Monoclinic form I of clopidogrel hydrogen sulfate from powder diffraction data
Chernyshev, Vladimir V.; Pirogov, Sergey V.; Shishkina, Irina N.; Velikodny, Yurii A.; Acta Crystallographica Section E 66 (2010) o2101–o2102; doi:10.1107/S1600536810028783

data_2226995
_publ_section_title
;
 Monoclinic form I of clopidogrel hydrogen sulfate from powder
 diffraction data
;
_journal_coeditor_code           LH5082
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2101
_journal_page_last               o2102
_journal_paper_doi               10.1107/S1600536810028783
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C16 H17 Cl N O2 S +, H S O4 -'
_chemical_formula_moiety         'C16 H17 Cl N O2 S +, H S O4 -'
_chemical_formula_sum            'C16 H18 Cl N O6 S2'
_chemical_formula_weight         419.89
_chemical_melting_point          455(3)
_chemical_name_common
;
Clopidogrel hydrogen sulfate
;
_chemical_name_systematic
;
(+)-(S)-5-[(2-chlorophenyl)(methoxycarbonyl)methyl]-4,5,6,7-
tetrahydrothieno[3,2-<i>c</i>]pyridin-5-ium hydrogen sulfate]
;
_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'
_audit_creation_method           'manual + SHELXL-97'
_cell_angle_alpha                90.00
_cell_angle_beta                 113.28(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4315(12)
_cell_length_b                   15.3345(18)
_cell_length_c                   12.6320(16)
_cell_measurement_reflns_used    1583
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      44.98
_cell_measurement_theta_min      3.82
_cell_volume                     1856.1(5)
_computing_cell_refinement       'MRIA (Zlokazov & Chernyshev, 1992)'
_computing_data_collection
'<i>G670 Imaging Plate Guinier Camera Software</i> (Huber, 2002)'
_computing_data_reduction
'<i>G670 Imaging Plate Guinier Camera Software</i> (Huber, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
'MRIA (Zlokazov & Chernyshev, 1992) and SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'MRIA (Zlokazov & Chernyshev, 1992)'
_computing_structure_solution
'simulated annealing (Zhukov <i>et al.</i>, 2001)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Guinier camera G670'
_diffrn_radiation_monochromator  'Curved Germanium (111)'
_diffrn_radiation_source         'line-focus sealed tube'
_diffrn_radiation_type           CuK\a~1~
_diffrn_radiation_wavelength     1.54059
_exptl_absorpt_coefficient_mu    4.230
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_pd_block_diffractogram_id       Form_I_pattern
_pd_char_colour                  white
_pd_char_particle_morphology     plate
_pd_instr_location
;
Dept. of Chemistry, Moscow State University, 119991 Moscow, Russian Federation
;
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        90.00
_pd_meas_2theta_range_min        4.00
_pd_meas_number_of_points        8601
_pd_meas_scan_method             cont
_pd_prep_pressure                101
_pd_prep_temperature             295(2)
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        90.00
_pd_proc_2theta_range_min        4.00
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_prof_R_factor        0.0193
_pd_proc_ls_prof_wR_expected     0.0145
_pd_proc_ls_prof_wR_factor       0.0250
_pd_proc_wavelength              1.54059
_pd_spec_mounting
;
thin layer in the specimen holder of the camera
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              15
_pd_spec_size_equat              1
_pd_spec_size_thick              1
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.7268
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    42
_refine_ls_number_parameters     205
_refine_ls_number_restraints     155
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            lh5082.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2226995