# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 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_cl003 # start Validation Reply Form _vrf_RINTA01_cl003 ; PROBLEM: The value of Rint is greater than 0.18 RESPONSE: Overall quality of the data is poor due to the crystal quality. ; _vrf_PLAT020_cl003 ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.185 RESPONSE: Overall quality of the data is poor due to the crystal quality. ; _vrf_PLAT230_cl003 ; PROBLEM: Hirshfeld Test Diff for C33 -- C34 .. 8.1 su RESPONSE: Disorder of alkyl chain that could not be solved. ; _vrf_PLAT420_cl003 ; PROBLEM: D-H Without Acceptor O99 - H99 ... Please Check RESPONSE: No other possibility found. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Fe12i(C8)(dmap)2]' _chemical_melting_point ? _chemical_formula_moiety 'C48 H70 Fe N6 O8, (C H4 O), 0.5(C H4 O)' _chemical_formula_sum 'C49.50 H76 Fe N6 O9.50' _chemical_formula_weight 963.01 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 10.599(5) _cell_length_b 31.295(5) _cell_length_c 15.997(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.404(5) _cell_angle_gamma 90.00 _cell_volume 5201(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 56290 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 24.6 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068 _exptl_absorpt_coefficient_mu 0.349 _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 133(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDSII _diffrn_measurement_method Omega-Scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56290 _diffrn_reflns_av_R_equivalents 0.1851 _diffrn_reflns_av_sigmaI/netI 0.1371 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 24.64 _reflns_number_total 8715 _reflns_number_gt 4166 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-AREA-STOE _computing_cell_refinement X-AREA-STOE _computing_data_reduction X-AREA-STOE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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^)+(0.1368P)^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 8715 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1626 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2514 _refine_ls_wR_factor_gt 0.2167 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _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 C1 C 1.2383(6) 0.2265(2) 0.4289(4) 0.0467(16) Uani 1 1 d . . . C2 C 1.2665(6) 0.2497(2) 0.3572(4) 0.0420(15) Uani 1 1 d . . . C3 C 1.1794(6) 0.2790(2) 0.3103(4) 0.0449(16) Uani 1 1 d . . . H3 H 1.2069 0.2934 0.2647 0.054 Uiso 1 1 calc R . . C4 C 0.9828(5) 0.31704(19) 0.2674(4) 0.0379(14) Uani 1 1 d . . . C5 C 1.0116(6) 0.3351(2) 0.1922(4) 0.0440(16) Uani 1 1 d . . . H5 H 1.0913 0.3290 0.1762 0.053 Uiso 1 1 calc R . . C6 C 0.9230(6) 0.3616(2) 0.1423(4) 0.0437(16) Uani 1 1 d . . . C7 C 0.8040(6) 0.3694(2) 0.1643(4) 0.0459(16) Uani 1 1 d . . . C8 C 0.7761(6) 0.3522(2) 0.2388(4) 0.0435(16) Uani 1 1 d . . . H8 H 0.6960 0.3584 0.2543 0.052 Uiso 1 1 calc R . . C9 C 0.8644(6) 0.32619(19) 0.2906(4) 0.0398(15) Uani 1 1 d . . . C10 C 0.7459(6) 0.3142(2) 0.3997(4) 0.0452(16) Uani 1 1 d . . . H10 H 0.6868 0.3346 0.3704 0.054 Uiso 1 1 calc R . . C11 C 0.7162(6) 0.2953(2) 0.4747(4) 0.0445(16) Uani 1 1 d . . . C12 C 0.7922(6) 0.2629(2) 0.5224(4) 0.0446(16) Uani 1 1 d . . . C13 C 1.3350(6) 0.1979(2) 0.4830(5) 0.0535(18) Uani 1 1 d . . . H13A H 1.3053 0.1907 0.5355 0.080 Uiso 1 1 calc R . . H13B H 1.4180 0.2126 0.4973 0.080 Uiso 1 1 calc R . . H13C H 1.3448 0.1717 0.4515 0.080 Uiso 1 1 calc R . . C14 C 1.3869(6) 0.2431(2) 0.3292(5) 0.0477(17) Uani 1 1 d . . . C15 C 1.5086(6) 0.2626(3) 0.2246(5) 0.062(2) Uani 1 1 d . . . H15A H 1.5883 0.2646 0.2675 0.093 Uiso 1 1 calc R . . H15B H 1.5095 0.2842 0.1803 0.093 Uiso 1 1 calc R . . H15C H 1.5018 0.2341 0.1988 0.093 Uiso 1 1 calc R . . C16 C 0.7589(6) 0.2433(2) 0.6016(4) 0.0490(17) Uani 1 1 d . . . H16A H 0.8240 0.2219 0.6249 0.073 Uiso 1 1 calc R . . H16B H 0.6743 0.2296 0.5870 0.073 Uiso 1 1 calc R . . H16C H 0.7568 0.2657 0.6441 0.073 Uiso 1 1 calc R . . C17 C 0.5972(6) 0.3093(2) 0.4998(5) 0.0533(18) Uani 1 1 d . . . C18 C 0.4058(7) 0.3508(3) 0.4605(6) 0.068(2) Uani 1 1 d . . . H18A H 0.3518 0.3253 0.4594 0.103 Uiso 1 1 calc R . . H18B H 0.3647 0.3708 0.4163 0.103 Uiso 1 1 calc R . . H18C H 0.4164 0.3645 0.5165 0.103 Uiso 1 1 calc R . . C19 C 1.0315(6) 0.3598(2) 0.0247(5) 0.0503(17) Uani 1 1 d . . . H19A H 1.0090 0.3292 0.0158 0.060 Uiso 1 1 calc R . . H19B H 1.1203 0.3619 0.0583 0.060 Uiso 1 1 calc R . . C20 C 1.0215(7) 0.3821(2) -0.0600(4) 0.0530(18) Uani 1 1 d . . . H20A H 0.9299 0.3827 -0.0892 0.064 Uiso 1 1 calc R . . H20B H 1.0693 0.3652 -0.0959 0.064 Uiso 1 1 calc R . . C21 C 1.0728(8) 0.4273(2) -0.0534(5) 0.065(2) Uani 1 1 d . . . H21A H 1.1677 0.4265 -0.0356 0.077 Uiso 1 1 calc R . . H21B H 1.0379 0.4428 -0.0091 0.077 Uiso 1 1 calc R . . C22 C 1.0356(9) 0.4522(3) -0.1408(5) 0.075(2) Uani 1 1 d . . . H22A H 1.0598 0.4348 -0.1869 0.090 Uiso 1 1 calc R . . H22B H 0.9413 0.4566 -0.1547 0.090 Uiso 1 1 calc R . . C23 C 1.1018(9) 0.4942(3) -0.1364(6) 0.082(3) Uani 1 1 d . . . H23A H 1.1960 0.4895 -0.1252 0.099 Uiso 1 1 calc R . . H23B H 1.0813 0.5108 -0.0880 0.099 Uiso 1 1 calc R . . C24 C 1.0628(9) 0.5202(3) -0.2180(6) 0.078(2) Uani 1 1 d . . . H24A H 1.1244 0.5442 -0.2157 0.094 Uiso 1 1 calc R . . H24B H 1.0731 0.5018 -0.2665 0.094 Uiso 1 1 calc R . . C25 C 0.9310(9) 0.5382(3) -0.2366(6) 0.082(3) Uani 1 1 d . . . H25A H 0.9163 0.5543 -0.1861 0.098 Uiso 1 1 calc R . . H25B H 0.8683 0.5144 -0.2465 0.098 Uiso 1 1 calc R . . C26 C 0.9058(8) 0.5677(3) -0.3136(5) 0.072(2) Uani 1 1 d . . . H26A H 0.9679 0.5912 -0.3047 0.108 Uiso 1 1 calc R . . H26B H 0.8183 0.5792 -0.3211 0.108 Uiso 1 1 calc R . . H26C H 0.9149 0.5516 -0.3646 0.108 Uiso 1 1 calc R . . C27 C 0.6531(7) 0.3728(2) 0.0342(5) 0.0570(19) Uani 1 1 d . . . H27A H 0.6011 0.3482 0.0471 0.068 Uiso 1 1 calc R . . H27B H 0.7203 0.3619 0.0046 0.068 Uiso 1 1 calc R . . C28 C 0.5680(7) 0.4048(2) -0.0217(5) 0.0572(19) Uani 1 1 d . . . H28A H 0.5019 0.4151 0.0094 0.069 Uiso 1 1 calc R . . H28B H 0.5226 0.3899 -0.0736 0.069 Uiso 1 1 calc R . . C29 C 0.6377(7) 0.4431(2) -0.0487(5) 0.0574(19) Uani 1 1 d . . . H29A H 0.7048 0.4330 -0.0792 0.069 Uiso 1 1 calc R . . H29B H 0.6813 0.4587 0.0028 0.069 Uiso 1 1 calc R . . C30 C 0.5476(8) 0.4739(2) -0.1065(5) 0.064(2) Uani 1 1 d . . . H30A H 0.5048 0.4580 -0.1579 0.076 Uiso 1 1 calc R . . H30B H 0.4798 0.4832 -0.0760 0.076 Uiso 1 1 calc R . . C31 C 0.6110(9) 0.5132(3) -0.1348(7) 0.091(3) Uani 1 1 d . . . H31A H 0.6823 0.5042 -0.1626 0.109 Uiso 1 1 calc R . . H31B H 0.6484 0.5304 -0.0841 0.109 Uiso 1 1 calc R . . C32 C 0.5153(11) 0.5412(3) -0.1977(7) 0.106(4) Uani 1 1 d . . . H32A H 0.4719 0.5225 -0.2447 0.127 Uiso 1 1 calc R . . H32B H 0.4484 0.5515 -0.1673 0.127 Uiso 1 1 calc R . . C33 C 0.5669(11) 0.5789(4) -0.2366(9) 0.117(4) Uani 1 1 d . . . H33A H 0.6326 0.5688 -0.2682 0.141 Uiso 1 1 calc R . . H33B H 0.4959 0.5918 -0.2785 0.141 Uiso 1 1 calc R . . C34 C 0.6226(11) 0.6110(4) -0.1786(9) 0.139(6) Uani 1 1 d . . . H34A H 0.5630 0.6185 -0.1413 0.208 Uiso 1 1 calc R . . H34B H 0.6403 0.6363 -0.2103 0.208 Uiso 1 1 calc R . . H34C H 0.7032 0.6003 -0.1439 0.208 Uiso 1 1 calc R . . C35 C 0.7793(6) 0.2044(2) 0.3376(5) 0.0503(17) Uani 1 1 d . . . H35 H 0.7329 0.2183 0.3749 0.060 Uiso 1 1 calc R . . C36 C 0.7198(6) 0.1707(2) 0.2900(5) 0.0533(18) Uani 1 1 d . . . H36 H 0.6359 0.1621 0.2954 0.064 Uiso 1 1 calc R . . C37 C 0.7836(7) 0.1491(2) 0.2331(5) 0.0549(18) Uani 1 1 d . . . C38 C 0.9061(7) 0.1650(2) 0.2285(5) 0.0535(18) Uani 1 1 d . . . H38 H 0.9532 0.1525 0.1899 0.064 Uiso 1 1 calc R . . C39 C 0.9577(6) 0.1982(2) 0.2791(4) 0.0475(17) Uani 1 1 d . . . H39 H 1.0415 0.2074 0.2747 0.057 Uiso 1 1 calc R . . C40 C 0.6009(8) 0.1016(3) 0.1877(6) 0.081(3) Uani 1 1 d . . . H40A H 0.5966 0.0930 0.2459 0.122 Uiso 1 1 calc R . . H40B H 0.5782 0.0772 0.1491 0.122 Uiso 1 1 calc R . . H40C H 0.5404 0.1251 0.1697 0.122 Uiso 1 1 calc R . . C41 C 0.7980(9) 0.0955(3) 0.1247(6) 0.080(3) Uani 1 1 d . . . H41A H 0.8098 0.1162 0.0810 0.119 Uiso 1 1 calc R . . H41B H 0.7469 0.0713 0.0977 0.119 Uiso 1 1 calc R . . H41C H 0.8822 0.0852 0.1547 0.119 Uiso 1 1 calc R . . C42 C 1.1314(6) 0.2959(2) 0.5784(5) 0.0457(16) Uani 1 1 d . . . H42 H 1.1282 0.2662 0.5903 0.055 Uiso 1 1 calc R . . C43 C 1.1920(6) 0.3218(2) 0.6421(5) 0.0470(16) Uani 1 1 d . . . H43 H 1.2315 0.3100 0.6956 0.056 Uiso 1 1 calc R . . C44 C 1.1959(6) 0.3662(2) 0.6286(5) 0.0475(17) Uani 1 1 d . . . C45 C 1.1384(6) 0.3804(2) 0.5465(5) 0.0483(17) Uani 1 1 d . . . H45 H 1.1391 0.4099 0.5330 0.058 Uiso 1 1 calc R . . C46 C 1.0810(6) 0.3516(2) 0.4859(5) 0.0450(16) Uani 1 1 d . . . H46 H 1.0431 0.3623 0.4311 0.054 Uiso 1 1 calc R . . C47 C 1.2997(7) 0.3778(2) 0.7780(5) 0.062(2) Uani 1 1 d . . . H47A H 1.2342 0.3598 0.7959 0.092 Uiso 1 1 calc R . . H47B H 1.3202 0.4019 0.8174 0.092 Uiso 1 1 calc R . . H47C H 1.3776 0.3609 0.7783 0.092 Uiso 1 1 calc R . . C48 C 1.2606(8) 0.4385(2) 0.6753(5) 0.065(2) Uani 1 1 d . . . H48A H 1.3053 0.4425 0.6278 0.098 Uiso 1 1 calc R . . H48B H 1.3090 0.4528 0.7262 0.098 Uiso 1 1 calc R . . H48C H 1.1741 0.4509 0.6604 0.098 Uiso 1 1 calc R . . Fe1 Fe 0.98410(8) 0.26657(3) 0.41245(6) 0.0422(3) Uani 1 1 d . . . N1 N 1.0639(4) 0.28852(16) 0.3232(3) 0.0393(12) Uani 1 1 d . . . N2 N 0.8486(5) 0.30566(16) 0.3677(3) 0.0414(13) Uani 1 1 d . . . N3 N 0.8983(5) 0.21918(17) 0.3356(4) 0.0484(14) Uani 1 1 d . . . N4 N 0.7315(6) 0.1157(2) 0.1851(4) 0.0634(17) Uani 1 1 d . . . N5 N 1.0751(5) 0.30943(16) 0.4989(4) 0.0442(13) Uani 1 1 d . . . N6 N 1.2508(6) 0.39385(18) 0.6923(4) 0.0579(16) Uani 1 1 d . . . O1 O 1.1302(4) 0.22854(13) 0.4525(3) 0.0450(11) Uani 1 1 d . . . O2 O 0.8951(4) 0.24807(13) 0.5028(3) 0.0474(11) Uani 1 1 d . . . O3 O 1.4692(4) 0.21610(16) 0.3540(3) 0.0607(13) Uani 1 1 d . . . O4 O 1.4002(4) 0.26999(16) 0.2644(3) 0.0574(12) Uani 1 1 d . . . O5 O 0.5519(5) 0.2977(2) 0.5592(4) 0.0811(18) Uani 1 1 d . . . O6 O 0.5307(5) 0.33858(17) 0.4446(3) 0.0649(14) Uani 1 1 d . . . O7 O 0.9428(4) 0.38063(14) 0.0684(3) 0.0495(11) Uani 1 1 d . . . O8 O 0.7119(4) 0.39437(14) 0.1122(3) 0.0496(12) Uani 1 1 d . . . C98 C 0.4626(13) 0.0268(4) 0.9608(10) 0.056(4) Uiso 0.50 1 d P A -1 H98A H 0.4515 0.0507 0.9982 0.083 Uiso 0.50 1 calc PR A -1 H98B H 0.3905 0.0068 0.9575 0.083 Uiso 0.50 1 calc PR A -1 H98C H 0.4650 0.0376 0.9037 0.083 Uiso 0.50 1 calc PR A -1 O98 O 0.6046(14) 0.0008(5) 1.0013(9) 0.110(4) Uiso 0.50 1 d P A -1 H98 H 0.6648 0.0121 0.9821 0.164 Uiso 0.50 1 calc PR A -1 C99 C 0.7782(10) 0.0677(3) 0.8983(7) 0.094(3) Uiso 1 1 d . . . H99A H 0.7110 0.0853 0.9152 0.140 Uiso 1 1 calc R . . H99B H 0.7501 0.0586 0.8389 0.140 Uiso 1 1 calc R . . H99C H 0.8575 0.0845 0.9037 0.140 Uiso 1 1 calc R . . O99 O 0.8032(9) 0.0287(3) 0.9556(6) 0.142(3) Uiso 1 1 d . . . H99 H 0.8821 0.0270 0.9768 0.213 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 0.042(4) 0.047(4) 0.051(4) -0.004(3) 0.009(3) -0.004(3) C2 0.033(3) 0.046(3) 0.048(4) 0.001(3) 0.009(3) 0.003(3) C3 0.045(4) 0.046(4) 0.046(4) -0.004(3) 0.015(3) -0.002(3) C4 0.031(3) 0.044(3) 0.040(4) 0.000(3) 0.008(3) 0.007(3) C5 0.036(3) 0.054(4) 0.046(4) -0.002(3) 0.017(3) 0.006(3) C6 0.044(4) 0.047(4) 0.042(4) 0.002(3) 0.014(3) 0.000(3) C7 0.037(3) 0.054(4) 0.047(4) 0.005(3) 0.010(3) 0.009(3) C8 0.034(3) 0.050(4) 0.047(4) -0.006(3) 0.009(3) 0.003(3) C9 0.037(3) 0.043(3) 0.039(4) -0.001(3) 0.007(3) -0.002(3) C10 0.041(4) 0.049(4) 0.045(4) 0.002(3) 0.006(3) 0.004(3) C11 0.041(4) 0.050(4) 0.047(4) 0.002(3) 0.020(3) 0.004(3) C12 0.041(4) 0.053(4) 0.043(4) 0.003(3) 0.015(3) -0.003(3) C13 0.050(4) 0.056(4) 0.056(5) 0.005(4) 0.014(4) 0.007(3) C14 0.044(4) 0.048(4) 0.051(4) -0.003(3) 0.010(3) -0.009(3) C15 0.043(4) 0.086(5) 0.064(5) 0.003(4) 0.030(4) 0.011(4) C16 0.048(4) 0.051(4) 0.049(4) 0.005(3) 0.014(3) 0.001(3) C17 0.042(4) 0.063(5) 0.055(5) 0.001(4) 0.012(4) 0.000(3) C18 0.049(4) 0.082(5) 0.080(6) 0.005(5) 0.028(4) 0.017(4) C19 0.050(4) 0.050(4) 0.056(5) -0.007(3) 0.020(4) 0.001(3) C20 0.062(4) 0.058(4) 0.043(4) 0.000(3) 0.021(3) 0.002(3) C21 0.086(6) 0.062(5) 0.052(5) 0.006(4) 0.028(4) -0.005(4) C22 0.090(6) 0.081(6) 0.060(6) 0.013(5) 0.029(5) -0.003(5) C23 0.093(7) 0.076(6) 0.084(7) 0.002(5) 0.033(5) -0.010(5) C24 0.100(7) 0.059(5) 0.078(6) 0.015(5) 0.026(5) 0.007(5) C25 0.088(6) 0.069(5) 0.098(7) 0.011(5) 0.043(6) 0.010(5) C26 0.077(6) 0.070(5) 0.073(6) 0.014(4) 0.023(5) -0.002(4) C27 0.050(4) 0.069(5) 0.049(5) -0.001(4) 0.001(4) -0.006(4) C28 0.053(4) 0.061(4) 0.055(5) 0.004(4) 0.007(4) -0.006(3) C29 0.052(4) 0.060(4) 0.059(5) 0.005(4) 0.009(4) -0.006(3) C30 0.076(5) 0.055(4) 0.064(5) 0.009(4) 0.023(4) -0.001(4) C31 0.092(7) 0.068(5) 0.126(9) 0.018(6) 0.056(6) 0.005(5) C32 0.156(10) 0.054(5) 0.129(9) 0.041(6) 0.080(8) 0.033(6) C33 0.098(8) 0.120(9) 0.145(11) 0.029(9) 0.052(8) 0.022(7) C34 0.106(8) 0.160(11) 0.169(12) -0.095(10) 0.072(8) -0.087(8) C35 0.042(4) 0.062(4) 0.048(4) -0.004(4) 0.012(3) 0.004(3) C36 0.039(4) 0.065(5) 0.059(5) 0.002(4) 0.015(4) -0.003(3) C37 0.050(4) 0.060(4) 0.056(5) -0.004(4) 0.012(4) -0.006(3) C38 0.052(4) 0.051(4) 0.060(5) -0.003(4) 0.020(4) -0.001(3) C39 0.034(3) 0.059(4) 0.052(4) -0.002(4) 0.015(3) -0.002(3) C40 0.066(5) 0.101(7) 0.077(6) -0.019(5) 0.012(5) -0.025(5) C41 0.081(6) 0.082(6) 0.077(6) -0.024(5) 0.022(5) -0.013(5) C42 0.043(4) 0.049(4) 0.050(5) 0.003(4) 0.019(3) 0.001(3) C43 0.044(4) 0.054(4) 0.044(4) 0.006(3) 0.012(3) -0.002(3) C44 0.044(4) 0.048(4) 0.051(5) -0.004(3) 0.009(3) -0.005(3) C45 0.044(4) 0.041(4) 0.061(5) 0.003(4) 0.012(4) -0.001(3) C46 0.041(4) 0.045(4) 0.050(4) 0.006(3) 0.011(3) 0.003(3) C47 0.065(5) 0.069(5) 0.047(5) 0.000(4) 0.002(4) -0.010(4) C48 0.078(5) 0.051(4) 0.063(5) -0.010(4) 0.005(4) -0.004(4) Fe1 0.0358(5) 0.0485(5) 0.0442(6) -0.0003(5) 0.0127(4) 0.0012(4) N1 0.031(3) 0.047(3) 0.040(3) -0.002(3) 0.006(2) -0.001(2) N2 0.036(3) 0.045(3) 0.047(3) 0.002(3) 0.016(3) -0.001(2) N3 0.039(3) 0.056(3) 0.051(4) 0.002(3) 0.012(3) 0.004(2) N4 0.053(4) 0.066(4) 0.073(5) -0.017(4) 0.019(3) -0.011(3) N5 0.041(3) 0.045(3) 0.051(4) 0.005(3) 0.020(3) 0.005(2) N6 0.065(4) 0.054(4) 0.052(4) 0.001(3) 0.008(3) -0.012(3) O1 0.041(2) 0.044(2) 0.051(3) 0.004(2) 0.012(2) -0.001(2) O2 0.046(3) 0.050(3) 0.048(3) -0.001(2) 0.013(2) -0.004(2) O3 0.046(3) 0.067(3) 0.072(4) 0.011(3) 0.020(3) 0.018(2) O4 0.044(3) 0.072(3) 0.061(3) 0.010(3) 0.023(2) 0.009(2) O5 0.069(4) 0.108(5) 0.078(4) 0.034(3) 0.044(3) 0.023(3) O6 0.048(3) 0.086(4) 0.067(4) 0.016(3) 0.026(3) 0.017(3) O7 0.048(3) 0.053(3) 0.052(3) 0.005(2) 0.022(2) 0.007(2) O8 0.044(3) 0.059(3) 0.048(3) 0.006(2) 0.013(2) 0.007(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 O1 1.278(7) . ? C1 C2 1.437(9) . ? C1 C13 1.499(9) . ? C2 C3 1.409(9) . ? C2 C14 1.448(9) . ? C3 N1 1.314(8) . ? C3 H3 0.9500 . ? C4 C9 1.407(8) . ? C4 C5 1.415(9) . ? C4 N1 1.425(8) . ? C5 C6 1.382(9) . ? C5 H5 0.9500 . ? C6 O7 1.377(7) . ? C6 C7 1.397(9) . ? C7 C8 1.392(9) . ? C7 O8 1.392(8) . ? C8 C9 1.385(9) . ? C8 H8 0.9500 . ? C9 N2 1.429(8) . ? C10 N2 1.319(8) . ? C10 C11 1.427(9) . ? C10 H10 0.9500 . ? C11 C12 1.420(9) . ? C11 C17 1.465(9) . ? C12 O2 1.279(7) . ? C12 C16 1.511(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 O3 1.223(8) . ? C14 O4 1.364(8) . ? C15 O4 1.439(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O5 1.202(8) . ? C17 O6 1.367(8) . ? C18 O6 1.448(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O7 1.435(7) . ? C19 C20 1.509(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.512(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.581(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.486(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.524(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.481(12) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.519(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O8 1.447(8) . ? C27 C28 1.515(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.517(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.531(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.514(10) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.551(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.486(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.416(15) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N3 1.350(8) . ? C35 C36 1.377(9) . ? C35 H35 0.9500 . ? C36 C37 1.411(10) . ? C36 H36 0.9500 . ? C37 N4 1.347(9) . ? C37 C38 1.406(9) . ? C38 C39 1.363(9) . ? C38 H38 0.9500 . ? C39 N3 1.368(8) . ? C39 H39 0.9500 . ? C40 N4 1.462(9) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 N4 1.449(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.360(9) . ? C42 N5 1.362(8) . ? C42 H42 0.9500 . ? C43 C44 1.408(9) . ? C43 H43 0.9500 . ? C44 N6 1.375(9) . ? C44 C45 1.406(10) . ? C45 C46 1.374(9) . ? C45 H45 0.9500 . ? C46 N5 1.340(8) . ? C46 H46 0.9500 . ? C47 N6 1.456(9) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 N6 1.432(9) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? Fe1 N2 1.914(5) . ? Fe1 N1 1.925(5) . ? Fe1 O1 1.957(4) . ? Fe1 O2 1.963(4) . ? Fe1 N3 2.024(6) . ? Fe1 N5 2.029(6) . ? C98 O98 1.720(18) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? O98 H98 0.8400 . ? C99 O99 1.519(12) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? O99 H99 0.8400 . ? 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 C1 C2 123.4(6) . . ? O1 C1 C13 114.2(6) . . ? C2 C1 C13 122.4(6) . . ? C3 C2 C1 122.4(6) . . ? C3 C2 C14 116.9(6) . . ? C1 C2 C14 120.7(6) . . ? N1 C3 C2 126.6(6) . . ? N1 C3 H3 116.7 . . ? C2 C3 H3 116.7 . . ? C9 C4 C5 119.8(6) . . ? C9 C4 N1 114.9(5) . . ? C5 C4 N1 125.3(5) . . ? C6 C5 C4 119.7(5) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? O7 C6 C5 123.7(5) . . ? O7 C6 C7 116.0(6) . . ? C5 C6 C7 120.2(6) . . ? C8 C7 O8 119.2(5) . . ? C8 C7 C6 120.2(6) . . ? O8 C7 C6 120.6(6) . . ? C9 C8 C7 120.5(6) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C4 119.6(6) . . ? C8 C9 N2 126.9(5) . . ? C4 C9 N2 113.5(5) . . ? N2 C10 C11 125.3(6) . . ? N2 C10 H10 117.3 . . ? C11 C10 H10 117.3 . . ? C12 C11 C10 123.5(6) . . ? C12 C11 C17 119.6(6) . . ? C10 C11 C17 116.8(6) . . ? O2 C12 C11 123.2(6) . . ? O2 C12 C16 114.2(6) . . ? C11 C12 C16 122.6(6) . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O3 C14 O4 119.9(6) . . ? O3 C14 C2 127.8(6) . . ? O4 C14 C2 112.2(6) . . ? O4 C15 H15A 109.5 . . ? O4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 O6 118.5(6) . . ? O5 C17 C11 128.8(7) . . ? O6 C17 C11 112.7(6) . . ? O6 C18 H18A 109.5 . . ? O6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O7 C19 C20 106.9(5) . . ? O7 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O7 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? C19 C20 C21 114.2(6) . . ? C19 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? C19 C20 H20B 108.7 . . ? C21 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 112.1(7) . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C21 111.2(7) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 112.7(8) . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C25 C24 C23 117.4(8) . . ? C25 C24 H24A 108.0 . . ? C23 C24 H24A 108.0 . . ? C25 C24 H24B 108.0 . . ? C23 C24 H24B 108.0 . . ? H24A C24 H24B 107.2 . . ? C24 C25 C26 113.7(7) . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? 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 . . ? O8 C27 C28 107.8(6) . . ? O8 C27 H27A 110.2 . . ? C28 C27 H27A 110.2 . . ? O8 C27 H27B 110.2 . . ? C28 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C27 C28 C29 115.1(6) . . ? C27 C28 H28A 108.5 . . ? C29 C28 H28A 108.5 . . ? C27 C28 H28B 108.5 . . ? C29 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C28 C29 C30 112.9(6) . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C29 115.5(7) . . ? C31 C30 H30A 108.4 . . ? C29 C30 H30A 108.4 . . ? C31 C30 H30B 108.4 . . ? C29 C30 H30B 108.4 . . ? H30A C30 H30B 107.5 . . ? C30 C31 C32 112.4(8) . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? C33 C32 C31 118.2(10) . . ? C33 C32 H32A 107.8 . . ? C31 C32 H32A 107.8 . . ? C33 C32 H32B 107.8 . . ? C31 C32 H32B 107.8 . . ? H32A C32 H32B 107.1 . . ? C34 C33 C32 115.5(12) . . ? C34 C33 H33A 108.4 . . ? C32 C33 H33A 108.4 . . ? C34 C33 H33B 108.4 . . ? C32 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 C36 125.2(6) . . ? N3 C35 H35 117.4 . . ? C36 C35 H35 117.4 . . ? C35 C36 C37 119.9(6) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? N4 C37 C38 121.5(7) . . ? N4 C37 C36 123.1(6) . . ? C38 C37 C36 115.4(7) . . ? C39 C38 C37 120.3(6) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 N3 125.2(6) . . ? C38 C39 H39 117.4 . . ? N3 C39 H39 117.4 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 N5 124.6(6) . . ? C43 C42 H42 117.7 . . ? N5 C42 H42 117.7 . . ? C42 C43 C44 119.9(7) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? N6 C44 C45 122.3(6) . . ? N6 C44 C43 121.9(7) . . ? C45 C44 C43 115.8(6) . . ? C46 C45 C44 120.1(6) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? N5 C46 C45 124.3(6) . . ? N5 C46 H46 117.9 . . ? C45 C46 H46 117.9 . . ? N6 C47 H47A 109.5 . . ? N6 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N6 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N6 C48 H48A 109.5 . . ? N6 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N6 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N2 Fe1 N1 84.4(2) . . ? N2 Fe1 O1 175.7(2) . . ? N1 Fe1 O1 91.41(19) . . ? N2 Fe1 O2 91.7(2) . . ? N1 Fe1 O2 175.8(2) . . ? O1 Fe1 O2 92.51(18) . . ? N2 Fe1 N3 91.6(2) . . ? N1 Fe1 N3 91.2(2) . . ? O1 Fe1 N3 89.1(2) . . ? O2 Fe1 N3 90.4(2) . . ? N2 Fe1 N5 93.0(2) . . ? N1 Fe1 N5 92.9(2) . . ? O1 Fe1 N5 86.6(2) . . ? O2 Fe1 N5 85.7(2) . . ? N3 Fe1 N5 174.1(2) . . ? C3 N1 C4 120.6(5) . . ? C3 N1 Fe1 126.5(5) . . ? C4 N1 Fe1 112.9(4) . . ? C10 N2 C9 119.3(5) . . ? C10 N2 Fe1 126.9(5) . . ? C9 N2 Fe1 113.8(4) . . ? C35 N3 C39 113.9(6) . . ? C35 N3 Fe1 123.1(5) . . ? C39 N3 Fe1 122.9(4) . . ? C37 N4 C41 121.4(6) . . ? C37 N4 C40 120.1(6) . . ? C41 N4 C40 118.3(6) . . ? C46 N5 C42 115.3(6) . . ? C46 N5 Fe1 125.1(5) . . ? C42 N5 Fe1 119.5(4) . . ? C44 N6 C48 120.7(6) . . ? C44 N6 C47 120.0(6) . . ? C48 N6 C47 119.3(6) . . ? C1 O1 Fe1 129.2(4) . . ? C12 O2 Fe1 129.0(4) . . ? C14 O4 C15 116.7(5) . . ? C17 O6 C18 115.8(6) . . ? C6 O7 C19 116.5(5) . . ? C7 O8 C27 112.7(5) . . ? O98 C98 H98A 109.5 . . ? O98 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? O98 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C98 O98 H98 109.5 . . ? O99 C99 H99A 109.5 . . ? O99 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? O99 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C99 O99 H99 109.5 . . ? 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 O1 C1 C2 C3 4.5(10) . . . . ? C13 C1 C2 C3 -175.1(6) . . . . ? O1 C1 C2 C14 -174.6(6) . . . . ? C13 C1 C2 C14 5.9(10) . . . . ? C1 C2 C3 N1 -1.5(11) . . . . ? C14 C2 C3 N1 177.6(6) . . . . ? C9 C4 C5 C6 0.0(9) . . . . ? N1 C4 C5 C6 178.4(6) . . . . ? C4 C5 C6 O7 179.8(6) . . . . ? C4 C5 C6 C7 -2.1(10) . . . . ? O7 C6 C7 C8 -178.7(6) . . . . ? C5 C6 C7 C8 3.1(10) . . . . ? O7 C6 C7 O8 1.3(9) . . . . ? C5 C6 C7 O8 -176.9(6) . . . . ? O8 C7 C8 C9 178.1(6) . . . . ? C6 C7 C8 C9 -2.0(10) . . . . ? C7 C8 C9 C4 -0.1(10) . . . . ? C7 C8 C9 N2 -178.6(6) . . . . ? C5 C4 C9 C8 1.1(9) . . . . ? N1 C4 C9 C8 -177.4(5) . . . . ? C5 C4 C9 N2 179.8(5) . . . . ? N1 C4 C9 N2 1.3(8) . . . . ? N2 C10 C11 C12 -3.1(11) . . . . ? N2 C10 C11 C17 179.7(6) . . . . ? C10 C11 C12 O2 0.7(11) . . . . ? C17 C11 C12 O2 177.8(6) . . . . ? C10 C11 C12 C16 -179.9(6) . . . . ? C17 C11 C12 C16 -2.9(10) . . . . ? C3 C2 C14 O3 -171.1(7) . . . . ? C1 C2 C14 O3 8.0(11) . . . . ? C3 C2 C14 O4 5.2(9) . . . . ? C1 C2 C14 O4 -175.7(6) . . . . ? C12 C11 C17 O5 1.9(12) . . . . ? C10 C11 C17 O5 179.1(8) . . . . ? C12 C11 C17 O6 -176.0(6) . . . . ? C10 C11 C17 O6 1.2(9) . . . . ? O7 C19 C20 C21 68.7(7) . . . . ? C19 C20 C21 C22 -168.7(6) . . . . ? C20 C21 C22 C23 -172.1(7) . . . . ? C21 C22 C23 C24 -177.0(7) . . . . ? C22 C23 C24 C25 70.9(11) . . . . ? C23 C24 C25 C26 173.5(8) . . . . ? O8 C27 C28 C29 62.1(8) . . . . ? C27 C28 C29 C30 178.8(7) . . . . ? C28 C29 C30 C31 179.2(7) . . . . ? C29 C30 C31 C32 176.3(7) . . . . ? C30 C31 C32 C33 -174.8(9) . . . . ? C31 C32 C33 C34 -63.0(13) . . . . ? N3 C35 C36 C37 -0.4(11) . . . . ? C35 C36 C37 N4 179.5(7) . . . . ? C35 C36 C37 C38 -1.4(11) . . . . ? N4 C37 C38 C39 -178.6(7) . . . . ? C36 C37 C38 C39 2.3(11) . . . . ? C37 C38 C39 N3 -1.4(11) . . . . ? N5 C42 C43 C44 1.9(10) . . . . ? C42 C43 C44 N6 177.0(6) . . . . ? C42 C43 C44 C45 -2.0(9) . . . . ? N6 C44 C45 C46 -177.9(6) . . . . ? C43 C44 C45 C46 1.1(9) . . . . ? C44 C45 C46 N5 0.0(10) . . . . ? C2 C3 N1 C4 -176.2(6) . . . . ? C2 C3 N1 Fe1 2.5(10) . . . . ? C9 C4 N1 C3 -177.0(6) . . . . ? C5 C4 N1 C3 4.6(9) . . . . ? C9 C4 N1 Fe1 4.1(7) . . . . ? C5 C4 N1 Fe1 -174.3(5) . . . . ? N2 Fe1 N1 C3 175.2(5) . . . . ? O1 Fe1 N1 C3 -4.2(5) . . . . ? N3 Fe1 N1 C3 -93.3(5) . . . . ? N5 Fe1 N1 C3 82.5(5) . . . . ? N2 Fe1 N1 C4 -6.0(4) . . . . ? O1 Fe1 N1 C4 174.6(4) . . . . ? N3 Fe1 N1 C4 85.5(4) . . . . ? N5 Fe1 N1 C4 -98.7(4) . . . . ? C11 C10 N2 C9 178.3(6) . . . . ? C11 C10 N2 Fe1 -0.4(10) . . . . ? C8 C9 N2 C10 -6.5(10) . . . . ? C4 C9 N2 C10 175.0(6) . . . . ? C8 C9 N2 Fe1 172.4(5) . . . . ? C4 C9 N2 Fe1 -6.2(7) . . . . ? N1 Fe1 N2 C10 -174.5(6) . . . . ? O2 Fe1 N2 C10 3.9(5) . . . . ? N3 Fe1 N2 C10 94.4(6) . . . . ? N5 Fe1 N2 C10 -81.9(5) . . . . ? N1 Fe1 N2 C9 6.8(4) . . . . ? O2 Fe1 N2 C9 -174.8(4) . . . . ? N3 Fe1 N2 C9 -84.3(4) . . . . ? N5 Fe1 N2 C9 99.4(4) . . . . ? C36 C35 N3 C39 1.4(10) . . . . ? C36 C35 N3 Fe1 -176.3(6) . . . . ? C38 C39 N3 C35 -0.4(10) . . . . ? C38 C39 N3 Fe1 177.2(5) . . . . ? N2 Fe1 N3 C35 -59.8(5) . . . . ? N1 Fe1 N3 C35 -144.2(5) . . . . ? O1 Fe1 N3 C35 124.4(5) . . . . ? O2 Fe1 N3 C35 31.9(5) . . . . ? N2 Fe1 N3 C39 122.8(5) . . . . ? N1 Fe1 N3 C39 38.4(5) . . . . ? O1 Fe1 N3 C39 -53.0(5) . . . . ? O2 Fe1 N3 C39 -145.5(5) . . . . ? C38 C37 N4 C41 -1.7(12) . . . . ? C36 C37 N4 C41 177.4(8) . . . . ? C38 C37 N4 C40 -176.4(7) . . . . ? C36 C37 N4 C40 2.7(12) . . . . ? C45 C46 N5 C42 -0.3(9) . . . . ? C45 C46 N5 Fe1 177.1(5) . . . . ? C43 C42 N5 C46 -0.7(9) . . . . ? C43 C42 N5 Fe1 -178.2(5) . . . . ? N2 Fe1 N5 C46 -35.7(5) . . . . ? N1 Fe1 N5 C46 48.8(5) . . . . ? O1 Fe1 N5 C46 140.1(5) . . . . ? O2 Fe1 N5 C46 -127.2(5) . . . . ? N2 Fe1 N5 C42 141.6(4) . . . . ? N1 Fe1 N5 C42 -133.9(4) . . . . ? O1 Fe1 N5 C42 -42.7(4) . . . . ? O2 Fe1 N5 C42 50.1(4) . . . . ? C45 C44 N6 C48 -5.0(10) . . . . ? C43 C44 N6 C48 176.2(7) . . . . ? C45 C44 N6 C47 174.9(6) . . . . ? C43 C44 N6 C47 -3.9(10) . . . . ? C2 C1 O1 Fe1 -8.4(9) . . . . ? C13 C1 O1 Fe1 171.2(4) . . . . ? N1 Fe1 O1 C1 7.3(5) . . . . ? O2 Fe1 O1 C1 -171.1(5) . . . . ? N3 Fe1 O1 C1 98.5(6) . . . . ? N5 Fe1 O1 C1 -85.5(5) . . . . ? C11 C12 O2 Fe1 5.0(9) . . . . ? C16 C12 O2 Fe1 -174.4(4) . . . . ? N2 Fe1 O2 C12 -6.4(6) . . . . ? O1 Fe1 O2 C12 172.9(5) . . . . ? N3 Fe1 O2 C12 -97.9(5) . . . . ? N5 Fe1 O2 C12 86.5(5) . . . . ? O3 C14 O4 C15 4.2(9) . . . . ? C2 C14 O4 C15 -172.5(6) . . . . ? O5 C17 O6 C18 -4.0(10) . . . . ? C11 C17 O6 C18 174.1(6) . . . . ? C5 C6 O7 C19 24.9(9) . . . . ? C7 C6 O7 C19 -153.2(6) . . . . ? C20 C19 O7 C6 171.2(5) . . . . ? C8 C7 O8 C27 -107.6(7) . . . . ? C6 C7 O8 C27 72.5(8) . . . . ? C28 C27 O8 C7 -172.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.64 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.561 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.092 _iucr_refine_instructions_details ; TITL cl003 in P -1 New: P21/c CELL 0.71069 10.5990 31.2950 15.9970 90.000 101.404 90.000 ZERR 4.00 0.0050 0.0050 0.0050 0.000 0.005 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H FE N O UNIT 198 304 4 24 38 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 20 TEMP -140.00 WGHT 0.136800 FVAR 0.26473 C1 1 1.238346 0.226492 0.428920 11.00000 0.04248 0.04693 = 0.05063 -0.00441 0.00889 -0.00360 C2 1 1.266506 0.249659 0.357238 11.00000 0.03293 0.04572 = 0.04791 0.00052 0.00918 0.00312 C3 1 1.179392 0.279010 0.310310 11.00000 0.04470 0.04642 = 0.04617 -0.00357 0.01492 -0.00196 AFIX 43 H3 2 1.206887 0.293384 0.264747 11.00000 -1.20000 AFIX 0 C4 1 0.982807 0.317044 0.267398 11.00000 0.03094 0.04373 = 0.03955 -0.00036 0.00815 0.00659 C5 1 1.011572 0.335088 0.192243 11.00000 0.03606 0.05416 = 0.04559 -0.00234 0.01726 0.00602 AFIX 43 H5 2 1.091344 0.329025 0.176205 11.00000 -1.20000 AFIX 0 C6 1 0.923023 0.361576 0.142290 11.00000 0.04424 0.04695 = 0.04214 0.00191 0.01387 0.00027 C7 1 0.803991 0.369366 0.164279 11.00000 0.03728 0.05412 = 0.04691 0.00463 0.00977 0.00920 C8 1 0.776137 0.352206 0.238835 11.00000 0.03398 0.04977 = 0.04701 -0.00558 0.00885 0.00303 AFIX 43 H8 2 0.696029 0.358386 0.254293 11.00000 -1.20000 AFIX 0 C9 1 0.864358 0.326187 0.290641 11.00000 0.03665 0.04332 = 0.03934 -0.00124 0.00727 -0.00243 C10 1 0.745868 0.314193 0.399687 11.00000 0.04092 0.04900 = 0.04470 0.00239 0.00635 0.00432 AFIX 43 H10 2 0.686808 0.334593 0.370441 11.00000 -1.20000 AFIX 0 C11 1 0.716177 0.295284 0.474666 11.00000 0.04086 0.05008 = 0.04718 0.00213 0.01973 0.00423 C12 1 0.792217 0.262903 0.522389 11.00000 0.04131 0.05253 = 0.04291 0.00265 0.01543 -0.00312 C13 1 1.334973 0.197893 0.482984 11.00000 0.04976 0.05624 = 0.05582 0.00485 0.01392 0.00702 AFIX 133 H13A 2 1.305273 0.190688 0.535505 11.00000 -1.50000 H13B 2 1.418005 0.212644 0.497337 11.00000 -1.50000 H13C 2 1.344804 0.171653 0.451453 11.00000 -1.50000 AFIX 0 C14 1 1.386911 0.243120 0.329229 11.00000 0.04355 0.04848 = 0.05111 -0.00307 0.00962 -0.00926 C15 1 1.508615 0.262647 0.224568 11.00000 0.04291 0.08574 = 0.06435 0.00282 0.02977 0.01104 AFIX 133 H15A 2 1.588346 0.264603 0.267521 11.00000 -1.50000 H15B 2 1.509549 0.284212 0.180274 11.00000 -1.50000 H15C 2 1.501831 0.234123 0.198783 11.00000 -1.50000 AFIX 0 C16 1 0.758907 0.243292 0.601555 11.00000 0.04814 0.05141 = 0.04919 0.00550 0.01395 0.00118 AFIX 133 H16A 2 0.823968 0.221924 0.624908 11.00000 -1.50000 H16B 2 0.674299 0.229564 0.586989 11.00000 -1.50000 H16C 2 0.756844 0.265665 0.644126 11.00000 -1.50000 AFIX 0 C17 1 0.597200 0.309315 0.499815 11.00000 0.04206 0.06330 = 0.05546 0.00131 0.01200 0.00038 C18 1 0.405810 0.350806 0.460499 11.00000 0.04926 0.08181 = 0.08020 0.00545 0.02804 0.01657 AFIX 133 H18A 2 0.351778 0.325324 0.459440 11.00000 -1.50000 H18B 2 0.364743 0.370835 0.416308 11.00000 -1.50000 H18C 2 0.416379 0.364535 0.516514 11.00000 -1.50000 AFIX 0 C19 1 1.031451 0.359751 0.024655 11.00000 0.04963 0.04965 = 0.05575 -0.00692 0.02016 0.00108 AFIX 23 H19A 2 1.009023 0.329152 0.015846 11.00000 -1.20000 H19B 2 1.120250 0.361892 0.058338 11.00000 -1.20000 AFIX 0 C20 1 1.021453 0.382073 -0.060027 11.00000 0.06220 0.05795 = 0.04322 0.00039 0.02081 0.00231 AFIX 23 H20A 2 0.929942 0.382677 -0.089222 11.00000 -1.20000 H20B 2 1.069268 0.365208 -0.095918 11.00000 -1.20000 AFIX 0 C21 1 1.072804 0.427268 -0.053441 11.00000 0.08574 0.06161 = 0.05204 0.00553 0.02773 -0.00474 AFIX 23 H21A 2 1.167697 0.426500 -0.035597 11.00000 -1.20000 H21B 2 1.037934 0.442786 -0.009066 11.00000 -1.20000 AFIX 0 C22 1 1.035573 0.452191 -0.140819 11.00000 0.09004 0.08108 = 0.06046 0.01348 0.02892 -0.00288 AFIX 23 H22A 2 1.059782 0.434836 -0.186943 11.00000 -1.20000 H22B 2 0.941266 0.456647 -0.154691 11.00000 -1.20000 AFIX 0 C23 1 1.101760 0.494241 -0.136357 11.00000 0.09334 0.07621 = 0.08353 0.00151 0.03307 -0.00987 AFIX 23 H23A 2 1.195965 0.489527 -0.125208 11.00000 -1.20000 H23B 2 1.081318 0.510784 -0.087983 11.00000 -1.20000 AFIX 0 C24 1 1.062839 0.520233 -0.217957 11.00000 0.09970 0.05942 = 0.07797 0.01538 0.02553 0.00709 AFIX 23 H24A 2 1.124385 0.544201 -0.215697 11.00000 -1.20000 H24B 2 1.073052 0.501824 -0.266509 11.00000 -1.20000 AFIX 0 C25 1 0.930955 0.538213 -0.236599 11.00000 0.08824 0.06922 = 0.09820 0.01060 0.04298 0.01004 AFIX 23 H25A 2 0.916286 0.554278 -0.186067 11.00000 -1.20000 H25B 2 0.868287 0.514398 -0.246477 11.00000 -1.20000 AFIX 0 C26 1 0.905773 0.567678 -0.313573 11.00000 0.07699 0.07025 = 0.07280 0.01415 0.02275 -0.00200 AFIX 133 H26A 2 0.967908 0.591235 -0.304655 11.00000 -1.50000 H26B 2 0.818280 0.579204 -0.321099 11.00000 -1.50000 H26C 2 0.914885 0.551603 -0.364619 11.00000 -1.50000 AFIX 0 C27 1 0.653076 0.372779 0.034194 11.00000 0.05019 0.06855 = 0.04852 -0.00080 0.00058 -0.00602 AFIX 23 H27A 2 0.601126 0.348248 0.047099 11.00000 -1.20000 H27B 2 0.720283 0.361947 0.004585 11.00000 -1.20000 AFIX 0 C28 1 0.567973 0.404766 -0.021697 11.00000 0.05324 0.06148 = 0.05545 0.00407 0.00700 -0.00596 AFIX 23 H28A 2 0.501921 0.415114 0.009396 11.00000 -1.20000 H28B 2 0.522597 0.389859 -0.073586 11.00000 -1.20000 AFIX 0 C29 1 0.637725 0.443134 -0.048736 11.00000 0.05236 0.05957 = 0.05931 0.00452 0.00863 -0.00575 AFIX 23 H29A 2 0.704770 0.433043 -0.079248 11.00000 -1.20000 H29B 2 0.681289 0.458719 0.002794 11.00000 -1.20000 AFIX 0 C30 1 0.547600 0.473867 -0.106510 11.00000 0.07604 0.05498 = 0.06417 0.00914 0.02346 -0.00067 AFIX 23 H30A 2 0.504834 0.458033 -0.157928 11.00000 -1.20000 H30B 2 0.479760 0.483234 -0.075993 11.00000 -1.20000 AFIX 0 C31 1 0.611044 0.513182 -0.134820 11.00000 0.09206 0.06781 = 0.12579 0.01836 0.05587 0.00459 AFIX 23 H31A 2 0.682290 0.504214 -0.162648 11.00000 -1.20000 H31B 2 0.648373 0.530448 -0.084090 11.00000 -1.20000 AFIX 0 C32 1 0.515317 0.541189 -0.197739 11.00000 0.15552 0.05380 = 0.12920 0.04131 0.07990 0.03264 AFIX 23 H32A 2 0.471894 0.522528 -0.244681 11.00000 -1.20000 H32B 2 0.448429 0.551498 -0.167310 11.00000 -1.20000 AFIX 0 C33 1 0.566851 0.578858 -0.236563 11.00000 0.09773 0.12027 = 0.14508 0.02914 0.05220 0.02238 AFIX 23 H33A 2 0.632575 0.568812 -0.268221 11.00000 -1.20000 H33B 2 0.495948 0.591822 -0.278503 11.00000 -1.20000 AFIX 0 C34 1 0.622632 0.610979 -0.178564 11.00000 0.10623 0.15956 = 0.16888 -0.09520 0.07171 -0.08689 AFIX 137 H34A 2 0.562951 0.618506 -0.141286 11.00000 -1.50000 H34B 2 0.640327 0.636336 -0.210305 11.00000 -1.50000 H34C 2 0.703233 0.600331 -0.143949 11.00000 -1.50000 AFIX 0 C35 1 0.779314 0.204365 0.337623 11.00000 0.04188 0.06201 = 0.04809 -0.00437 0.01180 0.00402 AFIX 43 H35 2 0.732928 0.218252 0.374916 11.00000 -1.20000 AFIX 0 C36 1 0.719818 0.170738 0.289985 11.00000 0.03854 0.06472 = 0.05902 0.00170 0.01509 -0.00287 AFIX 43 H36 2 0.635867 0.162139 0.295444 11.00000 -1.20000 AFIX 0 C37 1 0.783622 0.149063 0.233063 11.00000 0.04955 0.06024 = 0.05568 -0.00446 0.01196 -0.00562 C38 1 0.906118 0.164980 0.228465 11.00000 0.05248 0.05132 = 0.06022 -0.00331 0.02004 -0.00143 AFIX 43 H38 2 0.953175 0.152542 0.189902 11.00000 -1.20000 AFIX 0 C39 1 0.957662 0.198162 0.279060 11.00000 0.03431 0.05907 = 0.05187 -0.00215 0.01507 -0.00179 AFIX 43 H39 2 1.041481 0.207433 0.274740 11.00000 -1.20000 AFIX 0 C40 1 0.600916 0.101589 0.187673 11.00000 0.06552 0.10094 = 0.07675 -0.01939 0.01222 -0.02468 AFIX 133 H40A 2 0.596552 0.092980 0.245935 11.00000 -1.50000 H40B 2 0.578230 0.077244 0.149096 11.00000 -1.50000 H40C 2 0.540404 0.125058 0.169731 11.00000 -1.50000 AFIX 0 C41 1 0.797972 0.095471 0.124740 11.00000 0.08143 0.08209 = 0.07747 -0.02391 0.02169 -0.01322 AFIX 133 H41A 2 0.809781 0.116200 0.081012 11.00000 -1.50000 H41B 2 0.746887 0.071291 0.097689 11.00000 -1.50000 H41C 2 0.882195 0.085214 0.154698 11.00000 -1.50000 AFIX 0 C42 1 1.131432 0.295867 0.578447 11.00000 0.04262 0.04870 = 0.04986 0.00291 0.01925 0.00062 AFIX 43 H42 2 1.128233 0.266182 0.590276 11.00000 -1.20000 AFIX 0 C43 1 1.191956 0.321795 0.642098 11.00000 0.04442 0.05428 = 0.04365 0.00644 0.01162 -0.00161 AFIX 43 H43 2 1.231474 0.309984 0.695587 11.00000 -1.20000 AFIX 0 C44 1 1.195940 0.366185 0.628573 11.00000 0.04379 0.04790 = 0.05060 -0.00405 0.00871 -0.00476 C45 1 1.138351 0.380394 0.546506 11.00000 0.04413 0.04064 = 0.06086 0.00350 0.01224 -0.00064 AFIX 43 H45 2 1.139085 0.409938 0.532965 11.00000 -1.20000 AFIX 0 C46 1 1.081012 0.351626 0.485855 11.00000 0.04066 0.04533 = 0.04989 0.00636 0.01137 0.00311 AFIX 43 H46 2 1.043108 0.362341 0.431076 11.00000 -1.20000 AFIX 0 C47 1 1.299696 0.377826 0.777967 11.00000 0.06494 0.06946 = 0.04684 -0.00009 0.00224 -0.00986 AFIX 133 H47A 2 1.234174 0.359847 0.795934 11.00000 -1.50000 H47B 2 1.320214 0.401941 0.817394 11.00000 -1.50000 H47C 2 1.377586 0.360903 0.778282 11.00000 -1.50000 AFIX 0 C48 1 1.260574 0.438538 0.675311 11.00000 0.07765 0.05112 = 0.06257 -0.00988 0.00460 -0.00449 AFIX 133 H48A 2 1.305286 0.442468 0.627779 11.00000 -1.50000 H48B 2 1.308979 0.452811 0.726206 11.00000 -1.50000 H48C 2 1.174109 0.450914 0.660358 11.00000 -1.50000 AFIX 0 FE1 3 0.984103 0.266568 0.412451 11.00000 0.03578 0.04855 = 0.04425 -0.00025 0.01269 0.00120 N1 4 1.063948 0.288517 0.323183 11.00000 0.03072 0.04714 = 0.03980 -0.00166 0.00621 -0.00077 N2 4 0.848621 0.305656 0.367685 11.00000 0.03559 0.04487 = 0.04676 0.00181 0.01583 -0.00060 N3 4 0.898270 0.219179 0.335577 11.00000 0.03890 0.05617 = 0.05139 0.00155 0.01201 0.00398 N4 4 0.731539 0.115735 0.185075 11.00000 0.05317 0.06647 = 0.07326 -0.01711 0.01871 -0.01080 N5 4 1.075072 0.309433 0.498940 11.00000 0.04119 0.04486 = 0.05090 0.00456 0.01962 0.00474 N6 4 1.250849 0.393847 0.692253 11.00000 0.06535 0.05443 = 0.05241 0.00062 0.00774 -0.01177 O1 5 1.130151 0.228539 0.452516 11.00000 0.04120 0.04443 = 0.05053 0.00357 0.01176 -0.00129 O2 5 0.895069 0.248069 0.502826 11.00000 0.04597 0.05009 = 0.04794 -0.00054 0.01341 -0.00381 O3 5 1.469227 0.216105 0.354036 11.00000 0.04565 0.06749 = 0.07235 0.01144 0.01997 0.01803 O4 5 1.400163 0.269990 0.264386 11.00000 0.04394 0.07225 = 0.06114 0.00984 0.02318 0.00869 O5 5 0.551913 0.297744 0.559249 11.00000 0.06906 0.10828 = 0.07801 0.03375 0.04357 0.02295 O6 5 0.530700 0.338580 0.444593 11.00000 0.04835 0.08560 = 0.06675 0.01638 0.02628 0.01688 O7 5 0.942767 0.380625 0.068385 11.00000 0.04834 0.05265 = 0.05225 0.00502 0.02154 0.00669 O8 5 0.711852 0.394365 0.112193 11.00000 0.04417 0.05879 = 0.04765 0.00552 0.01332 0.00685 PART -1 C98 1 0.462632 0.026790 0.960826 10.50000 0.05565 AFIX 33 H98A 2 0.451525 0.050714 0.998233 10.50000 -1.50000 H98B 2 0.390542 0.006839 0.957505 10.50000 -1.50000 H98C 2 0.464980 0.037632 0.903681 10.50000 -1.50000 AFIX 0 O98 5 0.604552 0.000781 1.001302 10.50000 0.10955 AFIX 83 H98 2 0.664772 0.012132 0.982091 10.50000 -1.50000 AFIX 0 PART 0 C99 1 0.778240 0.067720 0.898267 11.00000 0.09350 AFIX 137 H99A 2 0.710963 0.085280 0.915213 11.00000 -1.50000 H99B 2 0.750133 0.058577 0.838909 11.00000 -1.50000 H99C 2 0.857534 0.084489 0.903700 11.00000 -1.50000 AFIX 0 O99 5 0.803176 0.028688 0.955575 11.00000 0.14186 AFIX 83 H99 2 0.882126 0.027049 0.976769 11.00000 -1.50000 HKLF 4 REM cl003 in P -1 New: P21/c REM R1 = 0.0852 for 4166 Fo > 4sig(Fo) and 0.1626 for all 8715 data REM 586 parameters refined using 0 restraints END WGHT 0.1368 0.0000 REM Highest difference peak 1.561, deepest hole -0.390, 1-sigma level 0.092 Q1 1 0.5405 0.0413 0.9362 11.00000 0.05 1.56 Q2 1 0.6448 0.0228 0.9651 11.00000 0.05 1.46 Q3 1 0.8935 0.0134 0.9973 11.00000 0.05 1.41 Q4 1 0.3651 0.0180 0.9659 11.00000 0.05 1.13 Q5 1 0.7455 0.0342 0.9433 11.00000 0.05 0.70 Q6 1 0.9847 0.4841 -0.1528 11.00000 0.05 0.43 Q7 1 0.5979 0.6231 -0.2476 11.00000 0.05 0.41 Q8 1 1.0914 0.2885 0.4545 11.00000 0.05 0.37 Q9 1 0.6616 0.5814 -0.1593 11.00000 0.05 0.35 Q10 1 1.1396 0.4579 -0.1073 11.00000 0.05 0.32 Q11 1 0.6065 0.5571 -0.1566 11.00000 0.05 0.31 Q12 1 0.9534 0.2612 0.3062 11.00000 0.05 0.30 Q13 1 0.8735 0.2474 0.3604 11.00000 0.05 0.30 Q14 1 0.9453 0.2246 0.4376 11.00000 0.05 0.28 Q15 1 0.5707 0.6136 -0.1748 11.00000 0.05 0.28 Q16 1 1.0303 0.3067 0.3866 11.00000 0.05 0.27 Q17 1 0.9605 0.3045 0.4512 11.00000 0.05 0.27 Q18 1 0.9926 0.2196 0.4330 11.00000 0.05 0.25 Q19 1 0.4972 0.5323 -0.1981 11.00000 0.05 0.23 Q20 1 0.6345 0.0531 0.8995 11.00000 0.05 0.22 ; _database_code_depnum_ccdc_archive 'CCDC 944434' ####################################################################### # # 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_j31 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H60 Fe N4 O8' _chemical_formula_sum 'C41 H60 Fe N4 O8' _chemical_formula_weight 792.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 11.9872(7) _cell_length_b 12.5380(8) _cell_length_c 14.6613(10) _cell_angle_alpha 95.394(5) _cell_angle_beta 102.327(5) _cell_angle_gamma 106.231(5) _cell_volume 2039.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 24231 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 24.6 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 0.425 _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 133(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDSII _diffrn_measurement_method Omega-Scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24231 _diffrn_reflns_av_R_equivalents 0.1417 _diffrn_reflns_av_sigmaI/netI 0.1438 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.63 _reflns_number_total 6827 _reflns_number_gt 3594 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-AREA-STOE _computing_cell_refinement X-AREA-STOE _computing_data_reduction X-AREA-STOE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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^)+(0.0495P)^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 6827 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1335 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.877 _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 C1 C 0.0988(4) 0.4434(4) 0.2366(4) 0.0394(12) Uani 1 1 d . . . C2 C 0.0738(4) 0.5086(4) 0.3082(3) 0.0370(12) Uani 1 1 d . . . C3 C 0.1364(4) 0.5273(4) 0.4055(4) 0.0398(12) Uani 1 1 d . . . H3 H 0.1210 0.5816 0.4468 0.048 Uiso 1 1 calc R . . C4 C 0.2745(4) 0.5095(3) 0.5412(3) 0.0328(11) Uani 1 1 d . . . C5 C 0.3221(4) 0.6185(4) 0.6970(3) 0.0324(11) Uani 1 1 d . . . C6 C 0.4181(4) 0.5722(4) 0.7274(3) 0.0328(11) Uani 1 1 d . . . C7 C 0.4362(4) 0.4946(4) 0.6637(3) 0.0355(12) Uani 1 1 d . . . H7 H 0.4989 0.4629 0.6840 0.043 Uiso 1 1 calc R . . C8 C 0.3665(4) 0.4607(4) 0.5712(3) 0.0350(12) Uani 1 1 d . . . C9 C 0.4675(4) 0.3371(4) 0.5206(3) 0.0338(11) Uani 1 1 d . . . H9 H 0.5228 0.3650 0.5808 0.041 Uiso 1 1 calc R . . C10 C 0.4908(4) 0.2541(4) 0.4609(3) 0.0350(11) Uani 1 1 d . . . C11 C 0.4237(4) 0.2126(4) 0.3654(3) 0.0355(12) Uani 1 1 d . . . C12 C 0.5926(4) 0.2132(4) 0.4998(4) 0.0356(12) Uani 1 1 d . . . C13 C 0.7228(5) 0.1956(5) 0.6377(4) 0.0564(15) Uani 1 1 d . . . H13A H 0.6971 0.1132 0.6235 0.085 Uiso 1 1 calc R . . H13B H 0.7456 0.2198 0.7064 0.085 Uiso 1 1 calc R . . H13C H 0.7918 0.2264 0.6118 0.085 Uiso 1 1 calc R . . C14 C 0.4479(5) 0.1260(4) 0.3018(3) 0.0425(13) Uani 1 1 d . . . H14A H 0.3767 0.0907 0.2493 0.064 Uiso 1 1 calc R . . H14B H 0.4667 0.0684 0.3376 0.064 Uiso 1 1 calc R . . H14C H 0.5161 0.1620 0.2767 0.064 Uiso 1 1 calc R . . C15 C -0.0148(4) 0.5709(4) 0.2911(4) 0.0379(12) Uani 1 1 d . . . C16 C -0.1944(4) 0.5793(4) 0.1915(4) 0.0465(13) Uani 1 1 d . . . H16A H -0.2234 0.5878 0.2486 0.070 Uiso 1 1 calc R . . H16B H -0.2607 0.5317 0.1395 0.070 Uiso 1 1 calc R . . H16C H -0.1632 0.6535 0.1742 0.070 Uiso 1 1 calc R . . C17 C 0.0517(5) 0.4412(4) 0.1329(4) 0.0488(14) Uani 1 1 d . . . H17A H 0.1051 0.4190 0.0981 0.073 Uiso 1 1 calc R . . H17B H 0.0483 0.5162 0.1220 0.073 Uiso 1 1 calc R . . H17C H -0.0289 0.3869 0.1109 0.073 Uiso 1 1 calc R . . C18 C 0.0265(4) 0.2125(4) 0.4394(4) 0.0393(12) Uani 1 1 d . . . H18 H 0.0421 0.2826 0.4784 0.047 Uiso 1 1 calc R . . C19 C -0.0688(4) 0.1238(4) 0.4458(3) 0.0399(12) Uani 1 1 d . . . H19 H -0.1173 0.1343 0.4872 0.048 Uiso 1 1 calc R . . C41 C 0.2546(4) 0.5866(4) 0.6060(3) 0.0352(12) Uani 1 1 d . . . H41 H 0.1917 0.6179 0.5859 0.042 Uiso 1 1 calc R . . C20 C -0.0940(4) 0.0175(4) 0.3907(4) 0.0385(12) Uani 1 1 d . . . C21 C -0.0192(4) 0.0124(4) 0.3305(4) 0.0451(13) Uani 1 1 d . . . H21 H -0.0316 -0.0566 0.2910 0.054 Uiso 1 1 calc R . . C22 C 0.0721(4) 0.1059(4) 0.3275(4) 0.0416(13) Uani 1 1 d . . . H22 H 0.1196 0.0993 0.2843 0.050 Uiso 1 1 calc R . . C23 C -0.2670(5) -0.0653(4) 0.4530(4) 0.0530(15) Uani 1 1 d . . . H23A H -0.2241 -0.0506 0.5200 0.080 Uiso 1 1 calc R . . H23B H -0.3326 -0.1363 0.4397 0.080 Uiso 1 1 calc R . . H23C H -0.2998 -0.0037 0.4386 0.080 Uiso 1 1 calc R . . C24 C -0.2016(5) -0.1830(4) 0.3422(4) 0.0524(15) Uani 1 1 d . . . H24A H -0.2318 -0.1831 0.2745 0.079 Uiso 1 1 calc R . . H24B H -0.2594 -0.2411 0.3634 0.079 Uiso 1 1 calc R . . H24C H -0.1245 -0.1985 0.3529 0.079 Uiso 1 1 calc R . . C25 C 0.2223(4) 0.7497(4) 0.7363(3) 0.0393(12) Uani 1 1 d . . . H25A H 0.1414 0.6949 0.7101 0.047 Uiso 1 1 calc R . . H25B H 0.2436 0.7949 0.6872 0.047 Uiso 1 1 calc R . . C26 C 0.2240(4) 0.8249(4) 0.8230(4) 0.0431(13) Uani 1 1 d . . . H26A H 0.2019 0.7778 0.8708 0.052 Uiso 1 1 calc R . . H26B H 0.1624 0.8631 0.8060 0.052 Uiso 1 1 calc R . . C27 C 0.3455(5) 0.9140(4) 0.8671(4) 0.0451(13) Uani 1 1 d . . . H27A H 0.3489 0.9406 0.9337 0.054 Uiso 1 1 calc R . . H27B H 0.4096 0.8785 0.8676 0.054 Uiso 1 1 calc R . . C28 C 0.3711(5) 1.0153(4) 0.8167(4) 0.0457(13) Uani 1 1 d . . . H28A H 0.3093 1.0533 0.8184 0.055 Uiso 1 1 calc R . . H28B H 0.3655 0.9892 0.7495 0.055 Uiso 1 1 calc R . . C29 C 0.4955(5) 1.0999(4) 0.8615(4) 0.0455(13) Uani 1 1 d . . . H29A H 0.5571 1.0629 0.8553 0.055 Uiso 1 1 calc R . . H29B H 0.5031 1.1207 0.9298 0.055 Uiso 1 1 calc R . . C30 C 0.5216(5) 1.2079(4) 0.8176(4) 0.0505(14) Uani 1 1 d . . . H30A H 0.4625 1.2470 0.8264 0.061 Uiso 1 1 calc R . . H30B H 0.5109 1.1873 0.7488 0.061 Uiso 1 1 calc R . . C31 C 0.6487(5) 1.2895(4) 0.8607(4) 0.0525(15) Uani 1 1 d . . . H31A H 0.7078 1.2499 0.8532 0.063 Uiso 1 1 calc R . . H31B H 0.6618 1.3531 0.8249 0.063 Uiso 1 1 calc R . . C32 C 0.6717(5) 1.3359(4) 0.9647(4) 0.0550(15) Uani 1 1 d . . . H32A H 0.6124 1.3737 0.9730 0.082 Uiso 1 1 calc R . . H32B H 0.7526 1.3899 0.9868 0.082 Uiso 1 1 calc R . . H32C H 0.6650 1.2740 1.0013 0.082 Uiso 1 1 calc R . . C33 C 0.5834(4) 0.5719(4) 0.8512(3) 0.0397(12) Uani 1 1 d . . . H33A H 0.6432 0.5990 0.8145 0.048 Uiso 1 1 calc R . . H33B H 0.5601 0.4886 0.8423 0.048 Uiso 1 1 calc R . . C34 C 0.6361(4) 0.6204(4) 0.9545(3) 0.0410(12) Uani 1 1 d . . . H34A H 0.7107 0.6007 0.9763 0.049 Uiso 1 1 calc R . . H34B H 0.5789 0.5843 0.9905 0.049 Uiso 1 1 calc R . . C35 C 0.6648(4) 0.7473(4) 0.9781(3) 0.0410(12) Uani 1 1 d . . . H35A H 0.6977 0.7704 1.0474 0.049 Uiso 1 1 calc R . . H35B H 0.5892 0.7666 0.9609 0.049 Uiso 1 1 calc R . . C36 C 0.7539(5) 0.8150(4) 0.9287(4) 0.0434(13) Uani 1 1 d . . . H36A H 0.8286 0.7938 0.9432 0.052 Uiso 1 1 calc R . . H36B H 0.7196 0.7963 0.8594 0.052 Uiso 1 1 calc R . . C37 C 0.7836(4) 0.9407(4) 0.9597(4) 0.0438(13) Uani 1 1 d . . . H37A H 0.8216 0.9590 1.0285 0.053 Uiso 1 1 calc R . . H37B H 0.7077 0.9601 0.9491 0.053 Uiso 1 1 calc R . . C38 C 0.8666(4) 1.0142(4) 0.9088(4) 0.0431(12) Uani 1 1 d . . . H38A H 0.9405 0.9918 0.9154 0.052 Uiso 1 1 calc R . . H38B H 0.8263 1.0008 0.8405 0.052 Uiso 1 1 calc R . . C39 C 0.9011(5) 1.1395(4) 0.9471(4) 0.0490(14) Uani 1 1 d . . . H39A H 0.9478 1.1541 1.0138 0.059 Uiso 1 1 calc R . . H39B H 0.8271 1.1606 0.9457 0.059 Uiso 1 1 calc R . . C40 C 0.9751(5) 1.2132(4) 0.8903(4) 0.0572(15) Uani 1 1 d . . . H40A H 1.0499 1.1947 0.8933 0.086 Uiso 1 1 calc R . . H40B H 0.9939 1.2927 0.9170 0.086 Uiso 1 1 calc R . . H40C H 0.9290 1.1996 0.8242 0.086 Uiso 1 1 calc R . . N1 N 0.2129(3) 0.4772(3) 0.4439(3) 0.0358(10) Uani 1 1 d . . . N2 N 0.3789(3) 0.3790(3) 0.5020(3) 0.0355(10) Uani 1 1 d . . . N3 N 0.0981(3) 0.2063(3) 0.3821(3) 0.0369(10) Uani 1 1 d . . . N4 N -0.1852(4) -0.0729(3) 0.3953(3) 0.0445(11) Uani 1 1 d . . . O1 O 0.1700(3) 0.3848(3) 0.2548(2) 0.0462(9) Uani 1 1 d . . . O2 O 0.3342(3) 0.2445(2) 0.3284(2) 0.0404(8) Uani 1 1 d . . . O3 O 0.6254(3) 0.2360(3) 0.5956(3) 0.0495(9) Uani 1 1 d . . . O4 O 0.6426(3) 0.1643(3) 0.4555(3) 0.0492(9) Uani 1 1 d . . . O5 O -0.1005(3) 0.5278(3) 0.2095(2) 0.0446(9) Uani 1 1 d . . . O6 O -0.0158(3) 0.6499(3) 0.3452(3) 0.0488(9) Uani 1 1 d . . . O7 O 0.3086(3) 0.6919(2) 0.7646(2) 0.0391(8) Uani 1 1 d . . . O8 O 0.4796(3) 0.6078(2) 0.8192(2) 0.0388(8) Uani 1 1 d . . . Fe1 Fe 0.24727(6) 0.34229(6) 0.37510(5) 0.0359(2) 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 0.032(3) 0.033(3) 0.050(3) 0.006(2) 0.011(2) 0.005(2) C2 0.035(3) 0.033(3) 0.041(3) 0.005(2) 0.010(2) 0.009(2) C3 0.041(3) 0.030(2) 0.050(3) 0.002(2) 0.013(2) 0.013(2) C4 0.036(3) 0.025(2) 0.034(3) 0.002(2) 0.006(2) 0.005(2) C5 0.031(3) 0.027(2) 0.038(3) 0.003(2) 0.013(2) 0.006(2) C6 0.034(3) 0.027(2) 0.035(3) 0.005(2) 0.009(2) 0.004(2) C7 0.030(3) 0.029(2) 0.045(3) 0.009(2) 0.006(2) 0.008(2) C8 0.031(3) 0.027(2) 0.044(3) 0.002(2) 0.011(2) 0.004(2) C9 0.030(3) 0.029(2) 0.039(3) 0.004(2) 0.010(2) 0.004(2) C10 0.035(3) 0.027(2) 0.046(3) 0.003(2) 0.015(2) 0.009(2) C11 0.030(3) 0.031(3) 0.045(3) 0.007(2) 0.013(2) 0.006(2) C12 0.036(3) 0.030(3) 0.043(3) 0.003(2) 0.016(2) 0.010(2) C13 0.057(4) 0.068(4) 0.051(4) 0.012(3) 0.005(3) 0.035(3) C14 0.043(3) 0.035(3) 0.046(3) -0.002(2) 0.013(3) 0.011(2) C15 0.038(3) 0.034(3) 0.039(3) 0.006(2) 0.007(2) 0.007(2) C16 0.037(3) 0.050(3) 0.054(3) 0.016(3) 0.006(3) 0.017(2) C17 0.047(3) 0.054(3) 0.046(3) 0.007(3) 0.007(3) 0.019(3) C18 0.042(3) 0.031(3) 0.045(3) 0.005(2) 0.007(3) 0.015(2) C19 0.042(3) 0.039(3) 0.043(3) 0.007(2) 0.015(2) 0.017(2) C41 0.029(3) 0.029(2) 0.044(3) 0.007(2) 0.006(2) 0.006(2) C20 0.033(3) 0.031(3) 0.053(3) 0.006(2) 0.013(2) 0.012(2) C21 0.042(3) 0.031(3) 0.055(3) -0.002(2) 0.008(3) 0.005(2) C22 0.036(3) 0.039(3) 0.049(3) 0.000(2) 0.017(2) 0.006(2) C23 0.049(4) 0.038(3) 0.077(4) 0.013(3) 0.024(3) 0.013(3) C24 0.040(3) 0.034(3) 0.076(4) 0.004(3) 0.009(3) 0.006(2) C25 0.035(3) 0.035(3) 0.046(3) 0.004(2) 0.005(2) 0.014(2) C26 0.038(3) 0.046(3) 0.049(3) 0.008(3) 0.011(2) 0.020(2) C27 0.050(3) 0.041(3) 0.044(3) 0.002(2) 0.009(3) 0.018(2) C28 0.049(3) 0.046(3) 0.043(3) 0.002(2) 0.004(3) 0.023(3) C29 0.049(3) 0.040(3) 0.046(3) 0.002(2) 0.006(3) 0.019(3) C30 0.051(4) 0.049(3) 0.056(4) 0.010(3) 0.010(3) 0.024(3) C31 0.049(4) 0.046(3) 0.064(4) 0.007(3) 0.011(3) 0.020(3) C32 0.055(4) 0.041(3) 0.063(4) 0.008(3) 0.004(3) 0.012(3) C33 0.032(3) 0.034(3) 0.051(3) 0.007(2) 0.008(2) 0.010(2) C34 0.036(3) 0.039(3) 0.047(3) 0.009(2) 0.008(2) 0.012(2) C35 0.035(3) 0.048(3) 0.039(3) 0.006(2) 0.009(2) 0.013(2) C36 0.043(3) 0.040(3) 0.045(3) 0.004(2) 0.010(2) 0.012(2) C37 0.034(3) 0.046(3) 0.050(3) 0.004(3) 0.011(2) 0.011(2) C38 0.036(3) 0.045(3) 0.046(3) 0.009(2) 0.006(2) 0.012(2) C39 0.043(3) 0.044(3) 0.058(4) 0.008(3) 0.010(3) 0.011(2) C40 0.060(4) 0.048(3) 0.065(4) 0.014(3) 0.015(3) 0.017(3) N1 0.033(2) 0.029(2) 0.043(3) 0.0062(18) 0.0086(19) 0.0073(18) N2 0.029(2) 0.025(2) 0.053(3) 0.0031(18) 0.0151(19) 0.0075(17) N3 0.033(2) 0.035(2) 0.041(2) -0.0003(19) 0.010(2) 0.0100(18) N4 0.041(3) 0.029(2) 0.065(3) 0.006(2) 0.016(2) 0.0113(19) O1 0.050(2) 0.0413(19) 0.048(2) 0.0013(16) 0.0107(18) 0.0192(17) O2 0.036(2) 0.0374(18) 0.045(2) 0.0022(16) 0.0096(16) 0.0080(16) O3 0.041(2) 0.060(2) 0.049(2) 0.0046(18) 0.0066(17) 0.0246(18) O4 0.052(2) 0.051(2) 0.054(2) 0.0094(18) 0.0175(19) 0.0272(19) O5 0.039(2) 0.045(2) 0.047(2) 0.0064(17) 0.0053(17) 0.0140(16) O6 0.044(2) 0.044(2) 0.054(2) -0.0020(18) 0.0027(18) 0.0178(17) O7 0.036(2) 0.0379(18) 0.042(2) 0.0023(16) 0.0042(16) 0.0160(15) O8 0.038(2) 0.0381(18) 0.039(2) -0.0005(15) 0.0059(16) 0.0135(15) Fe1 0.0322(4) 0.0304(4) 0.0424(5) 0.0028(3) 0.0070(3) 0.0083(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 C1 O1 1.276(6) . ? C1 C2 1.404(7) . ? C1 C17 1.499(7) . ? C2 C3 1.426(7) . ? C2 C15 1.479(7) . ? C3 N1 1.312(6) . ? C3 H3 0.9500 . ? C4 C41 1.395(6) . ? C4 C8 1.415(6) . ? C4 N1 1.421(6) . ? C5 O7 1.354(5) . ? C5 C41 1.361(6) . ? C5 C6 1.436(6) . ? C6 O8 1.354(5) . ? C6 C7 1.378(6) . ? C7 C8 1.388(6) . ? C7 H7 0.9500 . ? C8 N2 1.434(6) . ? C9 N2 1.302(6) . ? C9 C10 1.422(6) . ? C9 H9 0.9500 . ? C10 C11 1.424(7) . ? C10 C12 1.478(7) . ? C11 O2 1.280(5) . ? C11 C14 1.495(6) . ? C12 O4 1.207(5) . ? C12 O3 1.354(6) . ? C13 O3 1.442(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O6 1.213(5) . ? C15 O5 1.350(5) . ? C16 O5 1.437(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.335(6) . ? C18 C19 1.380(7) . ? C18 H18 0.9500 . ? C19 C20 1.409(6) . ? C19 H19 0.9500 . ? C41 H41 0.9500 . ? C20 N4 1.356(6) . ? C20 C21 1.395(7) . ? C21 C22 1.374(6) . ? C21 H21 0.9500 . ? C22 N3 1.344(6) . ? C22 H22 0.9500 . ? C23 N4 1.441(7) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N4 1.459(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O7 1.435(5) . ? C25 C26 1.502(7) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.530(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.519(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.532(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.535(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.537(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.518(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 O8 1.441(5) . ? C33 C34 1.506(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.520(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.525(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.516(6) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.526(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.525(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.528(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N1 Fe1 2.072(4) . ? N2 Fe1 2.085(4) . ? N3 Fe1 2.127(4) . ? O1 Fe1 2.002(3) . ? O2 Fe1 1.980(3) . ? 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 C1 C2 122.2(5) . . ? O1 C1 C17 113.8(5) . . ? C2 C1 C17 123.9(5) . . ? C1 C2 C3 123.4(5) . . ? C1 C2 C15 124.1(4) . . ? C3 C2 C15 112.3(4) . . ? N1 C3 C2 126.7(5) . . ? N1 C3 H3 116.7 . . ? C2 C3 H3 116.7 . . ? C41 C4 C8 119.1(4) . . ? C41 C4 N1 125.7(4) . . ? C8 C4 N1 115.2(4) . . ? O7 C5 C41 126.3(4) . . ? O7 C5 C6 114.7(4) . . ? C41 C5 C6 119.0(4) . . ? O8 C6 C7 126.5(4) . . ? O8 C6 C5 114.9(4) . . ? C7 C6 C5 118.6(4) . . ? C6 C7 C8 122.5(5) . . ? C6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C7 C8 C4 118.4(4) . . ? C7 C8 N2 125.4(4) . . ? C4 C8 N2 116.2(4) . . ? N2 C9 C10 127.3(5) . . ? N2 C9 H9 116.4 . . ? C10 C9 H9 116.4 . . ? C9 C10 C11 123.0(4) . . ? C9 C10 C12 117.7(4) . . ? C11 C10 C12 119.2(4) . . ? O2 C11 C10 121.8(4) . . ? O2 C11 C14 114.6(4) . . ? C10 C11 C14 123.5(4) . . ? O4 C12 O3 121.8(4) . . ? O4 C12 C10 126.8(5) . . ? O3 C12 C10 111.4(4) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 C15 O5 121.9(4) . . ? O6 C15 C2 124.9(4) . . ? O5 C15 C2 113.1(4) . . ? O5 C16 H16A 109.5 . . ? O5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C17 H17A 109.5 . . ? C1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C19 124.4(5) . . ? N3 C18 H18 117.8 . . ? C19 C18 H18 117.8 . . ? C18 C19 C20 119.8(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C5 C41 C4 122.3(5) . . ? C5 C41 H41 118.8 . . ? C4 C41 H41 118.8 . . ? N4 C20 C21 122.4(4) . . ? N4 C20 C19 122.3(5) . . ? C21 C20 C19 115.2(4) . . ? C22 C21 C20 120.8(5) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? N3 C22 C21 123.8(5) . . ? N3 C22 H22 118.1 . . ? C21 C22 H22 118.1 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 C25 C26 107.2(4) . . ? O7 C25 H25A 110.3 . . ? C26 C25 H25A 110.3 . . ? O7 C25 H25B 110.3 . . ? C26 C25 H25B 110.3 . . ? H25A C25 H25B 108.5 . . ? C25 C26 C27 113.8(4) . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C28 C27 C26 114.5(4) . . ? C28 C27 H27A 108.6 . . ? C26 C27 H27A 108.6 . . ? C28 C27 H27B 108.6 . . ? C26 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C27 C28 C29 112.4(4) . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C30 114.3(4) . . ? C28 C29 H29A 108.7 . . ? C30 C29 H29A 108.7 . . ? C28 C29 H29B 108.7 . . ? C30 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C29 C30 C31 113.4(4) . . ? C29 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? C29 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 113.7(5) . . ? C32 C31 H31A 108.8 . . ? C30 C31 H31A 108.8 . . ? C32 C31 H31B 108.8 . . ? C30 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O8 C33 C34 107.7(4) . . ? O8 C33 H33A 110.2 . . ? C34 C33 H33A 110.2 . . ? O8 C33 H33B 110.2 . . ? C34 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C33 C34 C35 115.0(4) . . ? C33 C34 H34A 108.5 . . ? C35 C34 H34A 108.5 . . ? C33 C34 H34B 108.5 . . ? C35 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? C34 C35 C36 114.6(4) . . ? C34 C35 H35A 108.6 . . ? C36 C35 H35A 108.6 . . ? C34 C35 H35B 108.6 . . ? C36 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C35 111.7(4) . . ? C37 C36 H36A 109.3 . . ? C35 C36 H36A 109.3 . . ? C37 C36 H36B 109.3 . . ? C35 C36 H36B 109.3 . . ? H36A C36 H36B 107.9 . . ? C36 C37 C38 114.7(4) . . ? C36 C37 H37A 108.6 . . ? C38 C37 H37A 108.6 . . ? C36 C37 H37B 108.6 . . ? C38 C37 H37B 108.6 . . ? H37A C37 H37B 107.6 . . ? C39 C38 C37 112.9(4) . . ? C39 C38 H38A 109.0 . . ? C37 C38 H38A 109.0 . . ? C39 C38 H38B 109.0 . . ? C37 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C38 C39 C40 112.6(5) . . ? C38 C39 H39A 109.1 . . ? C40 C39 H39A 109.1 . . ? C38 C39 H39B 109.1 . . ? C40 C39 H39B 109.1 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C3 N1 C4 120.5(4) . . ? C3 N1 Fe1 125.0(3) . . ? C4 N1 Fe1 114.4(3) . . ? C9 N2 C8 120.4(4) . . ? C9 N2 Fe1 126.2(3) . . ? C8 N2 Fe1 113.4(3) . . ? C18 N3 C22 115.9(4) . . ? C18 N3 Fe1 124.1(3) . . ? C22 N3 Fe1 120.0(3) . . ? C20 N4 C23 122.1(4) . . ? C20 N4 C24 120.0(4) . . ? C23 N4 C24 117.9(4) . . ? C1 O1 Fe1 132.7(3) . . ? C11 O2 Fe1 135.1(3) . . ? C12 O3 C13 113.9(4) . . ? C15 O5 C16 116.1(4) . . ? C5 O7 C25 117.4(4) . . ? C6 O8 C33 117.2(4) . . ? O2 Fe1 O1 101.62(14) . . ? O2 Fe1 N1 161.34(14) . . ? O1 Fe1 N1 86.14(14) . . ? O2 Fe1 N2 86.19(14) . . ? O1 Fe1 N2 151.55(14) . . ? N1 Fe1 N2 79.36(15) . . ? O2 Fe1 N3 94.64(14) . . ? O1 Fe1 N3 97.41(14) . . ? N1 Fe1 N3 101.22(15) . . ? N2 Fe1 N3 109.30(15) . . ? 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 O1 C1 C2 C3 8.6(7) . . . . ? C17 C1 C2 C3 -167.5(5) . . . . ? O1 C1 C2 C15 -175.2(4) . . . . ? C17 C1 C2 C15 8.7(7) . . . . ? C1 C2 C3 N1 -9.2(8) . . . . ? C15 C2 C3 N1 174.2(4) . . . . ? O7 C5 C6 O8 0.7(6) . . . . ? C41 C5 C6 O8 -179.3(4) . . . . ? O7 C5 C6 C7 178.3(4) . . . . ? C41 C5 C6 C7 -1.7(6) . . . . ? O8 C6 C7 C8 178.2(4) . . . . ? C5 C6 C7 C8 1.0(7) . . . . ? C6 C7 C8 C4 1.0(7) . . . . ? C6 C7 C8 N2 -178.8(4) . . . . ? C41 C4 C8 C7 -2.1(6) . . . . ? N1 C4 C8 C7 175.4(4) . . . . ? C41 C4 C8 N2 177.7(4) . . . . ? N1 C4 C8 N2 -4.8(6) . . . . ? N2 C9 C10 C11 6.6(7) . . . . ? N2 C9 C10 C12 -175.8(4) . . . . ? C9 C10 C11 O2 -3.0(7) . . . . ? C12 C10 C11 O2 179.4(4) . . . . ? C9 C10 C11 C14 179.6(4) . . . . ? C12 C10 C11 C14 2.0(7) . . . . ? C9 C10 C12 O4 -161.9(5) . . . . ? C11 C10 C12 O4 15.8(7) . . . . ? C9 C10 C12 O3 18.9(6) . . . . ? C11 C10 C12 O3 -163.4(4) . . . . ? C1 C2 C15 O6 -159.0(5) . . . . ? C3 C2 C15 O6 17.6(7) . . . . ? C1 C2 C15 O5 24.0(6) . . . . ? C3 C2 C15 O5 -159.4(4) . . . . ? N3 C18 C19 C20 1.2(7) . . . . ? O7 C5 C41 C4 -179.5(4) . . . . ? C6 C5 C41 C4 0.6(7) . . . . ? C8 C4 C41 C5 1.3(7) . . . . ? N1 C4 C41 C5 -175.9(4) . . . . ? C18 C19 C20 N4 178.9(4) . . . . ? C18 C19 C20 C21 -1.7(7) . . . . ? N4 C20 C21 C22 179.8(5) . . . . ? C19 C20 C21 C22 0.4(7) . . . . ? C20 C21 C22 N3 1.6(8) . . . . ? O7 C25 C26 C27 61.2(5) . . . . ? C25 C26 C27 C28 78.7(6) . . . . ? C26 C27 C28 C29 -177.9(4) . . . . ? C27 C28 C29 C30 -175.5(4) . . . . ? C28 C29 C30 C31 -177.5(5) . . . . ? C29 C30 C31 C32 -64.1(6) . . . . ? O8 C33 C34 C35 -54.4(5) . . . . ? C33 C34 C35 C36 -59.1(6) . . . . ? C34 C35 C36 C37 -176.9(4) . . . . ? C35 C36 C37 C38 -176.6(4) . . . . ? C36 C37 C38 C39 -175.9(4) . . . . ? C37 C38 C39 C40 -175.0(4) . . . . ? C2 C3 N1 C4 176.0(4) . . . . ? C2 C3 N1 Fe1 -8.0(7) . . . . ? C41 C4 N1 C3 5.7(7) . . . . ? C8 C4 N1 C3 -171.6(4) . . . . ? C41 C4 N1 Fe1 -170.6(4) . . . . ? C8 C4 N1 Fe1 12.1(5) . . . . ? C10 C9 N2 C8 178.5(4) . . . . ? C10 C9 N2 Fe1 -3.1(7) . . . . ? C7 C8 N2 C9 -6.3(7) . . . . ? C4 C8 N2 C9 174.0(4) . . . . ? C7 C8 N2 Fe1 175.1(4) . . . . ? C4 C8 N2 Fe1 -4.6(5) . . . . ? C19 C18 N3 C22 0.7(7) . . . . ? C19 C18 N3 Fe1 -178.4(4) . . . . ? C21 C22 N3 C18 -2.1(7) . . . . ? C21 C22 N3 Fe1 177.1(4) . . . . ? C21 C20 N4 C23 -175.8(5) . . . . ? C19 C20 N4 C23 3.5(7) . . . . ? C21 C20 N4 C24 5.4(7) . . . . ? C19 C20 N4 C24 -175.3(5) . . . . ? C2 C1 O1 Fe1 10.6(7) . . . . ? C17 C1 O1 Fe1 -172.9(3) . . . . ? C10 C11 O2 Fe1 -4.2(7) . . . . ? C14 C11 O2 Fe1 173.4(3) . . . . ? O4 C12 O3 C13 -0.6(6) . . . . ? C10 C12 O3 C13 178.6(4) . . . . ? O6 C15 O5 C16 -1.4(7) . . . . ? C2 C15 O5 C16 175.7(4) . . . . ? C41 C5 O7 C25 -6.0(7) . . . . ? C6 C5 O7 C25 173.9(4) . . . . ? C26 C25 O7 C5 179.9(4) . . . . ? C7 C6 O8 C33 8.0(6) . . . . ? C5 C6 O8 C33 -174.6(4) . . . . ? C34 C33 O8 C6 -179.6(4) . . . . ? C11 O2 Fe1 O1 158.2(4) . . . . ? C11 O2 Fe1 N1 44.9(7) . . . . ? C11 O2 Fe1 N2 5.8(4) . . . . ? C11 O2 Fe1 N3 -103.3(4) . . . . ? C1 O1 Fe1 O2 177.3(4) . . . . ? C1 O1 Fe1 N1 -19.8(4) . . . . ? C1 O1 Fe1 N2 -79.0(5) . . . . ? C1 O1 Fe1 N3 81.0(4) . . . . ? C3 N1 Fe1 O2 132.8(5) . . . . ? C4 N1 Fe1 O2 -51.0(6) . . . . ? C3 N1 Fe1 O1 17.3(4) . . . . ? C4 N1 Fe1 O1 -166.6(3) . . . . ? C3 N1 Fe1 N2 172.7(4) . . . . ? C4 N1 Fe1 N2 -11.1(3) . . . . ? C3 N1 Fe1 N3 -79.5(4) . . . . ? C4 N1 Fe1 N3 96.6(3) . . . . ? C9 N2 Fe1 O2 -1.9(4) . . . . ? C8 N2 Fe1 O2 176.6(3) . . . . ? C9 N2 Fe1 O1 -109.4(4) . . . . ? C8 N2 Fe1 O1 69.1(4) . . . . ? C9 N2 Fe1 N1 -170.1(4) . . . . ? C8 N2 Fe1 N1 8.5(3) . . . . ? C9 N2 Fe1 N3 91.6(4) . . . . ? C8 N2 Fe1 N3 -89.8(3) . . . . ? C18 N3 Fe1 O2 154.7(4) . . . . ? C22 N3 Fe1 O2 -24.3(4) . . . . ? C18 N3 Fe1 O1 -102.9(4) . . . . ? C22 N3 Fe1 O1 78.0(4) . . . . ? C18 N3 Fe1 N1 -15.4(4) . . . . ? C22 N3 Fe1 N1 165.5(3) . . . . ? C18 N3 Fe1 N2 67.1(4) . . . . ? C22 N3 Fe1 N2 -111.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.63 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.696 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.077 _iucr_refine_instructions_details ; TITL j31 in P -1 CELL 0.71069 11.9872 12.5380 14.6613 95.394 102.327 106.231 ZERR 2.00 0.0007 0.0008 0.0010 0.005 0.005 0.005 LATT 1 SFAC C H N O FE UNIT 82 120 8 16 2 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 20 TEMP -133.00 WGHT 0.049500 FVAR 0.26452 C1 1 0.098797 0.443411 0.236601 11.00000 0.03238 0.03337 = 0.04955 0.00572 0.01091 0.00546 C2 1 0.073779 0.508632 0.308238 11.00000 0.03526 0.03341 = 0.04086 0.00477 0.00958 0.00863 C3 1 0.136360 0.527348 0.405518 11.00000 0.04054 0.03021 = 0.04967 0.00227 0.01304 0.01266 AFIX 43 H3 2 0.121046 0.581637 0.446761 11.00000 -1.20000 AFIX 0 C4 1 0.274495 0.509509 0.541231 11.00000 0.03580 0.02458 = 0.03373 0.00239 0.00647 0.00480 C5 1 0.322115 0.618538 0.696995 11.00000 0.03135 0.02736 = 0.03788 0.00299 0.01294 0.00566 C6 1 0.418115 0.572223 0.727386 11.00000 0.03356 0.02677 = 0.03484 0.00500 0.00902 0.00371 C7 1 0.436229 0.494553 0.663748 11.00000 0.03002 0.02934 = 0.04528 0.00900 0.00593 0.00808 AFIX 43 H7 2 0.498877 0.462931 0.683961 11.00000 -1.20000 AFIX 0 C8 1 0.366461 0.460740 0.571244 11.00000 0.03069 0.02687 = 0.04429 0.00172 0.01089 0.00399 C9 1 0.467535 0.337053 0.520622 11.00000 0.02993 0.02919 = 0.03941 0.00363 0.00958 0.00449 AFIX 43 H9 2 0.522802 0.364972 0.580796 11.00000 -1.20000 AFIX 0 C10 1 0.490815 0.254104 0.460932 11.00000 0.03454 0.02676 = 0.04551 0.00339 0.01464 0.00941 C11 1 0.423743 0.212607 0.365404 11.00000 0.02987 0.03143 = 0.04510 0.00692 0.01345 0.00588 C12 1 0.592644 0.213226 0.499844 11.00000 0.03626 0.02994 = 0.04286 0.00290 0.01580 0.01011 C13 1 0.722790 0.195640 0.637710 11.00000 0.05701 0.06780 = 0.05109 0.01168 0.00497 0.03539 AFIX 137 H13A 2 0.697086 0.113218 0.623493 11.00000 -1.50000 H13B 2 0.745650 0.219814 0.706433 11.00000 -1.50000 H13C 2 0.791771 0.226443 0.611800 11.00000 -1.50000 AFIX 0 C14 1 0.447880 0.125979 0.301772 11.00000 0.04328 0.03545 = 0.04650 -0.00228 0.01254 0.01065 AFIX 137 H14A 2 0.376721 0.090744 0.249266 11.00000 -1.50000 H14B 2 0.466687 0.068400 0.337648 11.00000 -1.50000 H14C 2 0.516057 0.161995 0.276683 11.00000 -1.50000 AFIX 0 C15 1 -0.014768 0.570918 0.291078 11.00000 0.03753 0.03362 = 0.03878 0.00641 0.00690 0.00673 C16 1 -0.194401 0.579330 0.191531 11.00000 0.03668 0.04987 = 0.05410 0.01594 0.00617 0.01673 AFIX 137 H16A 2 -0.223381 0.587835 0.248608 11.00000 -1.50000 H16B 2 -0.260713 0.531715 0.139498 11.00000 -1.50000 H16C 2 -0.163158 0.653545 0.174244 11.00000 -1.50000 AFIX 0 C17 1 0.051743 0.441182 0.132934 11.00000 0.04674 0.05350 = 0.04588 0.00736 0.00745 0.01861 AFIX 137 H17A 2 0.105118 0.418978 0.098082 11.00000 -1.50000 H17B 2 0.048271 0.516245 0.122026 11.00000 -1.50000 H17C 2 -0.028931 0.386866 0.110907 11.00000 -1.50000 AFIX 0 C18 1 0.026451 0.212455 0.439394 11.00000 0.04177 0.03133 = 0.04541 0.00493 0.00719 0.01529 AFIX 43 H18 2 0.042081 0.282587 0.478365 11.00000 -1.20000 AFIX 0 C19 1 -0.068798 0.123750 0.445793 11.00000 0.04198 0.03902 = 0.04309 0.00666 0.01457 0.01660 AFIX 43 H19 2 -0.117276 0.134277 0.487220 11.00000 -1.20000 AFIX 0 C41 1 0.254592 0.586601 0.606031 11.00000 0.02933 0.02946 = 0.04373 0.00677 0.00588 0.00641 AFIX 43 H41 2 0.191655 0.617909 0.585927 11.00000 -1.20000 AFIX 0 C20 1 -0.093962 0.017537 0.390731 11.00000 0.03335 0.03138 = 0.05258 0.00572 0.01291 0.01177 C21 1 -0.019196 0.012405 0.330478 11.00000 0.04225 0.03071 = 0.05480 -0.00156 0.00800 0.00535 AFIX 43 H21 2 -0.031590 -0.056612 0.291046 11.00000 -1.20000 AFIX 0 C22 1 0.072120 0.105924 0.327470 11.00000 0.03574 0.03856 = 0.04878 -0.00035 0.01689 0.00628 AFIX 43 H22 2 0.119633 0.099268 0.284300 11.00000 -1.20000 AFIX 0 C23 1 -0.266997 -0.065250 0.453040 11.00000 0.04906 0.03776 = 0.07655 0.01334 0.02384 0.01270 AFIX 137 H23A 2 -0.224126 -0.050565 0.520037 11.00000 -1.50000 H23B 2 -0.332642 -0.136284 0.439686 11.00000 -1.50000 H23C 2 -0.299821 -0.003678 0.438632 11.00000 -1.50000 AFIX 0 C24 1 -0.201574 -0.182955 0.342175 11.00000 0.04038 0.03409 = 0.07558 0.00381 0.00931 0.00575 AFIX 137 H24A 2 -0.231799 -0.183142 0.274535 11.00000 -1.50000 H24B 2 -0.259395 -0.241097 0.363364 11.00000 -1.50000 H24C 2 -0.124513 -0.198500 0.352933 11.00000 -1.50000 AFIX 0 C25 1 0.222325 0.749662 0.736326 11.00000 0.03529 0.03530 = 0.04619 0.00450 0.00492 0.01387 AFIX 23 H25A 2 0.141354 0.694880 0.710073 11.00000 -1.20000 H25B 2 0.243637 0.794905 0.687203 11.00000 -1.20000 AFIX 0 C26 1 0.224016 0.824850 0.822961 11.00000 0.03776 0.04641 = 0.04941 0.00817 0.01058 0.01983 AFIX 23 H26A 2 0.201917 0.777769 0.870790 11.00000 -1.20000 H26B 2 0.162388 0.863122 0.805971 11.00000 -1.20000 AFIX 0 C27 1 0.345479 0.914046 0.867110 11.00000 0.05007 0.04129 = 0.04424 0.00200 0.00917 0.01816 AFIX 23 H27A 2 0.348921 0.940615 0.933711 11.00000 -1.20000 H27B 2 0.409605 0.878456 0.867586 11.00000 -1.20000 AFIX 0 C28 1 0.371123 1.015279 0.816683 11.00000 0.04873 0.04648 = 0.04277 0.00216 0.00446 0.02297 AFIX 23 H28A 2 0.309330 1.053325 0.818407 11.00000 -1.20000 H28B 2 0.365505 0.989164 0.749521 11.00000 -1.20000 AFIX 0 C29 1 0.495508 1.099946 0.861463 11.00000 0.04943 0.04050 = 0.04620 0.00176 0.00590 0.01946 AFIX 23 H29A 2 0.557084 1.062949 0.855310 11.00000 -1.20000 H29B 2 0.503056 1.120697 0.929845 11.00000 -1.20000 AFIX 0 C30 1 0.521623 1.207942 0.817636 11.00000 0.05082 0.04869 = 0.05640 0.00970 0.01024 0.02426 AFIX 23 H30A 2 0.462464 1.246997 0.826357 11.00000 -1.20000 H30B 2 0.510900 1.187281 0.748761 11.00000 -1.20000 AFIX 0 C31 1 0.648748 1.289499 0.860670 11.00000 0.04892 0.04609 = 0.06387 0.00693 0.01107 0.01985 AFIX 23 H31A 2 0.707821 1.249867 0.853171 11.00000 -1.20000 H31B 2 0.661777 1.353147 0.824908 11.00000 -1.20000 AFIX 0 C32 1 0.671736 1.335869 0.964668 11.00000 0.05485 0.04073 = 0.06253 0.00843 0.00418 0.01199 AFIX 137 H32A 2 0.612445 1.373724 0.973049 11.00000 -1.50000 H32B 2 0.752576 1.389875 0.986764 11.00000 -1.50000 H32C 2 0.665031 1.273952 1.001349 11.00000 -1.50000 AFIX 0 C33 1 0.583441 0.571850 0.851171 11.00000 0.03247 0.03382 = 0.05139 0.00741 0.00782 0.00997 AFIX 23 H33A 2 0.643212 0.598991 0.814532 11.00000 -1.20000 H33B 2 0.560104 0.488611 0.842260 11.00000 -1.20000 AFIX 0 C34 1 0.636072 0.620392 0.954512 11.00000 0.03616 0.03940 = 0.04714 0.00914 0.00845 0.01218 AFIX 23 H34A 2 0.710712 0.600673 0.976284 11.00000 -1.20000 H34B 2 0.578890 0.584264 0.990543 11.00000 -1.20000 AFIX 0 C35 1 0.664827 0.747313 0.978148 11.00000 0.03522 0.04841 = 0.03898 0.00608 0.00903 0.01303 AFIX 23 H35A 2 0.697653 0.770398 1.047404 11.00000 -1.20000 H35B 2 0.589215 0.766593 0.960852 11.00000 -1.20000 AFIX 0 C36 1 0.753922 0.815036 0.928708 11.00000 0.04336 0.04008 = 0.04495 0.00426 0.00963 0.01182 AFIX 23 H36A 2 0.828620 0.793830 0.943204 11.00000 -1.20000 H36B 2 0.719563 0.796300 0.859385 11.00000 -1.20000 AFIX 0 C37 1 0.783555 0.940711 0.959661 11.00000 0.03366 0.04647 = 0.04995 0.00421 0.01099 0.01120 AFIX 23 H37A 2 0.821571 0.959030 1.028482 11.00000 -1.20000 H37B 2 0.707701 0.960077 0.949142 11.00000 -1.20000 AFIX 0 C38 1 0.866614 1.014219 0.908807 11.00000 0.03608 0.04504 = 0.04640 0.00856 0.00640 0.01235 AFIX 23 H38A 2 0.940485 0.991798 0.915448 11.00000 -1.20000 H38B 2 0.826326 1.000759 0.840527 11.00000 -1.20000 AFIX 0 C39 1 0.901077 1.139533 0.947076 11.00000 0.04323 0.04360 = 0.05774 0.00764 0.01050 0.01115 AFIX 23 H39A 2 0.947839 1.154138 1.013823 11.00000 -1.20000 H39B 2 0.827138 1.160594 0.945744 11.00000 -1.20000 AFIX 0 C40 1 0.975106 1.213230 0.890329 11.00000 0.05956 0.04789 = 0.06480 0.01401 0.01465 0.01665 AFIX 137 H40A 2 1.049855 1.194693 0.893309 11.00000 -1.50000 H40B 2 0.993894 1.292700 0.917038 11.00000 -1.50000 H40C 2 0.929048 1.199564 0.824245 11.00000 -1.50000 AFIX 0 N1 3 0.212942 0.477240 0.443886 11.00000 0.03338 0.02873 = 0.04334 0.00617 0.00859 0.00729 N2 3 0.378943 0.379042 0.502047 11.00000 0.02911 0.02509 = 0.05347 0.00313 0.01508 0.00750 N3 3 0.098093 0.206269 0.382081 11.00000 0.03319 0.03523 = 0.04128 -0.00031 0.01049 0.01003 N4 3 -0.185216 -0.072936 0.395330 11.00000 0.04076 0.02942 = 0.06483 0.00622 0.01642 0.01133 O1 4 0.169969 0.384815 0.254809 11.00000 0.05006 0.04129 = 0.04846 0.00127 0.01074 0.01923 O2 4 0.334218 0.244482 0.328441 11.00000 0.03577 0.03745 = 0.04473 0.00217 0.00955 0.00800 O3 4 0.625445 0.236033 0.595623 11.00000 0.04137 0.06043 = 0.04931 0.00456 0.00664 0.02464 O4 4 0.642604 0.164250 0.455477 11.00000 0.05173 0.05100 = 0.05418 0.00942 0.01752 0.02718 O5 4 -0.100471 0.527847 0.209483 11.00000 0.03924 0.04526 = 0.04703 0.00643 0.00526 0.01397 O6 4 -0.015799 0.649871 0.345166 11.00000 0.04414 0.04441 = 0.05397 -0.00200 0.00275 0.01780 O7 4 0.308633 0.691868 0.764625 11.00000 0.03647 0.03795 = 0.04225 0.00231 0.00417 0.01595 O8 4 0.479615 0.607758 0.819169 11.00000 0.03750 0.03814 = 0.03878 -0.00047 0.00586 0.01346 FE1 5 0.247273 0.342287 0.375100 11.00000 0.03218 0.03044 = 0.04242 0.00275 0.00697 0.00826 HKLF 4 REM j31 in P -1 REM R1 = 0.0632 for 3594 Fo > 4sig(Fo) and 0.1335 for all 6827 data REM 495 parameters refined using 0 restraints END WGHT 0.0495 0.0000 REM Highest difference peak 0.696, deepest hole -0.257, 1-sigma level 0.077 Q1 1 0.2639 0.3744 0.4612 11.00000 0.05 0.70 Q2 1 0.2358 0.3199 0.2899 11.00000 0.05 0.66 Q3 1 0.2573 0.4365 0.3979 11.00000 0.05 0.49 Q4 1 0.2385 0.4226 0.4118 11.00000 0.05 0.47 Q5 1 0.3543 0.3635 0.4295 11.00000 0.05 0.46 Q6 1 0.3397 0.3338 0.3565 11.00000 0.05 0.43 Q7 1 0.3449 0.3244 0.3763 11.00000 0.05 0.43 Q8 1 0.1431 0.3407 0.3302 11.00000 0.05 0.38 Q9 1 0.4759 0.3158 0.4379 11.00000 0.05 0.31 Q10 1 0.3749 0.4294 0.5173 11.00000 0.05 0.27 Q11 1 0.3240 0.6057 0.7684 11.00000 0.05 0.27 Q12 1 -0.1029 0.5845 0.2687 11.00000 0.05 0.26 Q13 1 0.2719 0.5391 0.6213 11.00000 0.05 0.26 Q14 1 0.1779 0.4776 0.4003 11.00000 0.05 0.26 Q15 1 0.4312 0.5173 0.7357 11.00000 0.05 0.25 Q16 1 0.2212 0.4766 0.4660 11.00000 0.05 0.25 Q17 1 -0.0228 0.5007 0.1690 11.00000 0.05 0.25 Q18 1 0.4210 0.5714 0.6721 11.00000 0.05 0.25 Q19 1 -0.0155 0.6253 0.4126 11.00000 0.05 0.24 Q20 1 0.3080 0.4765 0.4916 11.00000 0.05 0.24 ; _database_code_depnum_ccdc_archive 'CCDC 944435' ####################################################################### # # 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_w022 # start Validation Reply Form _vrf_PLAT232_w022 ; PROBLEM: Hirshfeld Test Diff (M-X) Fe1 -- N4 .. 11.9 su RESPONSE: At the temperature of the measurement the spin transition of the iron centre is not 100% complete. This could be responsible for a higher motion of the nitrogen N4. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe12i(C8)(dmap)2 _chemical_melting_point ? _chemical_formula_moiety 'C48 H70 Fe N6 O8, C H4 O' _chemical_formula_sum 'C49 H74 Fe N6 O9' _chemical_formula_weight 946.99 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' Fe Fe 0.3463 0.8444 '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' _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 11.9287(5) _cell_length_b 13.1406(5) _cell_length_c 17.0569(7) _cell_angle_alpha 103.154(3) _cell_angle_beta 100.508(3) _cell_angle_gamma 100.246(3) _cell_volume 2491.75(17) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 27028 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 50.42 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.362 _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 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDSII _diffrn_measurement_method Omega-Scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30301 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 24.57 _reflns_number_total 8344 _reflns_number_gt 6388 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-AREA-STOE _computing_cell_refinement X-AREA-STOE _computing_data_reduction X-AREA-STOE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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^)+(0.0589P)^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 8344 _refine_ls_number_parameters 693 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _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 0.69830(2) 0.79683(2) 0.288135(17) 0.03220(10) Uani 1 1 d . . . O1 O 0.77631(12) 0.94849(11) 0.31284(8) 0.0374(3) Uani 1 1 d . A . O2 O 0.77894(12) 0.78702(11) 0.39531(8) 0.0358(3) Uani 1 1 d . . . O3 O 0.77349(17) 1.14006(13) 0.14507(11) 0.0655(5) Uani 1 1 d . A . O4 O 0.65864(15) 0.99848(11) 0.04772(9) 0.0479(4) Uani 1 1 d . A . O5 O 0.67423(14) 0.41143(12) 0.36155(9) 0.0472(4) Uani 1 1 d . . . O6 O 0.83884(13) 0.50879(11) 0.45080(9) 0.0423(4) Uani 1 1 d . . . O7 O 0.30197(12) 0.55307(10) -0.04851(8) 0.0359(3) Uani 1 1 d . A . O8 O 0.29667(13) 0.40495(11) 0.03041(9) 0.0445(4) Uani 1 1 d . . . N1 N 0.61649(14) 0.79689(12) 0.18099(10) 0.0312(4) Uani 1 1 d . A . N2 N 0.61846(14) 0.64856(13) 0.25672(9) 0.0311(4) Uani 1 1 d . . . N3 N 0.83708(14) 0.76020(12) 0.24584(10) 0.0338(4) Uani 1 1 d . . . N4 N 0.56749(15) 0.83892(13) 0.33893(10) 0.0369(4) Uani 1 1 d . . . N5 N 1.12921(15) 0.68353(14) 0.16080(11) 0.0412(4) Uani 1 1 d . . . N6 N 0.31089(17) 0.93658(15) 0.45911(12) 0.0484(5) Uani 1 1 d . . . C1 C 0.78933(18) 0.70361(16) 0.41842(12) 0.0348(5) Uani 1 1 d . . . C2 C 0.72638(17) 0.59778(16) 0.37139(12) 0.0334(4) Uani 1 1 d . . . C3 C 0.64099(17) 0.57810(16) 0.29562(12) 0.0328(4) Uani 1 1 d . . . H3 H 0.5966 0.5064 0.2716 0.039 Uiso 1 1 calc R . . C4 C 0.53363(16) 0.61881(15) 0.18004(11) 0.0306(4) Uani 1 1 d . A . C5 C 0.45509(17) 0.51846(15) 0.14430(12) 0.0324(4) Uani 1 1 d . . . H5 H 0.4541 0.4639 0.1726 0.039 Uiso 1 1 calc R A . C6 C 0.37950(17) 0.49895(15) 0.06831(12) 0.0327(4) Uani 1 1 d . A . C7 C 0.38057(17) 0.57847(16) 0.02606(11) 0.0320(4) Uani 1 1 d . . . C8 C 0.45699(17) 0.67764(16) 0.06184(12) 0.0344(5) Uani 1 1 d . A . H8 H 0.4571 0.7323 0.0338 0.041 Uiso 1 1 calc R . . C9 C 0.53411(16) 0.69819(15) 0.13901(11) 0.0306(4) Uani 1 1 d . . . C10 C 0.63389(17) 0.87367(15) 0.14499(12) 0.0332(4) Uani 1 1 d . . . H10 H 0.5910 0.8597 0.0895 0.040 Uiso 1 1 calc R A . C11 C 0.71097(18) 0.97641(15) 0.18075(12) 0.0360(5) Uani 1 1 d . A . C12 C 0.77726(18) 1.00912(16) 0.26473(13) 0.0383(5) Uani 1 1 d . . . C13 C 0.8727(2) 0.72636(18) 0.50192(13) 0.0490(6) Uani 1 1 d . . . H13A H 0.8884 0.8029 0.5304 0.074 Uiso 1 1 calc R . . H13B H 0.9463 0.7069 0.4942 0.074 Uiso 1 1 calc R . . H13C H 0.8373 0.6840 0.5353 0.074 Uiso 1 1 calc R . . C14 C 0.74105(18) 0.49971(17) 0.39322(12) 0.0367(5) Uani 1 1 d . . . C15 C 0.8560(2) 0.40997(18) 0.46826(14) 0.0488(6) Uani 1 1 d . . . H15A H 0.8704 0.3629 0.4194 0.073 Uiso 1 1 calc R . . H15B H 0.7858 0.3743 0.4822 0.073 Uiso 1 1 calc R . . H15C H 0.9235 0.4252 0.5150 0.073 Uiso 1 1 calc R . . C16 C 0.8534(2) 1.12088(18) 0.30278(15) 0.0542(6) Uani 1 1 d . A . H16A H 0.8981 1.1255 0.3582 0.081 Uiso 1 1 calc R . . H16B H 0.8040 1.1731 0.3068 0.081 Uiso 1 1 calc R . . H16C H 0.9077 1.1366 0.2680 0.081 Uiso 1 1 calc R . . C17 C 0.7203(2) 1.04769(17) 0.12746(14) 0.0426(5) Uani 1 1 d . . . C18 C 0.6592(3) 1.0633(2) -0.00879(15) 0.0613(7) Uani 1 1 d . . . H18A H 0.7402 1.0968 -0.0070 0.092 Uiso 1 1 calc R A . H18B H 0.6167 1.1192 0.0067 0.092 Uiso 1 1 calc R . . H18C H 0.6211 1.0184 -0.0649 0.092 Uiso 1 1 calc R . . C19 C 0.31074(19) 0.63151(17) -0.09501(13) 0.0389(5) Uani 1 1 d . . . H19A H 0.3901 0.6463 -0.1056 0.047 Uiso 1 1 calc R A . H19B H 0.2975 0.6995 -0.0630 0.047 Uiso 1 1 calc R . . C20 C 0.22019(18) 0.58905(17) -0.17605(12) 0.0372(5) Uani 1 1 d . A . H20A H 0.2220 0.5136 -0.2005 0.045 Uiso 1 1 calc R . . H20B H 0.2422 0.6310 -0.2146 0.045 Uiso 1 1 calc R . . C21 C 0.09641(18) 0.59320(16) -0.16955(12) 0.0368(5) Uani 1 1 d . . . H21A H 0.0933 0.6687 -0.1466 0.044 Uiso 1 1 calc R A . H21B H 0.0740 0.5521 -0.1307 0.044 Uiso 1 1 calc R . . C22 C 0.00910(18) 0.54763(18) -0.25251(13) 0.0413(5) Uani 1 1 d . A . H22A H 0.0321 0.5889 -0.2912 0.050 Uiso 1 1 calc R . . H22B H 0.0130 0.4724 -0.2754 0.050 Uiso 1 1 calc R . . C23 C -0.11614(18) 0.55025(18) -0.24836(13) 0.0412(5) Uani 1 1 d . . . H23A H -0.1192 0.6248 -0.2221 0.049 Uiso 1 1 calc R A . H23B H -0.1410 0.5050 -0.2127 0.049 Uiso 1 1 calc R . . C24 C -0.20216(19) 0.51116(19) -0.33253(13) 0.0446(5) Uani 1 1 d . A . H24A H -0.1777 0.5570 -0.3679 0.053 Uiso 1 1 calc R . . H24B H -0.1982 0.4370 -0.3590 0.053 Uiso 1 1 calc R . . C25 C -0.32811(19) 0.5122(2) -0.32901(13) 0.0474(6) Uani 1 1 d . . . H25A H -0.3306 0.5823 -0.2935 0.057 Uiso 1 1 calc R A . H25B H -0.3582 0.4558 -0.3034 0.057 Uiso 1 1 calc R . . C26 C -0.4073(2) 0.4932(2) -0.41433(14) 0.0544(6) Uani 1 1 d . A . H26A H -0.4044 0.4242 -0.4500 0.082 Uiso 1 1 calc R . . H26B H -0.3804 0.5511 -0.4388 0.082 Uiso 1 1 calc R . . H26C H -0.4879 0.4921 -0.4091 0.082 Uiso 1 1 calc R . . C27A C 0.2711(4) 0.3343(4) 0.0882(3) 0.0417(11) Uani 0.50 1 d P A 1 H27A H 0.3311 0.2917 0.0943 0.050 Uiso 0.50 1 calc PR A 1 H27B H 0.2737 0.3800 0.1437 0.050 Uiso 0.50 1 calc PR A 1 C28A C 0.1500(10) 0.2593(11) 0.0520(10) 0.044(3) Uani 0.50 1 d P A 1 H28A H 0.1263 0.2286 0.0960 0.053 Uiso 0.50 1 calc PR A 1 H28B H 0.0940 0.3030 0.0374 0.053 Uiso 0.50 1 calc PR A 1 C29A C 0.1377(7) 0.1689(5) -0.0223(5) 0.0391(16) Uani 0.50 1 d P A 1 H29A H 0.1816 0.1170 -0.0057 0.047 Uiso 0.50 1 calc PR A 1 H29B H 0.1738 0.1974 -0.0631 0.047 Uiso 0.50 1 calc PR A 1 C30A C 0.0110(8) 0.1099(7) -0.0637(6) 0.0391(19) Uani 0.50 1 d P A 1 H30A H -0.0245 0.0798 -0.0233 0.047 Uiso 0.50 1 calc PR A 1 H30B H -0.0334 0.1622 -0.0790 0.047 Uiso 0.50 1 calc PR A 1 C31A C -0.0020(6) 0.0196(6) -0.1406(5) 0.0403(16) Uani 0.50 1 d P A 1 H31A H 0.0389 -0.0346 -0.1249 0.048 Uiso 0.50 1 calc PR A 1 H31B H 0.0369 0.0489 -0.1799 0.048 Uiso 0.50 1 calc PR A 1 C32A C -0.1285(7) -0.0354(6) -0.1840(5) 0.0392(16) Uani 0.50 1 d P A 1 H32A H -0.1689 0.0182 -0.2015 0.047 Uiso 0.50 1 calc PR A 1 H32B H -0.1682 -0.0629 -0.1444 0.047 Uiso 0.50 1 calc PR A 1 C33A C -0.1399(6) -0.1286(6) -0.2600(5) 0.0475(15) Uani 0.50 1 d P A 1 H33A H -0.1043 -0.1006 -0.3012 0.057 Uiso 0.50 1 calc PR A 1 H33B H -0.0961 -0.1804 -0.2432 0.057 Uiso 0.50 1 calc PR A 1 C34A C -0.2665(5) -0.1859(5) -0.2996(4) 0.0537(14) Uani 0.50 1 d P A 1 H34A H -0.2998 -0.2198 -0.2608 0.081 Uiso 0.50 1 calc PR A 1 H34B H -0.2704 -0.2410 -0.3502 0.081 Uiso 0.50 1 calc PR A 1 H34C H -0.3112 -0.1340 -0.3133 0.081 Uiso 0.50 1 calc PR A 1 C27B C 0.3254(4) 0.3087(3) 0.0418(3) 0.0352(9) Uani 0.50 1 d P A 2 H27C H 0.4080 0.3226 0.0722 0.042 Uiso 0.50 1 calc PR A 2 H27D H 0.3139 0.2558 -0.0122 0.042 Uiso 0.50 1 calc PR A 2 C28B C 0.2441(4) 0.2677(5) 0.0912(3) 0.0392(10) Uani 0.50 1 d P A 2 H28C H 0.2516 0.3255 0.1419 0.047 Uiso 0.50 1 calc PR A 2 H28D H 0.2700 0.2072 0.1089 0.047 Uiso 0.50 1 calc PR A 2 C29B C 0.1149(11) 0.2297(10) 0.0461(9) 0.042(2) Uani 0.50 1 d P A 2 H29C H 0.0884 0.2897 0.0282 0.050 Uiso 0.50 1 calc PR A 2 H29D H 0.0684 0.2101 0.0852 0.050 Uiso 0.50 1 calc PR A 2 C30B C 0.0904(8) 0.1314(6) -0.0310(5) 0.0417(17) Uani 0.50 1 d P A 2 H30C H 0.1302 0.1538 -0.0724 0.050 Uiso 0.50 1 calc PR A 2 H30D H 0.1254 0.0747 -0.0139 0.050 Uiso 0.50 1 calc PR A 2 C31B C -0.0375(8) 0.0844(8) -0.0714(7) 0.046(2) Uani 0.50 1 d P A 2 H31C H -0.0739 0.1419 -0.0856 0.056 Uiso 0.50 1 calc PR A 2 H31D H -0.0766 0.0575 -0.0312 0.056 Uiso 0.50 1 calc PR A 2 C32B C -0.0586(7) -0.0068(6) -0.1493(5) 0.0460(19) Uani 0.50 1 d P A 2 H32C H -0.0198 0.0210 -0.1893 0.055 Uiso 0.50 1 calc PR A 2 H32D H -0.0202 -0.0630 -0.1349 0.055 Uiso 0.50 1 calc PR A 2 C33B C -0.1854(7) -0.0584(7) -0.1919(6) 0.059(2) Uani 0.50 1 d P A 2 H33C H -0.2231 -0.0044 -0.2113 0.070 Uiso 0.50 1 calc PR A 2 H33D H -0.2265 -0.0823 -0.1516 0.070 Uiso 0.50 1 calc PR A 2 C34B C -0.1983(7) -0.1535(6) -0.2650(5) 0.060(2) Uani 0.50 1 d P A 2 H34D H -0.1616 -0.1294 -0.3065 0.090 Uiso 0.50 1 calc PR A 2 H34E H -0.2817 -0.1858 -0.2894 0.090 Uiso 0.50 1 calc PR A 2 H34F H -0.1601 -0.2067 -0.2463 0.090 Uiso 0.50 1 calc PR A 2 C35 C 0.52093(19) 0.78611(17) 0.38873(12) 0.0396(5) Uani 1 1 d . . . H35 H 0.5483 0.7248 0.3967 0.047 Uiso 1 1 calc R . . C36 C 0.43709(19) 0.81456(17) 0.42853(13) 0.0413(5) Uani 1 1 d . . . H36 H 0.4085 0.7731 0.4627 0.050 Uiso 1 1 calc R . . C37 C 0.39280(19) 0.90434(17) 0.41956(12) 0.0403(5) Uani 1 1 d . . . C38 C 0.43976(19) 0.95870(17) 0.36616(13) 0.0416(5) Uani 1 1 d . . . H38 H 0.4133 1.0195 0.3560 0.050 Uiso 1 1 calc R . . C39 C 0.52354(19) 0.92357(17) 0.32913(13) 0.0400(5) Uani 1 1 d . . . H39 H 0.5530 0.9622 0.2936 0.048 Uiso 1 1 calc R . . C40 C 0.2596(2) 0.8743(2) 0.50893(16) 0.0596(7) Uani 1 1 d . . . H40A H 0.3220 0.8590 0.5474 0.089 Uiso 1 1 calc R . . H40B H 0.2087 0.8067 0.4728 0.089 Uiso 1 1 calc R . . H40C H 0.2133 0.9151 0.5403 0.089 Uiso 1 1 calc R . . C41 C 0.2625(2) 1.02610(19) 0.44583(15) 0.0528(6) Uani 1 1 d . . . H41A H 0.2070 1.0043 0.3918 0.079 Uiso 1 1 calc R . . H41B H 0.3258 1.0858 0.4473 0.079 Uiso 1 1 calc R . . H41C H 0.2218 1.0489 0.4894 0.079 Uiso 1 1 calc R . . C42 C 0.82693(18) 0.69022(15) 0.17190(12) 0.0332(4) Uani 1 1 d . . . H42 H 0.7503 0.6574 0.1386 0.040 Uiso 1 1 calc R . . C43 C 0.91986(17) 0.66355(15) 0.14180(12) 0.0335(4) Uani 1 1 d . . . H43 H 0.9059 0.6142 0.0889 0.040 Uiso 1 1 calc R . . C44 C 1.03521(18) 0.70822(16) 0.18802(12) 0.0352(5) Uani 1 1 d . . . C45 C 1.04592(18) 0.78087(16) 0.26586(13) 0.0387(5) Uani 1 1 d . . . H45 H 1.1212 0.8138 0.3012 0.046 Uiso 1 1 calc R . . C46 C 0.94775(18) 0.80365(16) 0.29022(13) 0.0387(5) Uani 1 1 d . . . H46 H 0.9586 0.8539 0.3423 0.046 Uiso 1 1 calc R . . C47 C 1.1163(2) 0.61703(19) 0.07745(13) 0.0459(5) Uani 1 1 d . . . H47A H 1.0727 0.5442 0.0720 0.069 Uiso 1 1 calc R . . H47B H 1.1940 0.6145 0.0669 0.069 Uiso 1 1 calc R . . H47C H 1.0736 0.6476 0.0373 0.069 Uiso 1 1 calc R . . C48 C 1.24717(19) 0.7308(2) 0.21023(15) 0.0539(6) Uani 1 1 d . . . H48A H 1.2533 0.7186 0.2653 0.081 Uiso 1 1 calc R . . H48B H 1.2654 0.8082 0.2157 0.081 Uiso 1 1 calc R . . H48C H 1.3026 0.6978 0.1832 0.081 Uiso 1 1 calc R . . O31A O 0.5412(10) 0.2028(9) 0.3275(8) 0.106(5) Uani 0.228(5) 1 d P B 3 H31E H 0.4841 0.2219 0.3442 0.159 Uiso 0.228(5) 1 calc PR B 3 C99A C 0.5188(16) 0.1819(16) 0.2433(10) 0.067(5) Uani 0.228(5) 1 d P B 3 H99A H 0.4706 0.2292 0.2252 0.100 Uiso 0.228(5) 1 calc PR B 3 H99B H 0.4768 0.1069 0.2183 0.100 Uiso 0.228(5) 1 calc PR B 3 H99C H 0.5929 0.1947 0.2261 0.100 Uiso 0.228(5) 1 calc PR B 3 O31B O 0.4959(2) 0.29561(18) 0.22645(15) 0.0648(9) Uani 0.772(5) 1 d P B 4 H31F H 0.5509 0.3341 0.2659 0.097 Uiso 0.772(5) 1 calc PR B 4 C99B C 0.5169(5) 0.1930(4) 0.2020(4) 0.0744(15) Uani 0.772(5) 1 d P B 4 H99D H 0.6010 0.1969 0.2182 0.112 Uiso 0.772(5) 1 calc PR B 4 H99E H 0.4898 0.1649 0.1417 0.112 Uiso 0.772(5) 1 calc PR B 4 H99F H 0.4745 0.1452 0.2287 0.112 Uiso 0.772(5) 1 calc PR B 4 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 0.03104(17) 0.03130(16) 0.03032(16) 0.00307(11) 0.00646(12) 0.00450(12) O1 0.0368(8) 0.0345(8) 0.0334(7) -0.0014(6) 0.0080(6) 0.0026(6) O2 0.0366(8) 0.0323(7) 0.0324(7) -0.0006(6) 0.0058(6) 0.0069(6) O3 0.0884(14) 0.0356(9) 0.0562(10) 0.0104(8) 0.0061(9) -0.0135(9) O4 0.0640(10) 0.0323(8) 0.0421(8) 0.0100(7) 0.0070(7) 0.0032(7) O5 0.0499(10) 0.0379(9) 0.0468(9) 0.0108(7) 0.0012(7) 0.0033(7) O6 0.0438(9) 0.0377(8) 0.0415(8) 0.0092(6) 0.0007(7) 0.0108(7) O7 0.0353(8) 0.0327(7) 0.0315(7) 0.0043(6) 0.0004(6) 0.0001(6) O8 0.0437(9) 0.0287(7) 0.0469(8) 0.0050(6) -0.0075(7) -0.0025(6) N1 0.0266(9) 0.0277(8) 0.0343(9) 0.0017(7) 0.0072(7) 0.0015(7) N2 0.0297(9) 0.0344(9) 0.0266(8) 0.0027(7) 0.0066(7) 0.0080(7) N3 0.0363(10) 0.0294(8) 0.0306(8) 0.0022(7) 0.0074(7) 0.0026(7) N4 0.0359(10) 0.0347(9) 0.0329(9) 0.0036(7) 0.0029(7) 0.0021(8) N5 0.0314(10) 0.0454(10) 0.0389(10) -0.0009(8) 0.0065(8) 0.0061(8) N6 0.0493(12) 0.0496(11) 0.0465(11) 0.0059(9) 0.0177(9) 0.0141(9) C1 0.0341(11) 0.0365(11) 0.0314(10) 0.0031(9) 0.0084(9) 0.0088(9) C2 0.0332(11) 0.0343(11) 0.0306(10) 0.0061(8) 0.0067(8) 0.0072(9) C3 0.0317(11) 0.0301(10) 0.0333(10) 0.0036(8) 0.0081(8) 0.0044(8) C4 0.0272(10) 0.0302(10) 0.0310(10) 0.0023(8) 0.0072(8) 0.0052(8) C5 0.0309(11) 0.0304(10) 0.0335(10) 0.0060(8) 0.0080(8) 0.0041(8) C6 0.0291(10) 0.0270(10) 0.0352(10) 0.0014(8) 0.0041(8) 0.0016(8) C7 0.0271(10) 0.0354(11) 0.0284(10) 0.0020(8) 0.0048(8) 0.0040(8) C8 0.0322(11) 0.0334(11) 0.0349(11) 0.0080(8) 0.0059(9) 0.0040(9) C9 0.0280(10) 0.0282(10) 0.0309(10) 0.0014(8) 0.0065(8) 0.0030(8) C10 0.0300(11) 0.0323(11) 0.0339(10) 0.0044(9) 0.0068(8) 0.0053(8) C11 0.0367(11) 0.0284(10) 0.0395(11) 0.0038(9) 0.0107(9) 0.0041(9) C12 0.0350(12) 0.0324(11) 0.0411(12) 0.0000(9) 0.0115(9) 0.0011(9) C13 0.0578(15) 0.0397(12) 0.0385(12) -0.0006(10) -0.0031(11) 0.0120(11) C14 0.0362(12) 0.0400(12) 0.0310(10) 0.0051(9) 0.0077(9) 0.0072(10) C15 0.0594(15) 0.0419(12) 0.0459(13) 0.0146(10) 0.0050(11) 0.0169(11) C16 0.0627(16) 0.0388(12) 0.0447(13) -0.0021(10) 0.0085(12) -0.0090(11) C17 0.0443(13) 0.0346(12) 0.0443(12) 0.0041(10) 0.0130(10) 0.0027(10) C18 0.086(2) 0.0444(14) 0.0500(14) 0.0198(11) 0.0090(13) 0.0035(13) C19 0.0376(12) 0.0363(11) 0.0372(11) 0.0085(9) 0.0043(9) 0.0009(9) C20 0.0373(12) 0.0366(11) 0.0318(10) 0.0049(9) 0.0039(9) 0.0033(9) C21 0.0386(12) 0.0339(11) 0.0329(10) 0.0040(8) 0.0038(9) 0.0061(9) C22 0.0398(12) 0.0454(12) 0.0343(11) 0.0071(9) 0.0044(9) 0.0077(10) C23 0.0387(12) 0.0452(12) 0.0357(11) 0.0078(9) 0.0044(9) 0.0078(10) C24 0.0407(13) 0.0535(14) 0.0362(11) 0.0111(10) 0.0051(10) 0.0078(10) C25 0.0384(13) 0.0583(14) 0.0400(12) 0.0096(10) 0.0028(10) 0.0081(11) C26 0.0417(14) 0.0703(17) 0.0450(13) 0.0121(12) 0.0014(11) 0.0104(12) C27A 0.044(3) 0.032(3) 0.041(3) 0.014(2) 0.003(2) -0.007(2) C28A 0.044(8) 0.045(6) 0.044(4) 0.012(4) 0.018(5) 0.003(4) C29A 0.045(5) 0.029(4) 0.040(3) 0.011(3) 0.005(3) 0.002(3) C30A 0.044(6) 0.029(4) 0.036(3) 0.005(3) 0.006(5) -0.003(4) C31A 0.042(4) 0.036(4) 0.041(3) 0.012(3) 0.007(4) 0.006(3) C32A 0.041(5) 0.034(4) 0.032(3) 0.001(3) 0.002(4) -0.001(4) C33A 0.043(4) 0.046(4) 0.045(3) 0.003(3) 0.010(3) 0.001(3) C34A 0.047(4) 0.051(3) 0.048(3) 0.001(3) 0.006(3) -0.003(3) C27B 0.036(2) 0.029(2) 0.037(2) 0.0033(17) 0.009(2) 0.0042(18) C28B 0.036(3) 0.039(3) 0.039(2) 0.008(2) 0.008(2) 0.003(2) C29B 0.036(6) 0.051(7) 0.043(4) 0.018(5) 0.015(4) 0.012(4) C30B 0.048(6) 0.031(4) 0.041(4) 0.006(3) 0.011(4) 0.000(4) C31B 0.048(6) 0.037(5) 0.051(4) 0.013(3) 0.011(5) 0.001(4) C32B 0.046(6) 0.039(5) 0.045(4) 0.007(4) 0.008(5) -0.001(4) C33B 0.053(5) 0.051(4) 0.057(4) 0.008(3) -0.005(4) -0.002(4) C34B 0.052(5) 0.053(5) 0.058(4) 0.007(3) -0.002(5) -0.006(4) C35 0.0422(13) 0.0366(11) 0.0364(11) 0.0065(9) 0.0073(10) 0.0064(10) C36 0.0422(13) 0.0410(12) 0.0372(11) 0.0054(9) 0.0114(10) 0.0051(10) C37 0.0389(12) 0.0385(11) 0.0343(11) -0.0033(9) 0.0062(9) 0.0042(10) C38 0.0437(13) 0.0345(11) 0.0422(12) 0.0032(9) 0.0088(10) 0.0077(10) C39 0.0395(12) 0.0350(11) 0.0404(12) 0.0057(9) 0.0085(9) 0.0022(9) C40 0.0633(17) 0.0647(16) 0.0591(16) 0.0139(13) 0.0321(13) 0.0211(14) C41 0.0539(15) 0.0458(13) 0.0534(14) -0.0015(11) 0.0158(12) 0.0139(11) C42 0.0343(11) 0.0296(10) 0.0318(10) 0.0056(8) 0.0057(9) 0.0033(8) C43 0.0368(12) 0.0301(10) 0.0298(10) 0.0020(8) 0.0083(9) 0.0050(9) C44 0.0356(12) 0.0322(10) 0.0362(11) 0.0060(8) 0.0102(9) 0.0058(9) C45 0.0331(11) 0.0359(11) 0.0378(11) 0.0005(9) 0.0042(9) 0.0005(9) C46 0.0414(13) 0.0335(11) 0.0336(11) -0.0010(9) 0.0070(9) 0.0036(9) C47 0.0383(13) 0.0551(14) 0.0404(12) 0.0014(10) 0.0134(10) 0.0114(11) C48 0.0327(13) 0.0620(15) 0.0540(14) -0.0041(12) 0.0071(11) 0.0062(11) O31A 0.109(9) 0.068(7) 0.124(10) 0.046(7) -0.006(7) -0.014(6) C99A 0.058(9) 0.065(9) 0.059(10) 0.015(8) 0.004(8) -0.021(6) O31B 0.0591(16) 0.0442(14) 0.0732(17) 0.0048(11) -0.0102(12) 0.0065(11) C99B 0.076(3) 0.044(2) 0.093(4) 0.006(3) 0.017(3) 0.009(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 Fe1 N1 1.9086(16) . ? Fe1 N2 1.9154(16) . ? Fe1 O2 1.9478(14) . ? Fe1 O1 1.9571(14) . ? Fe1 N3 2.0134(17) . ? Fe1 N4 2.0183(18) . ? O1 C12 1.267(3) . ? O2 C1 1.265(2) . ? O3 C17 1.207(3) . ? O4 C17 1.369(3) . ? O4 C18 1.424(3) . ? O5 C14 1.225(2) . ? O6 C14 1.349(2) . ? O6 C15 1.437(3) . ? O7 C7 1.367(2) . ? O7 C19 1.437(2) . ? O8 C6 1.375(2) . ? O8 C27B 1.413(4) . ? O8 C27A 1.534(5) . ? N1 C10 1.301(3) . ? N1 C9 1.424(2) . ? N2 C3 1.293(3) . ? N2 C4 1.425(2) . ? N3 C46 1.346(3) . ? N3 C42 1.352(2) . ? N4 C39 1.342(3) . ? N4 C35 1.347(3) . ? N5 C44 1.352(3) . ? N5 C48 1.447(3) . ? N5 C47 1.454(3) . ? N6 C37 1.359(3) . ? N6 C41 1.443(3) . ? N6 C40 1.447(3) . ? C1 C2 1.429(3) . ? C1 C13 1.513(3) . ? C2 C3 1.431(3) . ? C2 C14 1.451(3) . ? C3 H3 0.9500 . ? C4 C9 1.382(3) . ? C4 C5 1.405(3) . ? C5 C6 1.378(3) . ? C5 H5 0.9500 . ? C6 C7 1.398(3) . ? C7 C8 1.384(3) . ? C8 C9 1.400(3) . ? C8 H8 0.9500 . ? C10 C11 1.421(3) . ? C10 H10 0.9500 . ? C11 C12 1.431(3) . ? C11 C17 1.450(3) . ? C12 C16 1.510(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.510(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.510(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.517(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.515(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.522(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.517(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.524(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27A C28A 1.526(10) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A C29A 1.491(17) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? C29A C30A 1.527(8) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C30A C31A 1.518(14) . ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? C31A C32A 1.520(8) . ? C31A H31A 0.9900 . ? C31A H31B 0.9900 . ? C32A C33A 1.534(11) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A C34A 1.516(7) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C27B C28B 1.503(6) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B C29B 1.528(12) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C29B C30B 1.560(16) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30B C31B 1.507(8) . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31B C32B 1.521(14) . ? C31B H31C 0.9900 . ? C31B H31D 0.9900 . ? C32B C33B 1.511(8) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33B C34B 1.513(13) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35 C36 1.366(3) . ? C35 H35 0.9500 . ? C36 C37 1.403(3) . ? C36 H36 0.9500 . ? C37 C38 1.412(3) . ? C38 C39 1.369(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.371(3) . ? C42 H42 0.9500 . ? C43 C44 1.402(3) . ? C43 H43 0.9500 . ? C44 C45 1.417(3) . ? C45 C46 1.371(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? O31A C99A 1.364(18) . ? O31A H31E 0.8400 . ? C99A H99A 0.9800 . ? C99A H99B 0.9800 . ? C99A H99C 0.9800 . ? O31B C99B 1.399(5) . ? O31B H31F 0.8400 . ? C99B H99D 0.9800 . ? C99B H99E 0.9800 . ? C99B H99F 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 N1 Fe1 N2 84.57(7) . . ? N1 Fe1 O2 176.42(6) . . ? N2 Fe1 O2 91.94(6) . . ? N1 Fe1 O1 91.79(6) . . ? N2 Fe1 O1 176.31(6) . . ? O2 Fe1 O1 91.68(6) . . ? N1 Fe1 N3 92.35(7) . . ? N2 Fe1 N3 91.52(7) . . ? O2 Fe1 N3 86.93(6) . . ? O1 Fe1 N3 87.98(6) . . ? N1 Fe1 N4 91.49(7) . . ? N2 Fe1 N4 90.79(7) . . ? O2 Fe1 N4 89.35(6) . . ? O1 Fe1 N4 89.95(6) . . ? N3 Fe1 N4 175.69(7) . . ? C12 O1 Fe1 128.70(12) . . ? C1 O2 Fe1 128.36(12) . . ? C17 O4 C18 116.24(17) . . ? C14 O6 C15 115.15(16) . . ? C7 O7 C19 116.33(15) . . ? C6 O8 C27B 117.4(2) . . ? C6 O8 C27A 114.2(2) . . ? C27B O8 C27A 45.3(3) . . ? C10 N1 C9 120.79(16) . . ? C10 N1 Fe1 126.46(13) . . ? C9 N1 Fe1 112.67(13) . . ? C3 N2 C4 121.23(16) . . ? C3 N2 Fe1 125.87(13) . . ? C4 N2 Fe1 112.75(13) . . ? C46 N3 C42 114.99(18) . . ? C46 N3 Fe1 121.87(13) . . ? C42 N3 Fe1 123.14(13) . . ? C39 N4 C35 114.68(18) . . ? C39 N4 Fe1 123.27(15) . . ? C35 N4 Fe1 121.99(14) . . ? C44 N5 C48 121.29(17) . . ? C44 N5 C47 121.14(17) . . ? C48 N5 C47 117.29(18) . . ? C37 N6 C41 121.7(2) . . ? C37 N6 C40 120.5(2) . . ? C41 N6 C40 117.5(2) . . ? O2 C1 C2 123.44(18) . . ? O2 C1 C13 113.69(17) . . ? C2 C1 C13 122.85(19) . . ? C1 C2 C3 122.29(18) . . ? C1 C2 C14 125.10(18) . . ? C3 C2 C14 112.60(17) . . ? N2 C3 C2 126.21(18) . . ? N2 C3 H3 116.9 . . ? C2 C3 H3 116.9 . . ? C9 C4 C5 119.74(17) . . ? C9 C4 N2 114.30(16) . . ? C5 C4 N2 125.94(18) . . ? C6 C5 C4 120.15(19) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? O8 C6 C5 124.05(18) . . ? O8 C6 C7 115.54(16) . . ? C5 C6 C7 120.36(17) . . ? O7 C7 C8 123.90(18) . . ? O7 C7 C6 116.70(17) . . ? C8 C7 C6 119.37(17) . . ? C7 C8 C9 120.66(19) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C4 C9 C8 119.71(17) . . ? C4 C9 N1 115.10(16) . . ? C8 C9 N1 125.19(18) . . ? N1 C10 C11 126.22(18) . . ? N1 C10 H10 116.9 . . ? C11 C10 H10 116.9 . . ? C10 C11 C12 122.51(19) . . ? C10 C11 C17 116.57(18) . . ? C12 C11 C17 120.92(18) . . ? O1 C12 C11 123.51(18) . . ? O1 C12 C16 114.95(19) . . ? C11 C12 C16 121.5(2) . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 O6 119.33(19) . . ? O5 C14 C2 124.97(18) . . ? O6 C14 C2 115.65(17) . . ? O6 C15 H15A 109.5 . . ? O6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 O4 119.4(2) . . ? O3 C17 C11 128.6(2) . . ? O4 C17 C11 112.07(17) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O7 C19 C20 109.11(16) . . ? O7 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O7 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C19 C20 C21 114.79(17) . . ? C19 C20 H20A 108.6 . . ? C21 C20 H20A 108.6 . . ? C19 C20 H20B 108.6 . . ? C21 C20 H20B 108.6 . . ? H20A C20 H20B 107.5 . . ? C20 C21 C22 112.43(17) . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C21 113.91(17) . . ? C23 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? C23 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C22 C23 C24 113.66(18) . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? C22 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C25 C24 C23 114.10(18) . . ? C25 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 C25 C26 112.46(19) . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? 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 . . ? C28A C27A O8 109.2(6) . . ? C28A C27A H27A 109.8 . . ? O8 C27A H27A 109.8 . . ? C28A C27A H27B 109.8 . . ? O8 C27A H27B 109.8 . . ? H27A C27A H27B 108.3 . . ? C29A C28A C27A 117.0(10) . . ? C29A C28A H28A 108.0 . . ? C27A C28A H28A 108.0 . . ? C29A C28A H28B 108.0 . . ? C27A C28A H28B 108.0 . . ? H28A C28A H28B 107.3 . . ? C28A C29A C30A 113.8(8) . . ? C28A C29A H29A 108.8 . . ? C30A C29A H29A 108.8 . . ? C28A C29A H29B 108.8 . . ? C30A C29A H29B 108.8 . . ? H29A C29A H29B 107.7 . . ? C31A C30A C29A 113.8(7) . . ? C31A C30A H30A 108.8 . . ? C29A C30A H30A 108.8 . . ? C31A C30A H30B 108.8 . . ? C29A C30A H30B 108.8 . . ? H30A C30A H30B 107.7 . . ? C30A C31A C32A 113.6(6) . . ? C30A C31A H31A 108.8 . . ? C32A C31A H31A 108.8 . . ? C30A C31A H31B 108.8 . . ? C32A C31A H31B 108.8 . . ? H31A C31A H31B 107.7 . . ? C31A C32A C33A 112.9(6) . . ? C31A C32A H32A 109.0 . . ? C33A C32A H32A 109.0 . . ? C31A C32A H32B 109.0 . . ? C33A C32A H32B 109.0 . . ? H32A C32A H32B 107.8 . . ? C34A C33A C32A 112.0(6) . . ? C34A C33A H33A 109.2 . . ? C32A C33A H33A 109.2 . . ? C34A C33A H33B 109.2 . . ? C32A C33A H33B 109.2 . . ? H33A C33A H33B 107.9 . . ? O8 C27B C28B 105.8(4) . . ? O8 C27B H27C 110.6 . . ? C28B C27B H27C 110.6 . . ? O8 C27B H27D 110.6 . . ? C28B C27B H27D 110.6 . . ? H27C C27B H27D 108.7 . . ? C27B C28B C29B 115.4(6) . . ? C27B C28B H28C 108.4 . . ? C29B C28B H28C 108.4 . . ? C27B C28B H28D 108.4 . . ? C29B C28B H28D 108.4 . . ? H28C C28B H28D 107.5 . . ? C28B C29B C30B 113.2(10) . . ? C28B C29B H29C 108.9 . . ? C30B C29B H29C 108.9 . . ? C28B C29B H29D 108.9 . . ? C30B C29B H29D 108.9 . . ? H29C C29B H29D 107.7 . . ? C31B C30B C29B 114.6(8) . . ? C31B C30B H30C 108.6 . . ? C29B C30B H30C 108.6 . . ? C31B C30B H30D 108.6 . . ? C29B C30B H30D 108.6 . . ? H30C C30B H30D 107.6 . . ? C30B C31B C32B 113.5(9) . . ? C30B C31B H31C 108.9 . . ? C32B C31B H31C 108.9 . . ? C30B C31B H31D 108.9 . . ? C32B C31B H31D 108.9 . . ? H31C C31B H31D 107.7 . . ? C33B C32B C31B 115.9(7) . . ? C33B C32B H32C 108.3 . . ? C31B C32B H32C 108.3 . . ? C33B C32B H32D 108.3 . . ? C31B C32B H32D 108.3 . . ? H32C C32B H32D 107.4 . . ? C32B C33B C34B 112.3(8) . . ? C32B C33B H33C 109.1 . . ? C34B C33B H33C 109.1 . . ? C32B C33B H33D 109.1 . . ? C34B C33B H33D 109.1 . . ? H33C C33B H33D 107.9 . . ? C33B C34B H34D 109.5 . . ? C33B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? N4 C35 C36 124.6(2) . . ? N4 C35 H35 117.7 . . ? C36 C35 H35 117.7 . . ? C35 C36 C37 120.7(2) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? N6 C37 C36 122.7(2) . . ? N6 C37 C38 122.5(2) . . ? C36 C37 C38 114.9(2) . . ? C39 C38 C37 119.9(2) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? N4 C39 C38 125.3(2) . . ? N4 C39 H39 117.4 . . ? C38 C39 H39 117.4 . . ? N6 C40 H40A 109.5 . . ? N6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 H41A 109.5 . . ? N6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 C43 124.32(18) . . ? N3 C42 H42 117.8 . . ? C43 C42 H42 117.8 . . ? C42 C43 C44 120.86(18) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? N5 C44 C43 122.70(18) . . ? N5 C44 C45 122.43(18) . . ? C43 C44 C45 114.88(18) . . ? C46 C45 C44 120.06(19) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? N3 C46 C45 124.89(19) . . ? N3 C46 H46 117.6 . . ? C45 C46 H46 117.6 . . ? N5 C47 H47A 109.5 . . ? N5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N5 C48 H48A 109.5 . . ? N5 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N5 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.57 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.612 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.049 _iucr_refine_instructions_details ; TITL w022 P 1 New: P-1 CELL 0.71073 11.9287 13.1406 17.0569 103.154 100.508 100.246 ZERR 2.00 0.0005 0.0005 0.0007 0.003 0.003 0.003 LATT 1 SFAC C H FE N O UNIT 98 148 2 12 18 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H L.S. 20 TEMP -140 WGHT 0.058900 FVAR 0.41577 0.49486 0.22757 FE1 3 0.698299 0.796828 0.288135 11.00000 0.03104 0.03130 = 0.03032 0.00307 0.00646 0.00450 O1 5 0.776313 0.948492 0.312839 11.00000 0.03677 0.03447 = 0.03345 -0.00138 0.00804 0.00258 O2 5 0.778945 0.787017 0.395312 11.00000 0.03658 0.03227 = 0.03242 -0.00055 0.00576 0.00688 O3 5 0.773492 1.140055 0.145074 11.00000 0.08842 0.03556 = 0.05623 0.01039 0.00612 -0.01355 O4 5 0.658640 0.998483 0.047715 11.00000 0.06399 0.03225 = 0.04211 0.01002 0.00700 0.00317 O5 5 0.674234 0.411434 0.361546 11.00000 0.04986 0.03793 = 0.04677 0.01082 0.00118 0.00333 O6 5 0.838838 0.508789 0.450799 11.00000 0.04375 0.03772 = 0.04154 0.00925 0.00072 0.01082 O7 5 0.301973 0.553074 -0.048514 11.00000 0.03530 0.03268 = 0.03147 0.00429 0.00045 0.00006 O8 5 0.296666 0.404946 0.030411 11.00000 0.04374 0.02874 = 0.04692 0.00502 -0.00746 -0.00251 N1 4 0.616492 0.796888 0.180990 11.00000 0.02661 0.02767 = 0.03428 0.00174 0.00723 0.00150 N2 4 0.618456 0.648558 0.256724 11.00000 0.02975 0.03444 = 0.02661 0.00273 0.00656 0.00804 N3 4 0.837078 0.760198 0.245838 11.00000 0.03626 0.02945 = 0.03061 0.00218 0.00743 0.00257 N4 4 0.567490 0.838918 0.338934 11.00000 0.03593 0.03472 = 0.03289 0.00361 0.00289 0.00206 N5 4 1.129206 0.683529 0.160800 11.00000 0.03140 0.04540 = 0.03894 -0.00087 0.00648 0.00608 N6 4 0.310886 0.936582 0.459112 11.00000 0.04934 0.04960 = 0.04646 0.00585 0.01772 0.01410 C1 1 0.789335 0.703611 0.418422 11.00000 0.03414 0.03652 = 0.03142 0.00314 0.00841 0.00878 C2 1 0.726383 0.597783 0.371387 11.00000 0.03322 0.03432 = 0.03065 0.00605 0.00671 0.00718 C3 1 0.640991 0.578095 0.295619 11.00000 0.03169 0.03011 = 0.03325 0.00356 0.00810 0.00439 AFIX 43 H3 2 0.596636 0.506439 0.271610 11.00000 -1.20000 AFIX 0 C4 1 0.533627 0.618814 0.180041 11.00000 0.02721 0.03025 = 0.03104 0.00227 0.00720 0.00521 C5 1 0.455092 0.518463 0.144300 11.00000 0.03094 0.03042 = 0.03353 0.00598 0.00804 0.00413 AFIX 43 H5 2 0.454108 0.463947 0.172586 11.00000 -1.20000 AFIX 0 C6 1 0.379497 0.498945 0.068311 11.00000 0.02906 0.02697 = 0.03521 0.00138 0.00411 0.00159 C7 1 0.380572 0.578471 0.026058 11.00000 0.02712 0.03536 = 0.02839 0.00195 0.00479 0.00400 C8 1 0.456990 0.677644 0.061839 11.00000 0.03220 0.03340 = 0.03489 0.00801 0.00590 0.00402 AFIX 43 H8 2 0.457130 0.732342 0.033762 11.00000 -1.20000 AFIX 0 C9 1 0.534111 0.698193 0.139006 11.00000 0.02801 0.02819 = 0.03091 0.00141 0.00646 0.00301 C10 1 0.633885 0.873665 0.144989 11.00000 0.03003 0.03229 = 0.03391 0.00439 0.00678 0.00533 AFIX 43 H10 2 0.590961 0.859721 0.089499 11.00000 -1.20000 AFIX 0 C11 1 0.710972 0.976415 0.180746 11.00000 0.03667 0.02845 = 0.03949 0.00382 0.01073 0.00410 C12 1 0.777264 1.009116 0.264727 11.00000 0.03503 0.03238 = 0.04108 0.00004 0.01147 0.00114 C13 1 0.872662 0.726363 0.501922 11.00000 0.05781 0.03969 = 0.03852 -0.00064 -0.00314 0.01196 AFIX 137 H13A 2 0.888381 0.802935 0.530355 11.00000 -1.50000 H13B 2 0.946255 0.706892 0.494177 11.00000 -1.50000 H13C 2 0.837313 0.683998 0.535309 11.00000 -1.50000 AFIX 0 C14 1 0.741053 0.499710 0.393215 11.00000 0.03618 0.03999 = 0.03098 0.00511 0.00774 0.00725 C15 1 0.856017 0.409968 0.468259 11.00000 0.05936 0.04188 = 0.04588 0.01464 0.00505 0.01689 AFIX 137 H15A 2 0.870414 0.362942 0.419442 11.00000 -1.50000 H15B 2 0.785840 0.374346 0.482206 11.00000 -1.50000 H15C 2 0.923510 0.425229 0.515033 11.00000 -1.50000 AFIX 0 C16 1 0.853429 1.120876 0.302782 11.00000 0.06268 0.03881 = 0.04472 -0.00209 0.00846 -0.00904 AFIX 137 H16A 2 0.898085 1.125497 0.358225 11.00000 -1.50000 H16B 2 0.803974 1.173070 0.306782 11.00000 -1.50000 H16C 2 0.907660 1.136597 0.268037 11.00000 -1.50000 AFIX 0 C17 1 0.720292 1.047690 0.127463 11.00000 0.04434 0.03463 = 0.04426 0.00415 0.01297 0.00268 C18 1 0.659214 1.063264 -0.008794 11.00000 0.08596 0.04437 = 0.04998 0.01980 0.00896 0.00351 AFIX 137 H18A 2 0.740236 1.096760 -0.006986 11.00000 -1.50000 H18B 2 0.616707 1.119221 0.006655 11.00000 -1.50000 H18C 2 0.621093 1.018396 -0.064942 11.00000 -1.50000 AFIX 0 C19 1 0.310740 0.631511 -0.095005 11.00000 0.03762 0.03630 = 0.03718 0.00845 0.00430 0.00088 AFIX 23 H19A 2 0.390099 0.646254 -0.105650 11.00000 -1.20000 H19B 2 0.297463 0.699461 -0.063020 11.00000 -1.20000 AFIX 0 C20 1 0.220189 0.589054 -0.176046 11.00000 0.03728 0.03660 = 0.03184 0.00493 0.00394 0.00327 AFIX 23 H20A 2 0.222048 0.513616 -0.200491 11.00000 -1.20000 H20B 2 0.242190 0.630971 -0.214565 11.00000 -1.20000 AFIX 0 C21 1 0.096406 0.593203 -0.169551 11.00000 0.03857 0.03391 = 0.03285 0.00404 0.00383 0.00608 AFIX 23 H21A 2 0.093279 0.668682 -0.146608 11.00000 -1.20000 H21B 2 0.073961 0.552101 -0.130651 11.00000 -1.20000 AFIX 0 C22 1 0.009100 0.547629 -0.252506 11.00000 0.03980 0.04538 = 0.03432 0.00713 0.00444 0.00766 AFIX 23 H22A 2 0.032100 0.588850 -0.291198 11.00000 -1.20000 H22B 2 0.013029 0.472359 -0.275354 11.00000 -1.20000 AFIX 0 C23 1 -0.116143 0.550245 -0.248364 11.00000 0.03870 0.04524 = 0.03566 0.00784 0.00436 0.00780 AFIX 23 H23A 2 -0.119226 0.624766 -0.222102 11.00000 -1.20000 H23B 2 -0.141015 0.504977 -0.212684 11.00000 -1.20000 AFIX 0 C24 1 -0.202162 0.511160 -0.332534 11.00000 0.04074 0.05353 = 0.03619 0.01111 0.00512 0.00777 AFIX 23 H24A 2 -0.177661 0.557005 -0.367929 11.00000 -1.20000 H24B 2 -0.198154 0.437011 -0.359049 11.00000 -1.20000 AFIX 0 C25 1 -0.328108 0.512166 -0.329010 11.00000 0.03840 0.05833 = 0.03999 0.00962 0.00284 0.00814 AFIX 23 H25A 2 -0.330593 0.582334 -0.293493 11.00000 -1.20000 H25B 2 -0.358219 0.455755 -0.303362 11.00000 -1.20000 AFIX 0 C26 1 -0.407279 0.493192 -0.414334 11.00000 0.04170 0.07033 = 0.04499 0.01207 0.00140 0.01037 AFIX 137 H26A 2 -0.404380 0.424231 -0.450002 11.00000 -1.50000 H26B 2 -0.380449 0.551059 -0.438757 11.00000 -1.50000 H26C 2 -0.487925 0.492083 -0.409117 11.00000 -1.50000 AFIX 0 PART 1 C27A 1 0.271066 0.334313 0.088211 10.50000 0.04440 0.03248 = 0.04149 0.01413 0.00316 -0.00684 AFIX 23 H27A 2 0.331148 0.291694 0.094271 10.50000 -1.20000 H27B 2 0.273716 0.380024 0.143660 10.50000 -1.20000 AFIX 0 C28A 1 0.150048 0.259336 0.052024 10.50000 0.04409 0.04458 = 0.04370 0.01232 0.01830 0.00316 AFIX 23 H28A 2 0.126302 0.228557 0.095961 10.50000 -1.20000 H28B 2 0.093968 0.303023 0.037412 10.50000 -1.20000 AFIX 0 C29A 1 0.137722 0.168905 -0.022285 10.50000 0.04507 0.02907 = 0.03952 0.01055 0.00505 0.00245 AFIX 23 H29A 2 0.181574 0.116984 -0.005691 10.50000 -1.20000 H29B 2 0.173781 0.197352 -0.063107 10.50000 -1.20000 AFIX 0 C30A 1 0.010967 0.109861 -0.063747 10.50000 0.04415 0.02930 = 0.03597 0.00487 0.00580 -0.00297 AFIX 23 H30A 2 -0.024457 0.079843 -0.023331 10.50000 -1.20000 H30B 2 -0.033353 0.162158 -0.079018 10.50000 -1.20000 AFIX 0 C31A 1 -0.001965 0.019570 -0.140625 10.50000 0.04215 0.03608 = 0.04111 0.01165 0.00719 0.00568 AFIX 23 H31A 2 0.038918 -0.034632 -0.124879 10.50000 -1.20000 H31B 2 0.036919 0.048863 -0.179928 10.50000 -1.20000 AFIX 0 C32A 1 -0.128504 -0.035352 -0.184041 10.50000 0.04138 0.03433 = 0.03194 0.00135 0.00225 -0.00064 AFIX 23 H32A 2 -0.168889 0.018194 -0.201547 10.50000 -1.20000 H32B 2 -0.168221 -0.062901 -0.144394 10.50000 -1.20000 AFIX 0 C33A 1 -0.139864 -0.128558 -0.260028 10.50000 0.04260 0.04639 = 0.04512 0.00341 0.00976 0.00096 AFIX 23 H33A 2 -0.104297 -0.100565 -0.301230 10.50000 -1.20000 H33B 2 -0.096097 -0.180434 -0.243247 10.50000 -1.20000 AFIX 0 C34A 1 -0.266505 -0.185907 -0.299581 10.50000 0.04750 0.05120 = 0.04849 0.00135 0.00596 -0.00327 AFIX 137 H34A 2 -0.299793 -0.219849 -0.260830 10.50000 -1.50000 H34B 2 -0.270433 -0.240965 -0.350217 10.50000 -1.50000 H34C 2 -0.311177 -0.133988 -0.313271 10.50000 -1.50000 AFIX 0 PART 2 C27B 1 0.325396 0.308707 0.041838 10.50000 0.03615 0.02882 = 0.03678 0.00331 0.00939 0.00416 AFIX 23 H27C 2 0.408040 0.322614 0.072202 10.50000 -1.20000 H27D 2 0.313865 0.255801 -0.012208 10.50000 -1.20000 AFIX 0 C28B 1 0.244139 0.267673 0.091227 10.50000 0.03571 0.03924 = 0.03896 0.00819 0.00758 0.00327 AFIX 23 H28C 2 0.251607 0.325475 0.141862 10.50000 -1.20000 H28D 2 0.270047 0.207206 0.108897 10.50000 -1.20000 AFIX 0 C29B 1 0.114922 0.229664 0.046123 10.50000 0.03625 0.05112 = 0.04313 0.01758 0.01464 0.01238 AFIX 23 H29C 2 0.088370 0.289698 0.028157 10.50000 -1.20000 H29D 2 0.068446 0.210058 0.085199 10.50000 -1.20000 AFIX 0 C30B 1 0.090415 0.131424 -0.030951 10.50000 0.04793 0.03058 = 0.04114 0.00576 0.01063 -0.00001 AFIX 23 H30C 2 0.130225 0.153754 -0.072446 10.50000 -1.20000 H30D 2 0.125426 0.074686 -0.013896 10.50000 -1.20000 AFIX 0 C31B 1 -0.037494 0.084422 -0.071386 10.50000 0.04850 0.03683 = 0.05120 0.01345 0.01091 0.00081 AFIX 23 H31C 2 -0.073910 0.141942 -0.085559 10.50000 -1.20000 H31D 2 -0.076588 0.057540 -0.031207 10.50000 -1.20000 AFIX 0 C32B 1 -0.058640 -0.006772 -0.149340 10.50000 0.04616 0.03935 = 0.04488 0.00697 0.00785 -0.00124 AFIX 23 H32C 2 -0.019797 0.020975 -0.189290 10.50000 -1.20000 H32D 2 -0.020215 -0.063041 -0.134870 10.50000 -1.20000 AFIX 0 C33B 1 -0.185397 -0.058376 -0.191948 10.50000 0.05270 0.05086 = 0.05669 0.00797 -0.00511 -0.00220 AFIX 23 H33C 2 -0.223075 -0.004374 -0.211272 10.50000 -1.20000 H33D 2 -0.226546 -0.082345 -0.151620 10.50000 -1.20000 AFIX 0 C34B 1 -0.198320 -0.153451 -0.264966 10.50000 0.05203 0.05311 = 0.05778 0.00738 -0.00222 -0.00560 AFIX 137 H34D 2 -0.161573 -0.129407 -0.306523 10.50000 -1.50000 H34E 2 -0.281651 -0.185837 -0.289364 10.50000 -1.50000 H34F 2 -0.160108 -0.206693 -0.246309 10.50000 -1.50000 AFIX 0 PART 0 C35 1 0.520926 0.786109 0.388731 11.00000 0.04224 0.03664 = 0.03644 0.00651 0.00734 0.00644 AFIX 43 H35 2 0.548320 0.724773 0.396731 11.00000 -1.20000 AFIX 0 C36 1 0.437089 0.814561 0.428530 11.00000 0.04216 0.04095 = 0.03722 0.00537 0.01139 0.00513 AFIX 43 H36 2 0.408460 0.773118 0.462651 11.00000 -1.20000 AFIX 0 C37 1 0.392800 0.904342 0.419556 11.00000 0.03887 0.03847 = 0.03428 -0.00331 0.00616 0.00419 C38 1 0.439759 0.958700 0.366164 11.00000 0.04375 0.03446 = 0.04216 0.00324 0.00876 0.00770 AFIX 43 H38 2 0.413250 1.019538 0.355969 11.00000 -1.20000 AFIX 0 C39 1 0.523545 0.923569 0.329126 11.00000 0.03955 0.03500 = 0.04037 0.00567 0.00853 0.00221 AFIX 43 H39 2 0.552963 0.962233 0.293608 11.00000 -1.20000 AFIX 0 C40 1 0.259586 0.874298 0.508929 11.00000 0.06335 0.06473 = 0.05911 0.01389 0.03207 0.02114 AFIX 137 H40A 2 0.321966 0.858962 0.547404 11.00000 -1.50000 H40B 2 0.208708 0.806656 0.472813 11.00000 -1.50000 H40C 2 0.213346 0.915099 0.540306 11.00000 -1.50000 AFIX 0 C41 1 0.262478 1.026096 0.445830 11.00000 0.05389 0.04584 = 0.05345 -0.00147 0.01579 0.01391 AFIX 137 H41A 2 0.206996 1.004335 0.391759 11.00000 -1.50000 H41B 2 0.325799 1.085821 0.447294 11.00000 -1.50000 H41C 2 0.221775 1.048906 0.489420 11.00000 -1.50000 AFIX 0 C42 1 0.826929 0.690220 0.171900 11.00000 0.03434 0.02963 = 0.03184 0.00558 0.00569 0.00328 AFIX 43 H42 2 0.750337 0.657353 0.138606 11.00000 -1.20000 AFIX 0 C43 1 0.919857 0.663554 0.141797 11.00000 0.03683 0.03006 = 0.02978 0.00205 0.00829 0.00495 AFIX 43 H43 2 0.905919 0.614171 0.088929 11.00000 -1.20000 AFIX 0 C44 1 1.035205 0.708217 0.188019 11.00000 0.03562 0.03216 = 0.03621 0.00601 0.01016 0.00578 C45 1 1.045923 0.780866 0.265863 11.00000 0.03306 0.03594 = 0.03778 0.00053 0.00418 0.00051 AFIX 43 H45 2 1.121203 0.813801 0.301193 11.00000 -1.20000 AFIX 0 C46 1 0.947750 0.803653 0.290224 11.00000 0.04136 0.03346 = 0.03362 -0.00101 0.00703 0.00365 AFIX 43 H46 2 0.958624 0.853863 0.342324 11.00000 -1.20000 AFIX 0 C47 1 1.116332 0.617029 0.077450 11.00000 0.03834 0.05511 = 0.04045 0.00139 0.01344 0.01135 AFIX 137 H47A 2 1.072738 0.544185 0.072038 11.00000 -1.50000 H47B 2 1.193956 0.614507 0.066852 11.00000 -1.50000 H47C 2 1.073629 0.647590 0.037303 11.00000 -1.50000 AFIX 0 C48 1 1.247169 0.730842 0.210233 11.00000 0.03267 0.06198 = 0.05396 -0.00412 0.00709 0.00622 AFIX 137 H48A 2 1.253336 0.718558 0.265259 11.00000 -1.50000 H48B 2 1.265429 0.808206 0.215683 11.00000 -1.50000 H48C 2 1.302612 0.697797 0.183226 11.00000 -1.50000 AFIX 0 PART 3 O31A 5 0.541157 0.202797 0.327472 31.00000 0.10930 0.06827 = 0.12406 0.04620 -0.00584 -0.01364 AFIX 147 H31E 2 0.484128 0.221866 0.344176 31.00000 -1.50000 AFIX 0 C99A 1 0.518792 0.181929 0.243331 31.00000 0.05754 0.06473 = 0.05928 0.01456 0.00382 -0.02055 AFIX 137 H99A 2 0.470620 0.229175 0.225230 31.00000 -1.50000 H99B 2 0.476834 0.106875 0.218269 31.00000 -1.50000 H99C 2 0.592856 0.194748 0.226053 31.00000 -1.50000 AFIX 0 PART 4 O31B 5 0.495939 0.295611 0.226454 -31.00000 0.05906 0.04421 = 0.07315 0.00479 -0.01019 0.00647 AFIX 147 H31F 2 0.550921 0.334147 0.265933 -31.00000 -1.50000 AFIX 0 C99B 1 0.516854 0.192967 0.201951 -31.00000 0.07638 0.04447 = 0.09320 0.00561 0.01735 0.00926 AFIX 137 H99D 2 0.600989 0.196906 0.218234 -31.00000 -1.50000 H99E 2 0.489761 0.164885 0.141706 -31.00000 -1.50000 H99F 2 0.474460 0.145211 0.228747 -31.00000 -1.50000 HKLF 4 REM w022 P 1 New: P-1 REM R1 = 0.0384 for 6388 Fo > 4sig(Fo) and 0.0531 for all 8344 data REM 693 parameters refined using 0 restraints END WGHT 0.0588 0.0000 REM Highest difference peak 0.612, deepest hole -0.471, 1-sigma level 0.049 Q1 1 0.7653 0.7525 0.3080 11.00000 0.05 0.61 Q2 1 0.6333 0.8468 0.2669 11.00000 0.05 0.58 Q3 1 0.6669 0.7657 0.2074 11.00000 0.05 0.38 Q4 1 0.7244 0.8255 0.3661 11.00000 0.05 0.37 Q5 1 0.7784 0.8327 0.2524 11.00000 0.05 0.32 Q6 1 1.0220 0.9758 0.5336 11.00000 0.05 0.32 Q7 1 0.6413 0.8188 0.3536 11.00000 0.05 0.30 Q8 1 0.6216 0.7830 0.3372 11.00000 0.05 0.29 Q9 1 0.5679 0.6554 0.1506 11.00000 0.05 0.20 Q10 1 0.5757 0.6209 0.1965 11.00000 0.05 0.20 Q11 1 0.8885 0.7976 0.2507 11.00000 0.05 0.20 Q12 1 0.6889 1.0198 0.1621 11.00000 0.05 0.20 Q13 1 0.8413 0.7845 0.3928 11.00000 0.05 0.20 Q14 1 0.6763 0.6186 0.2654 11.00000 0.05 0.20 Q15 1 1.1731 0.5697 0.0857 11.00000 0.05 0.19 Q16 1 -0.0620 0.5254 -0.2494 11.00000 0.05 0.19 Q17 1 0.7343 0.9957 0.2198 11.00000 0.05 0.19 Q18 1 0.4916 0.6669 0.1718 11.00000 0.05 0.19 Q19 1 0.7031 0.5632 0.3935 11.00000 0.05 0.18 Q20 1 0.4850 0.7141 0.1318 11.00000 0.05 0.18 ; _database_code_depnum_ccdc_archive 'CCDC 944436' ####################################################################### # # 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_w023 # start Validation Reply Form _vrf_PLAT230_w023 ; PROBLEM: Hirshfeld Test Diff for O8 -- C41 .. 9.6 su RESPONSE: Disorder of alkyl chain that could not be resolved. PROBLEM: Hirshfeld Test Diff for C44 -- C45 .. 12.2 su RESPONSE: Disorder of alkyl chain that could not be resolved. PROBLEM: Hirshfeld Test Diff for C46 -- C47 .. 9.6 su RESPONSE: Disorder of alkyl chain that could not be resolved. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Fe12i(C8)(dmap)2]' _chemical_melting_point ? _chemical_formula_moiety 'C48 H70 Fe N6 O8, C H4 O' _chemical_formula_sum 'C49 H74 Fe N6 O9' _chemical_formula_weight 946.99 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' Fe Fe 0.3463 0.8444 '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' _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 12.0361(8) _cell_length_b 13.4241(10) _cell_length_c 17.3275(13) _cell_angle_alpha 103.289(6) _cell_angle_beta 101.608(6) _cell_angle_gamma 99.935(6) _cell_volume 2597.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 31745 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 24.6 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.347 _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 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDSII _diffrn_measurement_method Omega-Scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31745 _diffrn_reflns_av_R_equivalents 0.1538 _diffrn_reflns_av_sigmaI/netI 0.1188 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 24.59 _reflns_number_total 8697 _reflns_number_gt 4893 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-AREA-STOE _computing_cell_refinement X-AREA-STOE _computing_data_reduction X-AREA-STOE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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^)+(0.0891P)^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 8697 _refine_ls_number_parameters 618 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1596 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.879 _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 C1 C 0.2287(4) -0.0158(3) 0.2440(3) 0.0699(11) Uani 1 1 d . . . C2 C 0.2953(3) 0.0238(3) 0.3272(2) 0.0620(10) Uani 1 1 d . . . C3 C 0.3699(3) 0.1268(3) 0.3584(2) 0.0570(9) Uani 1 1 d . . . H3 H 0.4111 0.1447 0.4130 0.068 Uiso 1 1 calc R . . C4 C 0.4680(3) 0.2960(3) 0.3609(2) 0.0514(9) Uani 1 1 d . . . C5 C 0.5469(3) 0.3177(3) 0.4374(2) 0.0566(9) Uani 1 1 d . . . H5 H 0.5485 0.2652 0.4642 0.068 Uiso 1 1 calc R . . C6 C 0.6216(3) 0.4142(3) 0.4740(2) 0.0537(9) Uani 1 1 d . . . C7 C 0.6213(3) 0.4929(3) 0.4337(2) 0.0574(9) Uani 1 1 d . . . C8 C 0.5454(3) 0.4727(3) 0.3576(2) 0.0582(9) Uani 1 1 d . . . H8 H 0.5459 0.5250 0.3305 0.070 Uiso 1 1 calc R . . C9 C 0.4677(3) 0.3743(3) 0.3208(2) 0.0506(9) Uani 1 1 d . . . C10 C 0.3604(3) 0.4199(3) 0.2089(2) 0.0585(10) Uani 1 1 d . . . H10 H 0.4011 0.4887 0.2361 0.070 Uiso 1 1 calc R . . C11 C 0.2769(3) 0.4048(3) 0.1329(2) 0.0587(10) Uani 1 1 d . . . C12 C 0.2143(4) 0.3045(3) 0.0817(2) 0.0636(10) Uani 1 1 d . . . C13 C 0.2642(4) 0.5034(4) 0.1149(2) 0.0727(12) Uani 1 1 d . . . C14 C 0.1512(6) 0.5968(5) 0.0441(4) 0.127(2) Uani 1 1 d . . . H14A H 0.1215 0.6346 0.0865 0.190 Uiso 1 1 calc R . . H14B H 0.0968 0.5833 -0.0080 0.190 Uiso 1 1 calc R . . H14C H 0.2245 0.6381 0.0437 0.190 Uiso 1 1 calc R . . C15 C 0.1293(5) 0.2874(4) -0.0001(3) 0.1032(18) Uani 1 1 d . . . H15A H 0.1080 0.2139 -0.0287 0.155 Uiso 1 1 calc R . . H15B H 0.1651 0.3264 -0.0322 0.155 Uiso 1 1 calc R . . H15C H 0.0608 0.3109 0.0087 0.155 Uiso 1 1 calc R . . C16 C 0.1532(5) -0.1254(4) 0.2113(3) 0.1021(17) Uani 1 1 d . . . H16A H 0.1030 -0.1325 0.1588 0.153 Uiso 1 1 calc R . . H16B H 0.1068 -0.1384 0.2485 0.153 Uiso 1 1 calc R . . H16C H 0.2015 -0.1752 0.2058 0.153 Uiso 1 1 calc R . . C17 C 0.2898(4) -0.0407(4) 0.3833(3) 0.0787(12) Uani 1 1 d . . . C18 C 0.3511(5) -0.0484(4) 0.5197(3) 0.1056(17) Uani 1 1 d . . . H18A H 0.2727 -0.0776 0.5202 0.158 Uiso 1 1 calc R . . H18B H 0.3922 -0.0033 0.5731 0.158 Uiso 1 1 calc R . . H18C H 0.3898 -0.1042 0.5054 0.158 Uiso 1 1 calc R . . C19 C 0.4855(4) 0.0642(3) 0.1587(3) 0.0707(11) Uani 1 1 d . . . H19 H 0.4560 0.0241 0.1904 0.085 Uiso 1 1 calc R . . C20 C 0.5716(4) 0.0353(3) 0.1253(3) 0.0734(12) Uani 1 1 d . . . H20 H 0.5985 -0.0230 0.1343 0.088 Uiso 1 1 calc R . . C21 C 0.6204(4) 0.0930(4) 0.0774(2) 0.0692(11) Uani 1 1 d . . . C22 C 0.5735(4) 0.1794(4) 0.0685(2) 0.0727(11) Uani 1 1 d . . . H22 H 0.6010 0.2213 0.0374 0.087 Uiso 1 1 calc R . . C23 C 0.4877(4) 0.2021(3) 0.1055(2) 0.0710(11) Uani 1 1 d . . . H23 H 0.4607 0.2615 0.0994 0.085 Uiso 1 1 calc R . . C24 C 0.7544(5) -0.0216(4) 0.0534(3) 0.1020(17) Uani 1 1 d . . . H24A H 0.7871 -0.0115 0.1107 0.153 Uiso 1 1 calc R . . H24B H 0.8144 -0.0270 0.0245 0.153 Uiso 1 1 calc R . . H24C H 0.6942 -0.0850 0.0324 0.153 Uiso 1 1 calc R . . C25 C 0.7549(5) 0.1290(5) -0.0046(3) 0.1084(18) Uani 1 1 d . . . H25A H 0.6938 0.1381 -0.0456 0.163 Uiso 1 1 calc R . . H25B H 0.8064 0.0941 -0.0306 0.163 Uiso 1 1 calc R . . H25C H 0.7978 0.1965 0.0310 0.163 Uiso 1 1 calc R . . C26 C 0.0356(4) 0.1958(3) 0.2060(2) 0.0709(11) Uani 1 1 d . . . H26 H 0.0212 0.1475 0.1551 0.085 Uiso 1 1 calc R . . C27 C -0.0581(4) 0.2206(3) 0.2313(2) 0.0736(12) Uani 1 1 d . . . H27 H -0.1328 0.1895 0.1982 0.088 Uiso 1 1 calc R . . C28 C -0.0424(3) 0.2939(3) 0.3082(2) 0.0595(10) Uani 1 1 d . . . C29 C 0.0737(3) 0.3357(3) 0.3513(2) 0.0612(10) Uani 1 1 d . . . H29 H 0.0913 0.3847 0.4022 0.073 Uiso 1 1 calc R . . C30 C 0.1622(3) 0.3058(3) 0.3199(2) 0.0610(10) Uani 1 1 d . . . H30 H 0.2383 0.3370 0.3506 0.073 Uiso 1 1 calc R . . C31 C -0.2513(4) 0.2731(5) 0.2910(3) 0.1064(18) Uani 1 1 d . . . H31A H -0.2618 0.2805 0.2364 0.160 Uiso 1 1 calc R . . H31B H -0.3025 0.3076 0.3176 0.160 Uiso 1 1 calc R . . H31C H -0.2689 0.1998 0.2888 0.160 Uiso 1 1 calc R . . C32 C -0.1141(4) 0.3897(4) 0.4185(3) 0.0882(15) Uani 1 1 d . . . H32A H -0.0828 0.3563 0.4587 0.132 Uiso 1 1 calc R . . H32B H -0.1872 0.4039 0.4263 0.132 Uiso 1 1 calc R . . H32C H -0.0605 0.4545 0.4245 0.132 Uiso 1 1 calc R . . C33 C 0.6932(4) 0.3639(3) 0.5938(2) 0.0718(11) Uani 1 1 d . . . H33A H 0.7057 0.2984 0.5631 0.086 Uiso 1 1 calc R . . H33B H 0.6160 0.3500 0.6033 0.086 Uiso 1 1 calc R . . C34 C 0.7842(4) 0.4058(4) 0.6751(2) 0.0710(11) Uani 1 1 d . . . H34A H 0.7821 0.4781 0.6989 0.085 Uiso 1 1 calc R . . H34B H 0.7632 0.3655 0.7119 0.085 Uiso 1 1 calc R . . C35 C 0.9060(4) 0.4024(4) 0.6704(3) 0.0776(12) Uani 1 1 d . . . H35A H 0.9275 0.4420 0.6332 0.093 Uiso 1 1 calc R . . H35B H 0.9094 0.3301 0.6481 0.093 Uiso 1 1 calc R . . C36 C 0.9937(4) 0.4474(4) 0.7535(3) 0.0861(14) Uani 1 1 d . . . H36A H 0.9893 0.5195 0.7757 0.103 Uiso 1 1 calc R . . H36B H 0.9717 0.4076 0.7904 0.103 Uiso 1 1 calc R . . C37 C 1.1168(4) 0.4462(4) 0.7517(3) 0.0907(14) Uani 1 1 d . . . H37A H 1.1399 0.4882 0.7165 0.109 Uiso 1 1 calc R . . H37B H 1.1208 0.3745 0.7276 0.109 Uiso 1 1 calc R . . C38 C 1.2039(4) 0.4877(5) 0.8358(3) 0.1092(19) Uani 1 1 d . . . H38A H 1.2006 0.5596 0.8596 0.131 Uiso 1 1 calc R . . H38B H 1.1804 0.4462 0.8712 0.131 Uiso 1 1 calc R . . C39 C 1.3271(5) 0.4852(6) 0.8340(3) 0.123(2) Uani 1 1 d . . . H39A H 1.3284 0.4165 0.8012 0.148 Uiso 1 1 calc R . . H39B H 1.3556 0.5368 0.8072 0.148 Uiso 1 1 calc R . . C40 C 1.4049(6) 0.5063(8) 0.9138(4) 0.160(3) Uani 1 1 d . . . H40A H 1.3905 0.5651 0.9506 0.240 Uiso 1 1 calc R . . H40B H 1.4841 0.5223 0.9098 0.240 Uiso 1 1 calc R . . H40C H 1.3920 0.4456 0.9340 0.240 Uiso 1 1 calc R . . C41 C 0.6742(6) 0.6754(5) 0.4526(4) 0.118(2) Uani 1 1 d D . . H41A H 0.5950 0.6588 0.4190 0.142 Uiso 1 1 calc R . . H41B H 0.6802 0.7294 0.5022 0.142 Uiso 1 1 calc R . . C42 C 0.7515(7) 0.7122(8) 0.4101(5) 0.161(3) Uani 1 1 d D . . H42A H 0.7237 0.7664 0.3884 0.194 Uiso 1 1 calc R . . H42B H 0.7497 0.6548 0.3638 0.194 Uiso 1 1 calc R . . C43 C 0.8786(5) 0.7573(5) 0.4596(4) 0.1122(18) Uani 1 1 d . . . H43A H 0.9077 0.7030 0.4803 0.135 Uiso 1 1 calc R . . H43B H 0.9251 0.7766 0.4234 0.135 Uiso 1 1 calc R . . C44 C 0.8935(9) 0.8475(8) 0.5272(5) 0.162(4) Uani 1 1 d . . . H44A H 0.8522 0.8263 0.5656 0.194 Uiso 1 1 calc R . . H44B H 0.8576 0.8990 0.5069 0.194 Uiso 1 1 calc R . . C45 C 1.0222(7) 0.9009(5) 0.5739(4) 0.131(2) Uani 1 1 d . . . H45A H 1.0576 0.8484 0.5930 0.158 Uiso 1 1 calc R . . H45B H 1.0626 0.9215 0.5349 0.158 Uiso 1 1 calc R . . C46 C 1.0444(10) 0.9956(7) 0.6459(5) 0.162(3) Uani 1 1 d . . . H46A H 1.0111 1.0485 0.6260 0.195 Uiso 1 1 calc R . . H46B H 1.0009 0.9752 0.6834 0.195 Uiso 1 1 calc R . . C47 C 1.1604(8) 1.0445(7) 0.6920(6) 0.167(3) Uani 1 1 d . . . H47A H 1.2044 1.0624 0.6540 0.201 Uiso 1 1 calc R . . H47B H 1.1928 0.9919 0.7132 0.201 Uiso 1 1 calc R . . C48 C 1.1858(9) 1.1454(7) 0.7656(5) 0.184(4) Uani 1 1 d . . . H48A H 1.1577 1.2002 0.7463 0.276 Uiso 1 1 calc R . . H48B H 1.2682 1.1683 0.7896 0.276 Uiso 1 1 calc R . . H48C H 1.1470 1.1293 0.8061 0.276 Uiso 1 1 calc R . . Fe1 Fe 0.29739(5) 0.19067(4) 0.20423(3) 0.0585(2) Uani 1 1 d . . . N1 N 0.3875(2) 0.1978(2) 0.32085(17) 0.0535(7) Uani 1 1 d . . . N2 N 0.3851(3) 0.3481(2) 0.24356(16) 0.0530(7) Uani 1 1 d . . . N3 N 0.1468(3) 0.2344(3) 0.24782(18) 0.0630(8) Uani 1 1 d . . . N4 N 0.4393(3) 0.1464(3) 0.14952(18) 0.0660(9) Uani 1 1 d . . . N5 N -0.1322(3) 0.3202(3) 0.3365(2) 0.0759(10) Uani 1 1 d . . . N6 N 0.7056(4) 0.0671(3) 0.0420(2) 0.0855(11) Uani 1 1 d . . . O1 O 0.2302(2) 0.0386(2) 0.19329(16) 0.0718(8) Uani 1 1 d . . . O2 O 0.2259(2) 0.2206(2) 0.09974(14) 0.0635(7) Uani 1 1 d . . . O3 O 0.2394(4) -0.1307(3) 0.3684(2) 0.1339(16) Uani 1 1 d . . . O4 O 0.3492(3) 0.0106(2) 0.46135(19) 0.0873(9) Uani 1 1 d . . . O5 O 0.3332(3) 0.5885(3) 0.1494(2) 0.0952(10) Uani 1 1 d . . . O6 O 0.1673(3) 0.4988(2) 0.05928(19) 0.0932(10) Uani 1 1 d . . . O7 O 0.7013(2) 0.4395(2) 0.54801(14) 0.0641(7) Uani 1 1 d . . . O8 O 0.7002(2) 0.5857(2) 0.47249(17) 0.0749(8) Uani 1 1 d . . . C99A C 0.506(3) 0.177(3) 0.7389(14) 0.179(14) Uani 0.586(14) 1 d PD A 1 H99A H 0.4844 0.2366 0.7233 0.269 Uiso 0.586(14) 1 calc PR A 1 H99B H 0.4387 0.1196 0.7224 0.269 Uiso 0.586(14) 1 calc PR A 1 H99C H 0.5647 0.1567 0.7127 0.269 Uiso 0.586(14) 1 calc PR A 1 O9A O 0.5499(13) 0.2041(9) 0.8249(10) 0.228(7) Uani 0.586(14) 1 d PD A 1 H9A H 0.6036 0.2565 0.8395 0.343 Uiso 0.586(14) 1 calc PR A 1 C99B C 0.519(5) 0.196(3) 0.713(3) 0.21(2) Uani 0.414(14) 1 d P A 2 H99D H 0.6016 0.2051 0.7343 0.314 Uiso 0.414(14) 1 calc PR A 2 H99E H 0.4979 0.1589 0.6556 0.314 Uiso 0.414(14) 1 calc PR A 2 H99F H 0.4774 0.1565 0.7418 0.314 Uiso 0.414(14) 1 calc PR A 2 O9B O 0.4936(11) 0.2890(10) 0.7220(7) 0.136(6) Uani 0.414(14) 1 d P A 2 H9B H 0.4968 0.3147 0.7703 0.204 Uiso 0.414(14) 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 C1 0.072(3) 0.055(2) 0.076(3) -0.002(2) 0.029(2) 0.010(2) C2 0.061(2) 0.051(2) 0.066(2) 0.0050(19) 0.0171(19) 0.0066(19) C3 0.058(2) 0.053(2) 0.055(2) 0.0046(18) 0.0110(18) 0.0173(18) C4 0.048(2) 0.050(2) 0.0510(19) 0.0040(17) 0.0113(16) 0.0113(17) C5 0.056(2) 0.054(2) 0.052(2) 0.0088(17) 0.0056(17) 0.0097(18) C6 0.049(2) 0.058(2) 0.0488(19) 0.0070(18) 0.0097(16) 0.0131(18) C7 0.047(2) 0.054(2) 0.060(2) 0.0024(18) 0.0088(17) 0.0074(18) C8 0.055(2) 0.055(2) 0.059(2) 0.0077(18) 0.0095(18) 0.0133(18) C9 0.045(2) 0.054(2) 0.0463(19) 0.0051(17) 0.0067(16) 0.0123(17) C10 0.061(2) 0.057(2) 0.052(2) 0.0032(18) 0.0136(18) 0.0168(19) C11 0.061(2) 0.065(2) 0.049(2) 0.0100(18) 0.0094(17) 0.024(2) C12 0.069(3) 0.069(3) 0.049(2) 0.0061(19) 0.0084(18) 0.028(2) C13 0.078(3) 0.079(3) 0.059(2) 0.014(2) 0.011(2) 0.028(3) C14 0.173(6) 0.098(4) 0.106(4) 0.033(3) -0.007(4) 0.064(4) C15 0.126(4) 0.092(4) 0.066(3) 0.005(2) -0.022(3) 0.036(3) C16 0.109(4) 0.076(3) 0.089(3) -0.007(3) 0.016(3) -0.014(3) C17 0.079(3) 0.060(3) 0.095(3) 0.019(3) 0.025(3) 0.009(2) C18 0.133(5) 0.093(4) 0.099(4) 0.047(3) 0.025(3) 0.026(3) C19 0.072(3) 0.066(3) 0.069(3) 0.018(2) 0.010(2) 0.014(2) C20 0.073(3) 0.065(3) 0.071(3) 0.002(2) 0.008(2) 0.023(2) C21 0.066(3) 0.072(3) 0.053(2) -0.008(2) 0.005(2) 0.018(2) C22 0.077(3) 0.078(3) 0.066(2) 0.016(2) 0.025(2) 0.023(2) C23 0.081(3) 0.067(3) 0.064(2) 0.013(2) 0.016(2) 0.022(2) C24 0.090(4) 0.101(4) 0.098(4) -0.014(3) 0.017(3) 0.040(3) C25 0.107(4) 0.132(5) 0.091(4) 0.018(3) 0.042(3) 0.037(4) C26 0.063(3) 0.075(3) 0.057(2) -0.012(2) 0.011(2) 0.015(2) C27 0.061(3) 0.081(3) 0.057(2) -0.012(2) 0.003(2) 0.018(2) C28 0.055(2) 0.062(2) 0.054(2) 0.0002(18) 0.0128(18) 0.0164(19) C29 0.060(3) 0.067(3) 0.0450(19) -0.0039(17) 0.0080(18) 0.017(2) C30 0.057(2) 0.065(2) 0.053(2) 0.0021(18) 0.0100(18) 0.0158(19) C31 0.060(3) 0.133(5) 0.100(4) -0.015(3) 0.012(3) 0.027(3) C32 0.073(3) 0.109(4) 0.068(3) -0.013(2) 0.018(2) 0.034(3) C33 0.076(3) 0.074(3) 0.059(2) 0.016(2) 0.007(2) 0.013(2) C34 0.074(3) 0.076(3) 0.053(2) 0.010(2) 0.0035(19) 0.015(2) C35 0.077(3) 0.075(3) 0.068(3) 0.009(2) -0.002(2) 0.022(2) C36 0.076(3) 0.104(4) 0.069(3) 0.019(3) 0.002(2) 0.022(3) C37 0.082(3) 0.104(4) 0.077(3) 0.018(3) 0.003(2) 0.024(3) C38 0.074(3) 0.151(5) 0.085(3) 0.032(3) -0.010(3) 0.015(3) C39 0.084(4) 0.175(6) 0.094(4) 0.029(4) -0.001(3) 0.024(4) C40 0.100(5) 0.248(10) 0.132(6) 0.069(6) 0.009(4) 0.042(5) C41 0.105(5) 0.086(4) 0.130(5) 0.019(4) -0.012(4) -0.003(3) C42 0.137(7) 0.242(10) 0.124(6) 0.052(6) 0.046(5) 0.076(7) C43 0.111(5) 0.123(5) 0.114(4) 0.034(4) 0.042(4) 0.040(4) C44 0.244(11) 0.192(8) 0.133(6) 0.093(6) 0.096(7) 0.147(8) C45 0.164(7) 0.105(5) 0.130(5) 0.037(4) 0.032(5) 0.043(5) C46 0.267(12) 0.137(7) 0.119(6) 0.051(5) 0.067(7) 0.097(7) C47 0.178(8) 0.134(7) 0.165(8) 0.030(6) 0.014(7) 0.019(6) C48 0.307(12) 0.146(7) 0.120(6) 0.033(5) 0.068(7) 0.094(8) Fe1 0.0584(4) 0.0612(4) 0.0481(3) 0.0021(2) 0.0081(2) 0.0173(3) N1 0.0494(18) 0.0498(18) 0.0532(17) -0.0007(15) 0.0095(14) 0.0138(14) N2 0.0545(18) 0.0572(19) 0.0436(15) 0.0047(14) 0.0099(13) 0.0182(15) N3 0.063(2) 0.065(2) 0.0526(17) -0.0023(15) 0.0127(15) 0.0183(16) N4 0.071(2) 0.066(2) 0.0537(18) 0.0080(16) 0.0081(16) 0.0171(18) N5 0.055(2) 0.092(3) 0.063(2) -0.0095(18) 0.0081(16) 0.0212(19) N6 0.085(3) 0.096(3) 0.075(2) 0.006(2) 0.025(2) 0.037(2) O1 0.0720(19) 0.0669(18) 0.0587(16) -0.0063(14) 0.0130(14) 0.0049(14) O2 0.0733(18) 0.0614(17) 0.0480(14) 0.0008(12) 0.0079(12) 0.0232(14) O3 0.182(4) 0.072(2) 0.116(3) 0.028(2) 0.010(3) -0.026(3) O4 0.106(2) 0.0712(19) 0.080(2) 0.0252(17) 0.0122(18) 0.0153(17) O5 0.111(3) 0.068(2) 0.093(2) 0.0204(18) 0.001(2) 0.0158(19) O6 0.105(2) 0.079(2) 0.085(2) 0.0175(16) -0.0107(18) 0.0392(18) O7 0.0620(17) 0.0646(17) 0.0496(14) 0.0040(12) -0.0031(12) 0.0086(13) O8 0.0757(19) 0.0494(16) 0.0788(18) 0.0114(14) -0.0113(15) 0.0039(14) C99A 0.127(16) 0.18(3) 0.172(19) 0.000(16) -0.004(17) -0.001(13) O9A 0.266(14) 0.150(9) 0.231(15) 0.084(10) -0.006(12) -0.012(9) C99B 0.20(3) 0.097(19) 0.31(4) -0.04(2) 0.14(3) 0.024(19) O9B 0.116(9) 0.126(11) 0.129(8) 0.006(7) -0.021(7) 0.029(7) _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 O1 1.265(5) . ? C1 C2 1.429(6) . ? C1 C16 1.503(6) . ? C2 C3 1.429(5) . ? C2 C17 1.446(6) . ? C3 N1 1.283(5) . ? C3 H3 0.9300 . ? C4 C9 1.387(5) . ? C4 C5 1.402(5) . ? C4 N1 1.424(4) . ? C5 C6 1.371(5) . ? C5 H5 0.9300 . ? C6 O7 1.369(4) . ? C6 C7 1.394(5) . ? C7 O8 1.362(4) . ? C7 C8 1.382(5) . ? C8 C9 1.405(5) . ? C8 H8 0.9300 . ? C9 N2 1.425(4) . ? C10 N2 1.293(5) . ? C10 C11 1.435(5) . ? C10 H10 0.9300 . ? C11 C12 1.413(6) . ? C11 C13 1.454(6) . ? C12 O2 1.259(5) . ? C12 C15 1.515(5) . ? C13 O5 1.229(5) . ? C13 O6 1.338(5) . ? C14 O6 1.437(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 O3 1.198(5) . ? C17 O4 1.352(5) . ? C18 O4 1.420(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N4 1.345(5) . ? C19 C20 1.355(6) . ? C19 H19 0.9300 . ? C20 C21 1.403(6) . ? C20 H20 0.9300 . ? C21 N6 1.352(5) . ? C21 C22 1.400(6) . ? C22 C23 1.362(6) . ? C22 H22 0.9300 . ? C23 N4 1.332(5) . ? C23 H23 0.9300 . ? C24 N6 1.451(6) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N6 1.422(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N3 1.335(5) . ? C26 C27 1.355(5) . ? C26 H26 0.9300 . ? C27 C28 1.418(5) . ? C27 H27 0.9300 . ? C28 N5 1.341(5) . ? C28 C29 1.394(5) . ? C29 C30 1.368(5) . ? C29 H29 0.9300 . ? C30 N3 1.345(4) . ? C30 H30 0.9300 . ? C31 N5 1.442(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N5 1.462(5) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 O7 1.428(5) . ? C33 C34 1.518(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.493(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.524(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.490(6) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.530(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.495(7) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.441(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.391(7) . ? C41 O8 1.394(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.535(9) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.435(9) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.554(10) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.504(10) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.419(11) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.569(11) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? Fe1 O2 2.002(3) . ? Fe1 O1 2.012(3) . ? Fe1 N1 2.065(3) . ? Fe1 N2 2.080(3) . ? Fe1 N4 2.216(3) . ? Fe1 N3 2.217(3) . ? C99A O9A 1.414(18) . ? C99A H99A 0.9600 . ? C99A H99B 0.9600 . ? C99A H99C 0.9600 . ? O9A H9A 0.8200 . ? C99B O9B 1.32(4) . ? C99B H99D 0.9600 . ? C99B H99E 0.9600 . ? C99B H99F 0.9600 . ? O9B H9B 0.8200 . ? 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 C1 C2 122.3(4) . . ? O1 C1 C16 116.1(4) . . ? C2 C1 C16 121.7(4) . . ? C3 C2 C1 122.2(4) . . ? C3 C2 C17 117.4(4) . . ? C1 C2 C17 120.4(4) . . ? N1 C3 C2 128.5(4) . . ? N1 C3 H3 115.8 . . ? C2 C3 H3 115.8 . . ? C9 C4 C5 118.6(3) . . ? C9 C4 N1 117.3(3) . . ? C5 C4 N1 124.1(3) . . ? C6 C5 C4 121.9(3) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? O7 C6 C5 124.5(3) . . ? O7 C6 C7 116.0(3) . . ? C5 C6 C7 119.5(3) . . ? O8 C7 C8 124.1(4) . . ? O8 C7 C6 116.3(3) . . ? C8 C7 C6 119.6(3) . . ? C7 C8 C9 120.8(4) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C4 C9 C8 119.6(3) . . ? C4 C9 N2 116.2(3) . . ? C8 C9 N2 124.3(3) . . ? N2 C10 C11 126.9(4) . . ? N2 C10 H10 116.6 . . ? C11 C10 H10 116.6 . . ? C12 C11 C10 123.2(4) . . ? C12 C11 C13 124.2(3) . . ? C10 C11 C13 112.6(3) . . ? O2 C12 C11 122.6(3) . . ? O2 C12 C15 113.7(4) . . ? C11 C12 C15 123.7(4) . . ? O5 C13 O6 119.7(4) . . ? O5 C13 C11 124.4(4) . . ? O6 C13 C11 115.8(4) . . ? O6 C14 H14A 109.5 . . ? O6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 C16 H16A 109.5 . . ? C1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 O4 118.5(4) . . ? O3 C17 C2 128.0(5) . . ? O4 C17 C2 113.5(4) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C20 125.1(4) . . ? N4 C19 H19 117.5 . . ? C20 C19 H19 117.5 . . ? C19 C20 C21 120.3(4) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? N6 C21 C22 122.4(5) . . ? N6 C21 C20 122.8(4) . . ? C22 C21 C20 114.8(4) . . ? C23 C22 C21 120.1(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? N4 C23 C22 125.4(4) . . ? N4 C23 H23 117.3 . . ? C22 C23 H23 117.3 . . ? N6 C24 H24A 109.5 . . ? N6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C25 H25A 109.5 . . ? N6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 C27 125.8(3) . . ? N3 C26 H26 117.1 . . ? C27 C26 H26 117.1 . . ? C26 C27 C28 120.1(4) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? N5 C28 C29 123.3(3) . . ? N5 C28 C27 122.4(3) . . ? C29 C28 C27 114.3(3) . . ? C30 C29 C28 121.0(3) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? N3 C30 C29 124.5(4) . . ? N3 C30 H30 117.7 . . ? C29 C30 H30 117.7 . . ? N5 C31 H31A 109.5 . . ? N5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N5 C32 H32A 109.5 . . ? N5 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N5 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O7 C33 C34 109.4(3) . . ? O7 C33 H33A 109.8 . . ? C34 C33 H33A 109.8 . . ? O7 C33 H33B 109.8 . . ? C34 C33 H33B 109.8 . . ? H33A C33 H33B 108.2 . . ? C35 C34 C33 115.0(4) . . ? C35 C34 H34A 108.5 . . ? C33 C34 H34A 108.5 . . ? C35 C34 H34B 108.5 . . ? C33 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? C34 C35 C36 112.7(4) . . ? C34 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? C34 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C35 114.6(4) . . ? C37 C36 H36A 108.6 . . ? C35 C36 H36A 108.6 . . ? C37 C36 H36B 108.6 . . ? C35 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? C36 C37 C38 114.4(4) . . ? C36 C37 H37A 108.7 . . ? C38 C37 H37A 108.7 . . ? C36 C37 H37B 108.7 . . ? C38 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C39 C38 C37 114.3(5) . . ? C39 C38 H38A 108.7 . . ? C37 C38 H38A 108.7 . . ? C39 C38 H38B 108.7 . . ? C37 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C40 C39 C38 113.9(5) . . ? C40 C39 H39A 108.8 . . ? C38 C39 H39A 108.8 . . ? C40 C39 H39B 108.8 . . ? C38 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 O8 109.7(7) . . ? C42 C41 H41A 109.7 . . ? O8 C41 H41A 109.7 . . ? C42 C41 H41B 109.7 . . ? O8 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? C41 C42 C43 115.9(6) . . ? C41 C42 H42A 108.3 . . ? C43 C42 H42A 108.3 . . ? C41 C42 H42B 108.3 . . ? C43 C42 H42B 108.3 . . ? H42A C42 H42B 107.4 . . ? C44 C43 C42 113.5(7) . . ? C44 C43 H43A 108.9 . . ? C42 C43 H43A 108.9 . . ? C44 C43 H43B 108.9 . . ? C42 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C43 C44 C45 114.8(6) . . ? C43 C44 H44A 108.6 . . ? C45 C44 H44A 108.6 . . ? C43 C44 H44B 108.6 . . ? C45 C44 H44B 108.6 . . ? H44A C44 H44B 107.5 . . ? C46 C45 C44 117.8(8) . . ? C46 C45 H45A 107.9 . . ? C44 C45 H45A 107.9 . . ? C46 C45 H45B 107.9 . . ? C44 C45 H45B 107.9 . . ? H45A C45 H45B 107.2 . . ? C47 C46 C45 119.6(8) . . ? C47 C46 H46A 107.4 . . ? C45 C46 H46A 107.4 . . ? C47 C46 H46B 107.4 . . ? C45 C46 H46B 107.4 . . ? H46A C46 H46B 107.0 . . ? C46 C47 C48 120.4(9) . . ? C46 C47 H47A 107.2 . . ? C48 C47 H47A 107.2 . . ? C46 C47 H47B 107.2 . . ? C48 C47 H47B 107.2 . . ? H47A C47 H47B 106.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O2 Fe1 O1 107.16(11) . . ? O2 Fe1 N1 166.38(12) . . ? O1 Fe1 N1 86.36(12) . . ? O2 Fe1 N2 86.32(11) . . ? O1 Fe1 N2 166.46(11) . . ? N1 Fe1 N2 80.13(12) . . ? O2 Fe1 N4 88.72(11) . . ? O1 Fe1 N4 90.37(12) . . ? N1 Fe1 N4 92.86(11) . . ? N2 Fe1 N4 91.16(12) . . ? O2 Fe1 N3 86.30(11) . . ? O1 Fe1 N3 89.98(12) . . ? N1 Fe1 N3 92.25(11) . . ? N2 Fe1 N3 89.69(12) . . ? N4 Fe1 N3 174.89(11) . . ? C3 N1 C4 121.2(3) . . ? C3 N1 Fe1 125.8(2) . . ? C4 N1 Fe1 112.9(2) . . ? C10 N2 C9 121.2(3) . . ? C10 N2 Fe1 125.4(2) . . ? C9 N2 Fe1 112.9(2) . . ? C26 N3 C30 114.3(3) . . ? C26 N3 Fe1 124.5(2) . . ? C30 N3 Fe1 121.2(3) . . ? C23 N4 C19 114.3(4) . . ? C23 N4 Fe1 121.6(3) . . ? C19 N4 Fe1 124.1(3) . . ? C28 N5 C31 121.7(3) . . ? C28 N5 C32 121.4(3) . . ? C31 N5 C32 116.7(4) . . ? C21 N6 C25 121.2(4) . . ? C21 N6 C24 121.3(5) . . ? C25 N6 C24 117.4(4) . . ? C1 O1 Fe1 133.5(2) . . ? C12 O2 Fe1 132.7(2) . . ? C17 O4 C18 116.9(4) . . ? C13 O6 C14 116.2(4) . . ? C6 O7 C33 116.2(3) . . ? C7 O8 C41 117.0(3) . . ? C99A O9A H9A 109.5 . . ? O9B C99B H99D 109.5 . . ? O9B C99B H99E 109.5 . . ? H99D C99B H99E 109.5 . . ? O9B C99B H99F 109.5 . . ? H99D C99B H99F 109.5 . . ? H99E C99B H99F 109.5 . . ? C99B O9B H9B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.59 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.818 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.068 _iucr_refine_instructions_details ; TITL w023 P 1 New: P-1 CELL 0.71073 12.0361 13.4241 17.3275 103.289 101.608 99.935 ZERR 2.00 0.0008 0.0010 0.0013 0.006 0.006 0.006 LATT 1 SFAC C H FE N O UNIT 98 148 2 12 18 MERG 2 DFIX 1.43 C99a O9a DFIX 1.540 0.010 C41 C42 FMAP 2 PLAN 15 ACTA BOND $H L.S. 30 TEMP 0.00 WGHT 0.089100 FVAR 0.44968 0.58601 C1 1 0.228683 -0.015771 0.243972 11.00000 0.07154 0.05475 = 0.07636 -0.00189 0.02922 0.01002 C2 1 0.295306 0.023834 0.327243 11.00000 0.06056 0.05148 = 0.06640 0.00497 0.01714 0.00660 C3 1 0.369924 0.126795 0.358404 11.00000 0.05809 0.05317 = 0.05490 0.00460 0.01099 0.01734 AFIX 43 H3 2 0.411140 0.144702 0.413023 11.00000 -1.20000 AFIX 0 C4 1 0.468012 0.296007 0.360860 11.00000 0.04807 0.04967 = 0.05098 0.00404 0.01130 0.01130 C5 1 0.546874 0.317729 0.437422 11.00000 0.05616 0.05373 = 0.05217 0.00877 0.00556 0.00966 AFIX 43 H5 2 0.548513 0.265165 0.464185 11.00000 -1.20000 AFIX 0 C6 1 0.621631 0.414190 0.473975 11.00000 0.04941 0.05791 = 0.04884 0.00697 0.00973 0.01314 C7 1 0.621288 0.492899 0.433712 11.00000 0.04744 0.05406 = 0.06017 0.00241 0.00878 0.00739 C8 1 0.545448 0.472741 0.357631 11.00000 0.05491 0.05495 = 0.05868 0.00769 0.00950 0.01327 AFIX 43 H8 2 0.545918 0.524986 0.330467 11.00000 -1.20000 AFIX 0 C9 1 0.467654 0.374321 0.320810 11.00000 0.04541 0.05386 = 0.04635 0.00512 0.00669 0.01230 C10 1 0.360414 0.419924 0.208891 11.00000 0.06135 0.05719 = 0.05196 0.00319 0.01361 0.01682 AFIX 43 H10 2 0.401080 0.488681 0.236088 11.00000 -1.20000 AFIX 0 C11 1 0.276904 0.404772 0.132869 11.00000 0.06071 0.06488 = 0.04930 0.00999 0.00937 0.02427 C12 1 0.214284 0.304543 0.081681 11.00000 0.06940 0.06855 = 0.04933 0.00612 0.00835 0.02772 C13 1 0.264167 0.503448 0.114919 11.00000 0.07830 0.07914 = 0.05887 0.01375 0.01099 0.02799 C14 1 0.151160 0.596835 0.044103 11.00000 0.17267 0.09757 = 0.10614 0.03280 -0.00657 0.06389 AFIX 137 H14A 2 0.121452 0.634615 0.086493 11.00000 -1.50000 H14B 2 0.096787 0.583308 -0.007976 11.00000 -1.50000 H14C 2 0.224488 0.638071 0.043654 11.00000 -1.50000 AFIX 0 C15 1 0.129265 0.287369 -0.000125 11.00000 0.12572 0.09216 = 0.06641 0.00516 -0.02233 0.03583 AFIX 137 H15A 2 0.108035 0.213876 -0.028739 11.00000 -1.50000 H15B 2 0.165111 0.326417 -0.032178 11.00000 -1.50000 H15C 2 0.060765 0.310929 0.008693 11.00000 -1.50000 AFIX 0 C16 1 0.153154 -0.125367 0.211327 11.00000 0.10893 0.07585 = 0.08885 -0.00700 0.01564 -0.01350 AFIX 137 H16A 2 0.102991 -0.132511 0.158773 11.00000 -1.50000 H16B 2 0.106754 -0.138413 0.248546 11.00000 -1.50000 H16C 2 0.201485 -0.175166 0.205815 11.00000 -1.50000 AFIX 0 C17 1 0.289828 -0.040728 0.383260 11.00000 0.07905 0.06017 = 0.09468 0.01920 0.02540 0.00860 C18 1 0.351148 -0.048414 0.519750 11.00000 0.13265 0.09346 = 0.09934 0.04678 0.02468 0.02633 AFIX 137 H18A 2 0.272731 -0.077616 0.520235 11.00000 -1.50000 H18B 2 0.392199 -0.003250 0.573107 11.00000 -1.50000 H18C 2 0.389820 -0.104248 0.505387 11.00000 -1.50000 AFIX 0 C19 1 0.485463 0.064234 0.158688 11.00000 0.07220 0.06628 = 0.06918 0.01764 0.01026 0.01420 AFIX 43 H19 2 0.456011 0.024129 0.190359 11.00000 -1.20000 AFIX 0 C20 1 0.571634 0.035328 0.125339 11.00000 0.07329 0.06498 = 0.07116 0.00221 0.00755 0.02253 AFIX 43 H20 2 0.598544 -0.022999 0.134263 11.00000 -1.20000 AFIX 0 C21 1 0.620433 0.093015 0.077406 11.00000 0.06629 0.07194 = 0.05302 -0.00779 0.00466 0.01844 C22 1 0.573541 0.179379 0.068534 11.00000 0.07708 0.07810 = 0.06625 0.01630 0.02511 0.02283 AFIX 43 H22 2 0.601033 0.221288 0.037371 11.00000 -1.20000 AFIX 0 C23 1 0.487698 0.202146 0.105470 11.00000 0.08050 0.06687 = 0.06369 0.01275 0.01567 0.02158 AFIX 43 H23 2 0.460700 0.261479 0.099426 11.00000 -1.20000 AFIX 0 C24 1 0.754427 -0.021608 0.053365 11.00000 0.08960 0.10116 = 0.09784 -0.01415 0.01696 0.03997 AFIX 137 H24A 2 0.787065 -0.011462 0.110683 11.00000 -1.50000 H24B 2 0.814352 -0.027041 0.024529 11.00000 -1.50000 H24C 2 0.694151 -0.085021 0.032424 11.00000 -1.50000 AFIX 0 C25 1 0.754876 0.128991 -0.004556 11.00000 0.10657 0.13229 = 0.09076 0.01790 0.04153 0.03673 AFIX 137 H25A 2 0.693761 0.138107 -0.045560 11.00000 -1.50000 H25B 2 0.806369 0.094144 -0.030566 11.00000 -1.50000 H25C 2 0.797758 0.196496 0.031045 11.00000 -1.50000 AFIX 0 C26 1 0.035593 0.195752 0.206043 11.00000 0.06263 0.07546 = 0.05718 -0.01189 0.01105 0.01518 AFIX 43 H26 2 0.021169 0.147540 0.155108 11.00000 -1.20000 AFIX 0 C27 1 -0.058082 0.220574 0.231290 11.00000 0.06130 0.08095 = 0.05720 -0.01239 0.00254 0.01752 AFIX 43 H27 2 -0.132790 0.189496 0.198156 11.00000 -1.20000 AFIX 0 C28 1 -0.042389 0.293885 0.308175 11.00000 0.05536 0.06232 = 0.05356 0.00022 0.01276 0.01643 C29 1 0.073749 0.335706 0.351316 11.00000 0.05997 0.06731 = 0.04502 -0.00386 0.00803 0.01742 AFIX 43 H29 2 0.091337 0.384681 0.402204 11.00000 -1.20000 AFIX 0 C30 1 0.162208 0.305798 0.319932 11.00000 0.05739 0.06481 = 0.05260 0.00210 0.01004 0.01584 AFIX 43 H30 2 0.238257 0.336986 0.350562 11.00000 -1.20000 AFIX 0 C31 1 -0.251324 0.273050 0.291016 11.00000 0.05966 0.13311 = 0.10026 -0.01535 0.01180 0.02700 AFIX 137 H31A 2 -0.261807 0.280455 0.236379 11.00000 -1.50000 H31B 2 -0.302532 0.307566 0.317611 11.00000 -1.50000 H31C 2 -0.268937 0.199771 0.288812 11.00000 -1.50000 AFIX 0 C32 1 -0.114130 0.389693 0.418542 11.00000 0.07299 0.10943 = 0.06807 -0.01341 0.01827 0.03432 AFIX 137 H32A 2 -0.082811 0.356343 0.458659 11.00000 -1.50000 H32B 2 -0.187191 0.403894 0.426327 11.00000 -1.50000 H32C 2 -0.060536 0.454504 0.424548 11.00000 -1.50000 AFIX 0 C33 1 0.693155 0.363883 0.593801 11.00000 0.07587 0.07374 = 0.05895 0.01614 0.00727 0.01330 AFIX 23 H33A 2 0.705718 0.298427 0.563130 11.00000 -1.20000 H33B 2 0.615981 0.350040 0.603333 11.00000 -1.20000 AFIX 0 C34 1 0.784219 0.405836 0.675130 11.00000 0.07375 0.07580 = 0.05321 0.01046 0.00352 0.01454 AFIX 23 H34A 2 0.782146 0.478126 0.698925 11.00000 -1.20000 H34B 2 0.763204 0.365476 0.711942 11.00000 -1.20000 AFIX 0 C35 1 0.906045 0.402449 0.670370 11.00000 0.07729 0.07476 = 0.06827 0.00932 -0.00179 0.02239 AFIX 23 H35A 2 0.927495 0.442012 0.633183 11.00000 -1.20000 H35B 2 0.909369 0.330120 0.648056 11.00000 -1.20000 AFIX 0 C36 1 0.993744 0.447434 0.753482 11.00000 0.07630 0.10385 = 0.06948 0.01947 0.00223 0.02247 AFIX 23 H36A 2 0.989293 0.519454 0.775708 11.00000 -1.20000 H36B 2 0.971665 0.407633 0.790366 11.00000 -1.20000 AFIX 0 C37 1 1.116796 0.446178 0.751746 11.00000 0.08173 0.10385 = 0.07651 0.01798 0.00301 0.02367 AFIX 23 H37A 2 1.139904 0.488227 0.716527 11.00000 -1.20000 H37B 2 1.120795 0.374545 0.727638 11.00000 -1.20000 AFIX 0 C38 1 1.203938 0.487688 0.835791 11.00000 0.07439 0.15105 = 0.08462 0.03157 -0.00959 0.01539 AFIX 23 H38A 2 1.200644 0.559610 0.859639 11.00000 -1.20000 H38B 2 1.180373 0.446162 0.871220 11.00000 -1.20000 AFIX 0 C39 1 1.327112 0.485199 0.833966 11.00000 0.08417 0.17491 = 0.09442 0.02922 -0.00102 0.02355 AFIX 23 H39A 2 1.328436 0.416483 0.801246 11.00000 -1.20000 H39B 2 1.355603 0.536779 0.807239 11.00000 -1.20000 AFIX 0 C40 1 1.404910 0.506310 0.913758 11.00000 0.09986 0.24814 = 0.13205 0.06889 0.00929 0.04201 AFIX 137 H40A 2 1.390491 0.565113 0.950638 11.00000 -1.50000 H40B 2 1.484092 0.522303 0.909795 11.00000 -1.50000 H40C 2 1.391983 0.445581 0.934006 11.00000 -1.50000 AFIX 0 C41 1 0.674241 0.675395 0.452573 11.00000 0.10461 0.08634 = 0.12974 0.01892 -0.01170 -0.00282 AFIX 23 H41A 2 0.595027 0.658780 0.419004 11.00000 -1.20000 H41B 2 0.680213 0.729413 0.502199 11.00000 -1.20000 AFIX 0 C42 1 0.751477 0.712200 0.410096 11.00000 0.13688 0.24220 = 0.12400 0.05211 0.04582 0.07619 AFIX 23 H42A 2 0.723732 0.766409 0.388437 11.00000 -1.20000 H42B 2 0.749698 0.654836 0.363775 11.00000 -1.20000 AFIX 0 C43 1 0.878602 0.757300 0.459595 11.00000 0.11116 0.12340 = 0.11377 0.03394 0.04167 0.03969 AFIX 23 H43A 2 0.907725 0.702992 0.480300 11.00000 -1.20000 H43B 2 0.925122 0.776642 0.423378 11.00000 -1.20000 AFIX 0 C44 1 0.893457 0.847493 0.527167 11.00000 0.24404 0.19230 = 0.13263 0.09298 0.09626 0.14733 AFIX 23 H44A 2 0.852226 0.826338 0.565571 11.00000 -1.20000 H44B 2 0.857591 0.898974 0.506892 11.00000 -1.20000 AFIX 0 C45 1 1.022180 0.900881 0.573870 11.00000 0.16378 0.10502 = 0.12958 0.03651 0.03193 0.04286 AFIX 23 H45A 2 1.057552 0.848425 0.592995 11.00000 -1.20000 H45B 2 1.062592 0.921506 0.534899 11.00000 -1.20000 AFIX 0 C46 1 1.044447 0.995551 0.645882 11.00000 0.26717 0.13731 = 0.11868 0.05137 0.06730 0.09705 AFIX 23 H46A 2 1.011091 1.048503 0.625976 11.00000 -1.20000 H46B 2 1.000949 0.975242 0.683423 11.00000 -1.20000 AFIX 0 C47 1 1.160443 1.044482 0.691996 11.00000 0.17774 0.13414 = 0.16516 0.03025 0.01374 0.01914 AFIX 23 H47A 2 1.204402 1.062377 0.653974 11.00000 -1.20000 H47B 2 1.192750 0.991931 0.713246 11.00000 -1.20000 AFIX 0 C48 1 1.185801 1.145357 0.765623 11.00000 0.30711 0.14599 = 0.11973 0.03302 0.06798 0.09398 AFIX 137 H48A 2 1.157681 1.200164 0.746294 11.00000 -1.50000 H48B 2 1.268233 1.168326 0.789574 11.00000 -1.50000 H48C 2 1.147006 1.129312 0.806056 11.00000 -1.50000 AFIX 0 FE1 3 0.297387 0.190669 0.204227 11.00000 0.05841 0.06117 = 0.04814 0.00207 0.00807 0.01728 N1 4 0.387479 0.197777 0.320847 11.00000 0.04937 0.04979 = 0.05318 -0.00074 0.00949 0.01383 N2 4 0.385091 0.348121 0.243563 11.00000 0.05446 0.05722 = 0.04363 0.00473 0.00986 0.01821 N3 4 0.146799 0.234381 0.247817 11.00000 0.06267 0.06489 = 0.05255 -0.00226 0.01274 0.01826 N4 4 0.439270 0.146408 0.149521 11.00000 0.07073 0.06621 = 0.05372 0.00799 0.00808 0.01714 N5 4 -0.132175 0.320167 0.336460 11.00000 0.05520 0.09189 = 0.06343 -0.00951 0.00807 0.02125 N6 4 0.705624 0.067128 0.041965 11.00000 0.08511 0.09601 = 0.07455 0.00556 0.02490 0.03731 O1 5 0.230234 0.038619 0.193295 11.00000 0.07198 0.06686 = 0.05866 -0.00626 0.01301 0.00489 O2 5 0.225871 0.220611 0.099740 11.00000 0.07333 0.06135 = 0.04799 0.00076 0.00789 0.02319 O3 5 0.239409 -0.130702 0.368406 11.00000 0.18166 0.07202 = 0.11604 0.02755 0.01028 -0.02552 O4 5 0.349216 0.010560 0.461351 11.00000 0.10617 0.07119 = 0.07985 0.02525 0.01221 0.01528 O5 5 0.333167 0.588497 0.149391 11.00000 0.11098 0.06818 = 0.09261 0.02043 0.00080 0.01575 O6 5 0.167253 0.498837 0.059275 11.00000 0.10519 0.07860 = 0.08470 0.01746 -0.01071 0.03919 O7 5 0.701307 0.439533 0.548012 11.00000 0.06202 0.06465 = 0.04959 0.00401 -0.00311 0.00857 O8 5 0.700197 0.585689 0.472495 11.00000 0.07574 0.04939 = 0.07876 0.01145 -0.01133 0.00386 PART 1 C99A 1 0.505869 0.177078 0.738947 21.00000 0.12667 0.18140 = 0.17223 0.00008 -0.00423 -0.00122 AFIX 137 H99A 2 0.484372 0.236592 0.723287 21.00000 -1.50000 H99B 2 0.438662 0.119597 0.722447 21.00000 -1.50000 H99C 2 0.564687 0.156676 0.712734 21.00000 -1.50000 AFIX 0 O9A 5 0.549885 0.204129 0.824918 21.00000 0.26650 0.15022 = 0.23119 0.08383 -0.00624 -0.01204 AFIX 83 H9A 2 0.603647 0.256500 0.839477 21.00000 -1.50000 AFIX 0 PART 2 C99B 1 0.519379 0.196031 0.712791 -21.00000 0.20213 0.09701 = 0.31138 -0.03525 0.13809 0.02420 AFIX 137 H99D 2 0.601571 0.205072 0.734280 -21.00000 -1.50000 H99E 2 0.497943 0.158877 0.655643 -21.00000 -1.50000 H99F 2 0.477362 0.156505 0.741773 -21.00000 -1.50000 AFIX 0 O9B 5 0.493629 0.288964 0.721961 -21.00000 0.11572 0.12600 = 0.12906 0.00588 -0.02096 0.02919 AFIX 147 H9B 2 0.496796 0.314688 0.770320 -21.00000 -1.50000 HKLF 4 REM w023 P 1 New: P-1 REM R1 = 0.0660 for 4893 Fo > 4sig(Fo) and 0.1055 for all 8697 data REM 618 parameters refined using 2 restraints END WGHT 0.0891 0.0000 REM Highest difference peak 0.818, deepest hole -0.413, 1-sigma level 0.068 Q1 1 0.7636 0.7688 0.4868 11.00000 0.05 0.82 Q2 1 0.3327 0.2568 0.1766 11.00000 0.05 0.63 Q3 1 0.2656 0.1250 0.2307 11.00000 0.05 0.60 Q4 1 0.1990 0.1236 0.1815 11.00000 0.05 0.49 Q5 1 0.3997 0.2477 0.2151 11.00000 0.05 0.40 Q6 1 0.1975 0.2125 0.2152 11.00000 0.05 0.33 Q7 1 0.1826 0.1646 0.1314 11.00000 0.05 0.28 Q8 1 0.9881 0.8656 0.5022 11.00000 0.05 0.27 Q9 1 0.7258 0.6399 0.4192 11.00000 0.05 0.26 Q10 1 0.7278 0.5028 0.5122 11.00000 0.05 0.25 Q11 1 1.3187 0.3880 0.8533 11.00000 0.05 0.23 Q12 1 0.4533 0.1602 0.1357 11.00000 0.05 0.23 Q13 1 0.4265 0.3924 0.2198 11.00000 0.05 0.22 Q14 1 0.3604 0.1218 0.2252 11.00000 0.05 0.21 Q15 1 0.6600 0.4604 0.4498 11.00000 0.05 0.21 ; _database_code_depnum_ccdc_archive 'CCDC 944437' ####################################################################### # # 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_w027 # start Validation Reply Form _vrf_THETM01_w027 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: weakly diffracting crystal ; _vrf_PLAT220_w027 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.7 Ratio RESPONSE: disorder of alkyl chain that could not be resolved ; _vrf_PLAT234_w027 ; PROBLEM: Large Hirshfeld Difference C138 -- C139 .. 0.28 Ang. RESPONSE: disorder of alkyl chain that could not be resolved ; _vrf_PLAT241_w027 ; PROBLEM: High Ueq as Compared to Neighbors for ..... C140 Check RESPONSE: disorder of alkyl chain that could not be resolved ; _vrf_PLAT341_w027 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0171 Ang. RESPONSE: disorder of alkyl chain that could not be resolved ; _vrf_PLAT360_w027 ; PROBLEM: Short C(sp3)-C(sp3) Bond C140 - C141 ... 1.27 Ang. RESPONSE: disorder of alkyl chain that could not be resolved ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Fe12i(C8)(dmap)]' _chemical_melting_point ? _chemical_formula_moiety 'C41 H60 Fe N4 O8' _chemical_formula_sum 'C41 H60 Fe N4 O8' _chemical_formula_weight 792.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 19.8161(9) _cell_length_b 8.2415(4) _cell_length_c 25.5905(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.224(3) _cell_angle_gamma 90.00 _cell_volume 4136.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 38465 _cell_measurement_theta_min 1.04 _cell_measurement_theta_max 23.29 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.419 _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 133(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDSII _diffrn_measurement_method Omega-Scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5508 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 23.29 _reflns_number_total 5508 _reflns_number_gt 4397 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-AREA-STOE _computing_cell_refinement X-AREA-STOE _computing_data_reduction X-AREA-STOE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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. A twin refinement was conducted based on twin law 2-axis ( 0 0 1 ) [ 2 0 11 ], Angle () [] = 0.13 Deg, Freq = 60 (-1.000 0.000 0.000) (h1) (h2) Nr Overlap = 2373 ( 0.000 -1.000 0.000) * (k1) = (k2) BASF = 0.47 ( 0.369 0.000 1.000) (l1) (l2) DEL-R =-0.273 found by PLATON. ; _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^)+(0.0347P)^2^+32.6890P] 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 5508 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.2606 _refine_ls_wR_factor_gt 0.2535 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _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 0.25273(7) 1.0063(2) 0.19012(6) 0.0443(4) Uani 1 1 d . . . O101 O 0.3255(4) 1.1206(9) 0.1586(3) 0.0489(18) Uani 1 1 d . . . O102 O 0.1710(4) 1.1140(10) 0.1506(3) 0.053(2) Uani 1 1 d . . . O103 O -0.0076(4) 0.9867(11) 0.2452(3) 0.062(2) Uani 1 1 d . . . O104 O 0.5173(4) 1.1164(10) 0.2897(3) 0.061(2) Uani 1 1 d . . . O105 O 0.3434(3) 0.7303(9) 0.4330(3) 0.0450(18) Uani 1 1 d . . . O106 O 0.2129(3) 0.6934(9) 0.4223(2) 0.0445(17) Uani 1 1 d . . . O107 O -0.0284(4) 1.1754(10) 0.1836(3) 0.057(2) Uani 1 1 d . . . O108 O 0.5348(4) 1.1909(11) 0.2087(3) 0.065(2) Uani 1 1 d . . . N101 N 0.3252(4) 0.9754(10) 0.2560(3) 0.040(2) Uani 1 1 d . . . N102 N 0.1902(4) 0.9468(10) 0.2455(3) 0.040(2) Uani 1 1 d . . . N103 N 0.2537(4) 0.8006(11) 0.1400(3) 0.047(2) Uani 1 1 d . . . N104 N 0.2529(5) 0.4147(11) 0.0331(3) 0.053(2) Uani 1 1 d . . . C101 C 0.3889(6) 1.1511(13) 0.1734(4) 0.046(3) Uani 1 1 d . . . C102 C 0.4219(5) 1.1065(12) 0.2234(4) 0.043(3) Uani 1 1 d . . . C103 C 0.3885(5) 1.0258(12) 0.2614(4) 0.041(2) Uani 1 1 d . . . H103 H 0.4151 1.0059 0.2946 0.050 Uiso 1 1 calc R . . C104 C 0.2991(5) 0.9002(12) 0.2983(4) 0.039(2) Uani 1 1 d . . . C105 C 0.3390(5) 0.8461(12) 0.3450(4) 0.040(2) Uani 1 1 d . . . H105 H 0.3872 0.8557 0.3486 0.047 Uiso 1 1 calc R . . C106 C 0.3091(5) 0.7795(12) 0.3855(4) 0.036(2) Uani 1 1 d . . . C107 C 0.2380(5) 0.7593(13) 0.3794(4) 0.045(3) Uani 1 1 d . . . C108 C 0.1978(5) 0.8058(12) 0.3332(4) 0.040(2) Uani 1 1 d . . . H108 H 0.1500 0.7875 0.3287 0.048 Uiso 1 1 calc R . . C109 C 0.2281(5) 0.8807(12) 0.2930(4) 0.038(2) Uani 1 1 d . . . C110 C 0.1259(5) 0.9805(13) 0.2438(4) 0.041(2) Uani 1 1 d . . . H110 H 0.1050 0.9489 0.2733 0.050 Uiso 1 1 calc R . . C111 C 0.0833(5) 1.0615(12) 0.2012(4) 0.043(3) Uani 1 1 d . . . C112 C 0.1093(5) 1.1248(13) 0.1576(4) 0.049(3) Uani 1 1 d . . . C113 C 0.0119(6) 1.0832(15) 0.2084(4) 0.054(3) Uani 1 1 d . . . C114 C -0.0771(5) 1.004(2) 0.2539(5) 0.077(4) Uani 1 1 d . . . H11A H -0.0867 0.9265 0.2810 0.115 Uiso 1 1 calc R . . H11B H -0.1075 0.9817 0.2209 0.115 Uiso 1 1 calc R . . H11C H -0.0848 1.1145 0.2656 0.115 Uiso 1 1 calc R . . C115 C 0.0636(6) 1.2114(17) 0.1140(4) 0.064(3) Uani 1 1 d . . . H11D H 0.0908 1.2484 0.0871 0.096 Uiso 1 1 calc R . . H11E H 0.0424 1.3051 0.1287 0.096 Uiso 1 1 calc R . . H11F H 0.0281 1.1369 0.0978 0.096 Uiso 1 1 calc R . . C116 C 0.4233(6) 1.2412(15) 0.1326(4) 0.060(3) Uani 1 1 d . . . H11G H 0.3886 1.2790 0.1040 0.090 Uiso 1 1 calc R . . H11H H 0.4550 1.1682 0.1182 0.090 Uiso 1 1 calc R . . H11I H 0.4484 1.3345 0.1493 0.090 Uiso 1 1 calc R . . C117 C 0.4960(6) 1.1412(14) 0.2370(5) 0.053(3) Uani 1 1 d . . . C118 C 0.5900(6) 1.1456(18) 0.3060(5) 0.074(4) Uani 1 1 d . . . H11J H 0.6019 1.1191 0.3436 0.111 Uiso 1 1 calc R . . H11K H 0.6002 1.2601 0.3004 0.111 Uiso 1 1 calc R . . H11L H 0.6165 1.0773 0.2851 0.111 Uiso 1 1 calc R . . C119 C 0.2735(5) 0.8168(13) 0.0927(4) 0.044(3) Uani 1 1 d . . . H119 H 0.2890 0.9209 0.0838 0.052 Uiso 1 1 calc R . . C120 C 0.2733(5) 0.6966(14) 0.0560(5) 0.050(3) Uani 1 1 d . . . H120 H 0.2868 0.7196 0.0226 0.060 Uiso 1 1 calc R . . C121 C 0.2526(5) 0.5359(13) 0.0678(4) 0.047(3) Uani 1 1 d . . . C122 C 0.2329(6) 0.5197(14) 0.1186(4) 0.052(3) Uani 1 1 d . . . H122 H 0.2190 0.4166 0.1298 0.063 Uiso 1 1 calc R . . C123 C 0.2334(5) 0.6504(14) 0.1516(4) 0.047(3) Uani 1 1 d . . . H123 H 0.2186 0.6343 0.1849 0.057 Uiso 1 1 calc R . . C124 C 0.2757(7) 0.4400(15) -0.0177(4) 0.065(3) Uani 1 1 d . . . H12A H 0.2791 0.3351 -0.0352 0.098 Uiso 1 1 calc R . . H12B H 0.3205 0.4926 -0.0125 0.098 Uiso 1 1 calc R . . H12C H 0.2430 0.5092 -0.0398 0.098 Uiso 1 1 calc R . . C125 C 0.2292(8) 0.2545(15) 0.0437(5) 0.073(4) Uani 1 1 d . . . H12D H 0.2309 0.1852 0.0128 0.110 Uiso 1 1 calc R . . H12E H 0.1822 0.2608 0.0513 0.110 Uiso 1 1 calc R . . H12F H 0.2585 0.2085 0.0742 0.110 Uiso 1 1 calc R . . C126 C 0.4144(5) 0.7651(14) 0.4436(4) 0.045(3) Uani 1 1 d . . . H12G H 0.4229 0.8816 0.4376 0.054 Uiso 1 1 calc R . . H12H H 0.4399 0.7000 0.4204 0.054 Uiso 1 1 calc R . . C127 C 0.4365(6) 0.7207(15) 0.5014(4) 0.054(3) Uani 1 1 d . . . H12I H 0.4236 0.6068 0.5072 0.064 Uiso 1 1 calc R . . H12J H 0.4123 0.7909 0.5240 0.064 Uiso 1 1 calc R . . C128 C 0.5138(5) 0.7404(14) 0.5176(4) 0.050(3) Uani 1 1 d . . . H12K H 0.5383 0.6726 0.4945 0.060 Uiso 1 1 calc R . . H12L H 0.5267 0.8550 0.5130 0.060 Uiso 1 1 calc R . . C129 C 0.5349(5) 0.6902(14) 0.5751(4) 0.049(3) Uani 1 1 d . . . H12M H 0.5194 0.5776 0.5797 0.058 Uiso 1 1 calc R . . H12N H 0.5113 0.7612 0.5979 0.058 Uiso 1 1 calc R . . C130 C 0.6117(5) 0.6991(14) 0.5937(4) 0.046(3) Uani 1 1 d . . . H13A H 0.6356 0.6352 0.5692 0.056 Uiso 1 1 calc R . . H13B H 0.6267 0.8134 0.5919 0.056 Uiso 1 1 calc R . . C131 C 0.6329(5) 0.6368(15) 0.6492(4) 0.050(3) Uani 1 1 d . . . H13C H 0.6210 0.5203 0.6504 0.060 Uiso 1 1 calc R . . H13D H 0.6065 0.6951 0.6734 0.060 Uiso 1 1 calc R . . C32A C 0.7086(5) 0.6571(15) 0.6690(4) 0.052(3) Uani 1 1 d . . . H32A H 0.7350 0.5981 0.6450 0.063 Uiso 1 1 calc R . . H32B H 0.7205 0.7735 0.6677 0.063 Uiso 1 1 calc R . . C33A C 0.7292(6) 0.5952(15) 0.7249(4) 0.060(3) Uani 1 1 d . . . H33A H 0.7784 0.6096 0.7351 0.090 Uiso 1 1 calc R . . H33B H 0.7178 0.4797 0.7266 0.090 Uiso 1 1 calc R . . H33C H 0.7047 0.6562 0.7492 0.090 Uiso 1 1 calc R . . C134 C 0.1429(6) 0.6462(16) 0.4145(4) 0.054(3) Uani 1 1 d . . . H13J H 0.1363 0.5512 0.3906 0.065 Uiso 1 1 calc R . . H13K H 0.1143 0.7363 0.3982 0.065 Uiso 1 1 calc R . . C135 C 0.1224(6) 0.6034(15) 0.4679(4) 0.056(3) Uani 1 1 d . . . H13L H 0.0870 0.5179 0.4629 0.067 Uiso 1 1 calc R . . H13M H 0.1625 0.5585 0.4908 0.067 Uiso 1 1 calc R . . C136 C 0.0955(6) 0.7455(16) 0.4953(4) 0.061(3) Uani 1 1 d . . . H13N H 0.0574 0.7956 0.4715 0.073 Uiso 1 1 calc R . . H13O H 0.1320 0.8278 0.5029 0.073 Uiso 1 1 calc R . . C137 C 0.0706(6) 0.6961(19) 0.5466(5) 0.071(4) Uani 1 1 d . . . H13P H 0.0448 0.5933 0.5408 0.085 Uiso 1 1 calc R . . H13Q H 0.1106 0.6758 0.5737 0.085 Uiso 1 1 calc R . . C138 C 0.0256(10) 0.823(2) 0.5672(6) 0.117(7) Uani 1 1 d . . . H13R H -0.0142 0.8443 0.5400 0.140 Uiso 1 1 calc R . . H13S H 0.0516 0.9253 0.5735 0.140 Uiso 1 1 calc R . . C139 C 0.0001(13) 0.771(3) 0.6184(8) 0.164(11) Uani 1 1 d . . . H13T H -0.0105 0.6536 0.6161 0.197 Uiso 1 1 calc R . . H13U H 0.0377 0.7862 0.6480 0.197 Uiso 1 1 calc R . . C140 C -0.0576(13) 0.854(5) 0.6307(15) 0.237(18) Uani 1 1 d . . . H14A H -0.0608 0.8285 0.6681 0.285 Uiso 1 1 calc R . . H14B H -0.0469 0.9708 0.6293 0.285 Uiso 1 1 calc R . . C141 C -0.1170(11) 0.836(3) 0.6058(10) 0.166(11) Uani 1 1 d . . . H1 H -0.1168 0.8623 0.5684 0.250 Uiso 1 1 calc R . . H2 H -0.1484 0.9097 0.6205 0.250 Uiso 1 1 calc R . . H14C H -0.1319 0.7240 0.6091 0.250 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 0.0400(8) 0.0554(9) 0.0364(8) 0.0024(8) 0.0018(6) -0.0009(8) O101 0.046(5) 0.064(5) 0.036(4) 0.001(4) 0.002(3) -0.007(4) O102 0.042(5) 0.074(5) 0.042(4) 0.011(4) 0.003(3) 0.008(4) O103 0.035(4) 0.079(6) 0.074(5) 0.021(5) 0.012(4) 0.009(4) O104 0.044(4) 0.069(5) 0.067(5) 0.014(4) 0.001(4) -0.013(4) O105 0.040(4) 0.057(5) 0.037(4) 0.003(3) -0.001(3) -0.002(3) O106 0.039(4) 0.058(5) 0.034(4) 0.008(3) 0.001(3) -0.002(4) O107 0.051(5) 0.059(5) 0.059(5) 0.009(4) -0.003(4) 0.007(4) O108 0.050(5) 0.082(6) 0.068(5) 0.012(5) 0.022(4) -0.012(4) N101 0.037(5) 0.043(5) 0.040(5) -0.006(4) 0.004(4) -0.002(4) N102 0.037(5) 0.045(5) 0.036(5) 0.001(4) 0.005(4) 0.007(4) N103 0.044(5) 0.056(6) 0.041(5) 0.005(4) 0.003(4) 0.000(4) N104 0.065(6) 0.046(6) 0.048(5) -0.002(5) 0.011(5) -0.005(5) C101 0.057(7) 0.042(6) 0.042(6) -0.003(5) 0.019(5) -0.003(5) C102 0.042(6) 0.036(6) 0.053(7) 0.003(5) 0.013(5) -0.002(5) C103 0.040(6) 0.044(6) 0.041(6) -0.004(5) 0.009(5) 0.001(5) C104 0.035(5) 0.040(6) 0.043(6) -0.005(5) 0.003(5) -0.004(5) C105 0.036(5) 0.045(6) 0.036(6) 0.000(5) 0.000(5) 0.006(5) C106 0.036(5) 0.041(6) 0.030(5) -0.003(4) 0.000(4) 0.000(5) C107 0.042(6) 0.043(6) 0.050(6) -0.006(5) 0.010(5) -0.003(5) C108 0.032(5) 0.046(6) 0.039(6) -0.001(5) -0.006(5) 0.006(5) C109 0.040(6) 0.040(6) 0.032(5) 0.000(5) 0.003(4) 0.002(5) C110 0.037(6) 0.045(6) 0.042(6) 0.006(5) 0.005(4) 0.000(5) C111 0.055(6) 0.047(6) 0.026(5) 0.006(5) 0.006(5) 0.008(5) C112 0.043(7) 0.049(7) 0.049(7) 0.005(5) -0.006(5) 0.003(5) C113 0.060(7) 0.062(7) 0.036(6) 0.000(6) -0.013(6) 0.016(6) C114 0.039(7) 0.102(10) 0.088(9) 0.021(9) 0.005(6) -0.006(8) C115 0.053(7) 0.090(10) 0.046(7) 0.025(7) -0.003(6) 0.010(7) C116 0.068(8) 0.065(8) 0.045(6) 0.018(6) 0.008(6) -0.014(7) C117 0.059(7) 0.047(7) 0.053(7) 0.005(6) 0.006(6) 0.003(6) C118 0.040(7) 0.088(10) 0.086(9) 0.023(8) -0.016(7) -0.016(7) C119 0.047(6) 0.049(7) 0.036(6) 0.010(5) 0.006(5) -0.001(5) C120 0.044(6) 0.049(7) 0.057(7) 0.000(6) 0.011(5) -0.002(5) C121 0.045(6) 0.048(7) 0.049(6) 0.007(5) 0.007(5) -0.002(5) C122 0.066(7) 0.052(7) 0.038(6) 0.005(6) 0.002(5) -0.014(6) C123 0.047(6) 0.063(7) 0.033(6) 0.004(6) 0.012(5) -0.008(6) C124 0.090(9) 0.063(8) 0.051(7) -0.002(6) 0.038(7) -0.001(7) C125 0.107(11) 0.055(8) 0.055(8) 0.008(6) 0.002(7) -0.018(8) C126 0.040(6) 0.057(7) 0.036(6) 0.001(5) 0.000(5) -0.001(5) C127 0.056(7) 0.057(7) 0.043(6) 0.013(5) -0.009(5) 0.005(6) C128 0.051(7) 0.049(7) 0.045(6) 0.003(5) -0.010(5) 0.006(5) C129 0.046(6) 0.056(7) 0.040(6) 0.006(5) -0.007(5) 0.004(5) C130 0.051(6) 0.053(7) 0.034(6) 0.001(5) 0.003(5) 0.002(5) C131 0.042(6) 0.059(7) 0.045(6) 0.003(5) -0.005(5) -0.005(6) C32A 0.049(6) 0.061(7) 0.043(6) 0.004(6) -0.007(5) 0.006(6) C33A 0.060(7) 0.063(8) 0.050(7) 0.007(6) -0.018(6) 0.006(6) C134 0.050(7) 0.069(8) 0.045(6) 0.002(6) 0.011(5) -0.014(6) C135 0.050(7) 0.072(8) 0.044(6) 0.009(6) 0.007(5) -0.008(6) C136 0.053(7) 0.067(8) 0.058(7) 0.005(6) -0.009(6) -0.005(6) C137 0.054(7) 0.102(11) 0.058(8) -0.018(8) 0.011(6) -0.004(7) C138 0.161(17) 0.123(15) 0.082(11) -0.011(11) 0.065(12) 0.027(14) C139 0.20(3) 0.20(3) 0.093(14) 0.010(15) 0.013(15) 0.11(2) C140 0.093(18) 0.28(4) 0.35(5) -0.10(4) 0.06(2) 0.00(2) C141 0.112(17) 0.15(2) 0.23(3) -0.09(2) -0.015(18) 0.023(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O101 1.987(7) . ? Fe1 O102 1.992(7) . ? Fe1 N101 2.069(8) . ? Fe1 N102 2.070(8) . ? Fe1 N103 2.128(9) . ? O101 C101 1.284(12) . ? O102 C112 1.264(12) . ? O103 C113 1.331(14) . ? O103 C114 1.434(13) . ? O104 C117 1.370(13) . ? O104 C118 1.461(12) . ? O105 C106 1.366(11) . ? O105 C126 1.424(11) . ? O106 C107 1.379(12) . ? O106 C134 1.427(12) . ? O107 C113 1.214(12) . ? O108 C117 1.202(13) . ? N101 C103 1.308(12) . ? N101 C104 1.408(13) . ? N102 C110 1.298(12) . ? N102 C109 1.442(12) . ? N103 C119 1.330(13) . ? N103 C123 1.348(14) . ? N104 C121 1.338(14) . ? N104 C125 1.440(15) . ? N104 C124 1.451(13) . ? C101 C102 1.401(15) . ? C101 C116 1.518(14) . ? C102 C103 1.417(14) . ? C102 C117 1.487(16) . ? C103 H103 0.9500 . ? C104 C109 1.402(13) . ? C104 C105 1.408(13) . ? C105 C106 1.379(13) . ? C105 H105 0.9500 . ? C106 C107 1.405(14) . ? C107 C108 1.382(14) . ? C108 C109 1.407(14) . ? C108 H108 0.9500 . ? C110 C111 1.444(13) . ? C110 H110 0.9500 . ? C111 C112 1.395(14) . ? C111 C113 1.463(15) . ? C112 C115 1.511(14) . ? C114 H11A 0.9800 . ? C114 H11B 0.9800 . ? C114 H11C 0.9800 . ? C115 H11D 0.9800 . ? C115 H11E 0.9800 . ? C115 H11F 0.9800 . ? C116 H11G 0.9800 . ? C116 H11H 0.9800 . ? C116 H11I 0.9800 . ? C118 H11J 0.9800 . ? C118 H11K 0.9800 . ? C118 H11L 0.9800 . ? C119 C120 1.365(15) . ? C119 H119 0.9500 . ? C120 C121 1.431(15) . ? C120 H120 0.9500 . ? C121 C122 1.415(14) . ? C122 C123 1.369(15) . ? C122 H122 0.9500 . ? C123 H123 0.9500 . ? C124 H12A 0.9800 . ? C124 H12B 0.9800 . ? C124 H12C 0.9800 . ? C125 H12D 0.9800 . ? C125 H12E 0.9800 . ? C125 H12F 0.9800 . ? C126 C127 1.526(13) . ? C126 H12G 0.9900 . ? C126 H12H 0.9900 . ? C127 C128 1.537(15) . ? C127 H12I 0.9900 . ? C127 H12J 0.9900 . ? C128 C129 1.528(13) . ? C128 H12K 0.9900 . ? C128 H12L 0.9900 . ? C129 C130 1.530(14) . ? C129 H12M 0.9900 . ? C129 H12N 0.9900 . ? C130 C131 1.512(14) . ? C130 H13A 0.9900 . ? C130 H13B 0.9900 . ? C131 C32A 1.522(14) . ? C131 H13C 0.9900 . ? C131 H13D 0.9900 . ? C32A C33A 1.520(14) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C134 C135 1.522(14) . ? C134 H13J 0.9900 . ? C134 H13K 0.9900 . ? C135 C136 1.501(17) . ? C135 H13L 0.9900 . ? C135 H13M 0.9900 . ? C136 C137 1.522(16) . ? C136 H13N 0.9900 . ? C136 H13O 0.9900 . ? C137 C138 1.52(2) . ? C137 H13P 0.9900 . ? C137 H13Q 0.9900 . ? C138 C139 1.53(2) . ? C138 H13R 0.9900 . ? C138 H13S 0.9900 . ? C139 C140 1.41(3) . ? C139 H13T 0.9900 . ? C139 H13U 0.9900 . ? C140 C141 1.26(3) . ? C140 H14A 0.9900 . ? C140 H14B 0.9900 . ? C141 H1 0.9800 . ? C141 H2 0.9800 . ? C141 H14C 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 O101 Fe1 O102 99.7(3) . . ? O101 Fe1 N101 85.9(3) . . ? O102 Fe1 N101 152.7(3) . . ? O101 Fe1 N102 158.4(3) . . ? O102 Fe1 N102 86.0(3) . . ? N101 Fe1 N102 80.0(3) . . ? O101 Fe1 N103 93.6(3) . . ? O102 Fe1 N103 97.2(3) . . ? N101 Fe1 N103 109.2(3) . . ? N102 Fe1 N103 106.4(3) . . ? C101 O101 Fe1 135.3(7) . . ? C112 O102 Fe1 133.9(7) . . ? C113 O103 C114 115.7(9) . . ? C117 O104 C118 114.2(9) . . ? C106 O105 C126 117.5(8) . . ? C107 O106 C134 116.7(8) . . ? C103 N101 C104 120.8(8) . . ? C103 N101 Fe1 126.1(7) . . ? C104 N101 Fe1 113.0(6) . . ? C110 N102 C109 120.0(8) . . ? C110 N102 Fe1 127.4(7) . . ? C109 N102 Fe1 112.1(6) . . ? C119 N103 C123 115.4(9) . . ? C119 N103 Fe1 119.8(7) . . ? C123 N103 Fe1 124.7(7) . . ? C121 N104 C125 121.8(9) . . ? C121 N104 C124 121.3(9) . . ? C125 N104 C124 116.9(10) . . ? O101 C101 C102 121.7(9) . . ? O101 C101 C116 114.3(9) . . ? C102 C101 C116 124.0(10) . . ? C101 C102 C103 123.2(10) . . ? C101 C102 C117 118.6(9) . . ? C103 C102 C117 118.1(10) . . ? N101 C103 C102 127.7(10) . . ? N101 C103 H103 116.1 . . ? C102 C103 H103 116.1 . . ? C109 C104 N101 116.8(8) . . ? C109 C104 C105 118.7(9) . . ? N101 C104 C105 124.5(9) . . ? C106 C105 C104 120.9(9) . . ? C106 C105 H105 119.5 . . ? C104 C105 H105 119.5 . . ? O105 C106 C105 125.1(9) . . ? O105 C106 C107 115.2(9) . . ? C105 C106 C107 119.7(9) . . ? O106 C107 C108 124.0(9) . . ? O106 C107 C106 115.4(9) . . ? C108 C107 C106 120.6(10) . . ? C107 C108 C109 119.5(9) . . ? C107 C108 H108 120.3 . . ? C109 C108 H108 120.3 . . ? C104 C109 C108 120.5(9) . . ? C104 C109 N102 115.6(9) . . ? C108 C109 N102 123.8(8) . . ? N102 C110 C111 126.1(9) . . ? N102 C110 H110 116.9 . . ? C111 C110 H110 116.9 . . ? C112 C111 C110 122.2(10) . . ? C112 C111 C113 122.0(9) . . ? C110 C111 C113 115.6(9) . . ? O102 C112 C111 124.2(10) . . ? O102 C112 C115 114.7(10) . . ? C111 C112 C115 121.1(10) . . ? O107 C113 O103 120.6(11) . . ? O107 C113 C111 125.8(11) . . ? O103 C113 C111 113.6(9) . . ? O103 C114 H11A 109.5 . . ? O103 C114 H11B 109.5 . . ? H11A C114 H11B 109.5 . . ? O103 C114 H11C 109.5 . . ? H11A C114 H11C 109.5 . . ? H11B C114 H11C 109.5 . . ? C112 C115 H11D 109.5 . . ? C112 C115 H11E 109.5 . . ? H11D C115 H11E 109.5 . . ? C112 C115 H11F 109.5 . . ? H11D C115 H11F 109.5 . . ? H11E C115 H11F 109.5 . . ? C101 C116 H11G 109.5 . . ? C101 C116 H11H 109.5 . . ? H11G C116 H11H 109.5 . . ? C101 C116 H11I 109.5 . . ? H11G C116 H11I 109.5 . . ? H11H C116 H11I 109.5 . . ? O108 C117 O104 120.7(11) . . ? O108 C117 C102 128.3(11) . . ? O104 C117 C102 110.9(10) . . ? O104 C118 H11J 109.5 . . ? O104 C118 H11K 109.5 . . ? H11J C118 H11K 109.5 . . ? O104 C118 H11L 109.5 . . ? H11J C118 H11L 109.5 . . ? H11K C118 H11L 109.5 . . ? N103 C119 C120 125.5(10) . . ? N103 C119 H119 117.2 . . ? C120 C119 H119 117.2 . . ? C119 C120 C121 119.9(10) . . ? C119 C120 H120 120.1 . . ? C121 C120 H120 120.1 . . ? N104 C121 C122 124.5(10) . . ? N104 C121 C120 121.5(10) . . ? C122 C121 C120 114.0(10) . . ? C123 C122 C121 120.9(10) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? N103 C123 C122 124.3(9) . . ? N103 C123 H123 117.9 . . ? C122 C123 H123 117.9 . . ? N104 C124 H12A 109.5 . . ? N104 C124 H12B 109.5 . . ? H12A C124 H12B 109.5 . . ? N104 C124 H12C 109.5 . . ? H12A C124 H12C 109.5 . . ? H12B C124 H12C 109.5 . . ? N104 C125 H12D 109.5 . . ? N104 C125 H12E 109.5 . . ? H12D C125 H12E 109.5 . . ? N104 C125 H12F 109.5 . . ? H12D C125 H12F 109.5 . . ? H12E C125 H12F 109.5 . . ? O105 C126 C127 106.0(8) . . ? O105 C126 H12G 110.5 . . ? C127 C126 H12G 110.5 . . ? O105 C126 H12H 110.5 . . ? C127 C126 H12H 110.5 . . ? H12G C126 H12H 108.7 . . ? C126 C127 C128 111.9(9) . . ? C126 C127 H12I 109.2 . . ? C128 C127 H12I 109.2 . . ? C126 C127 H12J 109.2 . . ? C128 C127 H12J 109.2 . . ? H12I C127 H12J 107.9 . . ? C129 C128 C127 110.9(9) . . ? C129 C128 H12K 109.5 . . ? C127 C128 H12K 109.5 . . ? C129 C128 H12L 109.5 . . ? C127 C128 H12L 109.5 . . ? H12K C128 H12L 108.0 . . ? C128 C129 C130 114.2(9) . . ? C128 C129 H12M 108.7 . . ? C130 C129 H12M 108.7 . . ? C128 C129 H12N 108.7 . . ? C130 C129 H12N 108.7 . . ? H12M C129 H12N 107.6 . . ? C131 C130 C129 113.9(9) . . ? C131 C130 H13A 108.8 . . ? C129 C130 H13A 108.8 . . ? C131 C130 H13B 108.8 . . ? C129 C130 H13B 108.8 . . ? H13A C130 H13B 107.7 . . ? C130 C131 C32A 113.7(9) . . ? C130 C131 H13C 108.8 . . ? C32A C131 H13C 108.8 . . ? C130 C131 H13D 108.8 . . ? C32A C131 H13D 108.8 . . ? H13C C131 H13D 107.7 . . ? C33A C32A C131 113.3(10) . . ? C33A C32A H32A 108.9 . . ? C131 C32A H32A 108.9 . . ? C33A C32A H32B 108.9 . . ? C131 C32A H32B 108.9 . . ? H32A C32A H32B 107.7 . . ? C32A C33A H33A 109.5 . . ? C32A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C32A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? O106 C134 C135 108.5(9) . . ? O106 C134 H13J 110.0 . . ? C135 C134 H13J 110.0 . . ? O106 C134 H13K 110.0 . . ? C135 C134 H13K 110.0 . . ? H13J C134 H13K 108.4 . . ? C136 C135 C134 113.4(10) . . ? C136 C135 H13L 108.9 . . ? C134 C135 H13L 108.9 . . ? C136 C135 H13M 108.9 . . ? C134 C135 H13M 108.9 . . ? H13L C135 H13M 107.7 . . ? C135 C136 C137 112.0(11) . . ? C135 C136 H13N 109.2 . . ? C137 C136 H13N 109.2 . . ? C135 C136 H13O 109.2 . . ? C137 C136 H13O 109.2 . . ? H13N C136 H13O 107.9 . . ? C138 C137 C136 113.3(13) . . ? C138 C137 H13P 108.9 . . ? C136 C137 H13P 108.9 . . ? C138 C137 H13Q 108.9 . . ? C136 C137 H13Q 108.9 . . ? H13P C137 H13Q 107.7 . . ? C137 C138 C139 112.8(16) . . ? C137 C138 H13R 109.0 . . ? C139 C138 H13R 109.0 . . ? C137 C138 H13S 109.0 . . ? C139 C138 H13S 109.0 . . ? H13R C138 H13S 107.8 . . ? C140 C139 C138 116(2) . . ? C140 C139 H13T 108.4 . . ? C138 C139 H13T 108.4 . . ? C140 C139 H13U 108.4 . . ? C138 C139 H13U 108.4 . . ? H13T C139 H13U 107.4 . . ? C141 C140 C139 124(3) . . ? C141 C140 H14A 106.3 . . ? C139 C140 H14A 106.3 . . ? C141 C140 H14B 106.3 . . ? C139 C140 H14B 106.3 . . ? H14A C140 H14B 106.4 . . ? C140 C141 H1 109.5 . . ? C140 C141 H2 109.5 . . ? H1 C141 H2 109.5 . . ? C140 C141 H14C 109.5 . . ? H1 C141 H14C 109.5 . . ? H2 C141 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.596 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.111 _iucr_refine_instructions_details ; TITL w027 in P -1 New: P21/c CELL 0.71069 19.8161 8.2415 25.5905 90.000 98.224 90.000 ZERR 4.00 0.0009 0.0004 0.0011 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H FE N O UNIT 164 240 4 16 32 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H L.S. 25 TEMP -140.00 WGHT 0.034700 32.688999 BASF 0.46207 FVAR 3.82896 FE1 3 0.252730 1.006314 0.190120 11.00000 0.03999 0.05541 = 0.03642 0.00243 0.00177 -0.00090 O101 5 0.325496 1.120572 0.158632 11.00000 0.04552 0.06383 = 0.03605 0.00118 0.00188 -0.00703 O102 5 0.170958 1.113978 0.150608 11.00000 0.04183 0.07427 = 0.04222 0.01091 0.00334 0.00785 O103 5 -0.007601 0.986667 0.245218 11.00000 0.03536 0.07876 = 0.07413 0.02138 0.01193 0.00938 O104 5 0.517273 1.116407 0.289738 11.00000 0.04447 0.06861 = 0.06673 0.01355 0.00114 -0.01273 O105 5 0.343411 0.730308 0.432952 11.00000 0.03987 0.05678 = 0.03654 0.00324 -0.00076 -0.00173 O106 5 0.212947 0.693402 0.422275 11.00000 0.03944 0.05836 = 0.03439 0.00768 0.00126 -0.00247 O107 5 -0.028426 1.175357 0.183558 11.00000 0.05065 0.05864 = 0.05913 0.00909 -0.00288 0.00711 O108 5 0.534757 1.190912 0.208705 11.00000 0.05042 0.08189 = 0.06764 0.01230 0.02176 -0.01245 N101 4 0.325241 0.975422 0.256038 11.00000 0.03680 0.04309 = 0.03953 -0.00621 0.00427 -0.00171 N102 4 0.190195 0.946821 0.245458 11.00000 0.03721 0.04548 = 0.03638 0.00075 0.00465 0.00716 N103 4 0.253704 0.800605 0.139976 11.00000 0.04423 0.05619 = 0.04103 0.00535 0.00327 0.00044 N104 4 0.252874 0.414720 0.033065 11.00000 0.06475 0.04585 = 0.04821 -0.00160 0.01065 -0.00504 C101 1 0.388911 1.151149 0.173357 11.00000 0.05711 0.04246 = 0.04200 -0.00344 0.01945 -0.00288 C102 1 0.421872 1.106543 0.223412 11.00000 0.04181 0.03637 = 0.05313 0.00284 0.01291 -0.00154 C103 1 0.388459 1.025796 0.261367 11.00000 0.03955 0.04434 = 0.04145 -0.00361 0.00903 0.00051 AFIX 43 H103 2 0.415143 1.005884 0.294634 11.00000 -1.20000 AFIX 0 C104 1 0.299063 0.900154 0.298255 11.00000 0.03495 0.03978 = 0.04271 -0.00474 0.00278 -0.00376 C105 1 0.339017 0.846124 0.344951 11.00000 0.03622 0.04482 = 0.03603 0.00040 0.00018 0.00606 AFIX 43 H105 2 0.387239 0.855704 0.348613 11.00000 -1.20000 AFIX 0 C106 1 0.309128 0.779484 0.385451 11.00000 0.03631 0.04067 = 0.02994 -0.00348 -0.00015 0.00014 C107 1 0.238036 0.759286 0.379389 11.00000 0.04230 0.04279 = 0.05011 -0.00612 0.01021 -0.00312 C108 1 0.197759 0.805841 0.333214 11.00000 0.03225 0.04598 = 0.03852 -0.00107 -0.00632 0.00625 AFIX 43 H108 2 0.149950 0.787453 0.328674 11.00000 -1.20000 AFIX 0 C109 1 0.228140 0.880683 0.292994 11.00000 0.03984 0.04040 = 0.03190 -0.00005 0.00319 0.00218 C110 1 0.125911 0.980543 0.243766 11.00000 0.03679 0.04521 = 0.04187 0.00647 0.00502 0.00015 AFIX 43 H110 2 0.104975 0.948947 0.273340 11.00000 -1.20000 AFIX 0 C111 1 0.083260 1.061527 0.201177 11.00000 0.05464 0.04667 = 0.02642 0.00564 0.00631 0.00837 C112 1 0.109250 1.124764 0.157565 11.00000 0.04335 0.04914 = 0.04944 0.00521 -0.00615 0.00304 C113 1 0.011888 1.083158 0.208422 11.00000 0.05961 0.06181 = 0.03607 -0.00023 -0.01283 0.01645 C114 1 -0.077148 1.003655 0.253873 11.00000 0.03895 0.10206 = 0.08769 0.02143 0.00517 -0.00569 AFIX 33 H11A 2 -0.086692 0.926468 0.281014 11.00000 -1.50000 H11B 2 -0.107461 0.981655 0.220907 11.00000 -1.50000 H11C 2 -0.084833 1.114453 0.265615 11.00000 -1.50000 AFIX 0 C115 1 0.063620 1.211403 0.113972 11.00000 0.05306 0.09024 = 0.04586 0.02506 -0.00285 0.01026 AFIX 137 H11D 2 0.090807 1.248385 0.087141 11.00000 -1.50000 H11E 2 0.042381 1.305100 0.128679 11.00000 -1.50000 H11F 2 0.028079 1.136912 0.097824 11.00000 -1.50000 AFIX 0 C116 1 0.423284 1.241203 0.132621 11.00000 0.06830 0.06541 = 0.04539 0.01839 0.00842 -0.01394 AFIX 137 H11G 2 0.388646 1.279040 0.104018 11.00000 -1.50000 H11H 2 0.455041 1.168178 0.118219 11.00000 -1.50000 H11I 2 0.448354 1.334526 0.149330 11.00000 -1.50000 AFIX 0 C117 1 0.495963 1.141184 0.237042 11.00000 0.05916 0.04712 = 0.05298 0.00510 0.00563 0.00323 C118 1 0.589962 1.145614 0.306048 11.00000 0.03991 0.08837 = 0.08568 0.02260 -0.01578 -0.01568 AFIX 137 H11J 2 0.601919 1.119056 0.343558 11.00000 -1.50000 H11K 2 0.600227 1.260063 0.300395 11.00000 -1.50000 H11L 2 0.616495 1.077312 0.285129 11.00000 -1.50000 AFIX 0 C119 1 0.273455 0.816843 0.092740 11.00000 0.04662 0.04857 = 0.03571 0.01036 0.00569 -0.00126 AFIX 43 H119 2 0.289000 0.920870 0.083793 11.00000 -1.20000 AFIX 0 C120 1 0.273287 0.696639 0.056002 11.00000 0.04380 0.04882 = 0.05729 0.00025 0.01112 -0.00196 AFIX 43 H120 2 0.286848 0.719640 0.022643 11.00000 -1.20000 AFIX 0 C121 1 0.252646 0.535919 0.067830 11.00000 0.04538 0.04798 = 0.04857 0.00684 0.00652 -0.00155 C122 1 0.232868 0.519681 0.118567 11.00000 0.06574 0.05160 = 0.03755 0.00548 0.00197 -0.01404 AFIX 43 H122 2 0.219010 0.416643 0.129845 11.00000 -1.20000 AFIX 0 C123 1 0.233437 0.650434 0.151609 11.00000 0.04713 0.06347 = 0.03342 0.00399 0.01213 -0.00761 AFIX 43 H123 2 0.218577 0.634260 0.184910 11.00000 -1.20000 AFIX 0 C124 1 0.275711 0.439986 -0.017717 11.00000 0.08980 0.06279 = 0.05057 -0.00190 0.03779 -0.00107 AFIX 137 H12A 2 0.279089 0.335140 -0.035223 11.00000 -1.50000 H12B 2 0.320511 0.492646 -0.012470 11.00000 -1.50000 H12C 2 0.242957 0.509238 -0.039757 11.00000 -1.50000 AFIX 0 C125 1 0.229245 0.254496 0.043680 11.00000 0.10679 0.05462 = 0.05501 0.00797 0.00154 -0.01825 AFIX 137 H12D 2 0.230875 0.185161 0.012774 11.00000 -1.50000 H12E 2 0.182237 0.260752 0.051303 11.00000 -1.50000 H12F 2 0.258538 0.208521 0.074188 11.00000 -1.50000 AFIX 0 C126 1 0.414417 0.765103 0.443591 11.00000 0.04034 0.05673 = 0.03566 0.00098 0.00004 -0.00108 AFIX 23 H12G 2 0.422895 0.881559 0.437618 11.00000 -1.20000 H12H 2 0.439874 0.700012 0.420400 11.00000 -1.20000 AFIX 0 C127 1 0.436545 0.720685 0.501389 11.00000 0.05588 0.05743 = 0.04265 0.01332 -0.00885 0.00503 AFIX 23 H12I 2 0.423580 0.606819 0.507242 11.00000 -1.20000 H12J 2 0.412260 0.790918 0.523970 11.00000 -1.20000 AFIX 0 C128 1 0.513807 0.740364 0.517618 11.00000 0.05101 0.04905 = 0.04490 0.00341 -0.01017 0.00585 AFIX 23 H12K 2 0.538279 0.672580 0.494477 11.00000 -1.20000 H12L 2 0.526728 0.854959 0.513005 11.00000 -1.20000 AFIX 0 C129 1 0.534922 0.690190 0.575105 11.00000 0.04583 0.05584 = 0.04045 0.00596 -0.00734 0.00384 AFIX 23 H12M 2 0.519374 0.577595 0.579686 11.00000 -1.20000 H12N 2 0.511325 0.761171 0.597927 11.00000 -1.20000 AFIX 0 C130 1 0.611741 0.699108 0.593720 11.00000 0.05131 0.05252 = 0.03440 0.00099 0.00348 0.00201 AFIX 23 H13A 2 0.635637 0.635235 0.569199 11.00000 -1.20000 H13B 2 0.626670 0.813361 0.591937 11.00000 -1.20000 AFIX 0 C131 1 0.632859 0.636820 0.649236 11.00000 0.04214 0.05931 = 0.04483 0.00273 -0.00465 -0.00451 AFIX 23 H13C 2 0.621037 0.520290 0.650400 11.00000 -1.20000 H13D 2 0.606479 0.695147 0.673426 11.00000 -1.20000 AFIX 0 C32A 1 0.708579 0.657087 0.668983 11.00000 0.04873 0.06143 = 0.04309 0.00376 -0.00704 0.00552 AFIX 23 H32A 2 0.735019 0.598055 0.644994 11.00000 -1.20000 H32B 2 0.720527 0.773508 0.667659 11.00000 -1.20000 AFIX 0 C33A 1 0.729229 0.595161 0.724945 11.00000 0.06037 0.06275 = 0.05016 0.00730 -0.01817 0.00633 AFIX 33 H33A 2 0.778443 0.609575 0.735129 11.00000 -1.50000 H33B 2 0.717812 0.479745 0.726578 11.00000 -1.50000 H33C 2 0.704743 0.656241 0.749204 11.00000 -1.50000 AFIX 0 C134 1 0.142942 0.646226 0.414485 11.00000 0.04993 0.06915 = 0.04529 0.00224 0.01092 -0.01353 AFIX 23 H13J 2 0.136324 0.551249 0.390616 11.00000 -1.20000 H13K 2 0.114294 0.736300 0.398156 11.00000 -1.20000 AFIX 0 C135 1 0.122414 0.603439 0.467882 11.00000 0.05013 0.07247 = 0.04410 0.00881 0.00719 -0.00813 AFIX 23 H13L 2 0.087021 0.517859 0.462856 11.00000 -1.20000 H13M 2 0.162533 0.558512 0.490816 11.00000 -1.20000 AFIX 0 C136 1 0.095495 0.745474 0.495265 11.00000 0.05263 0.06721 = 0.05809 0.00548 -0.00930 -0.00531 AFIX 23 H13N 2 0.057377 0.795569 0.471474 11.00000 -1.20000 H13O 2 0.131958 0.827770 0.502947 11.00000 -1.20000 AFIX 0 C137 1 0.070611 0.696143 0.546570 11.00000 0.05417 0.10214 = 0.05812 -0.01784 0.01137 -0.00441 AFIX 23 H13P 2 0.044785 0.593329 0.540793 11.00000 -1.20000 H13Q 2 0.110598 0.675813 0.573684 11.00000 -1.20000 AFIX 0 C138 1 0.025594 0.822859 0.567214 11.00000 0.16078 0.12282 = 0.08156 -0.01118 0.06533 0.02698 AFIX 23 H13R 2 -0.014157 0.844258 0.539984 11.00000 -1.20000 H13S 2 0.051574 0.925299 0.573519 11.00000 -1.20000 AFIX 0 C139 1 0.000141 0.770984 0.618430 11.00000 0.19959 0.19821 = 0.09294 0.01040 0.01348 0.10524 AFIX 23 H13T 2 -0.010458 0.653591 0.616122 11.00000 -1.20000 H13U 2 0.037680 0.786249 0.647981 11.00000 -1.20000 AFIX 0 C140 1 -0.057599 0.853708 0.630670 11.00000 0.09273 0.27888 = 0.34689 -0.09753 0.05570 0.00447 AFIX 23 H14A 2 -0.060778 0.828516 0.668065 11.00000 -1.20000 H14B 2 -0.046919 0.970843 0.629293 11.00000 -1.20000 AFIX 0 C141 1 -0.117024 0.836459 0.605769 11.00000 0.11217 0.14924 = 0.22621 -0.09174 -0.01537 0.02332 AFIX 137 H1 2 -0.116800 0.862320 0.568416 11.00000 -1.50000 H2 2 -0.148408 0.909674 0.620515 11.00000 -1.50000 H14C 2 -0.131929 0.724010 0.609074 11.00000 -1.50000 HKLF 5 REM w027 in P -1 New: P21/c REM R1 = 0.1008 for 4397 Fo > 4sig(Fo) and 0.1147 for all 5508 data REM 494 parameters refined using 0 restraints END WGHT 0.0348 32.6842 REM Highest difference peak 0.596, deepest hole -0.628, 1-sigma level 0.111 Q1 1 0.5164 1.0029 0.1683 11.00000 0.05 0.60 Q2 1 0.0524 0.9846 0.1895 11.00000 0.05 0.56 Q3 1 0.3493 1.0029 0.1672 11.00000 0.05 0.53 Q4 1 0.2033 1.0891 0.1870 11.00000 0.05 0.52 Q5 1 0.5798 0.4864 0.6963 11.00000 0.05 0.48 Q6 1 0.2232 0.9064 0.2119 11.00000 0.05 0.45 Q7 1 0.5138 0.9371 0.5780 11.00000 0.05 0.45 Q8 1 0.4294 0.8594 0.3100 11.00000 0.05 0.44 Q9 1 0.2997 0.6522 0.3442 11.00000 0.05 0.43 Q10 1 0.5905 1.4308 0.3057 11.00000 0.05 0.42 Q11 1 0.1612 0.9886 0.1663 11.00000 0.05 0.42 Q12 1 -0.0246 1.0307 0.1541 11.00000 0.05 0.40 Q13 1 0.2860 0.9534 0.1401 11.00000 0.05 0.40 Q14 1 0.3123 1.0640 0.2370 11.00000 0.05 0.40 Q15 1 -0.0306 0.8330 0.5740 11.00000 0.05 0.40 Q16 1 0.2962 0.9363 0.2222 11.00000 0.05 0.39 Q17 1 0.4591 1.0064 0.1395 11.00000 0.05 0.39 Q18 1 -0.0296 0.8565 0.5496 11.00000 0.05 0.38 Q19 1 -0.1322 0.9963 0.1892 11.00000 0.05 0.38 Q20 1 0.2211 1.1429 0.1485 11.00000 0.05 0.37 ; _database_code_depnum_ccdc_archive 'CCDC 944438'