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_7713248
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H27 O2 Sb'
_chemical_formula_sum            'C24 H27 O2 Sb'
_chemical_formula_weight         469.20
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-12-07
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.1979(5)
_cell_length_b                   16.3230(8)
_cell_length_c                   16.9475(6)
_cell_measurement_reflns_used    19603
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9320
_cell_measurement_theta_min      4.7160
_cell_volume                     4204.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (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      100.00(10)
_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    -73.00 -48.00   0.50    0.95    --  -49.41 145.00 136.00   50
  2  \w   -119.00 -75.00   0.50    0.95    --  -49.41-127.00-107.00   88
  3  \w   -105.00 -61.00   0.50    0.95    --  -49.41-145.00  83.00   88
  4  \w    -65.00 -40.00   0.50    0.95    --  -49.41 127.00 -32.00   50
  5  \w     54.00 103.00   0.50    0.95    --   49.41-145.00  83.00   98
  6  \w     38.00  95.00   0.50    0.95    --   49.41-127.00-107.00  114
  7  \w    -75.00 -50.00   0.50    3.80    --  -84.25 127.00 -32.00   50
  8  \w    -62.00 -37.00   0.50    3.80    --  -84.25 145.00 136.00   50
  9  \w   -113.00 -75.00   0.50    3.80    --  -84.25-127.00-107.00   76
 10  \w    111.00 136.00   0.50    3.80    --  105.75 127.00 -32.00   50
 11  \w     75.00 112.00   0.50    3.80    --  105.75-127.00-107.00   74
 12  \w    101.00 126.00   0.50    3.80    --  105.75-145.00  83.00   50
 13  \w     81.00 141.00   0.50    3.80    --  105.75 145.00 136.00  120
 14  \w     46.00  71.00   0.50    3.80    --  105.75-127.00-107.00   50
 15  \w   -121.00 -94.00   0.50    0.95    --  -49.41 -57.00 -60.00   54
 16  \w   -120.00 -82.00   0.50    0.95    --  -49.41 -57.00  60.00   76
 17  \w    -23.00  23.00   0.50    0.95    --  -49.41  19.00  60.00   92
 18  \w    -25.00  10.00   0.50    0.95    --  -49.41  19.00 120.00   70
 19  \w   -120.00 -83.00   0.50    0.95    --  -49.41 -57.00 150.00   74
 20  \w   -115.00 -87.00   0.50    0.95    --  -49.41-125.00 -60.00   56
 21  \w   -118.00 -87.00   0.50    0.95    --  -49.41-125.00   0.00   62
 22  \w   -117.00 -83.00   0.50    0.95    --  -49.41 -57.00-150.00   68
 23  \w   -118.00 -84.00   0.50    0.95    --  -49.41 -57.00 -30.00   68
 24  \w     89.00 115.00   0.50    0.95    --   49.41  57.00 120.00   52
 25  \w   -143.00-117.00   0.50    3.80    --  -84.25 -57.00 -90.00   52
 26  \w    -41.00 -15.00   0.50    3.80    --  -84.25  38.00 -90.00   52
 27  \w   -131.00-106.00   0.50    3.80    --  -84.25-145.00  83.00   50
 28  \w    -42.00 -15.00   0.50    3.80    --  -84.25  38.00 -30.00   54
 29  \w     41.00 105.00   0.50    3.80    --  105.75-125.00  90.00  128
 30  \w     63.00  89.00   0.50    3.80    --  105.75 -77.00 -60.00   52
 31  \w     59.00 107.00   0.50    3.80    --  105.75-125.00 -60.00   96
 32  \w     35.00  67.00   0.50    3.80    --  105.75 -57.00-150.00   64
 33  \w     94.00 173.00   0.50    3.80    --  105.75  57.00-120.00  158
 34  \w     34.00  67.00   0.50    3.80    --  105.75 -57.00 -90.00   66
 35  \w     35.00  67.00   0.50    3.80    --  105.75 -57.00  60.00   64
 36  \w     98.00 177.00   0.50    3.80    --  105.75  38.00 -30.00  158
 37  \w     99.00 175.00   0.50    3.80    --  105.75  57.00 120.00  152
 38  \w     36.00  67.00   0.50    3.80    --  105.75 -57.00 -60.00   62
 39  \w     54.00 106.00   0.50    3.80    --  105.75 -99.00 120.00  104
 40  \w     41.00  90.00   0.50    3.80    --  105.75-125.00-180.00   98
 41  \w     43.00 103.00   0.50    3.80    --  105.75 -99.00 -30.00  120
 42  \w     36.00  64.00   0.50    3.80    --  105.75 -99.00-120.00   56
 43  \w     77.00 106.00   0.50    3.80    --  105.75 -99.00-120.00   58
 44  \w     64.00 106.00   0.50    3.80    --  105.75-125.00-150.00   84
 45  \w     36.00  66.00   0.50    3.80    --  105.75 -57.00-120.00   60
 46  \w     81.00 106.00   0.50    3.80    --  105.75 -99.00  60.00   50
 47  \w    102.00 164.00   0.50    3.80    --  105.75  77.00   0.00  124
 48  \w    102.00 176.00   0.50    3.80    --  105.75  38.00  60.00  148
 49  \w     37.00 106.00   0.50    3.80    --  105.75 -99.00  30.00  138
 50  \w     44.00  70.00   0.50    3.80    --  105.75 -77.00 150.00   52
 51  \w     34.00  61.00   0.50    3.80    --  105.75 -57.00  90.00   54
;
_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      -0.0774953000
_diffrn_orient_matrix_UB_12      0.0328366000
_diffrn_orient_matrix_UB_13      0.0493313000
_diffrn_orient_matrix_UB_21      -0.0320169000
_diffrn_orient_matrix_UB_22      -0.0884080000
_diffrn_orient_matrix_UB_23      0.0141116000
_diffrn_orient_matrix_UB_31      0.0569440000
_diffrn_orient_matrix_UB_32      -0.0050536000
_diffrn_orient_matrix_UB_33      0.0749703000
_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  0.0996
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60946
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.072
_diffrn_reflns_theta_min         3.760
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.519
_exptl_absorpt_correction_T_max  0.65037
_exptl_absorpt_correction_T_min  0.62586
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       Block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.047
_exptl_crystal_size_rad          0.030
_refine_diff_density_max         1.897
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.001(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+8.3502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6896
_reflns_number_total             7984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01623d2.cif
_cod_data_source_block           6
_cod_database_code               7713248
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Sb O2 C24 H27'
_chemical_oxdiff_usercomment     BLK0543
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.999(13)
 0.001(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C115(H115), C116(H116), C122(H122), C123(H123),
 C125(H125), C126(H126), C132(H132), C133(H133), C135(H135), C136(H136),
 C212(H212), C213(H213), C215(H215), C216(H216), C222(H222), C223(H223),
 C225(H225), C226(H226), C232(H232), C233(H233), C235(H235), C236(H236)
3.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C117(H11A,H11B,H11C), C127(H12A,H12B,H12C), C137(H13A,H13B,
 H13C), C6(H6A,H6B,H6C), C217(H21A,H21B,H21C), C227(H22A,H22B,H22C), C237(H23A,
 H23B,H23C)
;
_shelx_res_checksum              40130
_shelx_hkl_checksum              27836
_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 2.163
_oxdiff_exptl_absorpt_empirical_full_min 0.533