<i>N</i>,<i>N</i>'-Dibutyl-<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethane-1,2-diaminium μ-oxido-bis[trichloridoferrate(III)]
Närhi, Sari M.; Kostamo, Jatta; Asikkala, Janne; Oilunkaniemi, Raija; Laitinen, Risto S.; Acta Crystallographica Section E 68 (2012) m748–; doi:10.1107/S1600536812019964

data_2235024
_publ_section_title
;
 <i>N</i>,<i>N</i>'-Dibutyl-<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-tetramethylethane-1,2-diaminium
 \m-oxido-bis[trichloridoferrate(III)]
;
_journal_coeditor_code           HB6765
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m748
_journal_paper_doi               10.1107/S1600536812019964
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C14 H34 N2) [Fe2 Cl6 O]'
_chemical_formula_moiety         'C14 H34 N2 2+, Cl6 Fe2 O 2-'
_chemical_formula_sum            'C14 H34 Cl6 Fe2 N2 O'
_chemical_formula_weight         570.83
_chemical_name_systematic
;
<i>N</i>,<i>N</i>'-Dibutyl-<i>N</i>,<i>N</i>,<i>N</i>',<i>N</i>'-
tetramethylethane-1,2-diaminium \m-oxido-bis[trichloridoferrate(III)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.75(3)
_cell_angle_beta                 87.66(3)
_cell_angle_gamma                80.32(3)
_cell_formula_units_Z            4
_cell_length_a                   8.9803(18)
_cell_length_b                   14.689(3)
_cell_length_c                   19.249(4)
_cell_measurement_reflns_used    7321
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.30
_cell_volume                     2476.7(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Bruker, 2008)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29910
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.8677
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.814
_refine_ls_extinction_coef       0.0242(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0711P)^2^+1.9303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                7321
_reflns_number_total             8498
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6765.cif
_cod_data_source_block           I
_cod_original_cell_volume        2476.8(9)
_cod_database_code               2235024
_cod_database_fobs_code          2235024