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_1551285
_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 Cambridge, Chem dept, Lab 301'
_chemical_formula_moiety         'C21 H43 O5 P1 Ti1'
_chemical_formula_sum            'C21 H43 O5 P Ti'
_chemical_formula_weight         454.44
_chemical_name_systematic        '[Ti(OiPr)3(Cy2PO2)]2'
_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             2017-03-15
_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                92.5897(7)
_cell_angle_beta                 100.6998(7)
_cell_angle_gamma                93.1673(9)
_cell_formula_units_Z            4
_cell_length_a                   13.6325(2)
_cell_length_b                   13.7555(2)
_cell_length_c                   14.7582(2)
_cell_measurement_reflns_used    21549
_cell_measurement_temperature    180
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     2710.88(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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 0.979
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37059
_diffrn_reflns_theta_full        25.234
_diffrn_reflns_theta_max         27.428
_diffrn_reflns_theta_min         1.485
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984.000
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         12073
_refine_ls_number_restraints     1156
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.0036598
_refine_ls_shift/su_mean         0.0001719
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.18P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1404
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1403
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                8638
_reflns_number_total             12120
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.37
_oxford_diffrn_Wilson_scale      5.45
_oxford_refine_ls_r_factor_ref   0.0866
_oxford_refine_ls_scale          0.4879(6)
_oxford_reflns_number_all        12076
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'SP_K3_0001 At 11:26 on 15/ 2'
_cod_data_source_file            c9sc01241a2.cif
_cod_data_source_block           1
_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        2710.88(4)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C21 H43 O5 P1 Ti1'
_cod_database_code               1551285