Tetra-<i>n</i>-butylammonium tricyanido[<i>N</i>-(2-pyridylcarbonyl)pyridine-2-carboximidato]ferrate(III) dihydrate
Xiao, Yunyun; Shen, Xiaoping; Li, Yizhi; Acta Crystallographica Section E 67 (2011) m1879–; doi:10.1107/S1600536811049415

data_2233050
_publ_section_title
;
 Tetra-<i>n</i>-butylammonium
 tricyanido[<i>N</i>-(2-pyridylcarbonyl)pyridine-2-carboximidato]ferrate(III)
 dihydrate
;
_journal_coeditor_code           ZL2426
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1879
_journal_paper_doi               10.1107/S1600536811049415
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac
'(C16 H36 N) [Fe (C12 H8 N3 O2) (C N)3], 2H2 O'
_chemical_formula_moiety         'C16 H36 N +, C15 H8 Fe N6 O2 -, 2(H2 O)'
_chemical_formula_sum            'C31 H48 Fe N7 O4'
_chemical_formula_weight         638.61
_chemical_name_systematic
;
Tetra-<i>n</i>-butylammonium
tricyanido[<i>N</i>-(2-pyridylcarbonyl)pyridine-2-carboximidato]ferrate(III)
dihydrate
;
_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                90.00
_cell_angle_beta                 90.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.142(2)
_cell_length_b                   15.663(3)
_cell_length_c                   17.097(3)
_cell_measurement_reflns_used    4928
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.81
_cell_measurement_theta_min      2.11
_cell_volume                     3519.2(11)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn 724 CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17432
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.9035
_exptl_absorpt_correction_T_min  0.8873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6359
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      2.916
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0599
_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^)+(0.0648P)^2^+0.0340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                4300
_reflns_number_total             6359
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2426.cif
_cod_data_source_block           I
_cod_original_cell_volume        3519.0(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2233050
_cod_database_fobs_code          2233050