# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Fe(mes)2(IPr)] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C45 H58 Fe N2' _chemical_formula_sum 'C45 H58 Fe N2' _chemical_formula_weight 682.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.31630(10) _cell_length_b 17.94940(10) _cell_length_c 18.02220(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.3650(10) _cell_angle_gamma 90.00 _cell_volume 3941.79(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34409 _cell_measurement_theta_min 3.4910 _cell_measurement_theta_max 76.7652 _exptl_crystal_description needle _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 3.291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6558 _exptl_absorpt_correction_T_max 0.9371 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; . ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4102 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 82827 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 76.96 _reflns_number_total 8283 _reflns_number_gt 7426 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^ > 2\s(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^)+(0.0539P)^2^+1.1858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8283 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 C1 C 0.73377(11) 0.24644(7) 0.11474(7) 0.0221(3) Uani 1 1 d . . . C2 C 0.77908(12) 0.23219(8) 0.24105(8) 0.0275(3) Uani 1 1 d . . . H2 H 0.8198 0.2195 0.2882 0.033 Uiso 1 1 calc R . . C3 C 0.67893(12) 0.26379(8) 0.22884(8) 0.0274(3) Uani 1 1 d . . . H3 H 0.6352 0.2780 0.2658 0.033 Uiso 1 1 calc R . . C4 C 0.91341(11) 0.18686(8) 0.16016(7) 0.0258(3) Uani 1 1 d . . . C5 C 0.91784(12) 0.10909(8) 0.16137(8) 0.0312(3) Uani 1 1 d . . . C6 C 1.01861(14) 0.07618(10) 0.15461(10) 0.0410(4) Uani 1 1 d . . . H6 H 1.0256 0.0235 0.1566 0.049 Uiso 1 1 calc R . . C7 C 1.10830(13) 0.11944(11) 0.14505(10) 0.0451(4) Uani 1 1 d . . . H7 H 1.1764 0.0961 0.1408 0.054 Uiso 1 1 calc R . . C8 C 1.10032(12) 0.19617(10) 0.14164(9) 0.0394(4) Uani 1 1 d . . . H8 H 1.1626 0.2247 0.1339 0.047 Uiso 1 1 calc R . . C9 C 1.00230(12) 0.23249(9) 0.14943(8) 0.0299(3) Uani 1 1 d . . . C10 C 0.81741(13) 0.06184(8) 0.16895(9) 0.0348(3) Uani 1 1 d . . . H10 H 0.7509 0.0926 0.1515 0.042 Uiso 1 1 calc R . . C11 C 0.81086(15) -0.00844(9) 0.12014(10) 0.0434(4) Uani 1 1 d . . . H11A H 0.8213 0.0051 0.0690 0.065 Uiso 1 1 calc R . . H11B H 0.7388 -0.0318 0.1193 0.065 Uiso 1 1 calc R . . H11C H 0.8683 -0.0435 0.1410 0.065 Uiso 1 1 calc R . . C12 C 0.81393(18) 0.04090(10) 0.25103(10) 0.0491(4) Uani 1 1 d . . . H12A H 0.8779 0.0102 0.2696 0.074 Uiso 1 1 calc R . . H12B H 0.7467 0.0128 0.2547 0.074 Uiso 1 1 calc R . . H12C H 0.8150 0.0863 0.2813 0.074 Uiso 1 1 calc R . . C13 C 0.99185(11) 0.31691(8) 0.14560(8) 0.0319(3) Uani 1 1 d . . . H13 H 0.9191 0.3285 0.1154 0.038 Uiso 1 1 calc R . . C14 C 1.07983(13) 0.35398(10) 0.10628(9) 0.0415(4) Uani 1 1 d . . . H14A H 1.1516 0.3487 0.1374 0.062 Uiso 1 1 calc R . . H14B H 1.0625 0.4070 0.0986 0.062 Uiso 1 1 calc R . . H14C H 1.0817 0.3300 0.0576 0.062 Uiso 1 1 calc R . . C15 C 0.99225(15) 0.35185(10) 0.22325(10) 0.0428(4) Uani 1 1 d . . . H15A H 0.9336 0.3296 0.2473 0.064 Uiso 1 1 calc R . . H15B H 0.9802 0.4057 0.2179 0.064 Uiso 1 1 calc R . . H15C H 1.0632 0.3426 0.2541 0.064 Uiso 1 1 calc R . . C16 C 0.55428(11) 0.31019(7) 0.11759(7) 0.0249(3) Uani 1 1 d . . . C17 C 0.55584(12) 0.38800(8) 0.12051(8) 0.0301(3) Uani 1 1 d . . . C18 C 0.45925(13) 0.42523(9) 0.09189(9) 0.0369(3) Uani 1 1 d . . . H18 H 0.4571 0.4781 0.0935 0.044 Uiso 1 1 calc R . . C19 C 0.36685(12) 0.38640(9) 0.06129(9) 0.0372(3) Uani 1 1 d . . . H19 H 0.3016 0.4127 0.0427 0.045 Uiso 1 1 calc R . . C20 C 0.36843(11) 0.30949(9) 0.05753(8) 0.0323(3) Uani 1 1 d . . . H20 H 0.3046 0.2837 0.0352 0.039 Uiso 1 1 calc R . . C21 C 0.46206(11) 0.26910(8) 0.08585(8) 0.0260(3) Uani 1 1 d . . . C22 C 0.65897(13) 0.43160(8) 0.15062(10) 0.0378(3) Uani 1 1 d . . . H22 H 0.7221 0.3960 0.1582 0.045 Uiso 1 1 calc R . . C23 C 0.68312(16) 0.49113(10) 0.09369(12) 0.0502(4) Uani 1 1 d . . . H23A H 0.6298 0.5317 0.0928 0.075 Uiso 1 1 calc R . . H23B H 0.6776 0.4687 0.0437 0.075 Uiso 1 1 calc R . . H23C H 0.7574 0.5108 0.1084 0.075 Uiso 1 1 calc R . . C24 C 0.6503(2) 0.46850(13) 0.22535(12) 0.0660(6) Uani 1 1 d . . . H24A H 0.5880 0.5030 0.2194 0.099 Uiso 1 1 calc R . . H24B H 0.7180 0.4960 0.2425 0.099 Uiso 1 1 calc R . . H24C H 0.6392 0.4303 0.2624 0.099 Uiso 1 1 calc R . . C25 C 0.46363(11) 0.18433(8) 0.08213(8) 0.0287(3) Uani 1 1 d . . . H25 H 0.5367 0.1691 0.0692 0.034 Uiso 1 1 calc R . . C26 C 0.37564(13) 0.15305(9) 0.02141(9) 0.0373(3) Uani 1 1 d . . . H26A H 0.3030 0.1607 0.0363 0.056 Uiso 1 1 calc R . . H26B H 0.3882 0.0997 0.0152 0.056 Uiso 1 1 calc R . . H26C H 0.3794 0.1788 -0.0261 0.056 Uiso 1 1 calc R . . C27 C 0.45178(15) 0.14893(9) 0.15788(9) 0.0395(4) Uani 1 1 d . . . H27A H 0.5114 0.1663 0.1959 0.059 Uiso 1 1 calc R . . H27B H 0.4553 0.0946 0.1537 0.059 Uiso 1 1 calc R . . H27C H 0.3811 0.1633 0.1725 0.059 Uiso 1 1 calc R . . C28 C 0.88479(11) 0.27563(9) -0.04442(8) 0.0305(3) Uani 1 1 d . . . C29 C 0.95572(13) 0.21861(9) -0.06277(8) 0.0349(3) Uani 1 1 d . . . C30 C 1.05029(14) 0.23445(10) -0.09409(9) 0.0405(4) Uani 1 1 d . . . H30 H 1.0974 0.1947 -0.1035 0.049 Uiso 1 1 calc R . . C31 C 1.07730(13) 0.30627(10) -0.11180(9) 0.0409(4) Uani 1 1 d . . . C32 C 1.00818(13) 0.36322(10) -0.09485(9) 0.0385(3) Uani 1 1 d . . . H32 H 1.0243 0.4132 -0.1068 0.046 Uiso 1 1 calc R . . C33 C 0.91537(12) 0.34853(9) -0.06061(8) 0.0336(3) Uani 1 1 d . . . C34 C 0.92930(16) 0.13797(10) -0.04906(11) 0.0487(4) Uani 1 1 d . . . H34A H 0.8612 0.1351 -0.0270 0.073 Uiso 0.50 1 calc PR . . H34B H 0.9894 0.1157 -0.0145 0.073 Uiso 0.50 1 calc PR . . H34C H 0.9202 0.1108 -0.0967 0.073 Uiso 0.50 1 calc PR . . H34D H 0.9860 0.1060 -0.0652 0.073 Uiso 0.50 1 calc PR . . H34E H 0.8578 0.1254 -0.0777 0.073 Uiso 0.50 1 calc PR . . H34F H 0.9270 0.1303 0.0045 0.073 Uiso 0.50 1 calc PR . . C35 C 1.17901(16) 0.32153(13) -0.14702(11) 0.0556(5) Uani 1 1 d . . . H35A H 1.1852 0.3752 -0.1557 0.083 Uiso 0.50 1 calc PR . . H35B H 1.1741 0.2950 -0.1949 0.083 Uiso 0.50 1 calc PR . . H35C H 1.2438 0.3043 -0.1133 0.083 Uiso 0.50 1 calc PR . . H35D H 1.2169 0.2745 -0.1536 0.083 Uiso 0.50 1 calc PR . . H35E H 1.2280 0.3546 -0.1144 0.083 Uiso 0.50 1 calc PR . . H35F H 1.1582 0.3454 -0.1960 0.083 Uiso 0.50 1 calc PR . . C36 C 0.85128(14) 0.41452(10) -0.03834(10) 0.0433(4) Uani 1 1 d . . . H36A H 0.7888 0.3969 -0.0152 0.065 Uiso 0.50 1 calc PR . . H36B H 0.8245 0.4441 -0.0830 0.065 Uiso 0.50 1 calc PR . . H36C H 0.8989 0.4454 -0.0024 0.065 Uiso 0.50 1 calc PR . . H36D H 0.8860 0.4607 -0.0519 0.065 Uiso 0.50 1 calc PR . . H36E H 0.8503 0.4135 0.0159 0.065 Uiso 0.50 1 calc PR . . H36F H 0.7759 0.4122 -0.0646 0.065 Uiso 0.50 1 calc PR . . C37 C 0.60619(11) 0.21353(8) -0.07342(7) 0.0256(3) Uani 1 1 d . . . C38 C 0.53839(11) 0.26800(8) -0.11265(7) 0.0266(3) Uani 1 1 d . . . C39 C 0.44930(12) 0.24877(8) -0.16618(8) 0.0304(3) Uani 1 1 d . . . H39 H 0.4046 0.2870 -0.1910 0.037 Uiso 1 1 calc R . . C40 C 0.42476(11) 0.17510(9) -0.18382(8) 0.0327(3) Uani 1 1 d . . . C41 C 0.48969(12) 0.12051(9) -0.14516(8) 0.0331(3) Uani 1 1 d . . . H41 H 0.4739 0.0696 -0.1563 0.040 Uiso 1 1 calc R . . C42 C 0.57784(12) 0.13878(8) -0.09020(8) 0.0297(3) Uani 1 1 d . . . C43 C 0.56174(14) 0.34972(9) -0.09856(10) 0.0393(3) Uani 1 1 d . . . H43A H 0.6260 0.3553 -0.0600 0.059 Uiso 0.50 1 calc PR . . H43B H 0.4981 0.3734 -0.0815 0.059 Uiso 0.50 1 calc PR . . H43C H 0.5762 0.3735 -0.1451 0.059 Uiso 0.50 1 calc PR . . H43D H 0.5075 0.3795 -0.1310 0.059 Uiso 0.50 1 calc PR . . H43E H 0.6355 0.3614 -0.1096 0.059 Uiso 0.50 1 calc PR . . H43F H 0.5573 0.3613 -0.0459 0.059 Uiso 0.50 1 calc PR . . C44 C 0.32909(14) 0.15563(11) -0.24282(9) 0.0456(4) Uani 1 1 d . . . H44A H 0.3237 0.1014 -0.2481 0.068 Uiso 0.50 1 calc PR . . H44B H 0.3402 0.1777 -0.2909 0.068 Uiso 0.50 1 calc PR . . H44C H 0.2612 0.1751 -0.2278 0.068 Uiso 0.50 1 calc PR . . H44D H 0.2930 0.2015 -0.2631 0.068 Uiso 0.50 1 calc PR . . H44E H 0.2765 0.1251 -0.2203 0.068 Uiso 0.50 1 calc PR . . H44F H 0.3556 0.1277 -0.2833 0.068 Uiso 0.50 1 calc PR . . C45 C 0.64006(14) 0.07579(9) -0.04741(11) 0.0441(4) Uani 1 1 d . . . H45A H 0.6993 0.0963 -0.0110 0.066 Uiso 0.50 1 calc PR . . H45B H 0.6713 0.0432 -0.0825 0.066 Uiso 0.50 1 calc PR . . H45C H 0.5899 0.0470 -0.0210 0.066 Uiso 0.50 1 calc PR . . H45D H 0.6077 0.0281 -0.0654 0.066 Uiso 0.50 1 calc PR . . H45E H 0.6357 0.0811 0.0062 0.066 Uiso 0.50 1 calc PR . . H45F H 0.7171 0.0774 -0.0553 0.066 Uiso 0.50 1 calc PR . . N1 N 0.81113(9) 0.22185(6) 0.17113(6) 0.0233(2) Uani 1 1 d . . . N2 N 0.65210(9) 0.27159(6) 0.15167(6) 0.0233(2) Uani 1 1 d . . . Fe1 Fe 0.743215(16) 0.246246(11) -0.001477(11) 0.02392(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0212(6) 0.0212(6) 0.0229(6) 0.0001(4) -0.0001(5) -0.0011(4) C2 0.0307(7) 0.0299(7) 0.0210(6) 0.0016(5) 0.0008(5) -0.0017(5) C3 0.0306(7) 0.0291(7) 0.0225(6) -0.0004(5) 0.0040(5) -0.0009(5) C4 0.0226(6) 0.0324(7) 0.0209(6) 0.0013(5) -0.0025(5) 0.0037(5) C5 0.0303(7) 0.0332(7) 0.0283(7) 0.0033(6) -0.0018(5) 0.0054(6) C6 0.0380(8) 0.0385(8) 0.0452(9) 0.0023(7) 0.0012(7) 0.0129(7) C7 0.0285(7) 0.0559(10) 0.0500(10) 0.0016(8) 0.0026(7) 0.0132(7) C8 0.0240(7) 0.0540(10) 0.0388(8) 0.0027(7) 0.0000(6) 0.0007(6) C9 0.0246(7) 0.0390(8) 0.0238(7) 0.0021(6) -0.0041(5) 0.0000(6) C10 0.0374(8) 0.0265(7) 0.0392(8) 0.0035(6) 0.0012(6) 0.0017(6) C11 0.0545(10) 0.0309(8) 0.0424(9) 0.0002(7) -0.0007(7) 0.0007(7) C12 0.0681(12) 0.0365(9) 0.0447(10) 0.0033(7) 0.0144(8) -0.0070(8) C13 0.0257(7) 0.0368(8) 0.0306(7) 0.0028(6) -0.0043(5) -0.0072(6) C14 0.0317(8) 0.0534(10) 0.0364(8) 0.0079(7) -0.0049(6) -0.0145(7) C15 0.0445(9) 0.0427(9) 0.0404(9) -0.0049(7) 0.0032(7) -0.0130(7) C16 0.0235(6) 0.0269(7) 0.0245(6) 0.0025(5) 0.0037(5) 0.0030(5) C17 0.0314(7) 0.0266(7) 0.0326(7) 0.0015(5) 0.0057(6) 0.0014(5) C18 0.0384(8) 0.0281(7) 0.0451(9) 0.0074(6) 0.0091(7) 0.0083(6) C19 0.0306(7) 0.0413(8) 0.0400(8) 0.0115(7) 0.0062(6) 0.0108(6) C20 0.0244(7) 0.0400(8) 0.0321(7) 0.0040(6) 0.0024(5) 0.0013(6) C21 0.0251(6) 0.0298(7) 0.0235(6) 0.0015(5) 0.0044(5) 0.0000(5) C22 0.0374(8) 0.0254(7) 0.0502(9) -0.0016(6) 0.0046(7) -0.0034(6) C23 0.0523(10) 0.0395(9) 0.0629(12) 0.0014(8) 0.0222(9) -0.0058(8) C24 0.0808(15) 0.0711(14) 0.0484(11) -0.0176(10) 0.0167(10) -0.0373(12) C25 0.0285(7) 0.0284(7) 0.0290(7) -0.0020(5) 0.0035(5) -0.0039(5) C26 0.0358(8) 0.0416(8) 0.0340(8) -0.0062(6) 0.0039(6) -0.0104(6) C27 0.0529(10) 0.0319(8) 0.0326(8) 0.0021(6) 0.0027(7) -0.0088(7) C28 0.0269(7) 0.0418(8) 0.0216(6) -0.0030(6) -0.0004(5) -0.0007(6) C29 0.0338(7) 0.0443(9) 0.0263(7) -0.0068(6) 0.0030(6) 0.0004(6) C30 0.0348(8) 0.0517(10) 0.0349(8) -0.0124(7) 0.0051(6) 0.0033(7) C31 0.0335(8) 0.0585(10) 0.0307(8) -0.0096(7) 0.0045(6) -0.0085(7) C32 0.0388(8) 0.0446(9) 0.0305(7) -0.0004(6) 0.0000(6) -0.0085(7) C33 0.0294(7) 0.0442(8) 0.0255(7) -0.0026(6) -0.0017(5) -0.0013(6) C34 0.0508(10) 0.0451(10) 0.0523(10) -0.0054(8) 0.0141(8) 0.0028(8) C35 0.0429(10) 0.0773(14) 0.0494(10) -0.0120(10) 0.0159(8) -0.0146(9) C36 0.0399(9) 0.0411(9) 0.0484(9) -0.0019(7) 0.0049(7) 0.0011(7) C37 0.0235(6) 0.0320(7) 0.0206(6) -0.0011(5) 0.0011(5) -0.0004(5) C38 0.0238(6) 0.0336(7) 0.0222(6) 0.0010(5) 0.0032(5) 0.0000(5) C39 0.0230(7) 0.0426(8) 0.0253(7) 0.0063(5) 0.0020(5) 0.0003(5) C40 0.0253(7) 0.0502(9) 0.0219(6) -0.0007(6) 0.0015(5) -0.0078(6) C41 0.0326(7) 0.0346(7) 0.0317(7) -0.0062(6) 0.0038(6) -0.0072(6) C42 0.0282(7) 0.0323(7) 0.0279(7) -0.0015(5) 0.0017(5) -0.0007(5) C43 0.0367(8) 0.0321(8) 0.0468(9) 0.0013(7) -0.0021(7) 0.0039(6) C44 0.0361(8) 0.0642(11) 0.0331(8) -0.0011(7) -0.0064(6) -0.0142(8) C45 0.0424(9) 0.0319(8) 0.0547(10) 0.0044(7) -0.0039(7) 0.0011(7) N1 0.0223(5) 0.0251(5) 0.0215(5) 0.0004(4) -0.0008(4) 0.0002(4) N2 0.0227(5) 0.0236(5) 0.0231(5) -0.0002(4) 0.0013(4) 0.0006(4) Fe1 0.02274(11) 0.02771(12) 0.01995(11) -0.00077(8) -0.00145(8) -0.00006(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N2 1.3614(17) . ? C1 N1 1.3615(16) . ? C1 Fe1 2.1145(14) . ? C2 C3 1.346(2) . ? C2 N1 1.3867(17) . ? C2 H2 0.9500 . ? C3 N2 1.3889(17) . ? C3 H3 0.9500 . ? C4 C5 1.397(2) . ? C4 C9 1.403(2) . ? C4 N1 1.4467(17) . ? C5 C6 1.396(2) . ? C5 C10 1.522(2) . ? C6 C7 1.381(3) . ? C6 H6 0.9500 . ? C7 C8 1.382(3) . ? C7 H7 0.9500 . ? C8 C9 1.397(2) . ? C8 H8 0.9500 . ? C9 C13 1.521(2) . ? C10 C12 1.533(2) . ? C10 C11 1.533(2) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.530(2) . ? C13 C15 1.533(2) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.3978(19) . ? C16 C21 1.4043(19) . ? C16 N2 1.4469(16) . ? C17 C18 1.396(2) . ? C17 C22 1.523(2) . ? C18 C19 1.379(2) . ? C18 H18 0.9500 . ? C19 C20 1.382(2) . ? C19 H19 0.9500 . ? C20 C21 1.3946(19) . ? C20 H20 0.9500 . ? C21 C25 1.5232(19) . ? C22 C24 1.519(3) . ? C22 C23 1.540(2) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.5303(19) . ? C25 C27 1.532(2) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.404(2) . ? C28 C29 1.416(2) . ? C28 Fe1 2.0760(15) . ? C29 C30 1.396(2) . ? C29 C34 1.512(2) . ? C30 C31 1.380(3) . ? C30 H30 0.9500 . ? C31 C32 1.392(2) . ? C31 C35 1.510(2) . ? C32 C33 1.401(2) . ? C32 H32 0.9500 . ? C33 C36 1.510(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34 H34D 0.9800 . ? C34 H34E 0.9800 . ? C34 H34F 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C35 H35D 0.9800 . ? C35 H35E 0.9800 . ? C35 H35F 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C36 H36D 0.9800 . ? C36 H36E 0.9800 . ? C36 H36F 0.9800 . ? C37 C38 1.4076(19) . ? C37 C42 1.408(2) . ? C37 Fe1 2.0585(13) . ? C38 C39 1.395(2) . ? C38 C43 1.509(2) . ? C39 C40 1.383(2) . ? C39 H39 0.9500 . ? C40 C41 1.387(2) . ? C40 C44 1.5089(19) . ? C41 C42 1.398(2) . ? C41 H41 0.9500 . ? C42 C45 1.513(2) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C43 H43D 0.9800 . ? C43 H43E 0.9800 . ? C43 H43F 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C44 H44D 0.9800 . ? C44 H44E 0.9800 . ? C44 H44F 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C45 H45D 0.9800 . ? C45 H45E 0.9800 . ? C45 H45F 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 N2 C1 N1 103.25(11) . . ? N2 C1 Fe1 129.48(9) . . ? N1 C1 Fe1 127.26(10) . . ? C3 C2 N1 106.43(12) . . ? C3 C2 H2 126.8 . . ? N1 C2 H2 126.8 . . ? C2 C3 N2 106.56(12) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? C5 C4 C9 123.78(13) . . ? C5 C4 N1 117.68(12) . . ? C9 C4 N1 118.54(12) . . ? C6 C5 C4 117.04(14) . . ? C6 C5 C10 121.10(14) . . ? C4 C5 C10 121.85(13) . . ? C7 C6 C5 120.70(16) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 120.85(15) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 C9 121.19(15) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 116.39(14) . . ? C8 C9 C13 121.93(14) . . ? C4 C9 C13 121.68(13) . . ? C5 C10 C12 111.12(13) . . ? C5 C10 C11 112.49(13) . . ? C12 C10 C11 110.20(13) . . ? C5 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? C11 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 113.14(14) . . ? C9 C13 C15 112.15(13) . . ? C14 C13 C15 109.66(13) . . ? C9 C13 H13 107.2 . . ? C14 C13 H13 107.2 . . ? C15 C13 H13 107.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 123.10(13) . . ? C17 C16 N2 117.16(12) . . ? C21 C16 N2 119.71(12) . . ? C18 C17 C16 117.26(13) . . ? C18 C17 C22 120.49(13) . . ? C16 C17 C22 122.21(13) . . ? C19 C18 C17 121.00(14) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.51(14) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 121.20(14) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 116.92(13) . . ? C20 C21 C25 121.22(13) . . ? C16 C21 C25 121.86(12) . . ? C24 C22 C17 112.17(14) . . ? C24 C22 C23 109.49(15) . . ? C17 C22 C23 110.55(14) . . ? C24 C22 H22 108.2 . . ? C17 C22 H22 108.2 . . ? C23 C22 H22 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 112.69(12) . . ? C21 C25 C27 111.81(12) . . ? C26 C25 C27 109.61(12) . . ? C21 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C27 C25 H25 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 115.58(14) . . ? C33 C28 Fe1 125.42(11) . . ? C29 C28 Fe1 118.93(12) . . ? C30 C29 C28 121.81(16) . . ? C30 C29 C34 118.24(15) . . ? C28 C29 C34 119.95(14) . . ? C31 C30 C29 121.81(16) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 117.35(15) . . ? C30 C31 C35 120.62(17) . . ? C32 C31 C35 122.02(17) . . ? C31 C32 C33 121.50(16) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C32 C33 C28 121.86(15) . . ? C32 C33 C36 117.47(15) . . ? C28 C33 C36 120.62(14) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C29 C34 H34D 109.5 . . ? H34A C34 H34D 141.1 . . ? H34B C34 H34D 56.3 . . ? H34C C34 H34D 56.3 . . ? C29 C34 H34E 109.5 . . ? H34A C34 H34E 56.3 . . ? H34B C34 H34E 141.1 . . ? H34C C34 H34E 56.3 . . ? H34D C34 H34E 109.5 . . ? C29 C34 H34F 109.5 . . ? H34A C34 H34F 56.3 . . ? H34B C34 H34F 56.3 . . ? H34C C34 H34F 141.1 . . ? H34D C34 H34F 109.5 . . ? H34E C34 H34F 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C31 C35 H35D 109.5 . . ? H35A C35 H35D 141.1 . . ? H35B C35 H35D 56.3 . . ? H35C C35 H35D 56.3 . . ? C31 C35 H35E 109.5 . . ? H35A C35 H35E 56.3 . . ? H35B C35 H35E 141.1 . . ? H35C C35 H35E 56.3 . . ? H35D C35 H35E 109.5 . . ? C31 C35 H35F 109.5 . . ? H35A C35 H35F 56.3 . . ? H35B C35 H35F 56.3 . . ? H35C C35 H35F 141.1 . . ? H35D C35 H35F 109.5 . . ? H35E C35 H35F 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C36 H36D 109.5 . . ? H36A C36 H36D 141.1 . . ? H36B C36 H36D 56.3 . . ? H36C C36 H36D 56.3 . . ? C33 C36 H36E 109.5 . . ? H36A C36 H36E 56.3 . . ? H36B C36 H36E 141.1 . . ? H36C C36 H36E 56.3 . . ? H36D C36 H36E 109.5 . . ? C33 C36 H36F 109.5 . . ? H36A C36 H36F 56.3 . . ? H36B C36 H36F 56.3 . . ? H36C C36 H36F 141.1 . . ? H36D C36 H36F 109.5 . . ? H36E C36 H36F 109.5 . . ? C38 C37 C42 116.33(12) . . ? C38 C37 Fe1 119.36(10) . . ? C42 C37 Fe1 124.20(10) . . ? C39 C38 C37 121.67(13) . . ? C39 C38 C43 117.92(13) . . ? C37 C38 C43 120.40(13) . . ? C40 C39 C38 121.27(13) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 117.99(13) . . ? C39 C40 C44 120.37(15) . . ? C41 C40 C44 121.63(15) . . ? C40 C41 C42 121.45(14) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C41 C42 C37 121.23(13) . . ? C41 C42 C45 118.00(14) . . ? C37 C42 C45 120.75(13) . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C38 C43 H43D 109.5 . . ? H43A C43 H43D 141.1 . . ? H43B C43 H43D 56.3 . . ? H43C C43 H43D 56.3 . . ? C38 C43 H43E 109.5 . . ? H43A C43 H43E 56.3 . . ? H43B C43 H43E 141.1 . . ? H43C C43 H43E 56.3 . . ? H43D C43 H43E 109.5 . . ? C38 C43 H43F 109.5 . . ? H43A C43 H43F 56.3 . . ? H43B C43 H43F 56.3 . . ? H43C C43 H43F 141.1 . . ? H43D C43 H43F 109.5 . . ? H43E C43 H43F 109.5 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C40 C44 H44D 109.5 . . ? H44A C44 H44D 141.1 . . ? H44B C44 H44D 56.3 . . ? H44C C44 H44D 56.3 . . ? C40 C44 H44E 109.5 . . ? H44A C44 H44E 56.3 . . ? H44B C44 H44E 141.1 . . ? H44C C44 H44E 56.3 . . ? H44D C44 H44E 109.5 . . ? C40 C44 H44F 109.5 . . ? H44A C44 H44F 56.3 . . ? H44B C44 H44F 56.3 . . ? H44C C44 H44F 141.1 . . ? H44D C44 H44F 109.5 . . ? H44E C44 H44F 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C42 C45 H45D 109.5 . . ? H45A C45 H45D 141.1 . . ? H45B C45 H45D 56.3 . . ? H45C C45 H45D 56.3 . . ? C42 C45 H45E 109.5 . . ? H45A C45 H45E 56.3 . . ? H45B C45 H45E 141.1 . . ? H45C C45 H45E 56.3 . . ? H45D C45 H45E 109.5 . . ? C42 C45 H45F 109.5 . . ? H45A C45 H45F 56.3 . . ? H45B C45 H45F 56.3 . . ? H45C C45 H45F 141.1 . . ? H45D C45 H45F 109.5 . . ? H45E C45 H45F 109.5 . . ? C1 N1 C2 111.97(11) . . ? C1 N1 C4 124.58(11) . . ? C2 N1 C4 123.42(11) . . ? C1 N2 C3 111.78(11) . . ? C1 N2 C16 125.46(11) . . ? C3 N2 C16 122.37(11) . . ? C37 Fe1 C28 119.59(5) . . ? C37 Fe1 C1 117.79(5) . . ? C28 Fe1 C1 122.62(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 76.96 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.441 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.044 _iucr_refine_instructions_details ; TITL 1 in P2(1)/c CELL 1.54178 12.3163 17.9494 18.0222 90.000 98.365 90.000 ZERR 4.00 0.0001 0.0001 0.0001 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N FE UNIT 180 232 8 4 MERG 2 FMAP 2 PLAN 50 ACTA SIZE 0.020 0.060 0.140 BOND $H L.S. 8 TEMP -123.00 WGHT 0.053900 1.185800 FVAR 0.09271 MOLE 1 C1 1 0.733774 0.246444 0.114737 11.00000 0.02124 0.02123 = 0.02294 0.00013 -0.00011 -0.00114 C2 1 0.779084 0.232185 0.241051 11.00000 0.03073 0.02993 = 0.02098 0.00160 0.00077 -0.00168 AFIX 43 H2 2 0.819757 0.219474 0.288246 11.00000 -1.20000 AFIX 0 C3 1 0.678926 0.263794 0.228836 11.00000 0.03058 0.02909 = 0.02249 -0.00035 0.00404 -0.00087 AFIX 43 H3 2 0.635178 0.277985 0.265765 11.00000 -1.20000 AFIX 0 C4 1 0.913410 0.186856 0.160162 11.00000 0.02256 0.03242 = 0.02089 0.00127 -0.00246 0.00368 C5 1 0.917838 0.109087 0.161373 11.00000 0.03029 0.03321 = 0.02827 0.00327 -0.00184 0.00538 C6 1 1.018608 0.076184 0.154614 11.00000 0.03795 0.03853 = 0.04518 0.00227 0.00125 0.01292 AFIX 43 H6 2 1.025586 0.023486 0.156610 11.00000 -1.20000 AFIX 0 C7 1 1.108305 0.119437 0.145051 11.00000 0.02849 0.05590 = 0.04996 0.00158 0.00261 0.01317 AFIX 43 H7 2 1.176357 0.096118 0.140762 11.00000 -1.20000 AFIX 0 C8 1 1.100316 0.196171 0.141645 11.00000 0.02403 0.05396 = 0.03878 0.00265 -0.00003 0.00073 AFIX 43 H8 2 1.162603 0.224748 0.133871 11.00000 -1.20000 AFIX 0 C9 1 1.002299 0.232493 0.149426 11.00000 0.02459 0.03899 = 0.02385 0.00209 -0.00410 -0.00004 C10 1 0.817407 0.061835 0.168950 11.00000 0.03742 0.02652 = 0.03919 0.00355 0.00122 0.00170 AFIX 13 H10 2 0.750939 0.092648 0.151510 11.00000 -1.20000 AFIX 0 C11 1 0.810858 -0.008444 0.120143 11.00000 0.05448 0.03087 = 0.04243 0.00025 -0.00067 0.00075 AFIX 137 H11A 2 0.821276 0.005058 0.068964 11.00000 -1.50000 H11B 2 0.738780 -0.031824 0.119282 11.00000 -1.50000 H11C 2 0.868330 -0.043485 0.140988 11.00000 -1.50000 AFIX 0 C12 1 0.813927 0.040896 0.251026 11.00000 0.06810 0.03650 = 0.04467 0.00327 0.01437 -0.00695 AFIX 137 H12A 2 0.877912 0.010169 0.269584 11.00000 -1.50000 H12B 2 0.746666 0.012817 0.254669 11.00000 -1.50000 H12C 2 0.814976 0.086314 0.281300 11.00000 -1.50000 AFIX 0 C13 1 0.991852 0.316914 0.145599 11.00000 0.02566 0.03685 = 0.03061 0.00279 -0.00434 -0.00723 AFIX 13 H13 2 0.919145 0.328532 0.115386 11.00000 -1.20000 AFIX 0 C14 1 1.079831 0.353975 0.106282 11.00000 0.03171 0.05343 = 0.03641 0.00787 -0.00495 -0.01452 AFIX 137 H14A 2 1.151581 0.348728 0.137419 11.00000 -1.50000 H14B 2 1.062549 0.406961 0.098606 11.00000 -1.50000 H14C 2 1.081700 0.329968 0.057646 11.00000 -1.50000 AFIX 0 C15 1 0.992253 0.351850 0.223254 11.00000 0.04446 0.04274 = 0.04039 -0.00491 0.00324 -0.01296 AFIX 137 H15A 2 0.933615 0.329632 0.247346 11.00000 -1.50000 H15B 2 0.980160 0.405667 0.217915 11.00000 -1.50000 H15C 2 1.063242 0.342585 0.254144 11.00000 -1.50000 AFIX 0 C16 1 0.554276 0.310187 0.117592 11.00000 0.02346 0.02693 = 0.02450 0.00251 0.00372 0.00302 C17 1 0.555844 0.388003 0.120507 11.00000 0.03138 0.02656 = 0.03255 0.00150 0.00565 0.00141 C18 1 0.459247 0.425229 0.091888 11.00000 0.03844 0.02812 = 0.04513 0.00739 0.00907 0.00828 AFIX 43 H18 2 0.457130 0.478104 0.093516 11.00000 -1.20000 AFIX 0 C19 1 0.366854 0.386400 0.061293 11.00000 0.03061 0.04125 = 0.03999 0.01150 0.00622 0.01076 AFIX 43 H19 2 0.301633 0.412707 0.042660 11.00000 -1.20000 AFIX 0 C20 1 0.368426 0.309491 0.057531 11.00000 0.02441 0.04001 = 0.03208 0.00403 0.00242 0.00130 AFIX 43 H20 2 0.304566 0.283688 0.035247 11.00000 -1.20000 AFIX 0 C21 1 0.462058 0.269097 0.085854 11.00000 0.02508 0.02975 = 0.02347 0.00152 0.00437 0.00000 C22 1 0.658968 0.431600 0.150618 11.00000 0.03737 0.02542 = 0.05018 -0.00164 0.00463 -0.00340 AFIX 13 H22 2 0.722094 0.396023 0.158153 11.00000 -1.20000 AFIX 0 C23 1 0.683117 0.491129 0.093692 11.00000 0.05234 0.03951 = 0.06292 0.00141 0.02224 -0.00581 AFIX 137 H23A 2 0.629762 0.531744 0.092777 11.00000 -1.50000 H23B 2 0.677603 0.468713 0.043701 11.00000 -1.50000 H23C 2 0.757352 0.510813 0.108371 11.00000 -1.50000 AFIX 0 C24 1 0.650270 0.468501 0.225345 11.00000 0.08080 0.07110 = 0.04842 -0.01759 0.01673 -0.03727 AFIX 137 H24A 2 0.587986 0.503042 0.219355 11.00000 -1.50000 H24B 2 0.718024 0.495978 0.242544 11.00000 -1.50000 H24C 2 0.639187 0.430299 0.262363 11.00000 -1.50000 AFIX 0 C25 1 0.463631 0.184331 0.082129 11.00000 0.02849 0.02843 = 0.02895 -0.00204 0.00347 -0.00386 AFIX 13 H25 2 0.536696 0.169124 0.069170 11.00000 -1.20000 AFIX 0 C26 1 0.375641 0.153051 0.021414 11.00000 0.03583 0.04162 = 0.03401 -0.00623 0.00387 -0.01037 AFIX 137 H26A 2 0.302997 0.160653 0.036264 11.00000 -1.50000 H26B 2 0.388226 0.099651 0.015188 11.00000 -1.50000 H26C 2 0.379351 0.178820 -0.026092 11.00000 -1.50000 AFIX 0 C27 1 0.451781 0.148934 0.157879 11.00000 0.05287 0.03190 = 0.03258 0.00213 0.00271 -0.00877 AFIX 137 H27A 2 0.511412 0.166276 0.195949 11.00000 -1.50000 H27B 2 0.455272 0.094578 0.153691 11.00000 -1.50000 H27C 2 0.381079 0.163305 0.172458 11.00000 -1.50000 AFIX 0 C28 1 0.884787 0.275626 -0.044415 11.00000 0.02693 0.04179 = 0.02155 -0.00298 -0.00044 -0.00074 C29 1 0.955718 0.218614 -0.062765 11.00000 0.03381 0.04428 = 0.02633 -0.00680 0.00300 0.00036 C30 1 1.050286 0.234447 -0.094092 11.00000 0.03483 0.05168 = 0.03491 -0.01244 0.00510 0.00328 AFIX 43 H30 2 1.097370 0.194701 -0.103488 11.00000 -1.20000 AFIX 0 C31 1 1.077296 0.306266 -0.111803 11.00000 0.03346 0.05845 = 0.03072 -0.00963 0.00446 -0.00853 C32 1 1.008182 0.363222 -0.094852 11.00000 0.03880 0.04456 = 0.03054 -0.00038 0.00000 -0.00854 AFIX 43 H32 2 1.024338 0.413184 -0.106780 11.00000 -1.20000 AFIX 0 C33 1 0.915374 0.348533 -0.060614 11.00000 0.02943 0.04421 = 0.02547 -0.00263 -0.00169 -0.00134 C34 1 0.929304 0.137970 -0.049063 11.00000 0.05077 0.04507 = 0.05234 -0.00544 0.01413 0.00278 AFIX 123 H34A 2 0.861201 0.135118 -0.027049 10.50000 -1.50000 H34B 2 0.989388 0.115722 -0.014531 10.50000 -1.50000 H34C 2 0.920200 0.110792 -0.096726 10.50000 -1.50000 H34D 2 0.985992 0.105970 -0.065155 10.50000 -1.50000 H34E 2 0.857804 0.125367 -0.077673 10.50000 -1.50000 H34F 2 0.926992 0.130296 0.004522 10.50000 -1.50000 AFIX 0 C35 1 1.179013 0.321529 -0.147022 11.00000 0.04293 0.07730 = 0.04938 -0.01199 0.01586 -0.01463 AFIX 123 H35A 2 1.185178 0.375168 -0.155662 10.50000 -1.50000 H35B 2 1.174066 0.295020 -0.194934 10.50000 -1.50000 H35C 2 1.243829 0.304309 -0.113335 10.50000 -1.50000 H35D 2 1.216871 0.274497 -0.153625 10.50000 -1.50000 H35E 2 1.227983 0.354645 -0.114353 10.50000 -1.50000 H35F 2 1.158219 0.345356 -0.195952 10.50000 -1.50000 AFIX 0 C36 1 0.851276 0.414517 -0.038339 11.00000 0.03986 0.04114 = 0.04842 -0.00192 0.00495 0.00115 AFIX 123 H36A 2 0.788797 0.396881 -0.015159 10.50000 -1.50000 H36B 2 0.824485 0.444090 -0.082970 10.50000 -1.50000 H36C 2 0.898939 0.445412 -0.002430 10.50000 -1.50000 H36D 2 0.886016 0.460708 -0.051880 10.50000 -1.50000 H36E 2 0.850329 0.413499 0.015931 10.50000 -1.50000 H36F 2 0.775875 0.412177 -0.064609 10.50000 -1.50000 AFIX 0 C37 1 0.606195 0.213527 -0.073422 11.00000 0.02348 0.03203 = 0.02062 -0.00108 0.00115 -0.00043 C38 1 0.538388 0.267996 -0.112654 11.00000 0.02382 0.03362 = 0.02224 0.00103 0.00316 0.00004 C39 1 0.449303 0.248772 -0.166180 11.00000 0.02295 0.04255 = 0.02532 0.00635 0.00203 0.00027 AFIX 43 H39 2 0.404624 0.287017 -0.190998 11.00000 -1.20000 AFIX 0 C40 1 0.424761 0.175103 -0.183820 11.00000 0.02530 0.05017 = 0.02191 -0.00072 0.00147 -0.00779 C41 1 0.489687 0.120510 -0.145165 11.00000 0.03261 0.03460 = 0.03171 -0.00616 0.00381 -0.00716 AFIX 43 H41 2 0.473921 0.069570 -0.156277 11.00000 -1.20000 AFIX 0 C42 1 0.577841 0.138782 -0.090196 11.00000 0.02821 0.03227 = 0.02792 -0.00151 0.00168 -0.00073 C43 1 0.561735 0.349722 -0.098565 11.00000 0.03670 0.03209 = 0.04681 0.00130 -0.00208 0.00387 AFIX 123 H43A 2 0.626036 0.355309 -0.059988 10.50000 -1.50000 H43B 2 0.498098 0.373426 -0.081476 10.50000 -1.50000 H43C 2 0.576231 0.373500 -0.145082 10.50000 -1.50000 H43D 2 0.507541 0.379514 -0.131043 10.50000 -1.50000 H43E 2 0.635479 0.361397 -0.109555 10.50000 -1.50000 H43F 2 0.557346 0.361323 -0.045948 10.50000 -1.50000 AFIX 0 C44 1 0.329086 0.155628 -0.242816 11.00000 0.03611 0.06424 = 0.03313 -0.00114 -0.00638 -0.01420 AFIX 123 H44A 2 0.323702 0.101359 -0.248074 10.50000 -1.50000 H44B 2 0.340224 0.177740 -0.290853 10.50000 -1.50000 H44C 2 0.261191 0.175135 -0.227838 10.50000 -1.50000 H44D 2 0.293043 0.201464 -0.263103 10.50000 -1.50000 H44E 2 0.276521 0.125083 -0.220324 10.50000 -1.50000 H44F 2 0.355554 0.127687 -0.283338 10.50000 -1.50000 AFIX 0 C45 1 0.640061 0.075790 -0.047414 11.00000 0.04240 0.03193 = 0.05473 0.00445 -0.00390 0.00115 AFIX 123 H45A 2 0.699323 0.096314 -0.010967 10.50000 -1.50000 H45B 2 0.671254 0.043249 -0.082545 10.50000 -1.50000 H45C 2 0.589917 0.046998 -0.021013 10.50000 -1.50000 H45D 2 0.607673 0.028059 -0.065383 10.50000 -1.50000 H45E 2 0.635742 0.081125 0.006195 10.50000 -1.50000 H45F 2 0.717079 0.077376 -0.055337 10.50000 -1.50000 AFIX 0 N1 3 0.811132 0.221852 0.171128 11.00000 0.02228 0.02505 = 0.02148 0.00043 -0.00076 0.00015 N2 3 0.652098 0.271588 0.151668 11.00000 0.02267 0.02363 = 0.02311 -0.00022 0.00131 0.00055 FE1 4 0.743215 0.246246 -0.001477 11.00000 0.02274 0.02771 = 0.01995 -0.00077 -0.00145 -0.00006 HKLF 4 REM p21c in P2(1)/c REM R1 = 0.0356 for 7426 Fo > 4sig(Fo) and 0.0404 for all 8283 data REM 441 parameters refined using 0 restraints END WGHT 0.0539 1.1856 REM Highest difference peak 0.441, deepest hole -0.567, 1-sigma level 0.044 Q1 1 0.8297 0.2993 -0.0182 11.00000 0.05 0.44 Q2 1 0.7237 0.4471 0.1078 11.00000 0.05 0.32 Q3 1 0.6520 0.2200 -0.0436 11.00000 0.05 0.25 Q4 1 0.8994 0.1255 0.0036 11.00000 0.05 0.24 Q5 1 0.3555 0.1034 -0.2614 11.00000 0.05 0.20 Q6 1 0.9218 0.3034 -0.0549 11.00000 0.05 0.18 Q7 1 0.7993 0.4349 -0.0816 11.00000 0.05 0.18 Q8 1 0.8645 0.1223 -0.1001 11.00000 0.05 0.18 Q9 1 0.8679 0.0847 0.1680 11.00000 0.05 0.18 Q10 1 0.9977 0.2759 0.1458 11.00000 0.05 0.18 Q11 1 0.6134 0.4153 0.1378 11.00000 0.05 0.17 Q12 1 0.6525 0.4428 0.1903 11.00000 0.05 0.16 Q13 1 0.6938 0.2346 0.0244 11.00000 0.05 0.16 Q14 1 0.4595 0.2293 0.0836 11.00000 0.05 0.16 Q15 1 0.7362 0.2535 0.0706 11.00000 0.05 0.16 Q16 1 0.9137 0.1466 0.1636 11.00000 0.05 0.16 Q17 1 1.2435 0.3391 -0.1045 11.00000 0.05 0.15 Q18 1 1.0328 0.3386 0.1279 11.00000 0.05 0.15 Q19 1 0.7840 0.2431 0.0568 11.00000 0.05 0.15 Q20 1 1.0017 0.0978 -0.0436 11.00000 0.05 0.15 Q21 1 0.7937 0.4002 0.0051 11.00000 0.05 0.15 Q22 1 1.1608 0.3713 -0.1873 11.00000 0.05 0.14 Q23 1 0.5956 0.2931 0.1301 11.00000 0.05 0.14 Q24 1 0.4246 0.1656 0.0521 11.00000 0.05 0.14 Q25 1 0.3847 0.1628 -0.2117 11.00000 0.05 0.14 Q26 1 0.9617 0.0959 0.1542 11.00000 0.05 0.14 Q27 1 0.9540 0.3695 -0.0755 11.00000 0.05 0.14 Q28 1 0.5532 0.3463 0.1330 11.00000 0.05 0.13 Q29 1 0.6647 0.4585 0.1325 11.00000 0.05 0.13 Q30 1 0.5065 0.2573 -0.1428 11.00000 0.05 0.13 Q31 1 0.8143 0.0296 0.1478 11.00000 0.05 0.13 Q32 1 0.6878 0.5203 0.2461 11.00000 0.05 0.13 Q33 1 0.5941 0.1788 -0.0801 11.00000 0.05 0.13 Q34 1 0.6041 0.1095 -0.0640 11.00000 0.05 0.13 Q35 1 0.8196 0.0487 0.2087 11.00000 0.05 0.13 Q36 1 0.3765 0.1598 -0.0292 11.00000 0.05 0.13 Q37 1 0.8743 0.2012 0.1677 11.00000 0.05 0.13 Q38 1 0.6583 0.2638 0.1916 11.00000 0.05 0.13 Q39 1 0.4625 0.1441 -0.1686 11.00000 0.05 0.13 Q40 1 0.3016 0.1994 -0.2843 11.00000 0.05 0.13 Q41 1 0.5207 0.1222 -0.1096 11.00000 0.05 0.12 Q42 1 1.1180 0.3176 -0.1300 11.00000 0.05 0.12 Q43 1 0.5745 0.2407 -0.0954 11.00000 0.05 0.12 Q44 1 0.7820 0.2323 0.1404 11.00000 0.05 0.12 Q45 1 1.0585 0.3845 -0.1198 11.00000 0.05 0.12 Q46 1 0.8389 0.0823 0.2901 11.00000 0.05 0.12 Q47 1 0.4802 0.1726 0.2103 11.00000 0.05 0.12 Q48 1 0.5066 0.4062 0.1165 11.00000 0.05 0.12 Q49 1 0.6105 0.5181 0.2150 11.00000 0.05 0.12 Q50 1 0.9833 0.3354 0.1813 11.00000 0.05 0.11 ; _database_code_depnum_ccdc_archive 'CCDC 962247' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Fe(6-Xyl)(mes)2] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C38 H46 Fe N2' _chemical_formula_sum 'C38 H46 Fe N2' _chemical_formula_weight 586.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.1298(3) _cell_length_b 9.85550(10) _cell_length_c 17.0866(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.231(2) _cell_angle_gamma 90.00 _cell_volume 3191.77(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(2) _cell_measurement_reflns_used 5564 _cell_measurement_theta_min 2.8807 _cell_measurement_theta_max 76.0401 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 3.984 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5029 _exptl_absorpt_correction_T_max 0.6914 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; C3 of the 6-Xyl NHC displays disorder over two positions around a symmetry site. This was modelled by fixing it to half occupancy. Hydrogen atoms attached to the adjacent C2 atom were located in the difference map, and their positions and isotropic displacement parameters refined. ; _diffrn_ambient_temperature 150.0(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4102 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 8080 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.67 _diffrn_reflns_theta_max 76.22 _reflns_number_total 3317 _reflns_number_gt 3130 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^ > 2\s(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^)+(0.0567P)^2^+1.7292P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3317 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.24175(3) 0.2500 0.01801(10) Uani 1 2 d S . . N1 N 0.44173(6) -0.04632(13) 0.23560(9) 0.0272(3) Uani 1 1 d . . . C1 C 0.5000 0.02468(19) 0.2500 0.0211(4) Uani 1 2 d S . . C2 C 0.43683(10) -0.19607(18) 0.23174(19) 0.0501(6) Uani 1 1 d . . . C3 C 0.4944(3) -0.2552(3) 0.2105(4) 0.0605(15) Uani 0.50 1 d P . -1 H3A H 0.4962 -0.3549 0.2180 0.073 Uiso 0.50 1 calc PR . -1 H3B H 0.4832 -0.2354 0.1489 0.073 Uiso 0.50 1 calc PR . -1 C4 C 0.37775(7) 0.02475(14) 0.22076(10) 0.0233(3) Uani 1 1 d . . . C5 C 0.33427(7) 0.07401(15) 0.13723(10) 0.0263(3) Uani 1 1 d . . . C6 C 0.27279(8) 0.14192(17) 0.12468(11) 0.0330(3) Uani 1 1 d . . . H6 H 0.2433 0.1792 0.0691 0.040 Uiso 1 1 calc R . . C7 C 0.25411(8) 0.15573(19) 0.19248(12) 0.0377(4) Uani 1 1 d . . . H7 H 0.2120 0.2023 0.1831 0.045 Uiso 1 1 calc R . . C8 C 0.29638(9) 0.10213(18) 0.27339(12) 0.0351(4) Uani 1 1 d . . . H8 H 0.2826 0.1108 0.3191 0.042 Uiso 1 1 calc R . . C9 C 0.35889(8) 0.03556(16) 0.28933(10) 0.0284(3) Uani 1 1 d . . . C10 C 0.35113(9) 0.05193(19) 0.06132(11) 0.0358(4) Uani 1 1 d . . . H10A H 0.3959 0.0029 0.0812 0.054 Uiso 0.50 1 calc PR . . H10B H 0.3550 0.1399 0.0370 0.054 Uiso 0.50 1 calc PR . . H10C H 0.3134 -0.0014 0.0163 0.054 Uiso 0.50 1 calc PR . . H10D H 0.3136 0.0913 0.0085 0.054 Uiso 0.50 1 calc PR . . H10E H 0.3546 -0.0456 0.0527 0.054 Uiso 0.50 1 calc PR . . H10F H 0.3962 0.0957 0.0733 0.054 Uiso 0.50 1 calc PR . . C11 C 0.40307(10) -0.0255(2) 0.37792(12) 0.0430(4) Uani 1 1 d . . . H11A H 0.4450 -0.0684 0.3781 0.065 Uiso 0.50 1 calc PR . . H11B H 0.3753 -0.0937 0.3909 0.065 Uiso 0.50 1 calc PR . . H11C H 0.4177 0.0460 0.4223 0.065 Uiso 0.50 1 calc PR . . H11D H 0.3803 -0.0089 0.4161 0.065 Uiso 0.50 1 calc PR . . H11E H 0.4500 0.0163 0.4033 0.065 Uiso 0.50 1 calc PR . . H11F H 0.4076 -0.1234 0.3719 0.065 Uiso 0.50 1 calc PR . . C12 C 0.43667(7) 0.35980(14) 0.14479(9) 0.0213(3) Uani 1 1 d . . . C13 C 0.44519(7) 0.37095(14) 0.06759(9) 0.0233(3) Uani 1 1 d . . . C14 C 0.40706(8) 0.46555(15) 0.00299(10) 0.0274(3) Uani 1 1 d . . . H14 H 0.4144 0.4709 -0.0479 0.033 Uiso 1 1 calc R . . C15 C 0.35865(8) 0.55193(15) 0.01181(10) 0.0287(3) Uani 1 1 d . . . C16 C 0.34840(7) 0.54017(15) 0.08657(10) 0.0270(3) Uani 1 1 d . . . H16 H 0.3145 0.5965 0.0930 0.032 Uiso 1 1 calc R . . C17 C 0.38679(7) 0.44753(14) 0.15226(9) 0.0235(3) Uani 1 1 d . . . C18 C 0.49619(8) 0.27815(16) 0.05334(10) 0.0283(3) Uani 1 1 d . . . H18A H 0.5190 0.2179 0.1038 0.042 Uiso 0.50 1 calc PR . . H18B H 0.5321 0.3327 0.0464 0.042 Uiso 0.50 1 calc PR . . H18C H 0.4705 0.2237 0.0007 0.042 Uiso 0.50 1 calc PR . . H18D H 0.4954 0.2983 -0.0032 0.042 Uiso 0.50 1 calc PR . . H18E H 0.4823 0.1835 0.0542 0.042 Uiso 0.50 1 calc PR . . H18F H 0.5439 0.2925 0.0999 0.042 Uiso 0.50 1 calc PR . . C19 C 0.31896(9) 0.65643(19) -0.05729(12) 0.0399(4) Uani 1 1 d . . . H19A H 0.2874 0.7078 -0.0401 0.060 Uiso 0.50 1 calc PR . . H19B H 0.2911 0.6107 -0.1130 0.060 Uiso 0.50 1 calc PR . . H19C H 0.3526 0.7186 -0.0636 0.060 Uiso 0.50 1 calc PR . . H19D H 0.3334 0.6503 -0.1044 0.060 Uiso 0.50 1 calc PR . . H19E H 0.3296 0.7473 -0.0315 0.060 Uiso 0.50 1 calc PR . . H19F H 0.2682 0.6394 -0.0809 0.060 Uiso 0.50 1 calc PR . . C20 C 0.37512(8) 0.44454(17) 0.23358(11) 0.0302(3) Uani 1 1 d . . . H20A H 0.4055 0.3752 0.2737 0.045 Uiso 0.50 1 calc PR . . H20B H 0.3256 0.4231 0.2175 0.045 Uiso 0.50 1 calc PR . . H20C H 0.3867 0.5335 0.2621 0.045 Uiso 0.50 1 calc PR . . H20D H 0.3397 0.5126 0.2285 0.045 Uiso 0.50 1 calc PR . . H20E H 0.4196 0.4647 0.2847 0.045 Uiso 0.50 1 calc PR . . H20F H 0.3585 0.3543 0.2401 0.045 Uiso 0.50 1 calc PR . . H2A H 0.391(3) -0.223(5) 0.197(4) 0.042(12) Uiso 0.50 1 d P . . H2B H 0.443(5) -0.228(7) 0.293(5) 0.09(2) Uiso 0.50 1 d P . . H2C H 0.397(3) -0.223(5) 0.243(4) 0.037(12) Uiso 0.50 1 d P . . H2D H 0.418(4) -0.217(7) 0.162(5) 0.09(2) Uiso 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 0.01932(16) 0.01447(15) 0.01917(16) 0.000 0.00753(12) 0.000 N1 0.0229(6) 0.0163(6) 0.0409(7) -0.0020(5) 0.0127(5) -0.0024(4) C1 0.0231(9) 0.0171(9) 0.0221(8) 0.000 0.0091(7) 0.000 C2 0.0355(10) 0.0167(8) 0.0985(18) -0.0050(9) 0.0298(11) -0.0057(7) C3 0.039(2) 0.0191(16) 0.124(5) -0.0200(18) 0.036(3) -0.0051(14) C4 0.0206(6) 0.0185(6) 0.0305(7) -0.0036(5) 0.0111(5) -0.0051(5) C5 0.0247(7) 0.0250(7) 0.0284(7) -0.0051(6) 0.0112(6) -0.0077(6) C6 0.0226(7) 0.0314(8) 0.0375(8) -0.0001(7) 0.0067(6) -0.0031(6) C7 0.0237(7) 0.0351(9) 0.0552(10) -0.0098(8) 0.0184(7) -0.0023(6) C8 0.0338(8) 0.0369(8) 0.0442(9) -0.0144(7) 0.0260(7) -0.0131(7) C9 0.0294(7) 0.0264(7) 0.0295(7) -0.0050(6) 0.0132(6) -0.0116(6) C10 0.0371(8) 0.0419(9) 0.0290(7) -0.0097(7) 0.0151(7) -0.0129(7) C11 0.0492(10) 0.0437(10) 0.0324(8) 0.0043(7) 0.0147(7) -0.0158(8) C12 0.0198(6) 0.0171(6) 0.0235(6) 0.0006(5) 0.0065(5) -0.0020(5) C13 0.0227(6) 0.0201(6) 0.0245(6) -0.0014(5) 0.0081(5) -0.0040(5) C14 0.0281(7) 0.0257(7) 0.0238(7) 0.0023(6) 0.0075(5) -0.0050(6) C15 0.0261(7) 0.0212(7) 0.0288(7) 0.0041(6) 0.0029(6) -0.0027(6) C16 0.0221(6) 0.0201(7) 0.0329(7) -0.0013(6) 0.0069(6) 0.0007(5) C17 0.0207(6) 0.0200(6) 0.0268(7) -0.0010(5) 0.0078(5) -0.0019(5) C18 0.0310(7) 0.0272(7) 0.0292(7) -0.0014(6) 0.0156(6) -0.0006(6) C19 0.0381(8) 0.0297(8) 0.0391(9) 0.0115(7) 0.0055(7) 0.0034(7) C20 0.0282(7) 0.0309(8) 0.0336(8) 0.0000(6) 0.0156(6) 0.0042(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C12 2.0615(13) 2_655 ? Fe1 C12 2.0615(13) . ? Fe1 C1 2.1393(19) . ? N1 C1 1.3410(16) . ? N1 C4 1.4422(18) . ? N1 C2 1.479(2) . ? C1 N1 1.3410(16) 2_655 ? C2 C3 1.469(5) 2_655 ? C2 C3 1.530(5) . ? C2 H2A 0.92(5) . ? C2 H2B 1.05(8) . ? C2 H2C 0.98(5) . ? C2 H2D 1.10(7) . ? C3 C2 1.469(5) 2_655 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C9 1.398(2) . ? C4 C5 1.399(2) . ? C5 C6 1.391(2) . ? C5 C10 1.505(2) . ? C6 C7 1.386(2) . ? C6 H6 0.9500 . ? C7 C8 1.377(3) . ? C7 H7 0.9500 . ? C8 C9 1.390(2) . ? C8 H8 0.9500 . ? C9 C11 1.508(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C10 H10E 0.9800 . ? C10 H10F 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C12 C17 1.412(2) . ? C12 C13 1.4122(19) . ? C13 C14 1.397(2) . ? C13 C18 1.513(2) . ? C14 C15 1.389(2) . ? C14 H14 0.9500 . ? C15 C16 1.392(2) . ? C15 C19 1.511(2) . ? C16 C17 1.395(2) . ? C16 H16 0.9500 . ? C17 C20 1.515(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 H18D 0.9800 . ? C18 H18E 0.9800 . ? C18 H18F 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 H19D 0.9800 . ? C19 H19E 0.9800 . ? C19 H19F 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 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 C12 Fe1 C12 111.29(8) 2_655 . ? C12 Fe1 C1 124.36(4) 2_655 . ? C12 Fe1 C1 124.36(4) . . ? C1 N1 C4 119.48(13) . . ? C1 N1 C2 124.72(13) . . ? C4 N1 C2 115.79(12) . . ? N1 C1 N1 117.08(18) . 2_655 ? N1 C1 Fe1 121.46(9) . . ? N1 C1 Fe1 121.46(9) 2_655 . ? C3 C2 N1 109.7(2) 2_655 . ? C3 C2 C3 49.8(5) 2_655 . ? N1 C2 C3 110.07(19) . . ? C3 C2 H2A 140(3) 2_655 . ? N1 C2 H2A 110(3) . . ? C3 C2 H2A 117(4) . . ? C3 C2 H2B 64(5) 2_655 . ? N1 C2 H2B 106(4) . . ? C3 C2 H2B 111(4) . . ? H2A C2 H2B 101(5) . . ? C3 C2 H2C 116(3) 2_655 . ? N1 C2 H2C 108(3) . . ? C3 C2 H2C 142(3) . . ? H2A C2 H2C 46(4) . . ? H2B C2 H2C 57(5) . . ? C3 C2 H2D 116(4) 2_655 . ? N1 C2 H2D 103(4) . . ? C3 C2 H2D 68(4) . . ? H2A C2 H2D 58(4) . . ? H2B C2 H2D 149(5) . . ? H2C C2 H2D 103(5) . . ? C2 C3 C2 110.1(3) 2_655 . ? C2 C3 H3A 109.6 2_655 . ? C2 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 2_655 . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.2 . . ? C2 C3 H2D 141(3) 2_655 . ? H3A C3 H2D 106.8 . . ? H3B C3 H2D 70.9 . . ? C9 C4 C5 121.77(14) . . ? C9 C4 N1 118.80(13) . . ? C5 C4 N1 119.32(13) . . ? C6 C5 C4 118.13(14) . . ? C6 C5 C10 119.82(15) . . ? C4 C5 C10 122.02(14) . . ? C7 C6 C5 120.67(15) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 120.22(15) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.10(15) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 118.02(15) . . ? C8 C9 C11 119.87(15) . . ? C4 C9 C11 122.09(15) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C10 H10D 109.5 . . ? H10A C10 H10D 141.1 . . ? H10B C10 H10D 56.3 . . ? H10C C10 H10D 56.3 . . ? C5 C10 H10E 109.5 . . ? H10A C10 H10E 56.3 . . ? H10B C10 H10E 141.1 . . ? H10C C10 H10E 56.3 . . ? H10D C10 H10E 109.5 . . ? C5 C10 H10F 109.5 . . ? H10A C10 H10F 56.3 . . ? H10B C10 H10F 56.3 . . ? H10C C10 H10F 141.1 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.3 . . ? C9 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? C9 C11 H11F 109.5 . . ? H11A C11 H11F 56.3 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? C17 C12 C13 116.44(12) . . ? C17 C12 Fe1 119.31(10) . . ? C13 C12 Fe1 123.84(10) . . ? C14 C13 C12 121.53(13) . . ? C14 C13 C18 118.65(13) . . ? C12 C13 C18 119.82(13) . . ? C15 C14 C13 121.23(14) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 117.98(13) . . ? C14 C15 C19 120.92(15) . . ? C16 C15 C19 121.09(15) . . ? C15 C16 C17 121.46(14) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 121.32(14) . . ? C16 C17 C20 118.57(13) . . ? C12 C17 C20 120.10(13) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C18 H18D 109.5 . . ? H18A C18 H18D 141.1 . . ? H18B C18 H18D 56.3 . . ? H18C C18 H18D 56.3 . . ? C13 C18 H18E 109.5 . . ? H18A C18 H18E 56.3 . . ? H18B C18 H18E 141.1 . . ? H18C C18 H18E 56.3 . . ? H18D C18 H18E 109.5 . . ? C13 C18 H18F 109.5 . . ? H18A C18 H18F 56.3 . . ? H18B C18 H18F 56.3 . . ? H18C C18 H18F 141.1 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C19 H19D 109.5 . . ? H19A C19 H19D 141.1 . . ? H19B C19 H19D 56.3 . . ? H19C C19 H19D 56.3 . . ? C15 C19 H19E 109.5 . . ? H19A C19 H19E 56.3 . . ? H19B C19 H19E 141.1 . . ? H19C C19 H19E 56.3 . . ? H19D C19 H19E 109.5 . . ? C15 C19 H19F 109.5 . . ? H19A C19 H19F 56.3 . . ? H19B C19 H19F 56.3 . . ? H19C C19 H19F 141.1 . . ? H19D C19 H19F 109.5 . . ? H19E C19 H19F 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C20 H20D 109.5 . . ? H20A C20 H20D 141.1 . . ? H20B C20 H20D 56.3 . . ? H20C C20 H20D 56.3 . . ? C17 C20 H20E 109.5 . . ? H20A C20 H20E 56.3 . . ? H20B C20 H20E 141.1 . . ? H20C C20 H20E 56.3 . . ? H20D C20 H20E 109.5 . . ? C17 C20 H20F 109.5 . . ? H20A C20 H20F 56.3 . . ? H20B C20 H20F 56.3 . . ? H20C C20 H20F 141.1 . . ? H20D C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 76.22 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.316 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.054 _iucr_refine_instructions_details ; TITL c2c in C2/c CELL 1.54178 21.1298 9.8555 17.0866 90.000 116.231 90.000 ZERR 4.00 0.0003 0.0001 0.0003 0.000 0.002 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N FE UNIT 152 184 8 4 MERG 2 FREE C3 H2D FMAP 2 PLAN 100 SIZE 0.100 0.160 0.200 ACTA BOND $H L.S. 8 TEMP -123.00 WGHT 0.056700 1.729200 FVAR 0.08734 0.79626 FE1 4 0.500000 0.241754 0.250000 10.50000 0.01932 0.01447 = 0.01917 0.00000 0.00753 0.00000 N1 3 0.441734 -0.046324 0.235601 11.00000 0.02291 0.01633 = 0.04091 -0.00204 0.01273 -0.00243 C1 1 0.500000 0.024684 0.250000 10.50000 0.02306 0.01711 = 0.02210 0.00000 0.00907 0.00000 C2 1 0.436833 -0.196075 0.231745 11.00000 0.03546 0.01671 = 0.09845 -0.00502 0.02984 -0.00572 PART -1 C3 1 0.494381 -0.255170 0.210474 10.50000 0.03923 0.01912 = 0.12357 -0.01999 0.03623 -0.00511 AFIX 23 H3A 2 0.496202 -0.354912 0.218038 10.50000 -1.20000 H3B 2 0.483223 -0.235376 0.148936 10.50000 -1.20000 AFIX 0 PART 0 C4 1 0.377746 0.024752 0.220762 11.00000 0.02055 0.01847 = 0.03054 -0.00359 0.01107 -0.00515 C5 1 0.334274 0.074015 0.137234 11.00000 0.02474 0.02501 = 0.02845 -0.00513 0.01121 -0.00774 C6 1 0.272793 0.141920 0.124683 11.00000 0.02263 0.03143 = 0.03752 -0.00013 0.00667 -0.00308 AFIX 43 H6 2 0.243320 0.179201 0.069077 11.00000 -1.20000 AFIX 0 C7 1 0.254106 0.155733 0.192479 11.00000 0.02372 0.03505 = 0.05524 -0.00980 0.01839 -0.00229 AFIX 43 H7 2 0.211991 0.202334 0.183107 11.00000 -1.20000 AFIX 0 C8 1 0.296384 0.102130 0.273388 11.00000 0.03383 0.03688 = 0.04416 -0.01443 0.02599 -0.01311 AFIX 43 H8 2 0.282583 0.110804 0.319060 11.00000 -1.20000 AFIX 0 C9 1 0.358894 0.035565 0.289334 11.00000 0.02939 0.02641 = 0.02952 -0.00502 0.01319 -0.01159 C10 1 0.351126 0.051927 0.061320 11.00000 0.03714 0.04190 = 0.02897 -0.00967 0.01505 -0.01290 AFIX 123 H10A 2 0.395922 0.002926 0.081165 10.50000 -1.50000 H10B 2 0.355016 0.139864 0.037021 10.50000 -1.50000 H10C 2 0.313413 -0.001391 0.016341 10.50000 -1.50000 H10D 2 0.313646 0.091340 0.008520 10.50000 -1.50000 H10E 2 0.354551 -0.045598 0.052663 10.50000 -1.50000 H10F 2 0.396154 0.095657 0.073343 10.50000 -1.50000 AFIX 0 C11 1 0.403072 -0.025474 0.377924 11.00000 0.04924 0.04373 = 0.03245 0.00435 0.01475 -0.01576 AFIX 123 H11A 2 0.444974 -0.068437 0.378133 10.50000 -1.50000 H11B 2 0.375284 -0.093676 0.390875 10.50000 -1.50000 H11C 2 0.417659 0.046036 0.422317 10.50000 -1.50000 H11D 2 0.380304 -0.008948 0.416084 10.50000 -1.50000 H11E 2 0.449994 0.016292 0.403342 10.50000 -1.50000 H11F 2 0.407619 -0.123421 0.371899 10.50000 -1.50000 AFIX 0 C12 1 0.436665 0.359798 0.144785 11.00000 0.01985 0.01706 = 0.02352 0.00063 0.00652 -0.00203 C13 1 0.445192 0.370955 0.067591 11.00000 0.02266 0.02007 = 0.02447 -0.00143 0.00806 -0.00403 C14 1 0.407065 0.465550 0.002991 11.00000 0.02812 0.02573 = 0.02383 0.00229 0.00748 -0.00500 AFIX 43 H14 2 0.414373 0.470932 -0.047932 11.00000 -1.20000 AFIX 0 C15 1 0.358646 0.551932 0.011806 11.00000 0.02605 0.02120 = 0.02878 0.00414 0.00287 -0.00270 C16 1 0.348399 0.540167 0.086574 11.00000 0.02210 0.02014 = 0.03289 -0.00127 0.00685 0.00072 AFIX 43 H16 2 0.314512 0.596467 0.093026 11.00000 -1.20000 AFIX 0 C17 1 0.386787 0.447534 0.152257 11.00000 0.02068 0.02002 = 0.02676 -0.00095 0.00776 -0.00188 C18 1 0.496187 0.278152 0.053342 11.00000 0.03099 0.02716 = 0.02919 -0.00144 0.01557 -0.00065 AFIX 123 H18A 2 0.518990 0.217880 0.103768 10.50000 -1.50000 H18B 2 0.532133 0.332715 0.046357 10.50000 -1.50000 H18C 2 0.470473 0.223748 0.000671 10.50000 -1.50000 H18D 2 0.495407 0.298348 -0.003237 10.50000 -1.50000 H18E 2 0.482265 0.183513 0.054174 10.50000 -1.50000 H18F 2 0.543924 0.292480 0.099860 10.50000 -1.50000 AFIX 0 C19 1 0.318963 0.656433 -0.057295 11.00000 0.03806 0.02968 = 0.03914 0.01147 0.00545 0.00341 AFIX 123 H19A 2 0.287411 0.707752 -0.040068 10.50000 -1.50000 H19B 2 0.291133 0.610721 -0.113020 10.50000 -1.50000 H19C 2 0.352607 0.718608 -0.063618 10.50000 -1.50000 H19D 2 0.333356 0.650302 -0.104402 10.50000 -1.50000 H19E 2 0.329634 0.747333 -0.031451 10.50000 -1.50000 H19F 2 0.268160 0.639446 -0.080853 10.50000 -1.50000 AFIX 0 C20 1 0.375121 0.444541 0.233578 11.00000 0.02825 0.03094 = 0.03358 0.00002 0.01560 0.00424 AFIX 123 H20A 2 0.405493 0.375156 0.273691 10.50000 -1.50000 H20B 2 0.325616 0.423080 0.217501 10.50000 -1.50000 H20C 2 0.386709 0.533451 0.262147 10.50000 -1.50000 H20D 2 0.339719 0.512635 0.228535 10.50000 -1.50000 H20E 2 0.419596 0.464712 0.284725 10.50000 -1.50000 H20F 2 0.358503 0.354340 0.240079 10.50000 -1.50000 AFIX 0 H2A 2 0.391253 -0.222825 0.197078 10.50000 0.04150 H2B 2 0.443122 -0.228209 0.293119 10.50000 0.09374 H2C 2 0.397316 -0.223372 0.243218 10.50000 0.03750 H2D 2 0.417527 -0.217085 0.161856 10.50000 0.08535 HKLF 4 REM c2c in C2/c REM R1 = 0.0329 for 3130 Fo > 4sig(Fo) and 0.0352 for all 3317 data REM 208 parameters refined using 0 restraints END WGHT 0.0567 1.7293 REM Highest difference peak 0.316, deepest hole -0.368, 1-sigma level 0.054 Q1 1 0.5000 0.1057 0.2500 10.50000 0.05 0.30 Q2 1 0.3957 0.0406 0.4342 11.00000 0.05 0.24 Q3 1 0.4273 0.4253 0.0387 11.00000 0.05 0.17 Q4 1 0.3406 0.5878 -0.0217 11.00000 0.05 0.16 Q5 1 0.3583 0.0614 0.1810 11.00000 0.05 0.16 Q6 1 0.4421 0.3665 0.1082 11.00000 0.05 0.16 Q7 1 0.2688 0.1596 0.1618 11.00000 0.05 0.15 Q8 1 0.3814 0.4942 0.0059 11.00000 0.05 0.15 Q9 1 0.3009 0.0861 0.1296 11.00000 0.05 0.14 Q10 1 0.4601 0.3170 0.1806 11.00000 0.05 0.14 Q11 1 0.3793 0.4430 0.1900 11.00000 0.05 0.13 Q12 1 0.3786 0.0111 0.3298 11.00000 0.05 0.13 Q13 1 0.3491 0.5377 0.0410 11.00000 0.05 0.13 Q14 1 0.4163 0.4001 0.1499 11.00000 0.05 0.12 Q15 1 0.4664 0.3224 0.0581 11.00000 0.05 0.12 Q16 1 0.1411 0.1641 0.1675 11.00000 0.05 0.12 Q17 1 0.2822 0.1531 0.2389 11.00000 0.05 0.11 Q18 1 0.3610 0.0139 0.2541 11.00000 0.05 0.11 Q19 1 0.4727 0.5629 0.0354 11.00000 0.05 0.11 Q20 1 0.4943 0.4124 -0.0562 11.00000 0.05 0.11 Q21 1 0.2926 0.0706 0.3530 11.00000 0.05 0.11 Q22 1 0.5009 0.4343 0.0061 11.00000 0.05 0.11 Q23 1 0.3020 -0.0852 0.3596 11.00000 0.05 0.11 Q24 1 0.3801 0.3599 -0.1255 11.00000 0.05 0.11 Q25 1 0.4911 0.3759 -0.0235 11.00000 0.05 0.11 Q26 1 0.3093 0.2910 0.2325 11.00000 0.05 0.11 Q27 1 0.4547 0.0175 0.4947 11.00000 0.05 0.10 Q28 1 0.4635 0.3509 0.2291 11.00000 0.05 0.10 Q29 1 0.3643 0.2411 -0.0484 11.00000 0.05 0.10 Q30 1 0.4382 0.4497 -0.0621 11.00000 0.05 0.10 Q31 1 0.3883 0.1622 0.0625 11.00000 0.05 0.10 Q32 1 0.4796 0.1039 0.1367 11.00000 0.05 0.10 Q33 1 0.4130 -0.0108 0.2284 11.00000 0.05 0.10 Q34 1 0.3209 0.0445 0.2738 11.00000 0.05 0.10 Q35 1 0.2247 0.5845 -0.1733 11.00000 0.05 0.09 Q36 1 0.4703 0.5190 0.0595 11.00000 0.05 0.09 Q37 1 0.3730 0.3243 0.0038 11.00000 0.05 0.09 Q38 1 0.4168 0.1547 0.0038 11.00000 0.05 0.09 Q39 1 0.3902 0.1619 0.4113 11.00000 0.05 0.09 Q40 1 0.4481 0.4420 0.3435 11.00000 0.05 0.09 Q41 1 0.1910 0.2195 0.1347 11.00000 0.05 0.09 Q42 1 0.2502 0.6072 -0.2132 11.00000 0.05 0.09 Q43 1 0.2717 -0.0161 0.2815 11.00000 0.05 0.09 Q44 1 0.2795 -0.0184 0.3755 11.00000 0.05 0.09 Q45 1 0.4082 -0.2752 0.3967 11.00000 0.05 0.09 Q46 1 0.4528 0.4146 -0.0848 11.00000 0.05 0.09 Q47 1 0.4442 0.5837 0.3385 11.00000 0.05 0.09 Q48 1 0.3717 0.4935 0.1250 11.00000 0.05 0.09 Q49 1 0.4881 0.5408 0.3975 11.00000 0.05 0.09 Q50 1 0.3482 0.2232 0.3236 11.00000 0.05 0.09 Q51 1 0.3996 0.1753 0.2504 11.00000 0.05 0.09 Q52 1 0.3960 -0.2166 0.4422 11.00000 0.05 0.09 Q53 1 0.6213 0.2545 0.1405 11.00000 0.05 0.09 Q54 1 0.3845 -0.2135 0.1534 11.00000 0.05 0.09 Q55 1 0.2491 0.5196 -0.1688 11.00000 0.05 0.09 Q56 1 0.3886 0.6123 -0.1149 11.00000 0.05 0.09 Q57 1 0.4797 -0.0008 0.3440 11.00000 0.05 0.08 Q58 1 0.3980 0.2582 0.0518 11.00000 0.05 0.08 Q59 1 0.2568 0.4660 0.1851 11.00000 0.05 0.08 Q60 1 0.1517 0.2669 0.1586 11.00000 0.05 0.08 Q61 1 0.4011 0.1483 0.2030 11.00000 0.05 0.08 Q62 1 0.5938 0.2014 0.1285 11.00000 0.05 0.08 Q63 1 0.4516 0.3406 -0.0661 11.00000 0.05 0.08 Q64 1 0.2429 0.3891 0.1467 11.00000 0.05 0.08 Q65 1 0.3948 0.1831 0.3143 11.00000 0.05 0.08 Q66 1 0.5077 0.0575 0.3922 11.00000 0.05 0.08 Q67 1 0.4174 0.5321 -0.0523 11.00000 0.05 0.07 Q68 1 0.2282 0.0244 0.2656 11.00000 0.05 0.07 Q69 1 0.3164 0.7171 -0.1652 11.00000 0.05 0.07 Q70 1 0.3783 0.2346 0.1662 11.00000 0.05 0.07 Q71 1 0.2238 0.1152 0.0479 11.00000 0.05 0.07 Q72 1 0.3144 0.4774 -0.1389 11.00000 0.05 0.07 Q73 1 0.3533 0.3972 -0.0802 11.00000 0.05 0.07 Q74 1 0.2675 0.4954 0.1270 11.00000 0.05 0.07 Q75 1 0.4878 0.0840 0.0775 11.00000 0.05 0.07 Q76 1 0.1802 0.1468 0.1478 11.00000 0.05 0.07 Q77 1 0.3140 -0.1216 0.1904 11.00000 0.05 0.07 Q78 1 0.2682 0.0110 0.1499 11.00000 0.05 0.07 Q79 1 0.5155 -0.3667 0.1685 11.00000 0.05 0.07 Q80 1 0.4163 0.7931 0.0044 11.00000 0.05 0.07 Q81 1 0.4429 0.0669 0.5214 11.00000 0.05 0.07 Q82 1 0.3577 0.6425 -0.1496 11.00000 0.05 0.07 Q83 1 0.2103 0.6236 -0.0643 11.00000 0.05 0.07 Q84 1 0.3736 0.3072 0.1539 11.00000 0.05 0.07 Q85 1 0.2304 0.0547 0.3504 11.00000 0.05 0.07 Q86 1 0.3077 -0.0236 -0.0465 11.00000 0.05 0.07 Q87 1 0.4972 0.4204 0.1567 11.00000 0.05 0.07 Q88 1 0.5299 -0.3673 0.1286 11.00000 0.05 0.07 Q89 1 0.4111 0.3789 0.3506 11.00000 0.05 0.07 Q90 1 0.4677 -0.0169 0.2400 11.00000 0.05 0.07 Q91 1 0.2777 0.4451 0.1641 11.00000 0.05 0.07 Q92 1 0.4490 -0.0205 0.2048 11.00000 0.05 0.07 Q93 1 0.3112 0.7677 -0.1413 11.00000 0.05 0.06 Q94 1 0.4391 -0.0033 0.0719 11.00000 0.05 0.06 Q95 1 0.3018 0.1819 0.3437 11.00000 0.05 0.06 Q96 1 0.3436 -0.2005 0.3962 11.00000 0.05 0.06 Q97 1 0.4050 -0.2112 0.0584 11.00000 0.05 0.06 Q98 1 0.4408 0.4889 0.3704 11.00000 0.05 0.06 Q99 1 0.4594 0.1141 -0.0406 11.00000 0.05 0.06 Q100 1 0.3436 -0.2368 0.1375 11.00000 0.05 0.06 ; _database_code_depnum_ccdc_archive 'CCDC 962248' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; K[Fe(mes)(IPr-H)2]*hex*0.5THF ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C63 H81 Fe K N4, C6 H14, 0.5(C4 H8 O)' _chemical_formula_sum 'C71 H99 Fe K N4 O0.50' _chemical_formula_weight 1111.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7856(3) _cell_length_b 14.2917(5) _cell_length_c 19.9211(7) _cell_angle_alpha 71.953(3) _cell_angle_beta 85.004(2) _cell_angle_gamma 74.811(2) _cell_volume 3340.08(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11737 _cell_measurement_theta_min 3.3546 _cell_measurement_theta_max 76.5191 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 2.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5007 _exptl_absorpt_correction_T_max 0.9484 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4102 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 31883 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 66.50 _reflns_number_total 11766 _reflns_number_gt 9569 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^ > 2\s(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^)+(0.1204P)^2^+0.1629P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11766 _refine_ls_number_parameters 724 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1722 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _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 K1 K 1.0000 0.0000 1.0000 0.0620(3) Uani 1 2 d S . . K2 K 0.5000 0.5000 0.5000 0.0642(4) Uani 1 2 d S . . Fe1 Fe 0.83357(3) 0.43363(3) 0.752656(19) 0.02416(13) Uani 1 1 d . . . N1 N 1.00828(17) 0.29595(17) 0.94526(11) 0.0263(4) Uani 1 1 d . . . N2 N 0.93156(17) 0.24022(16) 0.88219(11) 0.0250(4) Uani 1 1 d . . . C1 C 0.9926(2) 0.2077(2) 0.94141(13) 0.0280(5) Uani 1 1 d . . . C2 C 0.9582(2) 0.37913(19) 0.88964(13) 0.0276(5) Uani 1 1 d . . . H2 H 0.9592 0.4478 0.8823 0.033 Uiso 1 1 calc R . . C3 C 0.9078(2) 0.34535(19) 0.84782(14) 0.0272(5) Uani 1 1 d . . . C4 C 1.0735(2) 0.3018(2) 0.99884(13) 0.0290(5) Uani 1 1 d . . . C5 C 1.0217(2) 0.3301(2) 1.05693(14) 0.0315(6) Uani 1 1 d . . . C6 C 1.0862(3) 0.3363(3) 1.10758(16) 0.0411(7) Uani 1 1 d . . . H6 H 1.0535 0.3549 1.1478 0.049 Uiso 1 1 calc R . . C7 C 1.1973(3) 0.3156(3) 1.09948(18) 0.0527(9) Uani 1 1 d . . . H7 H 1.2404 0.3218 1.1336 0.063 Uiso 1 1 calc R . . C8 C 1.2468(3) 0.2859(3) 1.04258(19) 0.0506(9) Uani 1 1 d . . . H8 H 1.3235 0.2713 1.0383 0.061 Uiso 1 1 calc R . . C9 C 1.1861(3) 0.2770(3) 0.99118(16) 0.0380(6) Uani 1 1 d . . . C10 C 0.9000(2) 0.3465(2) 1.06712(15) 0.0351(6) Uani 1 1 d . . . H10 H 0.8671 0.3582 1.0206 0.042 Uiso 1 1 calc R . . C11 C 0.8758(4) 0.2503(4) 1.1185(3) 0.0785(15) Uani 1 1 d . . . H11A H 0.7973 0.2602 1.1253 0.118 Uiso 0.50 1 calc PR . . H11B H 0.9102 0.2357 1.1639 0.118 Uiso 0.50 1 calc PR . . H11C H 0.9044 0.1932 1.0993 0.118 Uiso 0.50 1 calc PR . . H11D H 0.9440 0.1992 1.1337 0.118 Uiso 0.50 1 calc PR . . H11E H 0.8311 0.2237 1.0951 0.118 Uiso 0.50 1 calc PR . . H11F H 0.8368 0.2662 1.1598 0.118 Uiso 0.50 1 calc PR . . C12 C 0.8490(3) 0.4380(4) 1.0929(3) 0.0676(12) Uani 1 1 d . . . H12A H 0.7706 0.4453 1.0985 0.101 Uiso 0.50 1 calc PR . . H12B H 0.8631 0.4993 1.0584 0.101 Uiso 0.50 1 calc PR . . H12C H 0.8805 0.4283 1.1384 0.101 Uiso 0.50 1 calc PR . . H12D H 0.9055 0.4700 1.0984 0.101 Uiso 0.50 1 calc PR . . H12E H 0.8131 0.4160 1.1385 0.101 Uiso 0.50 1 calc PR . . H12F H 0.7956 0.4870 1.0585 0.101 Uiso 0.50 1 calc PR . . C13 C 1.2422(2) 0.2423(3) 0.92955(17) 0.0429(7) Uani 1 1 d . . . H13 H 1.1860 0.2325 0.9022 0.051 Uiso 1 1 calc R . . C14 C 1.2963(4) 0.3201(3) 0.8803(2) 0.0627(10) Uani 1 1 d . . . H14A H 1.3314 0.2949 0.8413 0.094 Uiso 0.50 1 calc PR . . H14B H 1.3509 0.3318 0.9063 0.094 Uiso 0.50 1 calc PR . . H14C H 1.2418 0.3839 0.8614 0.094 Uiso 0.50 1 calc PR . . H14D H 1.2846 0.3789 0.8980 0.094 Uiso 0.50 1 calc PR . . H14E H 1.2652 0.3420 0.8330 0.094 Uiso 0.50 1 calc PR . . H14F H 1.3743 0.2898 0.8780 0.094 Uiso 0.50 1 calc PR . . C15 C 1.3250(4) 0.1408(3) 0.9561(2) 0.0689(12) Uani 1 1 d . . . H15A H 1.2893 0.0908 0.9878 0.103 Uiso 0.50 1 calc PR . . H15B H 1.3823 0.1492 0.9816 0.103 Uiso 0.50 1 calc PR . . H15C H 1.3567 0.1172 0.9158 0.103 Uiso 0.50 1 calc PR . . H15D H 1.3963 0.1474 0.9357 0.103 Uiso 0.50 1 calc PR . . H15E H 1.3032 0.0889 0.9419 0.103 Uiso 0.50 1 calc PR . . H15F H 1.3288 0.1210 1.0077 0.103 Uiso 0.50 1 calc PR . . C16 C 0.9029(2) 0.16521(19) 0.85799(14) 0.0287(5) Uani 1 1 d . . . C17 C 0.8041(2) 0.1401(2) 0.88021(15) 0.0344(6) Uani 1 1 d . . . C18 C 0.7867(3) 0.0568(3) 0.86441(19) 0.0476(8) Uani 1 1 d . . . H18 H 0.7213 0.0366 0.8798 0.057 Uiso 1 1 calc R . . C19 C 0.8614(3) 0.0032(3) 0.8273(2) 0.0534(9) Uani 1 1 d . . . H19 H 0.8482 -0.0542 0.8183 0.064 Uiso 1 1 calc R . . C20 C 0.9561(3) 0.0332(2) 0.8030(2) 0.0463(8) Uani 1 1 d . . . H20 H 1.0063 -0.0025 0.7759 0.056 Uiso 1 1 calc R . . C21 C 0.9787(2) 0.1149(2) 0.81799(16) 0.0355(6) Uani 1 1 d . . . C22 C 0.7203(3) 0.2011(3) 0.91958(17) 0.0416(7) Uani 1 1 d . . . H22 H 0.7392 0.2676 0.9106 0.050 Uiso 1 1 calc R . . C23 C 0.6086(4) 0.2250(6) 0.8918(4) 0.103(2) Uani 1 1 d . . . H23A H 0.6086 0.2571 0.8406 0.155 Uiso 0.50 1 calc PR . . H23B H 0.5589 0.2714 0.9144 0.155 Uiso 0.50 1 calc PR . . H23C H 0.5848 0.1621 0.9021 0.155 Uiso 0.50 1 calc PR . . H23D H 0.5596 0.2032 0.9308 0.155 Uiso 0.50 1 calc PR . . H23E H 0.6093 0.1890 0.8570 0.155 Uiso 0.50 1 calc PR . . H23F H 0.5834 0.2983 0.8693 0.155 Uiso 0.50 1 calc PR . . C24 C 0.7260(6) 0.1519(5) 0.9977(3) 0.097(2) Uani 1 1 d . . . H24A H 0.8004 0.1383 1.0136 0.146 Uiso 0.50 1 calc PR . . H24B H 0.7042 0.0878 1.0092 0.146 Uiso 0.50 1 calc PR . . H24C H 0.6771 0.1972 1.0214 0.146 Uiso 0.50 1 calc PR . . H24D H 0.6541 0.1439 1.0159 0.146 Uiso 0.50 1 calc PR . . H24E H 0.7502 0.1944 1.0202 0.146 Uiso 0.50 1 calc PR . . H24F H 0.7774 0.0849 1.0081 0.146 Uiso 0.50 1 calc PR . . C25 C 1.0814(2) 0.1483(2) 0.79003(17) 0.0402(7) Uani 1 1 d . . . H25 H 1.0799 0.2093 0.8049 0.048 Uiso 1 1 calc R . . C26 C 1.0864(4) 0.1803(4) 0.7093(2) 0.0659(11) Uani 1 1 d . . . H26A H 1.0208 0.2328 0.6903 0.099 Uiso 0.50 1 calc PR . . H26B H 1.0914 0.1213 0.6930 0.099 Uiso 0.50 1 calc PR . . H26C H 1.1502 0.2073 0.6930 0.099 Uiso 0.50 1 calc PR . . H26D H 1.1541 0.1414 0.6939 0.099 Uiso 0.50 1 calc PR . . H26E H 1.0835 0.2530 0.6912 0.099 Uiso 0.50 1 calc PR . . H26F H 1.0247 0.1670 0.6911 0.099 Uiso 0.50 1 calc PR . . C27 C 1.1827(3) 0.0664(4) 0.8222(3) 0.0659(11) Uani 1 1 d . . . H27A H 1.2475 0.0903 0.8031 0.099 Uiso 0.50 1 calc PR . . H27B H 1.1849 0.0042 0.8104 0.099 Uiso 0.50 1 calc PR . . H27C H 1.1806 0.0522 0.8736 0.099 Uiso 0.50 1 calc PR . . H27D H 1.1612 0.0075 0.8549 0.099 Uiso 0.50 1 calc PR . . H27E H 1.2238 0.0936 0.8476 0.099 Uiso 0.50 1 calc PR . . H27F H 1.2281 0.0456 0.7844 0.099 Uiso 0.50 1 calc PR . . N3 N 0.68134(17) 0.42943(17) 0.63755(11) 0.0252(4) Uani 1 1 d . . . N4 N 0.70624(17) 0.27526(17) 0.64173(11) 0.0261(4) Uani 1 1 d . . . C28 C 0.6507(2) 0.3692(2) 0.60501(14) 0.0291(5) Uani 1 1 d . . . C29 C 0.7548(2) 0.3767(2) 0.69408(13) 0.0261(5) Uani 1 1 d . . . C30 C 0.7686(2) 0.2779(2) 0.69538(14) 0.0282(5) Uani 1 1 d . . . H30 H 0.8132 0.2204 0.7275 0.034 Uiso 1 1 calc R . . C31 C 0.6311(2) 0.5361(2) 0.61582(13) 0.0270(5) Uani 1 1 d . . . C32 C 0.6850(2) 0.6034(2) 0.56752(14) 0.0312(6) Uani 1 1 d . . . C33 C 0.6266(3) 0.7042(2) 0.54037(17) 0.0423(7) Uani 1 1 d . . . H33 H 0.6605 0.7513 0.5073 0.051 Uiso 1 1 calc R . . C34 C 0.5203(3) 0.7370(2) 0.56066(19) 0.0481(8) Uani 1 1 d . . . H34 H 0.4814 0.8054 0.5404 0.058 Uiso 1 1 calc R . . C35 C 0.4710(2) 0.6711(2) 0.60982(18) 0.0406(7) Uani 1 1 d . . . H35 H 0.3987 0.6952 0.6242 0.049 Uiso 1 1 calc R . . C36 C 0.5251(2) 0.5688(2) 0.63950(15) 0.0310(6) Uani 1 1 d . . . C37 C 0.7997(2) 0.5667(2) 0.54211(16) 0.0381(6) Uani 1 1 d . . . H37 H 0.8369 0.5058 0.5804 0.046 Uiso 1 1 calc R . . C38 C 0.7972(3) 0.5332(3) 0.4772(2) 0.0550(9) Uani 1 1 d . . . H38A H 0.8715 0.5097 0.4614 0.083 Uiso 0.50 1 calc PR . . H38B H 0.7578 0.5906 0.4394 0.083 Uiso 0.50 1 calc PR . . H38C H 0.7607 0.4778 0.4887 0.083 Uiso 0.50 1 calc PR . . H38D H 0.7218 0.5424 0.4649 0.083 Uiso 0.50 1 calc PR . . H38E H 0.8356 0.4614 0.4870 0.083 Uiso 0.50 1 calc PR . . H38F H 0.8327 0.5743 0.4376 0.083 Uiso 0.50 1 calc PR . . C39 C 0.8653(3) 0.6461(3) 0.52843(19) 0.0487(8) Uani 1 1 d . . . H39A H 0.9384 0.6191 0.5123 0.073 Uiso 0.50 1 calc PR . . H39B H 0.8702 0.6625 0.5721 0.073 Uiso 0.50 1 calc PR . . H39C H 0.8295 0.7077 0.4921 0.073 Uiso 0.50 1 calc PR . . H39D H 0.8204 0.7071 0.5387 0.073 Uiso 0.50 1 calc PR . . H39E H 0.8885 0.6637 0.4789 0.073 Uiso 0.50 1 calc PR . . H39F H 0.9292 0.6185 0.5589 0.073 Uiso 0.50 1 calc PR . . C40 C 0.4710(2) 0.4974(2) 0.69637(16) 0.0364(6) Uani 1 1 d . . . H40 H 0.5073 0.4266 0.6957 0.044 Uiso 1 1 calc R . . C41 C 0.3519(3) 0.5143(4) 0.6839(3) 0.0711(13) Uani 1 1 d . . . H41A H 0.3221 0.4660 0.7220 0.107 Uiso 0.50 1 calc PR . . H41B H 0.3423 0.5040 0.6386 0.107 Uiso 0.50 1 calc PR . . H41C H 0.3140 0.5838 0.6829 0.107 Uiso 0.50 1 calc PR . . H41D H 0.3301 0.5698 0.6403 0.107 Uiso 0.50 1 calc PR . . H41E H 0.3100 0.5319 0.7237 0.107 Uiso 0.50 1 calc PR . . H41F H 0.3383 0.4521 0.6795 0.107 Uiso 0.50 1 calc PR . . C42 C 0.4892(5) 0.5038(5) 0.7686(2) 0.0792(16) Uani 1 1 d . . . H42A H 0.4542 0.4572 0.8045 0.119 Uiso 0.50 1 calc PR . . H42B H 0.4579 0.5734 0.7703 0.119 Uiso 0.50 1 calc PR . . H42C H 0.5671 0.4851 0.7778 0.119 Uiso 0.50 1 calc PR . . H42D H 0.5320 0.5533 0.7639 0.119 Uiso 0.50 1 calc PR . . H42E H 0.5282 0.4370 0.7981 0.119 Uiso 0.50 1 calc PR . . H42F H 0.4191 0.5254 0.7906 0.119 Uiso 0.50 1 calc PR . . C43 C 0.7014(2) 0.1836(2) 0.62708(14) 0.0286(5) Uani 1 1 d . . . C44 C 0.7783(2) 0.1462(2) 0.58162(15) 0.0327(6) Uani 1 1 d . . . C45 C 0.7697(3) 0.0584(2) 0.56758(17) 0.0412(7) Uani 1 1 d . . . H45 H 0.8211 0.0308 0.5370 0.049 Uiso 1 1 calc R . . C46 C 0.6886(3) 0.0115(3) 0.59717(19) 0.0470(8) Uani 1 1 d . . . H46 H 0.6839 -0.0476 0.5864 0.056 Uiso 1 1 calc R . . C47 C 0.6139(3) 0.0495(3) 0.64227(19) 0.0478(8) Uani 1 1 d . . . H47 H 0.5586 0.0159 0.6627 0.057 Uiso 1 1 calc R . . C48 C 0.6183(3) 0.1369(2) 0.65845(16) 0.0376(6) Uani 1 1 d . . . C49 C 0.8648(2) 0.2000(2) 0.54580(16) 0.0363(6) Uani 1 1 d . . . H49 H 0.8700 0.2477 0.5722 0.044 Uiso 1 1 calc R . . C50 C 0.9765(3) 0.1278(3) 0.5469(3) 0.0571(9) Uani 1 1 d . . . H50A H 1.0289 0.1667 0.5231 0.086 Uiso 0.50 1 calc PR . . H50B H 0.9736 0.0788 0.5224 0.086 Uiso 0.50 1 calc PR . . H50C H 0.9987 0.0916 0.5959 0.086 Uiso 0.50 1 calc PR . . H50D H 0.9719 0.0580 0.5712 0.086 Uiso 0.50 1 calc PR . . H50E H 1.0272 0.1460 0.5719 0.086 Uiso 0.50 1 calc PR . . H50F H 1.0021 0.1331 0.4984 0.086 Uiso 0.50 1 calc PR . . C51 C 0.8303(4) 0.2636(3) 0.47061(19) 0.0563(9) Uani 1 1 d . . . H51A H 0.8864 0.2985 0.4477 0.084 Uiso 0.50 1 calc PR . . H51B H 0.7620 0.3140 0.4718 0.084 Uiso 0.50 1 calc PR . . H51C H 0.8205 0.2193 0.4440 0.084 Uiso 0.50 1 calc PR . . H51D H 0.7595 0.2560 0.4613 0.084 Uiso 0.50 1 calc PR . . H51E H 0.8840 0.2405 0.4372 0.084 Uiso 0.50 1 calc PR . . H51F H 0.8255 0.3352 0.4650 0.084 Uiso 0.50 1 calc PR . . C52 C 0.5338(3) 0.1796(3) 0.7068(2) 0.0505(8) Uani 1 1 d . . . H52 H 0.5632 0.2270 0.7233 0.061 Uiso 1 1 calc R . . C53 C 0.5103(4) 0.0976(4) 0.7722(2) 0.0668(12) Uani 1 1 d . . . H53A H 0.4556 0.1291 0.8015 0.100 Uiso 0.50 1 calc PR . . H53B H 0.5771 0.0624 0.7993 0.100 Uiso 0.50 1 calc PR . . H53C H 0.4832 0.0488 0.7577 0.100 Uiso 0.50 1 calc PR . . H53D H 0.5550 0.0311 0.7708 0.100 Uiso 0.50 1 calc PR . . H53E H 0.4335 0.0978 0.7730 0.100 Uiso 0.50 1 calc PR . . H53F H 0.5274 0.1114 0.8146 0.100 Uiso 0.50 1 calc PR . . C54 C 0.4301(4) 0.2417(4) 0.6658(3) 0.0693(11) Uani 1 1 d . . . H54A H 0.3763 0.2691 0.6975 0.104 Uiso 0.50 1 calc PR . . H54B H 0.4013 0.1980 0.6468 0.104 Uiso 0.50 1 calc PR . . H54C H 0.4463 0.2978 0.6269 0.104 Uiso 0.50 1 calc PR . . H54D H 0.4396 0.2409 0.6166 0.104 Uiso 0.50 1 calc PR . . H54E H 0.4146 0.3119 0.6673 0.104 Uiso 0.50 1 calc PR . . H54F H 0.3697 0.2121 0.6872 0.104 Uiso 0.50 1 calc PR . . C55 C 0.8758(2) 0.5708(2) 0.72302(13) 0.0277(5) Uani 1 1 d . . . C56 C 0.9861(2) 0.5705(2) 0.70882(14) 0.0328(6) Uani 1 1 d . . . C57 C 1.0221(2) 0.6577(2) 0.69608(14) 0.0363(6) Uani 1 1 d . . . H58 H 1.0972 0.6540 0.6879 0.044 Uiso 1 1 calc R . . C59 C 0.9512(3) 0.7510(2) 0.69490(15) 0.0386(7) Uani 1 1 d . . . C60 C 0.8422(3) 0.7528(2) 0.70763(15) 0.0365(6) Uani 1 1 d . . . H60 H 0.7917 0.8152 0.7067 0.044 Uiso 1 1 calc R . . C61 C 0.8050(2) 0.6650(2) 0.72179(13) 0.0297(5) Uani 1 1 d . . . C62 C 1.0683(2) 0.4734(3) 0.70666(18) 0.0434(7) Uani 1 1 d . . . H62A H 1.0318 0.4181 0.7166 0.065 Uiso 0.50 1 calc PR . . H62B H 1.1241 0.4561 0.7423 0.065 Uiso 0.50 1 calc PR . . H62C H 1.1021 0.4831 0.6597 0.065 Uiso 0.50 1 calc PR . . H62D H 1.1402 0.4868 0.6958 0.065 Uiso 0.50 1 calc PR . . H62E H 1.0479 0.4488 0.6701 0.065 Uiso 0.50 1 calc PR . . H62F H 1.0699 0.4218 0.7527 0.065 Uiso 0.50 1 calc PR . . C63 C 0.9900(4) 0.8460(3) 0.6806(2) 0.0560(9) Uani 1 1 d . . . H63A H 1.0686 0.8304 0.6729 0.084 Uiso 0.50 1 calc PR . . H63B H 0.9726 0.8725 0.7212 0.084 Uiso 0.50 1 calc PR . . H63C H 0.9540 0.8971 0.6385 0.084 Uiso 0.50 1 calc PR . . H63D H 0.9282 0.9029 0.6822 0.084 Uiso 0.50 1 calc PR . . H63E H 1.0242 0.8609 0.6338 0.084 Uiso 0.50 1 calc PR . . H63F H 1.0428 0.8362 0.7166 0.084 Uiso 0.50 1 calc PR . . C64 C 0.6856(2) 0.6736(2) 0.73586(17) 0.0380(6) Uani 1 1 d . . . H64A H 0.6487 0.7441 0.7330 0.057 Uiso 0.50 1 calc PR . . H64B H 0.6751 0.6292 0.7831 0.057 Uiso 0.50 1 calc PR . . H64C H 0.6554 0.6532 0.7006 0.057 Uiso 0.50 1 calc PR . . H64D H 0.6708 0.6069 0.7449 0.057 Uiso 0.50 1 calc PR . . H64E H 0.6443 0.7218 0.6947 0.057 Uiso 0.50 1 calc PR . . H64F H 0.6640 0.6978 0.7772 0.057 Uiso 0.50 1 calc PR . . C1H C 0.4497(11) 0.8278(7) 0.8353(6) 0.172(6) Uani 1 1 d . . . H1H1 H 0.5056 0.7834 0.8697 0.258 Uiso 0.50 1 calc PR . . H1H2 H 0.3893 0.8626 0.8595 0.258 Uiso 0.50 1 calc PR . . H1H3 H 0.4805 0.8781 0.7997 0.258 Uiso 0.50 1 calc PR . . H1H4 H 0.4114 0.8993 0.8163 0.258 Uiso 0.50 1 calc PR . . H1H5 H 0.5277 0.8202 0.8264 0.258 Uiso 0.50 1 calc PR . . H1H6 H 0.4364 0.8046 0.8863 0.258 Uiso 0.50 1 calc PR . . C2H C 0.4082(6) 0.7630(7) 0.7988(6) 0.150(4) Uani 1 1 d D . . H2H1 H 0.3768 0.7128 0.8353 0.180 Uiso 1 1 calc R . . H2H2 H 0.4708 0.7247 0.7774 0.180 Uiso 1 1 calc R . . C3H C 0.3121(7) 0.8316(7) 0.7343(6) 0.170(6) Uani 1 1 d D . . H3H1 H 0.2951 0.7872 0.7094 0.204 Uiso 1 1 calc R . . H3H2 H 0.2445 0.8643 0.7549 0.204 Uiso 1 1 calc R . . C4H C 0.3618(5) 0.9060(5) 0.6875(5) 0.114(3) Uani 1 1 d D . . H4H1 H 0.4353 0.8753 0.6726 0.136 Uiso 1 1 calc R . . H4H2 H 0.3649 0.9599 0.7081 0.136 Uiso 1 1 calc R . . C5H C 0.2748(5) 0.9475(5) 0.6231(3) 0.0922(17) Uani 1 1 d D . . H5H1 H 0.2835 0.8977 0.5965 0.111 Uiso 1 1 calc R . . H5H2 H 0.1994 0.9617 0.6411 0.111 Uiso 1 1 calc R . . C6H C 0.3026(7) 1.0418(6) 0.5786(5) 0.124(3) Uani 1 1 d . . . H6H1 H 0.2540 1.0731 0.5380 0.186 Uiso 0.50 1 calc PR . . H6H2 H 0.3777 1.0257 0.5620 0.186 Uiso 0.50 1 calc PR . . H6H3 H 0.2946 1.0892 0.6064 0.186 Uiso 0.50 1 calc PR . . H6H4 H 0.3636 1.0522 0.5996 0.186 Uiso 0.50 1 calc PR . . H6H5 H 0.2398 1.0996 0.5756 0.186 Uiso 0.50 1 calc PR . . H6H6 H 0.3229 1.0362 0.5312 0.186 Uiso 0.50 1 calc PR . . O1S O 0.5689(17) 0.4291(14) 0.9994(18) 0.251(16) Uani 0.50 1 d PD . . C1S C 0.5696(18) 0.5344(15) 0.9620(10) 0.116(6) Uani 0.50 1 d PD . . H1S1 H 0.5472 0.5511 0.9125 0.139 Uiso 0.50 1 calc PR . . H1S2 H 0.6441 0.5430 0.9616 0.139 Uiso 0.50 1 calc PR . . C2S C 0.507(2) 0.3934(11) 1.0029(11) 0.132(7) Uani 0.50 1 d PD . . H2S1 H 0.4693 0.3812 0.9661 0.159 Uiso 0.50 1 calc PR . . H2S2 H 0.5389 0.3276 1.0379 0.159 Uiso 0.50 1 calc PR . . C3S C 0.5935(13) 0.4536(19) 0.9703(16) 0.177(14) Uani 0.50 1 d PD . . H3S1 H 0.6106 0.4536 0.9208 0.212 Uiso 0.50 1 calc PR . . H3S2 H 0.6611 0.4254 0.9982 0.212 Uiso 0.50 1 calc PR . . C4S C 0.465(2) 0.4373(19) 1.025(3) 0.27(3) Uani 0.50 1 d PD . . H4S1 H 0.4670 0.3883 1.0733 0.323 Uiso 0.50 1 calc PR . . H4S2 H 0.4222 0.4182 0.9951 0.323 Uiso 0.50 1 calc PR . . 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 K1 0.0790(8) 0.0267(4) 0.0679(7) 0.0132(4) -0.0273(6) -0.0162(5) K2 0.0644(7) 0.0719(7) 0.0465(6) -0.0179(5) -0.0387(5) 0.0124(6) Fe1 0.0281(2) 0.0235(2) 0.0198(2) -0.00053(15) -0.00931(14) -0.00857(15) N1 0.0307(10) 0.0272(10) 0.0194(10) -0.0008(8) -0.0069(8) -0.0096(9) N2 0.0304(10) 0.0231(10) 0.0213(10) -0.0028(8) -0.0074(8) -0.0085(8) C1 0.0325(12) 0.0278(12) 0.0212(12) -0.0013(10) -0.0074(10) -0.0080(10) C2 0.0357(13) 0.0226(11) 0.0219(12) 0.0003(10) -0.0089(10) -0.0086(10) C3 0.0326(12) 0.0218(11) 0.0249(12) -0.0008(10) -0.0088(10) -0.0072(10) C4 0.0353(13) 0.0321(13) 0.0199(12) -0.0027(10) -0.0074(10) -0.0127(11) C5 0.0373(14) 0.0331(13) 0.0234(12) -0.0035(10) -0.0043(11) -0.0124(11) C6 0.0468(17) 0.0555(18) 0.0241(13) -0.0130(13) -0.0025(12) -0.0156(14) C7 0.0469(18) 0.088(3) 0.0322(16) -0.0232(17) -0.0105(14) -0.0228(18) C8 0.0343(15) 0.085(3) 0.0408(17) -0.0251(17) -0.0059(13) -0.0188(16) C9 0.0377(15) 0.0511(17) 0.0281(14) -0.0106(12) -0.0047(12) -0.0158(13) C10 0.0372(14) 0.0384(15) 0.0302(14) -0.0092(12) -0.0023(11) -0.0109(12) C11 0.055(2) 0.061(2) 0.097(4) 0.012(2) 0.014(2) -0.023(2) C12 0.0446(19) 0.067(3) 0.100(3) -0.046(3) 0.001(2) -0.0050(18) C13 0.0347(14) 0.063(2) 0.0349(15) -0.0178(14) -0.0013(12) -0.0143(14) C14 0.075(3) 0.056(2) 0.045(2) -0.0120(17) 0.0180(18) -0.0062(19) C15 0.091(3) 0.054(2) 0.050(2) -0.0115(18) 0.018(2) -0.009(2) C16 0.0382(14) 0.0235(12) 0.0242(12) -0.0024(10) -0.0117(10) -0.0092(10) C17 0.0417(15) 0.0298(13) 0.0294(13) 0.0015(11) -0.0133(11) -0.0133(12) C18 0.0558(19) 0.0394(16) 0.0511(19) -0.0022(14) -0.0143(16) -0.0266(15) C19 0.073(2) 0.0325(15) 0.063(2) -0.0165(15) -0.0193(19) -0.0174(16) C20 0.0548(19) 0.0345(15) 0.0536(19) -0.0195(14) -0.0139(16) -0.0059(14) C21 0.0431(15) 0.0282(13) 0.0327(14) -0.0061(11) -0.0146(12) -0.0039(12) C22 0.0417(16) 0.0448(16) 0.0402(16) -0.0063(13) -0.0035(13) -0.0203(13) C23 0.040(2) 0.176(7) 0.115(5) -0.093(5) -0.009(3) -0.001(3) C24 0.145(6) 0.077(3) 0.045(2) -0.007(2) 0.010(3) -0.001(3) C25 0.0382(15) 0.0410(16) 0.0423(17) -0.0189(13) -0.0040(13) -0.0027(13) C26 0.062(2) 0.094(3) 0.046(2) -0.023(2) 0.0036(17) -0.023(2) C27 0.0444(19) 0.064(2) 0.081(3) -0.020(2) -0.012(2) 0.0018(18) N3 0.0245(10) 0.0296(11) 0.0207(10) -0.0042(8) -0.0073(8) -0.0069(8) N4 0.0280(10) 0.0298(11) 0.0219(10) -0.0057(8) -0.0059(8) -0.0101(9) C28 0.0275(12) 0.0327(13) 0.0270(12) -0.0063(10) -0.0072(10) -0.0082(10) C29 0.0262(11) 0.0310(12) 0.0193(11) -0.0017(10) -0.0066(9) -0.0090(10) C30 0.0297(12) 0.0307(13) 0.0222(12) -0.0022(10) -0.0090(10) -0.0083(10) C31 0.0296(12) 0.0307(13) 0.0209(11) -0.0050(10) -0.0090(10) -0.0082(10) C32 0.0366(14) 0.0330(14) 0.0205(12) -0.0007(10) -0.0079(10) -0.0090(11) C33 0.0490(17) 0.0317(14) 0.0366(15) 0.0019(12) -0.0019(13) -0.0078(13) C34 0.0509(18) 0.0329(15) 0.0488(19) 0.0001(13) -0.0090(15) -0.0022(14) C35 0.0334(14) 0.0382(15) 0.0449(17) -0.0111(13) -0.0074(13) 0.0008(12) C36 0.0309(13) 0.0324(13) 0.0306(13) -0.0087(11) -0.0079(11) -0.0080(11) C37 0.0359(14) 0.0394(15) 0.0310(14) 0.0017(12) -0.0032(11) -0.0096(12) C38 0.0499(19) 0.065(2) 0.051(2) -0.0226(18) 0.0084(16) -0.0124(17) C39 0.0447(17) 0.056(2) 0.0404(17) -0.0013(15) 0.0013(14) -0.0210(15) C40 0.0303(14) 0.0416(15) 0.0381(15) -0.0106(12) 0.0002(11) -0.0121(12) C41 0.043(2) 0.094(3) 0.069(3) 0.001(2) -0.0055(18) -0.033(2) C42 0.105(4) 0.117(4) 0.0354(19) -0.011(2) 0.008(2) -0.078(3) C43 0.0335(13) 0.0295(13) 0.0234(12) -0.0045(10) -0.0085(10) -0.0105(10) C44 0.0383(14) 0.0314(13) 0.0279(13) -0.0065(11) -0.0072(11) -0.0085(11) C45 0.0493(17) 0.0381(15) 0.0416(16) -0.0175(13) -0.0007(13) -0.0131(13) C46 0.062(2) 0.0411(16) 0.0470(18) -0.0167(14) -0.0043(16) -0.0238(15) C47 0.0580(19) 0.0496(18) 0.0474(18) -0.0149(15) 0.0000(15) -0.0326(16) C48 0.0429(15) 0.0424(16) 0.0328(14) -0.0087(12) -0.0036(12) -0.0213(13) C49 0.0408(15) 0.0365(14) 0.0354(15) -0.0139(12) 0.0027(12) -0.0133(12) C50 0.0389(17) 0.052(2) 0.083(3) -0.0244(19) 0.0078(17) -0.0144(15) C51 0.072(2) 0.061(2) 0.0359(17) -0.0078(16) 0.0041(16) -0.0262(19) C52 0.0479(18) 0.070(2) 0.0497(19) -0.0287(17) 0.0098(15) -0.0332(17) C53 0.071(3) 0.102(3) 0.047(2) -0.028(2) 0.0139(18) -0.051(3) C54 0.054(2) 0.081(3) 0.075(3) -0.031(2) 0.008(2) -0.014(2) C55 0.0338(13) 0.0317(13) 0.0166(11) 0.0010(9) -0.0063(9) -0.0144(11) C56 0.0379(14) 0.0365(14) 0.0212(12) -0.0017(10) -0.0046(10) -0.0117(12) C57 0.0417(15) 0.0459(16) 0.0225(12) -0.0016(11) 0.0002(11) -0.0235(13) C59 0.0559(18) 0.0392(15) 0.0238(13) -0.0004(11) -0.0035(12) -0.0267(14) C60 0.0541(17) 0.0281(13) 0.0258(13) -0.0037(10) -0.0079(12) -0.0105(12) C61 0.0381(14) 0.0315(13) 0.0192(11) -0.0028(10) -0.0071(10) -0.0118(11) C62 0.0331(14) 0.0459(17) 0.0458(17) -0.0083(14) 0.0066(13) -0.0095(13) C63 0.082(3) 0.0488(19) 0.0463(19) -0.0068(15) -0.0006(18) -0.0406(19) C64 0.0349(14) 0.0388(15) 0.0399(15) -0.0119(12) -0.0102(12) -0.0049(12) C1H 0.233(13) 0.087(5) 0.142(8) -0.016(5) 0.091(9) -0.001(7) C2H 0.084(5) 0.115(6) 0.193(11) 0.006(7) 0.029(6) 0.004(4) C3H 0.156(8) 0.152(8) 0.280(14) -0.158(9) 0.145(9) -0.105(7) C4H 0.090(4) 0.094(4) 0.173(8) -0.069(5) 0.047(5) -0.029(4) C5H 0.085(3) 0.113(5) 0.069(3) -0.029(3) -0.001(3) -0.005(3) C6H 0.143(7) 0.110(5) 0.156(8) -0.069(5) 0.004(6) -0.061(5) O1S 0.22(2) 0.27(3) 0.38(4) -0.20(3) 0.12(2) -0.17(2) C1S 0.138(16) 0.099(12) 0.101(10) -0.033(9) 0.027(10) -0.016(12) C2S 0.167(17) 0.102(11) 0.159(16) -0.071(11) 0.063(14) -0.069(12) C3S 0.109(14) 0.14(2) 0.24(3) -0.02(2) -0.056(19) 0.020(15) C4S 0.18(3) 0.21(3) 0.52(8) -0.25(5) 0.14(4) -0.08(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 K1 C1 2.811(3) 2_757 ? K1 C1 2.811(3) . ? K1 C16 3.171(2) . ? K1 C16 3.171(2) 2_757 ? K1 C17 3.381(3) . ? K1 C17 3.381(3) 2_757 ? K1 N2 3.443(2) . ? K1 N2 3.443(2) 2_757 ? K1 C21 3.488(3) . ? K1 C21 3.488(3) 2_757 ? K2 C28 2.824(3) 2_666 ? K2 C28 2.824(3) . ? K2 C31 3.203(2) 2_666 ? K2 C31 3.203(2) . ? K2 C36 3.287(3) 2_666 ? K2 C36 3.287(3) . ? Fe1 C29 2.064(2) . ? Fe1 C55 2.065(3) . ? Fe1 C3 2.071(2) . ? N1 C1 1.354(4) . ? N1 C2 1.400(3) . ? N1 C4 1.445(3) . ? N2 C1 1.359(3) . ? N2 C3 1.406(3) . ? N2 C16 1.440(3) . ? C2 C3 1.359(4) . ? C2 H2 0.9500 . ? C4 C9 1.396(4) . ? C4 C5 1.399(4) . ? C5 C6 1.395(4) . ? C5 C10 1.517(4) . ? C6 C7 1.379(5) . ? C6 H6 0.9500 . ? C7 C8 1.377(5) . ? C7 H7 0.9500 . ? C8 C9 1.392(4) . ? C8 H8 0.9500 . ? C9 C13 1.518(5) . ? C10 C12 1.519(5) . ? C10 C11 1.526(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? C13 C14 1.513(5) . ? C13 C15 1.523(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 H15D 0.9800 . ? C15 H15E 0.9800 . ? C15 H15F 0.9800 . ? C16 C21 1.395(5) . ? C16 C17 1.401(4) . ? C17 C18 1.396(4) . ? C17 C22 1.520(5) . ? C18 C19 1.375(6) . ? C18 H18 0.9500 . ? C19 C20 1.388(6) . ? C19 H19 0.9500 . ? C20 C21 1.394(4) . ? C20 H20 0.9500 . ? C21 C25 1.516(5) . ? C22 C23 1.493(5) . ? C22 C24 1.495(6) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23D 0.9800 . ? C23 H23E 0.9800 . ? C23 H23F 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? C25 C26 1.530(5) . ? C25 C27 1.532(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? N3 C28 1.372(3) . ? N3 C29 1.416(3) . ? N3 C31 1.432(3) . ? N4 C28 1.350(4) . ? N4 C30 1.403(3) . ? N4 C43 1.445(3) . ? C29 C30 1.369(4) . ? C30 H30 0.9500 . ? C31 C36 1.404(4) . ? C31 C32 1.409(4) . ? C32 C33 1.396(4) . ? C32 C37 1.521(4) . ? C33 C34 1.385(5) . ? C33 H33 0.9500 . ? C34 C35 1.369(5) . ? C34 H34 0.9500 . ? C35 C36 1.404(4) . ? C35 H35 0.9500 . ? C36 C40 1.524(4) . ? C37 C38 1.518(5) . ? C37 C39 1.528(5) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C38 H38D 0.9800 . ? C38 H38E 0.9800 . ? C38 H38F 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C39 H39D 0.9800 . ? C39 H39E 0.9800 . ? C39 H39F 0.9800 . ? C40 C41 1.508(4) . ? C40 C42 1.512(5) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41 H41D 0.9800 . ? C41 H41E 0.9800 . ? C41 H41F 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C42 H42D 0.9800 . ? C42 H42E 0.9800 . ? C42 H42F 0.9800 . ? C43 C44 1.394(4) . ? C43 C48 1.400(4) . ? C44 C45 1.399(4) . ? C44 C49 1.515(4) . ? C45 C46 1.374(5) . ? C45 H45 0.9500 . ? C46 C47 1.376(6) . ? C46 H46 0.9500 . ? C47 C48 1.399(5) . ? C47 H47 0.9500 . ? C48 C52 1.518(5) . ? C49 C50 1.524(5) . ? C49 C51 1.525(5) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C50 H50D 0.9800 . ? C50 H50E 0.9800 . ? C50 H50F 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C51 H51D 0.9800 . ? C51 H51E 0.9800 . ? C51 H51F 0.9800 . ? C52 C53 1.527(6) . ? C52 C54 1.528(6) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C53 H53D 0.9800 . ? C53 H53E 0.9800 . ? C53 H53F 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C54 H54D 0.9800 . ? C54 H54E 0.9800 . ? C54 H54F 0.9800 . ? C55 C61 1.406(4) . ? C55 C56 1.413(4) . ? C56 C57 1.384(4) . ? C56 C62 1.515(4) . ? C57 C59 1.396(5) . ? C57 H58 0.9500 . ? C59 C60 1.390(5) . ? C59 C63 1.503(4) . ? C60 C61 1.396(4) . ? C60 H60 0.9500 . ? C61 C64 1.507(4) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C62 H62D 0.9800 . ? C62 H62E 0.9800 . ? C62 H62F 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C63 H63D 0.9800 . ? C63 H63E 0.9800 . ? C63 H63F 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C64 H64D 0.9800 . ? C64 H64E 0.9800 . ? C64 H64F 0.9800 . ? C1H C2H 1.552(15) . ? C1H H1H1 0.9800 . ? C1H H1H2 0.9800 . ? C1H H1H3 0.9800 . ? C1H H1H4 0.9800 . ? C1H H1H5 0.9800 . ? C1H H1H6 0.9800 . ? C2H C3H 1.727(13) . ? C2H H2H1 0.9900 . ? C2H H2H2 0.9900 . ? C3H C4H 1.429(10) . ? C3H H3H1 0.9900 . ? C3H H3H2 0.9900 . ? C4H C5H 1.633(9) . ? C4H H4H1 0.9900 . ? C4H H4H2 0.9900 . ? C5H C6H 1.479(10) . ? C5H H5H1 0.9900 . ? C5H H5H2 0.9900 . ? C6H H6H1 0.9800 . ? C6H H6H2 0.9800 . ? C6H H6H3 0.9800 . ? C6H H6H4 0.9800 . ? C6H H6H5 0.9800 . ? C6H H6H6 0.9800 . ? O1S C4S 1.372(17) . ? O1S C1S 1.459(17) . ? O1S C4S 1.76(3) 2_667 ? O1S C1S 1.88(3) 2_667 ? C1S C2S 1.518(15) 2_667 ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S C1S 1.518(15) 2_667 ? C2S C3S 1.558(17) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.569(16) 2_667 ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C3S 1.569(16) 2_667 ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? 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 C1 K1 C1 180.00(11) 2_757 . ? C1 K1 C16 133.15(7) 2_757 . ? C1 K1 C16 46.85(7) . . ? C1 K1 C16 46.85(7) 2_757 2_757 ? C1 K1 C16 133.15(7) . 2_757 ? C16 K1 C16 180.00(7) . 2_757 ? C1 K1 C17 117.06(7) 2_757 . ? C1 K1 C17 62.94(7) . . ? C16 K1 C17 24.42(7) . . ? C16 K1 C17 155.58(7) 2_757 . ? C1 K1 C17 62.94(7) 2_757 2_757 ? C1 K1 C17 117.06(7) . 2_757 ? C16 K1 C17 155.58(7) . 2_757 ? C16 K1 C17 24.42(7) 2_757 2_757 ? C17 K1 C17 180.000(1) . 2_757 ? C1 K1 N2 157.69(6) 2_757 . ? C1 K1 N2 22.31(6) . . ? C16 K1 N2 24.71(6) . . ? C16 K1 N2 155.29(6) 2_757 . ? C17 K1 N2 41.96(6) . . ? C17 K1 N2 138.04(6) 2_757 . ? C1 K1 N2 22.31(6) 2_757 2_757 ? C1 K1 N2 157.69(6) . 2_757 ? C16 K1 N2 155.29(6) . 2_757 ? C16 K1 N2 24.71(6) 2_757 2_757 ? C17 K1 N2 138.04(6) . 2_757 ? C17 K1 N2 41.96(6) 2_757 2_757 ? N2 K1 N2 180.0 . 2_757 ? C1 K1 C21 120.71(7) 2_757 . ? C1 K1 C21 59.29(7) . . ? C16 K1 C21 23.57(8) . . ? C16 K1 C21 156.43(8) 2_757 . ? C17 K1 C21 41.82(7) . . ? C17 K1 C21 138.18(8) 2_757 . ? N2 K1 C21 41.12(6) . . ? N2 K1 C21 138.88(6) 2_757 . ? C1 K1 C21 59.29(7) 2_757 2_757 ? C1 K1 C21 120.71(7) . 2_757 ? C16 K1 C21 156.43(8) . 2_757 ? C16 K1 C21 23.57(8) 2_757 2_757 ? C17 K1 C21 138.18(8) . 2_757 ? C17 K1 C21 41.82(7) 2_757 2_757 ? N2 K1 C21 138.88(6) . 2_757 ? N2 K1 C21 41.12(6) 2_757 2_757 ? C21 K1 C21 180.0 . 2_757 ? C28 K2 C28 180.00(9) 2_666 . ? C28 K2 C31 46.56(7) 2_666 2_666 ? C28 K2 C31 133.44(7) . 2_666 ? C28 K2 C31 133.44(7) 2_666 . ? C28 K2 C31 46.56(7) . . ? C31 K2 C31 180.000(1) 2_666 . ? C28 K2 C36 61.12(7) 2_666 2_666 ? C28 K2 C36 118.88(7) . 2_666 ? C31 K2 C36 24.94(7) 2_666 2_666 ? C31 K2 C36 155.06(7) . 2_666 ? C28 K2 C36 118.88(7) 2_666 . ? C28 K2 C36 61.12(7) . . ? C31 K2 C36 155.06(7) 2_666 . ? C31 K2 C36 24.94(7) . . ? C36 K2 C36 180.000(1) 2_666 . ? C29 Fe1 C55 128.36(10) . . ? C29 Fe1 C3 122.47(10) . . ? C55 Fe1 C3 108.38(10) . . ? C1 N1 C2 112.0(2) . . ? C1 N1 C4 123.4(2) . . ? C2 N1 C4 124.6(2) . . ? C1 N2 C3 115.7(2) . . ? C1 N2 C16 118.1(2) . . ? C3 N2 C16 126.0(2) . . ? C1 N2 K1 51.74(13) . . ? C3 N2 K1 166.44(16) . . ? C16 N2 K1 67.03(13) . . ? N1 C1 N2 101.6(2) . . ? N1 C1 K1 151.76(17) . . ? N2 C1 K1 105.95(16) . . ? C3 C2 N1 108.7(2) . . ? C3 C2 H2 125.7 . . ? N1 C2 H2 125.7 . . ? C2 C3 N2 102.0(2) . . ? C2 C3 Fe1 125.17(19) . . ? N2 C3 Fe1 132.42(18) . . ? C9 C4 C5 122.6(2) . . ? C9 C4 N1 118.5(2) . . ? C5 C4 N1 118.9(2) . . ? C6 C5 C4 117.9(3) . . ? C6 C5 C10 120.9(3) . . ? C4 C5 C10 121.1(2) . . ? C7 C6 C5 120.2(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 120.9(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 121.0(3) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C4 117.3(3) . . ? C8 C9 C13 120.3(3) . . ? C4 C9 C13 122.4(2) . . ? C5 C10 C12 112.7(3) . . ? C5 C10 C11 108.9(3) . . ? C12 C10 C11 110.7(4) . . ? C5 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.3 . . ? C10 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? C10 C11 H11F 109.5 . . ? H11A C11 H11F 56.3 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C12 H12D 109.5 . . ? H12A C12 H12D 141.1 . . ? H12B C12 H12D 56.3 . . ? H12C C12 H12D 56.3 . . ? C10 C12 H12E 109.5 . . ? H12A C12 H12E 56.3 . . ? H12B C12 H12E 141.1 . . ? H12C C12 H12E 56.3 . . ? H12D C12 H12E 109.5 . . ? C10 C12 H12F 109.5 . . ? H12A C12 H12F 56.3 . . ? H12B C12 H12F 56.3 . . ? H12C C12 H12F 141.1 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? C14 C13 C9 112.0(3) . . ? C14 C13 C15 110.0(3) . . ? C9 C13 C15 110.5(3) . . ? C14 C13 H13 108.1 . . ? C9 C13 H13 108.1 . . ? C15 C13 H13 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14A C14 H14D 141.1 . . ? H14B C14 H14D 56.3 . . ? H14C C14 H14D 56.3 . . ? C13 C14 H14E 109.5 . . ? H14A C14 H14E 56.3 . . ? H14B C14 H14E 141.1 . . ? H14C C14 H14E 56.3 . . ? H14D C14 H14E 109.5 . . ? C13 C14 H14F 109.5 . . ? H14A C14 H14F 56.3 . . ? H14B C14 H14F 56.3 . . ? H14C C14 H14F 141.1 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C15 H15D 109.5 . . ? H15A C15 H15D 141.1 . . ? H15B C15 H15D 56.3 . . ? H15C C15 H15D 56.3 . . ? C13 C15 H15E 109.5 . . ? H15A C15 H15E 56.3 . . ? H15B C15 H15E 141.1 . . ? H15C C15 H15E 56.3 . . ? H15D C15 H15E 109.5 . . ? C13 C15 H15F 109.5 . . ? H15A C15 H15F 56.3 . . ? H15B C15 H15F 56.3 . . ? H15C C15 H15F 141.1 . . ? H15D C15 H15F 109.5 . . ? H15E C15 H15F 109.5 . . ? C21 C16 C17 122.7(3) . . ? C21 C16 N2 118.4(2) . . ? C17 C16 N2 118.7(3) . . ? C21 C16 K1 91.07(16) . . ? C17 C16 K1 86.21(15) . . ? N2 C16 K1 88.26(13) . . ? C18 C17 C16 116.8(3) . . ? C18 C17 C22 122.0(3) . . ? C16 C17 C22 121.3(3) . . ? C18 C17 K1 94.72(18) . . ? C16 C17 K1 69.36(14) . . ? C22 C17 K1 104.83(17) . . ? C19 C18 C17 121.9(3) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 120.9(3) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C16 117.8(3) . . ? C20 C21 C25 120.4(3) . . ? C16 C21 C25 121.8(3) . . ? C20 C21 K1 95.4(2) . . ? C16 C21 K1 65.36(15) . . ? C25 C21 K1 109.38(17) . . ? C23 C22 C24 112.3(5) . . ? C23 C22 C17 112.2(3) . . ? C24 C22 C17 112.0(3) . . ? C23 C22 H22 106.6 . . ? C24 C22 H22 106.6 . . ? C17 C22 H22 106.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C23 H23D 109.5 . . ? H23A C23 H23D 141.1 . . ? H23B C23 H23D 56.3 . . ? H23C C23 H23D 56.3 . . ? C22 C23 H23E 109.5 . . ? H23A C23 H23E 56.3 . . ? H23B C23 H23E 141.1 . . ? H23C C23 H23E 56.3 . . ? H23D C23 H23E 109.5 . . ? C22 C23 H23F 109.5 . . ? H23A C23 H23F 56.3 . . ? H23B C23 H23F 56.3 . . ? H23C C23 H23F 141.1 . . ? H23D C23 H23F 109.5 . . ? H23E C23 H23F 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C24 H24D 109.5 . . ? H24A C24 H24D 141.1 . . ? H24B C24 H24D 56.3 . . ? H24C C24 H24D 56.3 . . ? C22 C24 H24E 109.5 . . ? H24A C24 H24E 56.3 . . ? H24B C24 H24E 141.1 . . ? H24C C24 H24E 56.3 . . ? H24D C24 H24E 109.5 . . ? C22 C24 H24F 109.5 . . ? H24A C24 H24F 56.3 . . ? H24B C24 H24F 56.3 . . ? H24C C24 H24F 141.1 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? C21 C25 C26 111.7(3) . . ? C21 C25 C27 111.5(3) . . ? C26 C25 C27 111.3(3) . . ? C21 C25 H25 107.3 . . ? C26 C25 H25 107.3 . . ? C27 C25 H25 107.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? C25 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? C25 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.3 . . ? C25 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.3 . . ? H27D C27 H27E 109.5 . . ? C25 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.3 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? C28 N3 C29 115.1(2) . . ? C28 N3 C31 118.3(2) . . ? C29 N3 C31 126.4(2) . . ? C28 N4 C30 111.8(2) . . ? C28 N4 C43 123.6(2) . . ? C30 N4 C43 124.5(2) . . ? N4 C28 N3 102.2(2) . . ? N4 C28 K2 151.18(18) . . ? N3 C28 K2 106.58(17) . . ? C30 C29 N3 101.8(2) . . ? C30 C29 Fe1 128.52(18) . . ? N3 C29 Fe1 129.36(19) . . ? C29 C30 N4 109.1(2) . . ? C29 C30 H30 125.5 . . ? N4 C30 H30 125.5 . . ? C36 C31 C32 122.2(3) . . ? C36 C31 N3 118.0(2) . . ? C32 C31 N3 119.6(2) . . ? C36 C31 K2 80.89(14) . . ? C32 C31 K2 96.09(15) . . ? N3 C31 K2 88.50(13) . . ? C33 C32 C31 117.3(3) . . ? C33 C32 C37 121.0(3) . . ? C31 C32 C37 121.6(2) . . ? C34 C33 C32 121.3(3) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C35 C34 C33 120.3(3) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 121.4(3) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C31 C36 C35 117.4(3) . . ? C31 C36 C40 121.7(2) . . ? C35 C36 C40 120.9(3) . . ? C31 C36 K2 74.17(14) . . ? C35 C36 K2 95.13(18) . . ? C40 C36 K2 101.38(16) . . ? C38 C37 C32 110.3(3) . . ? C38 C37 C39 111.2(3) . . ? C32 C37 C39 112.5(3) . . ? C38 C37 H37 107.5 . . ? C32 C37 H37 107.5 . . ? C39 C37 H37 107.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C38 H38D 109.5 . . ? H38A C38 H38D 141.1 . . ? H38B C38 H38D 56.3 . . ? H38C C38 H38D 56.3 . . ? C37 C38 H38E 109.5 . . ? H38A C38 H38E 56.3 . . ? H38B C38 H38E 141.1 . . ? H38C C38 H38E 56.3 . . ? H38D C38 H38E 109.5 . . ? C37 C38 H38F 109.5 . . ? H38A C38 H38F 56.3 . . ? H38B C38 H38F 56.3 . . ? H38C C38 H38F 141.1 . . ? H38D C38 H38F 109.5 . . ? H38E C38 H38F 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C39 H39D 109.5 . . ? H39A C39 H39D 141.1 . . ? H39B C39 H39D 56.3 . . ? H39C C39 H39D 56.3 . . ? C37 C39 H39E 109.5 . . ? H39A C39 H39E 56.3 . . ? H39B C39 H39E 141.1 . . ? H39C C39 H39E 56.3 . . ? H39D C39 H39E 109.5 . . ? C37 C39 H39F 109.5 . . ? H39A C39 H39F 56.3 . . ? H39B C39 H39F 56.3 . . ? H39C C39 H39F 141.1 . . ? H39D C39 H39F 109.5 . . ? H39E C39 H39F 109.5 . . ? C41 C40 C42 110.7(4) . . ? C41 C40 C36 113.5(3) . . ? C42 C40 C36 110.6(3) . . ? C41 C40 H40 107.2 . . ? C42 C40 H40 107.2 . . ? C36 C40 H40 107.2 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C41 H41D 109.5 . . ? H41A C41 H41D 141.1 . . ? H41B C41 H41D 56.3 . . ? H41C C41 H41D 56.3 . . ? C40 C41 H41E 109.5 . . ? H41A C41 H41E 56.3 . . ? H41B C41 H41E 141.1 . . ? H41C C41 H41E 56.3 . . ? H41D C41 H41E 109.5 . . ? C40 C41 H41F 109.5 . . ? H41A C41 H41F 56.3 . . ? H41B C41 H41F 56.3 . . ? H41C C41 H41F 141.1 . . ? H41D C41 H41F 109.5 . . ? H41E C41 H41F 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C42 H42D 109.5 . . ? H42A C42 H42D 141.1 . . ? H42B C42 H42D 56.3 . . ? H42C C42 H42D 56.3 . . ? C40 C42 H42E 109.5 . . ? H42A C42 H42E 56.3 . . ? H42B C42 H42E 141.1 . . ? H42C C42 H42E 56.3 . . ? H42D C42 H42E 109.5 . . ? C40 C42 H42F 109.5 . . ? H42A C42 H42F 56.3 . . ? H42B C42 H42F 56.3 . . ? H42C C42 H42F 141.1 . . ? H42D C42 H42F 109.5 . . ? H42E C42 H42F 109.5 . . ? C44 C43 C48 122.7(3) . . ? C44 C43 N4 118.8(2) . . ? C48 C43 N4 118.5(3) . . ? C43 C44 C45 117.2(3) . . ? C43 C44 C49 122.0(2) . . ? C45 C44 C49 120.7(3) . . ? C46 C45 C44 121.3(3) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C45 C46 C47 120.5(3) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C48 120.9(3) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C47 C48 C43 117.4(3) . . ? C47 C48 C52 120.4(3) . . ? C43 C48 C52 122.1(3) . . ? C44 C49 C50 113.1(3) . . ? C44 C49 C51 109.8(3) . . ? C50 C49 C51 111.3(3) . . ? C44 C49 H49 107.5 . . ? C50 C49 H49 107.5 . . ? C51 C49 H49 107.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C50 H50D 109.5 . . ? H50A C50 H50D 141.1 . . ? H50B C50 H50D 56.3 . . ? H50C C50 H50D 56.3 . . ? C49 C50 H50E 109.5 . . ? H50A C50 H50E 56.3 . . ? H50B C50 H50E 141.1 . . ? H50C C50 H50E 56.3 . . ? H50D C50 H50E 109.5 . . ? C49 C50 H50F 109.5 . . ? H50A C50 H50F 56.3 . . ? H50B C50 H50F 56.3 . . ? H50C C50 H50F 141.1 . . ? H50D C50 H50F 109.5 . . ? H50E C50 H50F 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C51 H51D 109.5 . . ? H51A C51 H51D 141.1 . . ? H51B C51 H51D 56.3 . . ? H51C C51 H51D 56.3 . . ? C49 C51 H51E 109.5 . . ? H51A C51 H51E 56.3 . . ? H51B C51 H51E 141.1 . . ? H51C C51 H51E 56.3 . . ? H51D C51 H51E 109.5 . . ? C49 C51 H51F 109.5 . . ? H51A C51 H51F 56.3 . . ? H51B C51 H51F 56.3 . . ? H51C C51 H51F 141.1 . . ? H51D C51 H51F 109.5 . . ? H51E C51 H51F 109.5 . . ? C48 C52 C53 112.7(4) . . ? C48 C52 C54 110.2(3) . . ? C53 C52 C54 111.2(3) . . ? C48 C52 H52 107.5 . . ? C53 C52 H52 107.5 . . ? C54 C52 H52 107.5 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C53 H53D 109.5 . . ? H53A C53 H53D 141.1 . . ? H53B C53 H53D 56.3 . . ? H53C C53 H53D 56.3 . . ? C52 C53 H53E 109.5 . . ? H53A C53 H53E 56.3 . . ? H53B C53 H53E 141.1 . . ? H53C C53 H53E 56.3 . . ? H53D C53 H53E 109.5 . . ? C52 C53 H53F 109.5 . . ? H53A C53 H53F 56.3 . . ? H53B C53 H53F 56.3 . . ? H53C C53 H53F 141.1 . . ? H53D C53 H53F 109.5 . . ? H53E C53 H53F 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C54 H54D 109.5 . . ? H54A C54 H54D 141.1 . . ? H54B C54 H54D 56.3 . . ? H54C C54 H54D 56.3 . . ? C52 C54 H54E 109.5 . . ? H54A C54 H54E 56.3 . . ? H54B C54 H54E 141.1 . . ? H54C C54 H54E 56.3 . . ? H54D C54 H54E 109.5 . . ? C52 C54 H54F 109.5 . . ? H54A C54 H54F 56.3 . . ? H54B C54 H54F 56.3 . . ? H54C C54 H54F 141.1 . . ? H54D C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? C61 C55 C56 116.2(2) . . ? C61 C55 Fe1 125.2(2) . . ? C56 C55 Fe1 118.4(2) . . ? C57 C56 C55 121.6(3) . . ? C57 C56 C62 118.2(3) . . ? C55 C56 C62 120.2(3) . . ? C56 C57 C59 121.9(3) . . ? C56 C57 H58 119.1 . . ? C59 C57 H58 119.1 . . ? C60 C59 C57 117.2(3) . . ? C60 C59 C63 120.8(3) . . ? C57 C59 C63 122.0(3) . . ? C59 C60 C61 121.6(3) . . ? C59 C60 H60 119.2 . . ? C61 C60 H60 119.2 . . ? C60 C61 C55 121.6(3) . . ? C60 C61 C64 118.0(3) . . ? C55 C61 C64 120.4(2) . . ? C56 C62 H62A 109.5 . . ? C56 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C56 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C56 C62 H62D 109.5 . . ? H62A C62 H62D 141.1 . . ? H62B C62 H62D 56.3 . . ? H62C C62 H62D 56.3 . . ? C56 C62 H62E 109.5 . . ? H62A C62 H62E 56.3 . . ? H62B C62 H62E 141.1 . . ? H62C C62 H62E 56.3 . . ? H62D C62 H62E 109.5 . . ? C56 C62 H62F 109.5 . . ? H62A C62 H62F 56.3 . . ? H62B C62 H62F 56.3 . . ? H62C C62 H62F 141.1 . . ? H62D C62 H62F 109.5 . . ? H62E C62 H62F 109.5 . . ? C59 C63 H63A 109.5 . . ? C59 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C59 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C59 C63 H63D 109.5 . . ? H63A C63 H63D 141.1 . . ? H63B C63 H63D 56.3 . . ? H63C C63 H63D 56.3 . . ? C59 C63 H63E 109.5 . . ? H63A C63 H63E 56.3 . . ? H63B C63 H63E 141.1 . . ? H63C C63 H63E 56.3 . . ? H63D C63 H63E 109.5 . . ? C59 C63 H63F 109.5 . . ? H63A C63 H63F 56.3 . . ? H63B C63 H63F 56.3 . . ? H63C C63 H63F 141.1 . . ? H63D C63 H63F 109.5 . . ? H63E C63 H63F 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C61 C64 H64D 109.5 . . ? H64A C64 H64D 141.1 . . ? H64B C64 H64D 56.3 . . ? H64C C64 H64D 56.3 . . ? C61 C64 H64E 109.5 . . ? H64A C64 H64E 56.3 . . ? H64B C64 H64E 141.1 . . ? H64C C64 H64E 56.3 . . ? H64D C64 H64E 109.5 . . ? C61 C64 H64F 109.5 . . ? H64A C64 H64F 56.3 . . ? H64B C64 H64F 56.3 . . ? H64C C64 H64F 141.1 . . ? H64D C64 H64F 109.5 . . ? H64E C64 H64F 109.5 . . ? C2H C1H H1H1 109.5 . . ? C2H C1H H1H2 109.5 . . ? H1H1 C1H H1H2 109.5 . . ? C2H C1H H1H3 109.5 . . ? H1H1 C1H H1H3 109.5 . . ? H1H2 C1H H1H3 109.5 . . ? C2H C1H H1H4 109.5 . . ? H1H1 C1H H1H4 141.1 . . ? H1H2 C1H H1H4 56.3 . . ? H1H3 C1H H1H4 56.3 . . ? C2H C1H H1H5 109.5 . . ? H1H1 C1H H1H5 56.3 . . ? H1H2 C1H H1H5 141.1 . . ? H1H3 C1H H1H5 56.3 . . ? H1H4 C1H H1H5 109.5 . . ? C2H C1H H1H6 109.5 . . ? H1H1 C1H H1H6 56.3 . . ? H1H2 C1H H1H6 56.3 . . ? H1H3 C1H H1H6 141.1 . . ? H1H4 C1H H1H6 109.5 . . ? H1H5 C1H H1H6 109.5 . . ? C1H C2H C3H 114.8(8) . . ? C1H C2H H2H1 108.6 . . ? C3H C2H H2H1 108.6 . . ? C1H C2H H2H2 108.6 . . ? C3H C2H H2H2 108.6 . . ? H2H1 C2H H2H2 107.5 . . ? C4H C3H C2H 104.2(7) . . ? C4H C3H H3H1 110.9 . . ? C2H C3H H3H1 110.9 . . ? C4H C3H H3H2 110.9 . . ? C2H C3H H3H2 110.9 . . ? H3H1 C3H H3H2 108.9 . . ? C3H C4H C5H 98.3(7) . . ? C3H C4H H4H1 112.1 . . ? C5H C4H H4H1 112.1 . . ? C3H C4H H4H2 112.1 . . ? C5H C4H H4H2 112.1 . . ? H4H1 C4H H4H2 109.8 . . ? C6H C5H C4H 103.1(6) . . ? C6H C5H H5H1 111.1 . . ? C4H C5H H5H1 111.1 . . ? C6H C5H H5H2 111.1 . . ? C4H C5H H5H2 111.1 . . ? H5H1 C5H H5H2 109.1 . . ? C5H C6H H6H1 109.5 . . ? C5H C6H H6H2 109.5 . . ? H6H1 C6H H6H2 109.5 . . ? C5H C6H H6H3 109.5 . . ? H6H1 C6H H6H3 109.5 . . ? H6H2 C6H H6H3 109.5 . . ? C5H C6H H6H4 109.5 . . ? H6H1 C6H H6H4 141.1 . . ? H6H2 C6H H6H4 56.3 . . ? H6H3 C6H H6H4 56.3 . . ? C5H C6H H6H5 109.5 . . ? H6H1 C6H H6H5 56.3 . . ? H6H2 C6H H6H5 141.1 . . ? H6H3 C6H H6H5 56.3 . . ? H6H4 C6H H6H5 109.5 . . ? C5H C6H H6H6 109.5 . . ? H6H1 C6H H6H6 56.3 . . ? H6H2 C6H H6H6 56.3 . . ? H6H3 C6H H6H6 141.1 . . ? H6H4 C6H H6H6 109.5 . . ? H6H5 C6H H6H6 109.5 . . ? C4S O1S C1S 102.9(16) . . ? C4S O1S C4S 85.5(15) . 2_667 ? C1S O1S C1S 93.1(12) . 2_667 ? C4S O1S C1S 74.9(12) 2_667 2_667 ? O1S C1S C2S 111.0(12) . 2_667 ? O1S C1S H1S1 109.4 . . ? C2S C1S H1S1 109.4 2_667 . ? O1S C1S H1S2 109.4 . . ? C2S C1S H1S2 109.4 2_667 . ? H1S1 C1S H1S2 108.0 . . ? C1S C2S C3S 101.4(10) 2_667 . ? C1S C2S H2S1 111.5 2_667 . ? C3S C2S H2S1 111.5 . . ? C1S C2S H2S2 111.5 2_667 . ? C3S C2S H2S2 111.5 . . ? H2S1 C2S H2S2 109.3 . . ? C2S C3S C4S 101.8(10) . 2_667 ? C2S C3S H3S1 111.4 . . ? C4S C3S H3S1 111.4 2_667 . ? C2S C3S H3S2 111.4 . . ? C4S C3S H3S2 111.4 2_667 . ? H3S1 C3S H3S2 109.3 . . ? O1S C4S C3S 113.7(13) . 2_667 ? O1S C4S H4S1 108.8 . . ? C3S C4S H4S1 108.8 2_667 . ? C3S C4S H4S2 108.8 2_667 . ? H4S1 C4S H4S2 107.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.157 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.068 _iucr_refine_instructions_details ; TITL p-1 in P-1 CELL 1.54178 12.7856 14.2917 19.9211 71.953 85.004 74.811 ZERR 2.00 0.0003 0.0005 0.0007 0.003 0.002 0.002 LATT 1 SFAC C H N K FE O UNIT 142 198 8 2 2 1 MERG 2 OMIT 0.00 133.00 EQIV $1 1-x, 1-y, 2-z DFIX 1.530 0.020 C2H C3H DFIX 1.530 0.020 C3H C4H DFIX 1.530 0.020 C4H C5H DFIX 1.400 O1S C1S DFIX 1.400 O1S C4S DFIX 1.500 C1S C2S_$1 DFIX 1.500 C2S C3S DFIX 1.500 C3S_$1 C4S DFIX 2.500 O1S C2S_$1 DFIX 2.500 O1S C3S_$1 DFIX 2.500 C1S C3S_$1 DFIX 2.500 C4S C2S_$1 FREE O1S C2S FREE O1S C3S FREE C1S C3S FREE C1S O1S_$1 FREE C1S C4S_$1 FREE C2S_$1 C4S_$1 FREE C2S_$1 O1S_$1 FREE C3S C4S FREE C3S_$1 O1S_$1 FREE C3S_$1 C1S_$1 FREE C4S O1S_$1 FREE C4S C1S_$1 FREE C4S C2S TEMP -123 SIZE 0.02 0.12 0.3 ACTA BOND $H L.S. 8 WGHT 0.120400 0.162900 FVAR 0.12735 K1 4 1.000000 0.000000 1.000000 10.50000 0.07902 0.02669 = 0.06792 0.01320 -0.02734 -0.01616 K2 4 0.500000 0.500000 0.500000 10.50000 0.06444 0.07193 = 0.04646 -0.01793 -0.03868 0.01237 FE1 5 0.833566 0.433632 0.752656 11.00000 0.02807 0.02347 = 0.01978 -0.00053 -0.00931 -0.00857 N1 3 1.008285 0.295950 0.945262 11.00000 0.03072 0.02722 = 0.01938 -0.00079 -0.00687 -0.00962 N2 3 0.931561 0.240219 0.882194 11.00000 0.03038 0.02312 = 0.02134 -0.00279 -0.00743 -0.00845 C1 1 0.992579 0.207651 0.941412 11.00000 0.03246 0.02777 = 0.02117 -0.00132 -0.00740 -0.00796 C2 1 0.958183 0.379129 0.889639 11.00000 0.03571 0.02263 = 0.02188 0.00033 -0.00891 -0.00865 AFIX 43 H2 2 0.959228 0.447797 0.882330 11.00000 -1.20000 AFIX 0 C3 1 0.907787 0.345348 0.847816 11.00000 0.03257 0.02179 = 0.02488 -0.00079 -0.00876 -0.00716 C4 1 1.073477 0.301771 0.998841 11.00000 0.03534 0.03209 = 0.01994 -0.00269 -0.00744 -0.01266 C5 1 1.021671 0.330075 1.056928 11.00000 0.03733 0.03306 = 0.02343 -0.00348 -0.00428 -0.01243 C6 1 1.086236 0.336298 1.107578 11.00000 0.04679 0.05546 = 0.02409 -0.01296 -0.00245 -0.01558 AFIX 43 H6 2 1.053527 0.354888 1.147791 11.00000 -1.20000 AFIX 0 C7 1 1.197334 0.315564 1.099477 11.00000 0.04689 0.08829 = 0.03218 -0.02318 -0.01053 -0.02276 AFIX 43 H7 2 1.240383 0.321822 1.133627 11.00000 -1.20000 AFIX 0 C8 1 1.246789 0.285910 1.042579 11.00000 0.03432 0.08469 = 0.04081 -0.02509 -0.00593 -0.01880 AFIX 43 H8 2 1.323525 0.271325 1.038332 11.00000 -1.20000 AFIX 0 C9 1 1.186087 0.276971 0.991184 11.00000 0.03773 0.05109 = 0.02810 -0.01059 -0.00469 -0.01576 C10 1 0.899964 0.346548 1.067124 11.00000 0.03717 0.03840 = 0.03024 -0.00921 -0.00229 -0.01092 AFIX 13 H10 2 0.867098 0.358185 1.020570 11.00000 -1.20000 AFIX 0 C11 1 0.875811 0.250312 1.118511 11.00000 0.05510 0.06107 = 0.09700 0.01157 0.01359 -0.02323 AFIX 123 H11A 2 0.797277 0.260216 1.125327 10.50000 -1.50000 H11B 2 0.910211 0.235739 1.163941 10.50000 -1.50000 H11C 2 0.904440 0.193196 1.099257 10.50000 -1.50000 H11D 2 0.944008 0.199218 1.133689 10.50000 -1.50000 H11E 2 0.831074 0.223695 1.095076 10.50000 -1.50000 H11F 2 0.836845 0.266238 1.159760 10.50000 -1.50000 AFIX 0 C12 1 0.849025 0.438010 1.092903 11.00000 0.04457 0.06729 = 0.10023 -0.04616 0.00145 -0.00505 AFIX 123 H12A 2 0.770645 0.445346 1.098484 10.50000 -1.50000 H12B 2 0.863075 0.499344 1.058423 10.50000 -1.50000 H12C 2 0.880498 0.428339 1.138432 10.50000 -1.50000 H12D 2 0.905500 0.470006 1.098409 10.50000 -1.50000 H12E 2 0.813070 0.416009 1.138470 10.50000 -1.50000 H12F 2 0.795647 0.487013 1.058461 10.50000 -1.50000 AFIX 0 C13 1 1.242163 0.242267 0.929550 11.00000 0.03471 0.06277 = 0.03492 -0.01783 -0.00131 -0.01427 AFIX 13 H13 2 1.186036 0.232461 0.902184 11.00000 -1.20000 AFIX 0 C14 1 1.296328 0.320086 0.880302 11.00000 0.07474 0.05642 = 0.04533 -0.01204 0.01801 -0.00623 AFIX 123 H14A 2 1.331403 0.294922 0.841348 10.50000 -1.50000 H14B 2 1.350877 0.331811 0.906290 10.50000 -1.50000 H14C 2 1.241794 0.383942 0.861361 10.50000 -1.50000 H14D 2 1.284647 0.378861 0.897984 10.50000 -1.50000 H14E 2 1.265172 0.341973 0.833043 10.50000 -1.50000 H14F 2 1.374255 0.289841 0.877972 10.50000 -1.50000 AFIX 0 C15 1 1.325011 0.140831 0.956065 11.00000 0.09117 0.05424 = 0.04991 -0.01150 0.01786 -0.00925 AFIX 123 H15A 2 1.289256 0.090805 0.987779 10.50000 -1.50000 H15B 2 1.382334 0.149248 0.981640 10.50000 -1.50000 H15C 2 1.356737 0.117192 0.915832 10.50000 -1.50000 H15D 2 1.396296 0.147358 0.935722 10.50000 -1.50000 H15E 2 1.303218 0.088915 0.941860 10.50000 -1.50000 H15F 2 1.328814 0.120971 1.007669 10.50000 -1.50000 AFIX 0 C16 1 0.902910 0.165206 0.857994 11.00000 0.03822 0.02350 = 0.02424 -0.00242 -0.01172 -0.00919 C17 1 0.804072 0.140115 0.880206 11.00000 0.04165 0.02976 = 0.02942 0.00149 -0.01335 -0.01328 C18 1 0.786673 0.056791 0.864410 11.00000 0.05575 0.03941 = 0.05112 -0.00218 -0.01435 -0.02657 AFIX 43 H18 2 0.721328 0.036552 0.879755 11.00000 -1.20000 AFIX 0 C19 1 0.861369 0.003194 0.827294 11.00000 0.07299 0.03248 = 0.06259 -0.01653 -0.01930 -0.01739 AFIX 43 H19 2 0.848166 -0.054191 0.818276 11.00000 -1.20000 AFIX 0 C20 1 0.956129 0.033166 0.803036 11.00000 0.05481 0.03454 = 0.05358 -0.01952 -0.01394 -0.00594 AFIX 43 H20 2 1.006288 -0.002489 0.775889 11.00000 -1.20000 AFIX 0 C21 1 0.978651 0.114901 0.817990 11.00000 0.04314 0.02823 = 0.03271 -0.00611 -0.01459 -0.00391 C22 1 0.720329 0.201077 0.919580 11.00000 0.04169 0.04481 = 0.04017 -0.00629 -0.00346 -0.02033 AFIX 13 H22 2 0.739170 0.267560 0.910611 11.00000 -1.20000 AFIX 0 C23 1 0.608559 0.224955 0.891798 11.00000 0.04003 0.17623 = 0.11544 -0.09286 -0.00871 -0.00105 AFIX 123 H23A 2 0.608641 0.257119 0.840621 10.50000 -1.50000 H23B 2 0.558898 0.271362 0.914403 10.50000 -1.50000 H23C 2 0.584790 0.162056 0.902138 10.50000 -1.50000 H23D 2 0.559579 0.203239 0.930821 10.50000 -1.50000 H23E 2 0.609322 0.188996 0.857038 10.50000 -1.50000 H23F 2 0.583430 0.298302 0.869303 10.50000 -1.50000 AFIX 0 C24 1 0.725996 0.151851 0.997671 11.00000 0.14487 0.07694 = 0.04511 -0.00728 0.00977 -0.00094 AFIX 123 H24A 2 0.800376 0.138251 1.013602 10.50000 -1.50000 H24B 2 0.704225 0.087793 1.009228 10.50000 -1.50000 H24C 2 0.677099 0.197241 1.021371 10.50000 -1.50000 H24D 2 0.654091 0.143939 1.015865 10.50000 -1.50000 H24E 2 0.750242 0.194397 1.020239 10.50000 -1.50000 H24F 2 0.777368 0.084949 1.008096 10.50000 -1.50000 AFIX 0 C25 1 1.081354 0.148317 0.790033 11.00000 0.03816 0.04104 = 0.04233 -0.01886 -0.00404 -0.00267 AFIX 13 H25 2 1.079851 0.209346 0.804939 11.00000 -1.20000 AFIX 0 C26 1 1.086366 0.180281 0.709320 11.00000 0.06157 0.09352 = 0.04555 -0.02318 0.00359 -0.02272 AFIX 123 H26A 2 1.020754 0.232809 0.690253 10.50000 -1.50000 H26B 2 1.091388 0.121256 0.692954 10.50000 -1.50000 H26C 2 1.150167 0.207254 0.693048 10.50000 -1.50000 H26D 2 1.154119 0.141404 0.693917 10.50000 -1.50000 H26E 2 1.083485 0.252957 0.691217 10.50000 -1.50000 H26F 2 1.024706 0.166959 0.691122 10.50000 -1.50000 AFIX 0 C27 1 1.182730 0.066377 0.822162 11.00000 0.04445 0.06448 = 0.08087 -0.02004 -0.01231 0.00180 AFIX 123 H27A 2 1.247493 0.090329 0.803081 10.50000 -1.50000 H27B 2 1.184920 0.004205 0.810381 10.50000 -1.50000 H27C 2 1.180643 0.052167 0.873581 10.50000 -1.50000 H27D 2 1.161211 0.007472 0.854948 10.50000 -1.50000 H27E 2 1.223784 0.093596 0.847648 10.50000 -1.50000 H27F 2 1.228061 0.045634 0.784447 10.50000 -1.50000 AFIX 0 N3 3 0.681340 0.429430 0.637553 11.00000 0.02452 0.02962 = 0.02069 -0.00424 -0.00732 -0.00693 N4 3 0.706239 0.275263 0.641726 11.00000 0.02800 0.02981 = 0.02189 -0.00569 -0.00595 -0.01007 C28 1 0.650720 0.369154 0.605008 11.00000 0.02747 0.03266 = 0.02701 -0.00633 -0.00716 -0.00819 C29 1 0.754753 0.376712 0.694081 11.00000 0.02624 0.03101 = 0.01928 -0.00171 -0.00660 -0.00898 C30 1 0.768568 0.277907 0.695378 11.00000 0.02971 0.03072 = 0.02220 -0.00220 -0.00898 -0.00834 AFIX 43 H30 2 0.813201 0.220356 0.727460 11.00000 -1.20000 AFIX 0 C31 1 0.631066 0.536081 0.615816 11.00000 0.02963 0.03066 = 0.02089 -0.00497 -0.00897 -0.00815 C32 1 0.684992 0.603359 0.567518 11.00000 0.03657 0.03302 = 0.02047 -0.00066 -0.00795 -0.00897 C33 1 0.626618 0.704191 0.540370 11.00000 0.04901 0.03167 = 0.03661 0.00185 -0.00191 -0.00778 AFIX 43 H33 2 0.660510 0.751259 0.507315 11.00000 -1.20000 AFIX 0 C34 1 0.520292 0.736972 0.560663 11.00000 0.05092 0.03285 = 0.04875 0.00011 -0.00899 -0.00221 AFIX 43 H34 2 0.481412 0.805416 0.540382 11.00000 -1.20000 AFIX 0 C35 1 0.471043 0.671134 0.609817 11.00000 0.03340 0.03821 = 0.04495 -0.01107 -0.00735 0.00082 AFIX 43 H35 2 0.398747 0.695175 0.624160 11.00000 -1.20000 AFIX 0 C36 1 0.525081 0.568815 0.639502 11.00000 0.03094 0.03245 = 0.03059 -0.00869 -0.00790 -0.00802 C37 1 0.799684 0.566717 0.542111 11.00000 0.03594 0.03944 = 0.03097 0.00168 -0.00322 -0.00962 AFIX 13 H37 2 0.836924 0.505813 0.580359 11.00000 -1.20000 AFIX 0 C38 1 0.797221 0.533244 0.477150 11.00000 0.04989 0.06488 = 0.05121 -0.02256 0.00843 -0.01241 AFIX 123 H38A 2 0.871540 0.509661 0.461424 10.50000 -1.50000 H38B 2 0.757820 0.590640 0.439355 10.50000 -1.50000 H38C 2 0.760713 0.477817 0.488723 10.50000 -1.50000 H38D 2 0.721842 0.542418 0.464910 10.50000 -1.50000 H38E 2 0.835562 0.461438 0.486980 10.50000 -1.50000 H38F 2 0.832669 0.574262 0.437612 10.50000 -1.50000 AFIX 0 C39 1 0.865325 0.646126 0.528434 11.00000 0.04475 0.05625 = 0.04045 -0.00129 0.00130 -0.02100 AFIX 123 H39A 2 0.938363 0.619069 0.512299 10.50000 -1.50000 H39B 2 0.870172 0.662517 0.572146 10.50000 -1.50000 H39C 2 0.829545 0.707728 0.492083 10.50000 -1.50000 H39D 2 0.820357 0.707140 0.538720 10.50000 -1.50000 H39E 2 0.888548 0.663692 0.478873 10.50000 -1.50000 H39F 2 0.929175 0.618481 0.558936 10.50000 -1.50000 AFIX 0 C40 1 0.471003 0.497353 0.696369 11.00000 0.03033 0.04157 = 0.03806 -0.01057 0.00023 -0.01211 AFIX 13 H40 2 0.507335 0.426578 0.695713 11.00000 -1.20000 AFIX 0 C41 1 0.351929 0.514276 0.683894 11.00000 0.04315 0.09370 = 0.06894 0.00091 -0.00548 -0.03282 AFIX 123 H41A 2 0.322140 0.466044 0.722045 10.50000 -1.50000 H41B 2 0.342309 0.503964 0.638648 10.50000 -1.50000 H41C 2 0.313952 0.583819 0.682882 10.50000 -1.50000 H41D 2 0.330127 0.569841 0.640338 10.50000 -1.50000 H41E 2 0.309958 0.531921 0.723735 10.50000 -1.50000 H41F 2 0.338315 0.452066 0.679501 10.50000 -1.50000 AFIX 0 C42 1 0.489162 0.503833 0.768597 11.00000 0.10459 0.11727 = 0.03538 -0.01057 0.00764 -0.07829 AFIX 123 H42A 2 0.454207 0.457195 0.804489 10.50000 -1.50000 H42B 2 0.457942 0.573439 0.770287 10.50000 -1.50000 H42C 2 0.567110 0.485066 0.777844 10.50000 -1.50000 H42D 2 0.531966 0.553272 0.763924 10.50000 -1.50000 H42E 2 0.528231 0.437028 0.798126 10.50000 -1.50000 H42F 2 0.419062 0.525400 0.790570 10.50000 -1.50000 AFIX 0 C43 1 0.701369 0.183604 0.627079 11.00000 0.03354 0.02955 = 0.02343 -0.00453 -0.00850 -0.01050 C44 1 0.778275 0.146160 0.581624 11.00000 0.03834 0.03144 = 0.02785 -0.00652 -0.00719 -0.00847 C45 1 0.769724 0.058438 0.567578 11.00000 0.04927 0.03811 = 0.04161 -0.01745 -0.00068 -0.01309 AFIX 43 H45 2 0.821054 0.030764 0.536975 11.00000 -1.20000 AFIX 0 C46 1 0.688564 0.011518 0.597166 11.00000 0.06248 0.04114 = 0.04703 -0.01674 -0.00430 -0.02377 AFIX 43 H46 2 0.683934 -0.047554 0.586417 11.00000 -1.20000 AFIX 0 C47 1 0.613908 0.049488 0.642273 11.00000 0.05795 0.04955 = 0.04737 -0.01485 0.00001 -0.03263 AFIX 43 H47 2 0.558622 0.015889 0.662698 11.00000 -1.20000 AFIX 0 C48 1 0.618338 0.136879 0.658446 11.00000 0.04294 0.04236 = 0.03282 -0.00872 -0.00358 -0.02131 C49 1 0.864832 0.200004 0.545796 11.00000 0.04083 0.03648 = 0.03540 -0.01390 0.00267 -0.01328 AFIX 13 H49 2 0.870028 0.247736 0.572246 11.00000 -1.20000 AFIX 0 C50 1 0.976481 0.127832 0.546930 11.00000 0.03893 0.05241 = 0.08318 -0.02436 0.00785 -0.01439 AFIX 123 H50A 2 1.028945 0.166733 0.523144 10.50000 -1.50000 H50B 2 0.973597 0.078755 0.522426 10.50000 -1.50000 H50C 2 0.998708 0.091589 0.595948 10.50000 -1.50000 H50D 2 0.971888 0.057985 0.571201 10.50000 -1.50000 H50E 2 1.027236 0.145963 0.571919 10.50000 -1.50000 H50F 2 1.002126 0.133129 0.498398 10.50000 -1.50000 AFIX 0 C51 1 0.830349 0.263639 0.470607 11.00000 0.07210 0.06092 = 0.03594 -0.00775 0.00412 -0.02618 AFIX 123 H51A 2 0.886449 0.298497 0.447690 10.50000 -1.50000 H51B 2 0.761973 0.314007 0.471825 10.50000 -1.50000 H51C 2 0.820465 0.219302 0.443991 10.50000 -1.50000 H51D 2 0.759476 0.256040 0.461314 10.50000 -1.50000 H51E 2 0.883952 0.240531 0.437179 10.50000 -1.50000 H51F 2 0.825460 0.335236 0.465013 10.50000 -1.50000 AFIX 0 C52 1 0.533819 0.179632 0.706766 11.00000 0.04786 0.07039 = 0.04972 -0.02871 0.00979 -0.03317 AFIX 13 H52 2 0.563235 0.226987 0.723254 11.00000 -1.20000 AFIX 0 C53 1 0.510318 0.097626 0.772164 11.00000 0.07112 0.10151 = 0.04653 -0.02796 0.01393 -0.05066 AFIX 123 H53A 2 0.455611 0.129099 0.801519 10.50000 -1.50000 H53B 2 0.577064 0.062369 0.799285 10.50000 -1.50000 H53C 2 0.483195 0.048779 0.757660 10.50000 -1.50000 H53D 2 0.554969 0.031066 0.770791 10.50000 -1.50000 H53E 2 0.433516 0.097795 0.773024 10.50000 -1.50000 H53F 2 0.527386 0.111386 0.814650 10.50000 -1.50000 AFIX 0 C54 1 0.430144 0.241710 0.665793 11.00000 0.05363 0.08123 = 0.07489 -0.03055 0.00833 -0.01380 AFIX 123 H54A 2 0.376326 0.269074 0.697452 10.50000 -1.50000 H54B 2 0.401313 0.198049 0.646762 10.50000 -1.50000 H54C 2 0.446287 0.297827 0.626880 10.50000 -1.50000 H54D 2 0.439624 0.240893 0.616611 10.50000 -1.50000 H54E 2 0.414638 0.311917 0.667301 10.50000 -1.50000 H54F 2 0.369663 0.212139 0.687182 10.50000 -1.50000 AFIX 0 C55 1 0.875817 0.570802 0.723019 11.00000 0.03384 0.03168 = 0.01660 0.00101 -0.00632 -0.01445 C56 1 0.986097 0.570481 0.708820 11.00000 0.03795 0.03652 = 0.02120 -0.00172 -0.00457 -0.01168 C57 1 1.022120 0.657703 0.696083 11.00000 0.04166 0.04592 = 0.02250 -0.00161 0.00020 -0.02350 AFIX 43 H58 2 1.097204 0.654023 0.687912 11.00000 -1.20000 AFIX 0 C59 1 0.951234 0.750979 0.694898 11.00000 0.05588 0.03917 = 0.02378 -0.00045 -0.00348 -0.02672 C60 1 0.842170 0.752765 0.707626 11.00000 0.05405 0.02813 = 0.02578 -0.00368 -0.00789 -0.01049 AFIX 43 H60 2 0.791740 0.815206 0.706661 11.00000 -1.20000 AFIX 0 C61 1 0.804999 0.664972 0.721792 11.00000 0.03807 0.03150 = 0.01923 -0.00281 -0.00713 -0.01177 C62 1 1.068273 0.473388 0.706665 11.00000 0.03312 0.04590 = 0.04578 -0.00833 0.00658 -0.00946 AFIX 123 H62A 2 1.031807 0.418125 0.716592 10.50000 -1.50000 H62B 2 1.124081 0.456117 0.742265 10.50000 -1.50000 H62C 2 1.102074 0.483132 0.659744 10.50000 -1.50000 H62D 2 1.140167 0.486791 0.695808 10.50000 -1.50000 H62E 2 1.047894 0.448799 0.670135 10.50000 -1.50000 H62F 2 1.069900 0.421784 0.752657 10.50000 -1.50000 AFIX 0 C63 1 0.989990 0.846026 0.680637 11.00000 0.08196 0.04883 = 0.04629 -0.00677 -0.00063 -0.04063 AFIX 123 H63A 2 1.068590 0.830443 0.672879 10.50000 -1.50000 H63B 2 0.972607 0.872481 0.721230 10.50000 -1.50000 H63C 2 0.954034 0.897105 0.638506 10.50000 -1.50000 H63D 2 0.928231 0.902910 0.682198 10.50000 -1.50000 H63E 2 1.024214 0.860872 0.633846 10.50000 -1.50000 H63F 2 1.042787 0.836248 0.716571 10.50000 -1.50000 AFIX 0 C64 1 0.685599 0.673625 0.735863 11.00000 0.03490 0.03880 = 0.03987 -0.01186 -0.01021 -0.00485 AFIX 123 H64A 2 0.648669 0.744104 0.732969 10.50000 -1.50000 H64B 2 0.675103 0.629199 0.783144 10.50000 -1.50000 H64C 2 0.655403 0.653196 0.700622 10.50000 -1.50000 H64D 2 0.670780 0.606896 0.744855 10.50000 -1.50000 H64E 2 0.644347 0.721801 0.694680 10.50000 -1.50000 H64F 2 0.664047 0.697803 0.777201 10.50000 -1.50000 AFIX 0 C1H 1 0.449724 0.827752 0.835313 11.00000 0.23332 0.08702 = 0.14248 -0.01591 0.09054 -0.00067 AFIX 123 H1H1 2 0.505577 0.783424 0.869727 10.50000 -1.50000 H1H2 2 0.389280 0.862595 0.859539 10.50000 -1.50000 H1H3 2 0.480546 0.878134 0.799710 10.50000 -1.50000 H1H4 2 0.411358 0.899344 0.816257 10.50000 -1.50000 H1H5 2 0.527656 0.820174 0.826445 10.50000 -1.50000 H1H6 2 0.436389 0.804635 0.886274 10.50000 -1.50000 AFIX 0 C2H 1 0.408178 0.762975 0.798827 11.00000 0.08439 0.11465 = 0.19320 0.00563 0.02902 0.00373 AFIX 23 H2H1 2 0.376834 0.712825 0.835340 11.00000 -1.20000 H2H2 2 0.470835 0.724665 0.777355 11.00000 -1.20000 AFIX 0 C3H 1 0.312148 0.831554 0.734305 11.00000 0.15567 0.15181 = 0.28015 -0.15774 0.14508 -0.10521 AFIX 23 H3H1 2 0.295145 0.787231 0.709409 11.00000 -1.20000 H3H2 2 0.244537 0.864270 0.754931 11.00000 -1.20000 AFIX 0 C4H 1 0.361798 0.905972 0.687460 11.00000 0.08958 0.09426 = 0.17288 -0.06941 0.04726 -0.02945 AFIX 23 H4H1 2 0.435325 0.875285 0.672569 11.00000 -1.20000 H4H2 2 0.364929 0.959882 0.708120 11.00000 -1.20000 AFIX 0 C5H 1 0.274765 0.947460 0.623107 11.00000 0.08467 0.11262 = 0.06916 -0.02906 -0.00136 -0.00462 AFIX 23 H5H1 2 0.283457 0.897733 0.596501 11.00000 -1.20000 H5H2 2 0.199410 0.961705 0.641074 11.00000 -1.20000 AFIX 0 C6H 1 0.302612 1.041833 0.578638 11.00000 0.14308 0.10988 = 0.15557 -0.06902 0.00396 -0.06080 AFIX 123 H6H1 2 0.253965 1.073138 0.537982 10.50000 -1.50000 H6H2 2 0.377712 1.025738 0.562034 10.50000 -1.50000 H6H3 2 0.294611 1.089160 0.606431 10.50000 -1.50000 H6H4 2 0.363560 1.052219 0.599649 10.50000 -1.50000 H6H5 2 0.239814 1.099620 0.575597 10.50000 -1.50000 H6H6 2 0.322915 1.036198 0.531200 10.50000 -1.50000 AFIX 0 O1S 6 0.568889 0.429147 0.999405 10.50000 0.22276 0.26730 = 0.37716 -0.19689 0.11750 -0.16963 C1S 1 0.569591 0.534411 0.962039 10.50000 0.13800 0.09882 = 0.10056 -0.03277 0.02742 -0.01598 AFIX 23 H1S1 2 0.547213 0.551061 0.912508 10.50000 -1.20000 H1S2 2 0.644052 0.542966 0.961564 10.50000 -1.20000 AFIX 0 C2S 1 0.506636 0.393360 1.002934 10.50000 0.16738 0.10185 = 0.15867 -0.07057 0.06308 -0.06883 AFIX 23 H2S1 2 0.469328 0.381184 0.966092 10.50000 -1.20000 H2S2 2 0.538925 0.327561 1.037865 10.50000 -1.20000 AFIX 0 C3S 1 0.593520 0.453573 0.970279 10.50000 0.10856 0.14258 = 0.23646 -0.02449 -0.05564 0.01962 AFIX 23 H3S1 2 0.610605 0.453610 0.920837 10.50000 -1.20000 H3S2 2 0.661051 0.425429 0.998221 10.50000 -1.20000 AFIX 0 C4S 1 0.465064 0.437258 1.025486 10.50000 0.17540 0.21072 = 0.51672 -0.25404 0.14087 -0.08100 AFIX 23 H4S1 2 0.466971 0.388334 1.073330 10.50000 -1.20000 H4S2 2 0.422229 0.418184 0.995059 10.50000 -1.20000 HKLF 4 REM p-1 in P-1 REM R1 = 0.0633 for 9569 Fo > 4sig(Fo) and 0.0772 for all 11766 data REM 724 parameters refined using 12 restraints END WGHT 0.1202 0.1674 REM Highest difference peak 1.157, deepest hole -0.691, 1-sigma level 0.068 Q1 1 0.3721 0.9728 0.6854 11.00000 0.05 1.16 Q2 1 0.3844 0.8721 0.7380 11.00000 0.05 0.74 Q3 1 0.2705 0.8778 0.6881 11.00000 0.05 0.69 Q4 1 0.3380 0.9920 0.6315 11.00000 0.05 0.68 Q5 1 0.6589 0.1305 0.9845 11.00000 0.05 0.47 Q6 1 0.8358 0.5195 0.7303 11.00000 0.05 0.42 Q7 1 0.8773 0.3766 0.8129 11.00000 0.05 0.40 Q8 1 0.8544 0.3387 0.7727 11.00000 0.05 0.34 Q9 1 0.7859 0.5361 0.7305 11.00000 0.05 0.34 Q10 1 0.8139 0.4410 0.7058 11.00000 0.05 0.33 Q11 1 0.6328 0.2781 0.8776 11.00000 0.05 0.29 Q12 1 0.3372 0.8989 0.6867 11.00000 0.05 0.26 Q13 1 0.6844 0.4243 0.6230 11.00000 0.05 0.26 Q14 1 0.8573 0.4579 1.0468 11.00000 0.05 0.26 Q15 1 0.7623 0.4548 0.7647 11.00000 0.05 0.25 Q16 1 1.0323 0.4336 0.6911 11.00000 0.05 0.24 Q17 1 0.7837 0.4835 0.6937 11.00000 0.05 0.23 Q18 1 0.4198 0.5598 0.7565 11.00000 0.05 0.23 Q19 1 0.4870 0.4203 0.9891 11.00000 0.05 0.23 Q20 1 0.6586 0.5584 0.5813 11.00000 0.05 0.23 ; _database_code_depnum_ccdc_archive 'CCDC 962249' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pbcn _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(18-crown-6)THF][Fe(mes)3] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C16 H32 K O7, C27 H33 Fe' _chemical_formula_sum 'C43 H65 Fe K O7' _chemical_formula_weight 788.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 33.7821(5) _cell_length_b 10.77070(10) _cell_length_c 24.2239(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8814.03(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23760 _cell_measurement_theta_min 3.1871 _cell_measurement_theta_max 76.7045 _exptl_crystal_description needle _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 3.942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3842 _exptl_absorpt_correction_T_max 0.9253 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4102 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 118437 _diffrn_reflns_av_R_equivalents 0.1174 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 66.50 _reflns_number_total 7773 _reflns_number_gt 5807 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^ > 2\s(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^)+(0.0499P)^2^+9.4438P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7773 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.133944(14) 0.31080(4) 0.363185(18) 0.03133(13) Uani 1 1 d . . . C1 C 0.16207(9) 0.1653(3) 0.40448(12) 0.0294(6) Uani 1 1 d . . . C2 C 0.20311(9) 0.1474(3) 0.39915(12) 0.0310(7) Uani 1 1 d . . . C3 C 0.22281(9) 0.0521(3) 0.42677(12) 0.0325(7) Uani 1 1 d . . . H3 H 0.2506 0.0438 0.4221 0.039 Uiso 1 1 calc R . . C4 C 0.20315(10) -0.0307(3) 0.46079(12) 0.0356(7) Uani 1 1 d . . . C5 C 0.16256(10) -0.0159(3) 0.46613(12) 0.0358(7) Uani 1 1 d . . . H5 H 0.1481 -0.0717 0.4889 0.043 Uiso 1 1 calc R . . C6 C 0.14234(9) 0.0791(3) 0.43886(12) 0.0328(7) Uani 1 1 d . . . C7 C 0.22727(9) 0.2314(3) 0.36173(13) 0.0383(7) Uani 1 1 d . . . H7A H 0.2099 0.2941 0.3452 0.058 Uiso 0.50 1 calc PR . . H7B H 0.2395 0.1816 0.3325 0.058 Uiso 0.50 1 calc PR . . H7C H 0.2480 0.2725 0.3834 0.058 Uiso 0.50 1 calc PR . . H7D H 0.2550 0.2047 0.3622 0.058 Uiso 0.50 1 calc PR . . H7E H 0.2254 0.3172 0.3749 0.058 Uiso 0.50 1 calc PR . . H7F H 0.2170 0.2263 0.3240 0.058 Uiso 0.50 1 calc PR . . C8 C 0.22532(11) -0.1328(3) 0.49027(15) 0.0493(9) Uani 1 1 d . . . H8A H 0.2535 -0.1276 0.4811 0.074 Uiso 0.50 1 calc PR . . H8B H 0.2149 -0.2136 0.4786 0.074 Uiso 0.50 1 calc PR . . H8C H 0.2219 -0.1235 0.5302 0.074 Uiso 0.50 1 calc PR . . H8D H 0.2067 -0.1822 0.5122 0.074 Uiso 0.50 1 calc PR . . H8E H 0.2453 -0.0962 0.5147 0.074 Uiso 0.50 1 calc PR . . H8F H 0.2384 -0.1863 0.4631 0.074 Uiso 0.50 1 calc PR . . C9 C 0.09794(9) 0.0875(4) 0.44613(14) 0.0454(8) Uani 1 1 d . . . H9A H 0.0877 0.1579 0.4248 0.068 Uiso 0.50 1 calc PR . . H9B H 0.0917 0.0994 0.4853 0.068 Uiso 0.50 1 calc PR . . H9C H 0.0856 0.0106 0.4330 0.068 Uiso 0.50 1 calc PR . . H9D H 0.0890 0.0207 0.4706 0.068 Uiso 0.50 1 calc PR . . H9E H 0.0850 0.0792 0.4101 0.068 Uiso 0.50 1 calc PR . . H9F H 0.0911 0.1680 0.4624 0.068 Uiso 0.50 1 calc PR . . C10 C 0.10195(9) 0.4430(3) 0.40777(11) 0.0312(7) Uani 1 1 d . . . C11 C 0.12088(9) 0.5407(3) 0.43588(12) 0.0341(7) Uani 1 1 d . . . C12 C 0.09968(11) 0.6312(3) 0.46462(12) 0.0413(8) Uani 1 1 d . . . H12 H 0.1136 0.6969 0.4822 0.050 Uiso 1 1 calc R . . C13 C 0.05880(11) 0.6271(3) 0.46808(13) 0.0411(8) Uani 1 1 d . . . C14 C 0.03975(10) 0.5308(3) 0.44169(12) 0.0389(8) Uani 1 1 d . . . H14 H 0.0117 0.5250 0.4442 0.047 Uiso 1 1 calc R . . C15 C 0.06038(9) 0.4412(3) 0.41127(12) 0.0339(7) Uani 1 1 d . . . C16 C 0.16573(10) 0.5509(4) 0.43616(14) 0.0450(8) Uani 1 1 d . . . H16A H 0.1771 0.4826 0.4146 0.068 Uiso 0.50 1 calc PR . . H16B H 0.1754 0.5464 0.4742 0.068 Uiso 0.50 1 calc PR . . H16C H 0.1736 0.6303 0.4198 0.068 Uiso 0.50 1 calc PR . . H16D H 0.1737 0.6236 0.4578 0.068 Uiso 0.50 1 calc PR . . H16E H 0.1753 0.5598 0.3982 0.068 Uiso 0.50 1 calc PR . . H16F H 0.1771 0.4759 0.4527 0.068 Uiso 0.50 1 calc PR . . C17 C 0.03634(13) 0.7253(4) 0.49954(16) 0.0610(11) Uani 1 1 d . . . H17A H 0.0550 0.7855 0.5151 0.091 Uiso 0.50 1 calc PR . . H17B H 0.0213 0.6863 0.5295 0.091 Uiso 0.50 1 calc PR . . H17C H 0.0181 0.7680 0.4745 0.091 Uiso 0.50 1 calc PR . . H17D H 0.0079 0.7077 0.4976 0.091 Uiso 0.50 1 calc PR . . H17E H 0.0416 0.8069 0.4832 0.091 Uiso 0.50 1 calc PR . . H17F H 0.0449 0.7252 0.5382 0.091 Uiso 0.50 1 calc PR . . C18 C 0.03705(10) 0.3416(3) 0.38166(14) 0.0438(8) Uani 1 1 d . . . H18A H 0.0087 0.3540 0.3884 0.066 Uiso 0.50 1 calc PR . . H18B H 0.0450 0.2598 0.3955 0.066 Uiso 0.50 1 calc PR . . H18C H 0.0423 0.3464 0.3419 0.066 Uiso 0.50 1 calc PR . . H18D H 0.0553 0.2861 0.3622 0.066 Uiso 0.50 1 calc PR . . H18E H 0.0190 0.3803 0.3551 0.066 Uiso 0.50 1 calc PR . . H18F H 0.0217 0.2937 0.4086 0.066 Uiso 0.50 1 calc PR . . C19 C 0.14026(10) 0.3215(3) 0.27755(13) 0.0391(8) Uani 1 1 d . . . C20 C 0.12250(11) 0.2315(3) 0.24343(14) 0.0470(9) Uani 1 1 d . . . C21 C 0.12960(13) 0.2296(4) 0.18632(15) 0.0597(11) Uani 1 1 d . . . H21 H 0.1177 0.1664 0.1645 0.072 Uiso 1 1 calc R . . C22 C 0.15327(13) 0.3165(4) 0.16094(15) 0.0595(11) Uani 1 1 d . . . C23 C 0.17022(11) 0.4069(4) 0.19373(14) 0.0528(10) Uani 1 1 d . . . H23 H 0.1865 0.4685 0.1771 0.063 Uiso 1 1 calc R . . C24 C 0.16412(10) 0.4101(3) 0.25034(13) 0.0422(8) Uani 1 1 d . . . C25 C 0.09478(13) 0.1354(4) 0.26754(17) 0.0615(11) Uani 1 1 d . . . H25A H 0.0926 0.1480 0.3075 0.092 Uiso 0.50 1 calc PR . . H25B H 0.1052 0.0521 0.2602 0.092 Uiso 0.50 1 calc PR . . H25C H 0.0686 0.1437 0.2505 0.092 Uiso 0.50 1 calc PR . . H25D H 0.0850 0.0812 0.2380 0.092 Uiso 0.50 1 calc PR . . H25E H 0.0724 0.1771 0.2853 0.092 Uiso 0.50 1 calc PR . . H25F H 0.1090 0.0855 0.2950 0.092 Uiso 0.50 1 calc PR . . C26 C 0.15989(18) 0.3142(5) 0.09886(16) 0.0905(18) Uani 1 1 d . . . H26A H 0.1774 0.3827 0.0883 0.136 Uiso 0.50 1 calc PR . . H26B H 0.1344 0.3232 0.0799 0.136 Uiso 0.50 1 calc PR . . H26C H 0.1721 0.2351 0.0884 0.136 Uiso 0.50 1 calc PR . . H26D H 0.1452 0.2446 0.0827 0.136 Uiso 0.50 1 calc PR . . H26E H 0.1882 0.3041 0.0912 0.136 Uiso 0.50 1 calc PR . . H26F H 0.1505 0.3922 0.0827 0.136 Uiso 0.50 1 calc PR . . C27 C 0.18335(11) 0.5123(3) 0.28328(14) 0.0473(9) Uani 1 1 d . . . H27A H 0.1766 0.5026 0.3224 0.071 Uiso 0.50 1 calc PR . . H27B H 0.1738 0.5930 0.2701 0.071 Uiso 0.50 1 calc PR . . H27C H 0.2121 0.5079 0.2788 0.071 Uiso 0.50 1 calc PR . . H27D H 0.1984 0.5664 0.2585 0.071 Uiso 0.50 1 calc PR . . H27E H 0.2012 0.4760 0.3107 0.071 Uiso 0.50 1 calc PR . . H27F H 0.1629 0.5611 0.3021 0.071 Uiso 0.50 1 calc PR . . K1 K 0.12956(2) 0.76029(8) 0.19094(3) 0.04442(19) Uani 1 1 d . A . O101 O 0.10906(7) 0.7310(2) 0.30111(9) 0.0428(5) Uani 1 1 d . . . O102 O 0.16763(7) 0.8974(2) 0.27121(9) 0.0484(6) Uani 1 1 d . . . O103 O 0.20135(8) 0.8837(3) 0.16602(11) 0.0581(7) Uani 1 1 d . . . O104 O 0.15576(8) 0.7738(3) 0.08209(10) 0.0585(7) Uani 1 1 d . . . O105 O 0.10023(8) 0.5948(3) 0.11426(10) 0.0550(7) Uani 1 1 d . . . O106 O 0.06412(7) 0.6100(2) 0.21993(10) 0.0474(6) Uani 1 1 d . . . C101 C 0.12071(12) 0.8277(3) 0.33688(13) 0.0474(9) Uani 1 1 d . . . H10A H 0.1173 0.8013 0.3757 0.057 Uiso 1 1 calc R . . H10B H 0.1040 0.9017 0.3305 0.057 Uiso 1 1 calc R . . C102 C 0.16329(12) 0.8594(4) 0.32642(14) 0.0510(9) Uani 1 1 d . . . H10C H 0.1717 0.9269 0.3515 0.061 Uiso 1 1 calc R . . H10D H 0.1801 0.7859 0.3336 0.061 Uiso 1 1 calc R . . C103 C 0.20690(11) 0.9391(4) 0.26022(17) 0.0609(11) Uani 1 1 d . . . H10E H 0.2259 0.8702 0.2659 0.073 Uiso 1 1 calc R . . H10F H 0.2139 1.0073 0.2858 0.073 Uiso 1 1 calc R . . C104 C 0.20920(12) 0.9838(4) 0.20181(18) 0.0641(11) Uani 1 1 d . . . H10G H 0.1896 1.0507 0.1957 0.077 Uiso 1 1 calc R . . H10H H 0.2359 1.0176 0.1943 0.077 Uiso 1 1 calc R . . C105 C 0.20519(13) 0.9150(4) 0.10913(16) 0.0663(12) Uani 1 1 d . . . H10I H 0.2326 0.9426 0.1015 0.080 Uiso 1 1 calc R . . H10J H 0.1871 0.9843 0.1001 0.080 Uiso 1 1 calc R . . C106 C 0.19554(13) 0.8055(4) 0.07423(17) 0.0669(12) Uani 1 1 d . . . H10K H 0.2003 0.8254 0.0349 0.080 Uiso 1 1 calc R . . H10L H 0.2127 0.7346 0.0845 0.080 Uiso 1 1 calc R . . C107 C 0.14332(14) 0.6752(4) 0.04693(15) 0.0662(12) Uani 1 1 d . . . H10M H 0.1608 0.6025 0.0521 0.079 Uiso 1 1 calc R . . H10N H 0.1452 0.7017 0.0079 0.079 Uiso 1 1 calc R . . C108 C 0.10175(14) 0.6404(4) 0.06007(15) 0.0642(12) Uani 1 1 d . . . H10O H 0.0843 0.7139 0.0565 0.077 Uiso 1 1 calc R . . H10P H 0.0924 0.5760 0.0340 0.077 Uiso 1 1 calc R . . C109 C 0.06295(12) 0.5413(4) 0.12729(16) 0.0595(11) Uani 1 1 d . . . H10Q H 0.0583 0.4679 0.1036 0.071 Uiso 1 1 calc R . . H10R H 0.0416 0.6023 0.1200 0.071 Uiso 1 1 calc R . . C110 C 0.06196(11) 0.5037(4) 0.18622(16) 0.0548(10) Uani 1 1 d . . . H11A H 0.0372 0.4580 0.1940 0.066 Uiso 1 1 calc R . . H11B H 0.0845 0.4480 0.1943 0.066 Uiso 1 1 calc R . . C111 C 0.06195(11) 0.5796(4) 0.27707(14) 0.0479(9) Uani 1 1 d . . . H11C H 0.0817 0.5147 0.2859 0.057 Uiso 1 1 calc R . . H11D H 0.0353 0.5466 0.2858 0.057 Uiso 1 1 calc R . . C112 C 0.06978(10) 0.6920(4) 0.31051(14) 0.0476(9) Uani 1 1 d . . . H11E H 0.0511 0.7588 0.3000 0.057 Uiso 1 1 calc R . . H11F H 0.0659 0.6732 0.3502 0.057 Uiso 1 1 calc R . . O301 O 0.06795(8) 0.9081(3) 0.15214(12) 0.0628(8) Uani 1 1 d . . . C301 C 0.0284(5) 0.893(2) 0.1765(8) 0.074(6) Uani 0.592(15) 1 d P A 1 H30A H 0.0231 0.9556 0.2054 0.089 Uiso 0.592(15) 1 calc PR A 1 H30B H 0.0246 0.8086 0.1920 0.089 Uiso 0.592(15) 1 calc PR A 1 C302 C 0.0022(3) 0.9145(14) 0.1241(4) 0.080(4) Uani 0.592(15) 1 d P A 1 H30C H -0.0104 0.8354 0.1130 0.096 Uiso 0.592(15) 1 calc PR A 1 H30D H -0.0190 0.9748 0.1328 0.096 Uiso 0.592(15) 1 calc PR A 1 C303 C 0.0268(3) 0.9626(10) 0.0782(4) 0.062(3) Uani 0.592(15) 1 d P A 1 H30E H 0.0150 1.0396 0.0630 0.074 Uiso 0.592(15) 1 calc PR A 1 H30F H 0.0285 0.9004 0.0482 0.074 Uiso 0.592(15) 1 calc PR A 1 C304 C 0.0676(5) 0.9889(18) 0.1018(5) 0.058(4) Uani 0.592(15) 1 d P A 1 H30G H 0.0887 0.9648 0.0756 0.070 Uiso 0.592(15) 1 calc PR A 1 H30H H 0.0707 1.0776 0.1116 0.070 Uiso 0.592(15) 1 calc PR A 1 C401 C 0.0318(9) 0.914(4) 0.1755(9) 0.073(9) Uani 0.408(15) 1 d P A 2 H40A H 0.0213 0.8287 0.1765 0.088 Uiso 0.408(15) 1 calc PR A 2 H40B H 0.0358 0.9402 0.2143 0.088 Uiso 0.408(15) 1 calc PR A 2 C402 C 0.0035(5) 0.985(2) 0.1554(10) 0.104(7) Uani 0.408(15) 1 d P A 2 H40C H -0.0061 1.0459 0.1830 0.125 Uiso 0.408(15) 1 calc PR A 2 H40D H -0.0190 0.9355 0.1415 0.125 Uiso 0.408(15) 1 calc PR A 2 C403 C 0.0245(5) 1.044(2) 0.1116(9) 0.116(9) Uani 0.408(15) 1 d P A 2 H40E H 0.0322 1.1301 0.1217 0.139 Uiso 0.408(15) 1 calc PR A 2 H40F H 0.0085 1.0466 0.0774 0.139 Uiso 0.408(15) 1 calc PR A 2 C404 C 0.0600(8) 0.964(3) 0.1047(11) 0.082(9) Uani 0.408(15) 1 d P A 2 H40G H 0.0549 0.9009 0.0758 0.098 Uiso 0.408(15) 1 calc PR A 2 H40H H 0.0829 1.0148 0.0931 0.098 Uiso 0.408(15) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0331(2) 0.0350(3) 0.0259(2) 0.0006(2) 0.0005(2) 0.0057(2) C1 0.0342(15) 0.0279(16) 0.0262(15) -0.0048(12) -0.0014(12) 0.0002(12) C2 0.0381(16) 0.0271(16) 0.0278(15) -0.0053(12) -0.0012(12) -0.0037(13) C3 0.0336(16) 0.0321(16) 0.0318(16) -0.0032(13) -0.0038(13) 0.0030(13) C4 0.0497(19) 0.0303(17) 0.0269(15) -0.0013(13) -0.0030(14) 0.0033(14) C5 0.0474(18) 0.0352(18) 0.0248(15) 0.0004(13) 0.0045(13) -0.0058(14) C6 0.0392(17) 0.0341(17) 0.0252(15) -0.0043(13) 0.0005(12) -0.0017(13) C7 0.0318(16) 0.0376(18) 0.0456(19) 0.0047(15) -0.0001(14) 0.0025(13) C8 0.063(2) 0.045(2) 0.0398(19) 0.0076(16) -0.0006(17) 0.0104(18) C9 0.0372(18) 0.057(2) 0.0420(19) 0.0052(17) 0.0082(15) -0.0009(16) C10 0.0358(16) 0.0361(17) 0.0217(14) 0.0083(13) 0.0023(12) 0.0056(13) C11 0.0434(17) 0.0371(18) 0.0219(14) 0.0051(13) 0.0022(13) 0.0022(14) C12 0.062(2) 0.0373(19) 0.0243(15) 0.0016(14) 0.0021(15) -0.0023(16) C13 0.058(2) 0.0358(19) 0.0296(16) 0.0049(14) 0.0093(15) 0.0112(16) C14 0.0376(17) 0.047(2) 0.0326(16) 0.0092(15) 0.0073(13) 0.0117(15) C15 0.0357(16) 0.0384(18) 0.0276(15) 0.0062(13) 0.0005(13) 0.0080(14) C16 0.0425(19) 0.058(2) 0.0347(17) -0.0025(17) -0.0009(15) -0.0071(16) C17 0.080(3) 0.054(2) 0.048(2) -0.0031(19) 0.020(2) 0.019(2) C18 0.0348(17) 0.053(2) 0.0437(19) -0.0005(16) -0.0001(14) -0.0006(15) C19 0.0490(19) 0.0395(18) 0.0288(16) 0.0001(14) -0.0032(14) 0.0158(15) C20 0.063(2) 0.041(2) 0.0378(18) -0.0025(16) -0.0099(16) 0.0164(17) C21 0.083(3) 0.054(2) 0.042(2) -0.0157(19) -0.019(2) 0.024(2) C22 0.083(3) 0.065(3) 0.0305(19) -0.0028(19) 0.0003(19) 0.030(2) C23 0.059(2) 0.063(3) 0.0358(19) 0.0055(18) 0.0079(17) 0.0184(19) C24 0.0490(19) 0.047(2) 0.0309(16) 0.0030(15) 0.0022(15) 0.0190(16) C25 0.087(3) 0.041(2) 0.056(2) -0.0077(19) -0.017(2) 0.002(2) C26 0.137(5) 0.104(4) 0.031(2) -0.010(2) 0.006(3) 0.035(4) C27 0.048(2) 0.052(2) 0.0419(19) 0.0081(17) 0.0055(16) 0.0055(17) K1 0.0416(4) 0.0679(5) 0.0238(3) -0.0059(3) 0.0016(3) -0.0078(4) O101 0.0495(13) 0.0455(14) 0.0333(12) -0.0028(10) 0.0050(10) 0.0052(11) O102 0.0515(14) 0.0546(15) 0.0391(13) -0.0008(11) -0.0060(11) -0.0010(12) O103 0.0552(16) 0.0636(18) 0.0555(16) 0.0090(14) 0.0067(13) -0.0043(13) O104 0.0736(18) 0.0666(18) 0.0354(13) 0.0009(13) 0.0149(12) 0.0139(14) O105 0.0679(17) 0.0632(17) 0.0339(13) -0.0059(12) -0.0102(12) 0.0045(14) O106 0.0487(14) 0.0488(15) 0.0446(14) -0.0017(11) -0.0041(11) 0.0012(11) C101 0.074(3) 0.042(2) 0.0269(16) -0.0054(15) 0.0026(16) 0.0095(18) C102 0.074(3) 0.043(2) 0.0360(19) -0.0066(16) -0.0127(18) 0.0050(19) C103 0.049(2) 0.068(3) 0.066(3) -0.009(2) -0.0081(19) -0.012(2) C104 0.050(2) 0.068(3) 0.074(3) 0.004(2) 0.002(2) -0.012(2) C105 0.065(3) 0.082(3) 0.052(2) 0.021(2) 0.019(2) 0.000(2) C106 0.075(3) 0.081(3) 0.045(2) 0.018(2) 0.023(2) 0.023(2) C107 0.109(4) 0.065(3) 0.0244(17) -0.0049(18) 0.009(2) 0.018(3) C108 0.095(3) 0.064(3) 0.033(2) -0.0099(19) -0.011(2) 0.013(2) C109 0.054(2) 0.068(3) 0.056(2) -0.014(2) -0.0141(19) -0.005(2) C110 0.044(2) 0.059(2) 0.061(2) -0.012(2) -0.0050(18) -0.0067(18) C111 0.0420(19) 0.060(2) 0.042(2) 0.0104(18) 0.0026(15) -0.0027(17) C112 0.0440(19) 0.062(2) 0.0369(18) 0.0106(18) 0.0059(15) 0.0114(17) O301 0.0539(17) 0.080(2) 0.0549(17) 0.0079(16) 0.0070(14) 0.0080(15) C301 0.034(5) 0.078(10) 0.110(13) 0.009(7) 0.025(6) 0.018(6) C302 0.052(5) 0.120(10) 0.069(6) 0.036(6) -0.008(4) -0.007(6) C303 0.054(5) 0.072(6) 0.061(5) 0.022(4) -0.009(4) -0.016(4) C304 0.064(7) 0.068(8) 0.042(5) 0.020(5) -0.010(5) -0.023(6) C401 0.100(19) 0.081(14) 0.040(9) 0.018(8) -0.002(9) -0.013(11) C402 0.082(10) 0.106(14) 0.124(17) 0.056(12) 0.030(11) 0.037(10) C403 0.122(13) 0.112(15) 0.114(15) 0.062(13) 0.048(11) 0.054(11) C404 0.083(15) 0.053(11) 0.110(16) 0.026(9) 0.060(12) -0.009(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 2.088(3) . ? Fe1 C19 2.089(3) . ? Fe1 C10 2.089(3) . ? C1 C2 1.405(4) . ? C1 C6 1.414(4) . ? C2 C3 1.394(4) . ? C2 C7 1.518(4) . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C5 1.387(4) . ? C4 C8 1.510(4) . ? C5 C6 1.396(4) . ? C5 H5 0.9500 . ? C6 C9 1.513(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C7 H7D 0.9800 . ? C7 H7E 0.9800 . ? C7 H7F 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8 H8D 0.9800 . ? C8 H8E 0.9800 . ? C8 H8F 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C9 H9D 0.9800 . ? C9 H9E 0.9800 . ? C9 H9F 0.9800 . ? C10 C11 1.407(4) . ? C10 C15 1.407(4) . ? C11 C12 1.395(4) . ? C11 C16 1.519(4) . ? C12 C13 1.384(5) . ? C12 H12 0.9500 . ? C13 C14 1.378(5) . ? C13 C17 1.508(5) . ? C14 C15 1.400(4) . ? C14 H14 0.9500 . ? C15 C18 1.512(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? C16 H16E 0.9800 . ? C16 H16F 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17D 0.9800 . ? C17 H17E 0.9800 . ? C17 H17F 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 H18D 0.9800 . ? C18 H18E 0.9800 . ? C18 H18F 0.9800 . ? C19 C20 1.408(5) . ? C19 C24 1.412(5) . ? C20 C21 1.404(5) . ? C20 C25 1.513(5) . ? C21 C22 1.376(6) . ? C21 H21 0.9500 . ? C22 C23 1.381(6) . ? C22 C26 1.520(5) . ? C23 C24 1.387(5) . ? C23 H23 0.9500 . ? C24 C27 1.507(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25D 0.9800 . ? C25 H25E 0.9800 . ? C25 H25F 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? K1 O105 2.758(3) . ? K1 O102 2.760(2) . ? K1 O101 2.775(2) . ? K1 O301 2.784(3) . ? K1 O104 2.785(2) . ? K1 O106 2.828(3) . ? K1 O103 2.830(3) . ? O101 C112 1.410(4) . ? O101 C101 1.411(4) . ? O102 C102 1.407(4) . ? O102 C103 1.425(4) . ? O103 C104 1.409(5) . ? O103 C105 1.425(4) . ? O104 C106 1.399(5) . ? O104 C107 1.425(5) . ? O105 C108 1.402(4) . ? O105 C109 1.420(5) . ? O106 C110 1.408(4) . ? O106 C111 1.424(4) . ? C101 C102 1.500(5) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.497(6) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.488(6) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.488(6) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.484(5) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.481(5) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? O301 C404 1.32(3) . ? O301 C401 1.35(3) . ? O301 C301 1.470(18) . ? O301 C304 1.498(15) . ? C301 C302 1.56(2) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 C303 1.482(11) . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.520(17) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C401 C402 1.31(3) . ? C401 C404 2.03(4) . ? C401 H40A 0.9900 . ? C401 H40B 0.9900 . ? C402 C403 1.428(19) . ? C402 H40C 0.9900 . ? C402 H40D 0.9900 . ? C403 C404 1.49(3) . ? C403 H40E 0.9900 . ? C403 H40F 0.9900 . ? C404 H40G 0.9900 . ? C404 H40H 0.9900 . ? 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 C1 Fe1 C19 118.08(12) . . ? C1 Fe1 C10 119.97(11) . . ? C19 Fe1 C10 121.93(12) . . ? C2 C1 C6 115.4(3) . . ? C2 C1 Fe1 120.5(2) . . ? C6 C1 Fe1 124.1(2) . . ? C3 C2 C1 121.8(3) . . ? C3 C2 C7 117.9(3) . . ? C1 C2 C7 120.2(3) . . ? C4 C3 C2 122.1(3) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 117.1(3) . . ? C3 C4 C8 120.9(3) . . ? C5 C4 C8 122.0(3) . . ? C4 C5 C6 121.6(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 121.9(3) . . ? C5 C6 C9 118.3(3) . . ? C1 C6 C9 119.8(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C7 H7D 109.5 . . ? H7A C7 H7D 141.1 . . ? H7B C7 H7D 56.3 . . ? H7C C7 H7D 56.3 . . ? C2 C7 H7E 109.5 . . ? H7A C7 H7E 56.3 . . ? H7B C7 H7E 141.1 . . ? H7C C7 H7E 56.3 . . ? H7D C7 H7E 109.5 . . ? C2 C7 H7F 109.5 . . ? H7A C7 H7F 56.3 . . ? H7B C7 H7F 56.3 . . ? H7C C7 H7F 141.1 . . ? H7D C7 H7F 109.5 . . ? H7E C7 H7F 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C8 H8D 109.5 . . ? H8A C8 H8D 141.1 . . ? H8B C8 H8D 56.3 . . ? H8C C8 H8D 56.3 . . ? C4 C8 H8E 109.5 . . ? H8A C8 H8E 56.3 . . ? H8B C8 H8E 141.1 . . ? H8C C8 H8E 56.3 . . ? H8D C8 H8E 109.5 . . ? C4 C8 H8F 109.5 . . ? H8A C8 H8F 56.3 . . ? H8B C8 H8F 56.3 . . ? H8C C8 H8F 141.1 . . ? H8D C8 H8F 109.5 . . ? H8E C8 H8F 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C9 H9D 109.5 . . ? H9A C9 H9D 141.1 . . ? H9B C9 H9D 56.3 . . ? H9C C9 H9D 56.3 . . ? C6 C9 H9E 109.5 . . ? H9A C9 H9E 56.3 . . ? H9B C9 H9E 141.1 . . ? H9C C9 H9E 56.3 . . ? H9D C9 H9E 109.5 . . ? C6 C9 H9F 109.5 . . ? H9A C9 H9F 56.3 . . ? H9B C9 H9F 56.3 . . ? H9C C9 H9F 141.1 . . ? H9D C9 H9F 109.5 . . ? H9E C9 H9F 109.5 . . ? C11 C10 C15 115.8(3) . . ? C11 C10 Fe1 121.7(2) . . ? C15 C10 Fe1 122.5(2) . . ? C12 C11 C10 122.0(3) . . ? C12 C11 C16 117.3(3) . . ? C10 C11 C16 120.6(3) . . ? C13 C12 C11 121.3(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 117.5(3) . . ? C14 C13 C17 121.8(3) . . ? C12 C13 C17 120.7(3) . . ? C13 C14 C15 122.1(3) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C14 C15 C10 121.2(3) . . ? C14 C15 C18 118.6(3) . . ? C10 C15 C18 120.1(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C16 H16D 109.5 . . ? H16A C16 H16D 141.1 . . ? H16B C16 H16D 56.3 . . ? H16C C16 H16D 56.3 . . ? C11 C16 H16E 109.5 . . ? H16A C16 H16E 56.3 . . ? H16B C16 H16E 141.1 . . ? H16C C16 H16E 56.3 . . ? H16D C16 H16E 109.5 . . ? C11 C16 H16F 109.5 . . ? H16A C16 H16F 56.3 . . ? H16B C16 H16F 56.3 . . ? H16C C16 H16F 141.1 . . ? H16D C16 H16F 109.5 . . ? H16E C16 H16F 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C17 H17D 109.5 . . ? H17A C17 H17D 141.1 . . ? H17B C17 H17D 56.3 . . ? H17C C17 H17D 56.3 . . ? C13 C17 H17E 109.5 . . ? H17A C17 H17E 56.3 . . ? H17B C17 H17E 141.1 . . ? H17C C17 H17E 56.3 . . ? H17D C17 H17E 109.5 . . ? C13 C17 H17F 109.5 . . ? H17A C17 H17F 56.3 . . ? H17B C17 H17F 56.3 . . ? H17C C17 H17F 141.1 . . ? H17D C17 H17F 109.5 . . ? H17E C17 H17F 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C18 H18D 109.5 . . ? H18A C18 H18D 141.1 . . ? H18B C18 H18D 56.3 . . ? H18C C18 H18D 56.3 . . ? C15 C18 H18E 109.5 . . ? H18A C18 H18E 56.3 . . ? H18B C18 H18E 141.1 . . ? H18C C18 H18E 56.3 . . ? H18D C18 H18E 109.5 . . ? C15 C18 H18F 109.5 . . ? H18A C18 H18F 56.3 . . ? H18B C18 H18F 56.3 . . ? H18C C18 H18F 141.1 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? C20 C19 C24 115.7(3) . . ? C20 C19 Fe1 120.1(3) . . ? C24 C19 Fe1 124.0(2) . . ? C21 C20 C19 121.0(4) . . ? C21 C20 C25 118.4(4) . . ? C19 C20 C25 120.5(3) . . ? C22 C21 C20 122.0(4) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 117.6(3) . . ? C21 C22 C26 121.0(4) . . ? C23 C22 C26 121.3(4) . . ? C22 C23 C24 121.6(4) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C19 122.0(4) . . ? C23 C24 C27 118.5(3) . . ? C19 C24 C27 119.5(3) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C25 H25D 109.5 . . ? H25A C25 H25D 141.1 . . ? H25B C25 H25D 56.3 . . ? H25C C25 H25D 56.3 . . ? C20 C25 H25E 109.5 . . ? H25A C25 H25E 56.3 . . ? H25B C25 H25E 141.1 . . ? H25C C25 H25E 56.3 . . ? H25D C25 H25E 109.5 . . ? C20 C25 H25F 109.5 . . ? H25A C25 H25F 56.3 . . ? H25B C25 H25F 56.3 . . ? H25C C25 H25F 141.1 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? C22 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? C22 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.3 . . ? C24 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.3 . . ? H27D C27 H27E 109.5 . . ? C24 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.3 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? O105 K1 O102 171.00(8) . . ? O105 K1 O101 118.98(8) . . ? O102 K1 O101 59.97(7) . . ? O105 K1 O301 82.73(8) . . ? O102 K1 O301 106.27(9) . . ? O101 K1 O301 101.72(8) . . ? O105 K1 O104 60.69(9) . . ? O102 K1 O104 119.40(8) . . ? O101 K1 O104 174.67(8) . . ? O301 K1 O104 83.58(8) . . ? O105 K1 O106 61.10(8) . . ? O102 K1 O106 119.70(7) . . ? O101 K1 O106 60.07(7) . . ? O301 K1 O106 80.02(8) . . ? O104 K1 O106 120.89(8) . . ? O105 K1 O103 117.88(8) . . ? O102 K1 O103 59.98(8) . . ? O101 K1 O103 118.18(8) . . ? O301 K1 O103 107.47(9) . . ? O104 K1 O103 60.08(8) . . ? O106 K1 O103 172.43(8) . . ? C112 O101 C101 112.5(3) . . ? C112 O101 K1 115.08(18) . . ? C101 O101 K1 115.93(19) . . ? C102 O102 C103 111.5(3) . . ? C102 O102 K1 117.7(2) . . ? C103 O102 K1 118.1(2) . . ? C104 O103 C105 113.4(3) . . ? C104 O103 K1 112.9(2) . . ? C105 O103 K1 113.3(2) . . ? C106 O104 C107 112.6(3) . . ? C106 O104 K1 116.5(2) . . ? C107 O104 K1 115.7(2) . . ? C108 O105 C109 112.5(3) . . ? C108 O105 K1 113.0(2) . . ? C109 O105 K1 115.5(2) . . ? C110 O106 C111 111.9(3) . . ? C110 O106 K1 111.2(2) . . ? C111 O106 K1 114.42(19) . . ? O101 C101 C102 109.4(3) . . ? O101 C101 H10A 109.8 . . ? C102 C101 H10A 109.8 . . ? O101 C101 H10B 109.8 . . ? C102 C101 H10B 109.8 . . ? H10A C101 H10B 108.2 . . ? O102 C102 C101 109.1(3) . . ? O102 C102 H10C 109.9 . . ? C101 C102 H10C 109.9 . . ? O102 C102 H10D 109.9 . . ? C101 C102 H10D 109.9 . . ? H10C C102 H10D 108.3 . . ? O102 C103 C104 109.0(3) . . ? O102 C103 H10E 109.9 . . ? C104 C103 H10E 109.9 . . ? O102 C103 H10F 109.9 . . ? C104 C103 H10F 109.9 . . ? H10E C103 H10F 108.3 . . ? O103 C104 C103 109.0(3) . . ? O103 C104 H10G 109.9 . . ? C103 C104 H10G 109.9 . . ? O103 C104 H10H 109.9 . . ? C103 C104 H10H 109.9 . . ? H10G C104 H10H 108.3 . . ? O103 C105 C106 110.0(3) . . ? O103 C105 H10I 109.7 . . ? C106 C105 H10I 109.7 . . ? O103 C105 H10J 109.7 . . ? C106 C105 H10J 109.7 . . ? H10I C105 H10J 108.2 . . ? O104 C106 C105 109.1(3) . . ? O104 C106 H10K 109.9 . . ? C105 C106 H10K 109.9 . . ? O104 C106 H10L 109.9 . . ? C105 C106 H10L 109.9 . . ? H10K C106 H10L 108.3 . . ? O104 C107 C108 109.8(3) . . ? O104 C107 H10M 109.7 . . ? C108 C107 H10M 109.7 . . ? O104 C107 H10N 109.7 . . ? C108 C107 H10N 109.7 . . ? H10M C107 H10N 108.2 . . ? O105 C108 C107 108.8(3) . . ? O105 C108 H10O 109.9 . . ? C107 C108 H10O 109.9 . . ? O105 C108 H10P 109.9 . . ? C107 C108 H10P 109.9 . . ? H10O C108 H10P 108.3 . . ? O105 C109 C110 110.1(3) . . ? O105 C109 H10Q 109.6 . . ? C110 C109 H10Q 109.6 . . ? O105 C109 H10R 109.6 . . ? C110 C109 H10R 109.6 . . ? H10Q C109 H10R 108.1 . . ? O106 C110 C109 109.6(3) . . ? O106 C110 H11A 109.8 . . ? C109 C110 H11A 109.8 . . ? O106 C110 H11B 109.8 . . ? C109 C110 H11B 109.8 . . ? H11A C110 H11B 108.2 . . ? O106 C111 C112 109.5(3) . . ? O106 C111 H11C 109.8 . . ? C112 C111 H11C 109.8 . . ? O106 C111 H11D 109.8 . . ? C112 C111 H11D 109.8 . . ? H11C C111 H11D 108.2 . . ? O101 C112 C111 108.9(3) . . ? O101 C112 H11E 109.9 . . ? C111 C112 H11E 109.9 . . ? O101 C112 H11F 109.9 . . ? C111 C112 H11F 109.9 . . ? H11E C112 H11F 108.3 . . ? C404 O301 C401 99.0(16) . . ? C404 O301 C301 102.4(14) . . ? C401 O301 C304 107.8(15) . . ? C301 O301 C304 112.6(11) . . ? C404 O301 K1 134.8(12) . . ? C401 O301 K1 124.4(13) . . ? C301 O301 K1 118.7(9) . . ? C304 O301 K1 127.8(8) . . ? O301 C301 C302 99.9(12) . . ? O301 C301 H30A 111.8 . . ? C302 C301 H30A 111.8 . . ? O301 C301 H30B 111.8 . . ? C302 C301 H30B 111.8 . . ? H30A C301 H30B 109.5 . . ? C303 C302 C301 110.1(10) . . ? C303 C302 H30C 109.6 . . ? C301 C302 H30C 109.6 . . ? C303 C302 H30D 109.6 . . ? C301 C302 H30D 109.6 . . ? H30C C302 H30D 108.1 . . ? C302 C303 C304 106.9(8) . . ? C302 C303 H30E 110.3 . . ? C304 C303 H30E 110.3 . . ? C302 C303 H30F 110.3 . . ? C304 C303 H30F 110.3 . . ? H30E C303 H30F 108.6 . . ? O301 C304 C303 101.8(11) . . ? O301 C304 H30G 111.4 . . ? C303 C304 H30G 111.4 . . ? O301 C304 H30H 111.4 . . ? C303 C304 H30H 111.4 . . ? H30G C304 H30H 109.3 . . ? C402 C401 O301 122(2) . . ? C402 C401 C404 82.9(18) . . ? C402 C401 H40A 106.8 . . ? O301 C401 H40A 106.8 . . ? C404 C401 H40A 115.7 . . ? C402 C401 H40B 106.8 . . ? O301 C401 H40B 106.8 . . ? C404 C401 H40B 131.6 . . ? H40A C401 H40B 106.6 . . ? C401 C402 C403 99.9(18) . . ? C401 C402 H40C 111.8 . . ? C403 C402 H40C 111.8 . . ? C401 C402 H40D 111.8 . . ? C403 C402 H40D 111.8 . . ? H40C C402 H40D 109.5 . . ? C402 C403 C404 102.9(14) . . ? C402 C403 H40E 111.2 . . ? C404 C403 H40E 111.2 . . ? C402 C403 H40F 111.2 . . ? C404 C403 H40F 111.2 . . ? H40E C403 H40F 109.1 . . ? O301 C404 C403 109.3(18) . . ? C403 C404 C401 71.4(14) . . ? O301 C404 H40G 109.8 . . ? C403 C404 H40G 109.8 . . ? C401 C404 H40G 109.7 . . ? O301 C404 H40H 109.8 . . ? C403 C404 H40H 109.8 . . ? C401 C404 H40H 138.7 . . ? H40G C404 H40H 108.3 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.533 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.053 _iucr_refine_instructions_details ; TITL pbcn in Pbcn CELL 1.54178 33.7821 10.7707 24.2239 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0001 0.0003 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, 1/2 + Z SYMM - X, Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O K FE UNIT 344 520 0 56 8 8 MERG 2 OMIT 0.00 133.00 FMAP 2 PLAN 100 SIZE 0.020 0.040 0.300 ACTA BOND $H L.S. 16 TEMP -123.00 WGHT 0.049900 9.443800 FVAR 0.13626 0.59243 FE1 6 0.133944 0.310804 0.363185 11.00000 0.03313 0.03497 = 0.02587 0.00063 0.00054 0.00574 C1 1 0.162074 0.165302 0.404483 11.00000 0.03416 0.02787 = 0.02616 -0.00482 -0.00140 0.00025 C2 1 0.203107 0.147419 0.399154 11.00000 0.03813 0.02710 = 0.02782 -0.00532 -0.00123 -0.00365 C3 1 0.222808 0.052112 0.426774 11.00000 0.03358 0.03214 = 0.03180 -0.00316 -0.00382 0.00299 AFIX 43 H3 2 0.250601 0.043763 0.422098 11.00000 -1.20000 AFIX 0 C4 1 0.203146 -0.030728 0.460793 11.00000 0.04972 0.03030 = 0.02687 -0.00129 -0.00303 0.00331 C5 1 0.162555 -0.015869 0.466127 11.00000 0.04738 0.03516 = 0.02484 0.00040 0.00447 -0.00584 AFIX 43 H5 2 0.148148 -0.071688 0.488893 11.00000 -1.20000 AFIX 0 C6 1 0.142336 0.079123 0.438858 11.00000 0.03916 0.03407 = 0.02518 -0.00428 0.00047 -0.00171 C7 1 0.227275 0.231361 0.361734 11.00000 0.03184 0.03756 = 0.04562 0.00474 -0.00010 0.00253 AFIX 123 H7A 2 0.209936 0.294110 0.345194 10.50000 -1.50000 H7B 2 0.239516 0.181639 0.332468 10.50000 -1.50000 H7C 2 0.247970 0.272512 0.383388 10.50000 -1.50000 H7D 2 0.255012 0.204731 0.362173 10.50000 -1.50000 H7E 2 0.225432 0.317202 0.374899 10.50000 -1.50000 H7F 2 0.216978 0.226328 0.323978 10.50000 -1.50000 AFIX 0 C8 1 0.225319 -0.132815 0.490273 11.00000 0.06296 0.04505 = 0.03976 0.00760 -0.00057 0.01041 AFIX 123 H8A 2 0.253524 -0.127597 0.481102 10.50000 -1.50000 H8B 2 0.214945 -0.213646 0.478623 10.50000 -1.50000 H8C 2 0.221877 -0.123459 0.530227 10.50000 -1.50000 H8D 2 0.206707 -0.182205 0.512199 10.50000 -1.50000 H8E 2 0.245285 -0.096155 0.514678 10.50000 -1.50000 H8F 2 0.238354 -0.186342 0.463074 10.50000 -1.50000 AFIX 0 C9 1 0.097944 0.087498 0.446126 11.00000 0.03723 0.05697 = 0.04202 0.00522 0.00816 -0.00088 AFIX 123 H9A 2 0.087748 0.157920 0.424818 10.50000 -1.50000 H9B 2 0.091715 0.099369 0.485284 10.50000 -1.50000 H9C 2 0.085611 0.010630 0.432984 10.50000 -1.50000 H9D 2 0.088968 0.020693 0.470573 10.50000 -1.50000 H9E 2 0.085001 0.079243 0.410107 10.50000 -1.50000 H9F 2 0.091105 0.167983 0.462406 10.50000 -1.50000 AFIX 0 C10 1 0.101953 0.443037 0.407768 11.00000 0.03584 0.03614 = 0.02167 0.00828 0.00226 0.00564 C11 1 0.120877 0.540693 0.435883 11.00000 0.04336 0.03706 = 0.02188 0.00515 0.00219 0.00220 C12 1 0.099683 0.631200 0.464615 11.00000 0.06228 0.03725 = 0.02435 0.00160 0.00206 -0.00227 AFIX 43 H12 2 0.113591 0.696935 0.482153 11.00000 -1.20000 AFIX 0 C13 1 0.058801 0.627127 0.468079 11.00000 0.05779 0.03577 = 0.02963 0.00488 0.00928 0.01123 C14 1 0.039750 0.530792 0.441693 11.00000 0.03755 0.04664 = 0.03264 0.00919 0.00730 0.01174 AFIX 43 H14 2 0.011748 0.525014 0.444223 11.00000 -1.20000 AFIX 0 C15 1 0.060377 0.441174 0.411274 11.00000 0.03566 0.03836 = 0.02759 0.00617 0.00053 0.00804 C16 1 0.165728 0.550894 0.436162 11.00000 0.04248 0.05794 = 0.03471 -0.00252 -0.00094 -0.00706 AFIX 123 H16A 2 0.177072 0.482558 0.414640 10.50000 -1.50000 H16B 2 0.175405 0.546407 0.474248 10.50000 -1.50000 H16C 2 0.173640 0.630299 0.419778 10.50000 -1.50000 H16D 2 0.173672 0.623618 0.457804 10.50000 -1.50000 H16E 2 0.175339 0.559769 0.398196 10.50000 -1.50000 H16F 2 0.177105 0.475877 0.452666 10.50000 -1.50000 AFIX 0 C17 1 0.036341 0.725318 0.499538 11.00000 0.08045 0.05436 = 0.04809 -0.00308 0.02006 0.01865 AFIX 123 H17A 2 0.055039 0.785478 0.515069 10.50000 -1.50000 H17B 2 0.021325 0.686258 0.529481 10.50000 -1.50000 H17C 2 0.018064 0.768016 0.474505 10.50000 -1.50000 H17D 2 0.007914 0.707690 0.497635 10.50000 -1.50000 H17E 2 0.041627 0.806910 0.483222 10.50000 -1.50000 H17F 2 0.044888 0.725152 0.538198 10.50000 -1.50000 AFIX 0 C18 1 0.037046 0.341567 0.381663 11.00000 0.03477 0.05296 = 0.04371 -0.00045 -0.00005 -0.00062 AFIX 123 H18A 2 0.008715 0.353999 0.388381 10.50000 -1.50000 H18B 2 0.044983 0.259754 0.395480 10.50000 -1.50000 H18C 2 0.042320 0.346397 0.341940 10.50000 -1.50000 H18D 2 0.055297 0.286101 0.362153 10.50000 -1.50000 H18E 2 0.019029 0.380346 0.355054 10.50000 -1.50000 H18F 2 0.021692 0.293703 0.408594 10.50000 -1.50000 AFIX 0 C19 1 0.140264 0.321478 0.277549 11.00000 0.04898 0.03953 = 0.02885 0.00005 -0.00322 0.01575 C20 1 0.122504 0.231517 0.243433 11.00000 0.06267 0.04052 = 0.03783 -0.00250 -0.00992 0.01637 C21 1 0.129597 0.229611 0.186317 11.00000 0.08311 0.05422 = 0.04183 -0.01570 -0.01862 0.02417 AFIX 43 H21 2 0.117700 0.166438 0.164550 11.00000 -1.20000 AFIX 0 C22 1 0.153269 0.316542 0.160939 11.00000 0.08296 0.06502 = 0.03052 -0.00278 0.00034 0.02957 C23 1 0.170222 0.406939 0.193732 11.00000 0.05894 0.06349 = 0.03583 0.00549 0.00786 0.01845 AFIX 43 H23 2 0.186464 0.468478 0.177112 11.00000 -1.20000 AFIX 0 C24 1 0.164118 0.410102 0.250343 11.00000 0.04897 0.04682 = 0.03093 0.00304 0.00218 0.01895 C25 1 0.094785 0.135351 0.267538 11.00000 0.08675 0.04142 = 0.05628 -0.00771 -0.01696 0.00179 AFIX 123 H25A 2 0.092566 0.147970 0.307483 10.50000 -1.50000 H25B 2 0.105240 0.052094 0.260209 10.50000 -1.50000 H25C 2 0.068599 0.143720 0.250529 10.50000 -1.50000 H25D 2 0.085037 0.081219 0.237998 10.50000 -1.50000 H25E 2 0.072364 0.177095 0.285272 10.50000 -1.50000 H25F 2 0.109005 0.085469 0.294952 10.50000 -1.50000 AFIX 0 C26 1 0.159887 0.314160 0.098863 11.00000 0.13689 0.10378 = 0.03070 -0.01047 0.00607 0.03478 AFIX 123 H26A 2 0.177409 0.382705 0.088341 10.50000 -1.50000 H26B 2 0.134431 0.323177 0.079881 10.50000 -1.50000 H26C 2 0.172087 0.235064 0.088357 10.50000 -1.50000 H26D 2 0.145209 0.244592 0.082712 10.50000 -1.50000 H26E 2 0.188187 0.304120 0.091171 10.50000 -1.50000 H26F 2 0.150531 0.392234 0.082696 10.50000 -1.50000 AFIX 0 C27 1 0.183355 0.512335 0.283282 11.00000 0.04818 0.05175 = 0.04186 0.00806 0.00550 0.00555 AFIX 123 H27A 2 0.176604 0.502610 0.322389 10.50000 -1.50000 H27B 2 0.173820 0.592988 0.270096 10.50000 -1.50000 H27C 2 0.212149 0.507884 0.278780 10.50000 -1.50000 H27D 2 0.198445 0.566378 0.258454 10.50000 -1.50000 H27E 2 0.201229 0.476000 0.310748 10.50000 -1.50000 H27F 2 0.162900 0.561104 0.302063 10.50000 -1.50000 AFIX 0 K1 5 0.129563 0.760288 0.190937 11.00000 0.04164 0.06787 = 0.02376 -0.00587 0.00158 -0.00780 O101 4 0.109062 0.731001 0.301113 11.00000 0.04954 0.04552 = 0.03327 -0.00277 0.00503 0.00521 O102 4 0.167627 0.897443 0.271210 11.00000 0.05155 0.05462 = 0.03912 -0.00081 -0.00603 -0.00097 O103 4 0.201350 0.883661 0.166020 11.00000 0.05520 0.06362 = 0.05551 0.00905 0.00674 -0.00427 O104 4 0.155764 0.773801 0.082092 11.00000 0.07357 0.06655 = 0.03536 0.00094 0.01492 0.01390 O105 4 0.100226 0.594817 0.114256 11.00000 0.06785 0.06321 = 0.03387 -0.00594 -0.01021 0.00452 O106 4 0.064123 0.610040 0.219932 11.00000 0.04873 0.04882 = 0.04460 -0.00172 -0.00412 0.00119 C101 1 0.120708 0.827681 0.336883 11.00000 0.07354 0.04168 = 0.02687 -0.00539 0.00263 0.00946 AFIX 23 H10A 2 0.117261 0.801250 0.375729 11.00000 -1.20000 H10B 2 0.103951 0.901701 0.330483 11.00000 -1.20000 AFIX 0 C102 1 0.163292 0.859356 0.326422 11.00000 0.07386 0.04302 = 0.03602 -0.00659 -0.01274 0.00499 AFIX 23 H10C 2 0.171742 0.926870 0.351527 11.00000 -1.20000 H10D 2 0.180136 0.785883 0.333581 11.00000 -1.20000 AFIX 0 C103 1 0.206897 0.939071 0.260223 11.00000 0.04887 0.06808 = 0.06574 -0.00880 -0.00811 -0.01186 AFIX 23 H10E 2 0.225850 0.870158 0.265944 11.00000 -1.20000 H10F 2 0.213926 1.007308 0.285789 11.00000 -1.20000 AFIX 0 C104 1 0.209203 0.983795 0.201811 11.00000 0.04953 0.06825 = 0.07442 0.00389 0.00182 -0.01225 AFIX 23 H10G 2 0.189601 1.050741 0.195736 11.00000 -1.20000 H10H 2 0.235909 1.017645 0.194282 11.00000 -1.20000 AFIX 0 C105 1 0.205187 0.915046 0.109129 11.00000 0.06465 0.08188 = 0.05243 0.02131 0.01854 0.00014 AFIX 23 H10I 2 0.232608 0.942576 0.101506 11.00000 -1.20000 H10J 2 0.187056 0.984334 0.100085 11.00000 -1.20000 AFIX 0 C106 1 0.195537 0.805476 0.074226 11.00000 0.07529 0.08060 = 0.04485 0.01771 0.02269 0.02261 AFIX 23 H10K 2 0.200302 0.825351 0.034881 11.00000 -1.20000 H10L 2 0.212692 0.734640 0.084515 11.00000 -1.20000 AFIX 0 C107 1 0.143321 0.675218 0.046929 11.00000 0.10909 0.06502 = 0.02441 -0.00495 0.00934 0.01752 AFIX 23 H10M 2 0.160837 0.602466 0.052144 11.00000 -1.20000 H10N 2 0.145188 0.701745 0.007886 11.00000 -1.20000 AFIX 0 C108 1 0.101746 0.640392 0.060074 11.00000 0.09503 0.06414 = 0.03329 -0.00990 -0.01074 0.01262 AFIX 23 H10O 2 0.084326 0.713859 0.056467 11.00000 -1.20000 H10P 2 0.092410 0.575992 0.033982 11.00000 -1.20000 AFIX 0 C109 1 0.062947 0.541319 0.127286 11.00000 0.05358 0.06839 = 0.05641 -0.01442 -0.01408 -0.00488 AFIX 23 H10Q 2 0.058302 0.467854 0.103595 11.00000 -1.20000 H10R 2 0.041643 0.602271 0.120002 11.00000 -1.20000 AFIX 0 C110 1 0.061957 0.503728 0.186217 11.00000 0.04422 0.05913 = 0.06117 -0.01191 -0.00497 -0.00670 AFIX 23 H11A 2 0.037158 0.457988 0.194003 11.00000 -1.20000 H11B 2 0.084536 0.448022 0.194295 11.00000 -1.20000 AFIX 0 C111 1 0.061949 0.579553 0.277069 11.00000 0.04199 0.05973 = 0.04200 0.01036 0.00256 -0.00266 AFIX 23 H11C 2 0.081714 0.514671 0.285915 11.00000 -1.20000 H11D 2 0.035330 0.546572 0.285849 11.00000 -1.20000 AFIX 0 C112 1 0.069784 0.691972 0.310510 11.00000 0.04402 0.06179 = 0.03688 0.01064 0.00592 0.01139 AFIX 23 H11E 2 0.051133 0.758826 0.300015 11.00000 -1.20000 H11F 2 0.065948 0.673220 0.350159 11.00000 -1.20000 AFIX 0 O301 4 0.067946 0.908108 0.152139 11.00000 0.05389 0.07963 = 0.05488 0.00793 0.00698 0.00801 PART 1 C301 1 0.028396 0.892883 0.176484 21.00000 0.03441 0.07750 = 0.11019 0.00946 0.02521 0.01779 AFIX 23 H30A 2 0.023140 0.955634 0.205432 21.00000 -1.20000 H30B 2 0.024631 0.808647 0.191972 21.00000 -1.20000 AFIX 0 C302 1 0.002202 0.914513 0.124142 21.00000 0.05201 0.11957 = 0.06925 0.03572 -0.00784 -0.00681 AFIX 23 H30C 2 -0.010365 0.835368 0.112972 21.00000 -1.20000 H30D 2 -0.019041 0.974761 0.132804 21.00000 -1.20000 AFIX 0 C303 1 0.026772 0.962620 0.078199 21.00000 0.05369 0.07195 = 0.06053 0.02224 -0.00863 -0.01582 AFIX 23 H30E 2 0.015033 1.039604 0.063015 21.00000 -1.20000 H30F 2 0.028521 0.900384 0.048224 21.00000 -1.20000 AFIX 0 C304 1 0.067610 0.988870 0.101781 21.00000 0.06441 0.06796 = 0.04225 0.01953 -0.00956 -0.02290 AFIX 23 H30G 2 0.088746 0.964834 0.075566 21.00000 -1.20000 H30H 2 0.070694 1.077595 0.111553 21.00000 -1.20000 AFIX 0 PART 2 C401 1 0.031786 0.914477 0.175461 -21.00000 0.09960 0.08064 = 0.04014 0.01764 -0.00173 -0.01327 AFIX 23 H40A 2 0.021252 0.828734 0.176473 -21.00000 -1.20000 H40B 2 0.035793 0.940168 0.214301 -21.00000 -1.20000 AFIX 0 C402 1 0.003540 0.985167 0.155408 -21.00000 0.08220 0.10646 = 0.12386 0.05603 0.03045 0.03669 AFIX 23 H40C 2 -0.006074 1.045856 0.183020 -21.00000 -1.20000 H40D 2 -0.019011 0.935461 0.141525 -21.00000 -1.20000 AFIX 0 C403 1 0.024545 1.044326 0.111556 -21.00000 0.12243 0.11165 = 0.11428 0.06177 0.04796 0.05400 AFIX 23 H40E 2 0.032186 1.130083 0.121696 -21.00000 -1.20000 H40F 2 0.008508 1.046567 0.077364 -21.00000 -1.20000 AFIX 0 C404 1 0.059990 0.963857 0.104708 -21.00000 0.08349 0.05275 = 0.10962 0.02637 0.05995 -0.00925 AFIX 23 H40G 2 0.054929 0.900917 0.075772 -21.00000 -1.20000 H40H 2 0.082924 1.014769 0.093095 -21.00000 -1.20000 PART 0 HKLF 4 REM pbcn in Pbcn REM R1 = 0.0557 for 5807 Fo > 4sig(Fo) and 0.0808 for all 7773 data REM 506 parameters refined using 0 restraints END WGHT 0.0498 9.4490 REM Highest difference peak 0.533, deepest hole -0.326, 1-sigma level 0.053 Q1 1 0.0670 0.5960 0.1733 11.00000 0.05 0.53 Q2 1 0.1253 0.6429 0.0908 11.00000 0.05 0.50 Q3 1 0.1967 0.8949 0.2178 11.00000 0.05 0.43 Q4 1 0.0859 0.6683 0.2772 11.00000 0.05 0.39 Q5 1 0.1379 0.8575 0.2946 11.00000 0.05 0.39 Q6 1 0.1786 0.8313 0.1037 11.00000 0.05 0.32 Q7 1 0.1465 0.6767 0.1968 11.00000 0.05 0.32 Q8 1 0.0517 0.5106 0.4106 11.00000 0.05 0.30 Q9 1 0.1239 0.2264 0.3467 11.00000 0.05 0.29 Q10 1 0.1460 0.2180 0.3892 11.00000 0.05 0.29 Q11 1 0.1728 0.4736 0.4305 11.00000 0.05 0.26 Q12 1 0.0371 0.2484 0.4143 11.00000 0.05 0.25 Q13 1 0.1018 0.3097 0.3622 11.00000 0.05 0.25 Q14 1 0.0609 0.5220 0.2285 11.00000 0.05 0.25 Q15 1 0.1280 0.3984 0.3434 11.00000 0.05 0.24 Q16 1 0.1147 0.3802 0.4087 11.00000 0.05 0.24 Q17 1 0.2114 0.2017 0.3964 11.00000 0.05 0.23 Q18 1 0.1384 0.8427 0.1845 11.00000 0.05 0.23 Q19 1 0.2086 -0.0968 0.4673 11.00000 0.05 0.22 Q20 1 0.2090 0.0855 0.4004 11.00000 0.05 0.22 Q21 1 0.2108 0.1160 0.4225 11.00000 0.05 0.22 Q22 1 0.2112 0.0340 0.4576 11.00000 0.05 0.22 Q23 1 0.1359 0.3063 0.3190 11.00000 0.05 0.22 Q24 1 0.1659 0.3112 0.3647 11.00000 0.05 0.21 Q25 1 0.0802 0.4556 0.4006 11.00000 0.05 0.21 Q26 1 0.1484 0.3974 0.3590 11.00000 0.05 0.21 Q27 1 0.0924 0.0503 0.2477 11.00000 0.05 0.21 Q28 1 0.0492 0.3999 0.3966 11.00000 0.05 0.20 Q29 1 0.2032 0.7123 0.0715 11.00000 0.05 0.20 Q30 1 0.1418 0.5464 0.4375 11.00000 0.05 0.20 Q31 1 0.2261 -0.2105 0.4687 11.00000 0.05 0.19 Q32 1 0.0461 0.3092 0.3461 11.00000 0.05 0.19 Q33 1 0.0709 0.6013 0.1006 11.00000 0.05 0.19 Q34 1 0.0109 0.3365 0.3730 11.00000 0.05 0.19 Q35 1 0.0340 1.0292 0.1967 11.00000 0.05 0.19 Q36 1 0.1777 0.2464 0.3951 11.00000 0.05 0.18 Q37 1 0.0874 0.2532 0.3771 11.00000 0.05 0.18 Q38 1 0.1481 0.2009 0.0871 11.00000 0.05 0.18 Q39 1 0.1584 0.0890 0.4104 11.00000 0.05 0.18 Q40 1 0.1470 0.0030 0.4333 11.00000 0.05 0.18 Q41 1 0.2175 0.9595 0.1496 11.00000 0.05 0.18 Q42 1 0.2030 0.7830 0.1665 11.00000 0.05 0.18 Q43 1 0.0661 0.1694 0.2687 11.00000 0.05 0.18 Q44 1 0.1251 0.2974 0.2610 11.00000 0.05 0.18 Q45 1 0.1327 0.1314 0.3631 11.00000 0.05 0.18 Q46 1 0.1845 0.1482 0.3968 11.00000 0.05 0.18 Q47 1 0.1245 0.0857 0.4416 11.00000 0.05 0.18 Q48 1 0.1201 0.8467 0.1846 11.00000 0.05 0.18 Q49 1 0.1743 0.6091 0.4763 11.00000 0.05 0.18 Q50 1 0.1142 0.6017 0.4466 11.00000 0.05 0.18 Q51 1 0.0798 0.2991 0.2943 11.00000 0.05 0.18 Q52 1 0.2189 0.8331 0.2465 11.00000 0.05 0.18 Q53 1 0.0860 0.3844 0.3618 11.00000 0.05 0.17 Q54 1 -0.0242 0.9064 0.1224 11.00000 0.05 0.17 Q55 1 0.1276 0.8612 0.2177 11.00000 0.05 0.17 Q56 1 0.1130 0.4994 0.4109 11.00000 0.05 0.17 Q57 1 0.1252 0.3153 0.1669 11.00000 0.05 0.17 Q58 1 0.1711 0.7034 0.0517 11.00000 0.05 0.17 Q59 1 0.1478 0.0338 0.4607 11.00000 0.05 0.17 Q60 1 0.0319 0.4423 0.4098 11.00000 0.05 0.16 Q61 1 0.0501 0.5615 0.4652 11.00000 0.05 0.16 Q62 1 0.1717 0.6152 0.4072 11.00000 0.05 0.16 Q63 1 0.1715 0.3251 0.2732 11.00000 0.05 0.16 Q64 1 0.2016 0.3596 0.0897 11.00000 0.05 0.16 Q65 1 0.0000 0.2245 0.2500 10.50000 0.05 0.16 Q66 1 0.2049 0.3250 0.4017 11.00000 0.05 0.16 Q67 1 0.1023 0.4422 0.4301 11.00000 0.05 0.16 Q68 1 0.0487 0.6742 0.4872 11.00000 0.05 0.16 Q69 1 0.0607 0.7810 0.3086 11.00000 0.05 0.16 Q70 1 0.0862 -0.0247 0.4707 11.00000 0.05 0.15 Q71 1 0.1049 0.6362 0.4834 11.00000 0.05 0.15 Q72 1 0.1977 0.5275 0.1791 11.00000 0.05 0.15 Q73 1 0.1635 0.5624 0.3159 11.00000 0.05 0.15 Q74 1 0.2241 0.8546 0.1349 11.00000 0.05 0.15 Q75 1 0.0998 0.5143 0.0927 11.00000 0.05 0.15 Q76 1 0.2028 0.6218 0.0369 11.00000 0.05 0.15 Q77 1 0.2207 0.8334 0.1237 11.00000 0.05 0.15 Q78 1 0.1620 0.1757 0.4269 11.00000 0.05 0.14 Q79 1 0.0593 0.8495 0.1274 11.00000 0.05 0.14 Q80 1 0.1348 0.4946 0.3586 11.00000 0.05 0.14 Q81 1 0.1532 -0.0569 0.4727 11.00000 0.05 0.14 Q82 1 0.0567 0.6100 0.4437 11.00000 0.05 0.14 Q83 1 0.1405 0.6826 0.0221 11.00000 0.05 0.14 Q84 1 0.1005 0.6854 0.4604 11.00000 0.05 0.14 Q85 1 0.1500 0.6857 0.1134 11.00000 0.05 0.14 Q86 1 0.0325 0.8230 0.2101 11.00000 0.05 0.14 Q87 1 0.0727 0.5003 0.2909 11.00000 0.05 0.14 Q88 1 0.1811 0.3981 0.3590 11.00000 0.05 0.14 Q89 1 0.1489 0.9579 0.1516 11.00000 0.05 0.14 Q90 1 0.2038 1.0451 0.2761 11.00000 0.05 0.14 Q91 1 0.1265 0.4098 0.0882 11.00000 0.05 0.14 Q92 1 0.1961 0.4036 0.2804 11.00000 0.05 0.14 Q93 1 0.2675 0.1174 0.4350 11.00000 0.05 0.14 Q94 1 0.0889 0.8372 0.1510 11.00000 0.05 0.14 Q95 1 0.1566 -0.1091 0.4299 11.00000 0.05 0.13 Q96 1 0.1170 0.9020 0.3390 11.00000 0.05 0.13 Q97 1 0.0307 0.5629 0.2521 11.00000 0.05 0.13 Q98 1 0.0776 0.6994 0.1957 11.00000 0.05 0.13 Q99 1 0.1280 0.2551 0.2862 11.00000 0.05 0.13 Q100 1 0.1548 0.5701 0.3278 11.00000 0.05 0.13 ; _database_code_depnum_ccdc_archive 'CCDC 962250' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)][Fe(Et3Al:aIPr-H)(aIPr-H)(mes)]*0.5THF ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C69 H96 Al Fe N4, C18 H36 K N2 O6, 0.5(C4 H8 O)' _chemical_formula_sum 'C89 H136 Al Fe K N6 O6.50' _chemical_formula_weight 1515.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.80940(10) _cell_length_b 25.7657(4) _cell_length_c 31.1703(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.2910(10) _cell_angle_gamma 90.00 _cell_volume 8656.96(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14220 _cell_measurement_theta_min 2.8409 _cell_measurement_theta_max 76.3333 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 2.344 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6514 _exptl_absorpt_correction_T_max 0.8722 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5035 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 42401 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 66.50 _reflns_number_total 15228 _reflns_number_gt 11934 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^ > 2\s(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^)+(0.0789P)^2^+0.7960P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 15228 _refine_ls_number_parameters 964 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.114 _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 0.19517(3) 0.254180(15) 0.587110(11) 0.02557(10) Uani 1 1 d . . . Al1 Al 0.45269(7) 0.25372(3) 0.40932(2) 0.03405(17) Uani 1 1 d . . . N1 N 0.32864(17) 0.18082(8) 0.47557(6) 0.0263(4) Uani 1 1 d . . . N2 N 0.32547(16) 0.25948(8) 0.49661(6) 0.0241(4) Uani 1 1 d . . . N3 N 0.19626(16) 0.34763(8) 0.65596(6) 0.0236(4) Uani 1 1 d . . . N4 N 0.22263(16) 0.41492(8) 0.61902(6) 0.0242(4) Uani 1 1 d . . . C1 C 0.35790(19) 0.22954(9) 0.46313(7) 0.0253(5) Uani 1 1 d . . . C2 C 0.2795(2) 0.18179(10) 0.51578(7) 0.0289(5) Uani 1 1 d . . . H2 H 0.2532 0.1521 0.5307 0.035 Uiso 1 1 calc R . . C3 C 0.2751(2) 0.23139(10) 0.53031(7) 0.0267(5) Uani 1 1 d . . . C4 C 0.3322(2) 0.13412(10) 0.45005(7) 0.0291(5) Uani 1 1 d . . . C5 C 0.4384(3) 0.10278(11) 0.45379(9) 0.0387(6) Uani 1 1 d . . . C6 C 0.4356(3) 0.05718(12) 0.42913(10) 0.0444(6) Uani 1 1 d . . . H6 H 0.5059 0.0349 0.4309 0.053 Uiso 1 1 calc R . . C7 C 0.3339(3) 0.04406(12) 0.40265(10) 0.0478(7) Uani 1 1 d . . . H7 H 0.3346 0.0131 0.3861 0.057 Uiso 1 1 calc R . . C8 C 0.2303(3) 0.07548(12) 0.39972(10) 0.0461(7) Uani 1 1 d . . . H8 H 0.1602 0.0657 0.3813 0.055 Uiso 1 1 calc R . . C9 C 0.2264(2) 0.12129(11) 0.42326(8) 0.0355(6) Uani 1 1 d . . . C10 C 0.5531(3) 0.11582(15) 0.48224(11) 0.0568(9) Uani 1 1 d . . . H10 H 0.5390 0.1490 0.4978 0.068 Uiso 1 1 calc R . . C11 C 0.6659(3) 0.12199(15) 0.45613(12) 0.0612(9) Uani 1 1 d . . . H11A H 0.7388 0.1304 0.4755 0.092 Uiso 0.50 1 calc PR . . H11B H 0.6508 0.1500 0.4352 0.092 Uiso 0.50 1 calc PR . . H11C H 0.6806 0.0895 0.4410 0.092 Uiso 0.50 1 calc PR . . H11D H 0.6413 0.1162 0.4256 0.092 Uiso 0.50 1 calc PR . . H11E H 0.7293 0.0966 0.4659 0.092 Uiso 0.50 1 calc PR . . H11F H 0.6996 0.1571 0.4601 0.092 Uiso 0.50 1 calc PR . . C12 C 0.5826(4) 0.0723(2) 0.51531(11) 0.0829(14) Uani 1 1 d . . . H12A H 0.6569 0.0816 0.5337 0.124 Uiso 0.50 1 calc PR . . H12B H 0.5974 0.0398 0.5002 0.124 Uiso 0.50 1 calc PR . . H12C H 0.5124 0.0679 0.5331 0.124 Uiso 0.50 1 calc PR . . H12D H 0.5209 0.0446 0.5110 0.124 Uiso 0.50 1 calc PR . . H12E H 0.5804 0.0864 0.5445 0.124 Uiso 0.50 1 calc PR . . H12F H 0.6654 0.0583 0.5115 0.124 Uiso 0.50 1 calc PR . . C13 C 0.1121(3) 0.15553(13) 0.41978(10) 0.0469(7) Uani 1 1 d . . . H13 H 0.1389 0.1917 0.4274 0.056 Uiso 1 1 calc R . . C14 C 0.0480(3) 0.15668(17) 0.37449(11) 0.0614(9) Uani 1 1 d . . . H14A H -0.0246 0.1795 0.3740 0.092 Uiso 0.50 1 calc PR . . H14B H 0.0214 0.1215 0.3661 0.092 Uiso 0.50 1 calc PR . . H14C H 0.1059 0.1697 0.3543 0.092 Uiso 0.50 1 calc PR . . H14D H 0.0931 0.1343 0.3556 0.092 Uiso 0.50 1 calc PR . . H14E H 0.0470 0.1923 0.3635 0.092 Uiso 0.50 1 calc PR . . H14F H -0.0374 0.1441 0.3753 0.092 Uiso 0.50 1 calc PR . . C15 C 0.0184(3) 0.1388(2) 0.45111(12) 0.0800(14) Uani 1 1 d . . . H15A H -0.0538 0.1619 0.4482 0.120 Uiso 0.50 1 calc PR . . H15B H 0.0566 0.1407 0.4806 0.120 Uiso 0.50 1 calc PR . . H15C H -0.0081 0.1031 0.4447 0.120 Uiso 0.50 1 calc PR . . H15D H 0.0503 0.1086 0.4675 0.120 Uiso 0.50 1 calc PR . . H15E H -0.0601 0.1298 0.4351 0.120 Uiso 0.50 1 calc PR . . H15F H 0.0046 0.1674 0.4710 0.120 Uiso 0.50 1 calc PR . . C16 C 0.3250(2) 0.31519(9) 0.49464(7) 0.0247(4) Uani 1 1 d . . . C17 C 0.4327(2) 0.34294(10) 0.50776(7) 0.0294(5) Uani 1 1 d . . . C18 C 0.4274(2) 0.39670(11) 0.50386(8) 0.0367(6) Uani 1 1 d . . . H18 H 0.4995 0.4167 0.5117 0.044 Uiso 1 1 calc R . . C19 C 0.3194(3) 0.42174(11) 0.48883(8) 0.0389(6) Uani 1 1 d . . . H19 H 0.3176 0.4585 0.4869 0.047 Uiso 1 1 calc R . . C20 C 0.2144(2) 0.39337(10) 0.47669(8) 0.0351(5) Uani 1 1 d . . . H20 H 0.1407 0.4109 0.4665 0.042 Uiso 1 1 calc R . . C21 C 0.2146(2) 0.33963(10) 0.47912(7) 0.0287(5) Uani 1 1 d . . . C22 C 0.5492(2) 0.31504(11) 0.52655(8) 0.0364(6) Uani 1 1 d . . . H22 H 0.5576 0.2820 0.5102 0.044 Uiso 1 1 calc R . . C23 C 0.6680(3) 0.34661(15) 0.52324(11) 0.0540(8) Uani 1 1 d . . . H23A H 0.7392 0.3267 0.5356 0.081 Uiso 0.50 1 calc PR . . H23B H 0.6619 0.3793 0.5391 0.081 Uiso 0.50 1 calc PR . . H23C H 0.6791 0.3541 0.4929 0.081 Uiso 0.50 1 calc PR . . H23D H 0.6475 0.3800 0.5095 0.081 Uiso 0.50 1 calc PR . . H23E H 0.7249 0.3274 0.5060 0.081 Uiso 0.50 1 calc PR . . H23F H 0.7077 0.3526 0.5521 0.081 Uiso 0.50 1 calc PR . . C24 C 0.5376(2) 0.30110(14) 0.57378(9) 0.0469(7) Uani 1 1 d . . . H24A H 0.6128 0.2830 0.5851 0.070 Uiso 0.50 1 calc PR . . H24B H 0.4655 0.2785 0.5761 0.070 Uiso 0.50 1 calc PR . . H24C H 0.5269 0.3329 0.5904 0.070 Uiso 0.50 1 calc PR . . H24D H 0.4573 0.3132 0.5826 0.070 Uiso 0.50 1 calc PR . . H24E H 0.6046 0.3178 0.5917 0.070 Uiso 0.50 1 calc PR . . H24F H 0.5433 0.2634 0.5774 0.070 Uiso 0.50 1 calc PR . . C25 C 0.0982(2) 0.30918(11) 0.46500(8) 0.0324(5) Uani 1 1 d . . . H25 H 0.1131 0.2720 0.4731 0.039 Uiso 1 1 calc R . . C26 C 0.0707(3) 0.31158(13) 0.41625(8) 0.0443(7) Uani 1 1 d . . . H26A H -0.0043 0.2915 0.4081 0.067 Uiso 0.50 1 calc PR . . H26B H 0.1409 0.2970 0.4021 0.067 Uiso 0.50 1 calc PR . . H26C H 0.0579 0.3478 0.4073 0.067 Uiso 0.50 1 calc PR . . H26D H 0.1340 0.3327 0.4036 0.067 Uiso 0.50 1 calc PR . . H26E H -0.0112 0.3271 0.4096 0.067 Uiso 0.50 1 calc PR . . H26F H 0.0718 0.2764 0.4043 0.067 Uiso 0.50 1 calc PR . . C27 C -0.0136(2) 0.32828(12) 0.48777(9) 0.0406(6) Uani 1 1 d . . . H27A H -0.0869 0.3078 0.4781 0.061 Uiso 0.50 1 calc PR . . H27B H -0.0289 0.3649 0.4808 0.061 Uiso 0.50 1 calc PR . . H27C H 0.0031 0.3244 0.5189 0.061 Uiso 0.50 1 calc PR . . H27D H 0.0118 0.3569 0.5071 0.061 Uiso 0.50 1 calc PR . . H27E H -0.0462 0.2998 0.5044 0.061 Uiso 0.50 1 calc PR . . H27F H -0.0782 0.3404 0.4663 0.061 Uiso 0.50 1 calc PR . . C28 C 0.20533(19) 0.40031(9) 0.66027(7) 0.0262(5) Uani 1 1 d . . . C29 C 0.20728(19) 0.32798(10) 0.61367(7) 0.0255(5) Uani 1 1 d . . . C30 C 0.22320(19) 0.37236(9) 0.59116(7) 0.0253(4) Uani 1 1 d . . . H30 H 0.2332 0.3742 0.5612 0.030 Uiso 1 1 calc R . . C31 C 0.1776(2) 0.31608(10) 0.69307(7) 0.0288(5) Uani 1 1 d . . . C32 C 0.2761(3) 0.30927(10) 0.72460(8) 0.0353(5) Uani 1 1 d . . . C33 C 0.2533(3) 0.28005(12) 0.76088(8) 0.0459(7) Uani 1 1 d . . . H33 H 0.3181 0.2748 0.7828 0.055 Uiso 1 1 calc R . . C34 C 0.1373(3) 0.25862(12) 0.76540(9) 0.0512(8) Uani 1 1 d . . . H34 H 0.1237 0.2387 0.7903 0.061 Uiso 1 1 calc R . . C35 C 0.0420(3) 0.26576(12) 0.73446(9) 0.0456(7) Uani 1 1 d . . . H35 H -0.0367 0.2506 0.7380 0.055 Uiso 1 1 calc R . . C36 C 0.0596(2) 0.29522(10) 0.69775(8) 0.0332(5) Uani 1 1 d . . . C37 C 0.4022(3) 0.33344(12) 0.71936(9) 0.0426(6) Uani 1 1 d . . . H37 H 0.3878 0.3702 0.7100 0.051 Uiso 1 1 calc R . . C38 C 0.4695(3) 0.30646(15) 0.68458(10) 0.0520(8) Uani 1 1 d . . . H38A H 0.5502 0.3231 0.6821 0.078 Uiso 0.50 1 calc PR . . H38B H 0.4198 0.3091 0.6570 0.078 Uiso 0.50 1 calc PR . . H38C H 0.4819 0.2698 0.6922 0.078 Uiso 0.50 1 calc PR . . H38D H 0.4178 0.2782 0.6721 0.078 Uiso 0.50 1 calc PR . . H38E H 0.5481 0.2922 0.6971 0.078 Uiso 0.50 1 calc PR . . H38F H 0.4861 0.3315 0.6620 0.078 Uiso 0.50 1 calc PR . . C39 C 0.4866(3) 0.33465(16) 0.76108(11) 0.0645(10) Uani 1 1 d . . . H39A H 0.5660 0.3507 0.7556 0.097 Uiso 0.50 1 calc PR . . H39B H 0.5011 0.2991 0.7715 0.097 Uiso 0.50 1 calc PR . . H39C H 0.4468 0.3548 0.7828 0.097 Uiso 0.50 1 calc PR . . H39D H 0.4432 0.3191 0.7844 0.097 Uiso 0.50 1 calc PR . . H39E H 0.5082 0.3707 0.7684 0.097 Uiso 0.50 1 calc PR . . H39F H 0.5625 0.3150 0.7571 0.097 Uiso 0.50 1 calc PR . . C40 C -0.0486(2) 0.30671(12) 0.66535(9) 0.0386(6) Uani 1 1 d . . . H40 H -0.0148 0.3109 0.6366 0.046 Uiso 1 1 calc R . . C41 C -0.1469(3) 0.26382(14) 0.66136(12) 0.0546(8) Uani 1 1 d . . . H41A H -0.1078 0.2310 0.6540 0.082 Uiso 0.50 1 calc PR . . H41B H -0.2110 0.2730 0.6388 0.082 Uiso 0.50 1 calc PR . . H41C H -0.1847 0.2600 0.6888 0.082 Uiso 0.50 1 calc PR . . H41D H -0.2279 0.2783 0.6670 0.082 Uiso 0.50 1 calc PR . . H41E H -0.1247 0.2363 0.6823 0.082 Uiso 0.50 1 calc PR . . H41F H -0.1510 0.2493 0.6322 0.082 Uiso 0.50 1 calc PR . . C42 C -0.1095(3) 0.35828(13) 0.67652(11) 0.0515(7) Uani 1 1 d . . . H42A H -0.1789 0.3656 0.6553 0.077 Uiso 0.50 1 calc PR . . H42B H -0.0483 0.3863 0.6761 0.077 Uiso 0.50 1 calc PR . . H42C H -0.1403 0.3559 0.7052 0.077 Uiso 0.50 1 calc PR . . H42D H -0.0661 0.3729 0.7025 0.077 Uiso 0.50 1 calc PR . . H42E H -0.1967 0.3522 0.6817 0.077 Uiso 0.50 1 calc PR . . H42F H -0.1047 0.3826 0.6526 0.077 Uiso 0.50 1 calc PR . . C43 C 0.2268(2) 0.46841(10) 0.60581(7) 0.0284(5) Uani 1 1 d . . . C44 C 0.3409(2) 0.49178(10) 0.59965(7) 0.0302(5) Uani 1 1 d . . . C45 C 0.3405(3) 0.54403(11) 0.58755(9) 0.0404(6) Uani 1 1 d . . . H45 H 0.4167 0.5607 0.5829 0.048 Uiso 1 1 calc R . . C46 C 0.2310(3) 0.57191(12) 0.58231(10) 0.0473(7) Uani 1 1 d . . . H46 H 0.2325 0.6076 0.5748 0.057 Uiso 1 1 calc R . . C47 C 0.1195(3) 0.54768(12) 0.58805(10) 0.0472(7) Uani 1 1 d . . . H47 H 0.0446 0.5669 0.5841 0.057 Uiso 1 1 calc R . . C48 C 0.1150(2) 0.49553(11) 0.59955(8) 0.0361(6) Uani 1 1 d . . . C49 C 0.4613(2) 0.46144(11) 0.60657(8) 0.0346(5) Uani 1 1 d . . . H49 H 0.4455 0.4254 0.5955 0.042 Uiso 1 1 calc R . . C50 C 0.5657(3) 0.48457(13) 0.58225(10) 0.0481(7) Uani 1 1 d . . . H50A H 0.6409 0.4636 0.5877 0.072 Uiso 0.50 1 calc PR . . H50B H 0.5821 0.5202 0.5921 0.072 Uiso 0.50 1 calc PR . . H50C H 0.5411 0.4847 0.5513 0.072 Uiso 0.50 1 calc PR . . H50D H 0.5351 0.5154 0.5664 0.072 Uiso 0.50 1 calc PR . . H50E H 0.5940 0.4588 0.5620 0.072 Uiso 0.50 1 calc PR . . H50F H 0.6350 0.4943 0.6027 0.072 Uiso 0.50 1 calc PR . . C51 C 0.5027(2) 0.45762(13) 0.65427(9) 0.0436(6) Uani 1 1 d . . . H51A H 0.5803 0.4379 0.6579 0.065 Uiso 0.50 1 calc PR . . H51B H 0.4385 0.4400 0.6694 0.065 Uiso 0.50 1 calc PR . . H51C H 0.5159 0.4926 0.6661 0.065 Uiso 0.50 1 calc PR . . H51D H 0.4429 0.4757 0.6711 0.065 Uiso 0.50 1 calc PR . . H51E H 0.5846 0.4737 0.6596 0.065 Uiso 0.50 1 calc PR . . H51F H 0.5072 0.4210 0.6628 0.065 Uiso 0.50 1 calc PR . . C52 C -0.0091(2) 0.46926(12) 0.60340(10) 0.0446(7) Uani 1 1 d . . . H52 H 0.0067 0.4347 0.6174 0.054 Uiso 1 1 calc R . . C53 C -0.0736(3) 0.46010(15) 0.55879(12) 0.0605(9) Uani 1 1 d . . . H53A H -0.1535 0.4430 0.5616 0.091 Uiso 0.50 1 calc PR . . H53B H -0.0213 0.4380 0.5420 0.091 Uiso 0.50 1 calc PR . . H53C H -0.0874 0.4935 0.5441 0.091 Uiso 0.50 1 calc PR . . H53D H -0.0213 0.4733 0.5369 0.091 Uiso 0.50 1 calc PR . . H53E H -0.1535 0.4783 0.5565 0.091 Uiso 0.50 1 calc PR . . H53F H -0.0874 0.4228 0.5544 0.091 Uiso 0.50 1 calc PR . . C54 C -0.0925(3) 0.50041(18) 0.63120(12) 0.0644(10) Uani 1 1 d . . . H54A H -0.1713 0.4821 0.6330 0.097 Uiso 0.50 1 calc PR . . H54B H -0.1082 0.5347 0.6183 0.097 Uiso 0.50 1 calc PR . . H54C H -0.0515 0.5045 0.6601 0.097 Uiso 0.50 1 calc PR . . H54D H -0.0493 0.5321 0.6413 0.097 Uiso 0.50 1 calc PR . . H54E H -0.1125 0.4795 0.6560 0.097 Uiso 0.50 1 calc PR . . H54F H -0.1692 0.5097 0.6142 0.097 Uiso 0.50 1 calc PR . . C55 C 0.0939(2) 0.19315(10) 0.60983(8) 0.0304(5) Uani 1 1 d . . . C56 C 0.1335(2) 0.16422(10) 0.64699(8) 0.0329(5) Uani 1 1 d . . . C57 C 0.0675(3) 0.12106(11) 0.66003(9) 0.0397(6) Uani 1 1 d . . . H57 H 0.0964 0.1029 0.6854 0.048 Uiso 1 1 calc R . . C58 C -0.0392(3) 0.10420(11) 0.63680(10) 0.0438(6) Uani 1 1 d . . . C59 C -0.0815(2) 0.13286(12) 0.60072(10) 0.0434(6) Uani 1 1 d . . . H59 H -0.1556 0.1225 0.5847 0.052 Uiso 1 1 calc R . . C60 C -0.0176(2) 0.17621(11) 0.58779(8) 0.0358(5) Uani 1 1 d . . . C61 C 0.2475(3) 0.18054(11) 0.67479(9) 0.0398(6) Uani 1 1 d . . . H61A H 0.2848 0.2110 0.6621 0.060 Uiso 0.50 1 calc PR . . H61B H 0.3076 0.1520 0.6766 0.060 Uiso 0.50 1 calc PR . . H61C H 0.2239 0.1892 0.7037 0.060 Uiso 0.50 1 calc PR . . H61D H 0.2594 0.1571 0.6995 0.060 Uiso 0.50 1 calc PR . . H61E H 0.2366 0.2161 0.6850 0.060 Uiso 0.50 1 calc PR . . H61F H 0.3203 0.1790 0.6579 0.060 Uiso 0.50 1 calc PR . . C62 C -0.1058(3) 0.05555(13) 0.64963(14) 0.0633(9) Uani 1 1 d . . . H62A H -0.0630 0.0409 0.6757 0.095 Uiso 0.50 1 calc PR . . H62B H -0.1061 0.0301 0.6263 0.095 Uiso 0.50 1 calc PR . . H62C H -0.1915 0.0642 0.6552 0.095 Uiso 0.50 1 calc PR . . H62D H -0.1774 0.0492 0.6291 0.095 Uiso 0.50 1 calc PR . . H62E H -0.1343 0.0600 0.6785 0.095 Uiso 0.50 1 calc PR . . H62F H -0.0490 0.0259 0.6496 0.095 Uiso 0.50 1 calc PR . . C63 C -0.0736(3) 0.20749(13) 0.54998(9) 0.0479(7) Uani 1 1 d . . . H63A H -0.0190 0.2368 0.5445 0.072 Uiso 0.50 1 calc PR . . H63B H -0.1551 0.2206 0.5566 0.072 Uiso 0.50 1 calc PR . . H63C H -0.0828 0.1853 0.5244 0.072 Uiso 0.50 1 calc PR . . H63D H -0.1523 0.1917 0.5391 0.072 Uiso 0.50 1 calc PR . . H63E H -0.0161 0.2078 0.5271 0.072 Uiso 0.50 1 calc PR . . H63F H -0.0885 0.2431 0.5593 0.072 Uiso 0.50 1 calc PR . . C64 C 0.4044(3) 0.32561(11) 0.38997(8) 0.0396(6) Uani 1 1 d . . . H64A H 0.3182 0.3252 0.3767 0.048 Uiso 1 1 calc R . . H64B H 0.4069 0.3489 0.4153 0.048 Uiso 1 1 calc R . . C65 C 0.4908(3) 0.34663(12) 0.35750(9) 0.0432(6) Uani 1 1 d . . . H65A H 0.4647 0.3817 0.3488 0.065 Uiso 0.50 1 calc PR . . H65B H 0.4873 0.3240 0.3322 0.065 Uiso 0.50 1 calc PR . . H65C H 0.5759 0.3477 0.3707 0.065 Uiso 0.50 1 calc PR . . H65D H 0.5539 0.3205 0.3523 0.065 Uiso 0.50 1 calc PR . . H65E H 0.5313 0.3783 0.3689 0.065 Uiso 0.50 1 calc PR . . H65F H 0.4426 0.3546 0.3304 0.065 Uiso 0.50 1 calc PR . . C66 C 0.6361(3) 0.25666(13) 0.43025(10) 0.0460(7) Uani 1 1 d . . . H66A H 0.6554 0.2920 0.4413 0.055 Uiso 1 1 calc R . . H66B H 0.6511 0.2322 0.4546 0.055 Uiso 1 1 calc R . . C67 C 0.7250(3) 0.24353(16) 0.39591(12) 0.0609(9) Uani 1 1 d . . . H67A H 0.8108 0.2458 0.4084 0.091 Uiso 0.50 1 calc PR . . H67B H 0.7128 0.2681 0.3720 0.091 Uiso 0.50 1 calc PR . . H67C H 0.7085 0.2082 0.3853 0.091 Uiso 0.50 1 calc PR . . H67D H 0.6773 0.2356 0.3687 0.091 Uiso 0.50 1 calc PR . . H67E H 0.7752 0.2133 0.4052 0.091 Uiso 0.50 1 calc PR . . H67F H 0.7796 0.2732 0.3918 0.091 Uiso 0.50 1 calc PR . . C68 C 0.4212(3) 0.20331(12) 0.36129(9) 0.0437(6) Uani 1 1 d . . . H68A H 0.5005 0.1966 0.3483 0.052 Uiso 1 1 calc R . . H68B H 0.3934 0.1701 0.3734 0.052 Uiso 1 1 calc R . . C69 C 0.3246(3) 0.22049(15) 0.32543(11) 0.0573(8) Uani 1 1 d . . . H69A H 0.3151 0.1933 0.3034 0.086 Uiso 0.50 1 calc PR . . H69B H 0.3522 0.2527 0.3124 0.086 Uiso 0.50 1 calc PR . . H69C H 0.2447 0.2264 0.3376 0.086 Uiso 0.50 1 calc PR . . H69D H 0.2929 0.2549 0.3322 0.086 Uiso 0.50 1 calc PR . . H69E H 0.2559 0.1956 0.3232 0.086 Uiso 0.50 1 calc PR . . H69F H 0.3633 0.2219 0.2980 0.086 Uiso 0.50 1 calc PR . . K101 K 0.52773(5) -0.04746(2) 0.277936(16) 0.03375(13) Uani 1 1 d . . . N101 N 0.3586(2) -0.13487(10) 0.24805(8) 0.0438(5) Uani 1 1 d . . . N102 N 0.6941(2) 0.03860(10) 0.30824(7) 0.0394(5) Uani 1 1 d . . . O101 O 0.27073(17) -0.02842(8) 0.25614(7) 0.0457(5) Uani 1 1 d . . . O102 O 0.43964(17) 0.05441(8) 0.27014(6) 0.0404(4) Uani 1 1 d . . . O103 O 0.58865(19) -0.10949(8) 0.20804(6) 0.0444(5) Uani 1 1 d . . . O104 O 0.76691(17) -0.04054(8) 0.24610(6) 0.0409(4) Uani 1 1 d . . . O105 O 0.47253(17) -0.12642(8) 0.33541(6) 0.0422(4) Uani 1 1 d . . . O106 O 0.59952(17) -0.03770(8) 0.36825(6) 0.0412(4) Uani 1 1 d . . . C101 C 0.2281(3) -0.11876(13) 0.24591(12) 0.0570(8) Uani 1 1 d . . . H10A H 0.1984 -0.1203 0.2752 0.068 Uiso 1 1 calc R . . H10B H 0.1782 -0.1436 0.2277 0.068 Uiso 1 1 calc R . . C102 C 0.2066(3) -0.06484(14) 0.22814(11) 0.0558(8) Uani 1 1 d . . . H10C H 0.2373 -0.0625 0.1991 0.067 Uiso 1 1 calc R . . H10D H 0.1167 -0.0570 0.2258 0.067 Uiso 1 1 calc R . . C103 C 0.2413(3) 0.02353(13) 0.24422(10) 0.0453(7) Uani 1 1 d . . . H10E H 0.1510 0.0293 0.2450 0.054 Uiso 1 1 calc R . . H10F H 0.2641 0.0301 0.2145 0.054 Uiso 1 1 calc R . . C104 C 0.3103(3) 0.05971(13) 0.27448(10) 0.0461(7) Uani 1 1 d . . . H10G H 0.2841 0.0959 0.2680 0.055 Uiso 1 1 calc R . . H10H H 0.2918 0.0517 0.3044 0.055 Uiso 1 1 calc R . . C105 C 0.5091(3) 0.09515(12) 0.29172(10) 0.0470(7) Uani 1 1 d . . . H10I H 0.4923 0.0956 0.3225 0.056 Uiso 1 1 calc R . . H10J H 0.4836 0.1290 0.2790 0.056 Uiso 1 1 calc R . . C106 C 0.6453(3) 0.08660(12) 0.28747(10) 0.0471(7) Uani 1 1 d . . . H10K H 0.6603 0.0854 0.2565 0.057 Uiso 1 1 calc R . . H10L H 0.6920 0.1166 0.3003 0.057 Uiso 1 1 calc R . . C107 C 0.3914(3) -0.15113(14) 0.20505(10) 0.0531(8) Uani 1 1 d . . . H10M H 0.3596 -0.1249 0.1837 0.064 Uiso 1 1 calc R . . H10N H 0.3493 -0.1844 0.1976 0.064 Uiso 1 1 calc R . . C108 C 0.5285(3) -0.15780(13) 0.20142(10) 0.0517(7) Uani 1 1 d . . . H10O H 0.5623 -0.1831 0.2232 0.062 Uiso 1 1 calc R . . H10P H 0.5436 -0.1713 0.1726 0.062 Uiso 1 1 calc R . . C109 C 0.7176(3) -0.11356(13) 0.20162(10) 0.0488(7) Uani 1 1 d . . . H10Q H 0.7287 -0.1293 0.1732 0.059 Uiso 1 1 calc R . . H10R H 0.7592 -0.1360 0.2241 0.059 Uiso 1 1 calc R . . C110 C 0.7736(3) -0.06067(13) 0.20382(9) 0.0470(7) Uani 1 1 d . . . H11G H 0.8612 -0.0624 0.1967 0.056 Uiso 1 1 calc R . . H11H H 0.7281 -0.0376 0.1827 0.056 Uiso 1 1 calc R . . C111 C 0.8237(2) 0.00926(13) 0.24987(10) 0.0449(7) Uani 1 1 d . . . H11I H 0.7789 0.0339 0.2299 0.054 Uiso 1 1 calc R . . H11J H 0.9107 0.0070 0.2422 0.054 Uiso 1 1 calc R . . C112 C 0.8202(3) 0.02834(13) 0.29537(10) 0.0464(7) Uani 1 1 d . . . H11K H 0.8600 0.0021 0.3151 0.056 Uiso 1 1 calc R . . H11L H 0.8694 0.0607 0.2987 0.056 Uiso 1 1 calc R . . C113 C 0.3794(3) -0.17808(12) 0.27835(10) 0.0489(7) Uani 1 1 d . . . H11M H 0.4612 -0.1938 0.2742 0.059 Uiso 1 1 calc R . . H11N H 0.3153 -0.2049 0.2716 0.059 Uiso 1 1 calc R . . C114 C 0.3759(3) -0.16271(13) 0.32508(10) 0.0473(7) Uani 1 1 d . . . H11O H 0.2946 -0.1470 0.3300 0.057 Uiso 1 1 calc R . . H11P H 0.3873 -0.1937 0.3437 0.057 Uiso 1 1 calc R . . C115 C 0.4872(3) -0.11562(13) 0.38009(9) 0.0469(7) Uani 1 1 d . . . H11Q H 0.4892 -0.1485 0.3966 0.056 Uiso 1 1 calc R . . H11R H 0.4162 -0.0947 0.3886 0.056 Uiso 1 1 calc R . . C116 C 0.6060(3) -0.08630(13) 0.38998(9) 0.0444(7) Uani 1 1 d . . . H11S H 0.6194 -0.0806 0.4214 0.053 Uiso 1 1 calc R . . H11T H 0.6766 -0.1067 0.3806 0.053 Uiso 1 1 calc R . . C117 C 0.7092(3) -0.00800(13) 0.37826(9) 0.0449(7) Uani 1 1 d . . . H11U H 0.7823 -0.0272 0.3693 0.054 Uiso 1 1 calc R . . H11V H 0.7207 -0.0021 0.4097 0.054 Uiso 1 1 calc R . . C118 C 0.6982(3) 0.04324(13) 0.35521(9) 0.0461(7) Uani 1 1 d . . . H11W H 0.6219 0.0609 0.3631 0.055 Uiso 1 1 calc R . . H11X H 0.7697 0.0653 0.3651 0.055 Uiso 1 1 calc R . . O1S O 0.8687(8) -0.0036(6) 0.4793(3) 0.183(5) Uani 0.50 1 d PDU A -1 C1S C 0.8959(17) 0.0231(11) 0.5188(6) 0.132(7) Uani 0.50 1 d PDU A -1 H1S1 H 0.8833 0.0610 0.5156 0.158 Uiso 0.50 1 calc PR A -1 H1S2 H 0.8458 0.0099 0.5418 0.158 Uiso 0.50 1 calc PR A -1 C2S C 1.0192(14) 0.0106(9) 0.5264(4) 0.123(6) Uani 0.50 1 d PDU A -1 H2S1 H 1.0274 -0.0135 0.5511 0.148 Uiso 0.50 1 calc PR A -1 H2S2 H 1.0649 0.0427 0.5351 0.148 Uiso 0.50 1 calc PR A -1 C3S C 1.0815(14) -0.0135(8) 0.4901(4) 0.115(6) Uani 0.50 1 d PDU A -1 H3S1 H 1.1279 -0.0453 0.4991 0.138 Uiso 0.50 1 calc PR A -1 H3S2 H 1.1376 0.0112 0.4768 0.138 Uiso 0.50 1 calc PR A -1 C4S C 0.9625(13) -0.0261(8) 0.4594(4) 0.118(6) Uani 0.50 1 d PDU A -1 H4S1 H 0.9693 -0.0110 0.4304 0.142 Uiso 0.50 1 calc PR A -1 H4S2 H 0.9498 -0.0640 0.4565 0.142 Uiso 0.50 1 calc PR A -1 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 0.02736(18) 0.0252(2) 0.02477(17) -0.00079(14) 0.00630(13) -0.00321(14) Al1 0.0394(4) 0.0303(4) 0.0343(4) -0.0012(3) 0.0150(3) -0.0019(3) N1 0.0275(9) 0.0247(11) 0.0269(9) -0.0021(8) 0.0047(7) -0.0013(8) N2 0.0219(8) 0.0264(10) 0.0244(9) 0.0010(7) 0.0042(7) -0.0012(7) N3 0.0236(9) 0.0233(10) 0.0241(9) 0.0015(7) 0.0029(7) 0.0006(7) N4 0.0232(8) 0.0248(10) 0.0248(9) 0.0027(7) 0.0024(7) -0.0031(7) C1 0.0209(10) 0.0265(12) 0.0286(11) -0.0031(9) 0.0032(8) -0.0003(9) C2 0.0321(11) 0.0283(13) 0.0269(11) 0.0014(9) 0.0054(9) -0.0009(9) C3 0.0260(10) 0.0274(12) 0.0272(11) 0.0026(9) 0.0037(8) -0.0019(9) C4 0.0351(12) 0.0230(12) 0.0302(11) -0.0029(9) 0.0077(9) -0.0013(10) C5 0.0411(14) 0.0353(15) 0.0396(13) -0.0058(11) 0.0037(11) 0.0051(11) C6 0.0504(16) 0.0322(15) 0.0513(16) -0.0063(12) 0.0092(12) 0.0074(12) C7 0.0587(17) 0.0308(15) 0.0549(17) -0.0134(13) 0.0104(14) -0.0055(13) C8 0.0436(15) 0.0437(17) 0.0510(16) -0.0152(13) 0.0031(12) -0.0107(13) C9 0.0361(13) 0.0343(14) 0.0365(13) -0.0053(11) 0.0062(10) -0.0073(11) C10 0.0465(16) 0.064(2) 0.0584(18) -0.0250(16) -0.0085(14) 0.0173(15) C11 0.0471(17) 0.059(2) 0.075(2) -0.0029(18) -0.0083(15) -0.0058(15) C12 0.066(2) 0.140(5) 0.0422(18) 0.007(2) -0.0003(16) 0.021(3) C13 0.0355(13) 0.0513(19) 0.0528(16) -0.0160(14) -0.0050(12) -0.0008(13) C14 0.0479(17) 0.079(3) 0.0557(19) 0.0008(17) -0.0081(14) 0.0056(17) C15 0.0419(17) 0.140(4) 0.059(2) -0.009(2) 0.0104(15) 0.014(2) C16 0.0276(10) 0.0242(12) 0.0231(10) 0.0005(8) 0.0071(8) -0.0014(9) C17 0.0303(11) 0.0339(14) 0.0249(10) -0.0023(9) 0.0084(9) -0.0045(10) C18 0.0413(13) 0.0363(15) 0.0337(12) -0.0030(11) 0.0109(10) -0.0142(11) C19 0.0558(16) 0.0274(14) 0.0346(13) 0.0029(10) 0.0101(11) -0.0027(12) C20 0.0434(14) 0.0311(14) 0.0310(12) 0.0034(10) 0.0037(10) 0.0039(11) C21 0.0327(12) 0.0310(13) 0.0226(10) -0.0001(9) 0.0046(8) 0.0013(10) C22 0.0260(11) 0.0438(16) 0.0400(13) -0.0053(11) 0.0058(9) -0.0048(11) C23 0.0300(13) 0.066(2) 0.067(2) -0.0101(16) 0.0105(13) -0.0119(14) C24 0.0315(13) 0.065(2) 0.0430(15) 0.0049(14) -0.0030(11) 0.0002(13) C25 0.0265(11) 0.0355(14) 0.0349(12) 0.0002(10) 0.0002(9) 0.0009(10) C26 0.0378(13) 0.059(2) 0.0357(13) -0.0047(13) 0.0007(10) -0.0059(13) C27 0.0317(12) 0.0478(17) 0.0426(14) 0.0018(12) 0.0061(10) 0.0038(12) C28 0.0225(10) 0.0273(12) 0.0286(11) 0.0018(9) 0.0008(8) 0.0007(9) C29 0.0220(10) 0.0303(13) 0.0244(10) -0.0014(9) 0.0037(8) -0.0025(9) C30 0.0230(10) 0.0285(12) 0.0249(10) -0.0008(9) 0.0039(8) -0.0035(9) C31 0.0377(12) 0.0242(12) 0.0252(11) 0.0007(9) 0.0059(9) 0.0029(10) C32 0.0485(14) 0.0269(13) 0.0299(12) 0.0001(10) -0.0011(10) 0.0069(11) C33 0.073(2) 0.0352(16) 0.0288(13) 0.0043(11) -0.0013(12) 0.0117(14) C34 0.082(2) 0.0384(17) 0.0355(14) 0.0109(12) 0.0205(14) 0.0073(15) C35 0.0610(18) 0.0380(16) 0.0409(14) 0.0075(12) 0.0232(13) -0.0003(13) C36 0.0420(13) 0.0283(13) 0.0312(12) 0.0007(10) 0.0148(10) 0.0006(11) C37 0.0453(15) 0.0345(15) 0.0452(15) 0.0038(12) -0.0149(12) 0.0033(12) C38 0.0393(14) 0.069(2) 0.0465(16) 0.0072(15) -0.0026(12) 0.0004(14) C39 0.062(2) 0.070(3) 0.0576(19) -0.0079(17) -0.0231(16) 0.0100(18) C40 0.0328(12) 0.0438(16) 0.0406(13) 0.0003(12) 0.0126(10) -0.0053(11) C41 0.0384(15) 0.058(2) 0.070(2) -0.0063(16) 0.0182(14) -0.0130(14) C42 0.0391(15) 0.0488(19) 0.0667(19) 0.0067(15) 0.0045(13) 0.0018(13) C43 0.0309(11) 0.0267(13) 0.0273(11) 0.0028(9) 0.0008(9) -0.0035(9) C44 0.0328(12) 0.0322(13) 0.0258(11) -0.0001(9) 0.0024(9) -0.0069(10) C45 0.0435(14) 0.0373(15) 0.0403(14) 0.0045(11) 0.0032(11) -0.0150(12) C46 0.0545(17) 0.0306(15) 0.0554(17) 0.0138(13) -0.0052(13) -0.0079(13) C47 0.0423(15) 0.0371(16) 0.0602(18) 0.0133(13) -0.0089(12) 0.0020(12) C48 0.0335(12) 0.0332(14) 0.0404(13) 0.0069(11) -0.0041(10) -0.0027(11) C49 0.0292(12) 0.0368(15) 0.0384(13) -0.0041(11) 0.0058(10) -0.0085(10) C50 0.0357(14) 0.0519(19) 0.0585(17) -0.0108(14) 0.0164(12) -0.0145(13) C51 0.0295(12) 0.0556(19) 0.0451(15) -0.0008(13) -0.0020(10) 0.0003(12) C52 0.0306(13) 0.0361(16) 0.0662(18) 0.0141(13) -0.0027(12) 0.0000(11) C53 0.0375(15) 0.061(2) 0.083(2) -0.0230(18) -0.0005(15) -0.0076(14) C54 0.0444(17) 0.090(3) 0.0595(19) -0.0112(19) 0.0090(14) -0.0128(18) C55 0.0329(12) 0.0269(13) 0.0322(11) -0.0026(10) 0.0086(9) -0.0025(10) C56 0.0364(12) 0.0244(13) 0.0384(13) 0.0004(10) 0.0064(10) 0.0017(10) C57 0.0457(14) 0.0276(14) 0.0467(15) 0.0049(11) 0.0103(12) 0.0027(11) C58 0.0442(15) 0.0281(14) 0.0606(17) 0.0016(13) 0.0126(13) -0.0063(12) C59 0.0339(13) 0.0387(16) 0.0579(17) -0.0046(13) 0.0061(11) -0.0078(12) C60 0.0334(12) 0.0362(15) 0.0382(13) -0.0026(11) 0.0053(10) -0.0036(11) C61 0.0438(14) 0.0340(15) 0.0407(14) 0.0002(11) -0.0035(11) 0.0036(11) C62 0.060(2) 0.0357(18) 0.096(3) 0.0076(17) 0.0177(18) -0.0141(15) C63 0.0412(14) 0.056(2) 0.0454(15) 0.0044(14) -0.0048(12) -0.0084(13) C64 0.0481(15) 0.0373(15) 0.0348(13) 0.0017(11) 0.0127(11) 0.0022(12) C65 0.0532(16) 0.0366(16) 0.0411(14) 0.0034(12) 0.0119(12) -0.0096(13) C66 0.0350(14) 0.0514(19) 0.0517(16) -0.0014(13) 0.0040(12) -0.0045(12) C67 0.0395(16) 0.076(3) 0.069(2) -0.0056(18) 0.0135(14) -0.0011(16) C68 0.0492(15) 0.0437(17) 0.0394(14) -0.0049(12) 0.0115(11) -0.0073(13) C69 0.0528(18) 0.061(2) 0.0571(19) -0.0153(16) 0.0006(14) -0.0015(16) K101 0.0317(2) 0.0350(3) 0.0345(3) 0.0009(2) 0.00162(19) 0.0005(2) N101 0.0436(12) 0.0399(14) 0.0468(13) 0.0048(10) -0.0036(10) -0.0068(10) N102 0.0362(11) 0.0389(13) 0.0428(12) -0.0024(10) 0.0017(9) -0.0020(10) O101 0.0361(9) 0.0474(12) 0.0520(11) 0.0103(9) -0.0061(8) -0.0024(9) O102 0.0357(9) 0.0347(11) 0.0510(11) -0.0032(8) 0.0044(8) 0.0045(8) O103 0.0515(11) 0.0391(11) 0.0431(10) -0.0002(8) 0.0063(8) 0.0013(9) O104 0.0422(10) 0.0447(12) 0.0369(9) 0.0044(8) 0.0104(7) 0.0013(8) O105 0.0408(10) 0.0478(12) 0.0384(10) 0.0053(8) 0.0050(7) -0.0047(9) O106 0.0398(9) 0.0462(12) 0.0368(9) -0.0002(8) -0.0015(7) 0.0023(8) C101 0.0431(16) 0.050(2) 0.076(2) 0.0054(16) -0.0123(14) -0.0128(14) C102 0.0397(15) 0.058(2) 0.067(2) 0.0098(16) -0.0172(13) -0.0081(14) C103 0.0341(13) 0.0519(18) 0.0494(16) 0.0104(13) 0.0001(11) 0.0070(12) C104 0.0391(14) 0.0484(18) 0.0516(16) 0.0032(13) 0.0085(12) 0.0109(13) C105 0.0522(16) 0.0312(15) 0.0570(17) -0.0053(13) 0.0001(13) 0.0038(12) C106 0.0492(16) 0.0357(16) 0.0558(17) 0.0010(13) -0.0001(13) -0.0067(13) C107 0.0660(19) 0.0492(19) 0.0420(15) -0.0007(13) -0.0107(13) -0.0135(15) C108 0.070(2) 0.0445(18) 0.0401(15) -0.0065(13) 0.0037(13) -0.0015(15) C109 0.0532(17) 0.0533(19) 0.0417(15) -0.0035(13) 0.0150(12) 0.0109(14) C110 0.0446(15) 0.058(2) 0.0401(14) 0.0015(13) 0.0157(12) 0.0055(14) C111 0.0332(13) 0.0503(18) 0.0522(16) 0.0063(13) 0.0108(11) -0.0010(12) C112 0.0337(13) 0.0533(19) 0.0521(16) 0.0009(14) 0.0025(11) -0.0065(13) C113 0.0547(17) 0.0384(17) 0.0532(17) 0.0046(13) 0.0009(13) -0.0081(14) C114 0.0462(15) 0.0451(18) 0.0510(16) 0.0117(13) 0.0063(12) -0.0076(13) C115 0.0472(15) 0.058(2) 0.0368(14) 0.0083(13) 0.0087(11) 0.0013(14) C116 0.0482(15) 0.0528(18) 0.0323(13) 0.0048(12) 0.0035(11) 0.0071(13) C117 0.0399(14) 0.0562(19) 0.0374(14) -0.0055(13) -0.0043(11) 0.0023(13) C118 0.0436(15) 0.0497(18) 0.0440(15) -0.0093(13) -0.0027(11) -0.0036(13) O1S 0.098(6) 0.344(15) 0.104(6) -0.087(8) -0.017(5) 0.070(8) C1S 0.123(12) 0.190(16) 0.084(9) -0.018(9) 0.013(8) 0.065(12) C2S 0.142(12) 0.162(15) 0.059(10) -0.004(9) -0.038(8) 0.033(11) C3S 0.104(9) 0.165(14) 0.075(9) 0.044(9) 0.003(8) 0.087(9) C4S 0.115(9) 0.181(14) 0.055(8) -0.027(8) -0.018(6) 0.089(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C55 2.071(2) . ? Fe1 C29 2.074(2) . ? Fe1 C3 2.110(2) . ? Al1 C68 1.992(3) . ? Al1 C64 2.005(3) . ? Al1 C66 2.042(3) . ? Al1 C1 2.123(2) . ? N1 C1 1.358(3) . ? N1 C2 1.398(3) . ? N1 C4 1.444(3) . ? N2 C1 1.364(3) . ? N2 C3 1.418(3) . ? N2 C16 1.437(3) . ? N3 C28 1.367(3) . ? N3 C29 1.426(3) . ? N3 C31 1.440(3) . ? N4 C28 1.366(3) . ? N4 C30 1.399(3) . ? N4 C43 1.440(3) . ? C2 C3 1.358(4) . ? C2 H2 0.9500 . ? C4 C5 1.401(4) . ? C4 C9 1.405(4) . ? C5 C6 1.403(4) . ? C5 C10 1.508(4) . ? C6 C7 1.367(4) . ? C6 H6 0.9500 . ? C7 C8 1.380(4) . ? C7 H7 0.9500 . ? C8 C9 1.392(4) . ? C8 H8 0.9500 . ? C9 C13 1.515(4) . ? C10 C11 1.524(5) . ? C10 C12 1.539(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? C13 C15 1.521(5) . ? C13 C14 1.526(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 H15D 0.9800 . ? C15 H15E 0.9800 . ? C15 H15F 0.9800 . ? C16 C17 1.401(3) . ? C16 C21 1.402(3) . ? C17 C18 1.391(4) . ? C17 C22 1.528(4) . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 C20 1.379(4) . ? C19 H19 0.9500 . ? C20 C21 1.387(4) . ? C20 H20 0.9500 . ? C21 C25 1.520(3) . ? C22 C24 1.530(4) . ? C22 C23 1.531(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23D 0.9800 . ? C23 H23E 0.9800 . ? C23 H23F 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? C25 C26 1.528(3) . ? C25 C27 1.529(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? C29 C30 1.359(3) . ? C30 H30 0.9500 . ? C31 C36 1.402(4) . ? C31 C32 1.405(4) . ? C32 C33 1.396(4) . ? C32 C37 1.519(4) . ? C33 C34 1.387(5) . ? C33 H33 0.9500 . ? C34 C35 1.370(5) . ? C34 H34 0.9500 . ? C35 C36 1.398(4) . ? C35 H35 0.9500 . ? C36 C40 1.516(4) . ? C37 C38 1.518(4) . ? C37 C39 1.532(4) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C38 H38D 0.9800 . ? C38 H38E 0.9800 . ? C38 H38F 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C39 H39D 0.9800 . ? C39 H39E 0.9800 . ? C39 H39F 0.9800 . ? C40 C41 1.531(4) . ? C40 C42 1.534(4) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41 H41D 0.9800 . ? C41 H41E 0.9800 . ? C41 H41F 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C42 H42D 0.9800 . ? C42 H42E 0.9800 . ? C42 H42F 0.9800 . ? C43 C48 1.398(4) . ? C43 C44 1.399(3) . ? C44 C45 1.398(4) . ? C44 C49 1.520(4) . ? C45 C46 1.384(4) . ? C45 H45 0.9500 . ? C46 C47 1.381(4) . ? C46 H46 0.9500 . ? C47 C48 1.392(4) . ? C47 H47 0.9500 . ? C48 C52 1.514(4) . ? C49 C51 1.523(4) . ? C49 C50 1.526(3) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C50 H50D 0.9800 . ? C50 H50E 0.9800 . ? C50 H50F 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C51 H51D 0.9800 . ? C51 H51E 0.9800 . ? C51 H51F 0.9800 . ? C52 C54 1.525(5) . ? C52 C53 1.527(5) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C53 H53D 0.9800 . ? C53 H53E 0.9800 . ? C53 H53F 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C54 H54D 0.9800 . ? C54 H54E 0.9800 . ? C54 H54F 0.9800 . ? C55 C60 1.411(4) . ? C55 C56 1.416(4) . ? C56 C57 1.398(4) . ? C56 C61 1.512(4) . ? C57 C58 1.385(4) . ? C57 H57 0.9500 . ? C58 C59 1.394(4) . ? C58 C62 1.514(4) . ? C59 C60 1.389(4) . ? C59 H59 0.9500 . ? C60 C63 1.516(4) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C61 H61D 0.9800 . ? C61 H61E 0.9800 . ? C61 H61F 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C62 H62D 0.9800 . ? C62 H62E 0.9800 . ? C62 H62F 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C63 H63D 0.9800 . ? C63 H63E 0.9800 . ? C63 H63F 0.9800 . ? C64 C65 1.527(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C65 H65D 0.9800 . ? C65 H65E 0.9800 . ? C65 H65F 0.9800 . ? C66 C67 1.529(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C67 H67D 0.9800 . ? C67 H67E 0.9800 . ? C67 H67F 0.9800 . ? C68 C69 1.537(4) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C69 H69D 0.9800 . ? C69 H69E 0.9800 . ? C69 H69F 0.9800 . ? K101 O102 2.797(2) . ? K101 O105 2.804(2) . ? K101 O103 2.819(2) . ? K101 O104 2.8434(18) . ? K101 O101 2.853(2) . ? K101 O106 2.8746(19) . ? K101 N102 2.965(2) . ? K101 N101 3.005(2) . ? N101 C113 1.466(4) . ? N101 C101 1.467(4) . ? N101 C107 1.473(4) . ? N102 C118 1.466(4) . ? N102 C112 1.473(3) . ? N102 C106 1.475(4) . ? O101 C103 1.419(4) . ? O101 C102 1.426(4) . ? O102 C104 1.421(3) . ? O102 C105 1.429(4) . ? O103 C108 1.412(4) . ? O103 C109 1.427(4) . ? O104 C110 1.423(3) . ? O104 C111 1.423(4) . ? O105 C115 1.417(3) . ? O105 C114 1.421(4) . ? O106 C116 1.423(4) . ? O106 C117 1.426(3) . ? C101 C102 1.507(5) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.486(4) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.505(4) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.505(5) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.490(5) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11G 0.9900 . ? C110 H11H 0.9900 . ? C111 C112 1.504(4) . ? C111 H11I 0.9900 . ? C111 H11J 0.9900 . ? C112 H11K 0.9900 . ? C112 H11L 0.9900 . ? C113 C114 1.513(4) . ? C113 H11M 0.9900 . ? C113 H11N 0.9900 . ? C114 H11O 0.9900 . ? C114 H11P 0.9900 . ? C115 C116 1.501(4) . ? C115 H11Q 0.9900 . ? C115 H11R 0.9900 . ? C116 H11S 0.9900 . ? C116 H11T 0.9900 . ? C117 C118 1.504(4) . ? C117 H11U 0.9900 . ? C117 H11V 0.9900 . ? C118 H11W 0.9900 . ? C118 H11X 0.9900 . ? O1S C4S 1.358(13) . ? O1S C1S 1.423(14) . ? C1S C2S 1.374(15) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S C3S 1.495(15) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.579(15) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? 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 C55 Fe1 C29 125.37(9) . . ? C55 Fe1 C3 109.62(9) . . ? C29 Fe1 C3 124.91(9) . . ? C68 Al1 C64 110.51(13) . . ? C68 Al1 C66 111.81(13) . . ? C64 Al1 C66 106.65(13) . . ? C68 Al1 C1 109.70(11) . . ? C64 Al1 C1 112.24(10) . . ? C66 Al1 C1 105.85(11) . . ? C1 N1 C2 110.6(2) . . ? C1 N1 C4 126.62(19) . . ? C2 N1 C4 122.4(2) . . ? C1 N2 C3 114.4(2) . . ? C1 N2 C16 122.18(18) . . ? C3 N2 C16 122.76(18) . . ? C28 N3 C29 115.67(18) . . ? C28 N3 C31 119.67(18) . . ? C29 N3 C31 124.7(2) . . ? C28 N4 C30 112.05(19) . . ? C28 N4 C43 122.84(19) . . ? C30 N4 C43 124.82(18) . . ? N1 C1 N2 103.04(18) . . ? N1 C1 Al1 129.28(16) . . ? N2 C1 Al1 127.24(17) . . ? C3 C2 N1 109.9(2) . . ? C3 C2 H2 125.0 . . ? N1 C2 H2 125.0 . . ? C2 C3 N2 102.01(19) . . ? C2 C3 Fe1 124.64(17) . . ? N2 C3 Fe1 133.14(17) . . ? C5 C4 C9 122.7(2) . . ? C5 C4 N1 119.3(2) . . ? C9 C4 N1 118.0(2) . . ? C4 C5 C6 116.9(3) . . ? C4 C5 C10 123.6(3) . . ? C6 C5 C10 119.5(3) . . ? C7 C6 C5 121.4(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 121.3(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 117.2(3) . . ? C8 C9 C13 120.8(2) . . ? C4 C9 C13 121.9(2) . . ? C5 C10 C11 111.4(3) . . ? C5 C10 C12 110.6(3) . . ? C11 C10 C12 107.4(3) . . ? C5 C10 H10 109.1 . . ? C11 C10 H10 109.1 . . ? C12 C10 H10 109.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.3 . . ? C10 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? C10 C11 H11F 109.5 . . ? H11A C11 H11F 56.3 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C12 H12D 109.5 . . ? H12A C12 H12D 141.1 . . ? H12B C12 H12D 56.3 . . ? H12C C12 H12D 56.3 . . ? C10 C12 H12E 109.5 . . ? H12A C12 H12E 56.3 . . ? H12B C12 H12E 141.1 . . ? H12C C12 H12E 56.3 . . ? H12D C12 H12E 109.5 . . ? C10 C12 H12F 109.5 . . ? H12A C12 H12F 56.3 . . ? H12B C12 H12F 56.3 . . ? H12C C12 H12F 141.1 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? C9 C13 C15 111.6(3) . . ? C9 C13 C14 112.9(3) . . ? C15 C13 C14 108.7(3) . . ? C9 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14A C14 H14D 141.1 . . ? H14B C14 H14D 56.3 . . ? H14C C14 H14D 56.3 . . ? C13 C14 H14E 109.5 . . ? H14A C14 H14E 56.3 . . ? H14B C14 H14E 141.1 . . ? H14C C14 H14E 56.3 . . ? H14D C14 H14E 109.5 . . ? C13 C14 H14F 109.5 . . ? H14A C14 H14F 56.3 . . ? H14B C14 H14F 56.3 . . ? H14C C14 H14F 141.1 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C15 H15D 109.5 . . ? H15A C15 H15D 141.1 . . ? H15B C15 H15D 56.3 . . ? H15C C15 H15D 56.3 . . ? C13 C15 H15E 109.5 . . ? H15A C15 H15E 56.3 . . ? H15B C15 H15E 141.1 . . ? H15C C15 H15E 56.3 . . ? H15D C15 H15E 109.5 . . ? C13 C15 H15F 109.5 . . ? H15A C15 H15F 56.3 . . ? H15B C15 H15F 56.3 . . ? H15C C15 H15F 141.1 . . ? H15D C15 H15F 109.5 . . ? H15E C15 H15F 109.5 . . ? C17 C16 C21 122.6(2) . . ? C17 C16 N2 119.8(2) . . ? C21 C16 N2 117.6(2) . . ? C18 C17 C16 117.1(2) . . ? C18 C17 C22 121.9(2) . . ? C16 C17 C22 121.0(2) . . ? C19 C18 C17 121.4(2) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.1(2) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 117.7(2) . . ? C20 C21 C25 120.1(2) . . ? C16 C21 C25 122.2(2) . . ? C17 C22 C24 110.8(2) . . ? C17 C22 C23 113.3(2) . . ? C24 C22 C23 108.6(2) . . ? C17 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C23 C22 H22 108.0 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C23 H23D 109.5 . . ? H23A C23 H23D 141.1 . . ? H23B C23 H23D 56.3 . . ? H23C C23 H23D 56.3 . . ? C22 C23 H23E 109.5 . . ? H23A C23 H23E 56.3 . . ? H23B C23 H23E 141.1 . . ? H23C C23 H23E 56.3 . . ? H23D C23 H23E 109.5 . . ? C22 C23 H23F 109.5 . . ? H23A C23 H23F 56.3 . . ? H23B C23 H23F 56.3 . . ? H23C C23 H23F 141.1 . . ? H23D C23 H23F 109.5 . . ? H23E C23 H23F 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C24 H24D 109.5 . . ? H24A C24 H24D 141.1 . . ? H24B C24 H24D 56.3 . . ? H24C C24 H24D 56.3 . . ? C22 C24 H24E 109.5 . . ? H24A C24 H24E 56.3 . . ? H24B C24 H24E 141.1 . . ? H24C C24 H24E 56.3 . . ? H24D C24 H24E 109.5 . . ? C22 C24 H24F 109.5 . . ? H24A C24 H24F 56.3 . . ? H24B C24 H24F 56.3 . . ? H24C C24 H24F 141.1 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? C21 C25 C26 111.3(2) . . ? C21 C25 C27 111.5(2) . . ? C26 C25 C27 110.3(2) . . ? C21 C25 H25 107.9 . . ? C26 C25 H25 107.9 . . ? C27 C25 H25 107.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? C25 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? C25 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.3 . . ? C25 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.3 . . ? H27D C27 H27E 109.5 . . ? C25 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.3 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? N4 C28 N3 101.25(19) . . ? C30 C29 N3 101.6(2) . . ? C30 C29 Fe1 124.89(16) . . ? N3 C29 Fe1 133.44(16) . . ? C29 C30 N4 109.43(19) . . ? C29 C30 H30 125.3 . . ? N4 C30 H30 125.3 . . ? C36 C31 C32 121.8(2) . . ? C36 C31 N3 118.9(2) . . ? C32 C31 N3 119.2(2) . . ? C33 C32 C31 117.6(3) . . ? C33 C32 C37 121.5(2) . . ? C31 C32 C37 120.8(2) . . ? C34 C33 C32 120.8(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C33 120.9(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 120.5(3) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 118.3(3) . . ? C35 C36 C40 120.4(2) . . ? C31 C36 C40 121.2(2) . . ? C38 C37 C32 111.8(2) . . ? C38 C37 C39 109.2(3) . . ? C32 C37 C39 113.5(3) . . ? C38 C37 H37 107.4 . . ? C32 C37 H37 107.4 . . ? C39 C37 H37 107.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C38 H38D 109.5 . . ? H38A C38 H38D 141.1 . . ? H38B C38 H38D 56.3 . . ? H38C C38 H38D 56.3 . . ? C37 C38 H38E 109.5 . . ? H38A C38 H38E 56.3 . . ? H38B C38 H38E 141.1 . . ? H38C C38 H38E 56.3 . . ? H38D C38 H38E 109.5 . . ? C37 C38 H38F 109.5 . . ? H38A C38 H38F 56.3 . . ? H38B C38 H38F 56.3 . . ? H38C C38 H38F 141.1 . . ? H38D C38 H38F 109.5 . . ? H38E C38 H38F 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C39 H39D 109.5 . . ? H39A C39 H39D 141.1 . . ? H39B C39 H39D 56.3 . . ? H39C C39 H39D 56.3 . . ? C37 C39 H39E 109.5 . . ? H39A C39 H39E 56.3 . . ? H39B C39 H39E 141.1 . . ? H39C C39 H39E 56.3 . . ? H39D C39 H39E 109.5 . . ? C37 C39 H39F 109.5 . . ? H39A C39 H39F 56.3 . . ? H39B C39 H39F 56.3 . . ? H39C C39 H39F 141.1 . . ? H39D C39 H39F 109.5 . . ? H39E C39 H39F 109.5 . . ? C36 C40 C41 114.1(3) . . ? C36 C40 C42 109.9(2) . . ? C41 C40 C42 109.7(2) . . ? C36 C40 H40 107.6 . . ? C41 C40 H40 107.6 . . ? C42 C40 H40 107.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C41 H41D 109.5 . . ? H41A C41 H41D 141.1 . . ? H41B C41 H41D 56.3 . . ? H41C C41 H41D 56.3 . . ? C40 C41 H41E 109.5 . . ? H41A C41 H41E 56.3 . . ? H41B C41 H41E 141.1 . . ? H41C C41 H41E 56.3 . . ? H41D C41 H41E 109.5 . . ? C40 C41 H41F 109.5 . . ? H41A C41 H41F 56.3 . . ? H41B C41 H41F 56.3 . . ? H41C C41 H41F 141.1 . . ? H41D C41 H41F 109.5 . . ? H41E C41 H41F 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C42 H42D 109.5 . . ? H42A C42 H42D 141.1 . . ? H42B C42 H42D 56.3 . . ? H42C C42 H42D 56.3 . . ? C40 C42 H42E 109.5 . . ? H42A C42 H42E 56.3 . . ? H42B C42 H42E 141.1 . . ? H42C C42 H42E 56.3 . . ? H42D C42 H42E 109.5 . . ? C40 C42 H42F 109.5 . . ? H42A C42 H42F 56.3 . . ? H42B C42 H42F 56.3 . . ? H42C C42 H42F 141.1 . . ? H42D C42 H42F 109.5 . . ? H42E C42 H42F 109.5 . . ? C48 C43 C44 121.9(2) . . ? C48 C43 N4 118.2(2) . . ? C44 C43 N4 119.9(2) . . ? C45 C44 C43 117.8(2) . . ? C45 C44 C49 121.3(2) . . ? C43 C44 C49 120.9(2) . . ? C46 C45 C44 121.1(2) . . ? C46 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? C47 C46 C45 119.8(3) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C48 121.2(3) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C47 C48 C43 118.1(2) . . ? C47 C48 C52 120.0(2) . . ? C43 C48 C52 121.8(2) . . ? C44 C49 C51 110.9(2) . . ? C44 C49 C50 112.7(2) . . ? C51 C49 C50 109.6(2) . . ? C44 C49 H49 107.8 . . ? C51 C49 H49 107.8 . . ? C50 C49 H49 107.8 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C50 H50D 109.5 . . ? H50A C50 H50D 141.1 . . ? H50B C50 H50D 56.3 . . ? H50C C50 H50D 56.3 . . ? C49 C50 H50E 109.5 . . ? H50A C50 H50E 56.3 . . ? H50B C50 H50E 141.1 . . ? H50C C50 H50E 56.3 . . ? H50D C50 H50E 109.5 . . ? C49 C50 H50F 109.5 . . ? H50A C50 H50F 56.3 . . ? H50B C50 H50F 56.3 . . ? H50C C50 H50F 141.1 . . ? H50D C50 H50F 109.5 . . ? H50E C50 H50F 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C51 H51D 109.5 . . ? H51A C51 H51D 141.1 . . ? H51B C51 H51D 56.3 . . ? H51C C51 H51D 56.3 . . ? C49 C51 H51E 109.5 . . ? H51A C51 H51E 56.3 . . ? H51B C51 H51E 141.1 . . ? H51C C51 H51E 56.3 . . ? H51D C51 H51E 109.5 . . ? C49 C51 H51F 109.5 . . ? H51A C51 H51F 56.3 . . ? H51B C51 H51F 56.3 . . ? H51C C51 H51F 141.1 . . ? H51D C51 H51F 109.5 . . ? H51E C51 H51F 109.5 . . ? C48 C52 C54 112.0(3) . . ? C48 C52 C53 110.1(2) . . ? C54 C52 C53 110.5(3) . . ? C48 C52 H52 108.0 . . ? C54 C52 H52 108.0 . . ? C53 C52 H52 108.0 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C53 H53D 109.5 . . ? H53A C53 H53D 141.1 . . ? H53B C53 H53D 56.3 . . ? H53C C53 H53D 56.3 . . ? C52 C53 H53E 109.5 . . ? H53A C53 H53E 56.3 . . ? H53B C53 H53E 141.1 . . ? H53C C53 H53E 56.3 . . ? H53D C53 H53E 109.5 . . ? C52 C53 H53F 109.5 . . ? H53A C53 H53F 56.3 . . ? H53B C53 H53F 56.3 . . ? H53C C53 H53F 141.1 . . ? H53D C53 H53F 109.5 . . ? H53E C53 H53F 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C54 H54D 109.5 . . ? H54A C54 H54D 141.1 . . ? H54B C54 H54D 56.3 . . ? H54C C54 H54D 56.3 . . ? C52 C54 H54E 109.5 . . ? H54A C54 H54E 56.3 . . ? H54B C54 H54E 141.1 . . ? H54C C54 H54E 56.3 . . ? H54D C54 H54E 109.5 . . ? C52 C54 H54F 109.5 . . ? H54A C54 H54F 56.3 . . ? H54B C54 H54F 56.3 . . ? H54C C54 H54F 141.1 . . ? H54D C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? C60 C55 C56 115.5(2) . . ? C60 C55 Fe1 121.49(19) . . ? C56 C55 Fe1 122.97(18) . . ? C57 C56 C55 121.8(2) . . ? C57 C56 C61 117.8(2) . . ? C55 C56 C61 120.4(2) . . ? C58 C57 C56 121.4(3) . . ? C58 C57 H57 119.3 . . ? C56 C57 H57 119.3 . . ? C57 C58 C59 117.8(3) . . ? C57 C58 C62 121.0(3) . . ? C59 C58 C62 121.2(3) . . ? C60 C59 C58 121.3(3) . . ? C60 C59 H59 119.3 . . ? C58 C59 H59 119.3 . . ? C59 C60 C55 122.2(3) . . ? C59 C60 C63 118.4(3) . . ? C55 C60 C63 119.4(2) . . ? C56 C61 H61A 109.5 . . ? C56 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C56 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C56 C61 H61D 109.5 . . ? H61A C61 H61D 141.1 . . ? H61B C61 H61D 56.3 . . ? H61C C61 H61D 56.3 . . ? C56 C61 H61E 109.5 . . ? H61A C61 H61E 56.3 . . ? H61B C61 H61E 141.1 . . ? H61C C61 H61E 56.3 . . ? H61D C61 H61E 109.5 . . ? C56 C61 H61F 109.5 . . ? H61A C61 H61F 56.3 . . ? H61B C61 H61F 56.3 . . ? H61C C61 H61F 141.1 . . ? H61D C61 H61F 109.5 . . ? H61E C61 H61F 109.5 . . ? C58 C62 H62A 109.5 . . ? C58 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C58 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C58 C62 H62D 109.5 . . ? H62A C62 H62D 141.1 . . ? H62B C62 H62D 56.3 . . ? H62C C62 H62D 56.3 . . ? C58 C62 H62E 109.5 . . ? H62A C62 H62E 56.3 . . ? H62B C62 H62E 141.1 . . ? H62C C62 H62E 56.3 . . ? H62D C62 H62E 109.5 . . ? C58 C62 H62F 109.5 . . ? H62A C62 H62F 56.3 . . ? H62B C62 H62F 56.3 . . ? H62C C62 H62F 141.1 . . ? H62D C62 H62F 109.5 . . ? H62E C62 H62F 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C60 C63 H63D 109.5 . . ? H63A C63 H63D 141.1 . . ? H63B C63 H63D 56.3 . . ? H63C C63 H63D 56.3 . . ? C60 C63 H63E 109.5 . . ? H63A C63 H63E 56.3 . . ? H63B C63 H63E 141.1 . . ? H63C C63 H63E 56.3 . . ? H63D C63 H63E 109.5 . . ? C60 C63 H63F 109.5 . . ? H63A C63 H63F 56.3 . . ? H63B C63 H63F 56.3 . . ? H63C C63 H63F 141.1 . . ? H63D C63 H63F 109.5 . . ? H63E C63 H63F 109.5 . . ? C65 C64 Al1 111.63(19) . . ? C65 C64 H64A 109.3 . . ? Al1 C64 H64A 109.3 . . ? C65 C64 H64B 109.3 . . ? Al1 C64 H64B 109.3 . . ? H64A C64 H64B 108.0 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C65 H65D 109.5 . . ? H65A C65 H65D 141.1 . . ? H65B C65 H65D 56.3 . . ? H65C C65 H65D 56.3 . . ? C64 C65 H65E 109.5 . . ? H65A C65 H65E 56.3 . . ? H65B C65 H65E 141.1 . . ? H65C C65 H65E 56.3 . . ? H65D C65 H65E 109.5 . . ? C64 C65 H65F 109.5 . . ? H65A C65 H65F 56.3 . . ? H65B C65 H65F 56.3 . . ? H65C C65 H65F 141.1 . . ? H65D C65 H65F 109.5 . . ? H65E C65 H65F 109.5 . . ? C67 C66 Al1 114.5(2) . . ? C67 C66 H66A 108.6 . . ? Al1 C66 H66A 108.6 . . ? C67 C66 H66B 108.6 . . ? Al1 C66 H66B 108.6 . . ? H66A C66 H66B 107.6 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C67 H67D 109.5 . . ? H67A C67 H67D 141.1 . . ? H67B C67 H67D 56.3 . . ? H67C C67 H67D 56.3 . . ? C66 C67 H67E 109.5 . . ? H67A C67 H67E 56.3 . . ? H67B C67 H67E 141.1 . . ? H67C C67 H67E 56.3 . . ? H67D C67 H67E 109.5 . . ? C66 C67 H67F 109.5 . . ? H67A C67 H67F 56.3 . . ? H67B C67 H67F 56.3 . . ? H67C C67 H67F 141.1 . . ? H67D C67 H67F 109.5 . . ? H67E C67 H67F 109.5 . . ? C69 C68 Al1 115.3(2) . . ? C69 C68 H68A 108.4 . . ? Al1 C68 H68A 108.4 . . ? C69 C68 H68B 108.4 . . ? Al1 C68 H68B 108.4 . . ? H68A C68 H68B 107.5 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C69 H69D 109.5 . . ? H69A C69 H69D 141.1 . . ? H69B C69 H69D 56.3 . . ? H69C C69 H69D 56.3 . . ? C68 C69 H69E 109.5 . . ? H69A C69 H69E 56.3 . . ? H69B C69 H69E 141.1 . . ? H69C C69 H69E 56.3 . . ? H69D C69 H69E 109.5 . . ? C68 C69 H69F 109.5 . . ? H69A C69 H69F 56.3 . . ? H69B C69 H69F 56.3 . . ? H69C C69 H69F 141.1 . . ? H69D C69 H69F 109.5 . . ? H69E C69 H69F 109.5 . . ? O102 K101 O105 130.47(6) . . ? O102 K101 O103 124.24(6) . . ? O105 K101 O103 98.95(6) . . ? O102 K101 O104 102.91(6) . . ? O105 K101 O104 120.73(6) . . ? O103 K101 O104 59.66(6) . . ? O102 K101 O101 59.91(6) . . ? O105 K101 O101 91.54(6) . . ? O103 K101 O101 101.13(6) . . ? O104 K101 O101 143.21(6) . . ? O102 K101 O106 93.90(6) . . ? O105 K101 O106 59.51(6) . . ? O103 K101 O106 138.15(6) . . ? O104 K101 O106 98.65(6) . . ? O101 K101 O106 113.88(6) . . ? O102 K101 N102 61.32(6) . . ? O105 K101 N102 119.48(6) . . ? O103 K101 N102 119.94(6) . . ? O104 K101 N102 61.23(6) . . ? O101 K101 N102 120.25(7) . . ? O106 K101 N102 60.63(6) . . ? O102 K101 N101 118.76(6) . . ? O105 K101 N101 60.05(6) . . ? O103 K101 N101 60.49(6) . . ? O104 K101 N101 119.14(7) . . ? O101 K101 N101 59.73(7) . . ? O106 K101 N101 118.86(6) . . ? N102 K101 N101 179.48(7) . . ? C113 N101 C101 110.2(2) . . ? C113 N101 C107 109.5(3) . . ? C101 N101 C107 109.6(3) . . ? C113 N101 K101 107.99(17) . . ? C101 N101 K101 111.27(19) . . ? C107 N101 K101 108.23(17) . . ? C118 N102 C112 109.1(2) . . ? C118 N102 C106 110.7(2) . . ? C112 N102 C106 109.8(2) . . ? C118 N102 K101 110.58(17) . . ? C112 N102 K101 109.29(17) . . ? C106 N102 K101 107.41(16) . . ? C103 O101 C102 111.8(2) . . ? C103 O101 K101 114.83(16) . . ? C102 O101 K101 116.93(18) . . ? C104 O102 C105 111.7(2) . . ? C104 O102 K101 114.38(17) . . ? C105 O102 K101 119.02(16) . . ? C108 O103 C109 111.0(2) . . ? C108 O103 K101 118.75(16) . . ? C109 O103 K101 115.93(17) . . ? C110 O104 C111 110.7(2) . . ? C110 O104 K101 114.24(16) . . ? C111 O104 K101 115.17(15) . . ? C115 O105 C114 112.2(2) . . ? C115 O105 K101 118.15(18) . . ? C114 O105 K101 121.38(16) . . ? C116 O106 C117 111.0(2) . . ? C116 O106 K101 112.90(16) . . ? C117 O106 K101 114.86(15) . . ? N101 C101 C102 113.5(3) . . ? N101 C101 H10A 108.9 . . ? C102 C101 H10A 108.9 . . ? N101 C101 H10B 108.9 . . ? C102 C101 H10B 108.9 . . ? H10A C101 H10B 107.7 . . ? O101 C102 C101 109.1(3) . . ? O101 C102 H10C 109.9 . . ? C101 C102 H10C 109.9 . . ? O101 C102 H10D 109.9 . . ? C101 C102 H10D 109.9 . . ? H10C C102 H10D 108.3 . . ? O101 C103 C104 109.5(2) . . ? O101 C103 H10E 109.8 . . ? C104 C103 H10E 109.8 . . ? O101 C103 H10F 109.8 . . ? C104 C103 H10F 109.8 . . ? H10E C103 H10F 108.2 . . ? O102 C104 C103 109.3(2) . . ? O102 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O102 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.3 . . ? O102 C105 C106 109.5(2) . . ? O102 C105 H10I 109.8 . . ? C106 C105 H10I 109.8 . . ? O102 C105 H10J 109.8 . . ? C106 C105 H10J 109.8 . . ? H10I C105 H10J 108.2 . . ? N102 C106 C105 113.8(2) . . ? N102 C106 H10K 108.8 . . ? C105 C106 H10K 108.8 . . ? N102 C106 H10L 108.8 . . ? C105 C106 H10L 108.8 . . ? H10K C106 H10L 107.7 . . ? N101 C107 C108 114.0(2) . . ? N101 C107 H10M 108.8 . . ? C108 C107 H10M 108.8 . . ? N101 C107 H10N 108.8 . . ? C108 C107 H10N 108.8 . . ? H10M C107 H10N 107.7 . . ? O103 C108 C107 109.5(3) . . ? O103 C108 H10O 109.8 . . ? C107 C108 H10O 109.8 . . ? O103 C108 H10P 109.8 . . ? C107 C108 H10P 109.8 . . ? H10O C108 H10P 108.2 . . ? O103 C109 C110 108.9(2) . . ? O103 C109 H10Q 109.9 . . ? C110 C109 H10Q 109.9 . . ? O103 C109 H10R 109.9 . . ? C110 C109 H10R 109.9 . . ? H10Q C109 H10R 108.3 . . ? O104 C110 C109 109.1(2) . . ? O104 C110 H11G 109.9 . . ? C109 C110 H11G 109.9 . . ? O104 C110 H11H 109.9 . . ? C109 C110 H11H 109.9 . . ? H11G C110 H11H 108.3 . . ? O104 C111 C112 109.3(2) . . ? O104 C111 H11I 109.8 . . ? C112 C111 H11I 109.8 . . ? O104 C111 H11J 109.8 . . ? C112 C111 H11J 109.8 . . ? H11I C111 H11J 108.3 . . ? N102 C112 C111 113.9(2) . . ? N102 C112 H11K 108.8 . . ? C111 C112 H11K 108.8 . . ? N102 C112 H11L 108.8 . . ? C111 C112 H11L 108.8 . . ? H11K C112 H11L 107.7 . . ? N101 C113 C114 114.1(3) . . ? N101 C113 H11M 108.7 . . ? C114 C113 H11M 108.7 . . ? N101 C113 H11N 108.7 . . ? C114 C113 H11N 108.7 . . ? H11M C113 H11N 107.6 . . ? O105 C114 C113 108.6(2) . . ? O105 C114 H11O 110.0 . . ? C113 C114 H11O 110.0 . . ? O105 C114 H11P 110.0 . . ? C113 C114 H11P 110.0 . . ? H11O C114 H11P 108.3 . . ? O105 C115 C116 109.4(2) . . ? O105 C115 H11Q 109.8 . . ? C116 C115 H11Q 109.8 . . ? O105 C115 H11R 109.8 . . ? C116 C115 H11R 109.8 . . ? H11Q C115 H11R 108.2 . . ? O106 C116 C115 109.5(2) . . ? O106 C116 H11S 109.8 . . ? C115 C116 H11S 109.8 . . ? O106 C116 H11T 109.8 . . ? C115 C116 H11T 109.8 . . ? H11S C116 H11T 108.2 . . ? O106 C117 C118 109.4(2) . . ? O106 C117 H11U 109.8 . . ? C118 C117 H11U 109.8 . . ? O106 C117 H11V 109.8 . . ? C118 C117 H11V 109.8 . . ? H11U C117 H11V 108.2 . . ? N102 C118 C117 113.7(3) . . ? N102 C118 H11W 108.8 . . ? C117 C118 H11W 108.8 . . ? N102 C118 H11X 108.8 . . ? C117 C118 H11X 108.8 . . ? H11W C118 H11X 107.7 . . ? C4S O1S C1S 119.3(9) . . ? C2S C1S O1S 99.8(9) . . ? C2S C1S H1S1 111.8 . . ? O1S C1S H1S1 111.8 . . ? C2S C1S H1S2 111.8 . . ? O1S C1S H1S2 111.8 . . ? H1S1 C1S H1S2 109.5 . . ? C1S C2S C3S 117.0(10) . . ? C1S C2S H2S1 108.0 . . ? C3S C2S H2S1 108.0 . . ? C1S C2S H2S2 108.0 . . ? C3S C2S H2S2 108.0 . . ? H2S1 C2S H2S2 107.3 . . ? C2S C3S C4S 98.7(9) . . ? C2S C3S H3S1 112.0 . . ? C4S C3S H3S1 112.0 . . ? C2S C3S H3S2 112.0 . . ? C4S C3S H3S2 112.0 . . ? H3S1 C3S H3S2 109.7 . . ? O1S C4S C3S 103.7(8) . . ? O1S C4S H4S1 111.0 . . ? C3S C4S H4S1 111.0 . . ? O1S C4S H4S2 111.0 . . ? C3S C4S H4S2 111.0 . . ? H4S1 C4S H4S2 109.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.901 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.050 _iucr_refine_instructions_details ; TITL p21n in P2(1)/n CELL 1.54178 10.8094 25.7657 31.1703 90.000 94.291 90.000 ZERR 4.00 0.0001 0.0004 0.0004 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O AL K FE UNIT 356 544 24 26 4 4 4 MERG 2 OMIT 0.00 133.00 DFIX 1.450 0.020 O1S C2S DFIX 1.450 0.020 O1S C1S DFIX 1.450 0.020 C1S C2S DFIX 1.450 0.020 C2S C3S DFIX 1.450 0.020 C3S C4S DFIX 1.450 0.020 C4S O1S DFIX 2.450 0.020 O1S C2S DFIX 2.450 0.020 O1S C3S DFIX 2.450 0.020 C1S C3S DFIX 2.450 0.020 C2S C4S DFIX 2.450 0.020 C4S C1S SIMU O1S C1S SIMU C1S C2S SIMU C2S C3S SIMU C3S C4S SIMU C4S O1S FMAP 2 PLAN 20 SIZE 0.06 0.06 0.20 ACTA BOND $H L.S. 12 TEMP -123.00 WGHT 0.078900 0.796000 FVAR 0.06314 FE1 7 0.195172 0.254180 0.587110 11.00000 0.02736 0.02524 = 0.02477 -0.00079 0.00630 -0.00321 AL1 5 0.452689 0.253715 0.409320 11.00000 0.03942 0.03026 = 0.03431 -0.00116 0.01498 -0.00187 N1 3 0.328639 0.180819 0.475567 11.00000 0.02755 0.02472 = 0.02694 -0.00206 0.00469 -0.00127 N2 3 0.325471 0.259476 0.496606 11.00000 0.02191 0.02638 = 0.02440 0.00100 0.00416 -0.00124 N3 3 0.196263 0.347626 0.655965 11.00000 0.02365 0.02334 = 0.02410 0.00153 0.00291 0.00063 N4 3 0.222633 0.414921 0.619020 11.00000 0.02318 0.02483 = 0.02479 0.00268 0.00236 -0.00310 C1 1 0.357896 0.229540 0.463130 11.00000 0.02089 0.02652 = 0.02863 -0.00314 0.00316 -0.00026 C2 1 0.279541 0.181786 0.515783 11.00000 0.03213 0.02826 = 0.02693 0.00137 0.00543 -0.00092 AFIX 43 H2 2 0.253170 0.152128 0.530743 11.00000 -1.20000 AFIX 0 C3 1 0.275103 0.231395 0.530314 11.00000 0.02595 0.02738 = 0.02718 0.00265 0.00370 -0.00193 C4 1 0.332193 0.134121 0.450054 11.00000 0.03510 0.02295 = 0.03017 -0.00288 0.00766 -0.00132 C5 1 0.438405 0.102782 0.453791 11.00000 0.04115 0.03531 = 0.03963 -0.00579 0.00365 0.00506 C6 1 0.435630 0.057177 0.429128 11.00000 0.05045 0.03217 = 0.05126 -0.00625 0.00922 0.00742 AFIX 43 H6 2 0.505939 0.034945 0.430870 11.00000 -1.20000 AFIX 0 C7 1 0.333907 0.044062 0.402649 11.00000 0.05868 0.03080 = 0.05492 -0.01335 0.01039 -0.00547 AFIX 43 H7 2 0.334587 0.013085 0.386139 11.00000 -1.20000 AFIX 0 C8 1 0.230267 0.075476 0.399724 11.00000 0.04359 0.04371 = 0.05098 -0.01521 0.00314 -0.01069 AFIX 43 H8 2 0.160210 0.065653 0.381292 11.00000 -1.20000 AFIX 0 C9 1 0.226353 0.121289 0.423257 11.00000 0.03608 0.03435 = 0.03647 -0.00533 0.00615 -0.00728 C10 1 0.553127 0.115820 0.482243 11.00000 0.04653 0.06354 = 0.05839 -0.02496 -0.00851 0.01733 AFIX 13 H10 2 0.539026 0.148971 0.497833 11.00000 -1.20000 AFIX 0 C11 1 0.665887 0.121986 0.456129 11.00000 0.04711 0.05920 = 0.07535 -0.00290 -0.00832 -0.00577 AFIX 123 H11A 2 0.738823 0.130376 0.475464 10.50000 -1.50000 H11B 2 0.650808 0.150048 0.435165 10.50000 -1.50000 H11C 2 0.680551 0.089500 0.440964 10.50000 -1.50000 H11D 2 0.641299 0.116240 0.425598 10.50000 -1.50000 H11E 2 0.729313 0.096569 0.465897 10.50000 -1.50000 H11F 2 0.699570 0.157116 0.460098 10.50000 -1.50000 AFIX 0 C12 1 0.582632 0.072344 0.515312 11.00000 0.06550 0.14044 = 0.04218 0.00665 -0.00030 0.02140 AFIX 123 H12A 2 0.656900 0.081615 0.533675 10.50000 -1.50000 H12B 2 0.597392 0.039828 0.500203 10.50000 -1.50000 H12C 2 0.512385 0.067913 0.533109 10.50000 -1.50000 H12D 2 0.520885 0.044622 0.510983 10.50000 -1.50000 H12E 2 0.580393 0.086409 0.544455 10.50000 -1.50000 H12F 2 0.665400 0.058325 0.511549 10.50000 -1.50000 AFIX 0 C13 1 0.112069 0.155526 0.419777 11.00000 0.03546 0.05127 = 0.05284 -0.01602 -0.00502 -0.00082 AFIX 13 H13 2 0.138876 0.191719 0.427417 11.00000 -1.20000 AFIX 0 C14 1 0.047951 0.156677 0.374489 11.00000 0.04794 0.07870 = 0.05566 0.00076 -0.00808 0.00565 AFIX 123 H14A 2 -0.024609 0.179531 0.374014 10.50000 -1.50000 H14B 2 0.021402 0.121521 0.366074 10.50000 -1.50000 H14C 2 0.105873 0.169719 0.354288 10.50000 -1.50000 H14D 2 0.093053 0.134316 0.355570 10.50000 -1.50000 H14E 2 0.047042 0.192326 0.363510 10.50000 -1.50000 H14F 2 -0.037429 0.144129 0.375296 10.50000 -1.50000 AFIX 0 C15 1 0.018364 0.138843 0.451110 11.00000 0.04191 0.14017 = 0.05882 -0.00937 0.01041 0.01407 AFIX 123 H15A 2 -0.053827 0.161931 0.448215 10.50000 -1.50000 H15B 2 0.056619 0.140736 0.480581 10.50000 -1.50000 H15C 2 -0.008088 0.103113 0.444725 10.50000 -1.50000 H15D 2 0.050296 0.108589 0.467466 10.50000 -1.50000 H15E 2 -0.060149 0.129784 0.435100 10.50000 -1.50000 H15F 2 0.004557 0.167407 0.470956 10.50000 -1.50000 AFIX 0 C16 1 0.324974 0.315192 0.494640 11.00000 0.02761 0.02420 = 0.02314 0.00053 0.00713 -0.00138 C17 1 0.432667 0.342941 0.507763 11.00000 0.03033 0.03394 = 0.02489 -0.00228 0.00838 -0.00455 C18 1 0.427448 0.396700 0.503862 11.00000 0.04134 0.03629 = 0.03366 -0.00300 0.01090 -0.01417 AFIX 43 H18 2 0.499532 0.416657 0.511678 11.00000 -1.20000 AFIX 0 C19 1 0.319409 0.421736 0.488828 11.00000 0.05577 0.02739 = 0.03461 0.00290 0.01015 -0.00266 AFIX 43 H19 2 0.317627 0.458527 0.486876 11.00000 -1.20000 AFIX 0 C20 1 0.214418 0.393369 0.476687 11.00000 0.04335 0.03113 = 0.03098 0.00336 0.00367 0.00395 AFIX 43 H20 2 0.140718 0.410928 0.466489 11.00000 -1.20000 AFIX 0 C21 1 0.214641 0.339628 0.479117 11.00000 0.03271 0.03100 = 0.02265 -0.00014 0.00463 0.00134 C22 1 0.549184 0.315036 0.526554 11.00000 0.02597 0.04383 = 0.03995 -0.00534 0.00584 -0.00479 AFIX 13 H22 2 0.557623 0.282009 0.510178 11.00000 -1.20000 AFIX 0 C23 1 0.668031 0.346610 0.523237 11.00000 0.03002 0.06572 = 0.06728 -0.01010 0.01048 -0.01185 AFIX 123 H23A 2 0.739246 0.326662 0.535578 10.50000 -1.50000 H23B 2 0.661886 0.379256 0.539069 10.50000 -1.50000 H23C 2 0.679054 0.354127 0.492940 10.50000 -1.50000 H23D 2 0.647545 0.380035 0.509480 10.50000 -1.50000 H23E 2 0.724904 0.327441 0.505989 10.50000 -1.50000 H23F 2 0.707737 0.352570 0.552118 10.50000 -1.50000 AFIX 0 C24 1 0.537555 0.301099 0.573784 11.00000 0.03149 0.06532 = 0.04298 0.00493 -0.00305 0.00018 AFIX 123 H24A 2 0.612805 0.283037 0.585139 10.50000 -1.50000 H24B 2 0.465518 0.278452 0.576090 10.50000 -1.50000 H24C 2 0.526893 0.332880 0.590382 10.50000 -1.50000 H24D 2 0.457339 0.313209 0.582602 10.50000 -1.50000 H24E 2 0.604626 0.317794 0.591651 10.50000 -1.50000 H24F 2 0.543251 0.263366 0.577358 10.50000 -1.50000 AFIX 0 C25 1 0.098248 0.309183 0.464995 11.00000 0.02646 0.03549 = 0.03489 0.00024 0.00015 0.00093 AFIX 13 H25 2 0.113056 0.272041 0.473150 11.00000 -1.20000 AFIX 0 C26 1 0.070728 0.311580 0.416249 11.00000 0.03776 0.05924 = 0.03570 -0.00472 0.00072 -0.00590 AFIX 123 H26A 2 -0.004273 0.291451 0.408063 10.50000 -1.50000 H26B 2 0.140874 0.297050 0.402075 10.50000 -1.50000 H26C 2 0.057928 0.347777 0.407336 10.50000 -1.50000 H26D 2 0.133959 0.332734 0.403586 10.50000 -1.50000 H26E 2 -0.011188 0.327136 0.409574 10.50000 -1.50000 H26F 2 0.071758 0.276408 0.404313 10.50000 -1.50000 AFIX 0 C27 1 -0.013639 0.328276 0.487768 11.00000 0.03174 0.04783 = 0.04258 0.00178 0.00605 0.00379 AFIX 123 H27A 2 -0.086886 0.307781 0.478129 10.50000 -1.50000 H27B 2 -0.028853 0.364932 0.480839 10.50000 -1.50000 H27C 2 0.003097 0.324353 0.518935 10.50000 -1.50000 H27D 2 0.011791 0.356930 0.507140 10.50000 -1.50000 H27E 2 -0.046241 0.299779 0.504430 10.50000 -1.50000 H27F 2 -0.078192 0.340357 0.466334 10.50000 -1.50000 AFIX 0 C28 1 0.205332 0.400315 0.660268 11.00000 0.02250 0.02730 = 0.02855 0.00184 0.00076 0.00074 C29 1 0.207283 0.327976 0.613665 11.00000 0.02201 0.03027 = 0.02442 -0.00144 0.00372 -0.00250 C30 1 0.223200 0.372358 0.591164 11.00000 0.02298 0.02848 = 0.02489 -0.00077 0.00388 -0.00347 AFIX 43 H30 2 0.233164 0.374193 0.561178 11.00000 -1.20000 AFIX 0 C31 1 0.177641 0.316083 0.693066 11.00000 0.03767 0.02417 = 0.02521 0.00073 0.00592 0.00287 C32 1 0.276118 0.309269 0.724600 11.00000 0.04851 0.02693 = 0.02989 0.00006 -0.00107 0.00688 C33 1 0.253309 0.280054 0.760885 11.00000 0.07295 0.03524 = 0.02883 0.00432 -0.00131 0.01165 AFIX 43 H33 2 0.318077 0.274783 0.782771 11.00000 -1.20000 AFIX 0 C34 1 0.137276 0.258616 0.765396 11.00000 0.08224 0.03836 = 0.03549 0.01094 0.02051 0.00732 AFIX 43 H34 2 0.123732 0.238717 0.790271 11.00000 -1.20000 AFIX 0 C35 1 0.041955 0.265761 0.734457 11.00000 0.06100 0.03795 = 0.04087 0.00754 0.02323 -0.00032 AFIX 43 H35 2 -0.036740 0.250584 0.737975 11.00000 -1.20000 AFIX 0 C36 1 0.059613 0.295216 0.697746 11.00000 0.04201 0.02835 = 0.03120 0.00072 0.01482 0.00064 C37 1 0.402219 0.333445 0.719359 11.00000 0.04528 0.03455 = 0.04518 0.00384 -0.01491 0.00334 AFIX 13 H37 2 0.387787 0.370213 0.710006 11.00000 -1.20000 AFIX 0 C38 1 0.469516 0.306460 0.684580 11.00000 0.03933 0.06916 = 0.04653 0.00719 -0.00263 0.00044 AFIX 123 H38A 2 0.550229 0.323068 0.682096 10.50000 -1.50000 H38B 2 0.419849 0.309083 0.657046 10.50000 -1.50000 H38C 2 0.481900 0.269815 0.692151 10.50000 -1.50000 H38D 2 0.417757 0.278242 0.672099 10.50000 -1.50000 H38E 2 0.548137 0.292228 0.697149 10.50000 -1.50000 H38F 2 0.486086 0.331496 0.662045 10.50000 -1.50000 AFIX 0 C39 1 0.486637 0.334651 0.761080 11.00000 0.06161 0.07010 = 0.05755 -0.00790 -0.02307 0.01005 AFIX 123 H39A 2 0.566039 0.350748 0.755558 10.50000 -1.50000 H39B 2 0.501120 0.299134 0.771529 10.50000 -1.50000 H39C 2 0.446751 0.354844 0.782841 10.50000 -1.50000 H39D 2 0.443234 0.319069 0.784394 10.50000 -1.50000 H39E 2 0.508153 0.370683 0.768423 10.50000 -1.50000 H39F 2 0.562522 0.314974 0.757111 10.50000 -1.50000 AFIX 0 C40 1 -0.048626 0.306706 0.665347 11.00000 0.03276 0.04384 = 0.04065 0.00031 0.01257 -0.00532 AFIX 13 H40 2 -0.014778 0.310871 0.636554 11.00000 -1.20000 AFIX 0 C41 1 -0.146888 0.263820 0.661361 11.00000 0.03836 0.05764 = 0.07000 -0.00633 0.01821 -0.01299 AFIX 123 H41A 2 -0.107848 0.231007 0.653974 10.50000 -1.50000 H41B 2 -0.211044 0.273003 0.638752 10.50000 -1.50000 H41C 2 -0.184657 0.260002 0.688805 10.50000 -1.50000 H41D 2 -0.227851 0.278335 0.667047 10.50000 -1.50000 H41E 2 -0.124655 0.236338 0.682268 10.50000 -1.50000 H41F 2 -0.151043 0.249340 0.632216 10.50000 -1.50000 AFIX 0 C42 1 -0.109514 0.358277 0.676521 11.00000 0.03907 0.04884 = 0.06669 0.00674 0.00453 0.00184 AFIX 123 H42A 2 -0.178869 0.365609 0.655317 10.50000 -1.50000 H42B 2 -0.048266 0.386285 0.676143 10.50000 -1.50000 H42C 2 -0.140293 0.355874 0.705239 10.50000 -1.50000 H42D 2 -0.066083 0.372903 0.702482 10.50000 -1.50000 H42E 2 -0.196686 0.352227 0.681657 10.50000 -1.50000 H42F 2 -0.104660 0.382638 0.652560 10.50000 -1.50000 AFIX 0 C43 1 0.226823 0.468409 0.605808 11.00000 0.03093 0.02670 = 0.02728 0.00276 0.00075 -0.00353 C44 1 0.340929 0.491776 0.599646 11.00000 0.03276 0.03220 = 0.02578 -0.00010 0.00237 -0.00691 C45 1 0.340519 0.544035 0.587552 11.00000 0.04352 0.03734 = 0.04028 0.00455 0.00316 -0.01501 AFIX 43 H45 2 0.416738 0.560693 0.582854 11.00000 -1.20000 AFIX 0 C46 1 0.231004 0.571912 0.582307 11.00000 0.05449 0.03061 = 0.05542 0.01382 -0.00517 -0.00788 AFIX 43 H46 2 0.232527 0.607622 0.574775 11.00000 -1.20000 AFIX 0 C47 1 0.119505 0.547679 0.588053 11.00000 0.04231 0.03713 = 0.06024 0.01332 -0.00889 0.00203 AFIX 43 H47 2 0.044565 0.566931 0.584092 11.00000 -1.20000 AFIX 0 C48 1 0.114951 0.495529 0.599547 11.00000 0.03354 0.03321 = 0.04045 0.00689 -0.00410 -0.00269 C49 1 0.461347 0.461436 0.606566 11.00000 0.02915 0.03680 = 0.03844 -0.00408 0.00577 -0.00847 AFIX 13 H49 2 0.445498 0.425415 0.595543 11.00000 -1.20000 AFIX 0 C50 1 0.565697 0.484566 0.582250 11.00000 0.03573 0.05189 = 0.05854 -0.01083 0.01638 -0.01449 AFIX 123 H50A 2 0.640921 0.463628 0.587702 10.50000 -1.50000 H50B 2 0.582081 0.520202 0.592091 10.50000 -1.50000 H50C 2 0.541088 0.484718 0.551346 10.50000 -1.50000 H50D 2 0.535139 0.515404 0.566390 10.50000 -1.50000 H50E 2 0.593979 0.458830 0.562002 10.50000 -1.50000 H50F 2 0.634972 0.494314 0.602747 10.50000 -1.50000 AFIX 0 C51 1 0.502707 0.457623 0.654267 11.00000 0.02950 0.05561 = 0.04507 -0.00081 -0.00204 0.00033 AFIX 123 H51A 2 0.580288 0.437893 0.657933 10.50000 -1.50000 H51B 2 0.438520 0.439951 0.669407 10.50000 -1.50000 H51C 2 0.515918 0.492570 0.666147 10.50000 -1.50000 H51D 2 0.442863 0.475717 0.671058 10.50000 -1.50000 H51E 2 0.584630 0.473658 0.659584 10.50000 -1.50000 H51F 2 0.507233 0.421039 0.662845 10.50000 -1.50000 AFIX 0 C52 1 -0.009063 0.469263 0.603396 11.00000 0.03058 0.03607 = 0.06619 0.01414 -0.00270 -0.00005 AFIX 13 H52 2 0.006655 0.434703 0.617353 11.00000 -1.20000 AFIX 0 C53 1 -0.073581 0.460104 0.558786 11.00000 0.03755 0.06059 = 0.08253 -0.02304 -0.00048 -0.00757 AFIX 123 H53A 2 -0.153487 0.442958 0.561616 10.50000 -1.50000 H53B 2 -0.021321 0.438017 0.542016 10.50000 -1.50000 H53C 2 -0.087352 0.493458 0.544087 10.50000 -1.50000 H53D 2 -0.021287 0.473331 0.536863 10.50000 -1.50000 H53E 2 -0.153453 0.478272 0.556464 10.50000 -1.50000 H53F 2 -0.087421 0.422831 0.554392 10.50000 -1.50000 AFIX 0 C54 1 -0.092457 0.500408 0.631200 11.00000 0.04440 0.08994 = 0.05950 -0.01121 0.00898 -0.01282 AFIX 123 H54A 2 -0.171331 0.482080 0.633027 10.50000 -1.50000 H54B 2 -0.108171 0.534698 0.618320 10.50000 -1.50000 H54C 2 -0.051471 0.504466 0.660127 10.50000 -1.50000 H54D 2 -0.049318 0.532082 0.641289 10.50000 -1.50000 H54E 2 -0.112477 0.479465 0.655996 10.50000 -1.50000 H54F 2 -0.169178 0.509697 0.614189 10.50000 -1.50000 AFIX 0 C55 1 0.093893 0.193148 0.609833 11.00000 0.03291 0.02686 = 0.03224 -0.00262 0.00859 -0.00246 C56 1 0.133482 0.164219 0.646995 11.00000 0.03645 0.02439 = 0.03841 0.00044 0.00643 0.00168 C57 1 0.067481 0.121062 0.660030 11.00000 0.04570 0.02761 = 0.04675 0.00495 0.01031 0.00267 AFIX 43 H57 2 0.096422 0.102917 0.685353 11.00000 -1.20000 AFIX 0 C58 1 -0.039239 0.104195 0.636800 11.00000 0.04416 0.02812 = 0.06057 0.00162 0.01259 -0.00633 C59 1 -0.081541 0.132857 0.600724 11.00000 0.03388 0.03872 = 0.05789 -0.00460 0.00605 -0.00780 AFIX 43 H59 2 -0.155600 0.122536 0.584654 11.00000 -1.20000 AFIX 0 C60 1 -0.017633 0.176205 0.587785 11.00000 0.03336 0.03621 = 0.03820 -0.00257 0.00526 -0.00355 C61 1 0.247488 0.180540 0.674794 11.00000 0.04376 0.03398 = 0.04072 0.00021 -0.00345 0.00363 AFIX 123 H61A 2 0.284798 0.211014 0.662071 10.50000 -1.50000 H61B 2 0.307614 0.152012 0.676628 10.50000 -1.50000 H61C 2 0.223937 0.189170 0.703700 10.50000 -1.50000 H61D 2 0.259435 0.157117 0.699528 10.50000 -1.50000 H61E 2 0.236619 0.216119 0.684971 10.50000 -1.50000 H61F 2 0.320296 0.178961 0.657899 10.50000 -1.50000 AFIX 0 C62 1 -0.105845 0.055547 0.649631 11.00000 0.06027 0.03568 = 0.09572 0.00758 0.01774 -0.01412 AFIX 123 H62A 2 -0.063037 0.040906 0.675699 10.50000 -1.50000 H62B 2 -0.106148 0.030077 0.626274 10.50000 -1.50000 H62C 2 -0.191461 0.064171 0.655226 10.50000 -1.50000 H62D 2 -0.177393 0.049197 0.629100 10.50000 -1.50000 H62E 2 -0.134282 0.060026 0.678526 10.50000 -1.50000 H62F 2 -0.048970 0.025932 0.649573 10.50000 -1.50000 AFIX 0 C63 1 -0.073561 0.207488 0.549979 11.00000 0.04121 0.05594 = 0.04540 0.00440 -0.00480 -0.00838 AFIX 123 H63A 2 -0.018972 0.236752 0.544541 10.50000 -1.50000 H63B 2 -0.155100 0.220613 0.556564 10.50000 -1.50000 H63C 2 -0.082774 0.185327 0.524387 10.50000 -1.50000 H63D 2 -0.152258 0.191709 0.539120 10.50000 -1.50000 H63E 2 -0.016131 0.207848 0.527098 10.50000 -1.50000 H63F 2 -0.088457 0.243135 0.559274 10.50000 -1.50000 AFIX 0 C64 1 0.404381 0.325611 0.389968 11.00000 0.04806 0.03730 = 0.03483 0.00174 0.01265 0.00225 AFIX 23 H64A 2 0.318247 0.325167 0.376714 11.00000 -1.20000 H64B 2 0.406903 0.348943 0.415253 11.00000 -1.20000 AFIX 0 C65 1 0.490806 0.346631 0.357502 11.00000 0.05324 0.03663 = 0.04110 0.00338 0.01193 -0.00963 AFIX 123 H65A 2 0.464674 0.381736 0.348778 10.50000 -1.50000 H65B 2 0.487264 0.323972 0.332188 10.50000 -1.50000 H65C 2 0.575947 0.347674 0.370705 10.50000 -1.50000 H65D 2 0.553916 0.320519 0.352336 10.50000 -1.50000 H65E 2 0.531326 0.378283 0.368926 10.50000 -1.50000 H65F 2 0.442643 0.354581 0.330409 10.50000 -1.50000 AFIX 0 C66 1 0.636139 0.256663 0.430248 11.00000 0.03505 0.05144 = 0.05171 -0.00143 0.00397 -0.00445 AFIX 23 H66A 2 0.655445 0.291998 0.441287 11.00000 -1.20000 H66B 2 0.651076 0.232169 0.454555 11.00000 -1.20000 AFIX 0 C67 1 0.725029 0.243533 0.395914 11.00000 0.03953 0.07551 = 0.06910 -0.00561 0.01349 -0.00114 AFIX 123 H67A 2 0.810768 0.245825 0.408425 10.50000 -1.50000 H67B 2 0.712809 0.268141 0.371999 10.50000 -1.50000 H67C 2 0.708497 0.208217 0.385308 10.50000 -1.50000 H67D 2 0.677281 0.235630 0.368730 10.50000 -1.50000 H67E 2 0.775240 0.213314 0.405156 10.50000 -1.50000 H67F 2 0.779552 0.273239 0.391846 10.50000 -1.50000 AFIX 0 C68 1 0.421221 0.203310 0.361293 11.00000 0.04922 0.04366 = 0.03945 -0.00489 0.01152 -0.00734 AFIX 23 H68A 2 0.500545 0.196565 0.348344 11.00000 -1.20000 H68B 2 0.393427 0.170132 0.373387 11.00000 -1.20000 AFIX 0 C69 1 0.324556 0.220492 0.325433 11.00000 0.05281 0.06146 = 0.05715 -0.01528 0.00065 -0.00148 AFIX 123 H69A 2 0.315126 0.193348 0.303407 10.50000 -1.50000 H69B 2 0.352171 0.252700 0.312421 10.50000 -1.50000 H69C 2 0.244738 0.226383 0.337606 10.50000 -1.50000 H69D 2 0.292897 0.254939 0.332215 10.50000 -1.50000 H69E 2 0.255852 0.195587 0.323201 10.50000 -1.50000 H69F 2 0.363285 0.221905 0.298017 10.50000 -1.50000 AFIX 0 K101 6 0.527729 -0.047464 0.277936 11.00000 0.03166 0.03501 = 0.03446 0.00085 0.00162 0.00051 N101 3 0.358567 -0.134874 0.248048 11.00000 0.04359 0.03989 = 0.04678 0.00477 -0.00358 -0.00676 N102 3 0.694060 0.038604 0.308242 11.00000 0.03618 0.03894 = 0.04282 -0.00241 0.00174 -0.00203 O101 4 0.270730 -0.028424 0.256144 11.00000 0.03612 0.04741 = 0.05201 0.01030 -0.00612 -0.00239 O102 4 0.439636 0.054411 0.270144 11.00000 0.03575 0.03469 = 0.05103 -0.00319 0.00437 0.00449 O103 4 0.588648 -0.109487 0.208040 11.00000 0.05148 0.03909 = 0.04308 -0.00023 0.00628 0.00127 O104 4 0.766906 -0.040535 0.246098 11.00000 0.04220 0.04474 = 0.03689 0.00444 0.01044 0.00133 O105 4 0.472526 -0.126420 0.335410 11.00000 0.04079 0.04778 = 0.03837 0.00530 0.00504 -0.00472 O106 4 0.599519 -0.037697 0.368249 11.00000 0.03983 0.04624 = 0.03683 -0.00017 -0.00151 0.00229 C101 1 0.228065 -0.118763 0.245913 11.00000 0.04314 0.04963 = 0.07567 0.00536 -0.01234 -0.01277 AFIX 23 H10A 2 0.198421 -0.120277 0.275178 11.00000 -1.20000 H10B 2 0.178168 -0.143650 0.227652 11.00000 -1.20000 AFIX 0 C102 1 0.206594 -0.064843 0.228140 11.00000 0.03966 0.05815 = 0.06651 0.00983 -0.01725 -0.00808 AFIX 23 H10C 2 0.237257 -0.062504 0.199060 11.00000 -1.20000 H10D 2 0.116707 -0.056953 0.225791 11.00000 -1.20000 AFIX 0 C103 1 0.241300 0.023530 0.244221 11.00000 0.03412 0.05191 = 0.04935 0.01043 0.00009 0.00697 AFIX 23 H10E 2 0.150966 0.029342 0.245011 11.00000 -1.20000 H10F 2 0.264136 0.030057 0.214527 11.00000 -1.20000 AFIX 0 C104 1 0.310303 0.059707 0.274483 11.00000 0.03909 0.04840 = 0.05162 0.00323 0.00850 0.01092 AFIX 23 H10G 2 0.284138 0.095870 0.268034 11.00000 -1.20000 H10H 2 0.291787 0.051666 0.304394 11.00000 -1.20000 AFIX 0 C105 1 0.509069 0.095151 0.291724 11.00000 0.05224 0.03121 = 0.05703 -0.00535 0.00009 0.00381 AFIX 23 H10I 2 0.492334 0.095650 0.322516 11.00000 -1.20000 H10J 2 0.483611 0.129039 0.278956 11.00000 -1.20000 AFIX 0 C106 1 0.645350 0.086596 0.287475 11.00000 0.04925 0.03569 = 0.05585 0.00098 -0.00013 -0.00674 AFIX 23 H10K 2 0.660267 0.085377 0.256539 11.00000 -1.20000 H10L 2 0.691973 0.116559 0.300319 11.00000 -1.20000 AFIX 0 C107 1 0.391384 -0.151129 0.205051 11.00000 0.06598 0.04924 = 0.04201 -0.00073 -0.01072 -0.01349 AFIX 23 H10M 2 0.359621 -0.124938 0.183747 11.00000 -1.20000 H10N 2 0.349299 -0.184409 0.197619 11.00000 -1.20000 AFIX 0 C108 1 0.528533 -0.157795 0.201424 11.00000 0.07031 0.04453 = 0.04010 -0.00647 0.00368 -0.00149 AFIX 23 H10O 2 0.562285 -0.183091 0.223164 11.00000 -1.20000 H10P 2 0.543589 -0.171341 0.172552 11.00000 -1.20000 AFIX 0 C109 1 0.717618 -0.113561 0.201615 11.00000 0.05319 0.05328 = 0.04167 -0.00352 0.01504 0.01094 AFIX 23 H10Q 2 0.728689 -0.129323 0.173191 11.00000 -1.20000 H10R 2 0.759217 -0.136019 0.224077 11.00000 -1.20000 AFIX 0 C110 1 0.773560 -0.060674 0.203820 11.00000 0.04463 0.05830 = 0.04010 0.00149 0.01566 0.00553 AFIX 23 H11G 2 0.861198 -0.062429 0.196704 11.00000 -1.20000 H11H 2 0.728144 -0.037577 0.182702 11.00000 -1.20000 AFIX 0 C111 1 0.823655 0.009261 0.249868 11.00000 0.03323 0.05030 = 0.05223 0.00629 0.01083 -0.00101 AFIX 23 H11I 2 0.778938 0.033894 0.229865 11.00000 -1.20000 H11J 2 0.910710 0.007011 0.242177 11.00000 -1.20000 AFIX 0 C112 1 0.820161 0.028337 0.295374 11.00000 0.03374 0.05328 = 0.05208 0.00090 0.00249 -0.00647 AFIX 23 H11K 2 0.860024 0.002122 0.315094 11.00000 -1.20000 H11L 2 0.869440 0.060667 0.298689 11.00000 -1.20000 AFIX 0 C113 1 0.379385 -0.178082 0.278353 11.00000 0.05474 0.03842 = 0.05321 0.00464 0.00090 -0.00806 AFIX 23 H11M 2 0.461165 -0.193812 0.274158 11.00000 -1.20000 H11N 2 0.315331 -0.204911 0.271563 11.00000 -1.20000 AFIX 0 C114 1 0.375894 -0.162710 0.325084 11.00000 0.04616 0.04512 = 0.05105 0.01170 0.00628 -0.00764 AFIX 23 H11O 2 0.294593 -0.146955 0.329955 11.00000 -1.20000 H11P 2 0.387330 -0.193744 0.343685 11.00000 -1.20000 AFIX 0 C115 1 0.487207 -0.115622 0.380087 11.00000 0.04723 0.05763 = 0.03679 0.00828 0.00867 0.00132 AFIX 23 H11Q 2 0.489203 -0.148487 0.396579 11.00000 -1.20000 H11R 2 0.416234 -0.094713 0.388621 11.00000 -1.20000 AFIX 0 C116 1 0.605954 -0.086297 0.389975 11.00000 0.04817 0.05278 = 0.03229 0.00481 0.00352 0.00706 AFIX 23 H11S 2 0.619429 -0.080582 0.421385 11.00000 -1.20000 H11T 2 0.676603 -0.106728 0.380554 11.00000 -1.20000 AFIX 0 C117 1 0.709227 -0.007999 0.378263 11.00000 0.03995 0.05616 = 0.03742 -0.00554 -0.00434 0.00226 AFIX 23 H11U 2 0.782337 -0.027158 0.369263 11.00000 -1.20000 H11V 2 0.720678 -0.002140 0.409699 11.00000 -1.20000 AFIX 0 C118 1 0.698198 0.043237 0.355207 11.00000 0.04360 0.04972 = 0.04399 -0.00927 -0.00267 -0.00357 AFIX 23 H11W 2 0.621863 0.060929 0.363129 11.00000 -1.20000 H11X 2 0.769716 0.065291 0.365109 11.00000 -1.20000 AFIX 0 PART -1 O1S 4 0.868683 -0.003637 0.479313 10.50000 0.09818 0.34433 = 0.10389 -0.08728 -0.01667 0.06981 C1S 1 0.895891 0.023080 0.518838 10.50000 0.12323 0.18970 = 0.08395 -0.01807 0.01259 0.06483 AFIX 23 H1S1 2 0.883330 0.060981 0.515616 10.50000 -1.20000 H1S2 2 0.845837 0.009865 0.541825 10.50000 -1.20000 AFIX 0 C2S 1 1.019184 0.010634 0.526381 10.50000 0.14225 0.16184 = 0.05894 -0.00425 -0.03803 0.03272 AFIX 23 H2S1 2 1.027447 -0.013500 0.551144 10.50000 -1.20000 H2S2 2 1.064889 0.042702 0.535068 10.50000 -1.20000 AFIX 0 C3S 1 1.081540 -0.013479 0.490061 10.50000 0.10392 0.16464 = 0.07492 0.04357 0.00339 0.08740 AFIX 23 H3S1 2 1.127922 -0.045254 0.499114 10.50000 -1.20000 H3S2 2 1.137616 0.011171 0.476767 10.50000 -1.20000 AFIX 0 C4S 1 0.962483 -0.026081 0.459366 10.50000 0.11511 0.18083 = 0.05542 -0.02745 -0.01785 0.08927 AFIX 23 H4S1 2 0.969275 -0.010973 0.430434 10.50000 -1.20000 H4S2 2 0.949806 -0.064014 0.456514 10.50000 -1.20000 HKLF 4 REM p21n in P2(1)/n REM R1 = 0.0483 for 11934 Fo > 4sig(Fo) and 0.0657 for all 15228 data REM 964 parameters refined using 41 restraints END WGHT 0.0789 0.7961 REM Highest difference peak 0.901, deepest hole -0.513, 1-sigma level 0.050 Q1 1 0.3842 0.2553 0.3926 11.00000 0.05 0.90 Q2 1 0.2667 0.2241 0.3514 11.00000 0.05 0.50 Q3 1 1.1363 0.0431 0.5203 11.00000 0.05 0.46 Q4 1 0.5717 0.2202 0.3899 11.00000 0.05 0.44 Q5 1 0.5596 0.1214 0.5195 11.00000 0.05 0.44 Q6 1 0.8830 0.0146 0.4683 11.00000 0.05 0.27 Q7 1 0.0131 0.1159 0.3779 11.00000 0.05 0.26 Q8 1 0.1957 0.3029 0.6087 11.00000 0.05 0.24 Q9 1 0.0112 0.2162 0.5271 11.00000 0.05 0.23 Q10 1 -0.1076 0.2225 0.6623 11.00000 0.05 0.22 Q11 1 -0.1619 0.3465 0.7078 11.00000 0.05 0.22 Q12 1 0.1378 0.2158 0.6077 11.00000 0.05 0.22 Q13 1 0.4990 0.3227 0.5146 11.00000 0.05 0.21 Q14 1 0.2844 0.1454 0.6917 11.00000 0.05 0.21 Q15 1 0.7393 0.3146 0.5317 11.00000 0.05 0.20 Q16 1 0.5202 0.2870 0.7688 11.00000 0.05 0.19 Q17 1 0.3288 0.1984 0.6552 11.00000 0.05 0.19 Q18 1 0.5186 0.4930 0.5466 11.00000 0.05 0.19 Q19 1 0.3401 0.3188 0.7215 11.00000 0.05 0.19 Q20 1 0.2898 0.2041 0.2964 11.00000 0.05 0.19 ; _database_code_depnum_ccdc_archive 'CCDC 962251' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)][Fe(Et3Al:aIPr-H)2(mes)] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C18 H36 K N2 O6, C75 H111 Al2 Fe N4' _chemical_formula_sum 'C93 H147 Al2 Fe K N6 O6' _chemical_formula_weight 1594.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 2(1)' _symmetry_space_group_name_Hall 'P 2c -2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 23.1194(5) _cell_length_b 37.1470(12) _cell_length_c 11.0300(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9472.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22877 _cell_measurement_theta_min 3.0483 _cell_measurement_theta_max 76.3102 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 2.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7153 _exptl_absorpt_correction_T_max 0.7590 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4102 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 48896 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 66.50 _reflns_number_total 15442 _reflns_number_gt 12935 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^ > 2\s(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^)+(0.0041P)^2^+20.8821P] 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 (1983), 6621 Friedel pairs' _refine_ls_abs_structure_Flack 0.043(6) _refine_ls_number_reflns 15442 _refine_ls_number_parameters 1000 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.33910(3) 0.15788(2) 0.21541(9) 0.03360(18) Uani 1 1 d . . . N1 N 0.48025(16) 0.12032(10) 0.4238(4) 0.0275(9) Uani 1 1 d . . . C1 C 0.5011(2) 0.15486(13) 0.4268(5) 0.0278(11) Uani 1 1 d . A . N2 N 0.45958(16) 0.17343(10) 0.3650(4) 0.0303(10) Uani 1 1 d . . . C2 C 0.42754(19) 0.11912(13) 0.3631(5) 0.0281(11) Uani 1 1 d . . . H2 H 0.4053 0.0979 0.3506 0.034 Uiso 1 1 calc R . . C3 C 0.4123(2) 0.15251(13) 0.3242(5) 0.0302(11) Uani 1 1 d . . . C4 C 0.5082(2) 0.08735(13) 0.4611(5) 0.0318(12) Uani 1 1 d . . . C5 C 0.5440(2) 0.07006(13) 0.3773(5) 0.0342(12) Uani 1 1 d . . . C6 C 0.5648(2) 0.03619(15) 0.4075(7) 0.0478(16) Uani 1 1 d . . . H6 H 0.5894 0.0237 0.3529 0.057 Uiso 1 1 calc R . . C7 C 0.5497(2) 0.02039(15) 0.5172(6) 0.0479(16) Uani 1 1 d . . . H7 H 0.5639 -0.0029 0.5366 0.057 Uiso 1 1 calc R . . C8 C 0.5146(2) 0.03804(15) 0.5976(6) 0.0447(15) Uani 1 1 d . . . H8 H 0.5052 0.0269 0.6726 0.054 Uiso 1 1 calc R . . C9 C 0.4926(2) 0.07215(14) 0.5710(5) 0.0363(13) Uani 1 1 d . . . C10 C 0.5587(2) 0.08636(15) 0.2557(5) 0.0406(14) Uani 1 1 d . . . H10 H 0.5524 0.1129 0.2612 0.049 Uiso 1 1 calc R . . C11 C 0.6223(2) 0.07987(17) 0.2189(7) 0.0587(17) Uani 1 1 d . . . H11A H 0.6296 0.0910 0.1399 0.070 Uiso 0.50 1 d PR . . H11B H 0.6296 0.0539 0.2136 0.070 Uiso 0.50 1 d PR . . H11C H 0.6480 0.0905 0.2798 0.070 Uiso 0.50 1 d PR . . H11D H 0.6418 0.0659 0.2823 0.070 Uiso 0.50 1 d PR . . H11E H 0.6418 0.1031 0.2086 0.070 Uiso 0.50 1 d PR . . H11F H 0.6234 0.0665 0.1424 0.070 Uiso 0.50 1 d PR . . C12 C 0.5193(3) 0.07165(18) 0.1554(6) 0.0616(19) Uani 1 1 d . . . H12A H 0.5296 0.0828 0.0779 0.074 Uiso 0.50 1 d PR . . H12B H 0.4789 0.0772 0.1748 0.074 Uiso 0.50 1 d PR . . H12C H 0.5242 0.0455 0.1494 0.074 Uiso 0.50 1 d PR . . H12D H 0.4922 0.0542 0.1902 0.074 Uiso 0.50 1 d PR . . H12E H 0.5429 0.0598 0.0932 0.074 Uiso 0.50 1 d PR . . H12F H 0.4976 0.0915 0.1186 0.074 Uiso 0.50 1 d PR . . C13 C 0.4508(3) 0.08989(17) 0.6595(6) 0.0521(17) Uani 1 1 d . . . H13 H 0.4501 0.1162 0.6411 0.062 Uiso 1 1 calc R . . C14 C 0.4686(4) 0.0855(2) 0.7914(6) 0.071(2) Uani 1 1 d . . . H14A H 0.4404 0.0976 0.8437 0.085 Uiso 0.50 1 d PR . . H14B H 0.5069 0.0962 0.8036 0.085 Uiso 0.50 1 d PR . . H14C H 0.4700 0.0598 0.8118 0.085 Uiso 0.50 1 d PR . . H14D H 0.5045 0.0715 0.7957 0.085 Uiso 0.50 1 d PR . . H14E H 0.4380 0.0729 0.8358 0.085 Uiso 0.50 1 d PR . . H14F H 0.4749 0.1093 0.8276 0.085 Uiso 0.50 1 d PR . . C15 C 0.3897(3) 0.07537(19) 0.6403(7) 0.066(2) Uani 1 1 d . . . H15A H 0.3631 0.0871 0.6974 0.079 Uiso 0.50 1 d PR . . H15B H 0.3894 0.0493 0.6543 0.079 Uiso 0.50 1 d PR . . H15C H 0.3772 0.0804 0.5571 0.079 Uiso 0.50 1 d PR . . H15D H 0.3900 0.0575 0.5751 0.079 Uiso 0.50 1 d PR . . H15E H 0.3638 0.0952 0.6182 0.079 Uiso 0.50 1 d PR . . H15F H 0.3759 0.0641 0.7154 0.079 Uiso 0.50 1 d PR . . C16 C 0.4650(2) 0.21182(12) 0.3383(5) 0.0283(11) Uani 1 1 d . . . C17 C 0.5034(2) 0.22224(13) 0.2480(5) 0.0343(12) Uani 1 1 d . . . C18 C 0.5094(2) 0.25900(13) 0.2268(6) 0.0413(13) Uani 1 1 d . . . H18 H 0.5356 0.2672 0.1664 0.050 Uiso 1 1 calc R . . C19 C 0.4777(3) 0.28361(14) 0.2926(6) 0.0486(16) Uani 1 1 d . . . H19 H 0.4823 0.3086 0.2774 0.058 Uiso 1 1 calc R . . C20 C 0.4395(2) 0.27238(14) 0.3796(6) 0.0453(15) Uani 1 1 d . . . H20 H 0.4176 0.2898 0.4229 0.054 Uiso 1 1 calc R . . C21 C 0.4320(2) 0.23618(13) 0.4062(6) 0.0360(13) Uani 1 1 d . . . C22 C 0.5373(2) 0.19502(15) 0.1731(5) 0.0418(14) Uani 1 1 d . . . H22 H 0.5489 0.1750 0.2287 0.050 Uiso 1 1 calc R . . C23 C 0.5931(3) 0.21048(18) 0.1179(7) 0.0623(19) Uani 1 1 d . . . H23A H 0.6168 0.2211 0.1822 0.075 Uiso 0.50 1 d PR . . H23B H 0.5832 0.2291 0.0582 0.075 Uiso 0.50 1 d PR . . H23C H 0.6148 0.1912 0.0780 0.075 Uiso 0.50 1 d PR . . H23D H 0.5931 0.2064 0.0301 0.075 Uiso 0.50 1 d PR . . H23E H 0.6267 0.1985 0.1540 0.075 Uiso 0.50 1 d PR . . H23F H 0.5951 0.2364 0.1343 0.075 Uiso 0.50 1 d PR . . C24 C 0.4997(3) 0.17860(17) 0.0735(6) 0.0540(17) Uani 1 1 d . . . H24A H 0.5225 0.1611 0.0271 0.065 Uiso 0.50 1 d PR . . H24B H 0.4861 0.1977 0.0192 0.065 Uiso 0.50 1 d PR . . H24C H 0.4664 0.1665 0.1102 0.065 Uiso 0.50 1 d PR . . H24D H 0.4608 0.1891 0.0772 0.065 Uiso 0.50 1 d PR . . H24E H 0.4973 0.1525 0.0852 0.065 Uiso 0.50 1 d PR . . H24F H 0.5169 0.1837 -0.0059 0.065 Uiso 0.50 1 d PR . . C25 C 0.3914(2) 0.22369(15) 0.5051(6) 0.0420(14) Uani 1 1 d . . . H25 H 0.3708 0.2017 0.4754 0.050 Uiso 1 1 calc R . . C26 C 0.4247(3) 0.21346(19) 0.6218(6) 0.0625(19) Uani 1 1 d . . . H26A H 0.3973 0.2054 0.6839 0.075 Uiso 0.50 1 d PR . . H26B H 0.4459 0.2345 0.6517 0.075 Uiso 0.50 1 d PR . . H26C H 0.4520 0.1940 0.6038 0.075 Uiso 0.50 1 d PR . . H26D H 0.4662 0.2172 0.6091 0.075 Uiso 0.50 1 d PR . . H26E H 0.4175 0.1881 0.6412 0.075 Uiso 0.50 1 d PR . . H26F H 0.4115 0.2286 0.6891 0.075 Uiso 0.50 1 d PR . . C27 C 0.3454(3) 0.25186(17) 0.5419(7) 0.0597(18) Uani 1 1 d . . . H27A H 0.3207 0.2419 0.6058 0.072 Uiso 0.50 1 d PR . . H27B H 0.3217 0.2580 0.4712 0.072 Uiso 0.50 1 d PR . . H27C H 0.3647 0.2736 0.5720 0.072 Uiso 0.50 1 d PR . . H27D H 0.3507 0.2737 0.4935 0.072 Uiso 0.50 1 d PR . . H27E H 0.3497 0.2577 0.6281 0.072 Uiso 0.50 1 d PR . . H27F H 0.3067 0.2420 0.5273 0.072 Uiso 0.50 1 d PR . . N3 N 0.24123(16) 0.09852(11) 0.2505(4) 0.0307(10) Uani 1 1 d . . . C28 C 0.2284(2) 0.06306(13) 0.2368(5) 0.0333(12) Uani 1 1 d . . . N4 N 0.27897(16) 0.04882(11) 0.1936(4) 0.0323(10) Uani 1 1 d . . . C29 C 0.29845(19) 0.10778(12) 0.2147(6) 0.0320(11) Uani 1 1 d . . . C30 C 0.3204(2) 0.07592(13) 0.1815(5) 0.0351(13) Uani 1 1 d . . . H30 H 0.3588 0.0723 0.1536 0.042 Uiso 1 1 calc R . . C31 C 0.1992(2) 0.12543(13) 0.2837(5) 0.0329(12) Uani 1 1 d . . . C32 C 0.1655(2) 0.14163(13) 0.1928(6) 0.0432(15) Uani 1 1 d . . . C33 C 0.1259(2) 0.16775(15) 0.2320(7) 0.0538(18) Uani 1 1 d . . . H33 H 0.1012 0.1788 0.1740 0.065 Uiso 1 1 calc R . . C34 C 0.1214(2) 0.17799(16) 0.3526(7) 0.0505(16) Uani 1 1 d . . . H34 H 0.0939 0.1957 0.3762 0.061 Uiso 1 1 calc R . . C35 C 0.1566(2) 0.16251(15) 0.4373(7) 0.0497(17) Uani 1 1 d . . . H35 H 0.1537 0.1701 0.5193 0.060 Uiso 1 1 calc R . . C36 C 0.1966(2) 0.13586(14) 0.4073(6) 0.0380(14) Uani 1 1 d . . . C37 C 0.1732(2) 0.13180(15) 0.0593(5) 0.0438(15) Uani 1 1 d . . . H37 H 0.2128 0.1215 0.0482 0.053 Uiso 1 1 calc R . . C38 C 0.1663(3) 0.16340(19) -0.0269(7) 0.070(2) Uani 1 1 d . . . H38A H 0.1715 0.1551 -0.1105 0.084 Uiso 0.50 1 d PR . . H38B H 0.1954 0.1818 -0.0081 0.084 Uiso 0.50 1 d PR . . H38C H 0.1275 0.1737 -0.0177 0.084 Uiso 0.50 1 d PR . . H38D H 0.1581 0.1853 0.0196 0.084 Uiso 0.50 1 d PR . . H38E H 0.1342 0.1586 -0.0828 0.084 Uiso 0.50 1 d PR . . H38F H 0.2021 0.1667 -0.0732 0.084 Uiso 0.50 1 d PR . . C39 C 0.1284(4) 0.10281(19) 0.0234(8) 0.083(3) Uani 1 1 d . . . H39A H 0.1334 0.0965 -0.0622 0.100 Uiso 0.50 1 d PR . . H39B H 0.0893 0.1122 0.0363 0.100 Uiso 0.50 1 d PR . . H39C H 0.1341 0.0813 0.0735 0.100 Uiso 0.50 1 d PR . . H39D H 0.1044 0.0969 0.0939 0.100 Uiso 0.50 1 d PR . . H39E H 0.1485 0.0812 -0.0046 0.100 Uiso 0.50 1 d PR . . H39F H 0.1037 0.1121 -0.0418 0.100 Uiso 0.50 1 d PR . . C40 C 0.2356(2) 0.12051(15) 0.5036(5) 0.0409(14) Uani 1 1 d . . . H40 H 0.2571 0.0997 0.4675 0.049 Uiso 1 1 calc R . . C41 C 0.2799(2) 0.14841(18) 0.5440(7) 0.0607(19) Uani 1 1 d . . . H41A H 0.3050 0.1380 0.6064 0.073 Uiso 0.50 1 d PR . . H41B H 0.2598 0.1694 0.5772 0.073 Uiso 0.50 1 d PR . . H41C H 0.3034 0.1558 0.4743 0.073 Uiso 0.50 1 d PR . . H41D H 0.2739 0.1708 0.4988 0.073 Uiso 0.50 1 d PR . . H41E H 0.3190 0.1393 0.5281 0.073 Uiso 0.50 1 d PR . . H41F H 0.2754 0.1530 0.6309 0.073 Uiso 0.50 1 d PR . . C42 C 0.2023(3) 0.10677(19) 0.6145(7) 0.067(2) Uani 1 1 d . . . H42A H 0.2297 0.0970 0.6740 0.080 Uiso 0.50 1 d PR . . H42B H 0.1754 0.0878 0.5895 0.080 Uiso 0.50 1 d PR . . H42C H 0.1807 0.1267 0.6511 0.080 Uiso 0.50 1 d PR . . H42D H 0.1608 0.1107 0.6024 0.080 Uiso 0.50 1 d PR . . H42E H 0.2151 0.1199 0.6869 0.080 Uiso 0.50 1 d PR . . H42F H 0.2098 0.0810 0.6253 0.080 Uiso 0.50 1 d PR . . C43 C 0.2901(2) 0.01198(14) 0.1594(6) 0.0399(14) Uani 1 1 d . . . C44 C 0.2741(2) 0.00025(17) 0.0447(6) 0.0484(16) Uani 1 1 d . . . C45 C 0.2874(3) -0.03485(19) 0.0122(6) 0.0571(19) Uani 1 1 d . . . H45 H 0.2766 -0.0436 -0.0655 0.069 Uiso 1 1 calc R . . C46 C 0.3160(3) -0.05707(17) 0.0919(7) 0.060(2) Uani 1 1 d . . . H46 H 0.3248 -0.0811 0.0688 0.073 Uiso 1 1 calc R . . C47 C 0.3319(2) -0.04478(14) 0.2045(7) 0.0475(15) Uani 1 1 d . . . H47 H 0.3517 -0.0606 0.2580 0.057 Uiso 1 1 calc R . . C48 C 0.3197(2) -0.01000(13) 0.2426(5) 0.0370(13) Uani 1 1 d . . . C49 C 0.2475(3) 0.0258(2) -0.0469(6) 0.0607(19) Uani 1 1 d . . . H49 H 0.2251 0.0444 -0.0012 0.073 Uiso 1 1 calc R . . C50 C 0.2945(3) 0.0451(2) -0.1188(8) 0.087(3) Uani 1 1 d . . . H50A H 0.2766 0.0619 -0.1760 0.104 Uiso 0.50 1 d PR . . H50B H 0.3176 0.0274 -0.1637 0.104 Uiso 0.50 1 d PR . . H50C H 0.3197 0.0584 -0.0631 0.104 Uiso 0.50 1 d PR . . H50D H 0.3326 0.0366 -0.0925 0.104 Uiso 0.50 1 d PR . . H50E H 0.2916 0.0711 -0.1048 0.104 Uiso 0.50 1 d PR . . H50F H 0.2895 0.0401 -0.2054 0.104 Uiso 0.50 1 d PR . . C51 C 0.2062(4) 0.0080(3) -0.1390(8) 0.109(3) Uani 1 1 d . . . H51A H 0.1902 0.0265 -0.1927 0.131 Uiso 0.50 1 d PR . . H51B H 0.1746 -0.0040 -0.0956 0.131 Uiso 0.50 1 d PR . . H51C H 0.2275 -0.0097 -0.1872 0.131 Uiso 0.50 1 d PR . . H51D H 0.2047 -0.0180 -0.1243 0.131 Uiso 0.50 1 d PR . . H51E H 0.2202 0.0125 -0.2214 0.131 Uiso 0.50 1 d PR . . H51F H 0.1673 0.0182 -0.1298 0.131 Uiso 0.50 1 d PR . . C52 C 0.3422(2) 0.00394(14) 0.3629(5) 0.0398(13) Uani 1 1 d . . . H52 H 0.3206 0.0265 0.3834 0.048 Uiso 1 1 calc R . . C53 C 0.4065(2) 0.01332(16) 0.3505(6) 0.0484(15) Uani 1 1 d . . . H53A H 0.4210 0.0224 0.4282 0.058 Uiso 0.50 1 d PR . . H53B H 0.4113 0.0319 0.2881 0.058 Uiso 0.50 1 d PR . . H53C H 0.4282 -0.0083 0.3273 0.058 Uiso 0.50 1 d PR . . H53D H 0.4193 0.0083 0.2676 0.058 Uiso 0.50 1 d PR . . H53E H 0.4290 -0.0012 0.4076 0.058 Uiso 0.50 1 d PR . . H53F H 0.4122 0.0389 0.3685 0.058 Uiso 0.50 1 d PR . . C54 C 0.3344(3) -0.02248(18) 0.4662(6) 0.0629(19) Uani 1 1 d . . . H54A H 0.3496 -0.0120 0.5411 0.076 Uiso 0.50 1 d PR . . H54B H 0.3553 -0.0448 0.4479 0.076 Uiso 0.50 1 d PR . . H54C H 0.2932 -0.0278 0.4763 0.076 Uiso 0.50 1 d PR . . H54D H 0.3158 -0.0444 0.4358 0.076 Uiso 0.50 1 d PR . . H54E H 0.3100 -0.0116 0.5290 0.076 Uiso 0.50 1 d PR . . H54F H 0.3722 -0.0285 0.5006 0.076 Uiso 0.50 1 d PR . . C55 C 0.3080(2) 0.19538(14) 0.0958(5) 0.0372(13) Uani 1 1 d . . . C56 C 0.3157(2) 0.19203(16) -0.0295(5) 0.0414(14) Uani 1 1 d . . . C57 C 0.2911(2) 0.21586(17) -0.1123(7) 0.0522(16) Uani 1 1 d . . . H57 H 0.2977 0.2129 -0.1968 0.063 Uiso 1 1 calc R . . C58 C 0.2565(3) 0.24428(17) -0.0701(6) 0.0525(17) Uani 1 1 d . . . C59 C 0.2472(2) 0.24774(16) 0.0526(6) 0.0474(15) Uani 1 1 d . . . H59 H 0.2232 0.2666 0.0815 0.057 Uiso 1 1 calc R . . C60 C 0.2722(2) 0.22432(14) 0.1346(6) 0.0416(15) Uani 1 1 d . . . C61 C 0.3514(3) 0.16061(17) -0.0807(6) 0.0553(17) Uani 1 1 d . . . H61A H 0.3658 0.1458 -0.0138 0.066 Uiso 0.50 1 d PR . . H61B H 0.3841 0.1701 -0.1273 0.066 Uiso 0.50 1 d PR . . H61C H 0.3269 0.1459 -0.1338 0.066 Uiso 0.50 1 d PR . . H61D H 0.3521 0.1621 -0.1694 0.066 Uiso 0.50 1 d PR . . H61E H 0.3338 0.1378 -0.0559 0.066 Uiso 0.50 1 d PR . . H61F H 0.3910 0.1620 -0.0494 0.066 Uiso 0.50 1 d PR . . C62 C 0.2309(3) 0.2710(2) -0.1608(7) 0.078(2) Uani 1 1 d . . . H62A H 0.2425 0.2642 -0.2432 0.094 Uiso 0.50 1 d PR . . H62B H 0.2452 0.2953 -0.1428 0.094 Uiso 0.50 1 d PR . . H62C H 0.1886 0.2707 -0.1547 0.094 Uiso 0.50 1 d PR . . H62D H 0.2084 0.2893 -0.1173 0.094 Uiso 0.50 1 d PR . . H62E H 0.2056 0.2582 -0.2176 0.094 Uiso 0.50 1 d PR . . H62F H 0.2622 0.2827 -0.2058 0.094 Uiso 0.50 1 d PR . . C63 C 0.2599(3) 0.22885(17) 0.2690(6) 0.0534(17) Uani 1 1 d . . . H63A H 0.2805 0.2102 0.3148 0.064 Uiso 0.50 1 d PR . . H63B H 0.2183 0.2266 0.2835 0.064 Uiso 0.50 1 d PR . . H63C H 0.2731 0.2527 0.2955 0.064 Uiso 0.50 1 d PR . . H63D H 0.2341 0.2494 0.2811 0.064 Uiso 0.50 1 d PR . . H63E H 0.2963 0.2331 0.3123 0.064 Uiso 0.50 1 d PR . . H63F H 0.2415 0.2070 0.3003 0.064 Uiso 0.50 1 d PR . . Al1 Al 0.57547(7) 0.17348(4) 0.51485(18) 0.0452(5) Uani 1 1 d . . . C64 C 0.5831(3) 0.22648(15) 0.5024(6) 0.0540(18) Uani 1 1 d . A . H64A H 0.5906 0.2332 0.4170 0.065 Uiso 1 1 calc R . . H64B H 0.5464 0.2379 0.5276 0.065 Uiso 1 1 calc R . . C65 C 0.6322(3) 0.24047(17) 0.5817(7) 0.069(2) Uani 1 1 d . . . H65A H 0.6349 0.2667 0.5736 0.082 Uiso 0.50 1 d PR A . H65B H 0.6688 0.2295 0.5560 0.082 Uiso 0.50 1 d PR . . H65C H 0.6246 0.2342 0.6666 0.082 Uiso 0.50 1 d PR . . H65D H 0.6506 0.2203 0.6238 0.082 Uiso 0.50 1 d PR . . H65E H 0.6168 0.2575 0.6415 0.082 Uiso 0.50 1 d PR . . H65F H 0.6609 0.2527 0.5309 0.082 Uiso 0.50 1 d PR . . C66 C 0.6421(5) 0.1497(3) 0.4696(11) 0.051(3) Uani 0.637(7) 1 d P A 1 H66A H 0.6670 0.1487 0.5425 0.061 Uiso 0.637(7) 1 calc PR A 1 H66B H 0.6308 0.1246 0.4510 0.061 Uiso 0.637(7) 1 calc PR A 1 C67 C 0.6794(7) 0.1619(4) 0.3683(17) 0.094(5) Uani 0.637(7) 1 d P A 1 H67A H 0.7121 0.1454 0.3593 0.141 Uiso 0.319(4) 1 calc PR A 1 H67B H 0.6939 0.1862 0.3855 0.141 Uiso 0.319(4) 1 calc PR A 1 H67C H 0.6569 0.1623 0.2930 0.141 Uiso 0.319(4) 1 calc PR A 1 H67D H 0.6631 0.1839 0.3326 0.141 Uiso 0.319(4) 1 calc PR A 1 H67E H 0.6814 0.1431 0.3064 0.141 Uiso 0.319(4) 1 calc PR A 1 H67F H 0.7184 0.1670 0.3988 0.141 Uiso 0.319(4) 1 calc PR A 1 C68 C 0.5560(4) 0.1653(3) 0.6969(10) 0.055(2) Uani 0.637(7) 1 d P A 1 H68A H 0.5461 0.1888 0.7338 0.066 Uiso 0.637(7) 1 calc PR A 1 H68B H 0.5214 0.1497 0.7023 0.066 Uiso 0.637(7) 1 calc PR A 1 C69 C 0.6043(5) 0.1482(4) 0.7710(10) 0.070(3) Uani 0.637(7) 1 d P A 1 H69A H 0.5915 0.1453 0.8552 0.105 Uiso 0.319(4) 1 calc PR A 1 H69B H 0.6386 0.1636 0.7684 0.105 Uiso 0.319(4) 1 calc PR A 1 H69C H 0.6138 0.1245 0.7370 0.105 Uiso 0.319(4) 1 calc PR A 1 H69D H 0.6377 0.1436 0.7186 0.105 Uiso 0.319(4) 1 calc PR A 1 H69E H 0.5907 0.1253 0.8053 0.105 Uiso 0.319(4) 1 calc PR A 1 H69F H 0.6155 0.1645 0.8368 0.105 Uiso 0.319(4) 1 calc PR A 1 C66A C 0.6460(9) 0.1511(6) 0.396(2) 0.051(3) Uani 0.363(7) 1 d P A 2 H66C H 0.6507 0.1250 0.4106 0.061 Uiso 0.363(7) 1 calc PR A 2 H66D H 0.6359 0.1546 0.3091 0.061 Uiso 0.363(7) 1 calc PR A 2 C67A C 0.7018(12) 0.1706(7) 0.424(3) 0.094(5) Uani 0.363(7) 1 d P A 2 H67G H 0.7329 0.1613 0.3728 0.141 Uiso 0.181(4) 1 calc PR A 2 H67H H 0.7118 0.1668 0.5098 0.141 Uiso 0.181(4) 1 calc PR A 2 H67I H 0.6969 0.1965 0.4094 0.141 Uiso 0.181(4) 1 calc PR A 2 H67J H 0.6948 0.1884 0.4885 0.141 Uiso 0.181(4) 1 calc PR A 2 H67K H 0.7159 0.1829 0.3516 0.141 Uiso 0.181(4) 1 calc PR A 2 H67L H 0.7309 0.1533 0.4520 0.141 Uiso 0.181(4) 1 calc PR A 2 C68A C 0.5897(8) 0.1482(6) 0.6616(17) 0.055(2) Uani 0.363(7) 1 d P A 2 H68C H 0.5750 0.1233 0.6528 0.066 Uiso 0.363(7) 1 calc PR A 2 H68D H 0.6321 0.1467 0.6741 0.066 Uiso 0.363(7) 1 calc PR A 2 C69A C 0.5622(10) 0.1651(6) 0.7754(18) 0.070(3) Uani 0.363(7) 1 d P A 2 H69G H 0.5716 0.1505 0.8465 0.105 Uiso 0.181(4) 1 calc PR A 2 H69H H 0.5201 0.1662 0.7653 0.105 Uiso 0.181(4) 1 calc PR A 2 H69I H 0.5774 0.1896 0.7867 0.105 Uiso 0.181(4) 1 calc PR A 2 H69J H 0.5411 0.1870 0.7525 0.105 Uiso 0.181(4) 1 calc PR A 2 H69K H 0.5926 0.1713 0.8337 0.105 Uiso 0.181(4) 1 calc PR A 2 H69L H 0.5354 0.1479 0.8123 0.105 Uiso 0.181(4) 1 calc PR A 2 Al2 Al 0.15434(7) 0.03373(5) 0.2875(2) 0.0509(5) Uani 1 1 d . C . C70 C 0.0935(2) 0.06678(16) 0.3473(7) 0.0537(18) Uani 1 1 d . . . H70A H 0.1089 0.0814 0.4150 0.064 Uiso 1 1 calc R . . H70B H 0.0819 0.0834 0.2814 0.064 Uiso 1 1 calc R . . C71 C 0.0398(3) 0.04533(17) 0.3913(8) 0.067(2) Uani 1 1 d . . . H71A H 0.0104 0.0621 0.4211 0.080 Uiso 0.50 1 d PR . . H71B H 0.0512 0.0290 0.4567 0.080 Uiso 0.50 1 d PR . . H71C H 0.0240 0.0314 0.3236 0.080 Uiso 0.50 1 d PR . . H71D H 0.0467 0.0195 0.3798 0.080 Uiso 0.50 1 d PR . . H71E H 0.0058 0.0527 0.3442 0.080 Uiso 0.50 1 d PR . . H71F H 0.0331 0.0503 0.4774 0.080 Uiso 0.50 1 d PR . . C72 C 0.1201(3) 0.00740(19) 0.1420(9) 0.093(3) Uani 1 1 d . . . H72A H 0.0778 0.0113 0.1429 0.111 Uiso 1 1 calc R . . H72B H 0.1353 0.0190 0.0677 0.111 Uiso 1 1 calc R . . C73 C 0.1305(4) -0.0314(2) 0.1314(11) 0.115(4) Uani 1 1 d . . . H73A H 0.1118 -0.0405 0.0578 0.138 Uiso 0.50 1 d PR . . H73B H 0.1145 -0.0438 0.2024 0.138 Uiso 0.50 1 d PR . . H73C H 0.1722 -0.0359 0.1268 0.138 Uiso 0.50 1 d PR . . H73D H 0.1539 -0.0396 0.2002 0.138 Uiso 0.50 1 d PR . . H73E H 0.1512 -0.0364 0.0557 0.138 Uiso 0.50 1 d PR . . H73F H 0.0934 -0.0442 0.1312 0.138 Uiso 0.50 1 d PR . . C74 C 0.1789(3) -0.0027(2) 0.4065(9) 0.095(3) Uani 1 1 d DU . . H74A H 0.1476 -0.0207 0.4152 0.114 Uiso 1 1 calc R B 3 H74B H 0.2133 -0.0153 0.3744 0.114 Uiso 1 1 calc R B 3 C75 C 0.1927(6) 0.0115(3) 0.5259(11) 0.085(4) Uani 0.794(16) 1 d PDU C 3 H75A H 0.2034 -0.0083 0.5800 0.128 Uiso 0.397(8) 1 calc PR C 3 H75B H 0.1589 0.0241 0.5589 0.128 Uiso 0.397(8) 1 calc PR C 3 H75C H 0.2252 0.0284 0.5192 0.128 Uiso 0.397(8) 1 calc PR C 3 H75D H 0.1882 0.0378 0.5254 0.128 Uiso 0.397(8) 1 calc PR C 3 H75E H 0.2327 0.0054 0.5465 0.128 Uiso 0.397(8) 1 calc PR C 3 H75F H 0.1665 0.0010 0.5861 0.128 Uiso 0.397(8) 1 calc PR C 3 C75A C 0.152(2) 0.0000(12) 0.539(2) 0.085(4) Uani 0.206(16) 1 d PD C 4 H75G H 0.1618 -0.0216 0.5853 0.128 Uiso 0.103(8) 1 calc PR C 4 H75H H 0.1095 0.0019 0.5326 0.128 Uiso 0.103(8) 1 calc PR C 4 H75I H 0.1670 0.0213 0.5801 0.128 Uiso 0.103(8) 1 calc PR C 4 H75J H 0.1304 0.0227 0.5467 0.128 Uiso 0.103(8) 1 calc PR C 4 H75K H 0.1827 -0.0008 0.5993 0.128 Uiso 0.103(8) 1 calc PR C 4 H75L H 0.1252 -0.0203 0.5519 0.128 Uiso 0.103(8) 1 calc PR C 4 K101 K 0.41059(5) 0.36669(3) 0.88214(15) 0.0482(3) Uani 1 1 d . . . N101 N 0.4878(2) 0.36338(14) 0.6583(5) 0.0540(14) Uani 1 1 d . . . N102 N 0.3335(2) 0.37004(18) 1.1055(5) 0.0642(16) Uani 1 1 d . . . O101 O 0.50380(16) 0.41502(11) 0.8580(4) 0.0519(11) Uani 1 1 d . . . O102 O 0.42376(19) 0.42249(13) 1.0504(5) 0.0683(14) Uani 1 1 d . . . O103 O 0.46639(18) 0.30179(11) 0.8133(4) 0.0553(12) Uani 1 1 d . . . O104 O 0.40818(18) 0.30793(11) 1.0402(5) 0.0603(12) Uani 1 1 d . . . O105 O 0.36256(17) 0.37611(11) 0.6535(5) 0.0585(13) Uani 1 1 d . . . O106 O 0.28903(17) 0.36907(13) 0.8568(5) 0.0662(14) Uani 1 1 d . . . C101 C 0.5399(3) 0.38577(19) 0.6801(7) 0.064(2) Uani 1 1 d . . . H10A H 0.5592 0.3906 0.6017 0.077 Uiso 1 1 calc R . . H10B H 0.5672 0.3722 0.7318 0.077 Uiso 1 1 calc R . . C102 C 0.5258(3) 0.42124(18) 0.7409(7) 0.063(2) Uani 1 1 d . . . H10C H 0.5612 0.4362 0.7462 0.076 Uiso 1 1 calc R . . H10D H 0.4969 0.4345 0.6920 0.076 Uiso 1 1 calc R . . C103 C 0.4942(3) 0.44811(18) 0.9187(8) 0.067(2) Uani 1 1 d . . . H10E H 0.4625 0.4615 0.8783 0.080 Uiso 1 1 calc R . . H10F H 0.5296 0.4631 0.9155 0.080 Uiso 1 1 calc R . . C104 C 0.4787(3) 0.4409(2) 1.0445(8) 0.073(2) Uani 1 1 d . . . H10G H 0.5090 0.4258 1.0826 0.088 Uiso 1 1 calc R . . H10H H 0.4764 0.4638 1.0899 0.088 Uiso 1 1 calc R . . C105 C 0.4041(3) 0.4168(3) 1.1683(9) 0.091(3) Uani 1 1 d . . . H10I H 0.4078 0.4394 1.2154 0.110 Uiso 1 1 calc R . . H10J H 0.4282 0.3982 1.2079 0.110 Uiso 1 1 calc R . . C106 C 0.3413(3) 0.4048(2) 1.1681(8) 0.091(3) Uani 1 1 d . . . H10K H 0.3277 0.4025 1.2528 0.109 Uiso 1 1 calc R . . H10L H 0.3174 0.4233 1.1275 0.109 Uiso 1 1 calc R . . C107 C 0.5064(3) 0.32653(18) 0.6307(7) 0.0644(19) Uani 1 1 d . . . H10M H 0.5419 0.3274 0.5807 0.077 Uiso 1 1 calc R . . H10N H 0.4759 0.3143 0.5829 0.077 Uiso 1 1 calc R . . C108 C 0.5181(3) 0.30523(18) 0.7434(7) 0.068(2) Uani 1 1 d . . . H10O H 0.5327 0.2810 0.7213 0.081 Uiso 1 1 calc R . . H10P H 0.5482 0.3175 0.7923 0.081 Uiso 1 1 calc R . . C109 C 0.4729(4) 0.27672(17) 0.9112(8) 0.073(2) Uani 1 1 d . . . H10Q H 0.5040 0.2848 0.9664 0.088 Uiso 1 1 calc R . . H10R H 0.4832 0.2527 0.8792 0.088 Uiso 1 1 calc R . . C110 C 0.4172(3) 0.27477(18) 0.9776(7) 0.072(2) Uani 1 1 d . . . H11G H 0.3851 0.2705 0.9200 0.087 Uiso 1 1 calc R . . H11H H 0.4182 0.2546 1.0363 0.087 Uiso 1 1 calc R . . C111 C 0.3595(3) 0.3056(2) 1.1216(8) 0.080(3) Uani 1 1 d . . . H11I H 0.3242 0.2992 1.0759 0.096 Uiso 1 1 calc R . . H11J H 0.3666 0.2867 1.1831 0.096 Uiso 1 1 calc R . . C112 C 0.3520(3) 0.3400(3) 1.1801(7) 0.084(3) Uani 1 1 d . . . H11K H 0.3892 0.3466 1.2186 0.100 Uiso 1 1 calc R . . H11L H 0.3233 0.3369 1.2459 0.100 Uiso 1 1 calc R . . C113 C 0.4552(3) 0.37783(19) 0.5571(7) 0.0618(19) Uani 1 1 d . . . H11M H 0.4754 0.3717 0.4808 0.074 Uiso 1 1 calc R . . H11N H 0.4543 0.4044 0.5638 0.074 Uiso 1 1 calc R . . C114 C 0.3937(3) 0.3641(2) 0.5500(8) 0.068(2) Uani 1 1 d . . . H11O H 0.3749 0.3731 0.4753 0.081 Uiso 1 1 calc R . . H11P H 0.3937 0.3374 0.5472 0.081 Uiso 1 1 calc R . . C115 C 0.3031(3) 0.3670(2) 0.6452(8) 0.072(2) Uani 1 1 d . . . H11Q H 0.2984 0.3405 0.6501 0.086 Uiso 1 1 calc R . . H11R H 0.2873 0.3752 0.5666 0.086 Uiso 1 1 calc R . . C116 C 0.2716(3) 0.3846(2) 0.7463(8) 0.074(2) Uani 1 1 d . . . H11S H 0.2800 0.4107 0.7469 0.088 Uiso 1 1 calc R . . H11T H 0.2294 0.3813 0.7353 0.088 Uiso 1 1 calc R . . C117 C 0.2581(3) 0.3853(2) 0.9559(8) 0.077(2) Uani 1 1 d . . . H11U H 0.2159 0.3843 0.9406 0.092 Uiso 1 1 calc R . . H11V H 0.2694 0.4109 0.9644 0.092 Uiso 1 1 calc R . . C118 C 0.2726(3) 0.3652(3) 1.0685(9) 0.093(3) Uani 1 1 d . . . H11W H 0.2470 0.3735 1.1349 0.112 Uiso 1 1 calc R . . H11X H 0.2650 0.3393 1.0554 0.112 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 0.0245(3) 0.0276(4) 0.0486(5) 0.0111(4) -0.0080(4) -0.0033(3) N1 0.0259(19) 0.023(2) 0.034(3) 0.0055(18) -0.0015(18) 0.0005(16) C1 0.029(2) 0.027(3) 0.027(3) 0.005(2) 0.000(2) -0.001(2) N2 0.0230(18) 0.019(2) 0.049(3) 0.000(2) -0.0078(19) -0.0022(15) C2 0.028(2) 0.028(3) 0.028(3) 0.002(2) -0.004(2) -0.0040(19) C3 0.025(2) 0.027(3) 0.038(3) 0.002(2) 0.001(2) -0.004(2) C4 0.030(2) 0.022(2) 0.043(3) 0.006(2) -0.004(2) 0.001(2) C5 0.030(2) 0.026(3) 0.047(3) -0.003(3) 0.004(2) 0.000(2) C6 0.034(3) 0.036(3) 0.073(5) 0.003(3) -0.006(3) 0.006(2) C7 0.041(3) 0.029(3) 0.074(5) 0.015(3) -0.011(3) 0.008(2) C8 0.050(3) 0.035(3) 0.049(4) 0.013(3) -0.012(3) -0.002(3) C9 0.039(3) 0.031(3) 0.039(3) 0.012(3) -0.010(3) -0.004(2) C10 0.045(3) 0.032(3) 0.045(4) 0.000(3) 0.004(3) 0.001(2) C11 0.060(4) 0.063(4) 0.053(4) -0.008(4) 0.023(4) 0.001(3) C12 0.074(5) 0.058(4) 0.053(4) 0.002(4) 0.005(4) -0.005(4) C13 0.073(4) 0.035(3) 0.049(4) 0.013(3) 0.010(3) 0.002(3) C14 0.114(6) 0.065(5) 0.034(4) 0.008(4) -0.002(4) -0.005(4) C15 0.056(4) 0.075(5) 0.067(5) 0.021(4) 0.012(4) 0.007(4) C16 0.032(2) 0.022(2) 0.031(3) 0.005(2) -0.011(2) -0.005(2) C17 0.033(2) 0.031(3) 0.040(3) 0.011(2) -0.007(2) -0.007(2) C18 0.045(3) 0.034(3) 0.044(4) 0.012(3) -0.008(3) -0.012(2) C19 0.057(4) 0.023(3) 0.066(4) 0.013(3) -0.012(3) -0.009(3) C20 0.050(3) 0.025(3) 0.061(4) -0.004(3) -0.011(3) -0.001(2) C21 0.030(2) 0.025(3) 0.054(4) 0.010(3) -0.004(2) 0.002(2) C22 0.040(3) 0.041(3) 0.044(4) 0.019(3) 0.006(3) -0.001(2) C23 0.046(3) 0.070(5) 0.071(5) 0.017(4) 0.010(3) -0.009(3) C24 0.057(4) 0.051(4) 0.054(4) -0.008(3) 0.007(3) -0.011(3) C25 0.041(3) 0.034(3) 0.051(4) -0.009(3) 0.002(3) 0.000(2) C26 0.056(4) 0.079(5) 0.052(4) 0.015(4) 0.000(3) 0.012(4) C27 0.058(4) 0.053(4) 0.068(5) -0.006(4) 0.019(4) 0.014(3) N3 0.0217(19) 0.028(2) 0.042(3) 0.0113(19) -0.0041(18) -0.0037(16) C28 0.032(2) 0.031(3) 0.037(3) 0.005(2) -0.008(2) -0.003(2) N4 0.030(2) 0.031(2) 0.036(3) 0.008(2) -0.0022(19) -0.0075(17) C29 0.026(2) 0.031(3) 0.039(3) 0.004(3) -0.010(2) -0.0046(19) C30 0.025(2) 0.038(3) 0.043(4) 0.013(3) 0.000(2) -0.010(2) C31 0.026(2) 0.026(3) 0.047(3) 0.011(2) -0.002(2) -0.003(2) C32 0.029(2) 0.033(3) 0.067(5) 0.017(3) -0.011(3) -0.003(2) C33 0.031(3) 0.045(3) 0.086(5) 0.017(4) -0.018(3) 0.006(2) C34 0.043(3) 0.038(3) 0.071(5) 0.008(3) 0.006(3) 0.008(3) C35 0.035(3) 0.036(3) 0.079(5) 0.008(3) 0.009(3) 0.007(3) C36 0.026(2) 0.031(3) 0.057(4) 0.011(3) -0.001(3) 0.000(2) C37 0.044(3) 0.044(3) 0.043(4) 0.010(3) -0.026(3) -0.003(3) C38 0.061(4) 0.057(4) 0.090(6) 0.029(4) -0.022(4) -0.021(3) C39 0.105(6) 0.060(5) 0.083(6) 0.016(5) -0.025(5) -0.041(4) C40 0.034(3) 0.042(3) 0.047(4) 0.014(3) -0.002(3) 0.005(2) C41 0.041(3) 0.074(5) 0.067(5) 0.006(4) -0.014(3) -0.007(3) C42 0.058(4) 0.070(5) 0.073(5) 0.020(4) -0.012(4) -0.002(3) C43 0.032(3) 0.029(3) 0.059(4) -0.002(3) 0.007(3) -0.009(2) C44 0.043(3) 0.056(4) 0.047(4) 0.004(3) 0.007(3) -0.021(3) C45 0.063(4) 0.068(5) 0.041(4) -0.013(4) 0.021(3) -0.032(4) C46 0.062(4) 0.038(3) 0.081(6) -0.013(4) 0.032(4) -0.021(3) C47 0.047(3) 0.031(3) 0.064(4) 0.007(3) 0.003(3) -0.004(2) C48 0.037(3) 0.026(3) 0.048(4) 0.006(3) 0.004(3) -0.004(2) C49 0.059(4) 0.100(6) 0.023(3) 0.005(4) -0.008(3) -0.013(4) C50 0.086(6) 0.111(7) 0.063(5) 0.029(5) -0.003(5) -0.013(5) C51 0.098(7) 0.164(10) 0.064(6) -0.013(7) -0.024(6) -0.020(7) C52 0.044(3) 0.029(3) 0.046(4) 0.002(3) -0.002(3) 0.006(2) C53 0.049(3) 0.042(3) 0.055(4) -0.005(3) -0.007(3) 0.002(3) C54 0.073(4) 0.057(4) 0.059(5) 0.018(4) -0.023(4) 0.005(4) C55 0.034(3) 0.034(3) 0.043(4) 0.009(3) -0.009(2) -0.008(2) C56 0.037(3) 0.048(3) 0.039(3) 0.013(3) -0.006(3) -0.003(3) C57 0.048(3) 0.058(4) 0.051(4) 0.024(3) -0.004(3) -0.007(3) C58 0.044(3) 0.047(4) 0.066(5) 0.027(3) -0.021(3) -0.003(3) C59 0.042(3) 0.042(3) 0.058(4) 0.011(3) -0.014(3) 0.003(3) C60 0.035(3) 0.027(3) 0.062(4) 0.019(3) -0.007(3) -0.005(2) C61 0.064(4) 0.057(4) 0.046(4) 0.006(3) 0.000(3) 0.008(3) C62 0.079(5) 0.070(5) 0.085(6) 0.034(5) -0.018(5) 0.011(4) C63 0.062(4) 0.044(4) 0.054(4) 0.006(3) -0.003(3) 0.008(3) Al1 0.0396(9) 0.0347(9) 0.0613(12) 0.0098(9) -0.0239(9) -0.0069(7) C64 0.053(4) 0.035(3) 0.074(5) -0.013(3) -0.030(4) -0.001(3) C65 0.065(4) 0.045(4) 0.095(6) -0.003(4) -0.041(4) -0.010(3) C66 0.047(4) 0.054(5) 0.051(7) -0.020(7) -0.001(6) 0.000(4) C67 0.101(12) 0.063(9) 0.118(15) -0.040(8) 0.048(10) -0.035(7) C68 0.049(5) 0.075(7) 0.042(6) 0.002(5) -0.017(5) 0.000(4) C69 0.078(7) 0.099(9) 0.034(5) 0.000(6) 0.005(5) 0.022(6) C66A 0.047(4) 0.054(5) 0.051(7) -0.020(7) -0.001(6) 0.000(4) C67A 0.101(12) 0.063(9) 0.118(15) -0.040(8) 0.048(10) -0.035(7) C68A 0.049(5) 0.075(7) 0.042(6) 0.002(5) -0.017(5) 0.000(4) C69A 0.078(7) 0.099(9) 0.034(5) 0.000(6) 0.005(5) 0.022(6) Al2 0.0339(8) 0.0328(9) 0.0861(15) 0.0100(10) 0.0093(9) -0.0062(7) C70 0.034(3) 0.042(3) 0.085(5) 0.012(3) -0.001(3) -0.011(3) C71 0.045(3) 0.049(4) 0.107(6) -0.005(4) 0.029(4) -0.010(3) C72 0.055(4) 0.057(4) 0.166(10) -0.047(6) 0.022(5) -0.010(3) C73 0.071(5) 0.079(6) 0.196(13) 0.019(7) 0.033(7) -0.008(5) C74 0.068(5) 0.066(5) 0.151(10) 0.056(6) 0.031(6) 0.011(4) C75 0.086(8) 0.070(7) 0.100(9) -0.019(7) 0.002(7) 0.012(6) C75A 0.086(8) 0.070(7) 0.100(9) -0.019(7) 0.002(7) 0.012(6) K101 0.0339(6) 0.0403(7) 0.0705(9) 0.0040(7) -0.0048(6) 0.0025(5) N101 0.043(3) 0.049(3) 0.070(4) -0.004(3) 0.000(3) 0.003(2) N102 0.037(3) 0.099(5) 0.057(4) 0.008(4) 0.011(3) 0.009(3) O101 0.043(2) 0.044(2) 0.068(3) -0.003(2) -0.002(2) -0.0011(18) O102 0.050(3) 0.072(3) 0.083(4) -0.019(3) -0.006(3) 0.007(2) O103 0.055(2) 0.043(2) 0.068(3) 0.002(2) -0.016(2) 0.010(2) O104 0.050(2) 0.052(3) 0.079(4) 0.017(3) -0.004(2) -0.004(2) O105 0.039(2) 0.052(3) 0.085(4) 0.011(3) -0.004(2) 0.0032(19) O106 0.036(2) 0.068(3) 0.095(4) 0.029(3) -0.002(2) 0.011(2) C101 0.048(4) 0.073(5) 0.071(5) -0.002(4) 0.009(3) -0.007(3) C102 0.053(4) 0.059(4) 0.078(6) -0.008(4) 0.003(4) -0.017(3) C103 0.054(4) 0.047(4) 0.100(7) -0.015(4) -0.010(4) -0.004(3) C104 0.053(4) 0.076(5) 0.091(7) -0.033(5) -0.014(4) 0.005(4) C105 0.073(5) 0.104(7) 0.097(8) -0.016(6) 0.002(5) 0.013(5) C106 0.071(5) 0.111(7) 0.091(7) -0.001(6) 0.019(5) 0.014(5) C107 0.059(4) 0.062(4) 0.072(5) -0.010(4) 0.000(4) 0.007(3) C108 0.058(4) 0.055(4) 0.090(6) -0.016(4) -0.009(4) 0.016(3) C109 0.097(6) 0.040(4) 0.083(6) -0.002(4) -0.038(5) 0.019(4) C110 0.086(6) 0.041(4) 0.089(6) 0.014(4) -0.026(5) -0.013(4) C111 0.045(4) 0.092(6) 0.102(7) 0.048(6) -0.012(4) -0.013(4) C112 0.046(4) 0.131(8) 0.075(6) 0.032(6) 0.019(4) 0.006(4) C113 0.061(4) 0.066(5) 0.059(5) 0.006(4) 0.007(4) 0.000(3) C114 0.062(4) 0.071(5) 0.071(5) 0.000(4) -0.011(4) 0.003(4) C115 0.046(4) 0.080(5) 0.088(6) 0.015(5) -0.015(4) -0.004(4) C116 0.041(3) 0.078(5) 0.102(7) 0.038(5) -0.007(4) 0.009(3) C117 0.040(4) 0.093(6) 0.097(7) 0.007(5) 0.005(4) 0.019(4) C118 0.033(3) 0.141(8) 0.105(7) 0.038(7) 0.014(4) 0.020(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C55 2.049(5) . ? Fe1 C3 2.085(5) . ? Fe1 C29 2.085(5) . ? N1 C1 1.371(6) . ? N1 C2 1.391(6) . ? N1 C4 1.445(6) . ? C1 N2 1.365(6) . ? C1 Al1 2.092(5) . ? N2 C3 1.414(6) . ? N2 C16 1.462(6) . ? C2 C3 1.359(7) . ? C2 H2 0.9500 . ? C4 C9 1.385(7) . ? C4 C5 1.397(7) . ? C5 C6 1.387(7) . ? C5 C10 1.510(8) . ? C6 C7 1.389(9) . ? C6 H6 0.9500 . ? C7 C8 1.368(8) . ? C7 H7 0.9500 . ? C8 C9 1.397(7) . ? C8 H8 0.9500 . ? C9 C13 1.524(8) . ? C10 C12 1.535(8) . ? C10 C11 1.542(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9797 . ? C11 H11D 0.9799 . ? C11 H11E 0.9799 . ? C11 H11F 0.9801 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9802 . ? C12 H12D 0.9804 . ? C12 H12E 0.9801 . ? C12 H12F 0.9799 . ? C13 C14 1.521(9) . ? C13 C15 1.527(9) . ? C13 H13 1.0000 . ? C14 H14A 0.9798 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9801 . ? C14 H14E 0.9799 . ? C14 H14F 0.9800 . ? C15 H15A 0.9799 . ? C15 H15B 0.9802 . ? C15 H15C 0.9799 . ? C15 H15D 0.9801 . ? C15 H15E 0.9798 . ? C15 H15F 0.9801 . ? C16 C17 1.391(7) . ? C16 C21 1.400(7) . ? C17 C18 1.392(7) . ? C17 C22 1.523(8) . ? C18 C19 1.379(8) . ? C18 H18 0.9500 . ? C19 C20 1.369(9) . ? C19 H19 0.9500 . ? C20 C21 1.387(7) . ? C20 H20 0.9500 . ? C21 C25 1.512(8) . ? C22 C24 1.528(8) . ? C22 C23 1.537(7) . ? C22 H22 1.0000 . ? C23 H23A 0.9799 . ? C23 H23B 0.9801 . ? C23 H23C 0.9800 . ? C23 H23D 0.9799 . ? C23 H23E 0.9799 . ? C23 H23F 0.9802 . ? C24 H24A 0.9799 . ? C24 H24B 0.9801 . ? C24 H24C 0.9799 . ? C24 H24D 0.9801 . ? C24 H24E 0.9801 . ? C24 H24F 0.9800 . ? C25 C27 1.546(7) . ? C25 C26 1.547(8) . ? C25 H25 1.0000 . ? C26 H26A 0.9801 . ? C26 H26B 0.9798 . ? C26 H26C 0.9800 . ? C26 H26D 0.9801 . ? C26 H26E 0.9801 . ? C26 H26F 0.9798 . ? C27 H27A 0.9799 . ? C27 H27B 0.9799 . ? C27 H27C 0.9802 . ? C27 H27D 0.9802 . ? C27 H27E 0.9801 . ? C27 H27F 0.9799 . ? N3 C28 1.359(6) . ? N3 C29 1.423(6) . ? N3 C31 1.441(6) . ? C28 N4 1.369(6) . ? C28 Al2 2.105(5) . ? N4 C30 1.396(6) . ? N4 C43 1.442(6) . ? C29 C30 1.339(7) . ? C30 H30 0.9500 . ? C31 C32 1.404(7) . ? C31 C36 1.419(8) . ? C32 C33 1.404(8) . ? C32 C37 1.528(9) . ? C33 C34 1.387(10) . ? C33 H33 0.9500 . ? C34 C35 1.366(9) . ? C34 H34 0.9500 . ? C35 C36 1.395(7) . ? C35 H35 0.9500 . ? C36 C40 1.506(7) . ? C37 C38 1.519(8) . ? C37 C39 1.545(8) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9801 . ? C38 H38D 0.9800 . ? C38 H38E 0.9800 . ? C38 H38F 0.9800 . ? C39 H39A 0.9799 . ? C39 H39B 0.9801 . ? C39 H39C 0.9799 . ? C39 H39D 0.9799 . ? C39 H39E 0.9799 . ? C39 H39F 0.9800 . ? C40 C41 1.523(8) . ? C40 C42 1.534(8) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9799 . ? C41 H41C 0.9800 . ? C41 H41D 0.9800 . ? C41 H41E 0.9800 . ? C41 H41F 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9802 . ? C42 H42D 0.9800 . ? C42 H42E 0.9801 . ? C42 H42F 0.9798 . ? C43 C44 1.389(8) . ? C43 C48 1.406(8) . ? C44 C45 1.386(9) . ? C44 C49 1.516(9) . ? C45 C46 1.375(10) . ? C45 H45 0.9500 . ? C46 C47 1.374(10) . ? C46 H46 0.9500 . ? C47 C48 1.387(7) . ? C47 H47 0.9500 . ? C48 C52 1.517(8) . ? C49 C50 1.526(9) . ? C49 C51 1.543(10) . ? C49 H49 1.0000 . ? C50 H50A 0.9799 . ? C50 H50B 0.9800 . ? C50 H50C 0.9799 . ? C50 H50D 0.9801 . ? C50 H50E 0.9800 . ? C50 H50F 0.9799 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C51 H51D 0.9799 . ? C51 H51E 0.9800 . ? C51 H51F 0.9800 . ? C52 C54 1.514(8) . ? C52 C53 1.533(7) . ? C52 H52 1.0000 . ? C53 H53A 0.9801 . ? C53 H53B 0.9798 . ? C53 H53C 0.9801 . ? C53 H53D 0.9800 . ? C53 H53E 0.9800 . ? C53 H53F 0.9799 . ? C54 H54A 0.9798 . ? C54 H54B 0.9797 . ? C54 H54C 0.9801 . ? C54 H54D 0.9800 . ? C54 H54E 0.9800 . ? C54 H54F 0.9797 . ? C55 C56 1.400(8) . ? C55 C60 1.422(8) . ? C56 C57 1.393(8) . ? C56 C61 1.537(8) . ? C57 C58 1.404(9) . ? C57 H57 0.9500 . ? C58 C59 1.377(9) . ? C58 C62 1.529(8) . ? C59 C60 1.382(8) . ? C59 H59 0.9500 . ? C60 C63 1.519(8) . ? C61 H61A 0.9798 . ? C61 H61B 0.9801 . ? C61 H61C 0.9801 . ? C61 H61D 0.9800 . ? C61 H61E 0.9798 . ? C61 H61F 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9798 . ? C62 H62C 0.9799 . ? C62 H62D 0.9797 . ? C62 H62E 0.9799 . ? C62 H62F 0.9800 . ? C63 H63A 0.9799 . ? C63 H63B 0.9799 . ? C63 H63C 0.9799 . ? C63 H63D 0.9800 . ? C63 H63E 0.9800 . ? C63 H63F 0.9799 . ? Al1 C66 1.844(10) . ? Al1 C68A 1.900(19) . ? Al1 C64 1.982(6) . ? Al1 C68 2.080(11) . ? Al1 C66A 2.26(2) . ? C64 C65 1.524(8) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9800 . ? C65 H65B 0.9799 . ? C65 H65C 0.9800 . ? C65 H65D 0.9799 . ? C65 H65E 0.9801 . ? C65 H65F 0.9799 . ? C66 C67 1.483(19) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C67 H67D 0.9800 . ? C67 H67E 0.9800 . ? C67 H67F 0.9800 . ? C68 C69 1.521(15) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C69 H69D 0.9800 . ? C69 H69E 0.9800 . ? C69 H69F 0.9800 . ? C66A C67A 1.51(3) . ? C66A H66C 0.9900 . ? C66A H66D 0.9900 . ? C67A H67G 0.9800 . ? C67A H67H 0.9800 . ? C67A H67I 0.9800 . ? C67A H67J 0.9800 . ? C67A H67K 0.9800 . ? C67A H67L 0.9800 . ? C68A C69A 1.54(3) . ? C68A H68C 0.9900 . ? C68A H68D 0.9900 . ? C69A H69G 0.9800 . ? C69A H69H 0.9800 . ? C69A H69I 0.9800 . ? C69A H69J 0.9800 . ? C69A H69K 0.9800 . ? C69A H69L 0.9800 . ? Al2 C74 1.969(8) . ? Al2 C70 1.981(6) . ? Al2 C72 2.040(9) . ? C70 C71 1.551(7) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9801 . ? C71 H71D 0.9802 . ? C71 H71E 0.9798 . ? C71 H71F 0.9800 . ? C72 C73 1.467(10) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9799 . ? C73 H73B 0.9800 . ? C73 H73C 0.9802 . ? C73 H73D 0.9800 . ? C73 H73E 0.9800 . ? C73 H73F 0.9800 . ? C74 C75 1.454(11) . ? C74 C75A 1.592(19) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C75 H75D 0.9800 . ? C75 H75E 0.9800 . ? C75 H75F 0.9800 . ? C75A H75G 0.9800 . ? C75A H75H 0.9800 . ? C75A H75I 0.9800 . ? C75A H75J 0.9800 . ? C75A H75K 0.9800 . ? C75A H75L 0.9800 . ? K101 O105 2.778(5) . ? K101 O104 2.794(5) . ? K101 O102 2.799(5) . ? K101 O101 2.817(4) . ? K101 O106 2.826(4) . ? K101 O103 2.838(4) . ? K101 N102 3.043(6) . ? K101 N101 3.049(6) . ? N101 C113 1.450(8) . ? N101 C107 1.466(8) . ? N101 C101 1.483(7) . ? N102 C112 1.451(9) . ? N102 C106 1.474(10) . ? N102 C118 1.478(8) . ? O101 C102 1.408(8) . ? O101 C103 1.417(7) . ? O102 C105 1.394(10) . ? O102 C104 1.444(8) . ? O103 C108 1.429(8) . ? O103 C109 1.434(8) . ? O104 C110 1.427(8) . ? O104 C111 1.442(8) . ? O105 C115 1.418(7) . ? O105 C114 1.422(9) . ? O106 C116 1.407(8) . ? O106 C117 1.439(9) . ? C101 C102 1.513(9) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.458(11) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.518(10) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.498(10) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.483(10) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11G 0.9900 . ? C110 H11H 0.9900 . ? C111 C112 1.441(11) . ? C111 H11I 0.9900 . ? C111 H11J 0.9900 . ? C112 H11K 0.9900 . ? C112 H11L 0.9900 . ? C113 C114 1.513(9) . ? C113 H11M 0.9900 . ? C113 H11N 0.9900 . ? C114 H11O 0.9900 . ? C114 H11P 0.9900 . ? C115 C116 1.484(11) . ? C115 H11Q 0.9900 . ? C115 H11R 0.9900 . ? C116 H11S 0.9900 . ? C116 H11T 0.9900 . ? C117 C118 1.489(11) . ? C117 H11U 0.9900 . ? C117 H11V 0.9900 . ? C118 H11W 0.9900 . ? C118 H11X 0.9900 . ? 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 C55 Fe1 C3 136.11(19) . . ? C55 Fe1 C29 116.5(2) . . ? C3 Fe1 C29 106.42(19) . . ? C1 N1 C2 110.5(4) . . ? C1 N1 C4 128.9(4) . . ? C2 N1 C4 120.1(4) . . ? N2 C1 N1 102.3(4) . . ? N2 C1 Al1 130.0(3) . . ? N1 C1 Al1 127.6(3) . . ? C1 N2 C3 115.1(4) . . ? C1 N2 C16 122.3(4) . . ? C3 N2 C16 122.5(4) . . ? C3 C2 N1 110.4(4) . . ? C3 C2 H2 124.8 . . ? N1 C2 H2 124.8 . . ? C2 C3 N2 101.6(4) . . ? C2 C3 Fe1 118.6(3) . . ? N2 C3 Fe1 139.3(4) . . ? C9 C4 C5 123.1(5) . . ? C9 C4 N1 118.6(5) . . ? C5 C4 N1 117.7(5) . . ? C6 C5 C4 117.5(5) . . ? C6 C5 C10 119.9(5) . . ? C4 C5 C10 122.5(4) . . ? C5 C6 C7 120.4(6) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 120.7(5) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 121.0(6) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C4 C9 C8 117.2(5) . . ? C4 C9 C13 123.4(5) . . ? C8 C9 C13 119.3(5) . . ? C5 C10 C12 111.3(5) . . ? C5 C10 C11 112.7(5) . . ? C12 C10 C11 108.7(5) . . ? C5 C10 H10 108.0 . . ? C12 C10 H10 108.0 . . ? C11 C10 H10 108.0 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.2 . . ? C10 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? C10 C11 H11F 109.4 . . ? H11A C11 H11F 56.2 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.4 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C12 H12D 109.5 . . ? H12A C12 H12D 141.1 . . ? H12B C12 H12D 56.3 . . ? H12C C12 H12D 56.2 . . ? C10 C12 H12E 109.5 . . ? H12A C12 H12E 56.3 . . ? H12B C12 H12E 141.0 . . ? H12C C12 H12E 56.2 . . ? H12D C12 H12E 109.4 . . ? C10 C12 H12F 109.5 . . ? H12A C12 H12F 56.2 . . ? H12B C12 H12F 56.2 . . ? H12C C12 H12F 141.0 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? C14 C13 C9 113.2(6) . . ? C14 C13 C15 110.2(6) . . ? C9 C13 C15 110.2(5) . . ? C14 C13 H13 107.7 . . ? C9 C13 H13 107.7 . . ? C15 C13 H13 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14A C14 H14D 141.1 . . ? H14B C14 H14D 56.2 . . ? H14C C14 H14D 56.3 . . ? C13 C14 H14E 109.5 . . ? H14A C14 H14E 56.2 . . ? H14B C14 H14E 141.0 . . ? H14C C14 H14E 56.3 . . ? H14D C14 H14E 109.5 . . ? C13 C14 H14F 109.5 . . ? H14A C14 H14F 56.3 . . ? H14B C14 H14F 56.3 . . ? H14C C14 H14F 141.1 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C15 H15D 109.5 . . ? H15A C15 H15D 141.0 . . ? H15B C15 H15D 56.2 . . ? H15C C15 H15D 56.3 . . ? C13 C15 H15E 109.5 . . ? H15A C15 H15E 56.3 . . ? H15B C15 H15E 141.0 . . ? H15C C15 H15E 56.3 . . ? H15D C15 H15E 109.5 . . ? C13 C15 H15F 109.5 . . ? H15A C15 H15F 56.2 . . ? H15B C15 H15F 56.2 . . ? H15C C15 H15F 141.0 . . ? H15D C15 H15F 109.4 . . ? H15E C15 H15F 109.5 . . ? C17 C16 C21 123.5(5) . . ? C17 C16 N2 118.1(5) . . ? C21 C16 N2 118.5(4) . . ? C16 C17 C18 117.2(5) . . ? C16 C17 C22 122.2(4) . . ? C18 C17 C22 120.6(5) . . ? C19 C18 C17 120.6(5) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 120.7(5) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 121.6(6) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C20 C21 C16 116.5(5) . . ? C20 C21 C25 121.8(5) . . ? C16 C21 C25 121.7(4) . . ? C17 C22 C24 111.3(5) . . ? C17 C22 C23 113.5(5) . . ? C24 C22 C23 110.0(5) . . ? C17 C22 H22 107.3 . . ? C24 C22 H22 107.3 . . ? C23 C22 H22 107.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.4 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C23 H23D 109.5 . . ? H23A C23 H23D 141.1 . . ? H23B C23 H23D 56.3 . . ? H23C C23 H23D 56.2 . . ? C22 C23 H23E 109.5 . . ? H23A C23 H23E 56.3 . . ? H23B C23 H23E 141.1 . . ? H23C C23 H23E 56.3 . . ? H23D C23 H23E 109.5 . . ? C22 C23 H23F 109.5 . . ? H23A C23 H23F 56.3 . . ? H23B C23 H23F 56.2 . . ? H23C C23 H23F 141.1 . . ? H23D C23 H23F 109.5 . . ? H23E C23 H23F 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C24 H24D 109.5 . . ? H24A C24 H24D 141.1 . . ? H24B C24 H24D 56.2 . . ? H24C C24 H24D 56.3 . . ? C22 C24 H24E 109.5 . . ? H24A C24 H24E 56.3 . . ? H24B C24 H24E 141.1 . . ? H24C C24 H24E 56.3 . . ? H24D C24 H24E 109.5 . . ? C22 C24 H24F 109.5 . . ? H24A C24 H24F 56.2 . . ? H24B C24 H24F 56.3 . . ? H24C C24 H24F 141.1 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? C21 C25 C27 114.1(5) . . ? C21 C25 C26 111.5(5) . . ? C27 C25 C26 106.9(5) . . ? C21 C25 H25 108.0 . . ? C27 C25 H25 108.0 . . ? C26 C25 H25 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26D 109.4 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? C25 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.2 . . ? H26D C26 H26E 109.5 . . ? C25 C26 H26F 109.5 . . ? H26A C26 H26F 56.2 . . ? H26B C26 H26F 56.2 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.4 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.2 . . ? C25 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.2 . . ? H27D C27 H27E 109.4 . . ? C25 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.2 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? C28 N3 C29 114.0(4) . . ? C28 N3 C31 123.6(4) . . ? C29 N3 C31 122.0(4) . . ? N3 C28 N4 103.1(4) . . ? N3 C28 Al2 130.5(4) . . ? N4 C28 Al2 126.0(3) . . ? C28 N4 C30 109.9(4) . . ? C28 N4 C43 127.5(4) . . ? C30 N4 C43 122.5(4) . . ? C30 C29 N3 102.4(4) . . ? C30 C29 Fe1 128.3(4) . . ? N3 C29 Fe1 129.3(3) . . ? C29 C30 N4 110.6(4) . . ? C29 C30 H30 124.7 . . ? N4 C30 H30 124.7 . . ? C32 C31 C36 123.0(5) . . ? C32 C31 N3 119.3(5) . . ? C36 C31 N3 117.5(5) . . ? C33 C32 C31 116.0(6) . . ? C33 C32 C37 122.6(5) . . ? C31 C32 C37 121.4(5) . . ? C34 C33 C32 122.3(6) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C35 C34 C33 119.7(6) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 122.1(7) . . ? C34 C35 H35 118.9 . . ? C36 C35 H35 118.9 . . ? C35 C36 C31 116.7(5) . . ? C35 C36 C40 120.0(6) . . ? C31 C36 C40 123.3(5) . . ? C38 C37 C32 114.0(5) . . ? C38 C37 C39 108.0(5) . . ? C32 C37 C39 109.6(5) . . ? C38 C37 H37 108.4 . . ? C32 C37 H37 108.4 . . ? C39 C37 H37 108.4 . . ? C37 C38 H38A 109.4 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C38 H38D 109.5 . . ? H38A C38 H38D 141.1 . . ? H38B C38 H38D 56.3 . . ? H38C C38 H38D 56.2 . . ? C37 C38 H38E 109.4 . . ? H38A C38 H38E 56.3 . . ? H38B C38 H38E 141.1 . . ? H38C C38 H38E 56.2 . . ? H38D C38 H38E 109.5 . . ? C37 C38 H38F 109.5 . . ? H38A C38 H38F 56.3 . . ? H38B C38 H38F 56.2 . . ? H38C C38 H38F 141.1 . . ? H38D C38 H38F 109.5 . . ? H38E C38 H38F 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.4 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C39 H39D 109.5 . . ? H39A C39 H39D 141.1 . . ? H39B C39 H39D 56.3 . . ? H39C C39 H39D 56.2 . . ? C37 C39 H39E 109.5 . . ? H39A C39 H39E 56.3 . . ? H39B C39 H39E 141.1 . . ? H39C C39 H39E 56.3 . . ? H39D C39 H39E 109.5 . . ? C37 C39 H39F 109.4 . . ? H39A C39 H39F 56.3 . . ? H39B C39 H39F 56.2 . . ? H39C C39 H39F 141.1 . . ? H39D C39 H39F 109.5 . . ? H39E C39 H39F 109.5 . . ? C36 C40 C41 110.6(5) . . ? C36 C40 C42 112.8(5) . . ? C41 C40 C42 109.3(6) . . ? C36 C40 H40 108.0 . . ? C41 C40 H40 108.0 . . ? C42 C40 H40 108.0 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C41 H41D 109.5 . . ? H41A C41 H41D 141.1 . . ? H41B C41 H41D 56.3 . . ? H41C C41 H41D 56.2 . . ? C40 C41 H41E 109.5 . . ? H41A C41 H41E 56.3 . . ? H41B C41 H41E 141.1 . . ? H41C C41 H41E 56.2 . . ? H41D C41 H41E 109.5 . . ? C40 C41 H41F 109.5 . . ? H41A C41 H41F 56.3 . . ? H41B C41 H41F 56.2 . . ? H41C C41 H41F 141.1 . . ? H41D C41 H41F 109.5 . . ? H41E C41 H41F 109.5 . . ? C40 C42 H42A 109.4 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C42 H42D 109.5 . . ? H42A C42 H42D 141.1 . . ? H42B C42 H42D 56.3 . . ? H42C C42 H42D 56.3 . . ? C40 C42 H42E 109.4 . . ? H42A C42 H42E 56.3 . . ? H42B C42 H42E 141.1 . . ? H42C C42 H42E 56.2 . . ? H42D C42 H42E 109.5 . . ? C40 C42 H42F 109.5 . . ? H42A C42 H42F 56.3 . . ? H42B C42 H42F 56.3 . . ? H42C C42 H42F 141.1 . . ? H42D C42 H42F 109.5 . . ? H42E C42 H42F 109.5 . . ? C44 C43 C48 122.8(5) . . ? C44 C43 N4 119.2(5) . . ? C48 C43 N4 117.9(5) . . ? C45 C44 C43 118.1(6) . . ? C45 C44 C49 120.4(6) . . ? C43 C44 C49 121.2(6) . . ? C46 C45 C44 120.4(6) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C47 C46 C45 120.5(6) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 121.9(6) . . ? C46 C47 H47 119.0 . . ? C48 C47 H47 119.0 . . ? C47 C48 C43 116.3(6) . . ? C47 C48 C52 120.9(5) . . ? C43 C48 C52 122.6(5) . . ? C44 C49 C50 110.6(6) . . ? C44 C49 C51 114.9(7) . . ? C50 C49 C51 107.5(6) . . ? C44 C49 H49 107.9 . . ? C50 C49 H49 107.9 . . ? C51 C49 H49 107.9 . . ? C49 C50 H50A 109.4 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C50 H50D 109.5 . . ? H50A C50 H50D 141.1 . . ? H50B C50 H50D 56.2 . . ? H50C C50 H50D 56.3 . . ? C49 C50 H50E 109.5 . . ? H50A C50 H50E 56.3 . . ? H50B C50 H50E 141.1 . . ? H50C C50 H50E 56.3 . . ? H50D C50 H50E 109.5 . . ? C49 C50 H50F 109.5 . . ? H50A C50 H50F 56.2 . . ? H50B C50 H50F 56.3 . . ? H50C C50 H50F 141.1 . . ? H50D C50 H50F 109.5 . . ? H50E C50 H50F 109.5 . . ? C49 C51 H51A 109.4 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C51 H51D 109.6 . . ? H51A C51 H51D 141.1 . . ? H51B C51 H51D 56.3 . . ? H51C C51 H51D 56.3 . . ? C49 C51 H51E 109.4 . . ? H51A C51 H51E 56.3 . . ? H51B C51 H51E 141.1 . . ? H51C C51 H51E 56.2 . . ? H51D C51 H51E 109.5 . . ? C49 C51 H51F 109.5 . . ? H51A C51 H51F 56.2 . . ? H51B C51 H51F 56.2 . . ? H51C C51 H51F 141.1 . . ? H51D C51 H51F 109.5 . . ? H51E C51 H51F 109.5 . . ? C54 C52 C48 113.3(5) . . ? C54 C52 C53 109.3(5) . . ? C48 C52 C53 109.4(5) . . ? C54 C52 H52 108.3 . . ? C48 C52 H52 108.3 . . ? C53 C52 H52 108.3 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C53 H53D 109.5 . . ? H53A C53 H53D 141.1 . . ? H53B C53 H53D 56.3 . . ? H53C C53 H53D 56.2 . . ? C52 C53 H53E 109.5 . . ? H53A C53 H53E 56.2 . . ? H53B C53 H53E 141.1 . . ? H53C C53 H53E 56.3 . . ? H53D C53 H53E 109.5 . . ? C52 C53 H53F 109.5 . . ? H53A C53 H53F 56.2 . . ? H53B C53 H53F 56.3 . . ? H53C C53 H53F 141.0 . . ? H53D C53 H53F 109.5 . . ? H53E C53 H53F 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C54 H54D 109.5 . . ? H54A C54 H54D 141.0 . . ? H54B C54 H54D 56.2 . . ? H54C C54 H54D 56.3 . . ? C52 C54 H54E 109.4 . . ? H54A C54 H54E 56.3 . . ? H54B C54 H54E 141.1 . . ? H54C C54 H54E 56.2 . . ? H54D C54 H54E 109.5 . . ? C52 C54 H54F 109.5 . . ? H54A C54 H54F 56.2 . . ? H54B C54 H54F 56.3 . . ? H54C C54 H54F 141.1 . . ? H54D C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? C56 C55 C60 116.0(5) . . ? C56 C55 Fe1 122.1(4) . . ? C60 C55 Fe1 121.6(4) . . ? C57 C56 C55 122.6(6) . . ? C57 C56 C61 117.4(6) . . ? C55 C56 C61 119.9(5) . . ? C56 C57 C58 119.5(6) . . ? C56 C57 H57 120.2 . . ? C58 C57 H57 120.2 . . ? C59 C58 C57 119.0(6) . . ? C59 C58 C62 121.5(6) . . ? C57 C58 C62 119.5(7) . . ? C58 C59 C60 121.3(6) . . ? C58 C59 H59 119.3 . . ? C60 C59 H59 119.3 . . ? C59 C60 C55 121.5(6) . . ? C59 C60 C63 119.4(6) . . ? C55 C60 C63 119.1(5) . . ? C56 C61 H61A 109.4 . . ? C56 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C56 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C56 C61 H61D 109.5 . . ? H61A C61 H61D 141.1 . . ? H61B C61 H61D 56.3 . . ? H61C C61 H61D 56.3 . . ? C56 C61 H61E 109.4 . . ? H61A C61 H61E 56.3 . . ? H61B C61 H61E 141.1 . . ? H61C C61 H61E 56.2 . . ? H61D C61 H61E 109.5 . . ? C56 C61 H61F 109.5 . . ? H61A C61 H61F 56.3 . . ? H61B C61 H61F 56.3 . . ? H61C C61 H61F 141.1 . . ? H61D C61 H61F 109.5 . . ? H61E C61 H61F 109.5 . . ? C58 C62 H62A 109.4 . . ? C58 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C58 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C58 C62 H62D 109.5 . . ? H62A C62 H62D 141.1 . . ? H62B C62 H62D 56.3 . . ? H62C C62 H62D 56.3 . . ? C58 C62 H62E 109.4 . . ? H62A C62 H62E 56.3 . . ? H62B C62 H62E 141.1 . . ? H62C C62 H62E 56.2 . . ? H62D C62 H62E 109.5 . . ? C58 C62 H62F 109.5 . . ? H62A C62 H62F 56.2 . . ? H62B C62 H62F 56.2 . . ? H62C C62 H62F 141.1 . . ? H62D C62 H62F 109.5 . . ? H62E C62 H62F 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.4 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C60 C63 H63D 109.5 . . ? H63A C63 H63D 141.1 . . ? H63B C63 H63D 56.3 . . ? H63C C63 H63D 56.3 . . ? C60 C63 H63E 109.4 . . ? H63A C63 H63E 56.2 . . ? H63B C63 H63E 141.1 . . ? H63C C63 H63E 56.2 . . ? H63D C63 H63E 109.5 . . ? C60 C63 H63F 109.5 . . ? H63A C63 H63F 56.3 . . ? H63B C63 H63F 56.3 . . ? H63C C63 H63F 141.1 . . ? H63D C63 H63F 109.5 . . ? H63E C63 H63F 109.5 . . ? C66 Al1 C68A 81.3(7) . . ? C66 Al1 C64 112.4(4) . . ? C68A Al1 C64 122.3(7) . . ? C66 Al1 C68 111.8(5) . . ? C68A Al1 C68 31.0(6) . . ? C64 Al1 C68 103.4(4) . . ? C66 Al1 C1 113.7(4) . . ? C68A Al1 C1 112.0(6) . . ? C64 Al1 C1 111.7(2) . . ? C68 Al1 C1 102.9(3) . . ? C66 Al1 C66A 20.2(7) . . ? C68A Al1 C66A 100.9(9) . . ? C64 Al1 C66A 105.1(6) . . ? C68 Al1 C66A 131.7(7) . . ? C1 Al1 C66A 101.6(5) . . ? C65 C64 Al1 111.5(4) . . ? C65 C64 H64A 109.3 . . ? Al1 C64 H64A 109.3 . . ? C65 C64 H64B 109.3 . . ? Al1 C64 H64B 109.3 . . ? H64A C64 H64B 108.0 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C65 H65D 109.5 . . ? H65A C65 H65D 141.1 . . ? H65B C65 H65D 56.3 . . ? H65C C65 H65D 56.3 . . ? C64 C65 H65E 109.5 . . ? H65A C65 H65E 56.2 . . ? H65B C65 H65E 141.1 . . ? H65C C65 H65E 56.2 . . ? H65D C65 H65E 109.5 . . ? C64 C65 H65F 109.5 . . ? H65A C65 H65F 56.2 . . ? H65B C65 H65F 56.3 . . ? H65C C65 H65F 141.1 . . ? H65D C65 H65F 109.5 . . ? H65E C65 H65F 109.5 . . ? C67 C66 Al1 122.9(10) . . ? C67 C66 H66A 106.6 . . ? Al1 C66 H66A 106.6 . . ? C67 C66 H66B 106.6 . . ? Al1 C66 H66B 106.6 . . ? H66A C66 H66B 106.6 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C67 H67D 109.5 . . ? H67A C67 H67D 141.1 . . ? H67B C67 H67D 56.3 . . ? H67C C67 H67D 56.3 . . ? C66 C67 H67E 109.5 . . ? H67A C67 H67E 56.3 . . ? H67B C67 H67E 141.1 . . ? H67C C67 H67E 56.3 . . ? H67D C67 H67E 109.5 . . ? C66 C67 H67F 109.5 . . ? H67A C67 H67F 56.3 . . ? H67B C67 H67F 56.3 . . ? H67C C67 H67F 141.1 . . ? H67D C67 H67F 109.5 . . ? H67E C67 H67F 109.5 . . ? C69 C68 Al1 114.9(8) . . ? C69 C68 H68A 108.5 . . ? Al1 C68 H68A 108.5 . . ? C69 C68 H68B 108.5 . . ? Al1 C68 H68B 108.5 . . ? H68A C68 H68B 107.5 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C69 H69D 109.5 . . ? H69A C69 H69D 141.1 . . ? H69B C69 H69D 56.3 . . ? H69C C69 H69D 56.3 . . ? C68 C69 H69E 109.5 . . ? H69A C69 H69E 56.3 . . ? H69B C69 H69E 141.1 . . ? H69C C69 H69E 56.3 . . ? H69D C69 H69E 109.5 . . ? C68 C69 H69F 109.5 . . ? H69A C69 H69F 56.3 . . ? H69B C69 H69F 56.3 . . ? H69C C69 H69F 141.1 . . ? H69D C69 H69F 109.5 . . ? H69E C69 H69F 109.5 . . ? C67A C66A Al1 108.5(15) . . ? C67A C66A H66C 110.0 . . ? Al1 C66A H66C 110.0 . . ? C67A C66A H66D 110.0 . . ? Al1 C66A H66D 110.0 . . ? H66C C66A H66D 108.4 . . ? C66A C67A H67G 109.5 . . ? C66A C67A H67H 109.5 . . ? H67G C67A H67H 109.5 . . ? C66A C67A H67I 109.5 . . ? H67G C67A H67I 109.5 . . ? H67H C67A H67I 109.5 . . ? C66A C67A H67J 109.5 . . ? H67G C67A H67J 141.1 . . ? H67H C67A H67J 56.3 . . ? H67I C67A H67J 56.3 . . ? C66A C67A H67K 109.5 . . ? H67G C67A H67K 56.3 . . ? H67H C67A H67K 141.1 . . ? H67I C67A H67K 56.3 . . ? H67J C67A H67K 109.5 . . ? C66A C67A H67L 109.5 . . ? H67G C67A H67L 56.3 . . ? H67H C67A H67L 56.3 . . ? H67I C67A H67L 141.1 . . ? H67J C67A H67L 109.5 . . ? H67K C67A H67L 109.5 . . ? C69A C68A Al1 114.9(15) . . ? C69A C68A H68C 108.5 . . ? Al1 C68A H68C 108.5 . . ? C69A C68A H68D 108.5 . . ? Al1 C68A H68D 108.5 . . ? H68C C68A H68D 107.5 . . ? C68A C69A H69G 109.5 . . ? C68A C69A H69H 109.5 . . ? H69G C69A H69H 109.5 . . ? C68A C69A H69I 109.5 . . ? H69G C69A H69I 109.5 . . ? H69H C69A H69I 109.5 . . ? C68A C69A H69J 109.5 . . ? H69G C69A H69J 141.1 . . ? H69H C69A H69J 56.3 . . ? H69I C69A H69J 56.3 . . ? C68A C69A H69K 109.5 . . ? H69G C69A H69K 56.3 . . ? H69H C69A H69K 141.1 . . ? H69I C69A H69K 56.3 . . ? H69J C69A H69K 109.5 . . ? C68A C69A H69L 109.5 . . ? H69G C69A H69L 56.3 . . ? H69H C69A H69L 56.3 . . ? H69I C69A H69L 141.1 . . ? H69J C69A H69L 109.5 . . ? H69K C69A H69L 109.5 . . ? C74 Al2 C70 114.1(4) . . ? C74 Al2 C72 107.9(4) . . ? C70 Al2 C72 106.5(3) . . ? C74 Al2 C28 107.4(3) . . ? C70 Al2 C28 110.2(2) . . ? C72 Al2 C28 110.7(3) . . ? C71 C70 Al2 110.7(4) . . ? C71 C70 H70A 109.5 . . ? Al2 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? Al2 C70 H70B 109.5 . . ? H70A C70 H70B 108.1 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.4 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C71 H71D 109.5 . . ? H71A C71 H71D 141.1 . . ? H71B C71 H71D 56.2 . . ? H71C C71 H71D 56.3 . . ? C70 C71 H71E 109.4 . . ? H71A C71 H71E 56.3 . . ? H71B C71 H71E 141.0 . . ? H71C C71 H71E 56.2 . . ? H71D C71 H71E 109.5 . . ? C70 C71 H71F 109.5 . . ? H71A C71 H71F 56.3 . . ? H71B C71 H71F 56.2 . . ? H71C C71 H71F 141.1 . . ? H71D C71 H71F 109.5 . . ? H71E C71 H71F 109.5 . . ? C73 C72 Al2 118.0(7) . . ? C73 C72 H72A 107.8 . . ? Al2 C72 H72A 107.8 . . ? C73 C72 H72B 107.8 . . ? Al2 C72 H72B 107.8 . . ? H72A C72 H72B 107.1 . . ? C72 C73 H73A 109.3 . . ? C72 C73 H73B 109.6 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C73 H73D 109.6 . . ? H73A C73 H73D 141.0 . . ? H73B C73 H73D 56.3 . . ? H73C C73 H73D 56.2 . . ? C72 C73 H73E 109.4 . . ? H73A C73 H73E 56.2 . . ? H73B C73 H73E 141.0 . . ? H73C C73 H73E 56.3 . . ? H73D C73 H73E 109.5 . . ? C72 C73 H73F 109.4 . . ? H73A C73 H73F 56.3 . . ? H73B C73 H73F 56.2 . . ? H73C C73 H73F 141.0 . . ? H73D C73 H73F 109.5 . . ? H73E C73 H73F 109.5 . . ? C75 C74 Al2 114.6(7) . . ? C75A C74 Al2 117.0(16) . . ? C75 C74 H74A 108.6 . . ? C75A C74 H74A 70.4 . . ? Al2 C74 H74A 108.6 . . ? C75 C74 H74B 108.6 . . ? C75A C74 H74B 132.5 . . ? Al2 C74 H74B 108.6 . . ? H74A C74 H74B 107.6 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C75 H75D 109.5 . . ? H75A C75 H75D 141.1 . . ? H75B C75 H75D 56.3 . . ? H75C C75 H75D 56.3 . . ? C74 C75 H75E 109.5 . . ? H75A C75 H75E 56.3 . . ? H75B C75 H75E 141.1 . . ? H75C C75 H75E 56.3 . . ? H75D C75 H75E 109.5 . . ? C74 C75 H75F 109.5 . . ? H75A C75 H75F 56.3 . . ? H75B C75 H75F 56.3 . . ? H75C C75 H75F 141.1 . . ? H75D C75 H75F 109.5 . . ? H75E C75 H75F 109.5 . . ? C74 C75A H75G 109.5 . . ? C74 C75A H75H 109.5 . . ? H75G C75A H75H 109.5 . . ? C74 C75A H75I 109.5 . . ? H75G C75A H75I 109.5 . . ? H75H C75A H75I 109.5 . . ? C74 C75A H75J 109.5 . . ? H75G C75A H75J 141.1 . . ? H75H C75A H75J 56.3 . . ? H75I C75A H75J 56.3 . . ? C74 C75A H75K 109.5 . . ? H75G C75A H75K 56.3 . . ? H75H C75A H75K 141.1 . . ? H75I C75A H75K 56.3 . . ? H75J C75A H75K 109.5 . . ? C74 C75A H75L 109.5 . . ? H75G C75A H75L 56.3 . . ? H75H C75A H75L 56.3 . . ? H75I C75A H75L 141.1 . . ? H75J C75A H75L 109.5 . . ? H75K C75A H75L 109.5 . . ? O105 K101 O104 131.06(14) . . ? O105 K101 O102 123.51(15) . . ? O104 K101 O102 99.63(16) . . ? O105 K101 O101 98.02(14) . . ? O104 K101 O101 124.90(13) . . ? O102 K101 O101 60.50(15) . . ? O105 K101 O106 60.57(14) . . ? O104 K101 O106 93.80(13) . . ? O102 K101 O106 98.66(15) . . ? O101 K101 O106 137.01(13) . . ? O105 K101 O103 92.62(14) . . ? O104 K101 O103 60.82(14) . . ? O102 K101 O103 139.23(14) . . ? O101 K101 O103 99.69(13) . . ? O106 K101 O103 116.89(15) . . ? O105 K101 N102 119.73(15) . . ? O104 K101 N102 61.00(16) . . ? O102 K101 N102 59.77(17) . . ? O101 K101 N102 119.88(17) . . ? O106 K101 N102 59.77(16) . . ? O103 K101 N102 121.18(17) . . ? O105 K101 N101 60.26(14) . . ? O104 K101 N101 119.04(15) . . ? O102 K101 N101 120.21(15) . . ? O101 K101 N101 60.09(14) . . ? O106 K101 N101 120.23(16) . . ? O103 K101 N101 58.86(14) . . ? N102 K101 N101 179.97(19) . . ? C113 N101 C107 109.8(6) . . ? C113 N101 C101 109.9(5) . . ? C107 N101 C101 108.6(5) . . ? C113 N101 K101 107.7(4) . . ? C107 N101 K101 112.1(4) . . ? C101 N101 K101 108.7(4) . . ? C112 N102 C106 111.9(7) . . ? C112 N102 C118 110.1(6) . . ? C106 N102 C118 110.6(6) . . ? C112 N102 K101 104.8(4) . . ? C106 N102 K101 110.1(4) . . ? C118 N102 K101 109.2(5) . . ? C102 O101 C103 110.4(5) . . ? C102 O101 K101 117.9(3) . . ? C103 O101 K101 112.8(4) . . ? C105 O102 C104 113.7(6) . . ? C105 O102 K101 118.1(5) . . ? C104 O102 K101 114.6(4) . . ? C108 O103 C109 112.1(5) . . ? C108 O103 K101 116.7(4) . . ? C109 O103 K101 113.4(4) . . ? C110 O104 C111 111.3(6) . . ? C110 O104 K101 111.7(4) . . ? C111 O104 K101 116.8(4) . . ? C115 O105 C114 111.3(6) . . ? C115 O105 K101 114.6(4) . . ? C114 O105 K101 119.1(4) . . ? C116 O106 C117 110.1(5) . . ? C116 O106 K101 112.6(4) . . ? C117 O106 K101 115.6(4) . . ? N101 C101 C102 112.7(5) . . ? N101 C101 H10A 109.0 . . ? C102 C101 H10A 109.0 . . ? N101 C101 H10B 109.0 . . ? C102 C101 H10B 109.0 . . ? H10A C101 H10B 107.8 . . ? O101 C102 C101 109.9(6) . . ? O101 C102 H10C 109.7 . . ? C101 C102 H10C 109.7 . . ? O101 C102 H10D 109.7 . . ? C101 C102 H10D 109.7 . . ? H10C C102 H10D 108.2 . . ? O101 C103 C104 109.1(6) . . ? O101 C103 H10E 109.9 . . ? C104 C103 H10E 109.9 . . ? O101 C103 H10F 109.9 . . ? C104 C103 H10F 109.9 . . ? H10E C103 H10F 108.3 . . ? O102 C104 C103 110.2(6) . . ? O102 C104 H10G 109.6 . . ? C103 C104 H10G 109.6 . . ? O102 C104 H10H 109.6 . . ? C103 C104 H10H 109.6 . . ? H10G C104 H10H 108.1 . . ? O102 C105 C106 110.8(8) . . ? O102 C105 H10I 109.5 . . ? C106 C105 H10I 109.5 . . ? O102 C105 H10J 109.5 . . ? C106 C105 H10J 109.5 . . ? H10I C105 H10J 108.1 . . ? N102 C106 C105 112.0(7) . . ? N102 C106 H10K 109.2 . . ? C105 C106 H10K 109.2 . . ? N102 C106 H10L 109.2 . . ? C105 C106 H10L 109.2 . . ? H10K C106 H10L 107.9 . . ? N101 C107 C108 112.0(6) . . ? N101 C107 H10M 109.2 . . ? C108 C107 H10M 109.2 . . ? N101 C107 H10N 109.2 . . ? C108 C107 H10N 109.2 . . ? H10M C107 H10N 107.9 . . ? O103 C108 C107 110.0(5) . . ? O103 C108 H10O 109.7 . . ? C107 C108 H10O 109.7 . . ? O103 C108 H10P 109.7 . . ? C107 C108 H10P 109.7 . . ? H10O C108 H10P 108.2 . . ? O103 C109 C110 108.3(6) . . ? O103 C109 H10Q 110.0 . . ? C110 C109 H10Q 110.0 . . ? O103 C109 H10R 110.0 . . ? C110 C109 H10R 110.0 . . ? H10Q C109 H10R 108.4 . . ? O104 C110 C109 108.9(6) . . ? O104 C110 H11G 109.9 . . ? C109 C110 H11G 109.9 . . ? O104 C110 H11H 109.9 . . ? C109 C110 H11H 109.9 . . ? H11G C110 H11H 108.3 . . ? C112 C111 O104 108.7(6) . . ? C112 C111 H11I 110.0 . . ? O104 C111 H11I 110.0 . . ? C112 C111 H11J 110.0 . . ? O104 C111 H11J 110.0 . . ? H11I C111 H11J 108.3 . . ? C111 C112 N102 117.6(8) . . ? C111 C112 H11K 107.9 . . ? N102 C112 H11K 107.9 . . ? C111 C112 H11L 107.9 . . ? N102 C112 H11L 107.9 . . ? H11K C112 H11L 107.2 . . ? N101 C113 C114 113.8(6) . . ? N101 C113 H11M 108.8 . . ? C114 C113 H11M 108.8 . . ? N101 C113 H11N 108.8 . . ? C114 C113 H11N 108.8 . . ? H11M C113 H11N 107.7 . . ? O105 C114 C113 109.1(6) . . ? O105 C114 H11O 109.9 . . ? C113 C114 H11O 109.9 . . ? O105 C114 H11P 109.9 . . ? C113 C114 H11P 109.9 . . ? H11O C114 H11P 108.3 . . ? O105 C115 C116 108.8(6) . . ? O105 C115 H11Q 109.9 . . ? C116 C115 H11Q 109.9 . . ? O105 C115 H11R 109.9 . . ? C116 C115 H11R 109.9 . . ? H11Q C115 H11R 108.3 . . ? O106 C116 C115 109.3(6) . . ? O106 C116 H11S 109.8 . . ? C115 C116 H11S 109.8 . . ? O106 C116 H11T 109.8 . . ? C115 C116 H11T 109.8 . . ? H11S C116 H11T 108.3 . . ? O106 C117 C118 108.1(6) . . ? O106 C117 H11U 110.1 . . ? C118 C117 H11U 110.1 . . ? O106 C117 H11V 110.1 . . ? C118 C117 H11V 110.1 . . ? H11U C117 H11V 108.4 . . ? N102 C118 C117 112.6(7) . . ? N102 C118 H11W 109.1 . . ? C117 C118 H11W 109.1 . . ? N102 C118 H11X 109.1 . . ? C117 C118 H11X 109.1 . . ? H11W C118 H11X 107.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.461 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.061 _iucr_refine_instructions_details ; TITL RM052 in Pmc2(1) New: Pna21 CELL 1.54180 23.1194 37.1470 11.0300 90.000 90.000 90.000 ZERR 4.00 0.0005 0.0012 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SFAC C H AL FE K N O UNIT 372 588 8 4 4 24 24 MERG 2 OMIT 0.00 133.00 TWIN EADP C66 C66A EADP C67 C67A EADP C68 C68A EADP C69 C69A EADP C75 C75A ISOR 0.10 0.20 C74 C75 DFIX 1.550 0.020 C74 C75 DFIX 1.550 0.020 C74 C75A SIZE 0.13 0.14 0.16 ACTA BOND $H L.S. 12 TEMP -123.00 WGHT 0.004100 20.882099 BASF 0.04251 FVAR 2.53118 0.63725 0.79364 FE1 4 0.339101 0.157880 0.215406 11.00000 0.02455 0.02762 = 0.04862 0.01111 -0.00796 -0.00330 N1 6 0.480253 0.120316 0.423753 11.00000 0.02590 0.02256 = 0.03399 0.00552 -0.00150 0.00045 C1 1 0.501134 0.154857 0.426751 11.00000 0.02917 0.02684 = 0.02725 0.00463 -0.00031 -0.00142 N2 6 0.459577 0.173426 0.365041 11.00000 0.02300 0.01891 = 0.04908 0.00035 -0.00775 -0.00219 C2 1 0.427540 0.119119 0.363067 11.00000 0.02788 0.02833 = 0.02806 0.00171 -0.00439 -0.00398 AFIX 43 H2 2 0.405302 0.097936 0.350574 11.00000 -1.20000 AFIX 0 C3 1 0.412339 0.152506 0.324184 11.00000 0.02538 0.02683 = 0.03825 0.00245 0.00081 -0.00408 C4 1 0.508217 0.087347 0.461144 11.00000 0.03013 0.02220 = 0.04294 0.00646 -0.00402 0.00075 C5 1 0.543985 0.070058 0.377258 11.00000 0.02970 0.02557 = 0.04738 -0.00307 0.00385 0.00016 C6 1 0.564764 0.036195 0.407528 11.00000 0.03415 0.03615 = 0.07323 0.00324 -0.00618 0.00617 AFIX 43 H6 2 0.589442 0.023741 0.352908 11.00000 -1.20000 AFIX 0 C7 1 0.549713 0.020387 0.517194 11.00000 0.04078 0.02868 = 0.07414 0.01488 -0.01112 0.00777 AFIX 43 H7 2 0.563901 -0.002911 0.536609 11.00000 -1.20000 AFIX 0 C8 1 0.514649 0.038037 0.597561 11.00000 0.05008 0.03501 = 0.04911 0.01347 -0.01234 -0.00164 AFIX 43 H8 2 0.505184 0.026929 0.672562 11.00000 -1.20000 AFIX 0 C9 1 0.492559 0.072148 0.570973 11.00000 0.03869 0.03073 = 0.03946 0.01176 -0.01046 -0.00373 C10 1 0.558741 0.086356 0.255712 11.00000 0.04473 0.03232 = 0.04478 -0.00024 0.00428 0.00122 AFIX 13 H10 2 0.552446 0.112939 0.261234 11.00000 -1.20000 AFIX 0 C11 1 0.622255 0.079866 0.218906 11.00000 0.05954 0.06322 = 0.05336 -0.00778 0.02349 0.00055 AFIX 3 H11A 2 0.629586 0.091036 0.139896 10.50000 -1.20000 H11B 2 0.629556 0.053926 0.213566 10.50000 -1.20000 H11C 2 0.647956 0.090506 0.279766 10.50000 -1.20000 H11D 2 0.641816 0.065946 0.282256 10.50000 -1.20000 H11E 2 0.641846 0.103056 0.208596 10.50000 -1.20000 H11F 2 0.623436 0.066476 0.142386 10.50000 -1.20000 AFIX 0 C12 1 0.519288 0.071648 0.155372 11.00000 0.07405 0.05798 = 0.05277 0.00173 0.00480 -0.00453 AFIX 3 H12A 2 0.529608 0.082838 0.077872 10.50000 -1.20000 H12B 2 0.478898 0.077198 0.174782 10.50000 -1.20000 H12C 2 0.524178 0.045498 0.149372 10.50000 -1.20000 H12D 2 0.492178 0.054178 0.190152 10.50000 -1.20000 H12E 2 0.542888 0.059818 0.093232 10.50000 -1.20000 H12F 2 0.497608 0.091518 0.118642 10.50000 -1.20000 AFIX 0 C13 1 0.450770 0.089890 0.659505 11.00000 0.07264 0.03486 = 0.04874 0.01308 0.00964 0.00222 AFIX 13 H13 2 0.450101 0.116248 0.641122 11.00000 -1.20000 AFIX 0 C14 1 0.468618 0.085490 0.791382 11.00000 0.11419 0.06510 = 0.03416 0.00830 -0.00234 -0.00476 AFIX 3 H14A 2 0.440418 0.097589 0.843703 10.50000 -1.20000 H14B 2 0.506908 0.096209 0.803632 10.50000 -1.20000 H14C 2 0.470049 0.059829 0.811792 10.50000 -1.20000 H14D 2 0.504499 0.071500 0.795713 10.50000 -1.20000 H14E 2 0.438009 0.072879 0.835793 10.50000 -1.20000 H14F 2 0.474869 0.109260 0.827623 10.50000 -1.20000 AFIX 0 C15 1 0.389657 0.075374 0.640342 11.00000 0.05624 0.07456 = 0.06660 0.02145 0.01173 0.00670 AFIX 3 H15A 2 0.363137 0.087074 0.697352 10.50000 -1.20000 H15B 2 0.389357 0.049314 0.654272 10.50000 -1.20000 H15C 2 0.377247 0.080404 0.557102 10.50000 -1.20000 H15D 2 0.390027 0.057453 0.575132 10.50000 -1.20000 H15E 2 0.363807 0.095214 0.618212 10.50000 -1.20000 H15F 2 0.375917 0.064124 0.715382 10.50000 -1.20000 AFIX 0 C16 1 0.464972 0.211821 0.338329 11.00000 0.03229 0.02198 = 0.03058 0.00507 -0.01136 -0.00537 C17 1 0.503439 0.222242 0.247989 11.00000 0.03279 0.03059 = 0.03950 0.01065 -0.00707 -0.00717 C18 1 0.509406 0.259001 0.226774 11.00000 0.04522 0.03426 = 0.04443 0.01213 -0.00783 -0.01235 AFIX 43 H18 2 0.535590 0.267202 0.166417 11.00000 -1.20000 AFIX 0 C19 1 0.477652 0.283614 0.292578 11.00000 0.05722 0.02280 = 0.06574 0.01304 -0.01170 -0.00896 AFIX 43 H19 2 0.482306 0.308618 0.277352 11.00000 -1.20000 AFIX 0 C20 1 0.439485 0.272383 0.379633 11.00000 0.05000 0.02506 = 0.06093 -0.00441 -0.01104 -0.00065 AFIX 43 H20 2 0.417599 0.289803 0.422897 11.00000 -1.20000 AFIX 0 C21 1 0.432005 0.236178 0.406178 11.00000 0.02956 0.02468 = 0.05382 0.00958 -0.00443 0.00166 C22 1 0.537317 0.195016 0.173056 11.00000 0.03970 0.04116 = 0.04445 0.01922 0.00554 -0.00137 AFIX 13 H22 2 0.548855 0.175024 0.228748 11.00000 -1.20000 AFIX 0 C23 1 0.593093 0.210482 0.117868 11.00000 0.04627 0.06996 = 0.07058 0.01740 0.00976 -0.00929 AFIX 3 H23A 2 0.616833 0.221092 0.182208 10.50000 -1.20000 H23B 2 0.583223 0.229052 0.058238 10.50000 -1.20000 H23C 2 0.614773 0.191152 0.077978 10.50000 -1.20000 H23D 2 0.593053 0.206432 0.030078 10.50000 -1.20000 H23E 2 0.626662 0.198482 0.154048 10.50000 -1.20000 H23F 2 0.595113 0.236382 0.134308 10.50000 -1.20000 AFIX 0 C24 1 0.499715 0.178598 0.073462 11.00000 0.05718 0.05075 = 0.05421 -0.00845 0.00696 -0.01074 AFIX 3 H24A 2 0.522514 0.161128 0.027132 10.50000 -1.20000 H24B 2 0.486105 0.197688 0.019162 10.50000 -1.20000 H24C 2 0.466415 0.166458 0.110192 10.50000 -1.20000 H24D 2 0.460835 0.189058 0.077192 10.50000 -1.20000 H24E 2 0.497255 0.152488 0.085162 10.50000 -1.20000 H24F 2 0.516944 0.183718 -0.005868 10.50000 -1.20000 AFIX 0 C25 1 0.391410 0.223690 0.505139 11.00000 0.04063 0.03438 = 0.05092 -0.00879 0.00239 0.00018 AFIX 13 H25 2 0.370773 0.201738 0.475427 11.00000 -1.20000 AFIX 0 C26 1 0.424706 0.213456 0.621821 11.00000 0.05627 0.07876 = 0.05236 0.01508 -0.00017 0.01172 AFIX 3 H26A 2 0.397256 0.205396 0.683851 10.50000 -1.20000 H26B 2 0.445946 0.234485 0.651701 10.50000 -1.20000 H26C 2 0.452006 0.193996 0.603801 10.50000 -1.20000 H26D 2 0.466226 0.217196 0.609051 10.50000 -1.20000 H26E 2 0.417536 0.188096 0.641201 10.50000 -1.20000 H26F 2 0.411476 0.228585 0.689101 10.50000 -1.20000 AFIX 0 C27 1 0.345410 0.251859 0.541889 11.00000 0.05791 0.05340 = 0.06786 -0.00567 0.01915 0.01414 AFIX 3 H27A 2 0.320700 0.241879 0.605770 10.50000 -1.20000 H27B 2 0.321690 0.257959 0.471189 10.50000 -1.20000 H27C 2 0.364680 0.273599 0.571969 10.50000 -1.20000 H27D 2 0.350680 0.273749 0.493519 10.50000 -1.20000 H27E 2 0.349690 0.257669 0.628099 10.50000 -1.20000 H27F 2 0.306700 0.242029 0.527309 10.50000 -1.20000 AFIX 0 N3 6 0.241230 0.098518 0.250504 11.00000 0.02170 0.02849 = 0.04190 0.01127 -0.00415 -0.00371 C28 1 0.228404 0.063057 0.236782 11.00000 0.03185 0.03080 = 0.03739 0.00524 -0.00764 -0.00288 N4 6 0.278970 0.048820 0.193551 11.00000 0.03006 0.03058 = 0.03612 0.00752 -0.00223 -0.00754 C29 1 0.298453 0.107781 0.214738 11.00000 0.02627 0.03067 = 0.03916 0.00411 -0.01001 -0.00460 C30 1 0.320410 0.075918 0.181489 11.00000 0.02532 0.03755 = 0.04258 0.01337 0.00006 -0.01037 AFIX 43 H30 2 0.358837 0.072262 0.153579 11.00000 -1.20000 AFIX 0 C31 1 0.199187 0.125430 0.283659 11.00000 0.02589 0.02621 = 0.04650 0.01052 -0.00168 -0.00280 C32 1 0.165528 0.141630 0.192788 11.00000 0.02922 0.03312 = 0.06734 0.01717 -0.01128 -0.00259 C33 1 0.125850 0.167751 0.232042 11.00000 0.03054 0.04506 = 0.08590 0.01661 -0.01783 0.00609 AFIX 43 H33 2 0.101208 0.178796 0.174019 11.00000 -1.20000 AFIX 0 C34 1 0.121373 0.177995 0.352596 11.00000 0.04268 0.03820 = 0.07061 0.00777 0.00643 0.00831 AFIX 43 H34 2 0.093947 0.195708 0.376153 11.00000 -1.20000 AFIX 0 C35 1 0.156552 0.162515 0.437293 11.00000 0.03459 0.03570 = 0.07871 0.00766 0.00864 0.00661 AFIX 43 H35 2 0.153678 0.170146 0.519276 11.00000 -1.20000 AFIX 0 C36 1 0.196572 0.135857 0.407312 11.00000 0.02635 0.03061 = 0.05690 0.01066 -0.00082 -0.00007 C37 1 0.173164 0.131799 0.059264 11.00000 0.04373 0.04430 = 0.04341 0.00973 -0.02591 -0.00256 AFIX 13 H37 2 0.212765 0.121486 0.048174 11.00000 -1.20000 AFIX 0 C38 1 0.166295 0.163400 -0.026888 11.00000 0.06118 0.05736 = 0.09040 0.02884 -0.02197 -0.02149 AFIX 3 H38A 2 0.171535 0.155089 -0.110498 10.50000 -1.20000 H38B 2 0.195375 0.181769 -0.008118 10.50000 -1.20000 H38C 2 0.127525 0.173719 -0.017708 10.50000 -1.20000 H38D 2 0.158085 0.185289 0.019622 10.50000 -1.20000 H38E 2 0.134245 0.158619 -0.082768 10.50000 -1.20000 H38F 2 0.202095 0.166669 -0.073168 10.50000 -1.20000 AFIX 0 C39 1 0.128371 0.102813 0.023424 11.00000 0.10536 0.06041 = 0.08332 0.01572 -0.02488 -0.04071 AFIX 3 H39A 2 0.133371 0.096533 -0.062226 10.50000 -1.20000 H39B 2 0.089251 0.112233 0.036274 10.50000 -1.20000 H39C 2 0.134061 0.081313 0.073504 10.50000 -1.20000 H39D 2 0.104421 0.096853 0.093924 10.50000 -1.20000 H39E 2 0.148541 0.081153 -0.004576 10.50000 -1.20000 H39F 2 0.103731 0.112073 -0.041796 10.50000 -1.20000 AFIX 0 C40 1 0.235648 0.120509 0.503579 11.00000 0.03356 0.04236 = 0.04665 0.01415 -0.00227 0.00544 AFIX 13 H40 2 0.257063 0.099715 0.467519 11.00000 -1.20000 AFIX 0 C41 1 0.279937 0.148408 0.543954 11.00000 0.04063 0.07397 = 0.06742 0.00602 -0.01436 -0.00718 AFIX 3 H41A 2 0.305007 0.137968 0.606374 10.50000 -1.20000 H41B 2 0.259847 0.169438 0.577154 10.50000 -1.20000 H41C 2 0.303438 0.155768 0.474294 10.50000 -1.20000 H41D 2 0.273858 0.170818 0.498844 10.50000 -1.20000 H41E 2 0.319017 0.139348 0.528054 10.50000 -1.20000 H41F 2 0.275418 0.153018 0.630924 10.50000 -1.20000 AFIX 0 C42 1 0.202339 0.106767 0.614548 11.00000 0.05793 0.06976 = 0.07266 0.01988 -0.01228 -0.00169 AFIX 3 H42A 2 0.229679 0.097008 0.673958 10.50000 -1.20000 H42B 2 0.175359 0.087827 0.589498 10.50000 -1.20000 H42C 2 0.180709 0.126697 0.651118 10.50000 -1.20000 H42D 2 0.160819 0.110677 0.602428 10.50000 -1.20000 H42E 2 0.215139 0.119858 0.686878 10.50000 -1.20000 H42F 2 0.209789 0.080998 0.625268 10.50000 -1.20000 AFIX 0 C43 1 0.290071 0.011977 0.159441 11.00000 0.03172 0.02872 = 0.05913 -0.00192 0.00661 -0.00892 C44 1 0.274097 0.000252 0.044662 11.00000 0.04267 0.05558 = 0.04702 0.00373 0.00708 -0.02100 C45 1 0.287368 -0.034848 0.012244 11.00000 0.06311 0.06773 = 0.04059 -0.01318 0.02100 -0.03249 AFIX 43 H45 2 0.276619 -0.043601 -0.065482 11.00000 -1.20000 AFIX 0 C46 1 0.315984 -0.057068 0.091853 11.00000 0.06210 0.03831 = 0.08098 -0.01319 0.03180 -0.02095 AFIX 43 H46 2 0.324841 -0.081083 0.068791 11.00000 -1.20000 AFIX 0 C47 1 0.331862 -0.044782 0.204542 11.00000 0.04734 0.03095 = 0.06419 0.00670 0.00308 -0.00400 AFIX 43 H47 2 0.351742 -0.060570 0.257971 11.00000 -1.20000 AFIX 0 C48 1 0.319714 -0.010003 0.242568 11.00000 0.03675 0.02626 = 0.04798 0.00589 0.00396 -0.00423 C49 1 0.247506 0.025792 -0.046877 11.00000 0.05918 0.10020 = 0.02279 0.00536 -0.00822 -0.01265 AFIX 13 H49 2 0.225085 0.044384 -0.001152 11.00000 -1.20000 AFIX 0 C50 1 0.294535 0.045132 -0.118848 11.00000 0.08637 0.11082 = 0.06289 0.02926 -0.00271 -0.01297 AFIX 3 H50A 2 0.276575 0.061942 -0.176028 10.50000 -1.20000 H50B 2 0.317555 0.027422 -0.163668 10.50000 -1.20000 H50C 2 0.319665 0.058442 -0.063088 10.50000 -1.20000 H50D 2 0.332625 0.036592 -0.092498 10.50000 -1.20000 H50E 2 0.291645 0.071122 -0.104848 10.50000 -1.20000 H50F 2 0.289535 0.040102 -0.205428 10.50000 -1.20000 AFIX 0 C51 1 0.206161 0.008008 -0.138985 11.00000 0.09828 0.16392 = 0.06422 -0.01321 -0.02356 -0.02010 AFIX 3 H51A 2 0.190151 0.026508 -0.192705 10.50000 -1.20000 H51B 2 0.174601 -0.004002 -0.095605 10.50000 -1.20000 H51C 2 0.227491 -0.009732 -0.187215 10.50000 -1.20000 H51D 2 0.204681 -0.017992 -0.124314 10.50000 -1.20000 H51E 2 0.220231 0.012518 -0.221405 10.50000 -1.20000 H51F 2 0.167341 0.018248 -0.129805 10.50000 -1.20000 AFIX 0 C52 1 0.342173 0.003943 0.362917 11.00000 0.04426 0.02913 = 0.04598 0.00219 -0.00158 0.00639 AFIX 13 H52 2 0.320618 0.026474 0.383422 11.00000 -1.20000 AFIX 0 C53 1 0.406478 0.013322 0.350515 11.00000 0.04862 0.04166 = 0.05485 -0.00517 -0.00724 0.00178 AFIX 3 H53A 2 0.421048 0.022372 0.428195 10.50000 -1.20000 H53B 2 0.411318 0.031862 0.288145 10.50000 -1.20000 H53C 2 0.428178 -0.008268 0.327295 10.50000 -1.20000 H53D 2 0.419318 0.008272 0.267565 10.50000 -1.20000 H53E 2 0.429038 -0.001218 0.407615 10.50000 -1.20000 H53F 2 0.412188 0.038912 0.368455 10.50000 -1.20000 AFIX 0 C54 1 0.334384 -0.022482 0.466158 11.00000 0.07292 0.05717 = 0.05874 0.01805 -0.02305 0.00523 AFIX 3 H54A 2 0.349584 -0.011952 0.541117 10.50000 -1.20000 H54B 2 0.355344 -0.044753 0.447887 10.50000 -1.20000 H54C 2 0.293154 -0.027832 0.476318 10.50000 -1.20000 H54D 2 0.315814 -0.044413 0.435758 10.50000 -1.20000 H54E 2 0.310044 -0.011602 0.528997 10.50000 -1.20000 H54F 2 0.372224 -0.028522 0.500567 10.50000 -1.20000 AFIX 0 C55 1 0.307993 0.195385 0.095819 11.00000 0.03389 0.03436 = 0.04333 0.00942 -0.00909 -0.00840 C56 1 0.315666 0.192032 -0.029549 11.00000 0.03699 0.04788 = 0.03944 0.01276 -0.00574 -0.00345 C57 1 0.291088 0.215863 -0.112342 11.00000 0.04803 0.05789 = 0.05070 0.02350 -0.00376 -0.00706 AFIX 43 H57 2 0.297711 0.212914 -0.196762 11.00000 -1.20000 AFIX 0 C58 1 0.256452 0.244276 -0.070141 11.00000 0.04428 0.04714 = 0.06597 0.02652 -0.02094 -0.00326 C59 1 0.247226 0.247743 0.052605 11.00000 0.04187 0.04192 = 0.05849 0.01114 -0.01367 0.00326 AFIX 43 H59 2 0.223178 0.266619 0.081525 11.00000 -1.20000 AFIX 0 C60 1 0.272240 0.224319 0.134596 11.00000 0.03548 0.02742 = 0.06195 0.01853 -0.00706 -0.00464 C61 1 0.351379 0.160609 -0.080724 11.00000 0.06353 0.05685 = 0.04566 0.00644 -0.00002 0.00755 AFIX 3 H61A 2 0.365838 0.145799 -0.013754 10.50000 -1.20000 H61B 2 0.384109 0.170109 -0.127254 10.50000 -1.20000 H61C 2 0.326938 0.145889 -0.133764 10.50000 -1.20000 H61D 2 0.352078 0.162069 -0.169424 10.50000 -1.20000 H61E 2 0.333818 0.137759 -0.055934 10.50000 -1.20000 H61F 2 0.390988 0.161969 -0.049424 10.50000 -1.20000 AFIX 0 C62 1 0.230880 0.271034 -0.160834 11.00000 0.07886 0.07045 = 0.08533 0.03354 -0.01822 0.01101 AFIX 3 H62A 2 0.242460 0.264204 -0.243154 10.50000 -1.20000 H62B 2 0.245210 0.295274 -0.142834 10.50000 -1.20000 H62C 2 0.188600 0.270734 -0.154704 10.50000 -1.20000 H62D 2 0.208390 0.289274 -0.117314 10.50000 -1.20000 H62E 2 0.205630 0.258204 -0.217624 10.50000 -1.20000 H62F 2 0.262240 0.282744 -0.205754 10.50000 -1.20000 AFIX 0 C63 1 0.259923 0.228853 0.269015 11.00000 0.06219 0.04427 = 0.05380 0.00602 -0.00290 0.00836 AFIX 3 H63A 2 0.280523 0.210223 0.314755 10.50000 -1.20000 H63B 2 0.218263 0.226603 0.283505 10.50000 -1.20000 H63C 2 0.273083 0.252663 0.295505 10.50000 -1.20000 H63D 2 0.234053 0.249443 0.281095 10.50000 -1.20000 H63E 2 0.296313 0.233053 0.312335 10.50000 -1.20000 H63F 2 0.241493 0.206993 0.300335 10.50000 -1.20000 AFIX 0 AL1 3 0.575468 0.173480 0.514854 11.00000 0.03955 0.03470 = 0.06134 0.00985 -0.02390 -0.00688 C64 1 0.583143 0.226481 0.502431 11.00000 0.05265 0.03549 = 0.07393 -0.01262 -0.02979 -0.00086 AFIX 23 H64A 2 0.590597 0.233177 0.416972 11.00000 -1.20000 H64B 2 0.546402 0.237943 0.527633 11.00000 -1.20000 AFIX 0 C65 1 0.632233 0.240473 0.581730 11.00000 0.06525 0.04537 = 0.09538 -0.00259 -0.04132 -0.01043 AFIX 3 H65A 2 0.634903 0.266693 0.573614 10.50000 -1.20000 H65B 2 0.668753 0.229483 0.555982 10.50000 -1.20000 H65C 2 0.624603 0.234242 0.666574 10.50000 -1.20000 H65D 2 0.650603 0.220252 0.623834 10.50000 -1.20000 H65E 2 0.616753 0.257463 0.641464 10.50000 -1.20000 H65F 2 0.660903 0.252703 0.530884 10.50000 -1.20000 AFIX 0 PART 1 C66 1 0.642100 0.149740 0.469606 21.00000 0.04736 0.05379 = 0.05086 -0.02003 -0.00135 0.00025 AFIX 23 H66A 2 0.667035 0.148686 0.542489 21.00000 -1.20000 H66B 2 0.630778 0.124638 0.451015 21.00000 -1.20000 AFIX 0 C67 1 0.679399 0.161945 0.368260 21.00000 0.10075 0.06321 = 0.11807 -0.03956 0.04758 -0.03541 AFIX 123 H67A 2 0.712119 0.145388 0.359264 20.50000 -1.50000 H67B 2 0.693870 0.186207 0.385513 20.50000 -1.50000 H67C 2 0.656859 0.162307 0.293024 20.50000 -1.50000 H67D 2 0.663113 0.183881 0.332603 20.50000 -1.50000 H67E 2 0.681362 0.143061 0.306355 20.50000 -1.50000 H67F 2 0.718373 0.166961 0.398843 20.50000 -1.50000 AFIX 0 C68 1 0.556037 0.165269 0.696937 21.00000 0.04920 0.07487 = 0.04179 0.00172 -0.01672 0.00011 AFIX 23 H68A 2 0.546076 0.188758 0.733846 21.00000 -1.20000 H68B 2 0.521352 0.149721 0.702288 21.00000 -1.20000 AFIX 0 C69 1 0.604274 0.148158 0.770983 21.00000 0.07775 0.09858 = 0.03447 0.00026 0.00548 0.02229 AFIX 123 H69A 2 0.591536 0.145324 0.855185 20.50000 -1.50000 H69B 2 0.638597 0.163621 0.768448 20.50000 -1.50000 H69C 2 0.613761 0.124507 0.737010 20.50000 -1.50000 H69D 2 0.637727 0.143644 0.718577 20.50000 -1.50000 H69E 2 0.590666 0.125347 0.805314 20.50000 -1.50000 H69F 2 0.615501 0.164461 0.836752 20.50000 -1.50000 AFIX 0 PART 2 C66A 1 0.646046 0.151098 0.395546 -21.00000 0.04736 0.05379 = 0.05086 -0.02003 -0.00135 0.00025 AFIX 23 H66C 2 0.650692 0.124983 0.410581 -21.00000 -1.20000 H66D 2 0.635895 0.154583 0.309143 -21.00000 -1.20000 AFIX 0 C67A 1 0.701839 0.170635 0.424453 -21.00000 0.10075 0.06321 = 0.11807 -0.03956 0.04758 -0.03541 AFIX 123 H67G 2 0.732929 0.161322 0.372841 -20.50000 -1.50000 H67H 2 0.711844 0.166779 0.509808 -20.50000 -1.50000 H67I 2 0.696858 0.196451 0.409419 -20.50000 -1.50000 H67J 2 0.694825 0.188379 0.488538 -20.50000 -1.50000 H67K 2 0.715910 0.182922 0.351570 -20.50000 -1.50000 H67L 2 0.730896 0.153250 0.451960 -20.50000 -1.50000 AFIX 0 C68A 1 0.589726 0.148225 0.661589 -21.00000 0.04920 0.07487 = 0.04179 0.00172 -0.01672 0.00011 AFIX 23 H68C 2 0.574969 0.123343 0.652819 -21.00000 -1.20000 H68D 2 0.632062 0.146712 0.674063 -21.00000 -1.20000 AFIX 0 C69A 1 0.562205 0.165147 0.775419 -21.00000 0.07775 0.09858 = 0.03447 0.00026 0.00548 0.02229 AFIX 123 H69G 2 0.571623 0.150463 0.846544 -20.50000 -1.50000 H69H 2 0.520123 0.166184 0.765333 -20.50000 -1.50000 H69I 2 0.577373 0.189551 0.786745 -20.50000 -1.50000 H69J 2 0.541123 0.187002 0.752537 -20.50000 -1.50000 H69K 2 0.592623 0.171281 0.833748 -20.50000 -1.50000 H69L 2 0.535373 0.147914 0.812336 -20.50000 -1.50000 AFIX 0 PART 0 AL2 3 0.154344 0.033726 0.287546 11.00000 0.03392 0.03278 = 0.08611 0.00996 0.00934 -0.00618 C70 1 0.093451 0.066778 0.347277 11.00000 0.03425 0.04191 = 0.08484 0.01238 -0.00062 -0.01053 AFIX 23 H70A 2 0.108915 0.081374 0.415019 11.00000 -1.20000 H70B 2 0.081897 0.083385 0.281388 11.00000 -1.20000 AFIX 0 C71 1 0.039824 0.045334 0.391253 11.00000 0.04463 0.04921 = 0.10704 -0.00451 0.02886 -0.00998 AFIX 3 H71A 2 0.010384 0.062114 0.421133 10.50000 -1.20000 H71B 2 0.051214 0.028974 0.456733 10.50000 -1.20000 H71C 2 0.023984 0.031364 0.323583 10.50000 -1.20000 H71D 2 0.046674 0.019514 0.379843 10.50000 -1.20000 H71E 2 0.005844 0.052654 0.344233 10.50000 -1.20000 H71F 2 0.033074 0.050264 0.477383 10.50000 -1.20000 AFIX 0 C72 1 0.120141 0.007403 0.141955 11.00000 0.05464 0.05742 = 0.16617 -0.04704 0.02167 -0.01017 AFIX 23 H72A 2 0.077777 0.011273 0.142902 11.00000 -1.20000 H72B 2 0.135261 0.019029 0.067668 11.00000 -1.20000 AFIX 0 C73 1 0.130528 -0.031417 0.131432 11.00000 0.07054 0.07877 = 0.19606 0.01886 0.03318 -0.00761 AFIX 3 H73A 2 0.111788 -0.040487 0.057831 10.50000 -1.20000 H73B 2 0.114488 -0.043767 0.202382 10.50000 -1.20000 H73C 2 0.172238 -0.035947 0.126841 10.50000 -1.20000 H73D 2 0.153888 -0.039647 0.200201 10.50000 -1.20000 H73E 2 0.151178 -0.036367 0.055651 10.50000 -1.20000 H73F 2 0.093438 -0.044187 0.131202 10.50000 -1.20000 AFIX 0 C74 1 0.178862 -0.002710 0.406532 11.00000 0.06801 0.06598 = 0.15107 0.05585 0.03122 0.01083 AFIX 23 H74A 2 0.147581 -0.020726 0.415228 11.00000 -1.20000 H74B 2 0.213309 -0.015346 0.374411 11.00000 -1.20000 AFIX 0 PART 3 C75 1 0.192724 0.011522 0.525885 31.00000 0.08603 0.06989 = 0.10008 -0.01860 0.00216 0.01239 AFIX 123 H75A 2 0.203425 -0.008318 0.579978 30.50000 -1.50000 H75B 2 0.158930 0.024082 0.558862 30.50000 -1.50000 H75C 2 0.225157 0.028393 0.519237 30.50000 -1.50000 H75D 2 0.188250 0.037756 0.525406 30.50000 -1.50000 H75E 2 0.232745 0.005356 0.546523 30.50000 -1.50000 H75F 2 0.166517 0.001044 0.586148 30.50000 -1.50000 AFIX 0 PART 4 C75A 1 0.151668 -0.000034 0.538830 -31.00000 0.08603 0.06989 = 0.10008 -0.01860 0.00216 0.01239 AFIX 123 H75G 2 0.161815 -0.021623 0.585256 -30.50000 -1.50000 H75H 2 0.109493 0.001857 0.532620 -30.50000 -1.50000 H75I 2 0.166959 0.021311 0.580052 -30.50000 -1.50000 H75J 2 0.130363 0.022653 0.546696 -30.50000 -1.50000 H75K 2 0.182685 -0.000827 0.599332 -30.50000 -1.50000 H75L 2 0.125219 -0.020281 0.551900 -30.50000 -1.50000 AFIX 0 PART 0 K101 5 0.410593 0.366687 0.882144 11.00000 0.03388 0.04031 = 0.07054 0.00403 -0.00484 0.00245 N101 6 0.487798 0.363377 0.658265 11.00000 0.04345 0.04902 = 0.06961 -0.00445 0.00030 0.00307 N102 6 0.333541 0.370038 1.105534 11.00000 0.03658 0.09942 = 0.05652 0.00798 0.01147 0.00943 O101 7 0.503801 0.415020 0.857982 11.00000 0.04337 0.04432 = 0.06799 -0.00254 -0.00218 -0.00113 O102 7 0.423756 0.422491 1.050370 11.00000 0.05033 0.07198 = 0.08256 -0.01919 -0.00572 0.00667 O103 7 0.466390 0.301788 0.813257 11.00000 0.05548 0.04268 = 0.06776 0.00169 -0.01552 0.00985 O104 7 0.408185 0.307931 1.040160 11.00000 0.05022 0.05154 = 0.07919 0.01706 -0.00354 -0.00414 O105 7 0.362562 0.376110 0.653513 11.00000 0.03881 0.05193 = 0.08488 0.01100 -0.00423 0.00322 O106 7 0.289028 0.369066 0.856829 11.00000 0.03594 0.06761 = 0.09494 0.02911 -0.00221 0.01099 C101 1 0.539863 0.385772 0.680143 11.00000 0.04766 0.07329 = 0.07085 -0.00216 0.00930 -0.00659 AFIX 23 H10A 2 0.559228 0.390584 0.601748 11.00000 -1.20000 H10B 2 0.567230 0.372176 0.731807 11.00000 -1.20000 AFIX 0 C102 1 0.525845 0.421237 0.740866 11.00000 0.05274 0.05924 = 0.07829 -0.00800 0.00315 -0.01653 AFIX 23 H10C 2 0.561235 0.436159 0.746181 11.00000 -1.20000 H10D 2 0.496925 0.434493 0.691996 11.00000 -1.20000 AFIX 0 C103 1 0.494150 0.448106 0.918661 11.00000 0.05427 0.04684 = 0.09992 -0.01491 -0.00988 -0.00418 AFIX 23 H10E 2 0.462511 0.461489 0.878331 11.00000 -1.20000 H10F 2 0.529569 0.463055 0.915505 11.00000 -1.20000 AFIX 0 C104 1 0.478714 0.440850 1.044460 11.00000 0.05308 0.07612 = 0.09099 -0.03285 -0.01363 0.00532 AFIX 23 H10G 2 0.508981 0.425769 1.082560 11.00000 -1.20000 H10H 2 0.476365 0.463795 1.089854 11.00000 -1.20000 AFIX 0 C105 1 0.404057 0.416809 1.168279 11.00000 0.07250 0.10412 = 0.09745 -0.01609 0.00150 0.01316 AFIX 23 H10I 2 0.407786 0.439369 1.215424 11.00000 -1.20000 H10J 2 0.428194 0.398204 1.207904 11.00000 -1.20000 AFIX 0 C106 1 0.341333 0.404767 1.168097 11.00000 0.07125 0.11091 = 0.09127 -0.00145 0.01881 0.01403 AFIX 23 H10K 2 0.327655 0.402516 1.252811 11.00000 -1.20000 H10L 2 0.317433 0.423307 1.127503 11.00000 -1.20000 AFIX 0 C107 1 0.506393 0.326530 0.630750 11.00000 0.05897 0.06180 = 0.07248 -0.01013 -0.00025 0.00734 AFIX 23 H10M 2 0.541906 0.327371 0.580677 11.00000 -1.20000 H10N 2 0.475919 0.314323 0.582940 11.00000 -1.20000 AFIX 0 C108 1 0.518146 0.305232 0.743447 11.00000 0.05770 0.05516 = 0.08987 -0.01638 -0.00914 0.01553 AFIX 23 H10O 2 0.532704 0.281045 0.721321 11.00000 -1.20000 H10P 2 0.548229 0.317462 0.792267 11.00000 -1.20000 AFIX 0 C109 1 0.472854 0.276716 0.911171 11.00000 0.09684 0.03951 = 0.08290 -0.00232 -0.03812 0.01886 AFIX 23 H10Q 2 0.504040 0.284773 0.966368 11.00000 -1.20000 H10R 2 0.483234 0.252670 0.879164 11.00000 -1.20000 AFIX 0 C110 1 0.417198 0.274769 0.977637 11.00000 0.08632 0.04099 = 0.08912 0.01354 -0.02569 -0.01276 AFIX 23 H11G 2 0.385115 0.270460 0.919992 11.00000 -1.20000 H11H 2 0.418160 0.254606 1.036295 11.00000 -1.20000 AFIX 0 C111 1 0.359539 0.305610 1.121600 11.00000 0.04529 0.09215 = 0.10235 0.04756 -0.01151 -0.01297 AFIX 23 H11I 2 0.324163 0.299201 1.075865 11.00000 -1.20000 H11J 2 0.366580 0.286711 1.183141 11.00000 -1.20000 AFIX 0 C112 1 0.352008 0.339969 1.180055 11.00000 0.04594 0.13060 = 0.07457 0.03155 0.01876 0.00649 AFIX 23 H11K 2 0.389197 0.346593 1.218557 11.00000 -1.20000 H11L 2 0.323330 0.336899 1.245902 11.00000 -1.20000 AFIX 0 C113 1 0.455187 0.377828 0.557122 11.00000 0.06057 0.06571 = 0.05902 0.00600 0.00721 -0.00024 AFIX 23 H11M 2 0.475444 0.371651 0.480830 11.00000 -1.20000 H11N 2 0.454344 0.404400 0.563793 11.00000 -1.20000 AFIX 0 C114 1 0.393696 0.364065 0.550037 11.00000 0.06151 0.07097 = 0.07104 -0.00038 -0.01136 0.00251 AFIX 23 H11O 2 0.374948 0.373123 0.475331 11.00000 -1.20000 H11P 2 0.393689 0.337427 0.547233 11.00000 -1.20000 AFIX 0 C115 1 0.303121 0.366996 0.645215 11.00000 0.04632 0.08043 = 0.08803 0.01493 -0.01461 -0.00408 AFIX 23 H11Q 2 0.298375 0.340550 0.650133 11.00000 -1.20000 H11R 2 0.287296 0.375248 0.566581 11.00000 -1.20000 AFIX 0 C116 1 0.271574 0.384560 0.746322 11.00000 0.04067 0.07841 = 0.10162 0.03782 -0.00678 0.00854 AFIX 23 H11S 2 0.280007 0.410688 0.746889 11.00000 -1.20000 H11T 2 0.229392 0.381337 0.735337 11.00000 -1.20000 AFIX 0 C117 1 0.258068 0.385343 0.955878 11.00000 0.04003 0.09279 = 0.09739 0.00698 0.00523 0.01863 AFIX 23 H11U 2 0.215907 0.384254 0.940610 11.00000 -1.20000 H11V 2 0.269403 0.410919 0.964373 11.00000 -1.20000 AFIX 0 C118 1 0.272577 0.365216 1.068538 11.00000 0.03334 0.14099 = 0.10509 0.03796 0.01373 0.01975 AFIX 23 H11W 2 0.247036 0.373515 1.134937 11.00000 -1.20000 H11X 2 0.265015 0.339276 1.055388 11.00000 -1.20000 HKLF 4 1.0 0.00 0.00 -1.00 0.00 -1.00 0.00 -1.00 0.00 0.00 REM RM052 in Pmc2(1) New: Pna21 REM R1 = 0.0706 for 12935 Fo > 4sig(Fo) and 0.0830 for all 15442 data REM 1000 parameters refined using 15 restraints END WGHT 0.0036 20.8943 REM Highest difference peak 0.461, deepest hole -0.458, 1-sigma level 0.061 Q1 1 0.1411 -0.0106 0.2165 11.00000 0.05 0.46 Q2 1 0.3359 0.3447 1.2732 11.00000 0.05 0.32 Q3 1 0.0968 -0.0058 0.0714 11.00000 0.05 0.30 Q4 1 0.1343 0.0111 0.5742 11.00000 0.05 0.30 Q5 1 0.4226 0.1300 0.4784 11.00000 0.05 0.29 Q6 1 0.4088 -0.0170 0.3734 11.00000 0.05 0.27 Q7 1 0.3612 0.1983 0.7387 11.00000 0.05 0.25 Q8 1 0.7473 0.2122 0.3059 11.00000 0.05 0.25 Q9 1 0.2028 0.0494 0.2547 11.00000 0.05 0.25 Q10 1 0.3878 0.1569 -0.1247 11.00000 0.05 0.25 Q11 1 0.5602 0.0206 0.1759 11.00000 0.05 0.24 Q12 1 0.1674 0.2272 -0.1341 11.00000 0.05 0.24 Q13 1 0.4742 0.3383 0.3633 11.00000 0.05 0.23 Q14 1 0.2868 0.3387 1.0271 11.00000 0.05 0.23 Q15 1 0.3158 0.3677 1.2471 11.00000 0.05 0.23 Q16 1 0.3396 0.1314 0.1950 11.00000 0.05 0.23 Q17 1 0.4957 0.0724 0.0313 11.00000 0.05 0.23 Q18 1 0.5120 0.0953 0.6894 11.00000 0.05 0.23 Q19 1 0.5838 0.2333 0.7207 11.00000 0.05 0.23 Q20 1 0.2935 0.0952 0.7189 11.00000 0.05 0.23 ; _database_code_depnum_ccdc_archive 'CCDC 962252' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pbca _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Fe(aIPr-H)(O6C10H20K)]2 ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C74 H110 Fe2 K2 N4 O12' _chemical_formula_sum 'C74 H110 Fe2 K2 N4 O12' _chemical_formula_weight 1437.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' 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' '-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 23.4906(7) _cell_length_b 20.2128(7) _cell_length_c 33.1958(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15761.7(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8599 _cell_measurement_theta_min 3.1741 _cell_measurement_theta_max 76.9911 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6144 _exptl_absorpt_coefficient_mu 4.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3970 _exptl_absorpt_correction_T_max 0.7219 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 10.4102 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 48423 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 66.50 _reflns_number_total 13877 _reflns_number_gt 7857 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^ > 2\s(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^)+(0.1057P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 13877 _refine_ls_number_parameters 899 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1338 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1787 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.006 _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 0.53522(3) 0.30438(4) 0.16126(2) 0.0473(2) Uani 1 1 d . D . Fe2 Fe 0.49925(3) 0.24012(4) 0.08103(2) 0.0489(2) Uani 1 1 d . D . C1 C 0.4303(2) 0.4347(3) 0.23504(13) 0.0478(11) Uani 1 1 d . . . N1 N 0.40434(16) 0.4353(2) 0.19823(11) 0.0461(9) Uani 1 1 d . . . C2 C 0.4342(2) 0.3981(3) 0.16968(14) 0.0513(12) Uani 1 1 d . . . H2 H 0.4235 0.3926 0.1423 0.062 Uiso 1 1 calc R . . C3 C 0.4807(2) 0.3714(2) 0.18719(13) 0.0466(11) Uani 1 1 d . . . N2 N 0.47620(16) 0.3954(2) 0.22714(11) 0.0466(9) Uani 1 1 d . . . C4 C 0.3503(2) 0.4658(3) 0.18954(14) 0.0544(13) Uani 1 1 d . . . C5 C 0.3025(2) 0.4249(4) 0.18523(17) 0.0705(17) Uani 1 1 d . . . C6 C 0.2527(3) 0.4518(5) 0.1734(2) 0.103(3) Uani 1 1 d . . . H6 H 0.2208 0.4238 0.1693 0.124 Uiso 1 1 calc R . . C7 C 0.2471(3) 0.5181(5) 0.1673(3) 0.112(3) Uani 1 1 d . . . H7 H 0.2115 0.5355 0.1589 0.135 Uiso 1 1 calc R . . C8 C 0.2932(3) 0.5608(4) 0.17322(19) 0.091(2) Uani 1 1 d . . . H8 H 0.2887 0.6073 0.1705 0.109 Uiso 1 1 calc R . . C9 C 0.3467(3) 0.5332(3) 0.18327(16) 0.0650(15) Uani 1 1 d . B . C10 C 0.3051(3) 0.3523(4) 0.1959(2) 0.0805(19) Uani 1 1 d . . . H10 H 0.3451 0.3373 0.1911 0.097 Uiso 1 1 calc R . . C11 C 0.2931(3) 0.3440(4) 0.2407(2) 0.098(2) Uani 1 1 d . . . H11A H 0.3190 0.3723 0.2562 0.147 Uiso 0.50 1 calc PR . . H11B H 0.2990 0.2977 0.2484 0.147 Uiso 0.50 1 calc PR . . H11C H 0.2537 0.3568 0.2464 0.147 Uiso 0.50 1 calc PR . . H11D H 0.2621 0.3122 0.2445 0.147 Uiso 0.50 1 calc PR . . H11E H 0.2821 0.3868 0.2522 0.147 Uiso 0.50 1 calc PR . . H11F H 0.3275 0.3278 0.2543 0.147 Uiso 0.50 1 calc PR . . C12 C 0.2670(3) 0.3093(5) 0.1704(2) 0.111(3) Uani 1 1 d . . . H12A H 0.2764 0.3155 0.1419 0.166 Uiso 0.50 1 calc PR . . H12B H 0.2272 0.3216 0.1749 0.166 Uiso 0.50 1 calc PR . . H12C H 0.2725 0.2628 0.1777 0.166 Uiso 0.50 1 calc PR . . H12D H 0.2410 0.2844 0.1878 0.166 Uiso 0.50 1 calc PR . . H12E H 0.2903 0.2783 0.1547 0.166 Uiso 0.50 1 calc PR . . H12F H 0.2449 0.3372 0.1520 0.166 Uiso 0.50 1 calc PR . . C13 C 0.3986(3) 0.5758(3) 0.18779(17) 0.0776(19) Uani 1 1 d . . . H13 H 0.4205 0.5602 0.2118 0.093 Uiso 1 1 calc R A 1 C14 C 0.3796(5) 0.6488(4) 0.1955(3) 0.081(3) Uani 0.728(13) 1 d P B 1 H14A H 0.3566 0.6508 0.2201 0.122 Uiso 0.364(7) 1 calc PR B 1 H14B H 0.3570 0.6645 0.1726 0.122 Uiso 0.364(7) 1 calc PR B 1 H14C H 0.4134 0.6769 0.1987 0.122 Uiso 0.364(7) 1 calc PR B 1 H14D H 0.3947 0.6773 0.1742 0.122 Uiso 0.364(7) 1 calc PR B 1 H14E H 0.3943 0.6636 0.2216 0.122 Uiso 0.364(7) 1 calc PR B 1 H14F H 0.3380 0.6513 0.1956 0.122 Uiso 0.364(7) 1 calc PR B 1 C15 C 0.4359(4) 0.5706(5) 0.1520(3) 0.074(3) Uani 0.728(13) 1 d P B 1 H15A H 0.4696 0.5985 0.1558 0.111 Uiso 0.364(7) 1 calc PR B 1 H15B H 0.4151 0.5854 0.1281 0.111 Uiso 0.364(7) 1 calc PR B 1 H15C H 0.4477 0.5245 0.1484 0.111 Uiso 0.364(7) 1 calc PR B 1 H15D H 0.4187 0.5405 0.1324 0.111 Uiso 0.364(7) 1 calc PR B 1 H15E H 0.4732 0.5535 0.1601 0.111 Uiso 0.364(7) 1 calc PR B 1 H15F H 0.4405 0.6144 0.1398 0.111 Uiso 0.364(7) 1 calc PR B 1 C14A C 0.4329(16) 0.598(3) 0.2323(12) 0.26(4) Uani 0.272(13) 1 d P B 2 H14G H 0.4671 0.6234 0.2260 0.384 Uiso 0.136(7) 1 calc PR B 2 H14H H 0.4438 0.5574 0.2469 0.384 Uiso 0.136(7) 1 calc PR B 2 H14I H 0.4073 0.6242 0.2489 0.384 Uiso 0.136(7) 1 calc PR B 2 H14J H 0.4117 0.5800 0.2553 0.384 Uiso 0.136(7) 1 calc PR B 2 H14K H 0.4350 0.6459 0.2343 0.384 Uiso 0.136(7) 1 calc PR B 2 H14L H 0.4715 0.5792 0.2323 0.384 Uiso 0.136(7) 1 calc PR B 2 C15A C 0.435(3) 0.618(4) 0.1538(14) 0.28(5) Uani 0.272(13) 1 d P B 2 H15G H 0.4645 0.6433 0.1671 0.421 Uiso 0.136(7) 1 calc PR B 2 H15H H 0.4088 0.6474 0.1394 0.421 Uiso 0.136(7) 1 calc PR B 2 H15I H 0.4519 0.5867 0.1346 0.421 Uiso 0.136(7) 1 calc PR B 2 H15J H 0.4190 0.6083 0.1270 0.421 Uiso 0.136(7) 1 calc PR B 2 H15K H 0.4747 0.6042 0.1546 0.421 Uiso 0.136(7) 1 calc PR B 2 H15L H 0.4315 0.6650 0.1595 0.421 Uiso 0.136(7) 1 calc PR B 2 C16 C 0.5173(2) 0.3797(2) 0.25769(14) 0.0466(11) Uani 1 1 d . C . C17 C 0.5685(2) 0.4155(3) 0.25873(14) 0.0540(13) Uani 1 1 d . . . C18 C 0.6074(2) 0.3998(3) 0.28930(17) 0.0643(15) Uani 1 1 d . C . H18 H 0.6422 0.4237 0.2909 0.077 Uiso 1 1 calc R . . C19 C 0.5968(2) 0.3503(3) 0.31721(16) 0.0642(15) Uani 1 1 d . . . H19 H 0.6236 0.3409 0.3378 0.077 Uiso 1 1 calc R C . C20 C 0.5467(3) 0.3151(3) 0.31462(17) 0.0659(15) Uani 1 1 d . C . H20 H 0.5394 0.2811 0.3337 0.079 Uiso 1 1 calc R . . C21 C 0.5061(2) 0.3281(3) 0.28435(15) 0.0541(12) Uani 1 1 d . . . C22 C 0.5804(2) 0.4706(3) 0.22902(17) 0.0643(15) Uani 0.74(2) 1 d P C 3 H22 H 0.5608 0.4576 0.2035 0.077 Uiso 0.74(2) 1 calc PR C 3 C23 C 0.5543(5) 0.5350(4) 0.2415(3) 0.074(4) Uani 0.74(2) 1 d P C 3 H23A H 0.5629 0.5689 0.2213 0.111 Uiso 0.371(11) 1 calc PR C 3 H23B H 0.5698 0.5485 0.2676 0.111 Uiso 0.371(11) 1 calc PR C 3 H23C H 0.5129 0.5297 0.2437 0.111 Uiso 0.371(11) 1 calc PR C 3 H23D H 0.5342 0.5292 0.2671 0.111 Uiso 0.371(11) 1 calc PR C 3 H23E H 0.5273 0.5496 0.2208 0.111 Uiso 0.371(11) 1 calc PR C 3 H23F H 0.5842 0.5683 0.2447 0.111 Uiso 0.371(11) 1 calc PR C 3 C24 C 0.6426(5) 0.4766(6) 0.2186(4) 0.076(3) Uani 0.74(2) 1 d P C 3 H24A H 0.6576 0.4330 0.2114 0.115 Uiso 0.371(11) 1 calc PR C 3 H24B H 0.6635 0.4940 0.2418 0.115 Uiso 0.371(11) 1 calc PR C 3 H24C H 0.6471 0.5068 0.1957 0.115 Uiso 0.371(11) 1 calc PR C 3 H24D H 0.6545 0.5229 0.2212 0.115 Uiso 0.371(11) 1 calc PR C 3 H24E H 0.6486 0.4618 0.1908 0.115 Uiso 0.371(11) 1 calc PR C 3 H24F H 0.6650 0.4490 0.2369 0.115 Uiso 0.371(11) 1 calc PR C 3 C22A C 0.5804(2) 0.4706(3) 0.22902(17) 0.0643(15) Uani 0.26(2) 1 d P C 4 H22A H 0.5460 0.4767 0.2116 0.077 Uiso 0.26(2) 1 calc PR C 4 C23A C 0.5904(17) 0.5378(13) 0.2545(10) 0.100(13) Uani 0.26(2) 1 d P C 4 H23G H 0.5976 0.5746 0.2359 0.150 Uiso 0.129(11) 1 calc PR C 4 H23H H 0.6233 0.5322 0.2723 0.150 Uiso 0.129(11) 1 calc PR C 4 H23I H 0.5564 0.5474 0.2706 0.150 Uiso 0.129(11) 1 calc PR C 4 H23J H 0.5873 0.5282 0.2833 0.150 Uiso 0.129(11) 1 calc PR C 4 H23K H 0.5616 0.5706 0.2469 0.150 Uiso 0.129(11) 1 calc PR C 4 H23L H 0.6284 0.5554 0.2486 0.150 Uiso 0.129(11) 1 calc PR C 4 C24A C 0.6353(17) 0.471(4) 0.2010(12) 0.23(4) Uani 0.26(2) 1 d P C 4 H24G H 0.6343 0.5102 0.1834 0.348 Uiso 0.129(11) 1 calc PR C 4 H24H H 0.6360 0.4310 0.1845 0.348 Uiso 0.129(11) 1 calc PR C 4 H24I H 0.6696 0.4728 0.2178 0.348 Uiso 0.129(11) 1 calc PR C 4 H24J H 0.6589 0.4325 0.2070 0.348 Uiso 0.129(11) 1 calc PR C 4 H24K H 0.6573 0.5116 0.2060 0.348 Uiso 0.129(11) 1 calc PR C 4 H24L H 0.6236 0.4699 0.1727 0.348 Uiso 0.129(11) 1 calc PR C 4 C25 C 0.4521(3) 0.2875(3) 0.2814(2) 0.0786(19) Uani 0.750(9) 1 d P C 5 H25 H 0.4336 0.3007 0.2555 0.094 Uiso 0.750(9) 1 calc PR C 5 C26 C 0.4114(4) 0.2991(6) 0.3118(3) 0.092(3) Uani 0.750(9) 1 d P C 5 H26A H 0.3782 0.2708 0.3072 0.138 Uiso 0.375(4) 1 calc PR C 5 H26B H 0.3997 0.3456 0.3110 0.138 Uiso 0.375(4) 1 calc PR C 5 H26C H 0.4280 0.2891 0.3381 0.138 Uiso 0.375(4) 1 calc PR C 5 H26D H 0.4257 0.3329 0.3304 0.138 Uiso 0.375(4) 1 calc PR C 5 H26E H 0.4042 0.2580 0.3266 0.138 Uiso 0.375(4) 1 calc PR C 5 H26F H 0.3759 0.3146 0.2995 0.138 Uiso 0.375(4) 1 calc PR C 5 C27 C 0.4660(5) 0.2118(4) 0.2772(3) 0.092(3) Uani 0.750(9) 1 d P C 5 H27A H 0.4949 0.2055 0.2562 0.139 Uiso 0.375(4) 1 calc PR C 5 H27B H 0.4313 0.1877 0.2698 0.139 Uiso 0.375(4) 1 calc PR C 5 H27C H 0.4804 0.1949 0.3029 0.139 Uiso 0.375(4) 1 calc PR C 5 H27D H 0.4429 0.1866 0.2964 0.139 Uiso 0.375(4) 1 calc PR C 5 H27E H 0.5064 0.2043 0.2828 0.139 Uiso 0.375(4) 1 calc PR C 5 H27F H 0.4573 0.1972 0.2497 0.139 Uiso 0.375(4) 1 calc PR C 5 C25A C 0.4521(3) 0.2875(3) 0.2814(2) 0.0786(19) Uani 0.250(9) 1 d P C 6 H25A H 0.4238 0.3231 0.2756 0.094 Uiso 0.250(9) 1 calc PR C 6 C26A C 0.4361(13) 0.2710(18) 0.3334(9) 0.092(3) Uani 0.250(9) 1 d P C 6 H26G H 0.4521 0.3061 0.3503 0.138 Uiso 0.125(4) 1 calc PR C 6 H26H H 0.4527 0.2284 0.3412 0.138 Uiso 0.125(4) 1 calc PR C 6 H26I H 0.3947 0.2694 0.3371 0.138 Uiso 0.125(4) 1 calc PR C 6 H26J H 0.4142 0.2298 0.3354 0.138 Uiso 0.125(4) 1 calc PR C 6 H26K H 0.4136 0.3075 0.3445 0.138 Uiso 0.125(4) 1 calc PR C 6 H26L H 0.4716 0.2666 0.3487 0.138 Uiso 0.125(4) 1 calc PR C 6 C27A C 0.4373(15) 0.2484(14) 0.2602(10) 0.092(3) Uani 0.250(9) 1 d P C 6 H27G H 0.4000 0.2321 0.2689 0.139 Uiso 0.125(4) 1 calc PR C 6 H27H H 0.4646 0.2117 0.2602 0.139 Uiso 0.125(4) 1 calc PR C 6 H27I H 0.4344 0.2669 0.2330 0.139 Uiso 0.125(4) 1 calc PR C 6 H27J H 0.4660 0.2417 0.2392 0.139 Uiso 0.125(4) 1 calc PR C 6 H27K H 0.4013 0.2621 0.2479 0.139 Uiso 0.125(4) 1 calc PR C 6 H27L H 0.4316 0.2069 0.2750 0.139 Uiso 0.125(4) 1 calc PR C 6 C28 C 0.35114(19) 0.2720(2) 0.00516(14) 0.0459(11) Uani 1 1 d . . . N3 N 0.33446(15) 0.29861(19) 0.04091(11) 0.0423(9) Uani 1 1 d . . . C29 C 0.37674(19) 0.2916(2) 0.07039(14) 0.0459(11) Uani 1 1 d . . . H29 H 0.3739 0.3067 0.0974 0.055 Uiso 1 1 calc R . . C30 C 0.42209(18) 0.2599(2) 0.05444(14) 0.0443(11) Uani 1 1 d . . . N4 N 0.40416(16) 0.24912(19) 0.01451(11) 0.0434(9) Uani 1 1 d . . . C31 C 0.2816(2) 0.3324(3) 0.04773(14) 0.0482(11) Uani 1 1 d . . . C32 C 0.2322(2) 0.2957(3) 0.05384(17) 0.0608(14) Uani 1 1 d . . . C33 C 0.1823(2) 0.3308(4) 0.0625(2) 0.0807(19) Uani 1 1 d . . . H33 H 0.1477 0.3072 0.0665 0.097 Uiso 1 1 calc R . . C34 C 0.1821(3) 0.3980(4) 0.0652(2) 0.089(2) Uani 1 1 d . . . H34 H 0.1478 0.4207 0.0715 0.107 Uiso 1 1 calc R . . C35 C 0.2306(3) 0.4326(3) 0.0591(2) 0.0802(19) Uani 1 1 d . . . H35 H 0.2297 0.4794 0.0611 0.096 Uiso 1 1 calc R . . C36 C 0.2823(2) 0.4013(3) 0.04984(16) 0.0585(13) Uani 1 1 d . . . C37 C 0.2320(3) 0.2206(3) 0.05054(19) 0.0724(17) Uani 1 1 d . . . H37 H 0.2724 0.2052 0.0488 0.087 Uiso 1 1 calc R . . C38 C 0.2020(3) 0.1997(4) 0.0130(2) 0.098(2) Uani 1 1 d . . . H38A H 0.2022 0.1513 0.0112 0.147 Uiso 0.50 1 calc PR . . H38B H 0.2214 0.2185 -0.0104 0.147 Uiso 0.50 1 calc PR . . H38C H 0.1626 0.2156 0.0138 0.147 Uiso 0.50 1 calc PR . . H38D H 0.1886 0.2389 -0.0015 0.147 Uiso 0.50 1 calc PR . . H38E H 0.1694 0.1718 0.0201 0.147 Uiso 0.50 1 calc PR . . H38F H 0.2282 0.1747 -0.0041 0.147 Uiso 0.50 1 calc PR . . C39 C 0.2049(5) 0.1893(5) 0.0876(3) 0.156(5) Uani 1 1 d . . . H39A H 0.2258 0.2032 0.1118 0.234 Uiso 0.50 1 calc PR . . H39B H 0.2065 0.1410 0.0852 0.234 Uiso 0.50 1 calc PR . . H39C H 0.1652 0.2035 0.0897 0.234 Uiso 0.50 1 calc PR . . H39D H 0.1725 0.1619 0.0794 0.234 Uiso 0.50 1 calc PR . . H39E H 0.1918 0.2241 0.1059 0.234 Uiso 0.50 1 calc PR . . H39F H 0.2331 0.1616 0.1014 0.234 Uiso 0.50 1 calc PR . . C40 C 0.3355(3) 0.4404(3) 0.04145(17) 0.0679(16) Uani 1 1 d . . . H40 H 0.3680 0.4085 0.0409 0.082 Uiso 1 1 calc R . . C41 C 0.3333(4) 0.4743(5) 0.0008(2) 0.142(4) Uani 1 1 d . . . H41A H 0.3687 0.4990 -0.0036 0.213 Uiso 0.50 1 calc PR . . H41B H 0.3010 0.5049 0.0000 0.213 Uiso 0.50 1 calc PR . . H41C H 0.3289 0.4410 -0.0205 0.213 Uiso 0.50 1 calc PR . . H41D H 0.2970 0.4643 -0.0124 0.213 Uiso 0.50 1 calc PR . . H41E H 0.3648 0.4583 -0.0160 0.213 Uiso 0.50 1 calc PR . . H41F H 0.3369 0.5222 0.0045 0.213 Uiso 0.50 1 calc PR . . C42 C 0.3486(4) 0.4917(4) 0.0730(2) 0.112(3) Uani 1 1 d . . . H42A H 0.3838 0.5148 0.0658 0.168 Uiso 0.50 1 calc PR . . H42B H 0.3532 0.4701 0.0992 0.168 Uiso 0.50 1 calc PR . . H42C H 0.3172 0.5236 0.0744 0.168 Uiso 0.50 1 calc PR . . H42D H 0.3190 0.4909 0.0938 0.168 Uiso 0.50 1 calc PR . . H42E H 0.3497 0.5356 0.0604 0.168 Uiso 0.50 1 calc PR . . H42F H 0.3856 0.4821 0.0852 0.168 Uiso 0.50 1 calc PR . . C43 C 0.4398(2) 0.2165(3) -0.01497(14) 0.0514(12) Uani 1 1 d . . . C44 C 0.4753(2) 0.2550(3) -0.03936(16) 0.0599(14) Uani 1 1 d . . . C45 C 0.5085(3) 0.2221(4) -0.06769(19) 0.0784(19) Uani 1 1 d . . . H45 H 0.5331 0.2468 -0.0848 0.094 Uiso 1 1 calc R . . C46 C 0.5063(3) 0.1551(4) -0.07128(18) 0.082(2) Uani 1 1 d . . . H46 H 0.5286 0.1339 -0.0913 0.099 Uiso 1 1 calc R . . C47 C 0.4728(3) 0.1179(3) -0.04675(17) 0.0730(17) Uani 1 1 d . . . H47 H 0.4727 0.0711 -0.0496 0.088 Uiso 1 1 calc R . . C48 C 0.4388(2) 0.1474(3) -0.01749(16) 0.0595(14) Uani 1 1 d . . . C49 C 0.4779(2) 0.3289(3) -0.03471(19) 0.0714(17) Uani 1 1 d . . . H49 H 0.4604 0.3404 -0.0082 0.086 Uiso 1 1 calc R . . C50 C 0.4423(3) 0.3612(4) -0.0676(3) 0.115(3) Uani 1 1 d . . . H50A H 0.4436 0.4094 -0.0644 0.173 Uiso 0.50 1 calc PR . . H50B H 0.4028 0.3460 -0.0654 0.173 Uiso 0.50 1 calc PR . . H50C H 0.4576 0.3491 -0.0941 0.173 Uiso 0.50 1 calc PR . . H50D H 0.4257 0.3269 -0.0848 0.173 Uiso 0.50 1 calc PR . . H50E H 0.4665 0.3903 -0.0839 0.173 Uiso 0.50 1 calc PR . . H50F H 0.4117 0.3873 -0.0552 0.173 Uiso 0.50 1 calc PR . . C51 C 0.5384(3) 0.3566(4) -0.0350(2) 0.094(2) Uani 1 1 d . . . H51A H 0.5371 0.4047 -0.0317 0.140 Uiso 0.50 1 calc PR . . H51B H 0.5568 0.3458 -0.0607 0.140 Uiso 0.50 1 calc PR . . H51C H 0.5602 0.3369 -0.0129 0.140 Uiso 0.50 1 calc PR . . H51D H 0.5656 0.3203 -0.0385 0.140 Uiso 0.50 1 calc PR . . H51E H 0.5460 0.3792 -0.0094 0.140 Uiso 0.50 1 calc PR . . H51F H 0.5425 0.3880 -0.0573 0.140 Uiso 0.50 1 calc PR . . C52 C 0.4028(3) 0.1071(3) 0.01137(18) 0.0688(16) Uani 1 1 d . . . H52 H 0.3953 0.1352 0.0356 0.083 Uiso 1 1 calc R . . C53 C 0.3464(3) 0.0910(4) -0.0075(2) 0.098(2) Uani 1 1 d . . . H53A H 0.3282 0.1319 -0.0166 0.147 Uiso 0.50 1 calc PR . . H53B H 0.3220 0.0692 0.0125 0.147 Uiso 0.50 1 calc PR . . H53C H 0.3523 0.0614 -0.0305 0.147 Uiso 0.50 1 calc PR . . H53D H 0.3401 0.0431 -0.0065 0.147 Uiso 0.50 1 calc PR . . H53E H 0.3463 0.1058 -0.0356 0.147 Uiso 0.50 1 calc PR . . H53F H 0.3160 0.1136 0.0074 0.147 Uiso 0.50 1 calc PR . . C54 C 0.4302(3) 0.0437(4) 0.0257(2) 0.103(2) Uani 1 1 d . . . H54A H 0.4045 0.0210 0.0444 0.154 Uiso 0.50 1 calc PR . . H54B H 0.4660 0.0540 0.0396 0.154 Uiso 0.50 1 calc PR . . H54C H 0.4380 0.0151 0.0026 0.154 Uiso 0.50 1 calc PR . . H54D H 0.4679 0.0391 0.0133 0.154 Uiso 0.50 1 calc PR . . H54E H 0.4063 0.0060 0.0181 0.154 Uiso 0.50 1 calc PR . . H54F H 0.4343 0.0450 0.0551 0.154 Uiso 0.50 1 calc PR . . K101 K 0.58019(5) 0.13509(6) 0.14921(4) 0.0610(3) Uani 1 1 d . . . O101 O 0.48953(14) 0.22444(16) 0.14169(10) 0.0528(8) Uani 1 1 d . D . O102 O 0.47127(18) 0.08765(19) 0.15608(12) 0.0722(11) Uani 1 1 d . D . O103 O 0.5574(2) 0.0032(2) 0.12811(12) 0.0746(11) Uani 1 1 d . D . O104 O 0.66338(19) 0.0313(2) 0.16807(11) 0.0723(11) Uani 1 1 d . D . O105 O 0.66879(16) 0.1554(2) 0.20463(12) 0.0661(10) Uani 1 1 d . D . O106 O 0.60819(14) 0.26536(18) 0.17133(10) 0.0566(9) Uani 1 1 d . D . C101 C 0.4405(2) 0.1994(3) 0.15976(18) 0.0642(14) Uani 1 1 d . . . H10A H 0.4083 0.2296 0.1543 0.077 Uiso 1 1 calc R D . H10B H 0.4462 0.1976 0.1893 0.077 Uiso 1 1 calc R . . C102 C 0.4258(3) 0.1312(3) 0.1447(2) 0.0768(18) Uani 1 1 d . D . H10C H 0.3895 0.1161 0.1567 0.092 Uiso 1 1 calc R . . H10D H 0.4214 0.1317 0.1150 0.092 Uiso 1 1 calc R . . C103 C 0.4609(3) 0.0213(3) 0.1440(2) 0.0817(19) Uani 1 1 d . . . H10E H 0.4526 0.0195 0.1148 0.098 Uiso 1 1 calc R D . H10F H 0.4278 0.0032 0.1588 0.098 Uiso 1 1 calc R . . C104 C 0.5129(3) -0.0181(3) 0.15333(19) 0.0790(19) Uani 1 1 d . D . H10G H 0.5237 -0.0119 0.1819 0.095 Uiso 1 1 calc R . . H10H H 0.5053 -0.0657 0.1488 0.095 Uiso 1 1 calc R . . C105 C 0.6064(3) -0.0382(3) 0.12856(18) 0.082(2) Uani 1 1 d . . . H10I H 0.6309 -0.0265 0.1054 0.098 Uiso 1 1 calc R D . H10J H 0.5941 -0.0847 0.1249 0.098 Uiso 1 1 calc R . . C106 C 0.6408(3) -0.0337(3) 0.16593(18) 0.0784(18) Uani 1 1 d . D . H10K H 0.6166 -0.0427 0.1898 0.094 Uiso 1 1 calc R . . H10L H 0.6720 -0.0666 0.1653 0.094 Uiso 1 1 calc R . . C107 C 0.6928(3) 0.0421(3) 0.2050(2) 0.0790(18) Uani 1 1 d . . . H10M H 0.7245 0.0101 0.2076 0.095 Uiso 1 1 calc R D . H10N H 0.6666 0.0355 0.2280 0.095 Uiso 1 1 calc R . . C108 C 0.7151(3) 0.1097(3) 0.2055(2) 0.0811(19) Uani 1 1 d . D . H10O H 0.7380 0.1168 0.2302 0.097 Uiso 1 1 calc R . . H10P H 0.7400 0.1169 0.1819 0.097 Uiso 1 1 calc R . . C109 C 0.6864(2) 0.2220(3) 0.20950(18) 0.0701(16) Uani 1 1 d . . . H10Q H 0.7126 0.2344 0.1874 0.084 Uiso 1 1 calc R D . H10R H 0.7071 0.2269 0.2353 0.084 Uiso 1 1 calc R . . C110 C 0.6355(2) 0.2666(3) 0.20917(17) 0.0643(14) Uani 1 1 d . D . H11G H 0.6084 0.2523 0.2303 0.077 Uiso 1 1 calc R . . H11H H 0.6476 0.3124 0.2154 0.077 Uiso 1 1 calc R . . K201 K 0.64964(4) 0.26668(6) 0.09560(4) 0.0570(3) Uani 1 1 d . D . O201 O 0.54171(13) 0.32236(16) 0.10073(10) 0.0508(8) Uani 1 1 d . . . O202 O 0.64141(16) 0.4012(2) 0.08609(12) 0.0703(10) Uani 1 1 d . . . O203 O 0.74812(17) 0.3416(2) 0.10371(13) 0.0747(11) Uani 1 1 d . . . O204 O 0.7572(4) 0.1978(5) 0.1116(2) 0.0662(18) Uani 0.790(12) 1 d P D 7 O205 O 0.6742(2) 0.1464(3) 0.0586(2) 0.0685(19) Uani 0.790(12) 1 d P D 7 O4A O 0.7555(19) 0.206(2) 0.0984(9) 0.0662(18) Uani 0.210(12) 1 d P D 8 O5A O 0.6659(9) 0.1257(12) 0.0818(9) 0.0685(19) Uani 0.210(12) 1 d P D 8 O206 O 0.56222(16) 0.1823(2) 0.07188(11) 0.0700(11) Uani 1 1 d . D . C201 C 0.5407(2) 0.3860(3) 0.08322(16) 0.0621(14) Uani 1 1 d . D . H20A H 0.5041 0.4077 0.0898 0.074 Uiso 1 1 calc R . . H20B H 0.5430 0.3817 0.0536 0.074 Uiso 1 1 calc R . . C202 C 0.5888(3) 0.4289(3) 0.0977(2) 0.0741(17) Uani 1 1 d . D . H20C H 0.5850 0.4738 0.0860 0.089 Uiso 1 1 calc R . . H20D H 0.5873 0.4328 0.1274 0.089 Uiso 1 1 calc R . . C203 C 0.6897(3) 0.4361(3) 0.0995(2) 0.085(2) Uani 1 1 d . D . H20E H 0.6881 0.4404 0.1292 0.102 Uiso 1 1 calc R . . H20F H 0.6892 0.4812 0.0879 0.102 Uiso 1 1 calc R . . C204 C 0.7412(3) 0.4038(4) 0.0884(3) 0.099(2) Uani 1 1 d . D . H20G H 0.7428 0.4011 0.0586 0.119 Uiso 1 1 calc R . . H20H H 0.7736 0.4314 0.0973 0.119 Uiso 1 1 calc R . . C205 C 0.7978(3) 0.3057(4) 0.0962(3) 0.103(3) Uani 1 1 d . D . H20I H 0.8308 0.3329 0.1045 0.123 Uiso 1 1 calc R . . H20J H 0.8009 0.2983 0.0668 0.123 Uiso 1 1 calc R . . C206 C 0.8014(3) 0.2442(4) 0.1157(3) 0.108(3) Uani 1 1 d . . . H20K H 0.8368 0.2225 0.1065 0.130 Uiso 1 1 calc R D 7 H20L H 0.8060 0.2530 0.1449 0.130 Uiso 1 1 calc R D 7 C207 C 0.7693(3) 0.1517(3) 0.0789(2) 0.0805(19) Uani 1 1 d . . . H20M H 0.7781 0.1769 0.0541 0.097 Uiso 1 1 calc R D 7 H20N H 0.8031 0.1249 0.0859 0.097 Uiso 1 1 calc R D 7 C208 C 0.7219(3) 0.1086(4) 0.0714(3) 0.092(2) Uani 1 1 d . D . H20O H 0.7321 0.0761 0.0503 0.111 Uiso 1 1 calc R E 7 H20P H 0.7123 0.0840 0.0963 0.111 Uiso 1 1 calc R E 7 C209 C 0.6312(3) 0.1124(4) 0.04287(19) 0.084(2) Uani 1 1 d . . . H20Q H 0.6239 0.0733 0.0601 0.101 Uiso 1 1 calc R D 7 H20R H 0.6429 0.0961 0.0160 0.101 Uiso 1 1 calc R D 7 C210 C 0.5796(2) 0.1486(3) 0.03867(17) 0.0720(17) Uani 1 1 d . D . H21A H 0.5843 0.1805 0.0163 0.086 Uiso 1 1 calc R . . H21B H 0.5491 0.1173 0.0308 0.086 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 0.0499(4) 0.0500(4) 0.0419(4) -0.0042(4) -0.0003(3) 0.0066(4) Fe2 0.0442(4) 0.0575(4) 0.0450(4) -0.0062(4) -0.0051(3) 0.0068(4) C1 0.053(3) 0.055(3) 0.035(2) -0.001(2) 0.007(2) 0.001(2) N1 0.046(2) 0.056(2) 0.036(2) -0.0044(18) 0.0067(16) 0.0031(19) C2 0.055(3) 0.058(3) 0.041(3) -0.012(2) 0.006(2) 0.003(2) C3 0.050(3) 0.054(3) 0.036(2) 0.000(2) 0.005(2) -0.002(2) N2 0.050(2) 0.050(2) 0.040(2) -0.0021(18) 0.0031(17) 0.0020(19) C4 0.057(3) 0.071(4) 0.035(2) 0.001(2) 0.012(2) 0.011(3) C5 0.042(3) 0.117(5) 0.053(3) 0.012(3) 0.009(2) 0.001(3) C6 0.058(4) 0.143(8) 0.109(6) 0.043(6) 0.014(4) 0.012(5) C7 0.061(4) 0.168(10) 0.108(6) 0.035(6) 0.016(4) 0.034(5) C8 0.101(5) 0.109(6) 0.064(4) 0.018(4) 0.010(4) 0.048(5) C9 0.079(4) 0.073(4) 0.043(3) 0.006(3) 0.011(3) 0.006(3) C10 0.057(3) 0.103(5) 0.081(4) 0.014(4) 0.009(3) -0.020(4) C11 0.110(6) 0.100(6) 0.083(5) 0.014(4) 0.000(4) -0.034(5) C12 0.080(5) 0.163(9) 0.088(5) -0.012(6) -0.004(4) -0.036(5) C13 0.137(6) 0.056(3) 0.040(3) 0.000(3) 0.003(3) 0.016(4) C14 0.115(8) 0.054(5) 0.074(6) -0.005(4) 0.011(5) 0.007(5) C15 0.079(6) 0.070(6) 0.074(7) -0.006(5) 0.007(5) -0.029(5) C14A 0.12(3) 0.49(10) 0.16(4) -0.23(6) 0.06(3) -0.11(5) C15A 0.37(9) 0.38(10) 0.09(3) 0.10(5) 0.00(4) -0.24(8) C16 0.053(3) 0.050(3) 0.037(2) -0.001(2) 0.004(2) 0.006(2) C17 0.061(3) 0.063(3) 0.039(3) -0.005(2) -0.001(2) 0.001(3) C18 0.061(3) 0.075(4) 0.057(3) -0.004(3) -0.005(3) -0.001(3) C19 0.068(3) 0.080(4) 0.045(3) -0.006(3) -0.008(3) 0.011(3) C20 0.082(4) 0.060(3) 0.055(3) 0.009(3) 0.003(3) 0.012(3) C21 0.063(3) 0.053(3) 0.047(3) 0.003(2) 0.000(2) 0.006(3) C22 0.064(3) 0.074(4) 0.055(3) 0.006(3) -0.005(3) -0.014(3) C23 0.079(8) 0.059(5) 0.084(7) 0.013(5) 0.007(6) 0.001(5) C24 0.066(6) 0.106(8) 0.058(7) 0.027(6) 0.004(5) -0.015(5) C22A 0.064(3) 0.074(4) 0.055(3) 0.006(3) -0.005(3) -0.014(3) C23A 0.10(2) 0.064(16) 0.14(3) 0.042(17) -0.07(2) -0.029(16) C24A 0.07(2) 0.59(13) 0.05(2) -0.04(4) 0.009(17) 0.10(4) C25 0.071(4) 0.070(4) 0.095(5) 0.031(4) -0.005(3) -0.006(3) C26 0.078(6) 0.128(9) 0.070(6) -0.007(6) 0.018(5) -0.037(6) C27 0.110(7) 0.055(5) 0.112(8) -0.001(5) -0.019(6) -0.002(5) C25A 0.071(4) 0.070(4) 0.095(5) 0.031(4) -0.005(3) -0.006(3) C26A 0.078(6) 0.128(9) 0.070(6) -0.007(6) 0.018(5) -0.037(6) C27A 0.110(7) 0.055(5) 0.112(8) -0.001(5) -0.019(6) -0.002(5) C28 0.046(2) 0.047(3) 0.045(3) 0.004(2) -0.007(2) -0.008(2) N3 0.0423(19) 0.043(2) 0.042(2) 0.0053(18) -0.0049(16) -0.0033(17) C29 0.044(2) 0.052(3) 0.043(2) 0.003(2) -0.007(2) -0.003(2) C30 0.041(2) 0.043(2) 0.048(3) -0.001(2) 0.001(2) -0.003(2) N4 0.046(2) 0.047(2) 0.0372(19) -0.0002(17) 0.0011(16) -0.0087(18) C31 0.050(3) 0.051(3) 0.045(3) 0.006(2) -0.005(2) 0.005(2) C32 0.047(3) 0.073(4) 0.062(3) 0.008(3) -0.011(2) -0.002(3) C33 0.046(3) 0.118(6) 0.078(4) 0.000(4) -0.003(3) 0.006(4) C34 0.067(4) 0.111(6) 0.089(5) -0.015(5) -0.012(4) 0.038(4) C35 0.096(5) 0.068(4) 0.077(4) -0.008(3) -0.023(4) 0.029(4) C36 0.071(3) 0.053(3) 0.052(3) 0.002(3) -0.012(3) 0.009(3) C37 0.060(3) 0.077(4) 0.080(4) 0.015(3) -0.008(3) -0.018(3) C38 0.108(6) 0.098(6) 0.088(5) -0.018(5) -0.007(4) -0.001(5) C39 0.259(14) 0.115(7) 0.095(6) 0.032(6) -0.004(7) -0.078(8) C40 0.097(4) 0.041(3) 0.066(4) 0.001(3) -0.008(3) -0.003(3) C41 0.189(10) 0.177(10) 0.059(4) 0.016(6) -0.018(5) -0.082(8) C42 0.166(8) 0.106(6) 0.063(4) -0.011(4) 0.011(5) -0.054(6) C43 0.049(3) 0.070(3) 0.035(2) -0.004(2) -0.003(2) -0.003(3) C44 0.050(3) 0.080(4) 0.049(3) 0.002(3) 0.001(2) -0.003(3) C45 0.061(4) 0.114(6) 0.060(4) 0.000(4) 0.008(3) 0.001(4) C46 0.078(4) 0.120(6) 0.049(3) -0.021(4) 0.003(3) 0.014(4) C47 0.085(4) 0.080(4) 0.053(3) -0.024(3) -0.005(3) 0.009(4) C48 0.066(3) 0.060(3) 0.052(3) -0.008(3) -0.010(3) -0.003(3) C49 0.056(3) 0.089(5) 0.069(4) 0.015(3) 0.014(3) -0.010(3) C50 0.089(5) 0.101(6) 0.157(8) 0.033(6) -0.028(5) -0.007(5) C51 0.077(4) 0.119(6) 0.085(5) 0.004(5) 0.007(4) -0.029(4) C52 0.092(4) 0.052(3) 0.062(3) -0.016(3) -0.002(3) -0.008(3) C53 0.091(5) 0.090(5) 0.112(6) 0.019(5) 0.003(4) -0.001(4) C54 0.121(6) 0.076(5) 0.111(6) 0.020(5) -0.029(5) -0.009(5) K101 0.0720(7) 0.0525(6) 0.0585(7) -0.0020(6) -0.0129(6) 0.0112(6) O101 0.0554(19) 0.0504(19) 0.0525(19) 0.0025(16) -0.0003(15) -0.0010(16) O102 0.086(3) 0.056(2) 0.074(3) 0.010(2) -0.009(2) -0.007(2) O103 0.109(3) 0.058(2) 0.057(2) 0.002(2) -0.005(2) 0.012(2) O104 0.098(3) 0.064(3) 0.055(2) 0.011(2) 0.007(2) 0.012(2) O105 0.063(2) 0.070(3) 0.066(2) 0.005(2) -0.0100(18) 0.008(2) O106 0.0581(19) 0.067(2) 0.0444(18) -0.0068(17) -0.0101(15) 0.0155(18) C101 0.059(3) 0.067(4) 0.066(3) 0.004(3) 0.006(3) -0.004(3) C102 0.066(4) 0.077(4) 0.088(4) 0.025(4) -0.010(3) -0.015(3) C103 0.103(5) 0.065(4) 0.077(4) 0.010(3) -0.019(4) -0.017(4) C104 0.118(5) 0.058(3) 0.060(4) 0.002(3) 0.003(4) -0.013(4) C105 0.126(6) 0.068(4) 0.052(3) 0.002(3) -0.003(4) 0.024(4) C106 0.112(5) 0.068(4) 0.055(3) 0.012(3) 0.003(3) 0.024(4) C107 0.081(4) 0.084(5) 0.071(4) 0.013(4) -0.007(3) 0.017(4) C108 0.069(4) 0.086(5) 0.088(5) 0.012(4) -0.008(3) 0.021(4) C109 0.066(3) 0.083(4) 0.062(4) 0.005(3) -0.017(3) -0.007(3) C110 0.062(3) 0.070(4) 0.061(3) -0.012(3) -0.007(3) 0.007(3) K201 0.0474(5) 0.0614(7) 0.0622(7) -0.0048(6) 0.0038(5) 0.0030(5) O201 0.0538(19) 0.0512(19) 0.0474(18) 0.0005(16) 0.0024(15) 0.0001(16) O202 0.063(2) 0.067(2) 0.081(3) 0.004(2) 0.009(2) -0.005(2) O203 0.058(2) 0.080(3) 0.086(3) -0.005(2) 0.007(2) -0.005(2) O204 0.055(2) 0.093(4) 0.050(5) 0.006(4) 0.006(4) 0.006(3) O205 0.047(2) 0.068(4) 0.091(5) -0.012(3) 0.005(3) 0.005(2) O4A 0.055(2) 0.093(4) 0.050(5) 0.006(4) 0.006(4) 0.006(3) O5A 0.047(2) 0.068(4) 0.091(5) -0.012(3) 0.005(3) 0.005(2) O206 0.061(2) 0.084(3) 0.065(2) -0.025(2) -0.0117(18) 0.023(2) C201 0.060(3) 0.071(4) 0.055(3) 0.015(3) -0.003(3) 0.007(3) C202 0.079(4) 0.059(3) 0.084(4) 0.016(3) 0.003(3) 0.003(3) C203 0.075(4) 0.070(4) 0.111(6) -0.007(4) 0.003(4) -0.019(4) C204 0.071(4) 0.100(6) 0.126(7) 0.016(5) -0.001(4) -0.024(4) C205 0.053(4) 0.117(6) 0.138(7) 0.022(6) 0.003(4) -0.017(4) C206 0.057(4) 0.099(6) 0.169(9) -0.016(6) -0.023(4) -0.002(4) C207 0.064(4) 0.079(4) 0.098(5) -0.010(4) 0.007(3) 0.017(3) C208 0.055(4) 0.080(4) 0.142(7) -0.018(5) 0.014(4) 0.012(3) C209 0.096(5) 0.094(5) 0.062(4) -0.020(4) 0.003(3) 0.028(4) C210 0.062(3) 0.097(5) 0.057(3) -0.026(3) -0.001(3) 0.005(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O106 1.916(3) . ? Fe1 O101 2.045(3) . ? Fe1 O201 2.048(3) . ? Fe1 C3 2.053(5) . ? Fe1 K201 3.5434(13) . ? Fe1 K101 3.6035(14) . ? Fe2 O206 1.910(4) . ? Fe2 O201 2.046(3) . ? Fe2 O101 2.051(3) . ? Fe2 C30 2.055(4) . ? Fe2 K201 3.6058(13) . ? Fe2 K101 3.6393(13) . ? C1 N1 1.365(6) . ? C1 N2 1.365(6) . ? N1 C2 1.399(6) . ? N1 C4 1.440(6) . ? C2 C3 1.350(7) . ? C2 H2 0.9500 . ? C3 N2 1.416(6) . ? N2 C16 1.435(6) . ? C4 C9 1.379(8) . ? C4 C5 1.403(8) . ? C5 C6 1.346(9) . ? C5 C10 1.512(10) . ? C6 C7 1.362(12) . ? C6 H6 0.9500 . ? C7 C8 1.399(11) . ? C7 H7 0.9500 . ? C8 C9 1.415(9) . ? C8 H8 0.9500 . ? C9 C13 1.501(9) . ? C10 C12 1.509(9) . ? C10 C11 1.523(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? C13 C15 1.480(12) . ? C13 C14 1.562(10) . ? C13 C15A 1.64(4) . ? C13 C14A 1.74(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 H15D 0.9800 . ? C15 H15E 0.9800 . ? C15 H15F 0.9800 . ? C14A H14G 0.9800 . ? C14A H14H 0.9800 . ? C14A H14I 0.9800 . ? C14A H14J 0.9800 . ? C14A H14K 0.9800 . ? C14A H14L 0.9800 . ? C15A H15G 0.9800 . ? C15A H15H 0.9800 . ? C15A H15I 0.9800 . ? C15A H15J 0.9800 . ? C15A H15K 0.9800 . ? C15A H15L 0.9800 . ? C16 C21 1.393(7) . ? C16 C17 1.404(7) . ? C17 C18 1.404(7) . ? C17 C22 1.515(7) . ? C18 C19 1.385(8) . ? C18 H18 0.9500 . ? C19 C20 1.378(8) . ? C19 H19 0.9500 . ? C20 C21 1.411(8) . ? C20 H20 0.9500 . ? C21 C25 1.513(8) . ? C22 C23 1.496(10) . ? C22 C24 1.506(12) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23 H23D 0.9800 . ? C23 H23E 0.9800 . ? C23 H23F 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? C23A H23G 0.9800 . ? C23A H23H 0.9800 . ? C23A H23I 0.9800 . ? C23A H23J 0.9800 . ? C23A H23K 0.9800 . ? C23A H23L 0.9800 . ? C24A H24G 0.9800 . ? C24A H24H 0.9800 . ? C24A H24I 0.9800 . ? C24A H24J 0.9800 . ? C24A H24K 0.9800 . ? C24A H24L 0.9800 . ? C25 C26 1.409(11) . ? C25 C27 1.570(11) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? C26A H26G 0.9800 . ? C26A H26H 0.9800 . ? C26A H26I 0.9800 . ? C26A H26J 0.9800 . ? C26A H26K 0.9800 . ? C26A H26L 0.9800 . ? C27A H27G 0.9800 . ? C27A H27H 0.9800 . ? C27A H27I 0.9800 . ? C27A H27J 0.9800 . ? C27A H27K 0.9800 . ? C27A H27L 0.9800 . ? C28 N3 1.360(6) . ? C28 N4 1.364(6) . ? N3 C29 1.402(6) . ? N3 C31 1.436(6) . ? C29 C30 1.351(6) . ? C29 H29 0.9500 . ? C30 N4 1.408(6) . ? N4 C43 1.447(6) . ? C31 C32 1.392(7) . ? C31 C36 1.393(7) . ? C32 C33 1.400(8) . ? C32 C37 1.522(8) . ? C33 C34 1.362(10) . ? C33 H33 0.9500 . ? C34 C35 1.351(10) . ? C34 H34 0.9500 . ? C35 C36 1.403(8) . ? C35 H35 0.9500 . ? C36 C40 1.504(8) . ? C37 C38 1.492(9) . ? C37 C39 1.523(10) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C38 H38D 0.9800 . ? C38 H38E 0.9800 . ? C38 H38F 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C39 H39D 0.9800 . ? C39 H39E 0.9800 . ? C39 H39F 0.9800 . ? C40 C42 1.505(8) . ? C40 C41 1.515(9) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41 H41D 0.9800 . ? C41 H41E 0.9800 . ? C41 H41F 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C42 H42D 0.9800 . ? C42 H42E 0.9800 . ? C42 H42F 0.9800 . ? C43 C44 1.398(7) . ? C43 C48 1.400(8) . ? C44 C45 1.391(8) . ? C44 C49 1.503(9) . ? C45 C46 1.361(10) . ? C45 H45 0.9500 . ? C46 C47 1.359(9) . ? C46 H46 0.9500 . ? C47 C48 1.393(8) . ? C47 H47 0.9500 . ? C48 C52 1.514(8) . ? C49 C50 1.523(9) . ? C49 C51 1.527(8) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C50 H50D 0.9800 . ? C50 H50E 0.9800 . ? C50 H50F 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C51 H51D 0.9800 . ? C51 H51E 0.9800 . ? C51 H51F 0.9800 . ? C52 C53 1.500(9) . ? C52 C54 1.511(9) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C53 H53D 0.9800 . ? C53 H53E 0.9800 . ? C53 H53F 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C54 H54D 0.9800 . ? C54 H54E 0.9800 . ? C54 H54F 0.9800 . ? K101 O102 2.742(4) . ? K101 O206 2.771(4) . ? K101 O101 2.804(3) . ? K101 O103 2.808(4) . ? K101 O105 2.808(4) . ? K101 O106 2.812(4) . ? K101 O104 2.934(4) . ? K101 O5A 3.02(3) . ? K101 C104 3.479(6) . ? K101 K201 3.5921(17) . ? O101 C101 1.393(6) . ? O102 C103 1.420(7) . ? O102 C102 1.436(7) . ? O103 C104 1.407(7) . ? O103 C105 1.423(7) . ? O104 C106 1.420(8) . ? O104 C107 1.425(7) . ? O105 C109 1.419(7) . ? O105 C108 1.427(7) . ? O106 C110 1.411(6) . ? O106 K201 2.696(4) . ? C101 C102 1.507(8) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.491(9) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.483(8) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.463(9) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.497(8) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11G 0.9900 . ? C110 H11H 0.9900 . ? K201 O202 2.745(4) . ? K201 O4A 2.77(4) . ? K201 O203 2.779(4) . ? K201 O201 2.779(3) . ? K201 O205 2.784(5) . ? K201 O206 2.784(4) . ? K201 O5A 2.91(2) . ? K201 O204 2.932(9) . ? K201 C210 3.460(6) . ? K201 C204 3.516(7) . ? O201 C201 1.412(6) . ? O202 C203 1.408(7) . ? O202 C202 1.409(7) . ? O203 C204 1.365(8) . ? O203 C205 1.397(8) . ? O204 C206 1.404(12) . ? O204 C207 1.461(12) . ? O205 C209 1.327(8) . ? O205 C208 1.422(8) . ? O4A C207 1.32(5) . ? O4A C206 1.44(5) . ? O5A C208 1.40(2) . ? O5A C209 1.55(3) . ? O206 C210 1.359(6) . ? C201 C202 1.503(8) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.426(9) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.406(10) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.435(9) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.422(8) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? 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 O106 Fe1 O101 101.52(15) . . ? O106 Fe1 O201 100.23(14) . . ? O101 Fe1 O201 82.40(14) . . ? O106 Fe1 C3 139.13(17) . . ? O101 Fe1 C3 109.09(17) . . ? O201 Fe1 C3 109.93(16) . . ? O106 Fe1 K201 48.73(10) . . ? O101 Fe1 K201 91.88(10) . . ? O201 Fe1 K201 51.54(9) . . ? C3 Fe1 K201 150.79(14) . . ? O106 Fe1 K101 50.68(11) . . ? O101 Fe1 K101 50.84(9) . . ? O201 Fe1 K101 92.16(10) . . ? C3 Fe1 K101 148.85(14) . . ? K201 Fe1 K101 60.34(3) . . ? O206 Fe2 O201 99.83(16) . . ? O206 Fe2 O101 98.49(15) . . ? O201 Fe2 O101 82.30(13) . . ? O206 Fe2 C30 137.19(17) . . ? O201 Fe2 C30 114.17(16) . . ? O101 Fe2 C30 110.70(16) . . ? O206 Fe2 K201 49.74(12) . . ? O201 Fe2 K201 50.10(9) . . ? O101 Fe2 K201 90.02(10) . . ? C30 Fe2 K201 153.22(13) . . ? O206 Fe2 K101 48.48(12) . . ? O201 Fe2 K101 91.17(10) . . ? O101 Fe2 K101 50.02(9) . . ? C30 Fe2 K101 147.27(13) . . ? K201 Fe2 K101 59.44(3) . . ? N1 C1 N2 100.7(4) . . ? C1 N1 C2 112.2(4) . . ? C1 N1 C4 125.2(4) . . ? C2 N1 C4 122.4(4) . . ? C3 C2 N1 109.2(4) . . ? C3 C2 H2 125.4 . . ? N1 C2 H2 125.4 . . ? C2 C3 N2 101.8(4) . . ? C2 C3 Fe1 126.0(3) . . ? N2 C3 Fe1 131.7(3) . . ? C1 N2 C3 116.0(4) . . ? C1 N2 C16 121.6(4) . . ? C3 N2 C16 122.4(4) . . ? C9 C4 C5 121.1(5) . . ? C9 C4 N1 120.5(5) . . ? C5 C4 N1 118.3(5) . . ? C6 C5 C4 119.2(7) . . ? C6 C5 C10 119.7(7) . . ? C4 C5 C10 121.0(5) . . ? C5 C6 C7 121.6(8) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C8 120.8(7) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C7 C8 C9 118.5(7) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C4 C9 C8 118.7(7) . . ? C4 C9 C13 120.1(5) . . ? C8 C9 C13 121.2(6) . . ? C12 C10 C5 113.8(6) . . ? C12 C10 C11 112.1(6) . . ? C5 C10 C11 109.1(6) . . ? C12 C10 H10 107.2 . . ? C5 C10 H10 107.2 . . ? C11 C10 H10 107.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.3 . . ? C10 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? C10 C11 H11F 109.5 . . ? H11A C11 H11F 56.3 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C12 H12D 109.5 . . ? H12A C12 H12D 141.1 . . ? H12B C12 H12D 56.3 . . ? H12C C12 H12D 56.3 . . ? C10 C12 H12E 109.5 . . ? H12A C12 H12E 56.3 . . ? H12B C12 H12E 141.1 . . ? H12C C12 H12E 56.3 . . ? H12D C12 H12E 109.5 . . ? C10 C12 H12F 109.5 . . ? H12A C12 H12F 56.3 . . ? H12B C12 H12F 56.3 . . ? H12C C12 H12F 141.1 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? C15 C13 C9 111.1(6) . . ? C15 C13 C14 111.6(7) . . ? C9 C13 C14 109.1(7) . . ? C9 C13 C15A 130(2) . . ? C14 C13 C15A 77(3) . . ? C15 C13 C14A 115.2(13) . . ? C9 C13 C14A 127.4(16) . . ? C14 C13 C14A 76(2) . . ? C15A C13 C14A 102(3) . . ? C15 C13 H13 108.3 . . ? C9 C13 H13 108.3 . . ? C14 C13 H13 108.3 . . ? C15A C13 H13 116.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C14 H14D 109.5 . . ? H14A C14 H14D 141.1 . . ? H14B C14 H14D 56.3 . . ? H14C C14 H14D 56.3 . . ? C13 C14 H14E 109.5 . . ? H14A C14 H14E 56.3 . . ? H14B C14 H14E 141.1 . . ? H14C C14 H14E 56.3 . . ? H14D C14 H14E 109.5 . . ? C13 C14 H14F 109.5 . . ? H14A C14 H14F 56.3 . . ? H14B C14 H14F 56.3 . . ? H14C C14 H14F 141.1 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C15 H15D 109.5 . . ? H15A C15 H15D 141.1 . . ? H15B C15 H15D 56.3 . . ? H15C C15 H15D 56.3 . . ? C13 C15 H15E 109.5 . . ? H15A C15 H15E 56.3 . . ? H15B C15 H15E 141.1 . . ? H15C C15 H15E 56.3 . . ? H15D C15 H15E 109.5 . . ? C13 C15 H15F 109.5 . . ? H15A C15 H15F 56.3 . . ? H15B C15 H15F 56.3 . . ? H15C C15 H15F 141.1 . . ? H15D C15 H15F 109.5 . . ? H15E C15 H15F 109.5 . . ? C13 C14A H14G 109.5 . . ? C13 C14A H14H 109.5 . . ? H14G C14A H14H 109.5 . . ? C13 C14A H14I 109.5 . . ? H14G C14A H14I 109.5 . . ? H14H C14A H14I 109.5 . . ? C13 C14A H14J 109.5 . . ? H14G C14A H14J 141.1 . . ? H14H C14A H14J 56.3 . . ? H14I C14A H14J 56.3 . . ? C13 C14A H14K 109.5 . . ? H14G C14A H14K 56.3 . . ? H14H C14A H14K 141.1 . . ? H14I C14A H14K 56.3 . . ? H14J C14A H14K 109.5 . . ? C13 C14A H14L 109.5 . . ? H14G C14A H14L 56.3 . . ? H14H C14A H14L 56.3 . . ? H14I C14A H14L 141.1 . . ? H14J C14A H14L 109.5 . . ? H14K C14A H14L 109.5 . . ? C13 C15A H15G 109.5 . . ? C13 C15A H15H 109.5 . . ? C13 C15A H15I 109.5 . . ? H15G C15A H15I 109.5 . . ? H15H C15A H15I 109.5 . . ? H15G C15A H15J 141.1 . . ? H15H C15A H15J 56.3 . . ? H15I C15A H15J 56.3 . . ? C13 C15A H15K 109.5 . . ? H15G C15A H15K 56.3 . . ? H15H C15A H15K 141.1 . . ? H15I C15A H15K 56.3 . . ? H15J C15A H15K 109.5 . . ? C13 C15A H15L 109.5 . . ? H15G C15A H15L 56.3 . . ? H15H C15A H15L 56.3 . . ? H15I C15A H15L 141.1 . . ? H15J C15A H15L 109.5 . . ? C21 C16 C17 122.1(5) . . ? C21 C16 N2 119.2(4) . . ? C17 C16 N2 118.6(4) . . ? C18 C17 C16 117.4(5) . . ? C18 C17 C22 121.1(5) . . ? C16 C17 C22 121.5(5) . . ? C19 C18 C17 121.9(5) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C20 C19 C18 119.1(5) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 121.7(5) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C16 C21 C20 117.7(5) . . ? C16 C21 C25 121.6(5) . . ? C20 C21 C25 120.7(5) . . ? C23 C22 C24 113.1(7) . . ? C23 C22 C17 112.6(5) . . ? C24 C22 C17 112.9(6) . . ? C23 C22 H22 105.9 . . ? C24 C22 H22 105.9 . . ? C17 C22 H22 105.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C23 H23D 109.5 . . ? H23A C23 H23D 141.1 . . ? H23B C23 H23D 56.3 . . ? H23C C23 H23D 56.3 . . ? C22 C23 H23E 109.5 . . ? H23A C23 H23E 56.3 . . ? H23B C23 H23E 141.1 . . ? H23C C23 H23E 56.3 . . ? H23D C23 H23E 109.5 . . ? C22 C23 H23F 109.5 . . ? H23A C23 H23F 56.3 . . ? H23B C23 H23F 56.3 . . ? H23C C23 H23F 141.1 . . ? H23D C23 H23F 109.5 . . ? H23E C23 H23F 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C24 H24D 109.5 . . ? H24A C24 H24D 141.1 . . ? H24B C24 H24D 56.3 . . ? H24C C24 H24D 56.3 . . ? C22 C24 H24E 109.5 . . ? H24A C24 H24E 56.3 . . ? H24B C24 H24E 141.1 . . ? H24C C24 H24E 56.3 . . ? H24D C24 H24E 109.5 . . ? C22 C24 H24F 109.5 . . ? H24A C24 H24F 56.3 . . ? H24B C24 H24F 56.3 . . ? H24C C24 H24F 141.1 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? H23G C23A H23H 109.5 . . ? H23G C23A H23I 109.5 . . ? H23H C23A H23I 109.5 . . ? H23G C23A H23J 141.1 . . ? H23H C23A H23J 56.3 . . ? H23I C23A H23J 56.3 . . ? H23G C23A H23K 56.3 . . ? H23H C23A H23K 141.1 . . ? H23I C23A H23K 56.3 . . ? H23J C23A H23K 109.5 . . ? H23G C23A H23L 56.3 . . ? H23H C23A H23L 56.3 . . ? H23I C23A H23L 141.1 . . ? H23J C23A H23L 109.5 . . ? H23K C23A H23L 109.5 . . ? H24G C24A H24H 109.5 . . ? H24G C24A H24I 109.5 . . ? H24H C24A H24I 109.5 . . ? H24G C24A H24J 141.1 . . ? H24H C24A H24J 56.3 . . ? H24I C24A H24J 56.3 . . ? H24G C24A H24K 56.3 . . ? H24H C24A H24K 141.1 . . ? H24I C24A H24K 56.3 . . ? H24J C24A H24K 109.5 . . ? H24G C24A H24L 56.3 . . ? H24H C24A H24L 56.3 . . ? H24I C24A H24L 141.1 . . ? H24J C24A H24L 109.5 . . ? H24K C24A H24L 109.5 . . ? C26 C25 C21 115.6(7) . . ? C26 C25 C27 111.6(8) . . ? C21 C25 C27 111.2(6) . . ? C26 C25 H25 105.9 . . ? C21 C25 H25 105.9 . . ? C27 C25 H25 105.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? C25 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? C25 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.3 . . ? C25 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.3 . . ? H27D C27 H27E 109.5 . . ? C25 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.3 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? H26G C26A H26H 109.5 . . ? H26G C26A H26I 109.5 . . ? H26H C26A H26I 109.5 . . ? H26G C26A H26J 141.1 . . ? H26H C26A H26J 56.3 . . ? H26I C26A H26J 56.3 . . ? H26G C26A H26K 56.3 . . ? H26H C26A H26K 141.1 . . ? H26I C26A H26K 56.3 . . ? H26J C26A H26K 109.5 . . ? H26G C26A H26L 56.3 . . ? H26H C26A H26L 56.3 . . ? H26I C26A H26L 141.1 . . ? H26J C26A H26L 109.5 . . ? H26K C26A H26L 109.5 . . ? H27G C27A H27H 109.5 . . ? H27G C27A H27I 109.5 . . ? H27H C27A H27I 109.5 . . ? H27G C27A H27J 141.1 . . ? H27H C27A H27J 56.3 . . ? H27I C27A H27J 56.3 . . ? H27G C27A H27K 56.3 . . ? H27H C27A H27K 141.1 . . ? H27I C27A H27K 56.3 . . ? H27J C27A H27K 109.5 . . ? H27G C27A H27L 56.3 . . ? H27H C27A H27L 56.3 . . ? H27I C27A H27L 141.1 . . ? H27J C27A H27L 109.5 . . ? H27K C27A H27L 109.5 . . ? N3 C28 N4 101.4(4) . . ? C28 N3 C29 111.4(4) . . ? C28 N3 C31 125.1(4) . . ? C29 N3 C31 123.5(4) . . ? C30 C29 N3 109.5(4) . . ? C30 C29 H29 125.3 . . ? N3 C29 H29 125.3 . . ? C29 C30 N4 101.9(4) . . ? C29 C30 Fe2 128.2(4) . . ? N4 C30 Fe2 129.7(3) . . ? C28 N4 C30 115.8(4) . . ? C28 N4 C43 122.0(4) . . ? C30 N4 C43 122.3(4) . . ? C32 C31 C36 122.3(5) . . ? C32 C31 N3 119.4(5) . . ? C36 C31 N3 118.2(5) . . ? C31 C32 C33 117.3(6) . . ? C31 C32 C37 121.6(5) . . ? C33 C32 C37 121.2(6) . . ? C34 C33 C32 121.4(6) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C35 C34 C33 120.2(6) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C36 122.0(6) . . ? C34 C35 H35 119.0 . . ? C36 C35 H35 119.0 . . ? C31 C36 C35 116.8(6) . . ? C31 C36 C40 121.7(5) . . ? C35 C36 C40 121.5(5) . . ? C38 C37 C32 110.1(6) . . ? C38 C37 C39 111.0(6) . . ? C32 C37 C39 111.0(6) . . ? C38 C37 H37 108.2 . . ? C32 C37 H37 108.2 . . ? C39 C37 H37 108.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C38 H38D 109.5 . . ? H38A C38 H38D 141.1 . . ? H38B C38 H38D 56.3 . . ? H38C C38 H38D 56.3 . . ? C37 C38 H38E 109.5 . . ? H38A C38 H38E 56.3 . . ? H38B C38 H38E 141.1 . . ? H38C C38 H38E 56.3 . . ? H38D C38 H38E 109.5 . . ? C37 C38 H38F 109.5 . . ? H38A C38 H38F 56.3 . . ? H38B C38 H38F 56.3 . . ? H38C C38 H38F 141.1 . . ? H38D C38 H38F 109.5 . . ? H38E C38 H38F 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C39 H39D 109.5 . . ? H39A C39 H39D 141.1 . . ? H39B C39 H39D 56.3 . . ? H39C C39 H39D 56.3 . . ? C37 C39 H39E 109.5 . . ? H39A C39 H39E 56.3 . . ? H39B C39 H39E 141.1 . . ? H39C C39 H39E 56.3 . . ? H39D C39 H39E 109.5 . . ? C37 C39 H39F 109.5 . . ? H39A C39 H39F 56.3 . . ? H39B C39 H39F 56.3 . . ? H39C C39 H39F 141.1 . . ? H39D C39 H39F 109.5 . . ? H39E C39 H39F 109.5 . . ? C36 C40 C42 113.8(6) . . ? C36 C40 C41 112.1(6) . . ? C42 C40 C41 108.3(6) . . ? C36 C40 H40 107.5 . . ? C42 C40 H40 107.5 . . ? C41 C40 H40 107.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C41 H41D 109.5 . . ? H41A C41 H41D 141.1 . . ? H41B C41 H41D 56.3 . . ? H41C C41 H41D 56.3 . . ? C40 C41 H41E 109.5 . . ? H41A C41 H41E 56.3 . . ? H41B C41 H41E 141.1 . . ? H41C C41 H41E 56.3 . . ? H41D C41 H41E 109.5 . . ? C40 C41 H41F 109.5 . . ? H41A C41 H41F 56.3 . . ? H41B C41 H41F 56.3 . . ? H41C C41 H41F 141.1 . . ? H41D C41 H41F 109.5 . . ? H41E C41 H41F 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C42 H42D 109.5 . . ? H42A C42 H42D 141.1 . . ? H42B C42 H42D 56.3 . . ? H42C C42 H42D 56.3 . . ? C40 C42 H42E 109.5 . . ? H42A C42 H42E 56.3 . . ? H42B C42 H42E 141.1 . . ? H42C C42 H42E 56.3 . . ? H42D C42 H42E 109.5 . . ? C40 C42 H42F 109.5 . . ? H42A C42 H42F 56.3 . . ? H42B C42 H42F 56.3 . . ? H42C C42 H42F 141.1 . . ? H42D C42 H42F 109.5 . . ? H42E C42 H42F 109.5 . . ? C44 C43 C48 122.1(5) . . ? C44 C43 N4 118.9(5) . . ? C48 C43 N4 119.0(5) . . ? C45 C44 C43 117.4(6) . . ? C45 C44 C49 121.4(6) . . ? C43 C44 C49 121.2(5) . . ? C46 C45 C44 120.9(6) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C47 C46 C45 121.4(6) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C46 C47 C48 120.9(6) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C47 C48 C43 117.3(6) . . ? C47 C48 C52 122.1(5) . . ? C43 C48 C52 120.6(5) . . ? C44 C49 C50 109.3(6) . . ? C44 C49 C51 113.7(6) . . ? C50 C49 C51 110.5(6) . . ? C44 C49 H49 107.7 . . ? C50 C49 H49 107.7 . . ? C51 C49 H49 107.7 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C50 H50D 109.5 . . ? H50A C50 H50D 141.1 . . ? H50B C50 H50D 56.3 . . ? H50C C50 H50D 56.3 . . ? C49 C50 H50E 109.5 . . ? H50A C50 H50E 56.3 . . ? H50B C50 H50E 141.1 . . ? H50C C50 H50E 56.3 . . ? H50D C50 H50E 109.5 . . ? C49 C50 H50F 109.5 . . ? H50A C50 H50F 56.3 . . ? H50B C50 H50F 56.3 . . ? H50C C50 H50F 141.1 . . ? H50D C50 H50F 109.5 . . ? H50E C50 H50F 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C51 H51D 109.5 . . ? H51A C51 H51D 141.1 . . ? H51B C51 H51D 56.3 . . ? H51C C51 H51D 56.3 . . ? C49 C51 H51E 109.5 . . ? H51A C51 H51E 56.3 . . ? H51B C51 H51E 141.1 . . ? H51C C51 H51E 56.3 . . ? H51D C51 H51E 109.5 . . ? C49 C51 H51F 109.5 . . ? H51A C51 H51F 56.3 . . ? H51B C51 H51F 56.3 . . ? H51C C51 H51F 141.1 . . ? H51D C51 H51F 109.5 . . ? H51E C51 H51F 109.5 . . ? C53 C52 C54 108.9(5) . . ? C53 C52 C48 110.2(5) . . ? C54 C52 C48 114.7(6) . . ? C53 C52 H52 107.6 . . ? C54 C52 H52 107.6 . . ? C48 C52 H52 107.6 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C53 H53D 109.5 . . ? H53A C53 H53D 141.1 . . ? H53B C53 H53D 56.3 . . ? H53C C53 H53D 56.3 . . ? C52 C53 H53E 109.5 . . ? H53A C53 H53E 56.3 . . ? H53B C53 H53E 141.1 . . ? H53C C53 H53E 56.3 . . ? H53D C53 H53E 109.5 . . ? C52 C53 H53F 109.5 . . ? H53A C53 H53F 56.3 . . ? H53B C53 H53F 56.3 . . ? H53C C53 H53F 141.1 . . ? H53D C53 H53F 109.5 . . ? H53E C53 H53F 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C54 H54D 109.5 . . ? H54A C54 H54D 141.1 . . ? H54B C54 H54D 56.3 . . ? H54C C54 H54D 56.3 . . ? C52 C54 H54E 109.5 . . ? H54A C54 H54E 56.3 . . ? H54B C54 H54E 141.1 . . ? H54C C54 H54E 56.3 . . ? H54D C54 H54E 109.5 . . ? C52 C54 H54F 109.5 . . ? H54A C54 H54F 56.3 . . ? H54B C54 H54F 56.3 . . ? H54C C54 H54F 141.1 . . ? H54D C54 H54F 109.5 . . ? H54E C54 H54F 109.5 . . ? O102 K101 O206 93.17(12) . . ? O102 K101 O101 61.57(11) . . ? O206 K101 O101 65.17(10) . . ? O102 K101 O103 60.73(13) . . ? O206 K101 O103 93.82(12) . . ? O101 K101 O103 116.42(12) . . ? O102 K101 O105 133.48(13) . . ? O206 K101 O105 132.05(13) . . ? O101 K101 O105 121.83(11) . . ? O103 K101 O105 116.30(12) . . ? O102 K101 O106 121.61(12) . . ? O206 K101 O106 87.44(11) . . ? O101 K101 O106 66.27(10) . . ? O103 K101 O106 177.31(12) . . ? O105 K101 O106 61.24(11) . . ? O102 K101 O104 110.72(12) . . ? O206 K101 O104 123.03(11) . . ? O101 K101 O104 170.20(11) . . ? O103 K101 O104 60.09(13) . . ? O105 K101 O104 58.05(12) . . ? O106 K101 O104 117.25(12) . . ? O102 K101 O5A 131.5(4) . . ? O206 K101 O5A 55.7(5) . . ? O101 K101 O5A 118.8(5) . . ? O103 K101 O5A 83.2(5) . . ? O105 K101 O5A 90.0(4) . . ? O106 K101 O5A 95.6(4) . . ? O104 K101 O5A 70.6(5) . . ? O102 K101 C104 42.41(15) . . ? O206 K101 C104 105.87(14) . . ? O101 K101 C104 103.40(14) . . ? O103 K101 C104 22.82(13) . . ? O105 K101 C104 116.15(14) . . ? O106 K101 C104 158.36(14) . . ? O104 K101 C104 70.00(15) . . ? O5A K101 C104 106.0(5) . . ? O102 K101 K201 136.38(9) . . ? O206 K101 K201 49.86(9) . . ? O101 K101 K201 79.85(7) . . ? O103 K101 K201 131.75(10) . . ? O105 K101 K201 83.11(9) . . ? O106 K101 K201 47.91(8) . . ? O104 K101 K201 109.42(9) . . ? O5A K101 K201 51.4(5) . . ? C104 K101 K201 152.23(11) . . ? O102 K101 Fe1 92.82(9) . . ? O206 K101 Fe1 74.42(8) . . ? O101 K101 Fe1 34.45(7) . . ? O103 K101 Fe1 150.87(10) . . ? O105 K101 Fe1 90.35(9) . . ? O106 K101 Fe1 31.82(7) . . ? O104 K101 Fe1 148.25(10) . . ? O5A K101 Fe1 109.8(5) . . ? C104 K101 Fe1 135.04(13) . . ? K201 K101 Fe1 59.00(3) . . ? O102 K101 Fe2 76.60(9) . . ? O206 K101 Fe2 31.07(8) . . ? O101 K101 Fe2 34.10(7) . . ? O103 K101 Fe2 107.42(9) . . ? O105 K101 Fe2 135.21(9) . . ? O106 K101 Fe2 74.83(7) . . ? O104 K101 Fe2 153.85(9) . . ? O5A K101 Fe2 85.6(5) . . ? C104 K101 Fe2 107.84(12) . . ? K201 K101 Fe2 59.82(3) . . ? Fe1 K101 Fe2 50.35(2) . . ? C101 O101 Fe1 125.7(3) . . ? C101 O101 Fe2 124.8(3) . . ? Fe1 O101 Fe2 97.54(14) . . ? C101 O101 K101 110.8(3) . . ? Fe1 O101 K101 94.71(12) . . ? Fe2 O101 K101 95.88(12) . . ? C103 O102 C102 112.1(5) . . ? C103 O102 K101 117.8(4) . . ? C102 O102 K101 117.3(3) . . ? C104 O103 C105 114.5(5) . . ? C104 O103 K101 106.5(3) . . ? C105 O103 K101 113.7(4) . . ? C106 O104 C107 111.5(5) . . ? C106 O104 K101 113.7(4) . . ? C107 O104 K101 113.4(4) . . ? C109 O105 C108 112.9(5) . . ? C109 O105 K101 115.4(3) . . ? C108 O105 K101 119.0(4) . . ? C110 O106 Fe1 123.7(3) . . ? C110 O106 K201 131.7(3) . . ? Fe1 O106 K201 98.99(13) . . ? C110 O106 K101 110.8(3) . . ? Fe1 O106 K101 97.50(14) . . ? K201 O106 K101 81.38(10) . . ? O101 C101 C102 112.3(5) . . ? O101 C101 H10A 109.1 . . ? C102 C101 H10A 109.1 . . ? O101 C101 H10B 109.1 . . ? C102 C101 H10B 109.1 . . ? H10A C101 H10B 107.9 . . ? O102 C102 C101 107.5(5) . . ? O102 C102 H10C 110.2 . . ? C101 C102 H10C 110.2 . . ? O102 C102 H10D 110.2 . . ? C101 C102 H10D 110.2 . . ? H10C C102 H10D 108.5 . . ? O102 C103 C104 107.8(5) . . ? O102 C103 H10E 110.1 . . ? C104 C103 H10E 110.1 . . ? O102 C103 H10F 110.1 . . ? C104 C103 H10F 110.1 . . ? H10E C103 H10F 108.5 . . ? O103 C104 C103 108.8(5) . . ? O103 C104 K101 50.7(3) . . ? C103 C104 K101 83.6(3) . . ? O103 C104 H10G 109.9 . . ? C103 C104 H10G 109.9 . . ? K101 C104 H10G 78.9 . . ? O103 C104 H10H 109.9 . . ? C103 C104 H10H 109.9 . . ? K101 C104 H10H 160.2 . . ? H10G C104 H10H 108.3 . . ? O103 C105 C106 114.4(5) . . ? O103 C105 H10I 108.7 . . ? C106 C105 H10I 108.7 . . ? O103 C105 H10J 108.7 . . ? C106 C105 H10J 108.7 . . ? H10I C105 H10J 107.6 . . ? O104 C106 C105 107.6(5) . . ? O104 C106 H10K 110.2 . . ? C105 C106 H10K 110.2 . . ? O104 C106 H10L 110.2 . . ? C105 C106 H10L 110.2 . . ? H10K C106 H10L 108.5 . . ? O104 C107 C108 109.0(5) . . ? O104 C107 H10M 109.9 . . ? C108 C107 H10M 109.9 . . ? O104 C107 H10N 109.9 . . ? C108 C107 H10N 109.9 . . ? H10M C107 H10N 108.3 . . ? O105 C108 C107 109.3(5) . . ? O105 C108 H10O 109.8 . . ? C107 C108 H10O 109.8 . . ? O105 C108 H10P 109.8 . . ? C107 C108 H10P 109.8 . . ? H10O C108 H10P 108.3 . . ? O105 C109 C110 109.7(5) . . ? O105 C109 H10Q 109.7 . . ? C110 C109 H10Q 109.7 . . ? O105 C109 H10R 109.7 . . ? C110 C109 H10R 109.7 . . ? H10Q C109 H10R 108.2 . . ? O106 C110 C109 111.1(5) . . ? O106 C110 H11G 109.4 . . ? C109 C110 H11G 109.4 . . ? O106 C110 H11H 109.4 . . ? C109 C110 H11H 109.4 . . ? H11G C110 H11H 108.0 . . ? O106 K201 O202 95.26(12) . . ? O106 K201 O4A 106.8(6) . . ? O202 K201 O4A 120.2(10) . . ? O106 K201 O203 102.46(12) . . ? O202 K201 O203 61.93(13) . . ? O4A K201 O203 59.3(10) . . ? O106 K201 O201 67.51(10) . . ? O202 K201 O201 62.71(11) . . ? O4A K201 O201 174.1(6) . . ? O203 K201 O201 122.19(12) . . ? O106 K201 O205 118.50(19) . . ? O202 K201 O205 146.0(2) . . ? O4A K201 O205 56.2(10) . . ? O203 K201 O205 110.29(15) . . ? O201 K201 O205 124.71(13) . . ? O106 K201 O206 89.50(12) . . ? O202 K201 O206 121.53(12) . . ? O4A K201 O206 113.6(11) . . ? O203 K201 O206 167.40(12) . . ? O201 K201 O206 65.96(10) . . ? O205 K201 O206 59.50(13) . . ? O106 K201 O5A 100.6(6) . . ? O202 K201 O5A 164.0(6) . . ? O4A K201 O5A 57.1(11) . . ? O203 K201 O5A 116.1(4) . . ? O201 K201 O5A 121.7(4) . . ? O205 K201 O5A 18.0(5) . . ? O206 K201 O5A 56.8(4) . . ? O106 K201 O204 97.88(15) . . ? O202 K201 O204 123.5(2) . . ? O4A K201 O204 8.9(6) . . ? O203 K201 O204 61.6(2) . . ? O201 K201 O204 165.20(16) . . ? O205 K201 O204 59.2(2) . . ? O206 K201 O204 113.3(2) . . ? O5A K201 O204 56.7(5) . . ? O106 K201 C210 109.32(13) . . ? O202 K201 C210 125.96(15) . . ? O4A K201 C210 98.1(10) . . ? O203 K201 C210 145.57(13) . . ? O201 K201 C210 83.06(12) . . ? O205 K201 C210 41.85(14) . . ? O206 K201 C210 21.88(12) . . ? O5A K201 C210 45.7(5) . . ? O204 K201 C210 100.4(2) . . ? O106 K201 C204 106.99(17) . . ? O202 K201 C204 41.79(15) . . ? O4A K201 C204 78.5(10) . . ? O203 K201 C204 21.16(15) . . ? O201 K201 C204 104.08(15) . . ? O205 K201 C204 122.1(2) . . ? O206 K201 C204 156.24(17) . . ? O5A K201 C204 132.9(5) . . ? O204 K201 C204 81.9(2) . . ? C210 K201 C204 142.87(18) . . ? O106 K201 Fe1 32.29(7) . . ? O202 K201 Fe1 78.71(9) . . ? O4A K201 Fe1 139.0(6) . . ? O203 K201 Fe1 117.05(9) . . ? O201 K201 Fe1 35.24(7) . . ? O205 K201 Fe1 128.02(15) . . ? O206 K201 Fe1 75.30(8) . . ? O5A K201 Fe1 114.0(5) . . ? O204 K201 Fe1 130.07(14) . . ? C210 K201 Fe1 97.11(10) . . ? C204 K201 Fe1 109.66(14) . . ? C201 O201 Fe2 126.9(3) . . ? C201 O201 Fe1 124.4(3) . . ? Fe2 O201 Fe1 97.65(14) . . ? C201 O201 K201 111.1(3) . . ? Fe2 O201 K201 95.52(12) . . ? Fe1 O201 K201 93.23(12) . . ? C203 O202 C202 114.9(5) . . ? C203 O202 K201 113.8(4) . . ? C202 O202 K201 115.0(3) . . ? C204 O203 C205 120.7(5) . . ? C204 O203 K201 111.5(4) . . ? C205 O203 K201 113.3(4) . . ? C206 O204 C207 110.7(7) . . ? C206 O204 K201 109.7(6) . . ? C207 O204 K201 109.6(5) . . ? C209 O205 C208 116.0(6) . . ? C209 O205 K201 117.9(4) . . ? C208 O205 K201 120.1(4) . . ? C207 O4A C206 117(3) . . ? C207 O4A K201 125(3) . . ? C206 O4A K201 117(3) . . ? C208 O5A C209 104.1(17) . . ? C208 O5A K201 113.7(13) . . ? C209 O5A K201 103.4(12) . . ? C208 O5A K101 145.5(17) . . ? C209 O5A K101 106.2(10) . . ? K201 O5A K101 74.6(5) . . ? C210 O206 Fe2 132.0(4) . . ? C210 O206 K101 122.3(4) . . ? Fe2 O206 K101 100.45(15) . . ? C210 O206 K201 108.3(3) . . ? Fe2 O206 K201 98.68(16) . . ? K101 O206 K201 80.59(10) . . ? O201 C201 C202 112.4(4) . . ? O201 C201 H20A 109.1 . . ? C202 C201 H20A 109.1 . . ? O201 C201 H20B 109.1 . . ? C202 C201 H20B 109.1 . . ? H20A C201 H20B 107.9 . . ? O202 C202 C201 110.1(5) . . ? O202 C202 H20C 109.6 . . ? C201 C202 H20C 109.6 . . ? O202 C202 H20D 109.6 . . ? C201 C202 H20D 109.6 . . ? H20C C202 H20D 108.2 . . ? O202 C203 C204 111.8(6) . . ? O202 C203 H20E 109.3 . . ? C204 C203 H20E 109.3 . . ? O202 C203 H20F 109.3 . . ? C204 C203 H20F 109.3 . . ? H20E C203 H20F 107.9 . . ? O203 C204 C203 115.3(6) . . ? O203 C204 K201 47.3(3) . . ? C203 C204 K201 79.9(4) . . ? O203 C204 H20G 108.5 . . ? C203 C204 H20G 108.5 . . ? K201 C204 H20G 92.8 . . ? O203 C204 H20H 108.5 . . ? C203 C204 H20H 108.5 . . ? K201 C204 H20H 153.5 . . ? H20G C204 H20H 107.5 . . ? O203 C205 C206 115.3(6) . . ? O203 C205 H20I 108.5 . . ? C206 C205 H20I 108.5 . . ? O203 C205 H20J 108.5 . . ? C206 C205 H20J 108.5 . . ? H20I C205 H20J 107.5 . . ? O204 C206 C205 120.1(7) . . ? C205 C206 O4A 104.0(17) . . ? O204 C206 H20K 107.3 . . ? C205 C206 H20K 107.3 . . ? O4A C206 H20K 105.6 . . ? O204 C206 H20L 107.3 . . ? C205 C206 H20L 107.3 . . ? O4A C206 H20L 124.7 . . ? H20K C206 H20L 106.9 . . ? O4A C207 C208 114(2) . . ? C208 C207 O204 111.4(6) . . ? O4A C207 H20M 91.7 . . ? C208 C207 H20M 109.3 . . ? O204 C207 H20M 109.3 . . ? O4A C207 H20N 122.6 . . ? C208 C207 H20N 109.3 . . ? O204 C207 H20N 109.3 . . ? H20M C207 H20N 108.0 . . ? O5A C208 C207 122.4(11) . . ? O205 C208 C207 109.7(6) . . ? O5A C208 H20O 124.4 . . ? O205 C208 H20O 109.7 . . ? C207 C208 H20O 109.7 . . ? O5A C208 H20P 72.7 . . ? O205 C208 H20P 109.7 . . ? C207 C208 H20P 109.7 . . ? H20O C208 H20P 108.2 . . ? O205 C209 C210 114.9(6) . . ? C210 C209 O5A 116.1(9) . . ? O205 C209 H20Q 108.6 . . ? C210 C209 H20Q 108.6 . . ? O5A C209 H20Q 75.5 . . ? O205 C209 H20R 108.6 . . ? C210 C209 H20R 108.6 . . ? O5A C209 H20R 131.6 . . ? H20Q C209 H20R 107.5 . . ? O206 C210 C209 115.7(5) . . ? O206 C210 K201 49.8(3) . . ? C209 C210 K201 84.0(4) . . ? O206 C210 H21A 108.3 . . ? C209 C210 H21A 108.3 . . ? K201 C210 H21A 84.7 . . ? O206 C210 H21B 108.3 . . ? C209 C210 H21B 108.3 . . ? K201 C210 H21B 158.1 . . ? H21A C210 H21B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.444 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.066 _iucr_refine_instructions_details ; TITL pbca in Pbca CELL 1.54178 23.4906 20.2128 33.1958 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0007 0.0008 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N K FE O UNIT 592 880 32 16 16 96 MERG 2 OMIT 0.00 133.00 EXYZ C22 C22A EADP C22 C22A EXYZ C25 C25A EADP C25 C25A EADP C26 C26A EADP C27 C27A EADP O204 O4A EADP O205 O5A FMAP 2 PLAN 20 SIZE 0.08 0.22 0.26 ACTA BOND $H L.S. 8 TEMP -123.00 WGHT 0.105700 FVAR 0.03664 0.72821 0.74246 0.75000 0.79037 FE1 5 0.535216 0.304380 0.161255 11.00000 0.04991 0.04999 = 0.04191 -0.00417 -0.00031 0.00660 FE2 5 0.499251 0.240121 0.081030 11.00000 0.04420 0.05749 = 0.04501 -0.00618 -0.00509 0.00675 C1 1 0.430261 0.434701 0.235041 11.00000 0.05329 0.05493 = 0.03511 -0.00084 0.00745 0.00117 N1 3 0.404344 0.435341 0.198230 11.00000 0.04575 0.05646 = 0.03603 -0.00438 0.00669 0.00309 C2 1 0.434211 0.398141 0.169676 11.00000 0.05460 0.05780 = 0.04136 -0.01180 0.00638 0.00311 AFIX 43 H2 2 0.423481 0.392577 0.142293 11.00000 -1.20000 AFIX 0 C3 1 0.480715 0.371382 0.187186 11.00000 0.04966 0.05436 = 0.03589 0.00008 0.00453 -0.00187 N2 3 0.476198 0.395410 0.227142 11.00000 0.05001 0.04970 = 0.04017 -0.00214 0.00305 0.00204 C4 1 0.350346 0.465840 0.189537 11.00000 0.05705 0.07091 = 0.03521 0.00102 0.01235 0.01136 C5 1 0.302467 0.424930 0.185226 11.00000 0.04163 0.11672 = 0.05305 0.01177 0.00936 0.00130 C6 1 0.252731 0.451788 0.173429 11.00000 0.05757 0.14316 = 0.10905 0.04282 0.01440 0.01157 AFIX 43 H6 2 0.220765 0.423812 0.169287 11.00000 -1.20000 AFIX 0 C7 1 0.247145 0.518098 0.167291 11.00000 0.06112 0.16777 = 0.10802 0.03452 0.01641 0.03416 AFIX 43 H7 2 0.211520 0.535543 0.158886 11.00000 -1.20000 AFIX 0 C8 1 0.293233 0.560813 0.173215 11.00000 0.10061 0.10946 = 0.06363 0.01761 0.00972 0.04817 AFIX 43 H8 2 0.288731 0.607314 0.170547 11.00000 -1.20000 AFIX 0 C9 1 0.346720 0.533173 0.183274 11.00000 0.07874 0.07347 = 0.04277 0.00646 0.01063 0.00595 C10 1 0.305127 0.352256 0.195893 11.00000 0.05711 0.10296 = 0.08145 0.01445 0.00854 -0.02008 AFIX 13 H10 2 0.345142 0.337301 0.191124 11.00000 -1.20000 AFIX 0 C11 1 0.293148 0.344049 0.240705 11.00000 0.11038 0.10041 = 0.08281 0.01440 -0.00001 -0.03441 AFIX 123 H11A 2 0.319034 0.372348 0.256167 10.50000 -1.50000 H11B 2 0.299008 0.297749 0.248421 10.50000 -1.50000 H11C 2 0.253692 0.356771 0.246362 10.50000 -1.50000 H11D 2 0.262122 0.312230 0.244466 10.50000 -1.50000 H11E 2 0.282148 0.386830 0.252212 10.50000 -1.50000 H11F 2 0.327464 0.327808 0.254271 10.50000 -1.50000 AFIX 0 C12 1 0.266972 0.309266 0.170369 11.00000 0.08041 0.16281 = 0.08840 -0.01212 -0.00426 -0.03557 AFIX 123 H12A 2 0.276443 0.315490 0.141869 10.50000 -1.50000 H12B 2 0.227151 0.321626 0.174936 10.50000 -1.50000 H12C 2 0.272537 0.262758 0.177723 10.50000 -1.50000 H12D 2 0.240977 0.284426 0.187816 10.50000 -1.50000 H12E 2 0.290270 0.278290 0.154749 10.50000 -1.50000 H12F 2 0.244884 0.337158 0.151963 10.50000 -1.50000 AFIX 0 C13 1 0.398626 0.575821 0.187789 11.00000 0.13701 0.05582 = 0.03993 -0.00050 0.00308 0.01638 AFIX 13 H13 2 0.420461 0.560154 0.211825 11.00000 -1.20000 AFIX 0 PART 1 C14 1 0.379632 0.648809 0.195514 21.00000 0.11511 0.05431 = 0.07445 -0.00494 0.01125 0.00664 AFIX 123 H14A 2 0.356598 0.650812 0.220098 20.50000 -1.50000 H14B 2 0.357028 0.664517 0.172618 20.50000 -1.50000 H14C 2 0.413355 0.676878 0.198671 20.50000 -1.50000 H14D 2 0.394723 0.677326 0.174160 20.50000 -1.50000 H14E 2 0.394293 0.663621 0.221640 20.50000 -1.50000 H14F 2 0.337966 0.651260 0.195587 20.50000 -1.50000 AFIX 0 C15 1 0.435910 0.570620 0.152003 21.00000 0.07872 0.06965 = 0.07404 -0.00578 0.00713 -0.02861 AFIX 123 H15A 2 0.469620 0.598484 0.155832 20.50000 -1.50000 H15B 2 0.415064 0.585429 0.128073 20.50000 -1.50000 H15C 2 0.447739 0.524504 0.148402 20.50000 -1.50000 H15D 2 0.418662 0.540461 0.132373 20.50000 -1.50000 H15E 2 0.473218 0.553515 0.160132 20.50000 -1.50000 H15F 2 0.440543 0.614441 0.139802 20.50000 -1.50000 AFIX 0 PART 2 C14A 1 0.432946 0.597582 0.232254 -21.00000 0.11834 0.48587 = 0.16468 -0.23044 0.05617 -0.11282 AFIX 123 H14G 2 0.467129 0.623377 0.225952 -20.50000 -1.50000 H14H 2 0.443800 0.557450 0.246931 -20.50000 -1.50000 H14I 2 0.407255 0.624187 0.248946 -20.50000 -1.50000 H14J 2 0.411661 0.579965 0.255267 -20.50000 -1.50000 H14K 2 0.434990 0.645893 0.234289 -20.50000 -1.50000 H14L 2 0.471535 0.579156 0.232273 -20.50000 -1.50000 AFIX 0 C15A 1 0.434572 0.617518 0.153799 -21.00000 0.37420 0.37854 = 0.08901 0.09556 -0.00155 -0.24204 AFIX 123 H15G 2 0.464490 0.643344 0.167068 -20.50000 -1.50000 H15H 2 0.408782 0.647442 0.139430 -20.50000 -1.50000 H15I 2 0.451898 0.586653 0.134615 -20.50000 -1.50000 H15J 2 0.418957 0.608282 0.127007 -20.50000 -1.50000 H15K 2 0.474665 0.604184 0.154645 -20.50000 -1.50000 H15L 2 0.431549 0.664972 0.159460 -20.50000 -1.50000 AFIX 0 PART 0 C16 1 0.517262 0.379694 0.257686 11.00000 0.05288 0.05008 = 0.03692 -0.00089 0.00380 0.00562 C17 1 0.568452 0.415483 0.258734 11.00000 0.06084 0.06256 = 0.03872 -0.00520 -0.00135 0.00056 C18 1 0.607445 0.399750 0.289305 11.00000 0.06089 0.07506 = 0.05686 -0.00370 -0.00529 -0.00135 AFIX 43 H18 2 0.642168 0.423701 0.290908 11.00000 -1.20000 AFIX 0 C19 1 0.596778 0.350315 0.317211 11.00000 0.06777 0.08006 = 0.04467 -0.00586 -0.00821 0.01078 AFIX 43 H19 2 0.623604 0.340859 0.337838 11.00000 -1.20000 AFIX 0 C20 1 0.546702 0.315051 0.314621 11.00000 0.08247 0.06029 = 0.05504 0.00943 0.00349 0.01194 AFIX 43 H20 2 0.539351 0.281086 0.333706 11.00000 -1.20000 AFIX 0 C21 1 0.506080 0.328110 0.284349 11.00000 0.06276 0.05306 = 0.04658 0.00316 -0.00037 0.00589 PART 3 C22 1 0.580401 0.470627 0.229019 31.00000 0.06382 0.07411 = 0.05495 0.00584 -0.00497 -0.01373 AFIX 13 H22 2 0.560769 0.457633 0.203488 31.00000 -1.20000 AFIX 0 C23 1 0.554260 0.534968 0.241477 31.00000 0.07904 0.05885 = 0.08389 0.01299 0.00724 0.00078 AFIX 123 H23A 2 0.562908 0.568861 0.221273 30.50000 -1.50000 H23B 2 0.569844 0.548476 0.267597 30.50000 -1.50000 H23C 2 0.512909 0.529703 0.243718 30.50000 -1.50000 H23D 2 0.534200 0.529165 0.267119 30.50000 -1.50000 H23E 2 0.527263 0.549551 0.220795 30.50000 -1.50000 H23F 2 0.584198 0.568323 0.244674 30.50000 -1.50000 AFIX 0 C24 1 0.642578 0.476618 0.218574 31.00000 0.06601 0.10569 = 0.05774 0.02707 0.00359 -0.01455 AFIX 123 H24A 2 0.657627 0.432957 0.211405 30.50000 -1.50000 H24B 2 0.663480 0.493997 0.241829 30.50000 -1.50000 H24C 2 0.647087 0.506798 0.195690 30.50000 -1.50000 H24D 2 0.654502 0.522877 0.221211 30.50000 -1.50000 H24E 2 0.648650 0.461838 0.190787 30.50000 -1.50000 H24F 2 0.665042 0.449037 0.236926 30.50000 -1.50000 AFIX 0 PART 4 C22A 1 0.580401 0.470627 0.229019 -31.00000 0.06382 0.07411 = 0.05495 0.00584 -0.00497 -0.01373 AFIX 13 H22A 2 0.546035 0.476671 0.211626 -31.00000 -1.20000 AFIX 0 C23A 1 0.590398 0.537820 0.254466 -31.00000 0.09700 0.06408 = 0.13971 0.04237 -0.06616 -0.02883 AFIX 123 H23G 2 0.597558 0.574584 0.235898 -30.50000 -1.50000 H23H 2 0.623254 0.532203 0.272333 -30.50000 -1.50000 H23I 2 0.556441 0.547407 0.270592 -30.50000 -1.50000 H23J 2 0.587278 0.528212 0.283318 -30.50000 -1.50000 H23K 2 0.561581 0.570593 0.246882 -30.50000 -1.50000 H23L 2 0.628395 0.555389 0.248623 -30.50000 -1.50000 AFIX 0 C24A 1 0.635348 0.471202 0.200989 -31.00000 0.06550 0.58598 = 0.04514 -0.03829 0.00881 0.10230 AFIX 123 H24G 2 0.634309 0.510168 0.183438 -30.50000 -1.50000 H24H 2 0.635965 0.431035 0.184462 -30.50000 -1.50000 H24I 2 0.669611 0.472758 0.217806 -30.50000 -1.50000 H24J 2 0.658948 0.432473 0.207032 -30.50000 -1.50000 H24K 2 0.657291 0.511606 0.206008 -30.50000 -1.50000 H24L 2 0.623646 0.469883 0.172664 -30.50000 -1.50000 AFIX 0 PART 5 C25 1 0.452147 0.287458 0.281427 41.00000 0.07093 0.06951 = 0.09547 0.03063 -0.00488 -0.00638 AFIX 13 H25 2 0.433622 0.300701 0.255530 41.00000 -1.20000 AFIX 0 C26 1 0.411408 0.299116 0.311764 41.00000 0.07810 0.12782 = 0.07036 -0.00670 0.01846 -0.03703 AFIX 123 H26A 2 0.378182 0.270757 0.307230 40.50000 -1.50000 H26B 2 0.399679 0.345628 0.311019 40.50000 -1.50000 H26C 2 0.428031 0.289070 0.338141 40.50000 -1.50000 H26D 2 0.425746 0.332880 0.330363 40.50000 -1.50000 H26E 2 0.404249 0.258009 0.326575 40.50000 -1.50000 H26F 2 0.375898 0.314567 0.299452 40.50000 -1.50000 AFIX 0 C27 1 0.465998 0.211774 0.277198 41.00000 0.11046 0.05476 = 0.11214 -0.00057 -0.01901 -0.00158 AFIX 123 H27A 2 0.494883 0.205482 0.256244 40.50000 -1.50000 H27B 2 0.431314 0.187727 0.269798 40.50000 -1.50000 H27C 2 0.480440 0.194879 0.302913 40.50000 -1.50000 H27D 2 0.442875 0.186577 0.296392 40.50000 -1.50000 H27E 2 0.506444 0.204332 0.282839 40.50000 -1.50000 H27F 2 0.457318 0.197179 0.249724 40.50000 -1.50000 AFIX 0 PART 6 C25A 1 0.452147 0.287458 0.281427 -41.00000 0.07093 0.06951 = 0.09547 0.03063 -0.00488 -0.00638 AFIX 13 H25A 2 0.423771 0.323068 0.275586 -41.00000 -1.20000 AFIX 0 C26A 1 0.436071 0.270955 0.333420 -41.00000 0.07810 0.12782 = 0.07036 -0.00670 0.01846 -0.03703 AFIX 123 H26G 2 0.452068 0.306134 0.350289 -40.50000 -1.50000 H26H 2 0.452685 0.228372 0.341233 -40.50000 -1.50000 H26I 2 0.394696 0.269362 0.337078 -40.50000 -1.50000 H26J 2 0.414231 0.229778 0.335445 -40.50000 -1.50000 H26K 2 0.413614 0.307540 0.344500 -40.50000 -1.50000 H26L 2 0.471604 0.266550 0.348655 -40.50000 -1.50000 AFIX 0 C27A 1 0.437340 0.248403 0.260238 -41.00000 0.11046 0.05476 = 0.11214 -0.00057 -0.01901 -0.00158 AFIX 123 H27G 2 0.399971 0.232141 0.268854 -40.50000 -1.50000 H27H 2 0.464642 0.211743 0.260164 -40.50000 -1.50000 H27I 2 0.434369 0.266937 0.233039 -40.50000 -1.50000 H27J 2 0.466017 0.241740 0.239184 -40.50000 -1.50000 H27K 2 0.401346 0.262138 0.247874 -40.50000 -1.50000 H27L 2 0.431619 0.206944 0.274999 -40.50000 -1.50000 AFIX 0 PART 0 C28 1 0.351138 0.272010 0.005163 11.00000 0.04609 0.04679 = 0.04476 0.00439 -0.00673 -0.00844 N3 3 0.334465 0.298611 0.040910 11.00000 0.04226 0.04325 = 0.04153 0.00525 -0.00489 -0.00335 C29 1 0.376741 0.291558 0.070392 11.00000 0.04356 0.05160 = 0.04259 0.00319 -0.00732 -0.00336 AFIX 43 H29 2 0.373944 0.306711 0.097410 11.00000 -1.20000 AFIX 0 C30 1 0.422090 0.259872 0.054439 11.00000 0.04117 0.04334 = 0.04840 -0.00111 0.00051 -0.00321 N4 3 0.404159 0.249116 0.014512 11.00000 0.04613 0.04686 = 0.03721 -0.00016 0.00114 -0.00870 C31 1 0.281574 0.332416 0.047726 11.00000 0.04953 0.05066 = 0.04453 0.00571 -0.00515 0.00460 C32 1 0.232198 0.295717 0.053837 11.00000 0.04741 0.07299 = 0.06189 0.00778 -0.01066 -0.00195 C33 1 0.182268 0.330800 0.062462 11.00000 0.04622 0.11784 = 0.07806 -0.00023 -0.00296 0.00647 AFIX 43 H33 2 0.147750 0.307209 0.066465 11.00000 -1.20000 AFIX 0 C34 1 0.182136 0.398034 0.065234 11.00000 0.06655 0.11122 = 0.08870 -0.01505 -0.01189 0.03802 AFIX 43 H34 2 0.147848 0.420723 0.071511 11.00000 -1.20000 AFIX 0 C35 1 0.230623 0.432566 0.059085 11.00000 0.09607 0.06768 = 0.07690 -0.00818 -0.02327 0.02891 AFIX 43 H35 2 0.229692 0.479438 0.061086 11.00000 -1.20000 AFIX 0 C36 1 0.282281 0.401264 0.049836 11.00000 0.07132 0.05252 = 0.05172 0.00245 -0.01249 0.00885 C37 1 0.232018 0.220636 0.050544 11.00000 0.06041 0.07730 = 0.07956 0.01467 -0.00791 -0.01803 AFIX 13 H37 2 0.272393 0.205212 0.048816 11.00000 -1.20000 AFIX 0 C38 1 0.201969 0.199712 0.013048 11.00000 0.10811 0.09753 = 0.08792 -0.01806 -0.00701 -0.00134 AFIX 123 H38A 2 0.202188 0.151326 0.011175 10.50000 -1.50000 H38B 2 0.221420 0.218477 -0.010436 10.50000 -1.50000 H38C 2 0.162564 0.215589 0.013780 10.50000 -1.50000 H38D 2 0.188593 0.238935 -0.001496 10.50000 -1.50000 H38E 2 0.169362 0.171784 0.020115 10.50000 -1.50000 H38F 2 0.228217 0.174673 -0.004101 10.50000 -1.50000 AFIX 0 C39 1 0.204948 0.189269 0.087615 11.00000 0.25907 0.11451 = 0.09508 0.03243 -0.00431 -0.07761 AFIX 123 H39A 2 0.225750 0.203170 0.111765 10.50000 -1.50000 H39B 2 0.206509 0.140978 0.085219 10.50000 -1.50000 H39C 2 0.165171 0.203478 0.089710 10.50000 -1.50000 H39D 2 0.172537 0.161914 0.079365 10.50000 -1.50000 H39E 2 0.191778 0.224106 0.105911 10.50000 -1.50000 H39F 2 0.233116 0.161607 0.101419 10.50000 -1.50000 AFIX 0 C40 1 0.335452 0.440374 0.041450 11.00000 0.09731 0.04084 = 0.06566 0.00095 -0.00757 -0.00264 AFIX 13 H40 2 0.368012 0.408517 0.040893 11.00000 -1.20000 AFIX 0 C41 1 0.333338 0.474313 0.000780 11.00000 0.18933 0.17715 = 0.05879 0.01646 -0.01784 -0.08158 AFIX 123 H41A 2 0.368740 0.498952 -0.003563 10.50000 -1.50000 H41B 2 0.300999 0.504920 0.000047 10.50000 -1.50000 H41C 2 0.328906 0.441017 -0.020450 10.50000 -1.50000 H41D 2 0.297023 0.464308 -0.012414 10.50000 -1.50000 H41E 2 0.364764 0.458339 -0.016025 10.50000 -1.50000 H41F 2 0.336857 0.522242 0.004472 10.50000 -1.50000 AFIX 0 C42 1 0.348574 0.491713 0.072963 11.00000 0.16630 0.10564 = 0.06326 -0.01143 0.01053 -0.05394 AFIX 123 H42A 2 0.383849 0.514794 0.065829 10.50000 -1.50000 H42B 2 0.353177 0.470134 0.099198 10.50000 -1.50000 H42C 2 0.317236 0.523634 0.074378 10.50000 -1.50000 H42D 2 0.318992 0.490914 0.093775 10.50000 -1.50000 H42E 2 0.349664 0.535574 0.060405 10.50000 -1.50000 H42F 2 0.385606 0.482074 0.085225 10.50000 -1.50000 AFIX 0 C43 1 0.439838 0.216521 -0.014973 11.00000 0.04890 0.07027 = 0.03497 -0.00437 -0.00296 -0.00262 C44 1 0.475320 0.254997 -0.039362 11.00000 0.04991 0.08048 = 0.04937 0.00194 0.00125 -0.00267 C45 1 0.508503 0.222105 -0.067686 11.00000 0.06079 0.11408 = 0.06027 -0.00015 0.00844 0.00099 AFIX 43 H45 2 0.533051 0.246763 -0.084768 11.00000 -1.20000 AFIX 0 C46 1 0.506305 0.155076 -0.071278 11.00000 0.07841 0.11989 = 0.04916 -0.02064 0.00290 0.01409 AFIX 43 H46 2 0.528631 0.133868 -0.091344 11.00000 -1.20000 AFIX 0 C47 1 0.472829 0.117856 -0.046751 11.00000 0.08505 0.08050 = 0.05339 -0.02420 -0.00530 0.00867 AFIX 43 H47 2 0.472671 0.071090 -0.049600 11.00000 -1.20000 AFIX 0 C48 1 0.438752 0.147373 -0.017492 11.00000 0.06617 0.06005 = 0.05227 -0.00813 -0.01030 -0.00310 C49 1 0.477940 0.328891 -0.034715 11.00000 0.05617 0.08874 = 0.06939 0.01540 0.01424 -0.00998 AFIX 13 H49 2 0.460378 0.340389 -0.008182 11.00000 -1.20000 AFIX 0 C50 1 0.442283 0.361235 -0.067593 11.00000 0.08861 0.10055 = 0.15726 0.03283 -0.02788 -0.00678 AFIX 123 H50A 2 0.443558 0.409420 -0.064445 10.50000 -1.50000 H50B 2 0.402794 0.346004 -0.065437 10.50000 -1.50000 H50C 2 0.457557 0.349090 -0.094051 10.50000 -1.50000 H50D 2 0.425715 0.326923 -0.084844 10.50000 -1.50000 H50E 2 0.466479 0.390339 -0.083852 10.50000 -1.50000 H50F 2 0.411715 0.387252 -0.055237 10.50000 -1.50000 AFIX 0 C51 1 0.538432 0.356568 -0.035016 11.00000 0.07650 0.11923 = 0.08482 0.00435 0.00680 -0.02852 AFIX 123 H51A 2 0.537101 0.404712 -0.031659 10.50000 -1.50000 H51B 2 0.556766 0.345809 -0.060713 10.50000 -1.50000 H51C 2 0.560246 0.336941 -0.012870 10.50000 -1.50000 H51D 2 0.565640 0.320263 -0.038502 10.50000 -1.50000 H51E 2 0.545976 0.379166 -0.009449 10.50000 -1.50000 H51F 2 0.542496 0.388034 -0.057291 10.50000 -1.50000 AFIX 0 C52 1 0.402810 0.107108 0.011369 11.00000 0.09239 0.05167 = 0.06242 -0.01571 -0.00157 -0.00758 AFIX 13 H52 2 0.395299 0.135177 0.035600 11.00000 -1.20000 AFIX 0 C53 1 0.346423 0.091006 -0.007455 11.00000 0.09058 0.09018 = 0.11227 0.01936 0.00305 -0.00129 AFIX 123 H53A 2 0.328152 0.131898 -0.016642 10.50000 -1.50000 H53B 2 0.322012 0.069178 0.012457 10.50000 -1.50000 H53C 2 0.352274 0.061425 -0.030475 10.50000 -1.50000 H53D 2 0.340140 0.043103 -0.006465 10.50000 -1.50000 H53E 2 0.346280 0.105823 -0.035564 10.50000 -1.50000 H53F 2 0.316018 0.113576 0.007369 10.50000 -1.50000 AFIX 0 C54 1 0.430232 0.043734 0.025734 11.00000 0.12073 0.07634 = 0.11051 0.02013 -0.02860 -0.00860 AFIX 123 H54A 2 0.404453 0.020994 0.044363 10.50000 -1.50000 H54B 2 0.465993 0.054036 0.039583 10.50000 -1.50000 H54C 2 0.438034 0.015070 0.002573 10.50000 -1.50000 H54D 2 0.467867 0.039073 0.013316 10.50000 -1.50000 H54E 2 0.406327 0.006030 0.018097 10.50000 -1.50000 H54F 2 0.434286 0.044997 0.055106 10.50000 -1.50000 AFIX 0 K101 4 0.580191 0.135090 0.149210 11.00000 0.07199 0.05254 = 0.05854 -0.00201 -0.01288 0.01123 O101 6 0.489531 0.224444 0.141691 11.00000 0.05539 0.05041 = 0.05253 0.00250 -0.00032 -0.00099 O102 6 0.471266 0.087647 0.156085 11.00000 0.08642 0.05612 = 0.07394 0.01027 -0.00890 -0.00658 O103 6 0.557444 0.003180 0.128106 11.00000 0.10884 0.05764 = 0.05730 0.00180 -0.00453 0.01220 O104 6 0.663382 0.031338 0.168068 11.00000 0.09779 0.06414 = 0.05491 0.01097 0.00664 0.01248 O105 6 0.668790 0.155350 0.204630 11.00000 0.06313 0.06951 = 0.06553 0.00465 -0.00997 0.00762 O106 6 0.608190 0.265361 0.171332 11.00000 0.05805 0.06743 = 0.04440 -0.00677 -0.01012 0.01552 C101 1 0.440527 0.199376 0.159763 11.00000 0.05897 0.06726 = 0.06629 0.00428 0.00601 -0.00438 AFIX 23 H10A 2 0.408305 0.229638 0.154290 11.00000 -1.20000 H10B 2 0.446208 0.197633 0.189295 11.00000 -1.20000 AFIX 0 C102 1 0.425753 0.131192 0.144661 11.00000 0.06556 0.07675 = 0.08800 0.02522 -0.01030 -0.01547 AFIX 23 H10C 2 0.389467 0.116103 0.156730 11.00000 -1.20000 H10D 2 0.421424 0.131683 0.114997 11.00000 -1.20000 AFIX 0 C103 1 0.460902 0.021304 0.144046 11.00000 0.10315 0.06489 = 0.07713 0.00988 -0.01854 -0.01701 AFIX 23 H10E 2 0.452590 0.019491 0.114829 11.00000 -1.20000 H10F 2 0.427773 0.003197 0.158820 11.00000 -1.20000 AFIX 0 C104 1 0.512921 -0.018098 0.153330 11.00000 0.11831 0.05838 = 0.06033 0.00179 0.00343 -0.01300 AFIX 23 H10G 2 0.523736 -0.011887 0.181905 11.00000 -1.20000 H10H 2 0.505346 -0.065706 0.148819 11.00000 -1.20000 AFIX 0 C105 1 0.606405 -0.038232 0.128558 11.00000 0.12625 0.06757 = 0.05234 0.00164 -0.00250 0.02359 AFIX 23 H10I 2 0.630875 -0.026484 0.105354 11.00000 -1.20000 H10J 2 0.594068 -0.084682 0.124915 11.00000 -1.20000 AFIX 0 C106 1 0.640762 -0.033699 0.165931 11.00000 0.11196 0.06810 = 0.05502 0.01195 0.00258 0.02361 AFIX 23 H10K 2 0.616620 -0.042721 0.189750 11.00000 -1.20000 H10L 2 0.671995 -0.066568 0.165331 11.00000 -1.20000 AFIX 0 C107 1 0.692842 0.042116 0.205032 11.00000 0.08145 0.08433 = 0.07121 0.01340 -0.00696 0.01668 AFIX 23 H10M 2 0.724547 0.010127 0.207614 11.00000 -1.20000 H10N 2 0.666580 0.035500 0.228006 11.00000 -1.20000 AFIX 0 C108 1 0.715110 0.109712 0.205545 11.00000 0.06914 0.08606 = 0.08807 0.01154 -0.00836 0.02066 AFIX 23 H10O 2 0.738029 0.116787 0.230199 11.00000 -1.20000 H10P 2 0.740014 0.116894 0.181887 11.00000 -1.20000 AFIX 0 C109 1 0.686412 0.222009 0.209505 11.00000 0.06579 0.08276 = 0.06189 0.00541 -0.01709 -0.00652 AFIX 23 H10Q 2 0.712568 0.234439 0.187379 11.00000 -1.20000 H10R 2 0.707077 0.226943 0.235322 11.00000 -1.20000 AFIX 0 C110 1 0.635503 0.266574 0.209168 11.00000 0.06247 0.06953 = 0.06086 -0.01166 -0.00724 0.00660 AFIX 23 H11G 2 0.608397 0.252254 0.230274 11.00000 -1.20000 H11H 2 0.647560 0.312375 0.215403 11.00000 -1.20000 AFIX 0 K201 4 0.649638 0.266679 0.095598 11.00000 0.04745 0.06137 = 0.06224 -0.00483 0.00384 0.00296 O201 6 0.541715 0.322358 0.100726 11.00000 0.05384 0.05117 = 0.04742 0.00053 0.00239 0.00007 O202 6 0.641412 0.401221 0.086086 11.00000 0.06278 0.06736 = 0.08081 0.00421 0.00888 -0.00461 O203 6 0.748122 0.341639 0.103709 11.00000 0.05790 0.08033 = 0.08582 -0.00493 0.00652 -0.00528 PART 7 O204 6 0.757167 0.197848 0.111634 51.00000 0.05489 0.09337 = 0.05039 0.00625 0.00593 0.00577 O205 6 0.674152 0.146391 0.058631 51.00000 0.04710 0.06776 = 0.09068 -0.01218 0.00548 0.00521 PART 8 O4A 6 0.755519 0.206230 0.098407 -51.00000 0.05489 0.09337 = 0.05039 0.00625 0.00593 0.00577 O5A 6 0.665870 0.125671 0.081816 -51.00000 0.04710 0.06776 = 0.09068 -0.01218 0.00548 0.00521 PART 0 O206 6 0.562220 0.182254 0.071880 11.00000 0.06110 0.08392 = 0.06499 -0.02494 -0.01170 0.02303 C201 1 0.540678 0.386017 0.083220 11.00000 0.05993 0.07093 = 0.05537 0.01491 -0.00300 0.00658 AFIX 23 H20A 2 0.504067 0.407719 0.089822 11.00000 -1.20000 H20B 2 0.542966 0.381676 0.053558 11.00000 -1.20000 AFIX 0 C202 1 0.588821 0.428871 0.097669 11.00000 0.07929 0.05941 = 0.08357 0.01604 0.00290 0.00300 AFIX 23 H20C 2 0.585026 0.473761 0.086046 11.00000 -1.20000 H20D 2 0.587256 0.432790 0.127376 11.00000 -1.20000 AFIX 0 C203 1 0.689659 0.436138 0.099525 11.00000 0.07468 0.06993 = 0.11086 -0.00659 0.00257 -0.01924 AFIX 23 H20E 2 0.688104 0.440428 0.129213 11.00000 -1.20000 H20F 2 0.689238 0.481224 0.087877 11.00000 -1.20000 AFIX 0 C204 1 0.741227 0.403767 0.088389 11.00000 0.07126 0.10028 = 0.12557 0.01569 -0.00124 -0.02394 AFIX 23 H20G 2 0.742846 0.401070 0.058633 11.00000 -1.20000 H20H 2 0.773638 0.431420 0.097326 11.00000 -1.20000 AFIX 0 C205 1 0.797808 0.305715 0.096174 11.00000 0.05266 0.11750 = 0.13840 0.02162 0.00272 -0.01704 AFIX 23 H20I 2 0.830847 0.332907 0.104461 11.00000 -1.20000 H20J 2 0.800903 0.298288 0.066778 11.00000 -1.20000 AFIX 0 C206 1 0.801350 0.244166 0.115728 11.00000 0.05650 0.09882 = 0.16897 -0.01616 -0.02350 -0.00175 AFIX 23 H20K 2 0.836817 0.222526 0.106460 11.00000 -1.20000 H20L 2 0.806020 0.253046 0.144871 11.00000 -1.20000 AFIX 0 C207 1 0.769287 0.151678 0.078870 11.00000 0.06405 0.07946 = 0.09789 -0.01042 0.00655 0.01658 AFIX 23 H20M 2 0.778129 0.176876 0.054074 11.00000 -1.20000 H20N 2 0.803131 0.124858 0.085881 11.00000 -1.20000 AFIX 0 C208 1 0.721905 0.108593 0.071396 11.00000 0.05541 0.07978 = 0.14170 -0.01788 0.01413 0.01186 AFIX 23 H20O 2 0.732119 0.076052 0.050311 11.00000 -1.20000 H20P 2 0.712260 0.084041 0.096282 11.00000 -1.20000 AFIX 0 C209 1 0.631223 0.112433 0.042866 11.00000 0.09614 0.09441 = 0.06154 -0.01990 0.00294 0.02799 AFIX 23 H20Q 2 0.623876 0.073324 0.060050 11.00000 -1.20000 H20R 2 0.642851 0.096105 0.015980 11.00000 -1.20000 AFIX 0 C210 1 0.579625 0.148589 0.038671 11.00000 0.06226 0.09661 = 0.05708 -0.02589 -0.00141 0.00488 AFIX 23 H21A 2 0.584274 0.180549 0.016313 11.00000 -1.20000 H21B 2 0.549118 0.117336 0.030844 11.00000 -1.20000 HKLF 4 REM pbca in Pbca REM R1 = 0.0751 for 7857 Fo > 4sig(Fo) and 0.1338 for all 13877 data REM 899 parameters refined using 0 restraints END WGHT 0.1059 0.0000 REM Highest difference peak 0.444, deepest hole -0.369, 1-sigma level 0.066 Q1 1 0.4941 0.2358 0.1086 11.00000 0.05 0.44 Q2 1 0.4939 0.3031 0.1654 11.00000 0.05 0.43 Q3 1 0.6217 0.1367 0.1473 11.00000 0.05 0.41 Q4 1 0.4554 0.2587 0.0524 11.00000 0.05 0.40 Q5 1 0.5357 0.2398 0.0791 11.00000 0.05 0.40 Q6 1 0.5178 0.2573 0.1679 11.00000 0.05 0.39 Q7 1 0.2636 0.1802 0.0803 11.00000 0.05 0.39 Q8 1 0.7940 0.3232 0.1271 11.00000 0.05 0.34 Q9 1 0.5195 0.3211 0.1955 11.00000 0.05 0.33 Q10 1 0.6521 0.2353 0.1325 11.00000 0.05 0.33 Q11 1 0.5296 0.2547 0.1204 11.00000 0.05 0.33 Q12 1 0.6493 0.2801 0.0684 11.00000 0.05 0.33 Q13 1 0.2685 0.4977 0.1912 11.00000 0.05 0.32 Q14 1 0.7330 0.4009 0.1251 11.00000 0.05 0.32 Q15 1 0.5597 0.1166 0.1813 11.00000 0.05 0.32 Q16 1 0.1933 0.2010 0.0860 11.00000 0.05 0.31 Q17 1 0.7601 0.1395 0.1131 11.00000 0.05 0.31 Q18 1 0.5762 0.3061 0.1650 11.00000 0.05 0.31 Q19 1 0.1777 0.1817 0.0412 11.00000 0.05 0.31 Q20 1 0.2911 0.5416 0.1721 11.00000 0.05 0.31 ; _database_code_depnum_ccdc_archive 'CCDC 962253' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]2[Fe3{O4[Si(Me)2]3}2{O3[Si(Me)2]2}2] ; _contact_author_fax '+44 1865 272690' _chemical_name_common . _chemical_melting_point . _chemical_formula_moiety 'C19.54 H58.62 Fe3 O13.77 Si9.77, 2(C18 H36 K N2 O6)' _chemical_formula_sum 'C55.54 H130.62 Fe3 K2 N4 O25.77 Si9.77' _chemical_formula_weight 1787.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6110(2) _cell_length_b 13.5342(2) _cell_length_c 16.7124(3) _cell_angle_alpha 102.789(2) _cell_angle_beta 95.550(2) _cell_angle_gamma 102.524(2) _cell_volume 2258.30(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21411 _cell_measurement_theta_min 3.4515 _cell_measurement_theta_max 76.3955 _exptl_crystal_description needle _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 959 _exptl_absorpt_coefficient_mu 6.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1923 _exptl_absorpt_correction_T_max 0.4642 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; . ; _diffrn_ambient_temperature 150.0(3) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4102 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 42915 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 66.50 _reflns_number_total 7970 _reflns_number_gt 7053 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution 'SIR 92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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^ > 2\s(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. There are two sizes of polydimethylsiloxane rings chelating the terminal Fe atoms; an eight membered ring (which is the major component) and a six membered ring. This disorder was modelled as two components and the occupancies freely refined. Due to some atoms from the separate components overlapping, DFIX and EADP restraints were required to give a stable solution. ; _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^)+(0.0598P)^2^+2.6611P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7970 _refine_ls_number_parameters 485 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.00937(5) 0.18478(4) 0.14471(3) 0.03437(13) Uani 1 1 d . . . Fe2 Fe 0.0000 0.0000 0.0000 0.02917(15) Uani 1 2 d S . . O1 O 0.0292(4) 0.1820(2) 0.25683(15) 0.0709(9) Uani 1 1 d . A . Si1 Si 0.05263(14) 0.25027(10) 0.34938(7) 0.0573(4) Uani 0.8853(19) 1 d P A 1 C1 C 0.0293(5) 0.1677(4) 0.4245(3) 0.0624(12) Uani 0.8853(19) 1 d P A 1 H1A H 0.0440 0.2126 0.4810 0.094 Uiso 0.8853(19) 1 calc PR A 1 H1B H 0.0915 0.1235 0.4201 0.094 Uiso 0.8853(19) 1 calc PR A 1 H1C H -0.0601 0.1235 0.4121 0.094 Uiso 0.8853(19) 1 calc PR A 1 C2 C 0.2233(8) 0.3323(5) 0.3764(4) 0.091(2) Uani 0.8853(19) 1 d P A 1 H2A H 0.2374 0.3741 0.4339 0.137 Uiso 0.8853(19) 1 calc PR A 1 H2B H 0.2379 0.3789 0.3391 0.137 Uiso 0.8853(19) 1 calc PR A 1 H2C H 0.2843 0.2872 0.3704 0.137 Uiso 0.8853(19) 1 calc PR A 1 O2 O -0.0494(8) 0.3229(6) 0.3681(3) 0.133(3) Uani 0.8853(19) 1 d PU A 1 Si2 Si -0.13236(11) 0.39255(8) 0.33062(6) 0.0408(3) Uani 0.8853(19) 1 d P A 1 C3 C -0.2918(7) 0.3069(6) 0.2821(5) 0.142(4) Uani 0.8853(19) 1 d P A 1 H3A H -0.3333 0.2750 0.3233 0.213 Uiso 0.8853(19) 1 calc PR A 1 H3B H -0.2807 0.2519 0.2361 0.213 Uiso 0.8853(19) 1 calc PR A 1 H3C H -0.3469 0.3477 0.2609 0.213 Uiso 0.8853(19) 1 calc PR A 1 C4 C -0.1553(4) 0.4960(3) 0.4167(2) 0.0466(9) Uani 0.8853(19) 1 d P A 1 H4A H -0.1991 0.4640 0.4570 0.070 Uiso 0.8853(19) 1 calc PR A 1 H4B H -0.2090 0.5374 0.3948 0.070 Uiso 0.8853(19) 1 calc PR A 1 H4C H -0.0700 0.5416 0.4440 0.070 Uiso 0.8853(19) 1 calc PR A 1 O3 O -0.0609(3) 0.4461(2) 0.26549(18) 0.0598(8) Uani 0.8853(19) 1 d P A 1 Si3 Si -0.03963(14) 0.42500(9) 0.16715(8) 0.0443(3) Uani 0.8853(19) 1 d P A 1 C5 C -0.1599(8) 0.4822(4) 0.1160(4) 0.096(2) Uani 0.8853(19) 1 d P A 1 H5A H -0.1457 0.5562 0.1444 0.144 Uiso 0.8853(19) 1 calc PR A 1 H5B H -0.2487 0.4447 0.1191 0.144 Uiso 0.8853(19) 1 calc PR A 1 H5C H -0.1487 0.4757 0.0577 0.144 Uiso 0.8853(19) 1 calc PR A 1 C6 C 0.1285(18) 0.5046(12) 0.1694(8) 0.090(3) Uani 0.8853(19) 1 d P A 1 H6A H 0.1350 0.5777 0.1972 0.135 Uiso 0.8853(19) 1 calc PR A 1 H6B H 0.1467 0.4998 0.1125 0.135 Uiso 0.8853(19) 1 calc PR A 1 H6C H 0.1920 0.4781 0.1998 0.135 Uiso 0.8853(19) 1 calc PR A 1 Si11 Si 0.0464(11) 0.2940(8) 0.3151(6) 0.0573(4) Uani 0.1147(19) 1 d PD A 2 C11 C -0.074(5) 0.321(6) 0.385(3) 0.0624(12) Uani 0.1147(19) 1 d PD A 2 H21A H -0.0398 0.3903 0.4230 0.094 Uiso 0.1147(19) 1 calc PR A 2 H21B H -0.0899 0.2679 0.4161 0.094 Uiso 0.1147(19) 1 calc PR A 2 H21C H -0.1559 0.3198 0.3513 0.094 Uiso 0.1147(19) 1 calc PR A 2 C12 C 0.191(7) 0.359(4) 0.396(4) 0.091(2) Uani 0.1147(19) 1 d P A 2 H12A H 0.1811 0.4264 0.4269 0.137 Uiso 0.1147(19) 1 calc PR A 2 H12B H 0.2702 0.3690 0.3703 0.137 Uiso 0.1147(19) 1 calc PR A 2 H12C H 0.1987 0.3143 0.4350 0.137 Uiso 0.1147(19) 1 calc PR A 2 O11 O 0.047(3) 0.3922(16) 0.2767(15) 0.063(7) Uani 0.1147(19) 1 d PU A 2 Si12 Si -0.0125(12) 0.4066(8) 0.1901(7) 0.0443(3) Uani 0.1147(19) 1 d PD A 2 C13 C -0.160(6) 0.459(3) 0.205(3) 0.096(2) Uani 0.1147(19) 1 d P A 2 H13A H -0.1360 0.5251 0.2473 0.144 Uiso 0.1147(19) 1 calc PR A 2 H13B H -0.2261 0.4084 0.2222 0.144 Uiso 0.1147(19) 1 calc PR A 2 H13C H -0.1962 0.4703 0.1522 0.144 Uiso 0.1147(19) 1 calc PR A 2 C14 C 0.116(16) 0.494(11) 0.153(8) 0.090(3) Uani 0.1147(19) 1 d PD A 2 H14A H 0.1476 0.5612 0.1944 0.135 Uiso 0.1147(19) 1 calc PR A 2 H14B H 0.0796 0.5067 0.1005 0.135 Uiso 0.1147(19) 1 calc PR A 2 H14C H 0.1890 0.4617 0.1430 0.135 Uiso 0.1147(19) 1 calc PR A 2 O4 O -0.0594(3) 0.30464(18) 0.12381(15) 0.0505(6) Uani 1 1 d . A . Si4 Si -0.26103(8) -0.02263(7) 0.09340(5) 0.0403(2) Uani 1 1 d . . . Si5 Si 0.24749(8) 0.20527(6) 0.04218(5) 0.0375(2) Uani 1 1 d . . . C7 C -0.2428(4) -0.0646(4) 0.1919(2) 0.0712(13) Uani 1 1 d . A . H7A H -0.3284 -0.1017 0.2009 0.107 Uiso 1 1 calc R . . H7B H -0.2071 -0.0030 0.2384 0.107 Uiso 1 1 calc R . . H7C H -0.1835 -0.1111 0.1884 0.107 Uiso 1 1 calc R . . C8 C -0.3802(4) 0.0594(3) 0.0989(3) 0.0676(12) Uani 1 1 d . A . H8A H -0.4638 0.0196 0.1084 0.101 Uiso 1 1 calc R . . H8B H -0.3925 0.0799 0.0466 0.101 Uiso 1 1 calc R . . H8C H -0.3472 0.1221 0.1447 0.101 Uiso 1 1 calc R . . C9 C 0.3662(4) 0.2730(3) 0.1380(2) 0.0557(9) Uani 1 1 d . A . H9A H 0.4454 0.3130 0.1234 0.084 Uiso 1 1 calc R . . H9B H 0.3886 0.2211 0.1658 0.084 Uiso 1 1 calc R . . H9C H 0.3272 0.3204 0.1753 0.084 Uiso 1 1 calc R . . C10 C 0.2087(4) 0.3018(3) -0.0147(3) 0.0607(10) Uani 1 1 d . A . H20A H 0.2897 0.3427 -0.0267 0.091 Uiso 1 1 calc R . . H20B H 0.1654 0.3488 0.0196 0.091 Uiso 1 1 calc R . . H20C H 0.1507 0.2647 -0.0669 0.091 Uiso 1 1 calc R . . O5 O -0.1208(2) 0.03864(16) 0.07783(13) 0.0387(5) Uani 1 1 d . A . O6 O 0.1143(2) 0.13773(16) 0.06212(13) 0.0392(5) Uani 1 1 d . A . O7 O -0.3188(2) -0.12693(17) 0.01660(14) 0.0421(5) Uani 1 1 d . . . K101 K 0.61587(6) 0.19106(5) 0.71776(4) 0.04032(17) Uani 1 1 d . . . N101 N 0.7943(3) 0.0694(3) 0.7629(2) 0.0628(9) Uani 1 1 d . . . N102 N 0.4294(3) 0.3103(2) 0.66331(19) 0.0496(7) Uani 1 1 d . . . O101 O 0.8513(2) 0.2007(2) 0.64666(19) 0.0611(7) Uani 1 1 d . . . O102 O 0.6961(3) 0.3371(2) 0.62501(16) 0.0555(6) Uani 1 1 d . . . O103 O 0.5359(3) -0.0304(2) 0.67107(19) 0.0596(7) Uani 1 1 d . . . O104 O 0.3881(2) 0.08281(19) 0.59709(16) 0.0523(6) Uani 1 1 d . . . O105 O 0.7113(3) 0.2237(2) 0.88383(17) 0.0605(7) Uani 1 1 d . . . O106 O 0.5064(3) 0.3105(2) 0.83887(16) 0.0550(6) Uani 1 1 d . . . C101 C 0.8876(5) 0.0612(4) 0.7033(4) 0.0810(15) Uani 1 1 d . . . H10Q H 0.8420 0.0107 0.6508 0.097 Uiso 1 1 calc R . . H10R H 0.9582 0.0331 0.7258 0.097 Uiso 1 1 calc R . . C102 C 0.9472(4) 0.1625(5) 0.6848(4) 0.0825(15) Uani 1 1 d . . . H10K H 0.9918 0.2141 0.7370 0.099 Uiso 1 1 calc R . . H10L H 1.0132 0.1524 0.6478 0.099 Uiso 1 1 calc R . . C103 C 0.9034(4) 0.2975(3) 0.6314(3) 0.0621(11) Uani 1 1 d . . . H10M H 0.9782 0.2931 0.6009 0.075 Uiso 1 1 calc R . . H10N H 0.9356 0.3507 0.6848 0.075 Uiso 1 1 calc R . . C104 C 0.8022(4) 0.3291(3) 0.5819(3) 0.0624(11) Uani 1 1 d . . . H10C H 0.8403 0.3972 0.5706 0.075 Uiso 1 1 calc R . . H10D H 0.7715 0.2767 0.5280 0.075 Uiso 1 1 calc R . . C105 C 0.6007(4) 0.3751(3) 0.5833(3) 0.0616(10) Uani 1 1 d . . . H10I H 0.5557 0.3217 0.5321 0.074 Uiso 1 1 calc R . . H10J H 0.6439 0.4388 0.5673 0.074 Uiso 1 1 calc R . . C106 C 0.5030(4) 0.3999(3) 0.6386(3) 0.0638(11) Uani 1 1 d . . . H10A H 0.5492 0.4538 0.6893 0.077 Uiso 1 1 calc R . . H10B H 0.4408 0.4301 0.6096 0.077 Uiso 1 1 calc R . . C107 C 0.7191(5) -0.0349(4) 0.7630(4) 0.0761(14) Uani 1 1 d . . . H10G H 0.6693 -0.0287 0.8103 0.091 Uiso 1 1 calc R . . H10H H 0.7806 -0.0784 0.7719 0.091 Uiso 1 1 calc R . . C108 C 0.6274(5) -0.0885(4) 0.6859(4) 0.0789(14) Uani 1 1 d . . . H10O H 0.6767 -0.0983 0.6386 0.095 Uiso 1 1 calc R . . H10P H 0.5806 -0.1584 0.6902 0.095 Uiso 1 1 calc R . . C109 C 0.4544(5) -0.0743(3) 0.5946(3) 0.0668(11) Uani 1 1 d . . . H10E H 0.4213 -0.1504 0.5877 0.080 Uiso 1 1 calc R . . H10F H 0.5049 -0.0640 0.5490 0.080 Uiso 1 1 calc R . . C110 C 0.3436(4) -0.0253(3) 0.5901(3) 0.0591(10) Uani 1 1 d . . . H11A H 0.2853 -0.0587 0.5365 0.071 Uiso 1 1 calc R . . H11B H 0.2928 -0.0363 0.6354 0.071 Uiso 1 1 calc R . . C111 C 0.2843(4) 0.1324(3) 0.5998(3) 0.0548(9) Uani 1 1 d . . . H11G H 0.2488 0.1319 0.6524 0.066 Uiso 1 1 calc R . . H11H H 0.2134 0.0939 0.5532 0.066 Uiso 1 1 calc R . . C112 C 0.3310(4) 0.2428(3) 0.5939(3) 0.0630(11) Uani 1 1 d . . . H11K H 0.3682 0.2419 0.5417 0.076 Uiso 1 1 calc R . . H11L H 0.2549 0.2738 0.5904 0.076 Uiso 1 1 calc R . . C113 C 0.8659(5) 0.1246(4) 0.8451(3) 0.0776(14) Uani 1 1 d . . . H11Q H 0.9278 0.1885 0.8404 0.093 Uiso 1 1 calc R . . H11R H 0.9180 0.0796 0.8645 0.093 Uiso 1 1 calc R . . C114 C 0.7830(5) 0.1551(4) 0.9092(3) 0.0708(12) Uani 1 1 d . . . H11O H 0.7219 0.0920 0.9159 0.085 Uiso 1 1 calc R . . H11P H 0.8390 0.1907 0.9632 0.085 Uiso 1 1 calc R . . C115 C 0.6314(4) 0.2563(4) 0.9403(3) 0.0623(10) Uani 1 1 d . . . H11I H 0.6818 0.2799 0.9970 0.075 Uiso 1 1 calc R . . H11J H 0.5575 0.1968 0.9392 0.075 Uiso 1 1 calc R . . C116 C 0.5808(4) 0.3421(3) 0.9203(2) 0.0580(10) Uani 1 1 d . . . H11M H 0.5251 0.3644 0.9615 0.070 Uiso 1 1 calc R . . H11N H 0.6547 0.4025 0.9236 0.070 Uiso 1 1 calc R . . C117 C 0.4548(4) 0.3887(3) 0.8171(3) 0.0596(10) Uani 1 1 d . . . H11C H 0.5266 0.4467 0.8126 0.072 Uiso 1 1 calc R . . H11D H 0.4059 0.4166 0.8607 0.072 Uiso 1 1 calc R . . C118 C 0.3647(4) 0.3457(4) 0.7351(3) 0.0630(11) Uani 1 1 d . . . H11E H 0.2954 0.2861 0.7399 0.076 Uiso 1 1 calc R . . H11F H 0.3218 0.4005 0.7240 0.076 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 0.0349(3) 0.0331(2) 0.0336(2) 0.00518(19) 0.00536(19) 0.0084(2) Fe2 0.0269(3) 0.0314(3) 0.0286(3) 0.0081(2) 0.0049(2) 0.0049(3) O1 0.125(3) 0.0631(17) 0.0315(12) 0.0042(12) 0.0022(14) 0.0495(18) Si1 0.0911(9) 0.0571(7) 0.0333(6) 0.0054(5) 0.0067(5) 0.0456(7) C1 0.067(3) 0.081(3) 0.043(2) 0.016(2) 0.007(2) 0.027(3) C2 0.132(6) 0.052(4) 0.074(4) -0.012(3) 0.034(4) 0.010(3) O2 0.225(7) 0.171(5) 0.068(3) 0.038(3) 0.044(3) 0.167(5) Si2 0.0498(6) 0.0356(5) 0.0404(5) 0.0092(4) 0.0122(4) 0.0156(4) C3 0.101(5) 0.134(6) 0.113(6) -0.048(5) 0.047(5) -0.067(5) C4 0.054(2) 0.049(2) 0.043(2) 0.0129(17) 0.0153(18) 0.0198(18) O3 0.086(2) 0.0419(15) 0.0437(15) 0.0028(12) 0.0253(15) 0.0000(15) Si3 0.0675(8) 0.0306(5) 0.0351(6) 0.0098(4) 0.0137(5) 0.0086(5) C5 0.153(6) 0.054(3) 0.081(4) 0.006(3) -0.015(4) 0.055(4) C6 0.102(6) 0.062(4) 0.080(7) -0.010(5) 0.046(6) -0.019(3) Si11 0.0911(9) 0.0571(7) 0.0333(6) 0.0054(5) 0.0067(5) 0.0456(7) C11 0.067(3) 0.081(3) 0.043(2) 0.016(2) 0.007(2) 0.027(3) C12 0.132(6) 0.052(4) 0.074(4) -0.012(3) 0.034(4) 0.010(3) O11 0.092(18) 0.029(10) 0.068(15) -0.008(10) 0.029(13) 0.025(11) Si12 0.0675(8) 0.0306(5) 0.0351(6) 0.0098(4) 0.0137(5) 0.0086(5) C13 0.153(6) 0.054(3) 0.081(4) 0.006(3) -0.015(4) 0.055(4) C14 0.102(6) 0.062(4) 0.080(7) -0.010(5) 0.046(6) -0.019(3) O4 0.0718(17) 0.0369(12) 0.0416(12) 0.0073(10) 0.0063(12) 0.0143(11) Si4 0.0313(4) 0.0470(5) 0.0359(4) 0.0027(4) 0.0103(3) 0.0013(4) Si5 0.0330(4) 0.0339(4) 0.0422(5) 0.0066(3) 0.0097(3) 0.0023(3) C7 0.061(3) 0.095(3) 0.046(2) 0.024(2) 0.0071(19) -0.013(2) C8 0.046(2) 0.067(3) 0.072(3) -0.018(2) 0.0116(19) 0.0113(19) C9 0.049(2) 0.046(2) 0.058(2) -0.0010(17) 0.0062(17) -0.0036(16) C10 0.065(3) 0.054(2) 0.072(3) 0.029(2) 0.020(2) 0.0175(19) O5 0.0350(11) 0.0386(11) 0.0349(11) 0.0007(9) 0.0079(9) 0.0007(9) O6 0.0359(11) 0.0329(11) 0.0434(12) 0.0033(9) 0.0106(9) 0.0012(9) O7 0.0300(11) 0.0424(12) 0.0478(13) 0.0024(10) 0.0110(9) 0.0027(9) K101 0.0322(3) 0.0455(4) 0.0484(4) 0.0182(3) 0.0079(3) 0.0129(3) N101 0.0437(18) 0.077(2) 0.083(2) 0.037(2) 0.0097(17) 0.0282(17) N102 0.0490(17) 0.0490(16) 0.0566(18) 0.0205(14) 0.0073(14) 0.0166(14) O101 0.0385(14) 0.0570(16) 0.089(2) 0.0208(14) 0.0175(13) 0.0085(12) O102 0.0503(15) 0.0604(16) 0.0577(15) 0.0218(13) 0.0167(12) 0.0068(12) O103 0.0547(16) 0.0499(14) 0.082(2) 0.0203(14) 0.0197(14) 0.0222(12) O104 0.0471(14) 0.0494(14) 0.0576(15) 0.0116(11) 0.0084(12) 0.0076(11) O105 0.0523(15) 0.0808(19) 0.0544(15) 0.0289(14) 0.0041(12) 0.0184(14) O106 0.0545(15) 0.0560(15) 0.0534(15) 0.0091(12) 0.0071(12) 0.0168(12) C101 0.058(3) 0.095(4) 0.116(4) 0.046(3) 0.033(3) 0.045(3) C102 0.039(2) 0.118(4) 0.104(4) 0.045(3) 0.019(2) 0.027(3) C103 0.045(2) 0.055(2) 0.076(3) 0.001(2) 0.026(2) -0.0014(18) C104 0.067(3) 0.054(2) 0.065(3) 0.0147(19) 0.030(2) 0.0042(19) C105 0.073(3) 0.052(2) 0.065(2) 0.0286(19) 0.016(2) 0.011(2) C106 0.068(3) 0.050(2) 0.081(3) 0.027(2) 0.011(2) 0.020(2) C107 0.066(3) 0.071(3) 0.116(4) 0.051(3) 0.019(3) 0.036(2) C108 0.077(3) 0.054(2) 0.121(4) 0.031(3) 0.026(3) 0.033(2) C109 0.079(3) 0.047(2) 0.071(3) 0.0058(19) 0.022(2) 0.012(2) C110 0.056(2) 0.050(2) 0.061(2) 0.0030(18) 0.0090(19) 0.0027(18) C111 0.0385(19) 0.065(2) 0.059(2) 0.0179(19) -0.0036(16) 0.0114(17) C112 0.053(2) 0.067(3) 0.072(3) 0.030(2) -0.006(2) 0.016(2) C113 0.058(3) 0.097(4) 0.090(3) 0.045(3) -0.001(2) 0.030(3) C114 0.067(3) 0.092(3) 0.067(3) 0.038(2) -0.001(2) 0.035(2) C115 0.056(2) 0.071(3) 0.055(2) 0.016(2) 0.0019(19) 0.008(2) C116 0.055(2) 0.064(2) 0.046(2) 0.0048(18) 0.0063(17) 0.0060(19) C117 0.060(2) 0.060(2) 0.062(2) 0.0117(19) 0.018(2) 0.022(2) C118 0.058(2) 0.070(3) 0.075(3) 0.025(2) 0.019(2) 0.034(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.889(3) . ? Fe1 O4 1.904(2) . ? Fe1 O5 2.076(2) . ? Fe1 O6 2.087(2) . ? Fe1 Si11 2.842(9) . ? Fe2 O5 1.980(2) . ? Fe2 O5 1.980(2) 2 ? Fe2 O6 1.985(2) . ? Fe2 O6 1.985(2) 2 ? O1 Si11 1.572(9) . ? O1 Si1 1.581(3) . ? Si1 O2 1.621(5) . ? Si1 C1 1.857(5) . ? Si1 C2 1.861(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O2 Si2 1.603(6) . ? Si2 O3 1.599(3) . ? Si2 C3 1.825(6) . ? Si2 C4 1.847(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O3 Si3 1.651(3) . ? Si3 O4 1.588(2) . ? Si3 C5 1.862(6) . ? Si3 C6 1.865(10) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? Si11 O11 1.60(3) . ? Si11 C11 1.848(10) . ? Si11 C12 1.86(7) . ? C11 H21A 0.9800 . ? C11 H21B 0.9800 . ? C11 H21C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O11 Si12 1.59(3) . ? Si12 O4 1.516(11) . ? Si12 C14 1.86(2) . ? Si12 C13 1.87(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? Si4 O5 1.614(2) . ? Si4 O7 1.639(2) . ? Si4 C8 1.850(4) . ? Si4 C7 1.863(4) . ? Si5 O6 1.616(2) . ? Si5 O7 1.641(2) 2 ? Si5 C9 1.857(4) . ? Si5 C10 1.868(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H20A 0.9800 . ? C10 H20B 0.9800 . ? C10 H20C 0.9800 . ? O7 Si5 1.641(2) 2 ? K101 O105 2.765(3) . ? K101 O106 2.807(3) . ? K101 O102 2.814(3) . ? K101 O103 2.837(3) . ? K101 O101 2.859(3) . ? K101 O104 2.876(3) . ? K101 N101 2.914(3) . ? K101 N102 3.005(3) . ? N101 C113 1.456(6) . ? N101 C107 1.464(6) . ? N101 C101 1.474(6) . ? N102 C106 1.457(5) . ? N102 C112 1.468(5) . ? N102 C118 1.479(5) . ? O101 C103 1.396(5) . ? O101 C102 1.398(5) . ? O102 C104 1.404(5) . ? O102 C105 1.422(5) . ? O103 C109 1.401(5) . ? O103 C108 1.411(5) . ? O104 C111 1.408(5) . ? O104 C110 1.411(5) . ? O105 C115 1.392(5) . ? O105 C114 1.427(5) . ? O106 C117 1.391(5) . ? O106 C116 1.431(5) . ? C101 C102 1.492(7) . ? C101 H10Q 0.9900 . ? C101 H10R 0.9900 . ? C102 H10K 0.9900 . ? C102 H10L 0.9900 . ? C103 C104 1.485(6) . ? C103 H10M 0.9900 . ? C103 H10N 0.9900 . ? C104 H10C 0.9900 . ? C104 H10D 0.9900 . ? C105 C106 1.497(6) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10A 0.9900 . ? C106 H10B 0.9900 . ? C107 C108 1.474(7) . ? C107 H10G 0.9900 . ? C107 H10H 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.473(6) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.497(6) . ? C111 H11G 0.9900 . ? C111 H11H 0.9900 . ? C112 H11K 0.9900 . ? C112 H11L 0.9900 . ? C113 C114 1.495(7) . ? C113 H11Q 0.9900 . ? C113 H11R 0.9900 . ? C114 H11O 0.9900 . ? C114 H11P 0.9900 . ? C115 C116 1.468(6) . ? C115 H11I 0.9900 . ? C115 H11J 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.511(6) . ? C117 H11C 0.9900 . ? C117 H11D 0.9900 . ? C118 H11E 0.9900 . ? C118 H11F 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O4 117.23(11) . . ? O1 Fe1 O5 108.88(12) . . ? O4 Fe1 O5 117.93(10) . . ? O1 Fe1 O6 118.64(12) . . ? O4 Fe1 O6 110.05(10) . . ? O5 Fe1 O6 78.39(8) . . ? O1 Fe1 Si11 31.3(2) . . ? O4 Fe1 Si11 86.7(2) . . ? O5 Fe1 Si11 135.0(3) . . ? O6 Fe1 Si11 130.7(2) . . ? O5 Fe2 O5 180.00(11) . 2 ? O5 Fe2 O6 83.12(8) . . ? O5 Fe2 O6 96.88(8) 2 . ? O5 Fe2 O6 96.88(8) . 2 ? O5 Fe2 O6 83.12(8) 2 2 ? O6 Fe2 O6 180.00(17) . 2 ? Si11 O1 Fe1 110.1(4) . . ? Si1 O1 Fe1 143.76(18) . . ? O1 Si1 O2 113.9(3) . . ? O1 Si1 C1 111.8(2) . . ? O2 Si1 C1 103.5(3) . . ? O1 Si1 C2 109.8(2) . . ? O2 Si1 C2 110.1(4) . . ? C1 Si1 C2 107.4(3) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 O2 Si1 144.8(3) . . ? O3 Si2 O2 112.0(3) . . ? O3 Si2 C3 111.1(3) . . ? O2 Si2 C3 107.2(5) . . ? O3 Si2 C4 108.80(17) . . ? O2 Si2 C4 108.7(2) . . ? C3 Si2 C4 108.8(3) . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 O3 Si3 142.85(19) . . ? O4 Si3 O3 112.87(15) . . ? O4 Si3 C5 111.4(2) . . ? O3 Si3 C5 105.5(3) . . ? O4 Si3 C6 113.2(6) . . ? O3 Si3 C6 104.4(4) . . ? C5 Si3 C6 108.9(8) . . ? Si3 C5 H5A 109.5 . . ? Si3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 C6 H6A 109.5 . . ? Si3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 Si11 O11 120.5(10) . . ? O1 Si11 C11 121(2) . . ? O11 Si11 C11 95(2) . . ? O1 Si11 C12 122.6(19) . . ? O11 Si11 C12 96(2) . . ? C11 Si11 C12 95(3) . . ? O11 Si11 Fe1 82.1(9) . . ? C11 Si11 Fe1 127(2) . . ? C12 Si11 Fe1 138.7(18) . . ? Si11 C11 H21A 109.5 . . ? Si11 C11 H21B 109.5 . . ? H21A C11 H21B 109.5 . . ? Si11 C11 H21C 109.5 . . ? H21A C11 H21C 109.5 . . ? H21B C11 H21C 109.5 . . ? Si11 C12 H12A 109.5 . . ? Si11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si12 O11 Si11 134.5(15) . . ? O4 Si12 O11 113.2(10) . . ? O4 Si12 C14 108(4) . . ? O11 Si12 C14 109(6) . . ? O4 Si12 C13 105.7(16) . . ? O11 Si12 C13 108.5(18) . . ? C14 Si12 C13 113(7) . . ? Si12 C13 H13A 109.5 . . ? Si12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si12 C14 H14A 109.5 . . ? Si12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si12 O4 Fe1 118.0(5) . . ? Si3 O4 Fe1 139.60(16) . . ? O5 Si4 O7 108.97(11) . . ? O5 Si4 C8 111.89(17) . . ? O7 Si4 C8 108.38(16) . . ? O5 Si4 C7 110.05(16) . . ? O7 Si4 C7 108.55(18) . . ? C8 Si4 C7 108.9(2) . . ? O6 Si5 O7 109.44(12) . 2 ? O6 Si5 C9 111.89(15) . . ? O7 Si5 C9 106.68(16) 2 . ? O6 Si5 C10 109.69(16) . . ? O7 Si5 C10 108.64(17) 2 . ? C9 Si5 C10 110.4(2) . . ? Si4 C7 H7A 109.5 . . ? Si4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si4 C8 H8A 109.5 . . ? Si4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si5 C9 H9A 109.5 . . ? Si5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si5 C10 H20A 109.5 . . ? Si5 C10 H20B 109.5 . . ? H20A C10 H20B 109.5 . . ? Si5 C10 H20C 109.5 . . ? H20A C10 H20C 109.5 . . ? H20B C10 H20C 109.5 . . ? Si4 O5 Fe2 132.98(12) . . ? Si4 O5 Fe1 127.41(12) . . ? Fe2 O5 Fe1 99.50(9) . . ? Si5 O6 Fe2 130.53(13) . . ? Si5 O6 Fe1 129.19(12) . . ? Fe2 O6 Fe1 98.97(9) . . ? Si4 O7 Si5 132.35(14) . 2 ? O105 K101 O106 60.40(8) . . ? O105 K101 O102 122.88(9) . . ? O106 K101 O102 100.23(8) . . ? O105 K101 O103 100.17(9) . . ? O106 K101 O103 121.81(8) . . ? O102 K101 O103 131.33(9) . . ? O105 K101 O101 100.92(9) . . ? O106 K101 O101 140.54(8) . . ? O102 K101 O101 58.79(8) . . ? O103 K101 O101 94.30(8) . . ? O105 K101 O104 141.18(8) . . ? O106 K101 O104 100.99(8) . . ? O102 K101 O104 92.40(8) . . ? O103 K101 O104 58.72(8) . . ? O101 K101 O104 112.07(8) . . ? O105 K101 N101 61.71(10) . . ? O106 K101 N101 121.17(10) . . ? O102 K101 N101 119.12(9) . . ? O103 K101 N101 60.35(10) . . ? O101 K101 N101 60.97(9) . . ? O104 K101 N101 117.68(10) . . ? O105 K101 N102 120.87(9) . . ? O106 K101 N102 61.28(8) . . ? O102 K101 N102 60.26(8) . . ? O103 K101 N102 117.88(9) . . ? O101 K101 N102 117.96(9) . . ? O104 K101 N102 60.18(8) . . ? N101 K101 N102 177.38(10) . . ? C113 N101 C107 110.9(4) . . ? C113 N101 C101 109.1(4) . . ? C107 N101 C101 110.0(4) . . ? C113 N101 K101 107.5(3) . . ? C107 N101 K101 109.2(2) . . ? C101 N101 K101 110.1(3) . . ? C106 N102 C112 110.3(3) . . ? C106 N102 C118 110.2(3) . . ? C112 N102 C118 109.7(3) . . ? C106 N102 K101 108.9(2) . . ? C112 N102 K101 110.4(2) . . ? C118 N102 K101 107.3(2) . . ? C103 O101 C102 111.9(3) . . ? C103 O101 K101 113.7(2) . . ? C102 O101 K101 116.4(3) . . ? C104 O102 C105 112.8(3) . . ? C104 O102 K101 118.8(2) . . ? C105 O102 K101 119.3(2) . . ? C109 O103 C108 112.6(4) . . ? C109 O103 K101 115.6(2) . . ? C108 O103 K101 119.1(3) . . ? C111 O104 C110 111.5(3) . . ? C111 O104 K101 114.8(2) . . ? C110 O104 K101 116.2(2) . . ? C115 O105 C114 113.1(3) . . ? C115 O105 K101 116.4(2) . . ? C114 O105 K101 119.6(3) . . ? C117 O106 C116 113.5(3) . . ? C117 O106 K101 117.3(2) . . ? C116 O106 K101 114.7(2) . . ? N101 C101 C102 113.7(4) . . ? N101 C101 H10Q 108.8 . . ? C102 C101 H10Q 108.8 . . ? N101 C101 H10R 108.8 . . ? C102 C101 H10R 108.8 . . ? H10Q C101 H10R 107.7 . . ? O101 C102 C101 110.5(4) . . ? O101 C102 H10K 109.5 . . ? C101 C102 H10K 109.5 . . ? O101 C102 H10L 109.5 . . ? C101 C102 H10L 109.5 . . ? H10K C102 H10L 108.1 . . ? O101 C103 C104 110.1(3) . . ? O101 C103 H10M 109.6 . . ? C104 C103 H10M 109.6 . . ? O101 C103 H10N 109.6 . . ? C104 C103 H10N 109.6 . . ? H10M C103 H10N 108.2 . . ? O102 C104 C103 110.3(3) . . ? O102 C104 H10C 109.6 . . ? C103 C104 H10C 109.6 . . ? O102 C104 H10D 109.6 . . ? C103 C104 H10D 109.6 . . ? H10C C104 H10D 108.1 . . ? O102 C105 C106 110.2(3) . . ? O102 C105 H10I 109.6 . . ? C106 C105 H10I 109.6 . . ? O102 C105 H10J 109.6 . . ? C106 C105 H10J 109.6 . . ? H10I C105 H10J 108.1 . . ? N102 C106 C105 114.2(3) . . ? N102 C106 H10A 108.7 . . ? C105 C106 H10A 108.7 . . ? N102 C106 H10B 108.7 . . ? C105 C106 H10B 108.7 . . ? H10A C106 H10B 107.6 . . ? N101 C107 C108 113.9(4) . . ? N101 C107 H10G 108.8 . . ? C108 C107 H10G 108.8 . . ? N101 C107 H10H 108.8 . . ? C108 C107 H10H 108.8 . . ? H10G C107 H10H 107.7 . . ? O103 C108 C107 111.0(4) . . ? O103 C108 H10O 109.4 . . ? C107 C108 H10O 109.4 . . ? O103 C108 H10P 109.4 . . ? C107 C108 H10P 109.4 . . ? H10O C108 H10P 108.0 . . ? O103 C109 C110 110.4(3) . . ? O103 C109 H10E 109.6 . . ? C110 C109 H10E 109.6 . . ? O103 C109 H10F 109.6 . . ? C110 C109 H10F 109.6 . . ? H10E C109 H10F 108.1 . . ? O104 C110 C109 110.8(3) . . ? O104 C110 H11A 109.5 . . ? C109 C110 H11A 109.5 . . ? O104 C110 H11B 109.5 . . ? C109 C110 H11B 109.5 . . ? H11A C110 H11B 108.1 . . ? O104 C111 C112 110.1(3) . . ? O104 C111 H11G 109.6 . . ? C112 C111 H11G 109.6 . . ? O104 C111 H11H 109.6 . . ? C112 C111 H11H 109.6 . . ? H11G C111 H11H 108.2 . . ? N102 C112 C111 114.8(3) . . ? N102 C112 H11K 108.6 . . ? C111 C112 H11K 108.6 . . ? N102 C112 H11L 108.6 . . ? C111 C112 H11L 108.6 . . ? H11K C112 H11L 107.5 . . ? N101 C113 C114 115.1(4) . . ? N101 C113 H11Q 108.5 . . ? C114 C113 H11Q 108.5 . . ? N101 C113 H11R 108.5 . . ? C114 C113 H11R 108.5 . . ? H11Q C113 H11R 107.5 . . ? O105 C114 C113 109.3(3) . . ? O105 C114 H11O 109.8 . . ? C113 C114 H11O 109.8 . . ? O105 C114 H11P 109.8 . . ? C113 C114 H11P 109.8 . . ? H11O C114 H11P 108.3 . . ? O105 C115 C116 110.9(3) . . ? O105 C115 H11I 109.5 . . ? C116 C115 H11I 109.5 . . ? O105 C115 H11J 109.5 . . ? C116 C115 H11J 109.5 . . ? H11I C115 H11J 108.1 . . ? O106 C116 C115 111.1(3) . . ? O106 C116 H11M 109.4 . . ? C115 C116 H11M 109.4 . . ? O106 C116 H11N 109.4 . . ? C115 C116 H11N 109.4 . . ? H11M C116 H11N 108.0 . . ? O106 C117 C118 110.2(3) . . ? O106 C117 H11C 109.6 . . ? C118 C117 H11C 109.6 . . ? O106 C117 H11D 109.6 . . ? C118 C117 H11D 109.6 . . ? H11C C117 H11D 108.1 . . ? N102 C118 C117 114.7(3) . . ? N102 C118 H11E 108.6 . . ? C117 C118 H11E 108.6 . . ? N102 C118 H11F 108.6 . . ? C117 C118 H11F 108.6 . . ? H11E C118 H11F 107.6 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.861 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.060 _iucr_refine_instructions_details ; TITL p-1 in P-1 CELL 1.54178 10.6110 13.5342 16.7124 102.789 95.550 102.524 ZERR 1.00 0.0002 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N O K FE P SI UNIT 56 131 4 26 2 3 0 10 MERG 2 OMIT 0.00 133.00 ISOR 0.10 0.20 O11 ISOR 0.05 0.20 O2 DFIX 1.860 0.01 SI11 C11 DFIX 1.860 0.020 SI12 C14 EADP SI3 SI12 EADP SI1 SI11 EADP C11 C1 EADP C12 C2 EADP C13 C5 EADP C14 C6 FMAP 2 PLAN 100 SIZE 0.140 0.160 0.380 ACTA BOND $H L.S. 16 TEMP -123.00 WGHT 0.059800 2.661100 FVAR 0.45996 0.88534 FE1 6 -0.009366 0.184779 0.144708 11.00000 0.03492 0.03314 = 0.03359 0.00518 0.00536 0.00842 FE2 6 0.000000 0.000000 0.000000 10.50000 0.02685 0.03141 = 0.02859 0.00805 0.00491 0.00488 O1 4 0.029180 0.182045 0.256834 11.00000 0.12496 0.06309 = 0.03148 0.00423 0.00215 0.04952 PART 1 SI1 8 0.052626 0.250269 0.349378 21.00000 0.09105 0.05709 = 0.03326 0.00542 0.00674 0.04557 C1 1 0.029255 0.167716 0.424496 21.00000 0.06682 0.08110 = 0.04338 0.01594 0.00680 0.02707 AFIX 33 H1A 2 0.044003 0.212579 0.480967 21.00000 -1.50000 H1B 2 0.091477 0.123515 0.420104 21.00000 -1.50000 H1C 2 -0.060050 0.123478 0.412067 21.00000 -1.50000 AFIX 0 C2 1 0.223284 0.332344 0.376383 21.00000 0.13235 0.05238 = 0.07386 -0.01178 0.03380 0.01035 AFIX 33 H2A 2 0.237441 0.374127 0.433881 21.00000 -1.50000 H2B 2 0.237924 0.378929 0.339087 21.00000 -1.50000 H2C 2 0.284340 0.287190 0.370400 21.00000 -1.50000 AFIX 0 O2 4 -0.049390 0.322908 0.368108 21.00000 0.22472 0.17088 = 0.06784 0.03797 0.04446 0.16746 SI2 8 -0.132361 0.392547 0.330621 21.00000 0.04976 0.03556 = 0.04040 0.00924 0.01218 0.01557 C3 1 -0.291757 0.306882 0.282128 21.00000 0.10057 0.13413 = 0.11335 -0.04849 0.04673 -0.06659 AFIX 33 H3A 2 -0.333272 0.274999 0.323265 21.00000 -1.50000 H3B 2 -0.280680 0.251916 0.236130 21.00000 -1.50000 H3C 2 -0.346921 0.347725 0.260946 21.00000 -1.50000 AFIX 0 C4 1 -0.155308 0.496008 0.416691 21.00000 0.05395 0.04872 = 0.04289 0.01293 0.01528 0.01975 AFIX 33 H4A 2 -0.199084 0.463988 0.457020 21.00000 -1.50000 H4B 2 -0.208979 0.537353 0.394760 21.00000 -1.50000 H4C 2 -0.070035 0.541567 0.443951 21.00000 -1.50000 AFIX 0 O3 4 -0.060913 0.446104 0.265487 21.00000 0.08586 0.04190 = 0.04365 0.00282 0.02534 -0.00003 SI3 8 -0.039626 0.424998 0.167151 21.00000 0.06755 0.03059 = 0.03512 0.00982 0.01374 0.00859 C5 1 -0.159915 0.482166 0.116022 21.00000 0.15330 0.05436 = 0.08141 0.00583 -0.01508 0.05461 AFIX 33 H5A 2 -0.145679 0.556152 0.144359 21.00000 -1.50000 H5B 2 -0.248688 0.444729 0.119077 21.00000 -1.50000 H5C 2 -0.148679 0.475701 0.057723 21.00000 -1.50000 AFIX 0 C6 1 0.128476 0.504607 0.169438 21.00000 0.10212 0.06231 = 0.07973 -0.01020 0.04584 -0.01948 AFIX 33 H6A 2 0.135001 0.577736 0.197197 21.00000 -1.50000 H6B 2 0.146702 0.499795 0.112511 21.00000 -1.50000 H6C 2 0.192046 0.478115 0.199807 21.00000 -1.50000 AFIX 0 PART 2 SI11 8 0.046419 0.294010 0.315147 -21.00000 0.09105 0.05709 = 0.03326 0.00542 0.00674 0.04557 C11 1 -0.073943 0.321196 0.384551 -21.00000 0.06682 0.08110 = 0.04338 0.01594 0.00680 0.02707 AFIX 33 H21A 2 -0.039826 0.390277 0.423006 -21.00000 -1.50000 H21B 2 -0.089922 0.267901 0.416132 -21.00000 -1.50000 H21C 2 -0.155925 0.319832 0.351331 -21.00000 -1.50000 AFIX 0 C12 1 0.191210 0.358559 0.396458 -21.00000 0.13235 0.05238 = 0.07386 -0.01178 0.03380 0.01035 AFIX 33 H12A 2 0.181080 0.426395 0.426946 -21.00000 -1.50000 H12B 2 0.270186 0.368957 0.370285 -21.00000 -1.50000 H12C 2 0.198662 0.314338 0.434989 -21.00000 -1.50000 AFIX 0 O11 4 0.046544 0.392213 0.276687 -21.00000 0.09152 0.02852 = 0.06838 -0.00769 0.02867 0.02501 SI12 8 -0.012505 0.406564 0.190128 -21.00000 0.06755 0.03059 = 0.03512 0.00982 0.01374 0.00859 C13 1 -0.160294 0.458828 0.204714 -21.00000 0.15330 0.05436 = 0.08141 0.00583 -0.01508 0.05461 AFIX 33 H13A 2 -0.135953 0.525133 0.247342 -21.00000 -1.50000 H13B 2 -0.226134 0.408397 0.222203 -21.00000 -1.50000 H13C 2 -0.196238 0.470342 0.152240 -21.00000 -1.50000 AFIX 0 C14 1 0.116135 0.494447 0.152555 -21.00000 0.10212 0.06231 = 0.07973 -0.01020 0.04584 -0.01948 AFIX 33 H14A 2 0.147602 0.561207 0.194350 -21.00000 -1.50000 H14B 2 0.079578 0.506725 0.100542 -21.00000 -1.50000 H14C 2 0.188955 0.461679 0.142991 -21.00000 -1.50000 AFIX 0 PART 0 O4 4 -0.059390 0.304643 0.123813 11.00000 0.07182 0.03695 = 0.04160 0.00731 0.00630 0.01431 SI4 8 -0.261030 -0.022627 0.093398 11.00000 0.03134 0.04703 = 0.03595 0.00271 0.01029 0.00134 SI5 8 0.247489 0.205274 0.042182 11.00000 0.03301 0.03388 = 0.04221 0.00663 0.00970 0.00232 C7 1 -0.242847 -0.064589 0.191924 11.00000 0.06063 0.09486 = 0.04553 0.02358 0.00711 -0.01320 AFIX 33 H7A 2 -0.328409 -0.101693 0.200856 11.00000 -1.50000 H7B 2 -0.207112 -0.003011 0.238366 11.00000 -1.50000 H7C 2 -0.183456 -0.111136 0.188376 11.00000 -1.50000 AFIX 0 C8 1 -0.380163 0.059365 0.098907 11.00000 0.04602 0.06731 = 0.07172 -0.01797 0.01159 0.01133 AFIX 33 H8A 2 -0.463816 0.019577 0.108365 11.00000 -1.50000 H8B 2 -0.392535 0.079867 0.046568 11.00000 -1.50000 H8C 2 -0.347235 0.122079 0.144707 11.00000 -1.50000 AFIX 0 C9 1 0.366176 0.272965 0.138012 11.00000 0.04876 0.04566 = 0.05828 -0.00095 0.00620 -0.00362 AFIX 33 H9A 2 0.445385 0.313045 0.123436 11.00000 -1.50000 H9B 2 0.388570 0.221128 0.165844 11.00000 -1.50000 H9C 2 0.327191 0.320435 0.175317 11.00000 -1.50000 AFIX 0 C10 1 0.208740 0.301837 -0.014738 11.00000 0.06530 0.05398 = 0.07240 0.02883 0.01996 0.01749 AFIX 33 H20A 2 0.289744 0.342684 -0.026695 11.00000 -1.50000 H20B 2 0.165415 0.348811 0.019554 11.00000 -1.50000 H20C 2 0.150734 0.264673 -0.066934 11.00000 -1.50000 AFIX 0 O5 4 -0.120817 0.038636 0.077830 11.00000 0.03495 0.03864 = 0.03494 0.00071 0.00788 0.00068 O6 4 0.114260 0.137731 0.062119 11.00000 0.03593 0.03287 = 0.04339 0.00326 0.01060 0.00116 O7 4 -0.318817 -0.126931 0.016598 11.00000 0.02996 0.04241 = 0.04782 0.00237 0.01097 0.00266 K101 5 0.615872 0.191064 0.717759 11.00000 0.03221 0.04549 = 0.04842 0.01823 0.00795 0.01290 N101 3 0.794348 0.069425 0.762856 11.00000 0.04365 0.07714 = 0.08263 0.03739 0.00972 0.02823 N102 3 0.429409 0.310274 0.663310 11.00000 0.04898 0.04897 = 0.05657 0.02052 0.00732 0.01665 O101 4 0.851333 0.200659 0.646661 11.00000 0.03847 0.05703 = 0.08902 0.02079 0.01748 0.00846 O102 4 0.696149 0.337117 0.625008 11.00000 0.05027 0.06036 = 0.05773 0.02179 0.01672 0.00680 O103 4 0.535929 -0.030439 0.671068 11.00000 0.05475 0.04986 = 0.08236 0.02026 0.01969 0.02217 O104 4 0.388066 0.082813 0.597092 11.00000 0.04710 0.04941 = 0.05759 0.01164 0.00838 0.00760 O105 4 0.711251 0.223651 0.883831 11.00000 0.05230 0.08082 = 0.05440 0.02891 0.00409 0.01840 O106 4 0.506397 0.310549 0.838866 11.00000 0.05451 0.05602 = 0.05344 0.00908 0.00710 0.01680 C101 1 0.887628 0.061164 0.703272 11.00000 0.05808 0.09541 = 0.11557 0.04563 0.03256 0.04526 AFIX 23 H10Q 2 0.841987 0.010667 0.650778 11.00000 -1.20000 H10R 2 0.958227 0.033053 0.725794 11.00000 -1.20000 AFIX 0 C102 1 0.947183 0.162505 0.684806 11.00000 0.03874 0.11835 = 0.10425 0.04548 0.01932 0.02663 AFIX 23 H10K 2 0.991817 0.214064 0.737031 11.00000 -1.20000 H10L 2 1.013192 0.152417 0.647777 11.00000 -1.20000 AFIX 0 C103 1 0.903414 0.297505 0.631447 11.00000 0.04545 0.05502 = 0.07573 0.00144 0.02625 -0.00142 AFIX 23 H10M 2 0.978221 0.293139 0.600871 11.00000 -1.20000 H10N 2 0.935579 0.350677 0.684806 11.00000 -1.20000 AFIX 0 C104 1 0.802186 0.329070 0.581899 11.00000 0.06707 0.05378 = 0.06533 0.01469 0.02984 0.00424 AFIX 23 H10C 2 0.840302 0.397236 0.570624 11.00000 -1.20000 H10D 2 0.771542 0.276697 0.528008 11.00000 -1.20000 AFIX 0 C105 1 0.600695 0.375113 0.583331 11.00000 0.07349 0.05157 = 0.06549 0.02858 0.01558 0.01116 AFIX 23 H10I 2 0.555668 0.321716 0.532132 11.00000 -1.20000 H10J 2 0.643857 0.438809 0.567262 11.00000 -1.20000 AFIX 0 C106 1 0.502980 0.399918 0.638650 11.00000 0.06768 0.05046 = 0.08085 0.02708 0.01060 0.01967 AFIX 23 H10A 2 0.549243 0.453843 0.689263 11.00000 -1.20000 H10B 2 0.440794 0.430071 0.609606 11.00000 -1.20000 AFIX 0 C107 1 0.719123 -0.034899 0.763021 11.00000 0.06572 0.07086 = 0.11561 0.05116 0.01909 0.03609 AFIX 23 H10G 2 0.669316 -0.028749 0.810256 11.00000 -1.20000 H10H 2 0.780572 -0.078385 0.771922 11.00000 -1.20000 AFIX 0 C108 1 0.627356 -0.088517 0.685886 11.00000 0.07668 0.05384 = 0.12080 0.03066 0.02619 0.03272 AFIX 23 H10O 2 0.676711 -0.098277 0.638599 11.00000 -1.20000 H10P 2 0.580620 -0.158434 0.690194 11.00000 -1.20000 AFIX 0 C109 1 0.454406 -0.074339 0.594555 11.00000 0.07897 0.04678 = 0.07104 0.00581 0.02161 0.01216 AFIX 23 H10E 2 0.421260 -0.150429 0.587674 11.00000 -1.20000 H10F 2 0.504856 -0.063983 0.548975 11.00000 -1.20000 AFIX 0 C110 1 0.343632 -0.025321 0.590065 11.00000 0.05647 0.04964 = 0.06103 0.00301 0.00900 0.00270 AFIX 23 H11A 2 0.285283 -0.058707 0.536548 11.00000 -1.20000 H11B 2 0.292814 -0.036297 0.635368 11.00000 -1.20000 AFIX 0 C111 1 0.284272 0.132408 0.599828 11.00000 0.03854 0.06536 = 0.05886 0.01787 -0.00362 0.01143 AFIX 23 H11G 2 0.248757 0.131900 0.652416 11.00000 -1.20000 H11H 2 0.213434 0.093891 0.553241 11.00000 -1.20000 AFIX 0 C112 1 0.330990 0.242784 0.593874 11.00000 0.05335 0.06745 = 0.07193 0.03007 -0.00618 0.01649 AFIX 23 H11K 2 0.368182 0.241922 0.541705 11.00000 -1.20000 H11L 2 0.254877 0.273763 0.590366 11.00000 -1.20000 AFIX 0 C113 1 0.865854 0.124575 0.845052 11.00000 0.05833 0.09741 = 0.09013 0.04492 -0.00115 0.03028 AFIX 23 H11Q 2 0.927780 0.188532 0.840401 11.00000 -1.20000 H11R 2 0.917963 0.079645 0.864529 11.00000 -1.20000 AFIX 0 C114 1 0.783011 0.155149 0.909173 11.00000 0.06706 0.09234 = 0.06674 0.03764 -0.00146 0.03516 AFIX 23 H11O 2 0.721911 0.092003 0.915932 11.00000 -1.20000 H11P 2 0.838981 0.190658 0.963231 11.00000 -1.20000 AFIX 0 C115 1 0.631398 0.256283 0.940323 11.00000 0.05626 0.07067 = 0.05534 0.01608 0.00187 0.00843 AFIX 23 H11I 2 0.681821 0.279870 0.997025 11.00000 -1.20000 H11J 2 0.557455 0.196831 0.939203 11.00000 -1.20000 AFIX 0 C116 1 0.580849 0.342082 0.920303 11.00000 0.05513 0.06427 = 0.04598 0.00477 0.00627 0.00604 AFIX 23 H11M 2 0.525071 0.364376 0.961519 11.00000 -1.20000 H11N 2 0.654720 0.402505 0.923571 11.00000 -1.20000 AFIX 0 C117 1 0.454802 0.388671 0.817059 11.00000 0.06045 0.06004 = 0.06209 0.01173 0.01780 0.02237 AFIX 23 H11C 2 0.526629 0.446681 0.812610 11.00000 -1.20000 H11D 2 0.405889 0.416598 0.860685 11.00000 -1.20000 AFIX 0 C118 1 0.364673 0.345718 0.735099 11.00000 0.05822 0.07020 = 0.07462 0.02480 0.01928 0.03447 AFIX 23 H11E 2 0.295439 0.286124 0.739931 11.00000 -1.20000 H11F 2 0.321828 0.400460 0.724050 11.00000 -1.20000 HKLF 4 REM p-1 in P-1 REM R1 = 0.0480 for 7053 Fo > 4sig(Fo) and 0.0544 for all 7970 data REM 485 parameters refined using 14 restraints END WGHT 0.0598 2.6610 REM Highest difference peak 0.861, deepest hole -0.655, 1-sigma level 0.060 Q1 1 -0.1312 0.3045 0.2954 11.00000 0.05 0.86 Q2 1 0.1183 0.2926 0.3438 11.00000 0.05 0.77 Q3 1 0.0246 0.3755 0.3550 11.00000 0.05 0.67 Q4 1 0.0767 0.1957 0.3581 11.00000 0.05 0.59 Q5 1 0.0039 0.1546 0.1782 11.00000 0.05 0.52 Q6 1 0.8824 0.2138 0.7072 11.00000 0.05 0.49 Q7 1 0.6632 0.2799 0.8977 11.00000 0.05 0.42 Q8 1 -0.0020 0.3183 0.3127 11.00000 0.05 0.41 Q9 1 0.7815 0.1031 0.8253 11.00000 0.05 0.38 Q10 1 -0.0890 0.2790 0.1993 11.00000 0.05 0.36 Q11 1 -0.0639 0.2474 0.3766 11.00000 0.05 0.33 Q12 1 0.9088 0.1011 0.7736 11.00000 0.05 0.32 Q13 1 0.0624 0.2141 0.1514 11.00000 0.05 0.32 Q14 1 0.7064 0.2708 0.5845 11.00000 0.05 0.31 Q15 1 0.0431 -0.0343 0.0276 11.00000 0.05 0.31 Q16 1 0.9695 0.1962 0.7565 11.00000 0.05 0.31 Q17 1 0.2035 0.2387 0.0170 11.00000 0.05 0.30 Q18 1 0.7097 0.0106 0.8397 11.00000 0.05 0.30 Q19 1 -0.2644 -0.1396 0.0425 11.00000 0.05 0.30 Q20 1 -0.0777 0.0058 0.0877 11.00000 0.05 0.30 Q21 1 0.0979 0.1428 0.2624 11.00000 0.05 0.29 Q22 1 -0.1453 0.4443 0.2419 11.00000 0.05 0.28 Q23 1 0.7079 0.2011 0.9437 11.00000 0.05 0.27 Q24 1 0.5330 0.4026 0.8993 11.00000 0.05 0.26 Q25 1 -0.1332 0.4593 0.3703 11.00000 0.05 0.26 Q26 1 -0.0874 0.0777 0.1048 11.00000 0.05 0.26 Q27 1 0.4785 0.3353 0.7965 11.00000 0.05 0.25 Q28 1 0.1667 0.1564 0.0639 11.00000 0.05 0.25 Q29 1 -0.3333 0.0124 0.0928 11.00000 0.05 0.25 Q30 1 -0.3145 0.3181 0.2660 11.00000 0.05 0.25 Q31 1 0.2645 0.1552 0.0096 11.00000 0.05 0.24 Q32 1 0.4495 0.4140 0.7630 11.00000 0.05 0.24 Q33 1 -0.2360 -0.0415 0.1421 11.00000 0.05 0.24 Q34 1 -0.0061 0.1530 0.1123 11.00000 0.05 0.24 Q35 1 -0.1769 0.0199 0.0879 11.00000 0.05 0.24 Q36 1 -0.0988 0.3775 0.2597 11.00000 0.05 0.24 Q37 1 0.4012 -0.0607 0.6419 11.00000 0.05 0.23 Q38 1 0.2861 0.3632 0.0113 11.00000 0.05 0.23 Q39 1 0.4592 0.4041 0.7371 11.00000 0.05 0.23 Q40 1 0.6788 0.2161 0.7106 11.00000 0.05 0.22 Q41 1 -0.2144 0.3024 0.3119 11.00000 0.05 0.22 Q42 1 0.1263 0.1596 0.0296 11.00000 0.05 0.21 Q43 1 0.0852 0.2403 0.2740 11.00000 0.05 0.21 Q44 1 -0.0996 0.0464 0.0467 11.00000 0.05 0.21 Q45 1 0.0991 0.1282 0.0838 11.00000 0.05 0.20 Q46 1 0.8365 0.2661 0.5837 11.00000 0.05 0.20 Q47 1 0.0841 0.2242 0.2396 11.00000 0.05 0.20 Q48 1 0.5801 0.2167 0.6921 11.00000 0.05 0.20 Q49 1 0.2983 0.3583 0.3990 11.00000 0.05 0.20 Q50 1 0.0592 0.4387 0.1666 11.00000 0.05 0.20 Q51 1 0.1653 0.3613 0.4182 11.00000 0.05 0.19 Q52 1 -0.0762 0.5924 0.1616 11.00000 0.05 0.19 Q53 1 0.9083 0.2281 0.6012 11.00000 0.05 0.19 Q54 1 0.1186 0.3168 -0.0076 11.00000 0.05 0.18 Q55 1 0.0109 0.2258 0.4082 11.00000 0.05 0.18 Q56 1 0.4260 0.2427 0.6287 11.00000 0.05 0.18 Q57 1 -0.0779 0.2401 0.2628 11.00000 0.05 0.18 Q58 1 0.0269 0.5987 0.1563 11.00000 0.05 0.18 Q59 1 0.0748 0.0351 0.0032 11.00000 0.05 0.18 Q60 1 0.3545 0.1047 0.6424 11.00000 0.05 0.18 Q61 1 0.7304 -0.0588 0.6973 11.00000 0.05 0.18 Q62 1 -0.0785 0.1783 0.1507 11.00000 0.05 0.18 Q63 1 -0.0225 0.3998 0.2319 11.00000 0.05 0.18 Q64 1 0.6160 0.2477 0.7557 11.00000 0.05 0.18 Q65 1 0.5710 0.3063 0.9561 11.00000 0.05 0.18 Q66 1 0.0782 0.1028 0.0319 11.00000 0.05 0.17 Q67 1 -0.0132 0.2050 0.4006 11.00000 0.05 0.17 Q68 1 0.0934 0.3029 0.2480 11.00000 0.05 0.17 Q69 1 -0.1443 0.4625 0.1646 11.00000 0.05 0.17 Q70 1 -0.1594 -0.0335 0.2270 11.00000 0.05 0.17 Q71 1 0.3400 0.2729 0.1744 11.00000 0.05 0.17 Q72 1 0.4417 0.3822 0.7104 11.00000 0.05 0.16 Q73 1 0.5168 0.3538 0.5929 11.00000 0.05 0.16 Q74 1 0.6134 0.3278 0.8372 11.00000 0.05 0.16 Q75 1 0.3314 0.3076 0.6555 11.00000 0.05 0.16 Q76 1 -0.3570 0.1289 0.0984 11.00000 0.05 0.16 Q77 1 0.4162 0.1856 0.5253 11.00000 0.05 0.16 Q78 1 0.4351 0.2181 0.5302 11.00000 0.05 0.16 Q79 1 0.4864 0.0857 0.6012 11.00000 0.05 0.16 Q80 1 -0.2750 -0.0855 0.0219 11.00000 0.05 0.16 Q81 1 0.4764 0.2958 0.6181 11.00000 0.05 0.15 Q82 1 -0.0480 0.4458 0.3254 11.00000 0.05 0.15 Q83 1 -0.0833 0.2449 0.1355 11.00000 0.05 0.15 Q84 1 0.0255 0.2625 0.3653 11.00000 0.05 0.15 Q85 1 -0.1612 0.3211 0.2197 11.00000 0.05 0.15 Q86 1 0.9528 0.1790 0.5471 11.00000 0.05 0.15 Q87 1 -0.4015 0.0581 0.1334 11.00000 0.05 0.15 Q88 1 -0.0977 0.2026 0.4277 11.00000 0.05 0.15 Q89 1 -0.2456 0.3872 0.3248 11.00000 0.05 0.15 Q90 1 -0.0159 0.0942 0.3861 11.00000 0.05 0.15 Q91 1 0.6026 0.1223 0.6904 11.00000 0.05 0.15 Q92 1 0.8015 0.1837 0.7642 11.00000 0.05 0.15 Q93 1 0.0177 0.1686 0.2722 11.00000 0.05 0.14 Q94 1 -0.0229 0.2049 0.2275 11.00000 0.05 0.14 Q95 1 -0.0614 0.3354 0.1389 11.00000 0.05 0.14 Q96 1 0.8644 0.1751 0.9021 11.00000 0.05 0.14 Q97 1 0.0137 0.0621 0.0280 11.00000 0.05 0.14 Q98 1 -0.0625 0.2184 0.4389 11.00000 0.05 0.14 Q99 1 -0.2119 0.0366 0.1039 11.00000 0.05 0.14 Q100 1 0.2014 0.3649 0.3586 11.00000 0.05 0.14 ; _database_code_depnum_ccdc_archive 'CCDC 962254'