(9<i>S</i>,13<i>R</i>,14<i>S</i>)-7,8-Didehydro-4-(4-iodobenzyloxy)-3,7-dimethoxy-17-methylmorphinan-6-one monohydrate
Zheng, Xing-Liang; Jiang, Ning-Fei; Acta Crystallographica Section E 66 (2010) o2817–; doi:10.1107/S1600536810040286

data_2227170
_publ_section_title
;
 (9<i>S</i>,13<i>R</i>,14<i>S</i>)-7,8-Didehydro-4-(4-iodobenzyloxy)-3,7-dimethoxy-17-methylmorphinan-6-one
 monohydrate
;
_journal_coeditor_code           BH2309
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2817
_journal_paper_doi               10.1107/S1600536810040286
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C26 H28 I N O4, H2 O'
_chemical_formula_moiety         'C26 H28 I N O4, H2 O'
_chemical_formula_sum            'C26 H30 I N O5'
_chemical_formula_weight         563.41
_chemical_melting_point          412
_chemical_name_systematic
;
(9<i>S</i>,13<i>R</i>,14<i>S</i>)-7,8-Didehydro-4-(4-iodobenzyloxy)-3,7-
dimethoxy-17-methylmorphinan-6-one monohydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 91.432(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.9005(8)
_cell_length_b                   14.9221(14)
_cell_length_c                   9.2426(9)
_cell_measurement_reflns_used    4522
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.406
_cell_measurement_theta_min      4.578
_cell_volume                     1227.2(2)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7231
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.233
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.492
_refine_ls_abs_structure_details 'Flack (1983), 2311 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.016(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5047
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                4844
_reflns_number_total             5047
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2309.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2227170
_cod_database_fobs_code          2227170