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_7713250
_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         'C27 H33 O2 Sb'
_chemical_formula_sum            'C27 H33 O2 Sb'
_chemical_formula_weight         511.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 90.7870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.82520(10)
_cell_length_b                   11.8813(2)
_cell_length_c                   20.2807(3)
_cell_measurement_reflns_used    20528
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.6150
_cell_measurement_theta_min      4.2790
_cell_volume                     2367.27(6)
_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 0.999
_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    -41.00 -15.00   0.50    0.30    --  -84.25  38.00-180.00   52
  2  \w    -42.00 -17.00   0.50    0.30    --  -84.25  38.00-120.00   50
  3  \w    -43.00 -12.00   0.50    0.30    --  -84.25  57.00 -90.00   62
  4  \w    -39.00 -13.00   0.50    0.30    --  -84.25  38.00   0.00   52
  5  \w    -40.00 -13.00   0.50    0.30    --  -84.25  38.00  30.00   54
  6  \w    -42.00 -16.00   0.50    0.30    --  -84.25  38.00  60.00   52
  7  \w     84.00 120.00   0.50    0.08    --   49.41  57.00-150.00   72
  8  \w     85.00 120.00   0.50    0.08    --   49.41  57.00-180.00   70
  9  \w    105.00 178.00   0.50    0.30    --  105.75  19.00-120.00  146
 10  \w     98.00 176.00   0.50    0.30    --  105.75  38.00 -30.00  156
 11  \w     98.00 178.00   0.50    0.30    --  105.75  19.00  60.00  160
 12  \w     87.00 121.00   0.50    0.08    --   49.41  57.00 -30.00   68
 13  \w     78.00 137.00   0.50    0.30    --  105.75 151.00  40.00  118
 14  \w     96.00 129.00   0.50    0.30    --  105.75 123.00-121.00   66
 15  \w     34.00  70.00   0.50    0.30    --  105.75 -77.00 -60.00   72
 16  \w     34.00  63.00   0.50    0.30    --  105.75 -57.00-180.00   58
 17  \w     79.00 104.00   0.50    0.30    --  105.75 -77.00 -60.00   50
 18  \w     35.00  67.00   0.50    0.30    --  105.75 -57.00   0.00   64
 19  \w     37.00  63.00   0.50    0.30    --  105.75 -57.00  30.00   52
 20  \w     34.00  59.00   0.50    0.30    --  105.75 -57.00 -30.00   50
 21  \w     34.00  67.00   0.50    0.30    --  105.75 -57.00  90.00   66
 22  \w     35.00  61.00   0.50    0.30    --  105.75 -57.00 120.00   52
 23  \w     34.00  67.00   0.50    0.30    --  105.75 -57.00 150.00   66
 24  \w     57.00 102.00   0.50    0.30    --  105.75 -99.00 150.00   90
 25  \w     86.00 111.00   0.50    0.30    --  105.75-125.00 120.00   50
 26  \w     40.00  71.00   0.50    0.30    --  105.75-125.00 120.00   62
 27  \w     38.00  72.00   0.50    0.30    --  105.75-125.00  90.00   68
 28  \w     56.00 108.00   0.50    0.08    --   49.41-151.00  -3.00  104
 29  \w     59.00 109.00   0.50    0.30    --  105.75-125.00-120.00  100
 30  \w     37.00 105.00   0.50    0.30    --  105.75-125.00 -90.00  136
 31  \w    100.00 130.00   0.50    0.30    --  105.75-151.00  -3.00   60
 32  \w     77.00 106.00   0.50    0.30    --  105.75-125.00  90.00   58
 33  \w     68.00 106.00   0.50    0.30    --  105.75 -99.00  90.00   76
 34  \w     49.00 100.00   0.50    0.30    --  105.75-123.00 158.00  102
 35  \w     33.00  82.00   0.50    0.08    --   49.41-123.00 158.00   98
 36  \w     55.00  80.00   0.50    0.30    --  105.75 -99.00  60.00   50
 37  \w     65.00 106.00   0.50    0.30    --  105.75 -99.00 -30.00   82
 38  \w     46.00 106.00   0.50    0.30    --  105.75 -99.00 -90.00  120
 39  \w   -111.00 -82.00   0.50    0.08    --  -49.41 -57.00 -30.00   58
 40  \w   -119.00 -94.00   0.50    0.08    --  -49.41 -57.00  90.00   50
 41  \w   -121.00 -82.00   0.50    0.08    --  -49.41 -57.00   0.00   78
 42  \w   -120.00 -83.00   0.50    0.08    --  -49.41 -57.00 -60.00   74
 43  \w   -120.00 -91.00   0.50    0.08    --  -49.41 -57.00-120.00   58
 44  \w   -111.00 -86.00   0.50    0.08    --  -49.41 -57.00-180.00   50
 45  \w   -141.00-115.00   0.50    0.30    --  -84.25 -77.00-180.00   52
 46  \w   -118.00 -93.00   0.50    0.08    --  -49.41-125.00-180.00   50
 47  \w   -118.00 -57.00   0.50    0.08    --  -49.41-151.00  -3.00  122
 48  \w   -114.00 -75.00   0.50    0.30    --  -84.25-151.00  -3.00   78
 49  \w   -127.00 -98.00   0.50    0.30    --  -84.25-123.00 158.00   58
 50  \w   -118.00 -93.00   0.50    0.08    --  -49.41-125.00  90.00   50
 51  \w    -89.00 -64.00   0.50    0.08    --  -49.41 151.00  40.00   50
 52  \w    -90.00 -65.00   0.50    0.30    --  -84.25 151.00  40.00   50
 53  \w    -61.00 -16.00   0.50    0.08    --  -49.41 123.00-121.00   90
 54  \w    -74.00 -49.00   0.50    0.30    --  -84.25 123.00-121.00   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      0.0403659000
_diffrn_orient_matrix_UB_12      0.1224160000
_diffrn_orient_matrix_UB_13      0.0158088000
_diffrn_orient_matrix_UB_21      -0.0826842000
_diffrn_orient_matrix_UB_22      0.0408466000
_diffrn_orient_matrix_UB_23      -0.0605322000
_diffrn_orient_matrix_UB_31      -0.1269925000
_diffrn_orient_matrix_UB_32      0.0123550000
_diffrn_orient_matrix_UB_33      0.0431111000
_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  0.0516
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33440
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.074
_diffrn_reflns_theta_min         4.313
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.388
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (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    1.435
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+1.1542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4118
_reflns_number_total             4482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01623d2.cif
_cod_data_source_block           1
_cod_database_code               7713250
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Sb C27 H33 O2'
_chemical_oxdiff_usercomment     BLK0487
_shelx_estimated_absorpt_t_max   0.603
_shelx_estimated_absorpt_t_min   0.315
_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 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.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C17(H17A,
 H17B,H17C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              92036
_shelx_hkl_checksum              25839
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.693