#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:49:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179991 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/85/7028508.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7028508
loop_
_publ_author_name
'Shin, Jong Won'
'Bae, Jeong Mi'
'Kim, Cheal'
'Min, Kil Sik'
_publ_section_title
;
 Catalysis and molecular magnetism of dinuclear iron(iii) complexes with
 N-(2-pyridylmethyl)-iminodiethanol/-ate.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3999
_journal_page_last               4008
_journal_paper_doi               10.1039/c3dt53376j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C22 H38 Fe2 N8 O18'
_chemical_formula_weight         814.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.06(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5580(17)
_cell_length_b                   18.487(4)
_cell_length_c                   11.217(2)
_cell_measurement_reflns_used    29105
_cell_measurement_temperature    96(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      0.43
_cell_volume                     1687.2(6)
_computing_cell_refinement       HKL3000
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        HKL3000
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (sheldrick, 2013)'
_diffrn_ambient_temperature      96(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.750
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14596
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        26.744
_diffrn_reflns_theta_max         29.834
_diffrn_reflns_theta_min         2.325
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000 Scalepack'
_exptl_crystal_colour            'greenish yellow'
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       plate
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.636
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.052(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1281P)²+2.2883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3524
_reflns_number_total             3919
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3dt53376j.txt
_cod_data_source_block           compd
_cod_database_code               7028508
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe 0.98008(5) 0.08573(2) 0.01334(4) 0.0223(2) Uani 1 1 d . .
N1 N 0.9715(3) 0.11514(14) -0.1676(3) 0.0279(6) Uani 1 1 d . .
N2 N 1.2127(3) 0.14811(13) 0.0474(2) 0.0247(5) Uani 1 1 d . .
N3 N 0.7463(3) 0.19427(14) -0.0205(3) 0.0282(6) Uani 1 1 d . .
N4 N 0.7258(4) 0.12401(16) 0.2972(3) 0.0318(6) Uani 1 1 d . .
O1 O 1.0394(3) 0.10519(13) 0.1975(2) 0.0293(5) Uani 1 1 d . .
H1 H 0.9646 0.1220 0.2233 0.044 Uiso 1 1 calc R U
O2 O 1.1378(3) 0.00725(11) 0.0067(2) 0.0248(4) Uani 1 1 d . .
O3 O 0.7453(3) 0.12457(12) -0.0167(2) 0.0298(5) Uani 1 1 d . .
O4 O 0.6168(3) 0.22751(13) -0.0410(3) 0.0364(6) Uani 1 1 d . .
O5 O 0.8813(3) 0.22452(13) -0.0019(3) 0.0364(6) Uani 1 1 d . .
O6 O 0.8217(4) 0.16913(15) 0.2740(3) 0.0420(6) Uani 1 1 d . .
O7 O 0.6106(3) 0.14387(15) 0.3338(3) 0.0398(6) Uani 1 1 d . .
O8 O 0.7460(5) 0.05718(16) 0.2834(3) 0.0564(8) Uani 1 1 d . .
C1 C 0.8681(5) 0.08290(18) -0.2680(3) 0.0332(7) Uani 1 1 d . .
H1A H 0.7875 0.0505 -0.2570 0.040 Uiso 1 1 calc R U
C2 C 0.8761(6) 0.0958(2) -0.3879(4) 0.0424(9) Uani 1 1 d . .
H2 H 0.8028 0.0723 -0.4586 0.051 Uiso 1 1 calc R U
C3 C 0.9934(5) 0.1439(2) -0.4023(3) 0.0436(9) Uani 1 1 d . .
H3 H 1.0001 0.1543 -0.4835 0.052 Uiso 1 1 calc R U
C4 C 1.1011(5) 0.1769(2) -0.2975(3) 0.0361(7) Uani 1 1 d . .
H4 H 1.1825 0.2096 -0.3060 0.043 Uiso 1 1 calc R U
C5 C 1.0878(4) 0.16115(17) -0.1810(3) 0.0287(6) Uani 1 1 d . .
C6 C 1.1957(4) 0.19552(17) -0.0622(3) 0.0302(6) Uani 1 1 d . .
H6A H 1.3057 0.2051 -0.0705 0.036 Uiso 1 1 calc R U
H6B H 1.1476 0.2424 -0.0490 0.036 Uiso 1 1 calc R U
C7 C 1.2354(4) 0.19015(17) 0.1647(3) 0.0305(7) Uani 1 1 d . .
H7A H 1.1632 0.2332 0.1471 0.037 Uiso 1 1 calc R U
H7B H 1.3508 0.2067 0.1985 0.037 Uiso 1 1 calc R U
C8 C 1.1924(4) 0.14168(19) 0.2599(3) 0.0324(7) Uani 1 1 d . .
H8A H 1.2809 0.1058 0.2939 0.039 Uiso 1 1 calc R U
H8B H 1.1808 0.1711 0.3304 0.039 Uiso 1 1 calc R U
C9 C 1.3488(4) 0.09479(16) 0.0640(3) 0.0278(6) Uani 1 1 d . .
H9A H 1.3924 0.0806 0.1533 0.033 Uiso 1 1 calc R U
H9B H 1.4392 0.1172 0.0393 0.033 Uiso 1 1 calc R U
C10 C 1.2870(4) 0.02842(16) -0.0155(3) 0.0256(6) Uani 1 1 d . .
H10A H 1.2663 0.0397 -0.1054 0.031 Uiso 1 1 calc R U
H10B H 1.3691 -0.0110 0.0084 0.031 Uiso 1 1 calc R U
C11 C 0.5604(10) -0.0867(4) 0.3803(8) 0.0837(19) Uiso 1 1 d . .
H11A H 0.6793 -0.0810 0.4190 0.126 Uiso 1 1 calc R U
H11B H 0.5391 -0.1156 0.3036 0.126 Uiso 1 1 calc R U
H11C H 0.5141 -0.1113 0.4391 0.126 Uiso 1 1 calc R U
O9 O 0.4887(7) -0.0197(3) 0.3512(6) 0.0961(15) Uiso 1 1 d . .
H9 H 0.4886 -0.0077 0.2789 0.144 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0070 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3650 0.9380 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Fe1 O2 71.95(10) 3_755 .
O2 Fe1 O1 103.40(10) 3_755 .
O2 Fe1 O1 102.17(10) . .
O2 Fe1 O3 81.18(9) 3_755 .
O2 Fe1 O3 151.92(9) . .
O1 Fe1 O3 91.64(10) . .
O2 Fe1 N1 104.76(10) 3_755 .
O2 Fe1 N1 88.47(10) . .
O1 Fe1 N1 151.77(11) . .
O3 Fe1 N1 90.68(11) . .
O2 Fe1 N2 150.39(9) 3_755 .
O2 Fe1 N2 78.72(9) . .
O1 Fe1 N2 78.61(10) . .
O3 Fe1 N2 128.43(9) . .
N1 Fe1 N2 77.97(11) . .
C1 N1 C5 120.3(3) . .
C1 N1 Fe1 121.3(2) . .
C5 N1 Fe1 117.9(2) . .
C6 N2 C7 112.2(2) . .
C6 N2 C9 111.5(3) . .
C7 N2 C9 110.6(3) . .
C6 N2 Fe1 108.15(19) . .
C7 N2 Fe1 106.66(19) . .
C9 N2 Fe1 107.49(18) . .
O4 N3 O5 123.1(3) . .
O4 N3 O3 119.5(3) . .
O5 N3 O3 117.4(3) . .
O7 N4 O6 120.8(3) . .
O7 N4 O8 119.0(3) . .
O6 N4 O8 120.2(3) . .
C8 O1 Fe1 119.07(19) . .
C8 O1 H1 109.5 . .
Fe1 O1 H1 116.5 . .
C10 O2 Fe1 132.25(17) . 3_755
C10 O2 Fe1 117.25(16) . .
Fe1 O2 Fe1 108.05(10) 3_755 .
N3 O3 Fe1 109.70(19) . .
N1 C1 C2 121.4(3) . .
N1 C1 H1A 119.3 . .
C2 C1 H1A 119.3 . .
C3 C2 C1 118.5(4) . .
C3 C2 H2 120.7 . .
C1 C2 H2 120.7 . .
C2 C3 C4 119.8(3) . .
C2 C3 H3 120.1 . .
C4 C3 H3 120.1 . .
C5 C4 C3 118.8(3) . .
C5 C4 H4 120.6 . .
C3 C4 H4 120.6 . .
N1 C5 C4 121.2(3) . .
N1 C5 C6 115.9(3) . .
C4 C5 C6 122.8(3) . .
N2 C6 C5 111.1(2) . .
N2 C6 H6A 109.4 . .
C5 C6 H6A 109.4 . .
N2 C6 H6B 109.4 . .
C5 C6 H6B 109.4 . .
H6A C6 H6B 108.0 . .
N2 C7 C8 108.6(2) . .
N2 C7 H7A 110.0 . .
C8 C7 H7A 110.0 . .
N2 C7 H7B 110.0 . .
C8 C7 H7B 110.0 . .
H7A C7 H7B 108.4 . .
O1 C8 C7 108.3(3) . .
O1 C8 H8A 110.0 . .
C7 C8 H8A 110.0 . .
O1 C8 H8B 110.0 . .
C7 C8 H8B 110.0 . .
H8A C8 H8B 108.4 . .
N2 C9 C10 110.2(3) . .
N2 C9 H9A 109.6 . .
C10 C9 H9A 109.6 . .
N2 C9 H9B 109.6 . .
C10 C9 H9B 109.6 . .
H9A C9 H9B 108.1 . .
O2 C10 C9 106.7(2) . .
O2 C10 H10A 110.4 . .
C9 C10 H10A 110.4 . .
O2 C10 H10B 110.4 . .
C9 C10 H10B 110.4 . .
H10A C10 H10B 108.6 . .
O9 C11 H11A 109.5 . .
O9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
O9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C11 O9 H9 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O2 1.970(2) 3_755
Fe1 O2 1.999(2) .
Fe1 O1 2.001(2) .
Fe1 O3 2.061(2) .
Fe1 N1 2.080(3) .
Fe1 N2 2.229(3) .
N1 C1 1.337(4) .
N1 C5 1.353(4) .
N2 C6 1.480(4) .
N2 C7 1.488(4) .
N2 C9 1.493(4) .
N3 O4 1.226(4) .
N3 O5 1.242(4) .
N3 O3 1.289(3) .
N4 O7 1.236(4) .
N4 O6 1.252(4) .
N4 O8 1.264(4) .
O1 C8 1.446(4) .
O1 H1 0.8400 .
O2 C10 1.429(3) .
O2 Fe1 1.970(2) 3_755
C1 C2 1.389(5) .
C1 H1A 0.9500 .
C2 C3 1.387(6) .
C2 H2 0.9500 .
C3 C4 1.389(6) .
C3 H3 0.9500 .
C4 C5 1.377(5) .
C4 H4 0.9500 .
C5 C6 1.506(5) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.524(5) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.513(4) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 O9 1.376(9) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
O9 H9 0.8400 .
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
_geom_torsion_site_symmetry_1
O4 N3 O3 Fe1 178.0(2) .
O5 N3 O3 Fe1 -2.5(3) .
C5 N1 C1 C2 -0.4(5) .
Fe1 N1 C1 C2 -171.9(3) .
N1 C1 C2 C3 -0.6(6) .
C1 C2 C3 C4 1.1(7) .
C2 C3 C4 C5 -0.4(6) .
C1 N1 C5 C4 1.1(5) .
Fe1 N1 C5 C4 172.8(3) .
C1 N1 C5 C6 178.9(3) .
Fe1 N1 C5 C6 -9.4(4) .
C3 C4 C5 N1 -0.6(5) .
C3 C4 C5 C6 -178.3(3) .
C7 N2 C6 C5 -149.3(3) .
C9 N2 C6 C5 86.1(3) .
Fe1 N2 C6 C5 -31.9(3) .
N1 C5 C6 N2 28.6(4) .
C4 C5 C6 N2 -153.6(3) .
C6 N2 C7 C8 160.5(3) .
C9 N2 C7 C8 -74.4(3) .
Fe1 N2 C7 C8 42.2(3) .
Fe1 O1 C8 C7 28.3(3) .
N2 C7 C8 O1 -46.3(3) .
C6 N2 C9 C10 -85.9(3) .
C7 N2 C9 C10 148.5(3) .
Fe1 N2 C9 C10 32.5(3) .
Fe1 O2 C10 C9 -157.4(2) 3_755
Fe1 O2 C10 C9 42.7(3) .
N2 C9 C10 O2 -48.0(3) .
