Syntheses, structures, properties and DFT study of hybrid inorganic-organic architectures constructed from trinuclear lanthanide frameworks and Keggin-type polyoxometalates.
Mirzaei, Masoud; Eshtiagh-Hosseini, Hossein; Lotfian, Nahid; Salimi, Alireza; Bauzá, Antonio; Van Deun, Rik; Decadt, Roel; Barceló-Oliver, Miquel; Frontera, Antonio; Dalton transactions (Cambridge, England : 2003) 43 (2014) 1906–1916; doi:10.1039/c3dt51971f

data_7028386
_publ_section_title
;
 Syntheses, structures, properties and DFT study of hybrid
 inorganic-organic architectures constructed from trinuclear lanthanide
 frameworks and Keggin-type polyoxometalates.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1906
_journal_page_last               1916
_journal_paper_doi               10.1039/c3dt51971f
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'O40 Si W12, 4(C5 H6 N), O'
_chemical_formula_sum            'C20 H24 N4 O41 Si W12'
_chemical_formula_weight         3210.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2013-10-17T13:20:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5140(4)
_cell_length_b                   20.8786(7)
_cell_length_c                   14.0532(4)
_cell_measurement_reflns_used    4740
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      2.467
_cell_measurement_wavelength     0.71073
_cell_volume                     4845.4(2)
_computing_cell_refinement       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_collection       'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_data_reduction        'X-Area 1.31 (Stoe & Cie GmbH, 2005)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1462
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24070
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.467
_exptl_absorpt_coefficient_mu    28.494
_exptl_absorpt_correction_T_max  0.0280
_exptl_absorpt_correction_T_min  0.0097
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5608
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_exptl_crystal_size_rad          0.1500
_refine_diff_density_max         3.79
_refine_diff_density_min         -4.611
_refine_diff_density_rms         0.492
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     385
_refine_ls_number_reflns         4740
_refine_ls_number_restraints     467
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.1011
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+709.8214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2104
_reflns_number_gt                3927
_reflns_number_total             4740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51971f.txt
_cod_data_source_block           shelx
_cod_database_code               7028386
_exptl_absorpt_correction_t_ave  0.0208