Two-dimensional hydrogen-bonded networks in two novel glycoluril derivatives
Li-Ping Cao; Xiang-Gao Meng; Meng Gao; Neng-Fang She; An-Xin Wu; Acta Crystallographica Section C 64 (2008) o69–o72; doi:10.1107/S0108270107067108

data_2016424
_publ_section_title
;
 Two-dimensional hydrogen-bonded networks in two novel glycoluril
 derivatives
;
_journal_coeditor_code           AV3132
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o69
_journal_page_last               o72
_journal_paper_doi               10.1107/S0108270107067108
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C20 H21 N5 O2'
_chemical_formula_moiety         'C20 H21 N5 O2'
_chemical_formula_sum            'C20 H21 N5 O2'
_chemical_formula_weight         363.42
_chemical_name_systematic
;
6-ethyl-2a,7b-diphenyl-2,2a,3,4,6,7-hexahydro-1H,5H-2,3,4a,6,7a-
pentaazacyclopenta[cd]azulene-1,4-dione
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.4620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0724(5)
_cell_length_b                   11.6462(7)
_cell_length_c                   19.2338(12)
_cell_measurement_reflns_used    2090
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      21.42
_cell_measurement_theta_min      2.60
_cell_volume                     1778.16(19)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.3\% wide \w exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube'
_diffrn_radiation_type           'Mo k\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16184
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_correction_T_min  0.9820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.4735P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1587
_reflns_number_gt                2581
_reflns_number_total             3860
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            av3132.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               2016424
_cod_database_fobs_code          2016424