Crystal structure of 4,10-dimethoxy-13-methyl-6<i>H</i>,12<i>H</i>-6,12-epiminodibenzo[<i>b</i>,<i>f</i>][1,5]dioxocine
Kasyanova, Katerina V.; Kokozay, Vladimir N.; Buvaylo, Elena A.; Vassilyeva, Olga Yu.; Skelton, Brian W.; Acta Crystallographica Section E 73 (2017) 410–412; doi:10.1107/S2056989017002328

data_2242039
_publ_section_title
;
 Crystal structure of
 4,10-dimethoxy-13-methyl-6<i>H</i>,12<i>H</i>-6,12-epiminodibenzo[<i>b</i>,<i>f</i>][1,5]dioxocine
;
_journal_coeditor_code           HG5482
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              410
_journal_page_last               412
_journal_paper_doi               10.1107/S2056989017002328
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C17 H17 N O4'
_chemical_formula_moiety         'C17 H17 N O4'
_chemical_formula_sum            'C17 H17 N O4'
_chemical_formula_weight         299.31
_chemical_name_systematic
4,10-Dimethoxy-13-methyl-6<i>H</i>,12<i>H</i>-6,12-epiminodibenzo[<i>b</i>,<i>f</i>][1,5]dioxocine
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                93.980(6)
_cell_angle_beta                 106.603(7)
_cell_angle_gamma                102.133(6)
_cell_formula_units_Z            2
_cell_length_a                   6.9956(5)
_cell_length_b                   8.8589(6)
_cell_length_c                   12.0938(9)
_cell_measurement_reflns_used    2735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.096
_cell_measurement_theta_min      3.857
_cell_volume                     695.46(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
WinGX (Farrugia, 1999)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5235
_diffrn_reflns_theta_full        67.243
_diffrn_reflns_theta_max         67.242
_diffrn_reflns_theta_min         3.851
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.81756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       plate
_exptl_crystal_F_000             316
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+0.1321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                2147
_reflns_number_total             2456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hg5482sup1.cif
_cod_data_source_block           I
_cod_database_code               2242039
_cod_database_fobs_code          2242039
_shelx_hkl_checksum              75840
_shelx_res_checksum              72678