An unprecedented non-classical polyinterhalogen anion made of [I2Cl]− and I2 at the 2-(p-tolyl)selenopheno[2,3-b]pyridinium cation template
Aragoni, M. Carla; Podda, Enrico; Arca, Massimiliano; Pintus, Anna; Lippolis, Vito; Caltagirone, Claudia; Bartz, Ricardo H.; Lenardão, Eder J.; Perin, Gelson; Schumacher, Ricardo F.; Coles, Simon J.; Orton, James B.; New Journal of Chemistry 46 (2022) 21921–21929; doi:10.1039/D2NJ04689J

data_7062047
_publ_section_title
;
 An unprecedented non-classical polyinterhalogen anion made of
 [I2Cl]&#x2212; and I2 at the 2-(p-tolyl)selenopheno[2,3-b]pyridinium
 cation template
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21921
_journal_page_last               21929
_journal_paper_doi               10.1039/D2NJ04689J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'Cl I2, 0.167(I2), C14 H12 N Se'
_chemical_formula_sum            'C14 H12 Cl I2.33 N Se'
_chemical_formula_weight         604.76
_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   geom
_audit_creation_date             2022-01-27
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-02 deposited with the CCDC.	2022-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                94.0460(10)
_cell_angle_beta                 95.4730(10)
_cell_angle_gamma                111.1560(10)
_cell_formula_units_Z            6
_cell_length_a                   11.76310(10)
_cell_length_b                   14.0582(2)
_cell_length_c                   16.4528(2)
_cell_measurement_reflns_used    50518
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5920
_cell_measurement_theta_min      1.8550
_cell_volume                     2509.62(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_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    -97.00  25.00   0.50    1.50    --   -7.30 -60.00 150.00  244
  2  \w    -40.00  82.00   0.50    1.50    --   -7.30  60.00  60.00  244
  3  \w    -40.00  82.00   0.50    1.50    --   -7.30  60.00 -30.00  244
  4  \w    -40.00  82.00   0.50    1.50    --   -7.30  60.00 -30.00  244
  5  \w    -43.00  82.00   0.50    1.50    --   -7.30  38.00  30.00  250
  6  \w    -43.00  82.00   0.50    1.50    --   -7.30  38.00 150.00  250
  7  \w    -97.00  24.00   0.50    1.50    --   -7.30 -57.00  30.00  242
  8  \w    -97.00  25.00   0.50    1.50    --   -7.30 -60.00 -90.00  244
  9  \w    -40.00  82.00   0.50    1.50    --   -7.30  60.00 -90.00  244
 10  \w    -40.00  82.00   0.50    1.50    --   -7.30  60.00-180.00  244
 11  \w    -97.00 -36.00   0.50    1.50    --   -7.30 -38.00-180.00  122
 12  \w    -43.00  82.00   0.50    1.50    --   -7.30  38.00-120.00  250
;
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            115623
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.563
_exptl_absorpt_coefficient_mu    6.697
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_description       '(cut) block'
_exptl_crystal_F_000             1666
_exptl_crystal_recrystallization_method
'The material was recrystallised from acetonitrile by slow evaporation'
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         11505
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0230P)^2^+8.2660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10395
_reflns_number_total             11505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04689j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7062046--7062047.cif.'
_cod_original_cell_volume        2509.62(5)
_cod_database_code               7062047
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 I3-I4A \\sim I3-I4B
 with sigma of 0.02
 I5-I6A \\sim I5-I6B
 with sigma of 0.02
 I1-I2A \\sim I1-I2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
I1 \\sim I2A \\sim I2B: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
I5 \\sim I6A \\sim I6B: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004 within 2A
4. Others
 Sof(I4B)=1-FVAR(1)
 Sof(I4A)=FVAR(1)
 Sof(I6B)=1-FVAR(2)
 Sof(I6A)=FVAR(2)
 Sof(I2B)=1-FVAR(3)
 Sof(I2A)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C3(H3), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13),
  N2(H2A), C15(H15), C16(H16), C17(H17), C20(H20), C23(H23), C24(H24), C26(H26),
  C27(H27), N3(H3A), C29(H29), C30(H30), C31(H31), C34(H34), C37(H37), C38(H38),
  C40(H40), C41(H41)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              14639
_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
- B-factor correction
;