#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/34/2213426.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_2213426
loop_
_publ_author_name
'Hua-Gang Yao'
'Min Ji'
'Sou-Hua Ji'
'Yong-Lin An'
_publ_section_title
catena-Poly[[bis(pyridine-κN)iron(II)]-μ-oxalato-κ²O,O':κ²O'',O''']
_journal_coeditor_code           KP2094
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1349
_journal_page_last               m1350
_journal_paper_doi               10.1107/S1600536807016789
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Fe (C2 O4) (C5 H5 N)2]'
_chemical_formula_moiety         'C12 H10 Fe N2 O4'
_chemical_formula_sum            'C12 H10 Fe N2 O4'
_chemical_formula_weight         302.07
_chemical_name_systematic
;
catena-poly[[bis(pyridine)iron(II)]-μ-oxalato-κ²O,O':κ²O'',O''']
;
_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                 91.688(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.714(6)
_cell_length_b                   8.895(6)
_cell_length_c                   15.359(10)
_cell_measurement_reflns_used    4154
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      3.11
_cell_volume                     1326.5(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART APEXII 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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12351
_diffrn_reflns_theta_full        31.56
_diffrn_reflns_theta_max         31.56
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.287
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.002(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4354
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0331
_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)+(0.0519P)²+0.1013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                3281
_reflns_number_total             4354
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kp2094.cif
_cod_data_source_block           I
_cod_original_cell_volume        1326.5(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2213426
_cod_database_fobs_code          2213426
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_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 0.753633(19) 0.42019(2) 0.074891(14) 0.03556(8) Uani d . 1
C C1 1.02045(14) 0.41575(16) -0.00009(10) 0.0338(3) Uani d . 1
O O4 0.93429(10) 0.32524(12) 0.03015(7) 0.0410(2) Uani d . 1
O O3 0.63518(11) 0.40632(13) -0.04807(7) 0.0434(3) Uani d . 1
O O2 0.57087(10) 0.53056(13) 0.10435(7) 0.0390(2) Uani d . 1
O O1 0.86576(10) 0.61682(12) 0.02993(8) 0.0425(3) Uani d . 1
C C2 0.51957(13) 0.46417(16) -0.04397(9) 0.0329(3) Uani d . 1
N N2 0.68163(13) 0.19369(15) 0.10675(9) 0.0438(3) Uani d . 1
N N1 0.82529(14) 0.46773(17) 0.20942(9) 0.0459(3) Uani d . 1
C C3 0.9001(2) 0.3726(3) 0.25699(15) 0.0699(6) Uani d . 1
H H3A 0.9206 0.2790 0.2336 0.084 Uiso calc R 1
C C4 0.9494(3) 0.4068(3) 0.34071(17) 0.0909(9) Uani d . 1
H H4A 1.0029 0.3375 0.3720 0.109 Uiso calc R 1
C C5 0.9192(3) 0.5402(3) 0.37595(15) 0.0810(8) Uani d . 1
H H5A 0.9518 0.5652 0.4316 0.097 Uiso calc R 1
C C6 0.8405(3) 0.6372(3) 0.32908(17) 0.0785(7) Uani d . 1
H H6A 0.8166 0.7297 0.3524 0.094 Uiso calc R 1
C C7 0.7960(2) 0.5980(2) 0.24637(16) 0.0675(6) Uani d . 1
H H7A 0.7424 0.6666 0.2147 0.081 Uiso calc R 1
C C8 0.6973(2) 0.0829(2) 0.04999(13) 0.0557(5) Uani d . 1
H H8A 0.7433 0.1032 -0.0009 0.067 Uiso calc R 1
C C9 0.6488(3) -0.0606(2) 0.06281(15) 0.0659(6) Uani d . 1
H H9A 0.6635 -0.1355 0.0219 0.079 Uiso calc R 1
C C10 0.5790(2) -0.0912(2) 0.13650(15) 0.0623(5) Uani d . 1
H H10A 0.5428 -0.1864 0.1458 0.075 Uiso calc R 1
C C11 0.5632(3) 0.0200(3) 0.19593(15) 0.0750(6) Uani d . 1
H H11A 0.5173 0.0017 0.2472 0.090 Uiso calc R 1
C C12 0.6164(2) 0.1606(2) 0.17906(14) 0.0670(6) Uani d . 1
H H12A 0.6060 0.2358 0.2204 0.080 Uiso calc R 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
O4 Fe1 O2 . . 172.52(4) y
O4 Fe1 O1 . . 77.73(6) y
O2 Fe1 O1 . . 97.30(6) y
O4 Fe1 O3 . . 96.85(6) y
O2 Fe1 O3 . . 77.57(5) y
O1 Fe1 O3 . . 91.53(5) y
O4 Fe1 N2 . . 88.76(6) ?
O2 Fe1 N2 . . 96.01(6) ?
O1 Fe1 N2 . . 166.42(4) ?
O3 Fe1 N2 . . 88.72(5) ?
O4 Fe1 N1 . . 98.13(6) ?
O2 Fe1 N1 . . 87.35(5) ?
O1 Fe1 N1 . . 89.78(6) ?
O3 Fe1 N1 . . 164.90(5) ?
N2 Fe1 N1 . . 93.51(6) ?
O1 C1 O4 3_765 . 126.48(14) ?
O1 C1 C1 3_765 3_765 117.16(15) ?
O4 C1 C1 . 3_765 116.36(15) ?
C1 O4 Fe1 . . 115.97(10) ?
C2 O3 Fe1 . . 112.80(9) ?
C2 O2 Fe1 3_665 . 115.89(10) ?
C1 O1 Fe1 3_765 . 112.78(10) ?
O3 C2 O2 . 3_665 126.29(13) ?
O3 C2 C2 . 3_665 117.45(15) ?
O2 C2 C2 3_665 3_665 116.26(15) ?
C8 N2 C12 . . 116.83(16) ?
C8 N2 Fe1 . . 119.48(12) ?
C12 N2 Fe1 . . 123.62(12) ?
C3 N1 C7 . . 116.42(19) ?
C3 N1 Fe1 . . 123.32(15) ?
C7 N1 Fe1 . . 120.25(13) ?
N2 C8 C9 . . 123.24(18) ?
C5 C4 C3 . . 119.5(2) ?
C11 C10 C9 . . 118.78(18) ?
N1 C7 C6 . . 123.5(2) ?
N2 C12 C11 . . 123.26(18) ?
C10 C9 C8 . . 118.97(19) ?
N1 C3 C4 . . 122.6(2) ?
C4 C5 C6 . . 118.6(2) ?
C5 C6 C7 . . 119.3(2) ?
C10 C11 C12 . . 118.90(19) ?
H3A C3 N1 . . 118.67 ?
H3A C3 C4 . . 118.70 ?
H4A C4 C3 . . 120.25 ?
H4A C4 C5 . . 120.22 ?
H5A C5 C4 . . 120.69 ?
H5A C5 C6 . . 120.71 ?
H6A C6 C5 . . 120.35 ?
H6A C6 C7 . . 120.35 ?
H7A C7 C6 . . 118.22 ?
H7A C7 N1 . . 118.28 ?
H8A C8 N2 . . 118.38 ?
H8A C8 C9 . . 118.39 ?
H9A C9 C8 . . 120.51 ?
H9A C9 C10 . . 120.52 ?
H10A C10 C9 . . 120.59 ?
H10A C10 C11 . . 120.64 ?
H11A C11 C10 . . 120.53 ?
H11A C11 C12 . . 120.57 ?
H12A C12 C11 . . 118.34 ?
H12A C12 N2 . . 118.41 ?
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 O4 . 2.0822(14) y
Fe1 O2 . 2.0898(14) y
Fe1 O1 . 2.1832(15) y
Fe1 O3 . 2.1858(15) y
Fe1 N2 . 2.1926(18) y
Fe1 N1 . 2.2017(19) y
C1 O1 3_765 1.2432(18) ?
C1 O4 . 1.2598(18) ?
C1 C1 3_765 1.550(3) ?
O3 C2 . 1.2385(18) ?
O2 C2 3_665 1.2594(18) ?
O1 C1 3_765 1.2432(18) ?
C2 O2 3_665 1.2594(18) ?
C2 C2 3_665 1.551(3) ?
N1 C3 . 1.322(3) ?
C3 H3A . 0.930 ?
N1 C7 . 1.325(3) ?
C4 C5 . 1.340(4) ?
C4 C3 . 1.392(3) ?
C4 H4A . 0.930 ?
C5 C6 . 1.347(4) ?
C5 H5A . 0.930 ?
C6 H6A . 0.930 ?
C7 H7A . 0.930 ?
C7 C6 . 1.375(3) ?
N2 C8 . 1.327(2) ?
N2 C12 . 1.328(2) ?
C8 C9 . 1.376(3) ?
C8 H8A . 0.930 ?
C9 H9A . 0.930 ?
C10 H10A . 0.930 ?
C10 C11 . 1.357(3) ?
C10 C9 . 1.364(3) ?
C11 H11A . 0.930 ?
C12 C11 . 1.381(3) ?
C12 H12A . 0.930 ?
