Photoactivation of titanium-oxo cluster [Ti<sub>6</sub>O<sub>6</sub>(OR)<sub>6</sub>(O<sub>2</sub>C <sup><i>t</i></sup> Bu)<sub>6</sub>]: mechanism, photoactivated structures, and onward reactivity with O<sub>2</sub> to a peroxide complex.
Brown, Stephen E.; Mantaloufa, Ioanna; Andrews, Ryan T.; Barnes, Thomas J.; Lees, Martin R.; De Proft, Frank; Cunha, Ana V.; Pike, Sebastian D.; Chemical science 14 (2023) 675–683; doi:10.1039/d2sc05671b

data_1568063
_publ_section_title
;
 Photoactivation of titanium-oxo cluster
 [Ti<sub>6</sub>O<sub>6</sub>(OR)<sub>6</sub>(O<sub>2</sub>C
 <sup><i>t</i></sup> Bu)<sub>6</sub>]: mechanism, photoactivated
 structures, and onward reactivity with O<sub>2</sub> to a peroxide
 complex.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              675
_journal_page_last               683
_journal_paper_doi               10.1039/d2sc05671b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C55.00 H104.00 O24 Ti6'
_chemical_formula_sum            'C55 H104 O24 Ti6'
_chemical_formula_weight         1436.82
_chemical_melting_point          ?
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2021-07-09
_audit_creation_method           CRYSTALS_ver_14.61_build_6999
_audit_update_record
;
2022-06-30 deposited with the CCDC.	2022-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.49600(10)
_cell_length_b                   15.49600(10)
_cell_length_c                   53.7557(7)
_cell_measurement_reflns_used    32728
_cell_measurement_temperature    150
_cell_measurement_theta_max      79
_cell_measurement_theta_min      3
_cell_volume                     11178.78(18)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.208
_diffrn_reflns_av_unetI/netI     0.093
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            49859
_diffrn_reflns_theta_full        78.190
_diffrn_reflns_theta_max         79.786
_diffrn_reflns_theta_min         3.394
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.781
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4548.000
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.98
_refine_diff_density_min         -1.46
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.9014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     444
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.1217
_refine_ls_shift/su_max          0.0118560
_refine_ls_shift/su_mean         0.0003530
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.20P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3993
_refine_ls_wR_factor_gt          0.3932
_refine_ls_wR_factor_ref         0.3940
_reflns_limit_h_max              9
_reflns_limit_h_min              -19
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              68
_reflns_limit_l_min              0
_reflns_number_gt                4716
_reflns_number_total             5387
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.58
_oxford_diffrn_Wilson_scale      6.02
_oxford_refine_ls_r_factor_ref   0.1219
_oxford_refine_ls_scale          0.507(4)
_oxford_reflns_number_all        5367
_oxford_structure_analysis_title '\SP_T29\T29_3a_auto.cif_od At 11:56 on 13/ 5'
_cod_data_source_file            d2sc05671b2.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1568063--1568068.cif.
;
_cod_original_cell_volume        11178.78(19)
_cod_original_sg_symbol_H-M      'R -3 '
_cod_original_formula_sum        'C55.00 H104.00 O24 Ti6'
_cod_database_code               1568063
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)