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_1573005
_publ_section_title
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 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         'C36 H38 As6 Ce2 Mo20 N6 O94 Se2'
_chemical_formula_sum            'C36 H38 As6 Ce2 Mo20 N6 O94 Se2'
_chemical_formula_weight         4865.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                99.665(4)
_cell_angle_beta                 94.683(4)
_cell_angle_gamma                108.620(4)
_cell_formula_units_Z            1
_cell_length_a                   12.1018(14)
_cell_length_b                   15.6636(19)
_cell_length_c                   22.209(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.293
_cell_measurement_theta_min      2.404
_cell_volume                     3891.5(8)
_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 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            87718
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         2.404
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.941
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1714 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.6060.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_description       block
_exptl_crystal_F_000             2270
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.983
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         19408
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+1.5993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15854
_reflns_number_total             19408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04634j2.cif
_cod_data_source_block           2022030207_0m_sq
_cod_database_code               1573005
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.671
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O4W) \\sim Ueq, Uanis(O4X) \\sim Ueq, Uanis(O6W) \\sim Ueq, Uanis(O6X)
\\sim Ueq, Uanis(O3X) \\sim Ueq, Uanis(O3W) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: O3W(0.75) O3X(0.25) O4W(0.5) O4X(0.5) O6W(0.65) O6X(0.35)
4.a Rotating group:
 N1(H1A,H1B), N2(H2A,H2B)
4.b 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)
4.c Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C)
;
_shelx_res_checksum              7238
_shelx_hkl_checksum              51865
_shelx_fab_checksum              61154
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'