7,8-Didehydro-4,5-epoxy-17-methylmorphinan-6-yl naphthalene-1-carboxylate
Gathergood, Nicholas; Scammells, Peter J.; Fallon, Gary D.; 7,8-didehydro-4,5-epoxy-17-methylmorphinan-6-(naphthalene-1-carboxylate); Acta Crystallographica Section E 59 (2003) o1918–o1919; doi:10.1107/S1600536803025121

data_2202727
_publ_section_title
;
 7,8-Didehydro-4,5-epoxy-17-methylmorphinan-6-yl
 naphthalene-1-carboxylate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1918
_journal_page_last               o1919
_journal_paper_doi               10.1107/S1600536803025121
_journal_volume                  59
_journal_year                    2003
_chemical_formula_moiety         'C28 H25 N1 O4'
_chemical_formula_sum            'C28 H25 N O4'
_chemical_formula_weight         439.49
_chemical_melting_point          .443E-305
_chemical_name_common            'morphine 3-(1-naphthoate)'
_chemical_name_systematic
7,8-didehydro-4,5-epoxy-17-methylmorphinan-6-(naphthalene-1-carboxylate)
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 111.9000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7421(2)
_cell_length_b                   7.19080(10)
_cell_length_c                   12.9536(3)
_cell_measurement_reflns_used    14873
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.8
_cell_volume                     1101.24(4)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14873
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         2909
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.1452P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                2423
_reflns_number_total             2909
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6134.cif
_cod_data_source_block           I
_cod_original_cell_volume        1101.23(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C28 H25 N1 O4'
_cod_database_code               2202727
_cod_database_fobs_code          2202727