Trimipraminium maleate
Jasinski, Jerry P.; Butcher, Ray J.; Hakim Al-Arique, Q. N. M.; Yathirajan, H. S.; Narayana, B.; Acta Crystallographica Section E 66 (2010) o366–o367; doi:10.1107/S1600536810000280

data_2225069
_publ_section_title
;
 Trimipraminium maleate
;
_journal_coeditor_code           NG2715
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o366
_journal_page_last               o367
_journal_paper_doi               10.1107/S1600536810000280
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C20 H27 N2 +, C4 H3 O4 -'
_chemical_formula_moiety         'C20 H27 N2 +, C4 H3 O4 -'
_chemical_formula_sum            'C24 H30 N2 O4'
_chemical_formula_weight         410.50
_chemical_name_systematic
;
3-(10,11-dihydro-5<i>H</i>-dibenzo[<i>b</i>,<i>f</i>]azepin-5-yl)-
<i>N</i>,<i>N</i>,2-trimethylpropan-1-aminium hydrogen maleate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.4356(4)
_cell_length_b                   11.0542(4)
_cell_length_c                   40.4107(13)
_cell_measurement_reflns_used    11412
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      74.1919
_cell_measurement_theta_min      3.9870
_cell_volume                     8682.0(5)
_computing_cell_refinement
'<i>CrysAlis Pro</i> (Oxford Diffraction, 2007)'
_computing_data_collection
'<i>CrysAlis Pro</i> (Oxford Diffraction, 2007)'
_computing_data_reduction
'<i>CrysAlis Pro</i> (Oxford Diffraction, 2007)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer with a Ruby (Gemini Cu) detector
;
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            27150
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         74.32
_diffrn_reflns_theta_min         4.15
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.200
_refine_ls_abs_structure_details 'Flack (1983), 8810 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.14(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         13174
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0612P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                11E3(8)
_reflns_number_total             13E3(9)
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2715.cif
_cod_data_source_block           I
_cod_database_code               2225069
_cod_database_fobs_code          2225069