Exploring untapped potential of the molecular precursor approach to control fluorine-doping in mesostructured titania for acid catalysis
Elgayar, Fouad; Jeanneau, Erwann; Bargiela, Pascal; Mesbah, Adel; Essayem, Nadine; Mishra, Shashank; Catalysis Science & Technology 15 (2025) 6744–6756; doi:10.1039/D5CY00688K

data_1575813
_publ_section_title
;
 Exploring untapped potential of the molecular precursor approach to
 control fluorine-doping in mesostructured titania for acid catalysis
;
_journal_issue                   22
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              6744
_journal_page_last               6756
_journal_paper_doi               10.1039/D5CY00688K
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C21 H30 F18 N2 O8 Ti2'
_chemical_formula_sum            'C21 H30 F18 N2 O8 Ti2'
_chemical_formula_weight         876.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-27
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-02-28 deposited with the CCDC.	2025-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5163(2)
_cell_length_b                   17.4673(2)
_cell_length_c                   19.7943(3)
_cell_measurement_reflns_used    16329
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      77.7460
_cell_measurement_theta_min      4.0260
_cell_volume                     6747.82(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 44.93a 64-bit (release 10-02-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     21.00  89.00   0.50    0.90    --   47.57-109.00-102.00  136
  2  \w     36.00 127.00   0.50    0.90    --   47.57  22.00 168.00  182
  3  \w    -67.00  -9.00   0.50    3.50    --  -84.52 109.00  -6.00  116
  4  \w    -72.00  -9.00   0.50    3.50    --  -84.52 114.00-101.00  126
  5  \w     89.00 155.00   0.50    3.50    --  100.54  22.00 168.00  132
  6  \w     36.00  93.00   0.50    3.50    --  111.19-109.00-102.00  114
  7  \w    -19.00  31.00   0.50    0.90    --  -48.82  38.00 -90.00  100
  8  \w   -126.00 -79.00   0.50    0.90    --  -48.82 -57.00 -30.00   94
  9  \w   -126.00 -79.00   0.50    0.90    --  -48.82 -57.00-150.00   94
 10  \w   -136.00 -64.00   0.50    3.50    --  -84.52 -15.00 -60.00  144
 11  \w    -51.00  -9.00   0.50    3.50    --  -84.52  61.00 120.00   84
 12  \w   -136.00 -64.00   0.50    3.50    --  -84.52 -15.00 -60.00  144
 13  \w     33.00  91.00   0.50    3.50    --  100.54 -95.00 -90.00  116
 14  \w     25.00  50.00   0.50    3.50    --  100.54 -61.00-180.00   50
 15  \w     34.00  67.00   0.50    3.50    --  100.54 -77.00 150.00   66
 16  \w     25.00  50.00   0.50    3.50    --  100.54 -61.00  30.00   50
 17  \w     25.00  51.00   0.50    3.50    --  100.54 -61.00 -60.00   52
 18  \w     41.00  68.00   0.50    3.50    --  111.19 -77.00  60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0449308000
_diffrn_orient_matrix_UB_12      0.0020105000
_diffrn_orient_matrix_UB_13      0.0639969000
_diffrn_orient_matrix_UB_21      -0.0626354000
_diffrn_orient_matrix_UB_22      0.0246871000
_diffrn_orient_matrix_UB_23      0.0421114000
_diffrn_orient_matrix_UB_31      -0.0171440000
_diffrn_orient_matrix_UB_32      -0.0846033000
_diffrn_orient_matrix_UB_33      0.0137683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39853
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.126
_diffrn_reflns_theta_min         4.065
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.388
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.124a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       needle
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         6706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0482
_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/[\s^2^(Fo^2^)+(0.0681P)^2^+8.4054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5726
_reflns_number_total             6706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy00688k2.cif
_cod_data_source_block           flgb70_autored
_cod_depositor_comments
'Adding full bibliography for 1575809--1575816.cif.'
_cod_original_cell_volume        6747.81(16)
_cod_database_code               1575813
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H60 F36 N4 O16 Ti4'
_chemical_oxdiff_usercomment     'CSD: UDIKOJ'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C20(H20A,H20B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              36204
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id FLGB70
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.525
_oxdiff_exptl_absorpt_empirical_full_min 0.675