#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321045.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_4321045
loop_
_publ_author_name
'Claire J. Carmalt'
'Christopher W. Dinnage'
'Ivan P. Parkin'
'Jonathan W. Steed'
_publ_section_title
;
 Synthesis and Characterization of a Homoleptic Thiolate Complex of
 Titanium(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2693
_journal_page_last               2695
_journal_paper_doi               10.1021/ic991382g
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C68 H75 S9 Ti2'
_chemical_formula_weight         1276.62
_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                 97.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.573(4)
_cell_length_b                   17.224(3)
_cell_length_c                   17.577(4)
_cell_measurement_temperature    100(2)
_cell_volume                     6478(2)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    RES2INS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            55504
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2684
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.00030(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         14854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0541P)²+6.1078P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                10677
_reflns_number_total             14854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991382g.cif
_cod_data_source_block           time42
_cod_original_cell_volume        6479(2)
_cod_database_code               4321045
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 0.25844(2) 0.03573(3) 0.43254(3) 0.01446(11) Uiso 1 1 d . . .
S1 S 0.17084(3) -0.03793(4) 0.48704(4) 0.01627(15) Uiso 1 1 d . . .
C1 C 0.12836(13) -0.10522(18) 0.41706(17) 0.0237(6) Uani 1 1 d . . .
H1A H 0.1185 -0.0783 0.3672 0.028 Uiso 1 1 calc R . .
H1B H 0.1557 -0.1500 0.4092 0.028 Uiso 1 1 calc R . .
Ti2 Ti 0.25635(2) -0.10542(3) 0.57267(3) 0.01572(12) Uiso 1 1 d . . .
S2 S 0.29339(3) 0.03373(4) 0.57604(4) 0.01540(14) Uiso 1 1 d . . .
C2 C 0.06855(13) -0.13459(17) 0.44278(17) 0.0213(6) Uani 1 1 d . . .
S3 S 0.31375(3) -0.09359(4) 0.45633(4) 0.01578(15) Uiso 1 1 d . . .
C3 C 0.06556(14) -0.20943(18) 0.47286(19) 0.0264(7) Uani 1 1 d . . .
H3 H 0.1019 -0.2411 0.4794 0.032 Uiso 1 1 calc R . .
S4 S 0.18876(3) 0.13947(4) 0.42892(4) 0.01728(15) Uiso 1 1 d . . .
C4 C 0.00962(14) -0.23772(18) 0.4933(2) 0.0290(7) Uani 1 1 d . . .
H4 H 0.0079 -0.2889 0.5131 0.035 Uiso 1 1 calc R . .
S5 S 0.34469(3) 0.10213(4) 0.39976(4) 0.01990(16) Uiso 1 1 d . . .
C5 C -0.04349(14) -0.19208(19) 0.48513(18) 0.0263(7) Uani 1 1 d . . .
H5 H -0.0817 -0.2120 0.4985 0.032 Uiso 1 1 calc R . .
S6 S 0.23262(3) -0.01181(4) 0.30670(4) 0.01852(15) Uiso 1 1 d . . .
C6 C -0.04065(14) -0.11714(19) 0.45721(18) 0.0266(7) Uani 1 1 d . . .
H6 H -0.0767 -0.0850 0.4528 0.032 Uiso 1 1 calc R . .
S7 S 0.19852(3) -0.09807(4) 0.67619(4) 0.01967(16) Uiso 1 1 d . . .
C7 C 0.01514(14) -0.08861(18) 0.43553(18) 0.0260(7) Uani 1 1 d . . .
H7 H 0.0166 -0.0374 0.4157 0.031 Uiso 1 1 calc R . .
S8 S 0.23727(3) -0.24000(4) 0.54050(4) 0.02097(16) Uiso 1 1 d . . .
C8 C 0.24167(13) 0.09053(16) 0.63132(16) 0.0179(6) Uani 1 1 d . . .
H8A H 0.1995 0.0935 0.6018 0.022 Uiso 1 1 calc R . .
H8B H 0.2378 0.0633 0.6801 0.022 Uiso 1 1 calc R . .
S9 S 0.34062(3) -0.14380(4) 0.66268(4) 0.02247(16) Uiso 1 1 d . . .
C9 C 0.26565(13) 0.17136(16) 0.64863(16) 0.0176(6) Uani 1 1 d . . .
C10 C 0.31293(14) 0.18451(18) 0.70936(18) 0.0254(7) Uani 1 1 d . . .
H10 H 0.3316 0.1419 0.7380 0.030 Uiso 1 1 calc R . .
C11 C 0.33266(15) 0.25944(19) 0.7280(2) 0.0326(8) Uani 1 1 d . . .
H11 H 0.3647 0.2680 0.7694 0.039 Uiso 1 1 calc R . .
C12 C 0.30575(15) 0.32201(19) 0.6864(2) 0.0343(8) Uani 1 1 d . . .
H12 H 0.3194 0.3733 0.6993 0.041 Uiso 1 1 calc R . .
C13 C 0.25911(16) 0.30966(18) 0.6262(2) 0.0323(8) Uani 1 1 d . . .
H13 H 0.2409 0.3524 0.5973 0.039 Uiso 1 1 calc R . .
C14 C 0.23870(15) 0.23416(17) 0.60792(18) 0.0257(7) Uani 1 1 d . . .
H14 H 0.2060 0.2259 0.5672 0.031 Uiso 1 1 calc R . .
C15 C 0.39781(13) -0.07771(18) 0.48928(17) 0.0220(6) Uani 1 1 d . . .
H15A H 0.4056 -0.0215 0.4972 0.026 Uiso 1 1 calc R . .
H15B H 0.4091 -0.1042 0.5391 0.026 Uiso 1 1 calc R . .
C16 C 0.43837(13) -0.10791(17) 0.43229(17) 0.0204(6) Uani 1 1 d . . .
C17 C 0.47289(15) -0.0588(2) 0.3925(2) 0.0369(8) Uani 1 1 d . . .
H17 H 0.4696 -0.0042 0.3988 0.044 Uiso 1 1 calc R . .
C18 C 0.51272(18) -0.0884(2) 0.3428(2) 0.0477(11) Uani 1 1 d . . .
H18 H 0.5367 -0.0537 0.3163 0.057 Uiso 1 1 calc R . .
C19 C 0.51763(15) -0.1664(2) 0.3320(2) 0.0366(8) Uani 1 1 d . . .
H19 H 0.5448 -0.1861 0.2981 0.044 Uiso 1 1 calc R . .
C20 C 0.48303(15) -0.2163(2) 0.3706(2) 0.0337(8) Uani 1 1 d . . .
H20 H 0.4857 -0.2707 0.3628 0.040 Uiso 1 1 calc R . .
C21 C 0.44415(15) -0.18756(19) 0.4211(2) 0.0295(7) Uani 1 1 d . . .
H21 H 0.4211 -0.2226 0.4484 0.035 Uiso 1 1 calc R . .
C22 C 0.22462(14) 0.22807(17) 0.3947(2) 0.0265(7) Uani 1 1 d . . .
H22A H 0.2519 0.2522 0.4378 0.032 Uiso 1 1 calc R . .
H22B H 0.2509 0.2140 0.3546 0.032 Uiso 1 1 calc R . .
C23 C 0.17576(13) 0.28548(16) 0.36256(18) 0.0221(6) Uani 1 1 d . . .
C24 C 0.14785(15) 0.33474(19) 0.4103(2) 0.0313(7) Uani 1 1 d . . .
H24 H 0.1599 0.3323 0.4641 0.038 Uiso 1 1 calc R . .
C25 C 0.10304(18) 0.3872(2) 0.3811(3) 0.0466(10) Uani 1 1 d . . .
H25 H 0.0849 0.4211 0.4147 0.056 Uiso 1 1 calc R . .
C26 C 0.08438(18) 0.3907(2) 0.3031(3) 0.0486(11) Uani 1 1 d . . .
H26 H 0.0524 0.4257 0.2831 0.058 Uiso 1 1 calc R . .
C27 C 0.11250(18) 0.3432(2) 0.2545(2) 0.0418(9) Uani 1 1 d . . .
H27 H 0.1007 0.3464 0.2007 0.050 Uiso 1 1 calc R . .
C28 C 0.15827(15) 0.29020(19) 0.28411(19) 0.0302(7) Uani 1 1 d . . .
H28 H 0.1774 0.2574 0.2505 0.036 Uiso 1 1 calc R . .
C29 C 0.38124(14) 0.16442(18) 0.47798(17) 0.0249(7) Uani 1 1 d . . .
H29A H 0.3489 0.1853 0.5076 0.030 Uiso 1 1 calc R . .
H29B H 0.4113 0.1338 0.5132 0.030 Uiso 1 1 calc R . .
C30 C 0.41474(13) 0.23038(17) 0.44374(17) 0.0213(6) Uani 1 1 d . . .
C31 C 0.39248(15) 0.30564(19) 0.44372(19) 0.0289(7) Uani 1 1 d . . .
H31 H 0.3563 0.3168 0.4674 0.035 Uiso 1 1 calc R . .
C32 C 0.42268(16) 0.3653(2) 0.4093(2) 0.0357(8) Uani 1 1 d . . .
H32 H 0.4067 0.4167 0.4093 0.043 Uiso 1 1 calc R . .
C33 C 0.47550(17) 0.3502(2) 0.3753(2) 0.0353(8) Uani 1 1 d . . .
H33 H 0.4963 0.3911 0.3526 0.042 Uiso 1 1 calc R . .
C34 C 0.49811(15) 0.2752(2) 0.3744(2) 0.0354(8) Uani 1 1 d . . .
H34 H 0.5345 0.2644 0.3509 0.042 Uiso 1 1 calc R . .
C35 C 0.46777(14) 0.21603(19) 0.40772(19) 0.0282(7) Uani 1 1 d . . .
H35 H 0.4833 0.1645 0.4061 0.034 Uiso 1 1 calc R . .
C36 C 0.17784(15) 0.05576(17) 0.25215(17) 0.0252(7) Uani 1 1 d . . .
H36A H 0.1447 0.0705 0.2836 0.030 Uiso 1 1 calc R . .
H36B H 0.2004 0.1035 0.2407 0.030 Uiso 1 1 calc R . .
C37 C 0.14840(14) 0.01968(17) 0.17832(17) 0.0229(6) Uani 1 1 d . . .
C38 C 0.08418(16) 0.0120(2) 0.1640(2) 0.0377(8) Uani 1 1 d . . .
H38 H 0.0587 0.0285 0.2013 0.045 Uiso 1 1 calc R . .
C39 C 0.05685(17) -0.0199(3) 0.0952(2) 0.0520(11) Uani 1 1 d . . .
H39 H 0.0126 -0.0240 0.0854 0.062 Uiso 1 1 calc R . .
C40 C 0.09311(18) -0.0457(2) 0.0412(2) 0.0442(9) Uani 1 1 d . . .
H40 H 0.0740 -0.0681 -0.0054 0.053 Uiso 1 1 calc R . .
C41 C 0.15689(16) -0.03876(19) 0.05501(18) 0.0305(7) Uani 1 1 d . . .
H41 H 0.1822 -0.0566 0.0181 0.037 Uiso 1 1 calc R . .
C42 C 0.18436(15) -0.00578(17) 0.12281(17) 0.0239(6) Uani 1 1 d . . .
H42 H 0.2285 -0.0004 0.1316 0.029 Uiso 1 1 calc R . .
C43 C 0.12123(14) -0.05150(17) 0.66348(19) 0.0250(7) Uani 1 1 d . . .
H43A H 0.1251 0.0027 0.6823 0.030 Uiso 1 1 calc R . .
H43B H 0.1049 -0.0502 0.6083 0.030 Uiso 1 1 calc R . .
C44 C 0.07625(13) -0.09522(16) 0.70681(17) 0.0202(6) Uani 1 1 d . . .
C45 C 0.08681(14) -0.10388(17) 0.78619(18) 0.0243(6) Uani 1 1 d . . .
H45 H 0.1221 -0.0798 0.8144 0.029 Uiso 1 1 calc R . .
C46 C 0.04659(15) -0.14697(19) 0.82435(18) 0.0284(7) Uani 1 1 d . . .
H46 H 0.0547 -0.1530 0.8784 0.034 Uiso 1 1 calc R . .
C47 C -0.00561(16) -0.1814(2) 0.7841(2) 0.0348(8) Uani 1 1 d . . .
H47 H -0.0330 -0.2117 0.8103 0.042 Uiso 1 1 calc R . .
C48 C -0.01747(16) -0.1715(2) 0.7060(2) 0.0379(8) Uani 1 1 d . . .
H48 H -0.0537 -0.1940 0.6782 0.045 Uiso 1 1 calc R . .
C49 C 0.02328(15) -0.12856(19) 0.66744(19) 0.0290(7) Uani 1 1 d . . .
H49 H 0.0147 -0.1220 0.6135 0.035 Uiso 1 1 calc R . .
C50 C 0.30186(15) -0.28144(18) 0.4938(2) 0.0304(7) Uani 1 1 d . . .
H50A H 0.3061 -0.2515 0.4466 0.036 Uiso 1 1 calc R . .
H50B H 0.3414 -0.2759 0.5287 0.036 Uiso 1 1 calc R . .
C51 C 0.29207(14) -0.36538(17) 0.47329(19) 0.0255(7) Uani 1 1 d . . .
C52 C 0.25566(15) -0.38745(18) 0.40605(19) 0.0272(7) Uani 1 1 d . . .
H52 H 0.2356 -0.3486 0.3733 0.033 Uiso 1 1 calc R . .
C53 C 0.24781(15) -0.46535(19) 0.38533(19) 0.0300(7) Uani 1 1 d . . .
H53 H 0.2232 -0.4793 0.3386 0.036 Uiso 1 1 calc R . .
C54 C 0.27615(15) -0.52206(19) 0.4335(2) 0.0323(8) Uani 1 1 d . . .
H54 H 0.2707 -0.5753 0.4202 0.039 Uiso 1 1 calc R . .
C55 C 0.31235(15) -0.50141(18) 0.5008(2) 0.0313(7) Uani 1 1 d . . .
H55 H 0.3316 -0.5404 0.5340 0.038 Uiso 1 1 calc R . .
C56 C 0.32068(15) -0.42384(19) 0.52010(19) 0.0297(7) Uani 1 1 d . . .
H56 H 0.3464 -0.4102 0.5661 0.036 Uiso 1 1 calc R . .
C57 C 0.36043(14) -0.06566(19) 0.73180(18) 0.0265(7) Uani 1 1 d . . .
H57A H 0.3614 -0.0159 0.7037 0.032 Uiso 1 1 calc R . .
H57B H 0.3272 -0.0618 0.7657 0.032 Uiso 1 1 calc R . .
C58 C 0.42250(14) -0.07715(17) 0.78064(18) 0.0235(6) Uani 1 1 d . . .
C59 C 0.47639(15) -0.0891(2) 0.7463(2) 0.0380(9) Uani 1 1 d . . .
H59 H 0.4734 -0.0949 0.6922 0.046 Uiso 1 1 calc R . .
C60 C 0.53401(17) -0.0926(2) 0.7898(3) 0.0580(13) Uani 1 1 d . . .
H60 H 0.5706 -0.0994 0.7656 0.070 Uiso 1 1 calc R . .
C61 C 0.5387(2) -0.0862(3) 0.8680(3) 0.0664(15) Uani 1 1 d . . .
H61 H 0.5786 -0.0886 0.8978 0.080 Uiso 1 1 calc R . .
C62 C 0.4853(2) -0.0763(2) 0.9042(3) 0.0581(13) Uani 1 1 d . . .
H62 H 0.4887 -0.0724 0.9584 0.070 Uiso 1 1 calc R . .
C63 C 0.42680(17) -0.07197(19) 0.8596(2) 0.0347(8) Uani 1 1 d . . .
H63 H 0.3901 -0.0655 0.8837 0.042 Uiso 1 1 calc R . .
C3S C 0.23948(19) -0.17971(17) 0.21535(18) 0.0352(9) Uani 1 1 d . . .
H3S1 H 0.2421 -0.2051 0.1653 0.042 Uiso 1 1 calc R . .
H3S2 H 0.2321 -0.1237 0.2055 0.042 Uiso 1 1 calc R . .
C4S C 0.1840(4) -0.2129(2) 0.2491(3) 0.082(2) Uani 1 1 d . . .
H4S1 H 0.1908 -0.2691 0.2589 0.098 Uiso 1 1 calc R . .
H4S2 H 0.1804 -0.1873 0.2987 0.098 Uiso 1 1 calc R . .
C1S C 0.3502(2) -0.1494(3) 0.2283(3) 0.0788(19) Uani 1 1 d . . .
H1S1 H 0.3541 -0.1730 0.1784 0.118 Uiso 1 1 calc R . .
H1S2 H 0.3899 -0.1548 0.2619 0.118 Uiso 1 1 calc R . .
H1S3 H 0.3400 -0.0942 0.2213 0.118 Uiso 1 1 calc R . .
C2S C 0.2998(3) -0.1890(3) 0.2638(2) 0.0793(19) Uani 1 1 d . . .
H2S1 H 0.3097 -0.2450 0.2701 0.095 Uiso 1 1 calc R . .
H2S2 H 0.2971 -0.1667 0.3151 0.095 Uiso 1 1 calc R . .
C5S C 0.1252(3) -0.2019(3) 0.1970(4) 0.0804(19) Uani 1 1 d . . .
H5S1 H 0.1184 -0.1464 0.1870 0.121 Uiso 1 1 calc R . .
H5S2 H 0.0902 -0.2230 0.2209 0.121 Uiso 1 1 calc R . .
H5S3 H 0.1281 -0.2289 0.1485 0.121 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'
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
S5 Ti1 S4 98.64(3) . . ?
S5 Ti1 S6 92.27(4) . . ?
S4 Ti1 S6 99.54(4) . . ?
S5 Ti1 S3 95.66(3) . . ?
S4 Ti1 S3 165.02(3) . . ?
S6 Ti1 S3 84.26(3) . . ?
S5 Ti1 S2 96.14(4) . . ?
S4 Ti1 S2 98.44(3) . . ?
S6 Ti1 S2 158.75(3) . . ?
S3 Ti1 S2 75.53(3) . . ?
S5 Ti1 S1 172.34(3) . . ?
S4 Ti1 S1 83.45(3) . . ?
S6 Ti1 S1 94.65(3) . . ?
S3 Ti1 S1 81.79(3) . . ?
S2 Ti1 S1 76.23(3) . . ?
C1 S1 Ti2 111.91(11) . . ?
C1 S1 Ti1 112.91(10) . . ?
Ti2 S1 Ti1 86.14(3) . . ?
C2 C1 S1 112.5(2) . . ?
S7 Ti2 S9 86.26(3) . . ?
S7 Ti2 S8 98.20(3) . . ?
S9 Ti2 S8 88.96(3) . . ?
S7 Ti2 S1 91.00(3) . . ?
S9 Ti2 S1 168.63(3) . . ?
S8 Ti2 S1 102.35(3) . . ?
S7 Ti2 S2 97.41(3) . . ?
S9 Ti2 S2 92.05(3) . . ?
S8 Ti2 S2 164.39(3) . . ?
S1 Ti2 S2 77.35(3) . . ?
S7 Ti2 S3 171.75(3) . . ?
S9 Ti2 S3 98.68(3) . . ?
S8 Ti2 S3 88.53(3) . . ?
S1 Ti2 S3 82.87(3) . . ?
S2 Ti2 S3 75.91(3) . . ?
C8 S2 Ti2 107.71(9) . . ?
C8 S2 Ti1 113.06(10) . . ?
Ti2 S2 Ti1 86.35(3) . . ?
C7 C2 C3 118.8(3) . . ?
C7 C2 C1 120.8(3) . . ?
C3 C2 C1 120.3(3) . . ?
C15 S3 Ti2 108.62(10) . . ?
C15 S3 Ti1 110.07(10) . . ?
Ti2 S3 Ti1 86.32(3) . . ?
C4 C3 C2 120.3(3) . . ?
C22 S4 Ti1 110.32(10) . . ?
C5 C4 C3 120.6(3) . . ?
C29 S5 Ti1 112.52(10) . . ?
C4 C5 C6 119.6(3) . . ?
C36 S6 Ti1 109.21(10) . . ?
C5 C6 C7 120.2(3) . . ?
C43 S7 Ti2 119.64(10) . . ?
C2 C7 C6 120.5(3) . . ?
C50 S8 Ti2 111.09(10) . . ?
C9 C8 S2 112.41(18) . . ?
C57 S9 Ti2 109.66(10) . . ?
C14 C9 C10 119.1(3) . . ?
C14 C9 C8 120.5(3) . . ?
C10 C9 C8 120.2(3) . . ?
C11 C10 C9 120.3(3) . . ?
C10 C11 C12 120.2(3) . . ?
C13 C12 C11 120.0(3) . . ?
C12 C13 C14 119.8(3) . . ?
C9 C14 C13 120.6(3) . . ?
C16 C15 S3 111.7(2) . . ?
C17 C16 C21 118.0(3) . . ?
C17 C16 C15 121.6(3) . . ?
C21 C16 C15 120.3(3) . . ?
C16 C17 C18 120.6(3) . . ?
C19 C18 C17 120.8(3) . . ?
C18 C19 C20 119.5(3) . . ?
C19 C20 C21 120.2(3) . . ?
C20 C21 C16 121.0(3) . . ?
C23 C22 S4 111.3(2) . . ?
C24 C23 C28 118.9(3) . . ?
C24 C23 C22 120.9(3) . . ?
C28 C23 C22 120.2(3) . . ?
C25 C24 C23 121.1(3) . . ?
C24 C25 C26 120.2(4) . . ?
C27 C26 C25 119.6(3) . . ?
C26 C27 C28 120.2(4) . . ?
C23 C28 C27 120.0(3) . . ?
C30 C29 S5 108.8(2) . . ?
C31 C30 C35 118.0(3) . . ?
C31 C30 C29 121.4(3) . . ?
C35 C30 C29 120.5(3) . . ?
C30 C31 C32 120.7(3) . . ?
C33 C32 C31 120.4(3) . . ?
C32 C33 C34 119.7(3) . . ?
C33 C34 C35 119.9(3) . . ?
C34 C35 C30 121.4(3) . . ?
C37 C36 S6 111.2(2) . . ?
C38 C37 C42 118.5(3) . . ?
C38 C37 C36 120.0(3) . . ?
C42 C37 C36 121.5(3) . . ?
C37 C38 C39 120.0(3) . . ?
C40 C39 C38 120.8(3) . . ?
C41 C40 C39 119.6(3) . . ?
C40 C41 C42 119.9(3) . . ?
C41 C42 C37 121.1(3) . . ?
C44 C43 S7 110.6(2) . . ?
C49 C44 C45 118.4(3) . . ?
C49 C44 C43 119.9(3) . . ?
C45 C44 C43 121.7(3) . . ?
C46 C45 C44 120.8(3) . . ?
C45 C46 C47 120.2(3) . . ?
C48 C47 C46 119.5(3) . . ?
C47 C48 C49 120.3(3) . . ?
C44 C49 C48 120.7(3) . . ?
C51 C50 S8 112.8(2) . . ?
C52 C51 C56 117.8(3) . . ?
C52 C51 C50 121.1(3) . . ?
C56 C51 C50 121.1(3) . . ?
C51 C52 C53 121.5(3) . . ?
C54 C53 C52 119.3(3) . . ?
C55 C54 C53 120.1(3) . . ?
C54 C55 C56 120.0(3) . . ?
C55 C56 C51 121.2(3) . . ?
C58 C57 S9 113.4(2) . . ?
C63 C58 C59 119.4(3) . . ?
C63 C58 C57 120.3(3) . . ?
C59 C58 C57 120.2(3) . . ?
C60 C59 C58 120.8(4) . . ?
C61 C60 C59 120.0(4) . . ?
C60 C61 C62 120.5(4) . . ?
C61 C62 C63 119.3(4) . . ?
C58 C63 C62 119.9(4) . . ?
C2S C3S C4S 114.7(4) . . ?
C5S C4S C3S 111.5(4) . . ?
C3S C2S C1S 110.4(4) . . ?
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 S5 2.3183(9) . ?
Ti1 S4 2.3308(9) . ?
Ti1 S6 2.3582(10) . ?
Ti1 S3 2.5364(9) . ?
Ti1 S2 2.5395(10) . ?
Ti1 S1 2.5609(9) . ?
S1 C1 1.847(3) . ?
S1 Ti2 2.5132(10) . ?
C1 C2 1.508(4) . ?
Ti2 S7 2.3366(11) . ?
Ti2 S9 2.3484(11) . ?
Ti2 S8 2.4090(10) . ?
Ti2 S2 2.5249(9) . ?
Ti2 S3 2.5295(10) . ?
S2 C8 1.850(3) . ?
C2 C7 1.391(4) . ?
C2 C3 1.398(4) . ?
S3 C15 1.853(3) . ?
C3 C4 1.391(4) . ?
S4 C22 1.846(3) . ?
C4 C5 1.382(4) . ?
S5 C29 1.841(3) . ?
C5 C6 1.385(5) . ?
S6 C36 1.839(3) . ?
C6 C7 1.397(4) . ?
S7 C43 1.838(3) . ?
S8 C50 1.848(3) . ?
C8 C9 1.503(4) . ?
S9 C57 1.827(3) . ?
C9 C14 1.384(4) . ?
C9 C10 1.398(4) . ?
C10 C11 1.385(4) . ?
C11 C12 1.388(5) . ?
C12 C13 1.381(5) . ?
C13 C14 1.397(4) . ?
C15 C16 1.504(4) . ?
C16 C17 1.376(4) . ?
C16 C21 1.394(4) . ?
C17 C18 1.396(5) . ?
C18 C19 1.364(5) . ?
C19 C20 1.373(5) . ?
C20 C21 1.387(4) . ?
C22 C23 1.503(4) . ?
C23 C24 1.383(4) . ?
C23 C28 1.385(5) . ?
C24 C25 1.374(5) . ?
C25 C26 1.380(6) . ?
C26 C27 1.379(6) . ?
C27 C28 1.395(5) . ?
C29 C30 1.512(4) . ?
C30 C31 1.382(4) . ?
C30 C35 1.398(4) . ?
C31 C32 1.396(5) . ?
C32 C33 1.377(5) . ?
C33 C34 1.381(5) . ?
C34 C35 1.381(5) . ?
C36 C37 1.505(4) . ?
C37 C38 1.383(4) . ?
C37 C42 1.392(4) . ?
C38 C39 1.390(5) . ?
C39 C40 1.379(5) . ?
C40 C41 1.372(5) . ?
C41 C42 1.384(4) . ?
C43 C44 1.509(4) . ?
C44 C49 1.383(4) . ?
C44 C45 1.393(4) . ?
C45 C46 1.379(4) . ?
C46 C47 1.385(5) . ?
C47 C48 1.376(5) . ?
C48 C49 1.389(5) . ?
C50 C51 1.499(4) . ?
C51 C52 1.387(5) . ?
C51 C56 1.394(4) . ?
C52 C53 1.395(4) . ?
C53 C54 1.383(5) . ?
C54 C55 1.379(5) . ?
C55 C56 1.384(5) . ?
C57 C58 1.509(4) . ?
C58 C63 1.383(5) . ?
C58 C59 1.391(4) . ?
C59 C60 1.375(5) . ?
C60 C61 1.370(7) . ?
C61 C62 1.394(7) . ?
C62 C63 1.401(5) . ?
C3S C2S 1.470(6) . ?
C3S C4S 1.513(7) . ?
C4S C5S 1.479(8) . ?
C1S C2S 1.486(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S5 Ti1 S1 C1 -148.3(3) . . . . ?
S4 Ti1 S1 C1 105.43(12) . . . . ?
S6 Ti1 S1 C1 6.33(12) . . . . ?
S3 Ti1 S1 C1 -77.17(12) . . . . ?
S2 Ti1 S1 C1 -154.19(11) . . . . ?
S5 Ti1 S1 Ti2 -36.1(2) . . . . ?
S4 Ti1 S1 Ti2 -142.39(3) . . . . ?
S6 Ti1 S1 Ti2 118.52(3) . . . . ?
S3 Ti1 S1 Ti2 35.02(3) . . . . ?
S2 Ti1 S1 Ti2 -42.01(3) . . . . ?
Ti2 S1 C1 C2 97.6(2) . . . . ?
Ti1 S1 C1 C2 -167.14(19) . . . . ?
C1 S1 Ti2 S7 -107.40(10) . . . . ?
Ti1 S1 Ti2 S7 139.44(3) . . . . ?
C1 S1 Ti2 S9 176.76(18) . . . . ?
Ti1 S1 Ti2 S9 63.59(17) . . . . ?
C1 S1 Ti2 S8 -8.77(10) . . . . ?
Ti1 S1 Ti2 S8 -121.94(3) . . . . ?
C1 S1 Ti2 S2 155.24(10) . . . . ?
Ti1 S1 Ti2 S2 42.07(2) . . . . ?
C1 S1 Ti2 S3 78.14(10) . . . . ?
Ti1 S1 Ti2 S3 -35.02(3) . . . . ?
S7 Ti2 S2 C8 -18.80(10) . . . . ?
S9 Ti2 S2 C8 -105.29(10) . . . . ?
S8 Ti2 S2 C8 161.22(14) . . . . ?
S1 Ti2 S2 C8 70.56(10) . . . . ?
S3 Ti2 S2 C8 156.28(10) . . . . ?
S7 Ti2 S2 Ti1 -131.86(3) . . . . ?
S9 Ti2 S2 Ti1 141.65(3) . . . . ?
S8 Ti2 S2 Ti1 48.15(12) . . . . ?
S1 Ti2 S2 Ti1 -42.50(3) . . . . ?
S3 Ti2 S2 Ti1 43.22(3) . . . . ?
S5 Ti1 S2 C8 114.85(10) . . . . ?
S4 Ti1 S2 C8 15.14(10) . . . . ?
S6 Ti1 S2 C8 -132.39(12) . . . . ?
S3 Ti1 S2 C8 -150.87(10) . . . . ?
S1 Ti1 S2 C8 -65.95(10) . . . . ?
S5 Ti1 S2 Ti2 -137.45(3) . . . . ?
S4 Ti1 S2 Ti2 122.84(3) . . . . ?
S6 Ti1 S2 Ti2 -24.69(9) . . . . ?
S3 Ti1 S2 Ti2 -43.16(3) . . . . ?
S1 Ti1 S2 Ti2 41.76(2) . . . . ?
S1 C1 C2 C7 78.6(3) . . . . ?
S1 C1 C2 C3 -102.8(3) . . . . ?
S7 Ti2 S3 C15 103.1(2) . . . . ?
S9 Ti2 S3 C15 -23.28(11) . . . . ?
S8 Ti2 S3 C15 -112.01(10) . . . . ?
S1 Ti2 S3 C15 145.35(11) . . . . ?
S2 Ti2 S3 C15 66.66(10) . . . . ?
S7 Ti2 S3 Ti1 -6.9(2) . . . . ?
S9 Ti2 S3 Ti1 -133.23(3) . . . . ?
S8 Ti2 S3 Ti1 138.04(3) . . . . ?
S1 Ti2 S3 Ti1 35.40(2) . . . . ?
S2 Ti2 S3 Ti1 -43.29(3) . . . . ?
S5 Ti1 S3 C15 29.48(11) . . . . ?
S4 Ti1 S3 C15 -133.21(15) . . . . ?
S6 Ti1 S3 C15 121.21(11) . . . . ?
S2 Ti1 S3 C15 -65.42(11) . . . . ?
S1 Ti1 S3 C15 -143.24(10) . . . . ?
S5 Ti1 S3 Ti2 137.97(3) . . . . ?
S4 Ti1 S3 Ti2 -24.72(13) . . . . ?
S6 Ti1 S3 Ti2 -130.31(3) . . . . ?
S2 Ti1 S3 Ti2 43.07(3) . . . . ?
S1 Ti1 S3 Ti2 -34.75(3) . . . . ?
C7 C2 C3 C4 1.5(5) . . . . ?
C1 C2 C3 C4 -177.1(3) . . . . ?
S5 Ti1 S4 C22 4.86(12) . . . . ?
S6 Ti1 S4 C22 -88.94(12) . . . . ?
S3 Ti1 S4 C22 167.42(16) . . . . ?
S2 Ti1 S4 C22 102.44(12) . . . . ?
S1 Ti1 S4 C22 177.42(12) . . . . ?
C2 C3 C4 C5 -0.8(5) . . . . ?
S4 Ti1 S5 C29 72.78(12) . . . . ?
S6 Ti1 S5 C29 172.79(11) . . . . ?
S3 Ti1 S5 C29 -102.76(11) . . . . ?
S2 Ti1 S5 C29 -26.75(11) . . . . ?
S1 Ti1 S5 C29 -32.5(3) . . . . ?
C3 C4 C5 C6 -0.9(5) . . . . ?
S5 Ti1 S6 C36 -91.70(12) . . . . ?
S4 Ti1 S6 C36 7.45(12) . . . . ?
S3 Ti1 S6 C36 172.83(11) . . . . ?
S2 Ti1 S6 C36 154.87(13) . . . . ?
S1 Ti1 S6 C36 91.58(12) . . . . ?
C4 C5 C6 C7 1.7(5) . . . . ?
S9 Ti2 S7 C43 168.46(12) . . . . ?
S8 Ti2 S7 C43 -103.13(12) . . . . ?
S1 Ti2 S7 C43 -0.50(12) . . . . ?
S2 Ti2 S7 C43 76.88(12) . . . . ?
S3 Ti2 S7 C43 41.4(3) . . . . ?
C3 C2 C7 C6 -0.7(5) . . . . ?
C1 C2 C7 C6 177.9(3) . . . . ?
C5 C6 C7 C2 -1.0(5) . . . . ?
S7 Ti2 S8 C50 -152.99(13) . . . . ?
S9 Ti2 S8 C50 -66.92(13) . . . . ?
S1 Ti2 S8 C50 114.17(13) . . . . ?
S2 Ti2 S8 C50 27.00(18) . . . . ?
S3 Ti2 S8 C50 31.79(13) . . . . ?
Ti2 S2 C8 C9 170.27(18) . . . . ?
Ti1 S2 C8 C9 -96.1(2) . . . . ?
S7 Ti2 S9 C57 -62.58(11) . . . . ?
S8 Ti2 S9 C57 -160.87(11) . . . . ?
S1 Ti2 S9 C57 13.7(2) . . . . ?
S2 Ti2 S9 C57 34.72(12) . . . . ?
S3 Ti2 S9 C57 110.78(11) . . . . ?
S2 C8 C9 C14 103.8(3) . . . . ?
S2 C8 C9 C10 -80.2(3) . . . . ?
C14 C9 C10 C11 -0.4(4) . . . . ?
C8 C9 C10 C11 -176.4(3) . . . . ?
C9 C10 C11 C12 -0.2(5) . . . . ?
C10 C11 C12 C13 0.1(5) . . . . ?
C11 C12 C13 C14 0.7(5) . . . . ?
C10 C9 C14 C13 1.1(5) . . . . ?
C8 C9 C14 C13 177.2(3) . . . . ?
C12 C13 C14 C9 -1.3(5) . . . . ?
Ti2 S3 C15 C16 152.12(18) . . . . ?
Ti1 S3 C15 C16 -115.0(2) . . . . ?
S3 C15 C16 C17 113.0(3) . . . . ?
S3 C15 C16 C21 -70.0(3) . . . . ?
C21 C16 C17 C18 -0.4(5) . . . . ?
C15 C16 C17 C18 176.6(3) . . . . ?
C16 C17 C18 C19 0.9(6) . . . . ?
C17 C18 C19 C20 -0.1(6) . . . . ?
C18 C19 C20 C21 -1.0(5) . . . . ?
C19 C20 C21 C16 1.4(5) . . . . ?
C17 C16 C21 C20 -0.7(5) . . . . ?
C15 C16 C21 C20 -177.8(3) . . . . ?
Ti1 S4 C22 C23 157.6(2) . . . . ?
S4 C22 C23 C24 82.1(3) . . . . ?
S4 C22 C23 C28 -98.4(3) . . . . ?
C28 C23 C24 C25 0.6(5) . . . . ?
C22 C23 C24 C25 -179.8(3) . . . . ?
C23 C24 C25 C26 1.0(6) . . . . ?
C24 C25 C26 C27 -2.2(6) . . . . ?
C25 C26 C27 C28 1.9(5) . . . . ?
C24 C23 C28 C27 -1.0(4) . . . . ?
C22 C23 C28 C27 179.5(3) . . . . ?
C26 C27 C28 C23 -0.2(5) . . . . ?
Ti1 S5 C29 C30 -153.95(17) . . . . ?
S5 C29 C30 C31 109.0(3) . . . . ?
S5 C29 C30 C35 -67.9(3) . . . . ?
C35 C30 C31 C32 -0.6(5) . . . . ?
C29 C30 C31 C32 -177.6(3) . . . . ?
C30 C31 C32 C33 -0.5(5) . . . . ?
C31 C32 C33 C34 0.9(5) . . . . ?
C32 C33 C34 C35 -0.2(5) . . . . ?
C33 C34 C35 C30 -1.0(5) . . . . ?
C31 C30 C35 C34 1.4(5) . . . . ?
C29 C30 C35 C34 178.4(3) . . . . ?
Ti1 S6 C36 C37 -166.74(19) . . . . ?
S6 C36 C37 C38 121.0(3) . . . . ?
S6 C36 C37 C42 -59.7(3) . . . . ?
C42 C37 C38 C39 -0.6(5) . . . . ?
C36 C37 C38 C39 178.7(4) . . . . ?
C37 C38 C39 C40 1.3(7) . . . . ?
C38 C39 C40 C41 -0.9(7) . . . . ?
C39 C40 C41 C42 -0.3(6) . . . . ?
C40 C41 C42 C37 1.0(5) . . . . ?
C38 C37 C42 C41 -0.6(5) . . . . ?
C36 C37 C42 C41 -179.9(3) . . . . ?
Ti2 S7 C43 C44 141.09(18) . . . . ?
S7 C43 C44 C49 -118.2(3) . . . . ?
S7 C43 C44 C45 61.2(3) . . . . ?
C49 C44 C45 C46 2.3(4) . . . . ?
C43 C44 C45 C46 -177.1(3) . . . . ?
C44 C45 C46 C47 -0.9(5) . . . . ?
C45 C46 C47 C48 -0.9(5) . . . . ?
C46 C47 C48 C49 1.4(5) . . . . ?
C45 C44 C49 C48 -1.8(5) . . . . ?
C43 C44 C49 C48 177.6(3) . . . . ?
C47 C48 C49 C44 0.0(5) . . . . ?
Ti2 S8 C50 C51 179.6(2) . . . . ?
S8 C50 C51 C52 83.2(3) . . . . ?
S8 C50 C51 C56 -98.6(3) . . . . ?
C56 C51 C52 C53 -0.2(5) . . . . ?
C50 C51 C52 C53 178.0(3) . . . . ?
C51 C52 C53 C54 1.0(5) . . . . ?
C52 C53 C54 C55 -0.8(5) . . . . ?
C53 C54 C55 C56 -0.4(5) . . . . ?
C54 C55 C56 C51 1.2(5) . . . . ?
C52 C51 C56 C55 -0.9(5) . . . . ?
C50 C51 C56 C55 -179.2(3) . . . . ?
Ti2 S9 C57 C58 -166.9(2) . . . . ?
S9 C57 C58 C63 -128.7(3) . . . . ?
S9 C57 C58 C59 54.6(4) . . . . ?
C63 C58 C59 C60 -2.7(5) . . . . ?
C57 C58 C59 C60 174.0(3) . . . . ?
C58 C59 C60 C61 1.6(6) . . . . ?
C59 C60 C61 C62 0.1(7) . . . . ?
C60 C61 C62 C63 -0.7(7) . . . . ?
C59 C58 C63 C62 2.1(5) . . . . ?
C57 C58 C63 C62 -174.7(3) . . . . ?
C61 C62 C63 C58 -0.4(6) . . . . ?
C2S C3S C4S C5S -179.6(3) . . . . ?
C4S C3S C2S C1S -175.7(3) . . . . ?
