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

data_7130222
_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 H80 Gd3 K3 Na21 O147 P1 Sb3 W28, 39(O)'
_chemical_formula_sum            'C6 H80 Gd3 K3 Na21 O147 P Sb3 W28'
_chemical_formula_weight         9120.56
_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'
_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                   30.6714(12)
_cell_length_b                   30.6714(12)
_cell_length_c                   14.4221(8)
_cell_measurement_reflns_used    39335
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.08
_cell_volume                     11749.7(9)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'EIGER2 500K'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 2500 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  0.0720
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29428
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.342
_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    22.480
_exptl_absorpt_correction_T_max  0.0776
_exptl_absorpt_correction_T_min  0.0335
_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            'light yellow'
_exptl_crystal_density_diffrn    3.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12036
_exptl_crystal_recrystallization_method
'evaporation from aqueous buffer solution'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.494
_refine_diff_density_min         -2.065
_refine_diff_density_rms         0.305
_refine_ls_abs_structure_details
;
 Flack x determined using 1603 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5006
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                3911
_reflns_number_total             5006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02223k1.cif
_cod_data_source_block           elta2431_gd
_cod_original_cell_volume        11749.7(11)
_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               7130222
_shelx_estimated_absorpt_t_max   0.212
_shelx_estimated_absorpt_t_min   0.133
_olex2_refinement_description
;
1. Restrained distances
 C2-C1
 1.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O30) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(O26) \\sim Ueq, Uanis(O1S) \\sim Ueq, Uanis(O2S) \\sim Ueq, Uanis(O4S)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O14S) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O20)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O24) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O5S) \\sim Ueq, Uanis(O21)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Na1) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O6S)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O21) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O7S) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(W5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(W1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq, Uanis(O10S) \\sim Ueq, Uanis(O12S) \\sim Ueq, Uanis(O8S)
\\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O9S) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O31) \\sim Ueq, Uanis(O22) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O11S) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) = Uanis(C1)
Uanis(O1) = Uanis(O6)
Uanis(O17) = Uanis(O30)
3. Others
 Fixed Sof: O22(0.3802) O27(0.5)
;
_shelx_res_checksum              36999
_shelx_hkl_checksum              8997
_olex2_submission_special_instructions 'No special instructions were received'