#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:49:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318584.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_4318584
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            'C16 H23 Cl3 N4 O3 Ti'
_chemical_formula_weight         473.63
_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                 100.470(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9870(10)
_cell_length_b                   16.2090(10)
_cell_length_c                   16.9960(10)
_cell_measurement_temperature    293(2)
_cell_volume                     2163.7(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1131
_diffrn_reflns_av_sigmaI/netI    0.2881
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5376
_diffrn_reflns_theta_full        28.03
_diffrn_reflns_theta_max         28.03
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.789
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.2943
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.184
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0807P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.2225
_reflns_number_gt                1761
_reflns_number_total             5208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020319f_4.cif
_cod_data_source_block           10
_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_database_code               4318584
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 0.33617(18) 0.29983(7) 0.42133(8) 0.0462(4) Uani 1 1 d . . .
Cl1 Cl 0.4547(3) 0.40991(11) 0.36647(12) 0.0630(6) Uani 1 1 d . . .
Cl2 Cl 0.2682(3) 0.37068(12) 0.52807(12) 0.0653(6) Uani 1 1 d . . .
Cl3 Cl -0.136(4) 0.5557(19) 0.207(3) 0.151(9) Uani 0.65(8) 1 d P A 1
Cl3A Cl -0.094(3) 0.5773(19) 0.254(5) 0.137(12) Uani 0.35(8) 1 d P A 2
O1 O 0.2900(6) 0.1916(3) 0.4676(3) 0.0511(13) Uani 1 1 d . . .
O2 O 0.3439(7) 0.0649(3) 0.5107(4) 0.0734(18) Uani 1 1 d . . .
O3 O 0.1372(7) 0.3023(3) 0.3606(3) 0.0606(14) Uani 1 1 d . . .
N1 N 0.5984(7) 0.2731(3) 0.4947(3) 0.0421(15) Uani 1 1 d . . .
N2 N 0.6601(7) 0.1933(3) 0.4964(3) 0.0419(14) Uani 1 1 d . . .
N3 N 0.4409(7) 0.2195(3) 0.3375(3) 0.0438(15) Uani 1 1 d . . .
N4 N 0.5292(7) 0.1492(3) 0.3664(3) 0.0430(14) Uani 1 1 d . . .
C1 C 0.5537(8) 0.1308(4) 0.4508(4) 0.0409(17) Uani 1 1 d . . .
H1 H 0.6103 0.0771 0.4604 0.049 Uiso 1 1 calc R . .
C2 C 0.3814(9) 0.1270(4) 0.4797(4) 0.0458(19) Uani 1 1 d . . .
C3 C 0.7284(10) 0.3167(4) 0.5350(4) 0.050(2) Uani 1 1 d . . .
C4 C 0.8660(11) 0.2656(5) 0.5622(5) 0.062(2) Uani 1 1 d . . .
H4 H 0.9691 0.2818 0.5930 0.074 Uiso 1 1 calc R . .
C5 C 0.8242(9) 0.1879(4) 0.5359(4) 0.0482(19) Uani 1 1 d . . .
C6 C 0.7190(10) 0.4083(4) 0.5487(5) 0.062(2) Uani 1 1 d . . .
H6A H 0.7677 0.4371 0.5089 0.074 Uiso 1 1 calc R . .
H6B H 0.7810 0.4217 0.6009 0.074 Uiso 1 1 calc R . .
H6C H 0.6021 0.4245 0.5448 0.074 Uiso 1 1 calc R . .
C7 C 0.9241(10) 0.1105(5) 0.5420(5) 0.072(3) Uani 1 1 d . . .
H7A H 0.8628 0.0678 0.5637 0.087 Uiso 1 1 calc R . .
H7B H 1.0319 0.1191 0.5765 0.087 Uiso 1 1 calc R . .
H7C H 0.9423 0.0946 0.4898 0.087 Uiso 1 1 calc R . .
C8 C 0.4438(10) 0.2195(4) 0.2592(4) 0.052(2) Uani 1 1 d . . .
C9 C 0.5321(10) 0.1528(5) 0.2383(5) 0.063(2) Uani 1 1 d . . .
H9 H 0.5508 0.1400 0.1873 0.076 Uiso 1 1 calc R . .
C10 C 0.5876(9) 0.1086(4) 0.3070(5) 0.0493(19) Uani 1 1 d . . .
C11 C 0.3529(12) 0.2849(5) 0.2041(5) 0.077(3) Uani 1 1 d . . .
H11A H 0.2345 0.2855 0.2079 0.092 Uiso 1 1 calc R . .
H11B H 0.3644 0.2729 0.1500 0.092 Uiso 1 1 calc R . .
H11C H 0.4022 0.3379 0.2193 0.092 Uiso 1 1 calc R . .
C12 C 0.6910(11) 0.0297(5) 0.3220(5) 0.077(3) Uani 1 1 d . . .
H12A H 0.7975 0.0412 0.3565 0.092 Uiso 1 1 calc R . .
H12B H 0.7120 0.0083 0.2720 0.092 Uiso 1 1 calc R . .
H12C H 0.6289 -0.0103 0.3469 0.092 Uiso 1 1 calc R . .
C13 C -0.0366(15) 0.2852(7) 0.3356(8) 0.115(4) Uani 1 1 d . . .
H13A H -0.0841 0.2662 0.3810 0.138 Uiso 1 1 calc R . .
H13B H -0.0494 0.2411 0.2962 0.138 Uiso 1 1 calc R . .
C14 C -0.1293(16) 0.3562(9) 0.3013(13) 0.207(10) Uani 1 1 d . . .
H14A H -0.1506 0.3462 0.2441 0.248 Uiso 1 1 calc R . .
H14B H -0.2392 0.3520 0.3176 0.248 Uiso 1 1 calc R . .
C15 C -0.092(2) 0.4311(11) 0.3085(15) 0.244(13) Uani 1 1 d . A .
H15A H 0.0036 0.4360 0.2805 0.293 Uiso 1 1 calc R . .
H15B H -0.0422 0.4364 0.3648 0.293 Uiso 1 1 calc R . .
C16 C -0.1754(19) 0.5032(10) 0.2917(9) 0.174(6) Uani 1 1 d . . .
H16A H -0.1459 0.5393 0.3377 0.209 Uiso 1 1 calc R A 1
H16B H -0.2966 0.4923 0.2848 0.209 Uiso 1 1 calc R A 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'
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'
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
O3 Ti1 O1 92.3(2) . . ?
O3 Ti1 N3 92.5(2) . . ?
O1 Ti1 N3 81.6(2) . . ?
O3 Ti1 N1 170.0(2) . . ?
O1 Ti1 N1 80.41(19) . . ?
N3 Ti1 N1 79.8(2) . . ?
O3 Ti1 Cl2 97.84(18) . . ?
O1 Ti1 Cl2 92.35(15) . . ?
N3 Ti1 Cl2 168.25(17) . . ?
N1 Ti1 Cl2 89.34(16) . . ?
O3 Ti1 Cl1 98.16(19) . . ?
O1 Ti1 Cl1 165.52(15) . . ?
N3 Ti1 Cl1 87.93(16) . . ?
N1 Ti1 Cl1 87.94(15) . . ?
Cl2 Ti1 Cl1 96.11(8) . . ?
C2 O1 Ti1 130.5(5) . . ?
C13 O3 Ti1 157.9(6) . . ?
C3 N1 N2 104.0(5) . . ?
C3 N1 Ti1 137.1(5) . . ?
N2 N1 Ti1 118.6(4) . . ?
C5 N2 N1 112.2(5) . . ?
C5 N2 C1 129.4(6) . . ?
N1 N2 C1 118.0(5) . . ?
C8 N3 N4 104.7(5) . . ?
C8 N3 Ti1 136.2(5) . . ?
N4 N3 Ti1 119.1(4) . . ?
C10 N4 N3 111.0(6) . . ?
C10 N4 C1 129.5(6) . . ?
N3 N4 C1 119.4(5) . . ?
N4 C1 N2 110.3(5) . . ?
N4 C1 C2 110.9(6) . . ?
N2 C1 C2 109.1(5) . . ?
O2 C2 O1 125.5(7) . . ?
O2 C2 C1 118.7(6) . . ?
O1 C2 C1 115.8(6) . . ?
N1 C3 C4 110.5(6) . . ?
N1 C3 C6 122.9(7) . . ?
C4 C3 C6 126.6(7) . . ?
C5 C4 C3 108.2(7) . . ?
C4 C5 N2 105.0(6) . . ?
C4 C5 C7 131.7(7) . . ?
N2 C5 C7 123.2(7) . . ?
N3 C8 C9 111.2(7) . . ?
N3 C8 C11 121.7(7) . . ?
C9 C8 C11 127.1(7) . . ?
C8 C9 C10 107.0(6) . . ?
N4 C10 C9 106.1(6) . . ?
N4 C10 C12 122.3(7) . . ?
C9 C10 C12 131.6(7) . . ?
O3 C13 C14 112.0(9) . . ?
C15 C14 C13 130.0(15) . . ?
C14 C15 C16 135.8(19) . . ?
C15 C16 Cl3A 121.7(16) . . ?
C15 C16 Cl3 116.0(15) . . ?
Cl3A C16 Cl3 30.3(14) . . ?
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 O3 1.731(5) . ?
Ti1 O1 1.984(4) . ?
Ti1 N3 2.204(6) . ?
Ti1 N1 2.276(6) . ?
Ti1 Cl2 2.294(2) . ?
Ti1 Cl1 2.296(2) . ?
Cl3 C16 1.75(2) . ?
Cl3A C16 1.56(3) . ?
O1 C2 1.272(7) . ?
O2 C2 1.200(8) . ?
O3 C13 1.403(11) . ?
N1 C3 1.337(8) . ?
N1 N2 1.382(7) . ?
N2 C5 1.362(8) . ?
N2 C1 1.453(8) . ?
N3 C8 1.335(8) . ?
N3 N4 1.382(7) . ?
N4 C10 1.356(8) . ?
N4 C1 1.444(8) . ?
C1 C2 1.544(9) . ?
C3 C4 1.385(10) . ?
C3 C6 1.508(10) . ?
C4 C5 1.358(10) . ?
C5 C7 1.479(10) . ?
C8 C9 1.372(10) . ?
C8 C11 1.511(10) . ?
C9 C10 1.373(10) . ?
C10 C12 1.518(10) . ?
C13 C14 1.434(16) . ?
C14 C15 1.252(18) . ?
C15 C16 1.351(17) . ?
