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_7717581
_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 Bi N3 O6 S3, H2 O'
_chemical_formula_sum            'C9 H20 Bi N3 O7 S3'
_chemical_formula_weight         587.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.10700(10)
_cell_length_b                   11.7830(3)
_cell_length_c                   28.0118(7)
_cell_measurement_reflns_used    4497
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.9260
_cell_measurement_theta_min      3.1270
_cell_volume                     1685.63(7)
_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      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_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    -40.00 -14.00   0.50    0.76    --  -84.25  38.00  38.00   52
  2  \w    -80.00 -54.00   0.50    0.19    --  -49.41 117.00-100.00   52
  3  \w    -22.00  10.00   0.50    0.19    --  -49.41  19.00 -60.00   64
  4  \w    -24.00  17.00   0.50    0.19    --  -49.41  19.00-180.00   82
  5  \w   -118.00 -92.00   0.50    0.19    --  -49.41-125.00 -30.00   52
  6  \w   -156.00-110.00   0.50    0.76    --  -84.25 -85.00  62.00   92
  7  \w   -140.00-115.00   0.50    0.76    --  -84.25 -38.00-115.00   50
  8  \w   -115.00 -87.00   0.50    0.19    --  -49.41-125.00 -90.00   56
  9  \w     35.00  72.00   0.50    0.76    --  105.75 -61.00  60.00   74
 10  \w     59.00 104.00   0.50    0.76    --  105.75 -95.00  60.00   90
 11  \w     34.00  59.00   0.50    0.76    --  105.75 -61.00 -90.00   50
 12  \w     34.00  66.00   0.50    0.76    --  105.75 -61.00-120.00   64
 13  \w    105.00 161.00   0.50    0.76    --  105.75  30.00-120.00  112
 14  \w    147.00 174.00   0.50    0.76    --  105.75 125.00-120.00   54
 15  \w    125.00 151.00   0.50    0.76    --  105.75 117.00-100.00   52
 16  \w     95.00 135.00   0.50    0.76    --  105.75 125.00-120.00   80
;
_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      0.1395962000
_diffrn_orient_matrix_UB_12      0.0500541000
_diffrn_orient_matrix_UB_13      0.0439402000
_diffrn_orient_matrix_UB_21      -0.2283822000
_diffrn_orient_matrix_UB_22      -0.0390652000
_diffrn_orient_matrix_UB_23      0.0320105000
_diffrn_orient_matrix_UB_31      0.1390889000
_diffrn_orient_matrix_UB_32      -0.1143099000
_diffrn_orient_matrix_UB_33      0.0082906000
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            6486
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         3.155
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.366
_exptl_absorpt_correction_T_max  0.26930
_exptl_absorpt_correction_T_min  0.18267
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.315
_exptl_crystal_description       lath
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.030
_refine_diff_density_max         1.887
_refine_diff_density_min         -1.612
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.043(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2915
_refine_ls_number_restraints     528
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0448P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.543
_reflns_Friedel_fraction_full    0.810
_reflns_Friedel_fraction_max     0.787
_reflns_number_gt                2679
_reflns_number_total             2915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02476a2.cif
_cod_data_source_block           Bi(Cys)3
_cod_depositor_comments
'Adding full bibliography for 7717579--7717581.cif.'
_cod_database_code               7717581
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'BiC9H25N3O8S3 '
_chemical_oxdiff_usercomment     'Bismuth tricysteine'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.0429
 -0.0429
2. Restrained distances
 O1WA-H1WA = O1WA-H1WB
 0.84 with sigma of 0.02
 H1WA-H1WB
 1.33 with sigma of 0.02
 O2WA-H2WA = O2WA-H2WB
 0.84 with sigma of 0.02
 H2WA-H2WB
 1.33 with sigma of 0.02
 H1WB-O32A \\sim H1WA-O11_$1
 with sigma of 0.02
3. 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
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Same fragment restrains
{S1, C11, C12, C13, O11, O12, N11} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S3B, C31B, C32B, C33B, O31B, O32B, N31B}
{S1, C11, C12, C13, O11, O12, N11} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S3A, C31A, C32A, C33A, O31A, O32A, N31A}
{S1, C11, C12, C13, O11, O12, N11} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S2, C21, C22, C23, O21, O22, N21}
6. Others
 Sof(S3B)=Sof(C31B)=Sof(H31F)=Sof(H31G)=Sof(C32B)=Sof(H32B)=Sof(C33B)=
 Sof(O31B)=Sof(O32B)=Sof(N31B)=Sof(H31H)=Sof(H31I)=Sof(H31J)=Sof(O2WA)=
 Sof(H2WA)=Sof(H2WB)=1-FVAR(1)
 Sof(S3A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(O31A)=Sof(O32A)=Sof(N31A)=Sof(H31C)=Sof(H31D)=Sof(H31E)=Sof(O1WA)=
 Sof(H1WA)=Sof(H1WB)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C12(H12), C22(H22), C32A(H32A), C32B(H32B)
7.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C21(H21A,H21B), C31A(H31A,H31B), C31B(H31F,H31G)
7.c Idealised Me refined as rotating group:
 N11(H11C,H11D,H11E), N21(H21C,H21D,H21E), N31A(H31C,H31D,H31E), N31B(H31H,
 H31I,H31J)
;
_shelx_res_checksum              48473
_shelx_hkl_checksum              43871
_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 2.130
_oxdiff_exptl_absorpt_empirical_full_min 0.659