7β,14β-Epoxyhydrocodone-6,6-dimethoxy ketal: an unusual oxetane-containing opioid
Deschamps, Jeffrey R.; Coop, Andrew; Parrish, Damon A.; Rice, Kenner C.; Acta Crystallographica Section E 60 (2004) o331–o333; doi:10.1107/S1600536804002077

data_2203342
_publ_section_title
;
 7\b,14\b-Epoxyhydrocodone-6,6-dimethoxy ketal: an unusual
 oxetane-containing opioid
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o331
_journal_page_last               o333
_journal_paper_doi               10.1107/S1600536804002077
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C20 H25 N O5'
_chemical_formula_moiety         'C20 H25 N O5'
_chemical_formula_sum            'C20 H25 N O5'
_chemical_formula_weight         359.41
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                83.776(6)
_cell_angle_beta                 68.993(5)
_cell_angle_gamma                71.511(5)
_cell_formula_units_Z            1
_cell_length_a                   7.509(2)
_cell_length_b                   7.777(2)
_cell_length_c                   8.430(2)
_cell_measurement_reflns_used    3226
_cell_measurement_temperature    103.0(10)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.59
_cell_volume                     435.84(19)
_computing_cell_refinement       'SMART and SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      103.0(10)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device       'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0098
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3770
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0.7
_diffrn_standards_interval_time  variable
_diffrn_standards_number         450
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         2063
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0566P)^2^+0.0944P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                2036
_reflns_number_total             2063
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6213.cif
_cod_data_source_block           4
_cod_original_cell_volume        435.81(19)
_cod_database_code               2203342