Selanyl and tellanyl electrophiles as a driving force in the construction of sophisticated polyaromatic hydrocarbons
Arsenyan, Pavel; Petrenko, Alla; Belyakov, Sergey; New Journal of Chemistry 45 (2021) 7247–7255; doi:10.1039/D1NJ00401H

data_7060488
_publ_section_title
;
 Selanyl and tellanyl electrophiles as a driving force in the construction
 of sophisticated polyaromatic hydrocarbons
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7247
_journal_page_last               7255
_journal_paper_doi               10.1039/D1NJ00401H
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H17 N Se'
_chemical_formula_sum            'C27 H17 N Se'
_chemical_formula_weight         434.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_Int_Tables_number      33
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2-ac4
(compiled 2018.05.17 svn.r3504 for Rigaku Oxford Diffraction, GUI svn.r5492)
;
_audit_update_record
;
2020-06-05 deposited with the CCDC.	2021-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.83567(8)
_cell_length_b                   15.85744(8)
_cell_length_c                   7.87700(3)
_cell_measurement_reflns_used    18777
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      76.9820
_cell_measurement_theta_min      3.9390
_cell_volume                     1978.019(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.8213
_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    -29.00  22.00   0.50    0.25    --  -49.35  23.00-136.00  102
  2  \w    -93.00 -67.00   0.50    0.25    --  -84.25 128.00  79.00   52
  3  \w   -141.00-116.00   0.50    0.25    --  -84.25 -23.00  58.00   50
  4  \w    144.00 170.00   0.50    0.25    --  105.75 128.00  79.00   52
  5  \w     90.00 129.00   0.50    0.25    --  105.75 128.00  79.00   78
  6  \w     69.00  95.00   0.50    0.25    --  105.75-102.00-101.00   52
  7  \w    -21.00  19.00   0.50    0.25    --  -49.35  19.00   0.00   80
  8  \w   -116.00 -88.00   0.50    0.25    --  -49.35-125.00 120.00   56
  9  \w   -117.00 -88.00   0.50    0.25    --  -49.35 -77.00 150.00   58
 10  \w   -120.00 -95.00   0.50    0.25    --  -49.35 -77.00 -60.00   50
 11  \w    -17.00  26.00   0.50    0.25    --   49.66 -19.00 -30.00   86
 12  \w    121.00 167.00   0.50    0.25    --  105.75 125.00  90.00   92
 13  \w    146.00 177.00   0.50    0.25    --  105.75 125.00 120.00   62
 14  \w     36.00  71.00   0.50    0.25    --  105.75 -61.00  60.00   70
 15  \w     92.00 119.00   0.50    0.25    --  105.75 125.00 120.00   54
 16  \w    147.00 172.00   0.50    0.25    --  105.75  15.00   0.00   50
 17  \w     88.00 147.00   0.50    0.25    --  105.75  77.00  30.00  118
 18  \w     35.00  65.00   0.50    0.25    --  105.75 -77.00  60.00   60
 19  \w     80.00 105.00   0.50    0.25    --  105.75 -77.00  60.00   50
 20  \w     78.00 104.00   0.50    0.25    --  105.75 -94.00-150.00   52
 21  \w     43.00  68.00   0.50    0.25    --  105.75 -61.00 -90.00   50
 22  \w     64.00  90.00   0.50    0.25    --  105.75-125.00  30.00   52
 23  \w    122.00 165.00   0.50    0.25    --  105.75 125.00-120.00   86
 24  \w     61.00 100.00   0.50    0.25    --  105.75 -77.00  30.00   78
 25  \w     42.00  68.00   0.50    0.25    --  105.75 -81.00-167.72   52
 26  \w    100.00 127.00   0.50    0.25    --  105.75 -81.00-167.72   54
 27  \w     40.00  65.00   0.50    0.25    --  105.75 -61.00 -60.00   50
 28  \w    123.00 161.00   0.50    0.25    --  105.75  15.00  90.00   76
 29  \w     78.00 132.00   0.50    0.25    --  105.75 148.00 153.56  108
 30  \w     40.00  65.00   0.50    0.25    --  105.75 -77.00 -90.00   50
 31  \w     75.00 101.00   0.50    0.25    --  105.75 -77.00 -90.00   52
 32  \w     38.00  63.00   0.50    0.25    --  105.75 -77.00 -30.00   50
 33  \w     34.00  82.00   0.50    0.25    --  105.75 -77.00 150.00   96
 34  \w     40.00  66.00   0.50    0.25    --  105.75 -94.00-150.00   52
 35  \w     98.00 123.00   0.50    0.25    --  105.75  77.00-180.00   50
 36  \w    100.00 178.00   0.50    0.25    --  105.75  15.00 -60.00  156
 37  \w     35.00  87.00   0.50    0.25    --  105.75 -94.00  30.00  104
 38  \w     37.00  66.00   0.50    0.25    --  105.75 -61.00 -30.00   58
 39  \w    102.00 127.00   0.50    0.25    --  105.75   0.00-180.00   50
 40  \w    124.00 153.00   0.50    0.25    --  105.75   0.00   0.00   58
 41  \w    112.00 138.00   0.50    0.25    --  105.75  23.00-136.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0725789000
_diffrn_orient_matrix_UB_12      -0.0606087000
_diffrn_orient_matrix_UB_13      0.0455934000
_diffrn_orient_matrix_UB_21      0.0645879000
_diffrn_orient_matrix_UB_22      0.0703381000
_diffrn_orient_matrix_UB_23      -0.0367214000
_diffrn_orient_matrix_UB_31      -0.0050261000
_diffrn_orient_matrix_UB_32      0.0286213000
_diffrn_orient_matrix_UB_33      0.1865870000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            20221
_diffrn_reflns_theta_full        75.0
_diffrn_reflns_theta_max         77.24
_diffrn_reflns_theta_min         3.95
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.651
_exptl_absorpt_correction_T_max  0.96704
_exptl_absorpt_correction_T_min  0.73145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Yellow '
_exptl_crystal_density_diffrn    1.4586
_exptl_crystal_description       Plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.2673
_refine_diff_density_min         -0.5366
_refine_diff_density_rms         0.0462
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.005(14)
_refine_ls_d_res_high            0.7904
_refine_ls_d_res_low             11.2052
_refine_ls_goodness_of_fit_ref   1.0500
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3428
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0500
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.1930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.615
_reflns_limit_h_max              20
_reflns_limit_h_min              -19
_reflns_limit_k_max              20
_reflns_limit_k_min              -19
_reflns_limit_l_max              9
_reflns_limit_l_min              -7
_reflns_number_gt                3405
_reflns_number_total             3428
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj00401h2.cif
_cod_data_source_block           A546new
_cod_depositor_comments
'Adding full bibliography for 7060487--7060492.cif.'
_cod_original_cell_volume        1978.020(16)
_cod_original_sg_symbol_Hall     ' P 2c -2n'
_cod_database_code               7060488
_chemical_oxdiff_formula         'C108 H68 N4 Se4'
_chemical_oxdiff_usercomment     'from Pavel'
_diffrn_oxdiff_digest_frames
;
01845d136f852998c3f8457f4f045b4c3000072ab60
;
_diffrn_oxdiff_digest_hkl
;
01199cb2a695c653d044f5e38df3fed12fc049
;
_reflns_odcompleteness_completeness 99.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C17(H17), C25(H25), C23(H23), C1(H1), C6(H6), C15(H15), C8(H8),
 C3(H3), C19(H19), C24(H24), C7(H7), C16(H16), C21(H21), C18(H18), C22(H22),
 C5(H5)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.531
_oxdiff_exptl_absorpt_empirical_full_min 0.665