2,2,7,7-Tetramethyl-1,2,3,6,7,8-hexahydrocinnolino[5,4,3-<i>cde</i>]cinnoline
Peng, Ju-Hua; Hao, Wen-Juan; Tu, Shu-Jiang; Acta Crystallographica Section E 65 (2009) o238–; doi:10.1107/S1600536808043912

data_2220824
_publ_section_title
2,2,7,7-Tetramethyl-1,2,3,6,7,8-hexahydrocinnolino[5,4,3-<i>cde</i>]cinnoline
_journal_coeditor_code           HK2606
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o238
_journal_paper_doi               10.1107/S1600536808043912
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C16 H20 N4'
_chemical_formula_moiety         'C16 H20 N4'
_chemical_formula_sum            'C16 H20 N4'
_chemical_formula_weight         268.36
_chemical_melting_point_gt       562
_chemical_melting_point_lt       563
_chemical_name_systematic
;
2,2,7,7-Tetramethyl-1,2,3,6,7,8-hexahydrocinnolino[5,4,3-cde]cinnoline
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.462(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.819(4)
_cell_length_b                   8.441(3)
_cell_length_c                   13.310(4)
_cell_measurement_reflns_used    1230
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.229
_cell_measurement_theta_min      2.319
_cell_volume                     1433.7(8)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0483
_diffrn_reflns_av_sigmaI/netI    0.1223
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7218
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9841
_exptl_absorpt_correction_T_min  0.9751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0521
_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^)+0.3048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1785
_reflns_number_gt                1416
_reflns_number_total             2518
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2606.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2220824
_cod_database_fobs_code          2220824