HBr or not HBr? That is the question: crystal structure of 6-hydroxy-1,4-diazepane-1,4-diium dibromide redetermined
Piontek, Mateusz; Morgenstern, Bernd; Steinbrück, Nils; Oberhausen, Bastian; Kickelbick, Guido; Hegetschweiler, Kaspar; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619005321

data_2021624
_publ_section_title
;
 HBr or not HBr? That is the question: crystal structure of
 6-hydroxy-1,4-diazepane-1,4-diium dibromide redetermined
;
_journal_coeditor_code           KU3242
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619005321
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C5 H14 N2 O 2+, 2Br -'
_chemical_formula_moiety         'C5 H14 N2 O 2+, 2(Br -)'
_chemical_formula_sum            'C5 H14 Br2 N2 O'
_chemical_formula_weight         278.00
_chemical_name_systematic
;
6-Hydroxy-1,4-diazepane-1,4-diium dibromide
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7005(4)
_cell_length_b                   9.2774(5)
_cell_length_c                   12.6853(6)
_cell_measurement_reflns_used    1133
_cell_measurement_temperature    142(2)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      3.80
_cell_volume                     906.25(8)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2007)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      142(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.585
_diffrn_reflns_theta_min         2.720
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.889
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.512
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 646 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2089
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                1789
_reflns_number_total             2089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ku3242sup1.cif
_cod_data_source_block           I
_cod_database_code               2021624
_cod_database_fobs_code          2021624
_shelx_estimated_absorpt_t_min   0.236
_shelx_estimated_absorpt_t_max   0.849
_shelx_hkl_checksum              36163
_shelx_res_checksum              40870
_shelxl_version_number           2014/6