Crystal structure of anagyrine perchlorate
Turgunov, Kambarali K.; Rakhimov, Shukhrat B.; Vinogradova, Valentina I.; Tashkhodjaev, Bakhodir; Acta Crystallographica Section E 71 (2015) o343–o344; doi:10.1107/S2056989015007781

data_2240591
_publ_section_title
;
 Crystal structure of anagyrine perchlorate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o343
_journal_page_last               o344
_journal_paper_doi               10.1107/S2056989015007781
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C15 H21 N2 O +, Cl O4 -'
_chemical_formula_moiety         'C15 H21 N2 O +, Cl O4 -'
_chemical_formula_sum            'C15 H21 Cl N2 O5'
_chemical_formula_weight         344.79
_chemical_melting_point          588(2)
_chemical_name_systematic
;
Anagyrine perchlorate
;
_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                 90.709(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.3550(3)
_cell_length_b                   32.9820(10)
_cell_length_c                   12.8849(4)
_cell_measurement_reflns_used    6414
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      74.96
_cell_measurement_theta_min      3.67
_cell_volume                     3125.41(19)
_computing_cell_refinement
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis PRO (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53652
_diffrn_reflns_theta_full        77.51
_diffrn_reflns_theta_max         77.50
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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(CrysAlis PRO; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.369
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3107 quotients
  [(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.024(12)
_refine_ls_extinction_coef       0.00064(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     846
_refine_ls_number_reflns         12780
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.7864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1892
_reflns_number_gt                9677
_reflns_number_total             12780
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7409sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2240591
_cod_database_fobs_code          2240591