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_7718463
_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
'C40 H54 B3 N20 S10 Sb2, 3(F6 P), C3 H6 O, [+0.7(C3 H6 O)]'
_chemical_formula_sum            'C45.1 H64.2 B3 F18 N20 O1.7 P3 S10 Sb2'
_chemical_formula_weight         1945.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-06-27
_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                 114.476(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.0046(9)
_cell_length_b                   14.8912(3)
_cell_length_c                   34.1458(12)
_cell_measurement_reflns_used    16571
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      62.0070
_cell_measurement_theta_min      3.1930
_cell_volume                     14811.0(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, 2015a)'
_computing_structure_solution    'SHELXT 2018/2(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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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     19.00  63.00   1.00   12.50    --   -0.78  38.00-120.00   44
  2  \w    -63.00  12.00   1.00   12.50    --   -0.78 -38.00 -60.00   75
  3  \w    -16.00  66.00   1.00   12.50    --   -0.78  38.00 120.00   82
  4  \w     14.00 101.00   1.00   37.50    --   73.78 -77.00 -90.00   87
  5  \w     36.00 112.00   1.00   37.50    --   73.78-125.00  60.00   76
  6  \w     16.00  56.00   1.00   37.50    --   73.78 -57.00  30.00   40
  7  \w     34.00 112.00   1.00   37.50    --   73.78-125.00 -90.00   78
  8  \w     47.00 143.00   1.00   37.50    --   73.78  77.00  90.00   96
  9  \w    -68.00 -15.00   1.00   37.50    --  -75.34   0.00 150.00   53
 10  \w    -43.00 -10.00   1.00   37.50    --  -75.34  38.00   0.00   33
 11  \w    -43.00 -10.00   1.00   37.50    --  -75.34  38.00-180.00   33
 12  \w    -37.00 -12.00   1.00   37.50    --  -75.34  38.00 150.00   25
 13  \w    -98.00 -17.00   1.00   37.50    --  -75.34  77.00-180.00   81
 14  \w    -42.00 -15.00   1.00   37.50    --  -75.34  38.00 -30.00   27
 15  \w    -79.00  -3.00   1.00   37.50    --  -75.34   0.00  90.00   76
;
_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      -0.0055606000
_diffrn_orient_matrix_UB_12      0.0424061000
_diffrn_orient_matrix_UB_13      0.0387524000
_diffrn_orient_matrix_UB_21      0.0261401000
_diffrn_orient_matrix_UB_22      0.0839683000
_diffrn_orient_matrix_UB_23      -0.0038253000
_diffrn_orient_matrix_UB_31      -0.0456239000
_diffrn_orient_matrix_UB_32      0.0429656000
_diffrn_orient_matrix_UB_33      -0.0307217000
_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  0.0583
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            46676
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        62.254
_diffrn_reflns_theta_max         62.254
_diffrn_reflns_theta_min         3.034
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.912
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.872
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       plate
_exptl_crystal_F_000             7779
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.602
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         11519
_refine_ls_number_restraints     1773
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0003P)^2^+346.9066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9671
_reflns_number_total             11519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00261c2.cif
_cod_data_source_block           sbpf6b_(4)
_cod_depositor_comments
'Adding full bibliography for 7718459--7718463.cif.'
_cod_original_cell_volume        14811.0(8)
_cod_original_formula_sum        'C45.10 H64.20 B3 F18 N20 O1.70 P3 S10 Sb2'
_cod_database_code               7718463
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C24H30N12OB2S6PF6Sb
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.406
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All B(H) groups, All C(H,H,H) groups
2. Restrained distances
 B1-H1 \\sim B2-H2 \\sim B3-H3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(P3) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, :
with sigma of 0.1 and sigma for terminal atoms of 0.2
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
{P3', F13', F14', F15', F16', F17', F18'} sigma for 1-2: 0.02, 1-3: 0.04
{P3, F13, F14, F15, F16, F17, F18} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P1, F1, F2, F3, F4, F5, F6}
6. Others
 Sof(P3')=Sof(F13')=Sof(F14')=Sof(F15')=Sof(F16')=Sof(F17')=Sof(F18')=1-FVAR(1)
 Sof(P3)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(F17)=Sof(F18)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 B2(H2)
7.b Aromatic/amide H refined with riding coordinates:
 N19(H19), C2(H2A), C3(H3A), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14),
 C15(H15), C18(H18), C19(H19A), C22(H22), C23(H23), C26(H26), C27(H27),
 C30(H30), C31(H31), C34(H34), C35(H35), C38(H38), C39(H39)
7.c 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), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76415
_shelx_hkl_checksum              52692
_shelx_fab_checksum              15002
_platon_squeeze_void_probe_radius 1.20
_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 1.548
_oxdiff_exptl_absorpt_empirical_full_min 0.731