(3<i>S</i>,4<i>R</i>,4a<i>S</i>,7a<i>R</i>,12b<i>S</i>)-3-Cyclopropylmethyl-4a,9-dihydroxy-3-methyl-7-oxo-2,3,4,4a,5,6,7,7a-octahydro-1<i>H</i>-4,12-methano-1-benzofuro[3,2-<i>e</i>]isoquinolin-3-ium 2,2,2-trifluoroacetate methanol solvate
Cai, Xu; Zhou, Xinbo; Zheng, Zhibing; Zhong, Wu; Li, Song; Acta Crystallographica Section E 66 (2010) o2868–; doi:10.1107/S1600536810041164

data_2227608
_publ_section_title
;
 (3<i>S</i>,4<i>R</i>,4a<i>S</i>,7a<i>R</i>,12b<i>S</i>)-3-Cyclopropylmethyl-4a,9-dihydroxy-3-methyl-7-oxo-2,3,4,4a,5,6,7,7a-octahydro-1<i>H</i>-4,12-methano-1-benzofuro[3,2-<i>e</i>]isoquinolin-3-ium
 2,2,2-trifluoroacetate methanol solvate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2868
_journal_paper_doi               10.1107/S1600536810041164
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C21 H26 N O4 +, C2 F3 O2 - , C H4 O'
_chemical_formula_moiety         'C21 H26 N O4 +, C2 F3 O2 - , C H4 O'
_chemical_formula_sum            'C24 H30 F3 N O7'
_chemical_formula_weight         501.49
_chemical_name_systematic
;
(3<i>S</i>,4<i>R</i>,4a<i>S</i>,7a<i>R</i>,12b<i>S</i>)-3-Cyclopropylmethyl-
4a,9-dihydroxy-3-methyl-7-oxo-2,3,4,4a,5,6,7,7a-octahydro-1<i>H</i>-4,12-
methano-1-benzofuro[3,2-<i>e</i>]isoquinolin-3-ium 2,2,2-trifluoroacetate
methanol solvate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.404(2)
_cell_length_b                   12.526(3)
_cell_length_c                   19.693(5)
_cell_measurement_reflns_used    8884
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.6
_cell_volume                     2319.7(9)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku Saturn CCD area detector'
_diffrn_measurement_method       '\w and \f 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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16033
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.9834
_exptl_absorpt_correction_T_min  0.9764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC, 2005)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         2336
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0510P)^2^+0.2916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0789
_reflns_number_gt                2261
_reflns_number_total             2336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hg2721.cif
_cod_data_source_block           I
_cod_original_cell_volume        2319.8(10)
_cod_database_code               2227608
_cod_database_fobs_code          2227608