# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Giovanni De Munno' _publ_contact_author_address ; Department of Chemistry University of Calabria P. Bucci 14/c Arcavacata di Rende 87030 ITALY ; _publ_contact_author_phone +390984492088 _publ_contact_author_fax +390984492044 _publ_contact_author_email demunno@unical.it loop_ _publ_author_name _publ_author_address 'Donatella Armentano' ; Dipartimento di Chimica Universita degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Giovanni De Munno' ; Dipartimento di Chimica Universita degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Teresa F. Mastropietro' ; Dipartimento di Chimica Università degli Studi della Calabria I-87030 Arcavacata di Rende, Cosenza Italy ; 'Francesc Lloret' ; Departament de Química Inorgánica/Instituto de Ciencia Molecular Facultat de Química, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; 'Miguel Julve' ; Departament de Química Inorgánica/Instituto de Ciencia Molecular Facultat de Química, Dr. Moliner 50 46100 Burjassot, Valencia Spain ; _publ_section_title ; A Novel Supramolecular Assembly in a Iron(III) compound Exhibiting Magnetic Ordering at 70 K ; #=============================================================================== # 5. CHEMICAL DATA #=============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 221514' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H32 Cl4 Fe5 N O33' _chemical_formula_weight 1139.44 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting orthorombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 27.328(6) _cell_length_b 32.125(6) _cell_length_c 18.424(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16175(6) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 30 _exptl_crystal_description rhombuses _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9168 _exptl_absorpt_coefficient_mu 2.118 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2821 _exptl_absorpt_correction_T_max 0.6647 _exptl_absorpt_process_details psi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'R3m/V automatic four-circle diffractometer' _diffrn_measurement_method omega/2-theta-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.1 _diffrn_reflns_number 3787 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3704 _reflns_number_gt 3258 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1658P)^2^+62.4210P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(10) _refine_ls_number_reflns 3704 _refine_ls_number_parameters 497 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.2120 _refine_ls_wR_factor_gt 0.2052 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.0000 0.22526(14) 0.0229(6) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 -0.18891(17) 0.0371(8) Uani 1 2 d S . . O1 O 0.4707(3) 0.0369(3) 0.1430(5) 0.029(2) Uani 1 1 d . . . O2 O 0.4366(3) -0.0308(3) 0.2055(5) 0.0251(19) Uani 1 1 d . . . O3 O 0.4071(3) 0.0396(3) 0.0678(6) 0.030(2) Uani 1 1 d . . . O4 O 0.3717(3) -0.0312(3) 0.1288(5) 0.028(2) Uani 1 1 d . . . Cl1 Cl 0.52569(16) -0.04681(13) 0.3107(2) 0.0483(10) Uani 1 1 d . . . Cl2 Cl 0.47579(19) -0.0460(2) -0.2768(3) 0.0777(18) Uani 1 1 d . . . C1 C 0.4106(4) -0.0164(4) 0.1535(7) 0.021(3) Uani 1 1 d . . . C2 C 0.4306(5) 0.0242(4) 0.1175(8) 0.029(3) Uani 1 1 d . . . O5 O 0.4694(4) -0.0354(3) -0.1090(6) 0.040(3) Uani 1 1 d . . . O6 O 0.4369(3) 0.0311(3) -0.1701(6) 0.037(2) Uani 1 1 d . . . O7 O 0.4081(4) -0.0361(3) -0.0305(6) 0.034(2) Uani 1 1 d . . . O8 O 0.3757(4) 0.0359(3) -0.0913(5) 0.035(2) Uani 1 1 d . . . C3 C 0.4313(4) -0.0218(4) -0.0823(8) 0.024(3) Uani 1 1 d . . . C4 C 0.4121(5) 0.0187(4) -0.1164(8) 0.027(3) Uani 1 1 d . . . Fe3 Fe 0.30724(6) -0.08050(5) -0.29593(9) 0.0199(4) Uani 1 1 d . . . Fe4 Fe 0.20435(6) -0.08500(5) -0.17724(9) 0.0189(4) Uani 1 1 d . . . Fe5 Fe 0.33880(8) 0.00110(8) 0.01721(17) 0.0428(5) Uani 1 1 d . . . Cl3 Cl 0.34961(12) -0.05348(11) -0.20147(19) 0.0347(8) Uani 1 1 d . . . Cl4 Cl 0.15800(12) -0.06084(11) -0.2713(2) 0.0345(8) Uani 1 1 d . . . O9 O 0.2783(3) -0.0244(3) -0.3199(5) 0.0245(19) Uani 1 1 d . . . O10 O 0.2659(3) -0.0943(3) -0.3892(5) 0.029(2) Uani 1 1 d . . . O11 O 0.2280(3) 0.0089(3) -0.3967(6) 0.031(2) Uani 1 1 d . . . O12 O 0.2072(3) -0.0660(3) -0.4568(6) 0.031(2) Uani 1 1 d . . . C5 C 0.2484(4) -0.0229(4) -0.3723(7) 0.024(3) Uani 1 1 d . . . C6 C 0.2384(4) -0.0647(4) -0.4106(7) 0.021(3) Uani 1 1 d . . . O13 O 0.1485(3) -0.0763(3) -0.1023(5) 0.027(2) Uani 1 1 d . . . O14 O 0.1752(3) -0.1441(2) -0.1735(5) 0.0232(18) Uani 1 1 d . . . O15 O 0.0874(3) -0.1111(3) -0.0511(5) 0.028(2) Uani 1 1 d . . . O16 O 0.1149(3) -0.1789(3) -0.1203(5) 0.0250(19) Uani 1 1 d . . . C7 C 0.1243(4) -0.1079(4) -0.0912(7) 0.022(3) Uani 1 1 d . . . C8 C 0.1389(4) -0.1472(4) -0.1313(7) 0.020(2) Uani 1 1 d . . . O17 O 0.2280(3) -0.0273(3) -0.1548(5) 0.0250(19) Uani 1 1 d . . . O18 O 0.2473(3) -0.0972(3) -0.0879(5) 0.025(2) Uani 1 1 d . . . O19 O 0.2752(4) 0.0073(3) -0.0754(6) 0.031(2) Uani 1 1 d . . . O20 O 0.3014(3) -0.0656(3) -0.0152(5) 0.026(2) Uani 1 1 d . . . C9 C 0.2567(4) -0.0251(4) -0.0994(7) 0.023(3) Uani 1 1 d . . . C10 C 0.2702(4) -0.0658(3) -0.0649(7) 0.020(2) Uani 1 1 d . . . O21 O 0.2558(3) -0.1058(3) -0.2388(6) 0.0252(17) Uani 1 1 d . . . Fe6 Fe 0.50473(11) -0.15742(7) 0.01657(19) 0.0501(6) Uani 1 1 d . . . O1W O 0.5653(4) -0.1178(3) 0.0228(8) 0.051(3) Uani 1 1 d . . . O2W O 0.4454(4) -0.2024(3) 0.0194(6) 0.042(3) Uani 1 1 d . . . O3W O 0.5008(5) -0.1640(4) 0.1284(7) 0.054(3) Uani 1 1 d . . . O4W O 0.4531(6) -0.1102(4) 0.0220(10) 0.079(5) Uani 1 1 d . . . O5W O 0.5556(4) -0.2092(3) 0.0087(7) 0.041(3) Uani 1 1 d . . . O6W O 0.5032(6) -0.1619(4) -0.0956(7) 0.064(4) Uani 1 1 d . . . N1 N 0.6539(8) -0.1683(6) 0.1679(10) 0.076(5) Uani 1 1 d . . . C11 C 0.6212(15) -0.2314(7) 0.2130(19) 0.133(15) Uani 1 1 d . . . C12 C 0.6374(11) -0.2085(10) 0.1545(12) 0.092(9) Uani 1 1 d . . . O7W O 0.6615(4) -0.1429(3) 0.0230(8) 0.052(3) Uani 1 1 d . . . O8W O 0.2469(5) -0.1875(4) -0.2758(9) 0.074(4) Uani 1 1 d . . . O9W O 0.3730(6) -0.1250(4) 0.1080(9) 0.078(5) Uani 1 1 d . . . O10W O 0.3395(9) -0.1533(5) -0.0304(12) 0.109(7) Uani 1 1 d . . . O11W O 0.4438(8) -0.1271(7) -0.1902(13) 0.118(8) Uani 1 1 d . . . O12W O 0.5629(5) -0.1272(3) 0.2314(8) 0.055(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0199(12) 0.0286(13) 0.0203(14) 0.000 0.000 -0.0005(9) Fe2 0.0193(13) 0.061(2) 0.0312(18) 0.000 0.000 0.0020(12) O1 0.025(5) 0.027(4) 0.036(6) 0.007(4) -0.014(4) -0.010(4) O2 0.027(4) 0.033(5) 0.016(4) 0.010(4) -0.002(4) -0.002(4) O3 0.032(5) 0.025(4) 0.034(5) 0.007(4) -0.016(4) -0.006(4) O4 0.023(4) 0.029(5) 0.032(5) 0.002(4) 0.000(4) -0.005(4) Cl1 0.055(2) 0.051(2) 0.039(2) 0.0143(17) -0.0023(18) 0.0173(18) Cl2 0.050(3) 0.115(5) 0.068(4) -0.036(3) -0.010(2) -0.001(3) C1 0.019(6) 0.021(6) 0.024(7) -0.003(5) 0.006(5) -0.004(5) C2 0.027(7) 0.033(7) 0.027(8) -0.003(6) 0.004(6) -0.003(6) O5 0.033(5) 0.047(6) 0.041(6) 0.008(5) 0.008(5) 0.008(5) O6 0.024(5) 0.045(6) 0.041(6) 0.016(5) 0.006(4) 0.002(4) O7 0.042(5) 0.025(5) 0.036(6) 0.006(4) 0.008(5) 0.003(4) O8 0.033(5) 0.045(6) 0.028(5) 0.000(4) 0.002(4) 0.015(4) C3 0.023(6) 0.017(6) 0.032(7) -0.006(5) -0.006(6) -0.001(5) C4 0.022(6) 0.030(7) 0.028(7) 0.008(6) -0.005(5) -0.005(5) Fe3 0.0165(7) 0.0235(8) 0.0198(9) 0.0004(7) 0.0042(7) 0.0042(6) Fe4 0.0163(7) 0.0213(8) 0.0192(9) -0.0014(7) 0.0041(7) -0.0033(6) Fe5 0.0434(12) 0.0444(11) 0.0407(11) 0.0022(9) -0.0002(12) -0.0005(10) Cl3 0.0265(15) 0.0453(19) 0.0323(18) -0.0077(15) -0.0047(13) -0.0026(13) Cl4 0.0279(15) 0.0417(18) 0.0339(19) 0.0058(15) -0.0066(14) -0.0010(13) O9 0.023(4) 0.025(4) 0.025(5) -0.006(4) -0.001(4) 0.004(3) O10 0.029(5) 0.025(5) 0.032(5) -0.003(4) -0.003(4) 0.006(4) O11 0.033(5) 0.020(4) 0.040(6) -0.001(4) -0.010(4) 0.004(4) O12 0.033(5) 0.030(5) 0.029(6) -0.001(4) -0.007(4) -0.001(4) C5 0.028(6) 0.021(6) 0.022(7) -0.003(5) -0.002(5) -0.001(5) C6 0.020(6) 0.020(6) 0.023(7) -0.003(5) 0.000(5) 0.002(5) O13 0.021(4) 0.023(4) 0.037(5) -0.011(4) 0.014(4) -0.008(3) O14 0.017(4) 0.024(4) 0.029(5) -0.008(4) 0.008(4) -0.006(3) O15 0.019(4) 0.034(5) 0.029(5) -0.006(4) 0.011(4) -0.002(4) O16 0.022(4) 0.027(4) 0.026(5) -0.004(4) 0.009(4) -0.003(4) C7 0.022(6) 0.028(6) 0.016(6) -0.006(5) 0.002(5) 0.001(5) C8 0.010(5) 0.029(6) 0.021(6) -0.001(5) -0.006(4) -0.004(5) O17 0.024(4) 0.024(4) 0.027(5) 0.001(4) -0.008(4) -0.003(3) O18 0.029(5) 0.023(5) 0.023(5) 0.004(4) -0.003(4) -0.005(3) O19 0.037(5) 0.024(4) 0.032(6) -0.006(4) -0.009(4) -0.001(4) O20 0.035(5) 0.022(4) 0.023(5) 0.000(4) -0.012(4) 0.003(4) C9 0.021(6) 0.029(7) 0.020(7) -0.002(5) 0.002(5) -0.003(5) C10 0.021(6) 0.018(6) 0.019(6) 0.001(5) 0.008(5) 0.002(5) O21 0.019(4) 0.033(4) 0.024(4) -0.004(4) 0.008(3) -0.006(4) Fe6 0.0612(15) 0.0439(12) 0.0451(12) 0.0001(14) 0.0002(11) -0.0047(12) O1W 0.054(7) 0.034(6) 0.064(8) -0.003(5) 0.003(6) -0.015(5) O2W 0.061(7) 0.028(5) 0.036(6) -0.002(4) -0.007(5) -0.008(4) O3W 0.092(10) 0.035(6) 0.033(7) 0.002(5) 0.000(6) -0.007(6) O4W 0.113(12) 0.048(7) 0.078(11) 0.024(7) 0.000(10) 0.030(8) O5W 0.050(6) 0.026(5) 0.047(7) -0.013(5) 0.009(5) 0.003(4) O6W 0.120(13) 0.047(7) 0.026(7) -0.004(5) -0.011(7) 0.014(7) N1 0.094(14) 0.075(12) 0.060(11) -0.016(9) -0.009(10) 0.001(10) C11 0.23(4) 0.054(13) 0.11(2) -0.035(15) -0.09(3) -0.023(19) C12 0.12(2) 0.12(2) 0.035(11) -0.017(13) -0.033(13) 0.019(17) O7W 0.045(6) 0.042(6) 0.069(8) -0.019(6) -0.001(6) -0.003(5) O8W 0.077(9) 0.062(8) 0.083(10) -0.021(8) 0.041(8) -0.025(7) O9W 0.110(13) 0.048(7) 0.077(10) -0.014(7) -0.003(10) 0.016(8) O10W 0.167(19) 0.071(11) 0.088(14) -0.007(10) -0.025(13) 0.000(11) O11W 0.103(14) 0.150(18) 0.100(17) 0.005(15) -0.021(13) 0.057(13) O12W 0.078(8) 0.034(5) 0.053(8) -0.004(5) 0.007(7) -0.012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 2.028(9) . ? Fe1 O2 2.028(9) 2_655 ? Fe1 O1 2.085(9) 2_655 ? Fe1 O1 2.085(9) . ? Fe1 Cl1 2.288(4) . ? Fe1 Cl1 2.288(4) 2_655 ? Fe2 O6 2.024(9) . ? Fe2 O6 2.024(9) 2_655 ? Fe2 O5 2.041(11) . ? Fe2 O5 2.041(11) 2_655 ? Fe2 Cl2 2.291(6) . ? Fe2 Cl2 2.291(6) 2_655 ? O1 C2 1.259(16) . ? O2 C1 1.278(16) . ? O3 C2 1.222(17) . ? O4 C1 1.250(15) . ? C1 C2 1.562(18) . ? O5 C3 1.232(17) . ? O6 C4 1.262(17) . ? O7 C3 1.235(17) . ? O8 C4 1.228(17) . ? C3 C4 1.537(18) . ? Fe3 O21 1.935(9) . ? Fe3 O9 2.016(9) . ? Fe3 O15 2.052(9) 7_544 ? Fe3 O10 2.104(10) . ? Fe3 O16 2.109(8) 7_544 ? Fe3 Cl3 2.263(4) . ? Fe4 O21 1.927(9) . ? Fe4 O17 2.006(8) . ? Fe4 O18 2.059(9) . ? Fe4 O14 2.061(8) . ? Fe4 O13 2.076(9) . ? Fe4 Cl4 2.282(4) . ? O3 FE5 2.425(9) . ? O4 FE5 2.472(10) . ? O7 FE5 2.404(10) . ? O8 FE5 2.502(11) . ? Fe5 O19 2.444(11) . ? Fe5 O20 2.448(9) . ? O11 Fe5 2.440(11) 10_555 ? O12 Fe5 2.480(9) 10_555 ? O9 C5 1.265(16) . ? O10 C6 1.273(15) . ? O11 C5 1.249(16) . ? O12 C6 1.207(15) . ? C5 C6 1.540(17) . ? O13 C7 1.229(15) . ? O14 C8 1.264(15) . ? O15 C7 1.255(16) . ? O15 Fe3 2.052(9) 15_445 ? O16 C8 1.229(15) . ? O16 Fe3 2.109(8) 15_445 ? C7 C8 1.516(16) . ? O17 C9 1.288(16) . ? O18 C10 1.260(15) . ? O19 C9 1.240(16) . ? O20 C10 1.252(16) . ? C9 C10 1.501(18) . ? Fe6 O6W 2.073(13) . ? Fe6 O3W 2.074(13) . ? Fe6 O4W 2.074(14) . ? Fe6 O1W 2.092(11) . ? Fe6 O5W 2.172(10) . ? Fe6 O2W 2.172(10) . ? N1 C12 1.39(3) . ? C11 C12 1.38(5) . ? 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 _geom_angle_publ_flag O2 Fe1 O2 159.3(5) . 2_655 ? O2 Fe1 O1 85.4(4) . 2_655 ? O2 Fe1 O1 79.5(3) 2_655 2_655 ? O2 Fe1 O1 79.5(3) . . ? O2 Fe1 O1 85.4(4) 2_655 . ? O1 Fe1 O1 86.7(6) 2_655 . ? O2 Fe1 Cl1 93.8(3) . . ? O2 Fe1 Cl1 100.5(3) 2_655 . ? O1 Fe1 Cl1 90.5(3) 2_655 . ? O1 Fe1 Cl1 172.9(3) . . ? O2 Fe1 Cl1 100.5(3) . 2_655 ? O2 Fe1 Cl1 93.8(3) 2_655 2_655 ? O1 Fe1 Cl1 172.9(3) 2_655 2_655 ? O1 Fe1 Cl1 90.5(3) . 2_655 ? Cl1 Fe1 Cl1 93.0(2) . 2_655 ? O6 Fe2 O6 160.3(7) . 2_655 ? O6 Fe2 O5 78.6(4) . . ? O6 Fe2 O5 87.1(4) 2_655 . ? O6 Fe2 O5 87.1(4) . 2_655 ? O6 Fe2 O5 78.6(4) 2_655 2_655 ? O5 Fe2 O5 87.6(7) . 2_655 ? O6 Fe2 Cl2 101.2(4) . . ? O6 Fe2 Cl2 92.8(3) 2_655 . ? O5 Fe2 Cl2 91.8(4) . . ? O5 Fe2 Cl2 171.4(3) 2_655 . ? O6 Fe2 Cl2 92.8(3) . 2_655 ? O6 Fe2 Cl2 101.2(4) 2_655 2_655 ? O5 Fe2 Cl2 171.4(3) . 2_655 ? O5 Fe2 Cl2 91.8(4) 2_655 2_655 ? Cl2 Fe2 Cl2 90.0(4) . 2_655 ? C2 O1 Fe1 114.9(8) . . ? C1 O2 Fe1 115.7(7) . . ? O4 C1 O2 127.4(12) . . ? O4 C1 C2 117.4(12) . . ? O2 C1 C2 115.2(10) . . ? O3 C2 O1 127.2(13) . . ? O3 C2 C1 118.1(11) . . ? O1 C2 C1 114.6(12) . . ? C3 O5 Fe2 115.8(9) . . ? C4 O6 Fe2 115.8(9) . . ? O5 C3 O7 127.6(13) . . ? O5 C3 C4 115.3(12) . . ? O7 C3 C4 117.1(11) . . ? O8 C4 O6 126.0(13) . . ? O8 C4 C3 120.1(12) . . ? O6 C4 C3 113.9(12) . . ? O21 Fe3 O9 102.1(4) . . ? O21 Fe3 O15 86.1(3) . 7_544 ? O9 Fe3 O15 164.7(4) . 7_544 ? O21 Fe3 O10 88.0(4) . . ? O9 Fe3 O10 78.3(3) . . ? O15 Fe3 O10 89.2(4) 7_544 . ? O21 Fe3 O16 162.9(4) . 7_544 ? O9 Fe3 O16 91.3(4) . 7_544 ? O15 Fe3 O16 78.5(3) 7_544 7_544 ? O10 Fe3 O16 84.3(4) . 7_544 ? O21 Fe3 Cl3 96.5(3) . . ? O9 Fe3 Cl3 91.5(3) . . ? O15 Fe3 Cl3 100.4(3) 7_544 . ? O10 Fe3 Cl3 169.6(3) . . ? O16 Fe3 Cl3 93.6(3) 7_544 . ? O21 Fe4 O17 101.9(4) . . ? O21 Fe4 O18 89.3(4) . . ? O17 Fe4 O18 80.1(4) . . ? O21 Fe4 O14 89.0(3) . . ? O17 Fe4 O14 165.7(4) . . ? O18 Fe4 O14 91.0(4) . . ? O21 Fe4 O13 167.0(4) . . ? O17 Fe4 O13 88.6(3) . . ? O18 Fe4 O13 85.0(4) . . ? O14 Fe4 O13 79.5(3) . . ? O21 Fe4 Cl4 94.4(3) . . ? O17 Fe4 Cl4 91.2(3) . . ? O18 Fe4 Cl4 171.1(3) . . ? O14 Fe4 Cl4 97.1(3) . . ? O13 Fe4 Cl4 92.9(3) . . ? C5 O9 Fe3 117.1(8) . . ? C6 O10 Fe3 114.4(8) . . ? O11 C5 O9 126.4(12) . . ? O11 C5 C6 118.1(11) . . ? O9 C5 C6 115.5(11) . . ? O12 C6 O10 127.6(12) . . ? O12 C6 C5 118.5(11) . . ? O10 C6 C5 113.9(11) . . ? C7 O13 Fe4 113.3(8) . . ? C8 O14 Fe4 113.4(7) . . ? C7 O15 Fe3 115.1(8) . 15_445 ? C8 O16 Fe3 112.8(8) . 15_445 ? O13 C7 O15 126.7(12) . . ? O13 C7 C8 117.7(10) . . ? O15 C7 C8 115.5(10) . . ? O16 C8 O14 125.9(12) . . ? O16 C8 C7 118.0(10) . . ? O14 C8 C7 116.1(10) . . ? C9 O17 Fe4 114.1(8) . . ? C10 O18 Fe4 113.5(8) . . ? O19 C9 O17 125.2(12) . . ? O19 C9 C10 118.7(12) . . ? O17 C9 C10 116.0(11) . . ? O20 C10 O18 126.1(11) . . ? O20 C10 C9 118.2(10) . . ? O18 C10 C9 115.6(11) . . ? Fe4 O21 Fe3 134.8(5) . . ? O3 Fe5 O4 67.3(3) . . ? O3 Fe5 O7 77.7(3) . . ? O3 Fe5 O8 76.6(3) . . ? O3 Fe5 O19 140.7(3) . . ? O3 Fe5 O20 149.4(3) . . ? O3 Fe5 O11 113.2(3) . 10_555 ? O3 Fe5 O12 83.6(3) . . ? O4 Fe5 O7 79.0(3) . . ? O4 Fe5 O8 134.8(3) . . ? O4 Fe5 O19 150.9(3) . . ? O4 Fe5 O20 89.3(3) . . ? O4 Fe5 O11 71.1(3) . 10_555 ? O4 Fe5 O12 112.1(3) . 10_555 ? O7 Fe5 O8 67.2(3) . . ? O7 Fe5 O19 110.2(3) . . ? O7 Fe5 O20 78.8(3) . . ? O7 Fe5 O11 139.6(3) . 10_555 ? O7 Fe5 O12 152.5(3) . 10_555 ? O8 Fe5 O19 72.1(3) . . ? O8 Fe5 O20 111.4(3) . . ? O8 Fe5 O11 151.6(3) . 10_555 ? O8 Fe5 O12 89.1(3) . 10_555 ? O19 Fe5 O20 66.7(3) . . ? O19 Fe5 O11 86.1(4) . 10_555 ? O19 Fe5 O12 72.9(3) . 10_555 ? O20 Fe5 O11 74.3(3) . 10_555 ? O20 Fe5 O12 124.8(3) . 10_555 ? O11 Fe5 O12 66.8(3) . 10_555 ? C2 O3 Fe5 119.1(8) . . ? C1 O4 Fe5 116.9(8) . . ? C3 O7 Fe5 120.2(9) . . ? C4 O8 Fe5 115.3(9) . . ? Fe5 O19 C9 118.1(8) . . ? Fe5 O20 C10 117.9(7) . . ? C5 O11 Fe5 117.3(8) . . ? C6 O12 Fe5 117.8(8) . . ? O6W Fe6 O3W 169.4(5) . . ? O6W Fe6 O4W 94.9(6) . . ? O3W Fe6 O4W 89.5(6) . . ? O6W Fe6 O1W 96.4(6) . . ? O3W Fe6 O1W 92.8(6) . . ? O4W Fe6 O1W 95.2(6) . . ? O6W Fe6 O5W 83.9(5) . . ? O3W Fe6 O5W 91.2(5) . . ? O4W Fe6 O5W 176.8(6) . . ? O1W Fe6 O5W 87.9(5) . . ? O6W Fe6 O2W 87.9(6) . . ? O3W Fe6 O2W 82.5(5) . . ? O4W Fe6 O2W 88.8(6) . . ? O1W Fe6 O2W 173.9(5) . . ? O5W Fe6 O2W 88.2(4) . . ? C11 C12 N1 117(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.015 _refine_diff_density_min -2.410 _refine_diff_density_rms 0.202