N-Substituted tetrahydropentaazadibenzocycloheptafluorenes – a new type of condensed polyazapolycyclic system
Rakhimova, Elena B.; Kirsanov, Victor Yu.; Mescheryakova, Ekaterina S.; Khalilov, Leonard M.; Ibragimov, Askhat G.; New Journal of Chemistry 45 (2021) 1240–1246; doi:10.1039/D0NJ05270A

data_7060140
_publ_section_title
;
 N-Substituted tetrahydropentaazadibenzocycloheptafluorenes -- a new type
 of condensed polyazapolycyclic system
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1240
_journal_page_last               1246
_journal_paper_doi               10.1039/D0NJ05270A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C22 H25 N5'
_chemical_formula_sum            'C22 H25 N5'
_chemical_formula_weight         359.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-13 deposited with the CCDC.	2020-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.070(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5806(4)
_cell_length_b                   18.4584(9)
_cell_length_c                   10.4334(4)
_cell_measurement_reflns_used    2524
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6520
_cell_measurement_theta_min      2.3070
_cell_volume                     1844.75(14)
_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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1709
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_details
;
  1 omega   14.00   42.00   1.0000    2.3450
omega____ theta____ kappa____ phi______ frames
    -      -16.4011   77.0000 -120.0000 28

  2 omega   25.00   51.00   1.0000    2.3450
omega____ theta____ kappa____ phi______ frames
    -      -16.4011   77.0000 -180.0000 26

  3 omega   10.00   84.00   1.0000    2.3450
omega____ theta____ kappa____ phi______ frames
    -       17.1042   77.0000  -30.0000 74

  4 omega   -8.00   81.00   1.0000    2.3450
omega____ theta____ kappa____ phi______ frames
    -       17.1042   77.0000   90.0000 89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0649318000
_diffrn_orient_matrix_UB_12      0.0085820000
_diffrn_orient_matrix_UB_13      0.0278597000
_diffrn_orient_matrix_UB_21      -0.0347804000
_diffrn_orient_matrix_UB_22      -0.0079419000
_diffrn_orient_matrix_UB_23      -0.0589735000
_diffrn_orient_matrix_UB_31      -0.0077648000
_diffrn_orient_matrix_UB_32      -0.0365637000
_diffrn_orient_matrix_UB_33      0.0193941000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8627
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.011
_diffrn_reflns_theta_min         2.395
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88333
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       prizm
_exptl_crystal_F_000             768.0
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0610P)^2^+0.0140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2637
_reflns_number_total             4221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05270a2.cif
_cod_data_source_block           kvy-219
_cod_depositor_comments          'Adding full bibliography for 7060140.cif.'
_cod_original_cell_volume        1844.74(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7060140
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13C(H13C), C13B(H13B), C1'(H1')
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C14(H14A,H14B), C13(H13A,H13D), C11(H11A,H11B), C5(H5A,H5B),
 C3'(H3'A,H3'B), C2'(H2'A,H2'B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C7(H7), C1(H1), C9(H9), C8(H8), C3(H3), C2(H2)
;
_shelx_res_checksum              73565
_shelx_hkl_checksum              96527