Reaction of imidazoline-2-selone derivatives with mesityltellurenyl iodide: a unique example of a 3c-4e Se→Te←Se three-body system embedding a tellurenyl cation
Aragoni, M. Carla; Arca, Massimiliano; Blake, Alexander J.; Cadoni, Enzo; Copolovici, Lucian O.; Isaia, Francesco; Lippolis, Vito; Murgia, Sergio; Pop, Alexandra M.; Silvestru, Cristian; Tidey, Jeremiah P.; Varga, Richard A.; New Journal of Chemistry 43 (2019) 11821–; doi:10.1039/C9NJ01593K

data_7058482
_publ_section_title
;
 Reaction of imidazoline-2-selone derivatives with mesityltellurenyl
 iodide: a unique example of a 3c-4e Se\\rightarrow Te\\leftarrow Se
 three-body system embedding a tellurenyl cation
;
_journal_issue                   30
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11821
_journal_paper_doi               10.1039/C9NJ01593K
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C38 H50 N8 Se4 Te2, 2(C9 H11 I2 Te)'
_chemical_formula_sum            'C56 H72 I4 N8 Se4 Te4'
_chemical_formula_weight         2191.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2019-05-24 deposited with the CCDC.    2019-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.7335(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.25477(18)
_cell_length_b                   16.5149(4)
_cell_length_c                   26.0208(5)
_cell_measurement_reflns_used    5596
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.329
_cell_measurement_theta_min      4.318
_cell_volume                     3547.04(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      'N~2~ gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N~2~'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -96.00  -16.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000   90.0000 80

  2 omega    0.00   28.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 28

  3 omega    6.00   98.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       43.0792 -125.0000    0.0000 92

  4 omega   61.00   91.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -90.0000 30

  5 omega   47.00   76.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  150.0000 29

  6 omega   61.00   93.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000    0.0000 32

  7 omega   60.00  160.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000   90.0000 100

  8 omega   60.00  108.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  -90.0000 48

  9 omega   40.00   91.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -180.0000 51

 10 omega   34.00  122.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  150.0000 88

 11 omega   37.00  116.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  -30.0000 79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      -0.0242035000
_diffrn_orient_matrix_UB_12      0.0844426000
_diffrn_orient_matrix_UB_13      -0.0240272000
_diffrn_orient_matrix_UB_21      -0.1390548000
_diffrn_orient_matrix_UB_22      0.0167921000
_diffrn_orient_matrix_UB_23      0.0374886000
_diffrn_orient_matrix_UB_31      0.1219710000
_diffrn_orient_matrix_UB_32      0.0358668000
_diffrn_orient_matrix_UB_33      0.0390878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_unetI/netI     0.050
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14667
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.569
_diffrn_reflns_theta_min         4.326
_diffrn_source                   'microfocus X-ray tube'
_diffrn_source_type              'Agilent SuperNova'
_exptl_absorpt_coefficient_mu    29.166
_exptl_absorpt_correction_T_max  0.523
_exptl_absorpt_correction_T_min  0.316
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            orange
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.0714
_exptl_crystal_size_mid          0.0358
_exptl_crystal_size_min          0.0266
_refine_diff_density_max         0.74
_refine_diff_density_min         -1.15
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         6935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.99
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0313P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0734
_reflns_number_gt                5784
_reflns_number_total             6935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01593k2.cif
_cod_data_source_block           Compound_II
_cod_depositor_comments
'Adding full bibliography for 7058482--7058483.cif.'
_cod_database_code               7058482
_nottingham_internal_coll_name   VLAJBA
_nottingham_internal_coll_number 14807
_nottingham_internal_coll_client VL/AJB
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '8.0, 32.0'
_nottingham_internal_coll_frame_width 1.0
_nottingham_internal_coll_frame_method omega
_nottingham_internal_coll_user   pcxjpti
_nottingham_internal_coll_date   15/06/2015
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_user pcxjpti
_nottingham_internal_process_date 15/06/2015
_nottingham_internal_solution_user 'Jeremiah Philip Tidey'
_nottingham_internal_solution_date 15/06/2015
_nottingham_internal_refinement_user 'Jeremiah Philip Tidey'
_nottingham_internal_refinement_date 15/06/2015
_nottingham_internal_self_validation_user 'Jeremiah Philip Tidey'
_nottingham_internal_self_validation_date 15/06/2015
_nottingham_internal_validation_user JPT/AJB
_nottingham_internal_validation_date 15/06/2015
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C28 H34 N4 I2 Se2 Te2'
_chemical_oxdiff_usercomment
;
GVB-599 VLAJBA #14807 orange plate mounted in fomblin film on micromount 
for JPT/VL/AJB
;
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, 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), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C15(H15), C13(H13), C24(H24), C22(H22), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C19(H19A,H19B,H19C), C4(H4A,H4B,H4C), C18(H18A,H18B,H18C), C17(H17A,
 H17B,H17C)
;
_shelx_res_checksum              51420
_olex2_submission_special_instructions 'No special instructions were received'