#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/79/2217918.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_2217918
loop_
_publ_author_name
'Song, Wen-Dong'
'Yan, Jian-Bin'
'Ji, Li-Li'
'Wang, Hao'
_publ_section_title
;
 Poly[[(μ₄-5-aminoisophthalato)aquairon(II)] dihydrate]
;
_journal_coeditor_code           GK2125
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m549
_journal_paper_doi               10.1107/S1600536808006326
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Fe (C8 H5 N O4) (H2 O)], 2H2 O'
_chemical_formula_moiety         'C8 H7 Fe N O5, 2(H2 O)'
_chemical_formula_sum            'C8 H11 Fe N O7'
_chemical_formula_weight         289.03
_chemical_name_systematic
;
Poly[[(μ₄-5-Aminoisophthalato)aquairon(II)] dihydrate]
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.5600(10)
_cell_angle_beta                 76.0580(10)
_cell_angle_gamma                66.6100(10)
_cell_formula_units_Z            2
_cell_length_a                   7.7418(2)
_cell_length_b                   8.5972(2)
_cell_length_c                   8.6938(2)
_cell_measurement_reflns_used    1800
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.36
_cell_volume                     515.34(2)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII 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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5025
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.7859
_exptl_absorpt_correction_T_min  0.7550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.567
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2009
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0303
_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)+(0.0536P)²+0.5412P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                1895
_reflns_number_total             2009
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gk2125.cif
_cod_data_source_block           I
_cod_database_code               2217918
_cod_database_fobs_code          2217918
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C C1 0.2799(3) 0.8073(3) 0.9011(2) 0.0165(4) Uani d . 1
C C2 0.4454(3) 0.7019(3) 0.7727(2) 0.0161(4) Uani d . 1
C C3 0.5442(3) 0.7791(3) 0.6593(2) 0.0172(4) Uani d . 1
H H3 0.5097 0.8957 0.6633 0.021 Uiso calc R 1
C C4 0.6955(3) 0.6798(3) 0.5397(2) 0.0168(4) Uani d . 1
C C5 0.7464(3) 0.5058(3) 0.5320(2) 0.0178(4) Uani d . 1
H H5 0.8434 0.4414 0.4487 0.021 Uiso calc R 1
C C6 0.6522(3) 0.4277(3) 0.6494(2) 0.0167(4) Uani d . 1
C C7 0.5018(3) 0.5267(3) 0.7692(2) 0.0178(4) Uani d . 1
H H7 0.4382 0.4755 0.8476 0.021 Uiso calc R 1
C C8 0.8096(3) 0.7607(3) 0.4223(2) 0.0178(4) Uani d . 1
Fe Fe1 0.02840(4) 0.88499(4) 1.21504(3) 0.01967(14) Uani d . 1
N N1 0.7168(3) 0.2480(2) 0.6517(2) 0.0204(4) Uani d . 1
H H1A 0.7573 0.2077 0.5513 0.025 Uiso calc R 1
H H1B 0.6164 0.2203 0.6995 0.025 Uiso calc R 1
O O1 0.2198(2) 0.7325(2) 1.01815(18) 0.0251(4) Uani d . 1
O O2 0.2094(2) 0.96615(19) 0.88749(19) 0.0208(3) Uani d . 1
O O3 0.8199(3) 0.8942(2) 0.46223(19) 0.0243(4) Uani d . 1
O O4 0.8971(2) 0.6932(2) 0.28758(18) 0.0252(4) Uani d . 1
O O1W 0.0523(3) 1.1127(2) 1.2728(2) 0.0341(4) Uani d D 1
H H1W 0.112(5) 1.105(4) 1.340(3) 0.051 Uiso d D 1
H H2W 0.065(5) 1.189(3) 1.217(3) 0.051 Uiso d D 1
O O2W 0.0978(4) 0.3865(3) 0.1118(3) 0.0480(6) Uani d D 1
H H4W 0.074(5) 0.464(4) 0.177(4) 0.072 Uiso d D 1
H H3W -0.001(3) 0.401(3) 0.078(3) 0.072 Uiso d D 1
O O3W 0.4365(3) 0.1532(3) 0.9066(3) 0.0482(6) Uani d D 1
H H5W 0.376(5) 0.110(5) 0.867(5) 0.072 Uiso d D 1
H H6W 0.360(4) 0.231(4) 0.972(4) 0.072 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
O1 C1 O2 . . 123.12(19)
O1 C1 C2 . . 118.08(19)
O2 C1 C2 . . 118.80(18)
C3 C2 C7 . . 120.2(2)
C3 C2 C1 . . 119.97(19)
C7 C2 C1 . . 119.81(19)
C2 C3 C4 . . 119.2(2)
C2 C3 H3 . . 120.4
C4 C3 H3 . . 120.4
C5 C4 C3 . . 120.64(19)
C5 C4 C8 . . 119.82(19)
C3 C4 C8 . . 119.5(2)
C4 C5 C6 . . 120.03(19)
C4 C5 H5 . . 120.0
C6 C5 H5 . . 120.0
C7 C6 C5 . . 119.3(2)
C7 C6 N1 . . 120.25(19)
C5 C6 N1 . . 120.36(19)
C6 C7 C2 . . 120.5(2)
C6 C7 H7 . . 119.7
C2 C7 H7 . . 119.7
O4 C8 O3 . . 120.90(19)
O4 C8 C4 . . 119.9(2)
O3 C8 C4 . . 119.15(19)
O1 Fe1 O2 . 2_577 100.34(7)
O1 Fe1 O1W . . 120.69(8)
O2 Fe1 O1W 2_577 . 89.59(7)
O1 Fe1 O4 . 1_456 90.79(6)
O2 Fe1 O4 2_577 1_456 89.97(6)
O1W Fe1 O4 . 1_456 148.03(7)
O1 Fe1 O3 . 1_456 145.97(6)
O2 Fe1 O3 2_577 1_456 91.37(6)
O1W Fe1 O3 . 1_456 90.96(7)
O4 Fe1 O3 1_456 1_456 57.10(6)
O1 Fe1 N1 . 2_667 85.72(7)
O2 Fe1 N1 2_577 2_667 172.50(6)
O1W Fe1 N1 . 2_667 83.48(7)
O4 Fe1 N1 1_456 2_667 94.39(7)
O3 Fe1 N1 1_456 2_667 85.91(6)
C6 N1 Fe1 . 2_667 113.51(14)
C6 N1 H1A . . 108.9
Fe1 N1 H1A 2_667 . 108.9
C6 N1 H1B . . 108.9
Fe1 N1 H1B 2_667 . 108.9
H1A N1 H1B . . 107.7
C1 O1 Fe1 . . 116.73(14)
C1 O2 Fe1 . 2_577 127.68(14)
C8 O3 Fe1 . 1_654 88.55(12)
C8 O4 Fe1 . 1_654 93.43(13)
Fe1 O1W H1W . . 116(2)
Fe1 O1W H2W . . 130(2)
H1W O1W H2W . . 105.6(16)
H4W O2W H3W . . 110.9(17)
H5W O3W H6W . . 111.2(18)
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
C1 O1 . 1.254(3) ?
C1 O2 . 1.262(3) ?
C1 C2 . 1.502(3) ?
C2 C3 . 1.392(3) ?
C2 C7 . 1.393(3) ?
C3 C4 . 1.392(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.390(3) ?
C4 C8 . 1.499(3) ?
C5 C6 . 1.396(3) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.390(3) ?
C6 N1 . 1.422(3) ?
C7 H7 . 0.9300 ?
C8 O4 . 1.256(3) ?
C8 O3 . 1.262(3) ?
Fe1 O1 . 2.1040(16) y
Fe1 O2 2_577 2.1364(16) y
Fe1 O1W . 2.1458(17) y
Fe1 O4 1_456 2.2387(17) y
Fe1 O3 1_456 2.3416(16) y
Fe1 N1 2_667 2.376(2) y
N1 H1A . 0.9000 ?
N1 H1B . 0.9000 ?
O1W H1W . 0.815(10) ?
O1W H2W . 0.809(9) ?
O2W H4W . 0.842(10) ?
O2W H3W . 0.844(10) ?
O3W H5W . 0.843(10) ?
O3W H6W . 0.840(10) ?
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
O2W H3W O2W 2_565 0.844(10) 2.377(9) 2.892(5) 119.9(9)
O3W H5W O2 1_545 0.843(10) 2.09(2) 2.852(3) 151(4)
O3W H6W O2W 1_556 0.840(10) 2.071(19) 2.865(3) 157(3)
O2W H4W O4 1_455 0.842(10) 2.05(2) 2.816(3) 151(3)
O1W H2W O2W 1_566 0.809(9) 1.943(12) 2.745(3) 171(3)
O1W H1W O3 2_677 0.815(10) 1.914(14) 2.705(3) 163(4)
N1 H1B O3W . 0.90 2.19 3.015(3) 153
