#------------------------------------------------------------------------------
#$Date: 2025-08-18 17:33:07 +0200 (Mon 18 de Aug de 2025) $
#$Revision: 301779 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/84/1548419.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_1548419
loop_
_publ_author_name
'Daniel Lundberg'
'Ingmar Persson'
_publ_section_title
;
 Structure of a Hydrated Sulfonatotitanyl(IV) Complex in Aqueous Solution
 and the Dimethylsulfoxide Solvated Titanyl(IV) Ion in Solution and Solid
 State
;
_journal_name_full               'Journal of Solution Chemistry'
_journal_page_first              476
_journal_page_last               487
_journal_paper_doi               10.1007/s10953-017-0581-3
_journal_volume                  46
_journal_year                    2017
_chemical_compound_source        synthesized
_chemical_formula_moiety         'Ti O6 S5 C10 H30, 2 (C F3 S O3)'
_chemical_formula_sum            'C12 H30 F6 O12 S7 Ti'
_chemical_formula_weight         752.68
_chemical_name_common            'pentakis(dmso)oxotitanium(IV) triflate'
_chemical_name_systematic
'pentakis(dimethylsulfoxide)oxotitanium(IV) trifluoromethanesulfonate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                99.002(9)
_cell_angle_beta                 110.814(8)
_cell_angle_gamma                110.231(8)
_cell_formula_units_Z            2
_cell_length_a                   10.198(5)
_cell_length_b                   13.495(6)
_cell_length_c                   13.797(6)
_cell_measurement_reflns_used    4797
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.93
_cell_volume                     1578.6(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Diamond 2.0'
_computing_publication_material  'Diamond 2.0'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'φ andω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5575
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        22.984
_diffrn_reflns_theta_max         22.984
_diffrn_reflns_theta_min         1.666
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART'
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.121029
_exptl_absorpt_correction_T_min  0.054932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_recrystallization_method 'crystallized from dmso'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         4170
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1597P)²+0.5380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2216
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3327
_reflns_number_total             4170
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            J-Solution-Chem-2017-46-476-487.cif
_cod_data_source_block           tidmso2m
_cod_original_cell_volume        1578.5(13)
_cod_database_code               1548419
_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. 
;
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 0.28116(11) 0.77445(7) 0.29752(8) 0.0581(4) Uani 1 1 d . . . . .
O1 O 0.4131(5) 0.9015(3) 0.3752(3) 0.0702(10) Uani 1 1 d . . . . .
O2 O 0.2718(5) 0.7013(3) 0.4139(3) 0.0791(11) Uani 1 1 d . . . . .
S2 S 0.3365(2) 0.75125(14) 0.53820(14) 0.0818(5) Uani 1 1 d . . . . .
C21 C 0.2865(12) 0.6326(8) 0.5799(8) 0.138(4) Uani 1 1 d . . . . .
H21A H 0.3224 0.6552 0.6578 0.206 Uiso 1 1 calc R U . . .
H21B H 0.1754 0.5899 0.5444 0.206 Uiso 1 1 calc R U . . .
H21C H 0.3345 0.5880 0.5604 0.206 Uiso 1 1 calc R U . . .
C22 C 0.5347(10) 0.8025(10) 0.5930(8) 0.157(5) Uani 1 1 d . . . . .
H22A H 0.5785 0.8344 0.6709 0.235 Uiso 1 1 calc R U . . .
H22B H 0.5625 0.7432 0.5762 0.235 Uiso 1 1 calc R U . . .
H22C H 0.5744 0.8587 0.5627 0.235 Uiso 1 1 calc R U . . .
O3 O 0.0964(4) 0.8028(3) 0.2950(3) 0.0716(10) Uani 1 1 d . . . . .
S3 S 0.10832(18) 0.92142(12) 0.33001(12) 0.0695(5) Uani 1 1 d . . . . .
C31 C 0.1986(8) 0.9675(6) 0.4756(5) 0.0870(19) Uani 1 1 d . . . . .
H31A H 0.2092 1.0413 0.5022 0.131 Uiso 1 1 calc R U . . .
H31B H 0.1357 0.9178 0.5011 0.131 Uiso 1 1 calc R U . . .
H31C H 0.2998 0.9682 0.5020 0.131 Uiso 1 1 calc R U . . .
C32 C -0.0838(8) 0.8947(6) 0.3064(6) 0.0848(18) Uani 1 1 d . . . . .
H32A H -0.0898 0.9639 0.3257 0.127 Uiso 1 1 calc R U . . .
H32B H -0.1528 0.8545 0.2304 0.127 Uiso 1 1 calc R U . . .
H32C H -0.1136 0.8510 0.3501 0.127 Uiso 1 1 calc R U . . .
O4 O 0.2497(5) 0.8050(3) 0.1521(3) 0.0705(10) Uani 1 1 d . . . . .
S4 S 0.32109(18) 0.92260(12) 0.14652(12) 0.0692(5) Uani 1 1 d . . . . .
C41 C 0.2611(10) 0.8970(6) 0.0047(6) 0.099(2) Uani 1 1 d . . . . .
H41A H 0.2998 0.9663 -0.0092 0.149 Uiso 1 1 calc R U . . .
H41B H 0.3014 0.8493 -0.0208 0.149 Uiso 1 1 calc R U . . .
H41C H 0.1493 0.8615 -0.0331 0.149 Uiso 1 1 calc R U . . .
C42 C 0.5208(8) 0.9600(7) 0.1889(6) 0.100(2) Uani 1 1 d . . . . .
H42A H 0.5709 1.0338 0.1867 0.150 Uiso 1 1 calc R U . . .
H42B H 0.5669 0.9583 0.2622 0.150 Uiso 1 1 calc R U . . .
H42C H 0.5336 0.9084 0.1408 0.150 Uiso 1 1 calc R U . . .
O5 O 0.4264(5) 0.7094(3) 0.2790(4) 0.0768(11) Uani 1 1 d . . . . .
S5 S 0.39056(19) 0.59353(14) 0.21376(14) 0.0803(5) Uani 1 1 d . . . . .
C51 C 0.5686(10) 0.6139(7) 0.2097(8) 0.115(3) Uani 1 1 d . . . . .
H51A H 0.5592 0.5448 0.1697 0.173 Uiso 1 1 calc R U . . .
H51B H 0.5942 0.6685 0.1742 0.173 Uiso 1 1 calc R U . . .
H51C H 0.6495 0.6394 0.2829 0.173 Uiso 1 1 calc R U . . .
C52 C 0.3939(11) 0.5162(6) 0.3054(7) 0.108(2) Uani 1 1 d . . . . .
H52A H 0.3720 0.4416 0.2690 0.162 Uiso 1 1 calc R U . . .
H52B H 0.4950 0.5505 0.3669 0.162 Uiso 1 1 calc R U . . .
H52C H 0.3166 0.5142 0.3303 0.162 Uiso 1 1 calc R U . . .
O6 O 0.0958(4) 0.6071(3) 0.1872(3) 0.0671(10) Uani 1 1 d . . . . .
S6 S -0.0761(2) 0.5540(3) 0.15284(16) 0.0768(10) Uani 0.886(12) 1 d . . P A 1
S6B S -0.034(3) 0.5074(16) 0.181(2) 0.093(10) Uani 0.114(12) 1 d . . P A 2
C61 C -0.1380(10) 0.4152(6) 0.0713(7) 0.107(2) Uani 1 1 d . . . . .
H61A H -0.2483 0.3741 0.0452 0.161 Uiso 1 1 calc R U . A 1
H61B H -0.1139 0.4174 0.0103 0.161 Uiso 1 1 calc R U . A 1
H61C H -0.0849 0.3796 0.1148 0.161 Uiso 1 1 calc R U . A 1
C62 C -0.1000(9) 0.5265(7) 0.2664(6) 0.100(2) Uani 1 1 d . . . . .
H62A H -0.2090 0.4922 0.2480 0.150 Uiso 1 1 calc R U . A 1
H62B H -0.0549 0.4771 0.2881 0.150 Uiso 1 1 calc R U . A 1
H62C H -0.0492 0.5949 0.3256 0.150 Uiso 1 1 calc R U . A 1
S20 S 0.4261(2) 0.24379(14) 0.07376(14) 0.0836(5) Uani 1 1 d D . . . .
O21 O 0.450(4) 0.182(2) 0.144(2) 0.176(14) Uani 0.46(3) 1 d D . P B 1
O22 O 0.508(4) 0.3571(13) 0.122(3) 0.171(16) Uani 0.46(3) 1 d D . P B 1
O23 O 0.418(4) 0.202(3) -0.0268(15) 0.187(14) Uani 0.46(3) 1 d D . P B 1
O21B O 0.426(4) 0.254(3) -0.0244(17) 0.223(14) Uani 0.54(3) 1 d D . P B 2
O22B O 0.499(3) 0.3447(13) 0.1566(19) 0.128(8) Uani 0.54(3) 1 d D . P B 2
O23B O 0.472(2) 0.1639(14) 0.107(2) 0.161(11) Uani 0.54(3) 1 d D . P B 2
C20 C 0.2217(12) 0.2042(9) 0.0388(8) 0.131(3) Uani 1 1 d D . . . .
F21 F 0.138(3) 0.1023(13) 0.005(3) 0.22(2) Uani 0.46(3) 1 d D . P B 1
F22 F 0.212(3) 0.253(3) 0.123(2) 0.30(2) Uani 0.46(3) 1 d D . P B 1
F23 F 0.179(4) 0.249(3) -0.035(2) 0.253(18) Uani 0.46(3) 1 d D . P B 1
F21B F 0.197(2) 0.171(3) 0.1181(13) 0.229(15) Uani 0.54(3) 1 d D . P B 2
F22B F 0.176(2) 0.2757(17) 0.021(3) 0.246(19) Uani 0.54(3) 1 d D . P B 2
F23B F 0.142(3) 0.1155(17) -0.0450(16) 0.196(12) Uani 0.54(3) 1 d D . P B 2
S10 S 0.8772(3) 0.71563(18) 0.55026(16) 0.0980(6) Uani 1 1 d . . . . .
O11 O 0.7334(8) 0.6367(6) 0.5409(7) 0.163(3) Uani 1 1 d . . . . .
O12 O 0.9481(12) 0.6649(10) 0.5095(9) 0.238(6) Uani 1 1 d . . . . .
O13 O 0.8626(10) 0.8063(7) 0.5181(7) 0.177(3) Uani 1 1 d . . . . .
C10 C 0.9929(14) 0.7738(8) 0.6929(9) 0.130(3) Uani 1 1 d . . . . .
F11 F 1.0006(14) 0.7097(8) 0.7443(7) 0.265(6) Uani 1 1 d . . . . .
F12 F 0.9456(13) 0.8373(8) 0.7403(7) 0.223(4) Uani 1 1 d . . . . .
F13 F 1.1330(8) 0.8453(9) 0.7113(7) 0.230(4) Uani 1 1 d . . . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
O1 Ti1 O2 100.05(19) . .
O1 Ti1 O5 98.28(18) . .
O2 Ti1 O5 88.34(18) . .
O1 Ti1 O3 95.14(18) . .
O2 Ti1 O3 88.78(18) . .
O5 Ti1 O3 166.57(16) . .
O1 Ti1 O4 95.58(18) . .
O2 Ti1 O4 164.32(17) . .
O5 Ti1 O4 88.13(17) . .
O3 Ti1 O4 91.13(17) . .
O1 Ti1 O6 176.92(18) . .
O2 Ti1 O6 82.23(17) . .
O5 Ti1 O6 83.81(15) . .
O3 Ti1 O6 82.80(15) . .
O4 Ti1 O6 82.20(15) . .
S2 O2 Ti1 131.2(3) . .
O2 S2 C22 107.6(4) . .
O2 S2 C21 102.9(4) . .
C22 S2 C21 101.7(5) . .
S3 O3 Ti1 122.6(2) . .
O3 S3 C32 102.4(3) . .
O3 S3 C31 105.7(3) . .
C32 S3 C31 99.1(3) . .
S4 O4 Ti1 122.1(2) . .
O4 S4 C42 106.4(3) . .
O4 S4 C41 101.8(3) . .
C42 S4 C41 99.0(4) . .
S5 O5 Ti1 130.4(2) . .
O5 S5 C52 105.3(3) . .
O5 S5 C51 102.3(3) . .
C52 S5 C51 99.7(5) . .
S6B O6 Ti1 142.8(8) . .
S6 O6 Ti1 131.7(2) . .
O6 S6 C62 106.6(3) . .
O6 S6 C61 103.3(3) . .
C62 S6 C61 99.3(4) . .
O6 S6B C61 118.0(13) . .
O6 S6B C62 116.0(11) . .
C61 S6B C62 120.3(14) . .
O22 S20 O23 115.9(15) . .
O21B S20 O22B 114.0(13) . .
O22 S20 O21 115.5(15) . .
O23 S20 O21 114.9(13) . .
O21B S20 O23B 114.4(13) . .
O22B S20 O23B 113.0(11) . .
O22 S20 C20 109.1(17) . .
O23 S20 C20 101.1(15) . .
O21B S20 C20 99.8(14) . .
O22B S20 C20 102.3(12) . .
O21 S20 C20 97.1(17) . .
O23B S20 C20 111.8(10) . .
F21 C20 F23 111.1(17) . .
F22B C20 F23B 110.3(15) . .
F21 C20 F22 111.8(16) . .
F23 C20 F22 106.3(16) . .
F22B C20 F21B 111.5(14) . .
F23B C20 F21B 104.3(14) . .
F22B C20 S20 116.0(12) . .
F21 C20 S20 114.8(16) . .
F23 C20 S20 103.9(15) . .
F23B C20 S20 107.3(14) . .
F22 C20 S20 108.3(14) . .
F21B C20 S20 106.7(11) . .
O12 S10 O13 118.2(8) . .
O12 S10 O11 111.5(7) . .
O13 S10 O11 111.9(6) . .
O12 S10 C10 107.1(6) . .
O13 S10 C10 103.5(5) . .
O11 S10 C10 102.9(6) . .
F11 C10 F12 104.2(12) . .
F11 C10 F13 111.4(11) . .
F12 C10 F13 102.6(10) . .
F11 C10 S10 117.0(8) . .
F12 C10 S10 112.6(8) . .
F13 C10 S10 108.1(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O1 1.644(4) .
Ti1 O2 2.025(4) .
Ti1 O5 2.032(4) .
Ti1 O3 2.037(4) .
Ti1 O4 2.047(4) .
Ti1 O6 2.217(4) .
O2 S2 1.536(4) .
S2 C22 1.708(9) .
S2 C21 1.757(9) .
O3 S3 1.547(4) .
S3 C32 1.760(7) .
S3 C31 1.780(7) .
O4 S4 1.528(4) .
S4 C42 1.759(7) .
S4 C41 1.764(7) .
O5 S5 1.523(4) .
S5 C52 1.760(8) .
S5 C51 1.763(8) .
O6 S6B 1.491(17) .
O6 S6 1.499(4) .
S6 C62 1.744(8) .
S6 C61 1.786(8) .
S6B C61 1.52(2) .
S6B C62 1.579(16) .
S20 O22 1.371(16) .
S20 O23 1.377(13) .
S20 O21B 1.381(14) .
S20 O22B 1.386(12) .
S20 O21 1.387(14) .
S20 O23B 1.397(14) .
S20 C20 1.816(10) .
C20 F22B 1.230(15) .
C20 F21 1.240(16) .
C20 F23 1.286(18) .
C20 F23B 1.286(16) .
C20 F22 1.294(15) .
C20 F21B 1.316(15) .
S10 O12 1.348(7) .
S10 O13 1.402(7) .
S10 O11 1.430(7) .
S10 C10 1.763(11) .
C10 F11 1.207(11) .
C10 F12 1.314(12) .
C10 F13 1.323(13) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139051566
