Synthesis and photocatalytic H2 evolution properties of four titanium-oxo-clusters based on a cyclohex-3-ene-1-carboxylate ligand.
Gao, Mei-Yan; Chen, Shumei; Hu, Lan-Xia; Zhang, Lei; Zhang, Jian; Dalton transactions (Cambridge, England : 2003)  (2017) –; doi:10.1039/c7dt00627f

data_7043807
_publ_section_title
;
 Synthesis and photocatalytic H2 evolution properties of four
 titanium-oxo-clusters based on a cyclohex-3-ene-1-carboxylate ligand.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt00627f
_journal_year                    2017
_chemical_formula_sum            'C32 H60 O12 Ti3'
_chemical_formula_weight         780.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-18 deposited with the CCDC.
2017-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                96.961(3)
_cell_angle_beta                 108.693(4)
_cell_angle_gamma                109.373(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3849(6)
_cell_length_b                   13.5963(5)
_cell_length_c                   15.4306(7)
_cell_measurement_reflns_used    5170
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.9490
_cell_measurement_theta_min      4.4350
_cell_volume                     2064.10(19)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14218
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.468
_diffrn_reflns_theta_min         3.563
_exptl_absorpt_coefficient_mu    5.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56408
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_exptl_transmission_factor_max   0.207
_exptl_transmission_factor_min   0.141
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8159
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1086P)^2^+0.3512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6242
_reflns_number_total             8159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00627f2.cif
_cod_data_source_block           PTC91
_cod_original_cell_volume        2064.10(18)
_cod_database_code               7043807
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.56408
_shelx_estimated_absorpt_t_max   1.00000
_shelx_res_checksum              63476