pH-induced conformational changes in histamine in the solid state
Kodchakorn, Kanchanok; Nimmanpipug, Piyarat; Phongtamrug, Suttinun; Tashiro, Kohji; RSC Advances 9 (2019) 19375–; doi:10.1039/C9RA03418H

data_7232929
_publ_section_title
;
 pH-induced conformational changes in histamine in the solid state
;
_journal_issue                   34
_journal_name_full               'RSC Advances'
_journal_page_first              19375
_journal_paper_doi               10.1039/C9RA03418H
_journal_volume                  9
_journal_year                    2019
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C5 H13 Cl2 N3 O2'
_chemical_formula_sum            'C5 H13 Cl2 N3 O2'
_chemical_formula_weight         218.08
_chemical_name_systematic        'Histamine dication form'
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.45(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   4.449(6)
_cell_length_b                   12.694(16)
_cell_length_c                   7.577(9)
_cell_measurement_reflns_used    386
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.13
_cell_volume                     427.8(9)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4129
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.132
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       dication
_exptl_crystal_F_000             228.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.290
_refine_diff_density_min         -1.320
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  926 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.67(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1325
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    11342.3000    15975.1000    5431.7200
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                1325
_reflns_number_total             1948
_reflns_threshold_expression     F^2^>4.0\s(F^2^)
_cod_data_source_file            c9ra03418h2.cif
_cod_data_source_block           histamine-A0-HCl-needle
_cod_original_cell_volume        427.7(9)
_cod_database_code               7232929