# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Catherine E Housecroft' 'Edwin Constable' 'Jennifer A Zampese' 'Guoqi Zhang.' _publ_contact_author_name 'Catherine E Housecroft' _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_section_title ; Mix and match: templating chiral Schiff base ligands to suit the needs of the metal ion ; # Attachment 'GQ114.CIF' data_gq114 _database_code_depnum_ccdc_archive 'CCDC 762383' #TrackingRef 'GQ114.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C50 H44 Fe N8), 2(F6 P), 2(Cl), H2 O' _chemical_formula_sum 'C100 H90 Cl2 F12 Fe2 N16 O P2' _chemical_formula_weight 2004.42 _chemical_absolute_configuration ad 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.068(2) _cell_length_b 15.986(3) _cell_length_c 25.723(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4551.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7544 _exptl_absorpt_correction_T_max 0.9901 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85405 _diffrn_reflns_av_R_equivalents 0.1587 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10448 _reflns_number_gt 9967 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0478P)^2^+2.1011P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(13) _refine_ls_number_reflns 10448 _refine_ls_number_parameters 625 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1146 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 0.87377(3) 0.98227(2) 0.053935(13) 0.01882(8) Uani 1 1 d . . . N1 N 0.7748(2) 0.92038(13) -0.00294(9) 0.0214(4) Uani 1 1 d D . . H1 H 0.819(3) 0.8775(16) -0.0148(13) 0.026 Uiso 1 1 d D . . N2 N 0.5643(2) 0.93243(15) -0.00636(10) 0.0272(5) Uani 1 1 d D . . H2 H 0.493(2) 0.907(2) -0.0036(15) 0.033 Uiso 1 1 d D . . N3 N 0.7407(2) 0.95371(12) 0.09609(9) 0.0216(4) Uani 1 1 d . . . N4 N 0.9250(2) 1.03822(12) 0.11825(9) 0.0238(4) Uani 1 1 d . . . C1 C 0.8753(3) 0.88681(19) -0.11182(12) 0.0356(6) Uani 1 1 d . . . H1A H 0.8678 0.8383 -0.0907 0.043 Uiso 1 1 calc R . . C2 C 0.9441(3) 0.8837(2) -0.15712(15) 0.0455(8) Uani 1 1 d . . . H2A H 0.9831 0.8330 -0.1667 0.055 Uiso 1 1 calc R . . C3 C 0.9559(3) 0.9536(3) -0.18827(13) 0.0453(8) Uani 1 1 d . . . H3A H 1.0022 0.9509 -0.2193 0.054 Uiso 1 1 calc R . . C4 C 0.9003(3) 1.0272(2) -0.17406(12) 0.0432(8) Uani 1 1 d . . . H4A H 0.9089 1.0755 -0.1952 0.052 Uiso 1 1 calc R . . C5 C 0.8318(3) 1.0310(2) -0.12893(12) 0.0347(6) Uani 1 1 d . . . H5A H 0.7941 1.0821 -0.1193 0.042 Uiso 1 1 calc R . . C6 C 0.8178(3) 0.96017(17) -0.09732(11) 0.0261(5) Uani 1 1 d . . . C7 C 0.7365(2) 0.96776(15) -0.05078(11) 0.0238(5) Uani 1 1 d . . . H7A H 0.7336 1.0283 -0.0412 0.029 Uiso 1 1 calc R . . C8 C 0.6059(2) 0.93951(16) -0.06015(11) 0.0264(5) Uani 1 1 d . . . H8A H 0.6040 0.8838 -0.0778 0.032 Uiso 1 1 calc R . . C9 C 0.5373(3) 1.00358(17) -0.09131(12) 0.0311(6) Uani 1 1 d . . . C10 C 0.5039(3) 1.0797(2) -0.06876(15) 0.0414(8) Uani 1 1 d . . . H10A H 0.5153 1.0885 -0.0326 0.050 Uiso 1 1 calc R . . C11 C 0.4542(4) 1.1425(2) -0.09919(19) 0.0549(10) Uani 1 1 d . . . H11A H 0.4322 1.1945 -0.0839 0.066 Uiso 1 1 calc R . . C12 C 0.4364(4) 1.1293(3) -0.15217(19) 0.0593(11) Uani 1 1 d . . . H12A H 0.4040 1.1728 -0.1731 0.071 Uiso 1 1 calc R . . C13 C 0.4654(4) 1.0544(3) -0.17405(17) 0.0615(12) Uani 1 1 d . . . H13A H 0.4505 1.0449 -0.2099 0.074 Uiso 1 1 calc R . . C14 C 0.5168(4) 0.9916(2) -0.14369(14) 0.0446(8) Uani 1 1 d . . . H14A H 0.5381 0.9398 -0.1593 0.053 Uiso 1 1 calc R . . C15 C 0.6590(2) 0.88716(16) 0.02065(11) 0.0231(5) Uani 1 1 d . . . H15A H 0.6514 0.8258 0.0137 0.028 Uiso 1 1 calc R . . C16 C 0.6530(2) 0.90370(15) 0.07824(11) 0.0229(5) Uani 1 1 d . . . C17 C 0.5647(3) 0.87193(19) 0.11072(12) 0.0310(6) Uani 1 1 d . . . H17A H 0.5043 0.8352 0.0978 0.037 Uiso 1 1 calc R . . C18 C 0.5666(3) 0.8952(2) 0.16285(13) 0.0376(7) Uani 1 1 d . . . H18A H 0.5072 0.8740 0.1860 0.045 Uiso 1 1 calc R . . C19 C 0.6544(3) 0.94883(19) 0.18088(12) 0.0321(6) Uani 1 1 d . . . H19A H 0.6552 0.9658 0.2163 0.038 Uiso 1 1 calc R . . C20 C 0.7416(3) 0.97764(16) 0.14672(10) 0.0244(5) Uani 1 1 d . . . C21 C 0.8453(3) 1.03177(16) 0.15849(11) 0.0260(5) Uani 1 1 d . . . C22 C 0.8635(3) 1.07249(19) 0.20542(12) 0.0352(6) Uani 1 1 d . . . H22A H 0.8064 1.0673 0.2328 0.042 Uiso 1 1 calc R . . C23 C 0.9661(4) 1.1207(2) 0.21181(13) 0.0414(8) Uani 1 1 d . . . H23A H 0.9809 1.1485 0.2438 0.050 Uiso 1 1 calc R . . C24 C 1.0471(3) 1.12815(19) 0.17110(13) 0.0369(7) Uani 1 1 d . . . H24A H 1.1177 1.1615 0.1746 0.044 Uiso 1 1 calc R . . C25 C 1.0233(3) 1.08597(17) 0.12501(12) 0.0295(6) Uani 1 1 d . . . H25A H 1.0790 1.0912 0.0971 0.035 Uiso 1 1 calc R . . N5 N 0.9681(2) 0.87350(12) 0.06926(9) 0.0204(4) Uani 1 1 d D . . H5 H 0.925(3) 0.8334(16) 0.0554(13) 0.024 Uiso 1 1 d D . . N6 N 1.1776(2) 0.87936(14) 0.07847(10) 0.0250(5) Uani 1 1 d D . . H6 H 1.247(2) 0.861(2) 0.0673(14) 0.030 Uiso 1 1 d D . . N7 N 1.0054(2) 1.00331(12) 0.00905(9) 0.0210(4) Uani 1 1 d . . . N8 N 0.8247(2) 1.09267(13) 0.02916(9) 0.0232(4) Uani 1 1 d . . . C26 C 0.8746(3) 0.72406(18) 0.13165(12) 0.0350(6) Uani 1 1 d . . . H26A H 0.8958 0.7094 0.0970 0.042 Uiso 1 1 calc R . . C27 C 0.7990(3) 0.6720(2) 0.16009(15) 0.0425(8) Uani 1 1 d . . . H27A H 0.7683 0.6224 0.1447 0.051 Uiso 1 1 calc R . . C28 C 0.7680(3) 0.6920(2) 0.21077(14) 0.0402(8) Uani 1 1 d . . . H28A H 0.7162 0.6562 0.2301 0.048 Uiso 1 1 calc R . . C29 C 0.8130(3) 0.7643(2) 0.23292(13) 0.0381(7) Uani 1 1 d . . . H29A H 0.7916 0.7787 0.2675 0.046 Uiso 1 1 calc R . . C30 C 0.8896(3) 0.81601(17) 0.20456(11) 0.0307(6) Uani 1 1 d . . . H30A H 0.9219 0.8648 0.2204 0.037 Uiso 1 1 calc R . . C31 C 0.9195(3) 0.79716(16) 0.15329(11) 0.0240(5) Uani 1 1 d . . . C32 C 1.0033(2) 0.85517(15) 0.12479(10) 0.0222(5) Uani 1 1 d . . . H32A H 1.0037 0.9096 0.1440 0.027 Uiso 1 1 calc R . . C33 C 1.1355(3) 0.82544(15) 0.12062(10) 0.0241(5) Uani 1 1 d . . . H33A H 1.1381 0.7655 0.1095 0.029 Uiso 1 1 calc R . . C34 C 1.2029(3) 0.83636(17) 0.17085(11) 0.0269(5) Uani 1 1 d . . . C35 C 1.2304(3) 0.76790(19) 0.20145(13) 0.0350(6) Uani 1 1 d . . . H35A H 1.2102 0.7132 0.1899 0.042 Uiso 1 1 calc R . . C36 C 1.2878(4) 0.7788(2) 0.24933(15) 0.0446(8) Uani 1 1 d . . . H36A H 1.3068 0.7315 0.2702 0.054 Uiso 1 1 calc R . . C37 C 1.3167(3) 0.8580(3) 0.26639(13) 0.0425(8) Uani 1 1 d . . . H37A H 1.3549 0.8654 0.2992 0.051 Uiso 1 1 calc R . . C38 C 1.2902(3) 0.9269(2) 0.23570(13) 0.0381(7) Uani 1 1 d . . . H38A H 1.3109 0.9814 0.2474 0.046 Uiso 1 1 calc R . . C39 C 1.2335(3) 0.91653(19) 0.18802(12) 0.0332(6) Uani 1 1 d . . . H39A H 1.2155 0.9639 0.1671 0.040 Uiso 1 1 calc R . . C40 C 1.0843(2) 0.87270(15) 0.03906(10) 0.0230(5) Uani 1 1 d . . . H40A H 1.0927 0.8186 0.0198 0.028 Uiso 1 1 calc R . . C41 C 1.0910(2) 0.94507(15) 0.00161(10) 0.0227(5) Uani 1 1 d . . . C42 C 1.1764(3) 0.95367(17) -0.03681(11) 0.0284(6) Uani 1 1 d . . . H42A H 1.2362 0.9118 -0.0418 0.034 Uiso 1 1 calc R . . C43 C 1.1742(3) 1.02484(18) -0.06849(11) 0.0314(6) Uani 1 1 d . . . H43A H 1.2331 1.0322 -0.0950 0.038 Uiso 1 1 calc R . . C44 C 1.0852(3) 1.08447(16) -0.06081(11) 0.0273(5) Uani 1 1 d . . . H44A H 1.0816 1.1328 -0.0823 0.033 Uiso 1 1 calc R . . C45 C 1.0012(3) 1.07278(15) -0.02128(10) 0.0235(5) Uani 1 1 d . . . C46 C 0.8988(2) 1.12604(15) -0.00748(10) 0.0231(5) Uani 1 1 d . . . C47 C 0.8756(3) 1.20392(16) -0.02983(12) 0.0306(6) Uani 1 1 d . . . H47A H 0.9278 1.2261 -0.0557 0.037 Uiso 1 1 calc R . . C48 C 0.7750(3) 1.24835(18) -0.01353(15) 0.0389(7) Uani 1 1 d . . . H48A H 0.7570 1.3015 -0.0282 0.047 Uiso 1 1 calc R . . C49 C 0.7018(3) 1.21467(19) 0.02396(14) 0.0379(7) Uani 1 1 d . . . H49A H 0.6327 1.2446 0.0356 0.045 Uiso 1 1 calc R . . C50 C 0.7287(3) 1.13661(16) 0.04493(11) 0.0277(6) Uani 1 1 d . . . H50A H 0.6776 1.1140 0.0711 0.033 Uiso 1 1 calc R . . Cl1 Cl 1.37261(7) 0.77312(4) 0.00907(3) 0.02822(13) Uani 1 1 d . . . P1 P 1.45697(9) 1.17530(5) 0.15959(4) 0.03829(19) Uani 1 1 d . . . F10 F 1.4534(2) 1.21845(16) 0.21545(9) 0.0575(6) Uani 1 1 d . . . F11 F 1.5313(2) 1.25382(14) 0.13787(10) 0.0546(6) Uani 1 1 d . . . F12 F 1.4621(3) 1.13634(16) 0.10274(10) 0.0638(7) Uani 1 1 d . . . F13 F 1.3820(3) 1.09885(16) 0.18135(11) 0.0749(8) Uani 1 1 d . . . F14 F 1.3341(2) 1.22131(19) 0.14452(11) 0.0657(7) Uani 1 1 d . . . F15 F 1.5804(2) 1.13188(15) 0.17471(12) 0.0659(7) Uani 1 1 d . . . O1 O 1.2694(6) 1.0523(3) 0.0640(3) 0.0595(15) Uani 0.50 1 d P . . 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 0.02310(16) 0.01494(14) 0.01843(15) -0.00093(12) 0.00223(14) 0.00005(13) N1 0.0255(11) 0.0194(9) 0.0193(10) 0.0010(8) 0.0014(9) -0.0021(8) N2 0.0224(11) 0.0309(11) 0.0282(12) 0.0030(9) -0.0014(10) -0.0019(9) N3 0.0258(10) 0.0167(9) 0.0224(10) 0.0015(8) 0.0018(9) 0.0026(8) N4 0.0327(11) 0.0156(9) 0.0231(10) -0.0020(7) 0.0002(9) 0.0004(8) C1 0.0423(15) 0.0371(14) 0.0273(14) -0.0001(11) 0.0054(14) 0.0040(14) C2 0.0456(19) 0.0542(19) 0.0366(17) -0.0061(15) 0.0086(16) 0.0041(16) C3 0.0415(18) 0.071(2) 0.0230(14) -0.0003(15) 0.0086(14) -0.0119(17) C4 0.054(2) 0.0540(19) 0.0219(13) 0.0074(13) -0.0002(13) -0.0192(16) C5 0.0433(16) 0.0347(15) 0.0262(14) 0.0045(11) -0.0021(13) -0.0105(13) C6 0.0271(13) 0.0304(13) 0.0210(12) -0.0008(10) -0.0030(11) -0.0049(10) C7 0.0276(12) 0.0224(11) 0.0215(11) 0.0007(9) -0.0028(11) -0.0023(9) C8 0.0294(14) 0.0262(11) 0.0236(12) 0.0012(10) -0.0045(11) -0.0033(10) C9 0.0293(13) 0.0308(14) 0.0333(14) 0.0070(11) -0.0045(12) -0.0027(11) C10 0.0458(18) 0.0342(15) 0.0441(19) 0.0068(14) -0.0090(15) 0.0075(13) C11 0.051(2) 0.0391(17) 0.074(3) 0.0163(19) -0.012(2) 0.0073(16) C12 0.057(2) 0.055(2) 0.066(3) 0.032(2) -0.022(2) -0.0002(19) C13 0.066(3) 0.074(3) 0.044(2) 0.025(2) -0.023(2) -0.012(2) C14 0.0509(19) 0.0454(17) 0.0373(17) 0.0084(14) -0.0136(15) -0.0078(16) C15 0.0262(13) 0.0194(11) 0.0236(12) 0.0016(9) 0.0011(10) -0.0031(9) C16 0.0216(12) 0.0205(10) 0.0266(12) -0.0005(9) 0.0007(10) 0.0010(9) C17 0.0267(13) 0.0350(14) 0.0312(14) 0.0036(12) 0.0029(12) -0.0058(12) C18 0.0354(16) 0.0482(17) 0.0292(15) 0.0080(13) 0.0082(14) -0.0015(14) C19 0.0369(16) 0.0350(14) 0.0243(13) -0.0008(11) 0.0067(12) 0.0028(12) C20 0.0297(12) 0.0206(11) 0.0228(12) -0.0018(10) 0.0038(10) 0.0030(10) C21 0.0315(14) 0.0229(11) 0.0236(12) -0.0019(9) 0.0032(11) 0.0038(10) C22 0.0438(17) 0.0367(14) 0.0252(13) -0.0084(11) 0.0018(14) 0.0028(14) C23 0.058(2) 0.0366(15) 0.0299(15) -0.0145(13) -0.0020(15) -0.0045(15) C24 0.0400(17) 0.0328(14) 0.0378(17) -0.0107(13) -0.0019(14) -0.0080(13) C25 0.0356(15) 0.0255(12) 0.0274(13) -0.0062(11) 0.0004(12) -0.0044(11) N5 0.0241(10) 0.0165(9) 0.0205(10) -0.0009(7) -0.0004(8) 0.0017(8) N6 0.0209(10) 0.0254(10) 0.0288(12) 0.0034(9) 0.0015(9) 0.0021(9) N7 0.0263(10) 0.0161(9) 0.0206(10) -0.0003(7) 0.0009(9) -0.0014(7) N8 0.0260(11) 0.0184(9) 0.0253(11) -0.0035(8) 0.0000(9) -0.0004(8) C26 0.0449(16) 0.0331(14) 0.0271(13) 0.0016(11) 0.0044(14) -0.0077(14) C27 0.049(2) 0.0369(16) 0.0411(18) 0.0069(14) 0.0050(16) -0.0133(15) C28 0.0424(18) 0.0381(16) 0.0401(18) 0.0145(13) 0.0094(15) -0.0034(14) C29 0.0450(18) 0.0415(16) 0.0278(14) 0.0103(13) 0.0083(14) 0.0089(14) C30 0.0397(16) 0.0284(12) 0.0240(12) 0.0030(10) 0.0008(12) 0.0030(12) C31 0.0261(12) 0.0220(11) 0.0240(12) 0.0025(10) 0.0000(11) 0.0034(10) C32 0.0272(13) 0.0200(11) 0.0194(12) 0.0000(9) 0.0009(10) 0.0030(10) C33 0.0250(12) 0.0212(10) 0.0263(12) 0.0002(9) 0.0009(11) 0.0025(10) C34 0.0257(13) 0.0288(13) 0.0262(13) 0.0015(11) 0.0008(11) 0.0020(10) C35 0.0387(16) 0.0290(13) 0.0373(16) 0.0067(12) -0.0057(14) 0.0012(12) C36 0.048(2) 0.0469(18) 0.0394(18) 0.0131(15) -0.0110(16) -0.0012(16) C37 0.0375(17) 0.063(2) 0.0269(15) 0.0025(15) -0.0074(13) -0.0057(16) C38 0.0370(16) 0.0450(17) 0.0324(16) -0.0081(13) -0.0043(14) -0.0068(14) C39 0.0367(16) 0.0329(14) 0.0299(14) -0.0019(11) -0.0041(13) -0.0032(12) C40 0.0275(12) 0.0172(10) 0.0244(12) 0.0007(9) 0.0024(10) 0.0030(9) C41 0.0252(12) 0.0194(10) 0.0235(12) -0.0028(9) 0.0027(10) 0.0023(9) C42 0.0316(13) 0.0278(12) 0.0258(13) 0.0010(10) 0.0061(12) 0.0048(10) C43 0.0365(14) 0.0301(13) 0.0275(13) 0.0028(11) 0.0102(12) -0.0017(12) C44 0.0331(13) 0.0208(11) 0.0279(13) 0.0031(10) 0.0051(12) -0.0038(10) C45 0.0304(13) 0.0171(10) 0.0228(12) -0.0003(9) -0.0003(11) -0.0009(10) C46 0.0299(13) 0.0171(10) 0.0224(11) -0.0005(9) -0.0013(10) 0.0004(9) C47 0.0348(14) 0.0206(11) 0.0366(14) 0.0055(10) 0.0003(14) 0.0016(11) C48 0.0446(18) 0.0221(12) 0.0500(19) 0.0083(12) 0.0003(16) 0.0072(12) C49 0.0406(17) 0.0262(13) 0.0468(19) 0.0002(13) 0.0043(15) 0.0107(12) C50 0.0325(14) 0.0197(11) 0.0309(14) -0.0011(10) 0.0033(12) 0.0078(10) Cl1 0.0330(3) 0.0205(2) 0.0312(3) -0.0049(2) 0.0024(3) 0.0004(3) P1 0.0443(5) 0.0341(4) 0.0365(4) 0.0086(3) 0.0095(4) 0.0019(3) F10 0.0585(14) 0.0715(15) 0.0424(12) -0.0054(11) 0.0127(11) -0.0078(12) F11 0.0621(14) 0.0469(11) 0.0549(14) 0.0194(10) 0.0032(11) -0.0126(10) F12 0.0769(17) 0.0668(14) 0.0476(13) -0.0177(12) 0.0127(13) -0.0097(14) F13 0.105(2) 0.0564(13) 0.0633(16) 0.0157(12) 0.0049(17) -0.0351(15) F14 0.0471(13) 0.0849(18) 0.0649(17) 0.0034(14) -0.0024(12) 0.0145(13) F15 0.0707(16) 0.0461(12) 0.0810(18) 0.0064(12) -0.0043(14) 0.0250(12) O1 0.069(4) 0.041(3) 0.069(4) 0.005(3) -0.005(3) -0.012(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 N3 1.885(2) . ? Fe1 N7 1.889(2) . ? Fe1 N8 1.954(2) . ? Fe1 N4 1.964(2) . ? Fe1 N5 2.066(2) . ? Fe1 N1 2.078(2) . ? N1 C7 1.506(3) . ? N1 C15 1.514(3) . ? N1 H1 0.894(18) . ? N2 C15 1.451(4) . ? N2 C8 1.463(4) . ? N2 H2 0.894(18) . ? N3 C16 1.339(3) . ? N3 C20 1.358(3) . ? N4 C25 1.340(4) . ? N4 C21 1.364(4) . ? C1 C6 1.385(4) . ? C1 C2 1.393(5) . ? C1 H1A 0.9500 . ? C2 C3 1.381(5) . ? C2 H2A 0.9500 . ? C3 C4 1.377(6) . ? C3 H3A 0.9500 . ? C4 C5 1.388(5) . ? C4 H4A 0.9500 . ? C5 C6 1.403(4) . ? C5 H5A 0.9500 . ? C6 C7 1.502(4) . ? C7 C8 1.533(4) . ? C7 H7A 1.0000 . ? C8 C9 1.506(4) . ? C8 H8A 1.0000 . ? C9 C14 1.380(5) . ? C9 C10 1.398(5) . ? C10 C11 1.387(5) . ? C10 H10A 0.9500 . ? C11 C12 1.393(7) . ? C11 H11A 0.9500 . ? C12 C13 1.362(7) . ? C12 H12A 0.9500 . ? C13 C14 1.393(5) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.506(4) . ? C15 H15A 1.0000 . ? C16 C17 1.382(4) . ? C17 C18 1.392(4) . ? C17 H17A 0.9500 . ? C18 C19 1.376(5) . ? C18 H18A 0.9500 . ? C19 C20 1.384(4) . ? C19 H19A 0.9500 . ? C20 C21 1.469(4) . ? C21 C22 1.386(4) . ? C22 C23 1.382(5) . ? C22 H22A 0.9500 . ? C23 C24 1.384(5) . ? C23 H23A 0.9500 . ? C24 C25 1.389(4) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N5 C40 1.503(3) . ? N5 C32 1.509(3) . ? N5 H5 0.873(18) . ? N6 C40 1.451(4) . ? N6 C33 1.461(3) . ? N6 H6 0.871(18) . ? N7 C41 1.342(3) . ? N7 C45 1.358(3) . ? N8 C50 1.337(3) . ? N8 C46 1.358(4) . ? C26 C31 1.386(4) . ? C26 C27 1.388(4) . ? C26 H26A 0.9500 . ? C27 C28 1.385(5) . ? C27 H27A 0.9500 . ? C28 C29 1.382(5) . ? C28 H28A 0.9500 . ? C29 C30 1.391(4) . ? C29 H29A 0.9500 . ? C30 C31 1.393(4) . ? C30 H30A 0.9500 . ? C31 C32 1.503(4) . ? C32 C33 1.542(4) . ? C32 H32A 1.0000 . ? C33 C34 1.503(4) . ? C33 H33A 1.0000 . ? C34 C35 1.382(4) . ? C34 C39 1.397(4) . ? C35 C36 1.397(5) . ? C35 H35A 0.9500 . ? C36 C37 1.378(5) . ? C36 H36A 0.9500 . ? C37 C38 1.386(5) . ? C37 H37A 0.9500 . ? C38 C39 1.388(4) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C41 1.507(3) . ? C40 H40A 1.0000 . ? C41 C42 1.375(4) . ? C42 C43 1.400(4) . ? C42 H42A 0.9500 . ? C43 C44 1.385(4) . ? C43 H43A 0.9500 . ? C44 C45 1.390(4) . ? C44 H44A 0.9500 . ? C45 C46 1.461(4) . ? C46 C47 1.395(3) . ? C47 C48 1.386(4) . ? C47 H47A 0.9500 . ? C48 C49 1.370(5) . ? C48 H48A 0.9500 . ? C49 C50 1.392(4) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? P1 F13 1.579(2) . ? P1 F15 1.581(3) . ? P1 F12 1.590(3) . ? P1 F14 1.594(3) . ? P1 F10 1.594(3) . ? P1 F11 1.602(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N7 175.75(9) . . ? N3 Fe1 N8 100.91(10) . . ? N7 Fe1 N8 81.61(9) . . ? N3 Fe1 N4 81.45(10) . . ? N7 Fe1 N4 102.18(10) . . ? N8 Fe1 N4 86.77(9) . . ? N3 Fe1 N5 94.66(9) . . ? N7 Fe1 N5 82.92(9) . . ? N8 Fe1 N5 164.38(9) . . ? N4 Fe1 N5 94.40(9) . . ? N3 Fe1 N1 82.98(9) . . ? N7 Fe1 N1 93.50(9) . . ? N8 Fe1 N1 93.09(9) . . ? N4 Fe1 N1 164.11(10) . . ? N5 Fe1 N1 90.01(9) . . ? C7 N1 C15 105.4(2) . . ? C7 N1 Fe1 118.97(15) . . ? C15 N1 Fe1 109.33(16) . . ? C7 N1 H1 105(2) . . ? C15 N1 H1 109(2) . . ? Fe1 N1 H1 109(2) . . ? C15 N2 C8 105.3(2) . . ? C15 N2 H2 112(2) . . ? C8 N2 H2 113(3) . . ? C16 N3 C20 120.1(2) . . ? C16 N3 Fe1 120.94(18) . . ? C20 N3 Fe1 118.59(19) . . ? C25 N4 C21 118.0(2) . . ? C25 N4 Fe1 127.1(2) . . ? C21 N4 Fe1 114.70(19) . . ? C6 C1 C2 120.5(3) . . ? C6 C1 H1A 119.8 . . ? C2 C1 H1A 119.8 . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 118.4(3) . . ? C1 C6 C7 123.9(3) . . ? C5 C6 C7 117.6(3) . . ? C6 C7 N1 116.2(2) . . ? C6 C7 C8 114.5(2) . . ? N1 C7 C8 104.2(2) . . ? C6 C7 H7A 107.1 . . ? N1 C7 H7A 107.1 . . ? C8 C7 H7A 107.1 . . ? N2 C8 C9 113.4(2) . . ? N2 C8 C7 99.8(2) . . ? C9 C8 C7 111.0(2) . . ? N2 C8 H8A 110.7 . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8A 110.7 . . ? C14 C9 C10 118.9(3) . . ? C14 C9 C8 120.6(3) . . ? C10 C9 C8 120.3(3) . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 119.9(4) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C9 C14 C13 121.0(4) . . ? C9 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? N2 C15 C16 110.6(2) . . ? N2 C15 N1 104.1(2) . . ? C16 C15 N1 111.7(2) . . ? N2 C15 H15A 110.1 . . ? C16 C15 H15A 110.1 . . ? N1 C15 H15A 110.1 . . ? N3 C16 C17 121.7(3) . . ? N3 C16 C15 114.2(2) . . ? C17 C16 C15 124.1(2) . . ? C16 C17 C18 118.2(3) . . ? C16 C17 H17A 120.9 . . ? C18 C17 H17A 120.9 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? N3 C20 C19 120.7(3) . . ? N3 C20 C21 111.6(2) . . ? C19 C20 C21 127.6(3) . . ? N4 C21 C22 122.1(3) . . ? N4 C21 C20 113.2(2) . . ? C22 C21 C20 124.7(3) . . ? C23 C22 C21 119.0(3) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C22 C23 C24 119.3(3) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C23 C24 C25 118.8(3) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? N4 C25 C24 122.8(3) . . ? N4 C25 H25A 118.6 . . ? C24 C25 H25A 118.6 . . ? C40 N5 C32 105.5(2) . . ? C40 N5 Fe1 109.94(15) . . ? C32 N5 Fe1 118.33(15) . . ? C40 N5 H5 104(2) . . ? C32 N5 H5 113(2) . . ? Fe1 N5 H5 105(2) . . ? C40 N6 C33 104.4(2) . . ? C40 N6 H6 112(2) . . ? C33 N6 H6 109(2) . . ? C41 N7 C45 120.6(2) . . ? C41 N7 Fe1 120.53(17) . . ? C45 N7 Fe1 118.06(18) . . ? C50 N8 C46 119.0(2) . . ? C50 N8 Fe1 126.6(2) . . ? C46 N8 Fe1 114.41(18) . . ? C31 C26 C27 120.6(3) . . ? C31 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C28 C27 C26 120.5(3) . . ? C28 C27 H27A 119.7 . . ? C26 C27 H27A 119.7 . . ? C29 C28 C27 119.4(3) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C28 C29 C30 120.1(3) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C29 C30 C31 120.9(3) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C26 C31 C30 118.5(3) . . ? C26 C31 C32 123.1(3) . . ? C30 C31 C32 118.4(2) . . ? C31 C32 N5 115.0(2) . . ? C31 C32 C33 115.4(2) . . ? N5 C32 C33 103.8(2) . . ? C31 C32 H32A 107.4 . . ? N5 C32 H32A 107.4 . . ? C33 C32 H32A 107.4 . . ? N6 C33 C34 114.3(2) . . ? N6 C33 C32 99.9(2) . . ? C34 C33 C32 112.1(2) . . ? N6 C33 H33A 110.1 . . ? C34 C33 H33A 110.1 . . ? C32 C33 H33A 110.1 . . ? C35 C34 C39 119.6(3) . . ? C35 C34 C33 120.5(3) . . ? C39 C34 C33 119.9(3) . . ? C34 C35 C36 120.2(3) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 119.9(3) . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? C37 C38 C39 120.3(3) . . ? C37 C38 H38A 119.8 . . ? C39 C38 H38A 119.8 . . ? C38 C39 C34 119.9(3) . . ? C38 C39 H39A 120.1 . . ? C34 C39 H39A 120.1 . . ? N6 C40 N5 104.3(2) . . ? N6 C40 C41 110.8(2) . . ? N5 C40 C41 111.5(2) . . ? N6 C40 H40A 110.0 . . ? N5 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? N7 C41 C42 121.2(2) . . ? N7 C41 C40 114.0(2) . . ? C42 C41 C40 124.7(2) . . ? C41 C42 C43 119.2(3) . . ? C41 C42 H42A 120.4 . . ? C43 C42 H42A 120.4 . . ? C44 C43 C42 119.3(3) . . ? C44 C43 H43A 120.4 . . ? C42 C43 H43A 120.4 . . ? C43 C44 C45 119.2(2) . . ? C43 C44 H44A 120.4 . . ? C45 C44 H44A 120.4 . . ? N7 C45 C44 120.5(2) . . ? N7 C45 C46 111.3(2) . . ? C44 C45 C46 128.2(2) . . ? N8 C46 C47 121.7(3) . . ? N8 C46 C45 114.1(2) . . ? C47 C46 C45 124.2(3) . . ? C48 C47 C46 118.7(3) . . ? C48 C47 H47A 120.6 . . ? C46 C47 H47A 120.6 . . ? C49 C48 C47 119.1(3) . . ? C49 C48 H48A 120.4 . . ? C47 C48 H48A 120.4 . . ? C48 C49 C50 119.9(3) . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? N8 C50 C49 121.6(3) . . ? N8 C50 H50A 119.2 . . ? C49 C50 H50A 119.2 . . ? F13 P1 F15 91.54(17) . . ? F13 P1 F12 92.39(15) . . ? F15 P1 F12 91.34(16) . . ? F13 P1 F14 89.73(17) . . ? F15 P1 F14 178.56(16) . . ? F12 P1 F14 89.29(16) . . ? F13 P1 F10 90.14(15) . . ? F15 P1 F10 89.39(15) . . ? F12 P1 F10 177.35(15) . . ? F14 P1 F10 89.92(15) . . ? F13 P1 F11 179.07(18) . . ? F15 P1 F11 89.19(14) . . ? F12 P1 F11 88.16(14) . . ? F14 P1 F11 89.53(15) . . ? F10 P1 F11 89.31(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.616 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.066 # Attachment 'GQ121R.CIF' data_gq121 _database_code_depnum_ccdc_archive 'CCDC 762384' #TrackingRef 'GQ121R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H38 Fe N6, 2(F6 P), C2 H3 N' _chemical_formula_sum 'C42 H41 F12 Fe N7 P2' _chemical_formula_weight 989.61 _chemical_absolute_configuration ad 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.908(2) _cell_length_b 15.486(3) _cell_length_c 27.657(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4243.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8583 _exptl_absorpt_correction_T_max 0.9493 _exptl_absorpt_process_details '(Blessing 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65615 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10228 _reflns_number_gt 9937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0435P)^2^+2.3680P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(10) _refine_ls_number_reflns 10228 _refine_ls_number_parameters 615 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.090 _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 0.67500(3) 0.038245(17) 0.143249(9) 0.01742(6) Uani 1 1 d . . . N1 N 0.78391(17) 0.14065(11) 0.12718(6) 0.0193(3) Uani 1 1 d . . . N2 N 0.81648(17) -0.01731(10) 0.10962(6) 0.0187(3) Uani 1 1 d . . . N3 N 0.60771(18) -0.08444(11) 0.15134(7) 0.0235(3) Uani 1 1 d . . . H3A H 0.5696 -0.0913 0.1814 0.028 Uiso 1 1 calc R . . H3C H 0.5432 -0.0965 0.1284 0.028 Uiso 1 1 calc R . . C1 C 0.7633(2) 0.22340(12) 0.13942(8) 0.0230(4) Uani 1 1 d . . . H1A H 0.6856 0.2376 0.1579 0.028 Uiso 1 1 calc R . . C2 C 0.8509(2) 0.28894(13) 0.12618(8) 0.0263(4) Uani 1 1 d . . . H2A H 0.8326 0.3470 0.1352 0.032 Uiso 1 1 calc R . . C3 C 0.9647(2) 0.26913(14) 0.09985(8) 0.0267(4) Uani 1 1 d . . . H3B H 1.0255 0.3133 0.0901 0.032 Uiso 1 1 calc R . . C4 C 0.9890(2) 0.18380(14) 0.08777(8) 0.0250(4) Uani 1 1 d . . . H4A H 1.0672 0.1683 0.0699 0.030 Uiso 1 1 calc R . . C5 C 0.8977(2) 0.12149(13) 0.10211(7) 0.0203(4) Uani 1 1 d . . . C6 C 0.91175(19) 0.02952(13) 0.09223(7) 0.0212(4) Uani 1 1 d . . . H6A H 0.9852 0.0062 0.0744 0.025 Uiso 1 1 calc R . . C7 C 0.80303(19) -0.11120(12) 0.10135(7) 0.0194(4) Uani 1 1 d . . . H7A H 0.7434 -0.1192 0.0725 0.023 Uiso 1 1 calc R . . C8 C 0.9347(2) -0.15590(12) 0.09070(8) 0.0218(4) Uani 1 1 d . . . C9 C 0.9723(2) -0.16877(14) 0.04260(9) 0.0286(4) Uani 1 1 d . . . H9A H 0.9130 -0.1515 0.0174 0.034 Uiso 1 1 calc R . . C10 C 1.0955(3) -0.20669(17) 0.03118(10) 0.0378(6) Uani 1 1 d . . . H10A H 1.1209 -0.2142 -0.0017 0.045 Uiso 1 1 calc R . . C11 C 1.1802(3) -0.23328(16) 0.06755(11) 0.0407(6) Uani 1 1 d . . . H11A H 1.2634 -0.2604 0.0598 0.049 Uiso 1 1 calc R . . C12 C 1.1454(2) -0.22085(17) 0.11515(11) 0.0395(6) Uani 1 1 d . . . H12A H 1.2049 -0.2391 0.1401 0.047 Uiso 1 1 calc R . . C13 C 1.0231(2) -0.18156(15) 0.12703(9) 0.0309(5) Uani 1 1 d . . . H13A H 1.0001 -0.1723 0.1600 0.037 Uiso 1 1 calc R . . C14 C 0.7249(2) -0.14394(12) 0.14573(8) 0.0204(3) Uani 1 1 d . . . H14A H 0.7843 -0.1367 0.1747 0.024 Uiso 1 1 calc R . . C15 C 0.6848(2) -0.23833(12) 0.14273(8) 0.0239(4) Uani 1 1 d . . . C16 C 0.5913(2) -0.26702(15) 0.10895(9) 0.0311(5) Uani 1 1 d . . . H16A H 0.5523 -0.2274 0.0868 0.037 Uiso 1 1 calc R . . C17 C 0.5550(3) -0.35333(16) 0.10750(11) 0.0402(6) Uani 1 1 d . . . H17A H 0.4907 -0.3725 0.0844 0.048 Uiso 1 1 calc R . . C18 C 0.6111(3) -0.41152(15) 0.13906(11) 0.0426(6) Uani 1 1 d . . . H18A H 0.5857 -0.4706 0.1377 0.051 Uiso 1 1 calc R . . C19 C 0.7035(3) -0.38438(16) 0.17252(10) 0.0425(6) Uani 1 1 d . . . H19A H 0.7423 -0.4247 0.1944 0.051 Uiso 1 1 calc R . . C20 C 0.7411(3) -0.29714(15) 0.17457(9) 0.0339(5) Uani 1 1 d . . . H20A H 0.8053 -0.2784 0.1978 0.041 Uiso 1 1 calc R . . N4 N 0.75105(17) 0.04145(11) 0.20905(6) 0.0205(3) Uani 1 1 d . . . N5 N 0.52968(17) 0.09210(10) 0.17548(6) 0.0195(3) Uani 1 1 d . . . N6 N 0.56062(17) 0.05771(11) 0.08426(6) 0.0216(3) Uani 1 1 d . . . H6B H 0.6138 0.0764 0.0591 0.026 Uiso 1 1 calc R . . H6C H 0.5201 0.0068 0.0752 0.026 Uiso 1 1 calc R . . C21 C 0.8729(2) 0.01555(13) 0.22418(8) 0.0247(4) Uani 1 1 d . . . H21A H 0.9311 -0.0125 0.2019 0.030 Uiso 1 1 calc R . . C22 C 0.9171(2) 0.02818(15) 0.27117(8) 0.0302(4) Uani 1 1 d . . . H22A H 1.0036 0.0081 0.2808 0.036 Uiso 1 1 calc R . . C23 C 0.8348(3) 0.07013(17) 0.30396(8) 0.0351(5) Uani 1 1 d . . . H23A H 0.8639 0.0795 0.3363 0.042 Uiso 1 1 calc R . . C24 C 0.7089(2) 0.09822(16) 0.28874(8) 0.0312(5) Uani 1 1 d . . . H24A H 0.6499 0.1269 0.3105 0.037 Uiso 1 1 calc R . . C25 C 0.6704(2) 0.08370(12) 0.24115(7) 0.0232(4) Uani 1 1 d . . . C26 C 0.5420(2) 0.10989(13) 0.22072(7) 0.0232(4) Uani 1 1 d . . . H26A H 0.4734 0.1376 0.2390 0.028 Uiso 1 1 calc R . . C27 C 0.40512(19) 0.10557(12) 0.14700(7) 0.0204(4) Uani 1 1 d . . . H27A H 0.3555 0.0494 0.1462 0.024 Uiso 1 1 calc R . . C28 C 0.3103(2) 0.17243(13) 0.16755(7) 0.0220(4) Uani 1 1 d . . . C29 C 0.1885(2) 0.14591(13) 0.18806(8) 0.0242(4) Uani 1 1 d . . . H29A H 0.1656 0.0863 0.1884 0.029 Uiso 1 1 calc R . . C30 C 0.1007(2) 0.20565(15) 0.20787(8) 0.0286(4) Uani 1 1 d . . . H30A H 0.0181 0.1869 0.2218 0.034 Uiso 1 1 calc R . . C31 C 0.1329(2) 0.29301(16) 0.20744(9) 0.0308(5) Uani 1 1 d . . . H31A H 0.0724 0.3341 0.2208 0.037 Uiso 1 1 calc R . . C32 C 0.2533(3) 0.31942(15) 0.18744(10) 0.0353(5) Uani 1 1 d . . . H32A H 0.2761 0.3790 0.1873 0.042 Uiso 1 1 calc R . . C33 C 0.3415(2) 0.25974(14) 0.16747(9) 0.0325(5) Uani 1 1 d . . . H33A H 0.4240 0.2788 0.1536 0.039 Uiso 1 1 calc R . . C34 C 0.4549(2) 0.12403(13) 0.09538(7) 0.0218(4) Uani 1 1 d . . . H34A H 0.4998 0.1819 0.0955 0.026 Uiso 1 1 calc R . . C35 C 0.3469(2) 0.12551(13) 0.05699(7) 0.0225(4) Uani 1 1 d . . . C36 C 0.3264(2) 0.19904(14) 0.02933(8) 0.0267(4) Uani 1 1 d . . . H36A H 0.3758 0.2501 0.0363 0.032 Uiso 1 1 calc R . . C37 C 0.2338(2) 0.19868(17) -0.00867(8) 0.0318(5) Uani 1 1 d . . . H37A H 0.2192 0.2498 -0.0269 0.038 Uiso 1 1 calc R . . C38 C 0.1633(3) 0.12458(17) -0.01996(8) 0.0337(5) Uani 1 1 d . . . H38A H 0.1020 0.1240 -0.0464 0.040 Uiso 1 1 calc R . . C39 C 0.1830(2) 0.05047(15) 0.00779(8) 0.0306(4) Uani 1 1 d . . . H39A H 0.1348 -0.0008 0.0003 0.037 Uiso 1 1 calc R . . C40 C 0.2721(2) 0.05125(14) 0.04611(8) 0.0263(4) Uani 1 1 d . . . H40A H 0.2828 0.0009 0.0653 0.032 Uiso 1 1 calc R . . P1 P 0.25740(7) 0.47022(4) 0.04511(2) 0.03295(13) Uani 1 1 d . . . F10 F 0.1052(3) 0.44486(19) 0.04614(19) 0.1381(17) Uani 1 1 d . . . F11 F 0.2187(3) 0.54411(14) 0.00729(9) 0.0733(6) Uani 1 1 d . . . F12 F 0.4088(2) 0.49733(16) 0.04026(14) 0.0921(9) Uani 1 1 d . . . F13 F 0.2802(3) 0.40592(14) 0.00050(8) 0.0780(8) Uani 1 1 d . . . F14 F 0.2364(4) 0.5369(2) 0.08634(9) 0.1080(11) Uani 1 1 d . . . F15 F 0.2921(4) 0.39451(17) 0.07968(9) 0.1037(11) Uani 1 1 d . . . P2 P 1.30451(8) -0.12277(4) 0.24151(3) 0.03782(15) Uani 1 1 d U . . F20 F 1.1879(2) -0.19481(17) 0.24140(10) 0.0785(7) Uani 1 1 d . A . F21 F 1.4189(4) -0.05394(19) 0.24058(9) 0.1061(12) Uani 1 1 d . A . F22 F 1.2049(5) -0.0739(2) 0.20308(17) 0.0827(17) Uani 0.618(6) 1 d P A 1 F23 F 1.2219(4) -0.0780(2) 0.28398(16) 0.0660(14) Uani 0.618(6) 1 d P A 1 F24 F 1.3677(4) -0.1719(3) 0.19643(16) 0.0656(14) Uani 0.618(6) 1 d P A 1 F25 F 1.3845(4) -0.1785(4) 0.2774(2) 0.0817(19) Uani 0.618(6) 1 d P A 1 F22' F 1.3206(8) -0.1118(6) 0.18551(19) 0.075(3) Uani 0.382(6) 1 d P A 2 F23' F 1.2335(14) -0.0373(7) 0.2451(5) 0.160(5) Uani 0.382(6) 1 d PU A 2 F24' F 1.4061(13) -0.1976(6) 0.2385(5) 0.144(4) Uani 0.382(6) 1 d PU A 2 F25' F 1.3214(9) -0.1185(6) 0.30000(19) 0.086(3) Uani 0.382(6) 1 d P A 2 N100 N -0.0390(2) 0.61548(14) -0.03570(9) 0.0390(5) Uani 1 1 d . . . C100 C -0.0633(3) 0.61193(16) 0.00456(10) 0.0354(5) Uani 1 1 d . . . C101 C -0.0957(3) 0.60539(19) 0.05575(10) 0.0435(6) Uani 1 1 d . . . H10B H -0.1691 0.6455 0.0635 0.065 Uiso 1 1 calc R . . H10C H -0.0158 0.6201 0.0750 0.065 Uiso 1 1 calc R . . H10D H -0.1239 0.5462 0.0632 0.065 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 0.01703(11) 0.01620(11) 0.01902(12) -0.00133(10) 0.00404(10) -0.00023(10) N1 0.0205(8) 0.0192(7) 0.0182(7) -0.0006(6) 0.0017(6) 0.0008(6) N2 0.0192(7) 0.0177(7) 0.0194(7) 0.0000(5) 0.0009(6) 0.0010(6) N3 0.0221(8) 0.0197(7) 0.0288(9) -0.0013(6) 0.0052(7) -0.0013(6) C1 0.0251(9) 0.0194(8) 0.0246(9) -0.0010(7) 0.0043(8) 0.0001(7) C2 0.0312(11) 0.0194(9) 0.0285(10) -0.0022(7) 0.0008(8) -0.0028(8) C3 0.0285(10) 0.0236(10) 0.0281(10) 0.0016(8) 0.0014(8) -0.0055(8) C4 0.0219(9) 0.0249(10) 0.0283(10) 0.0009(8) 0.0056(8) -0.0034(8) C5 0.0190(9) 0.0208(9) 0.0211(9) -0.0002(7) 0.0023(7) -0.0012(7) C6 0.0195(8) 0.0209(9) 0.0232(9) -0.0025(7) 0.0047(7) 0.0012(7) C7 0.0213(9) 0.0166(8) 0.0205(8) -0.0027(6) 0.0026(7) 0.0010(7) C8 0.0230(9) 0.0156(8) 0.0269(10) -0.0037(7) 0.0021(8) 0.0013(7) C9 0.0299(11) 0.0268(10) 0.0290(11) -0.0034(8) 0.0054(9) 0.0024(9) C10 0.0356(13) 0.0372(12) 0.0407(13) -0.0082(10) 0.0165(11) 0.0030(10) C11 0.0272(11) 0.0324(11) 0.0625(17) -0.0069(11) 0.0109(12) 0.0051(11) C12 0.0278(12) 0.0347(12) 0.0561(16) -0.0044(11) -0.0078(11) 0.0109(9) C13 0.0281(11) 0.0309(11) 0.0338(11) -0.0046(9) -0.0029(9) 0.0049(9) C14 0.0224(8) 0.0162(8) 0.0225(9) -0.0008(7) 0.0011(8) 0.0008(7) C15 0.0288(9) 0.0183(8) 0.0246(9) 0.0002(7) 0.0050(9) -0.0006(8) C16 0.0348(12) 0.0235(10) 0.0351(12) -0.0002(9) -0.0026(10) -0.0025(9) C17 0.0416(14) 0.0298(12) 0.0494(15) -0.0087(11) -0.0003(12) -0.0109(10) C18 0.0533(15) 0.0206(10) 0.0537(16) -0.0032(10) 0.0178(14) -0.0079(10) C19 0.0588(18) 0.0238(11) 0.0449(14) 0.0106(10) 0.0049(12) 0.0032(11) C20 0.0458(14) 0.0250(10) 0.0308(11) 0.0043(9) -0.0026(10) 0.0004(10) N4 0.0234(8) 0.0174(7) 0.0208(7) 0.0000(6) 0.0033(6) -0.0017(7) N5 0.0199(7) 0.0159(7) 0.0227(8) -0.0004(6) 0.0045(6) 0.0000(6) N6 0.0189(7) 0.0237(8) 0.0221(8) -0.0029(6) 0.0031(6) 0.0010(6) C21 0.0237(9) 0.0219(9) 0.0284(10) -0.0002(7) 0.0010(8) -0.0003(7) C22 0.0306(10) 0.0298(11) 0.0300(10) 0.0056(9) -0.0043(8) -0.0011(9) C23 0.0405(13) 0.0422(12) 0.0225(10) 0.0001(9) -0.0036(10) -0.0068(11) C24 0.0355(12) 0.0358(11) 0.0223(10) -0.0045(8) 0.0049(8) -0.0023(9) C25 0.0271(9) 0.0216(9) 0.0208(9) -0.0007(7) 0.0049(8) -0.0029(8) C26 0.0248(9) 0.0215(9) 0.0233(9) -0.0018(7) 0.0080(7) -0.0021(8) C27 0.0182(8) 0.0178(8) 0.0252(9) -0.0003(7) 0.0037(7) 0.0013(7) C28 0.0218(9) 0.0224(9) 0.0218(9) -0.0005(7) 0.0038(8) 0.0027(8) C29 0.0209(9) 0.0249(9) 0.0270(9) 0.0001(7) 0.0020(8) 0.0019(8) C30 0.0230(10) 0.0330(11) 0.0299(11) -0.0001(9) 0.0071(8) 0.0048(9) C31 0.0320(11) 0.0303(11) 0.0300(11) -0.0026(9) 0.0041(9) 0.0123(9) C32 0.0389(13) 0.0203(10) 0.0467(14) -0.0030(9) 0.0088(11) 0.0048(10) C33 0.0305(11) 0.0219(9) 0.0452(13) -0.0018(9) 0.0140(10) -0.0011(9) C34 0.0194(8) 0.0220(9) 0.0239(9) -0.0025(7) 0.0028(7) 0.0003(7) C35 0.0183(9) 0.0233(9) 0.0260(9) -0.0020(7) 0.0029(7) 0.0025(7) C36 0.0260(10) 0.0258(9) 0.0283(10) 0.0022(8) 0.0027(9) -0.0033(9) C37 0.0285(11) 0.0397(12) 0.0274(11) 0.0067(9) 0.0008(9) 0.0010(10) C38 0.0288(11) 0.0477(13) 0.0246(10) -0.0050(9) -0.0006(9) 0.0015(11) C39 0.0222(9) 0.0327(11) 0.0368(11) -0.0088(9) 0.0024(9) -0.0024(9) C40 0.0232(9) 0.0232(9) 0.0325(10) -0.0036(8) 0.0021(8) 0.0018(8) P1 0.0349(3) 0.0305(3) 0.0335(3) 0.0027(2) 0.0040(2) 0.0002(3) F10 0.0481(13) 0.0722(17) 0.294(5) 0.051(2) 0.040(2) -0.0165(13) F11 0.0855(16) 0.0522(11) 0.0822(15) 0.0295(11) -0.0012(12) 0.0081(11) F12 0.0317(10) 0.0757(15) 0.169(3) -0.0377(17) -0.0013(13) 0.0016(10) F13 0.132(2) 0.0515(11) 0.0507(11) -0.0186(9) -0.0085(13) 0.0007(13) F14 0.169(3) 0.0930(18) 0.0618(14) -0.0332(14) 0.0208(17) 0.050(2) F15 0.181(3) 0.0785(15) 0.0512(12) 0.0297(11) 0.0068(17) 0.055(2) P2 0.0496(4) 0.0266(3) 0.0373(3) 0.0062(2) 0.0148(3) 0.0032(3) F20 0.0587(13) 0.0844(15) 0.0924(17) -0.0129(13) 0.0242(13) -0.0247(12) F21 0.157(3) 0.101(2) 0.0604(13) -0.0130(13) 0.0384(16) -0.096(2) F22 0.111(4) 0.055(2) 0.082(3) 0.0168(19) -0.039(3) 0.007(2) F23 0.072(3) 0.054(2) 0.072(3) -0.0240(18) 0.027(2) -0.0088(18) F24 0.062(2) 0.065(2) 0.071(3) -0.026(2) 0.0404(19) -0.0225(19) F25 0.058(2) 0.100(4) 0.086(4) 0.061(3) -0.006(2) 0.001(2) F22' 0.084(5) 0.104(6) 0.035(3) -0.009(3) 0.009(3) -0.043(5) F23' 0.217(10) 0.116(7) 0.147(9) -0.020(7) -0.016(8) 0.127(7) F24' 0.187(10) 0.087(6) 0.157(10) -0.023(6) -0.042(8) 0.078(6) F25' 0.104(6) 0.117(6) 0.036(3) 0.018(3) 0.022(3) -0.050(6) N100 0.0438(12) 0.0309(10) 0.0423(12) -0.0037(9) 0.0049(10) -0.0043(9) C100 0.0308(12) 0.0261(11) 0.0494(15) -0.0068(10) 0.0020(10) -0.0027(9) C101 0.0473(15) 0.0413(14) 0.0419(14) -0.0064(11) 0.0101(12) -0.0014(12) _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 N5 1.8876(17) . ? Fe1 N2 1.8894(17) . ? Fe1 N1 1.9689(17) . ? Fe1 N4 1.9704(17) . ? Fe1 N6 2.0093(18) . ? Fe1 N3 2.0259(17) . ? N1 C1 1.341(2) . ? N1 C5 1.356(2) . ? N2 C6 1.284(3) . ? N2 C7 1.478(2) . ? N3 C14 1.490(3) . ? N3 H3A 0.9200 . ? N3 H3C 0.9200 . ? C1 C2 1.385(3) . ? C1 H1A 0.9500 . ? C2 C3 1.377(3) . ? C2 H2A 0.9500 . ? C3 C4 1.384(3) . ? C3 H3B 0.9500 . ? C4 C5 1.381(3) . ? C4 H4A 0.9500 . ? C5 C6 1.457(3) . ? C6 H6A 0.9500 . ? C7 C8 1.506(3) . ? C7 C14 1.537(3) . ? C7 H7A 1.0000 . ? C8 C13 1.391(3) . ? C8 C9 1.395(3) . ? C9 C10 1.391(3) . ? C9 H9A 0.9500 . ? C10 C11 1.374(4) . ? C10 H10A 0.9500 . ? C11 C12 1.374(4) . ? C11 H11A 0.9500 . ? C12 C13 1.395(3) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.517(3) . ? C14 H14A 1.0000 . ? C15 C20 1.384(3) . ? C15 C16 1.388(3) . ? C16 C17 1.385(3) . ? C16 H16A 0.9500 . ? C17 C18 1.372(4) . ? C17 H17A 0.9500 . ? C18 C19 1.368(4) . ? C18 H18A 0.9500 . ? C19 C20 1.403(3) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? N4 C21 1.339(3) . ? N4 C25 1.362(3) . ? N5 C26 1.287(3) . ? N5 C27 1.479(3) . ? N6 C34 1.499(3) . ? N6 H6B 0.9200 . ? N6 H6C 0.9200 . ? C21 C22 1.385(3) . ? C21 H21A 0.9500 . ? C22 C23 1.382(4) . ? C22 H22A 0.9500 . ? C23 C24 1.387(4) . ? C23 H23A 0.9500 . ? C24 C25 1.388(3) . ? C24 H24A 0.9500 . ? C25 C26 1.450(3) . ? C26 H26A 0.9500 . ? C27 C28 1.509(3) . ? C27 C34 1.538(3) . ? C27 H27A 1.0000 . ? C28 C33 1.387(3) . ? C28 C29 1.396(3) . ? C29 C30 1.383(3) . ? C29 H29A 0.9500 . ? C30 C31 1.390(3) . ? C30 H30A 0.9500 . ? C31 C32 1.377(4) . ? C31 H31A 0.9500 . ? C32 C33 1.386(3) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.508(3) . ? C34 H34A 1.0000 . ? C35 C36 1.387(3) . ? C35 C40 1.401(3) . ? C36 C37 1.395(3) . ? C36 H36A 0.9500 . ? C37 C38 1.379(4) . ? C37 H37A 0.9500 . ? C38 C39 1.394(4) . ? C38 H38A 0.9500 . ? C39 C40 1.379(3) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? P1 F15 1.551(2) . ? P1 F14 1.552(2) . ? P1 F10 1.559(3) . ? P1 F12 1.564(2) . ? P1 F11 1.597(2) . ? P1 F13 1.602(2) . ? P2 F23' 1.502(7) . ? P2 F25 1.536(4) . ? P2 F24' 1.537(8) . ? P2 F21 1.556(2) . ? P2 F22' 1.566(5) . ? P2 F24 1.589(3) . ? P2 F23 1.590(3) . ? P2 F20 1.606(2) . ? P2 F25' 1.628(6) . ? P2 F22 1.635(4) . ? N100 C100 1.141(4) . ? C100 C101 1.455(4) . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C101 H10D 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 N5 Fe1 N2 178.17(8) . . ? N5 Fe1 N1 99.72(7) . . ? N2 Fe1 N1 81.31(7) . . ? N5 Fe1 N4 81.05(7) . . ? N2 Fe1 N4 100.51(7) . . ? N1 Fe1 N4 88.78(7) . . ? N5 Fe1 N6 83.51(7) . . ? N2 Fe1 N6 95.00(7) . . ? N1 Fe1 N6 90.28(7) . . ? N4 Fe1 N6 164.14(7) . . ? N5 Fe1 N3 96.38(7) . . ? N2 Fe1 N3 82.62(7) . . ? N1 Fe1 N3 163.87(7) . . ? N4 Fe1 N3 92.72(7) . . ? N6 Fe1 N3 92.57(7) . . ? C1 N1 C5 117.69(17) . . ? C1 N1 Fe1 128.98(14) . . ? C5 N1 Fe1 113.25(13) . . ? C6 N2 C7 124.33(17) . . ? C6 N2 Fe1 118.21(13) . . ? C7 N2 Fe1 117.21(12) . . ? C14 N3 Fe1 108.17(12) . . ? C14 N3 H3A 110.1 . . ? Fe1 N3 H3A 110.1 . . ? C14 N3 H3C 110.1 . . ? Fe1 N3 H3C 110.1 . . ? H3A N3 H3C 108.4 . . ? N1 C1 C2 122.56(19) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 119.33(19) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 118.9(2) . . ? C2 C3 H3B 120.6 . . ? C4 C3 H3B 120.6 . . ? C5 C4 C3 118.9(2) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 122.58(19) . . ? N1 C5 C6 112.91(17) . . ? C4 C5 C6 124.51(18) . . ? N2 C6 C5 114.30(17) . . ? N2 C6 H6A 122.9 . . ? C5 C6 H6A 122.9 . . ? N2 C7 C8 113.85(16) . . ? N2 C7 C14 104.26(15) . . ? C8 C7 C14 116.16(16) . . ? N2 C7 H7A 107.4 . . ? C8 C7 H7A 107.4 . . ? C14 C7 H7A 107.4 . . ? C13 C8 C9 118.7(2) . . ? C13 C8 C7 122.37(19) . . ? C9 C8 C7 118.88(19) . . ? C10 C9 C8 120.7(2) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C11 C10 C9 119.8(2) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C8 C13 C12 120.1(2) . . ? C8 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? N3 C14 C15 113.41(16) . . ? N3 C14 C7 105.76(15) . . ? C15 C14 C7 113.96(16) . . ? N3 C14 H14A 107.8 . . ? C15 C14 H14A 107.8 . . ? C7 C14 H14A 107.8 . . ? C20 C15 C16 119.1(2) . . ? C20 C15 C14 119.6(2) . . ? C16 C15 C14 121.31(19) . . ? C17 C16 C15 120.1(2) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C16 120.7(3) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C19 C18 C17 120.0(2) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 120.1(2) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C15 C20 C19 120.1(2) . . ? C15 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C21 N4 C25 117.97(18) . . ? C21 N4 Fe1 128.74(14) . . ? C25 N4 Fe1 112.95(14) . . ? C26 N5 C27 124.53(17) . . ? C26 N5 Fe1 118.76(15) . . ? C27 N5 Fe1 116.58(13) . . ? C34 N6 Fe1 109.28(12) . . ? C34 N6 H6B 109.8 . . ? Fe1 N6 H6B 109.8 . . ? C34 N6 H6C 109.8 . . ? Fe1 N6 H6C 109.8 . . ? H6B N6 H6C 108.3 . . ? N4 C21 C22 122.4(2) . . ? N4 C21 H21A 118.8 . . ? C22 C21 H21A 118.8 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C22 C23 C24 118.6(2) . . ? C22 C23 H23A 120.7 . . ? C24 C23 H23A 120.7 . . ? C23 C24 C25 118.9(2) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? N4 C25 C24 122.3(2) . . ? N4 C25 C26 113.27(18) . . ? C24 C25 C26 124.4(2) . . ? N5 C26 C25 113.73(18) . . ? N5 C26 H26A 123.1 . . ? C25 C26 H26A 123.1 . . ? N5 C27 C28 114.57(16) . . ? N5 C27 C34 104.64(15) . . ? C28 C27 C34 114.97(16) . . ? N5 C27 H27A 107.4 . . ? C28 C27 H27A 107.4 . . ? C34 C27 H27A 107.4 . . ? C33 C28 C29 118.71(19) . . ? C33 C28 C27 121.97(19) . . ? C29 C28 C27 119.32(17) . . ? C30 C29 C28 120.5(2) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C31 120.2(2) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C32 C31 C30 119.4(2) . . ? C32 C31 H31A 120.3 . . ? C30 C31 H31A 120.3 . . ? C31 C32 C33 120.5(2) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C32 C33 C28 120.6(2) . . ? C32 C33 H33A 119.7 . . ? C28 C33 H33A 119.7 . . ? N6 C34 C35 111.22(16) . . ? N6 C34 C27 106.71(16) . . ? C35 C34 C27 115.38(16) . . ? N6 C34 H34A 107.8 . . ? C35 C34 H34A 107.8 . . ? C27 C34 H34A 107.8 . . ? C36 C35 C40 118.6(2) . . ? C36 C35 C34 120.31(19) . . ? C40 C35 C34 120.95(19) . . ? C35 C36 C37 120.6(2) . . ? C35 C36 H36A 119.7 . . ? C37 C36 H36A 119.7 . . ? C38 C37 C36 120.5(2) . . ? C38 C37 H37A 119.8 . . ? C36 C37 H37A 119.8 . . ? C37 C38 C39 119.3(2) . . ? C37 C38 H38A 120.4 . . ? C39 C38 H38A 120.4 . . ? C40 C39 C38 120.4(2) . . ? C40 C39 H39A 119.8 . . ? C38 C39 H39A 119.8 . . ? C39 C40 C35 120.7(2) . . ? C39 C40 H40A 119.6 . . ? C35 C40 H40A 119.6 . . ? F15 P1 F14 94.57(16) . . ? F15 P1 F10 90.7(2) . . ? F14 P1 F10 91.4(2) . . ? F15 P1 F12 92.5(2) . . ? F14 P1 F12 90.75(19) . . ? F10 P1 F12 176.0(2) . . ? F15 P1 F11 176.67(16) . . ? F14 P1 F11 88.41(15) . . ? F10 P1 F11 87.73(17) . . ? F12 P1 F11 88.94(16) . . ? F15 P1 F13 88.49(13) . . ? F14 P1 F13 176.74(16) . . ? F10 P1 F13 89.7(2) . . ? F12 P1 F13 88.01(16) . . ? F11 P1 F13 88.55(13) . . ? F23' P2 F25 133.9(5) . . ? F23' P2 F24' 167.0(8) . . ? F23' P2 F21 74.9(6) . . ? F25 P2 F21 91.1(2) . . ? F24' P2 F21 92.2(5) . . ? F23' P2 F22' 91.0(6) . . ? F25 P2 F22' 130.4(4) . . ? F24' P2 F22' 87.8(6) . . ? F21 P2 F22' 80.5(3) . . ? F23' P2 F24 131.2(6) . . ? F25 P2 F24 92.0(3) . . ? F24' P2 F24 48.6(5) . . ? F21 P2 F24 91.58(16) . . ? F23' P2 F23 47.6(5) . . ? F25 P2 F23 91.8(3) . . ? F24' P2 F23 134.8(6) . . ? F21 P2 F23 95.09(17) . . ? F22' P2 F23 137.4(4) . . ? F24 P2 F23 172.2(2) . . ? F23' P2 F20 106.0(6) . . ? F25 P2 F20 89.0(2) . . ? F24' P2 F20 87.0(5) . . ? F21 P2 F20 178.70(15) . . ? F22' P2 F20 98.4(3) . . ? F24 P2 F20 87.12(15) . . ? F23 P2 F20 86.21(16) . . ? F23' P2 F25' 86.9(6) . . ? F25 P2 F25' 47.7(4) . . ? F24' P2 F25' 91.0(6) . . ? F21 P2 F25' 85.1(2) . . ? F22' P2 F25' 165.5(3) . . ? F24 P2 F25' 139.4(4) . . ? F23 P2 F25' 45.6(4) . . ? F20 P2 F25' 96.0(2) . . ? F23' P2 F22 49.7(5) . . ? F25 P2 F22 172.4(2) . . ? F24' P2 F22 135.2(6) . . ? F21 P2 F22 96.4(2) . . ? F22' P2 F22 50.9(4) . . ? F24 P2 F22 87.1(3) . . ? F23 P2 F22 88.2(3) . . ? F20 P2 F22 83.5(2) . . ? F25' P2 F22 133.5(4) . . ? N100 C100 C101 178.7(3) . . ? C100 C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C100 C101 H10D 109.5 . . ? H10B C101 H10D 109.5 . . ? H10C C101 H10D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.714 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.054 # Attachment 'GQ128.CIF' data_gq128 _database_code_depnum_ccdc_archive 'CCDC 762385' #TrackingRef 'GQ128.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C72 H56 Fe2 N12), 16(F6 P), 8(C3 H6 O), 5(C2 H3 N), 3(H2 O)' _chemical_formula_sum 'C322 H293 F96 Fe8 N53 O11 P16' _chemical_formula_weight 7847.43 _chemical_absolute_configuration ad 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Tetragonal _symmetry_space_group_name_H-M I4(1) _symmetry_space_group_name_Hall I4bw loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' _cell_length_a 20.413(3) _cell_length_b 20.413(3) _cell_length_c 40.992(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17080(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7980 _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8380 _exptl_absorpt_correction_T_max 0.9025 _exptl_absorpt_process_details '(Blessing, 1951)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 188444 _diffrn_reflns_av_R_equivalents 0.1090 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.50 _reflns_number_total 21629 _reflns_number_gt 20883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS' _computing_cell_refinement 'Stoe IPDS' _computing_data_reduction 'Stoe IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0586P)^2^+15.7916P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.031(9) _refine_ls_number_reflns 21629 _refine_ls_number_parameters 1271 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.117 _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 Fe1A Fe 0.619742(16) 0.432380(16) 0.991288(8) 0.02566(7) Uani 1 1 d . . . N1A N 0.71099(11) 0.46232(11) 0.99415(6) 0.0356(5) Uani 1 1 d . . . N2A N 0.62314(10) 0.45316(11) 1.03590(5) 0.0300(4) Uani 1 1 d . . . N3A N 0.52810(10) 0.41229(9) 1.00349(5) 0.0260(4) Uani 1 1 d . . . N4A N 0.40600(10) 0.48422(10) 0.97050(5) 0.0268(4) Uani 1 1 d . . . N5A N 0.38248(10) 0.59469(11) 0.94779(6) 0.0298(4) Uani 1 1 d . . . N6A N 0.35111(10) 0.66003(10) 0.99657(6) 0.0311(4) Uani 1 1 d . . . C1A C 0.75248(15) 0.46934(16) 0.96924(9) 0.0461(7) Uani 1 1 d . . . H1AA H 0.7380 0.4588 0.9478 0.055 Uiso 1 1 calc R . . C2A C 0.81584(17) 0.4915(2) 0.97363(12) 0.0604(10) Uani 1 1 d . . . H2AA H 0.8444 0.4962 0.9555 0.073 Uiso 1 1 calc R . . C3A C 0.83674(17) 0.5066(2) 1.00428(12) 0.0647(11) Uani 1 1 d . . . H3AA H 0.8802 0.5220 1.0076 0.078 Uiso 1 1 calc R . . C4A C 0.79502(15) 0.49964(19) 1.03059(11) 0.0556(9) Uani 1 1 d . . . H4AA H 0.8094 0.5092 1.0521 0.067 Uiso 1 1 calc R . . C5A C 0.73198(13) 0.47831(14) 1.02475(8) 0.0401(6) Uani 1 1 d . . . C6A C 0.68057(14) 0.47164(14) 1.04942(7) 0.0378(6) Uani 1 1 d . . . C7A C 0.68444(17) 0.48091(18) 1.08308(8) 0.0499(7) Uani 1 1 d . . . H7AA H 0.7243 0.4950 1.0928 0.060 Uiso 1 1 calc R . . C8A C 0.63001(18) 0.46950(19) 1.10209(8) 0.0523(8) Uani 1 1 d . . . H8AA H 0.6326 0.4753 1.1250 0.063 Uiso 1 1 calc R . . C9A C 0.57128(16) 0.44957(17) 1.08798(7) 0.0440(6) Uani 1 1 d . . . H9AA H 0.5335 0.4415 1.1009 0.053 Uiso 1 1 calc R . . C10A C 0.56979(13) 0.44184(13) 1.05428(6) 0.0320(5) Uani 1 1 d . . . C11A C 0.51569(12) 0.41950(12) 1.03426(6) 0.0283(4) Uani 1 1 d . . . H11A H 0.4736 0.4107 1.0432 0.034 Uiso 1 1 calc R . . C12A C 0.47731(11) 0.38636(11) 0.98093(6) 0.0272(4) Uani 1 1 d . . . H12A H 0.4912 0.3988 0.9584 0.033 Uiso 1 1 calc R . . C13A C 0.40928(12) 0.41941(11) 0.98691(6) 0.0280(4) Uani 1 1 d . . . H13A H 0.4061 0.4279 1.0109 0.034 Uiso 1 1 calc R . . C14A C 0.47696(12) 0.31210(11) 0.98226(7) 0.0316(5) Uani 1 1 d . . . C15A C 0.46390(17) 0.27860(15) 1.01068(8) 0.0451(7) Uani 1 1 d . . . H15A H 0.4549 0.3020 1.0302 0.054 Uiso 1 1 calc R . . C16A C 0.4639(2) 0.21014(17) 1.01068(12) 0.0609(10) Uani 1 1 d . . . H16A H 0.4556 0.1866 1.0303 0.073 Uiso 1 1 calc R . . C17A C 0.4761(2) 0.17668(15) 0.98169(12) 0.0594(9) Uani 1 1 d . . . H17A H 0.4756 0.1301 0.9815 0.071 Uiso 1 1 calc R . . C18A C 0.48874(19) 0.20946(16) 0.95395(10) 0.0547(9) Uani 1 1 d . . . H18A H 0.4976 0.1860 0.9344 0.066 Uiso 1 1 calc R . . C19A C 0.48876(15) 0.27760(14) 0.95378(8) 0.0403(6) Uani 1 1 d . . . H19A H 0.4969 0.3006 0.9340 0.048 Uiso 1 1 calc R . . C20A C 0.35012(12) 0.37813(12) 0.97774(7) 0.0344(5) Uani 1 1 d . . . C21A C 0.30297(15) 0.36789(15) 1.00141(10) 0.0469(7) Uani 1 1 d . . . H21A H 0.3090 0.3851 1.0227 0.056 Uiso 1 1 calc R . . C22A C 0.24625(18) 0.33211(19) 0.99401(13) 0.0649(11) Uani 1 1 d . . . H22A H 0.2135 0.3258 1.0102 0.078 Uiso 1 1 calc R . . C23A C 0.23812(18) 0.3062(2) 0.96330(13) 0.0674(12) Uani 1 1 d . . . H23A H 0.1997 0.2820 0.9582 0.081 Uiso 1 1 calc R . . C24A C 0.28507(18) 0.31510(18) 0.94023(12) 0.0604(10) Uani 1 1 d . . . H24A H 0.2795 0.2964 0.9192 0.073 Uiso 1 1 calc R . . C25A C 0.34157(16) 0.35149(15) 0.94712(9) 0.0445(7) Uani 1 1 d . . . H25A H 0.3739 0.3578 0.9307 0.053 Uiso 1 1 calc R . . C26A C 0.40159(13) 0.55126(12) 0.92450(6) 0.0310(5) Uani 1 1 d . . . C27A C 0.41391(13) 0.48811(12) 0.93926(6) 0.0307(5) Uani 1 1 d . . . H27A H 0.4271 0.4514 0.9267 0.037 Uiso 1 1 calc R . . C28A C 0.40518(15) 0.56879(14) 0.89190(7) 0.0381(6) Uani 1 1 d . . . H28A H 0.4190 0.5383 0.8758 0.046 Uiso 1 1 calc R . . C29A C 0.38777(16) 0.63286(15) 0.88338(8) 0.0431(6) Uani 1 1 d . . . H29A H 0.3896 0.6464 0.8612 0.052 Uiso 1 1 calc R . . C30A C 0.36804(15) 0.67627(14) 0.90703(8) 0.0406(6) Uani 1 1 d . . . H30A H 0.3560 0.7198 0.9014 0.049 Uiso 1 1 calc R . . C31A C 0.36591(12) 0.65580(12) 0.93921(7) 0.0317(5) Uani 1 1 d . . . C32A C 0.34675(13) 0.69355(13) 0.96808(7) 0.0346(5) Uani 1 1 d . . . C33A C 0.32704(17) 0.75892(15) 0.96745(9) 0.0471(7) Uani 1 1 d . . . H33A H 0.3249 0.7822 0.9474 0.057 Uiso 1 1 calc R . . C34A C 0.3109(2) 0.78897(17) 0.99602(10) 0.0594(9) Uani 1 1 d . . . H34A H 0.2972 0.8335 0.9960 0.071 Uiso 1 1 calc R . . C35A C 0.31436(18) 0.75465(16) 1.02524(9) 0.0510(8) Uani 1 1 d . . . H35A H 0.3031 0.7750 1.0453 0.061 Uiso 1 1 calc R . . C36A C 0.33464(14) 0.68991(14) 1.02434(7) 0.0385(6) Uani 1 1 d . . . H36A H 0.3369 0.6660 1.0442 0.046 Uiso 1 1 calc R . . Fe1B Fe 0.581509(16) 0.111592(15) 0.728675(8) 0.02393(7) Uani 1 1 d . . . N1B N 0.56580(10) 0.20692(10) 0.72625(6) 0.0297(4) Uani 1 1 d . . . N2B N 0.56273(10) 0.12835(10) 0.77256(5) 0.0261(4) Uani 1 1 d . . . N3B N 0.59182(9) 0.02239(9) 0.74658(5) 0.0248(4) Uani 1 1 d . . . N4B N 0.50842(10) -0.09266(9) 0.71361(5) 0.0248(4) Uani 1 1 d . . . N5B N 0.40144(11) -0.09684(10) 0.68453(6) 0.0314(4) Uani 1 1 d . . . N6B N 0.32206(10) -0.12462(11) 0.72861(7) 0.0356(5) Uani 1 1 d . . . C1B C 0.56974(15) 0.24465(13) 0.69961(7) 0.0367(5) Uani 1 1 d . . . H1BA H 0.5836 0.2253 0.6797 0.044 Uiso 1 1 calc R . . C2B C 0.55450(16) 0.31049(14) 0.69995(8) 0.0427(6) Uani 1 1 d . . . H2BA H 0.5588 0.3363 0.6808 0.051 Uiso 1 1 calc R . . C3B C 0.53299(18) 0.33783(14) 0.72871(10) 0.0496(7) Uani 1 1 d . . . H3BA H 0.5206 0.3827 0.7293 0.060 Uiso 1 1 calc R . . C4B C 0.52936(16) 0.30022(14) 0.75685(8) 0.0423(6) Uani 1 1 d . . . H4BA H 0.5153 0.3188 0.7769 0.051 Uiso 1 1 calc R . . C5B C 0.54680(12) 0.23491(12) 0.75480(7) 0.0319(5) Uani 1 1 d . . . C6B C 0.54658(12) 0.18902(12) 0.78259(7) 0.0306(5) Uani 1 1 d . . . C7B C 0.53196(14) 0.20109(15) 0.81505(7) 0.0391(6) Uani 1 1 d . . . H7BA H 0.5202 0.2439 0.8220 0.047 Uiso 1 1 calc R . . C8B C 0.53471(17) 0.15017(16) 0.83715(7) 0.0447(7) Uani 1 1 d . . . H8BA H 0.5253 0.1580 0.8595 0.054 Uiso 1 1 calc R . . C9B C 0.55120(15) 0.08766(15) 0.82685(7) 0.0389(6) Uani 1 1 d . . . H9BA H 0.5532 0.0523 0.8419 0.047 Uiso 1 1 calc R . . C10B C 0.56455(12) 0.07829(12) 0.79420(6) 0.0295(5) Uani 1 1 d . . . C11B C 0.58189(12) 0.01813(12) 0.77755(6) 0.0296(5) Uani 1 1 d . . . H11B H 0.5857 -0.0223 0.7889 0.035 Uiso 1 1 calc R . . C12B C 0.61369(11) -0.03561(11) 0.72786(6) 0.0281(4) Uani 1 1 d . . . H12B H 0.6082 -0.0243 0.7043 0.034 Uiso 1 1 calc R . . C13B C 0.56755(11) -0.09516(11) 0.73457(6) 0.0255(4) Uani 1 1 d . . . H13B H 0.5516 -0.0898 0.7575 0.031 Uiso 1 1 calc R . . C14B C 0.68669(12) -0.04722(12) 0.73309(9) 0.0383(6) Uani 1 1 d . . . C15B C 0.71463(17) -0.0554(2) 0.76301(12) 0.0686(12) Uani 1 1 d . . . H15B H 0.6875 -0.0560 0.7818 0.082 Uiso 1 1 calc R . . C16B C 0.7817(2) -0.0628(3) 0.76660(17) 0.094(2) Uani 1 1 d . . . H16B H 0.8002 -0.0689 0.7876 0.113 Uiso 1 1 calc R . . C17B C 0.82117(17) -0.0611(2) 0.73955(16) 0.0773(15) Uani 1 1 d . . . H17B H 0.8674 -0.0640 0.7418 0.093 Uiso 1 1 calc R . . C18B C 0.7939(2) -0.0554(2) 0.70975(16) 0.0783(15) Uani 1 1 d . . . H18B H 0.8213 -0.0568 0.6910 0.094 Uiso 1 1 calc R . . C19B C 0.72657(17) -0.04753(19) 0.70564(11) 0.0574(9) Uani 1 1 d . . . H19B H 0.7083 -0.0425 0.6845 0.069 Uiso 1 1 calc R . . C20B C 0.59878(11) -0.16267(11) 0.73298(7) 0.0323(5) Uani 1 1 d . . . C21B C 0.61661(16) -0.19154(17) 0.76237(10) 0.0497(8) Uani 1 1 d . . . H21B H 0.6101 -0.1686 0.7823 0.060 Uiso 1 1 calc R . . C22B C 0.6439(2) -0.2538(2) 0.76265(14) 0.0701(13) Uani 1 1 d . . . H22B H 0.6560 -0.2734 0.7828 0.084 Uiso 1 1 calc R . . C23B C 0.6533(2) -0.28695(17) 0.73423(17) 0.0801(16) Uani 1 1 d . . . H23B H 0.6719 -0.3296 0.7344 0.096 Uiso 1 1 calc R . . C24B C 0.6359(2) -0.2584(2) 0.70542(15) 0.0788(15) Uani 1 1 d . . . H24B H 0.6425 -0.2817 0.6856 0.095 Uiso 1 1 calc R . . C25B C 0.60876(18) -0.19604(16) 0.70429(9) 0.0507(8) Uani 1 1 d . . . H25B H 0.5973 -0.1767 0.6840 0.061 Uiso 1 1 calc R . . C26B C 0.51290(13) -0.08178(12) 0.68265(6) 0.0307(5) Uani 1 1 d . . . H26B H 0.5537 -0.0728 0.6724 0.037 Uiso 1 1 calc R . . C27B C 0.45222(15) -0.08400(13) 0.66451(7) 0.0357(5) Uani 1 1 d . . . C28B C 0.4430(2) -0.07538(16) 0.63122(8) 0.0512(8) Uani 1 1 d . . . H28B H 0.4788 -0.0662 0.6172 0.061 Uiso 1 1 calc R . . C29B C 0.3796(2) -0.0807(2) 0.61921(9) 0.0644(11) Uani 1 1 d . . . H29B H 0.3718 -0.0742 0.5966 0.077 Uiso 1 1 calc R . . C30B C 0.3288(2) -0.09489(18) 0.63922(10) 0.0611(11) Uani 1 1 d . . . H30B H 0.2858 -0.0994 0.6307 0.073 Uiso 1 1 calc R . . C31B C 0.34031(15) -0.10282(14) 0.67257(8) 0.0424(7) Uani 1 1 d . . . C32B C 0.29454(14) -0.11880(15) 0.69868(9) 0.0459(7) Uani 1 1 d . . . C33B C 0.22695(19) -0.1259(2) 0.69445(14) 0.0754(14) Uani 1 1 d . . . H33B H 0.2079 -0.1219 0.6734 0.090 Uiso 1 1 calc R . . C34B C 0.18887(19) -0.1388(3) 0.72104(16) 0.0908(19) Uani 1 1 d . . . H34B H 0.1430 -0.1446 0.7185 0.109 Uiso 1 1 calc R . . C35B C 0.21709(17) -0.1434(2) 0.75176(14) 0.0697(13) Uani 1 1 d . . . H35B H 0.1907 -0.1509 0.7705 0.084 Uiso 1 1 calc R . . C36B C 0.28438(15) -0.13681(16) 0.75468(10) 0.0471(7) Uani 1 1 d . . . H36B H 0.3042 -0.1410 0.7756 0.057 Uiso 1 1 calc R . . P1 P 1.15145(6) 0.37586(6) 1.10712(3) 0.0662(3) Uani 1 1 d . . . F10 F 1.11464(19) 0.4222(3) 1.08315(12) 0.140(2) Uani 1 1 d . . . F11 F 1.1516(2) 0.3177(3) 1.08295(12) 0.156(2) Uani 1 1 d . . . F12 F 1.1452(3) 0.42891(18) 1.13623(12) 0.1253(14) Uani 1 1 d . . . F13 F 1.08247(17) 0.35042(19) 1.12104(11) 0.1091(12) Uani 1 1 d . . . F14 F 1.21850(18) 0.4011(3) 1.09509(14) 0.159(2) Uani 1 1 d . . . F15 F 1.18849(18) 0.32970(17) 1.13227(9) 0.0980(10) Uani 1 1 d . . . P2 P 0.42223(6) 0.37386(6) 0.85122(3) 0.0642(3) Uani 1 1 d . . . F20 F 0.4555(2) 0.3691(3) 0.88627(10) 0.0760(15) Uani 0.651(6) 1 d P A 1 F21 F 0.4585(2) 0.44731(19) 0.84984(12) 0.0783(14) Uani 0.651(6) 1 d P A 1 F22 F 0.4832(4) 0.3493(3) 0.83317(15) 0.0757(17) Uani 0.651(6) 1 d PD A 1 F23 F 0.3896(3) 0.3938(3) 0.81733(13) 0.0935(18) Uani 0.651(6) 1 d P A 1 F24 F 0.3608(2) 0.4146(2) 0.86992(12) 0.0789(14) Uani 0.651(6) 1 d P A 1 F25 F 0.3864(4) 0.3125(2) 0.8547(2) 0.119(3) Uani 0.651(6) 1 d P A 1 F20' F 0.4629(5) 0.3036(4) 0.8715(2) 0.089(3) Uani 0.349(6) 1 d P A 2 F21' F 0.4490(4) 0.4106(5) 0.8780(2) 0.074(3) Uani 0.349(6) 1 d P A 2 F22' F 0.4081(6) 0.3088(5) 0.8255(2) 0.103(4) Uani 0.349(6) 1 d P A 2 F23' F 0.3929(5) 0.4222(8) 0.8342(3) 0.116(5) Uani 0.349(6) 1 d P A 2 F24' F 0.3610(5) 0.3483(8) 0.8714(2) 0.102(4) Uani 0.349(6) 1 d P A 2 F25' F 0.4950(6) 0.3791(6) 0.8327(3) 0.070(3) Uani 0.349(6) 1 d PD A 2 P3 P 0.72729(5) 0.17953(6) 0.85949(2) 0.0575(2) Uani 1 1 d . . . F30 F 0.75919(13) 0.22203(14) 0.88806(7) 0.0737(7) Uani 1 1 d . . . F31 F 0.69073(15) 0.24326(18) 0.84595(7) 0.0914(10) Uani 1 1 d . . . F32 F 0.66608(12) 0.16583(15) 0.88242(6) 0.0733(7) Uani 1 1 d . . . F33 F 0.78867(14) 0.19519(17) 0.83674(7) 0.0838(9) Uani 1 1 d . . . F34 F 0.76421(13) 0.11713(14) 0.87351(7) 0.0722(6) Uani 1 1 d . . . F35 F 0.69554(16) 0.1358(2) 0.83154(7) 0.0960(10) Uani 1 1 d . . . P4 P 1.0000 0.5000 0.93297(3) 0.0434(2) Uani 1 2 d S . . F40 F 0.95260(14) 0.43817(14) 0.93215(10) 0.0914(10) Uani 1 1 d . B . F41 F 1.0000 0.5000 0.9717(4) 0.195(9) Uani 0.489(17) 2 d SPU B 1 F42 F 1.0000 0.5000 0.8975(2) 0.197(15) Uani 0.489(17) 2 d SP B 1 F43 F 1.0587(4) 0.4521(4) 0.9385(5) 0.121(7) Uani 0.489(17) 1 d P B 1 F41' F 1.0430(4) 0.4688(6) 0.9581(3) 0.113(6) Uani 0.511(17) 1 d P B 2 F42' F 1.0437(5) 0.4696(6) 0.9042(3) 0.123(5) Uani 0.511(17) 1 d P B 2 P5 P 0.5000 0.0000 0.91963(3) 0.0383(2) Uani 1 2 d S . . F50 F 0.54521(13) 0.06223(13) 0.91997(10) 0.0940(11) Uani 1 1 d . C . F51 F 0.4354(3) 0.0422(3) 0.9336(2) 0.079(2) Uani 0.50 1 d P C 1 F52 F 0.4769(4) 0.0294(4) 0.88478(14) 0.107(3) Uani 0.50 1 d P . 1 F51' F 0.4906(5) 0.0211(3) 0.95473(16) 0.110(3) Uani 0.50 1 d P . 2 F52' F 0.4445(3) 0.0341(4) 0.9062(4) 0.134(4) Uani 0.50 1 d P C 2 O100 O 0.61500(16) -0.08928(17) 0.82916(7) 0.0705(8) Uani 1 1 d . . . C100 C 0.64687(18) -0.09604(18) 0.85372(9) 0.0512(8) Uani 1 1 d . . . C101 C 0.6876(2) -0.0437(2) 0.86855(15) 0.0735(12) Uani 1 1 d . . . H10A H 0.7339 -0.0561 0.8673 0.110 Uiso 1 1 calc R . . H10B H 0.6750 -0.0378 0.8914 0.110 Uiso 1 1 calc R . . H10C H 0.6808 -0.0026 0.8567 0.110 Uiso 1 1 calc R . . C102 C 0.6452(3) -0.1599(2) 0.87141(12) 0.0739(13) Uani 1 1 d . . . H10D H 0.6205 -0.1920 0.8585 0.111 Uiso 1 1 calc R . . H10E H 0.6239 -0.1540 0.8926 0.111 Uiso 1 1 calc R . . H10F H 0.6900 -0.1758 0.8747 0.111 Uiso 1 1 calc R . . O200 O 0.39615(19) 0.37239(17) 1.07639(8) 0.0810(10) Uani 1 1 d . . . C200 C 0.3666(3) 0.3357(3) 1.09379(14) 0.0802(14) Uani 1 1 d . . . C201 C 0.3282(3) 0.2783(3) 1.08099(16) 0.0892(16) Uani 1 1 d . . . H20A H 0.3286 0.2790 1.0571 0.134 Uiso 1 1 calc R . . H20B H 0.2829 0.2811 1.0888 0.134 Uiso 1 1 calc R . . H20C H 0.3481 0.2375 1.0887 0.134 Uiso 1 1 calc R . . C202 C 0.3628(4) 0.3466(5) 1.12987(16) 0.136(3) Uani 1 1 d . . . H20D H 0.3805 0.3084 1.1413 0.204 Uiso 1 1 calc R . . H20E H 0.3170 0.3531 1.1362 0.204 Uiso 1 1 calc R . . H20F H 0.3883 0.3856 1.1357 0.204 Uiso 1 1 calc R . . N300 N 0.7982(4) 0.4007(5) 0.8933(3) 0.144(4) Uani 0.75 1 d P D 1 C300 C 0.7753(3) 0.4336(4) 0.87369(19) 0.085(2) Uani 0.75 1 d P D 1 C301 C 0.7488(5) 0.4583(6) 0.8431(2) 0.121(3) Uani 0.75 1 d P D 1 H30C H 0.7845 0.4644 0.8274 0.182 Uiso 0.75 1 calc PR D 1 H30D H 0.7269 0.5003 0.8469 0.182 Uiso 0.75 1 calc PR D 1 H30E H 0.7172 0.4267 0.8343 0.182 Uiso 0.75 1 calc PR D 1 N400 N 0.3859(5) 0.5860(4) 0.80278(18) 0.072(2) Uani 0.50 1 d P . . C400 C 0.4279(5) 0.5527(4) 0.79381(19) 0.0596(19) Uani 0.50 1 d P . . C401 C 0.4814(5) 0.5116(6) 0.7822(2) 0.078(3) Uani 0.50 1 d P . . H40A H 0.4998 0.5307 0.7622 0.118 Uiso 0.50 1 calc PR . . H40B H 0.4648 0.4676 0.7775 0.118 Uiso 0.50 1 calc PR . . H40C H 0.5155 0.5091 0.7990 0.118 Uiso 0.50 1 calc PR . . O1 O 0.9790(7) 0.4599(8) 1.0455(2) 0.184(8) Uani 0.50 1 d PU . . O2 O 0.7592(12) 0.4905(13) 0.8912(6) 0.141(9) Uani 0.25 1 d P E 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 Fe1A 0.02262(15) 0.02319(15) 0.03115(16) 0.00209(12) 0.00112(12) 0.00143(12) N1A 0.0272(10) 0.0310(10) 0.0484(13) 0.0020(9) 0.0018(9) 0.0001(8) N2A 0.0264(10) 0.0293(10) 0.0343(11) 0.0008(8) -0.0046(8) 0.0007(8) N3A 0.0262(9) 0.0205(8) 0.0314(10) 0.0039(7) -0.0004(7) 0.0015(7) N4A 0.0223(8) 0.0237(9) 0.0343(11) -0.0026(7) -0.0033(7) 0.0008(7) N5A 0.0274(10) 0.0266(10) 0.0353(11) -0.0032(8) -0.0025(8) 0.0039(7) N6A 0.0252(9) 0.0278(9) 0.0405(12) -0.0033(8) 0.0007(8) 0.0028(7) C1A 0.0319(13) 0.0449(16) 0.0615(19) 0.0002(13) 0.0110(12) -0.0059(12) C2A 0.0336(15) 0.062(2) 0.086(3) 0.0012(19) 0.0161(16) -0.0065(14) C3A 0.0317(15) 0.064(2) 0.098(3) -0.008(2) 0.0031(17) -0.0137(15) C4A 0.0306(14) 0.057(2) 0.080(3) -0.0077(17) -0.0082(15) -0.0075(13) C5A 0.0271(12) 0.0366(13) 0.0567(17) -0.0015(12) -0.0068(11) -0.0005(10) C6A 0.0325(12) 0.0354(13) 0.0455(15) -0.0018(11) -0.0093(11) -0.0017(10) C7A 0.0453(16) 0.0582(19) 0.0461(17) -0.0043(14) -0.0156(13) -0.0047(14) C8A 0.0531(19) 0.065(2) 0.0386(16) -0.0060(14) -0.0083(13) -0.0051(16) C9A 0.0431(15) 0.0529(17) 0.0360(14) -0.0011(12) -0.0026(11) 0.0000(13) C10A 0.0324(12) 0.0312(11) 0.0323(12) 0.0011(9) -0.0012(9) 0.0014(9) C11A 0.0257(10) 0.0291(11) 0.0300(11) 0.0027(9) 0.0012(8) 0.0005(8) C12A 0.0264(10) 0.0239(9) 0.0313(11) -0.0023(9) -0.0018(9) 0.0013(8) C13A 0.0264(10) 0.0246(10) 0.0332(11) 0.0015(8) 0.0004(8) 0.0010(8) C14A 0.0254(10) 0.0239(10) 0.0456(14) -0.0015(10) -0.0031(10) 0.0020(8) C15A 0.0546(18) 0.0308(13) 0.0500(17) 0.0036(12) 0.0041(14) -0.0039(12) C16A 0.074(3) 0.0312(15) 0.077(3) 0.0120(15) 0.002(2) -0.0050(15) C17A 0.068(2) 0.0234(12) 0.087(3) -0.0090(16) -0.003(2) 0.0011(13) C18A 0.059(2) 0.0329(15) 0.073(2) -0.0226(15) -0.0033(17) 0.0017(13) C19A 0.0414(14) 0.0298(12) 0.0496(16) -0.0056(11) -0.0027(12) 0.0023(10) C20A 0.0249(11) 0.0263(10) 0.0520(15) 0.0053(10) -0.0029(10) 0.0005(8) C21A 0.0353(14) 0.0359(14) 0.069(2) 0.0032(13) 0.0046(13) -0.0064(11) C22A 0.0371(16) 0.0501(19) 0.108(3) 0.005(2) 0.0049(19) -0.0119(14) C23A 0.0369(17) 0.051(2) 0.114(4) 0.000(2) -0.0118(19) -0.0165(15) C24A 0.0486(19) 0.0478(18) 0.085(3) -0.0096(18) -0.0239(18) -0.0101(15) C25A 0.0402(15) 0.0377(14) 0.0555(18) 0.0005(12) -0.0130(13) -0.0059(12) C26A 0.0361(12) 0.0254(10) 0.0314(12) -0.0024(9) -0.0050(9) 0.0021(9) C27A 0.0338(12) 0.0258(11) 0.0324(12) -0.0041(9) -0.0025(9) 0.0022(9) C28A 0.0478(15) 0.0340(13) 0.0324(13) -0.0018(10) -0.0014(11) 0.0035(11) C29A 0.0528(17) 0.0390(14) 0.0376(14) 0.0096(11) 0.0007(12) 0.0038(12) C30A 0.0419(14) 0.0308(12) 0.0493(16) 0.0085(11) -0.0016(12) 0.0072(11) C31A 0.0286(11) 0.0259(11) 0.0407(13) -0.0006(9) -0.0027(9) 0.0044(9) C32A 0.0294(12) 0.0286(12) 0.0458(14) -0.0009(10) -0.0010(10) 0.0059(9) C33A 0.0521(18) 0.0321(14) 0.0571(18) 0.0032(12) 0.0019(14) 0.0177(12) C34A 0.073(2) 0.0371(15) 0.069(2) -0.0050(15) 0.0076(19) 0.0240(16) C35A 0.0525(18) 0.0408(16) 0.060(2) -0.0116(14) 0.0101(15) 0.0162(14) C36A 0.0387(14) 0.0337(13) 0.0432(14) -0.0055(11) 0.0052(11) 0.0062(11) Fe1B 0.02231(14) 0.02015(14) 0.02933(16) -0.00012(12) 0.00250(12) -0.00091(11) N1B 0.0269(9) 0.0225(9) 0.0396(11) -0.0002(8) 0.0011(8) -0.0012(7) N2B 0.0241(9) 0.0220(9) 0.0321(10) -0.0033(7) -0.0010(7) -0.0023(7) N3B 0.0192(8) 0.0205(8) 0.0345(10) -0.0004(7) -0.0030(7) -0.0010(6) N4B 0.0265(9) 0.0201(8) 0.0279(9) 0.0000(7) 0.0018(7) -0.0005(7) N5B 0.0351(11) 0.0243(9) 0.0347(11) 0.0010(8) -0.0098(9) -0.0024(8) N6B 0.0254(9) 0.0279(10) 0.0536(14) 0.0015(10) -0.0062(10) -0.0025(7) C1B 0.0433(14) 0.0267(12) 0.0400(14) 0.0027(10) 0.0006(11) -0.0036(10) C2B 0.0528(17) 0.0272(12) 0.0481(16) 0.0082(11) -0.0014(13) -0.0004(11) C3B 0.0614(19) 0.0239(12) 0.0636(19) 0.0032(13) 0.0026(16) 0.0039(12) C4B 0.0475(16) 0.0276(12) 0.0518(17) -0.0066(11) 0.0050(13) 0.0041(11) C5B 0.0299(11) 0.0219(10) 0.0437(13) -0.0030(9) 0.0050(10) -0.0031(8) C6B 0.0278(11) 0.0271(11) 0.0369(13) -0.0063(9) 0.0017(9) -0.0005(9) C7B 0.0379(13) 0.0377(13) 0.0418(14) -0.0108(11) 0.0062(11) -0.0020(11) C8B 0.0518(17) 0.0498(16) 0.0326(13) -0.0094(12) 0.0060(12) -0.0049(13) C9B 0.0451(15) 0.0423(14) 0.0295(12) 0.0001(10) 0.0006(11) -0.0057(12) C10B 0.0298(11) 0.0295(11) 0.0293(11) 0.0014(9) -0.0028(9) -0.0028(9) C11B 0.0285(11) 0.0250(10) 0.0352(12) 0.0034(9) -0.0053(9) -0.0012(8) C12B 0.0236(10) 0.0249(10) 0.0357(12) -0.0023(9) 0.0052(9) 0.0005(8) C13B 0.0223(9) 0.0240(10) 0.0301(11) 0.0016(8) 0.0020(8) -0.0005(7) C14B 0.0251(10) 0.0215(10) 0.0684(19) 0.0034(11) 0.0070(12) 0.0005(8) C15B 0.0289(15) 0.097(3) 0.080(3) 0.036(2) -0.0025(16) 0.0061(17) C16B 0.0328(18) 0.113(4) 0.136(5) 0.057(4) -0.014(2) 0.009(2) C17B 0.0269(14) 0.058(2) 0.146(5) 0.016(3) 0.003(2) 0.0125(14) C18B 0.0355(18) 0.075(3) 0.125(4) -0.023(3) 0.029(2) 0.0064(18) C19B 0.0397(17) 0.055(2) 0.077(2) -0.0175(18) 0.0201(16) 0.0036(14) C20B 0.0266(10) 0.0221(10) 0.0482(14) 0.0017(9) 0.0006(10) 0.0004(8) C21B 0.0398(15) 0.0457(16) 0.064(2) 0.0207(15) 0.0040(14) 0.0085(13) C22B 0.053(2) 0.049(2) 0.108(4) 0.030(2) -0.005(2) 0.0144(17) C23B 0.0518(19) 0.0252(14) 0.163(5) -0.001(2) -0.024(3) 0.0124(14) C24B 0.078(3) 0.042(2) 0.116(4) -0.032(2) -0.020(3) 0.0267(19) C25B 0.0539(18) 0.0412(16) 0.0569(19) -0.0153(14) -0.0093(15) 0.0188(14) C26B 0.0351(12) 0.0267(10) 0.0302(11) -0.0006(9) 0.0038(9) -0.0001(9) C27B 0.0481(15) 0.0260(11) 0.0329(12) 0.0009(9) -0.0051(11) -0.0026(10) C28B 0.077(2) 0.0407(15) 0.0362(15) 0.0067(12) -0.0095(15) -0.0112(15) C29B 0.093(3) 0.061(2) 0.0385(17) 0.0169(15) -0.0301(18) -0.015(2) C30B 0.073(2) 0.0481(18) 0.062(2) 0.0181(16) -0.0416(19) -0.0180(17) C31B 0.0461(15) 0.0326(13) 0.0485(16) 0.0090(11) -0.0265(13) -0.0063(11) C32B 0.0301(13) 0.0361(14) 0.072(2) 0.0103(13) -0.0195(13) -0.0058(10) C33B 0.0433(19) 0.075(3) 0.108(4) 0.032(2) -0.039(2) -0.0149(18) C34B 0.0309(17) 0.098(4) 0.144(5) 0.048(3) -0.018(2) -0.014(2) C35B 0.0279(15) 0.068(2) 0.113(4) 0.021(2) 0.0083(18) -0.0045(15) C36B 0.0320(14) 0.0417(15) 0.068(2) 0.0045(14) 0.0051(13) -0.0060(11) P1 0.0727(7) 0.0649(6) 0.0610(6) -0.0111(5) 0.0154(5) -0.0232(5) F10 0.083(2) 0.206(5) 0.129(3) 0.080(3) 0.001(2) -0.011(3) F11 0.126(3) 0.200(5) 0.142(4) -0.120(4) 0.016(3) -0.014(3) F12 0.167(4) 0.076(2) 0.133(3) -0.033(2) -0.004(3) -0.003(2) F13 0.083(2) 0.104(2) 0.140(3) -0.009(2) 0.045(2) -0.0158(18) F14 0.072(2) 0.200(5) 0.206(5) 0.128(4) -0.007(3) -0.053(3) F15 0.108(2) 0.087(2) 0.099(2) 0.0196(18) 0.0229(19) -0.0005(18) P2 0.0751(7) 0.0783(7) 0.0391(5) -0.0076(4) -0.0054(4) -0.0076(5) F20 0.063(2) 0.120(5) 0.0446(19) 0.010(2) -0.0050(16) 0.012(3) F21 0.096(3) 0.049(2) 0.090(3) -0.0139(19) 0.020(2) -0.0041(19) F22 0.109(5) 0.060(3) 0.058(2) -0.024(3) 0.020(3) 0.024(3) F23 0.125(5) 0.099(4) 0.056(3) 0.008(2) -0.038(3) 0.014(3) F24 0.070(3) 0.082(3) 0.085(3) -0.002(2) -0.005(2) 0.016(2) F25 0.137(5) 0.051(3) 0.168(8) 0.023(3) -0.040(5) -0.027(3) F20' 0.132(8) 0.071(5) 0.065(5) 0.026(4) -0.026(5) -0.004(5) F21' 0.065(4) 0.092(6) 0.065(6) -0.047(5) -0.002(4) 0.008(4) F22' 0.139(9) 0.111(7) 0.059(5) -0.035(5) -0.028(5) -0.010(6) F23' 0.079(6) 0.172(13) 0.097(8) 0.016(8) -0.003(6) 0.070(8) F24' 0.065(5) 0.172(13) 0.069(5) -0.031(6) -0.008(4) -0.023(6) F25' 0.069(5) 0.078(7) 0.061(5) -0.011(6) 0.002(3) 0.001(5) P3 0.0519(5) 0.0789(7) 0.0418(4) 0.0024(4) 0.0042(4) 0.0149(5) F30 0.0701(15) 0.0828(17) 0.0681(15) -0.0167(13) -0.0024(12) 0.0038(13) F31 0.0835(19) 0.118(2) 0.0727(17) 0.0314(17) 0.0178(14) 0.0438(17) F32 0.0554(13) 0.101(2) 0.0636(14) -0.0061(13) 0.0100(11) 0.0008(12) F33 0.0666(15) 0.115(2) 0.0702(17) 0.0235(15) 0.0207(13) 0.0245(15) F34 0.0724(15) 0.0761(16) 0.0681(15) 0.0045(12) -0.0003(12) 0.0160(13) F35 0.0780(18) 0.147(3) 0.0628(16) -0.0322(18) -0.0102(14) 0.0206(19) P4 0.0327(5) 0.0545(6) 0.0431(6) 0.000 0.000 0.0051(4) F40 0.0595(15) 0.0675(16) 0.147(3) -0.0077(18) 0.0055(17) -0.0146(13) F41 0.269(18) 0.242(17) 0.076(8) 0.000 0.000 0.103(15) F42 0.30(3) 0.27(3) 0.022(4) 0.000 0.000 -0.20(3) F43 0.043(3) 0.046(3) 0.27(2) 0.010(6) -0.012(6) 0.008(2) F41' 0.064(6) 0.140(10) 0.134(8) 0.089(7) -0.055(5) -0.031(5) F42' 0.105(7) 0.137(7) 0.127(8) -0.018(7) 0.063(6) 0.040(6) P5 0.0367(5) 0.0423(5) 0.0360(5) 0.000 0.000 -0.0098(4) F50 0.0549(14) 0.0539(14) 0.173(3) 0.0177(16) -0.0316(17) -0.0219(11) F51 0.053(3) 0.056(3) 0.127(5) -0.023(3) 0.031(4) 0.001(2) F52 0.113(7) 0.161(8) 0.048(3) 0.030(3) -0.018(3) -0.060(5) F51' 0.141(7) 0.112(6) 0.079(4) -0.046(4) 0.066(5) -0.034(6) F52' 0.050(4) 0.088(5) 0.264(13) 0.062(7) -0.074(6) 0.008(3) O100 0.081(2) 0.084(2) 0.0463(14) 0.0213(14) -0.0065(13) 0.0160(16) C100 0.0510(18) 0.0542(19) 0.0484(17) 0.0032(14) 0.0042(14) 0.0167(15) C101 0.052(2) 0.058(2) 0.111(4) -0.003(2) 0.007(2) -0.0019(17) C102 0.091(3) 0.051(2) 0.080(3) 0.019(2) -0.026(2) -0.005(2) O200 0.093(2) 0.078(2) 0.0718(19) -0.0023(16) 0.0378(18) -0.0333(18) C200 0.082(3) 0.073(3) 0.085(3) 0.010(2) 0.039(3) -0.013(2) C201 0.099(4) 0.068(3) 0.100(4) 0.003(3) 0.018(3) -0.021(3) C202 0.148(7) 0.181(8) 0.078(4) -0.015(5) 0.023(4) -0.083(6) N300 0.084(5) 0.168(9) 0.180(9) 0.085(8) -0.037(5) -0.037(5) C300 0.061(4) 0.108(6) 0.086(5) 0.005(4) 0.000(3) -0.037(4) C301 0.110(7) 0.183(11) 0.070(5) 0.013(6) 0.015(5) 0.001(7) N400 0.095(6) 0.072(5) 0.048(4) -0.003(3) -0.004(4) 0.000(4) C400 0.079(5) 0.053(4) 0.047(4) 0.006(3) -0.006(4) -0.021(4) C401 0.087(8) 0.087(8) 0.061(5) 0.011(5) 0.009(4) 0.012(5) O1 0.169(12) 0.324(18) 0.060(4) 0.025(6) 0.002(5) 0.165(13) O2 0.16(2) 0.144(19) 0.121(17) -0.017(14) -0.066(15) 0.023(15) _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 Fe1A N5A 1.867(2) 6_554 ? Fe1A N2A 1.878(2) . ? Fe1A N1A 1.964(2) . ? Fe1A N4A 1.975(2) 6_554 ? Fe1A N3A 1.979(2) . ? Fe1A N6A 1.990(2) 6_554 ? N1A C1A 1.334(4) . ? N1A C5A 1.365(4) . ? N2A C10A 1.344(3) . ? N2A C6A 1.350(3) . ? N3A C11A 1.295(3) . ? N3A C12A 1.487(3) . ? N4A C27A 1.293(3) . ? N4A C13A 1.486(3) . ? N4A Fe1A 1.975(2) 6_554 ? N5A C31A 1.339(3) . ? N5A C26A 1.360(3) . ? N5A Fe1A 1.867(2) 6_554 ? N6A C36A 1.335(4) . ? N6A C32A 1.356(4) . ? N6A Fe1A 1.990(2) 6_554 ? C1A C2A 1.382(5) . ? C1A H1AA 0.9500 . ? C2A C3A 1.362(6) . ? C2A H2AA 0.9500 . ? C3A C4A 1.382(6) . ? C3A H3AA 0.9500 . ? C4A C5A 1.379(4) . ? C4A H4AA 0.9500 . ? C5A C6A 1.464(4) . ? C6A C7A 1.395(4) . ? C7A C8A 1.377(5) . ? C7A H7AA 0.9500 . ? C8A C9A 1.392(5) . ? C8A H8AA 0.9500 . ? C9A C10A 1.391(4) . ? C9A H9AA 0.9500 . ? C10A C11A 1.449(3) . ? C11A H11A 0.9500 . ? C12A C14A 1.517(3) . ? C12A C13A 1.563(3) . ? C12A H12A 1.0000 . ? C13A C20A 1.520(3) . ? C13A H13A 1.0000 . ? C14A C15A 1.377(4) . ? C14A C19A 1.385(4) . ? C15A C16A 1.398(4) . ? C15A H15A 0.9500 . ? C16A C17A 1.393(6) . ? C16A H16A 0.9500 . ? C17A C18A 1.344(6) . ? C17A H17A 0.9500 . ? C18A C19A 1.391(4) . ? C18A H18A 0.9500 . ? C19A H19A 0.9500 . ? C20A C25A 1.379(4) . ? C20A C21A 1.383(4) . ? C21A C22A 1.402(5) . ? C21A H21A 0.9500 . ? C22A C23A 1.376(7) . ? C22A H22A 0.9500 . ? C23A C24A 1.359(7) . ? C23A H23A 0.9500 . ? C24A C25A 1.401(4) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C26A C28A 1.386(4) . ? C26A C27A 1.446(3) . ? C27A H27A 0.9500 . ? C28A C29A 1.400(4) . ? C28A H28A 0.9500 . ? C29A C30A 1.374(4) . ? C29A H29A 0.9500 . ? C30A C31A 1.384(4) . ? C30A H30A 0.9500 . ? C31A C32A 1.465(4) . ? C32A C33A 1.394(4) . ? C33A C34A 1.363(5) . ? C33A H33A 0.9500 . ? C34A C35A 1.389(6) . ? C34A H34A 0.9500 . ? C35A C36A 1.385(4) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? Fe1B N5B 1.867(2) 6_544 ? Fe1B N2B 1.871(2) . ? Fe1B N3B 1.974(2) . ? Fe1B N1B 1.975(2) . ? Fe1B N4B 1.975(2) 6_544 ? Fe1B N6B 1.986(2) 6_544 ? N1B C1B 1.339(3) . ? N1B C5B 1.359(3) . ? N2B C6B 1.346(3) . ? N2B C10B 1.354(3) . ? N3B C11B 1.288(3) . ? N3B C12B 1.480(3) . ? N4B C26B 1.292(3) . ? N4B C13B 1.482(3) . ? N4B Fe1B 1.975(2) 6_544 ? N5B C31B 1.346(3) . ? N5B C27B 1.348(4) . ? N5B Fe1B 1.867(2) 6_544 ? N6B C36B 1.340(4) . ? N6B C32B 1.355(4) . ? N6B Fe1B 1.986(2) 6_544 ? C1B C2B 1.380(4) . ? C1B H1BA 0.9500 . ? C2B C3B 1.376(5) . ? C2B H2BA 0.9500 . ? C3B C4B 1.387(5) . ? C3B H3BA 0.9500 . ? C4B C5B 1.382(4) . ? C4B H4BA 0.9500 . ? C5B C6B 1.475(4) . ? C6B C7B 1.386(4) . ? C7B C8B 1.380(5) . ? C7B H7BA 0.9500 . ? C8B C9B 1.386(4) . ? C8B H8BA 0.9500 . ? C9B C10B 1.379(4) . ? C9B H9BA 0.9500 . ? C10B C11B 1.449(3) . ? C11B H11B 0.9500 . ? C12B C14B 1.524(3) . ? C12B C13B 1.562(3) . ? C12B H12B 1.0000 . ? C13B C20B 1.520(3) . ? C13B H13B 1.0000 . ? C14B C15B 1.363(5) . ? C14B C19B 1.389(5) . ? C15B C16B 1.384(5) . ? C15B H15B 0.9500 . ? C16B C17B 1.371(8) . ? C16B H16B 0.9500 . ? C17B C18B 1.347(8) . ? C17B H17B 0.9500 . ? C18B C19B 1.394(6) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? C20B C25B 1.374(4) . ? C20B C21B 1.389(4) . ? C21B C22B 1.388(5) . ? C21B H21B 0.9500 . ? C22B C23B 1.361(8) . ? C22B H22B 0.9500 . ? C23B C24B 1.364(8) . ? C23B H23B 0.9500 . ? C24B C25B 1.389(5) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B C27B 1.445(4) . ? C26B H26B 0.9500 . ? C27B C28B 1.389(4) . ? C28B C29B 1.389(6) . ? C28B H28B 0.9500 . ? C29B C30B 1.354(6) . ? C29B H29B 0.9500 . ? C30B C31B 1.396(5) . ? C30B H30B 0.9500 . ? C31B C32B 1.458(5) . ? C32B C33B 1.398(4) . ? C33B C34B 1.364(8) . ? C33B H33B 0.9500 . ? C34B C35B 1.388(8) . ? C34B H34B 0.9500 . ? C35B C36B 1.385(5) . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? P1 F14 1.543(3) . ? P1 F11 1.546(4) . ? P1 F10 1.558(4) . ? P1 F15 1.588(4) . ? P1 F13 1.606(3) . ? P1 F12 1.617(4) . ? P2 F23' 1.349(11) . ? P2 F21' 1.436(7) . ? P2 F25 1.457(5) . ? P2 F22 1.532(6) . ? P2 F24' 1.587(10) . ? P2 F20 1.591(4) . ? P2 F23 1.593(4) . ? P2 F25' 1.671(12) . ? P2 F21 1.673(4) . ? P2 F24 1.689(5) . ? P2 F22' 1.720(8) . ? P2 F20' 1.854(8) . ? P3 F34 1.588(3) . ? P3 F32 1.588(3) . ? P3 F35 1.591(3) . ? P3 F33 1.594(3) . ? P3 F30 1.596(3) . ? P3 F31 1.599(3) . ? P4 F42 1.455(9) . ? P4 F41' 1.494(6) 6_654 ? P4 F41' 1.494(6) . ? P4 F43 1.562(7) . ? P4 F43 1.562(7) 6_654 ? P4 F41 1.588(14) . ? P4 F40 1.591(3) . ? P4 F40 1.591(3) 6_654 ? P4 F42' 1.603(7) 6_654 ? P4 F42' 1.603(7) . ? P5 F52' 1.440(5) . ? P5 F52' 1.440(5) 6_544 ? P5 F51' 1.514(6) . ? P5 F51' 1.514(6) 6_544 ? P5 F50 1.570(2) 6_544 ? P5 F50 1.570(2) . ? P5 F52 1.619(6) 6_544 ? P5 F52 1.619(6) . ? P5 F51 1.675(5) 6_544 ? P5 F51 1.675(5) . ? F52 F52 1.525(19) 6_544 ? F51' F51' 0.944(15) 6_544 ? O100 C100 1.207(5) . ? C100 C101 1.484(6) . ? C100 C102 1.492(5) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? O200 C200 1.197(5) . ? C200 C202 1.498(8) . ? C200 C201 1.504(8) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 H20D 0.9800 . ? C202 H20E 0.9800 . ? C202 H20F 0.9800 . ? N300 C300 1.145(11) . ? C300 C301 1.457(12) . ? C301 H30C 0.9800 . ? C301 H30D 0.9800 . ? C301 H30E 0.9800 . ? N400 C400 1.154(12) . ? C400 C401 1.457(14) . ? C401 H40A 0.9800 . ? C401 H40B 0.9800 . ? C401 H40C 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 N5A Fe1A N2A 175.78(10) 6_554 . ? N5A Fe1A N1A 99.92(10) 6_554 . ? N2A Fe1A N1A 80.59(10) . . ? N5A Fe1A N4A 80.59(9) 6_554 6_554 ? N2A Fe1A N4A 103.61(9) . 6_554 ? N1A Fe1A N4A 90.57(9) . 6_554 ? N5A Fe1A N3A 99.04(9) 6_554 . ? N2A Fe1A N3A 80.54(9) . . ? N1A Fe1A N3A 161.04(10) . . ? N4A Fe1A N3A 92.08(8) 6_554 . ? N5A Fe1A N6A 80.24(10) 6_554 6_554 ? N2A Fe1A N6A 95.58(9) . 6_554 ? N1A Fe1A N6A 90.28(9) . 6_554 ? N4A Fe1A N6A 160.67(9) 6_554 6_554 ? N3A Fe1A N6A 93.37(8) . 6_554 ? C1A N1A C5A 118.6(3) . . ? C1A N1A Fe1A 126.1(2) . . ? C5A N1A Fe1A 115.28(19) . . ? C10A N2A C6A 121.4(2) . . ? C10A N2A Fe1A 118.49(18) . . ? C6A N2A Fe1A 119.6(2) . . ? C11A N3A C12A 120.7(2) . . ? C11A N3A Fe1A 114.05(17) . . ? C12A N3A Fe1A 125.14(16) . . ? C27A N4A C13A 119.8(2) . . ? C27A N4A Fe1A 114.05(17) . 6_554 ? C13A N4A Fe1A 125.74(16) . 6_554 ? C31A N5A C26A 119.7(2) . . ? C31A N5A Fe1A 121.34(19) . 6_554 ? C26A N5A Fe1A 118.97(18) . 6_554 ? C36A N6A C32A 119.2(2) . . ? C36A N6A Fe1A 127.0(2) . 6_554 ? C32A N6A Fe1A 113.84(17) . 6_554 ? N1A C1A C2A 122.0(4) . . ? N1A C1A H1AA 119.0 . . ? C2A C1A H1AA 119.0 . . ? C3A C2A C1A 119.2(4) . . ? C3A C2A H2AA 120.4 . . ? C1A C2A H2AA 120.4 . . ? C2A C3A C4A 120.2(3) . . ? C2A C3A H3AA 119.9 . . ? C4A C3A H3AA 119.9 . . ? C5A C4A C3A 118.2(4) . . ? C5A C4A H4AA 120.9 . . ? C3A C4A H4AA 120.9 . . ? N1A C5A C4A 121.9(3) . . ? N1A C5A C6A 112.8(2) . . ? C4A C5A C6A 125.3(3) . . ? N2A C6A C7A 119.5(3) . . ? N2A C6A C5A 111.4(3) . . ? C7A C6A C5A 129.1(3) . . ? C8A C7A C6A 119.4(3) . . ? C8A C7A H7AA 120.3 . . ? C6A C7A H7AA 120.3 . . ? C7A C8A C9A 120.6(3) . . ? C7A C8A H8AA 119.7 . . ? C9A C8A H8AA 119.7 . . ? C10A C9A C8A 117.7(3) . . ? C10A C9A H9AA 121.2 . . ? C8A C9A H9AA 121.2 . . ? N2A C10A C9A 121.3(3) . . ? N2A C10A C11A 110.7(2) . . ? C9A C10A C11A 127.9(3) . . ? N3A C11A C10A 116.0(2) . . ? N3A C11A H11A 122.0 . . ? C10A C11A H11A 122.0 . . ? N3A C12A C14A 109.68(19) . . ? N3A C12A C13A 111.61(19) . . ? C14A C12A C13A 114.92(19) . . ? N3A C12A H12A 106.7 . . ? C14A C12A H12A 106.7 . . ? C13A C12A H12A 106.7 . . ? N4A C13A C20A 110.2(2) . . ? N4A C13A C12A 110.69(19) . . ? C20A C13A C12A 115.34(19) . . ? N4A C13A H13A 106.7 . . ? C20A C13A H13A 106.7 . . ? C12A C13A H13A 106.7 . . ? C15A C14A C19A 119.6(2) . . ? C15A C14A C12A 121.8(2) . . ? C19A C14A C12A 118.5(3) . . ? C14A C15A C16A 119.8(3) . . ? C14A C15A H15A 120.1 . . ? C16A C15A H15A 120.1 . . ? C17A C16A C15A 119.3(4) . . ? C17A C16A H16A 120.3 . . ? C15A C16A H16A 120.3 . . ? C18A C17A C16A 120.8(3) . . ? C18A C17A H17A 119.6 . . ? C16A C17A H17A 119.6 . . ? C17A C18A C19A 120.2(3) . . ? C17A C18A H18A 119.9 . . ? C19A C18A H18A 119.9 . . ? C14A C19A C18A 120.3(3) . . ? C14A C19A H19A 119.9 . . ? C18A C19A H19A 119.9 . . ? C25A C20A C21A 119.4(3) . . ? C25A C20A C13A 123.0(3) . . ? C21A C20A C13A 117.6(3) . . ? C20A C21A C22A 120.1(4) . . ? C20A C21A H21A 119.9 . . ? C22A C21A H21A 119.9 . . ? C23A C22A C21A 119.9(4) . . ? C23A C22A H22A 120.1 . . ? C21A C22A H22A 120.1 . . ? C24A C23A C22A 120.0(3) . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C25A 120.8(4) . . ? C23A C24A H24A 119.6 . . ? C25A C24A H24A 119.6 . . ? C20A C25A C24A 119.8(3) . . ? C20A C25A H25A 120.1 . . ? C24A C25A H25A 120.1 . . ? N5A C26A C28A 121.6(2) . . ? N5A C26A C27A 109.7(2) . . ? C28A C26A C27A 128.7(2) . . ? N4A C27A C26A 116.6(2) . . ? N4A C27A H27A 121.7 . . ? C26A C27A H27A 121.7 . . ? C26A C28A C29A 118.0(3) . . ? C26A C28A H28A 121.0 . . ? C29A C28A H28A 121.0 . . ? C30A C29A C28A 120.1(3) . . ? C30A C29A H29A 120.0 . . ? C28A C29A H29A 120.0 . . ? C29A C30A C31A 119.1(3) . . ? C29A C30A H30A 120.4 . . ? C31A C30A H30A 120.4 . . ? N5A C31A C30A 121.6(2) . . ? N5A C31A C32A 110.2(2) . . ? C30A C31A C32A 128.2(2) . . ? N6A C32A C33A 121.2(3) . . ? N6A C32A C31A 114.4(2) . . ? C33A C32A C31A 124.4(3) . . ? C34A C33A C32A 119.0(3) . . ? C34A C33A H33A 120.5 . . ? C32A C33A H33A 120.5 . . ? C33A C34A C35A 120.1(3) . . ? C33A C34A H34A 119.9 . . ? C35A C34A H34A 119.9 . . ? C36A C35A C34A 118.3(3) . . ? C36A C35A H35A 120.9 . . ? C34A C35A H35A 120.9 . . ? N6A C36A C35A 122.3(3) . . ? N6A C36A H36A 118.9 . . ? C35A C36A H36A 118.9 . . ? N5B Fe1B N2B 178.31(10) 6_544 . ? N5B Fe1B N3B 101.05(9) 6_544 . ? N2B Fe1B N3B 80.39(9) . . ? N5B Fe1B N1B 98.07(9) 6_544 . ? N2B Fe1B N1B 80.50(9) . . ? N3B Fe1B N1B 160.87(9) . . ? N5B Fe1B N4B 80.72(9) 6_544 6_544 ? N2B Fe1B N4B 98.39(9) . 6_544 ? N3B Fe1B N4B 92.00(8) . 6_544 ? N1B Fe1B N4B 91.50(8) . 6_544 ? N5B Fe1B N6B 80.53(11) 6_544 6_544 ? N2B Fe1B N6B 100.37(10) . 6_544 ? N3B Fe1B N6B 91.06(9) . 6_544 ? N1B Fe1B N6B 91.66(9) . 6_544 ? N4B Fe1B N6B 161.24(10) 6_544 6_544 ? C1B N1B C5B 118.5(2) . . ? C1B N1B Fe1B 126.75(19) . . ? C5B N1B Fe1B 114.66(17) . . ? C6B N2B C10B 120.1(2) . . ? C6B N2B Fe1B 120.81(18) . . ? C10B N2B Fe1B 119.11(17) . . ? C11B N3B C12B 120.3(2) . . ? C11B N3B Fe1B 114.32(16) . . ? C12B N3B Fe1B 125.24(16) . . ? C26B N4B C13B 121.2(2) . . ? C26B N4B Fe1B 114.00(17) . 6_544 ? C13B N4B Fe1B 124.67(15) . 6_544 ? C31B N5B C27B 120.6(3) . . ? C31B N5B Fe1B 120.7(2) . 6_544 ? C27B N5B Fe1B 118.55(18) . 6_544 ? C36B N6B C32B 120.0(3) . . ? C36B N6B Fe1B 126.3(2) . 6_544 ? C32B N6B Fe1B 113.6(2) . 6_544 ? N1B C1B C2B 122.6(3) . . ? N1B C1B H1BA 118.7 . . ? C2B C1B H1BA 118.7 . . ? C3B C2B C1B 118.4(3) . . ? C3B C2B H2BA 120.8 . . ? C1B C2B H2BA 120.8 . . ? C2B C3B C4B 120.3(3) . . ? C2B C3B H3BA 119.8 . . ? C4B C3B H3BA 119.8 . . ? C5B C4B C3B 118.0(3) . . ? C5B C4B H4BA 121.0 . . ? C3B C4B H4BA 121.0 . . ? N1B C5B C4B 122.1(3) . . ? N1B C5B C6B 113.5(2) . . ? C4B C5B C6B 124.4(3) . . ? N2B C6B C7B 120.6(3) . . ? N2B C6B C5B 110.4(2) . . ? C7B C6B C5B 129.0(2) . . ? C8B C7B C6B 119.2(3) . . ? C8B C7B H7BA 120.4 . . ? C6B C7B H7BA 120.4 . . ? C7B C8B C9B 120.2(3) . . ? C7B C8B H8BA 119.9 . . ? C9B C8B H8BA 119.9 . . ? C10B C9B C8B 118.1(3) . . ? C10B C9B H9BA 120.9 . . ? C8B C9B H9BA 120.9 . . ? N2B C10B C9B 121.7(2) . . ? N2B C10B C11B 109.7(2) . . ? C9B C10B C11B 128.5(2) . . ? N3B C11B C10B 116.5(2) . . ? N3B C11B H11B 121.8 . . ? C10B C11B H11B 121.8 . . ? N3B C12B C14B 110.3(2) . . ? N3B C12B C13B 110.45(18) . . ? C14B C12B C13B 116.3(2) . . ? N3B C12B H12B 106.4 . . ? C14B C12B H12B 106.4 . . ? C13B C12B H12B 106.4 . . ? N4B C13B C20B 110.37(19) . . ? N4B C13B C12B 111.22(19) . . ? C20B C13B C12B 116.45(19) . . ? N4B C13B H13B 106.0 . . ? C20B C13B H13B 106.0 . . ? C12B C13B H13B 106.0 . . ? C15B C14B C19B 118.9(3) . . ? C15B C14B C12B 123.7(3) . . ? C19B C14B C12B 117.4(3) . . ? C14B C15B C16B 121.5(4) . . ? C14B C15B H15B 119.3 . . ? C16B C15B H15B 119.3 . . ? C17B C16B C15B 119.5(5) . . ? C17B C16B H16B 120.2 . . ? C15B C16B H16B 120.2 . . ? C18B C17B C16B 119.5(4) . . ? C18B C17B H17B 120.3 . . ? C16B C17B H17B 120.3 . . ? C17B C18B C19B 121.8(4) . . ? C17B C18B H18B 119.1 . . ? C19B C18B H18B 119.1 . . ? C14B C19B C18B 118.7(5) . . ? C14B C19B H19B 120.6 . . ? C18B C19B H19B 120.6 . . ? C25B C20B C21B 119.5(3) . . ? C25B C20B C13B 123.2(3) . . ? C21B C20B C13B 117.2(3) . . ? C22B C21B C20B 120.1(4) . . ? C22B C21B H21B 120.0 . . ? C20B C21B H21B 120.0 . . ? C23B C22B C21B 120.3(4) . . ? C23B C22B H22B 119.8 . . ? C21B C22B H22B 119.8 . . ? C22B C23B C24B 119.5(3) . . ? C22B C23B H23B 120.3 . . ? C24B C23B H23B 120.3 . . ? C23B C24B C25B 121.6(4) . . ? C23B C24B H24B 119.2 . . ? C25B C24B H24B 119.2 . . ? C20B C25B C24B 119.0(4) . . ? C20B C25B H25B 120.5 . . ? C24B C25B H25B 120.5 . . ? N4B C26B C27B 116.1(2) . . ? N4B C26B H26B 122.0 . . ? C27B C26B H26B 122.0 . . ? N5B C27B C28B 121.2(3) . . ? N5B C27B C26B 110.6(2) . . ? C28B C27B C26B 128.1(3) . . ? C29B C28B C27B 117.7(4) . . ? C29B C28B H28B 121.1 . . ? C27B C28B H28B 121.1 . . ? C30B C29B C28B 121.0(3) . . ? C30B C29B H29B 119.5 . . ? C28B C29B H29B 119.5 . . ? C29B C30B C31B 119.3(3) . . ? C29B C30B H30B 120.4 . . ? C31B C30B H30B 120.4 . . ? N5B C31B C30B 120.1(3) . . ? N5B C31B C32B 110.3(2) . . ? C30B C31B C32B 129.5(3) . . ? N6B C32B C33B 120.8(4) . . ? N6B C32B C31B 114.8(2) . . ? C33B C32B C31B 124.4(3) . . ? C34B C33B C32B 118.9(4) . . ? C34B C33B H33B 120.5 . . ? C32B C33B H33B 120.5 . . ? C33B C34B C35B 120.1(3) . . ? C33B C34B H34B 120.0 . . ? C35B C34B H34B 120.0 . . ? C36B C35B C34B 118.9(4) . . ? C36B C35B H35B 120.5 . . ? C34B C35B H35B 120.5 . . ? N6B C36B C35B 121.2(4) . . ? N6B C36B H36B 119.4 . . ? C35B C36B H36B 119.4 . . ? F14 P1 F11 92.9(3) . . ? F14 P1 F10 91.3(2) . . ? F11 P1 F10 93.6(3) . . ? F14 P1 F15 89.1(2) . . ? F11 P1 F15 87.7(3) . . ? F10 P1 F15 178.6(3) . . ? F14 P1 F13 177.8(3) . . ? F11 P1 F13 88.9(2) . . ? F10 P1 F13 89.9(2) . . ? F15 P1 F13 89.7(2) . . ? F14 P1 F12 94.7(3) . . ? F11 P1 F12 170.9(3) . . ? F10 P1 F12 91.2(3) . . ? F15 P1 F12 87.5(2) . . ? F13 P1 F12 83.4(2) . . ? F23' P2 F21' 100.5(9) . . ? F23' P2 F25 117.1(8) . . ? F21' P2 F25 124.4(6) . . ? F23' P2 F22 110.5(6) . . ? F21' P2 F22 103.3(4) . . ? F25 P2 F22 100.0(5) . . ? F23' P2 F24' 99.2(7) . . ? F21' P2 F24' 94.2(5) . . ? F22 P2 F24' 141.7(6) . . ? F23' P2 F20 134.5(8) . . ? F25 P2 F20 94.2(4) . . ? F22 P2 F20 94.0(3) . . ? F24' P2 F20 81.1(4) . . ? F21' P2 F23 133.7(6) . . ? F25 P2 F23 95.5(4) . . ? F22 P2 F23 90.1(4) . . ? F24' P2 F23 102.1(5) . . ? F20 P2 F23 168.7(4) . . ? F23' P2 F25' 96.5(7) . . ? F21' P2 F25' 88.6(5) . . ? F25 P2 F25' 123.0(6) . . ? F24' P2 F25' 163.3(7) . . ? F20 P2 F25' 92.0(4) . . ? F23 P2 F25' 87.6(5) . . ? F23' P2 F21 61.5(7) . . ? F21' P2 F21 52.4(5) . . ? F25 P2 F21 174.6(4) . . ? F22 P2 F21 85.2(3) . . ? F24' P2 F21 131.3(5) . . ? F20 P2 F21 84.1(3) . . ? F23 P2 F21 85.7(3) . . ? F25' P2 F21 62.3(4) . . ? F23' P2 F24 62.9(5) . . ? F21' P2 F24 71.3(4) . . ? F25 P2 F24 90.3(4) . . ? F22 P2 F24 169.6(3) . . ? F24' P2 F24 48.7(6) . . ? F20 P2 F24 86.4(2) . . ? F23 P2 F24 87.7(3) . . ? F25' P2 F24 146.6(4) . . ? F21 P2 F24 84.4(2) . . ? F23' P2 F22' 99.9(8) . . ? F21' P2 F22' 159.2(6) . . ? F25 P2 F22' 46.6(5) . . ? F22 P2 F22' 65.7(5) . . ? F24' P2 F22' 86.2(6) . . ? F20 P2 F22' 125.3(5) . . ? F23 P2 F22' 65.9(4) . . ? F25' P2 F22' 85.4(6) . . ? F21 P2 F22' 138.2(4) . . ? F24 P2 F22' 122.2(5) . . ? F23' P2 F20' 175.3(7) . . ? F21' P2 F20' 83.8(5) . . ? F25 P2 F20' 61.1(4) . . ? F22 P2 F20' 66.4(4) . . ? F24' P2 F20' 82.3(6) . . ? F20 P2 F20' 50.0(4) . . ? F23 P2 F20' 140.8(4) . . ? F25' P2 F20' 81.6(5) . . ? F21 P2 F20' 120.7(4) . . ? F24 P2 F20' 120.7(4) . . ? F22' P2 F20' 75.7(5) . . ? F34 P3 F32 91.03(16) . . ? F34 P3 F35 90.22(18) . . ? F32 P3 F35 90.40(17) . . ? F34 P3 F33 89.97(15) . . ? F32 P3 F33 178.55(19) . . ? F35 P3 F33 90.64(19) . . ? F34 P3 F30 88.68(16) . . ? F32 P3 F30 89.00(15) . . ? F35 P3 F30 178.7(2) . . ? F33 P3 F30 89.98(18) . . ? F34 P3 F31 178.8(2) . . ? F32 P3 F31 88.94(16) . . ? F35 P3 F31 90.9(2) . . ? F33 P3 F31 90.03(16) . . ? F30 P3 F31 90.17(19) . . ? F42 P4 F41' 133.5(6) . 6_654 ? F42 P4 F41' 133.5(6) . . ? F41' P4 F41' 93.0(12) 6_654 . ? F42 P4 F43 98.3(7) . . ? F41' P4 F43 128.1(11) 6_654 . ? F42 P4 F43 98.3(7) . 6_654 ? F41' P4 F43 128.1(11) . 6_654 ? F43 P4 F43 163.4(13) . 6_654 ? F42 P4 F41 180.000(6) . . ? F41' P4 F41 46.5(6) 6_654 . ? F41' P4 F41 46.5(6) . . ? F43 P4 F41 81.7(7) . . ? F43 P4 F41 81.7(7) 6_654 . ? F42 P4 F40 88.79(15) . . ? F41' P4 F40 89.7(4) 6_654 . ? F41' P4 F40 91.9(4) . . ? F43 P4 F40 88.5(3) . . ? F43 P4 F40 91.9(3) 6_654 . ? F41 P4 F40 91.21(15) . . ? F42 P4 F40 88.79(15) . 6_654 ? F41' P4 F40 91.9(4) 6_654 6_654 ? F41' P4 F40 89.7(4) . 6_654 ? F43 P4 F40 91.9(3) . 6_654 ? F43 P4 F40 88.5(3) 6_654 6_654 ? F41 P4 F40 91.21(15) . 6_654 ? F40 P4 F40 177.6(3) . 6_654 ? F41' P4 F42' 90.8(6) 6_654 6_654 ? F41' P4 F42' 176.1(8) . 6_654 ? F43 P4 F42' 140.8(9) . 6_654 ? F43 P4 F42' 55.8(6) 6_654 6_654 ? F41 P4 F42' 137.3(4) . 6_654 ? F40 P4 F42' 87.3(5) . 6_654 ? F40 P4 F42' 90.9(5) 6_654 6_654 ? F41' P4 F42' 176.1(8) 6_654 . ? F41' P4 F42' 90.8(6) . . ? F43 P4 F42' 55.8(6) . . ? F43 P4 F42' 140.8(9) 6_654 . ? F41 P4 F42' 137.3(4) . . ? F40 P4 F42' 90.9(5) . . ? F40 P4 F42' 87.3(5) 6_654 . ? F42' P4 F42' 85.3(8) 6_654 . ? F52' P5 F52' 135.1(13) . 6_544 ? F52' P5 F51' 97.2(7) . . ? F52' P5 F51' 126.9(8) 6_544 . ? F52' P5 F51' 126.9(8) . 6_544 ? F52' P5 F51' 97.2(7) 6_544 6_544 ? F52' P5 F50 86.1(3) . 6_544 ? F52' P5 F50 94.3(3) 6_544 6_544 ? F51' P5 F50 98.5(3) . 6_544 ? F51' P5 F50 80.6(3) 6_544 6_544 ? F52' P5 F50 94.3(3) . . ? F52' P5 F50 86.1(3) 6_544 . ? F51' P5 F50 80.6(3) . . ? F51' P5 F50 98.5(3) 6_544 . ? F50 P5 F50 179.0(3) 6_544 . ? F52' P5 F52 94.1(8) . 6_544 ? F51' P5 F52 168.7(5) . 6_544 ? F51' P5 F52 134.1(5) 6_544 6_544 ? F50 P5 F52 83.1(3) 6_544 6_544 ? F50 P5 F52 97.8(3) . 6_544 ? F52' P5 F52 94.1(8) 6_544 . ? F51' P5 F52 134.1(5) . . ? F51' P5 F52 168.7(5) 6_544 . ? F50 P5 F52 97.8(3) 6_544 . ? F50 P5 F52 83.1(3) . . ? F52 P5 F52 56.2(7) 6_544 . ? F52' P5 F51 177.1(8) . 6_544 ? F51' P5 F51 85.5(5) . 6_544 ? F51' P5 F51 55.2(5) 6_544 6_544 ? F50 P5 F51 92.5(2) 6_544 6_544 ? F50 P5 F51 87.2(2) . 6_544 ? F52 P5 F51 83.2(4) 6_544 6_544 ? F52 P5 F51 136.1(5) . 6_544 ? F52' P5 F51 177.1(8) 6_544 . ? F51' P5 F51 55.2(5) . . ? F51' P5 F51 85.5(5) 6_544 . ? F50 P5 F51 87.2(2) 6_544 . ? F50 P5 F51 92.5(2) . . ? F52 P5 F51 136.1(5) 6_544 . ? F52 P5 F51 83.2(4) . . ? F51 P5 F51 140.1(6) 6_544 . ? F52 F52 P5 61.9(3) 6_544 . ? F51' F51' P5 71.8(3) 6_544 . ? O100 C100 C101 124.2(4) . . ? O100 C100 C102 119.5(4) . . ? C101 C100 C102 116.3(4) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C100 C102 H10D 109.5 . . ? C100 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C100 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? O200 C200 C202 121.4(6) . . ? O200 C200 C201 122.8(5) . . ? C202 C200 C201 115.7(5) . . ? C200 C201 H20A 109.5 . . ? C200 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C200 C202 H20D 109.5 . . ? C200 C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? C200 C202 H20F 109.5 . . ? H20D C202 H20F 109.5 . . ? H20E C202 H20F 109.5 . . ? N300 C300 C301 163.2(12) . . ? N400 C400 C401 178.9(10) . . ? C400 C401 H40A 109.5 . . ? C400 C401 H40B 109.5 . . ? H40A C401 H40B 109.5 . . ? C400 C401 H40C 109.5 . . ? H40A C401 H40C 109.5 . . ? H40B C401 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.486 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.058