Different cationic forms of (‒)-cytisine in the crystal structures of its simple inorganic salts
Owczarzak, Agata; Przybył, Anna K.; Kubicki, Maciej; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618012585

data_2021287
_publ_section_title
;
 Different cationic forms of (--)-cytisine in the crystal structures of
 its simple inorganic salts
;
_journal_coeditor_code           YF3149
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618012585
_journal_volume                  74
_journal_year                    2018
_chemical_absolute_configuration rmad
_chemical_formula_iupac          'C22 H31 N4 O2 3+, 3Br -'
_chemical_formula_moiety         'C22 H31 N4 O2 3+, 3(Br -)'
_chemical_formula_sum            'C22 H31 Br3 N4 O2'
_chemical_formula_weight         623.24
_chemical_name_common
;
Hydrogen dicytisinium tribromide
;
_chemical_name_systematic
;
Hydrogen bis(6-oxo-7,11-diazatricyclo[7.3.1.0^2,7^]trideca-2,4-dien-11-ium)
tribromide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_alpha                90
_cell_angle_beta                 97.4435(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.78898(14)
_cell_length_b                   7.84934(11)
_cell_length_c                   14.37986(17)
_cell_measurement_reflns_used    4853
_cell_measurement_temperature    130.0(10)
_cell_measurement_theta_max      75.1320
_cell_measurement_theta_min      3.0970
_cell_volume                     1207.52(3)
_computing_cell_refinement
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
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;
CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      130.0(10)
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_diffrn_measurement_device       'four-circle diffractometer'
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'Rigaku OD SuperNova Dual source diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5286
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         75.444
_diffrn_reflns_theta_min         3.099
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    6.410
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39142
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_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            'pale red'
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.501
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1235 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.007(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3843
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.5197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                3835
_reflns_number_total             3843
_reflns_threshold_expression     'I > 2\s(I)'
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