#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179116 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/78/4307895.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_4307895
loop_
_publ_author_name
'Christian Lorber'
'Robert Choukroun'
'Laure Vendier'
_publ_contact_author
;
Christian Lorber
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       lorber@lcc-toulouse.fr
_publ_section_title
;
Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of
Electron-Deficient Imido Complexes of Early Transition Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3192
_journal_page_last               3202
_journal_paper_doi               10.1021/ic062404j
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C110 H210 Cl20 N31 O19 S10 Ti10'
_chemical_formula_sum            'C110 H210 Cl20 N31 O19 S10 Ti10'
_chemical_formula_weight         3779.69
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_cell_angle_beta                 128.269(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   35.005(2)
_cell_length_b                   12.4083(8)
_cell_length_c                   25.2366(17)
_cell_measurement_reflns_used    6000
_cell_measurement_temperature    180
_cell_measurement_theta_max      32.1424
_cell_measurement_theta_min      2.6356
_cell_measurement_wavelength     0.71073
_cell_volume                     8606.1(13)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_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  0.042
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29219
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3918
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.072
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8135
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.07
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0445P)²+67.8212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                5893
_reflns_number_total             8135
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic062404jsi20061215_111655_5.cif
_cod_data_source_block           (4)
_cod_database_code               4307895
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
C1 C 0.1887(2) 0.4764(4) 0.0375(3) 0.0432(10) Uani 1 1 d . . .
C2 C 0.1816(3) 0.4065(5) -0.0087(3) 0.081(3) Uani 1 1 d . . .
H2 H 0.1701 0.4315 -0.0511 0.097 Uiso 1 1 calc R . .
C3 C 0.1914(4) 0.2983(5) 0.0062(4) 0.090(3) Uani 1 1 d . . .
H3 H 0.1864 0.2518 -0.0265 0.108 Uiso 1 1 calc R . .
C4 C 0.2077(2) 0.2578(5) 0.0663(3) 0.0529(11) Uani 1 1 d . . .
C5 C 0.2167(2) 0.3298(5) 0.1130(3) 0.0529(11) Uani 1 1 d . . .
H5 H 0.2304 0.3056 0.1563 0.064 Uiso 1 1 calc R . .
C6 C 0.2061(2) 0.4381(4) 0.0985(3) 0.0432(10) Uani 1 1 d . . .
H6 H 0.2111 0.4847 0.1311 0.052 Uiso 1 1 calc R . .
C7 C 0.2170(3) 0.1395(5) 0.0821(4) 0.0639(19) Uani 1 1 d . . .
H7A H 0.1868 0.1037 0.064 0.096 Uiso 1 1 calc R . .
H7B H 0.2391 0.1296 0.1302 0.096 Uiso 1 1 calc R . .
H7C H 0.2308 0.1096 0.0624 0.096 Uiso 1 1 calc R . .
C8 C 0.3053(2) 0.5351(5) 0.0731(3) 0.0574(17) Uani 1 1 d . . .
H8A H 0.3334 0.4911 0.0904 0.086 Uiso 1 1 calc R . .
H8B H 0.2777 0.506 0.031 0.086 Uiso 1 1 calc R . .
H8C H 0.2988 0.5362 0.1049 0.086 Uiso 1 1 calc R . .
C9 C 0.3575(2) 0.6881(5) 0.1271(3) 0.0566(17) Uani 1 1 d . . .
H9A H 0.3509 0.6921 0.1587 0.085 Uiso 1 1 calc R . .
H9B H 0.3649 0.7588 0.1202 0.085 Uiso 1 1 calc R . .
H9C H 0.3848 0.6413 0.1445 0.085 Uiso 1 1 calc R . .
C10 C 0.2484(2) 0.9106(5) 0.2076(3) 0.0502(15) Uani 1 1 d . . .
H10A H 0.2473 0.9012 0.2444 0.075 Uiso 1 1 calc R . .
H10B H 0.2265 0.9673 0.1786 0.075 Uiso 1 1 calc R . .
H10C H 0.2809 0.9292 0.2249 0.075 Uiso 1 1 calc R . .
C11 C 0.26999(19) 0.7250(5) 0.2104(3) 0.0525(16) Uani 1 1 d . . .
H11A H 0.3015 0.7488 0.2259 0.079 Uiso 1 1 calc R . .
H11B H 0.2611 0.6607 0.184 0.079 Uiso 1 1 calc R . .
H11C H 0.271 0.7101 0.2486 0.079 Uiso 1 1 calc R . .
C12 C 0.0653(2) 0.6200(5) 0.0112(3) 0.0504(15) Uani 1 1 d . . .
H12A H 0.0331 0.6006 -0.0054 0.076 Uiso 1 1 calc R . .
H12B H 0.0878 0.5653 0.0415 0.076 Uiso 1 1 calc R . .
H12C H 0.0661 0.6265 -0.0261 0.076 Uiso 1 1 calc R . .
C13 C 0.04303(19) 0.8076(5) 0.0024(3) 0.0521(16) Uani 1 1 d . . .
H13A H 0.0417 0.8155 -0.0365 0.078 Uiso 1 1 calc R . .
H13B H 0.0524 0.8749 0.0262 0.078 Uiso 1 1 calc R . .
H13C H 0.0116 0.7867 -0.0115 0.078 Uiso 1 1 calc R . .
C14 C 0.11280(17) 1.0568(4) 0.1671(2) 0.0298(11) Uani 1 1 d . . .
C15 C 0.09788(19) 1.1180(4) 0.1971(3) 0.0383(12) Uani 1 1 d . . .
H15 H 0.0952 1.0868 0.2282 0.046 Uiso 1 1 calc R . .
C16 C 0.0870(2) 1.2246(5) 0.1807(3) 0.0480(15) Uani 1 1 d . . .
H16 H 0.0771 1.2653 0.2011 0.058 Uiso 1 1 calc R . .
C17 C 0.0904(2) 1.2734(4) 0.1347(3) 0.0462(15) Uani 1 1 d . . .
C18 C 0.1054(2) 1.2105(5) 0.1058(3) 0.0491(15) Uani 1 1 d . . .
H18 H 0.1085 1.2421 0.0753 0.059 Uiso 1 1 calc R . .
C19 C 0.1158(2) 1.1027(4) 0.1202(3) 0.0398(13) Uani 1 1 d . . .
H19 H 0.1248 1.0616 0.0986 0.048 Uiso 1 1 calc R . .
C20 C 0.0795(3) 1.3909(5) 0.1174(4) 0.079(2) Uani 1 1 d . . .
H20A H 0.1094 1.4303 0.1398 0.118 Uiso 1 1 calc R . .
H20B H 0.0615 1.4175 0.1318 0.118 Uiso 1 1 calc R . .
H20C H 0.0605 1.4 0.0695 0.118 Uiso 1 1 calc R . .
C21 C 0.1552(2) 0.7270(6) 0.3347(3) 0.0578(17) Uani 1 1 d . . .
H21A H 0.1421 0.727 0.3586 0.087 Uiso 1 1 calc R . .
H21B H 0.1629 0.7995 0.331 0.087 Uiso 1 1 calc R . .
H21C H 0.1843 0.684 0.3588 0.087 Uiso 1 1 calc R . .
C22 C 0.1143(3) 0.5651(5) 0.2726(4) 0.078(2) Uani 1 1 d . . .
H22A H 0.1448 0.53 0.2923 0.117 Uiso 1 1 calc R . .
H22B H 0.09 0.5361 0.2284 0.117 Uiso 1 1 calc R . .
H22C H 0.1047 0.5534 0.3005 0.117 Uiso 1 1 calc R . .
N2A N 0.21669(13) 0.6668(3) 0.02652(19) 0.0329(9) Uani 0.5 1 d P . .
O2B O 0.21669(13) 0.6668(3) 0.02652(19) 0.0329(9) Uani 0.5 1 d P . .
N8A N 0.02401(14) 0.6810(3) 0.22993(19) 0.0348(9) Uani 0.5 1 d P . .
O8B O 0.02401(14) 0.6810(3) 0.22993(19) 0.0348(9) Uani 0.5 1 d P . .
N1 N 0.31464(14) 0.6454(4) 0.0625(2) 0.0354(10) Uani 1 1 d . . .
H4 H 0.3249 0.6366 0.0373 0.043 Uiso 1 1 calc R . .
N3 N 0.23388(14) 0.8097(3) 0.1689(2) 0.0333(10) Uani 1 1 d . . .
H5A H 0.2379 0.8242 0.1373 0.04 Uiso 1 1 calc R . .
N4 N 0.07903(14) 0.7242(3) 0.0472(2) 0.0327(10) Uani 1 1 d . . .
H6A H 0.0741 0.7132 0.0782 0.039 Uiso 1 1 calc R . .
N6 N 0.11947(16) 0.6820(4) 0.2673(2) 0.0422(11) Uani 1 1 d . . .
H7 H 0.134 0.6864 0.2474 0.051 Uiso 1 1 calc R . .
N7 N -0.01909(15) 0.8595(4) 0.1330(2) 0.0397(11) Uani 1 1 d D . .
H8 H -0.0224 0.8961 0.1612 0.048 Uiso 1 1 calc R A 1
C28A C -0.0628(3) 0.7868(9) 0.0924(6) 0.0578(19) Uani 0.51 1 d PD B 1
H28A H -0.0916 0.8296 0.0631 0.087 Uiso 0.51 1 calc PR B 1
H28B H -0.0653 0.7456 0.1223 0.087 Uiso 0.51 1 calc PR B 1
H28C H -0.0593 0.7388 0.0657 0.087 Uiso 0.51 1 calc PR B 1
C29A C -0.0227(4) 0.9402(9) 0.0890(6) 0.0578(19) Uani 0.51 1 d PD B 1
H29A H -0.0159 0.908 0.061 0.087 Uiso 0.51 1 calc PR B 1
H29B H 0.0004 0.9966 0.1156 0.087 Uiso 0.51 1 calc PR B 1
H29C H -0.055 0.9698 0.061 0.087 Uiso 0.51 1 calc PR B 1
C28B C -0.0579(4) 0.8215(9) 0.0655(4) 0.0578(19) Uani 0.49 1 d PD B 2
H28D H -0.0859 0.8672 0.0456 0.087 Uiso 0.49 1 calc PR B 2
H28E H -0.0664 0.749 0.0678 0.087 Uiso 0.49 1 calc PR B 2
H28F H -0.0473 0.8233 0.0384 0.087 Uiso 0.49 1 calc PR B 2
C29B C -0.0111(4) 0.9775(7) 0.1270(6) 0.0578(19) Uani 0.49 1 d PD B 2
H29D H 0.0074 0.9834 0.1106 0.087 Uiso 0.49 1 calc PR B 2
H29E H 0.0065 1.0112 0.1704 0.087 Uiso 0.49 1 calc PR B 2
H29F H -0.0419 1.0125 0.096 0.087 Uiso 0.49 1 calc PR B 2
O1 O 0.12964(13) 0.6187(3) -0.05114(18) 0.0488(10) Uani 1 1 d . . .
O2A O 0.16985(13) 0.6558(3) 0.06918(18) 0.0321(8) Uani 0.5 1 d P . .
N2B N 0.16985(13) 0.6558(3) 0.06918(18) 0.0321(8) Uani 0.5 1 d P . .
N5A N 0.14121(14) 0.8791(3) 0.1473(2) 0.0349(9) Uani 0.5 1 d P . .
O5B O 0.14121(14) 0.8791(3) 0.1473(2) 0.0349(9) Uani 0.5 1 d P . .
O3 O 0.17080(13) 0.9220(3) 0.26274(18) 0.0494(10) Uani 1 1 d . . .
O4A O 0.08578(13) 0.8648(3) 0.17654(19) 0.0326(9) Uani 0.5 1 d P . .
N4B N 0.08578(13) 0.8648(3) 0.17654(19) 0.0326(9) Uani 0.5 1 d P . .
S1 S 0.17397(4) 0.61230(10) 0.01665(6) 0.0282(3) Uani 1 1 d . . .
S2 S 0.12997(4) 0.92204(10) 0.19246(6) 0.0284(3) Uani 1 1 d . B .
Cl1 Cl 0.27800(5) 0.87162(12) 0.08836(7) 0.0418(3) Uani 1 1 d . . .
Cl2 Cl 0.17159(5) 0.64466(11) 0.19062(7) 0.0397(3) Uani 1 1 d . . .
Cl3 Cl 0.14168(4) 0.89189(10) 0.02763(6) 0.0341(3) Uani 1 1 d . . .
Cl4 Cl 0.06924(5) 0.90193(11) 0.28148(7) 0.0400(3) Uani 1 1 d . . .
Cl5 Cl 0.02623(5) 0.65540(10) 0.11194(7) 0.0382(3) Uani 1 1 d . . .
Ti1 Ti 0.25 0.75 0 0.0396(4) Uani 1 2 d S . .
Ti2 Ti 0.15626(3) 0.76723(8) 0.10866(5) 0.0372(3) Uani 1 1 d . . .
Ti3 Ti 0.05139(3) 0.77432(8) 0.20006(5) 0.0381(3) Uani 1 1 d . B .
S3 S -0.02131(9) 0.63379(19) 0.21722(12) 0.0278(5) Uani 0.5 1 d P . .
C23 C 0 0.4952(7) 0.25 0.069(3) Uani 1 2 d S . .
C24 C -0.0223(3) 0.4412(8) 0.1905(4) 0.082(3) Uani 1 1 d . . .
H24 H -0.0375 0.4785 0.1501 0.098 Uiso 1 1 calc R . .
C25 C -0.0218(3) 0.3331(7) 0.1915(4) 0.073(2) Uani 1 1 d . C .
H25 H -0.0368 0.2953 0.1513 0.088 Uiso 1 1 calc R . .
C26 C 0 0.2781(7) 0.25 0.072(4) Uani 1 2 d S . .
C27 C -0.0080(7) 0.1574(8) 0.2245(7) 0.067(5) Uani 0.5 1 d P C -1
H27A H 0.0223 0.119 0.2526 0.1 Uiso 0.5 1 calc PR C -1
H27B H -0.0195 0.1567 0.1787 0.1 Uiso 0.5 1 calc PR C -1
H27C H -0.0315 0.1233 0.2269 0.1 Uiso 0.5 1 calc PR C -1
O5A O -0.0649(3) 0.6445(7) 0.1496(4) 0.048(2) Uani 0.25 1 d P . .
N5B N -0.0649(3) 0.6445(7) 0.1496(4) 0.048(2) Uani 0.25 1 d P . .
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 0 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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
_geom_angle_publ_flag
C6 C1 C2 118.3(5) . . ?
C6 C1 S1 121.8(4) . . ?
C2 C1 S1 119.9(4) . . ?
C1 C2 C3 120.6(6) . . ?
C4 C3 C2 122.2(6) . . ?
C3 C4 C5 116.3(6) . . ?
C3 C4 C7 122.5(6) . . ?
C5 C4 C7 121.2(6) . . ?
C4 C5 C6 122.2(6) . . ?
C1 C6 C5 120.3(5) . . ?
C19 C14 C15 120.0(5) . . ?
C19 C14 S2 121.0(4) . . ?
C15 C14 S2 118.9(4) . . ?
C16 C15 C14 119.6(5) . . ?
C15 C16 C17 121.8(5) . . ?
C18 C17 C16 117.2(5) . . ?
C18 C17 C20 120.7(6) . . ?
C16 C17 C20 122.0(6) . . ?
C17 C18 C19 122.7(5) . . ?
C18 C19 C14 118.6(5) . . ?
S1 N2A Ti1 156.2(3) . . ?
S3 N8A S3 54.0(2) 6_556 . ?
S3 N8A Ti3 153.5(3) 6_556 . ?
S3 N8A Ti3 148.3(3) . . ?
C8 N1 C9 108.9(4) . . ?
C8 N1 Ti1 115.7(3) . . ?
C9 N1 Ti1 118.2(4) . . ?
C11 N3 C10 110.1(4) . . ?
C11 N3 Ti2 118.0(3) . . ?
C10 N3 Ti2 115.7(3) . . ?
C13 N4 C12 110.1(4) . . ?
C13 N4 Ti2 117.7(3) . . ?
C12 N4 Ti2 115.9(3) . . ?
C21 N6 C22 109.5(5) . . ?
C21 N6 Ti3 115.9(4) . . ?
C22 N6 Ti3 116.4(4) . . ?
C29A N7 C28B 75.5(6) . . ?
C29A N7 C28A 108.9(6) . . ?
C28B N7 C29B 107.0(6) . . ?
C28A N7 C29B 133.2(7) . . ?
C29A N7 Ti3 116.4(5) . . ?
C28B N7 Ti3 122.3(6) . . ?
C28A N7 Ti3 114.6(5) . . ?
C29B N7 Ti3 110.5(5) . . ?
S1 O2A Ti2 153.3(2) . . ?
S2 N5A Ti2 154.8(2) . . ?
S2 O4A Ti3 153.5(3) . . ?
O1 S1 N2A 113.6(2) . . ?
O1 S1 O2A 113.8(2) . . ?
N2A S1 O2A 108.4(2) . . ?
O1 S1 C1 108.2(3) . . ?
N2A S1 C1 107.7(3) . . ?
O2A S1 C1 104.5(2) . . ?
O3 S2 O4A 113.6(2) . . ?
O3 S2 N5A 114.0(2) . . ?
O4A S2 N5A 109.5(2) . . ?
O3 S2 C14 107.8(2) . . ?
O4A S2 C14 106.7(2) . . ?
N5A S2 C14 104.5(2) . . ?
N2A Ti1 O2B 180.0(2) . 7_565 ?
N2A Ti1 N2A 180.0(2) . 7_565 ?
O2B Ti1 N2A 0.0(2) 7_565 7_565 ?
N2A Ti1 N1 90.53(15) . . ?
O2B Ti1 N1 89.47(15) 7_565 . ?
N2A Ti1 N1 89.47(15) 7_565 . ?
N2A Ti1 N1 89.47(15) . 7_565 ?
O2B Ti1 N1 90.53(15) 7_565 7_565 ?
N2A Ti1 N1 90.53(15) 7_565 7_565 ?
N1 Ti1 N1 180.0(2) . 7_565 ?
N2A Ti1 Cl1 89.94(11) . 7_565 ?
O2B Ti1 Cl1 90.06(11) 7_565 7_565 ?
N2A Ti1 Cl1 90.06(11) 7_565 7_565 ?
N1 Ti1 Cl1 86.63(12) . 7_565 ?
N1 Ti1 Cl1 93.37(12) 7_565 7_565 ?
N2A Ti1 Cl1 90.06(11) . . ?
O2B Ti1 Cl1 89.94(11) 7_565 . ?
N2A Ti1 Cl1 89.94(11) 7_565 . ?
N1 Ti1 Cl1 93.37(12) . . ?
N1 Ti1 Cl1 86.63(12) 7_565 . ?
Cl1 Ti1 Cl1 180.00(6) 7_565 . ?
O2A Ti2 N5A 178.90(17) . . ?
O2A Ti2 N4 92.89(16) . . ?
N5A Ti2 N4 86.01(16) . . ?
O2A Ti2 N3 86.25(16) . . ?
N5A Ti2 N3 94.85(16) . . ?
N4 Ti2 N3 178.98(16) . . ?
O2A Ti2 Cl2 89.75(12) . . ?
N5A Ti2 Cl2 90.32(12) . . ?
N4 Ti2 Cl2 88.52(11) . . ?
N3 Ti2 Cl2 92.03(12) . . ?
O2A Ti2 Cl3 90.72(12) . . ?
N5A Ti2 Cl3 89.22(12) . . ?
N4 Ti2 Cl3 92.11(11) . . ?
N3 Ti2 Cl3 87.35(11) . . ?
Cl2 Ti2 Cl3 179.19(8) . . ?
N8A Ti3 O4A 174.52(17) . . ?
N8A Ti3 N6 87.09(17) . . ?
O4A Ti3 N6 87.57(16) . . ?
N8A Ti3 N7 89.84(17) . . ?
O4A Ti3 N7 95.53(16) . . ?
N6 Ti3 N7 176.79(17) . . ?
N8A Ti3 Cl5 90.42(12) . . ?
O4A Ti3 Cl5 90.78(12) . . ?
N6 Ti3 Cl5 89.72(14) . . ?
N7 Ti3 Cl5 89.38(12) . . ?
N8A Ti3 Cl4 89.44(12) . . ?
O4A Ti3 Cl4 89.89(12) . . ?
N6 Ti3 Cl4 95.84(14) . . ?
N7 Ti3 Cl4 85.05(12) . . ?
Cl5 Ti3 Cl4 174.43(7) . . ?
S3 S3 O5A 174.6(4) 6_556 . ?
S3 S3 O8B 63.6(2) 6_556 6_556 ?
O5A S3 O8B 114.5(4) . 6_556 ?
S3 S3 N8A 63.6(2) 6_556 6_556 ?
O5A S3 N8A 114.5(4) . 6_556 ?
S3 S3 N8A 62.4(2) 6_556 . ?
O5A S3 N8A 114.7(5) . . ?
O8B S3 N8A 106.9(3) 6_556 . ?
N8A S3 N8A 106.9(3) 6_556 . ?
S3 S3 C23 68.14(12) 6_556 . ?
O5A S3 C23 117.2(4) . . ?
O8B S3 C23 101.2(2) 6_556 . ?
N8A S3 C23 101.2(2) 6_556 . ?
N8A S3 C23 100.6(2) . . ?
C24 C23 C24 121.2(9) . 6_556 ?
C24 C23 S3 138.1(5) . 6_556 ?
C24 C23 S3 99.6(4) 6_556 6_556 ?
C24 C23 S3 99.6(4) . . ?
C24 C23 S3 138.1(5) 6_556 . ?
C25 C24 C23 118.5(7) . . ?
C24 C25 C26 121.1(8) . . ?
C25 C26 C25 119.5(9) 6_556 . ?
C25 C26 C27 139.2(7) 6_556 . ?
C25 C26 C27 101.2(6) . . ?
C25 C26 C27 101.2(6) 6_556 6_556 ?
C25 C26 C27 139.2(7) . 6_556 ?
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
C1 C6 1.344(7) . ?
C1 C2 1.348(8) . ?
C1 S1 1.746(6) . ?
C2 C3 1.379(9) . ?
C3 C4 1.343(9) . ?
C4 C5 1.352(8) . ?
C4 C7 1.504(8) . ?
C5 C6 1.381(8) . ?
C8 N1 1.469(7) . ?
C9 N1 1.470(7) . ?
C10 N3 1.471(7) . ?
C11 N3 1.469(7) . ?
C12 N4 1.479(7) . ?
C13 N4 1.474(7) . ?
C14 C19 1.376(7) . ?
C14 C15 1.382(7) . ?
C14 S2 1.758(5) . ?
C15 C16 1.369(8) . ?
C16 C17 1.379(8) . ?
C17 C18 1.372(8) . ?
C17 C20 1.502(8) . ?
C18 C19 1.375(8) . ?
C21 N6 1.461(7) . ?
C22 N6 1.478(8) . ?
N2A S1 1.514(4) . ?
N2A Ti1 1.960(3) . ?
N8A S3 1.512(4) 6_556 ?
N8A S3 1.527(4) . ?
N8A Ti3 1.929(4) . ?
N1 Ti1 2.207(4) . ?
N3 Ti2 2.203(4) . ?
N4 Ti2 2.192(4) . ?
N6 Ti3 2.205(4) . ?
N7 C29A 1.442(7) . ?
N7 C28B 1.450(8) . ?
N7 C28A 1.504(8) . ?
N7 C29B 1.516(8) . ?
N7 Ti3 2.213(4) . ?
O1 S1 1.433(4) . ?
O2A S1 1.519(4) . ?
O2A Ti2 1.928(4) . ?
N5A S2 1.515(4) . ?
N5A Ti2 1.947(4) . ?
O3 S2 1.431(4) . ?
O4A S2 1.513(4) . ?
O4A Ti3 1.987(4) . ?
Cl1 Ti1 2.3459(13) . ?
Cl2 Ti2 2.3462(15) . ?
Cl3 Ti2 2.3541(14) . ?
Cl4 Ti3 2.3515(16) . ?
Cl5 Ti3 2.3394(16) . ?
Ti1 O2B 1.960(3) 7_565 ?
Ti1 N2A 1.960(3) 7_565 ?
Ti1 N1 2.207(4) 7_565 ?
Ti1 Cl1 2.3459(13) 7_565 ?
S3 S3 1.380(5) 6_556 ?
S3 O5A 1.425(8) . ?
S3 O8B 1.512(4) 6_556 ?
S3 N8A 1.512(4) 6_556 ?
S3 C23 1.853(8) . ?
C23 C24 1.365(10) . ?
C23 C24 1.365(10) 6_556 ?
C23 S3 1.853(8) 6_556 ?
C24 C25 1.341(11) . ?
C25 C26 1.353(9) . ?
C26 C25 1.353(9) 6_556 ?
C26 C27 1.586(13) . ?
C26 C27 1.586(13) 6_556 ?
