#------------------------------------------------------------------------------
#$Date: 2024-11-08 17:59:13 +0200 (Fri, 08 Nov 2024) $
#$Revision: 295836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/5/00/03/5000343.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_5000343
loop_
_publ_author_name
'Seddon, Elisa J.'
'Yoo, Jae'
'Folting, Kirsten'
'Huffman, John C.'
'Hendrickson, David N.'
'Christou, George'
_publ_section_title
;
 Dinuclear and hexanuclear iron(III) carboxylate clusters with a
 bis(bipyridine) ligand: supramolecular aggregation of [Fe2O2] units to
 give a [Fe6O6] ladder structure †
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3640
_journal_paper_doi               10.1039/b004925p
_journal_year                    2000
_chemical_formula_moiety         'C22 H18 Fe2 N8 O13'
_chemical_formula_sum            'C22 H18 Fe2 N8 O13'
_chemical_formula_weight         714.125
_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
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 104.750(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.759(2)
_cell_length_b                   18.811(6)
_cell_length_c                   16.618(5)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    107
_cell_measurement_theta_max      15.15
_cell_measurement_theta_min      9.65
_cell_volume                     2647.8(13)
_computing_cell_refinement       'XTEL, local package'
_computing_data_collection       'NPS, local program'
_computing_data_reduction        'XTEL, local package'
_computing_molecular_graphics    'XTEL, local package'
_computing_publication_material  'XTEL, local package'
_computing_structure_refinement  'XTEL, local package'
_computing_structure_solution    DIRDIF-96
_diffrn_ambient_temperature      107
_diffrn_measured_fraction_theta_full 0
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'refurbished Picker diffractometer'
_diffrn_measurement_method       'θ/2θ scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5921
_diffrn_reflns_theta_full        0
_diffrn_reflns_theta_max         25.0521
_diffrn_reflns_theta_min         3.01745
_diffrn_standards_decay_%        -0.6
_diffrn_standards_interval_count 300
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.1808
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Tompa
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.39
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       0.00000013(6)
_refine_ls_extinction_expression
;
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   0.9517
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         3121
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.0036
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w⁻¹=σ²(F)+(.07F)²
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0476
_reflns_number_gt                3121
_reflns_number_total             4689
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b004925p.txt
_cod_data_source_block           MSC98201
_cod_original_cell_volume        2647.7(22)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               5000343
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
x,1/2-y,1/2+z
-x,-y,-z
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_disorder_group
_atom_site_disorder_assembly
Fe1 Fe 0.12186(10) 0.11859(4) 0.32507(5) 0.0127(3) Uani 1 0 .
Fe2 Fe 0.36620(10) 0.10299(4) 0.19031(5) 0.0129(3) Uani 1 0 .
O3 O 0.2168(4) 0.1000(2) 0.2446(2) 0.0158(14) Uani 1 0 .
N4 N 0.0056(5) 0.1349(2) 0.4212(3) 0.0132(16) Uani 1 0 .
C5 C 0.0249(7) 0.1934(3) 0.4691(4) 0.0176(19) Uani 1 0 .
C6 C -0.0525(7) 0.2034(3) 0.5309(3) 0.0159(19) Uani 1 0 .
C7 C -0.1572(7) 0.1517(3) 0.5421(3) 0.018(2) Uani 1 0 .
C8 C -0.1785(6) 0.0910(3) 0.4933(3) 0.0143(18) Uani 1 0 .
C9 C -0.0939(6) 0.0839(3) 0.4338(3) 0.0133(18) Uani 1 0 .
C10 C -0.1040(7) 0.0195(3) 0.3808(3) 0.0145(19) Uani 1 0 .
C11 C -0.2043(7) -0.0364(3) 0.3861(4) 0.018(2) Uani 1 0 .
C12 C -0.2009(7) -0.0970(3) 0.3397(4) 0.0180(19) Uani 1 0 .
C13 C -0.0993(7) -0.0997(3) 0.2878(3) 0.0150(18) Uani 1 0 .
C14 C -0.0040(7) -0.0417(3) 0.2831(4) 0.0164(19) Uani 1 0 .
N15 N -0.0057(5) 0.0174(2) 0.3287(3) 0.0135(16) Uani 1 0 .
C16 C 0.1069(7) -0.0466(3) 0.2263(4) 0.019(2) Uani 1 0 .
C17 C 0.2804(7) -0.0539(3) 0.2761(4) 0.017(2) Uani 1 0 .
N18 N 0.4463(6) -0.0071(2) 0.1879(3) 0.0140(16) Uani 1 0 .
C19 C 0.3912(7) -0.0646(3) 0.2212(4) 0.0162(19) Uani 1 0 .
C20 C 0.4370(7) -0.1330(3) 0.2068(4) 0.0176(19) Uani 1 0 .
C21 C 0.5433(7) -0.1441(3) 0.1589(4) 0.020(2) Uani 1 0 .
C22 C 0.6031(7) -0.0851(3) 0.1268(4) 0.019(2) Uani 1 0 .
C23 C 0.5520(7) -0.0173(3) 0.1418(3) 0.0152(19) Uani 1 0 .
C24 C 0.6063(6) 0.0466(3) 0.1060(3) 0.0132(18) Uani 1 0 .
C25 C 0.7223(7) 0.0457(3) 0.0624(4) 0.022(2) Uani 1 0 .
C26 C 0.7556(7) 0.1069(3) 0.0239(4) 0.025(2) Uani 1 0 .
C27 C 0.6754(7) 0.1682(3) 0.0313(4) 0.022(2) Uani 1 0 .
C28 C 0.5662(7) 0.1675(3) 0.0786(4) 0.020(2) Uani 1 0 .
N29 N 0.5320(6) 0.1078(2) 0.1153(3) 0.0162(16) Uani 1 0 .
O30 O 0.3180(5) 0.1773(2) 0.4045(3) 0.0193(14) Uani 1 0 .
N31 N 0.3694(6) 0.1249(3) 0.4524(3) 0.0188(18) Uani 1 0 .
O32 O 0.2996(5) 0.0660(2) 0.4289(2) 0.0188(14) Uani 1 0 .
O33 O 0.4742(5) 0.1308(2) 0.5165(3) 0.0274(16) Uani 1 0 .
O34 O 0.0624(5) 0.2285(2) 0.2923(2) 0.0193(14) Uani 1 0 .
N35 N -0.0754(6) 0.2138(3) 0.2468(3) 0.0189(18) Uani 1 0 .
O36 O -0.1102(5) 0.1478(2) 0.2408(2) 0.0196(14) Uani 1 0 .
O37 O -0.1681(5) 0.2598(2) 0.2111(3) 0.0240(15) Uani 1 0 .
O38 O 0.5628(5) 0.1057(2) 0.3014(2) 0.0175(13) Uani 1 0 .
N39 N 0.5677(6) 0.1736(3) 0.3006(3) 0.0151(16) Uani 1 0 .
O40 O 0.4665(5) 0.20299(19) 0.2400(2) 0.0160(14) Uani 1 0 .
O41 O 0.6610(5) 0.2084(2) 0.3528(2) 0.0200(14) Uani 1 0 .
O42 O 0.2068(5) 0.0631(2) 0.0729(2) 0.0179(14) Uani 1 0 .
N43 N 0.1738(6) 0.1255(3) 0.0441(3) 0.0171(17) Uani 1 0 .
O44 O 0.2322(5) 0.1759(2) 0.0936(2) 0.0184(14) Uani 1 0 .
O45 O 0.0966(5) 0.1361(2) -0.0274(3) 0.0234(15) Uani 1 0 .
H1 H 0.095 0.2294 0.4601 0.0305 Uiso 1 0 .
H2 H -0.0342 0.2448 0.565 0.0285 Uiso 1 0 .
H3 H -0.2149 0.1578 0.583 0.0307 Uiso 1 0 .
H4 H -0.2505 0.0552 0.5003 0.027 Uiso 1 0 .
H5 H -0.2743 -0.0331 0.4213 0.0304 Uiso 1 0 .
H6 H -0.2674 -0.1361 0.343 0.0309 Uiso 1 0 .
H7 H -0.0949 -0.1412 0.2558 0.0276 Uiso 1 0 .
H8 H 0.0788 -0.0867 0.1911 0.0315 Uiso 1 0 .
H9 H 0.0962 -0.0046 0.1933 0.0315 Uiso 1 0 .
H10 H 0.3106 -0.012 0.308 0.03 Uiso 1 0 .
H11 H 0.2891 -0.0936 0.3123 0.03 Uiso 1 0 .
H12 H 0.3954 -0.1725 0.2299 0.0306 Uiso 1 0 .
H13 H 0.5747 -0.1908 0.1482 0.0324 Uiso 1 0 .
H14 H 0.6783 -0.0908 0.0949 0.0318 Uiso 1 0 .
H15 H 0.7785 0.0031 0.0589 0.0351 Uiso 1 0 .
H16 H 0.8327 0.1064 -0.0072 0.0378 Uiso 1 0 .
H17 H 0.6951 0.2107 0.0046 0.0345 Uiso 1 0 .
H18 H 0.5131 0.2104 0.0852 0.0322 Uiso 1 0 .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe Fe 0.301 0.845 'International Tables Vol. IV (1974) Table 2.2B'
O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B'
N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B'
C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B'
H H 0 0 'International Tables Vol. IV (1974) Table 2.2B'
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Fe2 Fe1 O30 85.04(11) . . . no
Fe2 Fe1 O32 92.15(11) . . . no
Fe2 Fe1 O34 93.83(11) . . . no
Fe2 Fe1 O36 103.22(11) . . . no
Fe2 Fe1 N4 170.71(13) . . . no
Fe2 Fe1 N15 109.99(12) . . . no
Fe1 Fe2 O38 86.32(11) . . . no
Fe1 Fe2 O40 86.39(11) . . . no
Fe1 Fe2 O42 103.99(11) . . . no
Fe1 Fe2 O44 96.65(11) . . . no
Fe1 Fe2 N18 110.10(12) . . . no
Fe1 Fe2 N29 171.52(13) . . . no
O3 Fe1 O30 96.17(16) . . . no
O3 Fe1 O32 97.24(16) . . . no
O3 Fe1 O34 97.29(17) . . . no
O3 Fe1 O36 95.87(16) . . . no
O3 Fe1 N4 176.95(18) . . . no
O3 Fe1 N15 100.79(17) . . . no
O30 Fe1 O32 58.10(15) . . . no
O30 Fe1 O34 76.74(15) . . . no
O30 Fe1 O36 135.10(15) . . . no
O30 Fe1 N4 85.78(16) . . . no
O30 Fe1 N15 138.03(17) . . . no
O32 Fe1 O34 133.68(15) . . . no
O32 Fe1 O36 159.96(15) . . . no
O32 Fe1 N4 81.78(16) . . . no
O32 Fe1 N15 81.72(16) . . . no
O34 Fe1 O36 58.89(14) . . . no
O34 Fe1 N4 85.42(16) . . . no
O34 Fe1 N15 137.36(16) . . . no
O36 Fe1 N4 84.34(17) . . . no
O36 Fe1 N15 80.98(16) . . . no
N4 Fe1 N15 76.23(17) . . . no
O3 Fe2 O38 95.52(16) . . . no
O3 Fe2 O40 96.57(16) . . . no
O3 Fe2 O42 93.23(16) . . . no
O3 Fe2 O44 93.75(16) . . . no
O3 Fe2 N18 105.16(18) . . . no
O3 Fe2 N29 175.27(18) . . . no
O38 Fe2 O40 59.81(14) . . . no
O38 Fe2 O42 159.35(15) . . . no
O38 Fe2 O44 139.47(15) . . . no
O38 Fe2 N18 81.35(16) . . . no
O38 Fe2 N29 89.15(17) . . . no
O40 Fe2 O42 137.47(15) . . . no
O40 Fe2 O44 79.97(15) . . . no
O40 Fe2 N18 137.11(17) . . . no
O40 Fe2 N29 85.14(16) . . . no
O42 Fe2 O44 58.11(14) . . . no
O42 Fe2 N18 78.32(16) . . . no
O42 Fe2 N29 82.58(16) . . . no
O44 Fe2 N18 133.41(16) . . . no
O44 Fe2 N29 82.18(16) . . . no
N18 Fe2 N29 76.22(18) . . . no
Fe1 O3 Fe2 157.6(2) . . . no
Fe1 O30 N31 94.8(3) . . . no
Fe1 O32 N31 92.1(3) . . . no
Fe1 O34 N35 94.2(3) . . . no
Fe1 O36 N35 91.7(3) . . . no
Fe2 O38 N39 92.0(3) . . . no
Fe2 O40 N39 93.3(3) . . . no
Fe2 O42 N43 92.9(3) . . . no
Fe2 O44 N43 93.4(3) . . . no
Fe1 N4 C5 123.5(4) . . . no
Fe1 N4 C9 117.8(4) . . . no
C5 N4 C9 118.7(5) . . . no
Fe1 N15 C10 113.3(4) . . . no
Fe1 N15 C14 127.9(4) . . . no
C10 N15 C14 118.7(5) . . . no
Fe2 N18 C19 126.6(4) . . . no
Fe2 N18 C23 114.3(4) . . . no
C19 N18 C23 118.8(5) . . . no
Fe2 N29 C24 116.6(4) . . . no
Fe2 N29 C28 124.1(4) . . . no
C24 N29 C28 119.2(5) . . . no
O30 N31 O32 114.5(5) . . . no
O30 N31 O33 122.8(5) . . . no
O32 N31 O33 122.7(5) . . . no
O34 N35 O36 115.2(5) . . . no
O34 N35 O37 122.6(5) . . . no
O36 N35 O37 122.2(5) . . . no
O38 N39 O40 114.9(4) . . . no
O38 N39 O41 123.1(5) . . . no
O40 N39 O41 122.0(5) . . . no
O42 N43 O44 115.3(5) . . . no
O42 N43 O45 122.0(5) . . . no
O44 N43 O45 122.6(5) . . . no
N4 C5 C6 122.8(5) . . . no
N4 C5 H1 118.7(6) . . . no
C6 C5 H1 118.6(6) . . . no
C5 C6 C7 118.2(5) . . . no
C5 C6 H2 120.9(6) . . . no
C7 C6 H2 120.9(6) . . . no
C6 C7 C8 119.8(5) . . . no
C6 C7 H3 120.2(6) . . . no
C8 C7 H3 120.0(6) . . . no
C7 C8 C9 118.8(5) . . . no
C7 C8 H4 120.5(5) . . . no
C9 C8 H4 120.7(5) . . . no
N4 C9 C8 121.7(5) . . . no
N4 C9 C10 115.6(5) . . . no
C8 C9 C10 122.7(5) . . . no
N15 C10 C9 116.5(5) . . . no
N15 C10 C11 121.9(5) . . . no
C9 C10 C11 121.5(5) . . . no
C10 C11 C12 119.1(5) . . . no
C10 C11 H5 120.6(6) . . . no
C12 C11 H5 120.4(6) . . . no
C11 C12 C13 119.1(5) . . . no
C11 C12 H6 120.5(6) . . . no
C13 C12 H6 120.4(6) . . . no
C12 C13 C14 119.7(5) . . . no
C12 C13 H7 120.2(6) . . . no
C14 C13 H7 120.2(5) . . . no
N15 C14 C13 121.5(5) . . . no
N15 C14 C16 120.0(5) . . . no
C13 C14 C16 118.4(5) . . . no
C14 C16 C17 111.8(5) . . . no
C14 C16 H8 109.0(5) . . . no
C14 C16 H9 108.8(5) . . . no
C17 C16 H8 109.0(5) . . . no
C17 C16 H9 108.8(5) . . . no
H8 C16 H9 109.4(6) . . . no
C16 C17 C19 112.8(5) . . . no
C16 C17 H10 108.7(5) . . . no
C16 C17 H11 108.6(5) . . . no
C19 C17 H10 108.6(5) . . . no
C19 C17 H11 108.7(5) . . . no
H10 C17 H11 109.4(6) . . . no
N18 C19 C17 119.5(5) . . . no
N18 C19 C20 121.3(5) . . . no
C17 C19 C20 119.2(5) . . . no
C19 C20 C21 120.4(5) . . . no
C19 C20 H12 119.9(6) . . . no
C21 C20 H12 119.8(6) . . . no
C20 C21 C22 118.2(5) . . . no
C20 C21 H13 121.0(6) . . . no
C22 C21 H13 120.8(6) . . . no
C21 C22 C23 119.5(5) . . . no
C21 C22 H14 120.3(6) . . . no
C23 C22 H14 120.2(6) . . . no
N18 C23 C22 121.8(5) . . . no
N18 C23 C24 116.7(5) . . . no
C22 C23 C24 121.5(5) . . . no
N29 C24 C23 115.8(5) . . . no
N29 C24 C25 120.5(5) . . . no
C23 C24 C25 123.7(5) . . . no
C24 C25 C26 119.9(6) . . . no
C24 C25 H15 120.0(6) . . . no
C26 C25 H15 120.1(6) . . . no
C25 C26 C27 119.0(6) . . . no
C25 C26 H16 120.3(6) . . . no
C27 C26 H16 120.6(6) . . . no
C26 C27 C28 119.1(6) . . . no
C26 C27 H17 120.5(6) . . . no
C28 C27 H17 120.4(6) . . . no
N29 C28 C27 122.1(6) . . . no
N29 C28 H18 118.8(6) . . . no
C27 C28 H18 119.1(6) . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 Fe2 3.482(1) . . no
Fe1 O3 1.779(4) . . no
Fe1 O30 2.182(4) . . no
Fe1 O32 2.239(4) . . no
Fe1 O34 2.167(4) . . no
Fe1 O36 2.223(4) . . no
Fe1 N4 2.124(4) . . no
Fe1 N15 2.217(5) . . no
Fe2 O3 1.770(4) . . no
Fe2 O38 2.181(4) . . no
Fe2 O40 2.150(4) . . no
Fe2 O42 2.221(4) . . no
Fe2 O44 2.210(4) . . no
Fe2 N18 2.190(5) . . no
Fe2 N29 2.143(5) . . no
O30 N31 1.275(6) . . no
O32 N31 1.278(6) . . no
O33 N31 1.221(6) . . no
O34 N35 1.281(6) . . no
O36 N35 1.276(6) . . no
O37 N35 1.231(6) . . no
O38 N39 1.279(6) . . no
O40 N39 1.284(6) . . no
O41 N39 1.220(6) . . no
O42 N43 1.273(6) . . no
O44 N43 1.274(6) . . no
O45 N43 1.224(6) . . no
N4 C5 1.344(7) . . no
N4 C9 1.348(7) . . no
N15 C10 1.368(7) . . no
N15 C14 1.347(7) . . no
N18 C19 1.358(7) . . no
N18 C23 1.358(7) . . no
N29 C24 1.350(7) . . no
N29 C28 1.347(7) . . no
C5 C6 1.380(8) . . no
C5 H1 0.951(6) . . no
C6 C7 1.381(8) . . no
C6 H2 0.951(6) . . no
C7 C8 1.385(8) . . no
C7 H3 0.952(6) . . no
C8 C9 1.385(8) . . no
C8 H4 0.951(5) . . no
C9 C10 1.486(8) . . no
C10 C11 1.387(8) . . no
C11 C12 1.381(8) . . no
C11 H5 0.951(6) . . no
C12 C13 1.389(8) . . no
C12 H6 0.949(6) . . no
C13 C14 1.389(8) . . no
C13 H7 0.951(6) . . no
C14 C16 1.519(8) . . no
C16 C17 1.540(8) . . no
C16 H8 0.949(6) . . no
C16 H9 0.952(6) . . no
C17 C19 1.504(8) . . no
C17 H10 0.950(6) . . no
C17 H11 0.950(6) . . no
C19 C20 1.387(8) . . no
C20 C21 1.387(8) . . no
C20 H12 0.951(6) . . no
C21 C22 1.391(8) . . no
C21 H13 0.951(6) . . no
C22 C23 1.394(8) . . no
C22 H14 0.951(6) . . no
C23 C24 1.473(8) . . no
C24 C25 1.391(8) . . no
C25 C26 1.383(9) . . no
C25 H15 0.950(6) . . no
C26 C27 1.371(9) . . no
C26 H16 0.950(6) . . no
C27 C28 1.384(8) . . no
C27 H17 0.952(6) . . no
C28 H18 0.952(6) . . no
