(8<i>S</i>,9<i>S</i>,10<i>R</i>)-4-(4-Chlorobenzyloxy)-7,8-didehydro-3,7-dimethoxy-17-methylmorphinan-6-one monohydrate
Zheng, Xing-Liang; Chen, Shu-Jun; Jiang, Ning-Fei; Zhan, Sue-Hui; Acta Crystallographica Section E 67 (2011) o1190–; doi:10.1107/S1600536811013973

data_2230060
_publ_section_title
;
 (8<i>S</i>,9<i>S</i>,10<i>R</i>)-4-(4-Chlorobenzyloxy)-7,8-didehydro-3,7-dimethoxy-17-methylmorphinan-6-one
 monohydrate
;
_journal_coeditor_code           KP2320
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1190
_journal_paper_doi               10.1107/S1600536811013973
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C26 H28 Cl N O4, H2 O'
_chemical_formula_moiety         'C26 H28 Cl N O4, H2 O'
_chemical_formula_sum            'C26 H30 Cl N O5'
_chemical_formula_weight         471.96
_chemical_melting_point          383
_chemical_name_systematic
;
(8<i>S</i>,9<i>S</i>,10<i>R</i>)-4-(4-Chlorobenzyloxy)-7,8-didehydro-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                 91.6180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.8866(4)
_cell_length_b                   14.6386(7)
_cell_length_c                   9.1860(4)
_cell_measurement_temperature    296(2)
_cell_volume                     1194.51(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13795
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.9165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.213
_refine_ls_abs_structure_details 'Flack (1983), <b>1991 Friedel pairs</b>'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4185
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0458P)^2^+0.1696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0820
_reflns_number_gt                3974
_reflns_number_total             4185
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2320.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2230060
_cod_database_fobs_code          2230060