14-Benzoylmesaconine hydrochloride methanol monosolvate
Mu, Yan; Li, Lin; Wei, Hai-Liu; Kuang, Tong-Chun; Hu, Song-Qing; Acta Crystallographica Section E 67 (2011) o974–o975; doi:10.1107/S1600536811010300

data_2229892
_publ_section_title
;
 14-Benzoylmesaconine hydrochloride methanol monosolvate
;
_journal_coeditor_code           ZL2352
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o974
_journal_page_last               o975
_journal_paper_doi               10.1107/S1600536811010300
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C31 H44 N O10 +, Cl -, C H4 O'
_chemical_formula_moiety         'C31 H44 N O10 +, Cl -, C H4 O'
_chemical_formula_sum            'C32 H48 Cl N O11'
_chemical_formula_weight         658.16
_chemical_name_common
;
14-Benzoylmesaconine hydrochloride methanol monosolvate
;
_chemical_name_systematic
;
8-benzoyloxy-4,9,11,11a-tetrahydroxy-6,10,13-trimethoxy-3-methoxymethyl-
1-methyltetradecahydro-1<i>H</i>-3,6a,12-(epiethane-1,1,2-triyl)-7,9-
methanonaphtho[2,3-<i>b</i>]azocin-1-ium chloride
methanol monosolvate
;
_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                   12.919(3)
_cell_length_b                   15.748(3)
_cell_length_c                   16.045(3)
_cell_measurement_reflns_used    5837
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      2.82
_cell_volume                     3264.3(12)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0464
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29100
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         2.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.503
_refine_ls_abs_structure_details 'Flack (1983), 1726 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.01(11)
_refine_ls_extinction_coef       0.0187(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+3.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                4585
_reflns_number_total             6908
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2352.cif
_cod_data_source_block           I
_cod_original_cell_volume        3264.2(11)
_cod_database_code               2229892
_cod_database_fobs_code          2229892