(7<i>R</i>,8<i>S</i>,9<i>S</i>,12<i>S</i>)-1-Benzyloxy-13,14-didehydro-12-hydroxy-2,13-dimethoxy-<i>N</i>-methylmorphinane
Zheng, Xing-Liang; Jiang, Ning-Fei; Luo, Dan; Gao, Hong-Sheng; Ding, Ai-Shun; Acta Crystallographica Section E 67 (2011) o2662–o2663; doi:10.1107/S1600536811037226

data_2231842
_publ_section_title
;
 (7<i>R</i>,8<i>S</i>,9<i>S</i>,12<i>S</i>)-1-Benzyloxy-13,14-didehydro-12-hydroxy-2,13-dimethoxy-<i>N</i>-methylmorphinane
;
_journal_coeditor_code           BX2370
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2662
_journal_page_last               o2663
_journal_paper_doi               10.1107/S1600536811037226
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C26 H31 N O4'
_chemical_formula_moiety         'C26 H31 N O4'
_chemical_formula_sum            'C26 H31 N O4'
_chemical_formula_weight         421.52
_chemical_name_systematic
;
(7<i>R</i>,8<i>S</i>,9<i>S</i>,12<i>S</i>)-1-Benzyloxy-13,14-
didehydro-12-hydroxy-2,13-dimethoxy-<i>N</i>-methylmorphinane
;
_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
_cell_angle_alpha                79.9710(10)
_cell_angle_beta                 67.6630(10)
_cell_angle_gamma                64.6050(10)
_cell_formula_units_Z            1
_cell_length_a                   7.7191(2)
_cell_length_b                   8.5100(2)
_cell_length_c                   9.9630(2)
_cell_measurement_reflns_used    9563
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      67.72
_cell_measurement_theta_min      4.80
_cell_volume                     546.81(2)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'APEX2 (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9789
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.00
_diffrn_reflns_theta_min         4.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.8983
_exptl_absorpt_correction_T_min  0.8639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             226
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.205
_refine_ls_abs_structure_details 'Flack (1983), <b>1075 Friedel pairs</b>'
_refine_ls_abs_structure_Flack   -0.09(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         2925
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0495P)^2^+0.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                2918
_reflns_number_total             2925
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bx2370.cif
_cod_data_source_block           I
_cod_database_code               2231842
_cod_database_fobs_code          2231842