Octahedron-shaped three-shell Ln14-substituted polyoxotungstogermanates encapsulating a W4O15 cluster: luminescence and frequency dependent magnetic properties
Wang, Yong-Jiang; Wu, Shi-Yu; Sun, Yan-Qiong; Li, Xin-Xiong; Zheng, Shou-Tian; Chemical Communications  (2019) –; doi:10.1039/C9CC00073A

data_7122931
_publ_section_title
;
 Octahedron-shaped three-shell Ln14-substituted polyoxotungstogermanates
 encapsulating a W4O15 cluster: luminescence and frequency dependent
 magnetic properties
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00073A
_journal_year                    2019
_chemical_formula_moiety         'Ge6 Na15.57 O283.65 Tb13.92 W68, 4.53(O)'
_chemical_formula_sum            'Ge6 Na15.66 O297.11 Tb13.92 W68'
_chemical_formula_weight         20263.29
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-08-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-11 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                97.093(2)
_cell_angle_beta                 96.008(2)
_cell_angle_gamma                97.663(2)
_cell_formula_units_Z            2
_cell_length_a                   24.294(2)
_cell_length_b                   25.167(2)
_cell_length_c                   27.200(3)
_cell_measurement_reflns_used    9589
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.31
_cell_volume                     16231(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            101517
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.52
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    27.636
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             17356
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details          ' ?'
_refine_diff_density_max         9.399
_refine_diff_density_min         -9.993
_refine_diff_density_rms         0.577
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2065
_refine_ls_number_reflns         55575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+2211.2632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1766
_reflns_number_gt                41343
_reflns_number_total             55575
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc00073a2.cif
_cod_data_source_block           a
_cod_database_code               7122931
_olex2_refinement_description
;
1. Others
 Fixed Sof: O5(0.5) O258(0.75) O259(0.5) O260(0.33333) O266(0.5) O289(0.5)
 O297(0.33333) O298(0.5)
;
_olex2_submission_special_instructions 'No special instructions were received'