Application of Solid-State 35Cl NMR to the Structural Characterization of Hydrochloride Pharmaceuticals and their Polymorphs
Hiyam Hamaed; Jenna M. Pawlowski; Benjamin F.T. Cooper; Riqiang Fu; S. Holger Eichhorn; Robert W. Schurko; Journal of the American Chemical Society 130 (2008) 11056–11065; doi:10.1021/ja802486q

data_4108196
_publ_section_title
;
 Application of Solid-State 35Cl NMR to the Structural Characterization of
 Hydrochloride Pharmaceuticals and their Polymorphs
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11056
_journal_page_last               11065
_journal_paper_doi               10.1021/ja802486q
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C14 H25 Cl N2 O2'
_chemical_formula_weight         288.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.414(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.391(2)
_cell_length_b                   7.0150(17)
_cell_length_c                   26.163(6)
_cell_measurement_temperature    173(2)
_cell_volume                     1539.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.1231
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15806
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.249
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_F_000             624
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.457
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.457
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.1396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+11.5989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2690
_refine_ls_wR_factor_ref         0.2812
_reflns_number_gt                2104
_reflns_number_total             3503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja802486q-file001_LidocaineHCl2007.cif
_cod_data_source_block           bfclidx
_cod_original_cell_volume        1539.5(6)
_cod_database_code               4108196