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_7713247
_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         'C36 H44 O5 Sb2'
_chemical_formula_sum            'C36 H44 O5 Sb2'
_chemical_formula_weight         800.21
_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
_audit_creation_date             2023-05-17
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_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            4
_cell_length_a                   12.17550(10)
_cell_length_b                   13.5809(2)
_cell_length_c                   20.6690(3)
_cell_measurement_reflns_used    36758
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      77.0010
_cell_measurement_theta_min      4.1770
_cell_volume                     3417.71(8)
_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      102(2)
_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 0.987
_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     39.00  66.00   0.50    0.91    --  105.75 -57.00-180.00   54
  2  \w     40.00 103.00   0.50    0.91    --  105.75 -77.00-120.00  126
  3  \w     34.00  65.00   0.50    0.91    --  105.75 -57.00 -60.00   62
  4  \w     34.00  59.00   0.50    0.91    --  105.75 -57.00   0.00   50
  5  \w     38.00  67.00   0.50    0.91    --  105.75 -57.00  30.00   58
  6  \w     38.00  63.00   0.50    0.91    --  105.75 -57.00-120.00   50
  7  \w     38.00  93.00   0.50    0.23    --   49.41-125.00-180.00  110
  8  \w     41.00  66.00   0.50    0.23    --   49.41-127.00-142.00   50
  9  \w     61.00 112.00   0.50    0.91    --  105.75-127.00-142.00  102
 10  \w     37.00 107.00   0.50    0.91    --  105.75-125.00-180.00  140
 11  \w     40.00  65.00   0.50    0.91    --  105.75-125.00 -90.00   50
 12  \w     42.00  67.00   0.50    0.91    --  105.75 -99.00-120.00   50
 13  \w     79.00 105.00   0.50    0.91    --  105.75 -99.00-120.00   52
 14  \w     71.00 105.00   0.50    0.91    --  105.75-125.00 -90.00   68
 15  \w     54.00 107.00   0.50    0.23    --   49.41-145.00  49.00  106
 16  \w     39.00  66.00   0.50    0.91    --  105.75 -99.00 120.00   54
 17  \w     94.00 125.00   0.50    0.91    --  105.75-145.00  49.00   62
 18  \w     37.00 106.00   0.50    0.91    --  105.75 -99.00  60.00  138
 19  \w     37.00 106.00   0.50    0.91    --  105.75 -99.00  30.00  138
 20  \w     79.00 104.00   0.50    0.91    --  105.75 -99.00 -60.00   50
 21  \w     40.00  65.00   0.50    0.91    --  105.75 -99.00 -60.00   50
 22  \w     37.00 106.00   0.50    0.91    --  105.75 -99.00-180.00  138
 23  \w    124.00 172.00   0.50    0.91    --  105.75  19.00  60.00   96
 24  \w    101.00 159.00   0.50    0.91    --  105.75  38.00  30.00  116
 25  \w    107.00 176.00   0.50    0.91    --  105.75  38.00 150.00  138
 26  \w     83.00 120.00   0.50    0.23    --   49.41  57.00  30.00   74
 27  \w    107.00 150.00   0.50    0.91    --  105.75  77.00-150.00   86
 28  \w     97.00 175.00   0.50    0.91    --  105.75 125.00-120.00  156
 29  \w    112.00 138.00   0.50    0.91    --  105.75 127.00 -66.00   52
 30  \w     84.00 137.00   0.50    0.91    --  105.75 145.00 101.00  106
 31  \w    -61.00 -23.00   0.50    0.91    --  -84.25 145.00 101.00   76
 32  \w    -86.00 -61.00   0.50    0.23    --  -49.41 145.00 101.00   50
 33  \w    -72.00 -45.00   0.50    0.91    --  -84.25 127.00 -66.00   54
 34  \w    -70.00 -45.00   0.50    0.23    --  -49.41 127.00 -66.00   50
 35  \w    -39.00 -14.00   0.50    0.91    --  -84.25  38.00-120.00   50
 36  \w    -41.00 -16.00   0.50    0.91    --  -84.25  38.00 -60.00   50
 37  \w    -42.00 -15.00   0.50    0.91    --  -84.25  38.00   0.00   54
 38  \w    -41.00 -15.00   0.50    0.91    --  -84.25  38.00  60.00   52
 39  \w    -40.00 -14.00   0.50    0.91    --  -84.25  38.00  90.00   52
 40  \w    -40.00 -13.00   0.50    0.91    --  -84.25  38.00 150.00   54
 41  \w    -39.00 -14.00   0.50    0.91    --  -84.25  38.00 -30.00   50
 42  \w   -121.00 -84.00   0.50    0.23    --  -49.41 -57.00 -90.00   74
 43  \w   -115.00 -82.00   0.50    0.23    --  -49.41 -57.00-150.00   66
 44  \w   -120.00 -82.00   0.50    0.23    --  -49.41 -57.00-180.00   76
 45  \w   -119.00 -83.00   0.50    0.23    --  -49.41 -57.00-120.00   72
 46  \w   -111.00 -83.00   0.50    0.23    --  -49.41 -57.00 -60.00   56
 47  \w   -121.00 -87.00   0.50    0.23    --  -49.41 -57.00 150.00   68
 48  \w   -131.00-106.00   0.50    0.91    --  -84.25-145.00  49.00   50
 49  \w   -131.00-100.00   0.50    0.91    --  -84.25 -99.00  60.00   62
 50  \w   -154.00-118.00   0.50    0.91    --  -84.25 -99.00-120.00   72
 51  \w   -116.00 -90.00   0.50    0.91    --  -84.25-127.00-142.00   52
 52  \w   -118.00 -93.00   0.50    0.23    --  -49.41-125.00 -90.00   50
 53  \w   -119.00 -74.00   0.50    0.23    --  -49.41-127.00-142.00   90
 54  \w   -108.00 -83.00   0.50    0.23    --  -49.41-145.00  49.00   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      0.0427328000
_diffrn_orient_matrix_UB_12      -0.0284051000
_diffrn_orient_matrix_UB_13      0.0676326000
_diffrn_orient_matrix_UB_21      -0.0193978000
_diffrn_orient_matrix_UB_22      -0.1095675000
_diffrn_orient_matrix_UB_23      -0.0156911000
_diffrn_orient_matrix_UB_31      0.1174621000
_diffrn_orient_matrix_UB_32      -0.0077012000
_diffrn_orient_matrix_UB_33      -0.0271477000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51012
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.563
_diffrn_reflns_theta_min         3.895
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.849
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.215
_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    1.555
_exptl_crystal_description       needle
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.475
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.015(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0471P)^2^+4.4568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                6824
_reflns_number_total             7095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01623d2.cif
_cod_data_source_block           ESI1
_cod_database_code               7713247
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Sb2 O5 C36 H44'
_chemical_oxdiff_usercomment     BLK0533
_shelx_estimated_absorpt_t_max   0.566
_shelx_estimated_absorpt_t_min   0.308
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.015(9)
 -0.015(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C2(H2), C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C13(H13), C35(H35), C36(H36), C12(H12), C15(H15), C46(H46),
 C33(H33), C45(H45), C16(H16), C32(H32), C23(H23), C42(H42), C25(H25), C26(H26),
  C43(H43)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C3(H3A,H3B,H3C), C27(H27A,H27B,H27C),
 C17(H17A,H17B,H17C), C7(H7A,H7B,H7C), C47(H47A,H47B,H47C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              20731
_shelx_hkl_checksum              11652
_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 1.786
_oxdiff_exptl_absorpt_empirical_full_min 0.670