#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/17/8101764.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8101764
loop_
_publ_author_name
'H.-Z. Shi'
'Z.-L. Li'
'Y.-K. Shan'
_publ_section_title
;
Crystal structure of catena-[diaqua-hexapyridinyl-bis(μ-sulfato)
diiron(II)] tetrahydrate, [Fe(C₅H₅N)₄][Fe(H₂O)₂(C₅H₅N)
~2~](SO~4~)~2 ~· 4H₂O
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              245
_journal_page_last               246
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety
'[Fe(py)~4~][Fe(H~2~O)~2~(py)~2~](SO~4~)~2~ &#x00B7; 4H~2~O'
_chemical_formula_sum            'C30 H42 Fe2 N6 O14 S2'
_chemical_formula_weight         886.52
_chemical_name_systematic
; 
catena-[diaqua-hexapyridinyl-bis(μ-sulfato)diiron(II)] 
tetrahydrate 
;
_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                 108.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.470(3)
_cell_length_b                   9.4980(19)
_cell_length_c                   17.043(3)
_cell_measurement_reflns_used    230
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2
_cell_volume                     1917.3(8)
_computing_cell_refinement       raxis
_computing_data_collection       raxis
_computing_data_reduction        raxis
_computing_molecular_graphics    texsan
_computing_publication_material  texsan
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IV'
_diffrn_measurement_method       omega/phi
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4969
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.8494
_exptl_absorpt_correction_T_min  0.7792
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0013(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2893
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0430
_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/[σ²(Fo²)+(0.0361P)²+1.7115P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                2608
_reflns_number_total             2893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1512.cff
_cod_data_source_block           Fesulfpyaqwa
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        1917.1(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               8101764
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.0000 0.0000 0.02193(17) Uani 1 2 a d S . .
Fe2 Fe 0.5000 0.0000 0.0000 0.02082(17) Uani 1 2 b d S . .
S1 S 0.25461(6) -0.13891(8) 0.01969(5) 0.02064(19) Uani 1 4 e d . . .
O1 O 0.17566(16) -0.0516(2) 0.05004(13) 0.0261(5) Uani 1 4 e d . . .
O2 O 0.20150(18) -0.1730(3) -0.06743(13) 0.0344(6) Uani 1 4 e d . . .
O3 O 0.2853(2) -0.2653(2) 0.07016(15) 0.0383(6) Uani 1 4 e d . . .
O4 O 0.35660(17) -0.0525(2) 0.03003(14) 0.0308(5) Uani 1 4 e d . . .
O5 O -0.0005(2) 0.0497(3) 0.12479(17) 0.0360(6) Uani 1 4 e d . . .
O6 O 0.2820(3) -0.0168(3) 0.22236(19) 0.0596(8) Uiso 1 4 e d D . .
O7 O 0.3419(3) -0.2976(4) 0.2398(2) 0.0549(8) Uiso 1 4 e d . . .
N1 N -0.0462(2) -0.2165(3) 0.02193(17) 0.0292(6) Uani 1 4 e d . . .
N2 N 0.4973(2) 0.2019(3) 0.07148(16) 0.0283(6) Uani 1 4 e d . . .
N3 N 0.6033(2) -0.1100(3) 0.11302(16) 0.0286(6) Uani 1 4 e d . . .
C1 C 0.0143(3) -0.2903(4) 0.0882(2) 0.0346(8) Uani 1 4 e d . . .
H1A H 0.0790 -0.2491 0.1236 0.042 Uiso 1 4 e calc R . .
C2 C -0.0140(3) -0.4233(4) 0.1067(2) 0.0439(10) Uani 1 4 e d . . .
H2B H 0.0298 -0.4703 0.1537 0.053 Uiso 1 4 e calc R . .
C3 C -0.1089(3) -0.4851(4) 0.0536(3) 0.0474(10) Uani 1 4 e d . . .
H3B H -0.1301 -0.5753 0.0640 0.057 Uiso 1 4 e calc R . .
C4 C -0.1719(3) -0.4124(4) -0.0148(3) 0.0453(10) Uani 1 4 e d . . .
H4A H -0.2363 -0.4526 -0.0513 0.054 Uiso 1 4 e calc R . .
C5 C -0.1384(3) -0.2790(4) -0.0287(2) 0.0371(9) Uani 1 4 e d . . .
H5B H -0.1816 -0.2302 -0.0752 0.045 Uiso 1 4 e calc R . .
C6 C 0.4460(3) 0.2098(4) 0.1303(2) 0.0367(9) Uani 1 4 e d . . .
H6A H 0.4077 0.1307 0.1398 0.044 Uiso 1 4 e calc R . .
C7 C 0.4470(3) 0.3279(4) 0.1769(2) 0.0486(10) Uani 1 4 e d . . .
H7A H 0.4107 0.3283 0.2170 0.058 Uiso 1 4 e calc R . .
C8 C 0.5024(4) 0.4449(5) 0.1632(3) 0.0546(11) Uani 1 4 e d . . .
H8A H 0.5046 0.5263 0.1940 0.066 Uiso 1 4 e calc R . .
C9 C 0.5552(4) 0.4406(4) 0.1030(3) 0.0498(11) Uani 1 4 e d . . .
H9A H 0.5938 0.5186 0.0927 0.060 Uiso 1 4 e calc R . .
C10 C 0.5493(3) 0.3183(4) 0.0588(2) 0.0356(8) Uani 1 4 e d . . .
H10A H 0.5837 0.3166 0.0176 0.043 Uiso 1 4 e calc R . .
C11 C 0.5684(3) -0.1307(4) 0.1793(2) 0.0386(9) Uani 1 4 e d . . .
H11A H 0.4991 -0.0933 0.1783 0.046 Uiso 1 4 e calc R . .
C12 C 0.6293(3) -0.2040(4) 0.2482(2) 0.0437(10) Uani 1 4 e d . . .
H12A H 0.6016 -0.2148 0.2925 0.052 Uiso 1 4 e calc R . .
C13 C 0.7309(3) -0.2607(4) 0.2510(2) 0.0476(10) Uani 1 4 e d . . .
H13A H 0.7736 -0.3110 0.2970 0.057 Uiso 1 4 e calc R . .
C14 C 0.7686(3) -0.2416(5) 0.1840(2) 0.0507(11) Uani 1 4 e d . . .
H14A H 0.8372 -0.2798 0.1837 0.061 Uiso 1 4 e calc R . .
C15 C 0.7035(3) -0.1654(4) 0.1172(2) 0.0419(9) Uani 1 4 e d . . .
H15A H 0.7307 -0.1517 0.0728 0.050 Uiso 1 4 e calc R . .
H5E H -0.063(4) 0.095(5) 0.113(3) 0.083(18) Uiso 1 4 e d . . .
H5F H 0.042(3) 0.100(4) 0.159(3) 0.044(13) Uiso 1 4 e d . . .
H6E H 0.230(7) -0.041(12) 0.160(3) 0.29(5) Uiso 1 4 e d D . .
H6F H 0.245(6) 0.079(5) 0.250(5) 0.18(3) Uiso 1 4 e d D . .
H7E H 0.329(6) -0.311(8) 0.188(5) 0.17(3) Uiso 1 4 e d . . .
H7F H 0.330(3) -0.234(5) 0.259(3) 0.055(14) Uiso 1 4 e d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 180.0 3_555 . ?
O1 Fe1 O5 91.37(10) 3_555 . ?
O1 Fe1 O5 88.63(10) . . ?
O1 Fe1 O5 88.63(10) 3_555 3_555 ?
O1 Fe1 O5 91.37(10) . 3_555 ?
O5 Fe1 O5 180.00(3) . 3_555 ?
O1 Fe1 N1 89.54(9) 3_555 . ?
O1 Fe1 N1 90.46(9) . . ?
O5 Fe1 N1 87.47(10) . . ?
O5 Fe1 N1 92.53(10) 3_555 . ?
O1 Fe1 N1 90.46(9) 3_555 3_555 ?
O1 Fe1 N1 89.54(9) . 3_555 ?
O5 Fe1 N1 92.53(10) . 3_555 ?
O5 Fe1 N1 87.47(10) 3_555 3_555 ?
N1 Fe1 N1 180.00(15) . 3_555 ?
O4 Fe2 O4 180.00(11) 3_655 . ?
O4 Fe2 N3 90.95(9) 3_655 . ?
O4 Fe2 N3 89.05(9) . . ?
O4 Fe2 N3 89.05(9) 3_655 3_655 ?
O4 Fe2 N3 90.95(9) . 3_655 ?
N3 Fe2 N3 180.00(13) . 3_655 ?
O4 Fe2 N2 95.03(9) 3_655 . ?
O4 Fe2 N2 84.97(9) . . ?
N3 Fe2 N2 91.94(10) . . ?
N3 Fe2 N2 88.06(10) 3_655 . ?
O4 Fe2 N2 84.97(9) 3_655 3_655 ?
O4 Fe2 N2 95.03(9) . 3_655 ?
N3 Fe2 N2 88.06(10) . 3_655 ?
N3 Fe2 N2 91.94(10) 3_655 3_655 ?
N2 Fe2 N2 180.00(14) . 3_655 ?
O3 S1 O2 111.67(15) . . ?
O3 S1 O4 109.30(14) . . ?
O2 S1 O4 110.14(13) . . ?
O3 S1 O1 109.37(14) . . ?
O2 S1 O1 109.63(13) . . ?
O4 S1 O1 106.60(13) . . ?
S1 O1 Fe1 133.58(13) . . ?
S1 O4 Fe2 152.00(15) . . ?
C5 N1 C1 116.9(3) . . ?
C5 N1 Fe1 121.5(2) . . ?
C1 N1 Fe1 121.6(2) . . ?
C10 N2 C6 116.2(3) . . ?
C10 N2 Fe2 121.5(2) . . ?
C6 N2 Fe2 122.3(2) . . ?
C15 N3 C11 116.1(3) . . ?
C15 N3 Fe2 120.7(2) . . ?
C11 N3 Fe2 123.1(2) . . ?
N1 C1 C2 123.8(3) . . ?
C1 C2 C3 118.1(4) . . ?
C4 C3 C2 119.4(4) . . ?
C3 C4 C5 119.0(4) . . ?
N1 C5 C4 122.8(3) . . ?
N2 C6 C7 123.7(4) . . ?
C8 C7 C6 118.7(4) . . ?
C7 C8 C9 119.1(4) . . ?
C10 C9 C8 118.4(4) . . ?
N2 C10 C9 123.9(3) . . ?
N3 C11 C12 123.7(3) . . ?
C13 C12 C11 119.4(4) . . ?
C12 C13 C14 118.2(4) . . ?
C13 C14 C15 119.2(4) . . ?
N3 C15 C14 123.3(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.144(2) 3_555 ?
Fe1 O1 2.144(2) . ?
Fe1 O5 2.181(3) . ?
Fe1 O5 2.181(3) 3_555 ?
Fe1 N1 2.199(3) . ?
Fe1 N1 2.199(3) 3_555 ?
Fe2 O4 2.069(2) 3_655 ?
Fe2 O4 2.069(2) . ?
Fe2 N3 2.215(3) . ?
Fe2 N3 2.215(3) 3_655 ?
Fe2 N2 2.278(3) . ?
Fe2 N2 2.278(3) 3_655 ?
S1 O3 1.456(2) . ?
S1 O2 1.460(2) . ?
S1 O4 1.477(2) . ?
S1 O1 1.498(2) . ?
N1 C5 1.341(4) . ?
N1 C1 1.343(4) . ?
N2 C10 1.333(4) . ?
N2 C6 1.350(4) . ?
N3 C15 1.337(4) . ?
N3 C11 1.345(4) . ?
C1 C2 1.374(5) . ?
C2 C3 1.375(5) . ?
C3 C4 1.371(6) . ?
C4 C5 1.377(5) . ?
C6 C7 1.372(5) . ?
C7 C8 1.367(6) . ?
C8 C9 1.382(6) . ?
C9 C10 1.374(5) . ?
C11 C12 1.371(5) . ?
C12 C13 1.363(5) . ?
C13 C14 1.377(5) . ?
C14 C15 1.379(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5E O2 0.85(5) 1.82(5) 2.660(4) 169(5) 3_555
O5 H5F O7 0.81(4) 2.11(4) 2.913(5) 171(4) 2
O6 H6E O1 1.08(2) 1.78(3) 2.838(5) 163(6) .
O6 H6F O7 1.18(2) 1.64(3) 2.786(5) 161(6) 2
O7 H7E O3 0.85(8) 1.96(8) 2.770(5) 158(7) .
O7 H7F O6 0.72(8) 2.18(8) 2.761(5) 137(7) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 S1 O1 Fe1 -110.67(19) . . . . ?
O2 S1 O1 Fe1 12.1(2) . . . . ?
O4 S1 O1 Fe1 131.27(18) . . . . ?
O1 Fe1 O1 S1 -38(8) 3_555 . . . ?
O5 Fe1 O1 S1 159.02(19) . . . . ?
O5 Fe1 O1 S1 -20.98(19) 3_555 . . . ?
N1 Fe1 O1 S1 71.56(19) . . . . ?
N1 Fe1 O1 S1 -108.44(19) 3_555 . . . ?
O3 S1 O4 Fe2 85.6(3) . . . . ?
O2 S1 O4 Fe2 -37.5(4) . . . . ?
O1 S1 O4 Fe2 -156.3(3) . . . . ?
O4 Fe2 O4 S1 125(100) 3_655 . . . ?
N3 Fe2 O4 S1 -102.4(3) . . . . ?
N3 Fe2 O4 S1 77.6(3) 3_655 . . . ?
N2 Fe2 O4 S1 165.6(3) . . . . ?
N2 Fe2 O4 S1 -14.4(3) 3_655 . . . ?
O1 Fe1 N1 C5 33.1(3) 3_555 . . . ?
O1 Fe1 N1 C5 -146.9(3) . . . . ?
O5 Fe1 N1 C5 124.5(3) . . . . ?
O5 Fe1 N1 C5 -55.5(3) 3_555 . . . ?
N1 Fe1 N1 C5 -62(7) 3_555 . . . ?
O1 Fe1 N1 C1 -144.4(3) 3_555 . . . ?
O1 Fe1 N1 C1 35.6(3) . . . . ?
O5 Fe1 N1 C1 -53.0(3) . . . . ?
O5 Fe1 N1 C1 127.0(3) 3_555 . . . ?
N1 Fe1 N1 C1 120(7) 3_555 . . . ?
O4 Fe2 N2 C10 22.0(3) 3_655 . . . ?
O4 Fe2 N2 C10 -158.0(3) . . . . ?
N3 Fe2 N2 C10 113.1(2) . . . . ?
N3 Fe2 N2 C10 -66.9(2) 3_655 . . . ?
N2 Fe2 N2 C10 -18(100) 3_655 . . . ?
O4 Fe2 N2 C6 -156.2(3) 3_655 . . . ?
O4 Fe2 N2 C6 23.8(3) . . . . ?
N3 Fe2 N2 C6 -65.1(3) . . . . ?
N3 Fe2 N2 C6 114.9(3) 3_655 . . . ?
N2 Fe2 N2 C6 164(100) 3_655 . . . ?
O4 Fe2 N3 C15 -26.9(3) 3_655 . . . ?
O4 Fe2 N3 C15 153.1(3) . . . . ?
N3 Fe2 N3 C15 7(100) 3_655 . . . ?
N2 Fe2 N3 C15 -122.0(3) . . . . ?
N2 Fe2 N3 C15 58.0(3) 3_655 . . . ?
O4 Fe2 N3 C11 156.0(3) 3_655 . . . ?
O4 Fe2 N3 C11 -24.0(3) . . . . ?
N3 Fe2 N3 C11 -170(100) 3_655 . . . ?
N2 Fe2 N3 C11 60.9(3) . . . . ?
N2 Fe2 N3 C11 -119.1(3) 3_655 . . . ?
C5 N1 C1 C2 -0.7(5) . . . . ?
Fe1 N1 C1 C2 176.9(3) . . . . ?
N1 C1 C2 C3 0.9(6) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
C2 C3 C4 C5 0.0(6) . . . . ?
C1 N1 C5 C4 0.2(5) . . . . ?
Fe1 N1 C5 C4 -177.4(3) . . . . ?
C3 C4 C5 N1 0.1(6) . . . . ?
C10 N2 C6 C7 -1.2(5) . . . . ?
Fe2 N2 C6 C7 177.1(3) . . . . ?
N2 C6 C7 C8 0.3(6) . . . . ?
C6 C7 C8 C9 0.1(6) . . . . ?
C7 C8 C9 C10 0.3(6) . . . . ?
C6 N2 C10 C9 1.7(5) . . . . ?
Fe2 N2 C10 C9 -176.6(3) . . . . ?
C8 C9 C10 N2 -1.3(6) . . . . ?
C15 N3 C11 C12 -0.2(6) . . . . ?
Fe2 N3 C11 C12 177.0(3) . . . . ?
N3 C11 C12 C13 -0.4(6) . . . . ?
C11 C12 C13 C14 0.2(6) . . . . ?
C12 C13 C14 C15 0.6(6) . . . . ?
C11 N3 C15 C14 1.0(6) . . . . ?
Fe2 N3 C15 C14 -176.3(3) . . . . ?
C13 C14 C15 N3 -1.3(7) . . . . ?
