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

data_7130223
_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 Na3 O114.998 P1 Sb3 W27.999 Y3, 46.799(O)'
_chemical_formula_sum            'C6 H82 K3 Na21 O148 P Sb3 W28 Y3'
_chemical_formula_weight         8933.37
_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                   30.6654(7)
_cell_length_b                   30.6654(7)
_cell_length_c                   14.5899(4)
_cell_measurement_reflns_used    9423
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      32.535
_cell_measurement_theta_min      2.302
_cell_volume                     11881.7(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32142
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.011
_diffrn_reflns_theta_min         2.074
_diffrn_source
;
sealed X-ray tube
;
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec IuS'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.080
_exptl_absorpt_correction_T_max  0.6056
_exptl_absorpt_correction_T_min  0.3611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0541 after correction.
The Ratio of minimum to maximum transmission is 0.5963.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.746
_exptl_crystal_description       block
_exptl_crystal_F_000             11841
_exptl_crystal_recrystallization_method
'evaporation fromm 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         1.955
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.209
_refine_ls_abs_structure_details
;
 Flack x determined using 2505 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5482
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0674P)^2^+349.1459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.987
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                5309
_reflns_number_total             5482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02223k1.cif
_cod_data_source_block           mo_emas2320_r3m
_cod_original_cell_volume        11881.8(6)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               7130223
_shelx_estimated_absorpt_t_max   0.096
_shelx_estimated_absorpt_t_min   0.096
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8S) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O21) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1S) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(W4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O3S) \\sim Ueq, Uanis(O4S)
\\sim Ueq, Uanis(O22) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O6S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
2. Others
 Fixed Sof: O21(0.3) O22(0.2) O20(0.2) O24(0.3) O3S(0.8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              77992
_shelx_hkl_checksum              88759
_shelx_fab_checksum              42824
_olex2_submission_special_instructions 'No special instructions were received'