11-[3-(Dimethylamino)propyl]-6,11-dihydrodibenzo[<i>b</i>,<i>e</i>]thiepin-11-ol
Jasinski, Jerry P.; Butcher, Ray J.; Hakim Al-arique, Q. N. M.; Yathirajan, H. S.; Ramesha, A.R.; Acta Crystallographica Section E 66 (2010) o161–o162; doi:10.1107/S1600536809053434

data_2224702
_publ_section_title
11-[3-(Dimethylamino)propyl]-6,11-dihydrodibenzo[<i>b</i>,<i>e</i>]thiepin-11-ol
_journal_coeditor_code           LH2968
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o161
_journal_page_last               o162
_journal_paper_doi               10.1107/S1600536809053434
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C19 H23 N O S'
_chemical_formula_moiety         'C19 H23 N O S'
_chemical_formula_sum            'C19 H23 N O S'
_chemical_formula_weight         313.44
_chemical_name_systematic
;
11-[3-(Dimethylamino)propyl]-6,11-dihydrodibenzo[<i>b</i>,<i>e</i>]thiepin-
11-ol
;
_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                 95.401(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.7215(4)
_cell_length_b                   15.3729(10)
_cell_length_c                   27.9274(16)
_cell_measurement_reflns_used    6805
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      73.9681
_cell_measurement_theta_min      4.2752
_cell_volume                     3300.3(3)
_computing_cell_refinement
'<i>CrysAlis RED</i> (Oxford Diffraction, 2007)'
_computing_data_collection
'<i>CrysAlis Pro</i> (Oxford Diffraction, 2007)'
_computing_data_reduction
'<i>CrysAlis RED</i> (Oxford Diffraction, 2007)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer with a Ruby (Gemini Cu) detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14666
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.18
_diffrn_reflns_theta_min         4.29
_diffrn_standards_decay_%        <2%
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.738
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.557
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1079P)^2^+0.6589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                5490
_reflns_number_total             6565
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2968.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2224702
_cod_database_fobs_code          2224702