Bis[4-(4-pyridyl)pyridinium] (4-carboxypyridine-2,6-dicarboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)(pyridine-2,4,6-tricarboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)ferrate(III) trihydrate
Zhao, Li; Dong, You-Ren; Xie, Hong-Zhen; Acta Crystallographica Section E 65 (2009) m450–m451; doi:10.1107/S1600536809010514

data_2221461
_publ_section_title
;Bis[4-(4-pyridyl)pyridinium]
 (4-carboxypyridine-2,6-dicarboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)(pyridine-2,4,6-tricarboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)ferrate(III)
 trihydrate
;
_journal_coeditor_code           NG2562
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m450
_journal_page_last               m451
_journal_paper_doi               10.1107/S1600536809010514
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'(C10 H9 N2)2 [Fe (C8 H2 N O6) (C8 H3 N O6)], 3H2 O'
_chemical_formula_moiety         'C36 H23 Fe N6 O12, 3(H2 O)'
_chemical_formula_sum            'C36 H29 Fe N6 O15'
_chemical_formula_weight         841.50
_chemical_name_systematic
;
Bis[4-(4-pyridyl)pyridinium] (4-carboxypyridine-2,6-dicarboxylato-
\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)(pyridine-2,4,6-tricarboxylato-
\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)ferrate(III) trihydrate
;
_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                77.13(3)
_cell_angle_beta                 79.82(3)
_cell_angle_gamma                76.15(3)
_cell_formula_units_Z            2
_cell_length_a                   10.568(2)
_cell_length_b                   12.386(3)
_cell_length_c                   14.344(3)
_cell_measurement_reflns_used    17019
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.2
_cell_volume                     1762.0(7)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17019
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.406
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         7934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.2949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                5458
_reflns_number_total             7934
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2562.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_hbond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (9 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_hbond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (9 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1761.9(6)
_cod_database_code               2221461
_cod_database_fobs_code          2221461