Hydrogen-bonding motifs and thermotropic polymorphism in redetermined halide salts of hexamethylenediamine
Blerk, Charmaine van; Kruger, Gert J.; Acta Crystallographica Section C 64 (2008) o537–o542; doi:10.1107/S0108270108022919

data_2016791
_publ_section_title
;
 Hydrogen-bonding motifs and thermotropic polymorphism in redetermined
 halide salts of hexamethylenediamine
;
_journal_coeditor_code           BM3056
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o537
_journal_page_last               o542
_journal_paper_doi               10.1107/S0108270108022919
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C6 H18 N2 2+ , 2I -'
_chemical_formula_moiety         'C6 H18 N2 2+ , 2(I -)'
_chemical_formula_sum            'C6 H18 I2 N2'
_chemical_formula_weight         372.02
_chemical_name_common            'Hexamethylenediammonium bishydroiodide'
_chemical_name_systematic
;
Hexane-1,6-diammonium diiodide
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.423(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.88840(10)
_cell_length_b                   12.8756(4)
_cell_length_c                   9.7488(3)
_cell_measurement_reflns_used    4034
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.62
_cell_volume                     613.58(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'SMART-NT (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
;
X-SEED (Barbour, 2001) and Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
PLATON (Spek, 2003) and publCIF (Westrip, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5135
_diffrn_reflns_theta_full        28.45
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         2.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.078
_exptl_absorpt_correction_T_max  0.4617
_exptl_absorpt_correction_T_min  0.1942
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(XPREP; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.244
_refine_diff_density_min         -0.513
_refine_ls_extinction_coef       0.197(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.6405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0595
_reflns_number_gt                1452
_reflns_number_total             1551
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm3056.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016791
_cod_database_fobs_code          2016791