#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100755.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100755 _publ_requested_journal 'Inorganic Chemistry' loop_ _publ_author_name 'Panagiotis Angaridis' ' Jeff W. Kampf ' 'Vincent L. Pecoraro' _chemical_formula_moiety '2(C39 H53 N4 O6 Fe), 2.5(C2 H3 N)' _chemical_formula_sum 'C41.50 H56.75 Fe N5.25 O6' _chemical_formula_weight 781.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.1085(11) _cell_length_b 17.2305(13) _cell_length_c 18.5398(14) _cell_angle_alpha 109.456(4) _cell_angle_beta 111.060(4) _cell_angle_gamma 90.560(4) _cell_volume 4200.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5529 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 23.31 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1666 _exptl_absorpt_coefficient_mu 0.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8533 _exptl_absorpt_correction_T_max 0.9525 _exptl_absorpt_process_details ; Blessing, R. Acta Cryst. (1995) A51 33-38 Sheldrick, G. TWINABS (Version 1.05), Bruker Nonius scaling and corrections for twinned crystals University of Gottingen, Germany 2003. ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37984 _diffrn_reflns_av_R_equivalents 0.1247 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 23.66 _reflns_number_total 26563 _reflns_number_gt 17077 _reflns_threshold_expression >2sigma(I) _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^)+(0.1378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 26563 _refine_ls_number_parameters 1028 _refine_ls_number_restraints 87 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2148 _refine_ls_wR_factor_gt 0.1898 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.992 _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 Fe1 Fe 0.35618(3) 0.34894(3) -0.00036(3) 0.01788(13) Uani 1 1 d . . . Fe2 Fe 0.85982(3) 0.15413(3) 0.00497(3) 0.01790(13) Uani 1 1 d . . . N1 N 0.34828(17) 0.23743(15) -0.09691(15) 0.0187(7) Uani 1 1 d . . . N2 N 0.48737(17) 0.38000(15) -0.00595(14) 0.0185(7) Uani 1 1 d . . . N3 N 0.44191(16) 0.30576(15) 0.09904(15) 0.0183(7) Uani 1 1 d . . . N4 N 0.53955(17) 0.31498(16) 0.22321(15) 0.0227(8) Uani 1 1 d . . . N5 N 0.85344(16) 0.19754(15) -0.09045(15) 0.0186(7) Uani 1 1 d . . . N6 N 0.98854(16) 0.11705(15) -0.00456(14) 0.0176(7) Uani 1 1 d . . . N7 N 0.94552(16) 0.26738(15) 0.10493(15) 0.0184(7) Uani 1 1 d . . . N8 N 1.04549(17) 0.34832(16) 0.23154(15) 0.0227(8) Uani 1 1 d . . . N9 N 0.6911(2) 0.1757(2) 0.3857(2) 0.0535(11) Uani 1 1 d . . . C1 C 0.2732(2) 0.20571(19) -0.16498(18) 0.0224(9) Uani 1 1 d . . . H1A H 0.2750 0.1532 -0.2028 0.027 Uiso 1 1 calc R . . C2 C 0.1868(2) 0.24263(19) -0.18900(18) 0.0194(9) Uani 1 1 d . . . C3 C 0.1802(2) 0.32431(19) -0.14499(18) 0.0191(9) Uani 1 1 d . . . C4 C 0.0914(2) 0.35614(19) -0.17188(18) 0.0194(9) Uani 1 1 d . . . C5 C 0.0194(2) 0.3058(2) -0.24302(19) 0.0238(9) Uani 1 1 d . . . H5A H -0.0391 0.3269 -0.2615 0.029 Uiso 1 1 calc R . . C6 C 0.0260(2) 0.2242(2) -0.29144(19) 0.0246(10) Uani 1 1 d . . . C7 C 0.1109(2) 0.1946(2) -0.26215(18) 0.0213(9) Uani 1 1 d . . . H7A H 0.1181 0.1402 -0.2925 0.026 Uiso 1 1 calc R . . C8 C 0.0801(2) 0.4435(2) -0.1201(2) 0.0242(10) Uani 1 1 d . . . C9 C 0.1537(2) 0.5104(2) -0.1132(2) 0.0270(10) Uani 1 1 d . . . H9A H 0.1434 0.5100 -0.1686 0.041 Uiso 1 1 calc R . . H9B H 0.2186 0.4988 -0.0874 0.041 Uiso 1 1 calc R . . H9C H 0.1461 0.5652 -0.0791 0.041 Uiso 1 1 calc R . . C10 C 0.0951(2) 0.4465(2) -0.03241(19) 0.0246(10) Uani 1 1 d . . . H10A H 0.0900 0.5025 0.0012 0.037 Uiso 1 1 calc R . . H10B H 0.1588 0.4327 -0.0066 0.037 Uiso 1 1 calc R . . H10C H 0.0460 0.4061 -0.0361 0.037 Uiso 1 1 calc R . . C11 C -0.0192(2) 0.4656(2) -0.1586(2) 0.0319(11) Uani 1 1 d . . . H11A H -0.0245 0.5204 -0.1228 0.048 Uiso 1 1 calc R . . H11B H -0.0682 0.4237 -0.1643 0.048 Uiso 1 1 calc R . . H11C H -0.0288 0.4668 -0.2133 0.048 Uiso 1 1 calc R . . C12 C -0.0568(2) 0.1766(2) -0.3741(2) 0.0341(11) Uani 1 1 d . . . C13 C -0.0423(3) 0.0861(2) -0.4110(2) 0.0508(15) Uani 1 1 d . . . H13A H -0.0990 0.0561 -0.4609 0.076 Uiso 1 1 calc R . . H13B H -0.0325 0.0593 -0.3702 0.076 Uiso 1 1 calc R . . H13C H 0.0141 0.0850 -0.4256 0.076 Uiso 1 1 calc R . . C14 C -0.0621(3) 0.2182(3) -0.4359(2) 0.0664(16) Uani 1 1 d . . . H14A H -0.1128 0.1863 -0.4896 0.100 Uiso 1 1 calc R . . H14B H -0.0005 0.2201 -0.4422 0.100 Uiso 1 1 calc R . . H14C H -0.0762 0.2750 -0.4157 0.100 Uiso 1 1 calc R . . C15 C -0.1521(2) 0.1748(2) -0.3628(2) 0.0446(13) Uani 1 1 d . . . H15A H -0.1661 0.2317 -0.3436 0.067 Uiso 1 1 calc R . . H15B H -0.1477 0.1494 -0.3218 0.067 Uiso 1 1 calc R . . H15C H -0.2034 0.1421 -0.4158 0.067 Uiso 1 1 calc R . . C16 C 0.4314(2) 0.1935(2) -0.0855(2) 0.0245(10) Uani 1 1 d . . . H16A H 0.4141 0.1383 -0.1305 0.029 Uiso 1 1 calc R . . H16B H 0.4503 0.1847 -0.0322 0.029 Uiso 1 1 calc R . . C17 C 0.5175(2) 0.24316(19) -0.0859(2) 0.0239(10) Uani 1 1 d . . . H17A H 0.5760 0.2432 -0.0392 0.029 Uiso 1 1 calc R . . H17B H 0.5270 0.2136 -0.1378 0.029 Uiso 1 1 calc R . . C18 C 0.5075(2) 0.33214(19) -0.07911(18) 0.0195(9) Uani 1 1 d . . . H18A H 0.5675 0.3594 -0.0759 0.023 Uiso 1 1 calc R . . H18B H 0.4549 0.3326 -0.1297 0.023 Uiso 1 1 calc R . . C19 C 0.5537(2) 0.43702(18) 0.05390(17) 0.0181(9) Uani 1 1 d . . . H19A H 0.6123 0.4444 0.0472 0.022 Uiso 1 1 calc R . . C20 C 0.5479(2) 0.49062(18) 0.12983(18) 0.0190(9) Uani 1 1 d . . . C21 C 0.4603(2) 0.50018(18) 0.14065(18) 0.0190(9) Uani 1 1 d . . . C22 C 0.4597(2) 0.55819(19) 0.21573(19) 0.0208(9) Uani 1 1 d . . . C23 C 0.5491(2) 0.5978(2) 0.2770(2) 0.0265(10) Uani 1 1 d . . . H23A H 0.5495 0.6354 0.3280 0.032 Uiso 1 1 calc R . . C24 C 0.6374(2) 0.58779(19) 0.27093(19) 0.0206(9) Uani 1 1 d . . . C25 C 0.6350(2) 0.53499(18) 0.19508(18) 0.0213(9) Uani 1 1 d . . . H25A H 0.6933 0.5284 0.1867 0.026 Uiso 1 1 calc R . . C26 C 0.3654(2) 0.57535(19) 0.22710(19) 0.0225(9) Uani 1 1 d . . . C27 C 0.3067(2) 0.4958(2) 0.2158(2) 0.0316(10) Uani 1 1 d . . . H27A H 0.3470 0.4684 0.2517 0.047 Uiso 1 1 calc R . . H27B H 0.2844 0.4580 0.1579 0.047 Uiso 1 1 calc R . . H27C H 0.2514 0.5102 0.2307 0.047 Uiso 1 1 calc R . . C28 C 0.3053(2) 0.6116(2) 0.1626(2) 0.0312(11) Uani 1 1 d . . . H28A H 0.2428 0.6189 0.1667 0.047 Uiso 1 1 calc R . . H28B H 0.2959 0.5734 0.1069 0.047 Uiso 1 1 calc R . . H28C H 0.3390 0.6656 0.1731 0.047 Uiso 1 1 calc R . . C29 C 0.3821(2) 0.6385(2) 0.3133(2) 0.0380(12) Uani 1 1 d . . . H29A H 0.4243 0.6188 0.3557 0.057 Uiso 1 1 calc R . . H29B H 0.3206 0.6448 0.3196 0.057 Uiso 1 1 calc R . . H29C H 0.4123 0.6924 0.3198 0.057 Uiso 1 1 calc R . . C30 C 0.7304(2) 0.6334(2) 0.34466(19) 0.0248(10) Uani 1 1 d . . . C31 C 0.8190(2) 0.6143(2) 0.3244(2) 0.0311(11) Uani 1 1 d . . . H31A H 0.8148 0.6304 0.2773 0.047 Uiso 1 1 calc R . . H31B H 0.8225 0.5547 0.3100 0.047 Uiso 1 1 calc R . . H31C H 0.8766 0.6458 0.3727 0.047 Uiso 1 1 calc R . . C32 C 0.7377(3) 0.6071(2) 0.4172(2) 0.0393(12) Uani 1 1 d . . . H32A H 0.7972 0.6360 0.4646 0.059 Uiso 1 1 calc R . . H32B H 0.7378 0.5469 0.4010 0.059 Uiso 1 1 calc R . . H32C H 0.6827 0.6215 0.4327 0.059 Uiso 1 1 calc R . . C33 C 0.7301(2) 0.7268(2) 0.3677(2) 0.0309(11) Uani 1 1 d . . . H33A H 0.6740 0.7417 0.3812 0.046 Uiso 1 1 calc R . . H33B H 0.7274 0.7426 0.3209 0.046 Uiso 1 1 calc R . . H33C H 0.7886 0.7564 0.4160 0.046 Uiso 1 1 calc R . . C34 C 0.2824(2) 0.2883(2) 0.0993(2) 0.0242(10) Uani 1 1 d . . . C35 C 0.3894(2) 0.29941(18) 0.14301(19) 0.0177(9) Uani 1 1 d . . . C36 C 0.5326(2) 0.31507(19) 0.15030(19) 0.0199(9) Uani 1 1 d . . . H36D H 0.5861 0.3211 0.1361 0.024 Uiso 1 1 calc R . . C37 C 0.4473(2) 0.30460(19) 0.22116(19) 0.0203(9) Uani 1 1 d . . . C38 C 0.6308(2) 0.3259(2) 0.2925(2) 0.0361(11) Uani 1 1 d . . . H38A H 0.6840 0.3359 0.2767 0.054 Uiso 1 1 calc R . . H38B H 0.6360 0.2756 0.3064 0.054 Uiso 1 1 calc R . . H38C H 0.6335 0.3736 0.3408 0.054 Uiso 1 1 calc R . . C39 C 0.4262(2) 0.3027(2) 0.2916(2) 0.0312(10) Uani 1 1 d . . . C40 C 0.7799(2) 0.18127(19) -0.15773(19) 0.0194(9) Uani 1 1 d . . . H40A H 0.7834 0.2069 -0.1949 0.023 Uiso 1 1 calc R . . C41 C 0.6911(2) 0.12720(19) -0.18276(19) 0.0188(9) Uani 1 1 d . . . C42 C 0.6827(2) 0.07581(19) -0.13997(18) 0.0166(9) Uani 1 1 d . . . C43 C 0.5932(2) 0.02567(18) -0.16644(18) 0.0174(9) Uani 1 1 d . . . C44 C 0.5220(2) 0.02659(19) -0.23708(18) 0.0188(9) Uani 1 1 d . . . H44A H 0.4630 -0.0083 -0.2562 0.023 Uiso 1 1 calc R . . C45 C 0.5282(2) 0.07427(19) -0.28357(18) 0.0181(9) Uani 1 1 d . . . C46 C 0.6143(2) 0.1255(2) -0.25381(19) 0.0204(9) Uani 1 1 d . . . H46A H 0.6215 0.1604 -0.2823 0.024 Uiso 1 1 calc R . . C47 C 0.5797(2) -0.02505(19) -0.11601(18) 0.0167(9) Uani 1 1 d . . . C48 C 0.6537(2) -0.08788(19) -0.1098(2) 0.0248(10) Uani 1 1 d . . . H48A H 0.6416 -0.1222 -0.0805 0.037 Uiso 1 1 calc R . . H48B H 0.7188 -0.0571 -0.0795 0.037 Uiso 1 1 calc R . . H48C H 0.6468 -0.1237 -0.1657 0.037 Uiso 1 1 calc R . . C49 C 0.5946(2) 0.0333(2) -0.02904(19) 0.0245(10) Uani 1 1 d . . . H49A H 0.5458 0.0705 -0.0322 0.037 Uiso 1 1 calc R . . H49B H 0.6584 0.0665 -0.0028 0.037 Uiso 1 1 calc R . . H49C H 0.5892 0.0007 0.0039 0.037 Uiso 1 1 calc R . . C50 C 0.4799(2) -0.0751(2) -0.15655(19) 0.0241(10) Uani 1 1 d . . . H50A H 0.4740 -0.1083 -0.1242 0.036 Uiso 1 1 calc R . . H50B H 0.4693 -0.1121 -0.2130 0.036 Uiso 1 1 calc R . . H50C H 0.4320 -0.0371 -0.1586 0.036 Uiso 1 1 calc R . . C51 C 0.4464(2) 0.0668(2) -0.36417(19) 0.0243(10) Uani 1 1 d . . . C52 C 0.4628(2) 0.1340(2) -0.3962(2) 0.0294(11) Uani 1 1 d . . . H52A H 0.4702 0.1890 -0.3541 0.044 Uiso 1 1 calc R . . H52B H 0.4077 0.1283 -0.4469 0.044 Uiso 1 1 calc R . . H52C H 0.5209 0.1282 -0.4082 0.044 Uiso 1 1 calc R . . C53 C 0.4377(3) -0.0189(2) -0.4301(2) 0.0348(11) Uani 1 1 d . . . H53A H 0.3800 -0.0273 -0.4798 0.052 Uiso 1 1 calc R . . H53B H 0.4333 -0.0625 -0.4081 0.052 Uiso 1 1 calc R . . H53C H 0.4943 -0.0213 -0.4445 0.052 Uiso 1 1 calc R . . C54 C 0.3514(2) 0.0755(2) -0.3507(2) 0.0358(11) Uani 1 1 d . . . H54A H 0.3584 0.1284 -0.3059 0.054 Uiso 1 1 calc R . . H54B H 0.3353 0.0293 -0.3357 0.054 Uiso 1 1 calc R . . H54C H 0.3000 0.0744 -0.4018 0.054 Uiso 1 1 calc R . . C55 C 0.9398(2) 0.2480(2) -0.07906(19) 0.0224(9) Uani 1 1 d . . . H55A H 0.9643 0.2921 -0.0233 0.027 Uiso 1 1 calc R . . H55B H 0.9232 0.2752 -0.1206 0.027 Uiso 1 1 calc R . . C56 C 1.0188(2) 0.1935(2) -0.0885(2) 0.0271(10) Uani 1 1 d . . . H56A H 1.0200 0.1828 -0.1440 0.033 Uiso 1 1 calc R . . H56B H 1.0816 0.2254 -0.0469 0.033 Uiso 1 1 calc R . . C57 C 1.0068(2) 0.10990(19) -0.07845(18) 0.0207(9) Uani 1 1 d . . . H57A H 0.9528 0.0724 -0.1279 0.025 Uiso 1 1 calc R . . H57B H 1.0656 0.0842 -0.0758 0.025 Uiso 1 1 calc R . . C58 C 1.0549(2) 0.10315(18) 0.05538(18) 0.0178(9) Uani 1 1 d . . . H58A H 1.1131 0.0914 0.0482 0.021 Uiso 1 1 calc R . . C59 C 1.0502(2) 0.10356(19) 0.13167(19) 0.0181(9) Uani 1 1 d . . . C60 C 0.9631(2) 0.10075(19) 0.14273(18) 0.0190(9) Uani 1 1 d . . . C61 C 0.9637(2) 0.0964(2) 0.21804(18) 0.0210(9) Uani 1 1 d . . . C62 C 1.0507(2) 0.0993(2) 0.27750(19) 0.0229(9) Uani 1 1 d . . . H62A H 1.0512 0.0976 0.3284 0.027 Uiso 1 1 calc R . . C63 C 1.1396(2) 0.10453(19) 0.26964(19) 0.0207(9) Uani 1 1 d . . . C64 C 1.1377(2) 0.10399(19) 0.19586(18) 0.0195(9) Uani 1 1 d . . . H64A H 1.1957 0.1039 0.1868 0.023 Uiso 1 1 calc R . . C65 C 0.8691(2) 0.0855(2) 0.2316(2) 0.0256(10) Uani 1 1 d . . . C66 C 0.8861(2) 0.0828(2) 0.3162(2) 0.0418(11) Uani 1 1 d . . . H66A H 0.9228 0.1356 0.3590 0.063 Uiso 1 1 calc R . . H66B H 0.9222 0.0372 0.3238 0.063 Uiso 1 1 calc R . . H66C H 0.8244 0.0736 0.3204 0.063 Uiso 1 1 calc R . . C67 C 0.8131(2) 0.1589(2) 0.2233(2) 0.0284(10) Uani 1 1 d . . . H67A H 0.7560 0.1534 0.2356 0.043 Uiso 1 1 calc R . . H67B H 0.7937 0.1582 0.1666 0.043 Uiso 1 1 calc R . . H67C H 0.8542 0.2115 0.2623 0.043 Uiso 1 1 calc R . . C68 C 0.8067(2) 0.0040(2) 0.1655(2) 0.0301(10) Uani 1 1 d . . . H68A H 0.8402 -0.0431 0.1720 0.045 Uiso 1 1 calc R . . H68B H 0.7942 0.0051 0.1102 0.045 Uiso 1 1 calc R . . H68C H 0.7457 -0.0020 0.1720 0.045 Uiso 1 1 calc R . . C69 C 1.2328(2) 0.1124(2) 0.34328(19) 0.0236(10) Uani 1 1 d . . . C70 C 1.3203(2) 0.1071(2) 0.3201(2) 0.0291(11) Uani 1 1 d . . . H70A H 1.3280 0.1532 0.3019 0.044 Uiso 1 1 calc R . . H70B H 1.3115 0.0541 0.2750 0.044 Uiso 1 1 calc R . . H70C H 1.3777 0.1108 0.3684 0.044 Uiso 1 1 calc R . . C71 C 1.2471(2) 0.1959(2) 0.4119(2) 0.0417(13) Uani 1 1 d . . . H71A H 1.3071 0.2020 0.4588 0.063 Uiso 1 1 calc R . . H71B H 1.1934 0.1987 0.4300 0.063 Uiso 1 1 calc R . . H71C H 1.2500 0.2408 0.3910 0.063 Uiso 1 1 calc R . . C72 C 1.2251(3) 0.0407(2) 0.3740(2) 0.0507(13) Uani 1 1 d . . . H72A H 1.2066 -0.0125 0.3273 0.076 Uiso 1 1 calc R . . H72B H 1.1765 0.0482 0.3984 0.076 Uiso 1 1 calc R . . H72C H 1.2872 0.0407 0.4159 0.076 Uiso 1 1 calc R . . C73 C 0.7876(2) 0.28351(19) 0.1060(2) 0.0221(9) Uani 1 1 d . . . C74 C 0.8933(2) 0.30593(19) 0.15063(19) 0.0182(9) Uani 1 1 d . . . C75 C 1.0369(2) 0.2962(2) 0.1563(2) 0.0265(10) Uani 1 1 d . . . H75A H 1.0899 0.2814 0.1413 0.032 Uiso 1 1 calc R . . C76 C 0.9532(2) 0.3554(2) 0.2281(2) 0.0247(10) Uani 1 1 d . . . C77 C 1.1372(2) 0.3884(2) 0.3002(2) 0.0377(12) Uani 1 1 d . . . H77A H 1.1412 0.3741 0.3481 0.057 Uiso 1 1 calc R . . H77B H 1.1417 0.4489 0.3152 0.057 Uiso 1 1 calc R . . H77C H 1.1899 0.3690 0.2833 0.057 Uiso 1 1 calc R . . C78 C 0.9325(2) 0.4058(2) 0.3011(2) 0.0345(11) Uani 1 1 d . . . C79 C 0.6205(3) 0.2498(3) 0.4939(2) 0.0542(14) Uani 1 1 d . . . H79A H 0.5571 0.2626 0.4658 0.081 Uiso 1 1 calc R . . H79B H 0.6629 0.3015 0.5337 0.081 Uiso 1 1 calc R . . H79C H 0.6145 0.2133 0.5232 0.081 Uiso 1 1 calc R . . C80 C 0.6603(3) 0.2085(2) 0.4335(2) 0.0355(11) Uani 1 1 d . . . O1 O 0.25470(13) 0.37327(12) -0.08048(12) 0.0187(6) Uani 1 1 d . . . O2 O 0.37858(14) 0.45842(13) 0.07961(12) 0.0213(6) Uani 1 1 d . . . O3 O 0.25546(14) 0.29811(13) 0.03071(13) 0.0225(6) Uani 1 1 d . . . O4 O 0.22969(14) 0.26991(14) 0.13153(14) 0.0286(7) Uani 1 1 d . . . O5 O 0.33391(15) 0.28925(14) 0.27838(14) 0.0341(7) Uani 1 1 d . . . H5B H 0.3003 0.2825 0.2289 0.041 Uiso 1 1 calc R . . O6 O 0.48752(18) 0.31283(18) 0.35869(15) 0.0530(9) Uani 1 1 d . . . O7 O 0.75739(14) 0.07178(12) -0.07689(12) 0.0198(6) Uani 1 1 d . . . O8 O 0.88108(14) 0.10091(12) 0.08323(12) 0.0192(6) Uani 1 1 d . . . O9 O 0.75918(14) 0.22582(13) 0.03679(13) 0.0224(6) Uani 1 1 d . . . O10 O 0.73494(14) 0.32347(13) 0.14012(14) 0.0286(7) Uani 1 1 d . . . O11 O 0.84080(15) 0.40650(14) 0.28813(14) 0.0370(8) Uani 1 1 d . . . H11D H 0.8074 0.3780 0.2384 0.055 Uiso 1 1 calc R . . O12 O 0.99534(18) 0.4427(2) 0.36780(16) 0.0635(11) Uani 1 1 d . . . C96 C 0.22811(14) 0.5805(6) 0.45860(19) 0.080(3) Uani 0.50 1 d PDU A 1 H96A H 0.2836 0.5564 0.4847 0.121 Uiso 0.50 1 calc PR A 1 H96B H 0.2501 0.6342 0.4586 0.121 Uiso 0.50 1 calc PR A 1 H96C H 0.1925 0.5428 0.4014 0.121 Uiso 0.50 1 calc PR A 1 C97 C 0.1643(4) 0.5930(9) 0.5060(5) 0.039(4) Uani 0.50 1 d PDU A 1 N97 N 0.0984(2) 0.6073(7) 0.5238(3) 0.030(3) Uani 0.50 1 d PDU A 1 C98 C 0.1302(2) 0.6028(4) 0.52149(17) 0.058(3) Uani 0.50 1 d PDU B 2 H98A H 0.1702 0.5749 0.5570 0.087 Uiso 0.50 1 calc PR B 2 H98B H 0.0636 0.5753 0.4964 0.087 Uiso 0.50 1 calc PR B 2 H98C H 0.1336 0.6612 0.5548 0.087 Uiso 0.50 1 calc PR B 2 C99 C 0.1616(4) 0.5987(5) 0.4625(3) 0.044(2) Uani 0.50 1 d PDU B 2 N98 N 0.1734(4) 0.6063(4) 0.3978(2) 0.079(3) Uani 0.50 1 d PDU B 2 N95 N 0.46050(11) 0.4955(6) 0.4981(4) 0.130(6) Uani 0.50 1 d PDU . 1 C95 C 0.46050(11) 0.4955(6) 0.4981(4) 0.130(6) Uani 0.50 1 d PU . 2 C94 C 0.35754(15) 0.5023(8) 0.4774(5) 0.148(6) Uani 0.50 1 d PDU . 2 H94A H 0.3312 0.4702 0.5018 0.222 Uiso 0.50 1 calc PR . 2 H94B H 0.3233 0.4803 0.4171 0.222 Uiso 0.50 1 calc PR . 2 H94C H 0.3498 0.5608 0.4997 0.222 Uiso 0.50 1 calc PR . 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 0.0131(2) 0.0165(2) 0.0274(2) 0.00839(19) 0.01101(18) 0.00820(19) Fe2 0.0124(2) 0.0198(2) 0.0263(2) 0.01126(19) 0.00996(18) 0.00693(19) N1 0.0183(12) 0.0157(13) 0.0291(13) 0.0109(11) 0.0140(10) 0.0099(11) N2 0.0188(13) 0.0165(13) 0.0227(13) 0.0081(11) 0.0096(11) 0.0121(11) N3 0.0141(12) 0.0171(14) 0.0279(13) 0.0082(11) 0.0126(10) 0.0069(11) N4 0.0156(13) 0.0252(15) 0.0290(14) 0.0135(12) 0.0070(11) 0.0055(12) N5 0.0152(12) 0.0180(14) 0.0297(13) 0.0111(11) 0.0144(10) 0.0072(11) N6 0.0131(13) 0.0197(13) 0.0265(13) 0.0112(11) 0.0120(11) 0.0103(11) N7 0.0134(13) 0.0163(14) 0.0273(13) 0.0080(11) 0.0097(11) 0.0061(11) N8 0.0182(13) 0.0171(14) 0.0313(14) 0.0065(12) 0.0099(11) 0.0065(12) N9 0.0529(19) 0.066(2) 0.0594(18) 0.0317(17) 0.0329(15) 0.0151(18) C1 0.0258(17) 0.0187(17) 0.0262(16) 0.0074(14) 0.0148(13) 0.0041(14) C2 0.0192(15) 0.0220(17) 0.0234(15) 0.0096(13) 0.0140(13) 0.0077(14) C3 0.0202(16) 0.0191(17) 0.0248(15) 0.0120(13) 0.0124(13) 0.0056(14) C4 0.0164(15) 0.0236(17) 0.0256(15) 0.0126(13) 0.0128(13) 0.0082(14) C5 0.0177(16) 0.0289(18) 0.0333(17) 0.0177(14) 0.0131(13) 0.0108(14) C6 0.0224(17) 0.0246(18) 0.0298(16) 0.0123(14) 0.0112(14) -0.0016(15) C7 0.0259(16) 0.0167(17) 0.0270(16) 0.0073(13) 0.0171(13) 0.0072(14) C8 0.0199(16) 0.0202(17) 0.0374(18) 0.0132(14) 0.0137(14) 0.0082(14) C9 0.0234(16) 0.0248(18) 0.0392(18) 0.0128(15) 0.0177(14) 0.0138(15) C10 0.0169(16) 0.0201(18) 0.0347(18) 0.0038(15) 0.0130(14) 0.0055(14) C11 0.0216(17) 0.032(2) 0.047(2) 0.0173(16) 0.0155(15) 0.0144(16) C12 0.0278(19) 0.026(2) 0.035(2) 0.0051(16) 0.0031(16) -0.0028(16) C13 0.027(2) 0.046(3) 0.051(2) -0.007(2) 0.0067(18) -0.0012(19) C14 0.066(3) 0.071(3) 0.041(2) 0.025(2) -0.007(2) -0.025(3) C15 0.025(2) 0.034(2) 0.061(2) 0.0120(19) 0.0064(18) 0.0052(17) C16 0.0220(16) 0.0245(18) 0.0259(17) 0.0080(14) 0.0088(14) 0.0140(15) C17 0.0125(15) 0.0194(18) 0.0341(18) 0.0027(15) 0.0091(14) 0.0065(14) C18 0.0180(15) 0.0213(17) 0.0216(15) 0.0065(13) 0.0113(13) 0.0071(14) C19 0.0187(15) 0.0238(17) 0.0204(15) 0.0129(13) 0.0123(12) 0.0129(14) C20 0.0229(16) 0.0104(16) 0.0266(16) 0.0077(13) 0.0117(13) 0.0052(13) C21 0.0227(16) 0.0126(16) 0.0295(16) 0.0098(13) 0.0166(13) 0.0108(13) C22 0.0177(15) 0.0210(17) 0.0319(16) 0.0127(14) 0.0158(13) 0.0057(14) C23 0.0282(17) 0.0194(18) 0.0351(18) 0.0067(15) 0.0183(14) 0.0116(15) C24 0.0227(16) 0.0122(16) 0.0307(16) 0.0080(13) 0.0141(13) 0.0074(14) C25 0.0218(16) 0.0184(17) 0.0344(17) 0.0140(14) 0.0184(13) 0.0111(14) C26 0.0208(15) 0.0159(17) 0.0342(17) 0.0037(14) 0.0192(13) 0.0072(14) C27 0.0339(17) 0.032(2) 0.0426(18) 0.0128(16) 0.0300(15) 0.0130(16) C28 0.0207(17) 0.0243(19) 0.054(2) 0.0149(16) 0.0192(15) 0.0114(15) C29 0.0292(18) 0.040(2) 0.049(2) 0.0074(18) 0.0273(16) 0.0061(17) C30 0.0240(17) 0.0181(17) 0.0316(17) 0.0075(14) 0.0110(14) 0.0039(14) C31 0.0191(17) 0.026(2) 0.0341(19) -0.0015(16) 0.0060(15) 0.0025(15) C32 0.041(2) 0.041(2) 0.0310(19) 0.0143(17) 0.0074(17) -0.0021(18) C33 0.0233(17) 0.0222(19) 0.0343(19) -0.0017(16) 0.0076(15) 0.0035(15) C34 0.0207(16) 0.0192(17) 0.0377(18) 0.0101(14) 0.0166(14) 0.0119(14) C35 0.0143(15) 0.0104(15) 0.0337(17) 0.0110(13) 0.0122(13) 0.0055(13) C36 0.0150(15) 0.0206(17) 0.0285(16) 0.0126(13) 0.0099(13) 0.0049(14) C37 0.0172(14) 0.0186(17) 0.0384(17) 0.0132(13) 0.0228(13) 0.0083(13) C38 0.0207(18) 0.055(2) 0.0404(19) 0.0298(17) 0.0087(15) 0.0073(17) C39 0.0326(18) 0.0255(19) 0.0480(19) 0.0169(15) 0.0261(15) 0.0149(15) C40 0.0220(16) 0.0179(16) 0.0280(16) 0.0147(13) 0.0144(13) 0.0092(14) C41 0.0175(16) 0.0165(17) 0.0297(16) 0.0104(13) 0.0152(13) 0.0056(13) C42 0.0067(14) 0.0166(17) 0.0253(16) 0.0060(13) 0.0061(13) 0.0054(13) C43 0.0189(16) 0.0143(16) 0.0227(15) 0.0066(13) 0.0118(13) 0.0089(13) C44 0.0178(16) 0.0122(16) 0.0233(16) 0.0028(13) 0.0078(13) 0.0041(13) C45 0.0158(15) 0.0175(17) 0.0239(16) 0.0083(13) 0.0103(13) 0.0084(13) C46 0.0187(16) 0.0214(16) 0.0289(16) 0.0171(13) 0.0103(13) 0.0141(14) C47 0.0128(15) 0.0170(16) 0.0245(16) 0.0105(13) 0.0093(13) 0.0047(13) C48 0.0324(18) 0.0136(17) 0.0372(17) 0.0125(14) 0.0198(14) 0.0101(15) C49 0.0281(17) 0.0180(17) 0.0380(18) 0.0113(14) 0.0234(14) 0.0089(15) C50 0.0231(17) 0.0233(18) 0.0312(17) 0.0121(14) 0.0144(14) 0.0056(15) C51 0.0217(17) 0.0250(18) 0.0297(17) 0.0135(14) 0.0105(14) 0.0075(15) C52 0.0264(18) 0.0286(19) 0.0280(18) 0.0130(15) 0.0019(15) 0.0050(16) C53 0.038(2) 0.027(2) 0.0324(19) 0.0112(16) 0.0052(16) 0.0052(17) C54 0.0266(19) 0.050(2) 0.0330(18) 0.0216(17) 0.0077(15) 0.0124(17) C55 0.0164(15) 0.0302(18) 0.0314(16) 0.0176(14) 0.0152(13) 0.0024(14) C56 0.0150(16) 0.034(2) 0.0397(18) 0.0188(15) 0.0133(14) 0.0071(15) C57 0.0147(15) 0.0261(18) 0.0243(16) 0.0108(14) 0.0090(13) 0.0112(14) C58 0.0127(15) 0.0164(17) 0.0240(16) 0.0064(13) 0.0074(13) 0.0058(13) C59 0.0165(15) 0.0162(16) 0.0290(16) 0.0095(13) 0.0156(13) 0.0076(13) C60 0.0137(16) 0.0176(17) 0.0203(16) 0.0041(14) 0.0029(13) 0.0083(14) C61 0.0265(17) 0.0218(17) 0.0216(16) 0.0101(13) 0.0148(13) 0.0085(15) C62 0.0262(17) 0.0276(19) 0.0239(16) 0.0129(14) 0.0163(13) 0.0130(15) C63 0.0212(17) 0.0183(17) 0.0224(16) 0.0046(14) 0.0105(13) 0.0083(14) C64 0.0137(15) 0.0206(17) 0.0267(17) 0.0113(14) 0.0077(13) 0.0117(14) C65 0.0244(16) 0.0338(19) 0.0379(17) 0.0234(14) 0.0234(14) 0.0196(15) C66 0.0384(19) 0.067(2) 0.0503(19) 0.0379(18) 0.0352(15) 0.0269(19) C67 0.0226(16) 0.036(2) 0.0426(18) 0.0205(15) 0.0241(14) 0.0171(15) C68 0.0206(17) 0.037(2) 0.0501(19) 0.0248(16) 0.0250(14) 0.0073(16) C69 0.0230(17) 0.0281(18) 0.0234(16) 0.0128(14) 0.0097(14) 0.0100(15) C70 0.0181(17) 0.034(2) 0.0282(18) 0.0112(15) 0.0010(14) 0.0077(16) C71 0.0278(19) 0.053(2) 0.037(2) 0.0105(19) 0.0084(17) 0.0200(18) C72 0.032(2) 0.068(2) 0.071(2) 0.0527(19) 0.0149(18) 0.012(2) C73 0.0178(16) 0.0189(17) 0.0392(18) 0.0182(14) 0.0144(14) 0.0104(14) C74 0.0182(15) 0.0181(16) 0.0315(16) 0.0142(13) 0.0194(13) 0.0100(13) C75 0.0248(17) 0.0232(19) 0.0394(18) 0.0124(15) 0.0200(14) 0.0103(15) C76 0.0267(18) 0.0142(18) 0.0311(18) 0.0022(15) 0.0142(15) 0.0063(15) C77 0.0199(18) 0.040(2) 0.039(2) -0.0014(18) 0.0091(16) 0.0031(17) C78 0.0326(19) 0.025(2) 0.043(2) 0.0025(17) 0.0194(16) 0.0036(17) C79 0.083(3) 0.049(2) 0.041(2) 0.0194(19) 0.033(2) 0.023(2) C80 0.041(2) 0.034(2) 0.0336(19) 0.0172(16) 0.0124(17) 0.0029(18) O1 0.0137(10) 0.0149(11) 0.0270(11) 0.0069(9) 0.0077(9) 0.0066(9) O2 0.0140(10) 0.0227(12) 0.0285(11) 0.0077(9) 0.0108(9) 0.0083(9) O3 0.0135(10) 0.0253(12) 0.0325(11) 0.0137(10) 0.0099(9) 0.0056(9) O4 0.0158(10) 0.0338(13) 0.0492(12) 0.0216(10) 0.0208(9) 0.0099(10) O5 0.0300(12) 0.0487(14) 0.0408(12) 0.0264(11) 0.0231(10) 0.0148(11) O6 0.0382(15) 0.093(2) 0.0349(13) 0.0318(13) 0.0139(11) 0.0141(15) O7 0.0167(11) 0.0172(11) 0.0299(11) 0.0146(9) 0.0084(9) 0.0072(9) O8 0.0126(10) 0.0219(12) 0.0264(11) 0.0121(9) 0.0080(9) 0.0064(9) O9 0.0196(11) 0.0251(12) 0.0298(11) 0.0134(10) 0.0140(9) 0.0118(10) O10 0.0206(11) 0.0260(13) 0.0481(13) 0.0136(10) 0.0228(10) 0.0149(10) O11 0.0303(12) 0.0321(14) 0.0500(14) 0.0019(12) 0.0289(11) 0.0091(11) O12 0.0387(15) 0.077(2) 0.0485(16) -0.0153(16) 0.0225(13) 0.0008(15) C96 0.076(5) 0.043(5) 0.084(5) 0.005(4) 0.005(4) -0.021(4) C97 0.048(5) 0.031(5) 0.034(5) 0.019(4) 0.003(4) -0.003(4) N97 0.023(5) 0.039(5) 0.031(5) 0.006(4) 0.020(4) 0.001(4) C98 0.021(4) 0.073(7) 0.086(6) 0.020(5) 0.035(4) 0.018(4) C99 0.043(3) 0.029(4) 0.056(4) -0.010(3) 0.038(3) -0.003(3) N98 0.066(5) 0.028(4) 0.098(6) -0.022(4) 0.023(5) -0.007(4) N95 0.100(9) 0.055(6) 0.164(9) -0.024(6) 0.033(9) -0.016(8) C95 0.100(9) 0.055(6) 0.164(9) -0.024(6) 0.033(9) -0.016(8) C94 0.213(12) 0.121(10) 0.106(8) 0.018(8) 0.082(8) -0.055(10)