The crystal structure and evidence of the phase transition in d-amphetamine sulfate, as studied by X-ray crystallography, DSC and NMR spectroscopy
Pogorzelec-Glaser, Katarzyna; Kaszyńska, Joanna; Rachocki, Adam; Tritt-Goc, Jadwiga; Piślewski, Narcyz; Pietraszko, Adam; New Journal of Chemistry 33 (2009) 1894–; doi:10.1039/b815325f

data_7053766
_publ_section_title
;
 The crystal structure and evidence of the phase transition in
 d-amphetamine sulfate, as studied by X-ray crystallography, DSC and NMR
 spectroscopy
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1894
_journal_paper_doi               10.1039/b815325f
_journal_volume                  33
_journal_year                    2009
_chemical_absolute_configuration rm
_chemical_formula_moiety         '2(C9 H14 n), O4 S'
_chemical_formula_sum            'C18 H28 N2 O4 S'
_chemical_formula_weight         368.48
_chemical_name_common            'Amphetamine sulphate'
_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                90.000(9)
_cell_angle_beta                 94.370(10)
_cell_angle_gamma                90.000(9)
_cell_formula_units_Z            4
_cell_length_a                   10.6090(12)
_cell_length_b                   6.3820(6)
_cell_length_c                   30.133(4)
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2
_cell_volume                     2034.3(4)
_computing_cell_refinement       'CrysAlis v171.32.18-Oxford Diffraction'
_computing_data_collection       'CrysAlis v171.32.18-Oxford Diffraction'
_computing_data_reduction        'CrysAlis v171.32.18-Oxford Diffraction'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'KM4CCD- Oxford Diffraction'
_diffrn_measurement_method       CCD
_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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            24561
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.9912
_exptl_absorpt_correction_T_min  0.9543
_exptl_absorpt_correction_type   'numerical- CrysAlis v171.32.18'
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         7997
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                6177
_reflns_number_total             7997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815325fsup1.cif
_cod_data_source_block           a120l
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7053766