Construction of polyoxometalates from dynamic lacunary polyoxotungstate building blocks and lanthanide linkers.
Li, Lu-Lu; Han, Hua-Yan; Wang, Yong-Hui; Tan, Hua-Qiao; Zang, Hong-Ying; Li, Yang-Guang; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11429–11436; doi:10.1039/c5dt00686d

data_7035268
_publ_section_title
;
 Construction of polyoxometalates from dynamic lacunary polyoxotungstate
 building blocks and lanthanide linkers.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11429
_journal_page_last               11436
_journal_paper_doi               10.1039/c5dt00686d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C12 H138 K2 Li16 N2 Na6 O209 Sb10 Tb4 W36'
_chemical_formula_weight         12454.20
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-04-17 deposited with the CCDC.
2015-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 77.005(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.1737(14)
_cell_length_b                   23.009(2)
_cell_length_c                   32.566(3)
_cell_measurement_reflns_used    64658
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0336
_cell_measurement_theta_min      2.2465
_cell_volume                     11078.6(17)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Oscillation
_diffrn_measurement_method       0.01
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1262
_diffrn_reflns_av_unetI/netI     0.1393
_diffrn_reflns_laue_measured_fraction_full 0.972
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            63232
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.559
_diffrn_source                   'Rigaku R-AXIS RAPID IP'
_exptl_absorpt_coefficient_mu    21.217
_exptl_absorpt_correction_T_max  0.101
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.733
_exptl_crystal_description       block
_exptl_crystal_F_000             10964
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         2.846
_refine_diff_density_min         -2.634
_refine_diff_density_rms         0.475
_refine_ls_extinction_coef       0.000048(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1093
_refine_ls_number_reflns         19489
_refine_ls_number_restraints     531
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1405
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12211
_reflns_number_total             19489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00686d2.cif
_cod_data_source_block           Tb-3
_cod_depositor_comments
'Adding full bibliography for 7035268--7035272.cif.'
_cod_original_cell_volume        11078.7(17)
_cod_database_code               7035268
_audit_block_doi                 10.5517/cc13z4px
_shelx_estimated_absorpt_t_min   0.089
_shelx_estimated_absorpt_t_max   0.101
_shelxl_version_number           2014-3
_shelx_res_checksum              79303