Diels–Alder Products of the Alkaloid ({-})-Thebaine with α-Chloroacrylnitrile and 1-Methoxy-1,3-cyclohexadiene with Tetracyanoethene
Schollmeyer, D.; Keilhofer, D.; Pindur, U.; Acta Crystallographica Section C 51 (1995) 502–505; doi:10.1107/S0108270194007900

data_2003296
_publ_section_title
;
 Diels--Alder Products of the Alkaloid ({-})-Thebaine with
 \a-Chloroacrylnitrile and 1-Methoxy-1,3-cyclohexadiene with
 Tetracyanoethene
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              502
_journal_page_last               505
_journal_paper_doi               10.1107/S0108270194007900
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
;
  diffusion of petroleum ether into a solution of (1) in ethyl acetate
;
_chemical_formula_sum            'C22 H23 Cl N2 O3'
_chemical_formula_weight         398.87
_chemical_name_systematic
;
(5R,6S,7R,9R,13S,14R)-7-Chloro-7-cyano-4,5-epoxy-3,6-dimethoxy-N-methyl-
6,14-ethenoisomorphinane
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_method           SHELXL93
_cell_angle_alpha                95.703(1)
_cell_angle_beta                 106.774(1)
_cell_angle_gamma                92.499(2)
_cell_formula_units_Z            1
_cell_length_a                   6.7639(2)
_cell_length_b                   8.0105(1)
_cell_length_c                   9.3111(1)
_cell_measurement_reflns_used    75
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      65
_cell_volume                     479.254(17)
_computing_cell_refinement       'CELSIUS (Reference, 19??)'
_computing_data_collection       'Enraf-Nonius CAD-4 Software'
_computing_data_reduction        'CORINC (Reference, 19??)'
_computing_molecular_graphics    'SCHAKAL92 (Keller, 1992)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0075
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3803
_diffrn_reflns_theta_max         69.85
_diffrn_reflns_theta_min         5.00
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       prism
_exptl_crystal_F_000             210
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.323
_refine_ls_abs_structure_details '\c = 0.03(2) (Flack, 1983)'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_coef       0.0217(28)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.126
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3569
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.125
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_obs          0.0475
_refine_ls_shift/esd_max         0.020
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(Fo^2^) + (0.0909P)^2^ + 0.1397P]
  where P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1362
_refine_ls_wR_factor_obs         0.1360
_reflns_number_observed          3558
_reflns_number_total             3569
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            se1061.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        479.25(2)
_cod_database_code               2003296