Crystal structure of octane-1,8-diaminium 4,4'-(diazene-1,2-diyl)dibenzoate monohydrate
Elkin, Igor; Maris, Thierry; Christopherson, Jan-Constantin; Borchers, Tristan H.; Barrett, Christopher J.; Acta Crystallographica Section E 74 (2018) 724–727; doi:10.1107/S2056989018006187

data_2242465
_publ_section_title
;
 Crystal structure of octane-1,8-diaminium
 4,4'-(diazene-1,2-diyl)dibenzoate monohydrate
;
_journal_coeditor_code           HB7747
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              724
_journal_page_last               727
_journal_paper_doi               10.1107/S2056989018006187
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C8 H22 N2 2+, C14 H8 N2 O4 2-, H2 O'
_chemical_formula_moiety         'C8 H22 N2 2+, C14 H8 N2 O4 2-, H2 O'
_chemical_formula_sum            'C22 H32 N4 O5'
_chemical_formula_weight         432.51
_chemical_name_systematic
;
Octane-1,8-diaminium 4,4'-(diazene-1,2-diyl)dibenzoate monohydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                83.0010(10)
_cell_angle_beta                 83.3640(10)
_cell_angle_gamma                73.9730(10)
_cell_formula_units_Z            2
_cell_length_a                   8.36040(10)
_cell_length_b                   11.4100(2)
_cell_length_c                   12.4661(2)
_cell_measurement_reflns_used    3920
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.143
_cell_measurement_theta_min      4.049
_cell_volume                     1130.24(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009) and Mercury (Macrae <i>et
al.</i>,
2008)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009) and <i>publCIF</i>
(Westrip,
2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28413
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.143
_diffrn_reflns_theta_min         4.049
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.5246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       Block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.303
_refine_ls_extinction_coef       0.0427(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0541P)^2^+0.3252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                3920
_reflns_number_total             4048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7747sup1.cif
_cod_data_source_block           I
_cod_database_code               2242465
_cod_database_fobs_code          2242465
_shelx_estimated_absorpt_t_min   0.755
_shelx_estimated_absorpt_t_max   0.929
_shelx_hkl_checksum              29062
_shelx_res_checksum              78122