A novel framework of N—H···Br hydrogen bonds forming Br(4,4'-bipyridinium)~4~ supramolecular synthons: bis(4,4'-bipyridinium) tris[tetrabromidoferrate(III)] bromide
Ali, Basem Fares; Al-Far, Rawhi; Acta Crystallographica Section C 63 (2007) m451–m453; doi:10.1107/S0108270107039856

data_2016179
_publ_section_title
;
 A novel framework of N---H&#x00B7;&#x00B7;&#x00B7;Br hydrogen bonds
 forming Br(4,4'-bipyridinium)~4~ supramolecular synthons:
 bis(4,4'-bipyridinium) tris[tetrabromidoferrate(III)] bromide
;
_journal_coeditor_code           BG3043
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m451
_journal_page_last               m453
_journal_paper_doi               10.1107/S0108270107039856
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C10 H10 N2)2 [Fe Br4]3 Br'
_chemical_formula_moiety         '2(C10 H10 N2 2+), 3(Br4 Fe -), Br -'
_chemical_formula_sum            'C20 H20 Br13 Fe3 N4'
_chemical_formula_weight         1522.65
_chemical_name_common            (4,4'-DPyH2)2.(FeBr4)3.Br
_chemical_name_systematic
;
bis(4,4'-bipyridinium) tris[tetrabromidoferrate(III)] bromide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5536(6)
_cell_length_b                   18.4508(9)
_cell_length_c                   18.9844(10)
_cell_measurement_reflns_used    7249
_cell_measurement_temperature    84(2)
_cell_measurement_theta_max      26.80
_cell_measurement_theta_min      2.34
_cell_volume                     4047.0(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2000)'
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        'CrystalClear (Rigaku, 2000)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'XL in SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'XS in SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      84(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46358
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    13.916
_exptl_absorpt_correction_T_max  0.0641
_exptl_absorpt_correction_T_min  0.0564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2804
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.426
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.010(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         9301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0102P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0547
_reflns_number_gt                7964
_reflns_number_total             9303
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3043.cif
_cod_data_source_block           I
_cod_database_code               2016179
_cod_database_fobs_code          2016179