(+)-<i>N</i>-Trichloroacetyl-7,8-dimethoxy-1-vinyl-2,3,4,5-tetrahydro-1<i>H</i>-3-benzazepine at 153 K
Pohl, Ehmke; Herbst-Irmer, Regine; Schimpf, Ralph; Tietze, Lutz F.; Acta Crystallographica Section C 50 (1994) 1978–1980; doi:10.1107/S010827019400538X

data_2010346
_publ_section_title
;(+)-<i>N</i>-Trichloroacetyl-7,8-dimethoxy-1-vinyl-2,3,4,5-tetrahydro-1<i>H</i>-3-benzazepine
 at 153 K
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1978
_journal_page_last               1980
_journal_paper_doi               10.1107/S010827019400538X
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C16 H18 Cl3 N O3'
_chemical_formula_weight         378.66
_chemical_name_systematic
(S)-N-trichloroacetyl-7,8-dimethoxy-1-vinyl-2,3,4,5-tetrahydro-1H-3-benzazepine
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.38(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.717(6)
_cell_length_b                   7.371(11)
_cell_length_c                   14.901(18)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     845.1(18)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick 1991)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Stoe-Siemens four-circle diffractometer'
_diffrn_measurement_method       'Profile data from 2\q/\w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2308
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Plates
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       Colorless
_exptl_crystal_F_000             392
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         .256
_refine_diff_density_min         -.359
_refine_ls_abs_structure_details 'Flack (1983), \c =0.04(6)'
_refine_ls_abs_structure_Flack   0.04(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.079
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2123
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_restrained_S_obs      1.079
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_obs          0.0328
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w=1/[s^2^(Fo^2^)+(0.0667P)^2^ +0.1913P] where P =
  (Fo^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0858
_refine_ls_wR_factor_obs         0.0841
_reflns_number_observed          2096
_reflns_number_total             2125
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sh1101.cif
_cod_data_source_block           ralph
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2010346