# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Stuart Batten' _publ_contact_author_email STUART.BATTEN@SCI.MONASH.EDU.AU _publ_section_title ; A Sheet of Clusters: Self-Assembly of a (4,4) Network of FeIII10 Clusters ; loop_ _publ_author_name 'Stuart Batten' 'John D Cashion' 'Boujemaa Moubaraki' 'Keith Murray' 'Sze Nee Pek.' 'David Turner' # Attachment 'SNH4.CIF' data_SNH4 _database_code_depnum_ccdc_archive 'CCDC 668847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Fe10(MeO)14(O)4(Cl)4(mcce)4].4MeOH ; _chemical_name_common (Fe10(MeO)14(O)4(Cl)4(mcce)4).4MeOH _chemical_melting_point ? _chemical_formula_moiety 'C34 H66 Cl4 Fe10 N12 O26, 4(C1 O1 H4)' _chemical_formula_sum 'C38 H82 Cl4 Fe10 N12 O30' _chemical_formula_weight 1887.46 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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' _cell_length_a 10.0043(10) _cell_length_b 20.9189(18) _cell_length_c 17.4170(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.856(3) _cell_angle_gamma 90.00 _cell_volume 3618.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 16030 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1924 _exptl_absorpt_coefficient_mu 2.172 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6819 _exptl_absorpt_correction_T_max 0.7081 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16030 _diffrn_reflns_av_R_equivalents 0.0917 _diffrn_reflns_av_sigmaI/netI 0.1254 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6355 _reflns_number_gt 4117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 6355 _refine_ls_number_parameters 458 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1320 _refine_ls_R_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.1569 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 -0.09916(13) 0.06263(6) 0.29288(7) 0.0237(3) Uani 1 1 d . . . Cl1 Cl 0.2616(3) 0.23312(12) 0.36938(15) 0.0377(6) Uani 1 1 d . . . O1 O -0.1169(6) 0.0386(3) 0.1804(3) 0.0309(16) Uani 1 1 d . . . N1 N -0.2266(11) -0.0062(5) 0.0764(6) 0.071(3) Uani 1 1 d . . . H2N H -0.1575 -0.0310 0.0708 0.085 Uiso 1 1 calc R . . H1N H -0.3003 -0.0087 0.0434 0.085 Uiso 1 1 calc R . . C1 C -0.3365(12) 0.0753(6) 0.1402(6) 0.053(3) Uani 1 1 d . . . Fe2 Fe 0.08799(13) 0.16309(6) 0.38086(8) 0.0241(3) Uani 1 1 d . . . Cl2 Cl -0.2844(2) 0.18666(11) 0.45955(13) 0.0286(6) Uani 1 1 d . . . O2 O -0.4628(8) 0.1517(4) 0.1952(4) 0.054(2) Uani 1 1 d . . . N2 N -0.2585(8) 0.1225(4) 0.2657(5) 0.036(2) Uani 1 1 d . . . H15 H -0.2692 0.1536 0.2985 0.044 Uiso 1 1 calc R . . C2 C -0.4503(15) 0.0716(7) 0.0833(8) 0.085(5) Uani 1 1 d . . . Fe3 Fe 0.09070(12) 0.02303(6) 0.44259(7) 0.0161(3) Uani 1 1 d . . . O3 O 0.1061(6) 0.1209(3) 0.7549(3) 0.0247(15) Uani 1 1 d . . . N3 N -0.5493(14) 0.0635(7) 0.0411(8) 0.138(7) Uani 1 1 d . . . C3 C -0.3452(11) 0.1189(6) 0.2046(7) 0.047(3) Uani 1 1 d . . . Fe4 Fe -0.10328(12) 0.12080(6) 0.50107(7) 0.0182(3) Uani 1 1 d . . . O4 O 0.4059(7) 0.2164(4) 0.6465(4) 0.045(2) Uani 1 1 d . . . N4 N 0.1765(9) 0.1726(4) 0.8600(5) 0.044(2) Uani 1 1 d . . . H3N H 0.1147 0.1539 0.8841 0.053 Uiso 1 1 calc R . . H4N H 0.2324 0.2002 0.8847 0.053 Uiso 1 1 calc R . . C4 C -0.4922(11) 0.1891(6) 0.2611(7) 0.057(3) Uani 1 1 d . . . H4A H -0.4656 0.1651 0.3088 0.085 Uiso 1 1 calc R . . H4B H -0.5889 0.1982 0.2566 0.085 Uiso 1 1 calc R . . H4C H -0.4420 0.2294 0.2626 0.085 Uiso 1 1 calc R . . Fe5 Fe 0.08601(13) 0.08265(6) 0.64771(7) 0.0216(3) Uani 1 1 d . . . O5 O 0.0541(6) 0.1223(3) 0.2786(3) 0.0288(16) Uani 1 1 d . . . N5 N 0.2335(7) 0.1430(3) 0.6211(4) 0.0267(19) Uani 1 1 d . . . H14 H 0.2511 0.1428 0.5728 0.032 Uiso 1 1 calc R . . C5 C -0.2195(12) 0.0371(6) 0.1373(6) 0.048(3) Uani 1 1 d . . . O6 O 0.0453(6) -0.0090(3) 0.3267(3) 0.0218(14) Uani 1 1 d . . . N6 N 0.4469(8) 0.2650(4) 0.8316(4) 0.035(2) Uani 1 1 d . . . C6 C 0.2899(10) 0.1903(5) 0.7480(6) 0.033(2) Uani 1 1 d . . . O7 O -0.0496(5) 0.0917(3) 0.4004(3) 0.0215(14) Uani 1 1 d . . . C7 C 0.3796(10) 0.2308(5) 0.7924(6) 0.034(3) Uani 1 1 d . . . O8 O 0.2176(6) 0.0919(3) 0.4225(3) 0.0188(13) Uani 1 1 d . . . C8 C 0.3043(10) 0.1817(5) 0.6680(5) 0.030(2) Uani 1 1 d . . . O9 O 0.0403(6) 0.1864(3) 0.4831(3) 0.0237(15) Uani 1 1 d . . . C9 C 0.4454(11) 0.2085(5) 0.5713(6) 0.046(3) Uani 1 1 d . . . H9A H 0.4606 0.1630 0.5619 0.069 Uiso 1 1 calc R . . H9B H 0.5286 0.2323 0.5676 0.069 Uiso 1 1 calc R . . H9C H 0.3741 0.2246 0.5327 0.069 Uiso 1 1 calc R . . O10 O 0.2188(5) -0.0438(3) 0.4794(3) 0.0207(14) Uani 1 1 d . . . C10 C 0.1856(10) 0.1590(5) 0.7850(5) 0.030(2) Uani 1 1 d . . . O11 O 0.0413(5) 0.0522(3) 0.5424(3) 0.0167(13) Uani 1 1 d . . . C11 C 0.0812(10) 0.1497(5) 0.2070(5) 0.038(3) Uani 1 1 d . . . H11A H 0.1344 0.1887 0.2171 0.057 Uiso 1 1 calc R . . H11B H -0.0040 0.1600 0.1756 0.057 Uiso 1 1 calc R . . H11C H 0.1317 0.1190 0.1791 0.057 Uiso 1 1 calc R . . O12 O -0.0729(6) 0.1393(3) 0.6133(3) 0.0227(14) Uani 1 1 d . . . C12 C 0.1485(9) -0.0227(5) 0.2783(5) 0.031(2) Uani 1 1 d . . . H12A H 0.2207 -0.0472 0.3078 0.047 Uiso 1 1 calc R . . H12B H 0.1851 0.0175 0.2608 0.047 Uiso 1 1 calc R . . H12C H 0.1101 -0.0477 0.2334 0.047 Uiso 1 1 calc R . . O13 O 0.2119(6) 0.0104(3) 0.6800(3) 0.0239(15) Uani 1 1 d . . . C13 C 0.3399(9) 0.0824(5) 0.3906(6) 0.037(3) Uani 1 1 d . . . H13A H 0.3672 0.0376 0.3967 0.055 Uiso 1 1 calc R . . H13B H 0.4100 0.1098 0.4174 0.055 Uiso 1 1 calc R . . H13C H 0.3270 0.0934 0.3355 0.055 Uiso 1 1 calc R . . C14 C 0.0428(10) 0.2498(4) 0.5145(6) 0.037(3) Uani 1 1 d . . . H14A H 0.1116 0.2751 0.4927 0.055 Uiso 1 1 calc R . . H14B H 0.0641 0.2477 0.5708 0.055 Uiso 1 1 calc R . . H14C H -0.0455 0.2699 0.5014 0.055 Uiso 1 1 calc R . . O14A O -0.261(2) 0.1177(11) 0.8697(16) 0.083(10) Uani 0.44(3) 1 d PD A 1 H14D H -0.2615 0.1572 0.8610 0.099 Uiso 0.44(3) 1 calc PR A 1 O14B O -0.272(2) 0.0543(12) 0.8884(12) 0.101(11) Uani 0.56(3) 1 d PD A 2 H14E H -0.3101 0.0239 0.9084 0.122 Uiso 0.56(3) 1 calc PR A 2 O15 O -0.0045(8) 0.0939(5) 0.9344(5) 0.060(2) Uani 1 1 d . . . H10 H -0.0838 0.0874 0.9142 0.073 Uiso 1 1 calc R . . C15 C 0.3442(10) -0.0330(5) 0.5246(7) 0.047(3) Uani 1 1 d . . . H15A H 0.3565 0.0129 0.5339 0.070 Uiso 1 1 calc R . . H15B H 0.4170 -0.0492 0.4970 0.070 Uiso 1 1 calc R . . H15C H 0.3457 -0.0553 0.5742 0.070 Uiso 1 1 calc R . . C16 C -0.1543(10) 0.1774(5) 0.6548(6) 0.042(3) Uani 1 1 d . . . H16A H -0.1586 0.2208 0.6334 0.064 Uiso 1 1 calc R . . H16B H -0.1160 0.1789 0.7093 0.064 Uiso 1 1 calc R . . H16C H -0.2451 0.1593 0.6507 0.064 Uiso 1 1 calc R . . C17 C 0.3481(10) 0.0226(5) 0.7116(6) 0.045(3) Uani 1 1 d . . . H17A H 0.3495 0.0424 0.7626 0.068 Uiso 1 1 calc R . . H17B H 0.3903 0.0514 0.6772 0.068 Uiso 1 1 calc R . . H17C H 0.3980 -0.0178 0.7166 0.068 Uiso 1 1 calc R . . C18A C -0.393(3) 0.0943(15) 0.859(3) 0.10(2) Uani 0.44(3) 1 d PD A 1 H18D H -0.3934 0.0500 0.8772 0.147 Uiso 0.44(3) 1 calc PR A 1 H18E H -0.4270 0.0960 0.8040 0.147 Uiso 0.44(3) 1 calc PR A 1 H18F H -0.4496 0.1205 0.8885 0.147 Uiso 0.44(3) 1 calc PR A 1 C18B C -0.369(3) 0.097(2) 0.855(4) 0.18(3) Uani 0.56(3) 1 d PD A 2 H18A H -0.4285 0.1095 0.8933 0.277 Uiso 0.56(3) 1 calc PR A 2 H18B H -0.4218 0.0771 0.8106 0.277 Uiso 0.56(3) 1 calc PR A 2 H18C H -0.3242 0.1355 0.8378 0.277 Uiso 0.56(3) 1 calc PR A 2 C19 C -0.006(2) 0.1148(10) 1.0092(9) 0.143(9) Uani 1 1 d . . . H19A H -0.0098 0.0779 1.0435 0.215 Uiso 1 1 calc R . . H19B H -0.0846 0.1421 1.0121 0.215 Uiso 1 1 calc R . . H19C H 0.0764 0.1393 1.0251 0.215 Uiso 1 1 calc R . . 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 0.0255(7) 0.0248(8) 0.0183(7) 0.0018(6) -0.0075(6) 0.0017(6) Cl1 0.0363(14) 0.0312(15) 0.0452(16) 0.0057(13) 0.0032(12) -0.0087(12) O1 0.031(4) 0.037(4) 0.022(4) -0.004(3) -0.008(3) -0.004(3) N1 0.070(8) 0.083(9) 0.052(7) -0.013(6) -0.021(6) 0.023(7) C1 0.053(8) 0.057(8) 0.041(7) -0.015(6) -0.022(6) 0.017(6) Fe2 0.0247(7) 0.0214(7) 0.0245(7) 0.0039(6) -0.0034(6) 0.0008(6) Cl2 0.0258(12) 0.0276(13) 0.0324(14) 0.0062(11) 0.0030(10) 0.0091(10) O2 0.048(5) 0.061(6) 0.048(5) -0.009(4) -0.018(4) 0.022(4) N2 0.032(5) 0.036(5) 0.038(5) 0.005(4) -0.006(4) 0.003(4) C2 0.082(11) 0.081(11) 0.079(10) -0.025(9) -0.049(9) 0.057(9) Fe3 0.0175(6) 0.0143(7) 0.0150(7) 0.0007(5) -0.0043(5) -0.0003(5) O3 0.022(3) 0.033(4) 0.018(3) -0.004(3) -0.001(3) -0.008(3) N3 0.119(12) 0.132(13) 0.132(13) -0.076(11) -0.107(11) 0.050(10) C3 0.046(7) 0.046(7) 0.049(7) 0.017(6) 0.002(6) 0.005(6) Fe4 0.0200(7) 0.0163(7) 0.0167(7) -0.0003(6) -0.0040(5) 0.0027(5) O4 0.043(5) 0.057(5) 0.035(4) -0.008(4) 0.009(3) -0.026(4) N4 0.058(6) 0.047(6) 0.027(5) -0.005(5) 0.001(4) -0.023(5) C4 0.045(7) 0.058(8) 0.065(9) -0.015(7) 0.001(6) 0.010(6) Fe5 0.0250(7) 0.0211(7) 0.0167(7) -0.0033(6) -0.0057(5) -0.0030(6) O5 0.038(4) 0.029(4) 0.019(3) 0.007(3) 0.003(3) 0.003(3) N5 0.031(4) 0.027(5) 0.021(4) -0.013(4) -0.002(3) -0.004(4) C5 0.063(9) 0.053(8) 0.030(6) 0.006(6) 0.009(6) 0.016(7) O6 0.032(4) 0.021(3) 0.011(3) 0.003(3) 0.001(3) -0.007(3) N6 0.047(6) 0.029(5) 0.027(5) -0.017(4) -0.011(4) -0.013(4) C6 0.029(6) 0.037(6) 0.033(6) -0.014(5) -0.002(5) -0.005(5) O7 0.018(3) 0.018(3) 0.025(3) 0.001(3) -0.009(3) -0.008(3) C7 0.038(6) 0.037(6) 0.028(6) -0.008(5) 0.005(5) 0.004(5) O8 0.023(3) 0.014(3) 0.019(3) 0.007(3) 0.002(3) 0.006(3) C8 0.038(6) 0.024(6) 0.031(6) -0.010(5) 0.013(5) 0.001(5) O9 0.031(4) 0.010(3) 0.027(4) 0.000(3) -0.008(3) 0.003(3) C9 0.057(8) 0.055(8) 0.031(6) -0.003(6) 0.024(5) -0.018(6) O10 0.014(3) 0.017(3) 0.029(4) 0.002(3) -0.005(3) 0.000(3) C10 0.050(7) 0.020(5) 0.020(5) 0.009(5) -0.001(5) 0.012(5) O11 0.016(3) 0.014(3) 0.017(3) 0.003(3) -0.010(2) -0.001(2) C11 0.040(6) 0.040(7) 0.034(6) 0.011(5) 0.003(5) 0.006(5) O12 0.030(4) 0.015(3) 0.022(3) -0.004(3) -0.003(3) 0.001(3) C12 0.035(6) 0.037(6) 0.023(5) 0.005(5) 0.009(4) 0.000(5) O13 0.020(3) 0.030(4) 0.018(3) -0.004(3) -0.013(3) -0.001(3) C13 0.028(6) 0.033(6) 0.048(7) 0.012(5) 0.001(5) 0.003(5) C14 0.035(6) 0.011(5) 0.063(8) -0.006(5) 0.004(5) -0.009(4) O14A 0.08(2) 0.037(15) 0.13(2) -0.007(16) 0.013(15) -0.022(13) O14B 0.092(18) 0.13(3) 0.081(16) -0.021(14) 0.021(12) -0.048(16) O15 0.062(6) 0.074(6) 0.047(5) -0.004(5) 0.013(4) -0.010(5) C15 0.028(6) 0.041(7) 0.069(8) 0.020(6) -0.005(5) -0.006(5) C16 0.046(7) 0.048(7) 0.031(6) -0.007(6) -0.007(5) 0.006(6) C17 0.031(6) 0.038(7) 0.060(8) 0.006(6) -0.023(5) 0.000(5) C18A 0.20(7) 0.009(17) 0.07(3) 0.001(18) -0.06(3) 0.00(2) C18B 0.020(18) 0.20(6) 0.33(8) -0.08(5) 0.02(3) 0.01(3) C19 0.19(2) 0.17(2) 0.084(13) -0.076(14) 0.069(13) -0.051(17) _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 O7 1.974(6) . ? Fe1 O13 1.989(6) 3_556 ? Fe1 O1 2.010(6) . ? Fe1 O5 2.015(6) . ? Fe1 N2 2.038(8) . ? Fe1 O6 2.116(6) . ? Cl1 Fe2 2.299(3) . ? O1 C5 1.197(12) . ? N1 C5 1.391(14) . ? N1 H2N 0.8800 . ? N1 H1N 0.8800 . ? C1 C2 1.420(15) . ? C1 C5 1.423(15) . ? C1 C3 1.457(15) . ? Fe2 O9 1.960(6) . ? Fe2 O5 1.968(6) . ? Fe2 O8 2.050(5) . ? Fe2 O7 2.087(6) . ? Fe2 N6 2.168(8) 4_565 ? Cl2 Fe4 2.322(2) . ? O2 C3 1.356(12) . ? O2 C4 1.448(12) . ? N2 C3 1.292(12) . ? N2 H15 0.8800 . ? C2 N3 1.173(15) . ? Fe3 O10 1.952(6) . ? Fe3 O11 1.960(6) . ? Fe3 O8 1.979(6) . ? Fe3 O7 2.080(6) . ? Fe3 O11 2.090(6) 3_556 ? Fe3 O6 2.124(6) . ? O3 C10 1.201(11) . ? O3 Fe5 2.018(6) . ? Fe4 O12 1.979(6) . ? Fe4 O7 1.990(6) . ? Fe4 O10 2.035(6) 3_556 ? Fe4 O9 2.038(6) . ? Fe4 O11 2.103(5) . ? O4 C8 1.338(11) . ? O4 C9 1.422(11) . ? N4 C10 1.350(11) . ? N4 H3N 0.8800 . ? N4 H4N 0.8800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? Fe5 O11 1.944(5) . ? Fe5 O13 2.004(6) . ? Fe5 O12 2.015(6) . ? Fe5 N5 2.037(8) . ? Fe5 O6 2.107(6) 3_556 ? O5 C11 1.427(10) . ? N5 C8 1.299(11) . ? N5 H14 0.8800 . ? O6 C12 1.436(10) . ? O6 Fe5 2.107(6) 3_556 ? N6 C7 1.151(11) . ? N6 Fe2 2.168(8) 4_666 ? C6 C7 1.398(13) . ? C6 C8 1.429(13) . ? C6 C10 1.448(14) . ? O8 C13 1.416(10) . ? O9 C14 1.432(10) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O10 C15 1.417(10) . ? O10 Fe4 2.035(6) 3_556 ? O11 Fe3 2.090(6) 3_556 ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O12 C16 1.402(11) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O13 C17 1.430(10) . ? O13 Fe1 1.989(6) 3_556 ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O14A C18A 1.398(10) . ? O14A H14D 0.8400 . ? O14B C18B 1.397(10) . ? O14B H14E 0.8400 . ? O15 C19 1.374(15) . ? O15 H10 0.8400 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C18B H18A 0.9800 . ? C18B H18B 0.9800 . ? C18B H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 O7 Fe1 O13 95.5(2) . 3_556 ? O7 Fe1 O1 169.8(3) . . ? O13 Fe1 O1 93.0(3) 3_556 . ? O7 Fe1 O5 79.5(2) . . ? O13 Fe1 O5 165.1(2) 3_556 . ? O1 Fe1 O5 90.8(3) . . ? O7 Fe1 N2 97.6(3) . . ? O13 Fe1 N2 94.4(3) 3_556 . ? O1 Fe1 N2 87.2(3) . . ? O5 Fe1 N2 100.2(3) . . ? O7 Fe1 O6 82.4(2) . . ? O13 Fe1 O6 77.2(2) 3_556 . ? O1 Fe1 O6 94.1(2) . . ? O5 Fe1 O6 88.2(2) . . ? N2 Fe1 O6 171.5(3) . . ? C5 O1 Fe1 125.9(7) . . ? C5 N1 H2N 120.0 . . ? C5 N1 H1N 120.0 . . ? H2N N1 H1N 120.0 . . ? C2 C1 C5 122.6(11) . . ? C2 C1 C3 117.1(11) . . ? C5 C1 C3 120.2(10) . . ? O9 Fe2 O5 153.7(3) . . ? O9 Fe2 O8 94.1(2) . . ? O5 Fe2 O8 92.2(2) . . ? O9 Fe2 O7 78.1(2) . . ? O5 Fe2 O7 77.9(2) . . ? O8 Fe2 O7 79.9(2) . . ? O9 Fe2 N6 88.2(3) . 4_565 ? O5 Fe2 N6 84.8(3) . 4_565 ? O8 Fe2 N6 176.9(3) . 4_565 ? O7 Fe2 N6 98.6(3) . 4_565 ? O9 Fe2 Cl1 100.87(19) . . ? O5 Fe2 Cl1 104.4(2) . . ? O8 Fe2 Cl1 92.36(18) . . ? O7 Fe2 Cl1 172.01(18) . . ? N6 Fe2 Cl1 89.2(2) 4_565 . ? C3 O2 C4 115.7(8) . . ? C3 N2 Fe1 125.8(8) . . ? C3 N2 H15 117.1 . . ? Fe1 N2 H15 117.1 . . ? N3 C2 C1 173(2) . . ? O10 Fe3 O11 99.0(2) . . ? O10 Fe3 O8 99.7(2) . . ? O11 Fe3 O8 99.5(2) . . ? O10 Fe3 O7 177.8(2) . . ? O11 Fe3 O7 82.4(2) . . ? O8 Fe3 O7 81.7(2) . . ? O10 Fe3 O11 79.6(2) . 3_556 ? O11 Fe3 O11 83.9(2) . 3_556 ? O8 Fe3 O11 176.6(2) . 3_556 ? O7 Fe3 O11 98.9(2) . 3_556 ? O10 Fe3 O6 98.3(2) . . ? O11 Fe3 O6 153.3(2) . . ? O8 Fe3 O6 97.5(2) . . ? O7 Fe3 O6 79.8(2) . . ? O11 Fe3 O6 79.4(2) 3_556 . ? C10 O3 Fe5 130.9(6) . . ? N2 C3 O2 123.9(11) . . ? N2 C3 C1 125.1(11) . . ? O2 C3 C1 110.8(9) . . ? O12 Fe4 O7 154.7(2) . . ? O12 Fe4 O10 90.7(2) . 3_556 ? O7 Fe4 O10 97.1(2) . 3_556 ? O12 Fe4 O9 89.5(2) . . ? O7 Fe4 O9 78.6(2) . . ? O10 Fe4 O9 169.7(2) 3_556 . ? O12 Fe4 O11 77.1(2) . . ? O7 Fe4 O11 81.1(2) . . ? O10 Fe4 O11 77.5(2) 3_556 . ? O9 Fe4 O11 92.5(2) . . ? O12 Fe4 Cl2 102.35(18) . . ? O7 Fe4 Cl2 100.94(17) . . ? O10 Fe4 Cl2 94.84(17) 3_556 . ? O9 Fe4 Cl2 95.18(17) . . ? O11 Fe4 Cl2 172.28(17) . . ? C8 O4 C9 119.8(8) . . ? C10 N4 H3N 120.0 . . ? C10 N4 H4N 120.0 . . ? H3N N4 H4N 120.0 . . ? O2 C4 H4A 109.5 . . ? O2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O11 Fe5 O13 94.8(2) . . ? O11 Fe5 O12 80.1(2) . . ? O13 Fe5 O12 166.8(2) . . ? O11 Fe5 O3 171.6(2) . . ? O13 Fe5 O3 92.8(2) . . ? O12 Fe5 O3 91.8(2) . . ? O11 Fe5 N5 94.6(3) . . ? O13 Fe5 N5 94.8(3) . . ? O12 Fe5 N5 97.8(3) . . ? O3 Fe5 N5 88.3(3) . . ? O11 Fe5 O6 83.2(2) . 3_556 ? O13 Fe5 O6 77.1(2) . 3_556 ? O12 Fe5 O6 90.2(2) . 3_556 ? O3 Fe5 O6 95.1(2) . 3_556 ? N5 Fe5 O6 171.3(3) . 3_556 ? C11 O5 Fe2 125.9(6) . . ? C11 O5 Fe1 125.7(6) . . ? Fe2 O5 Fe1 102.0(3) . . ? C8 N5 Fe5 126.8(7) . . ? C8 N5 H14 116.6 . . ? Fe5 N5 H14 116.6 . . ? O1 C5 N1 117.2(11) . . ? O1 C5 C1 127.7(11) . . ? N1 C5 C1 115.1(10) . . ? C12 O6 Fe5 119.2(5) . 3_556 ? C12 O6 Fe1 119.5(5) . . ? Fe5 O6 Fe1 98.9(2) 3_556 . ? C12 O6 Fe3 122.2(5) . . ? Fe5 O6 Fe3 95.6(2) 3_556 . ? Fe1 O6 Fe3 95.9(2) . . ? C7 N6 Fe2 166.9(8) . 4_666 ? C7 C6 C8 118.9(9) . . ? C7 C6 C10 118.5(9) . . ? C8 C6 C10 122.6(9) . . ? Fe1 O7 Fe4 150.0(3) . . ? Fe1 O7 Fe3 101.9(3) . . ? Fe4 O7 Fe3 98.1(2) . . ? Fe1 O7 Fe2 99.3(3) . . ? Fe4 O7 Fe2 100.2(2) . . ? Fe3 O7 Fe2 97.0(2) . . ? N6 C7 C6 175.7(11) . . ? C13 O8 Fe3 124.8(5) . . ? C13 O8 Fe2 120.1(5) . . ? Fe3 O8 Fe2 101.5(3) . . ? N5 C8 O4 122.6(9) . . ? N5 C8 C6 125.5(9) . . ? O4 C8 C6 111.9(8) . . ? C14 O9 Fe2 125.6(6) . . ? C14 O9 Fe4 123.1(6) . . ? Fe2 O9 Fe4 102.9(3) . . ? O4 C9 H9A 109.5 . . ? O4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 O10 Fe3 124.8(6) . . ? C15 O10 Fe4 121.1(5) . 3_556 ? Fe3 O10 Fe4 105.0(3) . 3_556 ? O3 C10 N4 116.5(9) . . ? O3 C10 C6 125.5(9) . . ? N4 C10 C6 118.0(9) . . ? Fe5 O11 Fe3 152.3(3) . . ? Fe5 O11 Fe3 101.9(2) . 3_556 ? Fe3 O11 Fe3 96.1(2) . 3_556 ? Fe5 O11 Fe4 99.8(2) . . ? Fe3 O11 Fe4 98.3(2) . . ? Fe3 O11 Fe4 97.9(2) 3_556 . ? O5 C11 H11A 109.5 . . ? O5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C16 O12 Fe4 126.2(5) . . ? C16 O12 Fe5 131.8(5) . . ? Fe4 O12 Fe5 101.7(3) . . ? O6 C12 H12A 109.5 . . ? O6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C17 O13 Fe1 125.9(6) . 3_556 ? C17 O13 Fe5 120.8(6) . . ? Fe1 O13 Fe5 106.9(3) 3_556 . ? O8 C13 H13A 109.5 . . ? O8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O9 C14 H14A 109.5 . . ? O9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18B O14B H14E 109.5 . . ? C19 O15 H10 109.5 . . ? O10 C15 H15A 109.5 . . ? O10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O12 C16 H16A 109.5 . . ? O12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O13 C17 H17A 109.5 . . ? O13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O14B C18B H18A 109.5 . . ? O14B C18B H18B 109.5 . . ? H18A C18B H18B 109.5 . . ? O14B C18B H18C 109.5 . . ? H18A C18B H18C 109.5 . . ? H18B C18B H18C 109.5 . . ? O15 C19 H19A 109.5 . . ? O15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H3N O15 0.88 2.00 2.868(12) 167.5 . N4 H4N Cl2 0.88 2.72 3.415(9) 137.3 4_666 O14A H14D Cl1 0.84 2.31 3.13(2) 165.3 4_566 O14B H14E N3 0.84 2.53 3.36(3) 173.1 3_456 O15 H10 O14A 0.84 1.95 2.72(3) 151.6 . O15 H10 O14B 0.84 2.01 2.82(2) 164.8 . N2 H15 Cl2 0.88 2.91 3.671(9) 145.6 . N1 H2N O15 0.88 2.10 2.976(14) 175.4 3_556 N1 H1N N3 0.88 2.28 3.091(14) 152.5 3_455 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.566 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.142