#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/35/2223526.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_2223526
loop_
_publ_author_name
'Jiang, Bin'
'Liu, Zhilu'
_publ_section_title
;Poly[[aqua(μ-4,4'-bipyridyl-κ²N:N')bis(μ-formato-κ²O:O')iron(II)]
 tetrahydrate]
;
_journal_coeditor_code           PV2199
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1189
_journal_page_last               m1190
_journal_paper_doi               10.1107/S1600536809034722
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Fe (C H O2)2 (C10 H8 N2) (H2 O)], 4H2 O'
_chemical_formula_moiety         'C12 H12 Fe N2 O5, 4(H2 O)'
_chemical_formula_sum            'C12 H20 Fe N2 O9'
_chemical_formula_weight         392.15
_chemical_name_systematic
;
Poly[[aqua(μ-4,4'-bipyridyl-κ²N:N')-μ-formato-
κ²O:O'-formato-κO-iron(II)] tetrahydrate]
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 102.3670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5021(6)
_cell_length_b                   20.1959(11)
_cell_length_c                   8.1256(4)
_cell_measurement_reflns_used    4008
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.23
_cell_volume                     1683.44(16)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4376
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.8952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.418
_refine_ls_abs_structure_details 'Flack  (1983), 1036 Friedel pairs'
_refine_ls_abs_structure_Flack   0.158(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         2523
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0336
_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/[σ²(Fo²)+(0.071P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                2468
_reflns_number_total             2523
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pv2199.cif
_cod_data_source_block           I
_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 1527 2010-12-29 10:47:43Z saulius 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2223526
_cod_database_fobs_code          2223526
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'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.99831(11) 0.753902(16) 0.64202(13) 0.01649(13) Uani d D 1 . .
C C1 0.7398(3) 0.72764(15) 0.4049(4) 0.0274(6) Uani d . 1 . .
H H1 0.7212 0.7713 0.4273 0.033 Uiso calc R 1 . .
C C2 1.0318(4) 0.76341(18) 0.2832(5) 0.0339(8) Uani d . 1 . .
H H2 0.9801 0.7256 0.2686 0.041 Uiso calc R 1 . .
C C3 0.7896(3) 0.85353(16) 0.6887(5) 0.0342(7) Uani d . 1 . .
H H3 0.7527 0.8158 0.7245 0.041 Uiso calc R 1 . .
C C4 0.7264(3) 0.91325(17) 0.6933(4) 0.0338(7) Uani d . 1 . .
H H4 0.6487 0.9149 0.7306 0.041 Uiso calc R 1 . .
C C5 0.7789(3) 0.97064(15) 0.6424(4) 0.0294(8) Uani d . 1 . .
C C6 0.8935(4) 0.96383(17) 0.5850(5) 0.0401(9) Uani d . 1 . .
H H6 0.9321 1.0007 0.5475 0.048 Uiso calc R 1 . .
C C7 0.9502(4) 0.90224(16) 0.5837(5) 0.0381(8) Uani d . 1 . .
H H7 1.0269 0.8989 0.5445 0.046 Uiso calc R 1 . .
C C8 0.7165(3) 1.03639(15) 0.6479(4) 0.0280(7) Uani d . 1 . .
C C9 0.5937(3) 1.04287(16) 0.6846(5) 0.0359(8) Uani d . 1 . .
H H9 0.5493 1.0055 0.7090 0.043 Uiso calc R 1 . .
C C10 0.5377(3) 1.10457(17) 0.6847(5) 0.0355(8) Uani d . 1 . .
H H10 0.4555 1.1076 0.7096 0.043 Uiso calc R 1 . .
C C11 0.7777(4) 1.09450(16) 0.6157(5) 0.0355(8) Uani d . 1 . .
H H11 0.8609 1.0932 0.5932 0.043 Uiso calc R 1 . .
C C12 0.7138(3) 1.15402(16) 0.6174(4) 0.0327(8) Uani d . 1 . .
H H12 0.7559 1.1923 0.5938 0.039 Uiso calc R 1 . .
N N1 0.5956(3) 1.16024(12) 0.6509(3) 0.0276(6) Uani d . 1 . .
N N2 0.9005(3) 0.84703(12) 0.6360(3) 0.0267(6) Uani d . 1 . .
O O1 0.8405(2) 0.70271(10) 0.4923(3) 0.0311(5) Uani d . 1 . .
O O2 0.6621(2) 0.69888(11) 0.2902(3) 0.0305(5) Uani d . 1 . .
O O3 1.0696(2) 0.78393(11) 0.4317(3) 0.0330(5) Uani d . 1 . .
O O4 1.0559(3) 0.78812(16) 0.1566(4) 0.0569(8) Uani d . 1 . .
O O5 0.9382(3) 0.73151(14) 0.8633(3) 0.0370(6) Uani d D 1 . .
O O6 0.7891(3) 0.63516(14) 0.9637(4) 0.0482(6) Uani d D 1 . .
O O7 0.6017(4) 0.5754(3) 0.4995(8) 0.1160(19) Uani d D 1 . .
O O8 0.7346(5) 0.51513(19) 0.7912(5) 0.0972(14) Uani d D 1 . .
O O9 0.8996(3) 0.40816(15) 0.7836(4) 0.0561(8) Uani d D 1 . .
H H1W 0.946(5) 0.7580(16) 0.942(5) 0.080 Uiso d D 1 . .
H H2W 0.892(4) 0.6994(13) 0.871(5) 0.080 Uiso d D 1 . .
H H3W 0.727(3) 0.660(2) 0.963(5) 0.080 Uiso d D 1 . .
H H4W 0.822(5) 0.620(2) 1.057(3) 0.080 Uiso d D 1 . .
H H5W 0.644(5) 0.5542(19) 0.444(7) 0.080 Uiso d D 1 . .
H H6W 0.626(5) 0.6138(10) 0.518(7) 0.080 Uiso d D 1 . .
H H7W 0.692(4) 0.531(2) 0.703(3) 0.080 Uiso d D 1 . .
H H8W 0.761(5) 0.5426(16) 0.865(4) 0.080 Uiso d D 1 . .
H H9W 0.850(4) 0.4397(15) 0.764(6) 0.080 Uiso d D 1 . .
H H10W 0.885(5) 0.383(2) 0.856(5) 0.080 Uiso d 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'
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O5 Fe1 O3 . . 174.46(10) ?
O5 Fe1 O1 . . 92.60(10) ?
O3 Fe1 O1 . . 92.62(10) ?
O5 Fe1 O2 . 4_565 88.06(9) ?
O3 Fe1 O2 . 4_565 86.81(9) ?
O1 Fe1 O2 . 4_565 177.17(10) ?
O5 Fe1 N2 . . 88.72(11) ?
O3 Fe1 N2 . . 88.90(10) ?
O1 Fe1 N2 . . 95.96(9) ?
O2 Fe1 N2 4_565 . 86.81(10) ?
O5 Fe1 N1 . 3_545 90.57(11) ?
O3 Fe1 N1 . 3_545 91.81(10) ?
O1 Fe1 N1 . 3_545 84.07(9) ?
O2 Fe1 N1 4_565 3_545 93.18(10) ?
N2 Fe1 N1 . 3_545 179.28(13) ?
O1 C1 O2 . . 125.4(3) ?
O1 C1 H1 . . 117.3 ?
O2 C1 H1 . . 117.3 ?
O4 C2 O3 . . 126.6(4) ?
O4 C2 H2 . . 116.7 ?
O3 C2 H2 . . 116.7 ?
N2 C3 C4 . . 123.6(3) ?
N2 C3 H3 . . 118.2 ?
C4 C3 H3 . . 118.2 ?
C3 C4 C5 . . 119.9(3) ?
C3 C4 H4 . . 120.1 ?
C5 C4 H4 . . 120.1 ?
C4 C5 C6 . . 116.6(3) ?
C4 C5 C8 . . 122.2(3) ?
C6 C5 C8 . . 121.3(3) ?
C7 C6 C5 . . 119.9(3) ?
C7 C6 H6 . . 120.1 ?
C5 C6 H6 . . 120.1 ?
N2 C7 C6 . . 123.4(3) ?
N2 C7 H7 . . 118.3 ?
C6 C7 H7 . . 118.3 ?
C9 C8 C11 . . 116.7(3) ?
C9 C8 C5 . . 121.7(3) ?
C11 C8 C5 . . 121.6(3) ?
C10 C9 C8 . . 120.0(3) ?
C10 C9 H9 . . 120.0 ?
C8 C9 H9 . . 120.0 ?
N1 C10 C9 . . 123.3(3) ?
N1 C10 H10 . . 118.4 ?
C9 C10 H10 . . 118.4 ?
C12 C11 C8 . . 119.3(3) ?
C12 C11 H11 . . 120.4 ?
C8 C11 H11 . . 120.4 ?
N1 C12 C11 . . 124.1(3) ?
N1 C12 H12 . . 117.9 ?
C11 C12 H12 . . 117.9 ?
C12 N1 C10 . . 116.6(3) ?
C12 N1 Fe1 . 3_455 122.3(2) ?
C10 N1 Fe1 . 3_455 121.0(2) ?
C3 N2 C7 . . 116.6(3) ?
C3 N2 Fe1 . . 121.9(2) ?
C7 N2 Fe1 . . 121.4(2) ?
C1 O1 Fe1 . . 126.7(2) ?
C1 O2 Fe1 . 4_464 122.8(2) ?
C2 O3 Fe1 . . 126.3(2) ?
Fe1 O5 H1W . . 122(3) ?
Fe1 O5 H2W . . 122(3) ?
H1W O5 H2W . . 115(4) ?
H3W O6 H4W . . 114(4) ?
H5W O7 H6W . . 114(5) ?
H7W O8 H8W . . 114(4) ?
H9W O9 H10W . . 115(5) ?
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 O5 . 2.079(3) ?
Fe1 O3 . 2.097(3) ?
Fe1 O1 . 2.105(2) ?
Fe1 O2 4_565 2.105(2) ?
Fe1 N2 . 2.139(3) ?
Fe1 N1 3_545 2.144(3) ?
C1 O1 . 1.247(4) ?
C1 O2 . 1.243(4) ?
C1 H1 . 0.9300 ?
C2 O4 . 1.218(5) ?
C2 O3 . 1.257(4) ?
C2 H2 . 0.9300 ?
C3 N2 . 1.330(4) ?
C3 C4 . 1.381(5) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.384(5) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.388(5) ?
C5 C8 . 1.486(4) ?
C6 C7 . 1.380(5) ?
C6 H6 . 0.9300 ?
C7 N2 . 1.338(4) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.390(5) ?
C8 C11 . 1.390(5) ?
C9 C10 . 1.378(5) ?
C9 H9 . 0.9300 ?
C10 N1 . 1.334(4) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.378(5) ?
C11 H11 . 0.9300 ?
C12 N1 . 1.333(5) ?
C12 H12 . 0.9300 ?
N1 Fe1 3_455 2.144(3) ?
O2 Fe1 4_464 2.105(2) ?
O5 H1W . 0.82(4) ?
O5 H2W . 0.82(3) ?
O6 H3W . 0.82(4) ?
O6 H4W . 0.82(3) ?
O7 H5W . 0.82(5) ?
O7 H6W . 0.82(3) ?
O8 H7W . 0.82(3) ?
O8 H8W . 0.82(3) ?
O9 H9W . 0.82(4) ?
O9 H10W . 0.82(4) ?
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
O5 H1W O4 1_556 0.82(4) 1.97(4) 2.693(4) 146(6)
O6 H3W O3 4_465 0.82(4) 1.98(4) 2.792(4) 173(4)
O6 H4W O9 2_565 0.82(3) 1.93(3) 2.753(4) 175(5)
O7 H5W O8 2_564 0.82(5) 2.22(5) 3.028(9) 171(4)
O7 H6W O4 4_465 0.82(3) 2.46(3) 3.117(7) 137(4)
O9 H10W O1 2_565 0.82(4) 2.16(4) 2.954(4) 165(5)
O7 H6W O2 . 0.82(3) 2.61(5) 3.158(5) 125(5)
O8 H7W O7 . 0.82(3) 1.94(3) 2.763(7) 174(5)
O8 H8W O6 . 0.82(3) 2.031(19) 2.797(5) 155(4)
O9 H9W O8 . 0.82(4) 1.99(4) 2.779(5) 163(5)
O5 H2W O6 . 0.82(3) 1.94(4) 2.729(4) 161(4)
