Photo-redox reactivity of titanium-oxo clusters: mechanistic insight into a two-electron intramolecular process, and structural characterisation of mixed-valent Ti(III)/Ti(IV) products
Kraemer, Tobias; Tuna, Floriana; Pike, Sebastian D.; Chemical Science  (2019) –; doi:10.1039/C9SC01241A

data_1551283
_publ_section_title
;
 Photo-redox reactivity of titanium-oxo clusters: mechanistic insight into
 a two-electron intramolecular process, and structural characterisation of
 mixed-valent Ti(III)/Ti(IV) products
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01241A
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_compound_source        'Lab 301, Dept Chem, Uni Cambridge'
_chemical_formula_moiety         'C72 H60 O16 P6 Ti4'
_chemical_formula_sum            'C72 H60 O16 P6 Ti4'
_chemical_formula_weight         1558.70
_chemical_name_systematic        '[Ti4O4(O2PPh2)6][O2}2'
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-04
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2019-04-24 deposited with the CCDC.    2019-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.069(9)
_cell_length_b                   15.069(9)
_cell_length_c                   15.069(9)
_cell_measurement_reflns_used    4136
_cell_measurement_temperature    180
_cell_measurement_theta_max      117
_cell_measurement_theta_min      8
_cell_volume                     3422(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.214
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4136
_diffrn_reflns_theta_full        58.538
_diffrn_reflns_theta_max         58.538
_diffrn_reflns_theta_min         4.149
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.743
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_recrystallization_method
'single crystal to single crystal transformation'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.68
_refine_diff_density_min         -0.85
_refine_ls_abs_structure_details 'Flack (1983), 215 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.07(8)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         489
_refine_ls_number_restraints     272
_refine_ls_R_factor_all          0.2717
_refine_ls_R_factor_gt           0.1390
_refine_ls_shift/su_max          0.0003973
_refine_ls_shift/su_mean         0.0000617
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +93.43P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2587
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2587
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              1
_reflns_number_gt                180
_reflns_number_total             494
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.36
_oxford_diffrn_Wilson_scale      945.63
_oxford_refine_ls_r_factor_ref   0.2717
_oxford_refine_ls_scale          0.0929(2)
_oxford_reflns_number_all        489
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'SP_B1_0068 in I-43m'
_cod_data_source_file            c9sc01241a2.cif
_cod_data_source_block           7ox
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3421.5176(13)
_cod_original_sg_symbol_Hall     'I -4 2 3 '
_cod_original_sg_symbol_H-M      'I -4 3 m '
_cod_database_code               1551283