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_1576334
_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         'C56 H104 O16 P4 Ti4'
_chemical_formula_sum            'C56 H104 O16 P4 Ti4'
_chemical_formula_weight         1348.93
_chemical_melting_point          ?
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2024-10-30
_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                90
_cell_angle_beta                 110.585(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9525(18)
_cell_length_b                   15.0452(13)
_cell_length_c                   21.236(2)
_cell_measurement_reflns_used    3908
_cell_measurement_temperature    100
_cell_measurement_theta_max      58
_cell_measurement_theta_min      4
_cell_volume                     6566.0(11)
_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 0.918
_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  0.082
_diffrn_reflns_av_unetI/netI     0.117
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24972
_diffrn_reflns_theta_full        66.281
_diffrn_reflns_theta_max         79.856
_diffrn_reflns_theta_min         3.641
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.427
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2864.000
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.67
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0748
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         4854
_refine_ls_number_restraints     824
_refine_ls_R_factor_all          0.1940
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.0051076
_refine_ls_shift/su_mean         0.0004468
_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         0.3610
_refine_ls_wR_factor_gt          0.2741
_refine_ls_wR_factor_ref         0.3226
_reflns_limit_h_max              25
_reflns_limit_h_min              -27
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                2561
_reflns_number_total             6584
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   6.04
_oxford_diffrn_Wilson_scale      16.22
_oxford_refine_ls_r_factor_ref   0.1490
_oxford_refine_ls_scale          0.3332(12)
_oxford_reflns_number_all        6559
_oxford_structure_analysis_title '_T144\SP_T144b_auto.cif_od At 14:21 on 19/ 4'
_cod_data_source_file            d5sc08522e2.cif
_cod_data_source_block           'global_CCDC1'
_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      'I 2/a '
_cod_database_code               1576334
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)