A 4-dimethylaminobenzoate-functionalized Ti <sub>6</sub> -oxo cluster with a narrow band gap and enhanced photoelectrochemical activity: a combined experimental and computational study
Lv, Hai-Ting; Cui, Ying; Zhang, Yu-Min; Li, Hua-Min; Zou, Guo-Dong; Duan, Rui-Huan; Cao, Jun-Tao; Jing, Qiang-Shan; Fan, Yang; Dalton Transactions 46 (2017) 12313–12319; doi:10.1039/C7DT02650A

data_1546856
_publ_section_title
;
 A 4-dimethylaminobenzoate-functionalized Ti <sub>6</sub> -oxo cluster
 with a narrow band gap and enhanced photoelectrochemical activity: a
 combined experimental and computational study
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              12313
_journal_page_last               12319
_journal_paper_doi               10.1039/C7DT02650A
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C72 H102 N6 O24 Ti6, 2(C7 H8)'
_chemical_formula_sum            'C86 H118 N6 O24 Ti6'
_chemical_formula_weight         1907.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.380(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6329(11)
_cell_length_b                   16.0739(7)
_cell_length_c                   27.4246(11)
_cell_measurement_reflns_used    6010
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.4190
_cell_measurement_theta_min      3.1460
_cell_volume                     9633.2(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'DIAMOND. Version 3.2k. Crystal Impact'
_computing_publication_material  'Windows Word 2010'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.1213
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23090
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.887
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       Block
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         9444
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+17.2642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1350
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7292
_reflns_number_total             9444
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02650a2.cif
_cod_data_source_block           C1
_cod_database_code               1546856
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              22473