Trisubstituted 4f – and 4d Tungstoantimonates as artificial Phosphoesterases for Nerve Agent Degradation
Tanuhadi, Elias; Rompel, Annette; Chemical Communications  (2022) –; doi:10.1039/D2CC02223K

data_7130225
_publ_section_title
;
 Trisubstituted 4f -- and 4d Tungstoantimonates as artificial
 Phosphoesterases for Nerve Agent Degradation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02223K
_journal_year                    2022
_chemical_formula_moiety         'C6 K3 Na21 O148 P Sb3 W28 Yb3, 28.5(O)'
_chemical_formula_sum            'C6 H80 K3 Na21 O147 P Sb3 W28 Yb3'
_chemical_formula_weight         9167.93
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_primary     direct
_audit_creation_date             2022-06-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-05 deposited with the CCDC.	2022-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   30.5334(6)
_cell_length_b                   30.5334(6)
_cell_length_c                   14.4965(4)
_cell_measurement_reflns_used    100211
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.91
_cell_measurement_theta_min      2.09
_cell_volume                     11704.3(5)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 500K'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      '9595 frames, detector distance = 40 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1124
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            160304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.711
_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'Axo Mo'
_diffrn_source_current           0.830
_diffrn_source_power             0.050
_diffrn_source_type              'Incoatec IuS'
_diffrn_source_voltage           60
_exptl_absorpt_coefficient_mu    23.090
_exptl_absorpt_correction_T_max  0.0129
_exptl_absorpt_correction_T_min  0.0025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             12090
_exptl_crystal_recrystallization_method
'evaporation from aqueous buffer solution'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.918
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.336
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_coef       0.000069(9)
_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   0.967
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         4704
_refine_ls_number_restraints     1039
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0857P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3713
_reflns_number_total             4704
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02223k1.cif
_cod_data_source_block           elta2431_yb
_cod_original_cell_volume        11704.3(6)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               7130225
_shelx_estimated_absorpt_t_max   0.091
_shelx_estimated_absorpt_t_min   0.091
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9568
 0.0432
2. Restrained distances
 C1-C2
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
Uanis(O37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O27) \\sim Ueq, Uanis(O2S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O38) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O35) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33)
\\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O34) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Na1(0.5) O5S(0.5) O26(0.6) O4S(0.25) Na3(0.25) O32(0.25) O34(0.25)
 O33(0.25) O35(0.25) O37(0.25) O40(0.4)
;
_shelx_res_checksum              17194
_shelx_hkl_checksum              1892
_olex2_submission_special_instructions 'No special instructions were received'