Crystal structure of 17-(cyclopropylmethyl)-6,7-didehydro-4,5α- epoxy-3-hydroxy-14β-(3-phenylpropyloxy)indolo[2,3:6,7]morphinan hydroiodide, (C~35~H~37~N~2~O~3~)I
F. Schüllner; G. Laus; K. Wurst; H. Schmidhammer; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 77–78; doi:

data_8101704
_publ_section_title
;
Crystal structure of 17-(cyclopropylmethyl)-6,7-didehydro-4,5\a-
epoxy-3-hydroxy-14\b-(3-phenylpropyloxy)indolo[2,3:6,7]morphinan 
hydroiodide, (C~35~H~37~N~2~O~3~)I
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              77
_journal_page_last               78
_journal_volume                  220
_journal_year                    2005
_chemical_formula_sum            'C35 H37 I N2 O3'
_chemical_formula_weight         660.57
_chemical_name_systematic
; 
17-(cyclopropylmethyl)-6,7-didehydro-4,5\a-epoxy-3-hydroxy-14\b-(3-
phenylpropyloxy)indolo[2,3:6,7]morphinan hydroiodide
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.528(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8202(3)
_cell_length_b                   8.4511(4)
_cell_length_c                   18.0106(7)
_cell_measurement_temperature    233(2)
_cell_volume                     1485.04(10)
_computing_data_collection       'Kappa CCD'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      233(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6805
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    'mixed; refined at N1, N2 and O1'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         3834
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0055P)^2^+2.0405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                3628
_reflns_number_total             3834
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1434.cff
_cod_data_source_block           CCDC251557
_cod_original_sg_symbol_H-M      P12(1)1
_cod_database_code               8101704