Diastereoisomeric forms of 11-ethyl-6,11-dihydro-5<i>H</i>-dibenzo[<i>b</i>,<i>e</i>]azepine-6-carboxamide: syntheses and the molecular and supramolecular structure of the minor form (6<i>RS</i>,11<i>RS</i>)-11-ethyl-6,11-dihydro-5<i>H</i>-dibenzo[<i>b</i>,<i>e</i>]azepine-6-carboxamide
Acosta Quintero, Lina M.; Palma, Alirio; Cobo, Justo; Glidewell, Christopher; Acta Crystallographica Section C 72 (2016) 549–554; doi:10.1107/S2053229616008950

data_2020536
_publ_section_title
;
 Diastereoisomeric forms of
 11-ethyl-6,11-dihydro-5<i>H</i>-dibenzo[<i>b</i>,<i>e</i>]azepine-6-carboxamide:
 syntheses and the molecular and supramolecular structure of the minor
 form
 (6<i>RS</i>,11<i>RS</i>)-11-ethyl-6,11-dihydro-5<i>H</i>-dibenzo[<i>b</i>,<i>e</i>]azepine-6-carboxamide
;
_journal_coeditor_code           SK3628
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              549
_journal_page_last               554
_journal_paper_doi               10.1107/S2053229616008950
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C17 H18 N2 O'
_chemical_formula_moiety         'C17 H18 N2 O'
_chemical_formula_sum            'C17 H18 N2 O'
_chemical_formula_weight         266.33
_chemical_name_systematic
(6<i>RS</i>,11<i>RS</i>)-11-Ethyl-6,11-dihydro-5<i>H</i>-dibenzo[<i>b</i>,<i>e</i>]azepine-6-carboxamide
_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   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                86.192(2)
_cell_angle_beta                 81.237(3)
_cell_angle_gamma                87.313(2)
_cell_formula_units_Z            2
_cell_length_a                   5.6051(2)
_cell_length_b                   8.6411(3)
_cell_length_c                   14.3853(6)
_cell_measurement_reflns_used    3148
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      2.838
_cell_volume                     686.61(4)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19423
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.608
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0654
_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^)+(0.0889P)^2^+0.4781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                2352
_reflns_number_total             3144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3628sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020536.cif.'
_cod_database_code               2020536
_cod_database_fobs_code          2020536
_shelx_estimated_absorpt_t_min   0.983
_shelx_estimated_absorpt_t_max   0.988
_shelx_hkl_checksum              72257
_shelx_res_checksum              27460
_shelxl_version_number           2.014