#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/90/4329056.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_4329056
loop_
_publ_author_name
'Alberto Donzelli'
'Imir Metushi'
'Pierre G. Potvin'
_publ_section_title
;
 Titanium(IV) Complexes of Disulfide-Linked Schiff Bases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5138
_journal_page_last               5145
_journal_paper_doi               10.1021/ic202709x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C84 H66 N6 O15 S6 Ti3'
_chemical_formula_sum            'C84 H66 N6 O15 S6 Ti3'
_chemical_formula_weight         1735.49
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                   21.2378(3)
_cell_length_b                   21.2378(3)
_cell_length_c                   31.7593(7)
_cell_measurement_reflns_used    28218
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.6
_cell_volume                     12405.7(4)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            74589
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             5364
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0543
_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)+(0.0959P)²+13.4816P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                3508
_reflns_number_total             4867
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic202709x_si_003.cif
_cod_data_source_block           k1004a
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4329056
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ti1 Ti 0.70188(3) 0.43730(3) 0.054248(19) 0.0401(2) Uani 1 1 d .
S2 S 0.85649(5) 0.70580(5) 0.04672(3) 0.0574(3) Uani 1 1 d .
S3 S 0.75152(6) 0.68562(6) 0.05454(3) 0.0598(3) Uani 1 1 d .
O1 O 0.70370(12) 0.44924(13) -0.00560(7) 0.0456(6) Uani 1 1 d .
O2 O 0.70732(12) 0.45717(13) 0.11318(7) 0.0466(6) Uani 1 1 d .
O3 O 0.75431(12) 0.39103(12) 0.05569(7) 0.0439(6) Uani 1 1 d .
O4 O 0.91486(17) 0.5520(2) -0.12849(9) 0.0980(12) Uani 1 1 d .
O5 O 0.5190(2) 0.4812(2) 0.22315(11) 0.1004(12) Uani 1 1 d .
N1 N 0.81224(15) 0.54065(14) 0.04900(8) 0.0416(6) Uani 1 1 d .
N2 N 0.65634(15) 0.51537(15) 0.05467(9) 0.0465(7) Uani 1 1 d .
C1 C 0.84860(18) 0.58365(19) 0.08555(11) 0.0447(8) Uani 1 1 d .
C2 C 0.86223(19) 0.5494(2) 0.11872(11) 0.0512(9) Uani 1 1 d .
H2A H 0.8472 0.4992 0.1170 0.061 Uiso 1 1 calc R
C3 C 0.8982(2) 0.5894(2) 0.15459(12) 0.0583(10) Uani 1 1 d .
H3A H 0.9084 0.5666 0.1772 0.070 Uiso 1 1 calc R
C4 C 0.9189(2) 0.6623(2) 0.15721(13) 0.0656(11) Uani 1 1 d .
H4A H 0.9430 0.6893 0.1817 0.079 Uiso 1 1 calc R
C5 C 0.9046(2) 0.6958(2) 0.12454(12) 0.0570(10) Uani 1 1 d .
H5A H 0.9191 0.7459 0.1267 0.068 Uiso 1 1 calc R
C6 C 0.86947(19) 0.65758(19) 0.08850(11) 0.0483(9) Uani 1 1 d .
C7 C 0.85076(19) 0.55793(18) 0.01529(11) 0.0465(8) Uani 1 1 d .
H7A H 0.9000 0.5955 0.0177 0.056 Uiso 1 1 calc R
C8 C 0.82676(19) 0.52591(19) -0.02614(11) 0.0468(8) Uani 1 1 d .
C9 C 0.8790(2) 0.5508(2) -0.05885(12) 0.0575(10) Uani 1 1 d .
H9A H 0.9283 0.5849 -0.0527 0.069 Uiso 1 1 calc R
C10 C 0.8595(2) 0.5268(3) -0.09861(12) 0.0638(11) Uani 1 1 d .
C11 C 0.7853(2) 0.4765(2) -0.10854(12) 0.0619(11) Uani 1 1 d .
H11A H 0.7712 0.4598 -0.1366 0.074 Uiso 1 1 calc R
C12 C 0.7356(2) 0.4531(2) -0.07722(12) 0.0545(9) Uani 1 1 d .
H12A H 0.6861 0.4206 -0.0840 0.065 Uiso 1 1 calc R
C13 C 0.75384(19) 0.47480(18) -0.03485(10) 0.0442(8) Uani 1 1 d .
C14 C 0.8947(3) 0.5569(3) -0.16986(13) 0.0947(17) Uani 1 1 d .
H14A H 0.9385 0.5853 -0.1869 0.142 Uiso 1 1 calc R
H14B H 0.8655 0.5809 -0.1698 0.142 Uiso 1 1 calc R
H14C H 0.8661 0.5080 -0.1818 0.142 Uiso 1 1 calc R
C15 C 0.7006(2) 0.6276(2) 0.01229(12) 0.0520(9) Uani 1 1 d .
C16 C 0.6991(2) 0.6584(2) -0.02626(13) 0.0626(11) Uani 1 1 d .
H16A H 0.7286 0.7095 -0.0298 0.075 Uiso 1 1 calc R
C17 C 0.6574(3) 0.6182(3) -0.05870(13) 0.0694(12) Uani 1 1 d .
H17A H 0.6595 0.6408 -0.0849 0.083 Uiso 1 1 calc R
C18 C 0.6118(3) 0.5445(3) -0.05377(13) 0.0677(11) Uani 1 1 d .
H18A H 0.5804 0.5166 -0.0760 0.081 Uiso 1 1 calc R
C19 C 0.6120(2) 0.5113(2) -0.01621(13) 0.0601(10) Uani 1 1 d .
H19A H 0.5816 0.4602 -0.0131 0.072 Uiso 1 1 calc R
C20 C 0.6563(2) 0.5523(2) 0.01697(11) 0.0498(9) Uani 1 1 d .
C21 C 0.6243(2) 0.52326(19) 0.08673(12) 0.0522(9) Uani 1 1 d .
H21A H 0.6014 0.5515 0.0829 0.063 Uiso 1 1 calc R
C22 C 0.6197(2) 0.4934(2) 0.12808(12) 0.0535(9) Uani 1 1 d .
C23 C 0.5734(2) 0.4987(2) 0.15745(14) 0.0642(11) Uani 1 1 d .
H23A H 0.5448 0.5196 0.1492 0.077 Uiso 1 1 calc R
C24 C 0.5685(3) 0.4743(2) 0.19782(15) 0.0719(12) Uani 1 1 d .
C25 C 0.6101(3) 0.4431(2) 0.20947(13) 0.0680(12) Uani 1 1 d .
H25A H 0.6061 0.4250 0.2373 0.082 Uiso 1 1 calc R
C26 C 0.6571(2) 0.4381(2) 0.18118(12) 0.0594(10) Uani 1 1 d .
H26A H 0.6860 0.4178 0.1900 0.071 Uiso 1 1 calc R
C27 C 0.6625(2) 0.46271(18) 0.13981(11) 0.0486(9) Uani 1 1 d .
C28 C 0.5143(3) 0.4595(3) 0.26355(16) 0.0924(16) Uani 1 1 d .
H28A H 0.4814 0.4711 0.2791 0.139 Uiso 1 1 calc R
H28B H 0.5626 0.4849 0.2765 0.139 Uiso 1 1 calc R
H28C H 0.4954 0.4070 0.2644 0.139 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'
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
O3 Ti1 O3 103.11(14) 2_655 .
O3 Ti1 O2 94.97(10) 2_655 .
O3 Ti1 O2 96.26(10) . .
O3 Ti1 O1 94.67(10) 2_655 .
O3 Ti1 O1 96.85(10) . .
O2 Ti1 O1 161.53(11) . .
O3 Ti1 N1 171.71(10) 2_655 .
O3 Ti1 N1 84.80(10) . .
O2 Ti1 N1 86.52(10) . .
O1 Ti1 N1 81.78(10) . .
O3 Ti1 N2 87.55(10) 2_655 .
O3 Ti1 N2 169.15(10) . .
O2 Ti1 N2 80.55(10) . .
O1 Ti1 N2 84.16(10) . .
N1 Ti1 N2 84.65(10) . .
O3 Ti1 Ti1 21.69(7) 2_655 2_655
O3 Ti1 Ti1 81.51(7) . 2_655
O2 Ti1 Ti1 99.43(7) . 2_655
O1 Ti1 Ti1 95.33(7) . 2_655
N1 Ti1 Ti1 165.58(7) . 2_655
N2 Ti1 Ti1 109.19(8) . 2_655
O3 Ti1 Ti1 81.64(7) 2_655 3_665
O3 Ti1 Ti1 21.56(7) . 3_665
O2 Ti1 Ti1 100.25(7) . 3_665
O1 Ti1 Ti1 96.72(7) . 3_665
N1 Ti1 Ti1 106.15(7) . 3_665
N2 Ti1 Ti1 169.19(8) . 3_665
Ti1 Ti1 Ti1 60.0 2_655 3_665
C6 S2 S3 104.64(13) . .
C15 S3 S2 105.88(13) . .
C13 O1 Ti1 135.9(2) . .
C27 O2 Ti1 132.9(2) . .
Ti1 O3 Ti1 136.76(14) 3_665 .
C10 O4 C14 115.9(4) . .
C28 O5 C24 116.5(4) . .
C7 N1 C1 115.3(3) . .
C7 N1 Ti1 122.5(2) . .
C1 N1 Ti1 121.3(2) . .
C21 N2 C20 116.6(3) . .
C21 N2 Ti1 122.8(2) . .
C20 N2 Ti1 120.3(2) . .
C2 C1 C6 120.1(3) . .
C2 C1 N1 117.7(3) . .
C6 C1 N1 122.1(3) . .
C1 C2 C3 119.5(4) . .
C4 C3 C2 120.0(4) . .
C5 C4 C3 120.4(4) . .
C4 C5 C6 120.8(4) . .
C5 C6 C1 119.1(3) . .
C5 C6 S2 118.1(3) . .
C1 C6 S2 122.7(3) . .
N1 C7 C8 126.7(3) . .
C13 C8 C9 120.0(3) . .
C13 C8 C7 122.3(3) . .
C9 C8 C7 117.7(3) . .
C10 C9 C8 120.8(4) . .
C9 C10 O4 117.0(4) . .
C9 C10 C11 120.3(4) . .
O4 C10 C11 122.7(4) . .
C12 C11 C10 118.7(4) . .
C11 C12 C13 123.0(4) . .
O1 C13 C8 122.3(3) . .
O1 C13 C12 120.5(3) . .
C8 C13 C12 117.2(3) . .
C16 C15 C20 118.0(4) . .
C16 C15 S3 119.1(3) . .
C20 C15 S3 122.7(3) . .
C17 C16 C15 122.4(4) . .
C16 C17 C18 119.9(4) . .
C17 C18 C19 119.8(4) . .
C18 C19 C20 120.4(4) . .
C19 C20 C15 119.4(3) . .
C19 C20 N2 118.5(3) . .
C15 C20 N2 122.1(3) . .
N2 C21 C22 126.2(3) . .
C23 C22 C27 120.2(4) . .
C23 C22 C21 117.8(4) . .
C27 C22 C21 121.9(3) . .
C24 C23 C22 121.1(4) . .
C23 C24 O5 114.9(4) . .
C23 C24 C25 119.0(4) . .
O5 C24 C25 126.1(4) . .
C26 C25 C24 121.1(4) . .
C25 C26 C27 120.5(4) . .
O2 C27 C26 119.8(3) . .
O2 C27 C22 122.1(3) . .
C26 C27 C22 118.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O3 1.807(2) 2_655
Ti1 O3 1.817(2) .
Ti1 O2 1.909(2) .
Ti1 O1 1.915(2) .
Ti1 N1 2.279(3) .
Ti1 N2 2.300(3) .
Ti1 Ti1 3.3691(10) 2_655
Ti1 Ti1 3.3691(10) 3_665
S2 C6 1.780(4) .
S2 S3 2.0639(15) .
S3 C15 1.776(4) .
O1 C13 1.309(4) .
O2 C27 1.321(4) .
O3 Ti1 1.807(2) 3_665
O4 C10 1.392(5) .
O4 C14 1.402(5) .
O5 C28 1.350(6) .
O5 C24 1.389(5) .
N1 C7 1.284(4) .
N1 C1 1.440(4) .
N2 C21 1.282(4) .
N2 C20 1.431(4) .
C1 C2 1.390(5) .
C1 C6 1.405(5) .
C2 C3 1.398(5) .
C3 C4 1.384(6) .
C4 C5 1.375(6) .
C5 C6 1.386(5) .
C7 C8 1.451(5) .
C8 C13 1.404(5) .
C8 C9 1.415(5) .
C9 C10 1.347(6) .
C10 C11 1.429(6) .
C11 C12 1.352(5) .
C12 C13 1.412(5) .
C15 C16 1.395(5) .
C15 C20 1.401(5) .
C16 C17 1.348(6) .
C17 C18 1.377(6) .
C18 C19 1.387(6) .
C19 C20 1.391(5) .
C21 C22 1.440(5) .
C22 C23 1.401(5) .
C22 C27 1.408(5) .
C23 C24 1.367(6) .
C24 C25 1.391(7) .
C25 C26 1.387(6) .
C26 C27 1.397(5) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139137245
