Ammonium bis(tetraethylammonium) hexacyanidoferrate(III) trihydrate
Miroslava Matiková Maľarová; Juraj Černák; Werner Massa; Acta Crystallographica Section C 63 (2007) m187–m189; doi:10.1107/S0108270107010499

data_2015934
_publ_section_title
;
 Ammonium bis(tetraethylammonium) hexacyanidoferrate(III) trihydrate
;
_journal_coeditor_code           DN3040
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m187
_journal_page_last               m189
_journal_paper_doi               10.1107/S0108270107010499
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(N H4) (C8 H20 N)2 [Fe (C N)6], 3H2 O'
_chemical_formula_moiety         'N1 H4 +, 2(C8 H20 N -), C6 Fe N6 3-, 3H2 O'
_chemical_formula_sum            'C22 H50 Fe N9 O3'
_chemical_formula_weight         544.56
_chemical_name_systematic
;
Ammonium bis(tetraethylammonium) hexacyanoferrate(III) trihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 99.051(9)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   10.4720(10)
_cell_length_b                   10.2339(7)
_cell_length_c                   14.518(2)
_cell_measurement_reflns_used    3710
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.24
_cell_volume                     1536.5(3)
_computing_cell_refinement       'CELL in IPDS Software'
_computing_data_collection       'EXPOSE in IPDS Software (Stoe, 1999)'
_computing_data_reduction        'INTEGRATE in IPDS Software'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13143
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.146
_exptl_absorpt_correction_T_min  0.055
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(XPREP in SHELXTL; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.468
_refine_ls_extinction_coef       0.0070(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3710
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0388
_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^)+(0.052P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                2472
_reflns_number_total             3710
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn3040.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2015934
_cod_database_fobs_code          2015934