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_7716506
_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         'C40 H100 N13 P4, C40 H16 F12 Se4, Cl'
_chemical_formula_sum            'C80 H116 Cl F12 N13 P4 Se4'
_chemical_formula_weight         1963.02
_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             2022-10-24
_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                90.139(4)
_cell_angle_beta                 100.496(5)
_cell_angle_gamma                92.831(4)
_cell_formula_units_Z            2
_cell_length_a                   10.7931(6)
_cell_length_b                   19.8342(8)
_cell_length_c                   21.4238(13)
_cell_measurement_reflns_used    7016
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4160
_cell_measurement_theta_min      4.2100
_cell_volume                     4503.7(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-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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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 -18.00   1.00   49.50    --  -38.50 -37.00  60.00   68
  2  \w    -82.00 -18.00   1.00   49.50    --  -38.50 -57.00   0.00   64
  3  \w    -63.00 -21.00   1.00   49.50    --  -38.50  57.00  30.00   42
  4  \w   -108.00 -28.00   1.00   49.50    --  -38.50 -37.00 150.00   80
  5  \w    -98.00 -13.00   1.00   49.50    --  -38.50 -57.00-120.00   85
  6  \w     48.00  93.00   1.00   49.50    --   42.45-125.00-180.00   45
  7  \w    121.00 172.00   1.00   82.50    --  111.00  77.00  30.00   51
  8  \w     73.00 113.00   1.00   82.50    --  111.00-125.00 -60.00   40
  9  \w     56.00 137.00   1.00   82.50    --  111.00 -61.00 -90.00   81
 10  \w    147.00 176.00   1.00   82.50    --  111.00  61.00  60.00   29
 11  \w     46.00 107.00   1.00   82.50    --  111.00 -94.00 120.00   61
 12  \w     89.00 138.00   1.00   82.50    --  111.00  45.00 -30.00   49
 13  \w    153.00 178.00   1.00   82.50    --  111.00  45.00 -30.00   25
 14  \w     43.00 107.00   1.00   82.50    --  111.00 -61.00  60.00   64
 15  \w    106.00 133.00   1.00   82.50    --  111.00  61.00  60.00   27
 16  \w     96.00 150.00   1.00   82.50    --  111.00 -15.00  30.00   54
 17  \w     85.00 129.00   1.00   82.50    --  111.00 -30.00 -60.00   44
 18  \w     39.00  74.00   1.00   82.50    --  111.00 -30.00 -60.00   35
 19  \w    108.00 174.00   1.00   82.50    --  111.00  77.00   0.00   66
 20  \w    115.00 177.00   1.00   82.50    --  111.00  77.00 -90.00   62
 21  \w     51.00 108.00   1.00   82.50    --  111.00-125.00-150.00   57
 22  \w     80.00 107.00   1.00   82.50    --  111.00 -94.00 -60.00   27
 23  \w     45.00 137.00   1.00   82.50    --  111.00 -61.00-180.00   92
 24  \w     32.00  79.00   1.00   82.50    --  111.00 -15.00  30.00   47
 25  \w     80.00 113.00   1.00   82.50    --  111.00-125.00  90.00   33
 26  \w     78.00 107.00   1.00   82.50    --  111.00 -94.00   0.00   29
 27  \w     48.00 107.00   1.00   82.50    --  111.00 -99.00  76.58   59
 28  \w     39.00 108.00   1.00   82.50    --  111.00-105.00-144.85   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0203542000
_diffrn_orient_matrix_UB_12      0.0743574000
_diffrn_orient_matrix_UB_13      -0.0178218000
_diffrn_orient_matrix_UB_21      0.0607640000
_diffrn_orient_matrix_UB_22      -0.0098211000
_diffrn_orient_matrix_UB_23      -0.0589006000
_diffrn_orient_matrix_UB_31      -0.1304625000
_diffrn_orient_matrix_UB_32      -0.0205671000
_diffrn_orient_matrix_UB_33      -0.0395248000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51472
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.602
_diffrn_reflns_theta_min         3.045
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.519
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.705
_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    1.448
_exptl_crystal_description       needle
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         26168
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1111P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17752
_reflns_number_total             26168
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9974\% 
around [0.00 -0.00 1.00] (reciprocal) or [0.34 0.01 0.94] (direct)
;
_cod_data_source_file            d4dt01730g2.cif
_cod_data_source_block           '[2xCl][7xH]'
_cod_depositor_comments
'Adding full bibliography for 7716503--7716512.cif.'
_cod_database_code               7716506
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C80H116ClF12N13P4Se4
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.586
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5757(8)
 0.4243(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-H1
 0.88 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
C67 \\sim C68B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
5. Others
 Sof(C65B)=Sof(H65C)=Sof(H65D)=Sof(C66B)=Sof(H66D)=Sof(H66E)=Sof(H66F)=1-FVAR(1)
 Sof(C65A)=Sof(H65A)=Sof(H65B)=Sof(C66A)=Sof(H66A)=Sof(H66B)=Sof(H66C)=FVAR(1)
 Sof(H67C)=Sof(H67D)=Sof(C68B)=Sof(H68D)=Sof(H68E)=Sof(H68F)=1-FVAR(2)
 Sof(H67A)=Sof(H67B)=Sof(C68A)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C23(H23), C30(H30)
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), C67(H67A,H67B), C67(H67C,H67D), C69(H69A,H69B), C71(H71A,H71B),
  C73(H73A,H73B), C75(H75A,H75B), C77(H77A,H77B), C79(H79A,H79B), C65A(H65A,
 H65B), C65B(H65C,H65D)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C26(H26), C27(H27),
 C28(H28), C32(H32), C33(H33), C34(H34)
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), C70(H70A,H70B,H70C), C72(H72A,H72B,
 H72C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C), C80(H80A,
 H80B,H80C), C66A(H66A,H66B,H66C), C68A(H68A,H68B,H68C), C66B(H66D,H66E,H66F),
 C68B(H68D,H68E,H68F)
;
_shelx_res_checksum              36271
_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 1.656
_oxdiff_exptl_absorpt_empirical_full_min 0.626
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2