(9<i>R</i>,13<i>R</i>,14<i>R</i>)-7-(<i>E</i>)-Benzylidene-14-hydroxy-3,4-dimethoxy-17-methylmorphinan-6-one
Parrish, Damon A.; Thatcher, Linn N.; Wu, Hui-Fang; Coop, Andrew; Deschamps, Jeffrey R.; Acta Crystallographica Section E 61 (2005) o2617–o2618; doi:10.1107/S1600536805019987

data_2206380
_publ_section_title
(9<i>R</i>,13<i>R</i>,14<i>R</i>)-7-(<i>E</i>)-Benzylidene-14-hydroxy-3,4-dimethoxy-17-methylmorphinan-6-one
_journal_coeditor_code           CI6602
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2617
_journal_page_last               o2618
_journal_paper_doi               10.1107/S1600536805019987
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C29 H33 N O4'
_chemical_formula_moiety         'C29 H33 N O4'
_chemical_formula_sum            'C29 H33 N O4'
_chemical_formula_weight         459.56
_chemical_name_systematic
(9R,13R,14R)-7-(E)-Benzylidene-14-hydroxy-3,4-dimethoxy-17-methylmorphinan-6-one
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3572(17)
_cell_length_b                   12.6676(11)
_cell_length_c                   15.874(3)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      22.51
_cell_measurement_theta_min      4.47
_cell_volume                     2484.9(6)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Bruker, 1997)'
_computing_data_reduction        'XSCANS and XPREP (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6038
_diffrn_reflns_theta_full        68.95
_diffrn_reflns_theta_max         68.95
_diffrn_reflns_theta_min         4.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         2615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0849P)^2^+0.1730P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1475
_reflns_number_gt                2091
_reflns_number_total             2615
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6602.cif
_cod_data_source_block           4
_cod_database_code               2206380
_cod_database_fobs_code          2206380