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_1551281
_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_compound_source        'Uni. of Cambridge, Chem. Dept, lab 301'
_chemical_formula_moiety         'C60 H116.00 O16 P4 Ti4'
_chemical_formula_sum            'C60 H116 O16 P4 Ti4'
_chemical_formula_weight         1409.07
_chemical_name_systematic        '[TiO(OiPr)(Cy2PO2)]4'
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_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            8
_cell_length_a                   15.2031(9)
_cell_length_b                   21.8563(13)
_cell_length_c                   43.312(3)
_cell_measurement_reflns_used    22823
_cell_measurement_temperature    180
_cell_measurement_theta_max      67
_cell_measurement_theta_min      1
_cell_volume                     14391.9(16)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.037
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            21757
_diffrn_reflns_theta_full        66.793
_diffrn_reflns_theta_max         66.793
_diffrn_reflns_theta_min         4.683
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.973
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6016.005
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9833
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3178
_refine_ls_number_restraints     324
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.0342010
_refine_ls_shift/su_mean         0.0017220
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.13P)^2^ +35.84P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1872
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1872
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              51
_reflns_limit_l_min              0
_reflns_number_gt                2693
_reflns_number_total             3192
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.34
_oxford_diffrn_Wilson_scale      653.39
_oxford_refine_ls_r_factor_ref   0.0661
_oxford_refine_ls_scale          0.044963(16)
_oxford_reflns_number_all        3178
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'SP_B2_0001 in F d d d'
_cod_data_source_file            c9sc01241a2.cif
_cod_data_source_block           4
_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        14391.8(9)
_cod_original_sg_symbol_H-M      'F d d d '
_cod_original_formula_sum        'C60 H116.00 O16 P4 Ti4'
_cod_database_code               1551281