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_7716510
_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 H16 F12 Se4, Cl, C24 H20 P, 2(C6 H6), 1[C6H6]'
_chemical_formula_sum            'C82 H54 Cl F12 P Se4'
_chemical_formula_weight         1649.51
_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             2023-08-03
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6804)
;
_audit_update_record
;
2024-03-05 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.640(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1681(8)
_cell_length_b                   21.1450(7)
_cell_length_c                   21.2518(10)
_cell_measurement_reflns_used    40323
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      31.9210
_cell_measurement_theta_min      3.6420
_cell_volume                     7171.1(6)
_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-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_environment      N~2~
_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 0.998
_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    -87.00   0.00   1.00   35.00    --  -16.48 -60.00  71.00   87
  2  \w    -27.00  54.00   1.00   35.00    --  -16.48  60.00-149.00   81
  3  \w      5.00  87.00   1.00   35.00    --   17.10  60.00-149.00   82
  4  \w    -53.00  44.00   1.00   35.00    --   17.10 -60.00  71.00   97
  5  \w    -91.00 -28.00   1.00   35.00    --  -16.48 153.00 -84.02   63
  6  \w    -91.00 -30.00   1.00   35.00    --  -16.48 153.00-165.15   61
  7  \w    -14.00  38.00   1.00   35.00    --   17.10  77.00  60.00   52
  8  \w     27.00  86.00   1.00   35.00    --   17.10-146.00-125.75   59
  9  \w    -38.00  30.00   1.00   35.00    --   17.10 -77.00 -30.00   68
 10  \w     -5.00  90.00   1.00   35.00    --   17.10  38.00   0.00   95
;
_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      -0.0370790000
_diffrn_orient_matrix_UB_12      0.0184813000
_diffrn_orient_matrix_UB_13      -0.0121354000
_diffrn_orient_matrix_UB_21      -0.0145479000
_diffrn_orient_matrix_UB_22      -0.0149561000
_diffrn_orient_matrix_UB_23      0.0234354000
_diffrn_orient_matrix_UB_31      0.0197566000
_diffrn_orient_matrix_UB_32      0.0236534000
_diffrn_orient_matrix_UB_33      0.0243223000
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            173219
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         3.233
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.182
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
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    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             3288
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         20941
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0299P)^2^+5.2615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17250
_reflns_number_total             20941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01730g2.cif
_cod_data_source_block           '[2xCl][PPh4]x2C6H6'
_cod_depositor_comments
'Adding full bibliography for 7716503--7716512.cif.'
_cod_database_code               7716510
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C82 H54 Cl F12 P Se4 '
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.590
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim
C79 \\sim C80 \\sim C81 \\sim C82: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
3. Others
 Sof(C71)=Sof(H8A)=Sof(C72)=Sof(H9A)=Sof(C73)=Sof(H1A)=Sof(C74)=Sof(H11A)=
 Sof(C75)=Sof(H4A)=Sof(C76)=Sof(H10A)=1-FVAR(1)
 Sof(C77)=Sof(H10)=Sof(C78)=Sof(H8)=Sof(C79)=Sof(H9)=Sof(C80)=Sof(H1)=Sof(C81)=
 Sof(H11)=Sof(C82)=Sof(H4)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C3(H00Q), C10(H01T), C21(H011), C28(H01G)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H01J), C7(H01U), C8(H00T), C12(H00W), C13(H013), C14(H01Q), C24(H01E),
 C25(H01V), C26(H00X), C30(H01B), C31(H01H), C32(H01O), C42(H028), C43(H02A),
 C44(H027), C45(H029), C46(H01W), C48(H01N), C49(H01L), C50(H01Y), C51(H02B),
 C52(H021), C54(H020), C55(H01X), C56(H01M), C57(H01R), C58(H019), C60(H01Z),
 C61(H023), C62(H024), C63(H022), C64(H01S), C65(H026), C66(H02E), C67(H02G),
 C68(H02D), C69(H02I), C70(H02H), C71(H8A), C72(H9A), C73(H1A), C74(H11A),
 C75(H4A), C76(H10A), C77(H10), C78(H8), C79(H9), C80(H1), C81(H11), C82(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2585
_shelx_fab_checksum              58021
_olex2_date_sample_data_collection 2023-08-02
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.852