# Electronic Supplementary Material (ESI) for Chemical Communications # 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_ast237_h82 _database_code_depnum_ccdc_archive 'CCDC 893652' #TrackingRef '12845_web_deposit_cif_file_0_CarmenRamirezdeArellano_1343213556.ast237_H82.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H36.50 Cr N2 O6.25' _chemical_formula_weight 673.19 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' Cr Cr 0.3209 0.6236 '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 11.6599(11) _cell_length_b 16.1539(14) _cell_length_c 19.2369(18) _cell_angle_alpha 86.011(7) _cell_angle_beta 88.184(8) _cell_angle_gamma 85.019(7) _cell_volume 3599.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2224 _cell_measurement_theta_min 2.954 _cell_measurement_theta_max 30.509 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1410 _exptl_absorpt_coefficient_mu 0.365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9575 _exptl_absorpt_correction_T_max 0.9856 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Oxford Diffraction SuperNova' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 16.026 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30853 _diffrn_reflns_av_R_equivalents 0.0970 _diffrn_reflns_av_sigmaI/netI 0.1942 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14699 _reflns_number_gt 6651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diff., 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford Diff., 2009)' _computing_data_reduction 'CrysAlisPro (Oxford Diff., 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalMaker 2.1.5 (1994-2009)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 14699 _refine_ls_number_parameters 890 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.2054 _refine_ls_R_factor_gt 0.1010 _refine_ls_wR_factor_ref 0.2850 _refine_ls_wR_factor_gt 0.2218 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.080 _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 Cr1 Cr 0.43116(8) 0.20568(6) 0.47984(5) 0.0314(3) Uani 1 1 d . . . Cr1A Cr 0.19735(9) 0.72607(7) 0.09716(6) 0.0386(3) Uani 1 1 d . . . C1 C 0.3348(5) 0.2160(4) 0.3862(3) 0.0296(15) Uani 1 1 d . . . C2 C 0.3621(5) 0.1737(4) 0.3315(3) 0.0309(15) Uani 1 1 d . . . C3 C 0.4158(5) 0.1407(4) 0.2768(3) 0.0275(14) Uani 1 1 d . . . O1 O 0.5474(4) 0.1850(3) 0.6181(3) 0.0538(14) Uani 1 1 d . . . O2 O 0.6384(4) 0.2847(3) 0.4132(3) 0.0517(13) Uani 1 1 d . . . O3 O 0.5615(4) 0.0442(3) 0.4405(2) 0.0490(13) Uani 1 1 d . . . O4 O 0.2180(4) 0.1313(3) 0.5452(3) 0.0538(14) Uani 1 1 d . . . O5 O 0.3374(4) 0.3818(3) 0.5098(2) 0.0404(11) Uani 1 1 d . . . O6 O 0.2338(3) 0.2694(2) 0.3885(2) 0.0318(10) Uani 1 1 d . . . C11 C 0.5032(5) 0.1934(4) 0.5655(4) 0.0373(17) Uani 1 1 d . . . C12 C 0.5571(6) 0.2545(4) 0.4383(4) 0.0378(16) Uani 1 1 d . . . C13 C 0.5055(5) 0.1034(4) 0.4560(3) 0.0352(16) Uani 1 1 d . . . C14 C 0.2974(6) 0.1577(4) 0.5200(3) 0.0361(16) Uani 1 1 d . . . C15 C 0.3694(5) 0.3135(4) 0.4983(3) 0.0329(15) Uani 1 1 d . . . C16 C 0.1685(5) 0.2789(4) 0.3262(3) 0.0327(15) Uani 1 1 d . . . H16A H 0.1597 0.2235 0.3091 0.039 Uiso 1 1 calc R . . H16B H 0.2097 0.3118 0.2896 0.039 Uiso 1 1 calc R . . C17 C 0.0522(5) 0.3222(4) 0.3406(4) 0.0445(18) Uani 1 1 d . . . H17A H 0.0106 0.2886 0.3758 0.058 Uiso 1 1 calc R . . H17B H 0.0087 0.3293 0.2975 0.058 Uiso 1 1 calc R . . H17C H 0.0612 0.3768 0.3578 0.058 Uiso 1 1 calc R . . C31 C 0.4992(6) 0.1911(4) 0.2332(3) 0.0322(15) Uani 1 1 d . . . C32 C 0.6094(5) 0.1971(4) 0.2558(4) 0.0391(17) Uani 1 1 d . . . H32 H 0.6339 0.1671 0.2977 0.047 Uiso 1 1 calc R . . C33 C 0.6852(7) 0.2465(4) 0.2182(5) 0.058(2) Uani 1 1 d . . . H33 H 0.7604 0.2508 0.2346 0.069 Uiso 1 1 calc R . . C34 C 0.6501(8) 0.2888(5) 0.1575(5) 0.055(2) Uani 1 1 d . . . H34 H 0.7017 0.3216 0.1310 0.066 Uiso 1 1 calc R . . C35 C 0.5432(9) 0.2841(5) 0.1352(4) 0.063(2) Uani 1 1 d . . . H35 H 0.5195 0.3148 0.0935 0.076 Uiso 1 1 calc R . . C36 C 0.4653(7) 0.2345(4) 0.1724(4) 0.0451(18) Uani 1 1 d . . . H36 H 0.3903 0.2311 0.1556 0.054 Uiso 1 1 calc R . . N41 N 0.2957(4) 0.0191(3) 0.2700(3) 0.0329(13) Uani 1 1 d . . . C42 C 0.3928(5) 0.0588(4) 0.2557(3) 0.0297(14) Uani 1 1 d . . . N43 N 0.4625(5) 0.0070(3) 0.2163(3) 0.0371(14) Uani 1 1 d . . . C44 C 0.4082(6) -0.0652(4) 0.2072(4) 0.0445(18) Uani 1 1 d . . . H44 H 0.4384 -0.1107 0.1815 0.053 Uiso 1 1 calc R . . C45 C 0.3053(6) -0.0588(4) 0.2414(3) 0.0409(17) Uani 1 1 d . . . H45 H 0.2502 -0.0990 0.2452 0.049 Uiso 1 1 calc R . . C51 C 0.1881(5) 0.0483(4) 0.3035(3) 0.0303(15) Uani 1 1 d . . . C52 C 0.1717(5) 0.0316(4) 0.3744(3) 0.0296(14) Uani 1 1 d . . . C53 C 0.0650(6) 0.0570(4) 0.4028(4) 0.0434(18) Uani 1 1 d . . . H53 H 0.0511 0.0467 0.4514 0.052 Uiso 1 1 calc R . . C54 C -0.0237(5) 0.0977(4) 0.3615(4) 0.0444(18) Uani 1 1 d . . . C55 C -0.0032(6) 0.1119(4) 0.2918(4) 0.049(2) Uani 1 1 d . . . H55 H -0.0633 0.1380 0.2637 0.059 Uiso 1 1 calc R . . C56 C 0.1048(6) 0.0889(4) 0.2600(4) 0.0379(16) Uani 1 1 d . . . C57 C 0.2633(5) -0.0143(4) 0.4183(3) 0.0395(17) Uani 1 1 d . . . H57A H 0.2783 -0.0712 0.4036 0.051 Uiso 1 1 calc R . . H57B H 0.2375 -0.0162 0.4674 0.051 Uiso 1 1 calc R . . H57C H 0.3341 0.0143 0.4128 0.051 Uiso 1 1 calc R . . C58 C -0.1385(6) 0.1248(5) 0.3947(5) 0.069(3) Uani 1 1 d . . . H58A H -0.1835 0.1621 0.3614 0.090 Uiso 1 1 calc R . . H58B H -0.1263 0.1542 0.4363 0.090 Uiso 1 1 calc R . . H58C H -0.1804 0.0758 0.4077 0.090 Uiso 1 1 calc R . . C59 C 0.1286(6) 0.1089(4) 0.1847(4) 0.052(2) Uani 1 1 d . . . H59A H 0.1993 0.1376 0.1790 0.067 Uiso 1 1 calc R . . H59B H 0.0641 0.1450 0.1650 0.067 Uiso 1 1 calc R . . H59C H 0.1381 0.0573 0.1605 0.067 Uiso 1 1 calc R . . C61 C 0.5743(5) 0.0199(4) 0.1828(4) 0.0355(16) Uani 1 1 d . . . C62 C 0.6715(6) -0.0023(4) 0.2199(4) 0.0428(18) Uani 1 1 d . . . C63 C 0.7786(6) 0.0051(4) 0.1853(4) 0.048(2) Uani 1 1 d . . . H63 H 0.8478 -0.0102 0.2095 0.058 Uiso 1 1 calc R . . C64 C 0.7836(6) 0.0347(5) 0.1157(4) 0.0493(19) Uani 1 1 d . . . C65 C 0.6821(5) 0.0559(4) 0.0806(4) 0.0398(17) Uani 1 1 d . . . H65 H 0.6859 0.0759 0.0330 0.048 Uiso 1 1 calc R . . C66 C 0.5768(5) 0.0488(4) 0.1126(4) 0.0363(16) Uani 1 1 d . . . C67 C 0.6656(6) -0.0349(5) 0.2955(4) 0.058(2) Uani 1 1 d . . . H67A H 0.6315 0.0093 0.3240 0.076 Uiso 1 1 calc R . . H67B H 0.7434 -0.0529 0.3113 0.076 Uiso 1 1 calc R . . H67C H 0.6181 -0.0822 0.3001 0.076 Uiso 1 1 calc R . . C68 C 0.8993(6) 0.0420(6) 0.0790(5) 0.076(3) Uani 1 1 d . . . H68A H 0.8962 0.0240 0.0316 0.098 Uiso 1 1 calc R . . H68B H 0.9586 0.0067 0.1047 0.098 Uiso 1 1 calc R . . H68C H 0.9182 0.1001 0.0770 0.098 Uiso 1 1 calc R . . C69 C 0.4675(5) 0.0700(4) 0.0733(4) 0.0454(18) Uani 1 1 d . . . H69A H 0.4859 0.0938 0.0264 0.059 Uiso 1 1 calc R . . H69B H 0.4173 0.1106 0.0981 0.059 Uiso 1 1 calc R . . H69C H 0.4279 0.0194 0.0697 0.059 Uiso 1 1 calc R . . C1A C 0.2451(5) 0.7213(4) 0.2060(3) 0.0302(14) Uani 1 1 d . . . C2A C 0.3311(5) 0.6785(4) 0.2351(3) 0.0271(14) Uani 1 1 d . . . C3A C 0.4302(5) 0.6365(4) 0.2570(3) 0.0273(14) Uani 1 1 d . . . O1A O 0.1112(4) 0.7394(4) -0.0497(3) 0.0689(17) Uani 1 1 d . . . O2A O 0.1611(6) 0.9135(4) 0.1024(3) 0.089(2) Uani 1 1 d U . . O3A O -0.0418(5) 0.7006(4) 0.1561(3) 0.0862(19) Uani 1 1 d U . . O4A O 0.2230(4) 0.5414(3) 0.0745(3) 0.0538(14) Uani 1 1 d . . . O5A O 0.4394(4) 0.7489(4) 0.0423(3) 0.0721(18) Uani 1 1 d . . . O6A O 0.1643(3) 0.7699(2) 0.2457(2) 0.0340(11) Uani 1 1 d . . . C11A C 0.1437(6) 0.7352(5) 0.0078(4) 0.053(2) Uani 1 1 d . . . C12A C 0.1733(7) 0.8412(5) 0.1022(4) 0.068(3) Uani 1 1 d . . . C13A C 0.0510(6) 0.7133(6) 0.1335(4) 0.063(2) Uani 1 1 d . . . C14A C 0.2163(6) 0.6104(5) 0.0868(3) 0.0394(17) Uani 1 1 d . . . C15A C 0.3492(7) 0.7399(5) 0.0649(4) 0.0474(19) Uani 1 1 d . . . C16A C 0.1816(5) 0.7678(4) 0.3184(3) 0.0354(16) Uani 1 1 d . . . H16C H 0.2538 0.7927 0.3276 0.043 Uiso 1 1 calc R . . H16D H 0.1873 0.7096 0.3386 0.043 Uiso 1 1 calc R . . C17A C 0.0799(5) 0.8170(4) 0.3508(4) 0.0440(18) Uani 1 1 d . . . H17D H 0.0716 0.8733 0.3281 0.057 Uiso 1 1 calc R . . H17E H 0.0923 0.8202 0.4007 0.057 Uiso 1 1 calc R . . H17F H 0.0097 0.7893 0.3447 0.057 Uiso 1 1 calc R . . C31A C 0.5417(5) 0.6754(4) 0.2589(3) 0.0271(14) Uani 1 1 d . . . C32A C 0.5762(5) 0.7277(4) 0.2030(4) 0.0393(16) Uani 1 1 d . . . H32A H 0.5299 0.7376 0.1631 0.047 Uiso 1 1 calc R . . C33A C 0.6793(6) 0.7656(4) 0.2058(4) 0.0478(19) Uani 1 1 d . . . H33A H 0.7017 0.8024 0.1681 0.057 Uiso 1 1 calc R . . C34A C 0.7479(6) 0.7503(5) 0.2621(4) 0.0440(18) Uani 1 1 d . . . H34A H 0.8188 0.7749 0.2633 0.053 Uiso 1 1 calc R . . C35A C 0.7140(5) 0.7000(4) 0.3158(4) 0.0414(18) Uani 1 1 d . . . H35A H 0.7607 0.6902 0.3557 0.050 Uiso 1 1 calc R . . C36A C 0.6121(5) 0.6620(4) 0.3142(3) 0.0330(15) Uani 1 1 d . . . H36A H 0.5910 0.6258 0.3527 0.040 Uiso 1 1 calc R . . N41A N 0.3514(4) 0.5093(3) 0.3194(2) 0.0264(11) Uani 1 1 d . . . C42A C 0.4316(5) 0.5482(4) 0.2797(3) 0.0234(13) Uani 1 1 d . . . N43A N 0.5125(4) 0.4874(3) 0.2609(3) 0.0293(12) Uani 1 1 d . . . C44A C 0.4818(5) 0.4104(4) 0.2907(3) 0.0320(15) Uani 1 1 d . . . H44A H 0.5238 0.3579 0.2864 0.038 Uiso 1 1 calc R . . C45A C 0.3816(5) 0.4246(4) 0.3265(3) 0.0281(14) Uani 1 1 d . . . H45A H 0.3397 0.3841 0.3519 0.034 Uiso 1 1 calc R . . C51A C 0.2524(5) 0.5469(4) 0.3564(3) 0.0277(14) Uani 1 1 d . . . C52A C 0.1461(5) 0.5493(4) 0.3249(3) 0.0308(15) Uani 1 1 d . . . C53A C 0.0493(5) 0.5773(4) 0.3644(4) 0.0388(17) Uani 1 1 d . . . H53A H -0.0245 0.5791 0.3445 0.047 Uiso 1 1 calc R . . C54A C 0.0569(5) 0.6019(4) 0.4304(4) 0.0429(18) Uani 1 1 d . . . C55A C 0.1657(5) 0.5997(4) 0.4596(3) 0.0360(16) Uani 1 1 d . . . H55A H 0.1721 0.6174 0.5052 0.043 Uiso 1 1 calc R . . C56A C 0.2654(5) 0.5717(4) 0.4225(3) 0.0289(14) Uani 1 1 d . . . C57A C 0.1336(5) 0.5226(4) 0.2520(3) 0.0393(17) Uani 1 1 d . . . H57D H 0.1946 0.5441 0.2215 0.051 Uiso 1 1 calc R . . H57E H 0.0583 0.5447 0.2344 0.051 Uiso 1 1 calc R . . H57F H 0.1397 0.4616 0.2529 0.051 Uiso 1 1 calc R . . C58A C -0.0497(6) 0.6302(5) 0.4723(4) 0.064(2) Uani 1 1 d . . . H58D H -0.1185 0.6210 0.4469 0.083 Uiso 1 1 calc R . . H58E H -0.0493 0.6896 0.4796 0.083 Uiso 1 1 calc R . . H58F H -0.0504 0.5983 0.5176 0.083 Uiso 1 1 calc R . . C59A C 0.3818(5) 0.5730(4) 0.4548(3) 0.0360(16) Uani 1 1 d . . . H59D H 0.4318 0.5242 0.4419 0.047 Uiso 1 1 calc R . . H59E H 0.3723 0.5719 0.5056 0.047 Uiso 1 1 calc R . . H59F H 0.4168 0.6238 0.4377 0.047 Uiso 1 1 calc R . . C61A C 0.6148(5) 0.4949(4) 0.2173(3) 0.0292(14) Uani 1 1 d . . . C62A C 0.6001(5) 0.5116(3) 0.1450(3) 0.0292(14) Uani 1 1 d . . . C63A C 0.6994(5) 0.5141(4) 0.1040(3) 0.0346(15) Uani 1 1 d . . . H63A H 0.6924 0.5266 0.0552 0.041 Uiso 1 1 calc R . . C64A C 0.8075(5) 0.4991(4) 0.1307(4) 0.0354(16) Uani 1 1 d . . . C65A C 0.8182(5) 0.4807(4) 0.2014(4) 0.0371(16) Uani 1 1 d . . . H65A H 0.8929 0.4692 0.2199 0.045 Uiso 1 1 calc R . . C66A C 0.7226(5) 0.4787(4) 0.2464(3) 0.0328(15) Uani 1 1 d . . . C67A C 0.4826(5) 0.5233(4) 0.1142(3) 0.0408(17) Uani 1 1 d . . . H67D H 0.4458 0.5781 0.1246 0.053 Uiso 1 1 calc R . . H67E H 0.4356 0.4798 0.1343 0.053 Uiso 1 1 calc R . . H67F H 0.4898 0.5198 0.0636 0.053 Uiso 1 1 calc R . . C68A C 0.9144(6) 0.5017(5) 0.0830(4) 0.059(2) Uani 1 1 d . . . H68D H 0.9212 0.4530 0.0551 0.077 Uiso 1 1 calc R . . H68E H 0.9829 0.5012 0.1113 0.077 Uiso 1 1 calc R . . H68F H 0.9079 0.5526 0.0521 0.077 Uiso 1 1 calc R . . C69A C 0.7386(5) 0.4560(4) 0.3233(4) 0.0441(18) Uani 1 1 d . . . H69D H 0.6867 0.4932 0.3506 0.057 Uiso 1 1 calc R . . H69E H 0.8185 0.4620 0.3351 0.057 Uiso 1 1 calc R . . H69F H 0.7210 0.3983 0.3342 0.057 Uiso 1 1 calc R . . O7 O 0.7645(7) 0.7469(5) 0.9456(4) 0.036(2) Uani 0.50 1 d PU . . C71 C 0.8115(12) 0.6770(8) 0.9338(7) 0.043(3) Uani 0.50 1 d PU . . H71A H 0.7635 0.6351 0.9570 0.052 Uiso 0.50 1 calc PR . . H71B H 0.8864 0.6708 0.9573 0.052 Uiso 0.50 1 calc PR . . C72 C 0.8333(11) 0.6548(7) 0.8625(6) 0.034(3) Uani 0.50 1 d PU . . H72A H 0.7599 0.6514 0.8399 0.044 Uiso 0.50 1 calc PR . . H72B H 0.8783 0.6006 0.8625 0.044 Uiso 0.50 1 calc PR . . H72C H 0.8764 0.6972 0.8370 0.044 Uiso 0.50 1 calc PR . . C73 C 0.7579(9) 0.7724(7) 1.0128(5) 0.021(2) Uani 0.50 1 d PU . . H73A H 0.7940 0.7272 1.0444 0.025 Uiso 0.50 1 calc PR . . H73B H 0.6759 0.7816 1.0273 0.025 Uiso 0.50 1 calc PR . . C74 C 0.8137(8) 0.8479(6) 1.0205(5) 0.017(2) Uani 0.50 1 d PU . . H74A H 0.8919 0.8421 1.0003 0.022 Uiso 0.50 1 calc PR . . H74B H 0.8172 0.8576 1.0701 0.022 Uiso 0.50 1 calc PR . . H74C H 0.7696 0.8952 0.9964 0.022 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 Cr1 0.0340(6) 0.0320(6) 0.0293(6) -0.0106(4) 0.0020(4) -0.0036(5) Cr1A 0.0342(6) 0.0451(7) 0.0372(7) -0.0135(5) -0.0029(5) 0.0030(5) C1 0.030(3) 0.020(3) 0.038(4) -0.005(3) 0.013(3) 0.001(3) C2 0.032(3) 0.035(4) 0.027(4) -0.005(3) 0.000(3) -0.013(3) C3 0.030(3) 0.026(3) 0.027(4) -0.011(3) -0.002(3) 0.000(3) O1 0.059(3) 0.059(3) 0.044(3) -0.011(3) -0.019(3) 0.010(3) O2 0.045(3) 0.052(3) 0.060(4) -0.015(3) 0.014(3) -0.011(3) O3 0.057(3) 0.043(3) 0.047(3) -0.013(2) 0.003(2) 0.007(3) O4 0.051(3) 0.068(4) 0.046(3) -0.009(3) 0.012(3) -0.021(3) O5 0.042(3) 0.031(3) 0.048(3) -0.010(2) 0.001(2) -0.001(2) O6 0.030(2) 0.032(2) 0.034(3) -0.0095(19) 0.0003(19) -0.002(2) C11 0.039(4) 0.026(4) 0.046(5) -0.012(3) -0.002(3) 0.011(3) C12 0.032(4) 0.039(4) 0.043(4) -0.016(3) -0.001(3) 0.001(3) C13 0.035(4) 0.038(4) 0.033(4) -0.010(3) -0.002(3) -0.001(3) C14 0.037(4) 0.042(4) 0.032(4) -0.008(3) 0.002(3) -0.010(3) C15 0.035(4) 0.038(4) 0.026(4) -0.003(3) 0.000(3) -0.007(3) C16 0.040(4) 0.025(3) 0.033(4) -0.005(3) -0.004(3) -0.001(3) C17 0.040(4) 0.041(4) 0.052(5) -0.003(3) -0.006(3) 0.002(3) C31 0.054(4) 0.023(3) 0.020(4) -0.009(3) 0.014(3) -0.005(3) C32 0.033(4) 0.031(4) 0.054(5) -0.010(3) 0.001(3) 0.001(3) C33 0.048(5) 0.033(4) 0.092(7) -0.016(4) 0.020(4) -0.008(4) C34 0.067(6) 0.039(5) 0.061(6) -0.022(4) 0.038(5) -0.009(4) C35 0.109(8) 0.039(5) 0.040(5) -0.003(4) 0.018(5) -0.002(5) C36 0.067(5) 0.035(4) 0.035(5) -0.016(3) 0.002(4) -0.008(4) N41 0.044(3) 0.028(3) 0.028(3) -0.008(2) 0.000(2) -0.007(3) C42 0.030(3) 0.027(3) 0.033(4) -0.007(3) -0.002(3) -0.007(3) N43 0.048(3) 0.031(3) 0.033(3) -0.009(2) 0.005(3) -0.001(3) C44 0.056(5) 0.024(4) 0.054(5) -0.013(3) 0.012(4) -0.004(3) C45 0.058(5) 0.031(4) 0.037(4) -0.013(3) 0.003(3) -0.012(3) C51 0.022(3) 0.030(4) 0.040(4) -0.010(3) 0.002(3) 0.000(3) C52 0.029(3) 0.028(3) 0.033(4) -0.010(3) 0.004(3) -0.008(3) C53 0.045(4) 0.043(4) 0.043(5) -0.006(3) 0.008(3) -0.013(4) C54 0.030(4) 0.044(4) 0.061(6) -0.007(4) 0.005(3) -0.014(3) C55 0.038(4) 0.037(4) 0.072(6) -0.005(4) -0.017(4) -0.002(3) C56 0.049(4) 0.027(4) 0.040(5) -0.004(3) -0.010(3) -0.012(3) C57 0.046(4) 0.040(4) 0.033(4) 0.001(3) -0.002(3) -0.009(3) C58 0.041(4) 0.069(6) 0.097(8) 0.002(5) 0.011(4) -0.006(4) C59 0.071(5) 0.037(4) 0.048(5) -0.010(3) -0.013(4) -0.003(4) C61 0.035(4) 0.027(4) 0.046(5) -0.016(3) 0.009(3) 0.000(3) C62 0.053(5) 0.039(4) 0.038(5) -0.018(3) 0.000(3) 0.003(4) C63 0.037(4) 0.043(4) 0.068(6) -0.027(4) -0.012(4) 0.006(3) C64 0.045(4) 0.054(5) 0.052(5) -0.019(4) 0.007(4) -0.008(4) C65 0.038(4) 0.039(4) 0.042(5) -0.011(3) 0.007(3) 0.000(3) C66 0.037(4) 0.032(4) 0.042(4) -0.016(3) 0.009(3) -0.005(3) C67 0.064(5) 0.054(5) 0.057(6) -0.021(4) -0.011(4) 0.007(4) C68 0.045(5) 0.096(7) 0.089(8) -0.026(6) 0.012(5) -0.009(5) C69 0.044(4) 0.056(5) 0.037(4) -0.012(3) 0.009(3) -0.001(4) C1A 0.037(4) 0.027(3) 0.028(4) -0.005(3) 0.000(3) -0.008(3) C2A 0.027(3) 0.036(4) 0.021(3) -0.013(3) 0.007(3) -0.011(3) C3A 0.027(3) 0.038(4) 0.017(3) -0.010(3) 0.009(2) -0.001(3) O1A 0.068(4) 0.092(4) 0.048(4) -0.027(3) -0.018(3) 0.011(3) O2A 0.119(4) 0.061(3) 0.086(4) -0.014(3) -0.031(3) 0.021(3) O3A 0.056(3) 0.122(4) 0.083(4) -0.032(3) 0.004(3) -0.008(3) O4A 0.056(3) 0.047(3) 0.062(4) -0.019(3) -0.003(3) -0.012(3) O5A 0.045(3) 0.121(5) 0.053(4) 0.008(3) -0.002(3) -0.030(3) O6A 0.033(2) 0.035(3) 0.033(3) -0.0108(19) 0.0028(19) 0.003(2) C11A 0.043(4) 0.057(5) 0.058(6) -0.021(4) -0.005(4) 0.011(4) C12A 0.089(6) 0.060(6) 0.055(6) -0.025(4) -0.039(5) 0.031(5) C13A 0.032(4) 0.108(7) 0.055(6) -0.039(5) 0.001(4) -0.013(5) C14A 0.040(4) 0.053(5) 0.027(4) -0.013(3) -0.001(3) -0.005(4) C15A 0.053(5) 0.060(5) 0.029(4) 0.000(3) -0.008(4) -0.003(4) C16A 0.035(4) 0.033(4) 0.039(4) -0.015(3) 0.005(3) 0.000(3) C17A 0.040(4) 0.047(4) 0.047(5) -0.022(3) 0.009(3) -0.006(3) C31A 0.022(3) 0.023(3) 0.037(4) -0.012(3) 0.006(3) 0.001(3) C32A 0.040(4) 0.045(4) 0.035(4) -0.015(3) 0.005(3) -0.009(3) C33A 0.051(4) 0.043(4) 0.052(5) -0.009(4) 0.015(4) -0.022(4) C34A 0.030(4) 0.058(5) 0.047(5) -0.016(4) 0.007(3) -0.009(3) C35A 0.029(3) 0.058(5) 0.041(5) -0.021(4) -0.005(3) -0.006(3) C36A 0.036(4) 0.034(4) 0.029(4) -0.004(3) 0.003(3) -0.005(3) N41A 0.024(3) 0.030(3) 0.026(3) -0.010(2) 0.006(2) -0.004(2) C42A 0.023(3) 0.028(3) 0.022(3) -0.015(3) -0.005(2) -0.001(3) N43A 0.028(3) 0.028(3) 0.032(3) -0.005(2) 0.002(2) -0.002(2) C44A 0.038(4) 0.021(3) 0.038(4) -0.005(3) -0.002(3) -0.002(3) C45A 0.024(3) 0.027(3) 0.034(4) -0.009(3) 0.004(3) -0.001(3) C51A 0.026(3) 0.032(4) 0.025(4) -0.004(3) 0.003(3) -0.002(3) C52A 0.029(3) 0.036(4) 0.029(4) -0.009(3) 0.002(3) -0.006(3) C53A 0.022(3) 0.056(5) 0.040(4) -0.010(3) 0.000(3) -0.004(3) C54A 0.037(4) 0.055(5) 0.036(4) -0.007(3) 0.011(3) 0.002(4) C55A 0.040(4) 0.045(4) 0.023(4) -0.011(3) 0.007(3) 0.003(3) C56A 0.035(3) 0.024(3) 0.027(4) -0.001(3) 0.000(3) -0.002(3) C57A 0.035(4) 0.049(4) 0.036(4) -0.012(3) 0.000(3) -0.011(3) C58A 0.043(4) 0.095(7) 0.046(5) -0.003(4) 0.022(4) 0.019(5) C59A 0.034(4) 0.040(4) 0.036(4) -0.015(3) 0.005(3) -0.009(3) C61A 0.029(3) 0.026(3) 0.034(4) -0.014(3) 0.012(3) -0.005(3) C62A 0.033(3) 0.018(3) 0.038(4) -0.013(3) 0.003(3) -0.002(3) C63A 0.046(4) 0.029(4) 0.030(4) -0.010(3) 0.010(3) -0.006(3) C64A 0.031(4) 0.034(4) 0.042(5) -0.008(3) 0.015(3) -0.010(3) C65A 0.032(4) 0.037(4) 0.045(5) -0.015(3) 0.006(3) -0.010(3) C66A 0.034(4) 0.031(4) 0.033(4) -0.005(3) 0.003(3) -0.004(3) C67A 0.045(4) 0.047(4) 0.029(4) -0.013(3) 0.002(3) 0.006(3) C68A 0.042(4) 0.080(6) 0.060(6) -0.014(4) 0.013(4) -0.025(4) C69A 0.027(3) 0.052(5) 0.053(5) -0.004(4) 0.007(3) -0.006(3) O7 0.060(4) 0.028(4) 0.017(4) -0.004(3) -0.008(3) 0.024(3) C71 0.058(5) 0.034(5) 0.035(5) 0.000(4) -0.004(4) 0.010(4) C72 0.053(5) 0.019(4) 0.028(5) -0.006(4) -0.004(4) 0.008(4) C73 0.026(4) 0.021(4) 0.013(4) 0.002(3) -0.001(3) 0.009(4) C74 0.017(4) 0.020(4) 0.012(4) -0.001(3) 0.000(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C12 1.859(8) . ? Cr1 C11 1.864(7) . ? Cr1 C13 1.877(6) . ? Cr1 C15 1.878(7) . ? Cr1 C14 1.919(7) . ? Cr1 C1 2.142(6) . ? Cr1A C11A 1.839(8) . ? Cr1A C13A 1.846(8) . ? Cr1A C12A 1.865(8) . ? Cr1A C15A 1.884(8) . ? Cr1A C14A 1.886(7) . ? Cr1A C1A 2.178(6) . ? C1 C2 1.310(8) . ? C1 O6 1.399(6) . ? C2 C3 1.328(8) . ? C3 C42 1.460(8) . ? C3 C31 1.517(8) . ? O1 C11 1.144(7) . ? O2 C12 1.178(8) . ? O3 C13 1.161(7) . ? O4 C14 1.133(7) . ? O5 C15 1.168(7) . ? O6 C16 1.433(7) . ? C16 C17 1.497(8) . ? C31 C36 1.372(9) . ? C31 C32 1.383(9) . ? C32 C33 1.394(10) . ? C33 C34 1.366(11) . ? C34 C35 1.342(11) . ? C35 C36 1.408(11) . ? N41 C42 1.360(8) . ? N41 C45 1.402(8) . ? N41 C51 1.449(7) . ? C42 N43 1.368(7) . ? N43 C44 1.398(8) . ? N43 C61 1.460(8) . ? C44 C45 1.350(9) . ? C51 C52 1.382(8) . ? C51 C56 1.393(8) . ? C52 C53 1.383(8) . ? C52 C57 1.496(8) . ? C53 C54 1.412(9) . ? C54 C55 1.362(10) . ? C54 C58 1.508(9) . ? C55 C56 1.414(9) . ? C56 C59 1.483(9) . ? C61 C62 1.367(9) . ? C61 C66 1.398(9) . ? C62 C63 1.407(10) . ? C62 C67 1.514(10) . ? C63 C64 1.391(10) . ? C64 C65 1.387(9) . ? C64 C68 1.513(10) . ? C65 C66 1.366(9) . ? C66 C69 1.505(9) . ? C1A C2A 1.288(8) . ? C1A O6A 1.414(7) . ? C2A C3A 1.352(8) . ? C3A C42A 1.461(8) . ? C3A C31A 1.494(8) . ? O1A C11A 1.176(8) . ? O2A C12A 1.165(9) . ? O3A C13A 1.182(9) . ? O4A C14A 1.150(8) . ? O5A C15A 1.142(8) . ? O6A C16A 1.416(7) . ? C16A C17A 1.512(8) . ? C31A C36A 1.359(8) . ? C31A C32A 1.391(9) . ? C32A C33A 1.400(9) . ? C33A C34A 1.362(9) . ? C34A C35A 1.340(10) . ? C35A C36A 1.387(9) . ? N41A C42A 1.358(7) . ? N41A C45A 1.381(7) . ? N41A C51A 1.447(7) . ? C42A N43A 1.361(7) . ? N43A C44A 1.403(8) . ? N43A C61A 1.445(7) . ? C44A C45A 1.348(8) . ? C51A C56A 1.376(8) . ? C51A C52A 1.394(8) . ? C52A C53A 1.400(8) . ? C52A C57A 1.511(8) . ? C53A C54A 1.365(9) . ? C54A C55A 1.400(9) . ? C54A C58A 1.515(9) . ? C55A C56A 1.402(8) . ? C56A C59A 1.513(8) . ? C61A C66A 1.389(8) . ? C61A C62A 1.410(8) . ? C62A C63A 1.383(8) . ? C62A C67A 1.501(8) . ? C63A C64A 1.373(8) . ? C64A C65A 1.379(9) . ? C64A C68A 1.526(9) . ? C65A C66A 1.390(8) . ? C66A C69A 1.514(9) . ? O7 C71 1.244(13) . ? O7 C73 1.381(13) . ? C71 C72 1.450(17) . ? C73 C74 1.451(15) . ? 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 Cr1 C11 90.9(3) . . ? C12 Cr1 C13 86.6(3) . . ? C11 Cr1 C13 89.7(3) . . ? C12 Cr1 C15 87.3(3) . . ? C11 Cr1 C15 91.0(3) . . ? C13 Cr1 C15 173.9(3) . . ? C12 Cr1 C14 177.7(3) . . ? C11 Cr1 C14 91.2(3) . . ? C13 Cr1 C14 94.5(3) . . ? C15 Cr1 C14 91.6(3) . . ? C12 Cr1 C1 94.3(3) . . ? C11 Cr1 C1 174.8(3) . . ? C13 Cr1 C1 91.2(2) . . ? C15 Cr1 C1 88.7(2) . . ? C14 Cr1 C1 83.7(2) . . ? C11A Cr1A C13A 91.0(3) . . ? C11A Cr1A C12A 90.5(3) . . ? C13A Cr1A C12A 90.5(4) . . ? C11A Cr1A C15A 91.9(3) . . ? C13A Cr1A C15A 177.0(3) . . ? C12A Cr1A C15A 88.8(4) . . ? C11A Cr1A C14A 85.9(3) . . ? C13A Cr1A C14A 88.8(3) . . ? C12A Cr1A C14A 176.4(3) . . ? C15A Cr1A C14A 92.0(3) . . ? C11A Cr1A C1A 174.5(3) . . ? C13A Cr1A C1A 84.4(3) . . ? C12A Cr1A C1A 86.5(3) . . ? C15A Cr1A C1A 92.6(3) . . ? C14A Cr1A C1A 97.0(3) . . ? C2 C1 O6 121.0(6) . . ? C2 C1 Cr1 124.4(5) . . ? O6 C1 Cr1 114.5(4) . . ? C1 C2 C3 164.6(7) . . ? C2 C3 C42 121.6(6) . . ? C2 C3 C31 119.1(6) . . ? C42 C3 C31 119.2(5) . . ? C1 O6 C16 115.9(4) . . ? O1 C11 Cr1 179.3(6) . . ? O2 C12 Cr1 178.4(6) . . ? O3 C13 Cr1 173.2(6) . . ? O4 C14 Cr1 177.9(6) . . ? O5 C15 Cr1 176.2(6) . . ? O6 C16 C17 110.0(5) . . ? C36 C31 C32 118.7(6) . . ? C36 C31 C3 120.8(6) . . ? C32 C31 C3 120.4(6) . . ? C31 C32 C33 121.2(7) . . ? C34 C33 C32 119.1(8) . . ? C35 C34 C33 120.3(8) . . ? C34 C35 C36 121.4(8) . . ? C31 C36 C35 119.2(7) . . ? C42 N41 C45 110.5(5) . . ? C42 N41 C51 129.8(5) . . ? C45 N41 C51 119.4(5) . . ? N41 C42 N43 105.7(5) . . ? N41 C42 C3 126.9(5) . . ? N43 C42 C3 127.4(6) . . ? C42 N43 C44 109.5(5) . . ? C42 N43 C61 129.6(5) . . ? C44 N43 C61 120.8(5) . . ? C45 C44 N43 107.9(6) . . ? C44 C45 N41 106.3(6) . . ? C52 C51 C56 124.1(6) . . ? C52 C51 N41 119.5(5) . . ? C56 C51 N41 116.3(6) . . ? C51 C52 C53 116.9(6) . . ? C51 C52 C57 121.9(5) . . ? C53 C52 C57 121.2(6) . . ? C52 C53 C54 121.9(7) . . ? C55 C54 C53 118.7(6) . . ? C55 C54 C58 121.1(7) . . ? C53 C54 C58 120.1(7) . . ? C54 C55 C56 122.0(6) . . ? C51 C56 C55 116.3(6) . . ? C51 C56 C59 122.0(6) . . ? C55 C56 C59 121.7(6) . . ? C62 C61 C66 123.1(6) . . ? C62 C61 N43 118.6(6) . . ? C66 C61 N43 118.2(6) . . ? C61 C62 C63 117.8(7) . . ? C61 C62 C67 121.7(7) . . ? C63 C62 C67 120.5(6) . . ? C64 C63 C62 120.3(6) . . ? C65 C64 C63 119.4(7) . . ? C65 C64 C68 120.9(7) . . ? C63 C64 C68 119.7(7) . . ? C66 C65 C64 121.7(7) . . ? C65 C66 C61 117.7(6) . . ? C65 C66 C69 121.1(6) . . ? C61 C66 C69 121.2(6) . . ? C2A C1A O6A 120.8(6) . . ? C2A C1A Cr1A 127.7(5) . . ? O6A C1A Cr1A 111.4(4) . . ? C1A C2A C3A 171.6(6) . . ? C2A C3A C42A 119.8(5) . . ? C2A C3A C31A 123.4(6) . . ? C42A C3A C31A 116.8(5) . . ? C1A O6A C16A 116.9(4) . . ? O1A C11A Cr1A 178.4(6) . . ? O2A C12A Cr1A 176.7(9) . . ? O3A C13A Cr1A 176.4(8) . . ? O4A C14A Cr1A 173.5(6) . . ? O5A C15A Cr1A 176.8(6) . . ? O6A C16A C17A 107.7(5) . . ? C36A C31A C32A 117.7(6) . . ? C36A C31A C3A 122.1(6) . . ? C32A C31A C3A 120.2(6) . . ? C31A C32A C33A 119.9(6) . . ? C34A C33A C32A 120.6(7) . . ? C35A C34A C33A 119.2(7) . . ? C34A C35A C36A 121.1(6) . . ? C31A C36A C35A 121.5(6) . . ? C42A N41A C45A 110.4(5) . . ? C42A N41A C51A 127.9(5) . . ? C45A N41A C51A 121.4(5) . . ? N41A C42A N43A 106.2(5) . . ? N41A C42A C3A 128.0(5) . . ? N43A C42A C3A 125.7(5) . . ? C42A N43A C44A 108.9(5) . . ? C42A N43A C61A 128.8(5) . . ? C44A N43A C61A 122.3(5) . . ? C45A C44A N43A 107.4(5) . . ? C44A C45A N41A 107.1(5) . . ? C56A C51A C52A 123.3(5) . . ? C56A C51A N41A 119.2(5) . . ? C52A C51A N41A 117.2(5) . . ? C51A C52A C53A 116.7(6) . . ? C51A C52A C57A 122.5(5) . . ? C53A C52A C57A 120.7(5) . . ? C54A C53A C52A 122.5(6) . . ? C53A C54A C55A 118.8(6) . . ? C53A C54A C58A 121.2(6) . . ? C55A C54A C58A 120.1(6) . . ? C54A C55A C56A 121.1(6) . . ? C51A C56A C55A 117.6(5) . . ? C51A C56A C59A 122.8(5) . . ? C55A C56A C59A 119.5(6) . . ? C66A C61A C62A 122.6(5) . . ? C66A C61A N43A 119.6(6) . . ? C62A C61A N43A 117.6(5) . . ? C63A C62A C61A 116.5(5) . . ? C63A C62A C67A 121.8(6) . . ? C61A C62A C67A 121.6(5) . . ? C64A C63A C62A 122.7(6) . . ? C63A C64A C65A 118.9(6) . . ? C63A C64A C68A 120.7(6) . . ? C65A C64A C68A 120.4(6) . . ? C64A C65A C66A 121.8(6) . . ? C61A C66A C65A 117.4(6) . . ? C61A C66A C69A 122.7(6) . . ? C65A C66A C69A 119.8(5) . . ? C71 O7 C73 120.0(9) . . ? O7 C71 C72 120.0(11) . . ? O7 C73 C74 113.5(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C45A H45A O6 0.95 2.37 3.299(7) 166.1 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.162 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.098 data_AST317b _database_code_depnum_ccdc_archive 'CCDC 893653' #TrackingRef 'web_deposit_cif_file_1_CarmenRamirezdeArellano_1343213556.AST317b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H90 Fe2 N4 O5' _chemical_formula_weight 1251.22 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 10.7606(10) _cell_length_b 12.5977(12) _cell_length_c 12.7837(12) _cell_angle_alpha 89.969(2) _cell_angle_beta 75.748(2) _cell_angle_gamma 85.623(2) _cell_volume 1674.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1835 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 21.00 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.487 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 12955 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.1193 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5745 _reflns_number_gt 2778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^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 5745 _refine_ls_number_parameters 379 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1275 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1655 _refine_ls_wR_factor_gt 0.1436 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.003 _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 0.4975(5) 0.3311(4) 0.9440(4) 0.0594(15) Uani 1 1 d . . . H1 H 0.4485 0.3807 0.9943 0.071 Uiso 1 1 calc R . . C2 C 0.4554(5) 0.2469(4) 0.9059(4) 0.0621(16) Uani 1 1 d . . . H2 H 0.3714 0.2271 0.9243 0.074 Uiso 1 1 calc R . . C3 C 0.6667(5) 0.2453(3) 0.8270(4) 0.0395(12) Uani 1 1 d . . . C4 C 0.7044(4) 0.4176(3) 0.9117(4) 0.0406(12) Uani 1 1 d . . . C5 C 0.7397(4) 0.4902(4) 0.8313(4) 0.0446(12) Uani 1 1 d . . . C6 C 0.8064(5) 0.5744(4) 0.8518(4) 0.0553(14) Uani 1 1 d . . . H6 H 0.8306 0.6239 0.7981 0.066 Uiso 1 1 calc R . . C7 C 0.8385(5) 0.5879(4) 0.9489(5) 0.0575(15) Uani 1 1 d . . . C8 C 0.7999(5) 0.5135(4) 1.0262(5) 0.0611(16) Uani 1 1 d . . . H8 H 0.8200 0.5213 1.0924 0.073 Uiso 1 1 calc R . . C9 C 0.7327(5) 0.4270(4) 1.0115(4) 0.0534(14) Uani 1 1 d . . . C10 C 0.7089(6) 0.4809(4) 0.7237(4) 0.0694(17) Uani 1 1 d . . . H10A H 0.7245 0.5461 0.6855 0.104 Uiso 1 1 calc R . . H10B H 0.6201 0.4674 0.7341 0.104 Uiso 1 1 calc R . . H10C H 0.7622 0.4233 0.6826 0.104 Uiso 1 1 calc R . . C11 C 0.9103(5) 0.6803(5) 0.9686(5) 0.092(2) Uani 1 1 d . . . H11A H 0.8556 0.7450 0.9732 0.139 Uiso 1 1 calc R . . H11B H 0.9852 0.6847 0.9101 0.139 Uiso 1 1 calc R . . H11C H 0.9359 0.6706 1.0350 0.139 Uiso 1 1 calc R . . C12 C 0.6922(6) 0.3474(4) 1.1001(4) 0.0805(19) Uani 1 1 d . . . H12A H 0.6056 0.3670 1.1402 0.121 Uiso 1 1 calc R . . H12B H 0.7486 0.3470 1.1477 0.121 Uiso 1 1 calc R . . H12C H 0.6966 0.2776 1.0686 0.121 Uiso 1 1 calc R . . C13 C 0.5572(4) 0.0872(4) 0.7922(4) 0.0455(13) Uani 1 1 d . . . C14 C 0.6189(4) 0.0037(4) 0.8358(4) 0.0489(13) Uani 1 1 d . . . C15 C 0.6167(5) -0.0974(4) 0.7937(5) 0.0593(15) Uani 1 1 d . . . H15 H 0.6578 -0.1547 0.8210 0.071 Uiso 1 1 calc R . . C16 C 0.5553(5) -0.1166(4) 0.7123(5) 0.0612(15) Uani 1 1 d . . . C17 C 0.4916(5) -0.0311(4) 0.6755(5) 0.0659(16) Uani 1 1 d . . . H17 H 0.4480 -0.0429 0.6227 0.079 Uiso 1 1 calc R . . C18 C 0.4899(5) 0.0724(4) 0.7145(4) 0.0531(14) Uani 1 1 d . . . C19 C 0.6825(6) 0.0188(4) 0.9257(4) 0.0736(17) Uani 1 1 d . . . H19A H 0.6958 -0.0485 0.9580 0.110 Uiso 1 1 calc R . . H19B H 0.6287 0.0670 0.9791 0.110 Uiso 1 1 calc R . . H19C H 0.7639 0.0477 0.8978 0.110 Uiso 1 1 calc R . . C20 C 0.5559(6) -0.2290(4) 0.6695(5) 0.088(2) Uani 1 1 d . . . H20A H 0.4692 -0.2492 0.6832 0.132 Uiso 1 1 calc R . . H20B H 0.6050 -0.2771 0.7049 0.132 Uiso 1 1 calc R . . H20C H 0.5938 -0.2317 0.5931 0.132 Uiso 1 1 calc R . . C21 C 0.4154(5) 0.1605(4) 0.6719(5) 0.0747(18) Uani 1 1 d . . . H21A H 0.4390 0.1576 0.5944 0.112 Uiso 1 1 calc R . . H21B H 0.4344 0.2278 0.6966 0.112 Uiso 1 1 calc R . . H21C H 0.3250 0.1524 0.6973 0.112 Uiso 1 1 calc R . . C22 C 0.7919(4) 0.2166(3) 0.7595(4) 0.0354(11) Uani 1 1 d . . . C23 C 0.8948(4) 0.2103(3) 0.8096(4) 0.0401(12) Uani 1 1 d . . . C24 C 1.0303(4) 0.1766(4) 0.7429(4) 0.0523(14) Uani 1 1 d . . . H24A H 1.0358 0.1925 0.6678 0.063 Uiso 1 1 calc R . . H24B H 1.0911 0.2179 0.7667 0.063 Uiso 1 1 calc R . . C25 C 1.0909(6) 0.0352(5) 0.8489(5) 0.084(2) Uani 1 1 d . . . H25A H 1.0131 0.0467 0.9064 0.100 Uiso 1 1 calc R . . H25B H 1.1551 0.0781 0.8651 0.100 Uiso 1 1 calc R . . C26 C 1.1377(6) -0.0778(5) 0.8441(5) 0.098(2) Uani 1 1 d . . . H26A H 1.0782 -0.1198 0.8211 0.147 Uiso 1 1 calc R . . H26B H 1.1452 -0.0998 0.9144 0.147 Uiso 1 1 calc R . . H26C H 1.2204 -0.0876 0.7938 0.147 Uiso 1 1 calc R . . C27 C 0.7948(4) 0.1789(3) 0.6491(4) 0.0377(11) Uani 1 1 d . . . C28 C 0.7185(4) 0.2272(4) 0.5830(4) 0.0451(13) Uani 1 1 d . . . H28 H 0.6669 0.2906 0.5991 0.054 Uiso 1 1 calc R . . C29 C 0.7335(5) 0.1637(4) 0.4891(4) 0.0552(14) Uani 1 1 d . . . H29 H 0.6924 0.1769 0.4339 0.066 Uiso 1 1 calc R . . C30 C 0.8219(5) 0.0766(4) 0.4941(4) 0.0544(14) Uani 1 1 d . . . H30 H 0.8495 0.0222 0.4426 0.065 Uiso 1 1 calc R . . C31 C 0.8613(4) 0.0863(3) 0.5912(4) 0.0445(12) Uani 1 1 d . . . H31 H 0.9208 0.0399 0.6136 0.053 Uiso 1 1 calc R . . C32 C 0.9526(6) 0.3649(4) 0.4471(5) 0.0705(17) Uani 1 1 d . . . H32 H 0.9003 0.4277 0.4653 0.085 Uiso 1 1 calc R . . C33 C 1.0370(6) 0.3206(5) 0.5039(5) 0.0702(17) Uani 1 1 d . . . H33 H 1.0516 0.3488 0.5666 0.084 Uiso 1 1 calc R . . C34 C 1.0971(5) 0.2251(5) 0.4506(6) 0.0747(18) Uani 1 1 d . . . H34 H 1.1573 0.1790 0.4722 0.090 Uiso 1 1 calc R . . C35 C 1.0494(6) 0.2126(5) 0.3592(5) 0.0768(18) Uani 1 1 d . . . H35 H 1.0731 0.1568 0.3089 0.092 Uiso 1 1 calc R . . C36 C 0.9595(6) 0.2987(5) 0.3566(5) 0.0727(17) Uani 1 1 d . . . H36 H 0.9130 0.3101 0.3046 0.087 Uiso 1 1 calc R . . Fe1 Fe 0.90335(7) 0.21657(5) 0.49505(6) 0.0462(3) Uani 1 1 d . . . N1 N 0.6282(4) 0.3322(3) 0.8955(3) 0.0439(10) Uani 1 1 d . . . N2 N 0.5586(4) 0.1935(3) 0.8338(3) 0.0455(10) Uani 1 1 d . . . O1 O 0.8814(3) 0.2276(2) 0.9083(3) 0.0584(10) Uani 1 1 d . . . O2 O 1.0654(3) 0.0667(3) 0.7516(3) 0.0706(11) Uani 1 1 d . . . O3 O 0.5000 0.5000 0.5000 0.253(5) Uiso 1 2 d SD . . C37 C 0.3881(6) 0.4832(9) 0.5808(7) 0.232(5) Uiso 1 1 d D . . H37A H 0.3323 0.5339 0.5530 0.278 Uiso 1 1 calc R . . H37B H 0.4116 0.5237 0.6365 0.278 Uiso 1 1 calc R . . C38 C 0.2795(11) 0.4310(12) 0.6574(11) 0.347(9) Uiso 1 1 d D . . H38A H 0.2700 0.3627 0.6284 0.521 Uiso 1 1 calc R . . H38B H 0.2009 0.4752 0.6657 0.521 Uiso 1 1 calc R . . H38C H 0.2991 0.4223 0.7263 0.521 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 C1 0.043(3) 0.047(3) 0.074(4) -0.011(3) 0.011(3) 0.000(3) C2 0.032(3) 0.052(3) 0.088(4) -0.003(3) 0.012(3) -0.003(3) C3 0.041(3) 0.032(3) 0.042(3) -0.002(2) -0.006(2) 0.000(2) C4 0.035(3) 0.035(3) 0.048(3) -0.007(2) -0.004(2) 0.003(2) C5 0.046(3) 0.038(3) 0.047(3) -0.002(3) -0.006(3) 0.000(2) C6 0.050(3) 0.046(3) 0.066(4) -0.001(3) -0.007(3) -0.008(3) C7 0.044(3) 0.052(3) 0.076(4) -0.012(3) -0.013(3) -0.005(3) C8 0.063(4) 0.063(4) 0.059(4) -0.022(3) -0.024(3) 0.009(3) C9 0.059(4) 0.047(3) 0.050(4) -0.005(3) -0.007(3) 0.008(3) C10 0.105(5) 0.046(3) 0.059(4) 0.003(3) -0.025(4) -0.004(3) C11 0.068(4) 0.088(5) 0.125(6) -0.033(4) -0.026(4) -0.022(4) C12 0.111(5) 0.074(4) 0.048(4) 0.005(3) -0.009(4) 0.009(4) C13 0.030(3) 0.039(3) 0.062(4) 0.001(3) 0.001(3) -0.006(2) C14 0.042(3) 0.044(3) 0.057(4) 0.009(3) -0.003(3) -0.008(2) C15 0.051(4) 0.041(3) 0.081(4) 0.015(3) -0.007(3) -0.008(3) C16 0.046(3) 0.047(3) 0.087(5) -0.005(3) -0.005(3) -0.017(3) C17 0.057(4) 0.059(4) 0.085(4) -0.002(3) -0.021(3) -0.017(3) C18 0.036(3) 0.047(3) 0.076(4) 0.010(3) -0.012(3) -0.011(2) C19 0.087(5) 0.065(4) 0.074(4) 0.016(3) -0.028(4) -0.011(3) C20 0.091(5) 0.053(4) 0.115(6) -0.010(4) -0.014(4) -0.017(3) C21 0.046(3) 0.072(4) 0.111(5) 0.017(4) -0.029(3) -0.005(3) C22 0.026(3) 0.032(2) 0.044(3) 0.001(2) -0.003(2) 0.001(2) C23 0.040(3) 0.034(3) 0.043(3) 0.001(2) -0.006(3) 0.000(2) C24 0.039(3) 0.055(3) 0.060(4) 0.009(3) -0.009(3) 0.002(3) C25 0.103(5) 0.088(5) 0.058(4) 0.007(3) -0.027(4) 0.025(4) C26 0.124(6) 0.079(5) 0.085(5) 0.013(4) -0.026(4) 0.032(4) C27 0.030(3) 0.036(3) 0.043(3) 0.000(2) -0.001(2) -0.003(2) C28 0.041(3) 0.045(3) 0.050(3) -0.008(2) -0.011(3) 0.001(2) C29 0.055(4) 0.064(3) 0.049(3) 0.000(3) -0.017(3) -0.009(3) C30 0.063(4) 0.045(3) 0.051(3) -0.010(3) -0.005(3) -0.005(3) C31 0.041(3) 0.036(3) 0.050(3) -0.002(2) 0.000(3) -0.001(2) C32 0.083(5) 0.052(3) 0.072(4) 0.012(3) -0.011(4) -0.010(3) C33 0.068(4) 0.076(4) 0.072(4) 0.018(4) -0.021(4) -0.029(4) C34 0.054(4) 0.080(5) 0.086(5) 0.031(4) -0.006(4) -0.012(3) C35 0.074(5) 0.076(4) 0.063(4) 0.013(3) 0.015(4) -0.006(4) C36 0.088(5) 0.076(4) 0.050(4) 0.023(3) -0.007(3) -0.017(4) Fe1 0.0453(5) 0.0437(4) 0.0464(5) 0.0016(3) -0.0049(4) -0.0047(3) N1 0.039(3) 0.034(2) 0.052(3) 0.0003(19) 0.002(2) -0.0011(19) N2 0.032(2) 0.037(2) 0.060(3) -0.002(2) 0.003(2) -0.0050(19) O1 0.061(2) 0.064(2) 0.051(2) -0.0106(18) -0.0190(19) 0.0113(18) O2 0.076(3) 0.074(3) 0.058(3) -0.005(2) -0.020(2) 0.029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.322(6) . ? C1 N1 1.392(5) . ? C2 N2 1.385(5) . ? C3 N2 1.362(5) . ? C3 N1 1.375(5) . ? C3 C22 1.430(6) . ? C4 C5 1.378(6) . ? C4 C9 1.390(6) . ? C4 N1 1.445(5) . ? C5 C6 1.385(6) . ? C5 C10 1.499(6) . ? C6 C7 1.381(7) . ? C7 C8 1.373(7) . ? C7 C11 1.499(7) . ? C8 C9 1.390(7) . ? C9 C12 1.518(7) . ? C13 C14 1.389(6) . ? C13 C18 1.387(6) . ? C13 N2 1.443(5) . ? C14 C15 1.388(6) . ? C14 C19 1.495(7) . ? C15 C16 1.393(7) . ? C16 C17 1.377(7) . ? C16 C20 1.517(6) . ? C17 C18 1.393(6) . ? C18 C21 1.500(6) . ? C22 C23 1.406(6) . ? C22 C27 1.481(6) . ? C23 O1 1.252(5) . ? C23 C24 1.525(6) . ? C24 O2 1.418(5) . ? C25 O2 1.390(6) . ? C25 C26 1.469(7) . ? C27 C28 1.423(6) . ? C27 C31 1.427(5) . ? C27 Fe1 2.102(4) . ? C28 C29 1.412(6) . ? C28 Fe1 2.024(5) . ? C29 C30 1.408(6) . ? C29 Fe1 2.011(5) . ? C30 C31 1.416(6) . ? C30 Fe1 2.030(5) . ? C31 Fe1 2.061(5) . ? C32 C33 1.383(7) . ? C32 C36 1.410(7) . ? C32 Fe1 2.035(5) . ? C33 C34 1.412(7) . ? C33 Fe1 2.041(5) . ? C34 C35 1.401(8) . ? C34 Fe1 2.033(6) . ? C35 C36 1.403(7) . ? C35 Fe1 2.033(6) . ? C36 Fe1 2.034(5) . ? O3 C37 1.4096(5) . ? O3 C37 1.4096(5) 2_666 ? C37 C38 1.5196(5) . ? 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 C2 C1 N1 107.8(4) . . ? C1 C2 N2 107.9(4) . . ? N2 C3 N1 105.3(4) . . ? N2 C3 C22 126.8(4) . . ? N1 C3 C22 127.9(4) . . ? C5 C4 C9 122.1(5) . . ? C5 C4 N1 119.6(4) . . ? C9 C4 N1 118.2(5) . . ? C6 C5 C4 118.1(5) . . ? C6 C5 C10 119.5(5) . . ? C4 C5 C10 122.4(4) . . ? C5 C6 C7 122.7(5) . . ? C8 C7 C6 116.6(5) . . ? C8 C7 C11 122.1(5) . . ? C6 C7 C11 121.3(6) . . ? C7 C8 C9 123.9(5) . . ? C4 C9 C8 116.6(5) . . ? C4 C9 C12 121.8(5) . . ? C8 C9 C12 121.6(5) . . ? C14 C13 C18 123.0(4) . . ? C14 C13 N2 118.2(4) . . ? C18 C13 N2 118.7(4) . . ? C15 C14 C13 116.9(5) . . ? C15 C14 C19 120.2(5) . . ? C13 C14 C19 123.0(4) . . ? C14 C15 C16 122.6(5) . . ? C17 C16 C15 117.7(5) . . ? C17 C16 C20 121.9(5) . . ? C15 C16 C20 120.3(5) . . ? C18 C17 C16 122.5(5) . . ? C17 C18 C13 117.2(5) . . ? C17 C18 C21 119.0(5) . . ? C13 C18 C21 123.8(5) . . ? C3 C22 C23 116.8(4) . . ? C3 C22 C27 115.4(4) . . ? C23 C22 C27 126.9(4) . . ? O1 C23 C22 123.5(4) . . ? O1 C23 C24 117.0(4) . . ? C22 C23 C24 119.5(4) . . ? O2 C24 C23 112.8(4) . . ? O2 C25 C26 111.0(5) . . ? C28 C27 C31 106.2(4) . . ? C28 C27 C22 124.3(4) . . ? C31 C27 C22 129.3(4) . . ? C28 C27 Fe1 66.9(3) . . ? C31 C27 Fe1 68.4(3) . . ? C22 C27 Fe1 133.1(3) . . ? C27 C28 C29 109.2(4) . . ? C27 C28 Fe1 72.8(3) . . ? C29 C28 Fe1 69.0(3) . . ? C30 C29 C28 107.7(4) . . ? C30 C29 Fe1 70.3(3) . . ? C28 C29 Fe1 70.0(3) . . ? C29 C30 C31 108.1(4) . . ? C29 C30 Fe1 68.9(3) . . ? C31 C30 Fe1 71.0(3) . . ? C27 C31 C30 108.7(4) . . ? C27 C31 Fe1 71.5(3) . . ? C30 C31 Fe1 68.6(3) . . ? C33 C32 C36 108.3(5) . . ? C33 C32 Fe1 70.4(3) . . ? C36 C32 Fe1 69.7(3) . . ? C32 C33 C34 108.4(6) . . ? C32 C33 Fe1 69.9(3) . . ? C34 C33 Fe1 69.4(3) . . ? C33 C34 C35 107.5(6) . . ? C33 C34 Fe1 70.0(3) . . ? C35 C34 Fe1 69.9(3) . . ? C36 C35 C34 108.2(6) . . ? C36 C35 Fe1 69.9(3) . . ? C34 C35 Fe1 69.8(3) . . ? C35 C36 C32 107.6(6) . . ? C35 C36 Fe1 69.8(3) . . ? C32 C36 Fe1 69.8(3) . . ? C29 Fe1 C28 40.96(17) . . ? C29 Fe1 C32 122.4(2) . . ? C28 Fe1 C32 108.8(2) . . ? C29 Fe1 C30 40.78(18) . . ? C28 Fe1 C30 68.36(19) . . ? C32 Fe1 C30 157.6(2) . . ? C29 Fe1 C36 104.9(2) . . ? C28 Fe1 C36 121.8(2) . . ? C32 Fe1 C36 40.6(2) . . ? C30 Fe1 C36 120.6(2) . . ? C29 Fe1 C33 159.5(2) . . ? C28 Fe1 C33 125.5(2) . . ? C32 Fe1 C33 39.7(2) . . ? C30 Fe1 C33 159.6(2) . . ? C36 Fe1 C33 67.5(2) . . ? C29 Fe1 C34 156.3(2) . . ? C28 Fe1 C34 161.9(2) . . ? C32 Fe1 C34 67.7(2) . . ? C30 Fe1 C34 121.9(2) . . ? C36 Fe1 C34 67.9(2) . . ? C33 Fe1 C34 40.6(2) . . ? C29 Fe1 C35 119.7(2) . . ? C28 Fe1 C35 156.6(2) . . ? C32 Fe1 C35 67.8(2) . . ? C30 Fe1 C35 105.5(2) . . ? C36 Fe1 C35 40.4(2) . . ? C33 Fe1 C35 67.7(2) . . ? C34 Fe1 C35 40.3(2) . . ? C29 Fe1 C31 68.3(2) . . ? C28 Fe1 C31 67.77(18) . . ? C32 Fe1 C31 160.9(2) . . ? C30 Fe1 C31 40.48(17) . . ? C36 Fe1 C31 157.7(2) . . ? C33 Fe1 C31 125.8(2) . . ? C34 Fe1 C31 109.4(2) . . ? C35 Fe1 C31 123.1(2) . . ? C29 Fe1 C27 68.32(19) . . ? C28 Fe1 C27 40.28(16) . . ? C32 Fe1 C27 125.2(2) . . ? C30 Fe1 C27 67.94(18) . . ? C36 Fe1 C27 159.1(2) . . ? C33 Fe1 C27 111.6(2) . . ? C34 Fe1 C27 126.1(2) . . ? C35 Fe1 C27 160.3(2) . . ? C31 Fe1 C27 40.06(15) . . ? C3 N1 C1 109.1(4) . . ? C3 N1 C4 127.5(4) . . ? C1 N1 C4 123.2(4) . . ? C3 N2 C2 109.8(4) . . ? C3 N2 C13 124.6(4) . . ? C2 N2 C13 124.1(4) . . ? C25 O2 C24 116.3(4) . . ? C37 O3 C37 179.998(1) . 2_666 ? O3 C37 C38 163.0(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 0.4(6) . . . . ? C9 C4 C5 C6 0.6(7) . . . . ? N1 C4 C5 C6 176.4(4) . . . . ? C9 C4 C5 C10 -179.7(4) . . . . ? N1 C4 C5 C10 -3.8(6) . . . . ? C4 C5 C6 C7 0.0(7) . . . . ? C10 C5 C6 C7 -179.8(4) . . . . ? C5 C6 C7 C8 -0.5(7) . . . . ? C5 C6 C7 C11 -179.7(4) . . . . ? C6 C7 C8 C9 0.5(8) . . . . ? C11 C7 C8 C9 179.6(5) . . . . ? C5 C4 C9 C8 -0.6(7) . . . . ? N1 C4 C9 C8 -176.5(4) . . . . ? C5 C4 C9 C12 179.3(4) . . . . ? N1 C4 C9 C12 3.3(6) . . . . ? C7 C8 C9 C4 0.0(7) . . . . ? C7 C8 C9 C12 -179.8(5) . . . . ? C18 C13 C14 C15 3.4(7) . . . . ? N2 C13 C14 C15 -179.6(4) . . . . ? C18 C13 C14 C19 -175.0(5) . . . . ? N2 C13 C14 C19 2.0(7) . . . . ? C13 C14 C15 C16 -0.5(8) . . . . ? C19 C14 C15 C16 177.9(5) . . . . ? C14 C15 C16 C17 -2.0(8) . . . . ? C14 C15 C16 C20 -180.0(5) . . . . ? C15 C16 C17 C18 1.8(8) . . . . ? C20 C16 C17 C18 179.7(5) . . . . ? C16 C17 C18 C13 0.8(8) . . . . ? C16 C17 C18 C21 -178.5(5) . . . . ? C14 C13 C18 C17 -3.6(8) . . . . ? N2 C13 C18 C17 179.5(4) . . . . ? C14 C13 C18 C21 175.8(5) . . . . ? N2 C13 C18 C21 -1.2(7) . . . . ? N2 C3 C22 C23 -129.6(5) . . . . ? N1 C3 C22 C23 53.0(6) . . . . ? N2 C3 C22 C27 40.3(6) . . . . ? N1 C3 C22 C27 -137.2(5) . . . . ? C3 C22 C23 O1 0.5(7) . . . . ? C27 C22 C23 O1 -168.0(4) . . . . ? C3 C22 C23 C24 178.0(4) . . . . ? C27 C22 C23 C24 9.6(7) . . . . ? O1 C23 C24 O2 81.0(5) . . . . ? C22 C23 C24 O2 -96.7(5) . . . . ? C3 C22 C27 C28 43.0(6) . . . . ? C23 C22 C27 C28 -148.3(5) . . . . ? C3 C22 C27 C31 -131.0(5) . . . . ? C23 C22 C27 C31 37.7(7) . . . . ? C3 C22 C27 Fe1 132.4(4) . . . . ? C23 C22 C27 Fe1 -59.0(6) . . . . ? C31 C27 C28 C29 2.4(5) . . . . ? C22 C27 C28 C29 -172.8(4) . . . . ? Fe1 C27 C28 C29 59.7(3) . . . . ? C31 C27 C28 Fe1 -57.3(3) . . . . ? C22 C27 C28 Fe1 127.5(4) . . . . ? C27 C28 C29 C30 -1.5(6) . . . . ? Fe1 C28 C29 C30 60.5(4) . . . . ? C27 C28 C29 Fe1 -62.0(3) . . . . ? C28 C29 C30 C31 0.1(6) . . . . ? Fe1 C29 C30 C31 60.4(3) . . . . ? C28 C29 C30 Fe1 -60.3(3) . . . . ? C28 C27 C31 C30 -2.3(5) . . . . ? C22 C27 C31 C30 172.6(4) . . . . ? Fe1 C27 C31 C30 -58.7(3) . . . . ? C28 C27 C31 Fe1 56.4(3) . . . . ? C22 C27 C31 Fe1 -128.8(5) . . . . ? C29 C30 C31 C27 1.4(5) . . . . ? Fe1 C30 C31 C27 60.5(3) . . . . ? C29 C30 C31 Fe1 -59.1(3) . . . . ? C36 C32 C33 C34 -0.7(7) . . . . ? Fe1 C32 C33 C34 58.9(4) . . . . ? C36 C32 C33 Fe1 -59.6(4) . . . . ? C32 C33 C34 C35 0.8(7) . . . . ? Fe1 C33 C34 C35 60.1(4) . . . . ? C32 C33 C34 Fe1 -59.3(4) . . . . ? C33 C34 C35 C36 -0.7(7) . . . . ? Fe1 C34 C35 C36 59.5(4) . . . . ? C33 C34 C35 Fe1 -60.2(4) . . . . ? C34 C35 C36 C32 0.3(7) . . . . ? Fe1 C35 C36 C32 59.8(4) . . . . ? C34 C35 C36 Fe1 -59.5(4) . . . . ? C33 C32 C36 C35 0.2(7) . . . . ? Fe1 C32 C36 C35 -59.8(4) . . . . ? C33 C32 C36 Fe1 60.0(4) . . . . ? C30 C29 Fe1 C28 -118.3(4) . . . . ? C30 C29 Fe1 C32 160.3(3) . . . . ? C28 C29 Fe1 C32 -81.4(4) . . . . ? C28 C29 Fe1 C30 118.3(4) . . . . ? C30 C29 Fe1 C36 119.9(3) . . . . ? C28 C29 Fe1 C36 -121.8(3) . . . . ? C30 C29 Fe1 C33 -174.8(6) . . . . ? C28 C29 Fe1 C33 -56.5(8) . . . . ? C30 C29 Fe1 C34 51.2(7) . . . . ? C28 C29 Fe1 C34 169.5(5) . . . . ? C30 C29 Fe1 C35 79.1(4) . . . . ? C28 C29 Fe1 C35 -162.6(3) . . . . ? C30 C29 Fe1 C31 -37.7(3) . . . . ? C28 C29 Fe1 C31 80.7(3) . . . . ? C30 C29 Fe1 C27 -80.9(3) . . . . ? C28 C29 Fe1 C27 37.4(3) . . . . ? C27 C28 Fe1 C29 119.2(4) . . . . ? C27 C28 Fe1 C32 -122.7(3) . . . . ? C29 C28 Fe1 C32 118.1(3) . . . . ? C27 C28 Fe1 C30 81.0(3) . . . . ? C29 C28 Fe1 C30 -38.2(3) . . . . ? C27 C28 Fe1 C36 -165.5(3) . . . . ? C29 C28 Fe1 C36 75.3(4) . . . . ? C27 C28 Fe1 C33 -81.8(3) . . . . ? C29 C28 Fe1 C33 159.0(3) . . . . ? C27 C28 Fe1 C34 -47.1(8) . . . . ? C29 C28 Fe1 C34 -166.3(6) . . . . ? C27 C28 Fe1 C35 159.9(5) . . . . ? C29 C28 Fe1 C35 40.7(6) . . . . ? C27 C28 Fe1 C31 37.2(2) . . . . ? C29 C28 Fe1 C31 -82.0(3) . . . . ? C29 C28 Fe1 C27 -119.2(4) . . . . ? C33 C32 Fe1 C29 166.6(3) . . . . ? C36 C32 Fe1 C29 -74.2(4) . . . . ? C33 C32 Fe1 C28 123.4(4) . . . . ? C36 C32 Fe1 C28 -117.4(4) . . . . ? C33 C32 Fe1 C30 -158.0(5) . . . . ? C36 C32 Fe1 C30 -38.8(8) . . . . ? C33 C32 Fe1 C36 -119.2(5) . . . . ? C36 C32 Fe1 C33 119.2(5) . . . . ? C33 C32 Fe1 C34 -37.6(4) . . . . ? C36 C32 Fe1 C34 81.6(4) . . . . ? C33 C32 Fe1 C35 -81.3(4) . . . . ? C36 C32 Fe1 C35 37.9(4) . . . . ? C33 C32 Fe1 C31 47.3(8) . . . . ? C36 C32 Fe1 C31 166.5(5) . . . . ? C33 C32 Fe1 C27 81.7(4) . . . . ? C36 C32 Fe1 C27 -159.1(3) . . . . ? C31 C30 Fe1 C29 -119.0(4) . . . . ? C29 C30 Fe1 C28 38.4(3) . . . . ? C31 C30 Fe1 C28 -80.7(3) . . . . ? C29 C30 Fe1 C32 -48.5(7) . . . . ? C31 C30 Fe1 C32 -167.5(5) . . . . ? C29 C30 Fe1 C36 -76.7(4) . . . . ? C31 C30 Fe1 C36 164.2(3) . . . . ? C29 C30 Fe1 C33 174.8(6) . . . . ? C31 C30 Fe1 C33 55.7(7) . . . . ? C29 C30 Fe1 C34 -158.3(3) . . . . ? C31 C30 Fe1 C34 82.6(4) . . . . ? C29 C30 Fe1 C35 -117.8(3) . . . . ? C31 C30 Fe1 C35 123.2(3) . . . . ? C29 C30 Fe1 C31 119.0(4) . . . . ? C29 C30 Fe1 C27 81.9(3) . . . . ? C31 C30 Fe1 C27 -37.1(2) . . . . ? C35 C36 Fe1 C29 -118.7(4) . . . . ? C32 C36 Fe1 C29 122.8(4) . . . . ? C35 C36 Fe1 C28 -159.6(4) . . . . ? C32 C36 Fe1 C28 81.8(4) . . . . ? C35 C36 Fe1 C32 118.6(5) . . . . ? C35 C36 Fe1 C30 -77.5(4) . . . . ? C32 C36 Fe1 C30 163.9(3) . . . . ? C35 C36 Fe1 C33 81.5(4) . . . . ? C32 C36 Fe1 C33 -37.1(3) . . . . ? C35 C36 Fe1 C34 37.5(4) . . . . ? C32 C36 Fe1 C34 -81.1(4) . . . . ? C32 C36 Fe1 C35 -118.6(5) . . . . ? C35 C36 Fe1 C31 -49.8(7) . . . . ? C32 C36 Fe1 C31 -168.4(5) . . . . ? C35 C36 Fe1 C27 173.4(5) . . . . ? C32 C36 Fe1 C27 54.8(7) . . . . ? C32 C33 Fe1 C29 -33.9(8) . . . . ? C34 C33 Fe1 C29 -153.6(6) . . . . ? C32 C33 Fe1 C28 -76.1(4) . . . . ? C34 C33 Fe1 C28 164.2(3) . . . . ? C34 C33 Fe1 C32 -119.7(5) . . . . ? C32 C33 Fe1 C30 155.9(6) . . . . ? C34 C33 Fe1 C30 36.1(8) . . . . ? C32 C33 Fe1 C36 37.9(4) . . . . ? C34 C33 Fe1 C36 -81.8(4) . . . . ? C32 C33 Fe1 C34 119.7(5) . . . . ? C32 C33 Fe1 C35 81.7(4) . . . . ? C34 C33 Fe1 C35 -38.0(3) . . . . ? C32 C33 Fe1 C31 -162.7(3) . . . . ? C34 C33 Fe1 C31 77.6(4) . . . . ? C32 C33 Fe1 C27 -119.6(4) . . . . ? C34 C33 Fe1 C27 120.7(4) . . . . ? C33 C34 Fe1 C29 157.2(5) . . . . ? C35 C34 Fe1 C29 38.9(7) . . . . ? C33 C34 Fe1 C28 -45.5(8) . . . . ? C35 C34 Fe1 C28 -163.8(6) . . . . ? C33 C34 Fe1 C32 36.8(3) . . . . ? C35 C34 Fe1 C32 -81.5(4) . . . . ? C33 C34 Fe1 C30 -166.0(3) . . . . ? C35 C34 Fe1 C30 75.7(4) . . . . ? C33 C34 Fe1 C36 80.8(4) . . . . ? C35 C34 Fe1 C36 -37.6(3) . . . . ? C35 C34 Fe1 C33 -118.3(5) . . . . ? C33 C34 Fe1 C35 118.3(5) . . . . ? C33 C34 Fe1 C31 -122.9(4) . . . . ? C35 C34 Fe1 C31 118.7(4) . . . . ? C33 C34 Fe1 C27 -81.3(4) . . . . ? C35 C34 Fe1 C27 160.3(3) . . . . ? C36 C35 Fe1 C29 77.6(4) . . . . ? C34 C35 Fe1 C29 -163.1(3) . . . . ? C36 C35 Fe1 C28 48.1(7) . . . . ? C34 C35 Fe1 C28 167.4(5) . . . . ? C36 C35 Fe1 C32 -38.1(4) . . . . ? C34 C35 Fe1 C32 81.2(4) . . . . ? C36 C35 Fe1 C30 119.3(4) . . . . ? C34 C35 Fe1 C30 -121.4(4) . . . . ? C34 C35 Fe1 C36 119.3(5) . . . . ? C36 C35 Fe1 C33 -81.1(4) . . . . ? C34 C35 Fe1 C33 38.2(3) . . . . ? C36 C35 Fe1 C34 -119.3(5) . . . . ? C36 C35 Fe1 C31 159.7(3) . . . . ? C34 C35 Fe1 C31 -81.0(4) . . . . ? C36 C35 Fe1 C27 -173.0(5) . . . . ? C34 C35 Fe1 C27 -53.7(8) . . . . ? C27 C31 Fe1 C29 -81.7(3) . . . . ? C30 C31 Fe1 C29 37.9(3) . . . . ? C27 C31 Fe1 C28 -37.4(3) . . . . ? C30 C31 Fe1 C28 82.3(3) . . . . ? C27 C31 Fe1 C32 45.8(7) . . . . ? C30 C31 Fe1 C32 165.5(6) . . . . ? C27 C31 Fe1 C30 -119.6(4) . . . . ? C27 C31 Fe1 C36 -157.7(5) . . . . ? C30 C31 Fe1 C36 -38.0(7) . . . . ? C27 C31 Fe1 C33 81.2(3) . . . . ? C30 C31 Fe1 C33 -159.2(3) . . . . ? C27 C31 Fe1 C34 123.5(3) . . . . ? C30 C31 Fe1 C34 -116.9(3) . . . . ? C27 C31 Fe1 C35 166.1(3) . . . . ? C30 C31 Fe1 C35 -74.2(4) . . . . ? C30 C31 Fe1 C27 119.6(4) . . . . ? C28 C27 Fe1 C29 -38.0(3) . . . . ? C31 C27 Fe1 C29 81.6(3) . . . . ? C22 C27 Fe1 C29 -154.1(5) . . . . ? C31 C27 Fe1 C28 119.6(4) . . . . ? C22 C27 Fe1 C28 -116.1(5) . . . . ? C28 C27 Fe1 C32 77.1(3) . . . . ? C31 C27 Fe1 C32 -163.3(3) . . . . ? C22 C27 Fe1 C32 -39.0(5) . . . . ? C28 C27 Fe1 C30 -82.1(3) . . . . ? C31 C27 Fe1 C30 37.5(3) . . . . ? C22 C27 Fe1 C30 161.8(5) . . . . ? C28 C27 Fe1 C36 36.5(7) . . . . ? C31 C27 Fe1 C36 156.1(6) . . . . ? C22 C27 Fe1 C36 -79.6(7) . . . . ? C28 C27 Fe1 C33 119.9(3) . . . . ? C31 C27 Fe1 C33 -120.5(3) . . . . ? C22 C27 Fe1 C33 3.8(5) . . . . ? C28 C27 Fe1 C34 163.6(3) . . . . ? C31 C27 Fe1 C34 -76.7(4) . . . . ? C22 C27 Fe1 C34 47.5(5) . . . . ? C28 C27 Fe1 C35 -156.2(6) . . . . ? C31 C27 Fe1 C35 -36.6(8) . . . . ? C22 C27 Fe1 C35 87.7(8) . . . . ? C28 C27 Fe1 C31 -119.6(4) . . . . ? C22 C27 Fe1 C31 124.3(5) . . . . ? N2 C3 N1 C1 0.8(5) . . . . ? C22 C3 N1 C1 178.7(5) . . . . ? N2 C3 N1 C4 -174.9(4) . . . . ? C22 C3 N1 C4 2.9(8) . . . . ? C2 C1 N1 C3 -0.8(6) . . . . ? C2 C1 N1 C4 175.2(5) . . . . ? C5 C4 N1 C3 70.6(6) . . . . ? C9 C4 N1 C3 -113.4(5) . . . . ? C5 C4 N1 C1 -104.6(5) . . . . ? C9 C4 N1 C1 71.5(6) . . . . ? N1 C3 N2 C2 -0.5(5) . . . . ? C22 C3 N2 C2 -178.4(4) . . . . ? N1 C3 N2 C13 -167.4(4) . . . . ? C22 C3 N2 C13 14.7(7) . . . . ? C1 C2 N2 C3 0.1(6) . . . . ? C1 C2 N2 C13 167.0(5) . . . . ? C14 C13 N2 C3 62.7(6) . . . . ? C18 C13 N2 C3 -120.2(5) . . . . ? C14 C13 N2 C2 -102.3(6) . . . . ? C18 C13 N2 C2 74.8(6) . . . . ? C26 C25 O2 C24 -174.6(5) . . . . ? C23 C24 O2 C25 -72.8(6) . . . . ? C37 O3 C37 C38 -68(11) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.827 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.063