#------------------------------------------------------------------------------
#$Date: 2024-12-06 22:19:49 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296637 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/34/7063458.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_7063458
loop_
_publ_author_name
'Schwitalla, Kevin'
'Claußen, Marie'
'Schmidtmann, Marc'
'Beckhaus, Rüdiger'
_publ_section_title
;
 Syntheses and coordination chemistry of thiosemicarbazone-based titanium
 complexes
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18066
_journal_page_last               18074
_journal_paper_doi               10.1039/D4NJ04061A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_structural     Ti(C15H18)(C15H19)(C9H9N3HS)
_chemical_formula_sum            'C39 H47 N3 S Ti'
_chemical_formula_weight         637.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-08-15 deposited with the CCDC.	2024-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                92.218(3)
_cell_angle_beta                 107.971(3)
_cell_angle_gamma                109.627(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6805(6)
_cell_length_b                   12.0032(6)
_cell_length_c                   12.9169(7)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.25
_cell_measurement_theta_min      2.27
_cell_volume                     1601.95(15)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         40.248
_diffrn_reflns_theta_min         1.679
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9319
_exptl_absorpt_correction_T_min  0.8918
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         20177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0400P)²+0.3000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17407
_reflns_number_total             20177
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj04061a2.cif
_cod_data_source_block           Ti1a
_cod_depositor_comments
'Adding full bibliography for 7063456--7063460.cif.'
_cod_database_code               7063458
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.868
_shelx_estimated_absorpt_t_max   0.914
_exptl_absorpt_special_details
;
 numerical absorption correction followed by scaling based on
 symmetry-related measurements (multi-scan)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.24484(2) 0.29837(2) 0.23427(2) 0.00881(2) Uani 1 1 d . . . . .
S1 S 0.33690(2) 0.25765(2) 0.08518(2) 0.01074(2) Uani 1 1 d . . . . .
N1 N 0.20847(5) 0.11085(4) 0.18171(4) 0.01137(7) Uani 1 1 d . . . . .
N2 N 0.13682(5) -0.00264(4) 0.19418(4) 0.01234(7) Uani 1 1 d . . . . .
N3 N 0.24997(5) 0.01497(4) 0.04243(4) 0.01388(8) Uani 1 1 d . . . . .
H3 H 0.2129(11) -0.0525(10) 0.0601(10) 0.024(3) Uiso 1 1 d . . . . .
C1 C 0.13525(5) 0.40594(5) 0.14413(5) 0.01183(8) Uani 1 1 d . . . . .
C2 C 0.10487(5) 0.39000(5) 0.24431(5) 0.01375(8) Uani 1 1 d . . . . .
H2 H 0.129415 0.451771 0.303971 0.017 Uiso 1 1 calc R U . . .
C3 C 0.03238(6) 0.26696(6) 0.23895(5) 0.01603(9) Uani 1 1 d . . . . .
H3A H 0.002562 0.231979 0.294987 0.019 Uiso 1 1 calc R U . . .
C4 C 0.01258(5) 0.20612(5) 0.13587(5) 0.01590(9) Uani 1 1 d . . . . .
H4 H -0.035115 0.123058 0.109914 0.019 Uiso 1 1 calc R U . . .
C5 C 0.07479(5) 0.28807(5) 0.07741(5) 0.01368(8) Uani 1 1 d . . . . .
H5 H 0.076814 0.269252 0.006033 0.016 Uiso 1 1 calc R U . . .
C6 C 0.24472(5) 0.49801(5) 0.13769(4) 0.01135(8) Uani 1 1 d . . . . .
C7 C 0.27687(6) 0.50833(5) 0.03273(5) 0.01302(8) Uani 1 1 d . . . . .
H7 H 0.247551 0.426936 -0.010632 0.016 Uiso 1 1 calc R U . . .
C8 C 0.42371(6) 0.57245(5) 0.06139(5) 0.01541(9) Uani 1 1 d . . . . .
H8A H 0.469518 0.524255 0.104503 0.018 Uiso 1 1 calc R U . . .
H8B H 0.444467 0.580120 -0.007356 0.018 Uiso 1 1 calc R U . . .
C9 C 0.46995(6) 0.69717(5) 0.12845(5) 0.01452(9) Uani 1 1 d . . . . .
H9 H 0.565283 0.737812 0.146001 0.017 Uiso 1 1 calc R U . . .
C10 C 0.43963(6) 0.68476(5) 0.23583(5) 0.01435(9) Uani 1 1 d . . . . .
H10A H 0.467966 0.765072 0.279020 0.017 Uiso 1 1 calc R U . . .
H10B H 0.486914 0.638729 0.280838 0.017 Uiso 1 1 calc R U . . .
C11 C 0.29339(6) 0.61983(5) 0.20816(5) 0.01269(8) Uani 1 1 d . . . . .
H11 H 0.272901 0.610229 0.277719 0.015 Uiso 1 1 calc R U . . .
C12 C 0.20738(6) 0.58462(5) -0.03538(5) 0.01625(9) Uani 1 1 d . . . . .
H12A H 0.227344 0.593003 -0.104450 0.020 Uiso 1 1 calc R U . . .
H12B H 0.112637 0.544486 -0.055046 0.020 Uiso 1 1 calc R U . . .
C13 C 0.39893(6) 0.77157(5) 0.06040(5) 0.01537(9) Uani 1 1 d . . . . .
H13A H 0.428297 0.852411 0.102950 0.018 Uiso 1 1 calc R U . . .
H13B H 0.419185 0.780696 -0.008496 0.018 Uiso 1 1 calc R U . . .
C14 C 0.22181(6) 0.69499(5) 0.13974(5) 0.01577(9) Uani 1 1 d . . . . .
H14A H 0.127390 0.654758 0.122114 0.019 Uiso 1 1 calc R U . . .
H14B H 0.249381 0.774972 0.183260 0.019 Uiso 1 1 calc R U . . .
C15 C 0.25268(6) 0.70891(5) 0.03266(5) 0.01521(9) Uani 1 1 d . . . . .
H15 H 0.206881 0.757895 -0.010919 0.018 Uiso 1 1 calc R U . . .
C16 C 0.44556(5) 0.28673(5) 0.36167(4) 0.01125(8) Uani 1 1 d . . . . .
C17 C 0.34785(6) 0.24493(5) 0.41040(5) 0.01375(8) Uani 1 1 d . . . . .
H17 H 0.315281 0.166319 0.426652 0.016 Uiso 1 1 calc R U . . .
C18 C 0.30749(6) 0.33948(6) 0.43050(5) 0.01543(9) Uani 1 1 d . . . . .
H18 H 0.244152 0.335948 0.463306 0.019 Uiso 1 1 calc R U . . .
C19 C 0.37801(6) 0.44043(5) 0.39319(5) 0.01382(8) Uani 1 1 d . . . . .
H19 H 0.369970 0.516567 0.395964 0.017 Uiso 1 1 calc R U . . .
C20 C 0.46258(5) 0.40804(5) 0.35103(5) 0.01193(8) Uani 1 1 d . . . . .
H20 H 0.521232 0.459073 0.320566 0.014 Uiso 1 1 calc R U . . .
C21 C 0.51857(6) 0.21581(5) 0.33070(5) 0.01319(8) Uani 1 1 d . . . . .
H21 H 0.461059 0.163520 0.258490 0.016 Uiso 1 1 calc R U . . .
C22 C 0.64448(6) 0.29515(6) 0.31422(5) 0.01723(10) Uani 1 1 d . . . . .
H22 H 0.625112 0.350942 0.261820 0.021 Uiso 1 1 calc R U . . .
C23 C 0.69838(8) 0.21353(8) 0.26556(6) 0.02545(15) Uani 1 1 d . . . . .
H23A H 0.633841 0.166389 0.194336 0.031 Uiso 1 1 calc R U . . .
H23B H 0.777649 0.262944 0.251908 0.031 Uiso 1 1 calc R U . . .
C24 C 0.72982(8) 0.12851(8) 0.34615(6) 0.02633(15) Uani 1 1 d . . . . .
H24 H 0.764903 0.075550 0.314302 0.032 Uiso 1 1 calc R U . . .
C25 C 0.60582(9) 0.05145(7) 0.36543(6) 0.02628(15) Uani 1 1 d . . . . .
H25A H 0.625045 -0.004203 0.416795 0.032 Uiso 1 1 calc R U . . .
H25B H 0.540939 0.003224 0.294763 0.032 Uiso 1 1 calc R U . . .
C26 C 0.55097(7) 0.13239(6) 0.41415(5) 0.01779(10) Uani 1 1 d . . . . .
H26 H 0.470470 0.081697 0.426865 0.021 Uiso 1 1 calc R U . . .
C27 C 0.74587(6) 0.36825(7) 0.42451(7) 0.02274(12) Uani 1 1 d . . . . .
H27A H 0.712386 0.421872 0.456029 0.027 Uiso 1 1 calc R U . . .
H27B H 0.825839 0.418427 0.412327 0.027 Uiso 1 1 calc R U . . .
C28 C 0.83046(8) 0.20169(9) 0.45633(6) 0.02987(17) Uani 1 1 d . . . . .
H28A H 0.910940 0.251280 0.444583 0.036 Uiso 1 1 calc R U . . .
H28B H 0.851348 0.147014 0.508207 0.036 Uiso 1 1 calc R U . . .
C29 C 0.65154(8) 0.20600(7) 0.52376(5) 0.02145(12) Uani 1 1 d . . . . .
H29A H 0.670498 0.151643 0.576669 0.026 Uiso 1 1 calc R U . . .
H29B H 0.616873 0.258446 0.555361 0.026 Uiso 1 1 calc R U . . .
C30 C 0.77623(7) 0.28273(8) 0.50525(6) 0.02428(13) Uani 1 1 d . . . . .
H30 H 0.841667 0.330346 0.577103 0.029 Uiso 1 1 calc R U . . .
C31 C 0.25957(5) 0.11373(4) 0.10207(4) 0.01030(7) Uani 1 1 d . . . . .
C32 C 0.30225(7) 0.01758(5) -0.04608(6) 0.01831(10) Uani 1 1 d . . . . .
H32A H 0.280947 0.075394 -0.092580 0.027 Uiso 1 1 calc R U . . .
H32B H 0.264729 -0.062223 -0.090629 0.027 Uiso 1 1 calc R U . . .
H32C H 0.396411 0.041316 -0.014854 0.027 Uiso 1 1 calc R U . . .
C33 C 0.07728(6) -0.00402(5) 0.26358(5) 0.01329(8) Uani 1 1 d . . . . .
H33 H 0.091491 0.069983 0.304153 0.016 Uiso 1 1 calc R U . . .
C34 C -0.01101(5) -0.11412(5) 0.28270(5) 0.01285(8) Uani 1 1 d . . . . .
C35 C -0.02141(6) -0.22856(5) 0.24307(5) 0.01716(10) Uani 1 1 d . . . . .
H35 H 0.032077 -0.237196 0.203292 0.021 Uiso 1 1 calc R U . . .
C36 C -0.10980(8) -0.32955(6) 0.26179(6) 0.02358(13) Uani 1 1 d . . . . .
H36 H -0.115630 -0.407012 0.235596 0.028 Uiso 1 1 calc R U . . .
C37 C -0.19001(7) -0.31797(7) 0.31879(7) 0.02569(14) Uani 1 1 d . . . . .
H37 H -0.251179 -0.387350 0.330390 0.031 Uiso 1 1 calc R U . . .
C38 C -0.18029(7) -0.20477(7) 0.35857(7) 0.02481(13) Uani 1 1 d . . . . .
H38 H -0.235014 -0.196573 0.397206 0.030 Uiso 1 1 calc R U . . .
C39 C -0.09023(7) -0.10338(6) 0.34172(6) 0.01872(10) Uani 1 1 d . . . . .
H39 H -0.082400 -0.026111 0.370535 0.022 Uiso 1 1 calc R U . . .
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'
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
N1 Ti1 C1 125.75(2) . . ?
N1 Ti1 C2 130.36(2) . . ?
C1 Ti1 C2 37.36(2) . . ?
N1 Ti1 C5 88.68(2) . . ?
C1 Ti1 C5 37.07(2) . . ?
C2 Ti1 C5 59.97(2) . . ?
N1 Ti1 C19 135.433(19) . . ?
C1 Ti1 C19 98.54(2) . . ?
C2 Ti1 C19 81.03(2) . . ?
C5 Ti1 C19 135.36(2) . . ?
N1 Ti1 C20 113.261(19) . . ?
C1 Ti1 C20 116.26(2) . . ?
C2 Ti1 C20 113.11(2) . . ?
C5 Ti1 C20 147.14(2) . . ?
C19 Ti1 C20 34.69(2) . . ?
N1 Ti1 C18 110.15(2) . . ?
C1 Ti1 C18 114.34(2) . . ?
C2 Ti1 C18 81.44(2) . . ?
C5 Ti1 C18 139.56(2) . . ?
C19 Ti1 C18 34.69(2) . . ?
C20 Ti1 C18 57.13(2) . . ?
N1 Ti1 C3 96.40(2) . . ?
C1 Ti1 C3 60.38(2) . . ?
C2 Ti1 C3 35.17(2) . . ?
C5 Ti1 C3 58.03(2) . . ?
C19 Ti1 C3 102.20(2) . . ?
C20 Ti1 C3 136.63(2) . . ?
C18 Ti1 C3 83.83(2) . . ?
N1 Ti1 C4 74.49(2) . . ?
C1 Ti1 C4 59.48(2) . . ?
C2 Ti1 C4 57.77(2) . . ?
C5 Ti1 C4 34.28(2) . . ?
C19 Ti1 C4 135.49(2) . . ?
C20 Ti1 C4 170.17(2) . . ?
C18 Ti1 C4 115.28(2) . . ?
C3 Ti1 C4 33.79(2) . . ?
N1 Ti1 C17 79.883(19) . . ?
C1 Ti1 C17 148.11(2) . . ?
C2 Ti1 C17 112.83(2) . . ?
C5 Ti1 C17 156.05(2) . . ?
C19 Ti1 C17 56.85(2) . . ?
C20 Ti1 C17 56.314(19) . . ?
C18 Ti1 C17 33.89(2) . . ?
C3 Ti1 C17 102.14(2) . . ?
C4 Ti1 C17 121.78(2) . . ?
N1 Ti1 C16 81.452(18) . . ?
C1 Ti1 C16 150.220(19) . . ?
C2 Ti1 C16 135.91(2) . . ?
C5 Ti1 C16 163.67(2) . . ?
C19 Ti1 C16 57.122(19) . . ?
C20 Ti1 C16 33.968(18) . . ?
C18 Ti1 C16 56.667(19) . . ?
C3 Ti1 C16 135.78(2) . . ?
C4 Ti1 C16 149.698(19) . . ?
C17 Ti1 C16 33.760(19) . . ?
N1 Ti1 S1 63.823(13) . . ?
C1 Ti1 S1 97.409(16) . . ?
C2 Ti1 S1 134.567(16) . . ?
C5 Ti1 S1 80.501(16) . . ?
C19 Ti1 S1 120.370(16) . . ?
C20 Ti1 S1 87.523(15) . . ?
C18 Ti1 S1 139.802(15) . . ?
C3 Ti1 S1 135.120(17) . . ?
C4 Ti1 S1 101.644(17) . . ?
C17 Ti1 S1 112.248(15) . . ?
C16 Ti1 S1 83.472(14) . . ?
C31 S1 Ti1 79.540(18) . . ?
C31 N1 N2 114.93(4) . . ?
C31 N1 Ti1 104.39(3) . . ?
N2 N1 Ti1 139.81(4) . . ?
C33 N2 N1 114.45(5) . . ?
C31 N3 C32 123.52(5) . . ?
C31 N3 H3 117.0(8) . . ?
C32 N3 H3 119.4(8) . . ?
C6 C1 C2 123.79(5) . . ?
C6 C1 C5 124.96(5) . . ?
C2 C1 C5 105.37(5) . . ?
C6 C1 Ti1 95.26(3) . . ?
C2 C1 Ti1 73.47(3) . . ?
C5 C1 Ti1 75.01(3) . . ?
C3 C2 C1 108.93(5) . . ?
C3 C2 Ti1 76.87(3) . . ?
C1 C2 Ti1 69.17(3) . . ?
C3 C2 H2 125.5 . . ?
C1 C2 H2 125.5 . . ?
Ti1 C2 H2 120.1 . . ?
C4 C3 C2 107.86(5) . . ?
C4 C3 Ti1 74.53(3) . . ?
C2 C3 Ti1 67.96(3) . . ?
C4 C3 H3A 126.1 . . ?
C2 C3 H3A 126.1 . . ?
Ti1 C3 H3A 123.0 . . ?
C3 C4 C5 109.08(5) . . ?
C3 C4 Ti1 71.68(3) . . ?
C5 C4 Ti1 68.37(3) . . ?
C3 C4 H4 125.5 . . ?
C5 C4 H4 125.5 . . ?
Ti1 C4 H4 126.1 . . ?
C4 C5 C1 108.73(5) . . ?
C4 C5 Ti1 77.34(3) . . ?
C1 C5 Ti1 67.92(3) . . ?
C4 C5 H5 125.6 . . ?
C1 C5 H5 125.6 . . ?
Ti1 C5 H5 120.7 . . ?
C1 C6 C7 122.31(5) . . ?
C1 C6 C11 119.34(5) . . ?
C7 C6 C11 111.50(4) . . ?
C6 C7 C8 109.61(5) . . ?
C6 C7 C12 108.28(5) . . ?
C8 C7 C12 108.60(5) . . ?
C6 C7 H7 110.1 . . ?
C8 C7 H7 110.1 . . ?
C12 C7 H7 110.1 . . ?
C9 C8 C7 110.59(5) . . ?
C9 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C8 C9 C10 109.37(5) . . ?
C8 C9 C13 109.10(5) . . ?
C10 C9 C13 109.48(5) . . ?
C8 C9 H9 109.6 . . ?
C10 C9 H9 109.6 . . ?
C13 C9 H9 109.6 . . ?
C9 C10 C11 109.29(5) . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
C6 C11 C10 111.57(5) . . ?
C6 C11 C14 106.92(5) . . ?
C10 C11 C14 108.78(5) . . ?
C6 C11 H11 109.8 . . ?
C10 C11 H11 109.8 . . ?
C14 C11 H11 109.8 . . ?
C15 C12 C7 109.44(5) . . ?
C15 C12 H12A 109.8 . . ?
C7 C12 H12A 109.8 . . ?
C15 C12 H12B 109.8 . . ?
C7 C12 H12B 109.8 . . ?
H12A C12 H12B 108.2 . . ?
C15 C13 C9 109.70(5) . . ?
C15 C13 H13A 109.7 . . ?
C9 C13 H13A 109.7 . . ?
C15 C13 H13B 109.7 . . ?
C9 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C15 C14 C11 109.75(5) . . ?
C15 C14 H14A 109.7 . . ?
C11 C14 H14A 109.7 . . ?
C15 C14 H14B 109.7 . . ?
C11 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C13 C15 C14 109.52(5) . . ?
C13 C15 C12 109.43(5) . . ?
C14 C15 C12 109.42(5) . . ?
C13 C15 H15 109.5 . . ?
C14 C15 H15 109.5 . . ?
C12 C15 H15 109.5 . . ?
C20 C16 C17 106.57(5) . . ?
C20 C16 C21 127.17(5) . . ?
C17 C16 C21 126.24(5) . . ?
C20 C16 Ti1 70.03(3) . . ?
C17 C16 Ti1 72.31(3) . . ?
C21 C16 Ti1 123.91(4) . . ?
C18 C17 C16 108.79(5) . . ?
C18 C17 Ti1 70.98(3) . . ?
C16 C17 Ti1 73.93(3) . . ?
C18 C17 H17 125.6 . . ?
C16 C17 H17 125.6 . . ?
Ti1 C17 H17 121.2 . . ?
C17 C18 C19 107.89(5) . . ?
C17 C18 Ti1 75.12(3) . . ?
C19 C18 Ti1 71.01(3) . . ?
C17 C18 H18 126.1 . . ?
C19 C18 H18 126.1 . . ?
Ti1 C18 H18 119.6 . . ?
C20 C19 C18 107.90(5) . . ?
C20 C19 Ti1 74.19(3) . . ?
C18 C19 Ti1 74.30(3) . . ?
C20 C19 H19 126.0 . . ?
C18 C19 H19 126.1 . . ?
Ti1 C19 H19 117.5 . . ?
C19 C20 C16 108.85(5) . . ?
C19 C20 Ti1 71.11(3) . . ?
C16 C20 Ti1 76.00(3) . . ?
C19 C20 H20 125.6 . . ?
C16 C20 H20 125.6 . . ?
Ti1 C20 H20 119.1 . . ?
C16 C21 C22 113.27(5) . . ?
C16 C21 C26 113.23(5) . . ?
C22 C21 C26 108.68(5) . . ?
C16 C21 H21 107.1 . . ?
C22 C21 H21 107.1 . . ?
C26 C21 H21 107.1 . . ?
C23 C22 C27 109.19(5) . . ?
C23 C22 C21 108.45(6) . . ?
C27 C22 C21 110.92(5) . . ?
C23 C22 H22 109.4 . . ?
C27 C22 H22 109.4 . . ?
C21 C22 H22 109.4 . . ?
C24 C23 C22 109.74(5) . . ?
C24 C23 H23A 109.7 . . ?
C22 C23 H23A 109.7 . . ?
C24 C23 H23B 109.7 . . ?
C22 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
C25 C24 C28 109.34(6) . . ?
C25 C24 C23 109.14(6) . . ?
C28 C24 C23 109.67(8) . . ?
C25 C24 H24 109.6 . . ?
C28 C24 H24 109.6 . . ?
C23 C24 H24 109.6 . . ?
C24 C25 C26 109.88(6) . . ?
C24 C25 H25A 109.7 . . ?
C26 C25 H25A 109.7 . . ?
C24 C25 H25B 109.7 . . ?
C26 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
C29 C26 C25 109.34(6) . . ?
C29 C26 C21 110.52(5) . . ?
C25 C26 C21 108.41(5) . . ?
C29 C26 H26 109.5 . . ?
C25 C26 H26 109.5 . . ?
C21 C26 H26 109.5 . . ?
C22 C27 C30 109.59(6) . . ?
C22 C27 H27A 109.8 . . ?
C30 C27 H27A 109.8 . . ?
C22 C27 H27B 109.8 . . ?
C30 C27 H27B 109.8 . . ?
H27A C27 H27B 108.2 . . ?
C24 C28 C30 109.47(6) . . ?
C24 C28 H28A 109.8 . . ?
C30 C28 H28A 109.8 . . ?
C24 C28 H28B 109.8 . . ?
C30 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
C26 C29 C30 109.86(5) . . ?
C26 C29 H29A 109.7 . . ?
C30 C29 H29A 109.7 . . ?
C26 C29 H29B 109.7 . . ?
C30 C29 H29B 109.7 . . ?
H29A C29 H29B 108.2 . . ?
C29 C30 C28 109.87(7) . . ?
C29 C30 C27 109.16(5) . . ?
C28 C30 C27 109.21(6) . . ?
C29 C30 H30 109.5 . . ?
C28 C30 H30 109.5 . . ?
C27 C30 H30 109.5 . . ?
N1 C31 N3 123.32(5) . . ?
N1 C31 S1 112.09(4) . . ?
N3 C31 S1 124.60(4) . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N2 C33 C34 123.09(5) . . ?
N2 C33 H33 118.5 . . ?
C34 C33 H33 118.5 . . ?
C35 C34 C39 119.02(5) . . ?
C35 C34 C33 123.11(5) . . ?
C39 C34 C33 117.86(5) . . ?
C36 C35 C34 120.12(6) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C37 120.43(7) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C38 C37 C36 119.86(6) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C39 119.86(7) . . ?
C37 C38 H38 120.1 . . ?
C39 C38 H38 120.1 . . ?
C38 C39 C34 120.67(6) . . ?
C38 C39 H39 119.7 . . ?
C34 C39 H39 119.7 . . ?
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 N1 2.1839(5) . ?
Ti1 C1 2.2289(5) . ?
Ti1 C2 2.2862(6) . ?
Ti1 C5 2.3234(6) . ?
Ti1 C19 2.3490(6) . ?
Ti1 C20 2.3888(5) . ?
Ti1 C18 2.3916(6) . ?
Ti1 C3 2.4021(6) . ?
Ti1 C4 2.4386(6) . ?
Ti1 C17 2.4449(6) . ?
Ti1 C16 2.4660(5) . ?
Ti1 S1 2.58107(19) . ?
S1 C31 1.7175(5) . ?
N1 C31 1.3354(7) . ?
N1 N2 1.3843(6) . ?
N2 C33 1.2906(7) . ?
N3 C31 1.3409(7) . ?
N3 C32 1.4497(8) . ?
N3 H3 0.858(12) . ?
C1 C6 1.4094(8) . ?
C1 C2 1.4470(8) . ?
C1 C5 1.4498(8) . ?
C2 C3 1.4208(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.4074(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.4078(8) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.5135(8) . ?
C6 C11 1.5196(8) . ?
C7 C8 1.5396(9) . ?
C7 C12 1.5467(8) . ?
C7 H7 1.0000 . ?
C8 C9 1.5332(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.5346(9) . ?
C9 C13 1.5385(8) . ?
C9 H9 1.0000 . ?
C10 C11 1.5364(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C14 1.5513(8) . ?
C11 H11 1.0000 . ?
C12 C15 1.5360(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C15 1.5331(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.5350(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15 1.0000 . ?
C16 C20 1.4200(7) . ?
C16 C17 1.4261(8) . ?
C16 C21 1.5112(8) . ?
C17 C18 1.4106(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.4138(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.4132(8) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.5438(9) . ?
C21 C26 1.5473(8) . ?
C21 H21 1.0000 . ?
C22 C23 1.5369(9) . ?
C22 C27 1.5382(10) . ?
C22 H22 1.0000 . ?
C23 C24 1.5356(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.5349(13) . ?
C24 C28 1.5349(12) . ?
C24 H24 1.0000 . ?
C25 C26 1.5394(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C29 1.5313(10) . ?
C26 H26 1.0000 . ?
C27 C30 1.5383(11) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C30 1.5363(11) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.5354(12) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.4621(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.3997(9) . ?
C34 C39 1.4006(8) . ?
C35 C36 1.3892(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.3944(12) . ?
C36 H36 0.9500 . ?
C37 C38 1.3891(12) . ?
C37 H37 0.9500 . ?
C38 C39 1.3917(9) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
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
C31 N1 N2 C33 -173.42(5) . . . . ?
Ti1 N1 N2 C33 -6.32(8) . . . . ?
C6 C1 C2 C3 -152.42(5) . . . . ?
C5 C1 C2 C3 1.60(6) . . . . ?
Ti1 C1 C2 C3 -67.21(4) . . . . ?
C6 C1 C2 Ti1 -85.21(5) . . . . ?
C5 C1 C2 Ti1 68.82(4) . . . . ?
C1 C2 C3 C4 -2.12(7) . . . . ?
Ti1 C2 C3 C4 -64.35(4) . . . . ?
C1 C2 C3 Ti1 62.23(4) . . . . ?
C2 C3 C4 C5 1.79(7) . . . . ?
Ti1 C3 C4 C5 -58.31(4) . . . . ?
C2 C3 C4 Ti1 60.11(4) . . . . ?
C3 C4 C5 C1 -0.79(7) . . . . ?
Ti1 C4 C5 C1 -61.13(4) . . . . ?
C3 C4 C5 Ti1 60.34(4) . . . . ?
C6 C1 C5 C4 153.13(5) . . . . ?
C2 C1 C5 C4 -0.51(6) . . . . ?
Ti1 C1 C5 C4 67.22(4) . . . . ?
C6 C1 C5 Ti1 85.91(5) . . . . ?
C2 C1 C5 Ti1 -67.73(4) . . . . ?
C2 C1 C6 C7 176.97(5) . . . . ?
C5 C1 C6 C7 27.98(8) . . . . ?
Ti1 C1 C6 C7 103.35(5) . . . . ?
C2 C1 C6 C11 -34.51(8) . . . . ?
C5 C1 C6 C11 176.51(5) . . . . ?
Ti1 C1 C6 C11 -108.12(5) . . . . ?
C1 C6 C7 C8 -153.11(5) . . . . ?
C11 C6 C7 C8 56.18(6) . . . . ?
C1 C6 C7 C12 88.58(6) . . . . ?
C11 C6 C7 C12 -62.14(6) . . . . ?
C6 C7 C8 C9 -58.43(6) . . . . ?
C12 C7 C8 C9 59.68(6) . . . . ?
C7 C8 C9 C10 60.13(6) . . . . ?
C7 C8 C9 C13 -59.60(6) . . . . ?
C8 C9 C10 C11 -58.56(6) . . . . ?
C13 C9 C10 C11 60.93(6) . . . . ?
C1 C6 C11 C10 151.79(5) . . . . ?
C7 C6 C11 C10 -56.53(6) . . . . ?
C1 C6 C11 C14 -89.39(6) . . . . ?
C7 C6 C11 C14 62.30(6) . . . . ?
C9 C10 C11 C6 57.10(6) . . . . ?
C9 C10 C11 C14 -60.61(6) . . . . ?
C6 C7 C12 C15 59.15(6) . . . . ?
C8 C7 C12 C15 -59.80(6) . . . . ?
C8 C9 C13 C15 59.52(6) . . . . ?
C10 C9 C13 C15 -60.14(6) . . . . ?
C6 C11 C14 C15 -60.50(6) . . . . ?
C10 C11 C14 C15 60.12(6) . . . . ?
C9 C13 C15 C14 59.39(6) . . . . ?
C9 C13 C15 C12 -60.55(6) . . . . ?
C11 C14 C15 C13 -59.54(6) . . . . ?
C11 C14 C15 C12 60.41(6) . . . . ?
C7 C12 C15 C13 60.77(6) . . . . ?
C7 C12 C15 C14 -59.22(6) . . . . ?
C20 C16 C17 C18 -0.82(6) . . . . ?
C21 C16 C17 C18 177.65(5) . . . . ?
Ti1 C16 C17 C18 -62.86(4) . . . . ?
C20 C16 C17 Ti1 62.04(4) . . . . ?
C21 C16 C17 Ti1 -119.48(5) . . . . ?
C16 C17 C18 C19 0.83(7) . . . . ?
Ti1 C17 C18 C19 -63.92(4) . . . . ?
C16 C17 C18 Ti1 64.76(4) . . . . ?
C17 C18 C19 C20 -0.52(7) . . . . ?
Ti1 C18 C19 C20 -67.16(4) . . . . ?
C17 C18 C19 Ti1 66.65(4) . . . . ?
C18 C19 C20 C16 0.01(6) . . . . ?
Ti1 C19 C20 C16 -67.23(4) . . . . ?
C18 C19 C20 Ti1 67.24(4) . . . . ?
C17 C16 C20 C19 0.50(6) . . . . ?
C21 C16 C20 C19 -177.96(5) . . . . ?
Ti1 C16 C20 C19 64.05(4) . . . . ?
C17 C16 C20 Ti1 -63.55(4) . . . . ?
C21 C16 C20 Ti1 118.00(5) . . . . ?
C20 C16 C21 C22 16.18(8) . . . . ?
C17 C16 C21 C22 -161.99(5) . . . . ?
Ti1 C16 C21 C22 105.80(5) . . . . ?
C20 C16 C21 C26 140.51(6) . . . . ?
C17 C16 C21 C26 -37.65(8) . . . . ?
Ti1 C16 C21 C26 -129.87(5) . . . . ?
C16 C21 C22 C23 -171.13(5) . . . . ?
C26 C21 C22 C23 62.10(6) . . . . ?
C16 C21 C22 C27 68.98(6) . . . . ?
C26 C21 C22 C27 -57.79(6) . . . . ?
C27 C22 C23 C24 59.63(9) . . . . ?
C21 C22 C23 C24 -61.34(8) . . . . ?
C22 C23 C24 C25 60.06(9) . . . . ?
C22 C23 C24 C28 -59.69(9) . . . . ?
C28 C24 C25 C26 60.09(7) . . . . ?
C23 C24 C25 C26 -59.87(8) . . . . ?
C24 C25 C26 C29 -59.72(7) . . . . ?
C24 C25 C26 C21 60.83(7) . . . . ?
C16 C21 C26 C29 -68.77(7) . . . . ?
C22 C21 C26 C29 58.02(7) . . . . ?
C16 C21 C26 C25 171.40(6) . . . . ?
C22 C21 C26 C25 -61.80(7) . . . . ?
C23 C22 C27 C30 -60.11(7) . . . . ?
C21 C22 C27 C30 59.35(7) . . . . ?
C25 C24 C28 C30 -59.77(9) . . . . ?
C23 C24 C28 C30 59.86(9) . . . . ?
C25 C26 C29 C30 59.16(7) . . . . ?
C21 C26 C29 C30 -60.10(7) . . . . ?
C26 C29 C30 C28 -59.41(7) . . . . ?
C26 C29 C30 C27 60.32(7) . . . . ?
C24 C28 C30 C29 59.55(9) . . . . ?
C24 C28 C30 C27 -60.16(9) . . . . ?
C22 C27 C30 C29 -59.68(7) . . . . ?
C22 C27 C30 C28 60.46(8) . . . . ?
N2 N1 C31 N3 -3.94(8) . . . . ?
Ti1 N1 C31 N3 -175.39(5) . . . . ?
N2 N1 C31 S1 175.60(4) . . . . ?
Ti1 N1 C31 S1 4.15(4) . . . . ?
C32 N3 C31 N1 178.28(6) . . . . ?
C32 N3 C31 S1 -1.21(9) . . . . ?
Ti1 S1 C31 N1 -3.46(4) . . . . ?
Ti1 S1 C31 N3 176.08(5) . . . . ?
N1 N2 C33 C34 175.35(5) . . . . ?
N2 C33 C34 C35 11.82(9) . . . . ?
N2 C33 C34 C39 -166.90(6) . . . . ?
C39 C34 C35 C36 0.38(10) . . . . ?
C33 C34 C35 C36 -178.32(6) . . . . ?
C34 C35 C36 C37 0.86(11) . . . . ?
C35 C36 C37 C38 -0.95(12) . . . . ?
C36 C37 C38 C39 -0.22(12) . . . . ?
C37 C38 C39 C34 1.49(12) . . . . ?
C35 C34 C39 C38 -1.56(10) . . . . ?
C33 C34 C39 C38 177.21(6) . . . . ?
