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_1568064
_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         'C30.50 H61 O13 Ti3'
_chemical_formula_sum            'C30.5 H61 O13 Ti3'
_chemical_formula_weight         779.51
_chemical_melting_point          ?
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2021-12-16
_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                63.032(3)
_cell_angle_beta                 64.038(2)
_cell_angle_gamma                65.591(3)
_cell_formula_units_Z            2
_cell_length_a                   13.2495(3)
_cell_length_b                   13.4140(4)
_cell_length_c                   14.7584(4)
_cell_measurement_reflns_used    11236
_cell_measurement_temperature    100
_cell_measurement_theta_max      77
_cell_measurement_theta_min      4
_cell_volume                     2024.99(11)
_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      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_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  0.077
_diffrn_reflns_av_unetI/netI     0.096
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29287
_diffrn_reflns_theta_full        71.943
_diffrn_reflns_theta_max         79.937
_diffrn_reflns_theta_min         3.532
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.376
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.51
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.86
_refine_diff_density_min         -1.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8575
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.0059936
_refine_ls_shift/su_mean         0.0001717
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.11P)^2^ + 1.79P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1734
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.1734
_reflns_limit_h_max              16
_reflns_limit_h_min              -14
_reflns_limit_k_max              17
_reflns_limit_k_min              -14
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6928
_reflns_number_total             8575
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.04
_oxford_diffrn_Wilson_scale      0.46
_oxford_refine_ls_r_factor_ref   0.0776
_oxford_refine_ls_scale          1.679(12)
_oxford_reflns_number_all        8575
_oxford_structure_analysis_title 'xcalibur in C:\Users\u1874775\OneDrive - Uni'
_cod_data_source_file            d2sc05671b2.cif
_cod_data_source_block           'global_CCDC1'
_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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C30.50 H61 O13 Ti3'
_cod_database_code               1568064
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)