#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/04/2220424.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_2220424
loop_
_publ_author_name
'Cheng, Lin'
'Zhang, Ya-Wen'
'Sun, Yan-Yan'
'Wang, Jian-Quan'
_publ_section_title
catena-Poly[bis[(1,10-phenanthroline)iron(II)]-bis(μ-5-carboxybenzene-1,3-dicarboxylato)]
_journal_coeditor_code           BT2819
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m14
_journal_paper_doi               10.1107/S160053680804018X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Fe (C9 H4 O6) (C12 H8 N2) (H2 O)]'
_chemical_formula_moiety         'C21 H14 Fe N2 O7'
_chemical_formula_sum            'C21 H14 Fe N2 O7'
_chemical_formula_weight         462.19
_chemical_name_systematic
;catena-Poly[bis[(1,10-phenanthroline)iron(II)]-bis(μ-5-carboxybenzene-
1,3-dicarboxylato)]
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                96.221(3)
_cell_angle_beta                 111.320(2)
_cell_angle_gamma                111.736(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5925(15)
_cell_length_b                   10.8971(16)
_cell_length_c                   11.1998(17)
_cell_measurement_reflns_used    785
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.45
_cell_volume                     972.3(3)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX CCD'
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7689
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  0.8658
_exptl_absorpt_correction_T_min  0.8205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.215
_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     292
_refine_ls_number_reflns         3798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0412
_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)+(0.0467P)²+0.209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                3228
_reflns_number_total             3798
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt2819.cif
_cod_data_source_block           I
_cod_database_code               2220424
_cod_database_fobs_code          2220424
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.61551(4) 0.98060(3) 0.64542(3) 0.02290(12) Uani d . 1 . .
C C1 0.4072(3) 0.4212(2) 0.3242(2) 0.0203(5) Uani d . 1 . .
C C2 0.5643(3) 0.4812(2) 0.3283(2) 0.0238(5) Uani d . 1 . .
H H2A 0.6162 0.4266 0.3174 0.029 Uiso calc R 1 . .
C C3 0.6454(3) 0.6223(2) 0.3487(2) 0.0240(5) Uani d . 1 . .
C C4 0.5696(3) 0.7048(2) 0.3685(2) 0.0239(5) Uani d . 1 . .
H H4A 0.6239 0.7994 0.3829 0.029 Uiso calc R 1 . .
C C5 0.4132(3) 0.6459(2) 0.3669(2) 0.0202(5) Uani d . 1 . .
C C6 0.3329(3) 0.5041(2) 0.3441(2) 0.0218(5) Uani d . 1 . .
H H6A 0.2277 0.4643 0.3421 0.026 Uiso calc R 1 . .
C C7 0.3235(3) 0.2700(2) 0.3103(2) 0.0244(5) Uani d . 1 . .
C C8 0.8159(3) 0.6886(3) 0.3565(3) 0.0320(6) Uani d . 1 . .
C C9 0.3293(3) 0.7313(2) 0.3927(2) 0.0234(5) Uani d . 1 . .
C C10 0.2781(3) 0.8910(3) 0.6674(3) 0.0393(7) Uani d . 1 . .
H H10A 0.2341 0.8235 0.5880 0.047 Uiso calc R 1 . .
C C11 0.1720(4) 0.8963(4) 0.7242(4) 0.0556(9) Uani d . 1 . .
H H11A 0.0602 0.8326 0.6841 0.067 Uiso calc R 1 . .
C C12 0.2347(5) 0.9959(4) 0.8387(4) 0.0585(10) Uani d . 1 . .
H H12A 0.1653 1.0011 0.8773 0.070 Uiso calc R 1 . .
C C13 0.4026(4) 1.0903(3) 0.8989(3) 0.0491(8) Uani d . 1 . .
C C14 0.4804(6) 1.1991(5) 1.0193(4) 0.0739(12) Uani d . 1 . .
H H14A 0.4165 1.2100 1.0615 0.089 Uiso calc R 1 . .
C C15 0.6433(6) 1.2854(4) 1.0726(4) 0.0753(12) Uani d . 1 . .
H H15A 0.6891 1.3571 1.1492 0.090 Uiso calc R 1 . .
C C16 0.7479(5) 1.2701(3) 1.0150(3) 0.0525(9) Uani d . 1 . .
C C17 0.9206(5) 1.3534(4) 1.0703(3) 0.0640(10) Uani d . 1 . .
H H17A 0.9726 1.4269 1.1465 0.077 Uiso calc R 1 . .
C C18 1.0113(4) 1.3257(4) 1.0116(3) 0.0648(10) Uani d . 1 . .
H H18A 1.1262 1.3788 1.0487 0.078 Uiso calc R 1 . .
C C19 0.9317(4) 1.2178(3) 0.8961(3) 0.0461(7) Uani d . 1 . .
H H19A 0.9955 1.2009 0.8568 0.055 Uiso calc R 1 . .
C C20 0.6769(4) 1.1637(3) 0.8977(3) 0.0349(6) Uani d . 1 . .
C C21 0.5017(4) 1.0749(3) 0.8375(3) 0.0340(6) Uani d . 1 . .
N N1 0.4379(3) 0.9776(2) 0.7216(2) 0.0291(5) Uani d . 1 . .
N N2 0.7682(3) 1.1375(2) 0.8391(2) 0.0322(5) Uani d . 1 . .
O O1 0.1824(2) 0.22146(18) 0.3066(2) 0.0449(5) Uani d . 1 . .
O O2 0.4051(2) 0.20291(16) 0.30592(18) 0.0295(4) Uani d . 1 . .
O O3 0.8788(3) 0.6020(2) 0.3450(3) 0.0548(7) Uani d . 1 . .
O O4 0.8901(2) 0.8094(2) 0.3733(3) 0.0625(7) Uani d . 1 . .
O O5 0.42061(19) 0.86215(15) 0.44513(16) 0.0249(4) Uani d . 1 . .
O O6 0.1789(2) 0.67369(18) 0.3605(2) 0.0378(5) Uani d . 1 . .
O O1W 0.8228(2) 0.9974(2) 0.6184(2) 0.0413(5) Uani d . 1 . .
H H1WA 0.847(4) 0.935(4) 0.648(4) 0.073(12) Uiso d . 1 . .
H H1WB 0.902(4) 1.053(4) 0.613(3) 0.065(12) Uiso d . 1 . .
H H3A 0.971(5) 0.642(4) 0.353(4) 0.093(15) Uiso 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
O1W Fe1 O2 . 2_666 89.06(7) ?
O1W Fe1 O5 . 2_676 96.92(7) ?
O2 Fe1 O5 2_666 2_676 166.10(7) ?
O1W Fe1 N1 . . 166.83(9) ?
O2 Fe1 N1 2_666 . 87.61(7) ?
O5 Fe1 N1 2_676 . 89.21(7) ?
O1W Fe1 O5 . . 100.00(8) ?
O2 Fe1 O5 2_666 . 89.38(6) ?
O5 Fe1 O5 2_676 . 77.25(6) ?
N1 Fe1 O5 . . 92.70(7) ?
O1W Fe1 N2 . . 92.32(9) ?
O2 Fe1 N2 2_666 . 103.69(7) ?
O5 Fe1 N2 2_676 . 88.65(7) ?
N1 Fe1 N2 . . 76.12(8) ?
O5 Fe1 N2 . . 162.22(7) ?
C2 C1 C6 . . 119.2(2) ?
C2 C1 C7 . . 120.7(2) ?
C6 C1 C7 . . 119.9(2) ?
C1 C2 C3 . . 120.6(2) ?
C1 C2 H2A . . 119.7 ?
C3 C2 H2A . . 119.7 ?
C2 C3 C4 . . 119.7(2) ?
C2 C3 C8 . . 121.2(2) ?
C4 C3 C8 . . 119.0(2) ?
C5 C4 C3 . . 120.1(2) ?
C5 C4 H4A . . 120.0 ?
C3 C4 H4A . . 120.0 ?
C4 C5 C6 . . 119.3(2) ?
C4 C5 C9 . . 122.0(2) ?
C6 C5 C9 . . 118.73(19) ?
C1 C6 C5 . . 121.0(2) ?
C1 C6 H6A . . 119.5 ?
C5 C6 H6A . . 119.5 ?
O1 C7 O2 . . 125.2(2) ?
O1 C7 C1 . . 118.0(2) ?
O2 C7 C1 . . 116.7(2) ?
O4 C8 O3 . . 122.9(2) ?
O4 C8 C3 . . 123.5(2) ?
O3 C8 C3 . . 113.5(2) ?
O6 C9 O5 . . 124.0(2) ?
O6 C9 C5 . . 118.6(2) ?
O5 C9 C5 . . 117.3(2) ?
N1 C10 C11 . . 122.7(3) ?
N1 C10 H10A . . 118.6 ?
C11 C10 H10A . . 118.6 ?
C12 C11 C10 . . 118.9(3) ?
C12 C11 H11A . . 120.5 ?
C10 C11 H11A . . 120.5 ?
C11 C12 C13 . . 120.3(3) ?
C11 C12 H12A . . 119.9 ?
C13 C12 H12A . . 119.9 ?
C12 C13 C21 . . 117.1(3) ?
C12 C13 C14 . . 124.5(3) ?
C21 C13 C14 . . 118.4(3) ?
C15 C14 C13 . . 121.4(3) ?
C15 C14 H14A . . 119.3 ?
C13 C14 H14A . . 119.3 ?
C14 C15 C16 . . 121.6(3) ?
C14 C15 H15A . . 119.2 ?
C16 C15 H15A . . 119.2 ?
C20 C16 C17 . . 117.3(3) ?
C20 C16 C15 . . 118.8(3) ?
C17 C16 C15 . . 123.9(3) ?
C18 C17 C16 . . 119.4(3) ?
C18 C17 H17A . . 120.3 ?
C16 C17 H17A . . 120.3 ?
C17 C18 C19 . . 119.7(3) ?
C17 C18 H18A . . 120.1 ?
C19 C18 H18A . . 120.1 ?
N2 C19 C18 . . 122.9(3) ?
N2 C19 H19A . . 118.5 ?
C18 C19 H19A . . 118.5 ?
N2 C20 C16 . . 122.8(3) ?
N2 C20 C21 . . 117.4(2) ?
C16 C20 C21 . . 119.8(3) ?
N1 C21 C13 . . 122.4(3) ?
N1 C21 C20 . . 117.5(2) ?
C13 C21 C20 . . 120.1(3) ?
C10 N1 C21 . . 118.4(2) ?
C10 N1 Fe1 . . 126.62(19) ?
C21 N1 Fe1 . . 114.93(17) ?
C19 N2 C20 . . 117.7(2) ?
C19 N2 Fe1 . . 128.4(2) ?
C20 N2 Fe1 . . 113.40(17) ?
C7 O2 Fe1 . 2_666 129.65(15) ?
C8 O3 H3A . . 110(3) ?
C9 O5 Fe1 . 2_676 125.52(15) ?
C9 O5 Fe1 . . 131.19(15) ?
Fe1 O5 Fe1 2_676 . 102.75(6) ?
Fe1 O1W H1WA . . 106(2) ?
Fe1 O1W H1WB . . 141(2) ?
H1WA O1W H1WB . . 109(3) ?
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 O1W . 2.063(2) ?
Fe1 O2 2_666 2.0873(16) ?
Fe1 O5 2_676 2.1554(15) ?
Fe1 N1 . 2.157(2) ?
Fe1 O5 . 2.1746(17) ?
Fe1 N2 . 2.192(2) ?
C1 C2 . 1.384(3) ?
C1 C6 . 1.387(3) ?
C1 C7 . 1.502(3) ?
C2 C3 . 1.390(3) ?
C2 H2A . 0.9300 ?
C3 C4 . 1.395(3) ?
C3 C8 . 1.487(3) ?
C4 C5 . 1.388(3) ?
C4 H4A . 0.9300 ?
C5 C6 . 1.392(3) ?
C5 C9 . 1.504(3) ?
C6 H6A . 0.9300 ?
C7 O1 . 1.240(3) ?
C7 O2 . 1.262(3) ?
C8 O4 . 1.196(3) ?
C8 O3 . 1.312(3) ?
C9 O6 . 1.228(3) ?
C9 O5 . 1.290(3) ?
C10 N1 . 1.318(3) ?
C10 C11 . 1.396(4) ?
C10 H10A . 0.9300 ?
C11 C12 . 1.356(5) ?
C11 H11A . 0.9300 ?
C12 C13 . 1.393(5) ?
C12 H12A . 0.9300 ?
C13 C21 . 1.404(4) ?
C13 C14 . 1.431(5) ?
C14 C15 . 1.339(5) ?
C14 H14A . 0.9300 ?
C15 C16 . 1.423(5) ?
C15 H15A . 0.9300 ?
C16 C20 . 1.402(4) ?
C16 C17 . 1.404(5) ?
C17 C18 . 1.358(5) ?
C17 H17A . 0.9300 ?
C18 C19 . 1.388(4) ?
C18 H18A . 0.9300 ?
C19 N2 . 1.329(3) ?
C19 H19A . 0.9300 ?
C20 N2 . 1.358(3) ?
C20 C21 . 1.430(4) ?
C21 N1 . 1.352(3) ?
O2 Fe1 2_666 2.0873(16) ?
O3 H3A . 0.79(4) ?
O5 Fe1 2_676 2.1554(15) ?
O1W H1WA . 0.85(4) ?
O1W H1WB . 0.80(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
O1W H1WA O1 2_666 0.85(4) 1.79(4) 2.602(3) 159(3)
O1W H1WB O4 2_776 0.80(4) 1.94(4) 2.740(3) 172(3)
O3 H3A O6 1_655 0.79(4) 1.86(4) 2.622(3) 160(4)
