1,4-Diazoniabicyclo[2.2.2]octane diaquadichlorido(oxalato-κ^2^<i>O</i>,<i>O</i>')iron(III) chloride
Cai, Ying; Acta Crystallographica Section E 65 (2009) m877–; doi:10.1107/S1600536809025628

data_2222648
_publ_section_title
;
 1,4-Diazoniabicyclo[2.2.2]octane
 diaquadichlorido(oxalato-\k^2^<i>O</i>,<i>O</i>')iron(III) chloride
;
_journal_coeditor_code           CV2580
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m877
_journal_paper_doi               10.1107/S1600536809025628
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C6 H14 N2) [Fe (C2 O4) Cl2 (H2 O)2] Cl'
_chemical_formula_moiety         'C6 H14 N2 2+, C2 H4 Cl2 Fe O6 -, Cl -'
_chemical_formula_sum            'C8 H18 Cl3 Fe N2 O6'
_chemical_formula_weight         400.44
_chemical_name_systematic
;
1,4-Diazoniabicyclo[2.2.2]octane
diaquadichlorido(oxalato-\k^2^<i>O</i>,<i>O</i>')iron(III) chloride
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_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                 109.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.872(2)
_cell_length_b                   9.6636(19)
_cell_length_c                   8.4268(17)
_cell_measurement_reflns_used    3950
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.04
_cell_volume                     757.5(3)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    '<i>SHELXTL</i>/<i>PC</i> (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3954
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.548
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             410
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.153
_refine_ls_abs_structure_details 'Flack (1983), 802 Friedel pairs'
_refine_ls_abs_structure_Flack   0.016(13)
_refine_ls_extinction_coef       0.0476(15)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1729
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0493
_reflns_number_gt                1684
_reflns_number_total             1729
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2580.cif
_cod_data_source_block           I
_cod_original_cell_volume        757.4(3)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2222648
_cod_database_fobs_code          2222648