Synthesis and structural characterization of the heavy tricysteinylpnictines, models of protein-bound As(III), Sb(III), and Bi(III).
Hollow, Sophia E.; Johnstone, Timothy C.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18890–18901; doi:10.1039/d4dt02476a

data_7717579
_publ_section_title
;
 Synthesis and structural characterization of the heavy
 tricysteinylpnictines, models of protein-bound As(III), Sb(III), and
 Bi(III).
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18890
_journal_page_last               18901
_journal_paper_doi               10.1039/d4dt02476a
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C9 H18 As N3 O6 S3'
_chemical_formula_sum            'C9 H18 As N3 O6 S3'
_chemical_formula_weight         435.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-08-28
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-29 deposited with the CCDC.	2024-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.718(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9981(3)
_cell_length_b                   5.10005(13)
_cell_length_c                   26.8857(7)
_cell_measurement_reflns_used    6481
_cell_measurement_temperature    104(6)
_cell_measurement_theta_max      75.6520
_cell_measurement_theta_min      3.8830
_cell_volume                     1641.70(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 42.96a 64-bit (release 27-07-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -72.00  23.00   0.50    2.00    --  -49.16  85.00 -83.00  190
  2  \w    -20.00   6.00   0.50    2.00    --   49.16 -85.00 157.00   52
  3  \w     11.00  42.00   0.50    2.00    --   49.16 -85.00 157.00   62
  4  \w   -150.00-116.00   0.50    4.00    --  -84.25 -85.00 157.00   68
  5  \w    102.00 177.00   0.50    4.00    --  105.75  85.00 -83.00  150
  6  \w     60.00 110.00   0.50    4.00    --  105.75 -85.00 157.00  100
  7  \w   -115.00 -82.00   0.50    2.00    --  -49.16 -57.00-150.00   66
  8  \w   -118.00 -83.00   0.50    2.00    --  -49.16 -57.00 150.00   70
  9  \w   -117.00 -92.00   0.50    2.00    --  -49.16-125.00 -60.00   50
 10  \w     92.00 120.00   0.50    2.00    --   49.16  57.00 -30.00   56
 11  \w     82.00 107.00   0.50    2.00    --   49.16  57.00  90.00   50
 12  \w    -45.00 -17.00   0.50    4.00    --  -84.25  45.00 120.00   56
 13  \w    -45.00 -18.00   0.50    4.00    --  -84.25  45.00 -90.00   54
 14  \w   -136.00 -92.00   0.50    4.00    --  -84.25 -61.00-150.00   88
 15  \w   -116.00 -83.00   0.50    4.00    --  -84.25 -45.00  90.00   66
 16  \w    -84.00 -59.00   0.50    4.00    --  -84.25  85.00 -83.00   50
 17  \w   -147.00-121.00   0.50    4.00    --  -84.25 -45.00  90.00   52
 18  \w     58.00 103.00   0.50    4.00    --  105.75 -95.00 150.00   90
 19  \w    101.00 175.00   0.50    4.00    --  105.75  30.00  60.00  148
 20  \w     34.00 100.00   0.50    4.00    --  105.75 -95.00 -90.00  132
 21  \w     36.00  71.00   0.50    4.00    --  105.75 -61.00 150.00   70
 22  \w     73.00  98.00   0.50    4.00    --  105.75 -95.00-120.00   50
 23  \w     72.00  99.00   0.50    4.00    --  105.75 -95.00  30.00   54
 24  \w     99.00 178.00   0.50    4.00    --  105.75  15.00  30.00  158
 25  \w     35.00  70.00   0.50    4.00    --  105.75 -61.00 -90.00   70
 26  \w     46.00  74.00   0.50    4.00    --  105.75 -77.00  60.00   56
 27  \w     97.00 177.00   0.50    4.00    --  105.75  45.00-120.00  160
 28  \w     37.00  63.00   0.50    4.00    --  105.75 -95.00-120.00   52
 29  \w    109.00 135.00   0.50    4.00    --  105.75  77.00   0.00   52
 30  \w     34.00  74.00   0.50    4.00    --  105.75 -95.00  60.00   80
 31  \w     41.00  66.00   0.50    4.00    --  105.75 -95.00  30.00   50
 32  \w    132.00 178.00   0.50    4.00    --  105.75  77.00 -30.00   92
 33  \w    100.00 128.00   0.50    4.00    --  105.75  77.00 -30.00   56
 34  \w     45.00  70.00   0.50    4.00    --  105.75 -61.00-120.00   50
 35  \w     64.00 103.00   0.50    4.00    --  105.75 -95.00 -30.00   78
 36  \w     43.00 111.00   0.50    4.00    --  105.75-125.00 150.00  136
 37  \w     39.00  72.00   0.50    4.00    --  105.75-125.00   0.00   66
 38  \w     36.00  64.00   0.50    4.00    --  105.75 -61.00 -30.00   56
 39  \w    -49.00 -24.00   0.50    2.00    --  -49.41  85.00 -83.00   50
 40  \w    115.00 140.00   0.50    4.00    --  105.75  85.00 -83.00   50
 41  \w    -49.00 -24.00   0.50    2.00    --  -49.41  85.00 -83.00   50
 42  \w    132.00 158.00   0.50    4.00    --  105.75  90.00  17.00   52
 43  \w     99.00 131.00   0.50    4.00    --  105.75  61.00 -60.00   64
 44  \w    139.00 165.00   0.50    4.00    --  105.75  61.00 -60.00   52
 45  \w     34.00  59.00   0.50    4.00    --  105.75 -61.00-150.00   50
 46  \w     34.00  59.00   0.50    4.00    --  105.75 -61.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0008983000
_diffrn_orient_matrix_UB_12      -0.2143359000
_diffrn_orient_matrix_UB_13      -0.0403446000
_diffrn_orient_matrix_UB_21      0.0847719000
_diffrn_orient_matrix_UB_22      -0.1589557000
_diffrn_orient_matrix_UB_23      0.0332125000
_diffrn_orient_matrix_UB_31      -0.0967742000
_diffrn_orient_matrix_UB_32      -0.1416612000
_diffrn_orient_matrix_UB_33      0.0237898000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9541
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.233
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.667
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.112a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       needle
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2977
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0656P)^2^+3.2344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2811
_reflns_number_total             2977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02476a2.cif
_cod_data_source_block           As(Cys)3
_cod_depositor_comments
'Adding full bibliography for 7717579--7717581.cif.'
_cod_database_code               7717579
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AsS3C9N3O6H18
_chemical_oxdiff_usercomment     'Sh0289- tricysteinyl arsine'
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.00434
 -0.00434
2.a Ternary CH refined with riding coordinates:
 C12(H12), C22(H22), C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C21(H21A,H21B), C31(H31A,H31B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C)
;
_shelx_res_checksum              46527
_shelx_hkl_checksum              270
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.557