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_1570289
_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         'I, C52 H16 F40 Sb4, C16 H36 N, C6 H6'
_chemical_formula_sum            'C74 H55 F40 I N Sb4'
_chemical_formula_weight         2332.09
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                72.1222(14)
_cell_angle_beta                 78.1365(13)
_cell_angle_gamma                83.5967(13)
_cell_formula_units_Z            2
_cell_length_a                   13.1683(2)
_cell_length_b                   15.0933(2)
_cell_length_c                   22.5113(3)
_cell_measurement_reflns_used    91842
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      30.0310
_cell_measurement_theta_min      2.6690
_cell_volume                     4161.56(11)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     14.00 106.00   1.00   32.00    --   35.84  38.00 -30.00   92
  2  \w    -33.00  54.00   1.00   32.00    --   35.84 -57.00-180.00   87
  3  \w     39.00 110.00   1.00   32.00    --   35.84 178.00-180.00   71
  4  \w      2.00  31.00   1.00   32.00    --   35.84  87.00   7.49   29
  5  \w     14.00 106.00   1.00   32.00    --   35.84  38.00-120.00   92
  6  \w    -15.00  76.00   1.00   32.00    --   35.84 -99.00-180.00   91
  7  \w     39.00 110.00   1.00   32.00    --   35.84 178.00   0.00   71
  8  \w     37.00 111.00   1.00   32.00    --   35.84-178.00 120.00   74
  9  \w      9.00  36.00   1.00   32.00    --   35.84  73.00 -23.51   27
 10  \w     14.00 106.00   1.00   32.00    --   35.84  38.00  60.00   92
 11  \w      8.00  36.00   1.00   32.00    --   35.84  75.00-106.45   28
 12  \w     11.00 104.00   1.00   32.00    --   35.84  70.00 -96.05   93
 13  \w      9.00  36.00   1.00   32.00    --   35.84  74.00  93.74   27
 14  \w      9.00  36.00   1.00   32.00    --   35.84  73.00-151.86   27
 15  \w    -15.00  76.00   1.00   32.00    --   35.84 -99.00   0.00   91
 16  \w     14.00 106.00   1.00   32.00    --   35.84  38.00 150.00   92
 17  \w      2.00  31.00   1.00   32.00    --   35.84  86.00 149.73   29
 18  \w      0.00  29.00   1.00   32.00    --   35.84  90.00-179.00   29
 19  \w    -33.00  54.00   1.00   32.00    --   35.84 -56.00-104.00   87
 20  \w    -15.00  76.00   1.00   32.00    --   35.84 -99.00 120.00   91
 21  \w     17.00 104.00   1.00   32.00    --   35.84  57.00-180.00   87
 22  \w    -15.00  76.00   1.00   32.00    --   35.84 -99.00-120.00   91
 23  \w     10.00  36.00   1.00   32.00    --   35.84  72.00 140.47   26
 24  \w     10.00  36.00   1.00   32.00    --   35.84  72.00 -73.08   26
 25  \w      8.00  36.00   1.00   32.00    --   35.84  75.00 122.82   28
 26  \w     17.00 104.00   1.00   32.00    --   35.84  57.00  60.00   87
 27  \w     17.00 104.00   1.00   32.00    --   35.84  57.00 -60.00   87
 28  \w     -2.00 108.00   1.00   32.00    --   35.84  19.00-150.00  110
 29  \w     17.00 104.00   1.00   32.00    --   35.84  57.00 150.00   87
 30  \w    -35.00 107.00   1.00   32.00    --   35.84   0.00-180.00  142
 31  \w    -35.00 107.00   1.00   32.00    --   35.84   0.00-150.00  142
 32  \w      9.00  36.00   1.00   32.00    --   35.84  74.00  55.40   27
 33  \w    -35.00 107.00   1.00   32.00    --   35.84   0.00 -90.00  142
 34  \w    -35.00 107.00   1.00   32.00    --   35.84   0.00 -60.00  142
 35  \w    -35.00  53.00   1.00   32.00    --   35.84   0.00 -30.00   88
 36  \w    -35.00 107.00   1.00   32.00    --   35.84   0.00-120.00  142
;
_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      0.0145421000
_diffrn_orient_matrix_UB_12      0.0453588000
_diffrn_orient_matrix_UB_13      -0.0188768000
_diffrn_orient_matrix_UB_21      -0.0484580000
_diffrn_orient_matrix_UB_22      0.0189452000
_diffrn_orient_matrix_UB_23      0.0125098000
_diffrn_orient_matrix_UB_31      0.0218623000
_diffrn_orient_matrix_UB_32      0.0053410000
_diffrn_orient_matrix_UB_33      0.0249091000
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            276351
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         2.266
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.586
_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            'dull colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_description       needle
_exptl_crystal_F_000             2246
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.066
_refine_diff_density_max         2.017
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         24364
_refine_ls_number_restraints     2083
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+7.0085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20916
_reflns_number_total             24364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04594c3.cif
_cod_data_source_block           TBAI
_cod_depositor_comments
'Adding full bibliography for 1570287--1570290.cif.'
_cod_original_cell_volume        4161.54(12)
_cod_database_code               1570289
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C74H58F40 I N Sb4'
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.653
_diffrn_oxdiff_digest_frames
;
01d50d8f145b6bb2be64b299d865873ba0027749970
;
_diffrn_oxdiff_digest_hkl
;
01d846cc3b7d201b9daab8cede9fd0b286ce10
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C45B-C46B \\sim C45-C46 \\sim C48B-C47B \\sim C48-C47 \\sim C50B-C49B \\sim
C50-C49 \\sim C52B-C51B ~
 C52-C51
 with sigma of 0.02
 F24-C46 \\sim F21B-C45B \\sim F22B-C45B \\sim F23-C46 \\sim F27-C47 \\sim
F27B-C47B \\sim F26-C47 ~
 F26B-C47B \\sim F31-C49 \\sim F31B-C49B \\sim F32B-C49B \\sim F32-C49 \\sim
F37-C51 \\sim F36-C51 ~
 F37B-C51B \\sim F36B-C51B \\sim F24B-C46B \\sim F21-C45 \\sim F23B-C46B \\sim
F22-C45
 with sigma of 0.02
 F29B-C48B \\sim F30-C48 \\sim F30B-C48B \\sim F28-C48 \\sim F28B-C48B \\sim
F29-C48 \\sim F24-C46 ~
 F25-C46 \\sim F23-C46 \\sim F23B-C46B \\sim F24B-C46B \\sim F25B-C46B \\sim
F34-C50 \\sim F34B-C50B ~
 F33-C50 \\sim F33B-C50B \\sim F35-C50 \\sim F35B-C50B \\sim F38B-C52B \\sim
F39B-C52B \\sim F40B-C52B
 \\sim F39-C52 \\sim F40-C52 \\sim F38-C52
 with sigma of 0.02
 F34B-F33B \\sim F33B-F35B
 with sigma of 0.02
 F40B-C51B \\sim C51B-F38B \\sim F40B-C51B \\sim C51B-F39B
 with sigma of 0.02
 C50B-F31B \\sim C50B-F32B
 with sigma of 0.02
 Sb4B-C51B \\sim Sb4-C51 \\sim Sb4-C49 \\sim Sb4B-C49B
 with sigma of 0.02
 F37B-F36B \\sim F37-F36
 with sigma of 0.02
 F39B-F38B \\sim F38B-F40B
 with sigma of 0.02
 C51-F38 \\sim C51-F39 \\sim C51-F40 \\sim C51B-F40B \\sim C51B-F38B \\sim
C51B-F39B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Sb4 \\sim Sb4B \\sim F21 \\sim F21B \\sim F22 \\sim F22B \\sim F23 \\sim F23B
\\sim F24 \\sim F24B \\sim F25 \\sim F25B \\sim F26 \\sim F26B \\sim F27 \\sim
F27B \\sim F28 \\sim F28B \\sim F29 \\sim F29B \\sim F30 \\sim F30B \\sim F31
\\sim F32 \\sim F33 \\sim F34 \\sim F35 \\sim F36 \\sim F37 \\sim F38 \\sim F39
\\sim F40 \\sim F37B \\sim F36B \\sim F38B \\sim F39B \\sim F40B \\sim F31B
\\sim F32B \\sim F35B \\sim F34B \\sim F33B \\sim C45 \\sim C45B \\sim C46
\\sim C46B \\sim C47 \\sim C47B \\sim C48 \\sim C48B \\sim C49 \\sim C49B \\sim
C50 \\sim C50B \\sim C51 \\sim C51B \\sim C52 \\sim C52B: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(F33B) = Uanis(F33)
Uanis(F35) = Uanis(F35B)
Uanis(F32) = Uanis(F32B)
Uanis(C49B) = Uanis(C49)
Uanis(F34) = Uanis(F34B)
Uanis(C50B) = Uanis(C50)
Uanis(F31) = Uanis(F31B)
Uanis(Sb4B) = Uanis(Sb4)
4. Rigid body (RIGU) restrains
 Sb4, Sb4B, F21, F21B, F22, F22B, F23, F23B, F24, F24B, F25, F25B, F26, F26B,
 F27, F27B, F28, F28B, F29, F29B, F30, F30B, F31, F32, F33, F34, F35, F36, F37,
 F38, F39, F40, F37B, F36B, F38B, F39B, F40B, F31B, F32B, F35B, F34B, F33B, C45,
  C45B, C46, C46B, C47, C47B, C48, C48B, C49, C49B, C50, C50B, C51, C51B, C52,
 C52B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Sb4B)=Sof(F37B)=Sof(F36B)=Sof(F38B)=Sof(F39B)=Sof(F40B)=Sof(F31B)=
 Sof(F32B)=Sof(F35B)=Sof(F34B)=Sof(F33B)=Sof(C49B)=Sof(C50B)=Sof(C51B)=
 Sof(C52B)=1-FVAR(1)
 Sof(Sb4)=Sof(F31)=Sof(F32)=Sof(F33)=Sof(F34)=Sof(F35)=Sof(F36)=Sof(F37)=
 Sof(F38)=Sof(F39)=Sof(F40)=Sof(C49)=Sof(C50)=Sof(C51)=Sof(C52)=FVAR(1)
 Fixed Sof: F21(0.5) F21B(0.5) F22(0.5) F22B(0.5) F23(0.5) F23B(0.5) F24(0.5)
 F24B(0.5) F25(0.5) F25B(0.5) F26(0.5) F26B(0.5) F27(0.5) F27B(0.5) F28(0.5)
 F28B(0.5) F29(0.5) F29B(0.5) F30(0.5) F30B(0.5) C45(0.5) C45B(0.5) C46(0.5)
 C46B(0.5) C47(0.5) C47B(0.5) C48(0.5) C48B(0.5)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C17(H17), C24(H24)
6.b Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B), C58(H58A,
 H58B), C59(H59A,H59B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C20(H20), C21(H21),
 C22(H22), C26(H26), C27(H27), C28(H28), C69(H69), C70(H70), C71(H71), C72(H72),
  C73(H73), C74(H74)
6.d Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C68(H68A,H68B,
 H68C)
;
_shelx_res_checksum              20738
_olex2_date_sample_data_collection 2022-02-11
_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 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.785