#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/74/2017408.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2017408
loop_
_publ_author_name
'Dols, Thomas S.'
'Spaniol, Thomas P.'
'Okuda, Jun'
_publ_section_title
;
 Titanium complexes with sulfur-linked bis(phenolate) ligands
;
_journal_coeditor_code           SK3350
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m443
_journal_page_last               m446
_journal_paper_doi               10.1107/S0108270109042280
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ti (C20 H22 O2 S2) Cl2]'
_chemical_formula_moiety         'C20 H22 Cl2 O2 S2 Ti'
_chemical_formula_sum            'C20 H22 Cl2 O2 S2 Ti'
_chemical_formula_weight         477.30
_chemical_name_systematic
;
dichlorido{4,4'-dimethyl-2,2'-[cyclohexane-1,2-
diylbis(sulfanediyl)]diphenolato}titanium(IV)
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 101.1050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7948(2)
_cell_length_b                   10.9672(2)
_cell_length_c                   18.5874(3)
_cell_measurement_reflns_used    6964
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      42.90
_cell_measurement_theta_min      2.67
_cell_volume                     2159.34(7)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            52551
_diffrn_reflns_theta_full        47.82
_diffrn_reflns_theta_max         47.82
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.8831
_exptl_absorpt_correction_T_min  0.7906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS in PLATON; Spek, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.752
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         10145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0423
_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/[σ²(Fo²)+(0.0479P)²+0.2037P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                7452
_reflns_number_total             10145
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sk3350.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2017408
_cod_database_fobs_code          2017408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti Ti1 0.5000 0.468358(18) 0.2500 0.01403(4) Uani d SU 1 . .
Cl Cl1 0.65277(2) 0.34440(2) 0.310568(12) 0.02210(5) Uani d U 1 . .
S S1 0.629178(16) 0.651102(19) 0.317412(11) 0.01551(4) Uani d . 1 . .
O O1 0.41634(6) 0.50037(5) 0.32706(3) 0.01667(10) Uani d . 1 . .
C C1 0.44142(7) 0.57781(7) 0.38397(4) 0.01485(11) Uani d . 1 . .
C C2 0.54474(7) 0.65682(7) 0.39009(4) 0.01555(12) Uani d . 1 . .
C C3 0.57655(8) 0.73407(9) 0.45066(4) 0.01971(14) Uani d . 1 . .
H H3 0.6491 0.7846 0.4552 0.025(3) Uiso calc R 1 . .
C C4 0.50272(8) 0.73765(9) 0.50438(4) 0.02122(15) Uani d . 1 . .
C C5 0.39833(8) 0.65958(9) 0.49692(4) 0.02047(14) Uani d . 1 . .
H H5 0.3470 0.6612 0.5331 0.030(4) Uiso calc R 1 . .
C C6 0.36794(7) 0.57997(8) 0.43824(4) 0.01809(13) Uani d . 1 . .
H H6 0.2974 0.5270 0.4349 0.030(4) Uiso calc R 1 . .
C C7 0.53420(12) 0.82285(12) 0.56888(6) 0.0332(2) Uani d . 1 . .
H H7A 0.5990 0.8808 0.5604 0.056(5) Uiso calc R 1 . .
H H7B 0.5659 0.7757 0.6134 0.064(6) Uiso calc R 1 . .
H H7C 0.4581 0.8675 0.5748 0.050(5) Uiso calc R 1 . .
C C8 0.57147(7) 0.78640(7) 0.26277(4) 0.01534(12) Uani d . 1 . .
H H8 0.6098 0.7849 0.2179 0.022(3) Uiso calc R 1 . .
C C9 0.61727(10) 0.90263(9) 0.30505(5) 0.02400(17) Uani d . 1 . .
H H9A 0.5856 0.9041 0.3516 0.019(3) Uiso calc R 1 . .
H H9B 0.7107 0.9027 0.3172 0.035(4) Uiso calc R 1 . .
C C10 0.57160(13) 1.01629(9) 0.26044(7) 0.0330(2) Uani d . 1 . .
H H10A 0.6003 1.0901 0.2896 0.044(4) Uiso calc R 1 . .
H H10B 0.6082 1.0182 0.2155 0.037(4) Uiso calc R 1 . .
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'
S S 0.1246 0.1234 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ti1 O1 . 2_655 158.33(4) ?
O1 Ti1 Cl1 . 2_655 94.633(19) ?
O1 Ti1 Cl1 2_655 2_655 98.34(2) ?
O1 Ti1 Cl1 . . 98.34(2) ?
O1 Ti1 Cl1 2_655 . 94.633(19) ?
Cl1 Ti1 Cl1 2_655 . 106.142(15) ?
O1 Ti1 S1 . . 77.337(19) ?
O1 Ti1 S1 2_655 . 86.07(2) ?
Cl1 Ti1 S1 2_655 . 165.407(9) ?
Cl1 Ti1 S1 . . 87.242(8) ?
O1 Ti1 S1 . 2_655 86.07(2) ?
O1 Ti1 S1 2_655 2_655 77.337(19) ?
Cl1 Ti1 S1 2_655 2_655 87.242(8) ?
Cl1 Ti1 S1 . 2_655 165.407(9) ?
S1 Ti1 S1 . 2_655 80.132(10) ?
C2 S1 C8 . . 102.92(3) ?
C2 S1 Ti1 . . 95.00(3) ?
C8 S1 Ti1 . . 105.12(3) ?
C1 O1 Ti1 . . 131.99(5) ?
O1 C1 C6 . . 121.51(7) ?
O1 C1 C2 . . 119.49(6) ?
C6 C1 C2 . . 118.99(7) ?
C3 C2 C1 . . 120.60(7) ?
C3 C2 S1 . . 123.59(6) ?
C1 C2 S1 . . 115.81(6) ?
C4 C3 C2 . . 120.57(8) ?
C4 C3 H3 . . 119.7 ?
C2 C3 H3 . . 119.7 ?
C3 C4 C5 . . 118.18(8) ?
C3 C4 C7 . . 121.03(9) ?
C5 C4 C7 . . 120.79(8) ?
C6 C5 C4 . . 121.79(8) ?
C6 C5 H5 . . 119.1 ?
C4 C5 H5 . . 119.1 ?
C5 C6 C1 . . 119.81(8) ?
C5 C6 H6 . . 120.1 ?
C1 C6 H6 . . 120.1 ?
C4 C7 H7A . . 109.5 ?
C4 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C4 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C8 C8 C9 2_655 . 111.58(5) ?
C8 C8 S1 2_655 . 112.77(4) ?
C9 C8 S1 . . 110.33(6) ?
C8 C8 H8 2_655 . 107.3 ?
C9 C8 H8 . . 107.3 ?
S1 C8 H8 . . 107.3 ?
C10 C9 C8 . . 111.30(8) ?
C10 C9 H9A . . 109.4 ?
C8 C9 H9A . . 109.4 ?
C10 C9 H9B . . 109.4 ?
C8 C9 H9B . . 109.4 ?
H9A C9 H9B . . 108.0 ?
C10 C10 C9 2_655 . 110.19(7) ?
C10 C10 H10A 2_655 . 109.6 ?
C9 C10 H10A . . 109.6 ?
C10 C10 H10B 2_655 . 109.6 ?
C9 C10 H10B . . 109.6 ?
H10A C10 H10B . . 108.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 O1 . 1.8678(6) ?
Ti1 O1 2_655 1.8678(6) ?
Ti1 Cl1 2_655 2.2628(2) ?
Ti1 Cl1 . 2.2628(2) ?
Ti1 S1 . 2.6188(2) ?
Ti1 S1 2_655 2.6188(2) ?
S1 C2 . 1.7703(8) ?
S1 C8 . 1.8378(8) ?
O1 C1 . 1.3428(9) ?
C1 C6 . 1.3984(10) ?
C1 C2 . 1.3996(11) ?
C2 C3 . 1.3979(11) ?
C3 C4 . 1.3930(12) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.4007(13) ?
C4 C7 . 1.5062(13) ?
C5 C6 . 1.3863(12) ?
C5 H5 . 0.9500 ?
C6 H6 . 0.9500 ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C8 C8 2_655 1.5246(15) ?
C8 C9 . 1.5288(11) ?
C8 H8 . 1.0000 ?
C9 C10 . 1.5255(15) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C10 C10 2_655 1.520(3) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
