Observation of an infrequent enantiomer/conformer substitutional disorder in ethyl 13-ethyl-4-oxo-8,13-dihydro-4H-benzo[5,6]azepino[3,2,1-ij]quinoline-5-carboxylate heptane hemisolvate
Macías, Mario A.; Sanabria, Elkin E.; Acosta-Quintero, Lina M.; Palma, Alirio; Suescun, Leopoldo; Acta Crystallographica Section C Structural Chemistry 74 (2018) –; doi:10.1107/S2053229618015152

data_2021330
_publ_section_title
;
 Observation of an infrequent enantiomer/conformer substitutional disorder
 in ethyl
 13-ethyl-4-oxo-8,13-dihydro-4H-benzo[5,6]azepino[3,2,1-ij]quinoline-5-carboxylate
 heptane hemisolvate
;
_journal_coeditor_code           LG3226
_journal_issue                   12
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229618015152
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C22 H21 N O3, 0.5C7 H16'
_chemical_formula_moiety         'C22 H21 N O3, 0.5(C7 H16)'
_chemical_formula_sum            'C25.5 H29 N O2'
_chemical_formula_weight         397.50
_chemical_name_systematic
'Ethyl 13-ethyl-4-oxo-8,13-dihydro-4<i>H</i>-benzo[5,6]azepino[3,2,1-<i>ij</i>]quinoline-5-carboxylate heptane hemisolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                89.4670(13)
_cell_angle_beta                 74.3830(12)
_cell_angle_gamma                68.1250(12)
_cell_formula_units_Z            4
_cell_length_a                   11.9894(3)
_cell_length_b                   13.6171(4)
_cell_length_c                   14.3939(4)
_cell_measurement_reflns_used    9513
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.586
_cell_measurement_theta_min      3.516
_cell_volume                     2089.34(10)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58149
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.735
_diffrn_reflns_theta_min         3.205
_diffrn_source                   'Cu Incoatec microsource'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.592
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     930
_refine_ls_number_reflns         8506
_refine_ls_number_restraints     2653
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0748P)^2^+1.6604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                7414
_reflns_number_total             8506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lg3226sup1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C25.5 H29 N1 O2'
_cod_database_code               2021330
_shelx_estimated_absorpt_t_min   0.776
_shelx_estimated_absorpt_t_max   0.944
_shelx_hkl_checksum              21906
_shelx_res_checksum              59550
_cod_database_fobs_code 2021330