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_7718461
_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         'C48 H64 B4 Cl8 N24 S12 Sb4, 4(C H4 O)'
_chemical_formula_sum            'C52 H80 B4 Cl8 N24 O4 S12 Sb4'
_chemical_formula_weight         2303.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-21
_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                 93.6973(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.86977(5)
_cell_length_b                   26.79870(10)
_cell_length_c                   15.13528(6)
_cell_measurement_reflns_used    65950
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.4350
_cell_measurement_theta_min      3.3550
_cell_volume                     4399.67(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (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 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2923
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -60.00  16.00   1.00    0.50    --    0.00 -38.00   0.00   76
  2  \w    -55.00  13.00   1.00    0.50    --    0.00 -77.00 -30.00   68
  3  \w    -28.00   6.00   1.00    0.50    --    0.00 -38.00  90.00   34
  4  \w    -20.00  71.00   1.00    0.50    --    0.00  19.00-120.00   91
  5  \w    -21.00   8.00   1.00    0.50    --    0.00  57.00 -30.00   29
  6  \w     26.00  58.00   1.00    0.50    --    0.00  57.00 -30.00   32
  7  \w    -21.00   7.00   1.00    0.50    --    0.00  19.00 120.00   28
  8  \w    -61.00 -33.00   1.00    0.50    --    0.00 -38.00  90.00   28
  9  \w    -17.00  66.00   1.00    0.50    --    0.00  57.00 120.00   83
 10  \w    -80.00 -53.00   1.00    0.61    --  -80.25 -77.00 -90.00   27
 11  \w    -85.00 -59.00   1.00    0.61    --  -80.25 -56.00 -88.96   26
 12  \w    -81.00 -55.00   1.00    0.61    --  -80.25 -72.00 154.32   26
 13  \w    -82.00 -56.00   1.00    0.61    --  -80.25 -66.00-121.00   26
 14  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -77.00-120.00   26
 15  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -77.00 172.86   26
 16  \w    -82.00 -56.00   1.00    0.61    --  -80.25 -67.00 -37.30   26
 17  \w    -80.00 -54.00   1.00    0.61    --  -80.25 -73.00  86.85   26
 18  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -76.00 -45.83   26
 19  \w    -78.00 -53.00   1.00    0.61    --  -80.25 -76.00 -68.78   25
 20  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -77.00  78.27   26
 21  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -77.00-150.00   26
 22  \w    -80.00 -54.00   1.00    0.61    --  -80.25 -73.00-143.84   26
 23  \w   -143.00-118.00   1.00    0.61    --  -80.25-125.00-180.00   25
 24  \w    -81.00 -55.00   1.00    0.61    --  -80.25 -69.00 -76.05   26
 25  \w    -80.00 -54.00   1.00    0.61    --  -80.25 -75.00   3.99   26
 26  \w    -82.00 -55.00   1.00    0.61    --  -80.25 -70.00 121.81   27
 27  \w    -84.00 -58.00   1.00    0.61    --  -80.25 -59.00 -15.58   26
 28  \w    -89.00 -62.00   1.00    0.61    --  -80.25 -45.00  60.00   27
 29  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -77.00  65.89   26
 30  \w    -82.00 -56.00   1.00    0.61    --  -80.25 -67.00 106.08   26
 31  \w    -79.00 -54.00   1.00    0.61    --  -80.25 -74.00 -85.59   25
 32  \w    -84.00 -58.00   1.00    0.61    --  -80.25 -59.00  33.05   26
 33  \w    -81.00 -55.00   1.00    0.61    --  -80.25 -69.00 -55.01   26
 34  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -77.00  -8.59   26
 35  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -77.00  30.00   26
 36  \w    -82.00 -55.00   1.00    0.61    --  -80.25 -69.00-174.34   27
 37  \w    -80.00 -55.00   1.00    0.61    --  -80.25 -70.00-119.37   25
 38  \w    -82.00 -56.00   1.00    0.61    --  -80.25 -67.00 125.88   26
 39  \w    -87.00 -51.00   1.00    0.61    --  -80.25 125.00  60.00   36
 40  \w    -86.00 -59.00   1.00    0.61    --  -80.25 -55.00 -31.09   27
 41  \w    -86.00 -60.00   1.00    0.61    --  -80.25 -54.00  -0.21   26
 42  \w    -78.00 -53.00   1.00    0.61    --  -80.25 -77.00 150.00   25
 43  \w    -79.00 -54.00   1.00    0.61    --  -80.25 -74.00 -32.22   25
 44  \w    -81.00 -55.00   1.00    0.61    --  -80.25 -69.00  90.81   26
 45  \w    -79.00 -53.00   1.00    0.61    --  -80.25 -77.00-180.00   26
 46  \w    -81.00 -54.00   1.00    0.61    --  -80.25 -73.00-174.24   27
 47  \w    -86.00 -60.00   1.00    0.61    --  -80.25 -52.00-175.37   26
 48  \w    -78.00 -53.00   1.00    0.61    --  -80.25 -77.00  48.35   25
 49  \w    -79.00 -54.00   1.00    0.61    --  -80.25 -74.00 112.50   25
 50  \w    -78.00 -53.00   1.00    0.61    --  -80.25 -77.00  13.61   25
 51  \w    -78.00 -53.00   1.00    0.61    --  -80.25 -76.00  82.50   25
 52  \w     72.00 154.00   1.00    0.61    --   99.06  77.00 -90.00   82
 53  \w     72.00 157.00   1.00    0.61    --   99.06  77.00 -30.00   85
 54  \w     33.00  82.00   1.00    0.61    --   99.06 -94.00-180.00   49
 55  \w     42.00 113.00   1.00    0.61    --   99.06-125.00  60.00   71
 56  \w     73.00 145.00   1.00    0.61    --   99.06  77.00  60.00   72
 57  \w     34.00  67.00   1.00    0.61    --   99.06 -61.00-180.00   33
 58  \w     38.00  91.00   1.00    0.61    --   99.06-125.00 -30.00   53
 59  \w     40.00  67.00   1.00    0.61    --   99.06 -61.00  30.00   27
 60  \w     35.00  68.00   1.00    0.61    --   99.06 -61.00 -30.00   33
 61  \w     73.00 150.00   1.00    0.61    --   99.06  77.00 150.00   77
 62  \w     36.00  62.00   1.00    0.61    --   99.06 -61.00  90.00   26
 63  \w     74.00 151.00   1.00    0.61    --   99.06  77.00 -60.00   77
 64  \w     74.00 167.00   1.00    0.61    --   99.06  77.00   0.00   93
 65  \w     73.00 165.00   1.00    0.61    --   99.06  72.00-118.69   92
 66  \w     44.00 111.00   1.00    0.61    --   99.06-125.00   0.00   67
 67  \w     74.00 101.00   1.00    0.61    --   99.06  76.00-104.86   27
 68  \w    115.00 155.00   1.00    0.61    --   99.06  77.00  30.00   40
 69  \w     72.00 109.00   1.00    0.61    --   99.06  77.00  30.00   37
 70  \w     52.00 123.00   1.00    0.61    --   99.06-139.00-160.15   71
 71  \w     57.00 113.00   1.00    0.61    --   99.06-125.00 -90.00   56
 72  \w    109.00 153.00   1.00    0.61    --   99.06  77.00-150.00   44
 73  \w     72.00 105.00   1.00    0.61    --   99.06  77.00-150.00   33
 74  \w     72.00 151.00   1.00    0.61    --   99.06  77.00  90.00   79
 75  \w     34.00  84.00   1.00    0.61    --   99.06 -94.00  90.00   50
 76  \w     73.00 166.00   1.00    0.61    --   99.06  77.00-180.00   93
 77  \w     31.00  57.00   1.00    0.61    --   99.06 -61.00-120.00   26
 78  \w     73.00 159.00   1.00    0.61    --   99.06  77.00 120.00   86
;
_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      0.0507626000
_diffrn_orient_matrix_UB_12      0.0336762000
_diffrn_orient_matrix_UB_13      -0.0716778000
_diffrn_orient_matrix_UB_21      0.1316792000
_diffrn_orient_matrix_UB_22      -0.0182504000
_diffrn_orient_matrix_UB_23      0.0264508000
_diffrn_orient_matrix_UB_31      -0.0161388000
_diffrn_orient_matrix_UB_32      -0.0428814000
_diffrn_orient_matrix_UB_33      -0.0675233000
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            111568
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.555
_diffrn_reflns_theta_min         3.298
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.993
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (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            'clear pale yellow'
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/water'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0189
_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^)+(0.0232P)^2^+3.4626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8701
_reflns_number_total             8952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00261c2.cif
_cod_data_source_block           sbtmecl_(1)
_cod_depositor_comments
'Adding full bibliography for 7718459--7718463.cif.'
_cod_original_cell_volume        4399.66(3)
_cod_database_code               7718461
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C12H15N6O2Cl2S3Sb
_shelx_estimated_absorpt_t_max   0.467
_shelx_estimated_absorpt_t_min   0.137
_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, All O(H) groups
2. Others
 Fixed Sof: O26(0.88) H26(0.88) C26(0.88) H26A(0.88) H26B(0.88) H26C(0.88)
 O27(0.12) H27(0.12) C27(0.12) H27A(0.12) H27B(0.12) H27C(0.12)
 Fixed Uiso: H27(0.05)
3.a Everything fixed:
 H27
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15),
 C18(H18), C19(H19), C22(H22), C23(H23)
3.c Tetrahedral OH refined with riding coordinates:
 O25(H25), O26(H26)
3.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              96751
_shelx_hkl_checksum              88083
_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 1.418
_oxdiff_exptl_absorpt_empirical_full_min 0.773