Three ring-shaped Zr(iv)-substituted silicotungstates: syntheses, structures and their properties.
Zhang, Zhong; Wang, Yue-Lin; Liu, Yan; Huang, Sheng-Li; Yang, Guo-Yu; Nanoscale 12 (2020) 18333–18341; doi:10.1039/d0nr02945a

data_1558791
_publ_section_title
;
 Three ring-shaped Zr(iv)-substituted silicotungstates: syntheses,
 structures and their properties.
;
_journal_issue                   35
_journal_name_full               Nanoscale
_journal_page_first              18333
_journal_page_last               18341
_journal_paper_doi               10.1039/d0nr02945a
_journal_volume                  12
_journal_year                    2020
_chemical_formula_sum            'C12 H88 N8 O168 Si4 W40 Zr8'
_chemical_formula_weight         11228.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-07-17 deposited with the CCDC.	2020-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                67.484(2)
_cell_angle_beta                 82.137(2)
_cell_angle_gamma                88.158(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7819(2)
_cell_length_b                   20.9415(5)
_cell_length_c                   21.9893(6)
_cell_measurement_reflns_used    16939
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5325
_cell_measurement_theta_min      2.8017
_cell_volume                     4963.5(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47834
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.807
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    23.588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21519
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.757
_exptl_crystal_description       needle
_exptl_crystal_F_000             4894
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         7.140
_refine_diff_density_min         -5.612
_refine_diff_density_rms         0.482
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         17439
_refine_ls_number_restraints     350
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0759
_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^)+(0.1011P)^2^+345.6176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13077
_reflns_number_total             17439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr02945a2.cif
_cod_data_source_block           x_sqd
_cod_depositor_comments
'Adding full bibliography for 1558789--1558791.cif.'
_cod_database_code               1558791
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.116
_shelx_estimated_absorpt_t_max   0.254
_shelx_res_checksum              55417
_shelx_fab_checksum              95083