Nimustine hydrochloride: the first crystal structure determination of a 2-chloroethyl-<i>N</i>-nitrosourea hydrochloride derivative by X-ray powder diffraction and solid-state NMR
Bekö, Sándor L.; Urmann, David; Lakatos, Andrea; Glaubitz, Clemens; Schmidt, Martin U.; Acta Crystallographica Section C 68 (2012) o144–o148; doi:10.1107/S0108270112005252

data_2018418
_publ_section_title
;
 Nimustine hydrochloride: the first crystal structure determination of a
 2-chloroethyl-<i>N</i>-nitrosourea hydrochloride derivative by X-ray
 powder diffraction and solid-state NMR
;
_journal_coeditor_code           LG3071
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o144
_journal_page_last               o148
_journal_paper_doi               10.1107/S0108270112005252
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C9 H14 Cl N6 O2 + , Cl -'
_chemical_formula_moiety         'C9 H14 Cl N6 O2 +, Cl -'
_chemical_formula_structural     'C9 H14 Cl2 N6 O2'
_chemical_formula_sum            'C9 H14 Cl2 N6 O2'
_chemical_formula_weight         309.16
_chemical_name_common            'Nimustine hydrochloride'
_chemical_name_systematic
;
4-amino-5-({[<i>N</i>-(2-chloroethyl)-<i>N</i>-nitrosocarbamoyl]amino}methyl)-
2-methylpyrimidin-1-ium chloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 93.2353(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.25191(12)
_cell_length_b                   12.2401(3)
_cell_length_c                   21.4088(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1374.05(6)
_computing_cell_refinement       'TOPAS Academic (Coelho, 2007)'
_computing_data_collection       'WINXPOW (Stoe & Cie, 2004)'
_computing_data_reduction        'DASH (David <i>et al.</i>, 2006)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'TOPAS Academic (Coelho, 2007)'
_computing_structure_solution    'DASH (David <i>et al.</i>, 2006)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type
'Stoe STADI-P with a linear position-sensitive detector'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  'primary focusing, Ge 111'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_number            853
_exptl_absorpt_coefficient_mu    4.350
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       powder
_exptl_crystal_F_000             640.0
_pd_char_colour                  white
_pd_char_particle_morphology     tablet
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        79.99
_pd_proc_2theta_range_min        2.0
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function
;
Bayesian high-pass filter with 20 terms
;
_pd_proc_ls_profile_function
;
modified Thompson--Cox--Hastings pseudo-Voigt
[Young, R. A. (1993). <i>The Rietveld Method</i>, pp. 115--118. New
York: Oxford University Press Inc.]
;
_pd_proc_ls_prof_R_factor        0.08648
_pd_proc_ls_prof_wR_expected     0.06068
_pd_proc_ls_prof_wR_factor       0.08421
_pd_proc_number_of_points        7600
_pd_spec_mounting                '0.7mm glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              10
_pd_spec_size_equat              0.7
_pd_spec_size_thick              0.7
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.1781
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     86
_refine_ls_number_restraints     42
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_details     'w = 1/\s[Y~obs~]^2^'
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            lg3071.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018418
_cod_database_fobs_code          2018418