Making an inverted Keggin ion lacunary.
Liu, Lu-Lu; Xu, Zi-Yu; Yi, Peng; Chen, Chao-Qin; Lang, Zhong-Ling; Yang, Peng; Chemical science 15 (2024) 16977–16986; doi:10.1039/d4sc04634j

data_1573003
_publ_section_title
;
 Making an inverted Keggin ion lacunary.
;
_journal_issue                   41
_journal_name_full               'Chemical science'
_journal_page_first              16977
_journal_page_last               16986
_journal_paper_doi               10.1039/d4sc04634j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C18 H21 As3 Mo10 N3 O41 Se, 0.125[], 0.125[]'
_chemical_formula_sum            'C18 H21 As3 Mo10 N3 O41 Se'
_chemical_formula_weight         2198.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-07-03 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.326(3)
_cell_length_b                   23.4652(19)
_cell_length_c                   24.275(2)
_cell_measurement_reflns_used    9112
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.293
_cell_measurement_theta_min      2.414
_cell_volume                     17844(3)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2492
_diffrn_reflns_av_unetI/netI     0.1034
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            136137
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.123
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.931
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1640 before and 0.0448 after correction.
The Ratio of minimum to maximum transmission is 0.5985.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       block
_exptl_crystal_F_000             8248
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.875
_refine_diff_density_min         -1.870
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         15705
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0922P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12345
_reflns_number_total             15705
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04634j2.cif
_cod_data_source_block           SeMo-1
_cod_database_code               1573003
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O00F) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim
Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq,
Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O20) \\sim Ueq,
Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq,
Uanis(O28) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O31)
\\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O34) \\sim Ueq,
Uanis(O35) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O38)
\\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18)
3.b Idealised Me refined as rotating group:
 N1(H1a,H1b,H1c), N2(H2a,H2b,H2c), N3(H3a,H3b,H3c)
;
_shelx_res_checksum              46741
_shelx_hkl_checksum              2259
_shelx_fab_checksum              29429
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'