7,7-Dimethyl-5<i>H</i>-dibenzo[<i>e</i>,<i>i</i>][1,4,8]triazacycloundecine-6,9,15(7<i>H</i>,8<i>H</i>,14<i>H</i>)-trione pyridine solvate
Morris, James C.; Gordon-Wylie, Scott W.; Clark, George R.; Acta Crystallographica Section C 62 (2006) o674–o676; doi:10.1107/S0108270106041242

data_2015686
_publ_section_title
;7,7-Dimethyl-5<i>H</i>-dibenzo[<i>e</i>,<i>i</i>][1,4,8]triazacycloundecine-6,9,15(7<i>H</i>,8<i>H</i>,14<i>H</i>)-trione
 pyridine solvate
;
_journal_coeditor_code           GA3020
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o674
_journal_page_last               o676
_journal_paper_doi               10.1107/S0108270106041242
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C18 H17 N3 O3,  C5 H5 N'
_chemical_formula_moiety         'C18 H17 N3 O3,  C5 H5 N'
_chemical_formula_sum            'C23 H22 N4 O3'
_chemical_formula_weight         402.45
_chemical_name_common            bba-py
_chemical_name_systematic
;
7,7-dimethyl-7,8-dihydro-5H-dibenzo[e,i][1,4,8]
triazacycloundecine-6,9,15(14H)-trione pyridine solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.42(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.107(2)
_cell_length_b                   11.050(2)
_cell_length_c                   14.627(3)
_cell_measurement_reflns_used    7879
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      1.68
_cell_volume                     1955.1(6)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11782
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9777
_exptl_absorpt_correction_T_min  0.7573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.519
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0409P)^2^+1.2338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                3360
_reflns_number_total             4001
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3020.cif
_cod_data_source_block           I
_cod_original_cell_volume        1955.1(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2015686
_cod_database_fobs_code          2015686