#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/82/2218286.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_2218286
loop_
_publ_author_name
'Ng, Seik Weng'
_publ_section_title
Poly[(μ₃-nicotinato-κ³O:O':N)(μ₂-nicotinato-κ³O,O':N)iron(II)]
_journal_coeditor_code           XU2410
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m728
_journal_paper_doi               10.1107/S1600536808011045
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Fe (C6 H4 N O2)2]'
_chemical_formula_moiety         'C12 H8 Fe N2 O4'
_chemical_formula_sum            'C12 H8 Fe N2 O4'
_chemical_formula_weight         300.05
_chemical_name_systematic
;
Poly[(μ₃-nicotinato-κ³O:O':N)(μ₂-nicotinato-
κ³O,O':N)iron(II)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.6190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8771(7)
_cell_length_b                   9.6066(6)
_cell_length_c                   12.7284(8)
_cell_measurement_reflns_used    6064
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     1236.45(14)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
'X-SEED (Barbour, 2001) and OLEX (Dolomanov et al.,  2003)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX'
_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  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7255
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.028
_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)+(0.0475P)²+0.2265P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.075
_refine_ls_wR_factor_ref         0.078
_reflns_number_gt                2428
_reflns_number_total             2762
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu2410.cif
_cod_data_source_block           I
_cod_original_cell_volume        1236.50(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2218286
_cod_database_fobs_code          2218286
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Fe Fe1 0.40603(2) 0.37707(2) 0.580119(18) 0.02707(10) Uani d . 1
O O1 0.28044(15) 0.19952(16) 0.64714(12) 0.0540(4) Uani d . 1
O O2 0.43525(13) 0.34442(14) 0.74858(11) 0.0398(3) Uani d . 1
O O3 0.32118(11) 0.33429(14) 0.41409(10) 0.0345(3) Uani d . 1
O O4 0.45693(13) 0.46511(14) 0.36328(12) 0.0477(3) Uani d . 1
N N1 0.25364(13) 0.02956(15) 0.94060(12) 0.0335(3) Uani d . 1
N N2 0.06748(13) 0.27149(15) 0.09200(12) 0.0335(3) Uani d . 1
C C1 0.35420(18) 0.24585(18) 0.73955(15) 0.0371(4) Uani d . 1
C C2 0.35386(17) 0.18565(18) 0.84835(14) 0.0336(4) Uani d . 1
C C3 0.25803(17) 0.09027(18) 0.84724(15) 0.0344(4) Uani d . 1
H H3 0.1932 0.0671 0.7780 0.041 Uiso calc R 1
C C4 0.34759(18) 0.0657(2) 1.03903(15) 0.0396(4) Uani d . 1
H H4 0.3462 0.0246 1.1047 0.048 Uiso calc R 1
C C5 0.4460(2) 0.1601(2) 1.04838(16) 0.0450(5) Uani d . 1
H H5 0.5090 0.1824 1.1187 0.054 Uiso calc R 1
C C6 0.44980(18) 0.2211(2) 0.95150(16) 0.0415(4) Uani d . 1
H H6 0.5156 0.2849 0.9554 0.050 Uiso calc R 1
C C7 0.35595(15) 0.39427(16) 0.34127(14) 0.0283(3) Uani d . 1
C C8 0.26579(15) 0.37708(15) 0.22048(14) 0.0281(3) Uani d . 1
C C9 0.15745(16) 0.29047(17) 0.19585(13) 0.0314(3) Uani d . 1
H H9 0.1464 0.2424 0.2552 0.038 Uiso calc R 1
C C10 0.08654(19) 0.3417(2) 0.00799(15) 0.0400(4) Uani d . 1
H H10 0.0251 0.3306 -0.0651 0.048 Uiso calc R 1
C C11 0.19213(19) 0.4291(2) 0.02432(15) 0.0432(4) Uani d . 1
H H11 0.2013 0.4753 -0.0366 0.052 Uiso calc R 1
C C12 0.28458(18) 0.44749(18) 0.13239(15) 0.0368(4) Uani d . 1
H H12 0.3572 0.5054 0.1456 0.044 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
O1 Fe1 O2 . . 56.18(5) yes
O1 Fe1 O3 . . 96.95(5) yes
O1 Fe1 O4 . 3_666 142.30(5) yes
O1 Fe1 N1 . 2_556 89.36(5) yes
O1 Fe1 N2 . 4_666 93.18(5) yes
O2 Fe1 O3 . . 153.10(6) yes
O2 Fe1 O4 . 3_666 86.23(5) yes
O2 Fe1 N1 . 2_556 92.17(5) yes
O2 Fe1 N2 . 4_666 90.93(5) yes
O3 Fe1 O4 . 3_666 120.67(6) yes
O3 Fe1 N1 . 2_556 88.50(5) yes
O3 Fe1 N2 . 4_666 89.17(5) yes
O4 Fe1 N1 3_666 2_556 89.39(6) yes
O4 Fe1 N2 3_666 4_666 89.83(6) yes
N1 Fe1 N2 2_556 4_666 176.74(5) yes
C1 O1 Fe1 . . 80.56(11) ?
C1 O2 Fe1 . . 100.52(11) ?
C7 O3 Fe1 . . 122.17(11) ?
C7 O4 Fe1 . 3_666 162.57(13) ?
C4 N1 C3 . . 116.93(15) ?
C4 N1 Fe1 . 2_546 125.34(12) ?
C3 N1 Fe1 . 2_546 117.73(11) ?
C9 N2 C10 . . 116.58(14) ?
C9 N2 Fe1 . 4_565 115.27(11) ?
C10 N2 Fe1 . 4_565 128.13(12) ?
O1 C1 O2 . . 122.67(17) ?
O1 C1 C2 . . 121.14(17) ?
O2 C1 C2 . . 116.18(16) ?
C3 C2 C6 . . 118.28(16) ?
C3 C2 C1 . . 120.21(16) ?
C6 C2 C1 . . 121.49(16) ?
N1 C3 C2 . . 123.49(16) ?
N1 C3 H3 . . 118.3 ?
C2 C3 H3 . . 118.3 ?
N1 C4 C5 . . 123.64(17) ?
N1 C4 H4 . . 118.2 ?
C5 C4 H4 . . 118.2 ?
C4 C5 C6 . . 118.78(18) ?
C4 C5 H5 . . 120.6 ?
C6 C5 H5 . . 120.6 ?
C5 C6 C2 . . 118.87(17) ?
C5 C6 H6 . . 120.6 ?
C2 C6 H6 . . 120.6 ?
O4 C7 O3 . . 124.60(16) ?
O4 C7 C8 . . 119.06(15) ?
O3 C7 C8 . . 116.33(14) ?
C9 C8 C12 . . 118.53(15) ?
C9 C8 C7 . . 118.75(15) ?
C12 C8 C7 . . 122.70(15) ?
N2 C9 C8 . . 124.03(15) ?
N2 C9 H9 . . 118.0 ?
C8 C9 H9 . . 118.0 ?
N2 C10 C11 . . 123.46(16) ?
N2 C10 H10 . . 118.3 ?
C11 C10 H10 . . 118.3 ?
C10 C11 C12 . . 119.27(17) ?
C10 C11 H11 . . 120.4 ?
C12 C11 H11 . . 120.4 ?
C11 C12 C8 . . 118.12(16) ?
C11 C12 H12 . . 120.9 ?
C8 C12 H12 . . 120.9 ?
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 O1 . 2.522(2) yes
Fe1 O2 . 2.0720(10) yes
Fe1 O3 . 2.0120(10) yes
Fe1 O4 3_666 2.0610(10) yes
Fe1 N1 2_556 2.2120(10) yes
Fe1 N2 4_666 2.2240(10) yes
O1 C1 . 1.237(2) ?
O2 C1 . 1.270(2) ?
O3 C7 . 1.262(2) ?
O4 C7 . 1.233(2) ?
O4 Fe1 3_666 2.0611(12) ?
N1 C4 . 1.338(2) ?
N1 C3 . 1.340(2) ?
N1 Fe1 2_546 2.2124(14) ?
N2 C9 . 1.336(2) ?
N2 C10 . 1.343(2) ?
N2 Fe1 4_565 2.2243(14) ?
C1 C2 . 1.502(2) ?
C2 C3 . 1.384(2) ?
C2 C6 . 1.385(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.375(3) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.379(3) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.497(2) ?
C8 C9 . 1.381(2) ?
C8 C12 . 1.388(2) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.375(3) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.384(2) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
O3 Fe1 O1 C1 . 177.00(11)
O4 Fe1 O1 C1 3_666 -6.40(16)
O2 Fe1 O1 C1 . -1.54(10)
N1 Fe1 O1 C1 2_556 -94.59(11)
N2 Fe1 O1 C1 4_666 87.45(11)
O3 Fe1 O2 C1 . -1.69(18)
O4 Fe1 O2 C1 3_666 178.53(11)
N1 Fe1 O2 C1 2_556 89.28(11)
N2 Fe1 O2 C1 4_666 -91.70(11)
O1 Fe1 O2 C1 . 1.51(10)
O4 Fe1 O3 C7 3_666 5.56(14)
O2 Fe1 O3 C7 . -174.18(11)
N1 Fe1 O3 C7 2_556 93.97(13)
N2 Fe1 O3 C7 4_666 -83.75(13)
O1 Fe1 O3 C7 . -176.85(12)
Fe1 O1 C1 O2 . 2.49(16)
Fe1 O1 C1 C2 . -176.46(16)
Fe1 O2 C1 O1 . -3.0(2)
Fe1 O2 C1 C2 . 175.95(12)
O1 C1 C2 C3 . -9.1(3)
O2 C1 C2 C3 . 171.91(16)
O1 C1 C2 C6 . 169.55(18)
O2 C1 C2 C6 . -9.5(2)
C4 N1 C3 C2 . 0.4(3)
Fe1 N1 C3 C2 2_546 -178.97(13)
C6 C2 C3 N1 . -0.5(3)
C1 C2 C3 N1 . 178.18(15)
C3 N1 C4 C5 . 0.0(3)
Fe1 N1 C4 C5 2_546 179.39(16)
N1 C4 C5 C6 . -0.4(3)
C4 C5 C6 C2 . 0.4(3)
C3 C2 C6 C5 . 0.1(3)
C1 C2 C6 C5 . -178.59(17)
Fe1 O4 C7 O3 3_666 -68.9(5)
Fe1 O4 C7 C8 3_666 110.7(4)
Fe1 O3 C7 O4 . 12.9(2)
Fe1 O3 C7 C8 . -166.66(10)
O4 C7 C8 C9 . 175.90(15)
O3 C7 C8 C9 . -4.5(2)
O4 C7 C8 C12 . -5.9(2)
O3 C7 C8 C12 . 173.73(15)
C10 N2 C9 C8 . 0.4(3)
Fe1 N2 C9 C8 4_565 179.22(13)
C12 C8 C9 N2 . -1.1(3)
C7 C8 C9 N2 . 177.20(15)
C9 N2 C10 C11 . 0.3(3)
Fe1 N2 C10 C11 4_565 -178.38(15)
N2 C10 C11 C12 . -0.2(3)
C10 C11 C12 C8 . -0.5(3)
C9 C8 C12 C11 . 1.1(3)
C7 C8 C12 C11 . -177.12(16)
