# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Samar Das' 'Sabbani Supriya' _publ_contact_author_name 'Dr Samar Das' _publ_contact_author_address ; School of Chemistry University of Hyderabad Hyderabad Andrapradesh 500 046 INDIA ; _publ_contact_author_email SKDSC@UOHYD.ERNET.IN _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; A cyclic (H2O)4 cluster characterized in the solid state disappears on heating and regenerates from water vapor: a supramolecular reversible gas-solid reaction ; data_1 _database_code_csd 178947 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Fe3(O)(CH3COO)6(C5H5NO)2(H2O).ClO4.4H2O _chemical_formula_sum 'C22 H38 Cl Fe3 N2 O24' _chemical_formula_weight 917.54 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' 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' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M p_b_c_a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.810(3) _cell_length_b 17.682(3) _cell_length_c 24.199(4) _cell_angle_alpha 90.000(14) _cell_angle_beta 90.000(14) _cell_angle_gamma 90.000(14) _cell_volume 7193(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.35 _cell_measurement_theta_max 10.58 _exptl_crystal_description block _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3768 _exptl_absorpt_coefficient_mu 1.362 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8322 _exptl_absorpt_correction_T_max 0.9228 _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 'Enraf-Nonius Mach3 four-circle' _diffrn_measurement_method 'w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% none _diffrn_reflns_number 6296 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 24.96 _reflns_number_total 6296 _reflns_number_gt 3133 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 Software' # already given above _computing_data_reduction Xtal _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2' _computing_publication_material SHELXL-97 # already given above _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 w=1/[\s^2^(Fo^2^)+(0.0794P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6296 _refine_ls_number_parameters 475 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1125 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1756 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.339 _refine_ls_shift/su_max 0.013 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.55205(7) 0.12889(6) 0.40432(5) 0.0310(3) Uani 1 d . . . Fe2 Fe 0.74694(6) 0.14552(6) 0.40364(5) 0.0287(3) Uani 1 d . . . Fe3 Fe 0.63354(7) 0.29479(6) 0.43054(5) 0.0284(3) Uani 1 d . . . O1 O 0.6444(3) 0.1899(3) 0.4127(2) 0.0289(12) Uani 1 d . . . O2 O 0.4501(4) 0.0673(3) 0.3927(3) 0.0536(18) Uani 1 d D . . H2X H 0.4061 0.0260 0.3929 0.064 Uiso 1 d RD . . H2Y H 0.4183 0.0979 0.3726 0.064 Uiso 1 d RD . . O3 O 0.4890(4) 0.2072(3) 0.3647(3) 0.0466(16) Uani 1 d . . . O4 O 0.5523(4) 0.3172(3) 0.3706(3) 0.0420(15) Uani 1 d . . . O5 O 0.5078(4) 0.1593(3) 0.4802(3) 0.0408(15) Uani 1 d . . . O6 O 0.5418(3) 0.2805(3) 0.4827(3) 0.0410(15) Uani 1 d . . . O7 O 0.5906(3) 0.0361(3) 0.4441(3) 0.0465(17) Uani 1 d . . . O8 O 0.7218(3) 0.0482(3) 0.4423(3) 0.0501(18) Uani 1 d . . . O9 O 0.5888(4) 0.0845(4) 0.3319(3) 0.0466(16) Uani 1 d . . . O10 O 0.7203(4) 0.0991(4) 0.3308(3) 0.0498(17) Uani 1 d . . . O11 O 0.7947(3) 0.2341(3) 0.3629(3) 0.0447(16) Uani 1 d . . . O12 O 0.7154(4) 0.3329(3) 0.3770(3) 0.0412(15) Uani 1 d . . . O13 O 0.7895(3) 0.1832(3) 0.4761(3) 0.0419(15) Uani 1 d . . . O14 O 0.7123(4) 0.2826(3) 0.4929(2) 0.0386(15) Uani 1 d . . . O15 O 0.6309(3) 0.4066(3) 0.4522(2) 0.0331(13) Uani 1 d . . . O16 O 0.8578(3) 0.0946(3) 0.3947(2) 0.0343(13) Uani 1 d . . . O21 O 0.4166(7) -0.0739(5) 0.4247(4) 0.117(4) Uani 1 d D . . H21X H 0.4198 -0.0262 0.4128 0.140 Uiso 1 d RD . . H21Y H 0.3545 -0.0940 0.4240 0.140 Uiso 1 d RD . . O22 O 0.3048(7) 0.0932(8) 0.3550(6) 0.157(5) Uani 1 d . . . N1 N 0.6023(4) 0.5171(3) 0.4943(3) 0.0326(16) Uani 1 d . . . H1 H 0.6111 0.5394 0.4633 0.039 Uiso 1 calc R . . N2 N 0.8709(4) -0.0091(4) 0.3406(3) 0.0429(18) Uani 1 d . . . H2 H 0.8505 -0.0355 0.3668 0.052 Uiso 1 calc R . . C1 C 0.5006(5) 0.2748(5) 0.3503(4) 0.037(2) Uani 1 d . . . C2 C 0.4442(7) 0.3054(5) 0.3077(5) 0.062(3) Uani 1 d . . . H2A H 0.3907 0.2919 0.3175 0.094 Uiso 1 calc R . . H2B H 0.4570 0.2843 0.2723 0.094 Uiso 1 calc R . . H2C H 0.4490 0.3594 0.3062 0.094 Uiso 1 calc R . . C3 C 0.5091(5) 0.2230(5) 0.5027(4) 0.034(2) Uani 1 d . . . C4 C 0.4665(6) 0.2339(6) 0.5567(4) 0.055(3) Uani 1 d . . . H4A H 0.4278 0.1945 0.5614 0.082 Uiso 1 calc R . . H4B H 0.4402 0.2821 0.5566 0.082 Uiso 1 calc R . . H4C H 0.5042 0.2321 0.5864 0.082 Uiso 1 calc R . . C5 C 0.6601(5) 0.0131(5) 0.4546(4) 0.035(2) Uani 1 d . . . C6 C 0.6684(6) -0.0600(5) 0.4839(5) 0.055(3) Uani 1 d . . . H6A H 0.6167 -0.0816 0.4897 0.083 Uiso 1 calc R . . H6B H 0.6939 -0.0519 0.5189 0.083 Uiso 1 calc R . . H6C H 0.6999 -0.0939 0.4620 0.083 Uiso 1 calc R . . C7 C 0.6555(5) 0.0791(5) 0.3089(4) 0.036(2) Uani 1 d . . . C8 C 0.6579(6) 0.0472(6) 0.2513(4) 0.058(3) Uani 1 d . . . H8A H 0.6427 0.0857 0.2254 0.087 Uiso 1 calc R . . H8B H 0.6217 0.0054 0.2487 0.087 Uiso 1 calc R . . H8C H 0.7109 0.0302 0.2432 0.087 Uiso 1 calc R . . C9 C 0.7744(5) 0.3013(5) 0.3551(4) 0.034(2) Uani 1 d . . . C10 C 0.8253(7) 0.3480(6) 0.3169(5) 0.065(3) Uani 1 d . . . H10A H 0.8799 0.3327 0.3205 0.098 Uiso 1 calc R . . H10B H 0.8203 0.4005 0.3264 0.098 Uiso 1 calc R . . H10C H 0.8082 0.3404 0.2794 0.098 Uiso 1 calc R . . C11 C 0.7661(5) 0.2370(4) 0.5056(4) 0.034(2) Uani 1 d . . . C12 C 0.8064(7) 0.2481(6) 0.5606(4) 0.061(3) Uani 1 d . . . H12A H 0.8546 0.2764 0.5555 0.092 Uiso 1 calc R . . H12B H 0.8187 0.1997 0.5764 0.092 Uiso 1 calc R . . H12C H 0.7715 0.2753 0.5849 0.092 Uiso 1 calc R . . C13 C 0.6132(5) 0.4406(4) 0.4968(3) 0.0305(19) Uani 1 d . . . C14 C 0.6070(6) 0.4086(5) 0.5496(4) 0.041(2) Uani 1 d . . . H14 H 0.6200 0.3579 0.5547 0.049 Uiso 1 calc R . . C15 C 0.5823(6) 0.4506(6) 0.5933(4) 0.054(3) Uani 1 d . . . H15 H 0.5764 0.4279 0.6277 0.065 Uiso 1 calc R . . C16 C 0.5654(6) 0.5278(6) 0.5871(5) 0.057(3) Uani 1 d . . . H16 H 0.5457 0.5561 0.6165 0.068 Uiso 1 calc R . . C17 C 0.5787(6) 0.5597(5) 0.5375(4) 0.049(3) Uani 1 d . . . H17 H 0.5714 0.6114 0.5329 0.059 Uiso 1 calc R . . C18 C 0.8806(5) 0.0660(5) 0.3487(4) 0.0328(19) Uani 1 d . . . C19 C 0.9172(6) 0.1064(6) 0.3057(4) 0.053(3) Uani 1 d . . . H19 H 0.9275 0.1578 0.3096 0.064 Uiso 1 calc R . . C20 C 0.9376(7) 0.0703(6) 0.2587(4) 0.062(3) Uani 1 d . . . H20 H 0.9609 0.0978 0.2302 0.075 Uiso 1 calc R . . C21 C 0.9249(7) -0.0060(6) 0.2515(4) 0.061(3) Uani 1 d . . . H21 H 0.9390 -0.0296 0.2186 0.073 Uiso 1 calc R . . C22 C 0.8920(6) -0.0454(5) 0.2927(4) 0.054(3) Uani 1 d . . . H22 H 0.8834 -0.0971 0.2889 0.065 Uiso 1 calc R . . Cl Cl 0.6282(5) 0.2687(2) 0.1913(2) 0.130(2) Uani 1 d . . . O17 O 0.6317(12) 0.2146(9) 0.1562(7) 0.228(9) Uani 1 d . . . O18 O 0.5735(17) 0.3262(10) 0.1748(9) 0.288(14) Uani 1 d . . . O19 O 0.6057(17) 0.2423(14) 0.2397(10) 0.350(19) Uani 1 d . . . O20 O 0.6826(17) 0.3118(15) 0.2006(13) 0.309(14) Uani 1 d . . . O23 O 0.2599(13) -0.0551(14) 0.3655(12) 0.358(15) Uani 1 d D . . H23X H 0.2719 -0.0762 0.4050 0.430 Uiso 1 d RD . . H23Y H 0.2793 0.0086 0.3743 0.430 Uiso 1 d RD . . O24 O 0.785(3) 0.312(2) 0.7163(15) 0.60(4) Uani 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 0.0258(6) 0.0311(6) 0.0362(7) 0.0008(5) -0.0005(6) -0.0014(5) Fe2 0.0245(6) 0.0275(6) 0.0340(7) -0.0028(5) 0.0024(6) 0.0016(5) Fe3 0.0293(6) 0.0266(6) 0.0293(6) -0.0010(5) 0.0013(5) 0.0025(5) O1 0.031(3) 0.023(2) 0.033(3) -0.003(2) 0.003(3) 0.001(2) O2 0.043(4) 0.049(4) 0.069(5) 0.009(4) -0.009(4) -0.009(3) O3 0.042(4) 0.042(3) 0.055(5) 0.007(3) -0.017(3) 0.005(3) O4 0.041(3) 0.038(3) 0.047(4) 0.003(3) -0.008(3) 0.001(3) O5 0.044(4) 0.035(3) 0.044(4) 0.002(3) 0.013(3) -0.004(3) O6 0.044(4) 0.036(3) 0.043(4) -0.001(3) 0.015(3) -0.004(3) O7 0.032(3) 0.043(3) 0.065(5) 0.015(3) -0.005(3) 0.003(3) O8 0.033(3) 0.035(3) 0.083(5) 0.021(3) 0.010(3) -0.003(3) O9 0.037(4) 0.062(4) 0.041(4) -0.018(3) 0.005(3) -0.008(3) O10 0.036(4) 0.064(4) 0.050(4) -0.025(3) 0.004(3) 0.004(3) O11 0.038(3) 0.040(3) 0.056(4) 0.004(3) 0.016(3) 0.001(3) O12 0.042(4) 0.038(3) 0.044(4) -0.006(3) 0.018(3) 0.001(3) O13 0.036(3) 0.046(3) 0.043(4) -0.010(3) -0.007(3) 0.008(3) O14 0.044(3) 0.034(3) 0.038(4) -0.012(3) -0.010(3) 0.010(3) O15 0.041(3) 0.021(3) 0.037(3) -0.004(2) 0.000(3) 0.003(2) O16 0.032(3) 0.034(3) 0.037(3) -0.002(3) 0.011(3) 0.000(2) O21 0.168(11) 0.083(6) 0.099(8) 0.012(6) 0.000(8) 0.005(7) O22 0.096(9) 0.222(14) 0.154(12) -0.067(11) -0.026(8) -0.003(9) N1 0.043(4) 0.021(3) 0.034(4) -0.003(3) 0.005(3) -0.002(3) N2 0.052(5) 0.037(4) 0.040(5) 0.003(3) 0.008(4) 0.008(4) C1 0.041(5) 0.036(5) 0.035(5) 0.001(4) -0.005(4) 0.006(4) C2 0.066(7) 0.055(6) 0.066(8) 0.013(6) -0.025(6) 0.003(6) C3 0.026(4) 0.048(5) 0.027(5) 0.001(4) 0.004(4) 0.010(4) C4 0.060(7) 0.062(6) 0.043(6) -0.005(5) 0.014(5) 0.003(5) C5 0.035(5) 0.034(4) 0.035(5) 0.005(4) 0.002(4) 0.006(4) C6 0.037(5) 0.046(5) 0.084(8) 0.027(5) 0.012(6) 0.004(4) C7 0.044(5) 0.036(4) 0.029(5) -0.005(4) -0.001(4) -0.005(4) C8 0.063(7) 0.072(7) 0.038(6) -0.015(5) -0.001(5) 0.008(5) C9 0.030(5) 0.039(5) 0.032(5) 0.010(4) 0.001(4) -0.004(4) C10 0.069(7) 0.062(7) 0.064(8) 0.018(6) 0.027(6) 0.000(6) C11 0.035(5) 0.031(4) 0.035(5) -0.001(4) -0.009(4) 0.000(4) C12 0.083(8) 0.065(6) 0.036(6) -0.015(5) -0.023(6) 0.027(6) C13 0.031(4) 0.022(4) 0.038(5) -0.006(4) 0.005(4) 0.000(3) C14 0.058(6) 0.031(4) 0.035(5) 0.007(4) 0.002(5) 0.000(4) C15 0.061(7) 0.063(6) 0.038(6) 0.001(5) 0.016(5) -0.004(5) C16 0.063(7) 0.054(6) 0.054(7) -0.024(5) -0.004(6) 0.008(5) C17 0.053(6) 0.032(5) 0.061(7) -0.014(5) -0.003(6) 0.003(4) C18 0.024(4) 0.045(5) 0.029(5) -0.001(4) 0.004(4) 0.004(4) C19 0.055(6) 0.050(6) 0.053(7) 0.015(5) 0.017(5) 0.003(5) C20 0.068(7) 0.083(8) 0.036(6) 0.005(6) 0.027(6) 0.004(6) C21 0.079(8) 0.067(7) 0.037(6) -0.005(5) 0.009(6) 0.020(6) C22 0.069(7) 0.047(5) 0.048(6) -0.005(5) -0.006(6) 0.008(5) Cl 0.241(7) 0.071(2) 0.079(3) -0.012(2) 0.002(4) -0.030(3) O17 0.31(2) 0.199(15) 0.170(14) -0.128(13) -0.024(15) 0.011(15) O18 0.48(4) 0.125(13) 0.26(2) -0.002(13) -0.16(3) 0.030(19) O19 0.49(4) 0.31(2) 0.25(2) 0.15(2) 0.24(3) 0.24(3) O20 0.33(3) 0.21(2) 0.38(4) -0.10(2) -0.09(3) -0.05(2) O23 0.24(2) 0.29(3) 0.54(4) -0.07(3) 0.09(3) 0.02(2) O24 0.85(9) 0.54(6) 0.41(5) -0.01(5) 0.12(6) 0.42(7) _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 O1 1.901(5) . ? Fe1 O3 1.989(6) . ? Fe1 O7 2.010(6) . ? Fe1 O9 2.017(6) . ? Fe1 O2 2.049(6) . ? Fe1 O5 2.052(6) . ? Fe2 O1 1.907(5) . ? Fe2 O10 1.996(6) . ? Fe2 O8 2.003(6) . ? Fe2 O13 2.008(6) . ? Fe2 O11 2.018(6) . ? Fe2 O16 2.081(5) . ? Fe3 O1 1.913(5) . ? Fe3 O12 2.007(6) . ? Fe3 O6 2.010(6) . ? Fe3 O14 2.019(6) . ? Fe3 O4 2.030(6) . ? Fe3 O15 2.046(5) . ? O3 C1 1.261(10) . ? O4 C1 1.250(10) . ? O5 C3 1.252(10) . ? O6 C3 1.254(9) . ? O7 C5 1.263(10) . ? O8 C5 1.246(10) . ? O9 C7 1.256(10) . ? O10 C7 1.262(10) . ? O11 C9 1.250(9) . ? O12 C9 1.254(10) . ? O13 C11 1.251(10) . ? O14 C11 1.250(9) . ? O15 C13 1.271(9) . ? O16 C18 1.282(9) . ? N1 C17 1.347(11) . ? N1 C13 1.367(9) . ? N2 C18 1.352(10) . ? N2 C22 1.372(12) . ? C1 C2 1.500(12) . ? C3 C4 1.501(12) . ? C5 C6 1.480(11) . ? C7 C8 1.504(12) . ? C9 C10 1.507(12) . ? C11 C12 1.507(12) . ? C13 C14 1.400(11) . ? C14 C15 1.358(12) . ? C15 C16 1.401(13) . ? C16 C17 1.346(13) . ? C18 C19 1.404(12) . ? C19 C20 1.348(13) . ? C20 C21 1.377(14) . ? C21 C22 1.336(14) . ? Cl O20 1.21(2) . ? Cl O17 1.280(12) . ? Cl O19 1.318(17) . ? Cl O18 1.43(2) . ? 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 O1 Fe1 O3 95.2(2) . . ? O1 Fe1 O7 98.6(2) . . ? O3 Fe1 O7 166.1(2) . . ? O1 Fe1 O9 93.6(2) . . ? O3 Fe1 O9 90.9(3) . . ? O7 Fe1 O9 90.0(3) . . ? O1 Fe1 O2 177.1(2) . . ? O3 Fe1 O2 81.9(2) . . ? O7 Fe1 O2 84.3(2) . . ? O9 Fe1 O2 86.0(3) . . ? O1 Fe1 O5 93.0(2) . . ? O3 Fe1 O5 93.2(3) . . ? O7 Fe1 O5 84.4(3) . . ? O9 Fe1 O5 171.9(2) . . ? O2 Fe1 O5 87.6(3) . . ? O1 Fe2 O10 93.9(2) . . ? O1 Fe2 O8 96.3(2) . . ? O10 Fe2 O8 90.7(3) . . ? O1 Fe2 O13 94.9(2) . . ? O10 Fe2 O13 171.1(2) . . ? O8 Fe2 O13 87.3(3) . . ? O1 Fe2 O11 95.5(2) . . ? O10 Fe2 O11 88.7(3) . . ? O8 Fe2 O11 168.2(2) . . ? O13 Fe2 O11 91.5(3) . . ? O1 Fe2 O16 178.5(2) . . ? O10 Fe2 O16 86.0(2) . . ? O8 Fe2 O16 82.3(2) . . ? O13 Fe2 O16 85.2(2) . . ? O11 Fe2 O16 85.9(2) . . ? O1 Fe3 O12 96.5(2) . . ? O1 Fe3 O6 95.4(2) . . ? O12 Fe3 O6 167.0(2) . . ? O1 Fe3 O14 90.2(2) . . ? O12 Fe3 O14 93.9(3) . . ? O6 Fe3 O14 91.2(3) . . ? O1 Fe3 O4 95.3(2) . . ? O12 Fe3 O4 86.2(3) . . ? O6 Fe3 O4 87.5(3) . . ? O14 Fe3 O4 174.5(2) . . ? O1 Fe3 O15 175.4(2) . . ? O12 Fe3 O15 81.7(2) . . ? O6 Fe3 O15 86.8(2) . . ? O14 Fe3 O15 85.8(2) . . ? O4 Fe3 O15 88.8(2) . . ? Fe1 O1 Fe2 119.5(2) . . ? Fe1 O1 Fe3 119.8(3) . . ? Fe2 O1 Fe3 120.7(3) . . ? C1 O3 Fe1 135.4(6) . . ? C1 O4 Fe3 129.2(5) . . ? C3 O5 Fe1 128.2(5) . . ? C3 O6 Fe3 132.9(5) . . ? C5 O7 Fe1 131.2(5) . . ? C5 O8 Fe2 135.7(6) . . ? C7 O9 Fe1 133.4(6) . . ? C7 O10 Fe2 132.7(6) . . ? C9 O11 Fe2 134.6(6) . . ? C9 O12 Fe3 131.7(5) . . ? C11 O13 Fe2 129.6(6) . . ? C11 O14 Fe3 136.6(5) . . ? C13 O15 Fe3 132.8(5) . . ? C18 O16 Fe2 121.9(5) . . ? C17 N1 C13 123.9(8) . . ? C18 N2 C22 123.4(8) . . ? O4 C1 O3 124.6(8) . . ? O4 C1 C2 119.6(8) . . ? O3 C1 C2 115.8(8) . . ? O5 C3 O6 124.7(8) . . ? O5 C3 C4 119.1(8) . . ? O6 C3 C4 116.1(8) . . ? O8 C5 O7 124.1(7) . . ? O8 C5 C6 118.2(8) . . ? O7 C5 C6 117.7(8) . . ? O9 C7 O10 124.4(8) . . ? O9 C7 C8 117.6(8) . . ? O10 C7 C8 118.0(8) . . ? O11 C9 O12 125.1(8) . . ? O11 C9 C10 117.2(8) . . ? O12 C9 C10 117.7(8) . . ? O14 C11 O13 125.2(8) . . ? O14 C11 C12 117.3(8) . . ? O13 C11 C12 117.5(8) . . ? O15 C13 N1 117.5(7) . . ? O15 C13 C14 126.9(7) . . ? N1 C13 C14 115.6(7) . . ? C15 C14 C13 120.7(8) . . ? C14 C15 C16 120.8(10) . . ? C17 C16 C15 118.0(9) . . ? C16 C17 N1 120.5(8) . . ? O16 C18 N2 118.5(8) . . ? O16 C18 C19 125.1(8) . . ? N2 C18 C19 116.4(8) . . ? C20 C19 C18 119.7(9) . . ? C19 C20 C21 122.0(10) . . ? C22 C21 C20 118.8(10) . . ? C21 C22 N2 119.5(9) . . ? O20 Cl O17 123.9(18) . . ? O20 Cl O19 106(2) . . ? O17 Cl O19 109.8(16) . . ? O20 Cl O18 95.2(15) . . ? O17 Cl O18 112.1(13) . . ? O19 Cl O18 108.4(15) . . ? 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 O2 H2Y O22 0.90 1.96 2.648(13) 132.1 . O21 H21X O2 0.89 1.80 2.675(11) 166.8 . O21 H21Y O23 1.10 2.24 3.02(3) 125.8 . O23 H23Y O22 1.19 1.63 2.74(3) 153.0 . _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.772 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.111