Three intersecting {V<sub>12</sub>} rings: {V<sub>30</sub>Sb<sub>8</sub>}, an ultra-large polyoxovanadate cluster shell.
Lühmann, Henning; Näther, Christian; van Leusen, Jan; Kögerler, Paul; Bensch, Wolfgang; Chemical communications (Cambridge, England) 57 (2021) 7661–7664; doi:10.1039/d1cc03028k

data_7128618
_publ_section_title
;
 Three intersecting {V<sub>12</sub>} rings:
 {V<sub>30</sub>Sb<sub>8</sub>}, an ultra-large polyoxovanadate cluster
 shell.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7661
_journal_page_last               7664
_journal_paper_doi               10.1039/d1cc03028k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_sum            'H48 N12 O78 Sb8 V30'
_chemical_formula_weight         3966.70
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-06-08 deposited with the CCDC.	2021-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2776(7)
_cell_length_b                   16.2776(7)
_cell_length_c                   17.7520(9)
_cell_measurement_reflns_used    14821
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.992
_cell_measurement_theta_min      2.503
_cell_volume                     4703.6(4)
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_collection       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14821
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.992
_diffrn_reflns_theta_min         2.503
_exptl_absorpt_coefficient_mu    5.177
_exptl_absorpt_correction_T_max  0.4809
_exptl_absorpt_correction_T_min  0.4385
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.801
_exptl_crystal_description       block
_exptl_crystal_F_000             3708
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.455
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.201
_refine_ls_extinction_coef       0.00032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0666P)^2^+0.1449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2229
_reflns_number_total             2925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03028k2.cif
_cod_data_source_block           hl394neu
_cod_depositor_comments          'Adding full bibliography for 7128618.cif.'
_cod_original_cell_volume        4703.6(5)
_cod_database_code               7128618
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              74500
_shelx_fab_checksum              32342