Interplay between geometry, electron density, and polarizability of the controversial drug atoxyl in crystal and biological environments
Balmohammadi, Yaser; Metry, Eduardo; Malaspina, Lorraine A.; Cametti, Georgia; Nakamura, Yuiga; Grabowsky, Simon; RSC Advances 15 (2025) 46749–46760; doi:10.1039/D5RA05936D

data_7251382
_publ_section_title
;
 Interplay between geometry, electron density, and polarizability of the
 controversial drug atoxyl in crystal and biological environments
;
_journal_issue                   54
_journal_name_full               'RSC Advances'
_journal_page_first              46749
_journal_page_last               46760
_journal_paper_doi               10.1039/D5RA05936D
_journal_volume                  15
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C6 H8 As N O3'
_chemical_formula_sum            'C6 H8 As N O3'
_chemical_formula_weight         217.057
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-10-02 deposited with the CCDC.	2025-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0397(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.23467(5)
_cell_length_b                   6.13615(4)
_cell_length_c                   8.69951(5)
_cell_measurement_reflns_used    72498
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      76.7250
_cell_measurement_theta_min      3.3550
_cell_volume                     379.051(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.9974
_diffrn_reflns_Laue_measured_fraction_max 0.9995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            156885
_diffrn_reflns_point_group_measured_fraction_full 0.9985
_diffrn_reflns_point_group_measured_fraction_max 0.9997
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         49.84
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    4.438
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             216.396
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.2943
_refine_diff_density_min         -0.2139
_refine_diff_density_rms         0.0406
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.0013(16)
_refine_ls_d_res_high            0.4650
_refine_ls_d_res_low             6.0598
_refine_ls_goodness_of_fit_ref   0.8278
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     197
_refine_ls_number_reflns         7911
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.8268
_refine_ls_R_factor_all          0.0104
_refine_ls_R_factor_gt           0.0094
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0199
_refine_ls_wR_factor_ref         0.0201
_reflns_Friedel_coverage         1.000
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              18
_reflns_limit_l_min              -18
_reflns_number_gt                7620
_reflns_number_total             7911
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ra05936d2.cif
_cod_data_source_block           Arsanilic_Acid_G4
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7251382
_olex2_refinement_description
;
1. Rigid bond restraints
 As1, O1, O2, O3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
2. Uiso/Uaniso restraints and constraints
Uanis(H1b) \\sim Ueq, Uanis(H3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         wB97X
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   2
   DATE:           2023-06-14_16-10-26
;
_olex2_submission_special_instructions 'No special instructions were received'