#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:57:47 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179086 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/48/4304862.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_4304862
loop_
_publ_author_name
'Yuri N. Belokon''
'William Clegg'
'Ross W. Harrington'
'Michael North'
'Carl Young'
_publ_section_title
;
In Situ Formation of Heterobimetallic Salen Complexes Containing Titanium
and/or Vanadium Ions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3801
_journal_page_last               3814
_journal_paper_doi               10.1021/ic702451a
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C111 H163 N6 O13 S Ti3 +,C2 H5 O4 S -,C14 H22 O2'
_chemical_formula_sum            'C127 H190 N6 O19 S2 Ti3'
_chemical_formula_weight         2312.67
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   27.380(2)
_cell_length_b                   27.380(2)
_cell_length_c                   38.033(3)
_cell_measurement_reflns_used    9567
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      3.09
_cell_volume                     24692(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX2 CCD diffractometer'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6709
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            59945
_diffrn_reflns_theta_full        19.60
_diffrn_reflns_theta_max         19.60
_diffrn_reflns_theta_min         3.32
_diffrn_standards_decay_%        5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7464
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       0.0036(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1452
_refine_ls_number_reflns         17038
_refine_ls_number_restraints     868
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0868P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                13456
_reflns_number_total             17038
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic702451a-file002.cif
_cod_data_source_block           mn8sq
_cod_database_code               4304862
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
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 0.06801(4) 0.51621(4) 0.51637(3) 0.0468(3) Uani 1 1 d . . .
Ti2 Ti 0.19592(4) 0.51056(4) 0.53941(2) 0.0386(3) Uani 1 1 d . . .
Ti3 Ti 0.34396(4) 0.55853(4) 0.56277(2) 0.0368(3) Uani 1 1 d . . .
S1 S -0.05726(7) 0.49922(7) 0.48184(5) 0.0620(5) Uani 1 1 d . . .
S2 S 0.26617(8) 0.69512(7) 0.38413(5) 0.0638(5) Uani 1 1 d . . .
O1 O 0.08884(15) 0.58683(16) 0.53629(11) 0.0539(10) Uani 1 1 d U . .
O2 O 0.00993(15) 0.45985(18) 0.54208(10) 0.0540(10) Uani 1 1 d U . .
O3 O 0.16769(13) 0.46383(14) 0.57778(9) 0.0402(9) Uani 1 1 d U . .
O4 O 0.19139(14) 0.46917(14) 0.50059(9) 0.0398(9) Uani 1 1 d U . .
O5 O 0.37523(13) 0.62957(14) 0.54181(9) 0.0399(9) Uani 1 1 d U . .
O6 O 0.36405(14) 0.51175(14) 0.53725(9) 0.0407(9) Uani 1 1 d U . .
O7 O 0.43147(15) 0.59572(17) 0.58279(10) 0.0454(9) Uani 1 1 d D . .
H7A H 0.4490(17) 0.5781(16) 0.5903(12) 0.039(16) Uiso 1 1 d D . .
H7B H 0.451(2) 0.6273(12) 0.5919(15) 0.06(2) Uiso 1 1 d D . .
O8 O 0.27381(14) 0.53030(13) 0.55010(8) 0.0391(9) Uani 1 1 d . . .
O9 O 0.12448(14) 0.50763(14) 0.52967(9) 0.0437(9) Uani 1 1 d . . .
O10 O 0.00173(15) 0.52963(15) 0.49357(11) 0.0574(11) Uani 1 1 d . . .
O11 O -0.06361(19) 0.4738(2) 0.44790(13) 0.1022(19) Uani 1 1 d . . .
O12 O -0.09518(18) 0.4618(2) 0.50671(12) 0.0810(14) Uani 1 1 d . . .
O13 O -0.0739(2) 0.5465(2) 0.47855(18) 0.1063(19) Uani 1 1 d U . .
O14 O 0.2216(2) 0.69897(19) 0.40130(17) 0.1078(19) Uani 1 1 d . . .
O15 O 0.2494(2) 0.6656(2) 0.35070(13) 0.1005(16) Uani 1 1 d . . .
O16 O 0.2955(2) 0.67617(19) 0.40619(13) 0.0907(15) Uani 1 1 d . . .
O17 O 0.3102(2) 0.7566(2) 0.37212(18) 0.1020(18) Uani 1 1 d U . .
O18 O 0.5963(2) 0.7884(3) 0.56739(18) 0.124(2) Uani 1 1 d U . .
H18 H 0.5678 0.7565 0.5705 0.149 Uiso 1 1 calc R . .
O19 O 0.5119(2) 0.7085(3) 0.59963(17) 0.1035(17) Uani 1 1 d U . .
N1 N 0.10989(18) 0.5634(2) 0.47027(13) 0.0515(13) Uani 1 1 d . . .
N2 N 0.03978(17) 0.45453(19) 0.47536(11) 0.0400(11) Uani 1 1 d . . .
N3 N 0.21127(16) 0.57729(18) 0.57462(11) 0.0361(11) Uani 1 1 d . . .
N4 N 0.23131(17) 0.58197(17) 0.50561(12) 0.0389(11) Uani 1 1 d . . .
N5 N 0.33660(17) 0.60054(18) 0.60875(11) 0.0361(11) Uani 1 1 d . . .
N6 N 0.32915(16) 0.50109(18) 0.60473(11) 0.0349(10) Uani 1 1 d . . .
C1 C 0.0973(2) 0.6360(3) 0.52247(19) 0.0559(17) Uani 1 1 d U . .
C2 C 0.0866(3) 0.6731(3) 0.5433(2) 0.073(2) Uani 1 1 d U . .
C3 C 0.1034(4) 0.7263(3) 0.5286(3) 0.093(3) Uani 1 1 d U . .
H3 H 0.0959 0.7514 0.5416 0.111 Uiso 1 1 calc R . .
C4 C 0.1298(4) 0.7447(4) 0.4967(3) 0.099(3) Uani 1 1 d U . .
C5 C 0.1367(3) 0.7082(3) 0.4769(2) 0.078(2) Uani 1 1 d U . .
H5 H 0.1539 0.7199 0.4544 0.093 Uiso 1 1 calc R . .
C6 C 0.1190(3) 0.6522(3) 0.48839(19) 0.0602(17) Uani 1 1 d U . .
C7 C 0.0553(3) 0.6528(3) 0.5784(2) 0.077(2) Uani 1 1 d U . .
C8 C 0.0431(4) 0.6963(4) 0.5951(3) 0.129(4) Uani 1 1 d U . .
H8A H 0.0233 0.6816 0.6174 0.193 Uiso 1 1 calc R . .
H8B H 0.0195 0.7039 0.5792 0.193 Uiso 1 1 calc R . .
H8C H 0.0787 0.7313 0.5994 0.193 Uiso 1 1 calc R . .
C9 C 0.0877(3) 0.6385(3) 0.6052(2) 0.092(2) Uani 1 1 d U . .
H9A H 0.0659 0.6254 0.6270 0.138 Uiso 1 1 calc R . .
H9B H 0.1242 0.6723 0.6100 0.138 Uiso 1 1 calc R . .
H9C H 0.0940 0.6088 0.5957 0.138 Uiso 1 1 calc R . .
C10 C -0.0038(3) 0.5992(3) 0.5726(2) 0.090(2) Uani 1 1 d U . .
H10A H -0.0232 0.5863 0.5953 0.135 Uiso 1 1 calc R . .
H10B H 0.0010 0.5692 0.5620 0.135 Uiso 1 1 calc R . .
H10C H -0.0264 0.6085 0.5569 0.135 Uiso 1 1 calc R . .
C11 C 0.1477(6) 0.8064(4) 0.4851(3) 0.133(4) Uani 1 1 d U . .
C12 C 0.0954(6) 0.8091(6) 0.4789(5) 0.219(8) Uani 1 1 d U . .
H12A H 0.0737 0.7834 0.4598 0.329 Uiso 1 1 calc R . .
H12B H 0.1054 0.8477 0.4726 0.329 Uiso 1 1 calc R . .
H12C H 0.0725 0.7980 0.5004 0.329 Uiso 1 1 calc R . .
C13 C 0.1837(8) 0.8455(5) 0.5133(4) 0.232(8) Uani 1 1 d U . .
H13A H 0.1959 0.8845 0.5064 0.348 Uiso 1 1 calc R . .
H13B H 0.2168 0.8413 0.5169 0.348 Uiso 1 1 calc R . .
H13C H 0.1620 0.8367 0.5352 0.348 Uiso 1 1 calc R . .
C14 C 0.1830(7) 0.8205(5) 0.4512(4) 0.216(7) Uani 1 1 d U . .
H14A H 0.1598 0.7952 0.4323 0.324 Uiso 1 1 calc R . .
H14B H 0.2156 0.8156 0.4553 0.324 Uiso 1 1 calc R . .
H14C H 0.1960 0.8597 0.4444 0.324 Uiso 1 1 calc R . .
C15 C 0.1265(3) 0.6155(3) 0.46481(18) 0.0590(17) Uani 1 1 d U . .
H15 H 0.1455 0.6314 0.4433 0.071 Uiso 1 1 calc R . .
C16 C 0.1155(2) 0.5300(2) 0.44250(15) 0.0517(16) Uani 1 1 d U . .
H16 H 0.1418 0.5173 0.4512 0.062 Uiso 1 1 calc R . .
C17 C 0.1374(3) 0.5581(3) 0.40680(17) 0.0660(18) Uani 1 1 d U . .
H17A H 0.1148 0.5751 0.3989 0.079 Uiso 1 1 calc R . .
H17B H 0.1770 0.5888 0.4094 0.079 Uiso 1 1 calc R . .
C18 C 0.1346(3) 0.5173(3) 0.37914(17) 0.0676(19) Uani 1 1 d U . .
H18A H 0.1468 0.5368 0.3562 0.081 Uiso 1 1 calc R . .
H18B H 0.1605 0.5033 0.3855 0.081 Uiso 1 1 calc R . .
C19 C 0.0755(2) 0.4685(2) 0.37612(16) 0.0569(16) Uani 1 1 d U . .
H19A H 0.0745 0.4416 0.3584 0.068 Uiso 1 1 calc R . .
H19B H 0.0503 0.4824 0.3680 0.068 Uiso 1 1 calc R . .
C20 C 0.0544(2) 0.4384(2) 0.41105(14) 0.0506(15) Uani 1 1 d U . .
H20A H 0.0153 0.4069 0.4082 0.061 Uiso 1 1 calc R . .
H20B H 0.0781 0.4222 0.4182 0.061 Uiso 1 1 calc R . .
C21 C 0.0557(2) 0.4766(2) 0.43908(15) 0.0440(14) Uani 1 1 d U . .
H21 H 0.0293 0.4900 0.4317 0.053 Uiso 1 1 calc R . .
C22 C 0.0116(2) 0.4011(3) 0.48098(15) 0.0425(14) Uani 1 1 d U . .
H22 H 0.0050 0.3774 0.4612 0.051 Uiso 1 1 calc R . .
C23 C -0.0109(2) 0.3735(2) 0.51397(15) 0.0435(14) Uani 1 1 d U . .
C24 C -0.0359(2) 0.3137(2) 0.51584(16) 0.0473(15) Uani 1 1 d U . .
H24 H -0.0338 0.2935 0.4961 0.057 Uiso 1 1 calc R . .
C25 C -0.0633(2) 0.2848(2) 0.54593(18) 0.0524(16) Uani 1 1 d U . .
C26 C -0.0662(2) 0.3177(3) 0.57450(16) 0.0564(17) Uani 1 1 d U . .
H26 H -0.0862 0.2979 0.5950 0.068 Uiso 1 1 calc R . .
C27 C -0.0430(2) 0.3745(3) 0.57474(15) 0.0469(15) Uani 1 1 d U . .
C28 C -0.0137(2) 0.4040(3) 0.54467(15) 0.0466(15) Uani 1 1 d U . .
C29 C -0.0896(3) 0.2215(3) 0.54956(17) 0.0620(18) Uani 1 1 d U . .
C30 C -0.1538(3) 0.1930(3) 0.55439(19) 0.078(2) Uani 1 1 d U . .
H30A H -0.1622 0.2097 0.5747 0.117 Uiso 1 1 calc R . .
H30B H -0.1693 0.1526 0.5584 0.117 Uiso 1 1 calc R . .
H30C H -0.1707 0.1987 0.5332 0.117 Uiso 1 1 calc R . .
C31 C -0.0789(3) 0.1946(3) 0.5180(2) 0.078(2) Uani 1 1 d U . .
H31A H -0.0969 0.1538 0.5217 0.117 Uiso 1 1 calc R . .
H31B H -0.0382 0.2104 0.5150 0.117 Uiso 1 1 calc R . .
H31C H -0.0947 0.2022 0.4970 0.117 Uiso 1 1 calc R . .
C32 C -0.0642(3) 0.2079(3) 0.5819(2) 0.090(2) Uani 1 1 d U . .
H32A H -0.0704 0.2248 0.6030 0.134 Uiso 1 1 calc R . .
H32B H -0.0236 0.2235 0.5783 0.134 Uiso 1 1 calc R . .
H32C H -0.0825 0.1670 0.5849 0.134 Uiso 1 1 calc R . .
C33 C -0.0491(2) 0.4055(3) 0.60636(16) 0.0615(18) Uani 1 1 d U . .
C34 C 0.0098(3) 0.4554(3) 0.61700(18) 0.073(2) Uani 1 1 d U . .
H34A H 0.0056 0.4752 0.6372 0.110 Uiso 1 1 calc R . .
H34B H 0.0260 0.4816 0.5972 0.110 Uiso 1 1 calc R . .
H34C H 0.0348 0.4408 0.6233 0.110 Uiso 1 1 calc R . .
C35 C -0.0706(3) 0.3673(3) 0.63873(18) 0.087(2) Uani 1 1 d U . .
H35A H -0.0742 0.3883 0.6584 0.131 Uiso 1 1 calc R . .
H35B H -0.0439 0.3548 0.6450 0.131 Uiso 1 1 calc R . .
H35C H -0.1075 0.3344 0.6335 0.131 Uiso 1 1 calc R . .
C36 C -0.0879(3) 0.4282(3) 0.59701(18) 0.076(2) Uani 1 1 d U . .
H36A H -0.0918 0.4479 0.6174 0.114 Uiso 1 1 calc R . .
H36B H -0.1250 0.3968 0.5904 0.114 Uiso 1 1 calc R . .
H36C H -0.0719 0.4544 0.5772 0.114 Uiso 1 1 calc R . .
C37 C 0.1503(2) 0.4655(3) 0.60998(15) 0.0441(15) Uani 1 1 d U . .
C38 C 0.1235(2) 0.4145(2) 0.62996(15) 0.0448(15) Uani 1 1 d U . .
C39 C 0.1082(2) 0.4186(3) 0.66402(16) 0.0556(17) Uani 1 1 d U . .
H39 H 0.0914 0.3854 0.6780 0.067 Uiso 1 1 calc R . .
C40 C 0.1159(2) 0.4693(3) 0.67964(16) 0.0557(16) Uani 1 1 d U . .
C41 C 0.1419(2) 0.5166(3) 0.65874(16) 0.0499(16) Uani 1 1 d U . .
H41 H 0.1478 0.5513 0.6682 0.060 Uiso 1 1 calc R . .
C42 C 0.1599(2) 0.5166(2) 0.62467(15) 0.0397(13) Uani 1 1 d U . .
C43 C 0.1139(2) 0.3590(2) 0.61462(16) 0.0523(16) Uani 1 1 d U . .
C44 C 0.0809(3) 0.3087(3) 0.63939(17) 0.0693(19) Uani 1 1 d U . .
H44A H 0.0758 0.2742 0.6282 0.104 Uiso 1 1 calc R . .
H44B H 0.0439 0.3046 0.6444 0.104 Uiso 1 1 calc R . .
H44C H 0.1018 0.3151 0.6614 0.104 Uiso 1 1 calc R . .
C45 C 0.1704(2) 0.3619(3) 0.60694(17) 0.0565(16) Uani 1 1 d U . .
H45A H 0.1633 0.3259 0.5970 0.085 Uiso 1 1 calc R . .
H45B H 0.1918 0.3693 0.6288 0.085 Uiso 1 1 calc R . .
H45C H 0.1920 0.3923 0.5901 0.085 Uiso 1 1 calc R . .
C46 C 0.0795(2) 0.3453(3) 0.57960(16) 0.0566(16) Uani 1 1 d U . .
H46A H 0.0737 0.3096 0.5700 0.085 Uiso 1 1 calc R . .
H46B H 0.1004 0.3756 0.5626 0.085 Uiso 1 1 calc R . .
H46C H 0.0428 0.3421 0.5843 0.085 Uiso 1 1 calc R . .
C47 C 0.0971(3) 0.4719(3) 0.71699(16) 0.075(2) Uani 1 1 d U . .
C48 C 0.0640(8) 0.4188(4) 0.7318(3) 0.252(10) Uani 1 1 d U . .
H48A H 0.0377 0.3931 0.7140 0.378 Uiso 1 1 calc R . .
H48B H 0.0428 0.4216 0.7516 0.378 Uiso 1 1 calc R . .
H48C H 0.0882 0.4043 0.7400 0.378 Uiso 1 1 calc R . .
C49 C 0.0522(4) 0.4953(4) 0.7138(2) 0.109(3) Uani 1 1 d U . .
H49A H 0.0716 0.5335 0.7040 0.164 Uiso 1 1 calc R . .
H49B H 0.0375 0.4959 0.7372 0.164 Uiso 1 1 calc R . .
H49C H 0.0210 0.4704 0.6983 0.164 Uiso 1 1 calc R . .
C50 C 0.1392(3) 0.5162(3) 0.73727(18) 0.091(2) Uani 1 1 d U . .
H50A H 0.1603 0.5496 0.7224 0.137 Uiso 1 1 calc R . .
H50B H 0.1650 0.5046 0.7469 0.137 Uiso 1 1 calc R . .
H50C H 0.1215 0.5253 0.7566 0.137 Uiso 1 1 calc R . .
C51 C 0.1901(2) 0.5693(2) 0.60553(16) 0.0408(14) Uani 1 1 d U . .
H51 H 0.1947 0.6019 0.6174 0.049 Uiso 1 1 calc R . .
C52 C 0.2463(2) 0.6344(2) 0.55931(14) 0.0416(14) Uani 1 1 d U . .
H52 H 0.2863 0.6430 0.5608 0.050 Uiso 1 1 calc R . .
C53 C 0.2442(3) 0.6834(2) 0.57835(16) 0.0528(16) Uani 1 1 d U . .
H53A H 0.2050 0.6761 0.5787 0.063 Uiso 1 1 calc R . .
H53B H 0.2570 0.6859 0.6030 0.063 Uiso 1 1 calc R . .
C54 C 0.2820(2) 0.7387(2) 0.55950(16) 0.0537(16) Uani 1 1 d U . .
H54A H 0.2786 0.7693 0.5710 0.064 Uiso 1 1 calc R . .
H54B H 0.3218 0.7479 0.5617 0.064 Uiso 1 1 calc R . .
C55 C 0.2672(2) 0.7362(2) 0.52107(15) 0.0466(14) Uani 1 1 d U . .
H55A H 0.2940 0.7723 0.5096 0.056 Uiso 1 1 calc R . .
H55B H 0.2289 0.7310 0.5188 0.056 Uiso 1 1 calc R . .
C56 C 0.2693(2) 0.6877(2) 0.50266(14) 0.0455(15) Uani 1 1 d U . .
H56A H 0.2566 0.6852 0.4780 0.055 Uiso 1 1 calc R . .
H56B H 0.3088 0.6955 0.5023 0.055 Uiso 1 1 calc R . .
C57 C 0.2331(2) 0.6327(2) 0.52060(14) 0.0444(15) Uani 1 1 d U . .
H57 H 0.1937 0.6259 0.5192 0.053 Uiso 1 1 calc R . .
C58 C 0.2491(2) 0.5819(2) 0.47394(16) 0.0410(14) Uani 1 1 d U . .
H58 H 0.2672 0.6171 0.4619 0.049 Uiso 1 1 calc R . .
C59 C 0.2439(2) 0.5336(2) 0.45515(14) 0.0363(13) Uani 1 1 d U . .
C60 C 0.2660(2) 0.5421(2) 0.42090(14) 0.0443(14) Uani 1 1 d U . .
H60 H 0.2869 0.5794 0.4119 0.053 Uiso 1 1 calc R . .
C61 C 0.2578(2) 0.4970(3) 0.39998(16) 0.0499(15) Uani 1 1 d U . .
C62 C 0.2280(2) 0.4439(2) 0.41385(16) 0.0478(15) Uani 1 1 d U . .
H62 H 0.2223 0.4132 0.3993 0.057 Uiso 1 1 calc R . .
C63 C 0.2053(2) 0.4313(2) 0.44781(15) 0.0427(14) Uani 1 1 d U . .
C64 C 0.2140(2) 0.4783(2) 0.46810(15) 0.0429(15) Uani 1 1 d U . .
C65 C 0.2814(3) 0.5060(3) 0.36268(16) 0.0576(17) Uani 1 1 d U . .
C66 C 0.2368(3) 0.4716(3) 0.33637(16) 0.076(2) Uani 1 1 d U . .
H66A H 0.2173 0.4319 0.3436 0.113 Uiso 1 1 calc R . .
H66B H 0.2542 0.4753 0.3133 0.113 Uiso 1 1 calc R . .
H66C H 0.2097 0.4849 0.3350 0.113 Uiso 1 1 calc R . .
C67 C 0.3140(4) 0.5670(3) 0.35343(19) 0.092(3) Uani 1 1 d U . .
H67A H 0.3427 0.5874 0.3715 0.139 Uiso 1 1 calc R . .
H67B H 0.2884 0.5822 0.3521 0.139 Uiso 1 1 calc R . .
H67C H 0.3324 0.5715 0.3306 0.139 Uiso 1 1 calc R . .
C68 C 0.3268(3) 0.4859(3) 0.3618(2) 0.080(2) Uani 1 1 d U . .
H68A H 0.3085 0.4456 0.3676 0.120 Uiso 1 1 calc R . .
H68B H 0.3565 0.5075 0.3791 0.120 Uiso 1 1 calc R . .
H68C H 0.3435 0.4921 0.3383 0.120 Uiso 1 1 calc R . .
C69 C 0.1728(2) 0.3712(2) 0.46292(15) 0.0470(15) Uani 1 1 d U . .
C70 C 0.1707(3) 0.3273(2) 0.43757(17) 0.0578(16) Uani 1 1 d U . .
H70A H 0.1530 0.3288 0.4155 0.087 Uiso 1 1 calc R . .
H70B H 0.1487 0.2897 0.4480 0.087 Uiso 1 1 calc R . .
H70C H 0.2092 0.3351 0.4328 0.087 Uiso 1 1 calc R . .
C71 C 0.2006(2) 0.3677(2) 0.49696(16) 0.0527(16) Uani 1 1 d U . .
H71A H 0.2020 0.3954 0.5138 0.079 Uiso 1 1 calc R . .
H71B H 0.2389 0.3756 0.4919 0.079 Uiso 1 1 calc R . .
H71C H 0.1785 0.3297 0.5069 0.079 Uiso 1 1 calc R . .
C72 C 0.1111(2) 0.3548(2) 0.47037(16) 0.0520(16) Uani 1 1 d U . .
H72A H 0.1102 0.3820 0.4867 0.078 Uiso 1 1 calc R . .
H72B H 0.0911 0.3170 0.4808 0.078 Uiso 1 1 calc R . .
H72C H 0.0926 0.3549 0.4483 0.078 Uiso 1 1 calc R . .
C73 C 0.3994(2) 0.6836(2) 0.55203(14) 0.0364(13) Uani 1 1 d U . .
C74 C 0.4338(2) 0.7273(2) 0.52805(14) 0.0419(14) Uani 1 1 d U . .
C75 C 0.4524(2) 0.7822(2) 0.53922(16) 0.0459(15) Uani 1 1 d U . .
H75 H 0.4752 0.8120 0.5235 0.055 Uiso 1 1 calc R . .
C76 C 0.4400(2) 0.7965(2) 0.57162(15) 0.0493(15) Uani 1 1 d U . .
C77 C 0.4107(2) 0.7532(2) 0.59543(15) 0.0469(15) Uani 1 1 d U . .
H77 H 0.4043 0.7620 0.6185 0.056 Uiso 1 1 calc R . .
C78 C 0.3904(2) 0.6967(2) 0.58621(14) 0.0371(13) Uani 1 1 d U . .
C79 C 0.4517(2) 0.7125(2) 0.49258(13) 0.0419(14) Uani 1 1 d U . .
C80 C 0.4911(3) 0.7660(2) 0.47193(16) 0.0544(16) Uani 1 1 d U . .
H80A H 0.4715 0.7868 0.4666 0.082 Uiso 1 1 calc R . .
H80B H 0.5024 0.7557 0.4500 0.082 Uiso 1 1 calc R . .
H80C H 0.5248 0.7898 0.4861 0.082 Uiso 1 1 calc R . .
C81 C 0.4016(2) 0.6773(2) 0.46885(14) 0.0463(15) Uani 1 1 d U . .
H81A H 0.3814 0.6977 0.4642 0.069 Uiso 1 1 calc R . .
H81B H 0.3762 0.6414 0.4804 0.069 Uiso 1 1 calc R . .
H81C H 0.4149 0.6700 0.4466 0.069 Uiso 1 1 calc R . .
C82 C 0.4840(3) 0.6818(3) 0.50021(16) 0.0580(17) Uani 1 1 d U . .
H82A H 0.4600 0.6476 0.5138 0.087 Uiso 1 1 calc R . .
H82B H 0.5180 0.7065 0.5138 0.087 Uiso 1 1 calc R . .
H82C H 0.4947 0.6716 0.4780 0.087 Uiso 1 1 calc R . .
C83 C 0.4593(3) 0.8593(2) 0.57961(17) 0.0599(17) Uani 1 1 d U . .
C84 C 0.4399(3) 0.8645(2) 0.61765(19) 0.082(2) Uani 1 1 d U . .
H84A H 0.4577 0.8518 0.6349 0.122 Uiso 1 1 calc R . .
H84B H 0.3988 0.8411 0.6194 0.122 Uiso 1 1 calc R . .
H84C H 0.4510 0.9040 0.6223 0.122 Uiso 1 1 calc R . .
C85 C 0.4309(3) 0.8804(3) 0.55293(19) 0.080(2) Uani 1 1 d U . .
H85A H 0.3898 0.8575 0.5551 0.120 Uiso 1 1 calc R . .
H85B H 0.4422 0.8771 0.5290 0.120 Uiso 1 1 calc R . .
H85C H 0.4429 0.9199 0.5578 0.120 Uiso 1 1 calc R . .
C86 C 0.5219(3) 0.8945(3) 0.5779(2) 0.086(2) Uani 1 1 d U . .
H86A H 0.5388 0.8809 0.5953 0.129 Uiso 1 1 calc R . .
H86B H 0.5332 0.9339 0.5830 0.129 Uiso 1 1 calc R . .
H86C H 0.5348 0.8918 0.5543 0.129 Uiso 1 1 calc R . .
C87 C 0.3598(2) 0.6546(2) 0.61266(14) 0.0415(14) Uani 1 1 d U . .
H87 H 0.3563 0.6678 0.6351 0.050 Uiso 1 1 calc R . .
C88 C 0.3082(2) 0.5622(2) 0.63824(13) 0.0389(14) Uani 1 1 d U . .
H88 H 0.2675 0.5388 0.6318 0.047 Uiso 1 1 calc R . .
C89 C 0.3107(2) 0.5896(2) 0.67373(14) 0.0472(15) Uani 1 1 d U . .
H89A H 0.3505 0.6156 0.6802 0.057 Uiso 1 1 calc R . .
H89B H 0.2914 0.6119 0.6719 0.057 Uiso 1 1 calc R . .
C90 C 0.2828(2) 0.5453(2) 0.70197(15) 0.0497(15) Uani 1 1 d U . .
H90A H 0.2866 0.5639 0.7249 0.060 Uiso 1 1 calc R . .
H90B H 0.2421 0.5217 0.6967 0.060 Uiso 1 1 calc R . .
C91 C 0.3090(3) 0.5089(3) 0.70405(16) 0.0564(16) Uani 1 1 d U . .
H91A H 0.2903 0.4804 0.7228 0.068 Uiso 1 1 calc R . .
H91B H 0.3494 0.5324 0.7104 0.068 Uiso 1 1 calc R . .
C92 C 0.3041(2) 0.4793(2) 0.66964(14) 0.0438(14) Uani 1 1 d U . .
H92A H 0.2639 0.4537 0.6640 0.053 Uiso 1 1 calc R . .
H92B H 0.3227 0.4563 0.6717 0.053 Uiso 1 1 calc R . .
C93 C 0.3318(2) 0.5224(2) 0.64057(14) 0.0395(14) Uani 1 1 d U . .
H93 H 0.3726 0.5458 0.6468 0.047 Uiso 1 1 calc R . .
C94 C 0.31541(19) 0.4483(2) 0.59922(15) 0.0381(14) Uani 1 1 d U . .
H94 H 0.3028 0.4241 0.6191 0.046 Uiso 1 1 calc R . .
C95 C 0.3173(2) 0.4239(2) 0.56729(14) 0.0349(13) Uani 1 1 d U . .
C96 C 0.2956(2) 0.3649(2) 0.56569(16) 0.0440(14) Uani 1 1 d U . .
H96 H 0.2756 0.3425 0.5854 0.053 Uiso 1 1 calc R . .
C97 C 0.3025(2) 0.3386(2) 0.53646(17) 0.0490(15) Uani 1 1 d U . .
C98 C 0.3357(2) 0.3740(2) 0.50896(16) 0.0502(15) Uani 1 1 d U . .
H98 H 0.3429 0.3568 0.4895 0.060 Uiso 1 1 calc R . .
C99 C 0.3588(2) 0.4324(2) 0.50825(15) 0.0424(14) Uani 1 1 d U . .
C100 C 0.3466(2) 0.4570(2) 0.53753(16) 0.0431(14) Uani 1 1 d U . .
C101 C 0.2779(3) 0.2748(2) 0.53286(17) 0.0551(17) Uani 1 1 d U . .
C102 C 0.2445(3) 0.2434(2) 0.56677(19) 0.0672(19) Uani 1 1 d U . .
H10D H 0.2293 0.2028 0.5640 0.101 Uiso 1 1 calc R . .
H10E H 0.2134 0.2510 0.5705 0.101 Uiso 1 1 calc R . .
H10F H 0.2699 0.2570 0.5871 0.101 Uiso 1 1 calc R . .
C103 C 0.2364(3) 0.2526(3) 0.5017(2) 0.079(2) Uani 1 1 d U . .
H10G H 0.2204 0.2117 0.4996 0.119 Uiso 1 1 calc R . .
H10H H 0.2564 0.2709 0.4800 0.119 Uiso 1 1 calc R . .
H10I H 0.2060 0.2609 0.5057 0.119 Uiso 1 1 calc R . .
C104 C 0.3250(3) 0.2604(3) 0.52788(18) 0.0636(18) Uani 1 1 d U . .
H10J H 0.3084 0.2194 0.5260 0.095 Uiso 1 1 calc R . .
H10K H 0.3506 0.2743 0.5481 0.095 Uiso 1 1 calc R . .
H10L H 0.3461 0.2784 0.5064 0.095 Uiso 1 1 calc R . .
C105 C 0.3940(2) 0.4684(2) 0.47756(15) 0.0510(15) Uani 1 1 d U . .
C106 C 0.4531(2) 0.5132(2) 0.49069(16) 0.0529(16) Uani 1 1 d U . .
H10M H 0.4757 0.5359 0.4708 0.079 Uiso 1 1 calc R . .
H10N H 0.4717 0.4943 0.5016 0.079 Uiso 1 1 calc R . .
H10O H 0.4494 0.5376 0.5080 0.079 Uiso 1 1 calc R . .
C107 C 0.3659(2) 0.4975(3) 0.45976(16) 0.0550(16) Uani 1 1 d U . .
H10P H 0.3895 0.5206 0.4402 0.082 Uiso 1 1 calc R . .
H10Q H 0.3612 0.5217 0.4768 0.082 Uiso 1 1 calc R . .
H10R H 0.3289 0.4691 0.4507 0.082 Uiso 1 1 calc R . .
C108 C 0.4017(3) 0.4327(3) 0.44886(17) 0.0692(19) Uani 1 1 d U . .
H10S H 0.4251 0.4575 0.4298 0.104 Uiso 1 1 calc R . .
H10T H 0.3647 0.4049 0.4395 0.104 Uiso 1 1 calc R . .
H10U H 0.4201 0.4132 0.4591 0.104 Uiso 1 1 calc R . .
C109 C -0.0402(4) 0.5943(4) 0.4574(3) 0.138(4) Uani 1 1 d U . .
H10V H -0.0453 0.5833 0.4323 0.165 Uiso 1 1 calc R . .
H10W H 0.0001 0.6101 0.4634 0.165 Uiso 1 1 calc R . .
C110 C -0.0574(6) 0.6380(5) 0.4635(6) 0.233(8) Uani 1 1 d U . .
H11A H -0.0345 0.6710 0.4487 0.350 Uiso 1 1 calc R . .
H11B H -0.0516 0.6493 0.4883 0.350 Uiso 1 1 calc R . .
H11C H -0.0973 0.6221 0.4575 0.350 Uiso 1 1 calc R . .
C111 C 0.3353(4) 0.7982(4) 0.4000(4) 0.147(4) Uani 1 1 d U . .
H11D H 0.3282 0.7788 0.4229 0.176 Uiso 1 1 calc R . .
H11E H 0.3766 0.8205 0.3964 0.176 Uiso 1 1 calc R . .
C112 C 0.3124(8) 0.8351(7) 0.4002(7) 0.309(12) Uani 1 1 d U . .
H11F H 0.3307 0.8635 0.4187 0.464 Uiso 1 1 calc R . .
H11G H 0.2718 0.8132 0.4048 0.464 Uiso 1 1 calc R . .
H11H H 0.3190 0.8539 0.3774 0.464 Uiso 1 1 calc R . .
C113 C 0.6025(4) 0.8233(4) 0.5958(3) 0.101(3) Uani 1 1 d U . .
C114 C 0.6470(4) 0.8791(4) 0.5948(2) 0.100(3) Uani 1 1 d U . .
C115 C 0.6483(4) 0.9125(4) 0.6222(3) 0.108(3) Uani 1 1 d U . .
H115 H 0.6762 0.9513 0.6213 0.130 Uiso 1 1 calc R . .
C116 C 0.6107(4) 0.8934(4) 0.6521(2) 0.099(3) Uani 1 1 d U A .
C117 C 0.5680(4) 0.8367(4) 0.6507(2) 0.100(3) Uani 1 1 d U . .
H117 H 0.5411 0.8219 0.6692 0.120 Uiso 1 1 calc R . .
C118 C 0.5639(4) 0.8018(4) 0.6232(2) 0.092(2) Uani 1 1 d U . .
C119 C 0.6877(4) 0.9042(4) 0.5638(3) 0.120(3) Uani 1 1 d U . .
C120 C 0.7316(5) 0.9666(4) 0.5690(3) 0.160(5) Uani 1 1 d U . .
H12D H 0.7524 0.9712 0.5909 0.240 Uiso 1 1 calc R . .
H12E H 0.7125 0.9888 0.5703 0.240 Uiso 1 1 calc R . .
H12F H 0.7580 0.9798 0.5491 0.240 Uiso 1 1 calc R . .
C121 C 0.7194(5) 0.8692(5) 0.5615(4) 0.164(4) Uani 1 1 d U . .
H12G H 0.7414 0.8750 0.5830 0.246 Uiso 1 1 calc R . .
H12H H 0.7447 0.8818 0.5412 0.246 Uiso 1 1 calc R . .
H12I H 0.6916 0.8290 0.5590 0.246 Uiso 1 1 calc R . .
C122 C 0.6557(4) 0.8956(5) 0.5300(3) 0.148(4) Uani 1 1 d U . .
H12J H 0.6280 0.8555 0.5271 0.221 Uiso 1 1 calc R . .
H12K H 0.6821 0.9083 0.5101 0.221 Uiso 1 1 calc R . .
H12L H 0.6362 0.9174 0.5306 0.221 Uiso 1 1 calc R . .
C123 C 0.6149(4) 0.9330(4) 0.6815(3) 0.104(3) Uani 1 1 d U . .
C124 C 0.6772(10) 0.9530(11) 0.6989(8) 0.127(10) Uani 0.397(18) 1 d PU A 1
H12M H 0.7068 0.9758 0.6818 0.190 Uiso 0.397(18) 1 calc PR A 1
H12N H 0.6798 0.9196 0.7051 0.190 Uiso 0.397(18) 1 calc PR A 1
H12O H 0.6822 0.9754 0.7200 0.190 Uiso 0.397(18) 1 calc PR A 1
C125 C 0.6149(18) 0.9794(14) 0.6658(8) 0.156(13) Uani 0.397(18) 1 d PU A 1
H12P H 0.6448 0.9960 0.6481 0.234 Uiso 0.397(18) 1 calc PR A 1
H12Q H 0.6216 1.0077 0.6839 0.234 Uiso 0.397(18) 1 calc PR A 1
H12R H 0.5783 0.9670 0.6546 0.234 Uiso 0.397(18) 1 calc PR A 1
C126 C 0.5753(14) 0.9041(15) 0.7067(10) 0.141(12) Uani 0.397(18) 1 d PU A 1
H12S H 0.5792 0.9299 0.7258 0.212 Uiso 0.397(18) 1 calc PR A 1
H12T H 0.5806 0.8737 0.7160 0.212 Uiso 0.397(18) 1 calc PR A 1
H12U H 0.5375 0.8880 0.6963 0.212 Uiso 0.397(18) 1 calc PR A 1
C24A C 0.6184(11) 0.9113(7) 0.7147(5) 0.132(8) Uani 0.603(18) 1 d PU A 2
H24A H 0.5874 0.8724 0.7170 0.197 Uiso 0.603(18) 1 calc PR A 2
H24B H 0.6157 0.9345 0.7334 0.197 Uiso 0.603(18) 1 calc PR A 2
H24C H 0.6545 0.9122 0.7166 0.197 Uiso 0.603(18) 1 calc PR A 2
C25A C 0.6657(10) 0.9918(9) 0.6785(6) 0.156(10) Uani 0.603(18) 1 d PU A 2
H25A H 0.6650 1.0082 0.6558 0.234 Uiso 0.603(18) 1 calc PR A 2
H25B H 0.7003 0.9897 0.6804 0.234 Uiso 0.603(18) 1 calc PR A 2
H25C H 0.6646 1.0155 0.6975 0.234 Uiso 0.603(18) 1 calc PR A 2
C26A C 0.5573(7) 0.9383(9) 0.6808(6) 0.146(8) Uani 0.603(18) 1 d PU A 2
H26A H 0.5544 0.9534 0.6580 0.220 Uiso 0.603(18) 1 calc PR A 2
H26B H 0.5593 0.9638 0.6995 0.220 Uiso 0.603(18) 1 calc PR A 2
H26C H 0.5241 0.9010 0.6843 0.220 Uiso 0.603(18) 1 calc PR A 2
C127 C 0.5196(4) 0.7440(4) 0.6241(3) 0.111(3) Uani 1 1 d U . .
H127 H 0.4948 0.7314 0.6438 0.133 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'
Ti Ti 0.1991 0.4022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0959 0.1108 '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 O2 109.73(18) . . ?
O1 Ti1 O9 100.80(16) . . ?
O1 Ti1 O10 80.71(15) . . ?
O1 Ti1 N1 85.06(19) . . ?
O1 Ti1 N2 155.46(18) . . ?
O2 Ti1 O9 100.61(17) . . ?
O2 Ti1 O10 84.88(16) . . ?
O2 Ti1 N1 156.34(17) . . ?
O2 Ti1 N2 84.62(17) . . ?
O9 Ti1 O10 173.31(17) . . ?
O9 Ti1 N1 94.30(17) . . ?
O9 Ti1 N2 95.71(16) . . ?
O10 Ti1 N1 79.29(16) . . ?
O10 Ti1 N2 80.92(15) . . ?
N1 Ti1 N2 75.65(18) . . ?
O3 Ti2 O4 109.60(15) . . ?
O3 Ti2 O8 92.77(14) . . ?
O3 Ti2 O9 93.33(15) . . ?
O3 Ti2 N3 86.10(16) . . ?
O3 Ti2 N4 163.82(17) . . ?
O4 Ti2 O8 93.77(15) . . ?
O4 Ti2 O9 93.73(15) . . ?
O4 Ti2 N3 164.30(17) . . ?
O4 Ti2 N4 86.57(17) . . ?
O8 Ti2 O9 168.15(14) . . ?
O8 Ti2 N3 84.97(14) . . ?
O8 Ti2 N4 86.51(15) . . ?
O9 Ti2 N3 85.33(15) . . ?
O9 Ti2 N4 84.81(15) . . ?
N3 Ti2 N4 77.74(17) . . ?
O5 Ti3 O6 110.40(15) . . ?
O5 Ti3 O7 80.85(15) . . ?
O5 Ti3 O8 100.00(15) . . ?
O5 Ti3 N5 84.67(16) . . ?
O5 Ti3 N6 155.08(17) . . ?
O6 Ti3 O7 82.77(15) . . ?
O6 Ti3 O8 100.76(15) . . ?
O6 Ti3 N5 155.76(16) . . ?
O6 Ti3 N6 84.09(16) . . ?
O7 Ti3 O8 175.73(16) . . ?
O7 Ti3 N5 81.04(15) . . ?
O7 Ti3 N6 81.08(15) . . ?
O8 Ti3 N5 94.85(15) . . ?
O8 Ti3 N6 96.83(16) . . ?
N5 Ti3 N6 75.68(16) . . ?
O10 S1 O11 112.4(3) . . ?
O10 S1 O12 114.4(3) . . ?
O10 S1 O13 104.2(3) . . ?
O11 S1 O12 112.8(3) . . ?
O11 S1 O13 108.2(4) . . ?
O12 S1 O13 104.0(3) . . ?
O14 S2 O15 113.3(4) . . ?
O14 S2 O16 114.4(4) . . ?
O14 S2 O17 106.2(3) . . ?
O15 S2 O16 113.1(3) . . ?
O15 S2 O17 101.6(4) . . ?
O16 S2 O17 106.9(3) . . ?
Ti1 O1 C1 132.8(4) . . ?
Ti1 O2 C28 136.0(4) . . ?
Ti2 O3 C37 138.1(4) . . ?
Ti2 O4 C64 138.0(3) . . ?
Ti3 O5 C73 137.9(3) . . ?
Ti3 O6 C100 134.3(3) . . ?
Ti2 O8 Ti3 169.9(2) . . ?
Ti1 O9 Ti2 169.5(2) . . ?
Ti1 O10 S1 142.2(2) . . ?
S1 O13 C109 118.9(6) . . ?
S2 O17 C111 116.0(6) . . ?
Ti1 N1 C15 126.2(5) . . ?
Ti1 N1 C16 114.2(3) . . ?
C15 N1 C16 119.5(5) . . ?
Ti1 N2 C21 116.2(3) . . ?
Ti1 N2 C22 123.5(4) . . ?
C21 N2 C22 120.4(5) . . ?
Ti2 N3 C51 123.5(4) . . ?
Ti2 N3 C52 113.8(3) . . ?
C51 N3 C52 122.6(4) . . ?
Ti2 N4 C57 114.6(3) . . ?
Ti2 N4 C58 124.0(4) . . ?
C57 N4 C58 121.4(4) . . ?
Ti3 N5 C87 125.4(4) . . ?
Ti3 N5 C88 113.3(3) . . ?
C87 N5 C88 120.8(4) . . ?
Ti3 N6 C93 116.6(3) . . ?
Ti3 N6 C94 122.4(4) . . ?
C93 N6 C94 120.9(4) . . ?
O1 C1 C2 119.8(7) . . ?
O1 C1 C6 120.5(5) . . ?
C2 C1 C6 119.7(7) . . ?
C1 C2 C3 115.8(7) . . ?
C1 C2 C7 120.1(7) . . ?
C3 C2 C7 124.0(7) . . ?
C2 C3 C4 125.0(8) . . ?
C3 C4 C5 118.0(8) . . ?
C3 C4 C11 117.9(9) . . ?
C5 C4 C11 124.1(9) . . ?
C4 C5 C6 122.0(8) . . ?
C1 C6 C5 119.1(6) . . ?
C1 C6 C15 122.9(6) . . ?
C5 C6 C15 117.9(7) . . ?
C2 C7 C8 112.3(7) . . ?
C2 C7 C9 112.5(6) . . ?
C2 C7 C10 110.3(6) . . ?
C8 C7 C9 107.7(7) . . ?
C8 C7 C10 105.2(6) . . ?
C9 C7 C10 108.5(7) . . ?
C4 C11 C12 108.0(10) . . ?
C4 C11 C13 108.0(10) . . ?
C4 C11 C14 109.0(8) . . ?
C12 C11 C13 112.6(11) . . ?
C12 C11 C14 110.8(12) . . ?
C13 C11 C14 108.4(12) . . ?
N1 C15 C6 125.7(6) . . ?
N1 C16 C17 117.9(5) . . ?
N1 C16 C21 105.0(5) . . ?
C17 C16 C21 111.1(5) . . ?
C16 C17 C18 112.7(5) . . ?
C17 C18 C19 110.2(6) . . ?
C18 C19 C20 111.4(5) . . ?
C19 C20 C21 112.3(5) . . ?
N2 C21 C16 105.1(4) . . ?
N2 C21 C20 119.0(4) . . ?
C16 C21 C20 111.4(5) . . ?
N2 C22 C23 126.9(5) . . ?
C22 C23 C24 118.8(5) . . ?
C22 C23 C28 122.0(5) . . ?
C24 C23 C28 119.0(5) . . ?
C23 C24 C25 120.7(6) . . ?
C24 C25 C26 116.8(5) . . ?
C24 C25 C29 122.9(6) . . ?
C26 C25 C29 120.3(6) . . ?
C25 C26 C27 125.7(6) . . ?
C26 C27 C28 117.5(6) . . ?
C26 C27 C33 121.6(6) . . ?
C28 C27 C33 120.9(5) . . ?
O2 C28 C23 117.6(5) . . ?
O2 C28 C27 122.2(5) . . ?
C23 C28 C27 120.2(5) . . ?
C25 C29 C30 111.2(5) . . ?
C25 C29 C31 112.8(5) . . ?
C25 C29 C32 109.5(5) . . ?
C30 C29 C31 107.4(5) . . ?
C30 C29 C32 108.7(5) . . ?
C31 C29 C32 107.1(6) . . ?
C27 C33 C34 109.9(5) . . ?
C27 C33 C35 111.5(6) . . ?
C27 C33 C36 109.6(5) . . ?
C34 C33 C35 105.5(5) . . ?
C34 C33 C36 109.3(6) . . ?
C35 C33 C36 111.0(5) . . ?
O3 C37 C38 118.4(5) . . ?
O3 C37 C42 120.8(5) . . ?
C38 C37 C42 120.7(5) . . ?
C37 C38 C39 116.5(6) . . ?
C37 C38 C43 121.3(5) . . ?
C39 C38 C43 122.2(5) . . ?
C38 C39 C40 124.5(6) . . ?
C39 C40 C41 115.5(5) . . ?
C39 C40 C47 122.9(6) . . ?
C41 C40 C47 121.5(6) . . ?
C40 C41 C42 123.9(6) . . ?
C37 C42 C41 118.8(5) . . ?
C37 C42 C51 121.4(5) . . ?
C41 C42 C51 119.8(5) . . ?
C38 C43 C44 113.0(5) . . ?
C38 C43 C45 110.8(4) . . ?
C38 C43 C46 110.4(5) . . ?
C44 C43 C45 106.8(5) . . ?
C44 C43 C46 107.0(5) . . ?
C45 C43 C46 108.7(5) . . ?
C40 C47 C48 112.8(7) . . ?
C40 C47 C49 106.4(6) . . ?
C40 C47 C50 113.5(6) . . ?
C48 C47 C49 102.3(9) . . ?
C48 C47 C50 120.2(8) . . ?
C49 C47 C50 98.7(7) . . ?
N3 C51 C42 128.0(5) . . ?
N3 C52 C53 116.4(4) . . ?
N3 C52 C57 109.3(4) . . ?
C53 C52 C57 111.7(4) . . ?
C52 C53 C54 109.9(5) . . ?
C53 C54 C55 112.2(5) . . ?
C54 C55 C56 110.9(5) . . ?
C55 C56 C57 111.8(5) . . ?
N4 C57 C52 107.4(4) . . ?
N4 C57 C56 117.7(4) . . ?
C52 C57 C56 112.8(4) . . ?
N4 C58 C59 126.4(5) . . ?
C58 C59 C60 118.0(5) . . ?
C58 C59 C64 123.4(5) . . ?
C60 C59 C64 118.4(5) . . ?
C59 C60 C61 121.3(5) . . ?
C60 C61 C62 118.0(5) . . ?
C60 C61 C65 121.5(5) . . ?
C62 C61 C65 120.5(5) . . ?
C61 C62 C63 124.9(5) . . ?
C62 C63 C64 115.3(5) . . ?
C62 C63 C69 123.8(5) . . ?
C64 C63 C69 120.9(5) . . ?
O4 C64 C59 119.2(5) . . ?
O4 C64 C63 118.6(5) . . ?
C59 C64 C63 122.2(5) . . ?
C61 C65 C66 112.0(5) . . ?
C61 C65 C67 111.6(5) . . ?
C61 C65 C68 107.7(5) . . ?
C66 C65 C67 113.0(6) . . ?
C66 C65 C68 107.6(5) . . ?
C67 C65 C68 104.5(6) . . ?
C63 C69 C70 112.5(5) . . ?
C63 C69 C71 110.2(4) . . ?
C63 C69 C72 110.1(4) . . ?
C70 C69 C71 108.0(5) . . ?
C70 C69 C72 106.5(5) . . ?
C71 C69 C72 109.4(5) . . ?
O5 C73 C74 119.7(5) . . ?
O5 C73 C78 119.9(5) . . ?
C74 C73 C78 120.4(5) . . ?
C73 C74 C75 116.4(5) . . ?
C73 C74 C79 120.0(5) . . ?
C75 C74 C79 123.5(5) . . ?
C74 C75 C76 124.6(5) . . ?
C75 C76 C77 117.3(5) . . ?
C75 C76 C83 119.4(5) . . ?
C77 C76 C83 123.4(5) . . ?
C76 C77 C78 121.4(5) . . ?
C73 C78 C77 119.4(5) . . ?
C73 C78 C87 123.2(5) . . ?
C77 C78 C87 117.3(5) . . ?
C74 C79 C80 111.1(4) . . ?
C74 C79 C81 112.2(4) . . ?
C74 C79 C82 108.9(4) . . ?
C80 C79 C81 106.5(4) . . ?
C80 C79 C82 107.4(4) . . ?
C81 C79 C82 110.6(5) . . ?
C76 C83 C84 109.7(5) . . ?
C76 C83 C85 109.1(5) . . ?
C76 C83 C86 110.6(5) . . ?
C84 C83 C85 108.2(5) . . ?
C84 C83 C86 108.3(5) . . ?
C85 C83 C86 111.0(6) . . ?
N5 C87 C78 126.2(5) . . ?
N5 C88 C89 116.5(4) . . ?
N5 C88 C93 107.2(4) . . ?
C89 C88 C93 111.7(4) . . ?
C88 C89 C90 110.7(4) . . ?
C89 C90 C91 110.7(5) . . ?
C90 C91 C92 111.7(5) . . ?
C91 C92 C93 109.8(4) . . ?
N6 C93 C88 106.0(4) . . ?
N6 C93 C92 117.5(4) . . ?
C88 C93 C92 112.1(4) . . ?
N6 C94 C95 127.2(5) . . ?
C94 C95 C96 119.2(5) . . ?
C94 C95 C100 122.0(5) . . ?
C96 C95 C100 118.3(5) . . ?
C95 C96 C97 122.5(5) . . ?
C96 C97 C98 116.6(5) . . ?
C96 C97 C101 124.5(6) . . ?
C98 C97 C101 118.8(6) . . ?
C97 C98 C99 124.7(5) . . ?
C98 C99 C100 116.6(5) . . ?
C98 C99 C105 122.4(5) . . ?
C100 C99 C105 120.9(5) . . ?
O6 C100 C95 119.7(5) . . ?
O6 C100 C99 119.4(5) . . ?
C95 C100 C99 120.8(5) . . ?
C97 C101 C102 110.7(5) . . ?
C97 C101 C103 109.6(5) . . ?
C97 C101 C104 110.9(5) . . ?
C102 C101 C103 107.7(5) . . ?
C102 C101 C104 107.3(5) . . ?
C103 C101 C104 110.6(5) . . ?
C99 C105 C106 109.8(5) . . ?
C99 C105 C107 111.2(5) . . ?
C99 C105 C108 111.9(5) . . ?
C106 C105 C107 109.5(5) . . ?
C106 C105 C108 107.9(5) . . ?
C107 C105 C108 106.4(5) . . ?
O13 C109 C110 109.2(10) . . ?
O17 C111 C112 110.9(13) . . ?
O18 C113 C114 117.9(9) . . ?
O18 C113 C118 119.0(8) . . ?
C114 C113 C118 123.0(8) . . ?
C113 C114 C115 115.2(8) . . ?
C113 C114 C119 123.6(9) . . ?
C115 C114 C119 120.8(9) . . ?
C114 C115 C116 125.4(9) . . ?
C115 C116 C117 114.8(9) . . ?
C115 C116 C123 122.3(9) . . ?
C117 C116 C123 122.7(9) . . ?
C116 C117 C118 121.9(8) . . ?
C113 C118 C117 119.5(8) . . ?
C113 C118 C127 122.0(9) . . ?
C117 C118 C127 118.4(9) . . ?
C114 C119 C120 113.1(9) . . ?
C114 C119 C121 105.4(9) . . ?
C114 C119 C122 110.6(8) . . ?
C120 C119 C121 108.7(9) . . ?
C120 C119 C122 110.8(10) . . ?
C121 C119 C122 108.0(10) . . ?
C116 C123 C124 103.2(13) . . ?
C116 C123 C125 107.4(14) . . ?
C116 C123 C126 110.4(15) . . ?
C116 C123 C24A 110.7(11) . . ?
C116 C123 C25A 113.9(11) . . ?
C116 C123 C26A 108.3(9) . . ?
C124 C123 C125 110(2) . . ?
C124 C123 C126 108(2) . . ?
C125 C123 C126 118(3) . . ?
C24A C123 C25A 106.9(16) . . ?
C24A C123 C26A 108.6(15) . . ?
C25A C123 C26A 108.3(15) . . ?
O19 C127 C118 123.0(10) . . ?
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 1.880(4) . ?
Ti1 O2 1.847(4) . ?
Ti1 O9 1.751(4) . ?
Ti1 O10 2.201(4) . ?
Ti1 N1 2.139(5) . ?
Ti1 N2 2.139(4) . ?
Ti2 O3 1.837(4) . ?
Ti2 O4 1.827(4) . ?
Ti2 O8 1.963(3) . ?
Ti2 O9 1.953(3) . ?
Ti2 N3 2.131(4) . ?
Ti2 N4 2.126(4) . ?
Ti3 O5 1.867(3) . ?
Ti3 O6 1.895(3) . ?
Ti3 O7 2.218(4) . ?
Ti3 O8 1.742(3) . ?
Ti3 N5 2.157(4) . ?
Ti3 N6 2.132(4) . ?
S1 O10 1.468(4) . ?
S1 O11 1.435(5) . ?
S1 O12 1.399(5) . ?
S1 O13 1.577(5) . ?
S2 O14 1.433(5) . ?
S2 O15 1.453(5) . ?
S2 O16 1.427(5) . ?
S2 O17 1.570(5) . ?
O1 C1 1.354(7) . ?
O2 C28 1.333(7) . ?
O3 C37 1.323(6) . ?
O4 C64 1.348(6) . ?
O5 C73 1.341(6) . ?
O6 C100 1.327(6) . ?
O13 C109 1.416(10) . ?
O17 C111 1.452(12) . ?
O18 C113 1.395(10) . ?
O19 C127 1.287(10) . ?
N1 C15 1.280(7) . ?
N1 C16 1.454(7) . ?
N2 C21 1.481(7) . ?
N2 C22 1.286(7) . ?
N3 C51 1.281(7) . ?
N3 C52 1.485(7) . ?
N4 C57 1.480(7) . ?
N4 C58 1.299(7) . ?
N5 C87 1.295(6) . ?
N5 C88 1.466(6) . ?
N6 C93 1.470(7) . ?
N6 C94 1.316(6) . ?
C1 C2 1.429(9) . ?
C1 C6 1.402(9) . ?
C2 C3 1.407(10) . ?
C2 C7 1.531(10) . ?
C3 C4 1.371(11) . ?
C4 C5 1.338(10) . ?
C4 C11 1.569(11) . ?
C5 C6 1.427(9) . ?
C6 C15 1.435(9) . ?
C7 C8 1.527(10) . ?
C7 C9 1.524(10) . ?
C7 C10 1.564(10) . ?
C11 C12 1.489(16) . ?
C11 C13 1.490(16) . ?
C11 C14 1.540(15) . ?
C16 C17 1.527(8) . ?
C16 C21 1.564(7) . ?
C17 C18 1.508(9) . ?
C18 C19 1.501(8) . ?
C19 C20 1.517(8) . ?
C20 C21 1.480(8) . ?
C22 C23 1.435(8) . ?
C23 C24 1.427(7) . ?
C23 C28 1.460(8) . ?
C24 C25 1.380(8) . ?
C25 C26 1.440(9) . ?
C25 C29 1.513(8) . ?
C26 C27 1.354(8) . ?
C27 C28 1.399(8) . ?
C27 C33 1.527(8) . ?
C29 C30 1.535(9) . ?
C29 C31 1.511(9) . ?
C29 C32 1.547(9) . ?
C33 C34 1.558(9) . ?
C33 C35 1.529(9) . ?
C33 C36 1.518(9) . ?
C37 C38 1.429(8) . ?
C37 C42 1.405(8) . ?
C38 C39 1.384(8) . ?
C38 C43 1.522(8) . ?
C39 C40 1.425(8) . ?
C40 C41 1.375(8) . ?
C40 C47 1.524(9) . ?
C41 C42 1.386(8) . ?
C42 C51 1.449(8) . ?
C43 C44 1.536(8) . ?
C43 C45 1.535(8) . ?
C43 C46 1.565(8) . ?
C47 C48 1.390(11) . ?
C47 C49 1.651(11) . ?
C47 C50 1.414(9) . ?
C52 C53 1.550(7) . ?
C52 C57 1.511(7) . ?
C53 C54 1.520(8) . ?
C54 C55 1.509(8) . ?
C55 C56 1.528(7) . ?
C56 C57 1.490(7) . ?
C58 C59 1.447(7) . ?
C59 C60 1.406(7) . ?
C59 C64 1.402(7) . ?
C60 C61 1.389(7) . ?
C61 C62 1.369(7) . ?
C61 C65 1.527(8) . ?
C62 C63 1.400(8) . ?
C63 C64 1.415(7) . ?
C63 C69 1.537(8) . ?
C65 C66 1.494(9) . ?
C65 C67 1.490(9) . ?
C65 C68 1.592(9) . ?
C69 C70 1.520(8) . ?
C69 C71 1.529(8) . ?
C69 C72 1.543(8) . ?
C73 C74 1.422(7) . ?
C73 C78 1.403(7) . ?
C74 C75 1.392(7) . ?
C74 C79 1.556(8) . ?
C75 C76 1.386(8) . ?
C76 C77 1.385(8) . ?
C76 C83 1.554(8) . ?
C77 C78 1.402(7) . ?
C78 C87 1.442(7) . ?
C79 C80 1.532(7) . ?
C79 C81 1.518(7) . ?
C79 C82 1.522(8) . ?
C83 C84 1.572(9) . ?
C83 C85 1.554(9) . ?
C83 C86 1.489(9) . ?
C88 C89 1.529(7) . ?
C88 C93 1.521(7) . ?
C89 C90 1.510(8) . ?
C90 C91 1.495(8) . ?
C91 C92 1.509(8) . ?
C92 C93 1.514(7) . ?
C94 C95 1.400(7) . ?
C95 C96 1.415(7) . ?
C95 C100 1.421(7) . ?
C96 C97 1.387(8) . ?
C97 C98 1.406(8) . ?
C97 C101 1.534(8) . ?
C98 C99 1.395(7) . ?
C99 C100 1.425(8) . ?
C99 C105 1.521(8) . ?
C101 C102 1.566(9) . ?
C101 C103 1.541(8) . ?
C101 C104 1.536(8) . ?
C105 C106 1.546(8) . ?
C105 C107 1.515(8) . ?
C105 C108 1.549(8) . ?
C109 C110 1.507(14) . ?
C111 C112 1.433(17) . ?
C113 C114 1.399(11) . ?
C113 C118 1.389(11) . ?
C114 C115 1.374(12) . ?
C114 C119 1.530(12) . ?
C115 C116 1.447(12) . ?
C116 C117 1.401(11) . ?
C116 C123 1.520(12) . ?
C117 C118 1.384(11) . ?
C118 C127 1.433(12) . ?
C119 C120 1.533(13) . ?
C119 C121 1.586(13) . ?
C119 C122 1.508(13) . ?
C123 C124 1.65(3) . ?
C123 C125 1.40(3) . ?
C123 C126 1.36(3) . ?
C123 C24A 1.42(2) . ?
C123 C25A 1.52(2) . ?
C123 C26A 1.66(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O11 0.882(19) 1.82(2) 2.684(6) 167(5) 5
O7 H7B O19 0.834(19) 2.02(3) 2.828(7) 162(6) .
O18 H18 O19 0.84 1.81 2.564(8) 148 .
