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_7716509
_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         'I, C40 H100 N13 P4, C3 H6 O'
_chemical_formula_sum            'C43 H106 I N13 O P4'
_chemical_formula_weight         1072.18
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-04
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-03-05 deposited with the CCDC.	2024-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2326(2)
_cell_length_b                   26.7724(4)
_cell_length_c                   19.2696(3)
_cell_measurement_reflns_used    59836
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      34.0940
_cell_measurement_theta_min      1.9390
_cell_volume                     5707.98(16)
_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      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_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    -39.00  61.00   1.00   22.00    --   31.19 -77.00-174.00  100
  2  \w      6.00 104.00   1.00   22.00    --   31.19  38.00 150.00   98
  3  \w     11.00 100.00   1.00   22.00    --   31.19  57.00  30.00   89
  4  \w    -38.00  53.00   1.00   22.00    --   31.19 -57.00  90.00   91
  5  \w     11.00 100.00   1.00   22.00    --   31.19  57.00 -30.00   89
  6  \w    -10.00  16.00   1.00   22.00    --   31.19  98.00  89.77   26
  7  \w    -41.00  57.00   1.00   22.00    --   31.19 -38.00 -30.00   98
  8  \w    -38.00  53.00   1.00   22.00    --   31.19 -57.00-120.00   91
  9  \w    -11.00  15.00   1.00   22.00    --   31.19  99.00-153.34   26
 10  \w    -15.00  73.00   1.00   22.00    --   31.19 -99.00  60.00   88
 11  \w    -11.00  15.00   1.00   22.00    --   31.19  99.00 -63.00   26
 12  \w    -11.00  15.00   1.00   22.00    --   31.19 100.00 145.18   26
 13  \w     39.00 107.00   1.00   22.00    --   31.19 178.00  60.00   68
 14  \w     11.00 100.00   1.00   22.00    --   31.19  57.00-120.00   89
 15  \w    -42.00   7.00   1.00   22.00    --  -23.50 -77.00  30.00   49
 16  \w    -99.00 -39.00   1.00   22.00    --  -23.50-178.00 -90.00   60
 17  \w    -11.00  15.00   1.00   22.00    --   31.19  99.00  21.60   26
 18  \w     37.00 108.00   1.00   22.00    --   31.19-178.00  30.00   71
 19  \w      6.00 104.00   1.00   22.00    --   31.19  38.00 -30.00   98
 20  \w     11.00 100.00   1.00   22.00    --   31.19  57.00-150.00   89
 21  \w     -7.00  23.00   1.00   22.00    --   31.19  92.00-137.15   30
 22  \w    -15.00  73.00   1.00   22.00    --   31.19 -99.00 -90.00   88
 23  \w    -10.00   4.00   1.00   22.00    --   31.19  98.00 123.21   14
;
_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      0.0606424000
_diffrn_orient_matrix_UB_12      0.0083240000
_diffrn_orient_matrix_UB_13      0.0031080000
_diffrn_orient_matrix_UB_21      -0.0196168000
_diffrn_orient_matrix_UB_22      0.0206628000
_diffrn_orient_matrix_UB_23      -0.0220797000
_diffrn_orient_matrix_UB_31      -0.0069526000
_diffrn_orient_matrix_UB_32      0.0143368000
_diffrn_orient_matrix_UB_33      0.0299842000
_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  0.0581
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            243682
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.441
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.533
_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    1.248
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.139
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         23174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0289P)^2^+3.0070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18704
_reflns_number_total             23174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01730g2.cif
_cod_data_source_block           '[7xH]IxMe2CO'
_cod_depositor_comments
'Adding full bibliography for 7716503--7716512.cif.'
_cod_database_code               7716509
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H106 N13 I O P4 '
_diffrn_oxdiff_digest_frames
;
01a80a082f80993de43b4eace4da755ab101532f233
;
_diffrn_oxdiff_digest_hkl
;
01179aaea4dffa4afaadb3b343cb2e2e3fccb5
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C43B) = Uanis(C43A)
3. Others
 Sof(C33B)=Sof(H33C)=Sof(H33D)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C33A)=Sof(H33A)=Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(I1B)=1-FVAR(2)
 Sof(I1A)=FVAR(2)
 Sof(O1B)=Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C42B)=Sof(C43B)=
 Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(3)
 Sof(O1A)=Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42A)=Sof(C43A)=
 Sof(H43A)=Sof(H43B)=Sof(H43C)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B),
 C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B),
  C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33A(H33A,
 H33B), C33B(H33C,H33D), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B)
4.b Me refined with riding coordinates:
 C41B(H41D,H41E,H41F), C43B(H43D,H43E,H43F)
4.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C34A(H34A,H34B,H34C), C34B(H34D,H34E,H34F),
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41A(H41A,H41B,
 H41C), C43A(H43A,H43B,H43C)
;
_shelx_res_checksum              77905
_olex2_date_sample_data_collection 2022-02-02
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.321
_oxdiff_exptl_absorpt_empirical_full_min 0.810