#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:42:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178578 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/88/4068859.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_4068859
loop_
_publ_author_name
'Jia, Ai-Quan'
'Jin, Guo-Xin'
_publ_section_title
;
 Syntheses, Reactions, and Ethylene Polymerization of Titanium Complexes
 with [N, O, S] Ligands
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1872
_journal_paper_doi               10.1021/om801131b
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C38 H46 N2 O6 S2 Ti2'
_chemical_formula_weight         786.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.860(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.591(7)
_cell_length_b                   12.380(4)
_cell_length_c                   16.618(5)
_cell_measurement_reflns_used    830
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.250
_cell_measurement_theta_min      2.692
_cell_volume                     4031(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9463
_diffrn_reflns_theta_full        27.16
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        3.47
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_correction_T_min  0.9376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4313
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0649P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                2542
_reflns_number_total             4313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801131b_si_001.cif
_cod_data_source_block           f81107b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4068859
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_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
Ti1 Ti 0.22134(3) 0.29554(4) 0.39066(4) 0.03499(18) Uani 1 1 d . . .
S1 S 0.29691(5) 0.37611(7) 0.34313(6) 0.0496(3) Uani 1 1 d . A .
O1 O 0.19861(10) 0.19166(14) 0.46430(13) 0.0335(5) Uani 1 1 d . . .
O2 O 0.19264(11) 0.42657(16) 0.40131(14) 0.0463(6) Uani 1 1 d . . .
O3 O 0.15416(11) 0.25571(18) 0.28136(14) 0.0524(6) Uani 1 1 d . . .
N1 N 0.28282(13) 0.15150(18) 0.39182(16) 0.0363(6) Uani 1 1 d . . .
C1 C 0.16877(15) 0.0947(2) 0.42619(19) 0.0361(7) Uani 1 1 d . A .
C2 C 0.11132(17) 0.0629(3) 0.4283(2) 0.0488(8) Uani 1 1 d . . .
H2 H 0.0926 0.1080 0.4545 0.059 Uiso 1 1 calc R . .
C3 C 0.08110(19) -0.0360(3) 0.3914(3) 0.0657(11) Uani 1 1 d . . .
H3 H 0.0416 -0.0562 0.3918 0.079 Uiso 1 1 calc R . .
C4 C 0.1093(2) -0.1043(3) 0.3541(3) 0.0671(11) Uani 1 1 d . . .
H4 H 0.0895 -0.1712 0.3308 0.081 Uiso 1 1 calc R . .
C5 C 0.16671(19) -0.0735(3) 0.3516(2) 0.0539(9) Uani 1 1 d . A .
H5 H 0.1857 -0.1200 0.3266 0.065 Uiso 1 1 calc R . .
C6 C 0.19716(16) 0.0280(2) 0.3864(2) 0.0389(7) Uani 1 1 d . . .
C7 C 0.25741(16) 0.0561(2) 0.3810(2) 0.0402(7) Uani 1 1 d . A .
H7 H 0.2795 0.0005 0.3687 0.048 Uiso 1 1 calc R . .
C8 C 0.34500(16) 0.1680(2) 0.3910(2) 0.0375(7) Uani 1 1 d . A .
C9 C 0.35636(16) 0.2724(2) 0.3683(2) 0.0409(8) Uani 1 1 d . . .
C10 C 0.41640(17) 0.2924(3) 0.3666(2) 0.0511(9) Uani 1 1 d . A .
H10 H 0.4245 0.3611 0.3516 0.061 Uiso 1 1 calc R . .
C11 C 0.46409(18) 0.2122(3) 0.3869(2) 0.0586(10) Uani 1 1 d . . .
H11 H 0.5037 0.2267 0.3847 0.070 Uiso 1 1 calc R A .
C12 C 0.45292(17) 0.1103(3) 0.4104(2) 0.0574(10) Uani 1 1 d . A .
H12 H 0.4852 0.0562 0.4246 0.069 Uiso 1 1 calc R . .
C13 C 0.39385(17) 0.0884(3) 0.4129(2) 0.0488(8) Uani 1 1 d . . .
H13 H 0.3869 0.0198 0.4295 0.059 Uiso 1 1 calc R A .
C14 C 0.1564(2) 0.5176(3) 0.3480(3) 0.0740(12) Uani 1 1 d . . .
H14 H 0.1372 0.4966 0.2828 0.089 Uiso 1 1 calc R . .
C15 C 0.2040(3) 0.6073(3) 0.3640(4) 0.1111(19) Uani 1 1 d . . .
H15A H 0.2200 0.6368 0.4248 0.167 Uiso 1 1 calc R . .
H15B H 0.1809 0.6626 0.3183 0.167 Uiso 1 1 calc R . .
H15C H 0.2421 0.5810 0.3592 0.167 Uiso 1 1 calc R . .
C16 C 0.0988(3) 0.5422(4) 0.3607(4) 0.130(2) Uani 1 1 d . . .
H16A H 0.0700 0.4797 0.3456 0.195 Uiso 1 1 calc R . .
H16B H 0.0732 0.6009 0.3207 0.195 Uiso 1 1 calc R . .
H16C H 0.1150 0.5623 0.4241 0.195 Uiso 1 1 calc R . .
C17 C 0.1151(5) 0.2208(7) 0.1923(4) 0.217(5) Uani 0.391(16) 1 d PD A 1
H17B H 0.0813 0.2790 0.1727 0.261 Uiso 0.391(16) 1 calc PR A 1
C18 C 0.1383(4) 0.2461(9) 0.1286(5) 0.233(5) Uani 0.391(16) 1 d PD A 1
H18A H 0.1357 0.1827 0.0937 0.350 Uiso 0.391(16) 1 calc PR A 1
H18B H 0.1847 0.2708 0.1624 0.350 Uiso 0.391(16) 1 calc PR A 1
H18C H 0.1100 0.3018 0.0870 0.350 Uiso 0.391(16) 1 calc PR A 1
C19 C 0.0677(7) 0.1360(9) 0.1587(10) 0.124(8) Uani 0.391(16) 1 d PD A 1
H19A H 0.0489 0.1262 0.1988 0.186 Uiso 0.391(16) 1 calc PR A 1
H19B H 0.0901 0.0708 0.1571 0.186 Uiso 0.391(16) 1 calc PR A 1
H19C H 0.0318 0.1531 0.0972 0.186 Uiso 0.391(16) 1 calc PR A 1
C17' C 0.1151(5) 0.2208(7) 0.1923(4) 0.217(5) Uani 0.609(16) 1 d P A 2
H17A H 0.1179 0.1419 0.1972 0.261 Uiso 0.609(16) 1 calc PR A 2
C18' C 0.1383(4) 0.2461(9) 0.1286(5) 0.233(5) Uani 0.609(16) 1 d P A 2
H18D H 0.1856 0.2274 0.1557 0.350 Uiso 0.609(16) 1 calc PR A 2
H18E H 0.1326 0.3220 0.1151 0.350 Uiso 0.609(16) 1 calc PR A 2
H18F H 0.1121 0.2059 0.0723 0.350 Uiso 0.609(16) 1 calc PR A 2
C19' C 0.0420(5) 0.2464(18) 0.1670(8) 0.289(18) Uani 0.609(16) 1 d PD A 2
H19D H 0.0395 0.2551 0.2226 0.433 Uiso 0.609(16) 1 calc PR A 2
H19E H 0.0127 0.1882 0.1309 0.433 Uiso 0.609(16) 1 calc PR A 2
H19F H 0.0277 0.3119 0.1314 0.433 Uiso 0.609(16) 1 calc PR A 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'
N N 0.0061 0.0033 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 Ti1 O2 100.79(10) . .
O3 Ti1 O1 95.65(10) . .
O2 Ti1 O1 107.76(9) . .
O3 Ti1 O1 166.93(9) . 7_556
O2 Ti1 O1 88.09(8) . 7_556
O1 Ti1 O1 72.34(9) . 7_556
O3 Ti1 N1 89.90(10) . .
O2 Ti1 N1 165.68(10) . .
O1 Ti1 N1 80.32(8) . .
O1 Ti1 N1 83.10(8) 7_556 .
O3 Ti1 S1 99.46(8) . .
O2 Ti1 S1 90.45(8) . .
O1 Ti1 S1 153.70(6) . .
O1 Ti1 S1 89.95(6) 7_556 .
N1 Ti1 S1 78.31(7) . .
O3 Ti1 Ti1 133.34(8) . 7_556
O2 Ti1 Ti1 99.18(7) . 7_556
O1 Ti1 Ti1 37.89(6) . 7_556
O1 Ti1 Ti1 34.45(5) 7_556 7_556
N1 Ti1 Ti1 79.79(6) . 7_556
S1 Ti1 Ti1 122.12(4) . 7_556
C9 S1 Ti1 101.62(11) . .
C1 O1 Ti1 119.73(17) . .
C1 O1 Ti1 121.42(16) . 7_556
Ti1 O1 Ti1 107.66(9) . 7_556
C14 O2 Ti1 141.8(2) . .
C17 O3 Ti1 165.7(5) . .
C7 N1 C8 120.2(3) . .
C7 N1 Ti1 119.7(2) . .
C8 N1 Ti1 119.48(18) . .
O1 C1 C2 119.6(3) . .
O1 C1 C6 120.1(3) . .
C2 C1 C6 120.3(3) . .
C1 C2 C3 120.4(3) . .
C4 C3 C2 120.3(3) . .
C5 C4 C3 120.0(3) . .
C4 C5 C6 120.6(3) . .
C1 C6 C5 118.4(3) . .
C1 C6 C7 123.6(3) . .
C5 C6 C7 117.9(3) . .
N1 C7 C6 125.3(3) . .
C13 C8 C9 119.8(3) . .
C13 C8 N1 123.7(3) . .
C9 C8 N1 116.5(3) . .
C10 C9 C8 118.6(3) . .
C10 C9 S1 120.3(2) . .
C8 C9 S1 121.1(2) . .
C11 C10 C9 121.2(3) . .
C10 C11 C12 119.8(3) . .
C11 C12 C13 120.2(3) . .
C12 C13 C8 120.5(3) . .
O2 C14 C16 111.0(4) . .
O2 C14 C15 110.1(3) . .
C16 C14 C15 116.3(4) . .
O3 C17 C19 128.6(8) . .
O3 C17 C18 117.2(6) . .
C19 C17 C18 110.9(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O3 1.761(2) .
Ti1 O2 1.788(2) .
Ti1 O1 2.0103(19) .
Ti1 O1 2.183(2) 7_556
Ti1 N1 2.254(2) .
Ti1 S1 2.4240(11) .
Ti1 Ti1 3.3864(14) 7_556
S1 C9 1.751(3) .
O1 C1 1.368(3) .
O1 Ti1 2.183(2) 7_556
O2 C14 1.415(4) .
O3 C17 1.362(6) .
N1 C7 1.287(3) .
N1 C8 1.426(4) .
C1 C2 1.373(4) .
C1 C6 1.397(4) .
C2 C3 1.387(4) .
C3 C4 1.378(5) .
C4 C5 1.372(5) .
C5 C6 1.411(4) .
C6 C7 1.450(4) .
C8 C13 1.386(4) .
C8 C9 1.406(4) .
C9 C10 1.392(4) .
C10 C11 1.378(5) .
C11 C12 1.380(5) .
C12 C13 1.383(5) .
C14 C16 1.451(6) .
C14 C15 1.476(6) .
C17 C19 1.402(8) .
C17 C18 1.430(7) .
