#------------------------------------------------------------------------------
#$Date: 2016-03-26 12:59:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180218 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/04/7110400.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7110400
loop_
_publ_author_name
'Corden, Jonathan P.'
'Errington, William'
'Moore, Peter'
'Wallbridge, Malcolm G. H.'
_publ_section_title
;
 Stereochemical control of cis- and trans-TiCl2 groups in six-coordinate
 complexes [(L)TiCl2] (L2− = N2O2-donor Schiff base) and reactions
 with trimethylaluminium to form cationic aluminium species
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              323
_journal_paper_doi               10.1039/a808372j
_journal_year                    1999
_chemical_formula_sum            'C25 H29 Cl5 N2 O2 Ti'
_chemical_formula_weight         614.65
_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                 111.32(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.446(3)
_cell_length_b                   9.796(2)
_cell_length_c                   18.160(4)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.29
_cell_volume                     2725.4(11)
_computing_cell_refinement       'MADNES (Plugrath & Messerschmidt, 1992)'
_computing_data_collection       'MADNES (Plugrath & Messerschmidt, 1992)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type
;
Delft Instruments FAST TV area-detector diffractometer
;
_diffrn_measurement_method       '/w scans'
_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  0.1880
_diffrn_reflns_av_sigmaI/netI    0.4004
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12060
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.597
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4283
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.596
_refine_ls_R_factor_all          0.1820
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                1206
_reflns_number_total             4283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            808372jsup1.cif
_cod_data_source_block           tiet
_cod_original_cell_volume        2725.3(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110400
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
Ti1 Ti 0.80459(10) 0.02738(13) 0.83364(9) 0.0251(4) Uani 1 1 d .
Cl1 Cl 0.78527(15) -0.18641(18) 0.88016(13) 0.0383(6) Uani 1 1 d .
Cl2 Cl 0.67224(14) 0.09302(19) 0.85014(13) 0.0320(6) Uani 1 1 d .
N1 N 0.7966(4) 0.2357(5) 0.7884(3) 0.0172(15) Uani 1 1 d U
N2 N 0.7157(4) 0.0082(6) 0.7094(3) 0.0207(16) Uani 1 1 d U
O1 O 0.8806(3) 0.1040(5) 0.9216(3) 0.0251(13) Uani 1 1 d U
O2 O 0.8813(3) -0.0430(4) 0.7918(3) 0.0271(14) Uani 1 1 d .
C1 C 0.8960(5) 0.2279(7) 0.9581(4) 0.0219(19) Uani 1 1 d DU
C2 C 0.9510(4) 0.2346(7) 1.0367(4) 0.028(2) Uani 1 1 d DU
H2A H 0.9797 0.1540 1.0624 0.033 Uiso 1 1 calc R
C3 C 0.9649(5) 0.3537(7) 1.0783(5) 0.033(2) Uani 1 1 d DU
H3A H 1.0023 0.3572 1.1323 0.040 Uiso 1 1 calc R
C4 C 0.9217(5) 0.4721(8) 1.0380(5) 0.035(2) Uani 1 1 d DU
H4A H 0.9292 0.5558 1.0662 0.042 Uiso 1 1 calc R
C5 C 0.8686(5) 0.4695(8) 0.9583(5) 0.029(2) Uani 1 1 d DU
H5A H 0.8413 0.5508 0.9326 0.034 Uiso 1 1 calc R
C6 C 0.8557(5) 0.3466(7) 0.9161(5) 0.0225(19) Uani 1 1 d DU
C7 C 0.8013(5) 0.3442(6) 0.8311(4) 0.0158(18) Uiso 1 1 d U
C8 C 0.7502(5) 0.4724(7) 0.7994(4) 0.030(2) Uani 1 1 d U
H8A H 0.7251 0.4686 0.7410 0.036 Uiso 1 1 calc R
H8B H 0.7894 0.5525 0.8151 0.036 Uiso 1 1 calc R
C9 C 0.6761(5) 0.4876(7) 0.8321(5) 0.048(3) Uani 1 1 d U
H9A H 0.6394 0.5658 0.8068 0.072 Uiso 1 1 calc R
H9B H 0.7013 0.5022 0.8893 0.072 Uiso 1 1 calc R
H9C H 0.6405 0.4044 0.8208 0.072 Uiso 1 1 calc R
C10 C 0.7483(5) 0.2467(7) 0.7001(4) 0.0214(18) Uani 1 1 d U
H10 H 0.6882 0.2820 0.6906 0.026 Uiso 1 1 calc R
C11 C 0.7921(5) 0.3425(6) 0.6579(4) 0.028(2) Uani 1 1 d U
H11A H 0.8038 0.4324 0.6845 0.034 Uiso 1 1 calc R
H11B H 0.8485 0.3031 0.6602 0.034 Uiso 1 1 calc R
C12 C 0.7318(5) 0.3596(7) 0.5721(4) 0.028(2) Uani 1 1 d U
H12A H 0.7606 0.4178 0.5443 0.033 Uiso 1 1 calc R
H12B H 0.6776 0.4063 0.5702 0.033 Uiso 1 1 calc R
C13 C 0.7085(5) 0.2224(7) 0.5301(4) 0.032(2) Uani 1 1 d U
H13A H 0.6613 0.2360 0.4781 0.038 Uiso 1 1 calc R
H13B H 0.7601 0.1864 0.5206 0.038 Uiso 1 1 calc R
C14 C 0.6790(5) 0.1181(7) 0.5770(4) 0.028(2) Uani 1 1 d U
H14A H 0.6202 0.1432 0.5756 0.034 Uiso 1 1 calc R
H14B H 0.6748 0.0274 0.5518 0.034 Uiso 1 1 calc R
C15 C 0.7399(5) 0.1090(7) 0.6610(4) 0.0216(18) Uani 1 1 d U
H15 H 0.7987 0.0832 0.6609 0.026 Uiso 1 1 calc R
C16 C 0.7181(5) -0.1333(7) 0.6806(5) 0.029(2) Uani 1 1 d U
C17 C 0.6457(5) -0.2067(8) 0.6583(4) 0.033(2) Uani 1 1 d U
H17A H 0.6593 -0.2857 0.6948 0.040 Uiso 1 1 calc R
H17B H 0.6396 -0.2441 0.6059 0.040 Uiso 1 1 calc R
C18 C 0.5560(5) -0.1633(7) 0.6503(5) 0.046(3) Uani 1 1 d U
H18A H 0.5213 -0.2439 0.6520 0.069 Uiso 1 1 calc R
H18B H 0.5283 -0.1158 0.5998 0.069 Uiso 1 1 calc R
H18C H 0.5593 -0.1018 0.6939 0.069 Uiso 1 1 calc R
C19 C 0.8015(5) -0.1848(8) 0.6797(4) 0.024(2) Uani 1 1 d D
C20 C 0.8059(6) -0.2749(7) 0.6245(5) 0.034(2) Uani 1 1 d D
H20A H 0.7537 -0.3089 0.5858 0.041 Uiso 1 1 calc R
C21 C 0.8884(6) -0.3187(7) 0.6242(5) 0.035(2) Uani 1 1 d D
H21A H 0.8906 -0.3822 0.5855 0.042 Uiso 1 1 calc R
C22 C 0.9642(6) -0.2708(7) 0.6788(5) 0.040(3) Uani 1 1 d D
H22A H 1.0189 -0.3032 0.6794 0.048 Uiso 1 1 calc R
C23 C 0.9607(5) -0.1769(8) 0.7319(5) 0.031(2) Uani 1 1 d D
H23A H 1.0136 -0.1406 0.7683 0.038 Uiso 1 1 calc R
C24 C 0.8813(6) -0.1315(7) 0.7349(5) 0.029(2) Uani 1 1 d D
Cl1S Cl 1.48431(15) -0.2286(2) 0.30268(14) 0.0528(7) Uani 1 1 d .
Cl2S Cl 1.49427(19) -0.4618(3) 0.39964(19) 0.0925(12) Uani 1 1 d .
Cl3S Cl 1.5901(2) -0.2180(3) 0.46531(17) 0.0973(11) Uani 1 1 d .
C1S C 1.5509(5) -0.3228(8) 0.3848(5) 0.044(2) Uani 1 1 d .
H1SA H 1.6018 -0.3577 0.3728 0.053 Uiso 1 1 calc R
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_publ_flag
O1 Ti1 O2 99.5(2) y
O1 Ti1 N1 82.6(2) ?
O2 Ti1 N1 98.8(2) ?
O1 Ti1 N2 159.0(2) ?
O2 Ti1 N2 81.0(2) ?
N1 Ti1 N2 76.6(2) y
O1 Ti1 Cl1 101.34(17) ?
O2 Ti1 Cl1 90.99(16) ?
N1 Ti1 Cl1 168.77(17) ?
N2 Ti1 Cl1 99.67(16) y
O1 Ti1 Cl2 98.44(18) ?
O2 Ti1 Cl2 161.99(18) ?
N1 Ti1 Cl2 82.11(16) ?
N2 Ti1 Cl2 81.70(17) ?
Cl1 Ti1 Cl2 86.89(9) y
C7 N1 C10 117.9(6) ?
C7 N1 Ti1 123.8(5) ?
C10 N1 Ti1 113.6(4) ?
C15 N2 C16 111.6(6) ?
C15 N2 Ti1 109.4(4) ?
C16 N2 Ti1 110.2(4) ?
C1 O1 Ti1 138.8(5) ?
C24 O2 Ti1 138.9(5) ?
O1 C1 C2 118.7(7) ?
O1 C1 C6 120.1(7) ?
C2 C1 C6 121.2(7) ?
C3 C2 C1 121.8(7) ?
C2 C3 C4 117.6(8) ?
C5 C4 C3 121.9(7) ?
C4 C5 C6 119.9(8) ?
C5 C6 C1 117.6(7) ?
C5 C6 C7 120.0(7) ?
C1 C6 C7 122.4(7) ?
N1 C7 C6 121.2(6) ?
N1 C7 C8 123.4(7) ?
C6 C7 C8 115.4(6) ?
C7 C8 C9 110.1(6) ?
C15 C10 N1 111.1(5) ?
C15 C10 C11 106.7(6) ?
N1 C10 C11 114.1(6) ?
C12 C11 C10 109.0(6) ?
C11 C12 C13 111.5(6) ?
C14 C13 C12 112.7(6) ?
C15 C14 C13 112.4(6) ?
N2 C15 C14 115.1(6) ?
N2 C15 C10 108.5(6) ?
C14 C15 C10 109.9(6) ?
C17 C16 C19 123.4(8) ?
C17 C16 N2 118.6(7) ?
C19 C16 N2 118.0(7) ?
C16 C17 C18 128.6(8) ?
C20 C19 C24 118.2(8) ?
C20 C19 C16 122.2(8) ?
C24 C19 C16 119.4(7) ?
C19 C20 C21 120.4(8) ?
C22 C21 C20 121.0(8) ?
C23 C22 C21 119.2(9) ?
C22 C23 C24 121.9(8) ?
O2 C24 C23 119.6(8) ?
O2 C24 C19 121.1(8) ?
C23 C24 C19 119.2(8) ?
Cl3S C1S Cl2S 113.4(5) ?
Cl3S C1S Cl1S 109.6(4) ?
Cl2S C1S Cl1S 110.0(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 O1 1.796(5) y
Ti1 O2 1.827(5) y
Ti1 N1 2.186(5) y
Ti1 N2 2.205(6) y
Ti1 Cl1 2.323(2) y
Ti1 Cl2 2.391(3) y
N1 C7 1.301(7) ?
N1 C10 1.512(8) ?
N2 C15 1.470(8) ?
N2 C16 1.488(8) ?
O1 C1 1.361(8) ?
O2 C24 1.349(8) ?
C1 C2 1.387(9) ?
C1 C6 1.417(9) ?
C2 C3 1.363(9) ?
C3 C4 1.417(9) ?
C4 C5 1.393(10) ?
C5 C6 1.401(9) ?
C6 C7 1.476(9) ?
C7 C8 1.504(8) ?
C8 C9 1.544(10) ?
C10 C15 1.507(9) ?
C10 C11 1.547(9) ?
C11 C12 1.521(9) ?
C12 C13 1.524(8) ?
C13 C14 1.518(9) ?
C14 C15 1.491(9) ?
C16 C17 1.321(9) ?
C16 C19 1.467(10) ?
C17 C18 1.492(10) ?
C19 C20 1.358(9) ?
C19 C24 1.429(10) ?
C20 C21 1.424(10) ?
C21 C22 1.363(10) ?
C22 C23 1.349(10) ?
C23 C24 1.400(10) ?
Cl1S C1S 1.757(8) ?
Cl2S C1S 1.725(8) ?
Cl3S C1S 1.709(8) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O1 Ti1 N1 C7 -35.5(6)
O2 Ti1 N1 C7 -134.0(6)
N2 Ti1 N1 C7 147.5(6)
Cl1 Ti1 N1 C7 75.8(11)
Cl2 Ti1 N1 C7 64.2(6)
O1 Ti1 N1 C10 169.3(5)
O2 Ti1 N1 C10 70.7(5)
N2 Ti1 N1 C10 -7.8(4)
Cl1 Ti1 N1 C10 -79.5(10)
Cl2 Ti1 N1 C10 -91.1(4)
O1 Ti1 N2 C15 23.4(9)
O2 Ti1 N2 C15 -69.8(5)
N1 Ti1 N2 C15 31.5(4)
Cl1 Ti1 N2 C15 -159.3(4)
Cl2 Ti1 N2 C15 115.4(4)
O1 Ti1 N2 C16 146.4(6)
O2 Ti1 N2 C16 53.2(5)
N1 Ti1 N2 C16 154.6(5)
Cl1 Ti1 N2 C16 -36.2(5)
Cl2 Ti1 N2 C16 -121.6(5)
O2 Ti1 O1 C1 125.7(7)
N1 Ti1 O1 C1 28.0(7)
N2 Ti1 O1 C1 36.0(11)
Cl1 Ti1 O1 C1 -141.3(6)
Cl2 Ti1 O1 C1 -52.8(7)
O1 Ti1 O2 C24 166.9(7)
N1 Ti1 O2 C24 -109.2(7)
N2 Ti1 O2 C24 -34.4(7)
Cl1 Ti1 O2 C24 65.2(7)
Cl2 Ti1 O2 C24 -17.7(11)
Ti1 O1 C1 C2 164.4(5)
Ti1 O1 C1 C6 -14.9(11)
O1 C1 C2 C3 -175.8(6)
C6 C1 C2 C3 3.6(10)
C1 C2 C3 C4 -0.6(10)
C2 C3 C4 C5 -1.8(11)
C3 C4 C5 C6 1.1(12)
C4 C5 C6 C1 1.9(11)
C4 C5 C6 C7 -178.4(7)
O1 C1 C6 C5 175.2(6)
C2 C1 C6 C5 -4.2(10)
O1 C1 C6 C7 -4.5(10)
C2 C1 C6 C7 176.1(6)
C10 N1 C7 C6 -172.8(6)
Ti1 N1 C7 C6 32.9(9)
C10 N1 C7 C8 9.6(10)
Ti1 N1 C7 C8 -144.7(6)
C5 C6 C7 N1 171.7(7)
C1 C6 C7 N1 -8.7(11)
C5 C6 C7 C8 -10.6(10)
C1 C6 C7 C8 169.1(6)
N1 C7 C8 C9 107.4(8)
C6 C7 C8 C9 -70.3(8)
C7 N1 C10 C15 -173.3(6)
Ti1 N1 C10 C15 -16.5(7)
C7 N1 C10 C11 66.0(8)
Ti1 N1 C10 C11 -137.2(5)
C15 C10 C11 C12 64.4(7)
N1 C10 C11 C12 -172.5(5)
C10 C11 C12 C13 -56.7(8)
C11 C12 C13 C14 48.6(9)
C12 C13 C14 C15 -49.0(9)
C16 N2 C15 C14 64.3(8)
Ti1 N2 C15 C14 -173.5(5)
C16 N2 C15 C10 -172.2(6)
Ti1 N2 C15 C10 -49.9(6)
C13 C14 C15 N2 -179.2(6)
C13 C14 C15 C10 58.0(8)
N1 C10 C15 N2 43.4(8)
C11 C10 C15 N2 168.4(6)
N1 C10 C15 C14 170.1(6)
C11 C10 C15 C14 -65.0(8)
C15 N2 C16 C17 -120.6(8)
Ti1 N2 C16 C17 117.7(7)
C15 N2 C16 C19 60.3(8)
Ti1 N2 C16 C19 -61.4(8)
C19 C16 C17 C18 -174.6(8)
N2 C16 C17 C18 6.4(13)
C17 C16 C19 C20 33.3(12)
N2 C16 C19 C20 -147.6(7)
C17 C16 C19 C24 -151.4(8)
N2 C16 C19 C24 27.7(10)
C24 C19 C20 C21 2.5(9)
C16 C19 C20 C21 177.9(7)
C19 C20 C21 C22 -0.4(10)
C20 C21 C22 C23 -2.3(11)
C21 C22 C23 C24 2.9(12)
Ti1 O2 C24 C23 -167.8(5)
Ti1 O2 C24 C19 9.3(11)
C22 C23 C24 O2 176.4(7)
C22 C23 C24 C19 -0.7(12)
C20 C19 C24 O2 -179.1(6)
C16 C19 C24 O2 5.3(11)
C20 C19 C24 C23 -2.0(10)
C16 C19 C24 C23 -177.5(7)
