Assembling molecular semiconductor composites for enhanced photocatalytic cyclohexene oxidation.
Yu, Haiyan; Wang, Xueting; Kong, Tingting; Gao, Mei-Yan; Cui, Xiaofeng; Chemical communications (Cambridge, England) 60 (2024) 15051–15054; doi:10.1039/d4cc04194a

data_7134014
_publ_section_title
;
 Assembling molecular semiconductor composites for enhanced photocatalytic
 cyclohexene oxidation.
;
_journal_issue                   100
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15051
_journal_page_last               15054
_journal_paper_doi               10.1039/d4cc04194a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'O40 P W12, C51 H119 O32 Ti12, C48 H112 O32 Ti12, 1.4[C3H8O], 2[H2O], 1.6[H2O]'
_chemical_formula_sum            'C103.2 H249.4 O109 P Ti24 W12'
_chemical_formula_weight         6621.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-16 deposited with the CCDC.	2024-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.927(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7675(4)
_cell_length_b                   29.1952(7)
_cell_length_c                   44.3515(14)
_cell_measurement_reflns_used    40147
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.2000
_cell_measurement_theta_min      1.7320
_cell_volume                     20405.0(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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      0.25 183.25   0.50   10.00    --   27.00  73.77 -25.75  366
  2  \w     -4.75 126.75   0.50   10.00    --   33.00  73.77  62.25  263
  3  \w     -2.75  69.25   0.50   10.00    --   33.00  73.77 154.25  144
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            68433
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        21.000
_diffrn_reflns_theta_max         21.000
_diffrn_reflns_theta_min         1.670
_exptl_absorpt_coefficient_mu    7.707
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.155
_exptl_crystal_description       strip
_exptl_crystal_F_000             12686
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.922
_refine_diff_density_min         -2.039
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2233
_refine_ls_number_reflns         21885
_refine_ls_number_restraints     3878
_refine_ls_restrained_S_all      41.532
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1369P)^2^+925.1064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2482
_refine_ls_wR_factor_ref         0.2739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15948
_reflns_number_total             21885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04194a2.cif
_cod_data_source_block           Ti12TPA
_cod_depositor_comments          'Adding full bibliography for 7134014.cif.'
_cod_original_formula_sum        'C103.20 H249.40 O109 P Ti24 W12'
_cod_database_code               7134014
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.206
_shelx_estimated_absorpt_t_min   0.163
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O39-C55
 1.45 with sigma of 0.01
 C55-C7 = C55-C57
 1.49 with sigma of 0.01
 C88-C62 = C72-C78
 1.49 with sigma of 0.01
 C61-C96
 1.49 with sigma of 0.01
 C59-C29 = C15-C59
 1.49 with sigma of 0.01
 O81-C59
 1.45 with sigma of 0.01
 O75-C61
 2.45 with sigma of 0.01
 C31-C2 = C63-C31
 1.49 with sigma of 0.01
 O29-C31
 1.45 with sigma of 0.01
 O77-C67
 1.45 with sigma of 0.01
 C67-C65 = C67-C33
 1.49 with sigma of 0.01
 O47-C9
 1.45 with sigma of 0.01
 C9-C71 = C73-C9
 1.49 with sigma of 0.01
 O47-C71
 2.45 with sigma of 0.01
 O21-C75
 1.45 with sigma of 0.01
 C19-C75 = C37-C75
 1.49 with sigma of 0.01
 Ti11-O25
 1.936 with sigma of 0.01
 Ti3-O25
 2 with sigma of 0.01
 Ti21-O25
 2.38 with sigma of 0.01
 O75-C96
 1.45 with sigma of 0.01
 C94-C96 = C61-C96
 1.49 with sigma of 0.01
 C90-C56 = C92-C56
 1.49 with sigma of 0.01
 O31-C56
 1.45 with sigma of 0.01
 C102-C13 = C51-C102
 1.49 with sigma of 0.01
 C94-C61
 2.55 with sigma of 0.01
 O3-C77
 1.45 with sigma of 0.01
 C79-C77 = C39-C77
 1.49 with sigma of 0.01
 C39-C79
 2.55 with sigma of 0.01
 O9-C5
 1.45 with sigma of 0.01
 C41-C5 = C81-C5
 1.49 with sigma of 0.01
 C81-C41
 2.55 with sigma of 0.01
 Ti7-C75
 3 with sigma of 0.01
 Ti11-O85
 1.97 with sigma of 0.01
 Ti23-O85
 1.99 with sigma of 0.01
 O19-C21
 1.45 with sigma of 0.01
 C21-C83 = C85-C21
 1.49 with sigma of 0.01
 C19-C37
 2.55 with sigma of 0.01
 Ti19-O103
 1.93 with sigma of 0.01
 Ti9A-O103
 2.07 with sigma of 0.01
 Ti13-O103
 1.91 with sigma of 0.01
 C11-C43 = C87-C43
 1.49 with sigma of 0.01
 Ti23-O41
 1.93 with sigma of 0.01
 Ti15-O41
 1.96 with sigma of 0.01
 O67-C89
 1.45 with sigma of 0.01
 C89-C91 = C89-C45
 1.49 with sigma of 0.01
 C82-C20
 1.49 with sigma of 0.01
 C80-C10
 1.49 with sigma of 0.01
 C73-O47
 2.45 with sigma of 0.01
 O81-C15
 2.45 with sigma of 0.01
 O49-C11
 2.45 with sigma of 0.01
 O67-C91
 2.45 with sigma of 0.01
 O49-C87
 2.45 with sigma of 0.01
 Ti9A-C43
 3.08 with sigma of 0.01
 C11-C87
 2.55 with sigma of 0.01
 O3-C39
 2.45 with sigma of 0.01
 O79-C47
 1.45 with sigma of 0.01
 C47-C23 = C47-C93
 1.49 with sigma of 0.01
 Ti5A-O79
 1.73 with sigma of 0.01
 C91-C45
 2.55 with sigma of 0.01
 C93-O79
 2.45 with sigma of 0.01
 O79-C23
 2.45 with sigma of 0.01
 O41-C95
 1.45 with sigma of 0.01
 C97-C95 = C95-C3
 1.49 with sigma of 0.01
 C98-C27 = C100-C98
 1.49 with sigma of 0.01
 C27-C100
 2.55 with sigma of 0.01
 O93-C49
 1.45 with sigma of 0.01
 C25-C49 = C99-C49
 1.49 with sigma of 0.01
 C86-C54 = C60-C54
 1.49 with sigma of 0.01
 O23-C100
 2.45 with sigma of 0.01
 O23-C27
 2.45 with sigma of 0.01
 C47-C93 = C47-C23
 1.49 with sigma of 0.01
 C93-C23
 2.55 with sigma of 0.01
 O81-C29
 2.45 with sigma of 0.01
 C65-C33
 2.55 with sigma of 0.01
 O77-C65
 2.45 with sigma of 0.01
 C67-Ti9A
 3.1 with sigma of 0.01
 C63-C2
 2.55 with sigma of 0.01
 C68-C76 = C68-C101
 1.49 with sigma of 0.01
 C72-C34
 1.49 with sigma of 0.01
 C6-C44 = C66-C6 = C70-C62 = C64-C32 = C74-C32
 1.49 with sigma of 0.01
 C8-C40 = C28-C10
 1.49 with sigma of 0.01
 Ti5A-C47
 3.07 with sigma of 0.01
 Ti5A-C93
 3.69 with sigma of 0.01
 C58-C14 = C50-C22
 1.49 with sigma of 0.01
 C42-C22
 1.49 with sigma of 0.01
 C24-C1
 1.49 with sigma of 0.01
 C52-C14
 1.49 with sigma of 0.01
 C36-C12 = C53-C12
 1.49 with sigma of 0.01
 C46-C4 = C4-C26
 1.49 with sigma of 0.01
 C84-C20 = C38-C1 = C67-C33
 1.49 with sigma of 0.001
 C59-C29 = C59-C15
 1.49 with sigma of 0.01
 C30-C18 = C30-C16
 1.49 with sigma of 0.01
 O49-C43
 1.46 with sigma of 0.01
 C7-C57
 2.55 with sigma of 0.01
 C81-C5
 1.49 with sigma of 0.01
 Ti9B-C43
 2.8 with sigma of 0.01
 O46-O22
 3 with sigma of 0.01
 H74A_$1-H45A
 2.1 with sigma of 0.01
 C8-C48
 1.49 with sigma of 0.01
 C101-C76
 2.55 with sigma of 0.01
 C5-C41
 1.493 with sigma of 0.01
 H41C-H5
 2.1 with sigma of 0.01
 H41B-H11C_$2
 2.1 with sigma of 0.01
 C66-C6
 1.49 with sigma of 0.01
 C8-C40
 1.49 with sigma of 0.01
 C10-O57 = C10-H10 = C10-C28 = C10-C80
 1.49 with sigma of 0.01
 C36-C12
 1.49 with sigma of 0.01
 C16-H16A = C16-H16B = C16-H16C = C16-C30
 1.49 with sigma of 0.01
 C32-H32 = C32-C64 = C32-C74 = C32-O92
 1.49 with sigma of 0.01
 C74-C32
 1.49 with sigma of 0.01
 C22-H22 = C22-C42 = C22-C50 = C22-O48
 1.49 with sigma of 0.01
 C34-H34A = C34-H34B = C34-H34C = C34-C72
 1.49 with sigma of 0.01
 C54-O59 = C54-H54 = C54-C60 = C54-C86
 1.49 with sigma of 0.01
 C86-C54
 1.49 with sigma of 0.01
 C56-O31 = C56-H56 = C56-C90 = C56-C92
 1.49 with sigma of 0.01
 C90-C56
 1.49 with sigma of 0.01
 C62-O53 = C62-H62 = C62-C70 = C62-C88
 1.49 with sigma of 0.01
 C88-C62
 1.49 with sigma of 0.01
 C72-C34 = C72-O69 = C72-H72 = C72-C78
 1.49 with sigma of 0.01
 C94-H94A = C94-H94B = C94-H94C = C94-C96
 1.49 with sigma of 0.01
 C96-C94 = C96-H96 = C96-C61 = C96-O75
 1.49 with sigma of 0.01
 C98-O23 = C98-H98 = C98-C100 = C98-C27
 1.49 with sigma of 0.01
 C98-C100
 1.49 with sigma of 0.01
 C102-H102 = C102-C51 = C102-C13 = C102-O55
 1.49 with sigma of 0.01
 C55-H55 = C55-C7 = C55-C57 = C55-O39
 1.49 with sigma of 0.01
 C31-O29 = C31-H31 = C31-C63 = C31-C2
 1.49 with sigma of 0.01
 C65-H65A = C65-H65B = C65-H65C = C65-C67
 1.49 with sigma of 0.01
 C71-H71B = C71-H71C = C71-H71A = C71-C9
 1.49 with sigma of 0.01
 C95-H95 = C95-C3 = C95-C97 = C95-O41
 1.49 with sigma of 0.01
 O35-C101
 2.45 with sigma of 0.01
 H3C-H25A
 2.1 with sigma of 0.01
 H48A-H74C
 2.1 with sigma of 0.01
 H5-H81B
 2.1 with sigma of 0.01
 H19C-H73C
 2.1 with sigma of 0.01
 H5-H81C
 2.1 with sigma of 0.01
 H46A-H70C
 2.1 with sigma of 0.01
 H10F-H42C
 2.1 with sigma of 0.01
 C43-C87
 1.49 with sigma of 0.01
 C49-C99
 1.49 with sigma of 0.01
 C49-C25
 1.49 with sigma of 0.01
 C83-C21
 1.49 with sigma of 0.01
 C89-C45
 1.49 with sigma of 0.01
 C97-C95
 1.53 with sigma of 0.01
 H95-H97B
 2.1 with sigma of 0.01
 C95-C3
 1.53 with sigma of 0.01
 H95-H3C
 2.1 with sigma of 0.01
 H83C-H97C
 2.1 with sigma of 0.01
 H3C-H25B
 2.1 with sigma of 0.001
 C82-C84
 2.55 with sigma of 0.01
 H76A-H71C_$3
 2.1 with sigma of 0.001
 Ti11-O71 = Ti5A-O71
 1.9 with sigma of 0.01
 W6-O43 = W4-O46 = W1-O27 = W7-O61 = W12-O15 = W11-O87 = W5-O33 = W9-O17 = W3-
 O89 = W2-O73 = W10-O45 = W8-O98
 1.69 with sigma of 0.01
 Ti24-O53
 1.73 with sigma of 0.01
 W10-O102 = W5-O84 = W9-O30 = W3-O4 = W3-O44 = W11-O104 = W7-O14 = W12-O12 =
 W12-O96 = W12-O78 = W4-O38 = W4-O6 = W4-O1 = W8-O68 = W1-O78 = W1-O8
 1.9 with sigma of 0.01
 Ti17-O39
 1.84 with sigma of 0.01
 Ti17-O5
 1.84 with sigma of 0.01
 Ti6-O62
 1.75 with sigma of 0.01
 Ti14-O16
 1.75 with sigma of 0.01
 Ti4-O76
 1.75 with sigma of 0.01
 Ti23-O51
 1.85 with sigma of 0.01
 Ti14-O69
 1.83 with sigma of 0.01
 Ti11-O83
 1.85 with sigma of 0.01
 W11-O87 = W12-O15 = W4-O46 = W8-O98 = W3-O89 = W9-O17 = W5-O33 = W10-O45 = W7-
 O61 = W1-O27 = W2-O73
 1.72 with sigma of 0.001
 Ti23-O19
 1.83 with sigma of 0.01
 Ti11-O3
 1.83 with sigma of 0.001
 W6-O43
 1.72 with sigma of 0.001
 W2-W8 = W7-W3 = W10-W4
 1.72 with sigma of 0.001
 Ti5B-C99
 3.5 with sigma of 0.01
 C68-C101
 1.54 with sigma of 0.02
 H23C_$4-H10A
 2.1 with sigma of 0.01
 H10B-C68
 1.9 with sigma of 0.01
 C68-H10B
 2.1 with sigma of 0.01
 C47-H23C
 2.1 with sigma of 0.01
3. Rigid bond restraints
 O41, C95
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O49, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O77, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O93, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O35, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O67, C89
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O57, C89, O67, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O48, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O13, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O53, C62
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O54, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O64, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O92, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O94, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O100, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Ti2, O21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti2, O65
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti2, O49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti5A, O63
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti5A, O71
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti3, O97
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti7, O47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti7, O97
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Ti7, O95
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Ti17, O99
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Ti21, O25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Ti23, O85
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti23, O51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O90, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti13, O51
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Ti15, O101
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti13, Ti13, O101
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti2, O95
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O69, C72
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 W9, O30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, O76
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O62, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O48, Ti1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O52, W2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O52, W5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 P1, O86
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti13, O67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti24, O53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Ti1, O48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O47, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim O4 \\sim O6 \\sim O8 \\sim O10 \\sim O12 \\sim O14 \\sim O16 \\sim O18
\\sim O20 \\sim O22 \\sim O24 \\sim O26 \\sim O28 \\sim O30 \\sim O32 \\sim O34
\\sim O36 \\sim O38 \\sim O40 \\sim O42 \\sim O44 \\sim O46 \\sim O48 \\sim O50
\\sim O52 \\sim O54 \\sim O56 \\sim O58 \\sim O60 \\sim O62 \\sim O64 \\sim O66
\\sim O68 \\sim O70 \\sim O72 \\sim O74 \\sim O76 \\sim O78 \\sim O80 \\sim O82
\\sim O84 \\sim O86 \\sim O88 \\sim O90 \\sim O92 \\sim O94 \\sim O96 \\sim O98
\\sim O100 \\sim O102 \\sim O104 \\sim O13 \\sim O53 \\sim O27 \\sim O55 \\sim
O7 \\sim O57 \\sim O29 \\sim O59 \\sim O15 \\sim O61 \\sim O31 \\sim O63 \\sim
O2 \\sim O65 \\sim O33 \\sim O67 \\sim O17 \\sim O69 \\sim O35 \\sim O71 \\sim
O9 \\sim O73 \\sim O37 \\sim O75 \\sim O19 \\sim O77 \\sim O39 \\sim O79 \\sim
O5 \\sim O81 \\sim O41 \\sim O83 \\sim O21 \\sim O85 \\sim O43 \\sim O87 \\sim
O11 \\sim O89 \\sim O45 \\sim O91 \\sim O23 \\sim O93 \\sim O47 \\sim O95 \\sim
O3 \\sim O97 \\sim O49 \\sim O99 \\sim O25 \\sim O101 \\sim O51 \\sim O103:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C1 \\sim C4 \\sim C6 \\sim C8 \\sim C10 \\sim C12 \\sim C14 \\sim C16 \\sim C18
\\sim C20 \\sim C22 \\sim C24 \\sim C26 \\sim C28 \\sim C30 \\sim C32 \\sim C34
\\sim C36 \\sim C38 \\sim C40 \\sim C42 \\sim C44 \\sim C46 \\sim C48 \\sim C50
\\sim C52 \\sim C54 \\sim C56 \\sim C58 \\sim C60 \\sim C62 \\sim C64 \\sim C66
\\sim C68 \\sim C70 \\sim C72 \\sim C74 \\sim C76 \\sim C78 \\sim C80 \\sim C82
\\sim C84 \\sim C86 \\sim C88 \\sim C90 \\sim C92 \\sim C94 \\sim C96 \\sim C98
\\sim C100 \\sim C102 \\sim C51 \\sim C13 \\sim C53 \\sim C27 \\sim C55 \\sim
C7 \\sim C57 \\sim C29 \\sim C59 \\sim C15 \\sim C61 \\sim C31 \\sim C63 \\sim
C2 \\sim C65 \\sim C33 \\sim C67 \\sim C71 \\sim C9 \\sim C73 \\sim C37 \\sim
C75 \\sim C19 \\sim C77 \\sim C39 \\sim C79 \\sim C5 \\sim C81 \\sim C41 \\sim
C83 \\sim C21 \\sim C85 \\sim C43 \\sim C87 \\sim C11 \\sim C89 \\sim C45 \\sim
C91 \\sim C23 \\sim C93 \\sim C47 \\sim C95 \\sim C3 \\sim C97 \\sim C49 \\sim
C99 \\sim C25 \\sim C101: within 3.8A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 3.8A
C11 \\sim C43: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O3 \\sim Ti11 \\sim C77: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C31 \\sim C63 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C75 \\sim C19 \\sim C37: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C102 \\sim C13 \\sim C51 \\sim O55: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C31 \\sim O29 \\sim C63 \\sim C2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C75 \\sim O21 \\sim C37 \\sim C19: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Ti3 \\sim O25 \\sim O65 \\sim O97 \\sim O59: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Ti13 \\sim O99 \\sim O101 \\sim O103 \\sim O51 \\sim O67: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Ti21 \\sim O88 \\sim O11 \\sim O97 \\sim O25 \\sim O75: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O19 \\sim Ti23 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O9 \\sim Ti2 \\sim C5: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O39 \\sim Ti17 \\sim C55: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O75 \\sim Ti21 \\sim C96: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O77 \\sim C67 \\sim Ti9A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O31 \\sim Ti16 \\sim C56: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C59 \\sim O81 \\sim C15 \\sim C29: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C9 \\sim O47 \\sim C73 \\sim C71: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O81 \\sim Ti19 \\sim C59: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O37 \\sim Ti9A \\sim Ti1A \\sim Ti7: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C68 \\sim O35 \\sim C76 \\sim C101: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O48 \\sim Ti1 \\sim C22: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(Ti9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C101) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C75) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C75) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C73) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C76) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O97) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C95) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C68) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C87) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Ti9A(0.5) Ti19(0.5) Ti5A(0.5) Ti11(0.5) Ti9(0.5) Ti9B(0.5)
 Ti1A(0.5) Ti5B(0.5)
6.a Riding coordinates:
 C20(H20), C38(H38A,H38B,H38C), C84(H84A,H84B,H84C), C51(H51A,H51B,H51C),
 C71(H71A,H71B,H71C), C37(H37A,H37B,H37C), C5(H5), C41(H41A,H41B,H41C),
 C87(H87A,H87B,H87C), C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C95(H95),
 C101(H10A,H10B,H10C)
6.b Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C8(H8), C10(H10), C12(H12), C14(H14), C22(H22),
 C30(H30), C32(H32), C54(H54), C56(H56), C62(H62), C68(H68), C72(H72), C96(H96),
  C98(H98), C102(H102), C55(H55), C59(H59), C31(H31), C67(H67), C9(H9),
 C75(H75), C77(H77), C21(H21), C43(H43), C89(H89), C47(H47), C49(H49)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C40(H40A,
 H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C),
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C58(H58A,H58B,
 H58C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C70(H70A,
 H70B,H70C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C),
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C86(H86A,H86B,H86C), C88(H88A,H88B,
 H88C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C),
 C100(H10D,H10E,H10F), C13(H13A,H13B,H13C), C53(H53A,H53B,H53C), C27(H27A,H27B,
 H27C), C7(H7A,H7B,H7C), C57(H57A,H57B,H57C), C29(H29A,H29B,H29C), C15(H15A,
 H15B,H15C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C2(H2A,H2B,H2C),
 C65(H65A,H65B,H65C), C33(H33A,H33B,H33C), C73(H73A,H73B,H73C), C19(H19A,H19B,
 H19C), C39(H39A,H39B,H39C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C83(H83A,
 H83B,H83C), C85(H85A,H85B,H85C), C45(H45A,H45B,H45C), C91(H91A,H91B,H91C),
 C93(H93A,H93B,H93C), C3(H3A,H3B,H3C), C97(H97A,H97B,H97C), C99(H99A,H99B,H99C),
  C25(H25A,H25B,H25C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_platon_squeeze_void_probe_radius 1.20
_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
- Detector area scaling
;