Crystal structure of (1<i>S</i>,4<i>S</i>)-2,5-diazo-niabi-cyclo[2.2.1]heptane dibromide.
Britvin, Sergey N.; Rumyantsev, Andrey M.; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 1861–1865; doi:10.1107/S2056989017015870

data_2311514
_publ_section_title
;
 Crystal structure of
 (1<i>S</i>,4<i>S</i>)-2,5-diazo-niabi-cyclo[2.2.1]heptane dibromide.
;
_journal_coeditor_code           LH5858
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1861
_journal_page_last               1865
_journal_paper_doi               10.1107/S2056989017015870
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C5 H12 N2 2+, 2Br -'
_chemical_formula_moiety         'C5 H12 N2 2+, 2(Br -)'
_chemical_formula_sum            'C5 H12 Br2 N2'
_chemical_formula_weight         259.99
_chemical_name_common
'1S,4S-2,5-diazabicyclo[2.2.1]heptane dihydrobromode'
_chemical_name_systematic
;
(1<i>S</i>,4<i>S</i>)-2,5-Diazoniabicyclo[2.2.1]heptane 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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.7298(6)
_cell_length_b                   11.8643(5)
_cell_length_c                   14.4933(7)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.52
_cell_volume                     1673.07(15)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008) and <i>OLEX2</i> (Dolomanov <i>et
al.</i>,  2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15838
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.218
_exptl_absorpt_coefficient_mu    9.613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.340
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1676 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   0.009(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0147
_refine_ls_R_factor_gt           0.0143
_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^)+(0.0162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0351
_refine_ls_wR_factor_ref         0.0353
_reflns_number_gt                3959
_reflns_number_total             4031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5858sup1.cif
_cod_data_source_block           I
_cod_database_code               2311514
_shelx_hkl_checksum              49623
_shelx_res_checksum              84170