Stereochemically (In)active lone pairs in Sb(III) complexes of a soft scorpionate ligand.
Møller, Mads Sondrup; McKee, Vickie; McKenzie, Christine J.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6665–6673; doi:10.1039/d5dt00261c

data_7718462
_publ_section_title
;
 Stereochemically (In)active lone pairs in Sb(III) complexes of a soft
 scorpionate ligand.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6665
_journal_page_last               6673
_journal_paper_doi               10.1039/d5dt00261c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C24 H32 B2 N12 S6 Sb, C2 F3 O2, 0.25(C6 H12 O2), 1.6[C2HF3O2]'
_chemical_formula_sum            'C30.7 H36.6 B2 F7.8 N12 O5.7 S6 Sb'
_chemical_formula_weight         1148.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-03 deposited with the CCDC.	2025-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.2010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.36050(10)
_cell_length_b                   17.2928(2)
_cell_length_c                   28.3074(3)
_cell_measurement_reflns_used    31961
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.2730
_cell_measurement_theta_min      2.9960
_cell_volume                     5070.50(9)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.115a 64-bit (release 15-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2008)'
_computing_publication_material
'Olex2 (Dolomanov et al. 2009), PublCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2923
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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    -15.00  23.00   1.00    0.50    --    0.00  38.00-180.00   38
  2  \w    -64.00  15.00   1.00    0.50    --    0.00 -38.00  90.00   79
  3  \w    -41.00  21.00   1.00    0.50    --    0.00 -57.00-150.00   62
  4  \w    -21.00  64.00   1.00    0.50    --    0.00  57.00-120.00   85
  5  \w    -15.00  66.00   1.00    0.50    --    0.00  38.00  60.00   81
  6  \w     38.00  66.00   1.00    0.50    --    0.00  38.00-180.00   28
  7  \w     -5.00  40.00   1.00    0.50    --    0.00  38.00 -30.00   45
  8  \w    -81.00 -54.00   1.00    1.65    --  -80.25 -73.00-130.94   27
  9  \w    -82.00 -55.00   1.00    1.65    --  -80.25 -69.00  19.26   27
 10  \w    -85.00 -57.00   1.00    1.65    --  -80.25 -63.00 145.97   28
 11  \w    -82.00 -55.00   1.00    1.65    --  -80.25 -70.00-122.95   27
 12  \w    -80.00 -53.00   1.00    1.65    --  -80.25 -77.00-150.00   27
 13  \w    -81.00 -54.00   1.00    1.65    --  -80.25 -73.00-106.56   27
 14  \w    -80.00 -53.00   1.00    1.65    --  -80.25 -77.00 120.00   27
 15  \w    -80.00 -53.00   1.00    1.65    --  -80.25 -77.00  90.00   27
 16  \w   -144.00-107.00   1.00    1.65    --  -80.25-125.00 -30.00   37
 17  \w    -81.00 -54.00   1.00    1.65    --  -80.25 -74.00  77.60   27
 18  \w    -81.00 -53.00   1.00    1.65    --  -80.25 -76.00-165.76   28
 19  \w    -80.00 -53.00   1.00    1.65    --  -80.25 -76.00 -51.73   27
 20  \w    -80.00 -53.00   1.00    1.65    --  -80.25 -77.00 -30.00   27
 21  \w    -82.00 -55.00   1.00    1.65    --  -80.25 -70.00  87.39   27
 22  \w    -82.00 -55.00   1.00    1.65    --  -80.25 -69.00 -21.93   27
 23  \w    -81.00 -54.00   1.00    1.65    --  -80.25 -73.00 -89.24   27
 24  \w    -78.00 -53.00   1.00    1.65    --  -80.25 -77.00 -90.00   25
 25  \w    -82.00 -55.00   1.00    1.65    --  -80.25 -71.00 145.86   27
 26  \w    -83.00 -55.00   1.00    1.65    --  -80.25 -70.00-147.69   28
 27  \w    -78.00 -53.00   1.00    1.65    --  -80.25 -77.00 -60.00   25
 28  \w    -80.00 -53.00   1.00    1.65    --  -80.25 -76.00 141.39   27
 29  \w    -81.00 -54.00   1.00    1.65    --  -80.25 -77.00  18.14   27
 30  \w    -86.00 -38.00   1.00    1.65    --  -80.25 125.00-120.00   48
 31  \w    -80.00 -53.00   1.00    1.65    --  -80.25 -76.00  44.90   27
 32  \w    -81.00 -54.00   1.00    1.65    --  -80.25 -75.00  59.24   27
 33  \w    -84.00 -57.00   1.00    1.65    --  -80.25 -62.00 156.61   27
 34  \w    -80.00 -53.00   1.00    1.65    --  -80.25 -76.00 130.45   27
 35  \w    -79.00 -54.00   1.00    1.65    --  -80.25 -75.00 -18.55   25
 36  \w    -81.00 -54.00   1.00    1.65    --  -80.25 -75.00   1.44   27
 37  \w    -87.00 -59.00   1.00    1.65    --  -80.25 -55.00-107.35   28
 38  \w    -85.00 -58.00   1.00    1.65    --  -80.25 -60.00 -73.55   27
 39  \w    -81.00 -54.00   1.00    1.65    --  -80.25 -77.00-180.00   27
 40  \w     50.00 113.00   1.00    1.65    --   99.06-125.00  30.00   63
 41  \w     41.00 113.00   1.00    1.65    --   99.06-125.00-150.00   72
 42  \w     74.00 164.00   1.00    1.65    --   99.06  77.00-150.00   90
 43  \w     36.00  72.00   1.00    1.65    --   99.06-125.00   0.00   36
 44  \w     72.00 147.00   1.00    1.65    --   99.06  77.00-120.00   75
 45  \w     40.00  68.00   1.00    1.65    --   99.06 -61.00-150.00   28
 46  \w     75.00 164.00   1.00    1.65    --   99.06  77.00 150.00   89
 47  \w     39.00  65.00   1.00    1.65    --   99.06 -61.00   0.00   26
 48  \w     72.00 165.00   1.00    1.65    --   99.06  77.00  60.00   93
 49  \w     72.00 159.00   1.00    1.65    --   99.06  77.00 120.00   87
 50  \w     44.00  71.00   1.00    1.65    --   99.06 -94.00  90.00   27
 51  \w     31.00  61.00   1.00    1.65    --   99.06 -61.00 120.00   30
 52  \w     73.00 154.00   1.00    1.65    --   99.06  77.00 -90.00   81
 53  \w     74.00 155.00   1.00    1.65    --   99.06  77.00 -30.00   81
 54  \w     72.00 152.00   1.00    1.65    --   99.06  77.00-180.00   80
 55  \w     35.00 106.00   1.00    1.65    --   99.06 -94.00-150.00   71
 56  \w     72.00 143.00   1.00    1.65    --   99.06  77.00  90.00   71
 57  \w     57.00  99.00   1.00    1.65    --   99.06-125.00 -30.00   42
 58  \w     72.00 162.00   1.00    1.65    --   99.06  77.00   0.00   90
 59  \w     43.00 112.00   1.00    1.65    --   99.06-125.00  90.00   69
 60  \w     44.00 113.00   1.00    1.65    --   99.06-125.00 150.00   69
 61  \w     72.00 168.00   1.00    1.65    --   99.06  77.00  30.00   96
 62  \w     72.00 152.00   1.00    1.65    --   99.06  77.00 -60.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1242095000
_diffrn_orient_matrix_UB_12      -0.0391784000
_diffrn_orient_matrix_UB_13      0.0170984000
_diffrn_orient_matrix_UB_21      0.0391226000
_diffrn_orient_matrix_UB_22      0.0187280000
_diffrn_orient_matrix_UB_23      0.0515265000
_diffrn_orient_matrix_UB_31      -0.0717982000
_diffrn_orient_matrix_UB_32      0.0778209000
_diffrn_orient_matrix_UB_33      -0.0038300000
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            55956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.520
_diffrn_reflns_theta_min         4.977
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.327
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
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            'intense red'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       prism
_exptl_crystal_F_000             2310
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/water'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5151
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0520P)^2^+8.5578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4787
_reflns_number_total             5151
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00261c2.cif
_cod_data_source_block           sbtfa_(3a)
_cod_depositor_comments
'Adding full bibliography for 7718459--7718463.cif.'
_cod_original_formula_sum        'C30.70 H36.60 B2 F7.80 N12 O5.70 S6 Sb'
_cod_database_code               7718462
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C24 H24 B2 N12 O2 F3 S6 Sb '
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.322
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H) groups, All C(H,H,H) groups
2. Restrained distances
 C22-F21 \\sim C22-F22 \\sim C22-F23
 with sigma of 0.02
 F21-F22 \\sim F21-F23 \\sim F22-F23
 with sigma of 0.02
3. Others
 Fixed Sof: C22(0.5) F21(0.5) F22(0.5) F23(0.5) C31(0.25) C32(0.25) H32A(0.25)
 H32B(0.25) H32C(0.25) C33(0.25) H33B(0.25) H33A(0.25) H33C(0.25) O31(0.25)
 Fixed X: C33(0.25)
 Fixed Y: C33(0.1706)
 Fixed Z: C33(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11)
4.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C32(H32A,H32B,H32C),
 C33(H33B,H33A,H33C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 344 electrons were found in a volume of 1030\%A^3^ in 1 
void per unit cell. This is consistent with the presence of 1.6[C2HF3O2] per formula unit 
which accounts for 358 electrons per unit cell. 
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17692
_shelx_hkl_checksum              5274
_shelx_fab_checksum              40869
_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 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.798