(7<i>R</i>,8<i>S</i>,9<i>S</i>,12<i>S</i>)-1-(4-Chlorobenzyloxy)-13,14-didehydro-12-hydroxy-2,13-dimethoxy-<i>N</i>-methylmorphinane
Zheng, Xing-Liang; Jiang, Ning-Fei; Gao, Hong-Sheng; Luo, Dan; Ding, Ai-Shun; Acta Crystallographica Section E 67 (2011) o2480–; doi:10.1107/S160053681103443X

data_2231792
_publ_section_title
;
 (7<i>R</i>,8<i>S</i>,9<i>S</i>,12<i>S</i>)-1-(4-Chlorobenzyloxy)-13,14-didehydro-12-hydroxy-2,13-dimethoxy-<i>N</i>-methylmorphinane
;
_journal_coeditor_code           ZS2138
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2480
_journal_paper_doi               10.1107/S160053681103443X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C26 H30 Cl N O4'
_chemical_formula_moiety         'C26 H30 Cl N O4'
_chemical_formula_sum            'C26 H30 Cl N O4'
_chemical_formula_weight         455.96
_chemical_melting_point          412
_chemical_name_systematic
;
(7<i>R</i>,8<i>S</i>,9<i>S</i>,12<i>S</i>)-
1-(4-Chlorobenzyloxy)-13,14-didehydro-12-hydroxy-
2,13-dimethoxy-<i>N</i>-methylmorphinane
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8073(9)
_cell_length_b                   9.7598(11)
_cell_length_c                   31.043(2)
_cell_measurement_reflns_used    3586
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      48.328
_cell_measurement_theta_min      5.203
_cell_volume                     2365.4(4)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (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      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12129
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5643
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.257
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.200
_refine_ls_abs_structure_details 'Flack, (1983), 1905 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0768P)^2^+0.0462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                3899
_reflns_number_total             4590
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2138.cif
_cod_data_source_block           I
_cod_database_code               2231792
_cod_database_fobs_code          2231792