(9<i>S</i>,13<i>R</i>,14<i>S</i>)-7,8-Didehydro-4-(4-fluorobenzyloxy)-3,7-dimethoxy-17-methylmorphinan-6-one sesquihydrate
Zheng, Xing-Liang; Jiang, Ning-Fei; Luo, Dan; Gao, Hong-Sheng; Ding, Ai-Shun; Acta Crystallographica Section E 67 (2011) o1988–; doi:10.1107/S1600536811026183

data_2230995
_publ_section_title
;
 (9<i>S</i>,13<i>R</i>,14<i>S</i>)-7,8-Didehydro-4-(4-fluorobenzyloxy)-3,7-dimethoxy-17-methylmorphinan-6-one
 sesquihydrate
;
_journal_coeditor_code           BH2361
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1988
_journal_paper_doi               10.1107/S1600536811026183
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C26 H28 F N O4, 1.5H2 O'
_chemical_formula_moiety         'C26 H28 F N O4, 1.5(H2 O)'
_chemical_formula_sum            'C26 H31 F N O5.5'
_chemical_formula_weight         464.52
_chemical_name_systematic
;
(9<i>S</i>,13<i>R</i>,14<i>S</i>)-7,8-Didehydro-4-(4-fluorobenzyloxy)-3,7-
dimethoxy-17-methylmorphinan-6-one sesquihydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.3240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0155(3)
_cell_length_b                   7.67760(10)
_cell_length_c                   18.1506(4)
_cell_measurement_reflns_used    6582
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      64.74
_cell_measurement_theta_min      2.58
_cell_volume                     2369.08(7)
_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 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7232
_diffrn_reflns_theta_full        64.96
_diffrn_reflns_theta_max         64.96
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_T_max  0.9248
_exptl_absorpt_correction_T_min  0.8263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.176
_refine_ls_abs_structure_details 'Flack (1983), 1359 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     312
_refine_ls_number_reflns         3415
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0555P)^2^+0.6114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0809
_reflns_number_gt                3402
_reflns_number_total             3415
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2361.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C26 H31 F N O5.50'
_cod_database_code               2230995
_cod_database_fobs_code          2230995