Switching on photoreactivity in Ti4-oxo clusters by increasing the size of 1,n-alkane diolate bridging ligands
Chikara, Ashwani; Veale, Alexander R.; Brown, Stephen E.; Woolley, Jack M.; De Proft, Frank; Pike, Sebastian D.; Chemical Science  (2025) –; doi:10.1039/D5SC08522E

data_1576337
_publ_section_title
;
 Switching on photoreactivity in Ti4-oxo clusters by increasing the size
 of 1,n-alkane diolate bridging ligands
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC08522E
_journal_year                    2025
_chemical_formula_moiety         'C68.50 H72 O16 P4 Ti4'
_chemical_formula_sum            'C68.5 H72 O16 P4 Ti4'
_chemical_formula_weight         1466.81
_chemical_melting_point          ?
_chemical_name_systematic        Ti4O4(O2PPh2)4(OCH2CH2CH2CH2CH2O)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             2023-08-08
_audit_creation_method           CRYSTALS_ver_14.61_build_6999
_audit_update_record
;
2025-06-30 deposited with the CCDC.	2025-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                93.84(2)
_cell_angle_beta                 92.043(13)
_cell_angle_gamma                109.294(9)
_cell_formula_units_Z            2
_cell_length_a                   12.8917(9)
_cell_length_b                   16.379(2)
_cell_length_c                   17.2133(12)
_cell_measurement_reflns_used    6875
_cell_measurement_temperature    100
_cell_measurement_theta_max      73
_cell_measurement_theta_min      3
_cell_volume                     3416.4(6)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_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
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_unetI/netI     0.054
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            71565
_diffrn_reflns_theta_full        67.375
_diffrn_reflns_theta_max         86.379
_diffrn_reflns_theta_min         2.868
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.280
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1518
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         13768
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.0096631
_refine_ls_shift/su_mean         0.0000638
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 8.46P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1412
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1412
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                11907
_reflns_number_total             13827
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.95
_oxford_diffrn_Wilson_scale      0.62
_oxford_refine_ls_r_factor_ref   0.0596
_oxford_refine_ls_scale          1.231(4)
_oxford_reflns_number_all        13768
_oxford_structure_analysis_title 'P_T127\SP_T127_auto.cif_od At 11:27 on 20/ 6'
_cod_data_source_file            d5sc08522e2.cif
_cod_data_source_block           'global_CCDC4'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C68.50 H72 O16 P4 Ti4'
_cod_database_code               1576337
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)