Crystal Structure of 6,7-Dihydro-5a,7a,13,14-tetraaza-pentaphene-5,8-dione
GUILLON, Jean; PEREIRA-ROSENFELD, Maria De Fatima; PINAUD, Noël; BESSON, Thierry; THIÉRY, Valérie; PICOT, Laurent; MARCHIVIE, Mathieu; X-ray Structure Analysis Online 35 (2019) 57–; doi:10.2116/xraystruct.35.57

data_1552775
_publ_section_title
;
 Crystal Structure of
 6,7-Dihydro-5a,7a,13,14-tetraaza-pentaphene-5,8-dione
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              57
_journal_paper_doi               10.2116/xraystruct.35.57
_journal_volume                  35
_journal_year                    2019
_chemical_formula_moiety         'C18 H12 N4 O2'
_chemical_formula_sum            'C18 H12 N4 O2'
_chemical_formula_weight         316.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-05
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.49(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   24.879(3)
_cell_length_b                   6.868(2)
_cell_length_c                   26.068(4)
_cell_measurement_reflns_used    7408
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      67.655
_cell_measurement_theta_min      3.449
_cell_volume                     4172.4(16)
_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, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49888
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.680
_diffrn_reflns_theta_max         67.655
_diffrn_reflns_theta_min         3.449
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.9460
_exptl_absorpt_correction_T_min  0.8725
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'A. C. T. North, D. C. Phillips and F. S. Mathews, Acta. Crystallogr. Sect A, 1968, 24, 351-359'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       needle
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         7408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.1353
_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^)+(0.0050P)^2^+22.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1898
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6846
_reflns_number_total             7408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            35_57_1.txt
_cod_data_source_block           fp
_cod_original_cell_volume        4172.4(15)
_cod_database_code               1552775
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.817
_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:
 C10B(H10A,H10B), C9B(H9BA,H9BB), C10A(H10C,H10D), C9A(H9AA,H9AB), C9C(H9CA,
 H9CB), C10C(H10E,H10F)
2.b Aromatic/amide H refined with riding coordinates:
 C3B(H3B), C6B(H6B), C13B(H13B), C4B(H4B), C16B(H16B), C5B(H5B), C15B(H15B),
 C16C(H16C), C14B(H14B), C14C(H14C), C3C(H3C), C4C(H4C), C15C(H15C), C6A(H6A),
 C5A(H5A), C3A(H3A), C13C(H13C), C6C(H6C), C13A(H13A), C5C(H5C), C4A(H4A),
 C16A(H16A), C15A(H15A), C14A(H14A)
;
_shelx_res_checksum              71754
_shelx_hkl_checksum              99499
_olex2_submission_special_instructions 'No special instructions were received'