#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:49:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318581.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_4318581
loop_
_publ_author_name
'A. Otero'
'J. Fernández-Baeza'
'A. Antiñolo'
'F. Carrillo-Hermosilla'
'J. Tejeda'
'A. Lara-Sánchez'
'L. Sánchez-Barba'
'M. Fernández-López'
'A. M. Rodríguez'
'I. López-Solera'
_publ_section_title
;
 Preparation of New Monoanionic "Scorpionate" Ligands: Synthesis and
 Structural Characterization of Titanium(IV) Complexes Bearing This Class
 of Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5193
_journal_page_last               5202
_journal_paper_doi               10.1021/ic020319f
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C17 H25 Cl5 N4 O S2 Ti'
_chemical_formula_weight         590.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1720(10)
_cell_length_b                   15.6450(10)
_cell_length_c                   14.3320(10)
_cell_measurement_temperature    200(2)
_cell_volume                     2519.3(4)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       'ω/2θ 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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4628
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.054
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.786
_refine_ls_shift/su_mean         0.058
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0389P)²+5.6245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1344
_reflns_number_gt                2588
_reflns_number_total             4435
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020319f_1.cif
_cod_data_source_block           11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2519.3(3)
_cod_database_code               4318581
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.34021(9) 0.18306(6) 0.66854(7) 0.0356(3) Uani 1 1 d . B .
Cl1 Cl 0.31191(14) 0.32382(10) 0.62141(11) 0.0539(4) Uani 1 1 d . . .
Cl2 Cl 0.54170(12) 0.18670(9) 0.76072(9) 0.0438(4) Uani 1 1 d . . .
Cl3 Cl -0.165(4) 0.2039(15) 0.723(3) 0.26(4) Uani 0.20(3) 1 d P A 1
Cl3A Cl -0.1708(3) 0.2194(5) 0.7100(4) 0.116(2) Uani 0.80(3) 1 d P A 2
S1 S 0.12991(13) 0.15783(10) 0.54792(11) 0.0448(4) Uani 1 1 d . . .
S2 S 0.01035(14) 0.04103(11) 0.37621(11) 0.0548(4) Uani 1 1 d . . .
O1 O 0.2884(3) 0.1880(3) 0.7661(3) 0.0525(11) Uani 1 1 d . . .
N1 N 0.3436(4) 0.0435(3) 0.6778(3) 0.0367(10) Uani 1 1 d . . .
N2 N 0.2921(4) -0.0084(3) 0.5949(3) 0.0330(10) Uani 1 1 d . B .
N3 N 0.3320(4) 0.0797(3) 0.4751(3) 0.0337(10) Uani 1 1 d . B .
N4 N 0.3793(4) 0.1503(3) 0.5325(3) 0.0335(10) Uani 1 1 d . . .
C1 C 0.2449(5) 0.0278(3) 0.4943(3) 0.0345(12) Uani 1 1 d . . .
H1 H 0.2270 -0.0204 0.4470 0.041 Uiso 1 1 calc R B .
C2 C 0.1278(5) 0.0754(3) 0.4713(4) 0.0356(13) Uani 1 1 d . B .
C3 C 0.2870(5) -0.0899(3) 0.6219(4) 0.0373(13) Uani 1 1 d . . .
C4 C 0.3400(5) -0.0923(4) 0.7250(4) 0.0420(14) Uani 1 1 d . B .
H4 H 0.3507 -0.1405 0.7656 0.050 Uiso 1 1 calc R . .
C5 C 0.3744(5) -0.0107(4) 0.7575(4) 0.0419(14) Uani 1 1 d . B .
C6 C 0.2331(5) -0.1589(3) 0.5472(4) 0.0490(15) Uani 1 1 d . B .
H6A H 0.1488 -0.1498 0.5149 0.059 Uiso 1 1 calc R . .
H6B H 0.2479 -0.2132 0.5810 0.059 Uiso 1 1 calc R . .
H6C H 0.2676 -0.1584 0.4972 0.059 Uiso 1 1 calc R . .
C7 C 0.4394(6) 0.0184(4) 0.8636(4) 0.0630(19) Uani 1 1 d . . .
H7A H 0.5223 0.0047 0.8847 0.076 Uiso 1 1 calc R B .
H7B H 0.4074 -0.0098 0.9071 0.076 Uiso 1 1 calc R . .
H7C H 0.4304 0.0791 0.8675 0.076 Uiso 1 1 calc R . .
C8 C 0.3698(5) 0.0716(3) 0.3982(4) 0.0378(13) Uani 1 1 d . . .
C9 C 0.4436(5) 0.1386(3) 0.4062(4) 0.0404(13) Uani 1 1 d . B .
H9 H 0.4835 0.1503 0.3638 0.048 Uiso 1 1 calc R . .
C10 C 0.4487(4) 0.1866(3) 0.4897(4) 0.0366(12) Uani 1 1 d . B .
C11 C 0.3311(6) 0.0008(4) 0.3231(4) 0.0572(17) Uani 1 1 d . B .
H11A H 0.3548 -0.0529 0.3573 0.069 Uiso 1 1 calc R . .
H11B H 0.3674 0.0076 0.2748 0.069 Uiso 1 1 calc R . .
H11C H 0.2461 0.0021 0.2888 0.069 Uiso 1 1 calc R . .
C12 C 0.5188(5) 0.2654(3) 0.5283(4) 0.0461(15) Uani 1 1 d . . .
H12A H 0.4690 0.3081 0.5401 0.055 Uiso 1 1 calc R B .
H12B H 0.5483 0.2862 0.4793 0.055 Uiso 1 1 calc R . .
H12C H 0.5845 0.2531 0.5904 0.055 Uiso 1 1 calc R . .
C13 C 0.2169(14) 0.1486(19) 0.8135(10) 0.060(5) Uani 0.59(4) 1 d P B 1
H13A H 0.2584 0.1459 0.8863 0.072 Uiso 0.59(4) 1 calc PR B 1
H13B H 0.1919 0.0916 0.7872 0.072 Uiso 0.59(4) 1 calc PR B 1
C13A C 0.2085(19) 0.210(3) 0.8184(14) 0.061(10) Uani 0.41(4) 1 d P B 2
H13C H 0.2513 0.1941 0.8885 0.073 Uiso 0.41(4) 1 calc PR B 2
H13D H 0.2042 0.2721 0.8174 0.073 Uiso 0.41(4) 1 calc PR B 2
C14 C 0.103(8) 0.216(3) 0.780(7) 0.08(2) Uani 0.24(8) 1 d P B 1
H14A H 0.0558 0.2160 0.7080 0.098 Uiso 0.24(8) 1 calc PR B 1
H14B H 0.1262 0.2739 0.8038 0.098 Uiso 0.24(8) 1 calc PR B 1
C14A C 0.116(2) 0.188(4) 0.7987(18) 0.165(14) Uani 0.76(8) 1 d P B 2
H14C H 0.1134 0.1371 0.7589 0.198 Uiso 0.76(8) 1 calc PR B 2
H14D H 0.0705 0.2302 0.7499 0.198 Uiso 0.76(8) 1 calc PR B 2
C15 C 0.0341(8) 0.1649(8) 0.8470(7) 0.117(4) Uani 1 1 d . . .
H15A H 0.0087 0.1081 0.8200 0.141 Uiso 1 1 calc R B 1
H15B H 0.0865 0.1600 0.9176 0.141 Uiso 1 1 calc R B 1
C16 C -0.0649(14) 0.2176(11) 0.8351(9) 0.069(6) Uani 0.62(3) 1 d P A 1
H16A H -0.0404 0.2770 0.8446 0.082 Uiso 0.62(3) 1 calc PR A 1
H16B H -0.0972 0.2028 0.8852 0.082 Uiso 0.62(3) 1 calc PR A 1
C16A C -0.101(3) 0.153(5) 0.802(4) 0.23(3) Uani 0.38(3) 1 d P A 2
H16C H -0.1306 0.1604 0.8554 0.276 Uiso 0.38(3) 1 calc PR A 2
H16D H -0.1187 0.0950 0.7771 0.276 Uiso 0.38(3) 1 calc PR A 2
C100 C -0.1185(13) 0.0812(11) 0.1031(9) 0.181(6) Uani 1 1 d . . .
H10A H -0.1161 0.0223 0.1252 0.217 Uiso 1 1 calc R C 1
H10B H -0.1334 0.1168 0.1523 0.217 Uiso 1 1 calc R C 1
Cl4 Cl 0.0211(3) 0.1072(3) 0.1042(3) 0.117(2) Uani 0.756(13) 1 d P D 1
Cl4A Cl -0.024(8) 0.111(6) 0.054(9) 1.17(18) Uani 0.244(13) 1 d P D 2
Cl5 Cl -0.2357(9) 0.0919(6) -0.0101(9) 0.086(7) Uani 0.41(5) 1 d P D 1
Cl5A Cl -0.216(2) 0.065(3) 0.0002(16) 0.248(7) Uani 0.59(5) 1 d P D 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 N1 89.99(18) . . ?
O1 Ti1 N4 166.74(18) . . ?
N1 Ti1 N4 79.56(16) . . ?
O1 Ti1 Cl1 97.72(15) . . ?
N1 Ti1 Cl1 167.18(12) . . ?
N4 Ti1 Cl1 91.23(12) . . ?
O1 Ti1 Cl2 99.99(13) . . ?
N1 Ti1 Cl2 89.93(13) . . ?
N4 Ti1 Cl2 88.23(11) . . ?
Cl1 Ti1 Cl2 98.74(7) . . ?
O1 Ti1 S1 88.36(13) . . ?
N1 Ti1 S1 82.83(12) . . ?
N4 Ti1 S1 82.30(11) . . ?
Cl1 Ti1 S1 87.15(6) . . ?
Cl2 Ti1 S1 168.97(6) . . ?
C2 S1 Ti1 108.96(19) . . ?
C13 O1 C13A 39.0(10) . . ?
C13 O1 Ti1 146.6(10) . . ?
C13A O1 Ti1 158.2(11) . . ?
C5 N1 N2 104.2(4) . . ?
C5 N1 Ti1 131.9(4) . . ?
N2 N1 Ti1 123.0(3) . . ?
C3 N2 N1 111.6(4) . . ?
C3 N2 C1 128.0(4) . . ?
N1 N2 C1 120.3(4) . . ?
C8 N3 N4 111.7(4) . . ?
C8 N3 C1 127.4(4) . . ?
N4 N3 C1 120.7(4) . . ?
C10 N4 N3 105.1(4) . . ?
C10 N4 Ti1 133.0(3) . . ?
N3 N4 Ti1 121.9(3) . . ?
N3 C1 N2 111.8(4) . . ?
N3 C1 C2 112.2(4) . . ?
N2 C1 C2 112.6(4) . . ?
C1 C2 S2 117.5(4) . . ?
C1 C2 S1 116.9(4) . . ?
S2 C2 S1 125.6(3) . . ?
N2 C3 C4 106.5(5) . . ?
N2 C3 C6 122.7(5) . . ?
C4 C3 C6 130.8(5) . . ?
C3 C4 C5 107.3(5) . . ?
N1 C5 C4 110.3(4) . . ?
N1 C5 C7 122.4(5) . . ?
C4 C5 C7 127.2(5) . . ?
C9 C8 N3 106.3(5) . . ?
C9 C8 C11 130.6(5) . . ?
N3 C8 C11 123.1(5) . . ?
C8 C9 C10 107.4(5) . . ?
N4 C10 C9 109.6(5) . . ?
N4 C10 C12 123.6(5) . . ?
C9 C10 C12 126.8(5) . . ?
O1 C13 C14 101(3) . . ?
C14A C13A O1 127(3) . . ?
C13 C14 C15 94(4) . . ?
C13A C14A C15 140(2) . . ?
C14A C15 C16 120(2) . . ?
C14A C15 C16A 131(2) . . ?
C16 C15 C16A 45(3) . . ?
C14A C15 C14 17(3) . . ?
C16 C15 C14 104(3) . . ?
C16A C15 C14 120(4) . . ?
C15 C16 Cl3 108.9(17) . . ?
C15 C16A Cl3A 114(4) . . ?
Cl5A C100 Cl4A 93(4) . . ?
Cl5A C100 Cl5 15.4(19) . . ?
Cl4A C100 Cl5 92(4) . . ?
Cl5A C100 Cl4 116.5(10) . . ?
Cl4A C100 Cl4 25(4) . . ?
Cl5 C100 Cl4 116.2(8) . . ?
C100 Cl4A Cl5A 42(2) . . ?
C100 Cl5A Cl4A 46(3) . . ?
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
Ti1 O1 1.742(4) . ?
Ti1 N1 2.188(4) . ?
Ti1 N4 2.237(4) . ?
Ti1 Cl1 2.2904(18) . ?
Ti1 Cl2 2.2960(17) . ?
Ti1 S1 2.5086(17) . ?
Cl3 C16 1.61(4) . ?
Cl3A C16A 1.64(6) . ?
S1 C2 1.687(5) . ?
S2 C2 1.641(5) . ?
O1 C13 1.433(18) . ?
O1 C13A 1.48(3) . ?
N1 C5 1.354(6) . ?
N1 N2 1.375(5) . ?
N2 C3 1.340(6) . ?
N2 C1 1.447(6) . ?
N3 C8 1.353(6) . ?
N3 N4 1.365(5) . ?
N3 C1 1.443(6) . ?
N4 C10 1.345(6) . ?
C1 C2 1.528(7) . ?
C3 C4 1.367(7) . ?
C3 C6 1.484(7) . ?
C4 C5 1.369(8) . ?
C5 C7 1.490(7) . ?
C8 C9 1.356(7) . ?
C8 C11 1.489(7) . ?
C9 C10 1.394(7) . ?
C10 C12 1.480(7) . ?
C13 C14 1.66(9) . ?
C13A C14A 1.11(4) . ?
C14 C15 1.69(7) . ?
C14A C15 1.46(3) . ?
C15 C16 1.416(15) . ?
C15 C16A 1.53(4) . ?
C100 Cl5A 1.52(2) . ?
C100 Cl4A 1.63(8) . ?
C100 Cl5 1.707(17) . ?
C100 Cl4 1.741(15) . ?
Cl4A Cl5A 2.28(8) . ?
