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_1551282
_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, Chemistry, 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]'
_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     other
_audit_creation_date             2018-10-17
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2019-03-09 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                   15.0884(5)
_cell_length_b                   15.0884(5)
_cell_length_c                   15.0884(5)
_cell_measurement_reflns_used    6439
_cell_measurement_temperature    180
_cell_measurement_theta_max      134
_cell_measurement_theta_min      8
_cell_volume                     3435.0(2)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_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  0.059
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6134
_diffrn_reflns_theta_full        66.875
_diffrn_reflns_theta_max         66.875
_diffrn_reflns_theta_min         4.143
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.721
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.38
_refine_ls_abs_structure_details 'Flack (1983), 262 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         597
_refine_ls_number_restraints     244
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.0113563
_refine_ls_shift/su_mean         0.0010846
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ + 1.28P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1193
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1193
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              1
_reflns_number_gt                534
_reflns_number_total             601
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.82
_oxford_diffrn_Wilson_scale      340.25
_oxford_refine_ls_r_factor_ref   0.0473
_oxford_refine_ls_scale          0.07349(6)
_oxford_reflns_number_all        597
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'SP_B1_0096 in I-43m'
_cod_data_source_file            c9sc01241a2.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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.

'_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        3435.02(11)
_cod_original_sg_symbol_Hall     'I -4 2 3 '
_cod_original_sg_symbol_H-M      'I -4 3 m '
_cod_database_code               1551282