Polydentate chalcogen bonding: anion trapping with a water-stable host compound carrying Se-CF<sub>3</sub> functions.
Beckmann, J. Louis; Tiessen, Natalia; Neumann, Beate; Stammler, Hans-Georg; Hoge, Berthold; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12234–12239; doi:10.1039/d4dt01730g

data_7716508
_publ_section_title
;
 Polydentate chalcogen bonding: anion trapping with a water-stable host
 compound carrying Se-CF<sub>3</sub> functions.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12234
_journal_page_last               12239
_journal_paper_doi               10.1039/d4dt01730g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'0.754(I), C40 H16 F12 Se4, C40 H100 N13 P4, 0.246(O)'
_chemical_formula_sum            'C80 H116 F12 I0.75 N13 O0.25 P4 Se4'
_chemical_formula_weight         2027.30
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-14
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-03-05 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                89.415(4)
_cell_angle_beta                 77.434(4)
_cell_angle_gamma                87.161(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7927(4)
_cell_length_b                   20.0311(9)
_cell_length_c                   21.5408(10)
_cell_measurement_reflns_used    13281
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      28.0920
_cell_measurement_theta_min      3.5430
_cell_volume                     4539.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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    -86.00 -60.00   1.00   32.00    --  -25.32  13.00 -16.00   26
  2  \w    -46.00 -21.00   1.00   32.00    --  -25.32 -13.00 171.00   25
  3  \w    -61.00 105.00   1.00   32.00    --   25.95  13.00 -16.00  166
  4  \w    -67.00 127.00   1.00   32.00    --   25.95 -13.00 171.00  194
  5  \w   -120.00 -37.00   1.00   32.00    --  -25.32 178.00 -90.00   83
  6  \w   -120.00 -52.00   1.00   32.00    --  -25.32 178.00  60.00   68
  7  \w   -114.00 -39.00   1.00   32.00    --  -25.32 178.00-180.00   75
  8  \w    -15.00  42.00   1.00   32.00    --   25.95  77.00   0.00   57
  9  \w    -15.00  42.00   1.00   32.00    --   25.95  77.00  60.00   57
 10  \w    -15.00  42.00   1.00   32.00    --   25.95  77.00 -90.00   57
 11  \w    -15.00  42.00   1.00   32.00    --   25.95  77.00-180.00   57
 12  \w     46.00 123.00   1.00   32.00    --   25.95-178.00-180.00   77
 13  \w    -15.00  42.00   1.00   32.00    --   25.95  77.00 120.00   57
 14  \w    -96.00 -60.00   1.00  128.00    --  -25.32 149.00 141.00   36
 15  \w    -12.00  14.00   1.00  128.00    --  -25.32 -77.00 150.00   26
 16  \w   -100.00 -74.00   1.00  128.00    --  -25.32  19.00  60.00   26
 17  \w     35.00  65.00   1.00  128.00    --  -25.32  19.00  60.00   30
 18  \w    -41.00 -15.00   1.00  128.00    --  -25.32 -77.00  30.00   26
 19  \w    -65.00  63.00   1.00  128.00    --  -25.32  57.00 -90.00  128
 20  \w   -115.00 -63.00   1.00  128.00    --  -25.32-149.00  94.00   52
 21  \w    -67.00 -42.00   1.00  128.00    --  -25.32  77.00  90.00   25
 22  \w   -124.00 -39.00   1.00  128.00    --  -25.32-178.00 120.00   85
 23  \w     39.00 125.00   1.00  128.00    --   25.95 178.00-120.00   86
 24  \w    -15.00  42.00   1.00  128.00    --   25.95  77.00  30.00   57
 25  \w    -13.00 114.00   1.00  128.00    --   25.95  57.00 150.00  127
 26  \w    -42.00  67.00   1.00  128.00    --   25.95 -77.00   0.00  109
 27  \w    -15.00  42.00   1.00  128.00    --   25.95  77.00-120.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0110707000
_diffrn_orient_matrix_UB_12      -0.0236441000
_diffrn_orient_matrix_UB_13      -0.0222340000
_diffrn_orient_matrix_UB_21      0.0639478000
_diffrn_orient_matrix_UB_22      -0.0125363000
_diffrn_orient_matrix_UB_23      -0.0044553000
_diffrn_orient_matrix_UB_31      -0.0182355000
_diffrn_orient_matrix_UB_32      -0.0232541000
_diffrn_orient_matrix_UB_33      0.0249786000
_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  0.1551
_diffrn_reflns_av_unetI/netI     0.3831
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            169633
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.491
_diffrn_reflns_theta_min         3.159
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.017
_exptl_absorpt_correction_T_max  0.90024
_exptl_absorpt_correction_T_min  0.90024
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    1.483
_exptl_crystal_description       needle
_exptl_crystal_F_000             2066
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.034
_exptl_crystal_size_rad          0.033
_refine_diff_density_max         0.984
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         24678
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.328
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0645
_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^)+39.9428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23694
_reflns_number_total             24678
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9707\% 
around [0.00 0.00 1.00] (reciprocal) or [-0.40 0.00 0.92] (direct)
;
_cod_data_source_file            d4dt01730g2.cif
_cod_data_source_block           '[2xI][7xH]'
_cod_depositor_comments
'Adding full bibliography for 7716503--7716512.cif.'
_cod_database_code               7716508
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C60 H60  F12 I N9 P4  Se4 '
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.761
_diffrn_oxdiff_digest_frames
;
0183bf93416122d5b686e89d4cff1fd2e2019017c60
;
_diffrn_oxdiff_digest_hkl
;
01a58abbca26bd7348c809e72c64e1b81ca74d
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5540(8)
 0.4460(8)
2. 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
3. Restrained distances
 N1-H1
 0.88 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(I1) = Uanis(O1)
5. Others
 Sof(O1)=1-FVAR(1)
 Sof(I1)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C21(H21), C28(H28)
6.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C47(H47A,H47B), C49(H49A,H49B), C51(H51A,H51B), C53(H53A,
 H53B), C55(H55A,H55B), C57(H57A,H57B), C59(H59A,H59B), C61(H61A,H61B),
 C63(H63A,H63B), C65(H65A,H65B), C67(H67A,H67B), C69(H69A,H69B), C71(H71A,H71B),
  C73(H73A,H73B), C75(H75A,H75B), C77(H77A,H77B), C79(H79A,H79B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26), C30(H30), C31(H31), C32(H32)
6.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C),
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C68(H68A,H68B,
 H68C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C76(H76A,
 H76B,H76C), C78(H78A,H78B,H78C), C80(H80A,H80B,H80C)
;
_shelx_res_checksum              87289
_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 1.937
_oxdiff_exptl_absorpt_empirical_full_min 0.739
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2