Tris[4-(dimethylamino)pyridinium] hexakis(thiocyanato-κ<i>N</i>)ferrate(III) monohydrate
Wöhlert, Susanne; Jess, Inke; Näther, Christian; Acta Crystallographica Section E 69 (2013) m33–; doi:10.1107/S1600536812049574

data_2237161
_publ_section_title
;
 Tris[4-(dimethylamino)pyridinium]
 hexakis(thiocyanato-\k<i>N</i>)ferrate(III) monohydrate
;
_journal_coeditor_code           HP2051
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m33
_journal_paper_doi               10.1107/S1600536812049574
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C7 H11 N2)3 [Fe (N C S)6], H2 O'
_chemical_formula_moiety         'C6 Fe N6 S6, 3 (C7 H11 N2), H2O'
_chemical_formula_sum            'C27 H35 Fe N12 O S6'
_chemical_formula_weight         791.88
_chemical_name_systematic
;
Tris[4-(dimethylamino)pyridinium] hexakis(thiocyanato-\k<i>N</i>)ferrate(III)
monohydrate
;
_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                81.260(7)
_cell_angle_beta                 71.550(7)
_cell_angle_gamma                62.950(6)
_cell_formula_units_Z            2
_cell_length_a                   11.5780(7)
_cell_length_b                   11.7620(7)
_cell_length_c                   16.5450(11)
_cell_measurement_reflns_used    13617
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.35
_cell_volume                     1903.4(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2008)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2008)'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2012)
;
_computing_publication_material  '<i>XCIF</i> in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       'phi scan'
_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  0.0754
_diffrn_reflns_av_sigmaI/netI    0.0869
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13617
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_correction_T_min  0.8081
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.1257
_exptl_crystal_size_mid          0.0769
_exptl_crystal_size_min          0.0550
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.501
_refine_ls_extinction_coef       0.0045(11)
_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   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         7356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                4936
_reflns_number_total             7356
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hp2051.cif
_cod_data_source_block           I
_cod_database_code               2237161
_cod_database_fobs_code          2237161