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_1570287
_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, C H2 Cl2'
_chemical_formula_sum            'C53 H18 Cl2 F40 Sb4'
_chemical_formula_weight         1972.57
_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             2022-03-24
_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                79.806(3)
_cell_angle_beta                 77.865(3)
_cell_angle_gamma                69.445(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5356(6)
_cell_length_b                   14.1129(5)
_cell_length_c                   17.7477(6)
_cell_measurement_reflns_used    21336
_cell_measurement_temperature    99.98(12)
_cell_measurement_theta_max      31.5940
_cell_measurement_theta_min      1.8040
_cell_volume                     3083.7(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 (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      99.98(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_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      9.00  87.00   1.00   36.30    --   26.50-130.00 171.71   78
  2  \w    -42.00  48.00   1.00   36.30    --   26.50 -57.00 -90.00   90
  3  \w      5.00  95.00   1.00   36.30    --   26.50  57.00-120.00   90
  4  \w     39.00 102.00   1.00   36.30    --   26.50 178.00 -30.00   63
  5  \w    -18.00  99.00   1.00   36.30    --   26.50  19.00 120.00  117
  6  \w      1.00  99.00   1.00   36.30    --   26.50  38.00-180.00   98
  7  \w      9.00  88.00   1.00   36.30    --   26.50-132.00 -12.38   79
  8  \w     -4.00  42.00   1.00   36.30    --   26.50  77.00 -30.00   46
  9  \w     -4.00  42.00   1.00   36.30    --   26.50  77.00  90.00   46
 10  \w     -4.00  42.00   1.00   36.30    --   26.50  77.00  30.00   46
 11  \w    -42.00  48.00   1.00   36.30    --   26.50 -57.00   0.00   90
 12  \w     -4.00  42.00   1.00   36.30    --   26.50  77.00-180.00   46
 13  \w    -46.00  42.00   1.00   36.30    --   26.50   0.00  30.00   88
;
_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      0.0442332000
_diffrn_orient_matrix_UB_12      0.0100027000
_diffrn_orient_matrix_UB_13      0.0082259000
_diffrn_orient_matrix_UB_21      0.0333606000
_diffrn_orient_matrix_UB_22      -0.0498340000
_diffrn_orient_matrix_UB_23      -0.0078392000
_diffrn_orient_matrix_UB_31      0.0120678000
_diffrn_orient_matrix_UB_32      0.0182957000
_diffrn_orient_matrix_UB_33      -0.0395411000
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0484
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68786
_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         30.081
_diffrn_reflns_theta_min         1.551
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.979
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.729
_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    2.124
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1868
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.078
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         18108
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0538P)^2^+15.2446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13324
_reflns_number_total             18108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04594c3.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 1570287--1570290.cif.'
_cod_database_code               1570287
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C53H18Cl2F40Sb4
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.742
_diffrn_oxdiff_digest_frames
;
01dd7afc8f9235ca4776c9016ae5ca09b900027c33f
;
_diffrn_oxdiff_digest_hkl
;
0168a5920578e03a514a5763f5e5f22b592c0d
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1A-C53A \\sim Cl1B-C53B \\sim Cl2A-C53A \\sim Cl2B-C53B
 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 0.0001 and sigma for terminal atoms of 0.0002
F36B \\sim F37B \\sim F38B \\sim F39B \\sim F40B \\sim C51B \\sim C52B: within
2A with sigma of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(F38A) = Uanis(F38B)
Uanis(F40B) = Uanis(F40A)
Uanis(F39B) = Uanis(F39A)
Uanis(F36A) = Uanis(F36B)
Uanis(F37A) = Uanis(F37B)
Uanis(C53A) = Uanis(C53B)
Uanis(Cl1B) = Uanis(Cl2B)
4. 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(Cl1B)=Sof(Cl2B)=Sof(C53B)=Sof(H53C)=Sof(H53D)=1-FVAR(2)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C53A)=Sof(H53A)=Sof(H53B)=FVAR(2)
5.a Free rotating group:
 C51A(F36A,F37A,F38A,F39A,F40A,C52A), C51B(F36B,F37B,F38B,F39B,F40B,C52B)
5.b Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C29(H29), C36(H36)
5.c Secondary CH2 refined with riding coordinates:
 C53A(H53A,H53B), C53B(H53C,H53D)
5.d 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)
;
_shelx_res_checksum              48281
_olex2_date_sample_data_collection 2022-03-17
_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 1.516
_oxdiff_exptl_absorpt_empirical_full_min 0.778