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_4345380
_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 O58 Sm4 Ti5'
_chemical_formula_weight         4761.52
_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                92.025(4)
_cell_angle_beta                 111.781(4)
_cell_angle_gamma                102.790(4)
_cell_formula_units_Z            2
_cell_length_a                   21.7272(9)
_cell_length_b                   23.2244(13)
_cell_length_c                   27.1406(13)
_cell_measurement_reflns_used    11599
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.5800
_cell_measurement_theta_min      3.8930
_cell_volume                     12297.1(11)
_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 0.702
_diffrn_measured_fraction_theta_max 0.950
_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  0.1382
_diffrn_reflns_av_unetI/netI     0.3146
_diffrn_reflns_Laue_measured_fraction_full 0.702
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61972
_diffrn_reflns_point_group_measured_fraction_full 0.702
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         56.764
_diffrn_reflns_theta_min         3.476
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    8.937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28175
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             4932
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_platon_squeeze_details
;
;
_refine_diff_density_max         2.687
_refine_diff_density_min         -1.015
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2285
_refine_ls_number_reflns         31260
_refine_ls_number_restraints     9568
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.2894
_refine_ls_R_factor_gt           0.1625
_refine_ls_shift/su_max          0.080
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1813P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3723
_refine_ls_wR_factor_ref         0.4386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8318
_reflns_number_total             31260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03072_si_004.cif
_cod_data_source_block           Sm8Ti10
_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        12297.0(11)
_cod_database_code               4345380
_shelx_estimated_absorpt_t_min   0.268
_shelx_estimated_absorpt_t_max   0.535
_platon_sm8ti10_details
;

 The SQUEEZE analysis estimate the electron count to be 1407 
within 3739 ?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              26704
_shelx_hkl_checksum              28689