Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ann Schmiedekamp' _publ_contact_author_address ; Science/Engineering Penn State University, Abington 1600 Woodland Rd. Abington Pennsylvania 19001 UNITED STATES OF AMERICA ; _publ_contact_author_email AMS@PSU.EDU _publ_section_title ;A DFT computational study of spin crossover in iron(III) and iron(II) tripodal imidazole complexes. A comparison of experiment with calculations ; loop_ _publ_author_name 'Ann Schmiedekamp' 'Greg Brewer' 'Myro Joy Olida' 'Carol Viragh' 'Peter Y Zavalij' # Attachment 'dftxraydata.cif' data_1295 _database_code_depnum_ccdc_archive 'CCDC 297396' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Fe-complex perchlorite ; _chemical_name_common 'Fe-complex perchlorite' _chemical_formula_moiety '(C18 H24 Fe N10), (C2 H6 O), 2(Cl O4), 0.817(H2 O)' _chemical_formula_sum 'C20 H31.64 Cl2 Fe N10 O9.82' _chemical_formula_weight 696.11 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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.5488(6) _cell_length_b 12.3949(6) _cell_length_c 18.2340(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.7830(10) _cell_angle_gamma 90.00 _cell_volume 3008.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7362 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 30.1 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 1441 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 223(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 'three-circle diffractometer' _diffrn_measurement_method '\w and \f omega scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 0.30 _diffrn_reflns_number 38532 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13657 _reflns_number_gt 12767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker, 1999)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+1.53P], P=(max(Fo^2^,0)+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_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack -0.027(9) _refine_ls_number_reflns 13657 # 7214 w/o Fiedel pairs _refine_ls_number_parameters 974 _refine_ls_number_restraints 242 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.008 _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 0.87681(2) 0.05037(2) 0.450915(17) 0.03445(7) Uani 1 1 d . . . N1 N 1.04653(15) 0.03305(18) 0.37924(12) 0.0454(5) Uani 1 1 d . . . N11 N 0.79749(15) -0.08651(17) 0.49261(11) 0.0401(4) Uani 1 1 d . . . C12 C 0.7573(2) -0.1178(2) 0.54915(16) 0.0514(6) Uani 1 1 d . . . H12 H 0.7623 -0.0794 0.5941 0.047(8) Uiso 1 1 calc R . . N13 N 0.70796(18) -0.2120(2) 0.53470(14) 0.0578(6) Uani 1 1 d . . . H13 H 0.6761 -0.2465 0.5647 0.062(9) Uiso 1 1 calc R . . C14 C 0.7168(2) -0.2436(2) 0.46484(17) 0.0547(7) Uani 1 1 d . . . H14 H 0.6903 -0.3064 0.4397 0.078(11) Uiso 1 1 calc R . . C15 C 0.77181(17) -0.16545(19) 0.43888(13) 0.0414(5) Uani 1 1 d . . . C16 C 0.8100(2) -0.1548(2) 0.37038(14) 0.0455(6) Uani 1 1 d . . . H16 H 0.7983 -0.2085 0.3334 0.044(7) Uiso 1 1 calc R . . N17 N 0.85990(16) -0.07036(17) 0.36187(11) 0.0415(4) Uani 1 1 d . . . C18 C 0.9098(2) -0.0622(3) 0.29775(15) 0.0576(7) Uani 1 1 d . . . H18A H 0.8870 0.0025 0.2686 0.078(11) Uiso 1 1 calc R . . H18B H 0.8939 -0.1254 0.2654 0.061(9) Uiso 1 1 calc R . . C19 C 1.0223(2) -0.0562(3) 0.32709(18) 0.0605(8) Uani 1 1 d . . . H19A H 1.0453 -0.1240 0.3522 0.058(9) Uiso 1 1 calc R . . H19B H 1.0574 -0.0466 0.2852 0.098(13) Uiso 1 1 calc R . . N21 N 0.72890(14) 0.12240(17) 0.40652(11) 0.0392(4) Uani 1 1 d . . . C22 C 0.63262(19) 0.1131(2) 0.40830(14) 0.0486(6) Uani 1 1 d . . . H22 H 0.6041 0.0548 0.4300 0.064(9) Uiso 1 1 calc R . . N23 N 0.58034(17) 0.1976(2) 0.37514(12) 0.0542(6) Uani 1 1 d . . . H23 H 0.5159 0.2071 0.3705 0.088(13) Uiso 1 1 calc RD . . C24 C 0.6445(2) 0.2647(2) 0.35039(15) 0.0502(6) Uani 1 1 d . . . H24 H 0.6289 0.3303 0.3250 0.076(10) Uiso 1 1 calc R . . C25 C 0.73698(18) 0.2182(2) 0.36964(13) 0.0407(5) Uani 1 1 d . . . C26 C 0.8364(2) 0.2523(2) 0.36170(14) 0.0432(5) Uani 1 1 d . . . H26 H 0.8456 0.3144 0.3341 0.060(9) Uiso 1 1 calc R . . N27 N 0.91122(15) 0.19629(16) 0.39306(12) 0.0398(4) Uani 1 1 d . . . C28 C 1.01286(19) 0.2261(2) 0.38436(18) 0.0515(6) Uani 1 1 d . . . H28A H 1.0556 0.2365 0.4335 0.072(10) Uiso 1 1 calc R . . H28B H 1.0112 0.2938 0.3564 0.053(8) Uiso 1 1 calc R . . C29 C 1.0544(2) 0.1372(3) 0.34307(17) 0.0550(7) Uani 1 1 d . . . H29A H 1.0172 0.1344 0.2915 0.055(8) Uiso 1 1 calc R . . H29B H 1.1250 0.1522 0.3416 0.080(11) Uiso 1 1 calc R . . N31 N 0.86665(16) 0.13283(17) 0.55809(11) 0.0424(4) Uani 1 1 d . . . C32 C 0.8047(2) 0.1878(2) 0.59128(18) 0.0564(7) Uani 1 1 d . . . H32 H 0.7438 0.2183 0.5669 0.073(11) Uiso 1 1 calc R . . N33 N 0.8405(3) 0.1945(2) 0.66499(16) 0.0723(8) Uani 1 1 d . . . H33 H 0.8111 0.2271 0.6973 0.077(11) Uiso 1 1 calc R . . C34 C 0.9285(3) 0.1431(3) 0.68060(17) 0.0720(10) Uani 1 1 d . . . H34 H 0.9703 0.1356 0.7276 0.087(12) Uiso 1 1 calc R . . C35 C 0.9453(2) 0.1033(2) 0.61365(14) 0.0491(6) Uani 1 1 d . . . C36 C 1.0247(2) 0.0392(2) 0.59329(14) 0.0533(7) Uani 1 1 d . . . H36 H 1.0814 0.0200 0.6290 0.065(9) Uiso 1 1 calc R . . N37 N 1.01611(15) 0.00925(17) 0.52579(11) 0.0422(4) Uani 1 1 d . . . C38 C 1.0974(2) -0.0506(2) 0.50192(17) 0.0540(7) Uani 1 1 d . . . H38A H 1.0737 -0.1224 0.4843 0.054(8) Uiso 1 1 calc R . . H38B H 1.1535 -0.0593 0.5440 0.051(8) Uiso 1 1 calc R . . C39 C 1.1315(2) 0.0112(3) 0.43983(17) 0.0551(7) Uani 1 1 d . . . H39A H 1.1621 0.0795 0.4593 0.082(11) Uiso 1 1 calc R . . H39B H 1.1824 -0.0308 0.4205 0.050(8) Uiso 1 1 calc R . . Fe2 Fe 0.62726(2) 0.07179(2) 0.065112(17) 0.03668(8) Uani 1 1 d . . . N2 N 0.45008(15) 0.08481(19) 0.14178(11) 0.0435(5) Uani 1 1 d . . . N41 N 0.70011(16) -0.07451(17) 0.03448(11) 0.0422(4) Uani 1 1 d . . . C42 C 0.7484(2) -0.1149(2) -0.01588(16) 0.0525(7) Uani 1 1 d . . . H42 H 0.7528 -0.0816 -0.0615 0.049(8) Uiso 1 1 calc R . . N43 N 0.79028(19) -0.2104(2) 0.00721(15) 0.0615(6) Uani 1 1 d . . . H43 H 0.8255 -0.2507 -0.0173 0.118(16) Uiso 1 1 calc R . . C44 C 0.7684(2) -0.2335(3) 0.07511(19) 0.0594(7) Uani 1 1 d . . . H44 H 0.7873 -0.2953 0.1042 0.083(12) Uiso 1 1 calc R . . C45 C 0.71335(18) -0.1487(2) 0.09233(14) 0.0443(5) Uani 1 1 d . . . C46 C 0.67271(19) -0.1231(2) 0.15791(14) 0.0445(6) Uani 1 1 d . . . H46 H 0.6768 -0.1726 0.1975 0.064(9) Uiso 1 1 calc R . . N47 N 0.63113(14) -0.03160(18) 0.16058(10) 0.0399(4) Uani 1 1 d . . . C48 C 0.5880(2) -0.0041(3) 0.22609(14) 0.0536(7) Uani 1 1 d . . . H48A H 0.6168 0.0638 0.2479 0.063(9) Uiso 1 1 calc R . . H48B H 0.6035 -0.0609 0.2639 0.080(11) Uiso 1 1 calc R . . C49 C 0.4751(2) 0.0072(3) 0.20211(15) 0.0519(6) Uani 1 1 d . . . H49A H 0.4460 -0.0631 0.1856 0.046(8) Uiso 1 1 calc R . . H49B H 0.4460 0.0307 0.2448 0.072(10) Uiso 1 1 calc R . . N51 N 0.63260(16) 0.14320(18) -0.04378(12) 0.0444(5) Uani 1 1 d . . . C52 C 0.6920(2) 0.1963(2) -0.08046(17) 0.0534(7) Uani 1 1 d . . . H52 H 0.7574 0.2195 -0.0599 0.056(9) Uiso 1 1 calc R . . N53 N 0.6458(2) 0.2128(2) -0.15179(14) 0.0621(7) Uani 1 1 d . . . H53 H 0.6716 0.2459 -0.1858 0.111(15) Uiso 1 1 calc R . . C54 C 0.5529(3) 0.1696(3) -0.16148(16) 0.0588(7) Uani 1 1 d . . . H54 H 0.5041 0.1690 -0.2055 0.067(10) Uiso 1 1 calc R . . C55 C 0.5446(2) 0.1270(2) -0.09443(13) 0.0465(6) Uani 1 1 d . . . C56 C 0.46460(19) 0.0693(3) -0.06853(13) 0.0495(6) Uani 1 1 d . . . H56 H 0.4025 0.0576 -0.1004 0.077(10) Uiso 1 1 calc R . . N57 N 0.48061(16) 0.03502(18) -0.00184(11) 0.0445(5) Uani 1 1 d . . . C58 C 0.3982(2) -0.0170(3) 0.02685(16) 0.0576(7) Uani 1 1 d . . . H58A H 0.4208 -0.0867 0.0494 0.067(10) Uiso 1 1 calc R . . H58B H 0.3416 -0.0300 -0.0142 0.068(9) Uiso 1 1 calc R . . C59 C 0.36551(18) 0.0552(3) 0.08452(14) 0.0545(7) Uani 1 1 d . . . H59A H 0.3343 0.1205 0.0602 0.081(11) Uiso 1 1 calc R . . H59B H 0.3153 0.0176 0.1074 0.071(10) Uiso 1 1 calc R . . N61 N 0.77806(15) 0.13569(18) 0.10810(11) 0.0423(4) Uani 1 1 d . . . C62 C 0.8738(2) 0.1151(3) 0.11103(15) 0.0554(7) Uani 1 1 d . . . H62 H 0.8995 0.0498 0.0962 0.051(8) Uiso 1 1 calc R . . N63 N 0.93008(18) 0.2012(3) 0.13837(15) 0.0668(7) Uani 1 1 d . . . H63 H 0.9952 0.2053 0.1445 0.119(17) Uiso 1 1 calc R . . C64 C 0.8688(2) 0.2793(3) 0.15457(18) 0.0624(8) Uani 1 1 d . . . H64 H 0.8877 0.3475 0.1750 0.068(9) Uiso 1 1 calc R . . C65 C 0.7738(2) 0.2394(2) 0.13543(14) 0.0461(6) Uani 1 1 d . . . C66 C 0.6760(2) 0.2832(2) 0.13802(16) 0.0484(6) Uani 1 1 d . . . H66 H 0.6694 0.3517 0.1588 0.065(9) Uiso 1 1 calc R . . N67 N 0.59920(15) 0.22777(17) 0.11184(12) 0.0426(4) Uani 1 1 d . . . C68 C 0.4991(2) 0.2691(2) 0.11610(19) 0.0565(7) Uani 1 1 d . . . H68A H 0.4572 0.2709 0.0661 0.052(8) Uiso 1 1 calc R . . H68B H 0.5045 0.3428 0.1360 0.065(9) Uiso 1 1 calc R . . C69 C 0.4516(2) 0.1969(2) 0.16628(17) 0.0537(7) Uani 1 1 d . . . H69A H 0.4894 0.2022 0.2175 0.059(9) Uiso 1 1 calc R . . H69B H 0.3827 0.2210 0.1662 0.064(9) Uiso 1 1 calc R . . Cl1 Cl 0.72254(10) 0.54908(10) 0.26563(5) 0.0463(3) Uani 0.797(3) 1 d PDU A 1 O11 O 0.6289(2) 0.4953(2) 0.23931(16) 0.0679(8) Uani 0.797(3) 1 d PDU A 1 O12 O 0.7373(2) 0.5653(4) 0.34351(13) 0.0854(11) Uani 0.797(3) 1 d PDU A 1 O13 O 0.8030(2) 0.4819(3) 0.24926(19) 0.0729(10) Uani 0.797(3) 1 d PDU A 1 O14 O 0.7224(4) 0.6490(3) 0.2282(2) 0.1086(16) Uani 0.797(3) 1 d PDU A 1 Cl1A Cl 0.7541(4) 0.5682(4) 0.2417(4) 0.0652(16) Uani 0.203(3) 1 d PDU A 2 O11A O 0.7524(10) 0.5281(11) 0.1678(6) 0.097(4) Uani 0.203(3) 1 d PDU A 2 O12A O 0.8309(8) 0.6433(9) 0.2584(6) 0.078(4) Uani 0.203(3) 1 d PDU A 2 O13A O 0.6601(9) 0.6246(14) 0.2452(9) 0.114(6) Uani 0.203(3) 1 d PDU A 2 O14A O 0.7631(10) 0.4809(10) 0.2927(9) 0.107(6) Uani 0.203(3) 1 d PDU A 2 Cl2 Cl 0.56569(6) 0.31904(7) 0.63491(4) 0.0649(2) Uani 0.711(6) 1 d PDU B 1 O21 O 0.56833(19) 0.2586(2) 0.56930(13) 0.0746(6) Uani 0.711(6) 1 d PDU B 1 O22 O 0.6531(3) 0.3083(4) 0.6912(2) 0.0666(11) Uani 0.711(6) 1 d PDU B 1 O23 O 0.4818(3) 0.2674(3) 0.67110(19) 0.0822(13) Uani 0.711(6) 1 d PDU B 1 O24 O 0.5373(4) 0.4235(3) 0.6206(3) 0.0787(14) Uani 0.711(6) 1 d PDU B 1 Cl2A Cl 0.56569(6) 0.31904(7) 0.63491(4) 0.0649(2) Uani 0.289(6) 1 d PDU B 2 O21A O 0.56833(19) 0.2586(2) 0.56930(13) 0.0746(6) Uani 0.289(6) 1 d PDU B 2 O22A O 0.4904(8) 0.3936(11) 0.6311(8) 0.107(5) Uani 0.289(6) 1 d PDU B 2 O23A O 0.6547(7) 0.4013(8) 0.6219(7) 0.107(4) Uani 0.289(6) 1 d PDU B 2 O24A O 0.6086(12) 0.2637(11) 0.6942(6) 0.130(5) Uani 0.289(6) 1 d PDU B 2 Cl3 Cl 0.90579(6) 0.36665(8) 0.86288(4) 0.0668(2) Uani 1 1 d U . . O31 O 0.8300(2) 0.3176(3) 0.80976(14) 0.0903(9) Uani 1 1 d U . . O32 O 0.8921(3) 0.3399(4) 0.93578(14) 0.1314(15) Uani 1 1 d U . . O33 O 0.9017(3) 0.4813(3) 0.85203(19) 0.1272(13) Uani 1 1 d U . . O34 O 0.9995(2) 0.3357(4) 0.8504(2) 0.1485(18) Uani 1 1 d U . . Cl4 Cl 0.17598(6) 0.34186(8) 0.21541(4) 0.0649(2) Uani 0.66(3) 1 d PU C 1 O41 O 0.0861(7) 0.3795(13) 0.2397(7) 0.094(3) Uani 0.66(3) 1 d PU C 1 O42 O 0.1514(7) 0.2607(11) 0.1612(6) 0.097(3) Uani 0.66(3) 1 d PU C 1 O43 O 0.2336(3) 0.4254(3) 0.19279(19) 0.1361(15) Uani 0.66(3) 1 d PU C 1 O44 O 0.2405(6) 0.3014(11) 0.2798(4) 0.110(3) Uani 0.66(3) 1 d PU C 1 Cl4A Cl 0.17598(6) 0.34186(8) 0.21541(4) 0.0649(2) Uani 0.34(3) 1 d PU C 2 O41A O 0.2345(11) 0.248(2) 0.2516(18) 0.126(8) Uani 0.34(3) 1 d PU C 2 O42A O 0.111(2) 0.376(2) 0.2561(14) 0.104(6) Uani 0.34(3) 1 d PU C 2 O43A O 0.2336(3) 0.4254(3) 0.19279(19) 0.1361(15) Uani 0.34(3) 1 d PU C 2 O44A O 0.1276(14) 0.301(2) 0.1445(9) 0.085(5) Uani 0.34(3) 1 d PU C 2 O71 O 0.4303(3) 0.3795(3) 0.3333(2) 0.0909(14) Uani 0.761(6) 1 d PD D 1 H71 H 0.3925 0.3789 0.2919 0.136 Uiso 0.761(6) 1 calc PR D 1 C72 C 0.4489(3) 0.4866(3) 0.3571(2) 0.0815(10) Uani 0.761(6) 1 d PD D 1 H72A H 0.3854 0.5224 0.3604 0.098 Uiso 0.761(6) 1 calc PR D 1 H72B H 0.4802 0.5260 0.3209 0.098 Uiso 0.761(6) 1 calc PR D 1 C73 C 0.5141(4) 0.4881(4) 0.4287(2) 0.1000(14) Uani 0.761(6) 1 d PD D 1 H73A H 0.5065 0.4214 0.4548 0.150 Uiso 0.761(6) 1 calc PR D 1 H73B H 0.4967 0.5486 0.4575 0.150 Uiso 0.761(6) 1 calc PR D 1 H73C H 0.5832 0.4954 0.4221 0.150 Uiso 0.761(6) 1 calc PR D 1 O71A O 0.5395(9) 0.5719(7) 0.4751(5) 0.086(4) Uani 0.239(6) 1 d PDU D 2 H71A H 0.5788 0.5512 0.5130 0.128 Uiso 0.239(6) 1 calc PR D 2 C72A C 0.5141(4) 0.4881(4) 0.4287(2) 0.1000(14) Uani 0.239(6) 1 d PDU D 2 H72C H 0.4865 0.4339 0.4584 0.120 Uiso 0.239(6) 1 calc PR D 2 H72D H 0.5780 0.4586 0.4199 0.120 Uiso 0.239(6) 1 calc PR D 2 C73A C 0.4489(3) 0.4866(3) 0.3571(2) 0.0815(10) Uani 0.239(6) 1 d PDU D 2 H73D H 0.3847 0.4555 0.3619 0.122 Uiso 0.239(6) 1 calc PR D 2 H73E H 0.4791 0.4437 0.3227 0.122 Uiso 0.239(6) 1 calc PR D 2 H73F H 0.4387 0.5598 0.3383 0.122 Uiso 0.239(6) 1 calc PR D 2 O81 O 0.9162(4) 0.6177(4) -0.0236(2) 0.0698(11) Uani 0.658(6) 1 d PDU E 1 H81 H 0.9459 0.6324 -0.0582 0.105 Uiso 0.658(6) 1 calc PRD E 1 C82 C 0.9843(6) 0.5761(8) 0.0362(3) 0.111(3) Uani 0.658(6) 1 d PDU E 1 H82A H 1.0157 0.5135 0.0171 0.133 Uiso 0.658(6) 1 calc PR E 1 H82B H 1.0372 0.6305 0.0491 0.133 Uiso 0.658(6) 1 calc PR E 1 C83 C 0.9584(10) 0.5440(13) 0.1026(6) 0.194(5) Uani 0.658(6) 1 d PDU E 1 H83A H 0.8959 0.5039 0.0922 0.291 Uiso 0.658(6) 1 calc PR E 1 H83B H 0.9500 0.6071 0.1323 0.291 Uiso 0.658(6) 1 calc PR E 1 H83C H 1.0110 0.4986 0.1299 0.291 Uiso 0.658(6) 1 calc PR E 1 O81A O 0.8789(6) 0.5920(8) -0.0049(5) 0.0698(11) Uani 0.342(6) 1 d PDU E 2 H81A H 0.8805 0.5538 -0.0421 0.105 Uiso 0.342(6) 1 calc PR E 2 C82A C 0.9342(8) 0.5441(14) 0.0571(6) 0.094(4) Uani 0.342(6) 1 d PDU E 2 H82C H 0.9065 0.4717 0.0609 0.113 Uiso 0.342(6) 1 calc PR E 2 H82D H 0.9222 0.5849 0.1007 0.113 Uiso 0.342(6) 1 calc PR E 2 C83A C 1.0402(8) 0.5329(13) 0.0641(8) 0.105(4) Uani 0.342(6) 1 d PDU E 2 H83D H 1.0705 0.5240 0.1163 0.158 Uiso 0.342(6) 1 calc PR E 2 H83E H 1.0674 0.5968 0.0445 0.158 Uiso 0.342(6) 1 calc PR E 2 H83F H 1.0548 0.4701 0.0362 0.158 Uiso 0.342(6) 1 calc PR E 2 O1W O 0.3735(2) 0.1404(2) 0.37483(17) 0.0853(8) Uani 1 1 d D . . H11W H 0.360(3) 0.1855(19) 0.3371(11) 0.128 Uiso 1 1 d D . . H12W H 0.344(3) 0.084(2) 0.353(2) 0.128 Uiso 1 1 d D . . O2W O 0.2573(4) 0.0422(6) 0.2708(4) 0.145(4) Uani 0.633(10) 1 d PD . . H21W H 0.242(10) 0.078(6) 0.230(3) 0.217 Uiso 0.633(10) 1 d PD . . H22W H 0.263(7) -0.023(3) 0.258(4) 0.217 Uiso 0.633(10) 1 d PD . . 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 0.03605(15) 0.03326(18) 0.03336(14) 0.00057(13) 0.00469(11) -0.00128(13) N1 0.0426(10) 0.0467(13) 0.0500(11) -0.0037(9) 0.0170(9) -0.0002(9) N11 0.0418(10) 0.0397(10) 0.0400(10) 0.0040(8) 0.0105(8) -0.0015(8) C12 0.0539(15) 0.0538(16) 0.0498(14) 0.0083(12) 0.0187(12) 0.0034(13) N13 0.0545(13) 0.0584(15) 0.0642(15) 0.0177(12) 0.0208(12) -0.0084(11) C14 0.0525(15) 0.0449(15) 0.0640(17) 0.0073(13) 0.0040(13) -0.0108(12) C15 0.0390(11) 0.0369(12) 0.0467(12) 0.0034(10) 0.0035(10) -0.0056(10) C16 0.0517(14) 0.0408(14) 0.0413(12) -0.0081(10) 0.0018(11) -0.0088(11) N17 0.0454(11) 0.0458(12) 0.0334(9) -0.0036(8) 0.0080(8) -0.0032(9) C18 0.0720(19) 0.0674(19) 0.0372(13) -0.0130(13) 0.0197(13) -0.0146(15) C19 0.0640(18) 0.063(2) 0.0625(18) -0.0194(15) 0.0324(15) -0.0043(15) N21 0.0336(9) 0.0440(11) 0.0392(10) 0.0017(8) 0.0045(8) -0.0005(8) C22 0.0393(12) 0.0677(18) 0.0389(12) -0.0014(12) 0.0076(10) -0.0050(12) N23 0.0376(11) 0.0787(17) 0.0446(12) -0.0039(11) 0.0035(9) 0.0136(11) C24 0.0494(14) 0.0579(16) 0.0423(13) 0.0024(12) 0.0058(11) 0.0145(12) C25 0.0430(12) 0.0404(13) 0.0379(11) 0.0004(9) 0.0054(10) 0.0040(10) C26 0.0503(14) 0.0351(13) 0.0452(13) 0.0039(10) 0.0115(11) -0.0032(11) N27 0.0395(10) 0.0349(10) 0.0468(11) 0.0020(8) 0.0128(9) -0.0042(8) C28 0.0422(13) 0.0439(14) 0.0711(18) 0.0046(13) 0.0179(13) -0.0084(11) C29 0.0511(15) 0.0622(18) 0.0581(16) 0.0070(14) 0.0270(13) -0.0048(13) N31 0.0451(11) 0.0406(11) 0.0437(11) -0.0072(9) 0.0143(9) -0.0024(9) C32 0.0581(17) 0.0481(16) 0.0701(19) -0.0096(13) 0.0305(15) -0.0031(13) N33 0.106(2) 0.0612(16) 0.0632(16) -0.0189(13) 0.0509(17) -0.0143(16) C34 0.111(3) 0.065(2) 0.0414(15) -0.0095(14) 0.0188(17) -0.013(2) C35 0.0629(16) 0.0486(15) 0.0352(12) -0.0045(10) 0.0074(11) -0.0082(12) C36 0.0560(15) 0.0543(16) 0.0427(12) 0.0016(12) -0.0088(11) 0.0000(13) N37 0.0390(10) 0.0423(11) 0.0444(11) 0.0043(9) 0.0054(8) 0.0034(8) C38 0.0441(14) 0.0545(17) 0.0622(16) 0.0058(13) 0.0069(12) 0.0144(12) C39 0.0363(12) 0.0591(17) 0.0714(18) -0.0014(14) 0.0140(12) 0.0039(12) Fe2 0.04067(16) 0.0358(2) 0.03288(14) 0.00017(13) 0.00500(12) -0.00313(13) N2 0.0423(10) 0.0514(13) 0.0372(9) 0.0014(9) 0.0084(8) 0.0018(9) N41 0.0452(11) 0.0417(11) 0.0420(10) -0.0063(9) 0.0141(9) -0.0042(9) C42 0.0521(15) 0.0584(17) 0.0502(14) -0.0166(13) 0.0182(12) -0.0123(13) N43 0.0572(14) 0.0584(15) 0.0726(16) -0.0213(13) 0.0219(13) 0.0012(12) C44 0.0612(17) 0.0475(16) 0.0710(19) -0.0083(14) 0.0161(15) 0.0066(13) C45 0.0425(12) 0.0382(12) 0.0522(13) -0.0021(10) 0.0089(11) 0.0011(10) C46 0.0459(13) 0.0442(14) 0.0427(13) 0.0099(11) 0.0064(10) 0.0020(11) N47 0.0396(10) 0.0476(12) 0.0336(9) 0.0010(8) 0.0096(8) 0.0017(9) C48 0.0572(16) 0.0727(19) 0.0328(12) 0.0040(12) 0.0128(11) 0.0147(14) C49 0.0517(14) 0.0658(18) 0.0441(13) 0.0096(12) 0.0239(11) 0.0015(13) N51 0.0468(11) 0.0457(12) 0.0429(11) 0.0032(9) 0.0145(9) -0.0061(9) C52 0.0549(16) 0.0495(15) 0.0607(17) 0.0087(13) 0.0236(13) -0.0009(13) N53 0.0821(18) 0.0568(15) 0.0562(14) 0.0155(12) 0.0359(13) 0.0043(13) C54 0.072(2) 0.0662(19) 0.0408(14) 0.0076(13) 0.0176(13) -0.0015(15) C55 0.0537(14) 0.0516(15) 0.0345(11) 0.0002(10) 0.0096(10) -0.0028(12) C56 0.0498(13) 0.0610(17) 0.0369(11) -0.0045(12) 0.0057(9) -0.0121(13) N57 0.0490(11) 0.0477(12) 0.0387(9) -0.0042(9) 0.0129(8) -0.0134(9) C58 0.0589(16) 0.0679(19) 0.0478(14) -0.0061(13) 0.0143(13) -0.0287(15) C59 0.0365(11) 0.080(2) 0.0480(12) 0.0035(15) 0.0101(10) -0.0059(14) N61 0.0370(10) 0.0483(12) 0.0413(10) -0.0014(9) 0.0065(8) -0.0019(9) C62 0.0398(13) 0.075(2) 0.0522(15) -0.0042(14) 0.0100(11) 0.0022(13) N63 0.0361(12) 0.099(2) 0.0642(15) -0.0087(15) 0.0061(11) -0.0152(13) C64 0.0522(16) 0.069(2) 0.0637(18) -0.0110(15) 0.0056(14) -0.0198(15) C65 0.0458(13) 0.0465(14) 0.0446(13) -0.0046(11) 0.0050(10) -0.0094(11) C66 0.0518(15) 0.0383(14) 0.0543(15) -0.0054(11) 0.0079(12) -0.0004(11) N67 0.0419(11) 0.0391(11) 0.0469(11) 0.0036(9) 0.0085(9) 0.0025(9) C68 0.0460(14) 0.0483(16) 0.0758(19) 0.0049(14) 0.0129(14) 0.0130(12) C69 0.0446(14) 0.0583(17) 0.0605(16) -0.0104(13) 0.0161(13) 0.0095(13) Cl1 0.0583(6) 0.0383(6) 0.0384(4) 0.0005(4) -0.0012(4) 0.0043(4) O11 0.0616(16) 0.0696(18) 0.0676(17) -0.0057(14) -0.0001(13) -0.0072(13) O12 0.0739(18) 0.135(3) 0.0424(13) -0.0223(18) -0.0008(12) 0.018(2) O13 0.072(2) 0.073(2) 0.072(2) -0.0195(17) 0.0091(16) 0.0088(17) O14 0.153(4) 0.0451(19) 0.113(3) 0.0286(19) -0.012(3) -0.008(2) Cl1A 0.069(3) 0.036(2) 0.077(3) 0.001(2) -0.020(2) 0.002(2) O11A 0.101(9) 0.078(9) 0.105(7) -0.032(6) 0.003(7) -0.015(7) O12A 0.100(8) 0.064(6) 0.060(6) -0.002(5) -0.007(6) -0.022(6) O13A 0.093(8) 0.123(13) 0.133(12) 0.066(9) 0.042(9) 0.044(8) O14A 0.089(9) 0.078(9) 0.130(10) 0.066(9) -0.045(8) 0.000(7) Cl2 0.0726(5) 0.0610(4) 0.0537(4) -0.0122(3) -0.0075(3) 0.0213(4) O21 0.0853(16) 0.0737(15) 0.0635(13) -0.0214(12) 0.0105(12) 0.0092(13) O22 0.0594(19) 0.087(3) 0.0498(17) -0.0033(18) -0.0002(14) 0.0120(18) O23 0.067(2) 0.114(3) 0.067(2) 0.021(2) 0.0156(16) -0.005(2) O24 0.112(4) 0.055(2) 0.069(2) 0.0025(17) 0.015(3) 0.028(2) Cl2A 0.0726(5) 0.0610(4) 0.0537(4) -0.0122(3) -0.0075(3) 0.0213(4) O21A 0.0853(16) 0.0737(15) 0.0635(13) -0.0214(12) 0.0105(12) 0.0092(13) O22A 0.070(6) 0.144(12) 0.109(9) -0.046(8) 0.021(6) 0.040(7) O23A 0.106(7) 0.093(7) 0.132(9) -0.026(6) 0.044(7) -0.034(6) O24A 0.190(14) 0.120(10) 0.066(5) 0.046(6) -0.012(8) -0.004(8) Cl3 0.0625(4) 0.0867(6) 0.0544(4) -0.0093(4) 0.0194(3) -0.0252(4) O31 0.0919(18) 0.121(2) 0.0624(14) -0.0290(15) 0.0257(13) -0.0489(17) O32 0.150(3) 0.195(4) 0.0559(14) -0.0215(19) 0.0359(16) -0.108(3) O33 0.207(4) 0.0787(19) 0.106(2) -0.0259(17) 0.057(3) -0.045(2) O34 0.0717(18) 0.244(5) 0.139(3) 0.092(3) 0.0429(19) 0.041(3) Cl4 0.0549(4) 0.0922(6) 0.0480(4) -0.0014(4) 0.0105(3) -0.0206(4) O41 0.069(3) 0.119(6) 0.099(6) -0.021(5) 0.025(3) -0.002(3) O42 0.059(3) 0.127(6) 0.102(5) -0.055(4) 0.006(3) -0.013(3) O43 0.174(3) 0.149(3) 0.099(2) -0.009(2) 0.060(2) -0.094(3) O44 0.114(4) 0.138(7) 0.064(3) 0.002(3) -0.017(3) 0.010(4) Cl4A 0.0549(4) 0.0922(6) 0.0480(4) -0.0014(4) 0.0105(3) -0.0206(4) O41A 0.067(7) 0.165(12) 0.154(14) 0.078(12) 0.037(7) 0.037(7) O42A 0.146(14) 0.108(10) 0.079(8) 0.009(7) 0.078(10) 0.013(10) O43A 0.174(3) 0.149(3) 0.099(2) -0.009(2) 0.060(2) -0.094(3) O44A 0.056(7) 0.137(12) 0.070(5) -0.023(6) 0.032(5) -0.038(7) O71 0.077(2) 0.065(2) 0.119(3) -0.017(2) -0.014(2) 0.0065(17) C72 0.077(2) 0.063(2) 0.106(3) -0.001(2) 0.020(2) -0.0030(18) C73 0.125(4) 0.087(3) 0.086(3) -0.022(2) 0.013(3) 0.001(3) O71A 0.110(9) 0.057(6) 0.087(7) -0.002(5) 0.012(6) -0.002(6) C72A 0.125(4) 0.087(3) 0.086(3) -0.022(2) 0.013(3) 0.001(3) C73A 0.077(2) 0.063(2) 0.106(3) -0.001(2) 0.020(2) -0.0030(18) O81 0.069(3) 0.072(2) 0.070(2) -0.0094(17) 0.0155(17) 0.013(2) C82 0.130(6) 0.127(6) 0.073(4) 0.002(4) 0.014(4) 0.009(5) C83 0.220(9) 0.222(9) 0.152(7) 0.068(7) 0.066(7) 0.061(8) O81A 0.069(3) 0.072(2) 0.070(2) -0.0094(17) 0.0155(17) 0.013(2) C82A 0.097(6) 0.111(8) 0.077(6) -0.019(6) 0.025(6) 0.021(7) C83A 0.095(6) 0.122(9) 0.092(7) 0.010(7) 0.004(6) 0.040(7) O1W 0.0659(15) 0.0795(17) 0.120(2) -0.0211(16) 0.0414(15) 0.0033(13) O2W 0.063(3) 0.163(6) 0.208(7) -0.110(5) 0.025(3) -0.004(3) _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 N37 2.173(2) . ? Fe1 N27 2.188(2) . ? Fe1 N17 2.188(2) . ? Fe1 N21 2.2048(19) . ? Fe1 N11 2.217(2) . ? Fe1 N31 2.232(2) . ? N1 C19 1.456(3) . ? N1 C29 1.462(4) . ? N1 C39 1.464(4) . ? N11 C12 1.312(3) . ? N11 C15 1.382(3) . ? C12 N13 1.347(4) . ? C12 H12 0.9400 . ? N13 C14 1.359(4) . ? N13 H13 0.8700 . ? C14 C15 1.360(4) . ? C14 H14 0.9400 . ? C15 C16 1.445(4) . ? C16 N17 1.271(3) . ? C16 H16 0.9400 . ? N17 C18 1.460(3) . ? C18 C19 1.519(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? N21 C22 1.316(3) . ? N21 C25 1.379(3) . ? C22 N23 1.343(4) . ? C22 H22 0.9400 . ? N23 C24 1.341(4) . ? N23 H23 0.8700 . ? C24 C25 1.365(3) . ? C24 H24 0.9400 . ? C25 C26 1.445(4) . ? C26 N27 1.273(3) . ? C26 H26 0.9400 . ? N27 C28 1.463(3) . ? C28 C29 1.502(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? N31 C32 1.313(3) . ? N31 C35 1.375(3) . ? C32 N33 1.343(4) . ? C32 H32 0.9400 . ? N33 C34 1.334(5) . ? N33 H33 0.8700 . ? C34 C35 1.374(4) . ? C34 H34 0.9400 . ? C35 C36 1.441(4) . ? C36 N37 1.270(3) . ? C36 H36 0.9400 . ? N37 C38 1.460(3) . ? C38 C39 1.509(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? Fe2 N47 2.154(2) . ? Fe2 N67 2.175(2) . ? Fe2 N57 2.177(2) . ? Fe2 N41 2.187(2) . ? Fe2 N51 2.187(2) . ? Fe2 N61 2.195(2) . ? N2 C59 1.446(3) . ? N2 C49 1.453(3) . ? N2 C69 1.458(4) . ? N41 C42 1.321(3) . ? N41 C45 1.386(3) . ? C42 N43 1.346(4) . ? C42 H42 0.9400 . ? N43 C44 1.357(4) . ? N43 H43 0.8700 . ? C44 C45 1.358(4) . ? C44 H44 0.9400 . ? C45 C46 1.442(4) . ? C46 N47 1.272(3) . ? C46 H46 0.9400 . ? N47 C48 1.465(3) . ? C48 C49 1.516(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? N51 C52 1.315(3) . ? N51 C55 1.379(3) . ? C52 N53 1.349(4) . ? C52 H52 0.9400 . ? N53 C54 1.348(4) . ? N53 H53 0.8700 . ? C54 C55 1.355(4) . ? C54 H54 0.9400 . ? C55 C56 1.450(4) . ? C56 N57 1.268(3) . ? C56 H56 0.9400 . ? N57 C58 1.468(3) . ? C58 C59 1.509(4) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? N61 C62 1.313(3) . ? N61 C65 1.384(3) . ? C62 N63 1.352(4) . ? C62 H62 0.9400 . ? N63 C64 1.344(4) . ? N63 H63 0.8700 . ? C64 C65 1.362(4) . ? C64 H64 0.9400 . ? C65 C66 1.441(4) . ? C66 N67 1.263(3) . ? C66 H66 0.9400 . ? N67 C68 1.466(3) . ? C68 C69 1.508(4) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? Cl1 O12 1.411(3) . ? Cl1 O14 1.415(3) . ? Cl1 O11 1.434(3) . ? Cl1 O13 1.447(3) . ? Cl1A O12A 1.386(8) . ? Cl1A O14A 1.418(8) . ? Cl1A O11A 1.433(8) . ? Cl1A O13A 1.465(9) . ? Cl2 O24 1.362(4) . ? Cl2 O21 1.418(2) . ? Cl2 O22 1.421(3) . ? Cl2 O23 1.555(3) . ? Cl3 O34 1.386(3) . ? Cl3 O31 1.411(2) . ? Cl3 O32 1.416(3) . ? Cl3 O33 1.435(4) . ? Cl4 O43 1.404(3) . ? Cl4 O42 1.406(9) . ? Cl4 O44 1.417(7) . ? Cl4 O41 1.448(10) . ? O71 C72 1.405(4) . ? O71 H71 0.8300 . ? C72 C73 1.432(5) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C73 H73C 0.9700 . ? O71A H71A 0.8300 . ? O81 C82 1.390(6) . ? O81 H81 0.8300 . ? C82 C83 1.380(7) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C83 H83C 0.9700 . ? O81A C82A 1.370(8) . ? O81A H81A 0.8300 . ? C82A C83A 1.424(9) . ? C82A H82C 0.9800 . ? C82A H82D 0.9800 . ? C83A H83D 0.9700 . ? C83A H83E 0.9700 . ? C83A H83F 0.9700 . ? O1W H11W 0.878(10) . ? O1W H12W 0.858(10) . ? O2W H21W 0.850(11) . ? O2W H22W 0.845(11) . ? 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 N37 Fe1 N27 104.97(8) . . ? N37 Fe1 N17 105.30(8) . . ? N27 Fe1 N17 102.11(8) . . ? N37 Fe1 N21 161.55(8) . . ? N27 Fe1 N21 75.48(8) . . ? N17 Fe1 N21 92.45(8) . . ? N37 Fe1 N11 91.42(8) . . ? N27 Fe1 N11 163.46(7) . . ? N17 Fe1 N11 74.99(8) . . ? N21 Fe1 N11 88.29(8) . . ? N37 Fe1 N31 75.28(8) . . ? N27 Fe1 N31 95.58(8) . . ? N17 Fe1 N31 161.37(8) . . ? N21 Fe1 N31 86.29(8) . . ? N11 Fe1 N31 86.38(8) . . ? C19 N1 C29 113.7(2) . . ? C19 N1 C39 113.7(2) . . ? C29 N1 C39 113.0(2) . . ? C12 N11 C15 105.1(2) . . ? C12 N11 Fe1 142.68(19) . . ? C15 N11 Fe1 111.86(15) . . ? N11 C12 N13 111.5(3) . . ? N11 C12 H12 124.2 . . ? N13 C12 H12 124.2 . . ? C12 N13 C14 107.8(2) . . ? C12 N13 H13 126.1 . . ? C14 N13 H13 126.1 . . ? N13 C14 C15 105.7(2) . . ? N13 C14 H14 127.1 . . ? C15 C14 H14 127.1 . . ? C14 C15 N11 109.8(2) . . ? C14 C15 C16 132.4(3) . . ? N11 C15 C16 117.7(2) . . ? N17 C16 C15 117.7(2) . . ? N17 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? C16 N17 C18 119.4(2) . . ? C16 N17 Fe1 117.17(17) . . ? C18 N17 Fe1 123.18(17) . . ? N17 C18 C19 107.8(2) . . ? N17 C18 H18A 110.1 . . ? C19 C18 H18A 110.1 . . ? N17 C18 H18B 110.1 . . ? C19 C18 H18B 110.1 . . ? H18A C18 H18B 108.5 . . ? N1 C19 C18 110.9(2) . . ? N1 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C22 N21 C25 104.9(2) . . ? C22 N21 Fe1 142.41(18) . . ? C25 N21 Fe1 112.22(15) . . ? N21 C22 N23 111.2(2) . . ? N21 C22 H22 124.4 . . ? N23 C22 H22 124.4 . . ? C24 N23 C22 108.4(2) . . ? C24 N23 H23 125.8 . . ? C22 N23 H23 125.8 . . ? N23 C24 C25 105.8(2) . . ? N23 C24 H24 127.1 . . ? C25 C24 H24 127.1 . . ? C24 C25 N21 109.7(2) . . ? C24 C25 C26 132.8(3) . . ? N21 C25 C26 117.5(2) . . ? N27 C26 C25 118.3(2) . . ? N27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? C26 N27 C28 120.0(2) . . ? C26 N27 Fe1 116.36(16) . . ? C28 N27 Fe1 123.42(17) . . ? N27 C28 C29 108.5(2) . . ? N27 C28 H28A 110.0 . . ? C29 C28 H28A 110.0 . . ? N27 C28 H28B 110.0 . . ? C29 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? N1 C29 C28 110.8(2) . . ? N1 C29 H29A 109.5 . . ? C28 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C32 N31 C35 105.8(2) . . ? C32 N31 Fe1 142.2(2) . . ? C35 N31 Fe1 110.91(16) . . ? N31 C32 N33 110.5(3) . . ? N31 C32 H32 124.7 . . ? N33 C32 H32 124.7 . . ? C34 N33 C32 109.0(3) . . ? C34 N33 H33 125.5 . . ? C32 N33 H33 125.5 . . ? N33 C34 C35 105.8(3) . . ? N33 C34 H34 127.1 . . ? C35 C34 H34 127.1 . . ? C34 C35 N31 108.9(3) . . ? C34 C35 C36 133.0(3) . . ? N31 C35 C36 118.0(2) . . ? N37 C36 C35 118.2(2) . . ? N37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C36 N37 C38 120.0(2) . . ? C36 N37 Fe1 116.87(18) . . ? C38 N37 Fe1 123.15(17) . . ? N37 C38 C39 108.6(2) . . ? N37 C38 H38A 110.0 . . ? C39 C38 H38A 110.0 . . ? N37 C38 H38B 110.0 . . ? C39 C38 H38B 110.0 . . ? H38A C38 H38B 108.3 . . ? N1 C39 C38 110.6(2) . . ? N1 C39 H39A 109.5 . . ? C38 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 108.1 . . ? N47 Fe2 N67 101.06(8) . . ? N47 Fe2 N57 102.14(8) . . ? N67 Fe2 N57 101.41(8) . . ? N47 Fe2 N41 76.65(8) . . ? N67 Fe2 N41 163.28(8) . . ? N57 Fe2 N41 95.25(8) . . ? N47 Fe2 N51 166.96(8) . . ? N67 Fe2 N51 91.94(8) . . ? N57 Fe2 N51 75.96(8) . . ? N41 Fe2 N51 90.60(8) . . ? N47 Fe2 N61 92.62(8) . . ? N67 Fe2 N61 76.03(8) . . ? N57 Fe2 N61 165.22(8) . . ? N41 Fe2 N61 87.47(8) . . ? N51 Fe2 N61 89.51(8) . . ? C59 N2 C49 114.8(2) . . ? C59 N2 C69 115.3(2) . . ? C49 N2 C69 114.3(2) . . ? C42 N41 C45 105.5(2) . . ? C42 N41 Fe2 142.9(2) . . ? C45 N41 Fe2 110.89(15) . . ? N41 C42 N43 110.5(3) . . ? N41 C42 H42 124.7 . . ? N43 C42 H42 124.7 . . ? C42 N43 C44 108.6(2) . . ? C42 N43 H43 125.7 . . ? C44 N43 H43 125.7 . . ? N43 C44 C45 105.8(3) . . ? N43 C44 H44 127.1 . . ? C45 C44 H44 127.1 . . ? C44 C45 N41 109.6(2) . . ? C44 C45 C46 132.3(3) . . ? N41 C45 C46 118.0(2) . . ? N47 C46 C45 117.9(2) . . ? N47 C46 H46 121.0 . . ? C45 C46 H46 121.0 . . ? C46 N47 C48 119.1(2) . . ? C46 N47 Fe2 116.34(16) . . ? C48 N47 Fe2 124.58(17) . . ? N47 C48 C49 108.7(2) . . ? N47 C48 H48A 109.9 . . ? C49 C48 H48A 109.9 . . ? N47 C48 H48B 109.9 . . ? C49 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? N2 C49 C48 111.1(2) . . ? N2 C49 H49A 109.4 . . ? C48 C49 H49A 109.4 . . ? N2 C49 H49B 109.4 . . ? C48 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? C52 N51 C55 105.5(2) . . ? C52 N51 Fe2 142.3(2) . . ? C55 N51 Fe2 112.20(16) . . ? N51 C52 N53 110.4(3) . . ? N51 C52 H52 124.8 . . ? N53 C52 H52 124.8 . . ? C54 N53 C52 108.6(2) . . ? C54 N53 H53 125.7 . . ? C52 N53 H53 125.7 . . ? N53 C54 C55 105.6(3) . . ? N53 C54 H54 127.2 . . ? C55 C54 H54 127.2 . . ? C54 C55 N51 109.9(2) . . ? C54 C55 C56 132.8(3) . . ? N51 C55 C56 117.3(2) . . ? N57 C56 C55 118.3(2) . . ? N57 C56 H56 120.9 . . ? C55 C56 H56 120.9 . . ? C56 N57 C58 119.0(2) . . ? C56 N57 Fe2 116.24(17) . . ? C58 N57 Fe2 124.56(17) . . ? N57 C58 C59 109.3(2) . . ? N57 C58 H58A 109.8 . . ? C59 C58 H58A 109.8 . . ? N57 C58 H58B 109.8 . . ? C59 C58 H58B 109.8 . . ? H58A C58 H58B 108.3 . . ? N2 C59 C58 110.9(2) . . ? N2 C59 H59A 109.5 . . ? C58 C59 H59A 109.5 . . ? N2 C59 H59B 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 108.0 . . ? C62 N61 C65 105.9(2) . . ? C62 N61 Fe2 142.2(2) . . ? C65 N61 Fe2 111.40(16) . . ? N61 C62 N63 110.3(3) . . ? N61 C62 H62 124.9 . . ? N63 C62 H62 124.9 . . ? C64 N63 C62 108.7(2) . . ? C64 N63 H63 125.6 . . ? C62 N63 H63 125.6 . . ? N63 C64 C65 106.0(3) . . ? N63 C64 H64 127.0 . . ? C65 C64 H64 127.0 . . ? C64 C65 N61 109.1(3) . . ? C64 C65 C66 133.3(3) . . ? N61 C65 C66 117.6(2) . . ? N67 C66 C65 118.7(2) . . ? N67 C66 H66 120.7 . . ? C65 C66 H66 120.7 . . ? C66 N67 C68 119.6(2) . . ? C66 N67 Fe2 116.10(18) . . ? C68 N67 Fe2 124.26(18) . . ? N67 C68 C69 109.2(2) . . ? N67 C68 H68A 109.8 . . ? C69 C68 H68A 109.8 . . ? N67 C68 H68B 109.8 . . ? C69 C68 H68B 109.8 . . ? H68A C68 H68B 108.3 . . ? N2 C69 C68 111.3(2) . . ? N2 C69 H69A 109.4 . . ? C68 C69 H69A 109.4 . . ? N2 C69 H69B 109.4 . . ? C68 C69 H69B 109.4 . . ? H69A C69 H69B 108.0 . . ? O12 Cl1 O14 110.4(3) . . ? O12 Cl1 O11 110.6(2) . . ? O14 Cl1 O11 109.0(2) . . ? O12 Cl1 O13 108.6(2) . . ? O14 Cl1 O13 109.7(3) . . ? O11 Cl1 O13 108.5(2) . . ? O12A Cl1A O14A 113.6(7) . . ? O12A Cl1A O11A 108.6(8) . . ? O14A Cl1A O11A 109.7(9) . . ? O12A Cl1A O13A 107.0(9) . . ? O14A Cl1A O13A 107.7(9) . . ? O11A Cl1A O13A 110.2(9) . . ? O24 Cl2 O21 113.1(2) . . ? O24 Cl2 O22 113.2(3) . . ? O21 Cl2 O22 114.26(19) . . ? O24 Cl2 O23 105.7(3) . . ? O21 Cl2 O23 106.0(2) . . ? O22 Cl2 O23 103.4(2) . . ? O34 Cl3 O31 109.9(3) . . ? O34 Cl3 O32 112.0(2) . . ? O31 Cl3 O32 109.70(16) . . ? O34 Cl3 O33 105.4(3) . . ? O31 Cl3 O33 109.1(2) . . ? O32 Cl3 O33 110.7(2) . . ? O43 Cl4 O42 113.1(5) . . ? O43 Cl4 O44 102.3(4) . . ? O42 Cl4 O44 111.0(4) . . ? O43 Cl4 O41 113.4(6) . . ? O42 Cl4 O41 110.0(6) . . ? O44 Cl4 O41 106.5(6) . . ? C72 O71 H71 109.5 . . ? O71 C72 C73 109.7(4) . . ? O71 C72 H72A 109.7 . . ? C73 C72 H72A 109.7 . . ? O71 C72 H72B 109.7 . . ? C73 C72 H72B 109.7 . . ? H72A C72 H72B 108.2 . . ? C82 O81 H81 109.5 . . ? C83 C82 O81 123.7(8) . . ? C83 C82 H82A 106.4 . . ? O81 C82 H82A 106.4 . . ? C83 C82 H82B 106.4 . . ? O81 C82 H82B 106.4 . . ? H82A C82 H82B 106.5 . . ? C82A O81A H81A 109.5 . . ? O81A C82A C83A 120.1(11) . . ? O81A C82A H82C 107.3 . . ? C83A C82A H82C 107.3 . . ? O81A C82A H82D 107.3 . . ? C83A C82A H82D 107.3 . . ? H82C C82A H82D 106.9 . . ? C82A C83A H83D 109.5 . . ? C82A C83A H83E 109.5 . . ? H83D C83A H83E 109.5 . . ? C82A C83A H83F 109.5 . . ? H83D C83A H83F 109.5 . . ? H83E C83A H83F 109.5 . . ? H11W O1W H12W 98(2) . . ? H21W O2W H22W 106(3) . . ? 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 N13 H13 O1W 0.87 1.98 2.822(3) 163.6 2_646 N23 H23 O1W 0.87 2.11 2.890(4) 148.2 . N23 H23 O71 0.87 2.46 3.036(4) 123.8 . N33 H33 O31 0.87 2.31 3.075(4) 147.0 . N33 H33 O22 0.87 2.35 3.020(5) 134.1 . N43 H43 O81 0.87 2.06 2.850(5) 150.9 1_545 N43 H43 O81A 0.87 2.08 2.755(9) 134.1 1_545 N43 H43 O44A 0.87 2.60 3.172(14) 124.6 2_645 N53 H53 O24A 0.87 2.21 2.830(9) 128.5 1_554 N53 H53 O22 0.87 2.34 3.116(5) 148.7 1_554 N53 H53 O31 0.87 2.34 3.010(4) 134.2 1_554 N63 H63 O44A 0.87 2.15 2.930(14) 149.2 1_655 N63 H63 O42 0.87 2.19 3.040(9) 165.1 1_655 O71 H71 O44 0.83 2.25 2.750(8) 119.5 . O71A H71A O1W 0.83 2.31 2.897(9) 128.2 2_656 O81 H81 O42 0.83 2.62 3.068(10) 115.3 2_655 O81A H81A O33 0.83 2.20 3.014(10) 168.0 1_554 O1W H11W O41A 0.878(10) 2.22(3) 2.966(18) 142(3) . O1W H11W O44 0.878(10) 2.27(2) 3.011(10) 142(3) . O1W H11W O71 0.878(10) 2.59(3) 3.188(5) 126(3) . O1W H12W O2W 0.858(10) 1.81(3) 2.538(6) 142(4) . O1W H12W O23A 0.858(10) 2.31(3) 2.990(11) 136(3) 2_646 O2W H21W O41A 0.850(11) 2.15(9) 2.59(3) 111(7) . O2W H22W O22 0.845(11) 2.48(4) 3.170(9) 140(6) 2_646 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.416 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.042 _exptl_crystal_id 'Brewer CTBF53E' _diffrn_measurement_details 606,606,606,1206,50 _diffrn_measurement_total_frames-CCD 3074 _diffrn_measurement_frame_width-CCD 0.3 _diffrn_detector_distance-CCD 4.958 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_frame_time-CCD 13 _diffrn_measurement_total_time-CCD 17.21 _diffrn_measurement_frame_size-CCD 512 _chemical_absolute_configuration ad _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 0.0099053 _diffrn_orient_matrix_UB_12 -0.0718963 _diffrn_orient_matrix_UB_13 -0.0224361 _diffrn_orient_matrix_UB_21 -0.0555766 _diffrn_orient_matrix_UB_22 -0.0306574 _diffrn_orient_matrix_UB_23 0.0227310 _diffrn_orient_matrix_UB_31 -0.0495807 _diffrn_orient_matrix_UB_32 0.0200006 _diffrn_orient_matrix_UB_33 -0.0457902 _symmetry_space_group_name_Hall 'P 2yb' _diffrn_measurement_specimen_support 'glass capillary' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' _reflns_Friedel_coverage 0.893 #_______________________________________________________________________________ # _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Flack, H.D. (1983), Acta Cryst. A39, 876-881. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (1990). Acta Cryst., A46, C-34. ; #===END data_1296 _database_code_depnum_ccdc_archive 'CCDC 603955' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Fe(LH3-x) complex (I,I3)1.38 ; _chemical_name_common 'Fe(LH3-x) complex (I,I3)1.38' _chemical_formula_structural '[FeN(CH2CH2NCHC3H2N2)H2.39] (I3)0.62 (I)0.77' _chemical_formula_moiety '(C18 H23.39 Fe N10), (I3)0.62, (I)0.77' _chemical_formula_sum 'C18 H23.39 Fe I2.63 N10' _chemical_formula_weight 768.82 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P 32 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 11.9397(5) _cell_length_b 11.9397(5) _cell_length_c 35.951(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4438.4(4) _cell_formula_units_Z 6 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6281 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 24.7 _exptl_crystal_description pyramid _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 2199 _exptl_absorpt_coefficient_mu 3.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_T_max 0.537 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 223(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 'three-circle diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 0 _diffrn_reflns_number 36811 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5180 _reflns_number_gt 4283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker, 1999)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+50.4P], P=(max(Fo^2^,0)+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_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack 0.00(7) _refine_ls_number_reflns 5180 # 2984 w/o Fiedel pairs _refine_ls_number_parameters 631 _refine_ls_number_restraints 397 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.978 _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 0.32977(15) 0.31651(14) 0.31437(5) 0.0477(5) Uani 1 1 d PD A 1 N1 N 0.3279(9) 0.3156(10) 0.3940(3) 0.062(3) Uani 1 1 d PD A 1 N11 N 0.3453(12) 0.1757(11) 0.2763(3) 0.067(3) Uani 1 1 d PD A 1 C12 C 0.3916(14) 0.1674(15) 0.2449(4) 0.066(4) Uani 1 1 d PD A 1 H12 H 0.4519 0.2385 0.2309 0.079 Uiso 1 1 calc PR A 1 N13 N 0.3413(14) 0.0406(14) 0.2346(4) 0.082(4) Uani 1 1 d PD A 1 H13 H 0.3615 0.0126 0.2148 0.099 Uiso 0.39 1 calc PR A 1 C14 C 0.255(2) -0.0323(16) 0.2607(5) 0.082(5) Uani 1 1 d PD A 1 H14 H 0.2025 -0.1228 0.2603 0.098 Uiso 1 1 calc PR A 1 C15 C 0.2577(14) 0.0482(12) 0.2877(4) 0.058(3) Uani 1 1 d PD A 1 C16 C 0.1833(14) 0.0262(11) 0.3216(4) 0.058(3) Uani 1 1 d PD A 1 H16 H 0.1276 -0.0572 0.3309 0.070 Uiso 1 1 calc PR A 1 N17 N 0.1992(10) 0.1299(9) 0.3381(3) 0.052(2) Uani 1 1 d PD A 1 C18 C 0.1344(14) 0.1096(14) 0.3735(5) 0.080(5) Uani 1 1 d PD A 1 H181 H 0.0829 0.0168 0.3787 0.096 Uiso 1 1 calc PR A 1 H182 H 0.0760 0.1450 0.3727 0.096 Uiso 1 1 calc PR A 1 C19 C 0.2378(15) 0.1784(12) 0.4047(3) 0.064(4) Uani 1 1 d PD A 1 H191 H 0.1947 0.1756 0.4282 0.077 Uiso 1 1 calc PR A 1 H192 H 0.2866 0.1333 0.4083 0.077 Uiso 1 1 calc PR A 1 N21 N 0.1849(10) 0.3105(11) 0.2749(3) 0.063(3) Uani 1 1 d PD A 1 C22 C 0.1329(14) 0.2716(13) 0.2423(4) 0.069(4) Uani 1 1 d PD A 1 H22 H 0.1425 0.2113 0.2279 0.083 Uiso 1 1 calc PR A 1 N23 N 0.0637(12) 0.3268(14) 0.2315(4) 0.083(4) Uani 1 1 d PD A 1 H23 H 0.0221 0.3135 0.2106 0.100 Uiso 1 1 calc PR A 1 C24 C 0.0712(15) 0.4085(18) 0.2597(5) 0.079(4) Uani 1 1 d PD A 1 H24 H 0.0325 0.4604 0.2602 0.095 Uiso 1 1 calc PR A 1 C25 C 0.1457(13) 0.3993(13) 0.2869(4) 0.062(3) Uani 1 1 d PD A 1 C26 C 0.1922(13) 0.4636(11) 0.3220(3) 0.049(3) Uani 1 1 d PD A 1 H26 H 0.1618 0.5162 0.3320 0.059 Uiso 1 1 calc PR A 1 N27 N 0.2742(12) 0.4471(9) 0.3387(3) 0.060(3) Uani 1 1 d PD A 1 C28 C 0.3249(16) 0.5076(13) 0.3746(4) 0.078(4) Uani 1 1 d PD A 1 H281 H 0.2925 0.5664 0.3806 0.094 Uiso 1 1 calc PR A 1 H282 H 0.4195 0.5583 0.3735 0.094 Uiso 1 1 calc PR A 1 C29 C 0.2826(17) 0.4030(15) 0.4050(3) 0.072(4) Uani 1 1 d PD A 1 H291 H 0.3201 0.4429 0.4290 0.086 Uiso 1 1 calc PR A 1 H292 H 0.1882 0.3557 0.4074 0.086 Uiso 1 1 calc PR A 1 N31 N 0.4787(11) 0.4666(10) 0.2772(3) 0.057(3) Uani 1 1 d PD A 1 C32 C 0.4895(17) 0.5222(13) 0.2446(4) 0.072(4) Uani 1 1 d PD A 1 H32 H 0.4200 0.5144 0.2303 0.086 Uiso 1 1 calc PR A 1 N33 N 0.6176(14) 0.5933(12) 0.2347(4) 0.080(4) Uani 1 1 d PD A 1 H33 H 0.6478 0.6372 0.2142 0.096 Uiso 1 1 calc PR A 1 C34 C 0.6874(15) 0.5829(15) 0.2620(5) 0.077(4) Uani 1 1 d PD A 1 H34 H 0.7780 0.6218 0.2626 0.093 Uiso 1 1 calc PR A 1 C35 C 0.6027(13) 0.5047(12) 0.2892(4) 0.063(4) Uani 1 1 d PD A 1 C36 C 0.6165(12) 0.4515(14) 0.3241(4) 0.057(3) Uani 1 1 d PD A 1 H36 H 0.6991 0.4766 0.3336 0.069 Uiso 1 1 calc PR A 1 N37 N 0.5201(10) 0.3741(10) 0.3410(3) 0.054(2) Uani 1 1 d PD A 1 C38 C 0.5307(15) 0.3222(17) 0.3761(4) 0.068(4) Uani 1 1 d PD A 1 H381 H 0.6220 0.3608 0.3831 0.082 Uiso 1 1 calc PR A 1 H382 H 0.4941 0.2285 0.3740 0.082 Uiso 1 1 calc PR A 1 C39 C 0.4571(17) 0.3522(17) 0.4063(4) 0.079(5) Uani 1 1 d PD A 1 H391 H 0.4521 0.3050 0.4291 0.095 Uiso 1 1 calc PR A 1 H392 H 0.5046 0.4449 0.4120 0.095 Uiso 1 1 calc PR A 1 I1 I 0.6766(4) 0.3952(4) 0.16410(12) 0.0998(10) Uani 0.518(5) 1 d P B 1 I2 I 0.4034(3) 0.2945(3) 0.14799(6) 0.0849(7) Uani 0.518(5) 1 d P B 1 I3 I 0.1276(3) 0.1699(3) 0.13607(6) 0.1015(10) Uani 0.518(5) 1 d P B 1 I1A I 0.974(4) -0.003(3) 0.1581(8) 0.161(16) Uani 0.0623(19) 1 d P . 3 I2AB I 0.6962(6) 0.0000 0.1667 0.089(3) Uani 0.202(4) 2 d SP . 3 I3A I 0.465(4) 0.035(6) 0.1633(16) 0.14(2) Uani 0.0623(19) 1 d P . 3 I3B I 0.903(2) 0.2886(18) 0.1687(5) 0.114(8) Uani 0.077(4) 1 d P . 3 I4 I 0.3461(5) 0.3526(6) 0.0075(3) 0.088(2) Uani 0.443(4) 1 d PU C 1 I5 I 0.6949(18) 0.3617(16) 0.1703(5) 0.149(7) Uani 0.185(6) 1 d PU D 2 I6 I 0.491(3) 0.331(2) 0.1480(6) 0.161(11) Uani 0.103(5) 1 d PU E 3 I7 I -0.029(5) 0.239(5) 0.1564(13) 0.13(2) Uani 0.038(6) 1 d PU F 2 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 0.0411(9) 0.0358(8) 0.0671(11) 0.0030(8) -0.0018(8) 0.0199(7) N1 0.045(5) 0.053(6) 0.084(7) -0.003(5) -0.001(5) 0.021(5) N11 0.092(9) 0.061(7) 0.052(6) -0.007(5) -0.010(6) 0.041(7) C12 0.075(9) 0.077(10) 0.058(8) -0.022(7) -0.006(7) 0.047(8) N13 0.107(11) 0.090(10) 0.069(8) -0.018(7) -0.010(8) 0.064(9) C14 0.131(15) 0.066(10) 0.075(10) -0.032(9) -0.034(11) 0.070(11) C15 0.076(9) 0.041(7) 0.069(8) -0.011(6) -0.020(7) 0.038(7) C16 0.056(8) 0.042(6) 0.066(8) 0.004(6) -0.020(7) 0.016(6) N17 0.054(6) 0.040(5) 0.064(6) -0.011(5) 0.001(5) 0.025(5) C18 0.056(9) 0.056(9) 0.118(13) -0.010(9) -0.024(9) 0.020(7) C19 0.097(11) 0.054(7) 0.045(6) 0.009(6) 0.012(7) 0.040(8) N21 0.044(6) 0.056(7) 0.075(7) -0.008(6) -0.013(5) 0.013(5) C22 0.081(10) 0.058(8) 0.060(8) -0.002(7) -0.019(7) 0.028(8) N23 0.064(8) 0.101(11) 0.075(8) 0.014(8) -0.023(7) 0.034(8) C24 0.068(10) 0.094(12) 0.096(11) 0.007(10) -0.003(9) 0.056(9) C25 0.063(8) 0.060(8) 0.080(9) 0.003(7) 0.000(7) 0.043(7) C26 0.054(8) 0.034(6) 0.074(8) 0.001(6) -0.002(6) 0.033(6) N27 0.083(8) 0.038(5) 0.065(6) -0.006(5) 0.002(6) 0.035(6) C28 0.084(11) 0.045(8) 0.093(10) -0.006(8) -0.018(9) 0.022(8) C29 0.114(14) 0.083(11) 0.051(7) -0.008(7) -0.002(8) 0.075(10) N31 0.072(7) 0.049(6) 0.052(6) 0.001(5) 0.002(5) 0.032(6) C32 0.109(13) 0.045(7) 0.052(7) -0.008(6) -0.010(8) 0.031(8) N33 0.089(10) 0.057(8) 0.076(8) 0.018(7) 0.020(8) 0.024(7) C34 0.055(9) 0.071(10) 0.089(11) 0.001(9) 0.024(8) 0.019(8) C35 0.049(7) 0.038(7) 0.093(10) -0.009(7) 0.004(7) 0.015(6) C36 0.037(6) 0.064(9) 0.075(9) 0.003(7) 0.003(6) 0.028(7) N37 0.053(6) 0.059(6) 0.058(6) -0.004(5) -0.004(5) 0.035(5) C38 0.057(8) 0.081(11) 0.064(8) 0.007(8) -0.004(7) 0.032(8) C39 0.092(12) 0.092(12) 0.063(8) -0.009(8) -0.009(8) 0.053(10) I1 0.105(2) 0.093(2) 0.110(2) 0.0176(16) 0.0282(17) 0.0565(17) I2 0.129(2) 0.0799(16) 0.0524(9) -0.0049(10) -0.0040(12) 0.0576(16) I3 0.127(2) 0.1213(19) 0.0837(14) -0.0080(12) -0.0207(13) 0.0830(17) I1A 0.30(4) 0.088(13) 0.13(3) -0.069(16) -0.08(2) 0.13(2) I2AB 0.104(4) 0.105(6) 0.057(3) 0.012(3) 0.0059(17) 0.052(3) I3A 0.15(3) 0.22(7) 0.10(2) -0.02(3) 0.016(19) 0.13(4) I3B 0.124(15) 0.095(12) 0.111(12) 0.030(10) 0.014(11) 0.046(11) I4 0.0289(12) 0.0393(13) 0.194(8) -0.021(2) 0.009(2) 0.0152(7) I5 0.141(10) 0.112(10) 0.208(12) 0.037(7) -0.002(7) 0.073(7) I6 0.22(2) 0.098(12) 0.124(12) 0.015(8) -0.003(13) 0.055(13) I7 0.14(3) 0.13(3) 0.13(3) 0.002(16) 0.019(16) 0.060(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 N17 2.156(10) . ? Fe1 N27 2.161(9) . ? Fe1 N21 2.211(11) . ? Fe1 N31 2.230(11) . ? Fe1 N37 2.234(10) . ? Fe1 N11 2.247(11) . ? N1 C39 1.446(18) . ? N1 C29 1.450(15) . ? N1 C19 1.493(15) . ? N11 C12 1.280(16) . ? N11 C15 1.410(17) . ? C12 N13 1.372(18) . ? N13 C14 1.34(2) . ? C14 C15 1.357(18) . ? C15 C16 1.452(19) . ? C16 N17 1.299(15) . ? N17 C18 1.445(18) . ? C18 C19 1.563(19) . ? N21 C22 1.297(16) . ? N21 C25 1.423(16) . ? C22 N23 1.348(19) . ? N23 C24 1.38(2) . ? C24 C25 1.36(2) . ? C25 C26 1.437(18) . ? C26 N27 1.246(15) . ? N27 C28 1.456(17) . ? C28 C29 1.542(19) . ? N31 C32 1.320(16) . ? N31 C35 1.383(17) . ? C32 N33 1.37(2) . ? N33 C34 1.33(2) . ? C34 C35 1.38(2) . ? C35 C36 1.454(19) . ? C36 N37 1.218(15) . ? N37 C38 1.439(16) . ? C38 C39 1.55(2) . ? I1 I2 2.916(5) . ? I2 I3 2.888(4) . ? 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 N17 Fe1 N27 105.2(4) . . ? N17 Fe1 N21 94.1(4) . . ? N27 Fe1 N21 76.4(4) . . ? N17 Fe1 N31 160.3(4) . . ? N27 Fe1 N31 94.1(4) . . ? N21 Fe1 N31 86.4(4) . . ? N17 Fe1 N37 104.3(4) . . ? N27 Fe1 N37 103.7(4) . . ? N21 Fe1 N37 160.7(4) . . ? N31 Fe1 N37 74.3(4) . . ? N17 Fe1 N11 75.9(4) . . ? N27 Fe1 N11 163.0(4) . . ? N21 Fe1 N11 86.6(4) . . ? N31 Fe1 N11 84.5(4) . . ? N37 Fe1 N11 92.3(4) . . ? C39 N1 C29 115.1(12) . . ? C39 N1 C19 109.1(11) . . ? C29 N1 C19 113.3(11) . . ? C12 N11 C15 106.8(12) . . ? C12 N11 Fe1 142.7(10) . . ? C15 N11 Fe1 109.6(9) . . ? N11 C12 N13 110.9(14) . . ? C14 N13 C12 107.3(12) . . ? N13 C14 C15 107.6(15) . . ? C14 C15 N11 107.3(14) . . ? C14 C15 C16 132.7(14) . . ? N11 C15 C16 119.8(11) . . ? N17 C16 C15 115.2(11) . . ? C16 N17 C18 115.6(11) . . ? C16 N17 Fe1 119.3(9) . . ? C18 N17 Fe1 124.9(8) . . ? N17 C18 C19 109.1(11) . . ? N1 C19 C18 109.7(10) . . ? C22 N21 C25 105.3(12) . . ? C22 N21 Fe1 144.8(11) . . ? C25 N21 Fe1 109.0(8) . . ? N21 C22 N23 112.8(14) . . ? C22 N23 C24 107.0(12) . . ? C25 C24 N23 106.6(13) . . ? C24 C25 N21 108.4(13) . . ? C24 C25 C26 132.8(13) . . ? N21 C25 C26 118.8(11) . . ? N27 C26 C25 117.6(10) . . ? C26 N27 C28 120.9(11) . . ? C26 N27 Fe1 118.0(8) . . ? C28 N27 Fe1 121.0(9) . . ? N27 C28 C29 109.8(11) . . ? N1 C29 C28 107.5(11) . . ? C32 N31 C35 106.9(13) . . ? C32 N31 Fe1 140.7(11) . . ? C35 N31 Fe1 111.7(8) . . ? N31 C32 N33 109.9(14) . . ? C34 N33 C32 107.8(13) . . ? N33 C34 C35 107.7(14) . . ? C34 C35 N31 107.7(14) . . ? C34 C35 C36 134.6(14) . . ? N31 C35 C36 117.5(12) . . ? N37 C36 C35 119.4(12) . . ? C36 N37 C38 120.7(12) . . ? C36 N37 Fe1 116.8(9) . . ? C38 N37 Fe1 122.6(9) . . ? N37 C38 C39 109.4(12) . . ? N1 C39 C38 111.0(11) . . ? I3 I2 I1 173.89(14) . . ? 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 N17 Fe1 N11 C12 169.9(17) . . . . ? N27 Fe1 N11 C12 74(2) . . . . ? N21 Fe1 N11 C12 74.8(17) . . . . ? N31 Fe1 N11 C12 -11.9(16) . . . . ? N37 Fe1 N11 C12 -86.0(17) . . . . ? N17 Fe1 N11 C15 3.5(8) . . . . ? N27 Fe1 N11 C15 -92.2(16) . . . . ? N21 Fe1 N11 C15 -91.6(9) . . . . ? N31 Fe1 N11 C15 -178.3(9) . . . . ? N37 Fe1 N11 C15 107.6(9) . . . . ? C15 N11 C12 N13 -0.8(16) . . . . ? Fe1 N11 C12 N13 -167.4(12) . . . . ? N11 C12 N13 C14 2.6(18) . . . . ? C12 N13 C14 C15 -3.3(18) . . . . ? N13 C14 C15 N11 2.9(17) . . . . ? N13 C14 C15 C16 177.1(14) . . . . ? C12 N11 C15 C14 -1.3(16) . . . . ? Fe1 N11 C15 C14 170.1(10) . . . . ? C12 N11 C15 C16 -176.4(12) . . . . ? Fe1 N11 C15 C16 -5.0(14) . . . . ? C14 C15 C16 N17 -170.0(15) . . . . ? N11 C15 C16 N17 3.7(18) . . . . ? C15 C16 N17 C18 -174.8(11) . . . . ? C15 C16 N17 Fe1 -0.1(15) . . . . ? N27 Fe1 N17 C16 160.6(9) . . . . ? N21 Fe1 N17 C16 83.5(10) . . . . ? N31 Fe1 N17 C16 -7.2(18) . . . . ? N37 Fe1 N17 C16 -90.6(10) . . . . ? N11 Fe1 N17 C16 -1.9(10) . . . . ? N27 Fe1 N17 C18 -25.3(11) . . . . ? N21 Fe1 N17 C18 -102.3(10) . . . . ? N31 Fe1 N17 C18 167.0(11) . . . . ? N37 Fe1 N17 C18 83.5(10) . . . . ? N11 Fe1 N17 C18 172.2(11) . . . . ? C16 N17 C18 C19 117.1(13) . . . . ? Fe1 N17 C18 C19 -57.3(15) . . . . ? C39 N1 C19 C18 -143.0(12) . . . . ? C29 N1 C19 C18 87.3(13) . . . . ? N17 C18 C19 N1 51.5(15) . . . . ? N17 Fe1 N21 C22 -85.9(17) . . . . ? N27 Fe1 N21 C22 169.4(17) . . . . ? N31 Fe1 N21 C22 74.4(17) . . . . ? N37 Fe1 N21 C22 77(2) . . . . ? N11 Fe1 N21 C22 -10.4(17) . . . . ? N17 Fe1 N21 C25 107.9(9) . . . . ? N27 Fe1 N21 C25 3.2(8) . . . . ? N31 Fe1 N21 C25 -91.8(9) . . . . ? N37 Fe1 N21 C25 -89.5(15) . . . . ? N11 Fe1 N21 C25 -176.6(9) . . . . ? C25 N21 C22 N23 0.5(16) . . . . ? Fe1 N21 C22 N23 -166.0(12) . . . . ? N21 C22 N23 C24 -0.3(18) . . . . ? C22 N23 C24 C25 0.0(18) . . . . ? N23 C24 C25 N21 0.2(18) . . . . ? N23 C24 C25 C26 177.1(15) . . . . ? C22 N21 C25 C24 -0.4(16) . . . . ? Fe1 N21 C25 C24 171.4(11) . . . . ? C22 N21 C25 C26 -177.8(13) . . . . ? Fe1 N21 C25 C26 -6.0(15) . . . . ? C24 C25 C26 N27 -170.3(16) . . . . ? N21 C25 C26 N27 6(2) . . . . ? C25 C26 N27 C28 -179.2(12) . . . . ? C25 C26 N27 Fe1 -3.0(17) . . . . ? N17 Fe1 N27 C26 -90.8(10) . . . . ? N21 Fe1 N27 C26 -0.2(10) . . . . ? N31 Fe1 N27 C26 85.1(11) . . . . ? N37 Fe1 N27 C26 159.9(10) . . . . ? N11 Fe1 N27 C26 0(2) . . . . ? N17 Fe1 N27 C28 85.4(11) . . . . ? N21 Fe1 N27 C28 176.0(11) . . . . ? N31 Fe1 N27 C28 -98.7(10) . . . . ? N37 Fe1 N27 C28 -23.9(11) . . . . ? N11 Fe1 N27 C28 176.6(13) . . . . ? C26 N27 C28 C29 114.1(15) . . . . ? Fe1 N27 C28 C29 -61.9(15) . . . . ? C39 N1 C29 C28 88.4(14) . . . . ? C19 N1 C29 C28 -145.0(12) . . . . ? N27 C28 C29 N1 57.0(17) . . . . ? N17 Fe1 N31 C32 84.6(19) . . . . ? N27 Fe1 N31 C32 -83.5(14) . . . . ? N21 Fe1 N31 C32 -7.4(14) . . . . ? N37 Fe1 N31 C32 173.4(15) . . . . ? N11 Fe1 N31 C32 79.5(14) . . . . ? N17 Fe1 N31 C35 -84.6(14) . . . . ? N27 Fe1 N31 C35 107.3(9) . . . . ? N21 Fe1 N31 C35 -176.6(9) . . . . ? N37 Fe1 N31 C35 4.2(8) . . . . ? N11 Fe1 N31 C35 -89.7(9) . . . . ? C35 N31 C32 N33 1.4(15) . . . . ? Fe1 N31 C32 N33 -168.2(10) . . . . ? N31 C32 N33 C34 -1.0(17) . . . . ? C32 N33 C34 C35 0.1(17) . . . . ? N33 C34 C35 N31 0.7(17) . . . . ? N33 C34 C35 C36 176.1(15) . . . . ? C32 N31 C35 C34 -1.3(15) . . . . ? Fe1 N31 C35 C34 171.6(9) . . . . ? C32 N31 C35 C36 -177.6(12) . . . . ? Fe1 N31 C35 C36 -4.7(14) . . . . ? C34 C35 C36 N37 -173.3(16) . . . . ? N31 C35 C36 N37 1.7(19) . . . . ? C35 C36 N37 C38 -178.5(12) . . . . ? C35 C36 N37 Fe1 2.4(17) . . . . ? N17 Fe1 N37 C36 156.0(10) . . . . ? N27 Fe1 N37 C36 -94.1(10) . . . . ? N21 Fe1 N37 C36 -6.1(18) . . . . ? N31 Fe1 N37 C36 -3.7(10) . . . . ? N11 Fe1 N37 C36 80.0(11) . . . . ? N17 Fe1 N37 C38 -23.1(11) . . . . ? N27 Fe1 N37 C38 86.8(10) . . . . ? N21 Fe1 N37 C38 174.8(12) . . . . ? N31 Fe1 N37 C38 177.2(11) . . . . ? N11 Fe1 N37 C38 -99.1(10) . . . . ? C36 N37 C38 C39 122.4(15) . . . . ? Fe1 N37 C38 C39 -58.5(15) . . . . ? C29 N1 C39 C38 -141.9(13) . . . . ? C19 N1 C39 C38 89.4(14) . . . . ? N37 C38 C39 N1 49.8(17) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.955 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.127 _exptl_crystal_id 'Walker/Burden 3,5 dm PNP' _diffrn_measurement_details 606,606,606,50,606,606,606,50,1209 _diffrn_measurement_total_frames-CCD 4945 _diffrn_measurement_frame_width-CCD 0.3 _diffrn_detector_distance-CCD 7.908 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_frame_time-CCD 13 _diffrn_measurement_total_time-CCD 27.68 _diffrn_measurement_frame_size-CCD 512 _chemical_absolute_configuration ad _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 -0.0895452 _diffrn_orient_matrix_UB_12 -0.0741956 _diffrn_orient_matrix_UB_13 0.0038403 _diffrn_orient_matrix_UB_21 -0.0351421 _diffrn_orient_matrix_UB_22 0.0435646 _diffrn_orient_matrix_UB_23 -0.0160944 _diffrn_orient_matrix_UB_31 0.0098899 _diffrn_orient_matrix_UB_32 -0.0441730 _diffrn_orient_matrix_UB_33 -0.0223589 _symmetry_space_group_name_Hall 'P 32 2"' _diffrn_measurement_specimen_support 'glass capillary' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' _reflns_Friedel_coverage 0.736 #_______________________________________________________________________________ # _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Flack, H.D. (1983), Acta Cryst. A39, 876-881. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (1990). Acta Cryst., A46, C-34. ; #===END