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_1570290
_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, Br, C16 H36 N, C6 H6'
_chemical_formula_sum            'C74 H58 Br F40 N Sb4'
_chemical_formula_weight         2288.12
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-16
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.584(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9954(5)
_cell_length_b                   19.9387(5)
_cell_length_c                   26.1599(6)
_cell_measurement_reflns_used    54520
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      34.1090
_cell_measurement_theta_min      2.6440
_cell_volume                     8109.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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_temperature      100.0(1)
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_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    -15.00  11.00   1.00   18.00    --  -28.13 -99.00 101.12   26
  2  \w    -94.00 -37.00   1.00   18.00    --  -28.13 144.00  93.04   57
  3  \w    -87.00 -30.00   1.00   18.00    --  -28.13 132.00 -38.25   57
  4  \w    -15.00  12.00   1.00   18.00    --  -28.13-101.00   1.77   27
  5  \w    -61.00  49.00   1.00   18.00    --  -28.13  19.00-120.00  110
  6  \w      3.00  97.00   1.00   18.00    --   28.13  57.00   0.00   94
  7  \w    -43.00  49.00   1.00   18.00    --   28.13 -38.00 -30.00   92
  8  \w      0.00  97.00   1.00   18.00    --   28.13  67.00-124.15   97
  9  \w      6.00  82.00   1.00   18.00    --   28.13-125.00 -39.28   76
 10  \w    -40.00  53.00   1.00   18.00    --   28.13 -57.00  90.00   93
 11  \w      7.00  99.00   1.00   18.00    --   28.13  38.00  90.00   92
 12  \w      7.00  99.00   1.00   18.00    --   28.13  38.00 150.00   92
 13  \w    -14.00  13.00   1.00   18.00    --  -28.13-103.00  59.20   27
 14  \w    -58.00  21.00   1.00   18.00    --  -28.13  77.00 -90.00   79
 15  \w    -16.00  10.00   1.00   18.00    --  -28.13 -98.00-133.25   26
 16  \w    -53.00  40.00   1.00   18.00    --  -28.13  57.00 120.00   93
 17  \w    -15.00  11.00   1.00   18.00    --  -28.13 -99.00 -58.58   26
 18  \w    -94.00 -37.00   1.00   18.00    --  -28.13 144.00  45.11   57
 19  \w   -113.00 -58.00   1.00   18.00    --  -28.13 178.00-180.00   55
 20  \w      7.00  99.00   1.00   18.00    --   28.13  38.00 -90.00   92
 21  \w     39.00 112.00   1.00   18.00    --   28.13 178.00   0.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0832
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            314023
_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         2.452
_exptl_absorpt_coefficient_mu    1.946
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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    1.874
_exptl_crystal_description       plate
_exptl_crystal_F_000             4432
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.802
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         23701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0589P)^2^+42.7570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17906
_reflns_number_total             23701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04594c3.cif
_cod_data_source_block           2xTBABr
_cod_depositor_comments
'Adding full bibliography for 1570287--1570290.cif.'
_cod_database_code               1570290
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.584
_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.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C17(H17), C24(H24)
2.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)
2.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)
2.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              39248
_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
;