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_7062046
_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         'C14 H12 N Se, Cl, 2(H2 O)'
_chemical_formula_sum            'C14 H16 Cl N O2 Se'
_chemical_formula_weight         344.69
_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
_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                70.419(2)
_cell_angle_beta                 80.430(2)
_cell_angle_gamma                88.427(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3040(2)
_cell_length_b                   9.1476(2)
_cell_length_c                   11.7026(2)
_cell_measurement_reflns_used    6819
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      70.3150
_cell_measurement_theta_min      4.0660
_cell_volume                     726.09(3)
_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_type            'Hybrid Photon Counting Detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_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    -89.00  89.00   0.50    0.50    --    0.00   0.00-180.00  356
  2  \w    -84.00  94.00   0.50    1.00    --    5.00  49.00 -30.00  356
  3  \w   -179.00  -1.00   0.50    1.00    --  -90.00  10.00   0.00  356
  4  \w   -179.00  -1.00   0.50    1.00    --  -90.00  56.00  97.00  356
  5  \w   -179.00  -1.00   0.50    1.00    --  -90.00  58.00 174.44  356
  6  \w   -179.00 -19.00   0.50    1.00    --  -90.00  56.00 134.61  320
  7  \w   -179.00  -1.00   0.50    1.00    --  -90.00  30.00 -30.00  356
  8  \w   -179.00  -1.00   0.50    1.00    --  -90.00  59.00 -27.03  356
  9  \w   -179.00  -1.00   0.50    1.00    --  -90.00  55.00  22.04  356
 10  \w   -179.00  -1.00   0.50    1.00    --  -90.00  55.00  22.04  356
 11  \w   -179.00  -1.00   0.50    1.00    --  -90.00  30.00-150.00  356
 12  \w   -179.00 -19.00   0.50    1.00    --  -90.00  56.00 134.61  320
 13  \w    -48.00 -10.00   0.50    1.00    --  -90.00  30.00 -30.00   76
 14  \w   -157.00-114.00   0.50    1.00    --  -90.00  58.00  27.20   86
 15  \w   -178.00-103.00   0.50    1.00    --  -90.00  59.00 -97.26  150
;
_diffrn_measurement_device       'three-circle quarter \c goniometer'
_diffrn_measurement_device_type  'Rigaku AFC11'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13289
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.225
_diffrn_reflns_theta_min         4.066
_exptl_absorpt_coefficient_mu    5.176
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.968
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       lath
_exptl_crystal_F_000             348
_exptl_crystal_recrystallization_method
'The material was recrystallised from acetonitrile by slow evaporation'
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.003
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2632
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0369P)^2^+0.6573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2466
_reflns_number_total             2632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj04689j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7062046--7062047.cif.'
_cod_database_code               7062046
_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, All O(H,H) groups
2. Restrained distances
 O2-H2C
 0.84 with sigma of 0.02
 O1-H1C
 0.84 with sigma of 0.02
3. Others
 Fixed Sof: H1B(0.5) H2B(0.5) H2C(0.5) H1C(0.5)
4.a Free rotating group:
 O1(H1AA,H1B), O2(H2A,H2B)
4.b 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)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              43022
_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
;