Hybrid dimers based on metal-substituted Keggin polyoxometalates (metal = Ti, Ln) for cyanosilylation catalysis.
An, Haiyan; Zhang, Yumeng; Hou, Yujiao; Hu, Tao; Yang, Wei; Chang, Shenzhen; Zhang, Jianjun; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9079–9089; doi:10.1039/c8dt00389k

data_7046601
_publ_section_title
;
 Hybrid dimers based on metal-substituted Keggin polyoxometalates (metal =
 Ti, Ln) for cyanosilylation catalysis.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9079
_journal_page_last               9089
_journal_paper_doi               10.1039/c8dt00389k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C18 H59 La2 N3 O66.5 P W11'
_chemical_formula_weight         3712.71
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-06-07 deposited with the CCDC.
2018-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                96.428(2)
_cell_angle_beta                 91.620(2)
_cell_angle_gamma                95.623(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0114(5)
_cell_length_b                   14.3598(6)
_cell_length_c                   21.4373(8)
_cell_measurement_reflns_used    27811
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.630
_cell_volume                     3957.9(3)
_computing_data_collection       'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27811
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.630
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.094
_exptl_absorpt_correction_T_max  0.181
_exptl_absorpt_correction_T_min  0.058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.115
_exptl_crystal_description       block
_exptl_crystal_F_000             3325
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.822
_refine_diff_density_min         -3.053
_refine_diff_density_rms         0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         13825
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0721P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10400
_reflns_number_total             13825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00389k2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7046596--7046601.cif.'
_cod_original_formula_sum        'C18 H59 La2 N3 O66.50 P W11'
_cod_database_code               7046601
_shelxl_version_number           2014-3
_shelx_res_checksum              67659
_platon_squeeze_void_probe_radius 1.20