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_1573004
_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
'C12 H13 As2 Mo10 N2 O41 Se1.44, C12 H14 As2 Mo10 N2 O41 Se1.19'
_chemical_formula_sum            'C24 H27 As4 Mo20 N4 O82 Se2.63'
_chemical_formula_weight         4109.64
_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             2024-06-01
_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                91.991(7)
_cell_angle_beta                 99.609(8)
_cell_angle_gamma                90.075(8)
_cell_formula_units_Z            2
_cell_length_a                   13.930(3)
_cell_length_b                   20.189(5)
_cell_length_c                   24.369(6)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.322
_cell_measurement_theta_min      2.607
_cell_volume                     6753(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
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            77446
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.162
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.550
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1743 before and 0.0811 after correction.
The Ratio of minimum to maximum transmission is 0.5416.
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    2.021
_exptl_crystal_description       block
_exptl_crystal_F_000             3833
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         7.396
_refine_diff_density_min         -3.177
_refine_diff_density_rms         0.507
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         23326
_refine_ls_number_restraints     4298
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1878
_refine_ls_R_factor_gt           0.1410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+1083.4930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3559
_refine_ls_wR_factor_ref         0.3731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15266
_reflns_number_total             23326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04634j2.cif
_cod_data_source_block           SeMo10-2
_cod_database_code               1573004
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.567
_shelx_estimated_absorpt_t_min   0.509
_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. Restrained distances
 Mo19-O79
 1.7 with sigma of 0.02
 Mo20-O76
 1.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O01J \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O13 \\sim O14
\\sim O15 \\sim O16 \\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22
\\sim O23 \\sim O24 \\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30
\\sim O31 \\sim O32 \\sim O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38
\\sim O39 \\sim O40 \\sim O41 \\sim O42 \\sim O43 \\sim O44 \\sim O45 \\sim O46
\\sim O7 \\sim O8 \\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O47 \\sim O48
\\sim O49 \\sim O50 \\sim O51 \\sim O52 \\sim O53 \\sim O54 \\sim O55 \\sim O56
\\sim O57 \\sim O58 \\sim O59 \\sim O60 \\sim O61 \\sim O62 \\sim O63 \\sim O64
\\sim O65 \\sim O66 \\sim O67 \\sim O68 \\sim O69 \\sim O70 \\sim O71 \\sim O72
\\sim O73 \\sim O74 \\sim O75 \\sim O76 \\sim O77 \\sim O78 \\sim O79 \\sim O80
\\sim O81: within 5A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 5A
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(N1) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(Se1) \\sim Ueq, Uanis(Se2) \\sim Ueq, Uanis(Se3) \\sim Ueq, Uanis(Se4)
\\sim Ueq, Uanis(Se5) \\sim Ueq, Uanis(Se6) \\sim Ueq, Uanis(Se7) \\sim Ueq,
Uanis(Se8) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O01J) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq,
Uanis(O6) \\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(O41) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O43)
\\sim Ueq, Uanis(O44) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O46) \\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(O47) \\sim Ueq,
Uanis(O48) \\sim Ueq, Uanis(O49) \\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(O51)
\\sim Ueq, Uanis(O52) \\sim Ueq, Uanis(O53) \\sim Ueq, Uanis(O54) \\sim Ueq,
Uanis(O55) \\sim Ueq, Uanis(O56) \\sim Ueq, Uanis(O57) \\sim Ueq, Uanis(O58)
\\sim Ueq, Uanis(O59) \\sim Ueq, Uanis(O60) \\sim Ueq, Uanis(O61) \\sim Ueq,
Uanis(O62) \\sim Ueq, Uanis(O63) \\sim Ueq, Uanis(O64) \\sim Ueq, Uanis(O65)
\\sim Ueq, Uanis(O66) \\sim Ueq, Uanis(O67) \\sim Ueq, Uanis(O68) \\sim Ueq,
Uanis(O69) \\sim Ueq, Uanis(O70) \\sim Ueq, Uanis(O71) \\sim Ueq, Uanis(O72)
\\sim Ueq, Uanis(O73) \\sim Ueq, Uanis(O74) \\sim Ueq, Uanis(O75) \\sim Ueq,
Uanis(O76) \\sim Ueq, Uanis(O77) \\sim Ueq, Uanis(O78) \\sim Ueq, Uanis(O79)
\\sim Ueq, Uanis(O80) \\sim Ueq, Uanis(O81) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
4. Others
 Fixed Sof: Se1(0.32) Se2(0.36) Se3(0.6) Se4(0.16) Se5(0.24) Se6(0.22)
 Se7(0.59) Se8(0.14)
5.a Riding coordinates:
 C24(H24)
5.b Rotating group:
 N2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C17(H17),
 C15(H15), C14(H14), C18(H18), C20(H20), C21(H21), C23(H23)
5.d Fitted hexagon refined as free rotating group:
 C17(C16,C15,C14,C13,C18), C20(C21,C22,C23,C24,C19)
5.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N3(H3A,H3B,H3C), N4(H4A,H4B,H4C)
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_shelx_res_checksum              83498
_shelx_hkl_checksum              46954
_shelx_fab_checksum              91162
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'