Crystallographic investigations of select cathinones: emerging illicit street drugs known as `bath salts'
Wood, Matthew R.; Lalancette, Roger A.; Bernal, Ivan; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229614025637

data_2019760
_publ_section_title
;
 Crystallographic investigations of select cathinones: emerging illicit
 street drugs known as `bath salts'
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614025637
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'H7 O3 +, C16 H22 N O3 +, 2Cl -'
_chemical_formula_moiety         'H7 O3 +, C16 H22 N O3 +, 2(Cl -)'
_chemical_formula_sum            'C16 H29 Cl2 N O6'
_chemical_formula_weight         402.30
_chemical_name_systematic
;
Hydroxonium
1-(benzo[<i>d</i>][1,3]dioxol-5-yl)-2-(pyrrolidin-1-ium-1-yl)pentan-1-one
dichloride
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.4200(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8084(3)
_cell_length_b                   11.4143(2)
_cell_length_c                   11.6289(2)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.80
_cell_measurement_theta_min      2.93
_cell_volume                     2002.10(6)
_computing_cell_refinement
;
APEX2 (Bruker, 2006)
;
_computing_data_collection
;
APEX2 (Bruker, 2006)
;
_computing_data_reduction
;
SAINT (Bruker, 2005)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008<i>b</i>)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008<i>b</i>)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2014)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008<i>b</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART CCD APEXII area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18712
_diffrn_reflns_theta_full        67.700
_diffrn_reflns_theta_max         68.574
_diffrn_reflns_theta_min         2.930
_exptl_absorpt_coefficient_mu    3.184
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.322
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008<i>a</i>)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.529
_refine_diff_density_min         -0.390
_refine_ls_extinction_coef       0.0018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2014)
;
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+3.7517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1512
_reflns_number_gt                3393
_reflns_number_total             3588
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3326sup1.cif
_cod_data_source_block           V
_cod_database_code               2019760
_cod_database_fobs_code          2019760
_shelx_estimated_absorpt_t_min   0.322
_shelx_estimated_absorpt_t_max   0.827
_shelx_hkl_checksum              7941
_shelx_res_checksum              10615