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_7717580
_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 N3 O6 S3 Sb'
_chemical_formula_sum            'C9 H18 N3 O6 S3 Sb'
_chemical_formula_weight         482.19
_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     dual
_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                 94.891(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1577(8)
_cell_length_b                   5.0648(4)
_cell_length_c                   27.3420(15)
_cell_measurement_reflns_used    1362
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      76.5170
_cell_measurement_theta_min      3.2070
_cell_volume                     1677.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -54.00  21.00   0.50    0.05    --  -49.41 100.00 148.00  150
  2  \w    -73.00 -35.00   0.50    0.05    --  -84.25 100.00 148.00   76
  3  \w    -50.00 -25.00   0.50    0.05    --  -84.25  45.00   0.00   50
  4  \w    -40.00 -14.00   0.50    0.05    --  -84.25  45.00 -60.00   52
  5  \w    -50.00 -25.00   0.50    0.05    --  -84.25  45.00 -90.00   50
  6  \w     82.00 107.00   0.50    0.05    --   49.41  57.00-150.00   50
  7  \w     88.00 113.00   0.50    0.05    --   49.41  57.00-180.00   50
  8  \w     83.00 108.00   0.50    0.05    --   49.41  57.00-120.00   50
  9  \w     84.00 111.00   0.50    0.05    --   49.41  57.00   0.00   54
 10  \w    112.00 176.00   0.50    0.05    --  105.75  30.00-120.00  128
 11  \w    138.00 171.00   0.50    0.05    --  105.75  45.00-150.00   66
 12  \w     97.00 131.00   0.50    0.05    --  105.75  45.00-150.00   68
 13  \w    128.00 177.00   0.50    0.05    --  105.75  30.00 -90.00   98
 14  \w    109.00 166.00   0.50    0.05    --  105.75  45.00   0.00  114
 15  \w    109.00 160.00   0.50    0.05    --  105.75 100.00 148.00  102
 16  \w     71.00  96.00   0.50    0.05    --  105.75 -77.00  60.00   50
 17  \w     34.00  68.00   0.50    0.05    --  105.75 -77.00  60.00   68
 18  \w     45.00  70.00   0.50    0.05    --  105.75 -61.00  60.00   50
 19  \w     40.00  65.00   0.50    0.05    --  105.75 -61.00  90.00   50
 20  \w     36.00  65.00   0.50    0.05    --  105.75 -61.00 -90.00   58
 21  \w     40.00  65.00   0.50    0.05    --  105.75 -61.00-120.00   50
 22  \w     34.00  70.00   0.50    0.05    --  105.75 -61.00-150.00   72
 23  \w     34.00  59.00   0.50    0.05    --  105.75 -61.00-180.00   50
 24  \w     38.00  83.00   0.50    0.05    --  105.75 -77.00-150.00   90
 25  \w     45.00  70.00   0.50    0.05    --  105.75-125.00-150.00   50
 26  \w     38.00  69.00   0.50    0.05    --  105.75-125.00-120.00   62
 27  \w     40.00  74.00   0.50    0.05    --  105.75-125.00-180.00   68
 28  \w     80.00 111.00   0.50    0.05    --  105.75-125.00-150.00   62
 29  \w     74.00 100.00   0.50    0.05    --  105.75-125.00-120.00   52
 30  \w     74.00 104.00   0.50    0.05    --  105.75 -95.00-120.00   60
 31  \w     39.00 100.00   0.50    0.05    --  105.75 -95.00 -30.00  122
 32  \w     54.00 102.00   0.50    0.05    --  105.75-125.00  30.00   96
 33  \w     55.00 107.00   0.50    0.05    --  105.75-100.00  43.00  104
 34  \w     35.00  88.00   0.50    0.05    --  105.75 -95.00 150.00  106
 35  \w     15.00  77.00   0.50    0.05    --   49.41-100.00  43.00  124
 36  \w   -121.00 -84.00   0.50    0.05    --  -49.41 -57.00  60.00   74
 37  \w   -120.00 -94.00   0.50    0.05    --  -49.41 -57.00 120.00   52
 38  \w   -113.00 -84.00   0.50    0.05    --  -49.41 -57.00  90.00   58
 39  \w   -113.00 -88.00   0.50    0.05    --  -49.41 -57.00  30.00   50
 40  \w   -156.00-131.00   0.50    0.05    --  -84.25 -77.00 -30.00   50
 41  \w   -156.00-128.00   0.50    0.05    --  -84.25 -77.00   0.00   56
 42  \w   -131.00-104.00   0.50    0.05    --  -84.25-100.00  43.00   54
 43  \w   -116.00 -88.00   0.50    0.05    --  -49.41-125.00 -60.00   56
;
_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      0.0845859000
_diffrn_orient_matrix_UB_12      0.0312097000
_diffrn_orient_matrix_UB_13      -0.0384765000
_diffrn_orient_matrix_UB_21      -0.0217574000
_diffrn_orient_matrix_UB_22      -0.2867220000
_diffrn_orient_matrix_UB_23      -0.0169230000
_diffrn_orient_matrix_UB_31      -0.0925150000
_diffrn_orient_matrix_UB_32      0.0962437000
_diffrn_orient_matrix_UB_33      -0.0378288000
_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  0.1154
_diffrn_reflns_av_unetI/netI     0.1160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9272
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.102
_diffrn_reflns_theta_min         3.245
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.828
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.279
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
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    1.909
_exptl_crystal_description       needle
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.016(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3062
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0420P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2581
_reflns_number_total             3062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02476a2.cif
_cod_data_source_block           Sb(Cys)3
_cod_depositor_comments
'Adding full bibliography for 7717579--7717581.cif.'
_cod_database_code               7717580
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         SbC9H18N3O6S3
_chemical_oxdiff_usercomment     'antimony tricysteine'
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.162
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.01585
 -0.01585
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Ternary CH refined with riding coordinates:
 C12(H12), C22(H22), C32(H32)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C21(H21A,H21B), C31(H31A,H31B)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3A,H3B,H3C)
;
_shelx_res_checksum              75026
_shelx_hkl_checksum              7875
_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 1.498
_oxdiff_exptl_absorpt_empirical_full_min 0.714