Photo-induced metal-free dehydrogenative N-N homo-coupling.
Balakrishna, Bugga; Mossin, Susanne; Kramer, Søren; Chemical communications (Cambridge, England) 58 (2022) 10977–10980; doi:10.1039/d2cc04204e

data_7130632
_publ_section_title
;
 Photo-induced metal-free dehydrogenative N-N homo-coupling.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10977
_journal_page_last               10980
_journal_paper_doi               10.1039/d2cc04204e
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C26 H20 N2'
_chemical_formula_sum            'C26 H20 N2'
_chemical_formula_weight         360.44
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-20
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-05-06 deposited with the CCDC.	2022-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.488(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8743(10)
_cell_length_b                   5.4117(2)
_cell_length_c                   16.0179(7)
_cell_measurement_reflns_used    7329
_cell_measurement_temperature    119.97(11)
_cell_measurement_theta_max      29.3760
_cell_measurement_theta_min      4.1030
_cell_volume                     1890.34(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      119.97(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3073
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -28.00  43.00   1.00    3.02    --   10.87 -77.00-120.00   71
  2  \w    -13.00  78.00   1.00    3.02    --   10.87  37.00  90.00   91
  3  \w    -10.00  83.00   1.00    3.02    --   10.87  37.00 -30.00   93
  4  \w    -42.00  14.00   1.00    3.02    --   10.87 -77.00 150.00   56
  5  \w    -13.00  81.00   1.00    3.02    --   10.87  57.00-180.00   94
  6  \w    -58.00  39.00   1.00    3.02    --   10.87 -57.00  30.00   97
  7  \w    -66.00 -40.00   1.00    3.02    --  -11.58 122.00 -88.50   26
  8  \w     17.00  42.00   1.00    3.02    --  -11.58  19.00  30.00   25
  9  \w    -84.00 -56.00   1.00    3.02    --  -11.58 150.00  47.74   28
 10  \w    -50.00  -5.00   1.00    3.02    --  -11.58  19.00  30.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0310484000
_diffrn_orient_matrix_UB_12      -0.0236667000
_diffrn_orient_matrix_UB_13      -0.0137843000
_diffrn_orient_matrix_UB_21      0.0076215000
_diffrn_orient_matrix_UB_22      0.0045813000
_diffrn_orient_matrix_UB_23      -0.0421931000
_diffrn_orient_matrix_UB_31      0.0059766000
_diffrn_orient_matrix_UB_32      -0.1288770000
_diffrn_orient_matrix_UB_33      0.0010368000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13668
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         3.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+1.9589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1609
_reflns_number_total             1807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04204e2.cif
_cod_data_source_block           bb-296
_cod_depositor_comments
'Adding full bibliography for 7130632--7130634.cif.'
_cod_database_code               7130632
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C26 H20 N2'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C005(H005), C006(H006), C007(H007), C008(H008), C009(H009), C00A(H00A),
 C00B(H00B), C00C(H00C), C00D(H00D), C00E(H00E)
;
_shelx_res_checksum              71708
_shelx_hkl_checksum              58116
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.269
_oxdiff_exptl_absorpt_empirical_full_min 0.610