Amitriptylinium picrate: conformational disorder
Bindya, S.; Wong, Wing-Tak; Ashok, M. A.; Yathirajan, H. S.; Rathore, R. S.; Acta Crystallographica Section C 63 (2007) o546–o548; doi:10.1107/S0108270107037468

data_2016136
_publ_section_title
;
 Amitriptylinium picrate: conformational disorder
;
_journal_coeditor_code           FA3097
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o546
_journal_page_last               o548
_journal_paper_doi               10.1107/S0108270107037468
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C20 H24 N + , C6 H2 N3 O7 -'
_chemical_formula_moiety         'C20 H24 N + , C6 H2 N3 O7 -'
_chemical_formula_sum            'C26 H26 N4 O7'
_chemical_formula_weight         506.51
_chemical_melting_point          393
_chemical_name_common
;
Amitriptylinium picrate
;
_chemical_name_systematic
;
3-(10,11-dihydro-5H-dibenzo[a,d][7]annulen-5-ylidene)-N,N-dimethylpropan-1-
aminium 2,4,6-trinitrophenolate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                73.357(2)
_cell_angle_beta                 79.305(3)
_cell_angle_gamma                85.411(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0649(11)
_cell_length_b                   11.0187(12)
_cell_length_c                   12.0352(13)
_cell_measurement_reflns_used    8561
_cell_measurement_temperature    301.0(10)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      1.9
_cell_volume                     1256.1(2)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      301.0(10)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7632
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4802
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0969P)^2^+0.2066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                3598
_reflns_number_total             4802
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3097.cif
_cod_data_source_block           I
_cod_database_code               2016136
_cod_database_fobs_code          2016136