#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/51/2015146.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_2015146
loop_
_publ_author_name
'Zun-Ting Zhang'
'Xin-Li Cheng'
_publ_section_title
;
 Hydrogen bonding and π--π stacking in hexaaquairon(II)
 bis(4',7-dimethoxyisoflavone-3'-sulfonate) octahydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m529
_journal_page_last               m531
_journal_paper_doi               10.1107/S0108270105036218
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe (H2 O)6] (C17 H13 O7 S)2 , 8H2 O'
_chemical_formula_moiety         'Fe H12 O6 2+ , 2C17 H13 O7 S - , 8H2 O'
_chemical_formula_sum            'C34 H54 Fe O28 S2'
_chemical_formula_weight         1030.74
_chemical_name_systematic
;
Hexaaquairon(II) bis(4',7-dimethoxyisoflavone-3'-sulfonate) octahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.552(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.892(7)
_cell_length_b                   7.336(3)
_cell_length_c                   18.357(7)
_cell_measurement_reflns_used    2854
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.587
_cell_measurement_theta_min      2.411
_cell_volume                     2275.8(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11468
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  0.9218
_exptl_absorpt_correction_T_min  0.7967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0418
_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)+(0.0498P)²+0.9561P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                2643
_reflns_number_total             4000
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ga1112.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      'P 21/c'
_cod_database_code               2015146
_cod_database_fobs_code          2015146
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_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
_atom_site_type_symbol
O1 0.55831(12) 0.1756(3) 0.89512(12) 0.0455(6) Uani d . 1 . . O
O2 0.32825(13) 0.2899(4) 0.83678(13) 0.0590(7) Uani d . 1 . . O
O3 0.63099(14) 0.2406(3) 1.17776(13) 0.0585(7) Uani d . 1 . . O
O4 0.20929(13) 0.2127(3) 0.45852(12) 0.0460(6) Uani d . 1 . . O
O5 0.22848(14) 0.6887(3) 0.60148(13) 0.0558(7) Uani d . 1 . . O
O6 0.12787(13) 0.4958(3) 0.50765(15) 0.0575(7) Uani d . 1 . . O
O7 0.22723(14) 0.6130(3) 0.47266(13) 0.0536(6) Uani d . 1 . . O
O11 0.18072(15) 0.1818(3) 0.72658(15) 0.0556(7) Uani d . 1 . . O
O12 0.10666(18) 0.4873(5) 0.30998(17) 0.0711(9) Uani d . 1 . . O
S1 0.20970(5) 0.55516(11) 0.53763(5) 0.0383(2) Uani d . 1 . . S
C1 0.50141(18) 0.1791(5) 0.81726(18) 0.0438(8) Uani d . 1 . . C
H1 0.5168 0.1509 0.7770 0.053 Uiso calc R 1 . . H
C2 0.42489(17) 0.2193(4) 0.79258(18) 0.0357(7) Uani d . 1 . . C
C3 0.39813(18) 0.2578(4) 0.85406(18) 0.0392(8) Uani d . 1 . . C
C4 0.45915(17) 0.2521(4) 0.93798(17) 0.0352(7) Uani d . 1 . . C
C5 0.44210(19) 0.2841(5) 1.00360(19) 0.0490(9) Uani d . 1 . . C
H5 0.3904 0.3091 0.9939 0.059 Uiso calc R 1 . . H
C6 0.5004(2) 0.2792(5) 1.0815(2) 0.0522(9) Uani d . 1 . . C
H6 0.4882 0.3012 1.1245 0.063 Uiso calc R 1 . . H
C7 0.57855(19) 0.2414(4) 1.09754(19) 0.0430(8) Uani d . 1 . . C
C8 0.59740(18) 0.2068(4) 1.03452(18) 0.0409(8) Uani d . 1 . . C
H8 0.6491 0.1805 1.0445 0.049 Uiso calc R 1 . . H
C9 0.53676(18) 0.2123(4) 0.95578(18) 0.0361(7) Uani d . 1 . . C
C10 0.36767(17) 0.2146(4) 0.70502(17) 0.0337(7) Uani d . 1 . . C
C11 0.32168(16) 0.3664(4) 0.66634(17) 0.0343(7) Uani d . 1 . . C
H11 0.3264 0.4720 0.6962 0.041 Uiso calc R 1 . . H
C12 0.26918(16) 0.3625(4) 0.58447(17) 0.0306(7) Uani d . 1 . . C
C13 0.26148(17) 0.2054(4) 0.53842(18) 0.0332(7) Uani d . 1 . . C
C14 0.30607(18) 0.0535(4) 0.57656(18) 0.0388(8) Uani d . 1 . . C
H14 0.3013 -0.0525 0.5469 0.047 Uiso calc R 1 . . H
C15 0.35776(18) 0.0590(4) 0.65871(18) 0.0390(8) Uani d . 1 . . C
H15 0.3867 -0.0448 0.6836 0.047 Uiso calc R 1 . . H
C16 0.7118(2) 0.2118(6) 1.1984(2) 0.0683(12) Uani d . 1 . . C
H16A 0.7423 0.2146 1.2565 0.102 Uiso calc R 1 . . H
H16B 0.7300 0.3060 1.1745 0.102 Uiso calc R 1 . . H
H16C 0.7180 0.0953 1.1781 0.102 Uiso calc R 1 . . H
C17 0.1978(2) 0.0536(5) 0.4097(2) 0.0592(10) Uani d . 1 . . C
H17A 0.1596 0.0790 0.3547 0.089 Uiso calc R 1 . . H
H17B 0.1789 -0.0442 0.4311 0.089 Uiso calc R 1 . . H
H17C 0.2471 0.0191 0.4103 0.089 Uiso calc R 1 . . H
H25 0.230(2) 0.202(5) 0.758(2) 0.080 Uiso d . 1 . . H
H26 0.156(2) 0.272(6) 0.706(2) 0.080 Uiso d . 1 . . H
H27 0.134(2) 0.433(6) 0.288(2) 0.080 Uiso d . 1 . . H
H28 0.135(3) 0.500(6) 0.353(3) 0.080 Uiso d . 1 . . H
Fe1 0.0000 1.0000 0.5000 0.0421(2) Uani d SU 1 . . Fe
O8 -0.04029(18) 0.8245(5) 0.55955(18) 0.0792(10) Uani d DU 1 . . O
O10 0.11841(14) 0.9613(4) 0.59238(16) 0.0578(7) Uani d U 1 . . O
H19 -0.072(2) 0.743(5) 0.540(2) 0.080 Uiso d D 1 . . H
H20 -0.027(3) 0.817(6) 0.605(2) 0.080 Uiso d . 1 . . H
H23 0.142(2) 1.027(5) 0.634(2) 0.080 Uiso d . 1 . . H
H24 0.153(2) 0.883(6) 0.591(2) 0.080 Uiso d . 1 . . H
O9 0.01432(17) 0.7765(4) 0.43155(19) 0.0781(10) Uani d U 1 . . O
H21 0.053(2) 0.712(6) 0.452(2) 0.080 Uiso d . 1 . . H
H22 -0.020(2) 0.708(6) 0.416(3) 0.080 Uiso d . 1 . . H
O13 0.1013(2) 0.4825(5) 0.6551(2) 0.0801(10) Uani d . 1 . . O
H29 0.087(2) 0.590(5) 0.678(2) 0.080 Uiso d . 1 . . H
H30 0.112(3) 0.523(6) 0.626(3) 0.080 Uiso d . 1 . . H
O14 0.0310(2) 0.7164(5) 0.7174(2) 0.0861(10) Uani d . 1 . . O
H31 0.061(2) 0.797(6) 0.762(2) 0.080 Uiso d . 1 . . H
H32 -0.005(2) 0.658(6) 0.729(2) 0.080 Uiso d . 1 . . H
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'
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'
S S 0.1246 0.1234 '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
C1 O1 C9 . . 118.1(2)
C7 O3 C16 . . 117.8(3)
C13 O4 C17 . . 118.7(2)
H25 O11 H26 . . 114(4)
H27 O12 H28 . . 104(5)
O7 S1 O5 . . 114.14(15)
O7 S1 O6 . . 111.97(15)
O5 S1 O6 . . 110.10(15)
O7 S1 C12 . . 107.89(13)
O5 S1 C12 . . 105.95(13)
O6 S1 C12 . . 106.29(13)
C2 C1 O1 . . 126.1(3)
C2 C1 H1 . . 116.9
O1 C1 H1 . . 116.9
C1 C2 C3 . . 118.4(3)
C1 C2 C10 . . 121.0(3)
C3 C2 C10 . . 120.5(3)
O2 C3 C4 . . 121.8(3)
O2 C3 C2 . . 122.7(3)
C4 C3 C2 . . 115.5(3)
C9 C4 C5 . . 117.4(3)
C9 C4 C3 . . 120.7(3)
C5 C4 C3 . . 121.9(3)
C6 C5 C4 . . 120.7(3)
C6 C5 H5 . . 119.7
C4 C5 H5 . . 119.7
C5 C6 C7 . . 120.6(3)
C5 C6 H6 . . 119.7
C7 C6 H6 . . 119.7
O3 C7 C8 . . 124.9(3)
O3 C7 C6 . . 114.8(3)
C8 C7 C6 . . 120.3(3)
C7 C8 C9 . . 117.8(3)
C7 C8 H8 . . 121.1
C9 C8 H8 . . 121.1
O1 C9 C4 . . 121.1(3)
O1 C9 C8 . . 115.7(3)
C4 C9 C8 . . 123.2(3)
C15 C10 C11 . . 117.6(3)
C15 C10 C2 . . 121.1(3)
C11 C10 C2 . . 121.3(3)
C12 C11 C10 . . 121.2(3)
C12 C11 H11 . . 119.4
C10 C11 H11 . . 119.4
C11 C12 C13 . . 120.3(3)
C11 C12 S1 . . 120.2(2)
C13 C12 S1 . . 119.5(2)
O4 C13 C14 . . 124.3(3)
O4 C13 C12 . . 116.8(2)
C14 C13 C12 . . 118.9(3)
C15 C14 C13 . . 120.1(3)
C15 C14 H14 . . 119.9
C13 C14 H14 . . 119.9
C14 C15 C10 . . 122.0(3)
C14 C15 H15 . . 119.0
C10 C15 H15 . . 119.0
O3 C16 H16A . . 109.5
O3 C16 H16B . . 109.5
H16A C16 H16B . . 109.5
O3 C16 H16C . . 109.5
H16A C16 H16C . . 109.5
H16B C16 H16C . . 109.5
O4 C17 H17A . . 109.5
O4 C17 H17B . . 109.5
H17A C17 H17B . . 109.5
O4 C17 H17C . . 109.5
H17A C17 H17C . . 109.5
H17B C17 H17C . . 109.5
O8 Fe1 O8 3_576 . 180.0000(10)
O8 Fe1 O10 3_576 . 90.02(12)
O8 Fe1 O10 . . 89.98(12)
O8 Fe1 O10 3_576 3_576 89.98(12)
O8 Fe1 O10 . 3_576 90.02(12)
O10 Fe1 O10 . 3_576 180.0000(10)
O8 Fe1 O9 3_576 3_576 90.37(15)
O8 Fe1 O9 . 3_576 89.63(15)
O10 Fe1 O9 . 3_576 89.90(10)
O10 Fe1 O9 3_576 3_576 90.10(10)
O8 Fe1 O9 3_576 . 89.63(15)
O8 Fe1 O9 . . 90.37(15)
O10 Fe1 O9 . . 90.10(10)
O10 Fe1 O9 3_576 . 89.90(10)
O9 Fe1 O9 3_576 . 180.0000(10)
Fe1 O8 H19 . . 127(3)
Fe1 O8 H20 . . 128(4)
H19 O8 H20 . . 105(5)
Fe1 O10 H23 . . 126(3)
Fe1 O10 H24 . . 127(2)
H23 O10 H24 . . 107(4)
Fe1 O9 H21 . . 120(3)
Fe1 O9 H22 . . 114(3)
H21 O9 H22 . . 104(4)
H29 O13 H30 . . 103(5)
H31 O14 H32 . . 108(4)
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
O1 C1 . 1.351(3) ?
O1 C9 . 1.372(3) ?
O2 C3 . 1.235(3) ?
O3 C7 . 1.359(4) ?
O3 C16 . 1.416(4) ?
O4 C13 . 1.354(3) ?
O4 C17 . 1.428(4) ?
O5 S1 . 1.445(2) ?
O6 S1 . 1.457(2) ?
O7 S1 . 1.437(2) ?
O11 H25 . 0.87(4) ?
O11 H26 . 0.80(4) ?
O12 H27 . 0.87(4) ?
O12 H28 . 0.73(4) ?
S1 C12 . 1.771(3) ?
C1 C2 . 1.340(4) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.456(4) ?
C2 C10 . 1.483(4) ?
C3 C4 . 1.455(4) ?
C4 C9 . 1.383(4) ?
C4 C5 . 1.399(4) ?
C5 C6 . 1.361(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.397(5) ?
C6 H6 . 0.9300 ?
C7 C8 . 1.378(4) ?
C8 C9 . 1.387(4) ?
C8 H8 . 0.9300 ?
C10 C15 . 1.385(4) ?
C10 C11 . 1.395(4) ?
C11 C12 . 1.382(4) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.398(4) ?
C13 C14 . 1.383(4) ?
C14 C15 . 1.383(4) ?
C14 H14 . 0.9300 ?
C15 H15 . 0.9300 ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 0.9600 ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C17 H17C . 0.9600 ?
Fe1 O8 3_576 2.043(3) ?
Fe1 O8 . 2.043(3) ?
Fe1 O10 . 2.138(2) ?
Fe1 O10 3_576 2.138(2) ?
Fe1 O9 3_576 2.155(3) ?
Fe1 O9 . 2.155(3) ?
O8 H19 . 0.80(2) ?
O8 H20 . 0.76(4) ?
O10 H23 . 0.84(4) ?
O10 H24 . 0.88(4) ?
O9 H21 . 0.81(4) ?
O9 H22 . 0.77(4) ?
O13 H29 . 0.99(4) ?
O13 H30 . 0.72(4) ?
O14 H31 . 0.97(4) ?
O14 H32 . 0.90(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
O11 H25 O2 . 0.87(4) 1.88(4) 2.729(3) 166(4)
O11 H26 O13 . 0.80(4) 1.86(4) 2.661(4) 178(5)
O12 H27 O11 4_565 0.87(4) 1.92(4) 2.785(4) 172(4)
O12 H28 O7 . 0.73(4) 2.27(4) 2.979(4) 165(5)
O8 H19 O6 3_566 0.80(2) 2.03(3) 2.820(4) 166(4)
O8 H20 O14 . 0.76(4) 1.99(4) 2.711(4) 157(5)
O9 H21 O6 . 0.81(4) 2.06(4) 2.849(3) 162(4)
O9 H22 O13 3_566 0.77(4) 2.05(4) 2.794(5) 161(5)
O10 H23 O11 1_565 0.84(4) 1.90(4) 2.735(4) 172(4)
O10 H24 O5 . 0.88(4) 1.96(4) 2.836(3) 172(4)
O13 H29 O14 . 0.99(4) 1.78(4) 2.716(5) 156(3)
O13 H30 O6 . 0.72(4) 2.33(4) 2.966(4) 149(5)
O14 H31 O12 4_576 0.97(4) 1.83(4) 2.736(4) 156(3)
O14 H32 O12 3_566 0.90(4) 2.03(4) 2.843(5) 149(4)
C8 H8 O7 2_646 0.93 2.54 3.444(5) 164
C16 H16A O5 3_667 0.96 2.51 3.405(4) 155
