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_7716505
_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_absolute_configuration ad
_chemical_formula_moiety         'Br, C40 H100 N13 P4'
_chemical_formula_sum            'C40 H100 Br N13 P4'
_chemical_formula_weight         967.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                 98.985(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6557(3)
_cell_length_b                   23.7019(5)
_cell_length_c                   17.6543(4)
_cell_measurement_reflns_used    28096
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.5040
_cell_measurement_theta_min      3.1270
_cell_volume                     5230.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (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(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 0.933
_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    -32.00   6.00   1.00    8.00    --  -17.14 -77.00-180.00   38
  2  \w     46.00  76.00   1.00    8.00    --   17.14-132.00  -2.39   30
  3  \w    -51.00  42.00   1.00    8.00    --   17.14 -57.00 -60.00   93
  4  \w     -6.00  84.00   1.00    8.00    --   17.14  57.00-150.00   90
  5  \w     -6.00  86.00   1.00    8.00    --   17.14  57.00 -30.00   92
  6  \w    -42.00  47.00   1.00    8.00    --   17.14 -77.00  60.00   89
  7  \w     -4.00  86.00   1.00    8.00    --   17.14  57.00  90.00   90
  8  \w    -51.00  42.00   1.00    8.00    --   17.14 -57.00-180.00   93
  9  \w     15.00  41.00   1.00    8.00    --   17.14-132.00  -2.39   26
 10  \w      9.00  76.00   1.00    8.00    --   17.14-132.00-158.69   67
;
_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      0.0045870000
_diffrn_orient_matrix_UB_12      0.0256504000
_diffrn_orient_matrix_UB_13      -0.0199223000
_diffrn_orient_matrix_UB_21      -0.0553800000
_diffrn_orient_matrix_UB_22      -0.0011128000
_diffrn_orient_matrix_UB_23      -0.0148988000
_diffrn_orient_matrix_UB_31      -0.0115930000
_diffrn_orient_matrix_UB_32      0.0153680000
_diffrn_orient_matrix_UB_33      0.0321620000
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59330
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.940
_diffrn_reflns_theta_min         2.768
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (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    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 7369 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0069(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         17628
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0298P)^2^+1.5836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                16556
_reflns_number_total             17628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01730g2.cif
_cod_data_source_block           '[7xH]Br'
_cod_depositor_comments
'Adding full bibliography for 7716503--7716512.cif.'
_cod_database_code               7716505
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H100 N13 P4 Br'
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.784
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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.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), C33(H33A,
 H33B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B)
2.b 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), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              59891
_olex2_date_sample_data_collection 2022-02-04
_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 1.146
_oxdiff_exptl_absorpt_empirical_full_min 0.908