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_1551286
_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. Cabridge, Chem Dept, Lab 301'
_chemical_formula_moiety         'C136 H159.00 O32 P8 Ti8'
_chemical_formula_sum            'C136 H159 O32 P8 Ti8'
_chemical_formula_weight         2936.74
_chemical_name_systematic        '[TiO(OtBu)(O2PPh2)]4'
_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             2018-03-14
_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                96.740(2)
_cell_angle_beta                 93.665(3)
_cell_angle_gamma                102.553(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2500(3)
_cell_length_b                   16.5507(3)
_cell_length_c                   33.5428(10)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     7100.0(3)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.8.2-g5331de77-release'
_computing_data_collection       'PILATUS_2M_S_N_24_0107_Diamond '
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.8.2-g5331de77-release
pointless (Evans, P., 2006)
XIA2 0.5.476-ge008241c-dials-1.8 (Winter, G., 2010)
;
_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(2)
_diffrn_detector                 'Photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.728
_diffrn_measured_fraction_theta_max 0.608
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            44780
_diffrn_reflns_theta_full        25.169
_diffrn_reflns_theta_max         35.955
_diffrn_reflns_theta_min         0.595
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.588
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.048: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3054
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.43
_refine_diff_density_min         -1.70
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.3078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1847
_refine_ls_number_reflns         22022
_refine_ls_number_restraints     3696
_refine_ls_R_factor_all          0.1718
_refine_ls_R_factor_gt           0.1100
_refine_ls_shift/su_max          10.8149014
_refine_ls_shift/su_mean         0.0589012
_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         0.3843
_refine_ls_wR_factor_gt          0.3587
_refine_ls_wR_factor_ref         0.3843
_reflns_limit_h_max              15
_reflns_limit_h_min              -13
_reflns_limit_k_max              27
_reflns_limit_k_min              -27
_reflns_limit_l_max              55
_reflns_limit_l_min              0
_reflns_number_gt                11050
_reflns_number_total             44780
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.65
_oxford_diffrn_Wilson_scale      21.26
_oxford_refine_ls_r_factor_ref   0.1718
_oxford_refine_ls_scale          0.14383(15)
_oxford_reflns_number_all        22022
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'shelxt in P -1'
_cod_data_source_file            c9sc01241a2.cif
_cod_data_source_block           5Bu4
_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.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        7100.0(2)
_cod_original_sg_symbol_Hall     '- P1'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C136 H159.00 O32 P8 Ti8'
_cod_database_code               1551286