 02:44:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179202 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/37/4313784.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313784
loop_
_publ_author_name
'Miguel A. Casado'
'Jesús J. Pérez-Torrente'
'Miguel A. Ciriano'
'Isabel T. Dobrinovitch'
'Fernando J. Lahoz'
'Luis A. Oro'
_publ_contact_author_address
;
  Dr. Fernando J. Lahoz
  Departamento de Química Inorgánica - 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       'ω 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/[σ²(Fo²)+(0.0242P)²+131.0070P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.77916(4) 0.2500 0.66104(3) 0.01704(15) Uani 1 2 d S . .
Ir2 Ir 0.95949(4) 0.2500 0.65348(3) 0.01536(15) Uani 1 2 d S . .
I1 I 0.60262(9) 0.2500 0.61236(7) 0.0388(3) Uani 1 2 d S . .
I2 I 1.13067(7) 0.2500 0.58775(6) 0.0234(2) Uani 1 2 d S . .
Ti Ti 0.82608(19) 0.2500 0.48430(14) 0.0160(5) Uani 1 2 d S . .
S S 0.86471(19) 0.0996(3) 0.58454(14) 0.0178(5) Uani 1 1 d . . .
O1 O 0.7297(6) 0.1191(12) 0.4633(4) 0.038(3) Uani 1 1 d . . .
O2 O 0.7397(7) 0.0293(10) 0.7643(6) 0.041(2) Uani 1 1 d DU . .
O3 O 1.0085(7) 0.0204(11) 0.7528(5) 0.040(2) Uani 1 1 d DU . .
C1 C 0.6509(11) 0.130(2) 0.4308(7) 0.052(4) Uani 1 1 d U . .
C2 C 0.617(3) 0.2500 0.412(2) 0.091(9) Uani 1 2 d SU . .
H2 H 0.5643 0.2500 0.3810 0.109 Uiso 1 2 calc SR . .
C3 C 0.6045(14) 0.001(2) 0.4194(11) 0.068(5) Uani 1 1 d U . .
H3A H 0.6506 -0.0666 0.4065 0.101 Uiso 1 1 calc R . .
H3B H 0.5593 0.0099 0.3797 0.101 Uiso 1 1 calc R . .
H3C H 0.5726 -0.0252 0.4644 0.101 Uiso 1 1 calc R . .
C4 C 0.8577(14) 0.2500 0.3582(10) 0.030(4) Uani 1 2 d S . .
H4 H 0.8082 0.2500 0.3240 0.036 Uiso 1 2 calc SR . .
C5 C 0.9003(8) 0.1371(13) 0.3876(6) 0.024(2) Uani 1 1 d . . .
H5 H 0.8856 0.0467 0.3766 0.029 Uiso 1 1 calc R . .
C6 C 0.9696(8) 0.1816(13) 0.4367(6) 0.022(2) Uani 1 1 d U . .
H6 H 1.0092 0.1260 0.4649 0.027 Uiso 1 1 calc R . .
C7 C 0.7506(8) 0.1053(13) 0.7293(6) 0.024(2) Uani 1 1 d DU . .
C8 C 0.9942(8) 0.1041(13) 0.7184(6) 0.025(2) Uani 1 1 d DU . .
C9 C 0.7824(19) 0.7500 0.6189(13) 0.047(6) Uani 1 2 d S . .
Cl1 Cl 0.8470(4) 0.7500 0.6967(4) 0.0547(15) Uani 1 2 d S . .
Cl2A Cl 0.6615(12) 0.776(2) 0.6414(10) 0.052(6) Uiso 0.25 1 d P . 1
Cl2B Cl 0.6659(19) 0.678(3) 0.6312(15) 0.071(7) Uiso 0.25 1 d P . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Ir1 C7 95.5(6) 7_565 . ?
C7 Ir1 S 161.1(3) 7_565 . ?
C7 Ir1 S 91.0(3) . . ?
C7 Ir1 S 91.0(3) 7_565 7_565 ?
C7 Ir1 S 161.1(3) . 7_565 ?
S Ir1 S 77.76(13) . 7_565 ?
C7 Ir1 Ir2 104.2(3) 7_565 . ?
C7 Ir1 Ir2 104.2(3) . . ?
S Ir1 Ir2 56.95(7) . . ?
S Ir1 Ir2 56.95(7) 7_565 . ?
C7 Ir1 I1 90.6(3) 7_565 . ?
C7 Ir1 I1 90.6(3) . . ?
S Ir1 I1 107.08(7) . . ?
S Ir1 I1 107.08(7) 7_565 . ?
Ir2 Ir1 I1 157.70(4) . . ?
C7 Ir1 Ti 131.9(3) 7_565 . ?
C7 Ir1 Ti 131.9(3) . . ?
S Ir1 Ti 47.40(7) . . ?
S Ir1 Ti 47.40(7) 7_565 . ?
Ir2 Ir1 Ti 75.12(5) . . ?
I1 Ir1 Ti 82.57(6) . . ?
C8 Ir2 C8 97.1(8) 7_565 . ?
C8 Ir2 S 160.0(4) 7_565 . ?
C8 Ir2 S 89.8(4) . . ?
C8 Ir2 S 89.8(4) 7_565 7_565 ?
C8 Ir2 S 160.0(4) . 7_565 ?
S Ir2 S 77.93(13) . 7_565 ?
C8 Ir2 Ir1 103.0(3) 7_565 . ?
C8 Ir2 Ir1 103.0(3) . . ?
S Ir2 Ir1 57.12(7) . . ?
S Ir2 Ir1 57.12(7) 7_565 . ?
C8 Ir2 I2 92.0(3) 7_565 . ?
C8 Ir2 I2 92.0(3) . . ?
S Ir2 I2 106.47(7) . . ?
S Ir2 I2 106.47(7) 7_565 . ?
Ir1 Ir2 I2 157.10(4) . . ?
O1 Ti O1 84.4(7) . 7_565 ?
O1 Ti C6 138.8(4) . 7_565 ?
O1 Ti C6 111.2(4) 7_565 7_565 ?
O1 Ti C6 111.2(4) . . ?
O1 Ti C6 138.8(4) 7_565 . ?
C6 Ti C6 33.9(6) 7_565 . ?
O1 Ti C4 86.9(4) . . ?
O1 Ti C4 86.9(4) 7_565 . ?
C6 Ti C4 57.7(5) 7_565 . ?
C6 Ti C4 57.7(5) . . ?
O1 Ti C5 81.7(4) . . ?
O1 Ti C5 119.9(4) 7_565 . ?
C6 Ti C5 57.3(4) 7_565 . ?
C6 Ti C5 35.0(4) . . ?
C4 Ti C5 34.4(4) . . ?
O1 Ti C5 119.9(4) . 7_565 ?
O1 Ti C5 81.7(4) 7_565 7_565 ?
C6 Ti C5 35.0(4) 7_565 7_565 ?
C6 Ti C5 57.3(4) . 7_565 ?
C4 Ti C5 34.4(4) . 7_565 ?
C5 Ti C5 57.3(6) . 7_565 ?
O1 Ti S 136.6(3) . 7_565 ?
O1 Ti S 84.1(3) 7_565 7_565 ?
C6 Ti S 84.1(3) 7_565 7_565 ?
C6 Ti S 104.9(3) . 7_565 ?
C4 Ti S 133.9(3) . 7_565 ?
C5 Ti S 139.2(3) . 7_565 ?
C5 Ti S 99.5(3) 7_565 7_565 ?
O1 Ti S 84.1(3) . . ?
O1 Ti S 136.6(3) 7_565 . ?
C6 Ti S 104.9(3) 7_565 . ?
C6 Ti S 84.1(3) . . ?
C4 Ti S 133.9(3) . . ?
C5 Ti S 99.5(3) . . ?
C5 Ti S 139.2(3) 7_565 . ?
S Ti S 76.28(15) 7_565 . ?
O1 Ti Ir1 92.6(3) . . ?
O1 Ti Ir1 92.6(3) 7_565 . ?
C6 Ti Ir1 122.9(3) 7_565 . ?
C6 Ti Ir1 122.9(3) . . ?
C4 Ti Ir1 179.4(5) . . ?
C5 Ti Ir1 145.9(3) . . ?
C5 Ti Ir1 145.9(3) 7_565 . ?
S Ti Ir1 46.40(8) 7_565 . ?
S Ti Ir1 46.40(8) . . ?
Ir2 S Ir1 65.93(7) . . ?
Ir2 S Ti 97.99(11) . . ?
Ir1 S Ti 86.20(10) . . ?
C1 O1 Ti 131.7(13) . . ?
O1 C1 C2 121(2) . . ?
O1 C1 C3 113.3(19) . . ?
C2 C1 C3 126(2) . . ?
C1 C2 C1 127(4) 7_565 . ?
C1 C2 H2 116.4 7_565 . ?
C1 C2 H2 116.4 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C5 108.3(16) 7_565 . ?
C5 C4 Ti 73.0(8) 7_565 . ?
C5 C4 Ti 73.0(8) . . ?
C5 C4 H4 125.9 7_565 . ?
C5 C4 H4 125.9 . . ?
Ti C4 H4 119.9 . . ?
C4 C5 C6 107.5(12) . . ?
C4 C5 Ti 72.6(9) . . ?
C6 C5 Ti 72.2(6) . . ?
C4 C5 H5 126.2 . . ?
C6 C5 H5 126.2 . . ?
Ti C5 H5 120.8 . . ?
C6 C6 C5 108.3(7) 7_565 . ?
C6 C6 Ti 73.1(3) 7_565 . ?
C5 C6 Ti 72.8(6) . . ?
C6 C6 H6 125.8 7_565 . ?
C5 C6 H6 125.8 . . ?
Ti C6 H6 120.1 . . ?
O2 C7 Ir1 176.7(11) . . ?
O3 C8 Ir2 175.6(12) . . ?
Cl1 C9 Cl2A 109.7(13) . 7_575 ?
Cl1 C9 Cl2A 109.7(13) . . ?
Cl1 C9 Cl2B 113.4(14) . . ?
Cl1 C9 Cl2B 113.4(14) . 7_575 ?
Cl2B C9 Cl2B 45.9(18) . 7_575 ?
Cl2A Cl2A C9 81.8(8) 7_575 . ?
Cl2B Cl2B C9 67.1(9) 7_575 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 C7 1.955(13) 7_565 ?
Ir1 C7 1.955(13) . ?
Ir1 S 2.396(3) . ?
Ir1 S 2.396(3) 7_565 ?
Ir1 Ir2 2.6056(8) . ?
Ir1 I1 2.6983(15) . ?
Ir1 Ti 3.302(3) . ?
Ir2 C8 1.947(12) 7_565 ?
Ir2 C8 1.947(11) . ?
Ir2 S 2.392(3) . ?
Ir2 S 2.392(3) 7_565 ?
Ir2 I2 2.7469(12) . ?
Ti O1 1.948(9) . ?
Ti O1 1.948(9) 7_565 ?
Ti C6 2.347(11) 7_565 ?
Ti C6 2.347(11) . ?
Ti C4 2.350(18) . ?
Ti C5 2.356(11) . ?
Ti C5 2.356(11) 7_565 ?
Ti S 2.436(3) 7_565 ?
Ti S 2.436(3) . ?
O1 C1 1.288(18) . ?
O2 C7 1.006(13) . ?
O3 C8 1.067(13) . ?
C1 C2 1.34(3) . ?
C1 C3 1.46(3) . ?
C2 C1 1.34(3) 7_565 ?
C2 H2 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.393(17) 7_565 ?
C4 C5 1.393(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.416(16) . ?
C5 H5 0.9500 . ?
C6 C6 1.37(3) 7_565 ?
C6 H6 0.9500 . ?
C9 Cl1 1.70(3) . ?
C9 Cl2A 1.81(3) 7_575 ?
C9 Cl2A 1.81(3) . ?
C9 Cl2B 1.84(4) . ?
C9 Cl2B 1.84(4) 7_575 ?
Cl2A Cl2A 0.52(5) 7_575 ?
Cl2B Cl2B 1.44(5) 7_575 ?
