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_7239797
_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      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
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-09-26
_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                77.499(2)
_cell_angle_beta                 78.664(2)
_cell_angle_gamma                73.377(2)
_cell_formula_units_Z            1
_cell_length_a                   5.7832(5)
_cell_length_b                   7.7601(7)
_cell_length_c                   12.0835(11)
_cell_measurement_reflns_used    7888
_cell_measurement_temperature    200
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.78
_cell_volume                     502.02(8)
_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    'olex2.solve (Bourhis et al., 2015)'
_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 0.999
_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  0.1471
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32771
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         1.744
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.695
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0939 before and 0.0542 after correction. The Ratio of minimum to maximum transmission is 0.7917. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_description       plate
_exptl_crystal_F_000             246
_exptl_crystal_preparation       Cocrystallization
_exptl_crystal_recrystallization_method 'Solvent evaporation'
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0282P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1637
_reflns_number_total             1978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cp06267j2.cif
_cod_data_source_block           red_a
_cod_depositor_comments
'Adding full bibliography for 7239797--7239799.cif.'
_cod_database_code               7239797
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.497
_shelx_estimated_absorpt_t_min   0.366
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C006(H00C,H00F)
2.b Aromatic/amide H refined with riding coordinates:
 C004(H004), C005(H005), C009(H009), C00B(H00B), C00D(H00D), C00A(H00A),
 C00E(H00E)
;
_shelx_res_checksum              70044
_shelx_hkl_checksum              65700
_olex2_submission_special_instructions 'No special instructions were received'