Crystal structures of five new substituted tetrahydro-1-benzazepines with potential antiparasitic activity
Macías, Mario A.; Acosta, Lina M.; Sanabria, Carlos M.; Palma, Alirio; Roussel, Pascal; Gauthier, Gilles H.; Suescun, Leopoldo; Acta Crystallographica Section C 72 (2016) 363–372; doi:10.1107/S2053229616004885

data_2020478
_publ_section_title
;
 Crystal structures of five new substituted tetrahydro-1-benzazepines with
 potential antiparasitic activity
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              363
_journal_page_last               372
_journal_paper_doi               10.1107/S2053229616004885
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C15 H20 F N O'
_chemical_formula_moiety         'C15 H20 F N O'
_chemical_formula_sum            'C15 H20 F N O'
_chemical_formula_weight         249.32
_chemical_name_systematic
7-Fluoro-<i>cis</i>-2-[(<i>E</i>)-pent-1-enyl]-2,3,4,5-tetrahydro-1<i>H</i>-1-benzazepin-4-ol
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            72
_cell_length_a                   49.395(2)
_cell_length_b                   49.395(2)
_cell_length_c                   11.1802(5)
_cell_measurement_reflns_used    9791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.422
_cell_measurement_theta_min      2.857
_cell_volume                     23623.6(17)
_computing_cell_refinement
;
SAINT (Bruker, 2006)
;
_computing_data_collection
;
APEX2 (Bruker, 2006)
;
_computing_data_reduction
;
SAINT (Bruker, 2006)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII'
_diffrn_measurement_method       '\p and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       64
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            124259
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         1.428
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2006)
;
_exptl_crystal_colour            less
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             9648
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.279
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         12035
_refine_ls_number_restraints     459
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+28.8932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                8771
_reflns_number_total             12035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wq3111sup1.cif
_cod_data_source_block           Compound_5b
_cod_depositor_comments
'Adding full bibliography for 2020473--2020478.cif.'
_cod_original_cell_volume        23623(2)
_cod_database_code               2020478
_cod_database_fobs_code          2020478
_shelx_hkl_checksum              1
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