Structures of the hydrate and dihydrate forms of the DNA-binding radioprotector methylproamine
White, Jonathan Michael; Brydon, Samuel Charles; Fellowes, Thomas; Acta Crystallographica Section E 74 (2018) 1903–1907; doi:10.1107/S2056989018016791

data_2242768
_publ_section_title
;
 Structures of the hydrate and dihydrate forms of the DNA-binding
 radioprotector methylproamine
;
_journal_coeditor_code           SJ5567
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1903
_journal_page_last               1907
_journal_paper_doi               10.1107/S2056989018016791
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C28 H31 N7, 2H2 O1'
_chemical_formula_moiety         'C28 H31 N7, 2(H2 O1)'
_chemical_formula_sum            'C28 H35 N7 O2'
_chemical_formula_weight         501.63
_chemical_name_systematic
;<i>N</i>,<i>N</i>,3-Trimethyl-4-[6-(4-methylpiperazin-1-yl)-1<i>H</i>,3'<i>H</i>-[2,5'-bibenzo[<i>d</i>]imidazol]-2'-yl]aniline
dihydrate
;
_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
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.806(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7190(3)
_cell_length_b                   12.0891(3)
_cell_length_c                   24.6794(7)
_cell_measurement_reflns_used    4889
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      75.0040
_cell_measurement_theta_min      3.5560
_cell_volume                     2601.07(13)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
Crystalmaker (Palmer 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15892
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.755
_diffrn_reflns_theta_min         3.582
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2015)
;
_exptl_crystal_colour            BROWN
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.7255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                4425
_reflns_number_total             5318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sj5567sup1.cif
_cod_data_source_block           1_dihydrate
_cod_database_code               2242768
_cod_database_fobs_code          2242768
_shelx_hkl_checksum              80895
_shelx_res_checksum              45899