Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Pradip Mascharak' 'Aura A. Eroy-Reveles' 'Gianna Hoffman-Luca' _publ_contact_author_name 'Pradip Mascharak' _publ_contact_author_address ; Chemistry and Biochemistry University of California, Santa Cruz 1156 High Street Santa Cruz CA 95064 UNITED STATES OF AMERICA ; _publ_contact_author_email PRADIP@CHEMISTRY.UCSC.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Formation of a Triply Bridged ?-oxo Diiron(III) Core Stabilized by Two Deprotonated Carboxamide Groups upon Photorelease of NO ; data_xsc07006 _database_code_depnum_ccdc_archive 'CCDC 652712' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[(PaPy2Q)FeNO](ClO4)2' _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 Fe N6 O2, C2 H3 N, 2(Cl O4)' _chemical_formula_sum 'C26 H25 Cl2 Fe N7 O10' _chemical_formula_weight 722.28 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6291(6) _cell_length_b 12.4527(10) _cell_length_c 15.9134(13) _cell_angle_alpha 73.0200(10) _cell_angle_beta 84.9210(10) _cell_angle_gamma 81.7960(10) _cell_volume 1429.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7774 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.31 _exptl_crystal_description blade _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7925 _exptl_absorpt_correction_T_max 0.9543 _exptl_absorpt_process_details 'Sheldrick, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16200 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.36 _reflns_number_total 6977 _reflns_number_gt 6061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-II v2.1' _computing_cell_refinement 'Bruker SAINT v7.34' _computing_data_reduction 'Bruker SAINT v7.34' _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^)+(0.0368P)^2^+0.7782P] 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_number_reflns 6977 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _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 0.42301(3) 0.295213(18) 0.272890(14) 0.01245(6) Uani 1 1 d . . . Cl1 Cl 0.35138(6) -0.21287(3) 0.36262(3) 0.02203(9) Uani 1 1 d . . . Cl2 Cl 1.08669(5) 0.73536(4) 0.03051(3) 0.02223(9) Uani 1 1 d . . . O1 O 0.93713(15) 0.22524(11) 0.31289(9) 0.0249(3) Uani 1 1 d . . . O2 O 0.13180(17) 0.37253(11) 0.16563(9) 0.0270(3) Uani 1 1 d . . . O3 O 0.2807(2) -0.31307(12) 0.41769(9) 0.0346(3) Uani 1 1 d . . . O4 O 0.4415(2) -0.23881(13) 0.28673(9) 0.0386(4) Uani 1 1 d . . . O5 O 0.4745(2) -0.17910(13) 0.41031(11) 0.0406(4) Uani 1 1 d . . . O6 O 0.2083(2) -0.12307(12) 0.33657(10) 0.0372(3) Uani 1 1 d . . . O7 O 1.00221(18) 0.71922(12) -0.04157(9) 0.0307(3) Uani 1 1 d . . . O8 O 1.26095(18) 0.76621(12) 0.00086(10) 0.0328(3) Uani 1 1 d . . . O9 O 1.1002(2) 0.63113(13) 0.10023(10) 0.0417(4) Uani 1 1 d . . . O10 O 0.9831(2) 0.82267(15) 0.06146(11) 0.0491(4) Uani 1 1 d . . . N1 N 0.55863(17) 0.16676(11) 0.23023(9) 0.0142(3) Uani 1 1 d . . . N2 N 0.63864(17) 0.28002(11) 0.32913(9) 0.0155(3) Uani 1 1 d . . . N3 N 0.34510(17) 0.41058(11) 0.33668(9) 0.0143(3) Uani 1 1 d . . . N4 N 0.52265(17) 0.42280(11) 0.18310(9) 0.0156(3) Uani 1 1 d . . . N5 N 0.31410(17) 0.19512(11) 0.37935(9) 0.0145(3) Uani 1 1 d . . . N6 N 0.24157(17) 0.32972(11) 0.21318(9) 0.0155(3) Uani 1 1 d . . . N7 N 0.8208(3) 0.55887(14) 0.42132(12) 0.0347(4) Uani 1 1 d . . . C1 C 0.5004(2) 0.09907(13) 0.18539(10) 0.0153(3) Uani 1 1 d . . . C2 C 0.3223(2) 0.10954(15) 0.16462(12) 0.0216(3) Uani 1 1 d . . . H2A H 0.2376 0.1640 0.1816 0.026 Uiso 1 1 calc R . . C3 C 0.2704(2) 0.04131(15) 0.11984(12) 0.0222(3) Uani 1 1 d . . . H3A H 0.1502 0.0509 0.1048 0.027 Uiso 1 1 calc R . . C4 C 0.3904(2) -0.04210(14) 0.09577(11) 0.0226(4) Uani 1 1 d . . . H4A H 0.3512 -0.0898 0.0662 0.027 Uiso 1 1 calc R . . C5 C 0.5636(2) -0.05428(14) 0.11503(11) 0.0217(3) Uani 1 1 d . . . H5A H 0.6453 -0.1104 0.0983 0.026 Uiso 1 1 calc R . . C6 C 0.6240(2) 0.01563(13) 0.15975(10) 0.0177(3) Uani 1 1 d . . . C7 C 0.8027(2) 0.00307(14) 0.17989(11) 0.0204(3) Uani 1 1 d . . . H7A H 0.8867 -0.0502 0.1610 0.024 Uiso 1 1 calc R . . C8 C 0.8549(2) 0.06786(14) 0.22670(11) 0.0186(3) Uani 1 1 d . . . H8A H 0.9742 0.0585 0.2429 0.022 Uiso 1 1 calc R . . C9 C 0.7286(2) 0.14839(13) 0.25037(10) 0.0155(3) Uani 1 1 d . . . C10 C 0.7812(2) 0.22194(14) 0.30065(10) 0.0168(3) Uani 1 1 d . . . C11 C 0.6623(2) 0.37084(14) 0.36672(11) 0.0181(3) Uani 1 1 d . . . H11A H 0.7062 0.4354 0.3210 0.022 Uiso 1 1 calc R . . H11B H 0.7474 0.3435 0.4141 0.022 Uiso 1 1 calc R . . C12 C 0.4801(2) 0.40490(14) 0.40276(11) 0.0176(3) Uani 1 1 d . . . H12A H 0.4756 0.4797 0.4135 0.021 Uiso 1 1 calc R . . H12B H 0.4529 0.3489 0.4593 0.021 Uiso 1 1 calc R . . C13 C 0.3245(2) 0.52337(13) 0.26935(11) 0.0182(3) Uani 1 1 d . . . H13A H 0.3359 0.5836 0.2969 0.022 Uiso 1 1 calc R . . H13B H 0.2057 0.5379 0.2450 0.022 Uiso 1 1 calc R . . C14 C 0.4655(2) 0.52452(14) 0.19678(11) 0.0173(3) Uani 1 1 d . . . C15 C 0.5277(2) 0.62223(15) 0.14486(12) 0.0225(4) Uani 1 1 d . . . H15A H 0.4863 0.6930 0.1555 0.027 Uiso 1 1 calc R . . C16 C 0.6522(2) 0.61563(15) 0.07672(12) 0.0262(4) Uani 1 1 d . . . H16A H 0.6961 0.6820 0.0397 0.031 Uiso 1 1 calc R . . C17 C 0.7115(2) 0.51119(16) 0.06330(12) 0.0259(4) Uani 1 1 d . . . H17A H 0.7976 0.5051 0.0175 0.031 Uiso 1 1 calc R . . C18 C 0.6441(2) 0.41590(15) 0.11737(11) 0.0211(3) Uani 1 1 d . . . H18A H 0.6840 0.3443 0.1080 0.025 Uiso 1 1 calc R . . C19 C 0.1747(2) 0.37893(13) 0.38557(11) 0.0167(3) Uani 1 1 d . . . H19A H 0.0763 0.4012 0.3449 0.020 Uiso 1 1 calc R . . H19B H 0.1464 0.4176 0.4322 0.020 Uiso 1 1 calc R . . C20 C 0.1994(2) 0.25330(13) 0.42519(10) 0.0153(3) Uani 1 1 d . . . C21 C 0.1090(2) 0.19861(15) 0.50117(11) 0.0195(3) Uani 1 1 d . . . H21A H 0.0287 0.2405 0.5324 0.023 Uiso 1 1 calc R . . C22 C 0.1373(2) 0.08183(15) 0.53102(11) 0.0216(3) Uani 1 1 d . . . H22A H 0.0760 0.0426 0.5830 0.026 Uiso 1 1 calc R . . C23 C 0.2555(2) 0.02251(15) 0.48463(11) 0.0216(3) Uani 1 1 d . . . H23A H 0.2771 -0.0577 0.5046 0.026 Uiso 1 1 calc R . . C24 C 0.3416(2) 0.08186(13) 0.40875(11) 0.0180(3) Uani 1 1 d . . . H24A H 0.4224 0.0413 0.3766 0.022 Uiso 1 1 calc R . . C25 C 0.8442(3) 0.63292(16) 0.36164(13) 0.0273(4) Uani 1 1 d . . . C26 C 0.8744(3) 0.7286(2) 0.28585(15) 0.0411(5) Uani 1 1 d . . . H26A H 0.7673 0.7835 0.2769 0.062 Uiso 1 1 calc R . . H26B H 0.9029 0.7021 0.2334 0.062 Uiso 1 1 calc R . . H26C H 0.9735 0.7646 0.2962 0.062 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 0.01116(11) 0.01440(11) 0.01341(11) -0.00664(8) -0.00037(8) -0.00128(8) Cl1 0.0257(2) 0.01999(19) 0.0210(2) -0.00780(15) 0.00123(16) -0.00218(15) Cl2 0.0222(2) 0.0255(2) 0.0196(2) -0.00900(16) -0.00169(15) 0.00133(16) O1 0.0127(5) 0.0360(7) 0.0316(7) -0.0184(6) -0.0029(5) -0.0013(5) O2 0.0252(6) 0.0269(7) 0.0298(7) -0.0074(5) -0.0128(5) -0.0002(5) O3 0.0427(8) 0.0271(7) 0.0296(7) -0.0031(6) 0.0099(6) -0.0071(6) O4 0.0486(9) 0.0405(8) 0.0297(8) -0.0168(6) 0.0164(7) -0.0121(7) O5 0.0430(9) 0.0342(8) 0.0528(10) -0.0229(7) -0.0194(7) 0.0013(7) O6 0.0344(8) 0.0293(7) 0.0433(9) -0.0063(6) -0.0079(7) 0.0061(6) O7 0.0275(7) 0.0433(8) 0.0253(7) -0.0144(6) -0.0052(5) -0.0048(6) O8 0.0282(7) 0.0396(8) 0.0360(8) -0.0163(6) 0.0008(6) -0.0113(6) O9 0.0423(9) 0.0406(9) 0.0329(8) 0.0067(7) -0.0080(7) -0.0063(7) O10 0.0507(10) 0.0542(10) 0.0465(10) -0.0328(8) -0.0029(8) 0.0194(8) N1 0.0138(6) 0.0150(6) 0.0150(6) -0.0062(5) 0.0007(5) -0.0019(5) N2 0.0125(6) 0.0193(7) 0.0178(7) -0.0101(5) -0.0020(5) -0.0017(5) N3 0.0142(6) 0.0155(6) 0.0143(6) -0.0063(5) 0.0005(5) -0.0016(5) N4 0.0159(6) 0.0165(6) 0.0153(6) -0.0062(5) 0.0003(5) -0.0022(5) N5 0.0121(6) 0.0169(6) 0.0158(6) -0.0064(5) -0.0010(5) -0.0026(5) N6 0.0150(6) 0.0169(6) 0.0165(7) -0.0079(5) -0.0006(5) -0.0024(5) N7 0.0455(10) 0.0267(9) 0.0350(10) -0.0126(8) -0.0035(8) -0.0051(7) C1 0.0184(7) 0.0143(7) 0.0142(7) -0.0055(6) 0.0020(6) -0.0039(6) C2 0.0195(8) 0.0214(8) 0.0272(9) -0.0125(7) -0.0003(7) -0.0022(6) C3 0.0218(8) 0.0240(9) 0.0242(9) -0.0105(7) -0.0017(7) -0.0059(7) C4 0.0334(9) 0.0208(8) 0.0177(8) -0.0096(7) 0.0014(7) -0.0102(7) C5 0.0290(9) 0.0175(8) 0.0208(8) -0.0103(7) 0.0026(7) -0.0024(7) C6 0.0217(8) 0.0156(7) 0.0162(8) -0.0060(6) 0.0022(6) -0.0021(6) C7 0.0203(8) 0.0175(8) 0.0224(8) -0.0074(6) 0.0032(6) 0.0014(6) C8 0.0146(7) 0.0199(8) 0.0208(8) -0.0063(6) 0.0010(6) -0.0002(6) C9 0.0148(7) 0.0164(7) 0.0155(7) -0.0049(6) 0.0012(6) -0.0026(6) C10 0.0149(7) 0.0193(8) 0.0165(8) -0.0059(6) -0.0002(6) -0.0018(6) C11 0.0157(7) 0.0219(8) 0.0214(8) -0.0123(7) -0.0021(6) -0.0043(6) C12 0.0182(8) 0.0213(8) 0.0175(8) -0.0115(6) -0.0016(6) -0.0030(6) C13 0.0205(8) 0.0162(7) 0.0178(8) -0.0060(6) 0.0014(6) -0.0013(6) C14 0.0185(8) 0.0178(8) 0.0162(8) -0.0058(6) -0.0021(6) -0.0014(6) C15 0.0253(9) 0.0187(8) 0.0235(9) -0.0056(7) 0.0002(7) -0.0042(7) C16 0.0278(9) 0.0235(9) 0.0243(9) -0.0009(7) 0.0037(7) -0.0085(7) C17 0.0237(9) 0.0292(9) 0.0225(9) -0.0056(7) 0.0061(7) -0.0041(7) C18 0.0218(8) 0.0229(8) 0.0189(8) -0.0081(7) 0.0026(6) -0.0020(7) C19 0.0131(7) 0.0193(8) 0.0187(8) -0.0084(6) 0.0023(6) -0.0002(6) C20 0.0124(7) 0.0191(8) 0.0164(7) -0.0080(6) -0.0015(6) -0.0022(6) C21 0.0161(7) 0.0269(9) 0.0182(8) -0.0099(7) 0.0010(6) -0.0050(6) C22 0.0219(8) 0.0265(9) 0.0169(8) -0.0050(7) 0.0016(6) -0.0093(7) C23 0.0232(8) 0.0190(8) 0.0225(8) -0.0040(7) -0.0032(7) -0.0052(7) C24 0.0168(7) 0.0171(8) 0.0213(8) -0.0078(6) -0.0012(6) -0.0013(6) C25 0.0271(9) 0.0281(10) 0.0311(10) -0.0153(8) -0.0030(8) -0.0020(7) C26 0.0352(11) 0.0445(13) 0.0373(12) -0.0010(10) -0.0014(9) -0.0064(10) _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 N6 1.6817(14) . ? Fe1 N2 1.9016(13) . ? Fe1 N5 1.9817(13) . ? Fe1 N3 1.9873(13) . ? Fe1 N4 1.9925(13) . ? Fe1 N1 2.0316(13) . ? Cl1 O4 1.4330(14) . ? Cl1 O5 1.4356(15) . ? Cl1 O6 1.4406(14) . ? Cl1 O3 1.4440(14) . ? Cl2 O10 1.4310(15) . ? Cl2 O8 1.4375(14) . ? Cl2 O9 1.4377(15) . ? Cl2 O7 1.4402(14) . ? O1 C10 1.231(2) . ? O2 N6 1.1435(18) . ? N1 C9 1.335(2) . ? N1 C1 1.390(2) . ? N2 C10 1.338(2) . ? N2 C11 1.463(2) . ? N3 C13 1.494(2) . ? N3 C19 1.4962(19) . ? N3 C12 1.516(2) . ? N4 C18 1.348(2) . ? N4 C14 1.352(2) . ? N5 C24 1.342(2) . ? N5 C20 1.3556(19) . ? N7 C25 1.136(3) . ? C1 C2 1.405(2) . ? C1 C6 1.427(2) . ? C2 C3 1.373(2) . ? C2 H2A 0.9500 . ? C3 C4 1.401(2) . ? C3 H3A 0.9500 . ? C4 C5 1.360(3) . ? C4 H4A 0.9500 . ? C5 C6 1.418(2) . ? C5 H5A 0.9500 . ? C6 C7 1.404(2) . ? C7 C8 1.364(2) . ? C7 H7A 0.9500 . ? C8 C9 1.399(2) . ? C8 H8A 0.9500 . ? C9 C10 1.493(2) . ? C11 C12 1.508(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.505(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.377(2) . ? C15 C16 1.390(2) . ? C15 H15A 0.9500 . ? C16 C17 1.385(3) . ? C16 H16A 0.9500 . ? C17 C18 1.383(2) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.497(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.381(2) . ? C21 C22 1.383(2) . ? C21 H21A 0.9500 . ? C22 C23 1.383(2) . ? C22 H22A 0.9500 . ? C23 C24 1.383(2) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.455(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 N6 Fe1 N2 170.47(6) . . ? N6 Fe1 N5 96.53(6) . . ? N2 Fe1 N5 91.88(6) . . ? N6 Fe1 N3 93.26(6) . . ? N2 Fe1 N3 83.43(6) . . ? N5 Fe1 N3 82.18(5) . . ? N6 Fe1 N4 86.37(6) . . ? N2 Fe1 N4 84.40(6) . . ? N5 Fe1 N4 165.98(5) . . ? N3 Fe1 N4 83.96(5) . . ? N6 Fe1 N1 102.51(6) . . ? N2 Fe1 N1 81.12(5) . . ? N5 Fe1 N1 94.98(5) . . ? N3 Fe1 N1 164.20(6) . . ? N4 Fe1 N1 97.78(5) . . ? O4 Cl1 O5 109.37(10) . . ? O4 Cl1 O6 110.27(10) . . ? O5 Cl1 O6 109.69(9) . . ? O4 Cl1 O3 108.46(9) . . ? O5 Cl1 O3 109.68(10) . . ? O6 Cl1 O3 109.35(9) . . ? O10 Cl2 O8 110.06(10) . . ? O10 Cl2 O9 109.64(10) . . ? O8 Cl2 O9 109.68(9) . . ? O10 Cl2 O7 109.64(9) . . ? O8 Cl2 O7 109.04(8) . . ? O9 Cl2 O7 108.76(9) . . ? C9 N1 C1 118.29(13) . . ? C9 N1 Fe1 111.80(10) . . ? C1 N1 Fe1 129.91(11) . . ? C10 N2 C11 119.41(13) . . ? C10 N2 Fe1 117.56(11) . . ? C11 N2 Fe1 116.52(10) . . ? C13 N3 C19 113.18(12) . . ? C13 N3 C12 111.72(12) . . ? C19 N3 C12 108.64(12) . . ? C13 N3 Fe1 107.26(9) . . ? C19 N3 Fe1 105.90(9) . . ? C12 N3 Fe1 109.95(9) . . ? C18 N4 C14 119.65(14) . . ? C18 N4 Fe1 127.25(11) . . ? C14 N4 Fe1 112.95(10) . . ? C24 N5 C20 119.32(14) . . ? C24 N5 Fe1 127.95(11) . . ? C20 N5 Fe1 112.72(10) . . ? O2 N6 Fe1 166.66(13) . . ? N1 C1 C2 122.10(14) . . ? N1 C1 C6 119.40(14) . . ? C2 C1 C6 118.50(15) . . ? C3 C2 C1 120.25(15) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 121.56(16) . . ? C2 C3 H3A 119.2 . . ? C4 C3 H3A 119.2 . . ? C5 C4 C3 119.51(16) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 120.92(15) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C7 C6 C5 121.04(15) . . ? C7 C6 C1 119.72(15) . . ? C5 C6 C1 119.23(15) . . ? C8 C7 C6 119.60(15) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C7 C8 C9 118.46(15) . . ? C7 C8 H8A 120.8 . . ? C9 C8 H8A 120.8 . . ? N1 C9 C8 124.44(15) . . ? N1 C9 C10 115.52(13) . . ? C8 C9 C10 120.03(14) . . ? O1 C10 N2 126.68(15) . . ? O1 C10 C9 122.29(14) . . ? N2 C10 C9 111.03(13) . . ? N2 C11 C12 104.65(12) . . ? N2 C11 H11A 110.8 . . ? C12 C11 H11A 110.8 . . ? N2 C11 H11B 110.8 . . ? C12 C11 H11B 110.8 . . ? H11A C11 H11B 108.9 . . ? C11 C12 N3 108.90(12) . . ? C11 C12 H12A 109.9 . . ? N3 C12 H12A 109.9 . . ? C11 C12 H12B 109.9 . . ? N3 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N3 C13 C14 109.21(13) . . ? N3 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? N3 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C15 121.63(15) . . ? N4 C14 C13 115.30(14) . . ? C15 C14 C13 123.01(15) . . ? C14 C15 C16 118.93(16) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C17 C16 C15 119.30(16) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C18 C17 C16 119.27(16) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? N4 C18 C17 121.22(16) . . ? N4 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? N3 C19 C20 106.99(12) . . ? N3 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? N3 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? N5 C20 C21 121.51(15) . . ? N5 C20 C19 115.08(13) . . ? C21 C20 C19 123.38(14) . . ? C20 C21 C22 118.94(15) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C21 C22 C23 119.54(15) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C24 C23 C22 118.92(16) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? N5 C24 C23 121.75(15) . . ? N5 C24 H24A 119.1 . . ? C23 C24 H24A 119.1 . . ? N7 C25 C26 179.3(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Fe1 N1 C9 162.13(11) . . . . ? N2 Fe1 N1 C9 -8.91(11) . . . . ? N5 Fe1 N1 C9 -100.03(11) . . . . ? N3 Fe1 N1 C9 -21.2(3) . . . . ? N4 Fe1 N1 C9 74.14(11) . . . . ? N6 Fe1 N1 C1 -18.02(14) . . . . ? N2 Fe1 N1 C1 170.94(14) . . . . ? N5 Fe1 N1 C1 79.81(14) . . . . ? N3 Fe1 N1 C1 158.65(17) . . . . ? N4 Fe1 N1 C1 -106.01(13) . . . . ? N6 Fe1 N2 C10 -97.2(4) . . . . ? N5 Fe1 N2 C10 110.78(12) . . . . ? N3 Fe1 N2 C10 -167.31(13) . . . . ? N4 Fe1 N2 C10 -82.76(12) . . . . ? N1 Fe1 N2 C10 16.03(12) . . . . ? N6 Fe1 N2 C11 54.4(4) . . . . ? N5 Fe1 N2 C11 -97.64(11) . . . . ? N3 Fe1 N2 C11 -15.74(11) . . . . ? N4 Fe1 N2 C11 68.81(11) . . . . ? N1 Fe1 N2 C11 167.60(12) . . . . ? N6 Fe1 N3 C13 -59.54(11) . . . . ? N2 Fe1 N3 C13 111.49(10) . . . . ? N5 Fe1 N3 C13 -155.70(10) . . . . ? N4 Fe1 N3 C13 26.46(10) . . . . ? N1 Fe1 N3 C13 123.71(19) . . . . ? N6 Fe1 N3 C19 61.59(10) . . . . ? N2 Fe1 N3 C19 -127.37(10) . . . . ? N5 Fe1 N3 C19 -34.56(10) . . . . ? N4 Fe1 N3 C19 147.59(10) . . . . ? N1 Fe1 N3 C19 -115.16(19) . . . . ? N6 Fe1 N3 C12 178.78(10) . . . . ? N2 Fe1 N3 C12 -10.19(10) . . . . ? N5 Fe1 N3 C12 82.63(10) . . . . ? N4 Fe1 N3 C12 -95.22(10) . . . . ? N1 Fe1 N3 C12 2.0(2) . . . . ? N6 Fe1 N4 C18 -102.69(15) . . . . ? N2 Fe1 N4 C18 79.68(14) . . . . ? N5 Fe1 N4 C18 154.8(2) . . . . ? N3 Fe1 N4 C18 163.64(15) . . . . ? N1 Fe1 N4 C18 -0.54(15) . . . . ? N6 Fe1 N4 C14 81.91(12) . . . . ? N2 Fe1 N4 C14 -95.72(12) . . . . ? N5 Fe1 N4 C14 -20.6(3) . . . . ? N3 Fe1 N4 C14 -11.77(11) . . . . ? N1 Fe1 N4 C14 -175.94(11) . . . . ? N6 Fe1 N5 C24 106.99(14) . . . . ? N2 Fe1 N5 C24 -77.49(14) . . . . ? N3 Fe1 N5 C24 -160.60(14) . . . . ? N4 Fe1 N5 C24 -151.7(2) . . . . ? N1 Fe1 N5 C24 3.76(14) . . . . ? N6 Fe1 N5 C20 -73.09(11) . . . . ? N2 Fe1 N5 C20 102.43(11) . . . . ? N3 Fe1 N5 C20 19.33(11) . . . . ? N4 Fe1 N5 C20 28.2(3) . . . . ? N1 Fe1 N5 C20 -176.32(11) . . . . ? N2 Fe1 N6 O2 -2.9(8) . . . . ? N5 Fe1 N6 O2 148.9(6) . . . . ? N3 Fe1 N6 O2 66.4(6) . . . . ? N4 Fe1 N6 O2 -17.3(6) . . . . ? N1 Fe1 N6 O2 -114.5(6) . . . . ? C9 N1 C1 C2 177.45(15) . . . . ? Fe1 N1 C1 C2 -2.4(2) . . . . ? C9 N1 C1 C6 -2.2(2) . . . . ? Fe1 N1 C1 C6 177.94(11) . . . . ? N1 C1 C2 C3 179.69(15) . . . . ? C6 C1 C2 C3 -0.6(2) . . . . ? C1 C2 C3 C4 1.8(3) . . . . ? C2 C3 C4 C5 -1.7(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C4 C5 C6 C7 179.87(16) . . . . ? C4 C5 C6 C1 0.6(2) . . . . ? N1 C1 C6 C7 -0.1(2) . . . . ? C2 C1 C6 C7 -179.82(15) . . . . ? N1 C1 C6 C5 179.18(14) . . . . ? C2 C1 C6 C5 -0.5(2) . . . . ? C5 C6 C7 C8 -176.81(16) . . . . ? C1 C6 C7 C8 2.5(2) . . . . ? C6 C7 C8 C9 -2.4(2) . . . . ? C1 N1 C9 C8 2.4(2) . . . . ? Fe1 N1 C9 C8 -177.76(13) . . . . ? C1 N1 C9 C10 -178.40(13) . . . . ? Fe1 N1 C9 C10 1.47(17) . . . . ? C7 C8 C9 N1 0.0(3) . . . . ? C7 C8 C9 C10 -179.22(15) . . . . ? C11 N2 C10 O1 10.7(3) . . . . ? Fe1 N2 C10 O1 161.40(14) . . . . ? C11 N2 C10 C9 -169.69(13) . . . . ? Fe1 N2 C10 C9 -18.97(17) . . . . ? N1 C9 C10 O1 -169.67(15) . . . . ? C8 C9 C10 O1 9.6(2) . . . . ? N1 C9 C10 N2 10.7(2) . . . . ? C8 C9 C10 N2 -170.05(14) . . . . ? C10 N2 C11 C12 -172.17(14) . . . . ? Fe1 N2 C11 C12 36.81(16) . . . . ? N2 C11 C12 N3 -42.94(16) . . . . ? C13 N3 C12 C11 -86.16(15) . . . . ? C19 N3 C12 C11 148.28(13) . . . . ? Fe1 N3 C12 C11 32.81(15) . . . . ? C19 N3 C13 C14 -152.27(13) . . . . ? C12 N3 C13 C14 84.72(15) . . . . ? Fe1 N3 C13 C14 -35.84(15) . . . . ? C18 N4 C14 C15 0.2(2) . . . . ? Fe1 N4 C14 C15 176.03(13) . . . . ? C18 N4 C14 C13 177.58(15) . . . . ? Fe1 N4 C14 C13 -6.62(18) . . . . ? N3 C13 C14 N4 28.66(19) . . . . ? N3 C13 C14 C15 -154.03(16) . . . . ? N4 C14 C15 C16 0.1(3) . . . . ? C13 C14 C15 C16 -177.03(16) . . . . ? C14 C15 C16 C17 -0.6(3) . . . . ? C15 C16 C17 C18 0.7(3) . . . . ? C14 N4 C18 C17 -0.1(3) . . . . ? Fe1 N4 C18 C17 -175.22(13) . . . . ? C16 C17 C18 N4 -0.4(3) . . . . ? C13 N3 C19 C20 160.21(13) . . . . ? C12 N3 C19 C20 -75.08(15) . . . . ? Fe1 N3 C19 C20 42.98(14) . . . . ? C24 N5 C20 C21 -0.5(2) . . . . ? Fe1 N5 C20 C21 179.56(12) . . . . ? C24 N5 C20 C19 -178.48(14) . . . . ? Fe1 N5 C20 C19 1.59(17) . . . . ? N3 C19 C20 N5 -29.98(18) . . . . ? N3 C19 C20 C21 152.09(15) . . . . ? N5 C20 C21 C22 0.3(2) . . . . ? C19 C20 C21 C22 178.07(16) . . . . ? C20 C21 C22 C23 0.3(3) . . . . ? C21 C22 C23 C24 -0.5(3) . . . . ? C20 N5 C24 C23 0.2(2) . . . . ? Fe1 N5 C24 C23 -179.87(12) . . . . ? C22 C23 C24 N5 0.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.409 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.060 #==== end data_mn1815 _database_code_depnum_ccdc_archive 'CCDC 652713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[QPaPy2)FeOFe(QPaPy2)](ClO4)2.3CH3CN.Et2O' _chemical_melting_point ? _chemical_formula_moiety ; C48 H44 Fe2 N10 O3, C4 H10 O, 2(Cl O4), 2(C2 H3 N), C2 H3 N ; _chemical_formula_sum 'C58 H63 Cl2 Fe2 N13 O12' _chemical_formula_weight 1316.81 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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.6095(10) _cell_length_b 16.2853(8) _cell_length_c 19.6444(10) _cell_angle_alpha 90.00 _cell_angle_beta 110.332(4) _cell_angle_gamma 90.00 _cell_volume 5882.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8275 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 26.4 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details 'SADABS 2.10(Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'Bruker SMART ApexII' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37288 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6751 _reflns_number_gt 4775 _reflns_threshold_expression I>2\\s(I) _computing_data_collection 'Apex2 (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Sheldrick, 1994)' _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^)+(0.0737P)^2^+19.1497P] 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_number_reflns 6751 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1523 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.009 _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 0.43348(2) 0.58805(3) 0.18148(2) 0.01820(13) Uani 1 1 d . . . O1 O 0.49859(11) 0.65968(13) 0.34940(11) 0.0221(5) Uani 1 1 d . . . O2 O 0.5000 0.52964(18) 0.2500 0.0203(6) Uani 1 2 d S . . N1 N 0.33327(16) 0.73826(18) 0.34000(15) 0.0302(6) Uani 1 1 d . . . N2 N 0.40762(14) 0.68307(16) 0.24100(13) 0.0217(5) Uani 1 1 d . . . N3 N 0.34168(13) 0.52161(16) 0.19016(13) 0.0219(5) Uani 1 1 d . . . N4 N 0.34045(14) 0.64573(17) 0.09456(13) 0.0226(5) Uani 1 1 d . . . N5 N 0.42228(13) 0.51910(16) 0.08344(13) 0.0216(5) Uani 1 1 d . . . C1 C 0.3029(2) 0.7787(2) 0.38371(19) 0.0359(9) Uani 1 1 d . . . C2 C 0.2261(2) 0.7765(3) 0.3642(2) 0.0463(10) Uani 1 1 d . . . H2 H 0.1973 0.7472 0.3222 0.056 Uiso 1 1 calc R . . C3 C 0.1934(3) 0.8169(3) 0.4061(3) 0.0575(13) Uani 1 1 d . . . H3 H 0.1420 0.8154 0.3931 0.069 Uiso 1 1 calc R . . C4 C 0.2351(3) 0.8599(3) 0.4675(3) 0.0600(15) Uani 1 1 d . . . H4 H 0.2116 0.8872 0.4961 0.072 Uiso 1 1 calc R . . C5 C 0.3084(3) 0.8639(3) 0.4877(2) 0.0562(13) Uani 1 1 d . . . H5 H 0.3357 0.8939 0.5298 0.067 Uiso 1 1 calc R . . C6 C 0.3450(2) 0.8225(3) 0.4453(2) 0.0433(10) Uani 1 1 d . . . C7 C 0.4205(2) 0.8253(3) 0.46149(19) 0.0447(10) Uani 1 1 d . . . H7 H 0.4506 0.8545 0.5029 0.054 Uiso 1 1 calc R . . C8 C 0.4503(2) 0.7858(2) 0.41749(19) 0.0360(8) Uani 1 1 d . . . H8 H 0.5013 0.7871 0.4278 0.043 Uiso 1 1 calc R . . C9 C 0.40430(18) 0.7431(2) 0.35639(17) 0.0271(7) Uani 1 1 d . . . C10 C 0.43781(16) 0.69324(19) 0.31092(16) 0.0211(6) Uani 1 1 d . . . C11 C 0.34138(18) 0.7291(2) 0.19855(16) 0.0262(7) Uani 1 1 d . . . H11A H 0.3435 0.7857 0.2176 0.031 Uiso 1 1 calc R . . H11B H 0.2976 0.7018 0.2020 0.031 Uiso 1 1 calc R . . C12 C 0.33795(18) 0.7310(2) 0.11993(17) 0.0262(7) Uani 1 1 d . . . H12A H 0.2924 0.7581 0.0892 0.031 Uiso 1 1 calc R . . H12B H 0.3795 0.7628 0.1161 0.031 Uiso 1 1 calc R . . C13 C 0.34746(17) 0.4654(2) 0.24201(16) 0.0239(6) Uani 1 1 d . . . H13 H 0.3945 0.4508 0.2743 0.029 Uiso 1 1 calc R . . C14 C 0.28754(18) 0.4282(2) 0.25008(18) 0.0281(7) Uani 1 1 d . . . H14 H 0.2931 0.3877 0.2865 0.034 Uiso 1 1 calc R . . C15 C 0.21882(18) 0.4512(2) 0.20376(19) 0.0320(8) Uani 1 1 d . . . H15 H 0.1766 0.4270 0.2085 0.038 Uiso 1 1 calc R . . C16 C 0.21256(17) 0.5093(2) 0.15100(18) 0.0308(8) Uani 1 1 d . . . H16 H 0.1660 0.5262 0.1193 0.037 Uiso 1 1 calc R . . C17 C 0.27547(16) 0.5431(2) 0.14474(16) 0.0229(6) Uani 1 1 d . . . C18 C 0.27141(17) 0.6006(2) 0.08384(17) 0.0276(7) Uani 1 1 d . . . H18A H 0.2583 0.5689 0.0381 0.033 Uiso 1 1 calc R . . H18B H 0.2322 0.6410 0.0785 0.033 Uiso 1 1 calc R . . C19 C 0.35834(18) 0.6422(2) 0.02707(16) 0.0251(7) Uani 1 1 d . . . H19A H 0.3953 0.6843 0.0288 0.030 Uiso 1 1 calc R . . H19B H 0.3143 0.6535 -0.0156 0.030 Uiso 1 1 calc R . . C20 C 0.38727(16) 0.5577(2) 0.02059(16) 0.0237(7) Uani 1 1 d . . . C21 C 0.38088(19) 0.5235(2) -0.04609(18) 0.0320(8) Uani 1 1 d . . . H21A H 0.3565 0.5522 -0.0899 0.038 Uiso 1 1 calc R . . C22 C 0.4107(2) 0.4468(2) -0.0475(2) 0.0364(8) Uani 1 1 d . . . H22 H 0.4069 0.4220 -0.0925 0.044 Uiso 1 1 calc R . . C23 C 0.44593(19) 0.4067(2) 0.0170(2) 0.0322(8) Uani 1 1 d . . . H23 H 0.4663 0.3537 0.0170 0.039 Uiso 1 1 calc R . . C24 C 0.45124(17) 0.4446(2) 0.08150(18) 0.0259(7) Uani 1 1 d . . . H24 H 0.4761 0.4172 0.1259 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.60520(5) 0.22206(6) 0.12159(5) 0.0374(2) Uani 1 1 d . . . O4 O 0.60004(17) 0.1753(2) 0.05837(16) 0.0603(9) Uani 1 1 d . A . O5 O 0.6239(9) 0.1773(11) 0.1838(9) 0.076(5) Uani 0.533(11) 1 d P A 1 O6 O 0.6748(3) 0.2692(4) 0.1288(3) 0.048(2) Uani 0.533(11) 1 d P A 1 O7 O 0.5524(5) 0.2769(7) 0.1065(4) 0.078(4) Uani 0.533(11) 1 d P A 1 O5B O 0.6519(10) 0.1893(13) 0.1865(10) 0.087(7) Uani 0.467(11) 1 d P A 2 O6B O 0.6086(11) 0.3059(6) 0.1219(5) 0.134(8) Uani 0.467(11) 1 d P A 2 O7B O 0.5304(5) 0.2083(10) 0.1267(6) 0.111(5) Uani 0.467(11) 1 d P A 2 N6 N 0.6930(2) 0.9347(3) 0.3872(2) 0.0508(9) Uani 1 1 d . . . C25 C 0.6916(4) 0.9935(3) 0.3609(3) 0.0672(15) Uani 1 1 d . . . C26 C 0.6929(7) 1.0729(4) 0.3276(4) 0.167(5) Uani 1 1 d . . . H26A H 0.7154 1.1136 0.3655 0.250 Uiso 1 1 calc R . . H26B H 0.6430 1.0898 0.2996 0.250 Uiso 1 1 calc R . . H26C H 0.7211 1.0687 0.2952 0.250 Uiso 1 1 calc R . . N7 N 0.494(2) 0.3267(12) 0.2463(16) 0.196(10) Uani 0.50 1 d P B -1 C27 C 0.4916(16) 0.2683(8) 0.242(2) 0.102(11) Uani 0.50 1 d P B -1 C28 C 0.4593(9) 0.1920(10) 0.1995(11) 0.149(9) Uani 0.50 1 d P B -1 H28A H 0.4983 0.1580 0.1941 0.223 Uiso 0.50 1 calc PR B -1 H28B H 0.4256 0.2076 0.1514 0.223 Uiso 0.50 1 calc PR B -1 H28C H 0.4331 0.1610 0.2253 0.223 Uiso 0.50 1 calc PR B -1 O3 O 0.5000 -0.0150(4) 0.2500 0.124(3) Uani 1 2 d S . . C29 C 0.4985(4) -0.0684(4) 0.3117(5) 0.102(2) Uani 1 1 d . . . H29A H 0.5404 -0.1066 0.3262 0.122 Uiso 1 1 calc R . . H29B H 0.4531 -0.1009 0.2975 0.122 Uiso 1 1 calc R . . C30 C 0.5029(6) -0.0090(5) 0.3755(7) 0.162(5) Uani 1 1 d . . . H30A H 0.5105 -0.0410 0.4198 0.243 Uiso 1 1 calc R . . H30B H 0.4573 0.0219 0.3634 0.243 Uiso 1 1 calc R . . H30C H 0.5435 0.0292 0.3832 0.243 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 0.0163(2) 0.0248(2) 0.0145(2) -0.00053(17) 0.00659(16) 0.00013(17) O1 0.0231(11) 0.0272(12) 0.0166(10) 0.0003(9) 0.0076(9) 0.0034(9) O2 0.0200(14) 0.0243(15) 0.0184(14) 0.000 0.0088(12) 0.000 N1 0.0349(16) 0.0354(16) 0.0272(14) 0.0087(12) 0.0193(12) 0.0112(13) N2 0.0216(13) 0.0256(13) 0.0186(12) 0.0004(10) 0.0077(10) 0.0038(11) N3 0.0198(12) 0.0306(14) 0.0172(12) -0.0034(11) 0.0088(10) -0.0011(11) N4 0.0214(13) 0.0305(14) 0.0172(12) 0.0016(11) 0.0082(10) 0.0007(11) N5 0.0178(12) 0.0274(14) 0.0209(12) -0.0028(10) 0.0084(10) -0.0037(10) C1 0.047(2) 0.042(2) 0.0259(17) 0.0155(16) 0.0220(16) 0.0212(17) C2 0.048(2) 0.058(3) 0.046(2) 0.020(2) 0.033(2) 0.021(2) C3 0.063(3) 0.072(3) 0.056(3) 0.027(3) 0.044(2) 0.034(3) C4 0.075(3) 0.074(3) 0.049(3) 0.031(2) 0.045(3) 0.051(3) C5 0.083(3) 0.067(3) 0.0258(19) 0.0126(19) 0.028(2) 0.041(3) C6 0.056(2) 0.052(2) 0.0264(18) 0.0119(17) 0.0210(18) 0.033(2) C7 0.055(2) 0.052(2) 0.0208(17) -0.0056(17) 0.0057(17) 0.022(2) C8 0.038(2) 0.040(2) 0.0253(17) -0.0026(15) 0.0051(15) 0.0150(16) C9 0.0354(18) 0.0289(17) 0.0172(14) 0.0030(13) 0.0097(13) 0.0108(14) C10 0.0248(15) 0.0222(15) 0.0193(14) 0.0026(12) 0.0114(12) 0.0030(12) C11 0.0294(17) 0.0309(17) 0.0182(15) 0.0012(13) 0.0079(13) 0.0093(14) C12 0.0303(17) 0.0285(17) 0.0202(15) 0.0016(13) 0.0093(13) 0.0060(14) C13 0.0234(15) 0.0318(17) 0.0172(14) -0.0017(13) 0.0081(12) -0.0018(13) C14 0.0309(17) 0.0344(18) 0.0219(15) -0.0015(13) 0.0127(14) -0.0064(14) C15 0.0256(17) 0.043(2) 0.0316(18) -0.0063(16) 0.0152(14) -0.0113(15) C16 0.0194(16) 0.045(2) 0.0280(17) -0.0045(15) 0.0078(13) -0.0025(14) C17 0.0199(15) 0.0313(17) 0.0187(14) -0.0038(13) 0.0081(12) -0.0010(13) C18 0.0189(15) 0.042(2) 0.0208(15) 0.0016(14) 0.0050(12) 0.0007(14) C19 0.0257(16) 0.0330(18) 0.0162(14) 0.0005(13) 0.0069(12) -0.0005(13) C20 0.0217(15) 0.0323(17) 0.0196(15) -0.0031(13) 0.0101(12) -0.0088(13) C21 0.0351(19) 0.041(2) 0.0214(16) -0.0054(15) 0.0118(14) -0.0092(16) C22 0.045(2) 0.040(2) 0.0309(19) -0.0165(16) 0.0222(17) -0.0143(17) C23 0.0341(18) 0.0298(18) 0.0402(19) -0.0101(16) 0.0224(16) -0.0074(15) C24 0.0231(16) 0.0278(16) 0.0303(17) -0.0052(14) 0.0137(14) -0.0083(13) Cl1 0.0366(5) 0.0412(5) 0.0292(4) 0.0088(4) 0.0048(4) 0.0074(4) O4 0.0545(19) 0.083(2) 0.0342(15) -0.0024(16) 0.0036(14) 0.0148(17) O5 0.119(14) 0.068(6) 0.046(6) 0.040(4) 0.034(9) 0.010(8) O6 0.049(4) 0.063(4) 0.032(3) -0.003(3) 0.015(3) -0.015(3) O7 0.056(5) 0.130(10) 0.045(4) 0.004(5) 0.012(3) 0.062(6) O5B 0.096(12) 0.113(14) 0.030(5) 0.003(7) -0.004(6) 0.071(10) O6B 0.24(2) 0.042(5) 0.062(6) 0.008(4) -0.029(8) -0.034(8) O7B 0.057(5) 0.211(14) 0.084(7) -0.068(8) 0.050(5) -0.049(7) N6 0.054(2) 0.056(2) 0.043(2) 0.0060(18) 0.0165(17) 0.0041(18) C25 0.122(5) 0.050(3) 0.036(2) -0.001(2) 0.036(3) 0.016(3) C26 0.410(17) 0.055(4) 0.077(5) 0.021(3) 0.136(8) 0.059(7) N7 0.29(2) 0.208(16) 0.149(15) 0.145(17) 0.147(16) 0.18(2) C27 0.095(18) 0.067(7) 0.19(3) 0.082(17) 0.10(2) 0.065(13) C28 0.172(17) 0.104(11) 0.27(2) 0.005(12) 0.202(18) 0.010(10) O3 0.135(6) 0.081(5) 0.207(9) 0.000 0.123(7) 0.000 C29 0.090(5) 0.075(4) 0.173(8) 0.014(5) 0.087(5) -0.007(4) C30 0.194(10) 0.099(6) 0.281(13) -0.076(7) 0.195(10) -0.054(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 1.7883(16) . ? Fe1 O1 2.016(2) 2_655 ? Fe1 N2 2.105(3) . ? Fe1 N3 2.157(3) . ? Fe1 N5 2.173(3) . ? Fe1 N4 2.227(3) . ? O1 C10 1.290(4) . ? O1 Fe1 2.016(2) 2_655 ? O2 Fe1 1.7883(16) 2_655 ? N1 C9 1.319(4) . ? N1 C1 1.372(4) . ? N2 C10 1.304(4) . ? N2 C11 1.481(4) . ? N3 C17 1.342(4) . ? N3 C13 1.344(4) . ? N4 C12 1.483(4) . ? N4 C19 1.486(4) . ? N4 C18 1.489(4) . ? N5 C20 1.342(4) . ? N5 C24 1.346(4) . ? C1 C6 1.400(6) . ? C1 C2 1.419(6) . ? C2 C3 1.375(6) . ? C2 H2 0.9500 . ? C3 C4 1.388(8) . ? C3 H3 0.9500 . ? C4 C5 1.353(7) . ? C4 H4 0.9500 . ? C5 C6 1.442(5) . ? C5 H5 0.9500 . ? C6 C7 1.402(6) . ? C7 C8 1.362(5) . ? C7 H7 0.9500 . ? C8 C9 1.409(5) . ? C8 H8 0.9500 . ? C9 C10 1.516(4) . ? C11 C12 1.523(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.379(4) . ? C13 H13 0.9500 . ? C14 C15 1.390(5) . ? C14 H14 0.9500 . ? C15 C16 1.378(5) . ? C15 H15 0.9500 . ? C16 C17 1.395(4) . ? C16 H16 0.9500 . ? C17 C18 1.500(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.510(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.389(4) . ? C21 C22 1.383(5) . ? C21 H21A 0.9500 . ? C22 C23 1.379(5) . ? C22 H22 0.9500 . ? C23 C24 1.381(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? Cl1 O7 1.321(6) . ? Cl1 O5 1.360(13) . ? Cl1 O6B 1.367(9) . ? Cl1 O5B 1.392(18) . ? Cl1 O4 1.430(3) . ? Cl1 O7B 1.522(8) . ? Cl1 O6 1.529(5) . ? N6 C25 1.083(6) . ? C25 C26 1.454(8) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N7 C27 0.95(2) . ? C27 C28 1.51(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O3 C29 1.501(8) . ? O3 C29 1.501(8) 2_655 ? C29 C30 1.561(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 O2 Fe1 O1 98.56(8) . 2_655 ? O2 Fe1 N2 103.08(9) . . ? O1 Fe1 N2 93.07(9) 2_655 . ? O2 Fe1 N3 94.83(9) . . ? O1 Fe1 N3 166.11(9) 2_655 . ? N2 Fe1 N3 87.48(10) . . ? O2 Fe1 N5 102.41(9) . . ? O1 Fe1 N5 84.62(9) 2_655 . ? N2 Fe1 N5 154.46(10) . . ? N3 Fe1 N5 88.90(9) . . ? O2 Fe1 N4 172.00(10) . . ? O1 Fe1 N4 88.63(9) 2_655 . ? N2 Fe1 N4 79.89(10) . . ? N3 Fe1 N4 77.79(10) . . ? N5 Fe1 N4 74.63(10) . . ? C10 O1 Fe1 129.89(19) . 2_655 ? Fe1 O2 Fe1 115.74(16) 2_655 . ? C9 N1 C1 118.1(3) . . ? C10 N2 C11 121.2(3) . . ? C10 N2 Fe1 124.7(2) . . ? C11 N2 Fe1 113.14(18) . . ? C17 N3 C13 119.3(3) . . ? C17 N3 Fe1 117.2(2) . . ? C13 N3 Fe1 123.2(2) . . ? C12 N4 C19 112.4(2) . . ? C12 N4 C18 112.0(2) . . ? C19 N4 C18 109.9(2) . . ? C12 N4 Fe1 104.57(18) . . ? C19 N4 Fe1 106.46(18) . . ? C18 N4 Fe1 111.26(19) . . ? C20 N5 C24 118.8(3) . . ? C20 N5 Fe1 115.8(2) . . ? C24 N5 Fe1 125.2(2) . . ? N1 C1 C6 122.1(3) . . ? N1 C1 C2 118.0(4) . . ? C6 C1 C2 119.9(3) . . ? C3 C2 C1 119.8(5) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 121.5(4) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 120.0(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C7 118.2(3) . . ? C1 C6 C5 118.3(4) . . ? C7 C6 C5 123.5(4) . . ? C8 C7 C6 119.5(4) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C9 119.0(4) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? N1 C9 C8 123.1(3) . . ? N1 C9 C10 117.5(3) . . ? C8 C9 C10 119.1(3) . . ? O1 C10 N2 123.5(3) . . ? O1 C10 C9 112.5(3) . . ? N2 C10 C9 123.9(3) . . ? N2 C11 C12 107.6(2) . . ? N2 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? N2 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N4 C12 C11 109.1(3) . . ? N4 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N4 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N3 C13 C14 122.4(3) . . ? N3 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C13 C14 C15 118.5(3) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 119.4(3) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? N3 C17 C16 121.3(3) . . ? N3 C17 C18 117.7(3) . . ? C16 C17 C18 120.9(3) . . ? N4 C18 C17 113.7(3) . . ? N4 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? N4 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? N4 C19 C20 108.8(3) . . ? N4 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? N4 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? N5 C20 C21 121.9(3) . . ? N5 C20 C19 115.9(3) . . ? C21 C20 C19 122.1(3) . . ? C22 C21 C20 118.8(3) . . ? C22 C21 H21A 120.6 . . ? C20 C21 H21A 120.6 . . ? C23 C22 C21 119.3(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.0(3) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? N5 C24 C23 122.1(3) . . ? N5 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? O7 Cl1 O5 120.7(8) . . ? O5 Cl1 O6B 122.3(10) . . ? O7 Cl1 O5B 132.8(8) . . ? O6B Cl1 O5B 111.3(10) . . ? O7 Cl1 O4 110.6(4) . . ? O5 Cl1 O4 114.3(9) . . ? O6B Cl1 O4 121.6(6) . . ? O5B Cl1 O4 114.7(8) . . ? O6B Cl1 O7B 101.2(10) . . ? O5B Cl1 O7B 103.0(9) . . ? O4 Cl1 O7B 101.5(4) . . ? O7 Cl1 O6 106.7(6) . . ? O5 Cl1 O6 103.5(7) . . ? O4 Cl1 O6 98.0(3) . . ? N6 C25 C26 177.7(9) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N7 C27 C28 150(3) . . ? C29 O3 C29 109.1(7) . 2_655 ? O3 C29 C30 106.2(6) . . ? O3 C29 H29A 110.5 . . ? C30 C29 H29A 110.5 . . ? O3 C29 H29B 110.5 . . ? C30 C29 H29B 110.5 . . ? H29A C29 H29B 108.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.803 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.086