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_7713246
_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         'C21 H21 Sb'
_chemical_formula_sum            'C21 H21 Sb'
_chemical_formula_weight         395.13
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                120
_cell_formula_units_Z            6
_cell_length_a                   12.6758(3)
_cell_length_b                   12.6758(3)
_cell_length_c                   19.8058(4)
_cell_measurement_reflns_used    4743
_cell_measurement_temperature    101.1(6)
_cell_measurement_theta_max      76.7580
_cell_measurement_theta_min      4.5810
_cell_volume                     2755.97(11)
_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      101.1(6)
_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     52.00 111.00   0.50    0.15    --  105.75-125.00-180.00  118
  2  \w      9.00  81.00   0.50    0.05    --   49.41-100.00-109.00  144
  3  \w    -30.00   7.00   0.50    0.05    --  -49.41  38.00  60.00   74
  4  \w    -74.00 -41.00   0.50    0.15    --  -84.25 100.00  -4.00   66
  5  \w    -42.00 -15.00   0.50    0.15    --  -84.25  38.00 -60.00   54
  6  \w    -16.00  24.00   0.50    0.05    --  -49.41  19.00 -90.00   80
  7  \w     82.00 114.00   0.50    0.05    --   49.41  57.00-180.00   64
  8  \w     86.00 111.00   0.50    0.05    --   49.41  57.00 -90.00   50
  9  \w    131.00 174.00   0.50    0.15    --  105.75  19.00-180.00   86
 10  \w    136.00 178.00   0.50    0.15    --  105.75  21.00 -15.00   84
 11  \w    103.00 131.00   0.50    0.15    --  105.75  21.00 -15.00   56
 12  \w    104.00 137.00   0.50    0.15    --  105.75  38.00 120.00   66
 13  \w     41.00  66.00   0.50    0.15    --  105.75 -57.00 150.00   50
 14  \w     35.00  70.00   0.50    0.15    --  105.75 -67.00  70.00   70
 15  \w     57.00 105.00   0.50    0.15    --  105.75 -77.00  60.00   96
 16  \w     39.00  67.00   0.50    0.15    --  105.75 -57.00  30.00   56
 17  \w     37.00 105.00   0.50    0.15    --  105.75 -77.00 -30.00  136
 18  \w     34.00  61.00   0.50    0.15    --  105.75 -57.00   0.00   54
 19  \w     64.00 104.00   0.50    0.15    --  105.75 -77.00 -90.00   80
 20  \w     39.00  88.00   0.50    0.15    --  105.75 -71.00-127.00   98
 21  \w     34.00  62.00   0.50    0.15    --  105.75 -57.00-180.00   56
 22  \w   -151.00 -87.00   0.50    0.15    --  -84.25 -21.00 177.00  128
 23  \w   -119.00 -93.00   0.50    0.05    --  -49.41 -57.00 150.00   52
 24  \w   -121.00 -94.00   0.50    0.05    --  -49.41-125.00 -30.00   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      -0.0723695000
_diffrn_orient_matrix_UB_12      0.0063683000
_diffrn_orient_matrix_UB_13      0.0608456000
_diffrn_orient_matrix_UB_21      0.1117400000
_diffrn_orient_matrix_UB_22      0.0385266000
_diffrn_orient_matrix_UB_23      0.0457490000
_diffrn_orient_matrix_UB_31      0.0445612000
_diffrn_orient_matrix_UB_32      0.1347665000
_diffrn_orient_matrix_UB_33      -0.0159169000
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6111
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.036
_diffrn_reflns_theta_max         67.036
_diffrn_reflns_theta_min         4.605
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.844
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.240
_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            Yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+2.2207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1071
_reflns_number_total             1099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01623d2.cif
_cod_data_source_block           Sbtol3
_cod_original_cell_volume        2755.96(14)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7713246
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Sb C21 H21'
_chemical_oxdiff_usercomment     BLK0489
_shelx_estimated_absorpt_t_max   0.649
_shelx_estimated_absorpt_t_min   0.190
_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)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              8305
_shelx_hkl_checksum              16933
_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 1.614
_oxdiff_exptl_absorpt_empirical_full_min 0.654