#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/18/2211822.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2211822
loop_
_publ_author_name
'Ock Keum Kawk'
'Kil Sik Min'
'Bong Gon Kim'
_publ_section_title
;
 Tetraaqua(2,2'-bipyridine-5,5'-dicarboxylato)iron(II) dihydrate
;
_journal_coeditor_code           HB2212
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m17
_journal_page_last               m19
_journal_paper_doi               10.1107/S1600536806050914
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Fe (C12 H6 N2 O4) (H2 O)4], 2H2 O'
_chemical_formula_moiety         'C12 H14 Fe N2 O8, 2(H2 O)'
_chemical_formula_sum            'C12 H18 Fe N2 O10'
_chemical_formula_weight         406.13
_chemical_name_systematic
;
Tetraaqua(2,2'-bipyridine-5,5'-dicarboxylato)iron(II) dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.620(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7597(11)
_cell_length_b                   9.2615(8)
_cell_length_c                   13.2195(11)
_cell_measurement_reflns_used    3035
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.72
_cell_volume                     1559.1(2)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SHELXTL (Siemens, 1996)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       ω
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4812
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.789
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0386
_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)+(0.0294P)²+2.755P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0847
_reflns_number_gt                1666
_reflns_number_total             1827
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2212.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2211822
_cod_database_fobs_code          2211822
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Fe Fe1 0.0000 0.69530(5) 0.2500 0.01321(13) Uani d S 1
O O1 0.25315(12) 1.08141(18) 0.61965(12) 0.0221(4) Uani d . 1
O O2 0.20853(13) 0.84945(18) 0.62409(12) 0.0232(4) Uani d . 1
O O1W -0.04583(15) 0.5442(2) 0.14090(15) 0.0279(4) Uani d . 1
H H1A -0.100(3) 0.504(4) 0.138(2) 0.041(10) Uiso d . 1
H H1B -0.006(3) 0.494(4) 0.123(2) 0.035(10) Uiso d . 1
O O2W -0.16387(12) 0.6825(2) 0.29257(13) 0.0190(3) Uani d . 1
H H2A -0.205(3) 0.670(3) 0.241(3) 0.039(9) Uiso d . 1
H H2B -0.184(3) 0.748(4) 0.320(3) 0.047(11) Uiso d . 1
O O3W 0.13099(15) 0.4237(2) 0.09342(17) 0.0366(5) Uani d . 1
H H3A 0.153(3) 0.340(5) 0.120(3) 0.076(14) Uiso d . 1
H H3B 0.162(3) 0.480(5) 0.132(3) 0.066(13) Uiso d . 1
N N1 0.04329(13) 0.8811(2) 0.34370(13) 0.0148(4) Uani d . 1
C C1 0.09674(16) 0.8717(2) 0.43480(15) 0.0157(4) Uani d . 1
H H1 0.1059 0.7793 0.4653 0.019 Uiso calc R 1
C C2 0.13880(15) 0.9911(2) 0.48570(15) 0.0146(4) Uani d . 1
C C3 0.12427(17) 1.1260(2) 0.44117(16) 0.0170(4) Uani d . 1
H H3 0.1522 1.2100 0.4741 0.020 Uiso calc R 1
C C4 0.06813(17) 1.1367(2) 0.34745(16) 0.0175(4) Uani d . 1
H H4 0.0568 1.2282 0.3162 0.021 Uiso calc R 1
C C5 0.02926(15) 1.0129(2) 0.30055(15) 0.0142(4) Uani d . 1
C C6 0.20443(16) 0.9727(2) 0.58463(16) 0.0159(4) Uani d . 1
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'
Fe Fe 0.3463 0.8444 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1W Fe1 N1 . . 170.08(8) n
O1W Fe1 O2W . . 84.87(8) n
N1 Fe1 O2W . . 96.22(7) n
O1W Fe1 O1W . 2 94.81(12) n
O1W Fe1 N1 2 . 95.03(7) ?
O1W Fe1 N1 . 2 95.03(7) ?
O1W Fe1 N1 2 2 170.08(8) ?
N1 Fe1 N1 . 2 75.17(9) y
O1W Fe1 O2W . 2 90.95(7) ?
O1W Fe1 O2W 2 2 84.87(8) ?
N1 Fe1 O2W . 2 88.68(6) ?
N1 Fe1 O2W 2 2 96.22(7) ?
O1W Fe1 O2W 2 . 90.95(7) ?
N1 Fe1 O2W 2 . 88.68(6) ?
O2W Fe1 O2W 2 . 173.83(10) ?
Fe1 O1W H1A . . 125(2) ?
Fe1 O1W H1B . . 119(2) ?
H1A O1W H1B . . 108(4) ?
Fe1 O2W H2A . . 110(2) ?
Fe1 O2W H2B . . 115(3) ?
H2A O2W H2B . . 107(3) ?
H3A O3W H3B . . 100(4) ?
C1 N1 C5 . . 118.68(18) ?
C1 N1 Fe1 . . 123.68(15) ?
C5 N1 Fe1 . . 116.86(13) ?
N1 C1 C2 . . 122.8(2) ?
N1 C1 H1 . . 118.6 ?
C2 C1 H1 . . 118.6 ?
C1 C2 C3 . . 118.37(19) ?
C1 C2 C6 . . 120.35(19) ?
C3 C2 C6 . . 121.18(19) ?
C2 C3 C4 . . 119.2(2) ?
C2 C3 H3 . . 120.4 ?
C4 C3 H3 . . 120.4 ?
C5 C4 C3 . . 119.3(2) ?
C5 C4 H4 . . 120.3 ?
C3 C4 H4 . . 120.3 ?
N1 C5 C4 . . 121.67(18) ?
N1 C5 C5 . 2 115.05(11) ?
C4 C5 C5 . 2 123.27(13) ?
O1 C6 O2 . . 124.69(19) yes
O1 C6 C2 . . 117.5(2) yes
O2 C6 C2 . . 117.80(19) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N1 . 2.1709(19) yes
Fe1 N1 2 2.1709(18) ?
Fe1 O1W . 2.0671(18) yes
Fe1 O1W 2 2.0671(18) ?
Fe1 O2W . 2.2026(16) yes
Fe1 O2W 2 2.2026(16) ?
C6 O1 . 1.256(3) yes
C6 O2 . 1.255(3) yes
O1W H1A . 0.79(3) ?
O1W H1B . 0.74(3) ?
O2W H2A . 0.84(3) ?
O2W H2B . 0.76(4) ?
O3W H3A . 0.88(5) ?
O3W H3B . 0.82(4) ?
N1 C1 . 1.349(3) n
N1 C5 . 1.355(3) ?
C1 C2 . 1.385(3) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.389(3) ?
C2 C6 . 1.517(3) n
C3 C4 . 1.395(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.381(3) ?
C4 H4 . 0.9500 ?
C5 C5 2 1.489(4) n
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1W H1A O1 8_465 0.79(3) 2.03(4) 2.815(3) 173(3) y
O1W H1B O3W 1_555 0.74(3) 1.93(4) 2.629(3) 158(3) y
O2W H2A O2 8_465 0.84(3) 1.85(4) 2.691(2) 177(3) y
O2W H2B O1 5_576 0.76(4) 2.00(4) 2.755(3) 172(4) y
O3W H3A O2 6_565 0.88(5) 1.89(5) 2.737(3) 159(4) y
O3W H3B O2W 2_555 0.82(4) 2.12(4) 2.848(3) 148(4) y
C1 H1 O3W 6_566 0.95 2.54 3.458(3) 163 y
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
O1W Fe1 N1 C1 2 . 8.45(17)
N1 Fe1 N1 C1 2 . -173.1(2)
O2W Fe1 N1 C1 2 . -76.28(17)
O2W Fe1 N1 C1 . . 99.96(17)
O1W Fe1 N1 C5 2 . 178.18(16)
N1 Fe1 N1 C5 2 . -3.34(11)
O2W Fe1 N1 C5 2 . 93.45(15)
O2W Fe1 N1 C5 . . -90.31(15)
C5 N1 C1 C2 . . -0.6(3)
Fe1 N1 C1 C2 . . 168.92(16)
N1 C1 C2 C3 . . 0.6(3)
N1 C1 C2 C6 . . -175.87(19)
C1 C2 C3 C4 . . 0.1(3)
C6 C2 C3 C4 . . 176.51(19)
C2 C3 C4 C5 . . -0.7(3)
C1 N1 C5 C4 . . 0.0(3)
Fe1 N1 C5 C4 . . -170.29(16)
C1 N1 C5 C5 . 2 179.2(2)
Fe1 N1 C5 C5 . 2 8.9(3)
C3 C4 C5 N1 . . 0.7(3)
C3 C4 C5 C5 . 2 -178.5(2)
C1 C2 C6 O2 . . -8.3(3)
C3 C2 C6 O2 . . 175.3(2)
C1 C2 C6 O1 . . 169.8(2)
C3 C2 C6 O1 . . -6.6(3)
