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_7718459
_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, F6 P, C3 H6 O'
_chemical_formula_sum            'C27 H38 B2 F6 N12 O P S6 Sb'
_chemical_formula_weight         1027.39
_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
_audit_creation_date             2024-04-16
_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                 96.992(5)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   45.083(3)
_cell_length_b                   9.2529(5)
_cell_length_c                   30.1304(17)
_cell_measurement_reflns_used    6253
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      62.1810
_cell_measurement_theta_min      3.7570
_cell_volume                     12475.4(13)
_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    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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    -13.00  25.00   1.00   12.50    --   -0.78 -77.00 -90.00   38
  2  \w    -66.00  14.00   1.00   12.50    --   -0.78 -38.00   0.00   80
  3  \w    -19.00  72.00   1.00   12.50    --   -0.78  19.00-180.00   91
  4  \w     56.00 110.00   1.00   37.50    --   73.78-125.00 120.00   54
  5  \w     53.00 110.00   1.00   37.50    --   73.78-125.00-120.00   57
  6  \w     45.00  84.00   1.00   37.50    --   73.78-125.00 -60.00   39
  7  \w     52.00 110.00   1.00   37.50    --   73.78-125.00   0.00   58
  8  \w    -45.00  -9.00   1.00   37.50    --  -75.34  38.00  90.00   36
  9  \w    -48.00  -9.00   1.00   37.50    --  -75.34  57.00   0.00   39
 10  \w    -86.00 -55.00   1.00   37.50    --  -75.34 125.00 -30.00   31
 11  \w    -45.00 -20.00   1.00   37.50    --  -75.34  38.00 120.00   25
 12  \w    -45.00  -9.00   1.00   37.50    --  -75.34  38.00-120.00   36
 13  \w    -79.00 -14.00   1.00   37.50    --  -75.34 125.00  60.00   65
 14  \w    -40.00  -9.00   1.00   37.50    --  -75.34  38.00 -30.00   31
 15  \w    -69.00  -9.00   1.00   37.50    --  -75.34  57.00-180.00   60
 16  \w    -45.00 -10.00   1.00   37.50    --  -75.34  38.00  60.00   35
 17  \w    -79.00  -8.00   1.00   37.50    --  -75.34   0.00  60.00   71
 18  \w   -142.00 -67.00   1.00   37.50    --  -75.34 -38.00-120.00   75
;
_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      -0.0081002000
_diffrn_orient_matrix_UB_12      -0.1567305000
_diffrn_orient_matrix_UB_13      -0.0138474000
_diffrn_orient_matrix_UB_21      0.0059864000
_diffrn_orient_matrix_UB_22      -0.0475302000
_diffrn_orient_matrix_UB_23      0.0492468000
_diffrn_orient_matrix_UB_31      -0.0329003000
_diffrn_orient_matrix_UB_32      0.0299071000
_diffrn_orient_matrix_UB_33      0.0058022000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15324
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        62.497
_diffrn_reflns_theta_max         62.497
_diffrn_reflns_theta_min         2.955
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.052
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       lath
_exptl_crystal_F_000             6216
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.812
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         15324
_refine_ls_number_restraints     774
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0523P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9817
_reflns_number_total             15324
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.4683\% 
around [0.06 1.00 0.06] (reciprocal) or [0.00 1.00 0.01] (direct)
;
_cod_data_source_file            d5dt00261c2.cif
_cod_data_source_block           sbpf6_hklf5_(3b)
_cod_depositor_comments
'Adding full bibliography for 7718459--7718463.cif.'
_cod_original_cell_volume        12475.4(12)
_cod_database_code               7718459
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C30H30N10O1F6PS6B2Sb
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.278
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5697(11)
 0.4303(11)
2. 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
3. Restrained distances
 B1-H1 \\sim B2-H2 \\sim B3-H3A
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O41, C41, C42, C43} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O51, C51, C52, C53}
6. Others
 Fixed Sof: P2(0.5) F7(0.5) F8(0.5) F9(0.5) F101(0.5) F11(0.5) F12(0.5)
 O51(0.5) C51(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) H53C(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15),
 C18(H18), C19(H19), C22(H22), C23(H23), C26(H26), C27(H27), C30(H30), C31(H31),
  C34(H34), C35(H35)
7.b 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), C28(H28A,H28B,H28C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C52(H52A,
 H52B,H52C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              38443
_shelx_hkl_checksum              10215
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.619
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2