Models of the putative antimony(V)-diolate motifs in antileishmanial pentavalent antimonial drugs.
Lindquist-Kleissler, Brent; Johnstone, Timothy C.; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01623d

data_7713251
_publ_section_title
;
 Models of the putative antimony(V)-diolate motifs in antileishmanial
 pentavalent antimonial drugs.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01623d
_journal_year                    2023
_chemical_formula_moiety         'C25 H29 O2 Sb'
_chemical_formula_sum            'C25 H29 O2 Sb'
_chemical_formula_weight         483.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-12-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-05-27 deposited with the CCDC.	2023-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                79.804(2)
_cell_angle_beta                 83.183(2)
_cell_angle_gamma                80.822(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6242(2)
_cell_length_b                   9.3045(2)
_cell_length_c                   14.1213(3)
_cell_measurement_reflns_used    18710
_cell_measurement_temperature    101(1)
_cell_measurement_theta_max      76.2090
_cell_measurement_theta_min      3.1770
_cell_volume                     1096.19(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_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      101(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.957
_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     13.00  38.00   0.50    0.05    --   28.00  63.00   8.63   50
  2  \w    -70.00 -15.00   0.50    0.05    --  -49.41 107.00 -38.00  110
  3  \w    -49.00 -24.00   0.50    0.09    --  -84.25 107.00 -38.00   50
  4  \w    -60.00  19.00   0.50    0.05    --  -49.41  57.00 -60.00  158
  5  \w     25.00  53.00   0.50    0.05    --   36.00  59.00-169.97   56
  6  \w     27.00  52.00   0.50    0.05    --   40.00  59.00-146.60   50
  7  \w     27.00  52.00   0.50    0.05    --   40.00  59.00 -54.26   50
  8  \w     27.00  52.00   0.50    0.05    --   40.00  58.00-114.15   50
  9  \w     27.00  52.00   0.50    0.05    --   40.00  59.00  29.68   50
 10  \w     23.00  53.00   0.50    0.05    --   36.00  59.00  82.47   60
 11  \w     27.00  52.00   0.50    0.05    --   40.00  59.00 152.70   50
 12  \w    103.00 178.00   0.50    0.09    --  105.75  77.00 150.00  150
 13  \w    146.00 178.00   0.50    0.09    --  105.75  57.00 120.00   64
 14  \w     93.00 141.00   0.50    0.09    --  105.75  57.00 120.00   96
 15  \w    101.00 172.00   0.50    0.09    --  105.75  57.00  30.00  142
 16  \w    139.00 178.00   0.50    0.09    --  105.75  57.00 -60.00   78
 17  \w     98.00 135.00   0.50    0.09    --  105.75  57.00 -60.00   74
 18  \w     97.00 150.00   0.50    0.09    --  105.75  57.00-150.00  106
 19  \w    110.00 173.00   0.50    0.09    --  105.75  77.00-150.00  126
 20  \w     90.00 127.00   0.50    0.05    --   56.00  56.00 -16.99   74
 21  \w    150.00 176.00   0.50    0.09    --  105.75  57.00  90.00   52
 22  \w     95.00 140.00   0.50    0.09    --  105.75  57.00  90.00   90
 23  \w     44.00  69.00   0.50    0.05    --   56.00  56.00 -16.99   50
 24  \w     98.00 128.00   0.50    0.09    --  105.75  38.00 -60.00   60
 25  \w    136.00 162.00   0.50    0.09    --  105.75  38.00 -60.00   52
 26  \w    140.00 167.00   0.50    0.09    --  105.75  19.00  90.00   54
 27  \w     99.00 131.00   0.50    0.09    --  105.75  19.00  90.00   64
 28  \w     37.00  67.00   0.50    0.09    --  105.75 -57.00 120.00   60
 29  \w     35.00  60.00   0.50    0.09    --  105.75 -77.00  60.00   50
 30  \w     81.00 106.00   0.50    0.09    --  105.75 -77.00  60.00   50
 31  \w     35.00  65.00   0.50    0.09    --  105.75 -57.00  90.00   60
 32  \w     38.00  64.00   0.50    0.09    --  105.75 -57.00 -90.00   52
 33  \w     38.00  66.00   0.50    0.09    --  105.75 -57.00-120.00   56
 34  \w     36.00  64.00   0.50    0.09    --  105.75 -57.00-180.00   56
 35  \w    105.00 158.00   0.50    0.09    --  105.75 107.00 -38.00  106
 36  \w    -38.00 -13.00   0.50    0.05    --    4.00 122.00 166.95   50
 37  \w     36.00  64.00   0.50    0.09    --  105.75 -99.00 120.00   56
 38  \w     38.00 106.00   0.50    0.09    --  105.75 -99.00  60.00  136
 39  \w     36.00  64.00   0.50    0.09    --  105.75 -99.00 -90.00   56
 40  \w     69.00 101.00   0.50    0.09    --  105.75 -99.00 -90.00   64
 41  \w     69.00 106.00   0.50    0.09    --  105.75-107.00-137.00   74
 42  \w     46.00  92.00   0.50    0.09    --  105.75 -99.00-180.00   92
 43  \w     23.00  82.00   0.50    0.05    --   49.41-107.00-137.00  118
 44  \w     46.00 105.00   0.50    0.09    --  105.75 -99.00 -30.00  118
 45  \w     77.00 103.00   0.50    0.09    --  105.75 -99.00  30.00   52
 46  \w     36.00  64.00   0.50    0.09    --  105.75 -99.00  30.00   56
 47  \w     74.00 103.00   0.50    0.09    --  105.75 -99.00 120.00   58
 48  \w    -42.00 -17.00   0.50    0.05    --  -32.00 -64.00 -47.18   50
 49  \w    -76.00 -39.00   0.50    0.05    --  -52.00 -56.00 -33.95   74
 50  \w    -70.00 -44.00   0.50    0.05    --  -56.00 -56.00 -10.97   52
 51  \w    -85.00 -59.00   0.50    0.09    --  -72.00 -56.00 -42.66   52
 52  \w   -111.00 -85.00   0.50    0.05    --  -56.00 -56.00 -10.97   52
 53  \w   -126.00-100.00   0.50    0.09    --  -72.00 -56.00 -42.66   52
 54  \w    -88.00 -63.00   0.50    0.09    --  -76.00 -56.00  -4.65   50
 55  \w    -89.00 -63.00   0.50    0.09    --  -76.00 -56.00 -90.03   52
 56  \w    -89.00 -63.00   0.50    0.09    --  -76.00 -56.00-101.33   52
 57  \w    -91.00 -65.00   0.50    0.09    --  -76.00 -56.00-174.77   52
 58  \w   -142.00-116.00   0.50    0.09    --  -76.00 -56.00-101.33   52
 59  \w    -91.00 -65.00   0.50    0.09    --  -76.00 -55.00 -68.25   52
 60  \w    -69.00 -40.00   0.50    0.05    --  -52.00 -55.00  39.37   58
 61  \w    -70.00 -44.00   0.50    0.05    --  -56.00 -55.00  82.15   52
 62  \w   -102.00 -76.00   0.50    0.09    --  -84.25 -56.00 163.27   52
 63  \w    -85.00 -56.00   0.50    0.09    --  -68.00 -55.00  92.01   58
 64  \w   -122.00 -97.00   0.50    0.05    --  -52.00 -55.00  39.37   50
 65  \w    -93.00 -68.00   0.50    0.09    --  -80.00 -54.00  20.12   50
 66  \w    -89.00 -64.00   0.50    0.09    --  -76.00 -55.00-123.22   50
 67  \w    -89.00 -64.00   0.50    0.09    --  -76.00 -54.00-144.55   50
 68  \w   -105.00 -73.00   0.50    0.09    --  -84.25 -55.00-134.65   64
 69  \w    -70.00 -45.00   0.50    0.05    --  -56.00 -54.00-156.83   50
 70  \w   -127.00 -85.00   0.50    0.05    --  -56.00 -54.00-156.83   84
 71  \w   -100.00 -72.00   0.50    0.09    --  -84.25 -54.00-166.64   56
 72  \w   -148.00-122.00   0.50    0.09    --  -80.00 -54.00  20.12   52
 73  \w   -134.00 -77.00   0.50    0.09    --  -84.25 -53.00 -15.41  114
 74  \w    -97.00 -64.00   0.50    0.09    --  -76.00 -54.00  62.60   66
 75  \w    -97.00 -72.00   0.50    0.09    --  -84.25 -54.00  85.75   50
 76  \w   -107.00 -72.00   0.50    0.09    --  -84.25 -54.00 126.46   70
 77  \w   -155.00-130.00   0.50    0.09    --  -84.25 -54.00  85.75   50
 78  \w   -134.00-109.00   0.50    0.09    --  -84.25 -53.00   6.63   50
 79  \w   -151.00-125.00   0.50    0.09    --  -84.25 -53.00 -83.46   52
 80  \w   -131.00 -96.00   0.50    0.05    --  -60.00 -53.00 -93.59   70
 81  \w   -103.00 -73.00   0.50    0.09    --  -84.25 -53.00 -83.46   60
 82  \w   -101.00 -76.00   0.50    0.09    --  -84.25 -53.00   6.63   50
 83  \w    -85.00 -49.00   0.50    0.05    --  -60.00 -53.00 -93.59   72
 84  \w   -100.00 -73.00   0.50    0.09    --  -84.25 -53.00  49.52   54
 85  \w   -102.00 -48.00   0.50    0.05    --  -60.00 -53.00 147.33  108
 86  \w    -85.00 -60.00   0.50    0.09    --  -72.00 -53.00 139.64   50
 87  \w    -99.00 -74.00   0.50    0.09    --  -84.25 -53.00 170.56   50
 88  \w   -101.00 -73.00   0.50    0.09    --  -84.25 -53.00 143.52   56
 89  \w   -152.00-110.00   0.50    0.09    --  -84.25 -53.00 170.56   84
 90  \w   -150.00-125.00   0.50    0.09    --  -84.25 -53.00 143.52   50
 91  \w    -96.00 -62.00   0.50    0.09    --  -72.00 -50.00 117.48   68
 92  \w   -100.00 -74.00   0.50    0.09    --  -84.25 -51.00 100.86   52
 93  \w    -98.00 -73.00   0.50    0.09    --  -84.25 -50.00  31.23   50
 94  \w    -85.00 -59.00   0.50    0.09    --  -68.00 -52.00  27.63   52
 95  \w   -125.00 -99.00   0.50    0.09    --  -68.00 -52.00  27.63   52
 96  \w   -156.00-131.00   0.50    0.09    --  -84.25 -50.00 -59.44   50
 97  \w   -113.00 -74.00   0.50    0.09    --  -84.25 -50.00 -59.44   78
 98  \w    -91.00 -65.00   0.50    0.09    --  -72.00 -51.00-165.35   52
 99  \w   -102.00 -74.00   0.50    0.09    --  -84.25 -49.00-125.14   56
100  \w   -154.00-126.00   0.50    0.09    --  -84.25 -49.00-125.14   56
101  \w   -142.00-117.00   0.50    0.09    --  -84.25-107.00-137.00   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      0.1564254000
_diffrn_orient_matrix_UB_12      -0.1059987000
_diffrn_orient_matrix_UB_13      -0.0041525000
_diffrn_orient_matrix_UB_21      0.0118028000
_diffrn_orient_matrix_UB_22      0.0012776000
_diffrn_orient_matrix_UB_23      0.1078442000
_diffrn_orient_matrix_UB_31      -0.0917626000
_diffrn_orient_matrix_UB_32      -0.1328296000
_diffrn_orient_matrix_UB_33      0.0273224000
_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  0.0689
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27604
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.384
_diffrn_reflns_theta_min         3.194
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.103
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.64a (Rigaku Oxford Diffraction, 2022)
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    1.464
_exptl_crystal_description       Plate
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0524P)^2^+0.2344P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4266
_reflns_number_total             4461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01623d2.cif
_cod_data_source_block           2
_cod_database_code               7713251
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Sb O2 C25 H29'
_chemical_oxdiff_usercomment     'BLK0536-Sat MeCN'
_shelx_estimated_absorpt_t_max   0.582
_shelx_estimated_absorpt_t_min   0.313
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C141(H14A,H14B,H14C), C241(H24A,H24B,H24C),
 C341(H34A,H34B,H34C)
;
_shelx_res_checksum              19825
_shelx_hkl_checksum              73490
_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 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.687