Poly-pnictogen bonding: trapping halide ions by a tetradentate antimony(iii) Lewis acid.
Beckmann, J. Louis; Krieft, Jonas; Vishnevskiy, Yury V.; Neumann, Beate; Stammler, Hans-Georg; Mitzel, Norbert W.; Chemical science 14 (2023) 13551–13559; doi:10.1039/d3sc04594c

data_1570288
_publ_section_title
;
 Poly-pnictogen bonding: trapping halide ions by a tetradentate
 antimony(iii) Lewis acid.
;
_journal_issue                   46
_journal_name_full               'Chemical science'
_journal_page_first              13551
_journal_page_last               13559
_journal_paper_doi               10.1039/d3sc04594c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C52 H16 F40 Sb4, Cl, C4 H12 N, 2(C6 H6)'
_chemical_formula_sum            'C68 H40 Cl F40 N Sb4'
_chemical_formula_weight         2153.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7731(2)
_cell_length_b                   21.2235(4)
_cell_length_c                   22.9543(4)
_cell_measurement_reflns_used    42568
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.7900
_cell_measurement_theta_min      1.9720
_cell_volume                     7496.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1901
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -42.00 -17.00   1.00  115.00    --  -18.43 -77.00  60.00   25
  2  \w     68.00  94.00   1.00  115.00    --   18.50 178.00   0.00   26
  3  \w    -33.00  88.00   1.00  115.00    --   18.50   0.00   0.00  121
  4  \w    -16.00  44.00   1.00  115.00    --   18.50 -38.00 120.00   60
  5  \w     21.00  68.00   1.00   75.00    --   26.04 -99.00 -60.00   47
  6  \w     -4.00  36.00   1.00   75.00    --   26.04  77.00 -30.00   40
  7  \w      5.00  95.00   1.00   75.00    --   26.04  57.00 150.00   90
  8  \w    -12.00  96.00   1.00   75.00    --   26.04  19.00   0.00  108
  9  \w    -43.00  43.00   1.00   75.00    --   26.04 -57.00   0.00   86
 10  \w     -3.00  42.00   1.00   75.00    --   26.04  77.00  30.00   45
 11  \w     -7.00  68.00   1.00   75.00    --   26.04 -99.00 120.00   75
 12  \w      5.00  92.00   1.00   75.00    --   26.04  57.00-120.00   87
 13  \w    -41.00  37.00   1.00   75.00    --   26.04 -57.00 -90.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0431901000
_diffrn_orient_matrix_UB_12      -0.0060788000
_diffrn_orient_matrix_UB_13      0.0157047000
_diffrn_orient_matrix_UB_21      -0.0151647000
_diffrn_orient_matrix_UB_22      -0.0248586000
_diffrn_orient_matrix_UB_23      0.0157116000
_diffrn_orient_matrix_UB_31      0.0053365000
_diffrn_orient_matrix_UB_32      -0.0215186000
_diffrn_orient_matrix_UB_33      -0.0225612000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            117638
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.635
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.585
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       block
_exptl_crystal_F_000             4144
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         5.439
_refine_diff_density_min         -2.387
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1167
_refine_ls_number_reflns         14779
_refine_ls_number_restraints     704
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0885
_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^)+(0.1386P)^2^+83.9715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2426
_refine_ls_wR_factor_ref         0.2530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12520
_reflns_number_total             14779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04594c3.cif
_cod_data_source_block           2xTMACl
_cod_depositor_comments
'Adding full bibliography for 1570287--1570290.cif.'
_cod_database_code               1570288
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C68H42ClF40NSb4
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.581
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sb3-C45B \\sim Sb3-C45A
 with sigma of 0.02
 Sb4-C49B \\sim Sb4-C49A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F36A \\sim F37A \\sim F38A \\sim F39A \\sim F40A \\sim C51A \\sim C52A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F31A \\sim F32A \\sim F33A \\sim F34A \\sim F35A \\sim C49A \\sim C50A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F26A \\sim F27A \\sim F28A \\sim F29A \\sim F30A \\sim C45A \\sim C46A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F21A \\sim F22A \\sim F23A \\sim F24A \\sim F25A \\sim C43A \\sim C44A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F21B \\sim F22B \\sim F23B \\sim F24B \\sim F25B \\sim C43B \\sim C44B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F26B \\sim F27B \\sim F28B \\sim F29B \\sim F30B \\sim C45B \\sim C46B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F36B \\sim F37B \\sim F38B \\sim F39B \\sim F40B \\sim C51B \\sim C52B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F31B \\sim F32B \\sim F33B \\sim F34B \\sim F35B \\sim C49B \\sim C50B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C50A \\sim F35B \\sim C50B \\sim C49A \\sim C49B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C51B \\sim C51A \\sim C52A \\sim C52B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 F36A, F37A, F38A, F39A, F40A, C51A, C52A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F26A, F27A, F28A, F29A, F30A, C45A, C46A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F31A, F32A, F33A, F34A, F35A, C49A, C50A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F21A, F22A, F23A, F24A, F25A, C43A, C44A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F21B, F22B, F23B, F24B, F25B, C43B, C44B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F26B, F27B, F28B, F29B, F30B, C45B, C46B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F36B, F37B, F38B, F39B, F40B, C51B, C52B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F31B, F32B, F33B, F34B, F35B, C49B, C50B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C51B)=Sof(F36B)=Sof(F37B)=Sof(F38B)=Sof(F39B)=Sof(F40B)=Sof(C52B)=1-FVAR(1)
 Sof(C51A)=Sof(F36A)=Sof(F37A)=Sof(F38A)=Sof(F39A)=Sof(F40A)=Sof(C52A)=FVAR(1)
 Sof(C49B)=Sof(F31B)=Sof(F32B)=Sof(F33B)=Sof(F34B)=Sof(F35B)=Sof(C50B)=1-FVAR(2)
 Sof(C49A)=Sof(F31A)=Sof(F32A)=Sof(F33A)=Sof(F34A)=Sof(F35A)=Sof(C50A)=FVAR(2)
 Sof(C45B)=Sof(F26B)=Sof(F27B)=Sof(F28B)=Sof(F29B)=Sof(F30B)=Sof(C46B)=1-FVAR(3)
 Sof(C45A)=Sof(F26A)=Sof(F27A)=Sof(F28A)=Sof(F29A)=Sof(F30A)=Sof(C46A)=FVAR(3)
 Sof(C43B)=Sof(F21B)=Sof(F22B)=Sof(F23B)=Sof(F24B)=Sof(F25B)=Sof(C44B)=1-FVAR(4)
 Sof(C43A)=Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=Sof(F25A)=Sof(C44A)=FVAR(4)
6.a Free rotating group:
 C43A(F21A,F22A,F23A,F24A,F25A,C44A), C45A(F26A,F27A,F28A,F29A,F30A,C46A),
 C49A(F31A,F32A,F33A,F34A,F35A,C50A), C51A(F36A,F37A,F38A,F39A,F40A,C52A),
 C43B(F21B,F22B,F23B,F24B,F25B,C44B), C45B(F26B,F27B,F28B,F29B,F30B,C46B),
 C49B(F31B,F32B,F33B,F34B,F35B,C50B), C51B(F36B,F37B,F38B,F39B,F40B,C52B)
6.b Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C29(H29), C36(H36)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C32(H32), C33(H33),
 C34(H34), C38(H38), C39(H39), C40(H40), C57(H57), C58(H58), C59(H59), C60(H60),
  C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
6.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C)
;
_shelx_res_checksum              22634
_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 3.012
_oxdiff_exptl_absorpt_empirical_full_min 0.555