Direct investigation of chalcogen bonds by multinuclear solid-state magnetic resonance and vibrational spectroscopy.
Kumar, Vijith; Xu, Yijue; Leroy, César; Bryce, David L.; Physical chemistry chemical physics : PCCP 22 (2020) 3817–3824; doi:10.1039/c9cp06267j

data_7239798
_publ_section_title
;
 Direct investigation of chalcogen bonds by multinuclear solid-state
 magnetic resonance and vibrational spectroscopy.
;
_journal_issue                   7
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              3817
_journal_page_last               3824
_journal_paper_doi               10.1039/c9cp06267j
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C10 H8 N2 Se2, C12 H10 N2'
_chemical_formula_sum            'C22 H18 N4 Se2'
_chemical_formula_weight         496.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-27 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.162(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7217(7)
_cell_length_b                   14.197(2)
_cell_length_c                   25.666(3)
_cell_measurement_reflns_used    2450
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.42
_cell_measurement_theta_min      2.87
_cell_volume                     2083.4(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1498
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37092
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.588
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.564
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0856 before and 0.0670 after correction. The Ratio of minimum to maximum transmission is 0.8692. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0050(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2057
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0712P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1326
_reflns_number_total             2057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cp06267j2.cif
_cod_data_source_block           red
_cod_depositor_comments
'Adding full bibliography for 7239797--7239799.cif.'
_cod_original_cell_volume        2083.3(5)
_cod_database_code               7239798
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.551
_shelx_estimated_absorpt_t_min   0.458
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H1 of C1, H8 of C8, H12A of C12A, H11 of C11, H10 of C10,
   H10A of C10A, H8A of C8A, H7 of C7, H12 of C12, H3 of C3, H4 of C4
 At 1.5 times of:
  H7A of C7A, H11A of C11A
2. Restrained distances
 C9-C12 = C9A-C12A
 1.33 with sigma of 0.01
 N1-C11 \\sim N1-C7
 with sigma of 0.02
 C11-C10 \\sim C10-C9 \\sim C9-C8 \\sim C8-C7
 with sigma of 0.02
 N1-C11A \\sim N1-C7A
 with sigma of 0.02
3. Restrained planarity
 N1, C11, C10, C9, C8, C7
 with sigma of 0.1
 N1, C11A, C10A, C9A, C8A, C7A
 with sigma of 0.1
4. Rigid bond restraints
 N1, C7, C7A, C8, C8A, C9, C9A, C10, C10A, C11, C11A, C12, C12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N1 \\sim C7 \\sim C7A \\sim C8 \\sim C8A \\sim C9 \\sim C9A \\sim C10 \\sim
C10A \\sim C11 \\sim C11A \\sim C12 \\sim C12A: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04
6. Others
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=
 Sof(H11A)=Sof(C12A)=Sof(H12A)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=
 Sof(C12)=Sof(H12)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A), C12A(H12A)
;
_shelx_res_checksum              95018
_shelx_hkl_checksum              3812
_olex2_submission_special_instructions 'No special instructions were received'