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_7718460
_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, C12 H16 B N6 S3, C3 H6 O, 3.4(H2 O)'
_chemical_formula_sum            'C39 H60.8 B3 N18 O4.4 S9 Sb'
_chemical_formula_weight         1294.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-03-25
_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                77.2890(10)
_cell_angle_beta                 79.4900(10)
_cell_angle_gamma                72.973(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5707(2)
_cell_length_b                   14.9955(3)
_cell_length_c                   19.6610(3)
_cell_measurement_reflns_used    38639
_cell_measurement_temperature    100.00(12)
_cell_measurement_theta_max      74.8060
_cell_measurement_theta_min      4.2020
_cell_volume                     2883.54(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.115a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.115a 64-bit (release 15-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.115a (Rigaku OD, 2024)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(12)
_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 0.974
_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    -21.00  25.00   1.00    1.79    --    0.00  57.00 150.00   46
  2  \w     24.00  65.00   1.00    1.79    --    0.00  38.00 -60.00   41
  3  \w    -35.00  12.00   1.00    1.79    --    0.00 -57.00 120.00   47
  4  \w    -63.00  16.00   1.00    1.79    --    0.00 -38.00 -90.00   79
  5  \w    -64.00  10.00   1.00    1.79    --    0.00 -57.00-180.00   74
  6  \w    -13.00  55.00   1.00    1.79    --    0.00  38.00-120.00   68
  7  \w    -58.00  16.00   1.00    1.79    --    0.00 -38.00  30.00   74
  8  \w    -79.00 -53.00   1.00    7.15    --  -80.25 -77.00 150.00   26
  9  \w    -82.00 -55.00   1.00    7.15    --  -80.25 -70.00 100.66   27
 10  \w    -87.00 -61.00   1.00    7.15    --  -80.25 -49.00-160.04   26
 11  \w    -81.00 -55.00   1.00    7.15    --  -80.25 -72.00  94.32   26
 12  \w    -80.00 -53.00   1.00    7.15    --  -80.25 -77.00  69.32   27
 13  \w    -80.00 -54.00   1.00    7.15    --  -80.25 -74.00-132.75   26
 14  \w    -79.00 -53.00   1.00    7.15    --  -80.25 -76.00  -6.09   26
 15  \w    -82.00 -56.00   1.00    7.15    --  -80.25 -66.00 174.45   26
 16  \w    -80.00 -53.00   1.00    7.15    --  -80.25 -77.00  60.00   27
 17  \w    -83.00 -57.00   1.00    7.15    --  -80.25 -65.00 105.33   26
 18  \w    -91.00 -60.00   1.00    7.15    --  -80.25 -52.00 -94.10   31
 19  \w    -80.00 -53.00   1.00    7.15    --  -80.25 -77.00 -30.00   27
 20  \w    -79.00 -53.00   1.00    7.15    --  -80.25 -77.00-105.89   26
 21  \w    -80.00 -54.00   1.00    7.15    --  -80.25 -74.00 153.83   26
 22  \w    -79.00 -53.00   1.00    7.15    --  -80.25 -77.00 -60.00   26
 23  \w    -80.00 -54.00   1.00    7.15    --  -80.25 -75.00 -21.61   26
 24  \w    -83.00 -57.00   1.00    7.15    --  -80.25 -62.00 -28.87   26
 25  \w    -81.00 -55.00   1.00    7.15    --  -80.25 -70.00-152.67   26
 26  \w    -80.00 -54.00   1.00    7.15    --  -80.25 -75.00   9.39   26
 27  \w    -80.00 -53.00   1.00    7.15    --  -80.25 -77.00  82.20   27
 28  \w    -81.00 -55.00   1.00    7.15    --  -80.25 -70.00 126.87   26
 29  \w    -94.00 -59.00   1.00    7.15    --  -80.25 -59.00  18.22   35
 30  \w    -79.00 -31.00   1.00    7.15    --  -80.25 125.00-150.00   48
 31  \w    -89.00 -62.00   1.00    7.15    --  -80.25 -45.00 -30.00   27
 32  \w    -83.00 -56.00   1.00    7.15    --  -80.25 -66.00 162.90   27
 33  \w    -77.00 -43.00   1.00    7.15    --  -80.25 125.00  30.00   34
 34  \w    -80.00 -54.00   1.00    7.15    --  -80.25 -75.00 -46.72   26
 35  \w    -79.00 -54.00   1.00    7.15    --  -80.25 -73.00 -92.92   25
 36  \w    -78.00 -53.00   1.00    7.15    --  -80.25 -77.00-153.71   25
 37  \w    -81.00 -56.00   1.00    7.15    --  -80.25 -67.00 -88.16   25
 38  \w    -81.00 -55.00   1.00    7.15    --  -80.25 -70.00 160.57   26
 39  \w    -84.00 -57.00   1.00    7.15    --  -80.25 -63.00 -37.75   27
 40  \w    -78.00 -53.00   1.00    7.15    --  -80.25 -76.00 -75.69   25
 41  \w    -78.00 -53.00   1.00    7.15    --  -80.25 -77.00 120.00   25
 42  \w    -79.00 -53.00   1.00    7.15    --  -80.25 -76.00  49.36   26
 43  \w    -84.00 -58.00   1.00    7.15    --  -80.25 -61.00  60.00   26
 44  \w    -78.00 -53.00   1.00    7.15    --  -80.25 -77.00  30.00   25
 45  \w    -81.00 -55.00   1.00    7.15    --  -80.25 -70.00-107.44   26
 46  \w     34.00  66.00   1.00    7.15    --   99.69 -61.00-150.00   32
 47  \w     77.00 104.00   1.00    7.15    --   99.69  61.00 -60.00   27
 48  \w    110.00 153.00   1.00    7.15    --   99.69  77.00-120.00   43
 49  \w     74.00 101.00   1.00    7.15    --   99.69  77.00-120.00   27
 50  \w     74.00 157.00   1.00    7.15    --   99.69  77.00 120.00   83
 51  \w     75.00 169.00   1.00    7.15    --   99.69  77.00 150.00   94
 52  \w     75.00 149.00   1.00    7.15    --   99.69  77.00  30.00   74
 53  \w     73.00 144.00   1.00    7.15    --   99.69  77.00  60.00   71
 54  \w     73.00 162.00   1.00    7.15    --   99.69  77.00-180.00   89
 55  \w     80.00 112.00   1.00    7.15    --   99.69-125.00  60.00   32
 56  \w     32.00  57.00   1.00    7.15    --   99.69 -61.00 120.00   25
 57  \w     74.00 165.00   1.00    7.15    --   99.69  77.00 -30.00   91
 58  \w     35.00  62.00   1.00    7.15    --   99.69 -61.00  60.00   27
 59  \w     73.00 148.00   1.00    7.15    --   99.69  77.00 -60.00   75
 60  \w     27.00  73.00   1.00    7.15    --   99.69 -94.00-180.00   46
 61  \w     51.00  94.00   1.00    7.15    --   99.69-125.00 -60.00   43
 62  \w     32.00  61.00   1.00    7.15    --   99.69 -61.00  30.00   29
 63  \w    102.00 127.00   1.00    7.15    --   99.69 -77.00 -30.00   25
 64  \w    117.00 166.00   1.00    7.15    --   99.69  61.00 -90.00   49
 65  \w     34.00  97.00   1.00    7.15    --   99.69 -77.00 -30.00   63
 66  \w     81.00 106.00   1.00    7.15    --   99.69  61.00 -90.00   25
 67  \w     75.00 155.00   1.00    7.15    --   99.69  77.00-150.00   80
 68  \w     35.00 112.00   1.00    7.15    --   99.69-125.00 -30.00   77
 69  \w     73.00 160.00   1.00    7.15    --   99.69  77.00   0.00   87
 70  \w     74.00 165.00   1.00    7.15    --   99.69  77.00  90.00   91
 71  \w     55.00 112.00   1.00    7.15    --   99.69-125.00-120.00   57
 72  \w     47.00 118.00   1.00    7.15    --   99.69-132.00 169.23   71
;
_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      -0.1100255000
_diffrn_orient_matrix_UB_12      0.0929748000
_diffrn_orient_matrix_UB_13      0.0047636000
_diffrn_orient_matrix_UB_21      0.1042290000
_diffrn_orient_matrix_UB_22      0.0569913000
_diffrn_orient_matrix_UB_23      -0.0284388000
_diffrn_orient_matrix_UB_31      -0.0253029000
_diffrn_orient_matrix_UB_32      0.0051408000
_diffrn_orient_matrix_UB_33      -0.0756674000
_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  0.0357
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69071
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.344
_diffrn_reflns_theta_min         3.132
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.307
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.115a (Rigaku Oxford Diffraction, 2024)
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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             1332
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/water'
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.690
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         11622
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0687P)^2^+4.0565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10825
_reflns_number_total             11622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00261c2.cif
_cod_data_source_block           sbs5_(2)
_cod_depositor_comments
'Adding full bibliography for 7718459--7718463.cif.'
_cod_original_formula_sum        'C39 H60.80 B3 N18 O4.40 S9 Sb'
_cod_database_code               7718460
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C50H40N2O4B3S9Sb '
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.370
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 O3-H3B = O3-H3C
 0.83 with sigma of 0.02
 O4-H4D = O4-H4E
 0.83 with sigma of 0.02
 H3B-H3C
 1.35 with sigma of 0.02
 H4D-H4E
 1.35 with sigma of 0.02
 B1-H1 \\sim B2-H2A \\sim B3-H3A
 with sigma of 0.02
3. Restrained planarity
 O41, C41, C42, C43
 with sigma of 0.05
 O41', C41', C42', C43'
 with sigma of 0.05
4. Rigid bond restraints
 O41, C41, C42, C43, O41', C41', C42', C43'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O41 \\sim C41 \\sim C42 \\sim C43 \\sim O41' \\sim C41' \\sim C42' \\sim C43':
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(O41) \\sim Ueq, Uanis(O41') \\sim Ueq, : with sigma of 0.05 and sigma for
terminal atoms of 0.1
6. Same fragment restrains
{O41', C41', C42', C43'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O41, C41, C42, C43}
7. Others
 Fixed Sof: H1A(0.666667) H1B(0.666667) H1C(0.666667) O3(0.8) H3B(0.8)
 H3C(0.8) O4(0.6) H4D(0.6) H4E(0.6) O41(0.6) C41(0.6) C42(0.6) H42A(0.6)
 H42B(0.6) H42C(0.6) C43(0.6) H43A(0.6) H43B(0.6) H43C(0.6) O41'(0.4) C41'(0.4)
 C42'(0.4) H42D(0.4) H42E(0.4) H42F(0.4) C43'(0.4) H43D(0.4) H43E(0.4) H43F(0.4)
8.a Riding coordinates:
 O1(H1A,H1B,H1C), O2(H2B,H2C)
8.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C26(H26), C27(H27),
 C30(H30), C31(H31), C34(H34), C35(H35), C14(H14), C15(H15), C18(H18), C19(H19),
  C22(H22), C23(H23)
8.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C28(H28A,H28B,H28C),
 C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C16(H16A,H16B,H16C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C42'(H42D,H42E,H42F), C43'(H43D,H43E,H43F)
;
_shelx_res_checksum              80542
_shelx_hkl_checksum              93218
_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 1.290
_oxdiff_exptl_absorpt_empirical_full_min 0.859