Heterometallic Lanthanide-Titanium Oxo Clusters: A New Family of Water Oxidation Catalysts.
Lu, Dong-Fei; Kong, Xiang-Jian; Lu, Tong-Bu; Long, La-Sheng; Zheng, Lan-Sun; Inorganic chemistry 56 (2017) 1057–1060; doi:10.1021/acs.inorgchem.6b03072

data_4345382
_publ_section_title
;
 Heterometallic Lanthanide-Titanium Oxo Clusters: A New Family of Water
 Oxidation Catalysts.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1057
_journal_page_last               1060
_journal_paper_doi               10.1021/acs.inorgchem.6b03072
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C224 H300 Gd4 O58 Ti5'
_chemical_formula_weight         4789.12
_chemical_name_systematic
;
 ?
;
_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-2013
_cell_angle_alpha                91.204(3)
_cell_angle_beta                 112.068(4)
_cell_angle_gamma                104.052(4)
_cell_formula_units_Z            2
_cell_length_a                   21.7883(9)
_cell_length_b                   23.4738(11)
_cell_length_c                   27.2517(9)
_cell_measurement_reflns_used    13607
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.1980
_cell_measurement_theta_min      3.7520
_cell_volume                     12432.3(10)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4741
_diffrn_measured_fraction_theta_full 0.843
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1376
_diffrn_reflns_av_unetI/netI     0.1987
_diffrn_reflns_Laue_measured_fraction_full 0.843
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            64200
_diffrn_reflns_point_group_measured_fraction_full 0.843
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.939
_diffrn_reflns_theta_min         3.364
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30663
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             4948
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
;
_refine_diff_density_max         1.614
_refine_diff_density_min         -1.085
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2285
_refine_ls_number_reflns         37911
_refine_ls_number_restraints     9524
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.2525
_refine_ls_R_factor_gt           0.1459
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3500
_refine_ls_wR_factor_ref         0.4044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13601
_reflns_number_total             37911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03072_si_003.cif
_cod_data_source_block           Gd8Ti10
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        12432.5(9)
_cod_database_code               4345382
_shelx_estimated_absorpt_t_min   0.277
_shelx_estimated_absorpt_t_max   0.672
_platon_gd8ti10_details
;

 The SQUEEZE analysis estimate the electron count to be 1878 
within 3917 ?3 void per formula unit. According to the electron counts and 
the void per formula unit, there are 10 guest water and 10 THF
and 2 tert-butylbenzoic acid. 
However, they are however severely disordered and were therefore 
removed by SQUEEZE in structural refinement.
;
_shelxl_version_number           2013-2
_shelx_res_checksum              68403
_shelx_hkl_checksum              57544