A tetrahedron-shaped polyoxoantimotungstate encapsulating a hexanuclear octahedral lanthanide-oxo cluster for an amperometric bromate sensor.
Yu, Lan; Ye, Jing; Li, Da-Huan; Sun, Yan-Qiong; Li, Xin-Xiong; Zheng, Shou-Tian; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5258–5265; doi:10.1039/d3dt03789d

data_7715167
_publ_section_title
;
 A tetrahedron-shaped polyoxoantimotungstate encapsulating a hexanuclear
 octahedral lanthanide-oxo cluster for an amperometric bromate sensor.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5258
_journal_page_last               5265
_journal_paper_doi               10.1039/d3dt03789d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'0.5(K Na2 Nd6 O144 Sb4 W36), 0.5(K Na Nd6 O144 Sb4 W36)'
_chemical_formula_sum            'K Na1.5 Nd6 O144 Sb4 W36'
_chemical_formula_weight         10348.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-11-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.17 svn.r577a77a9 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-13 deposited with the CCDC.	2024-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.856(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.023(6)
_cell_length_b                   21.827(4)
_cell_length_c                   33.519(7)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.78
_cell_measurement_theta_min      2.17
_cell_volume                     21231(7)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            380145
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.228
_diffrn_reflns_theta_max         25.228
_diffrn_reflns_theta_min         1.532
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.443
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.2982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1515 before and 0.1042 after correction.
The Ratio of minimum to maximum transmission is 0.4002.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.237
_exptl_crystal_description       block
_exptl_crystal_F_000             17662
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.376
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.294
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.395(4)
_refine_ls_extinction_coef       0.000008(2)
_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   1.012
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1974
_refine_ls_number_reflns         75583
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0615P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                63257
_reflns_number_total             75583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03789d2.cif
_cod_data_source_block           fen8_2
_cod_depositor_comments          'Adding full bibliography for 7715167.cif.'
_cod_original_cell_volume        21232(7)
_cod_original_formula_sum        'K Na1.50 Nd6 O144 Sb4 W36'
_cod_database_code               7715167
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.201
_shelx_estimated_absorpt_t_min   0.167
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.605(4)
 0.395(4)
2. Uiso/Uaniso restraints and constraints
O193 \\sim O667: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O273 \\sim O286: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O69 \\sim O276: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(W57) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na3) \\sim Ueq, Uanis(Na2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed X: O217(-0.532371) O272(-0.158899) O273(-0.6185) O274(-0.339099) O275(-
 0.1616) O276(-0.304) O277(-0.136) O278(-0.578) O279(-0.828) O280(-0.596001)
 O281(-0.044001) O283(-0.2075) O284(-0.90199) O285(-0.5988) O286(-0.68024)
 O287(-0.641899) O288(-0.763931) O667(-0.9395)
 Fixed Y: O217(0.13913) O272(0.0909) O273(0.2051) O274(-0.1186) O275(-0.0038)
 O276(0.268201) O277(-0.1215) O278(-0.0453) O279(0.318501) O280(0.087)
 O281(0.322301) O283(0.556) O284(0.2523) O285(0.259549) O286(0.13345)
 O287(0.4149) O288(0.350321) O667(0.118901)
 Fixed Z: O217(-1.103311) O272(-0.9243) O273(-1.0917) O274(-0.5213) O275(-
 0.564601) O276(-0.8466) O277(-0.5187) O278(-0.9353) O279(-0.956699) O280(-
 1.0618) O281(-0.623501) O283(-0.5267) O284(-0.79969) O285(-0.79882) O286(-
 1.07925) O287(-1.0172) O288(-1.027161) O667(-1.0599)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22185
_shelx_fab_checksum              4147
_olex2_submission_special_instructions 'No special instructions were received'