# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a16ce2 _database_code_depnum_ccdc_archive 'CCDC 918951' #TrackingRef 'fe2ln2_monster_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C54 H58 Ce2 Fe2 N2 O20), 3(C2 H3 N)' _chemical_formula_sum 'C60 H67 Ce2 Fe2 N5 O20' _chemical_formula_weight 1570.13 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' Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.389(2) _cell_length_b 12.4258(12) _cell_length_c 23.558(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.454(2) _cell_angle_gamma 90.00 _cell_volume 6260.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11401 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.13 _exptl_crystal_description block _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 1.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.619 _exptl_absorpt_correction_T_max 0.773 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21193 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.13 _reflns_number_total 7005 _reflns_number_gt 6384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The phenyl ring of one benzoate ligand was disordered, and refined using partial-occupancy carbon atoms in two rigid hexagons. One lattice MeCN was four-fold disordered across a twofold axis and was refined using partial occupancy isotropic atoms. The geometries of the disordered part-molecules were restrained to be similar to that of the ordered MeCN: SAME N31 C31 C32. O-H distances were restrained: DFIX 0.92 0.04 O1 H1 O4 H4 ; _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^)+(0.0522P)^2^+31.5387P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7005 _refine_ls_number_parameters 388 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _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 Ce1 Ce 0.251851(10) 0.493815(15) 0.535922(8) 0.01493(8) Uani 1 1 d . . . Fe1 Fe 0.28181(3) 0.28165(4) 0.43999(2) 0.01468(12) Uani 1 1 d . . . O1 O 0.20966(12) 0.3241(2) 0.49259(11) 0.0147(5) Uani 1 1 d D . . H1 H 0.1727(16) 0.334(4) 0.4803(19) 0.018 Uiso 1 1 d D . . N1 N 0.36594(16) 0.4801(3) 0.58508(15) 0.0190(7) Uani 1 1 d . . . C1 C 0.41079(19) 0.4211(3) 0.54845(18) 0.0228(8) Uani 1 1 d . . . H1A H 0.4143 0.3459 0.5620 0.027 Uiso 1 1 calc R . . H1B H 0.4526 0.4548 0.5521 0.027 Uiso 1 1 calc R . . C2 C 0.39136(19) 0.4203(3) 0.48578(18) 0.0228(8) Uani 1 1 d . . . H2A H 0.3992 0.4920 0.4689 0.027 Uiso 1 1 calc R . . H2B H 0.4165 0.3666 0.4650 0.027 Uiso 1 1 calc R . . O2 O 0.32722(13) 0.3946(2) 0.48074(12) 0.0185(5) Uani 1 1 d . . . C3 C 0.35497(19) 0.4225(3) 0.63922(17) 0.0213(8) Uani 1 1 d . . . H3A H 0.3304 0.4691 0.6648 0.026 Uiso 1 1 calc R . . H3B H 0.3956 0.4074 0.6579 0.026 Uiso 1 1 calc R . . C4 C 0.32012(19) 0.3173(3) 0.62994(17) 0.0210(8) Uani 1 1 d . . . H4A H 0.3477 0.2651 0.6106 0.025 Uiso 1 1 calc R . . H4B H 0.3081 0.2864 0.6670 0.025 Uiso 1 1 calc R . . O3 O 0.26584(13) 0.3356(2) 0.59642(11) 0.0175(5) Uani 1 1 d . . . C5 C 0.3877(2) 0.5907(3) 0.59816(19) 0.0253(9) Uani 1 1 d . . . H5A H 0.4305 0.5874 0.6145 0.030 Uiso 1 1 calc R . . H5B H 0.3600 0.6231 0.6269 0.030 Uiso 1 1 calc R . . C6 C 0.3880(2) 0.6605(3) 0.5459(2) 0.0259(9) Uani 1 1 d . . . H6A H 0.3959 0.7364 0.5565 0.031 Uiso 1 1 calc R . . H6B H 0.4215 0.6369 0.5198 0.031 Uiso 1 1 calc R . . O4 O 0.32832(14) 0.6508(2) 0.51866(14) 0.0262(6) Uani 1 1 d D . . H4 H 0.323(2) 0.705(3) 0.4955(19) 0.031 Uiso 1 1 d D . . O5 O 0.25213(13) 0.3880(2) 0.38084(11) 0.0181(5) Uani 1 1 d . . . O6 O 0.22557(14) 0.5302(2) 0.43485(11) 0.0195(6) Uani 1 1 d . . . C7 C 0.23284(18) 0.4842(3) 0.38759(18) 0.0191(8) Uani 1 1 d . . . C8 C 0.21966(18) 0.5470(3) 0.33473(15) 0.0164(7) Uani 1 1 d . . . C9 C 0.2217(2) 0.4982(3) 0.28135(18) 0.0238(9) Uani 1 1 d . . . H9A H 0.2315 0.4239 0.2784 0.029 Uiso 1 1 calc R . . C10 C 0.2094(2) 0.5574(3) 0.23258(17) 0.0245(9) Uani 1 1 d . . . H10A H 0.2100 0.5231 0.1965 0.029 Uiso 1 1 calc R . . C11 C 0.1964(2) 0.6661(3) 0.23630(18) 0.0241(8) Uani 1 1 d . . . H11A H 0.1887 0.7067 0.2028 0.029 Uiso 1 1 calc R . . C12 C 0.1947(2) 0.7157(3) 0.28903(18) 0.0242(9) Uani 1 1 d . . . H12A H 0.1861 0.7906 0.2916 0.029 Uiso 1 1 calc R . . C13 C 0.20552(19) 0.6562(3) 0.33825(16) 0.0199(8) Uani 1 1 d . . . H13A H 0.2033 0.6902 0.3743 0.024 Uiso 1 1 calc R . . O7 O 0.36069(13) 0.2292(2) 0.40448(11) 0.0193(6) Uani 1 1 d . . . O8 O 0.35318(13) 0.0525(2) 0.42243(11) 0.0195(6) Uani 1 1 d . . . C14 C 0.37978(18) 0.1321(3) 0.40103(16) 0.0185(8) Uani 1 1 d . . . C15 C 0.43910(18) 0.1143(3) 0.36888(16) 0.0194(8) Uani 1 1 d . . . C16 C 0.4588(2) 0.0098(3) 0.3573(2) 0.0261(9) Uani 1 1 d . . . H16A H 0.4349 -0.0499 0.3699 0.031 Uiso 1 1 calc R . . C17 C 0.5133(2) -0.0070(4) 0.3274(2) 0.0332(11) Uani 1 1 d . . . H17A H 0.5267 -0.0783 0.3197 0.040 Uiso 1 1 calc R . . C18 C 0.5485(2) 0.0792(4) 0.3087(2) 0.0336(10) Uani 1 1 d . . . H18A H 0.5859 0.0671 0.2881 0.040 Uiso 1 1 calc R . . C19 C 0.5291(2) 0.1829(4) 0.3200(2) 0.0322(10) Uani 1 1 d . . . H19A H 0.5533 0.2421 0.3072 0.039 Uiso 1 1 calc R . . C20 C 0.4744(2) 0.2012(4) 0.35020(19) 0.0268(9) Uani 1 1 d . . . H20A H 0.4613 0.2727 0.3580 0.032 Uiso 1 1 calc R . . O9 O 0.23361(13) 0.6114(2) 0.62277(12) 0.0210(6) Uani 1 1 d . A . O10 O 0.18882(14) 0.6726(2) 0.54420(12) 0.0220(6) Uani 1 1 d . A . C21 C 0.19327(19) 0.6688(3) 0.59849(17) 0.0210(8) Uani 1 1 d . . . C22A C 0.1424(2) 0.7178(4) 0.63360(19) 0.0249(15) Uiso 0.62 1 d PG A 1 C23A C 0.0884(2) 0.7575(5) 0.60803(16) 0.0332(16) Uiso 0.62 1 d PG A 1 H23A H 0.0851 0.7602 0.5678 0.040 Uiso 0.62 1 calc PR A 1 C24A C 0.0392(2) 0.7933(5) 0.6413(2) 0.044(2) Uiso 0.62 1 d PG A 1 H24A H 0.0023 0.8205 0.6238 0.052 Uiso 0.62 1 calc PR A 1 C25A C 0.0441(2) 0.7894(5) 0.7001(2) 0.048(2) Uiso 0.62 1 d PG A 1 H25A H 0.0105 0.8139 0.7229 0.058 Uiso 0.62 1 calc PR A 1 C26A C 0.0981(3) 0.7496(5) 0.72570(16) 0.0402(19) Uiso 0.62 1 d PG A 1 H26A H 0.1014 0.7470 0.7659 0.048 Uiso 0.62 1 calc PR A 1 C27A C 0.1473(2) 0.7138(4) 0.6924(2) 0.023(3) Uiso 0.62 1 d PG A 1 H27A H 0.1842 0.6867 0.7099 0.028 Uiso 0.62 1 calc PR A 1 C22B C 0.1568(4) 0.7502(6) 0.6340(3) 0.024(2) Uiso 0.38 1 d PG A 2 C23B C 0.1361(4) 0.8486(7) 0.6130(3) 0.033(3) Uiso 0.38 1 d PG A 2 H23B H 0.1451 0.8686 0.5750 0.040 Uiso 0.38 1 calc PR A 2 C24B C 0.1022(4) 0.9175(6) 0.6475(3) 0.042(3) Uiso 0.38 1 d PG A 2 H24B H 0.0880 0.9847 0.6332 0.051 Uiso 0.38 1 calc PR A 2 C25B C 0.0890(4) 0.8881(6) 0.7031(3) 0.034(3) Uiso 0.38 1 d PG A 2 H25B H 0.0658 0.9352 0.7267 0.041 Uiso 0.38 1 calc PR A 2 C26B C 0.1097(4) 0.7897(7) 0.7241(3) 0.033(3) Uiso 0.38 1 d PG A 2 H26B H 0.1007 0.7696 0.7621 0.040 Uiso 0.38 1 calc PR A 2 C27B C 0.1436(5) 0.7208(6) 0.6896(4) 0.047(8) Uiso 0.38 1 d PG A 2 H27B H 0.1578 0.6536 0.7040 0.057 Uiso 0.38 1 calc PR A 2 N31 N 0.0671(2) 0.3486(3) 0.4603(2) 0.0440(11) Uani 1 1 d D . . C31 C 0.0690(2) 0.4389(4) 0.4621(2) 0.0321(10) Uani 1 1 d D . . C32 C 0.0747(2) 0.5556(4) 0.4648(2) 0.0355(11) Uani 1 1 d D . . H32A H 0.0827 0.5776 0.5042 0.053 Uiso 1 1 calc R . . H32B H 0.0358 0.5887 0.4513 0.053 Uiso 1 1 calc R . . H32C H 0.1094 0.5790 0.4409 0.053 Uiso 1 1 calc R . . N32A N 0.4680(9) 0.4355(19) 0.2463(10) 0.059(6) Uiso 0.25 1 d PD B -1 C33A C 0.4255(10) 0.4462(19) 0.2755(10) 0.040(5) Uiso 0.25 1 d PD B -1 C34A C 0.3830(9) 0.4590(17) 0.3230(8) 0.027(3) Uiso 0.25 1 d PD B -1 N32B N 0.4939(7) 0.4414(15) 0.2800(8) 0.044(4) Uiso 0.25 1 d PD C -2 C33B C 0.4432(7) 0.4495(14) 0.2935(8) 0.023(4) Uiso 0.25 1 d PD C -2 C34B C 0.3772(7) 0.4582(17) 0.3068(8) 0.027(3) Uiso 0.25 1 d PD C -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 Ce1 0.02117(13) 0.01275(11) 0.01087(12) -0.00031(7) -0.00009(8) 0.00058(7) Fe1 0.0205(3) 0.0136(2) 0.0099(2) 0.00021(18) 0.00124(19) 0.00070(19) O1 0.0191(13) 0.0133(12) 0.0117(12) 0.0018(9) -0.0023(10) 0.0022(10) N1 0.0244(17) 0.0143(15) 0.0181(17) -0.0003(12) -0.0050(13) -0.0008(12) C1 0.0184(19) 0.0206(19) 0.030(2) -0.0042(16) -0.0029(16) -0.0004(15) C2 0.024(2) 0.0215(19) 0.023(2) -0.0042(15) 0.0054(16) -0.0022(16) O2 0.0203(13) 0.0169(13) 0.0183(14) -0.0021(10) -0.0004(11) -0.0006(10) C3 0.026(2) 0.0202(19) 0.0178(19) 0.0005(15) -0.0089(16) -0.0001(15) C4 0.027(2) 0.0181(18) 0.0178(19) 0.0026(14) -0.0054(16) 0.0016(15) O3 0.0234(14) 0.0163(12) 0.0127(13) -0.0003(10) -0.0027(10) 0.0000(10) C5 0.030(2) 0.0191(19) 0.027(2) -0.0026(16) -0.0064(17) -0.0043(16) C6 0.027(2) 0.0165(18) 0.034(2) -0.0015(16) -0.0033(18) -0.0032(16) O4 0.0285(16) 0.0176(14) 0.0324(17) 0.0083(12) -0.0049(13) -0.0038(12) O5 0.0266(14) 0.0135(12) 0.0142(13) 0.0008(10) 0.0008(11) 0.0029(10) O6 0.0303(15) 0.0194(13) 0.0089(13) -0.0007(10) -0.0013(11) 0.0028(11) C7 0.0177(18) 0.0200(18) 0.020(2) 0.0015(15) 0.0005(15) -0.0033(14) C8 0.0201(18) 0.0192(18) 0.0100(17) 0.0015(14) 0.0009(14) -0.0027(14) C9 0.031(2) 0.021(2) 0.019(2) -0.0015(15) -0.0001(17) 0.0029(16) C10 0.033(2) 0.029(2) 0.0112(18) -0.0030(15) 0.0024(16) 0.0026(17) C11 0.029(2) 0.027(2) 0.017(2) 0.0081(16) -0.0014(16) -0.0010(17) C12 0.035(2) 0.0160(18) 0.021(2) 0.0022(15) -0.0036(17) 0.0000(16) C13 0.028(2) 0.0207(19) 0.0113(18) -0.0006(14) -0.0026(15) 0.0007(15) O7 0.0229(14) 0.0181(13) 0.0168(14) 0.0004(10) 0.0030(11) 0.0022(11) O8 0.0242(14) 0.0184(13) 0.0160(14) -0.0013(10) 0.0023(11) 0.0003(11) C14 0.0231(19) 0.0227(19) 0.0095(17) -0.0026(14) -0.0029(14) -0.0005(15) C15 0.0200(19) 0.0251(19) 0.0129(18) 0.0003(14) -0.0017(15) 0.0006(15) C16 0.025(2) 0.027(2) 0.027(2) -0.0021(16) 0.0008(18) 0.0041(16) C17 0.032(2) 0.036(3) 0.033(3) -0.0089(19) 0.003(2) 0.0092(19) C18 0.021(2) 0.051(3) 0.029(2) -0.003(2) 0.0067(18) 0.004(2) C19 0.028(2) 0.037(2) 0.032(2) -0.0013(19) 0.0062(19) -0.0077(19) C20 0.025(2) 0.027(2) 0.029(2) -0.0026(17) 0.0002(17) 0.0002(17) O9 0.0301(15) 0.0172(13) 0.0157(14) -0.0024(10) -0.0037(11) 0.0035(11) O10 0.0332(16) 0.0164(13) 0.0165(14) 0.0007(10) -0.0015(12) 0.0031(11) C21 0.024(2) 0.0200(18) 0.019(2) -0.0030(15) -0.0002(16) -0.0005(15) N31 0.050(3) 0.033(2) 0.049(3) -0.0063(19) -0.015(2) 0.0091(19) C31 0.032(2) 0.034(3) 0.031(3) -0.0009(19) -0.0094(19) 0.0054(19) C32 0.032(2) 0.029(2) 0.045(3) -0.001(2) -0.007(2) 0.0057(19) _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 Ce1 O2 2.417(3) . ? Ce1 O3 2.445(3) . ? Ce1 O6 2.484(3) . ? Ce1 O1 2.508(3) . ? Ce1 O8 2.525(3) 7_556 ? Ce1 O9 2.546(3) . ? Ce1 O4 2.580(3) . ? Ce1 O10 2.607(3) . ? Ce1 N1 2.698(3) . ? Fe1 O2 1.955(3) . ? Fe1 O3 1.971(3) 7_556 ? Fe1 O7 1.998(3) . ? Fe1 O5 2.019(3) . ? Fe1 O1 2.055(3) . ? Fe1 O1 2.068(3) 7_556 ? O1 Fe1 2.068(3) 7_556 ? O1 H1 0.85(3) . ? N1 C5 1.482(5) . ? N1 C3 1.483(5) . ? N1 C1 1.489(5) . ? C1 C2 1.531(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.413(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.519(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.417(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.971(3) 7_556 ? C5 C6 1.507(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.430(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.87(3) . ? O5 C7 1.275(5) . ? O6 C7 1.262(5) . ? C7 C8 1.495(5) . ? C8 C13 1.393(5) . ? C8 C9 1.397(5) . ? C9 C10 1.387(6) . ? C9 H9A 0.9500 . ? C10 C11 1.381(6) . ? C10 H10A 0.9500 . ? C11 C12 1.388(6) . ? C11 H11A 0.9500 . ? C12 C13 1.393(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O7 C14 1.276(5) . ? O8 C14 1.250(5) . ? O8 Ce1 2.525(3) 7_556 ? C14 C15 1.499(5) . ? C15 C20 1.392(6) . ? C15 C16 1.393(6) . ? C16 C17 1.382(7) . ? C16 H16A 0.9500 . ? C17 C18 1.383(7) . ? C17 H17A 0.9500 . ? C18 C19 1.380(7) . ? C18 H18A 0.9500 . ? C19 C20 1.392(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? O9 C21 1.254(5) . ? O10 C21 1.283(5) . ? C21 C22A 1.500(5) . ? C21 C22B 1.530(7) . ? C22A C23A 1.3900 . ? C22A C27A 1.3900 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A H27A 0.9500 . ? C22B C23B 1.3900 . ? C22B C27B 1.3900 . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B H27B 0.9500 . ? N31 C31 1.124(6) . ? C31 C32 1.456(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32A C33A 1.152(15) . ? C33A C34A 1.456(15) . ? N32B C33B 1.138(14) . ? C33B C34B 1.451(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ce1 O3 79.89(9) . . ? O2 Ce1 O6 73.98(9) . . ? O3 Ce1 O6 136.95(9) . . ? O2 Ce1 O1 65.89(9) . . ? O3 Ce1 O1 66.61(9) . . ? O6 Ce1 O1 71.63(9) . . ? O2 Ce1 O8 133.81(9) . 7_556 ? O3 Ce1 O8 72.27(9) . 7_556 ? O6 Ce1 O8 102.64(9) . 7_556 ? O1 Ce1 O8 69.41(9) . 7_556 ? O2 Ce1 O9 146.28(9) . . ? O3 Ce1 O9 90.67(9) . . ? O6 Ce1 O9 129.12(9) . . ? O1 Ce1 O9 138.80(9) . . ? O8 Ce1 O9 71.09(9) 7_556 . ? O2 Ce1 O4 82.78(9) . . ? O3 Ce1 O4 128.68(9) . . ? O6 Ce1 O4 81.39(10) . . ? O1 Ce1 O4 142.95(9) . . ? O8 Ce1 O4 143.18(9) 7_556 . ? O9 Ce1 O4 78.13(10) . . ? O2 Ce1 O10 145.33(9) . . ? O3 Ce1 O10 134.64(9) . . ? O6 Ce1 O10 78.66(9) . . ? O1 Ce1 O10 124.23(9) . . ? O8 Ce1 O10 72.71(9) 7_556 . ? O9 Ce1 O10 50.84(9) . . ? O4 Ce1 O10 72.32(10) . . ? O2 Ce1 N1 66.04(10) . . ? O3 Ce1 N1 65.99(9) . . ? O6 Ce1 N1 128.32(10) . . ? O1 Ce1 N1 116.29(9) . . ? O8 Ce1 N1 128.55(10) 7_556 . ? O9 Ce1 N1 80.51(10) . . ? O4 Ce1 N1 62.81(10) . . ? O10 Ce1 N1 119.22(9) . . ? O2 Fe1 O3 176.38(11) . 7_556 ? O2 Fe1 O7 91.26(11) . . ? O3 Fe1 O7 90.69(11) 7_556 . ? O2 Fe1 O5 91.23(11) . . ? O3 Fe1 O5 91.40(11) 7_556 . ? O7 Fe1 O5 100.75(11) . . ? O2 Fe1 O1 83.81(11) . . ? O3 Fe1 O1 93.66(11) 7_556 . ? O7 Fe1 O1 167.52(11) . . ? O5 Fe1 O1 90.85(10) . . ? O2 Fe1 O1 92.21(11) . 7_556 ? O3 Fe1 O1 84.65(11) 7_556 7_556 ? O7 Fe1 O1 92.56(11) . 7_556 ? O5 Fe1 O1 166.18(11) . 7_556 ? O1 Fe1 O1 76.23(11) . 7_556 ? Fe1 O1 Fe1 103.77(11) . 7_556 ? Fe1 O1 Ce1 101.05(10) . . ? Fe1 O1 Ce1 101.09(10) 7_556 . ? Fe1 O1 H1 122(3) . . ? Fe1 O1 H1 116(3) 7_556 . ? Ce1 O1 H1 110(3) . . ? C5 N1 C3 108.7(3) . . ? C5 N1 C1 112.0(3) . . ? C3 N1 C1 111.6(3) . . ? C5 N1 Ce1 108.2(2) . . ? C3 N1 Ce1 104.5(2) . . ? C1 N1 Ce1 111.5(2) . . ? N1 C1 C2 113.0(3) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C1 109.8(3) . . ? O2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 O2 Fe1 133.0(2) . . ? C2 O2 Ce1 119.4(2) . . ? Fe1 O2 Ce1 107.42(12) . . ? N1 C3 C4 111.9(3) . . ? N1 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N1 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 109.9(3) . . ? O3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 O3 Fe1 122.9(2) . 7_556 ? C4 O3 Ce1 123.3(2) . . ? Fe1 O3 Ce1 106.27(11) 7_556 . ? N1 C5 C6 111.6(3) . . ? N1 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N1 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? O4 C6 C5 108.0(3) . . ? O4 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O4 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C6 O4 Ce1 123.9(2) . . ? C6 O4 H4 110(3) . . ? Ce1 O4 H4 127(3) . . ? C7 O5 Fe1 128.9(3) . . ? C7 O6 Ce1 137.3(3) . . ? O6 C7 O5 125.2(4) . . ? O6 C7 C8 118.3(3) . . ? O5 C7 C8 116.4(4) . . ? C13 C8 C9 119.0(4) . . ? C13 C8 C7 119.9(3) . . ? C9 C8 C7 121.1(3) . . ? C10 C9 C8 120.6(4) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C11 C10 C9 120.2(4) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C12 C13 C8 120.1(4) . . ? C12 C13 H13A 119.9 . . ? C8 C13 H13A 119.9 . . ? C14 O7 Fe1 127.3(3) . . ? C14 O8 Ce1 138.3(3) . 7_556 ? O8 C14 O7 125.1(4) . . ? O8 C14 C15 118.5(3) . . ? O7 C14 C15 116.4(3) . . ? C20 C15 C16 119.7(4) . . ? C20 C15 C14 120.6(4) . . ? C16 C15 C14 119.7(4) . . ? C17 C16 C15 119.9(4) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 120.6(4) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 120.5(4) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C15 119.6(4) . . ? C19 C20 H20A 120.2 . . ? C15 C20 H20A 120.2 . . ? C21 O9 Ce1 94.0(2) . . ? C21 O10 Ce1 90.5(2) . . ? O9 C21 O10 121.4(4) . . ? O9 C21 C22A 118.6(4) . . ? O10 C21 C22A 119.1(4) . . ? O9 C21 C22B 118.6(5) . . ? O10 C21 C22B 119.1(5) . . ? C23A C22A C27A 120.0 . . ? C23A C22A C21 120.6(3) . . ? C27A C22A C21 119.1(3) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C25A C26A C27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C26A C27A C22A 120.0 . . ? C26A C27A H27A 120.0 . . ? C22A C27A H27A 120.0 . . ? C23B C22B C27B 120.0 . . ? C23B C22B C21 123.3(5) . . ? C27B C22B C21 116.7(5) . . ? C24B C23B C22B 120.0 . . ? C24B C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C27B C26B C25B 120.0 . . ? C27B C26B H26B 120.0 . . ? C25B C26B H26B 120.0 . . ? C26B C27B C22B 120.0 . . ? C26B C27B H27B 120.0 . . ? C22B C27B H27B 120.0 . . ? N31 C31 C32 177.3(5) . . ? 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 . . ? N32A C33A C34A 166(3) . . ? N32B C33B C34B 176(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N31 0.85(3) 2.31(3) 3.151(5) 171(4) . O4 H4 O10 0.87(3) 1.80(3) 2.671(4) 173(5) 7_566 _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.315 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.143 data_amer16b _database_code_depnum_ccdc_archive 'CCDC 918952' #TrackingRef 'fe2ln2_monster_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H58 Fe2 Gd2 N2 O20, 3(C2 H3 N)' _chemical_formula_sum 'C60 H67 Fe2 Gd2 N5 O20' _chemical_formula_weight 1604.39 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.4105(14) _cell_length_b 12.3502(8) _cell_length_c 23.3265(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.210(1) _cell_angle_gamma 90.00 _cell_volume 6168.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15437 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 26.68 _exptl_crystal_description block _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 2.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details 'TWINABS 1.05 (Bruker AXS Inc., 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19191 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_unetI/netI 0.0852 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.63 _reflns_number_total 6423 _reflns_number_gt 4791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The phenyl ring of one benzoate ligand was disordered, and refined using partial-occupancy (66% or 34%) isotropic carbon atoms in two rigid hexagons. A similarity restraint was applied to the U(iso) of the two closely-spaced disordered partial C(ipso) atoms: SIMU 0.01 C23A C23B O-H distances were restrained: DFIX 0.88 0.04 O1 H1 O4 H4 One lattice MeCN (N32-C33-C34) was two-fold disordered across a twofold axis; its geometry was restrained to be similar to that of the ordered molecule: SAME N31 > C32 ; _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^)+(0.0432P)^2^+1.1810P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6423 _refine_ls_number_parameters 378 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Gd1 Gd 0.253470(13) 0.51053(2) 0.464558(11) 0.01826(10) Uani 1 1 d . . . Fe1 Fe 0.28197(4) 0.71891(6) 0.56051(3) 0.01819(19) Uani 1 1 d . . . O1 O 0.21038(18) 0.6737(3) 0.50674(15) 0.0173(8) Uani 1 1 d D . . H1 H 0.1733(18) 0.669(5) 0.518(2) 0.021 Uiso 1 1 d D . . N1 N 0.3640(2) 0.5178(4) 0.4154(2) 0.0239(11) Uani 1 1 d . . . C1 C 0.4096(3) 0.5769(4) 0.4522(2) 0.0238(13) Uani 1 1 d . . . H1A H 0.4139 0.6520 0.4379 0.029 Uiso 1 1 calc R . . H1B H 0.4510 0.5416 0.4490 0.029 Uiso 1 1 calc R . . C2 C 0.3907(3) 0.5801(5) 0.5149(2) 0.0245(13) Uani 1 1 d . . . H2A H 0.3992 0.5090 0.5330 0.029 Uiso 1 1 calc R . . H2B H 0.4157 0.6357 0.5354 0.029 Uiso 1 1 calc R . . O2 O 0.32659(18) 0.6049(3) 0.51949(16) 0.0214(9) Uani 1 1 d . . . C3 C 0.3529(3) 0.5743(4) 0.3602(2) 0.0232(13) Uani 1 1 d . . . H3A H 0.3280 0.5271 0.3345 0.028 Uiso 1 1 calc R . . H3B H 0.3934 0.5889 0.3414 0.028 Uiso 1 1 calc R . . C4 C 0.3184(3) 0.6806(4) 0.3695(2) 0.0228(13) Uani 1 1 d . . . H4A H 0.3464 0.7334 0.3885 0.027 Uiso 1 1 calc R . . H4B H 0.3053 0.7110 0.3321 0.027 Uiso 1 1 calc R . . O3 O 0.26519(18) 0.6627(3) 0.40400(15) 0.0205(8) Uani 1 1 d . . . C5 C 0.3846(3) 0.4063(4) 0.4039(3) 0.0268(14) Uani 1 1 d . . . H5A H 0.4275 0.4076 0.3881 0.032 Uiso 1 1 calc R . . H5B H 0.3568 0.3732 0.3748 0.032 Uiso 1 1 calc R . . C6 C 0.3839(3) 0.3386(5) 0.4575(3) 0.0298(14) Uani 1 1 d . . . H6A H 0.3893 0.2612 0.4478 0.036 Uiso 1 1 calc R . . H6B H 0.4183 0.3607 0.4834 0.036 Uiso 1 1 calc R . . O4 O 0.3247(2) 0.3553(3) 0.48481(18) 0.0291(10) Uani 1 1 d D . . H4 H 0.315(3) 0.296(4) 0.503(3) 0.035 Uiso 1 1 d D . . O5 O 0.25250(18) 0.6108(3) 0.61864(15) 0.0206(8) Uani 1 1 d . . . O6 O 0.22651(19) 0.4688(3) 0.56272(15) 0.0220(9) Uani 1 1 d . . . C7 C 0.2337(2) 0.5136(4) 0.6113(2) 0.0183(11) Uani 1 1 d . . . C8 C 0.2194(3) 0.4500(4) 0.6637(2) 0.0220(12) Uani 1 1 d . . . C9 C 0.2048(3) 0.3411(4) 0.6595(2) 0.0210(12) Uani 1 1 d . . . H9A H 0.2027 0.3074 0.6230 0.025 Uiso 1 1 calc R . . C10 C 0.1933(3) 0.2809(5) 0.7088(2) 0.0261(13) Uani 1 1 d . . . H10A H 0.1842 0.2058 0.7060 0.031 Uiso 1 1 calc R . . C11 C 0.1950(3) 0.3306(5) 0.7621(2) 0.0260(13) Uani 1 1 d . . . H11A H 0.1866 0.2896 0.7956 0.031 Uiso 1 1 calc R . . C12 C 0.2090(3) 0.4396(5) 0.7666(2) 0.0270(14) Uani 1 1 d . . . H12A H 0.2101 0.4738 0.8031 0.032 Uiso 1 1 calc R . . C13 C 0.2214(3) 0.4984(5) 0.7174(2) 0.0245(12) Uani 1 1 d . . . H13A H 0.2315 0.5731 0.7205 0.029 Uiso 1 1 calc R . . O7 O 0.36037(18) 0.7733(3) 0.59611(15) 0.0218(8) Uani 1 1 d . . . O8 O 0.35057(18) 0.9511(3) 0.57640(15) 0.0215(9) Uani 1 1 d . . . C14 C 0.3793(3) 0.8713(4) 0.5984(2) 0.0216(12) Uani 1 1 d . . . C15 C 0.4385(3) 0.8903(5) 0.6306(2) 0.0242(13) Uani 1 1 d . . . C16 C 0.4584(3) 0.9961(5) 0.6414(3) 0.0312(14) Uani 1 1 d . . . H16A H 0.4345 1.0558 0.6281 0.037 Uiso 1 1 calc R . . C17 C 0.5129(3) 1.0133(6) 0.6716(3) 0.0355(16) Uani 1 1 d . . . H17A H 0.5260 1.0855 0.6790 0.043 Uiso 1 1 calc R . . C18 C 0.5485(3) 0.9294(6) 0.6912(3) 0.0378(17) Uani 1 1 d . . . H18A H 0.5860 0.9425 0.7121 0.045 Uiso 1 1 calc R . . C19 C 0.5288(3) 0.8241(6) 0.6800(3) 0.0394(17) Uani 1 1 d . . . H19A H 0.5532 0.7646 0.6929 0.047 Uiso 1 1 calc R . . C20 C 0.4739(3) 0.8055(5) 0.6502(3) 0.0307(14) Uani 1 1 d . . . H20A H 0.4606 0.7333 0.6432 0.037 Uiso 1 1 calc R . . O9 O 0.23589(19) 0.3968(3) 0.37909(15) 0.0225(9) Uani 1 1 d . A . O10 O 0.19242(19) 0.3346(3) 0.45762(15) 0.0244(9) Uani 1 1 d . A . C21 C 0.1962(3) 0.3368(4) 0.4031(2) 0.0221(12) Uani 1 1 d . . . C22A C 0.1454(3) 0.2839(6) 0.3671(3) 0.034(3) Uiso 0.66 1 d PG A 1 C23A C 0.1495(3) 0.2894(7) 0.3077(3) 0.036(3) Uiso 0.66 1 d PGU A 1 H23A H 0.1860 0.3179 0.2902 0.044 Uiso 0.66 1 calc PR A 1 C24A C 0.1002(4) 0.2531(8) 0.2738(2) 0.056(4) Uiso 0.66 1 d PG A 1 H24A H 0.1030 0.2568 0.2332 0.067 Uiso 0.66 1 calc PR A 1 C25A C 0.0468(3) 0.2113(7) 0.2993(3) 0.054(3) Uiso 0.66 1 d PG A 1 H25A H 0.0131 0.1865 0.2762 0.065 Uiso 0.66 1 calc PR A 1 C26A C 0.0427(3) 0.2058(6) 0.3587(3) 0.052(3) Uiso 0.66 1 d PG A 1 H26A H 0.0062 0.1773 0.3761 0.063 Uiso 0.66 1 calc PR A 1 C27A C 0.0920(3) 0.2421(6) 0.3926(2) 0.044(3) Uiso 0.66 1 d PG A 1 H27A H 0.0892 0.2383 0.4332 0.052 Uiso 0.66 1 calc PR A 1 C22B C 0.1614(7) 0.2586(11) 0.3678(6) 0.024(4) Uiso 0.34 1 d PG A 2 C23B C 0.1479(8) 0.2917(11) 0.3122(7) 0.052(7) Uiso 0.34 1 d PGU A 2 H23B H 0.1626 0.3596 0.2987 0.062 Uiso 0.34 1 calc PR A 2 C24B C 0.1129(8) 0.2254(14) 0.2762(5) 0.051(7) Uiso 0.34 1 d PG A 2 H24B H 0.1037 0.2480 0.2382 0.061 Uiso 0.34 1 calc PR A 2 C25B C 0.0914(7) 0.1259(12) 0.2959(6) 0.047(5) Uiso 0.34 1 d PG A 2 H25B H 0.0675 0.0806 0.2713 0.056 Uiso 0.34 1 calc PR A 2 C26B C 0.1049(7) 0.0928(10) 0.3515(6) 0.056(6) Uiso 0.34 1 d PG A 2 H26B H 0.0902 0.0249 0.3650 0.067 Uiso 0.34 1 calc PR A 2 C27B C 0.1399(7) 0.1591(11) 0.3875(5) 0.048(6) Uiso 0.34 1 d PG A 2 H27B H 0.1492 0.1365 0.4255 0.057 Uiso 0.34 1 calc PR A 2 N31 N 0.0686(3) 0.6539(4) 0.5386(3) 0.0455(16) Uani 1 1 d D . . C31 C 0.0702(3) 0.5610(5) 0.5377(3) 0.0332(15) Uani 1 1 d D . . C32 C 0.0750(3) 0.4461(5) 0.5349(3) 0.0375(16) Uani 1 1 d D . . H32A H 0.0721 0.4228 0.4948 0.056 Uiso 1 1 calc R . . H32B H 0.0410 0.4133 0.5569 0.056 Uiso 1 1 calc R . . H32C H 0.1153 0.4232 0.5509 0.056 Uiso 1 1 calc R . . N32 N 0.4963(10) 0.4407(19) 0.2228(9) 0.132(9) Uiso 0.50 1 d PD B -1 C33 C 0.4399(8) 0.4457(17) 0.2176(8) 0.075(6) Uiso 0.50 1 d PD B -1 C34 C 0.3825(6) 0.4551(12) 0.1885(6) 0.041(3) Uiso 0.50 1 d PD B -1 H34A H 0.3848 0.4162 0.1519 0.061 Uiso 0.50 1 calc PR B -1 H34B H 0.3735 0.5317 0.1812 0.061 Uiso 0.50 1 calc PR B -1 H34C H 0.3492 0.4240 0.2120 0.061 Uiso 0.50 1 calc PR B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.02687(17) 0.01304(14) 0.01491(13) 0.00053(11) 0.00542(10) -0.00008(12) Fe1 0.0268(5) 0.0136(4) 0.0142(4) 0.0008(3) 0.0035(3) -0.0007(3) O1 0.020(2) 0.0187(19) 0.0128(17) 0.0021(15) 0.0027(16) -0.0001(17) N1 0.030(3) 0.017(2) 0.024(2) 0.0007(19) 0.008(2) 0.003(2) C1 0.027(3) 0.016(3) 0.028(3) 0.001(2) 0.005(3) 0.001(2) C2 0.032(4) 0.016(3) 0.026(3) -0.001(2) -0.001(3) 0.000(2) O2 0.027(2) 0.0141(19) 0.024(2) -0.0004(15) 0.0064(17) -0.0017(16) C3 0.029(3) 0.020(3) 0.021(3) 0.002(2) 0.012(3) 0.002(2) C4 0.030(3) 0.018(3) 0.020(3) 0.000(2) 0.012(2) 0.000(2) O3 0.029(2) 0.0173(19) 0.0147(18) 0.0032(15) 0.0066(17) -0.0013(17) C5 0.037(4) 0.015(3) 0.029(3) -0.006(2) 0.014(3) 0.001(3) C6 0.036(4) 0.018(3) 0.036(3) 0.001(3) 0.012(3) 0.005(3) O4 0.036(3) 0.019(2) 0.032(2) 0.0085(18) 0.011(2) 0.0030(19) O5 0.030(2) 0.0155(19) 0.0166(18) 0.0018(15) 0.0058(17) -0.0008(16) O6 0.031(2) 0.0197(19) 0.0148(19) -0.0021(15) 0.0062(17) -0.0032(17) C7 0.016(3) 0.021(3) 0.018(3) 0.003(2) -0.002(2) -0.001(2) C8 0.030(3) 0.018(3) 0.018(3) 0.002(2) 0.007(2) 0.002(2) C9 0.031(3) 0.017(3) 0.015(3) 0.000(2) 0.005(2) -0.002(2) C10 0.036(4) 0.019(3) 0.024(3) 0.001(2) 0.000(3) 0.001(3) C11 0.033(4) 0.029(3) 0.016(3) 0.007(2) 0.004(3) 0.003(3) C12 0.037(4) 0.027(3) 0.017(3) -0.002(2) 0.004(3) -0.007(3) C13 0.032(3) 0.022(3) 0.020(3) 0.001(2) 0.004(2) -0.003(3) O7 0.028(2) 0.0164(19) 0.0213(19) -0.0019(15) 0.0043(17) -0.0013(17) O8 0.031(2) 0.0145(19) 0.0189(19) -0.0017(15) 0.0042(17) -0.0050(17) C14 0.030(3) 0.020(3) 0.015(3) -0.002(2) 0.007(2) -0.003(2) C15 0.030(3) 0.023(3) 0.019(3) -0.001(2) 0.008(3) -0.002(3) C16 0.028(3) 0.037(4) 0.029(3) 0.000(3) 0.003(3) -0.005(3) C17 0.035(4) 0.037(4) 0.034(3) -0.010(3) 0.007(3) -0.012(3) C18 0.027(4) 0.059(5) 0.028(3) -0.005(3) 0.002(3) -0.007(3) C19 0.040(4) 0.044(4) 0.035(4) 0.001(3) 0.006(3) 0.000(3) C20 0.031(4) 0.030(3) 0.032(3) -0.002(3) 0.000(3) -0.002(3) O9 0.035(2) 0.0163(19) 0.0163(19) -0.0041(15) 0.0066(17) -0.0001(17) O10 0.038(3) 0.020(2) 0.0152(19) 0.0014(15) 0.0061(17) -0.0061(18) C21 0.031(3) 0.012(3) 0.023(3) -0.001(2) 0.005(3) 0.000(2) N31 0.060(4) 0.026(3) 0.050(4) -0.004(3) 0.016(3) -0.010(3) C31 0.029(4) 0.039(4) 0.032(3) -0.003(3) 0.015(3) -0.007(3) C32 0.038(4) 0.028(3) 0.046(4) 0.000(3) 0.009(3) 0.002(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 Gd1 O2 2.331(4) . ? Gd1 O3 2.365(3) . ? Gd1 O6 2.419(4) . ? Gd1 O1 2.426(4) . ? Gd1 O9 2.466(4) . ? Gd1 O8 2.466(4) 7_566 ? Gd1 O4 2.493(4) . ? Gd1 O10 2.540(4) . ? Gd1 N1 2.636(5) . ? Fe1 O2 1.954(4) . ? Fe1 O3 1.962(4) 7_566 ? Fe1 O7 1.987(4) . ? Fe1 O5 2.007(4) . ? Fe1 O1 2.054(4) . ? Fe1 O1 2.061(4) 7_566 ? O1 Fe1 2.061(4) 7_566 ? O1 H1 0.84(3) . ? N1 C5 1.471(7) . ? N1 C3 1.483(7) . ? N1 C1 1.490(7) . ? C1 C2 1.519(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.411(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.523(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.414(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.962(4) 7_566 ? C5 C6 1.504(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.436(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.87(4) . ? O5 C7 1.277(6) . ? O6 C7 1.269(6) . ? C7 C8 1.486(7) . ? C8 C9 1.383(7) . ? C8 C13 1.390(7) . ? C9 C10 1.392(7) . ? C9 H9A 0.9500 . ? C10 C11 1.387(8) . ? C10 H10A 0.9500 . ? C11 C12 1.383(8) . ? C11 H11A 0.9500 . ? C12 C13 1.385(8) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O7 C14 1.278(7) . ? O8 C14 1.270(7) . ? O8 Gd1 2.466(4) 7_566 ? C14 C15 1.488(8) . ? C15 C20 1.370(9) . ? C15 C16 1.398(8) . ? C16 C17 1.376(9) . ? C16 H16A 0.9500 . ? C17 C18 1.366(10) . ? C17 H17A 0.9500 . ? C18 C19 1.392(10) . ? C18 H18A 0.9500 . ? C19 C20 1.383(9) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? O9 C21 1.261(6) . ? O10 C21 1.276(6) . ? C21 C22B 1.469(12) . ? C21 C22A 1.519(8) . ? C22A C23A 1.3900 . ? C22A C27A 1.3900 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A H27A 0.9500 . ? C22B C23B 1.3900 . ? C22B C27B 1.3900 . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B H27B 0.9500 . ? N31 C31 1.147(8) . ? C31 C32 1.424(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32 C33 1.214(17) . ? C33 C34 1.408(16) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 O2 Gd1 O3 81.88(13) . . ? O2 Gd1 O6 75.41(13) . . ? O3 Gd1 O6 139.54(13) . . ? O2 Gd1 O1 67.52(13) . . ? O3 Gd1 O1 67.89(12) . . ? O6 Gd1 O1 72.57(12) . . ? O2 Gd1 O9 145.99(13) . . ? O3 Gd1 O9 89.18(12) . . ? O6 Gd1 O9 127.43(12) . . ? O1 Gd1 O9 138.04(13) . . ? O2 Gd1 O8 136.12(12) . 7_566 ? O3 Gd1 O8 73.36(13) . 7_566 ? O6 Gd1 O8 100.91(13) . 7_566 ? O1 Gd1 O8 69.72(12) . 7_566 ? O9 Gd1 O8 70.19(12) . 7_566 ? O2 Gd1 O4 82.59(14) . . ? O3 Gd1 O4 131.14(13) . . ? O6 Gd1 O4 78.75(13) . . ? O1 Gd1 O4 142.64(13) . . ? O9 Gd1 O4 78.86(14) . . ? O8 Gd1 O4 140.51(13) 7_566 . ? O2 Gd1 O10 143.77(13) . . ? O3 Gd1 O10 134.21(13) . . ? O6 Gd1 O10 75.74(12) . . ? O1 Gd1 O10 122.67(13) . . ? O9 Gd1 O10 52.02(12) . . ? O8 Gd1 O10 71.08(13) 7_566 . ? O4 Gd1 O10 70.65(14) . . ? O2 Gd1 N1 67.65(14) . . ? O3 Gd1 N1 67.38(14) . . ? O6 Gd1 N1 129.57(14) . . ? O1 Gd1 N1 119.45(13) . . ? O9 Gd1 N1 78.60(14) . . ? O8 Gd1 N1 129.50(14) 7_566 . ? O4 Gd1 N1 63.84(14) . . ? O10 Gd1 N1 117.66(13) . . ? O2 Fe1 O3 175.62(16) . 7_566 ? O2 Fe1 O7 91.98(16) . . ? O3 Fe1 O7 90.40(16) 7_566 . ? O2 Fe1 O5 90.38(15) . . ? O3 Fe1 O5 92.72(15) 7_566 . ? O7 Fe1 O5 102.11(15) . . ? O2 Fe1 O1 82.54(16) . . ? O3 Fe1 O1 94.36(16) 7_566 . ? O7 Fe1 O1 166.99(15) . . ? O5 Fe1 O1 89.77(15) . . ? O2 Fe1 O1 92.91(15) . 7_566 ? O3 Fe1 O1 83.34(15) 7_566 7_566 ? O7 Fe1 O1 91.79(15) . 7_566 ? O5 Fe1 O1 165.60(16) . 7_566 ? O1 Fe1 O1 76.78(16) . 7_566 ? Fe1 O1 Fe1 103.22(16) . 7_566 ? Fe1 O1 Gd1 100.91(15) . . ? Fe1 O1 Gd1 101.20(14) 7_566 . ? Fe1 O1 H1 123(4) . . ? Fe1 O1 H1 111(4) 7_566 . ? Gd1 O1 H1 115(4) . . ? C5 N1 C3 109.2(4) . . ? C5 N1 C1 111.6(5) . . ? C3 N1 C1 111.9(4) . . ? C5 N1 Gd1 108.5(3) . . ? C3 N1 Gd1 104.6(3) . . ? C1 N1 Gd1 110.7(3) . . ? N1 C1 C2 113.1(5) . . ? N1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C1 109.9(5) . . ? O2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 O2 Fe1 132.1(3) . . ? C2 O2 Gd1 120.1(3) . . ? Fe1 O2 Gd1 107.50(17) . . ? N1 C3 C4 111.0(4) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 109.8(4) . . ? O3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 O3 Fe1 122.7(3) . 7_566 ? C4 O3 Gd1 123.5(3) . . ? Fe1 O3 Gd1 106.52(15) 7_566 . ? N1 C5 C6 111.3(5) . . ? N1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O4 C6 C5 107.6(5) . . ? O4 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O4 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 O4 Gd1 124.5(3) . . ? C6 O4 H4 108(4) . . ? Gd1 O4 H4 126(4) . . ? C7 O5 Fe1 129.3(3) . . ? C7 O6 Gd1 136.3(3) . . ? O6 C7 O5 124.5(5) . . ? O6 C7 C8 118.6(5) . . ? O5 C7 C8 116.9(5) . . ? C9 C8 C13 119.2(5) . . ? C9 C8 C7 120.2(5) . . ? C13 C8 C7 120.6(5) . . ? C8 C9 C10 120.1(5) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 120.0(5) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 C11 C10 120.3(5) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C13 119.3(5) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C12 C13 C8 121.1(5) . . ? C12 C13 H13A 119.4 . . ? C8 C13 H13A 119.4 . . ? C14 O7 Fe1 127.3(4) . . ? C14 O8 Gd1 137.9(4) . 7_566 ? O8 C14 O7 124.4(5) . . ? O8 C14 C15 119.5(5) . . ? O7 C14 C15 116.1(5) . . ? C20 C15 C16 119.1(6) . . ? C20 C15 C14 121.1(5) . . ? C16 C15 C14 119.8(5) . . ? C17 C16 C15 119.7(6) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C18 C17 C16 121.7(6) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C17 C18 C19 118.5(7) . . ? C17 C18 H18A 120.8 . . ? C19 C18 H18A 120.8 . . ? C20 C19 C18 120.5(7) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C15 C20 C19 120.6(6) . . ? C15 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C21 O9 Gd1 94.4(3) . . ? C21 O10 Gd1 90.6(3) . . ? O9 C21 O10 120.0(5) . . ? O9 C21 C22B 118.6(7) . . ? O10 C21 C22B 120.7(7) . . ? O9 C21 C22A 119.4(5) . . ? O10 C21 C22A 119.7(5) . . ? C23A C22A C27A 120.0 . . ? C23A C22A C21 118.8(5) . . ? C27A C22A C21 120.7(5) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C25A C26A C27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C26A C27A C22A 120.0 . . ? C26A C27A H27A 120.0 . . ? C22A C27A H27A 120.0 . . ? C23B C22B C27B 120.0 . . ? C23B C22B C21 115.6(10) . . ? C27B C22B C21 124.3(10) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C26B 120.0 . . ? C24B C25B H25B 120.0 . . ? C26B C25B H25B 120.0 . . ? C27B C26B C25B 120.0 . . ? C27B C26B H26B 120.0 . . ? C25B C26B H26B 120.0 . . ? C26B C27B C22B 120.0 . . ? C26B C27B H27B 120.0 . . ? C22B C27B H27B 120.0 . . ? N31 C31 C32 177.0(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 . . ? N32 C33 C34 157(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N31 0.84(3) 2.30(4) 3.137(7) 175(5) . O4 H4 O10 0.87(4) 1.86(4) 2.728(5) 170(6) 7_556 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.606 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.164 data_am16tb2 _database_code_depnum_ccdc_archive 'CCDC 918953' #TrackingRef 'fe2ln2_monster_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C54 H58 Fe2 N2 O20 TB2), 3(C2 H3 N)' _chemical_formula_sum 'C60 H67 Fe2 N5 O20 Tb2' _chemical_formula_weight 1607.73 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.8689(19) _cell_length_b 15.9021(18) _cell_length_c 21.929(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.222(7) _cell_angle_gamma 90.00 _cell_volume 6174.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 5320 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 25.33 _exptl_crystal_description block _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 2.803 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19451 _diffrn_reflns_av_R_equivalents 0.1064 _diffrn_reflns_av_unetI/netI 0.1277 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5647 _reflns_number_gt 3189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. All H atoms were placed in calculated positions, including H(1) (AFIX 13) and H(4) (AFIX 43) ; _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^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5647 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 Tb1 Tb 0.15453(3) 0.40605(3) 0.49582(3) 0.03434(14) Uani 1 1 d . . . Fe1 Fe 0.17393(7) 0.19757(9) 0.46315(7) 0.0354(3) Uani 1 1 d . . . O1 O 0.2195(3) 0.2783(4) 0.5400(3) 0.0321(15) Uani 1 1 d . . . H1 H 0.2171 0.2599 0.5829 0.039 Uiso 1 1 calc R . . N1 N 0.1538(4) 0.4620(5) 0.3832(4) 0.040(2) Uani 1 1 d . . . C1 C 0.1343(6) 0.3932(7) 0.3325(5) 0.051(3) Uani 1 1 d . . . H1A H 0.1812 0.3726 0.3269 0.061 Uiso 1 1 calc R . . H1B H 0.1014 0.4164 0.2904 0.061 Uiso 1 1 calc R . . C2 C 0.0942(6) 0.3200(6) 0.3518(5) 0.046(3) Uani 1 1 d . . . H2A H 0.0412 0.3355 0.3447 0.055 Uiso 1 1 calc R . . H2B H 0.0942 0.2704 0.3245 0.055 Uiso 1 1 calc R . . O2 O 0.1317(4) 0.3005(4) 0.4175(3) 0.0376(16) Uani 1 1 d . . . C3 C 0.2325(6) 0.4940(7) 0.3963(6) 0.048(3) Uani 1 1 d . . . H3A H 0.2389 0.5090 0.3547 0.058 Uiso 1 1 calc R . . H3B H 0.2406 0.5455 0.4233 0.058 Uiso 1 1 calc R . . C4 C 0.2899(6) 0.4291(6) 0.4308(5) 0.044(3) Uani 1 1 d . . . H4A H 0.2870 0.3809 0.4016 0.052 Uiso 1 1 calc R . . H4B H 0.3413 0.4535 0.4434 0.052 Uiso 1 1 calc R . . O3 O 0.2759(3) 0.4015(4) 0.4871(3) 0.0358(14) Uani 1 1 d . . . C5 C 0.0992(6) 0.5320(7) 0.3627(6) 0.050(3) Uani 1 1 d . . . H5A H 0.0951 0.5507 0.3186 0.060 Uiso 1 1 calc R . . H5B H 0.1173 0.5801 0.3927 0.060 Uiso 1 1 calc R . . C6 C 0.0229(6) 0.5045(8) 0.3627(6) 0.061(3) Uani 1 1 d . . . H6A H -0.0104 0.5540 0.3579 0.073 Uiso 1 1 calc R . . H6B H -0.0008 0.4659 0.3258 0.073 Uiso 1 1 calc R . . O4 O 0.0329(3) 0.4625(4) 0.4231(4) 0.0447(18) Uani 1 1 d . . . H4 H -0.0101 0.4561 0.4358 0.054 Uiso 1 1 calc R . . O5 O 0.0834(3) 0.1828(4) 0.4896(3) 0.0420(17) Uani 1 1 d . . . O6 O 0.0651(3) 0.3146(4) 0.5206(3) 0.0382(16) Uani 1 1 d . . . C7 C 0.0499(5) 0.2386(6) 0.5136(5) 0.036(2) Uani 1 1 d . . . C8 C -0.0117(5) 0.2026(6) 0.5350(5) 0.036(2) Uani 1 1 d . . . C9 C -0.0482(7) 0.2556(8) 0.5654(7) 0.069(4) Uani 1 1 d . . . H9A H -0.0350 0.3134 0.5719 0.083 Uiso 1 1 calc R . . C10 C -0.1050(8) 0.2217(9) 0.5865(8) 0.085(5) Uani 1 1 d . . . H10A H -0.1297 0.2566 0.6081 0.103 Uiso 1 1 calc R . . C11 C -0.1250(7) 0.1370(9) 0.5755(7) 0.070(4) Uani 1 1 d . . . H11A H -0.1636 0.1144 0.5893 0.085 Uiso 1 1 calc R . . C12 C -0.0887(6) 0.0862(8) 0.5447(6) 0.059(3) Uani 1 1 d . . . H12A H -0.1019 0.0284 0.5382 0.070 Uiso 1 1 calc R . . C13 C -0.0321(6) 0.1186(6) 0.5227(6) 0.047(3) Uani 1 1 d . . . H13A H -0.0085 0.0838 0.5001 0.057 Uiso 1 1 calc R . . O7 O 0.1437(4) 0.1333(4) 0.3800(3) 0.0420(17) Uani 1 1 d . . . O8 O 0.2557(4) 0.0680(4) 0.3958(3) 0.0431(18) Uani 1 1 d . . . C14 C 0.1882(6) 0.0846(8) 0.3628(5) 0.045(3) Uani 1 1 d . . . C15 C 0.1549(6) 0.0444(7) 0.2971(5) 0.045(3) Uani 1 1 d . . . C16 C 0.0897(6) 0.0758(8) 0.2526(5) 0.056(3) Uani 1 1 d . . . H16A H 0.0638 0.1212 0.2638 0.067 Uiso 1 1 calc R . . C17 C 0.0616(8) 0.0400(10) 0.1897(7) 0.081(4) Uani 1 1 d . . . H17A H 0.0178 0.0629 0.1580 0.097 Uiso 1 1 calc R . . C18 C 0.0978(9) -0.0289(11) 0.1741(7) 0.085(5) Uani 1 1 d . . . H18A H 0.0785 -0.0535 0.1321 0.101 Uiso 1 1 calc R . . C19 C 0.1619(8) -0.0606(10) 0.2203(7) 0.084(5) Uani 1 1 d . . . H19A H 0.1866 -0.1078 0.2102 0.100 Uiso 1 1 calc R . . C20 C 0.1909(7) -0.0239(8) 0.2822(6) 0.064(3) Uani 1 1 d . . . H20A H 0.2352 -0.0461 0.3138 0.076 Uiso 1 1 calc R . . O9 O 0.1744(4) 0.5559(4) 0.5099(4) 0.0479(19) Uani 1 1 d . . . O10 O 0.0983(4) 0.5062(4) 0.5591(4) 0.0427(17) Uani 1 1 d . . . C21 C 0.1401(6) 0.5657(6) 0.5503(6) 0.043(3) Uani 1 1 d . . . C22 C 0.1497(6) 0.6451(7) 0.5863(6) 0.052(3) Uani 1 1 d . . . C23 C 0.1915(8) 0.7092(8) 0.5713(7) 0.072(4) Uani 1 1 d . . . H23A H 0.2127 0.7008 0.5383 0.087 Uiso 1 1 calc R . . C24 C 0.2025(10) 0.7867(10) 0.6051(10) 0.108(6) Uani 1 1 d . . . H24A H 0.2324 0.8295 0.5959 0.130 Uiso 1 1 calc R . . C25 C 0.1707(9) 0.7993(10) 0.6501(9) 0.093(5) Uani 1 1 d . . . H25A H 0.1758 0.8521 0.6715 0.112 Uiso 1 1 calc R . . C26 C 0.1306(10) 0.7360(10) 0.6653(9) 0.106(6) Uani 1 1 d . . . H26A H 0.1096 0.7450 0.6984 0.128 Uiso 1 1 calc R . . C27 C 0.1197(8) 0.6589(9) 0.6335(8) 0.081(4) Uani 1 1 d . . . H27A H 0.0913 0.6160 0.6448 0.098 Uiso 1 1 calc R . . N31 N 0.2150(8) 0.2513(8) 0.6724(6) 0.091(4) Uani 1 1 d . . . C31 C 0.1899(8) 0.3073(9) 0.6882(7) 0.070(4) Uani 1 1 d . . . C32 C 0.1586(8) 0.3816(10) 0.7085(9) 0.097(5) Uani 1 1 d . . . H32A H 0.1459 0.4238 0.6738 0.145 Uiso 1 1 calc R . . H32B H 0.1959 0.4050 0.7479 0.145 Uiso 1 1 calc R . . H32C H 0.1129 0.3660 0.7174 0.145 Uiso 1 1 calc R . . N32 N 0.0000 0.3178(13) 0.7500 0.101(6) Uani 1 2 d S . . C33 C 0.0000 0.2497(16) 0.7500 0.083(6) Uani 1 2 d S . . C34 C 0.0000 0.1613(16) 0.7500 0.180(17) Uani 1 2 d S . . H34A H -0.0477 0.1407 0.7530 0.271 Uiso 0.50 1 calc PR . . H34B H 0.0422 0.1407 0.7873 0.271 Uiso 0.50 1 calc PR . . H34C H 0.0054 0.1407 0.7097 0.271 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0325(2) 0.0363(2) 0.0397(3) 0.0008(3) 0.01936(18) 0.0028(3) Fe1 0.0319(7) 0.0388(8) 0.0399(9) -0.0032(7) 0.0180(7) 0.0010(6) O1 0.034(3) 0.034(4) 0.035(4) 0.000(3) 0.020(3) 0.005(3) N1 0.041(5) 0.043(5) 0.044(5) 0.009(4) 0.025(4) 0.004(4) C1 0.051(6) 0.059(8) 0.048(7) 0.010(6) 0.023(5) 0.008(6) C2 0.054(6) 0.043(6) 0.043(7) 0.003(5) 0.019(5) 0.001(5) O2 0.040(4) 0.039(4) 0.035(4) 0.000(3) 0.014(3) 0.006(3) C3 0.049(6) 0.051(6) 0.055(7) 0.013(6) 0.032(6) -0.002(5) C4 0.043(6) 0.052(7) 0.045(6) 0.007(5) 0.028(5) 0.003(5) O3 0.032(3) 0.043(3) 0.040(4) 0.004(4) 0.022(3) 0.006(3) C5 0.053(7) 0.053(7) 0.055(8) 0.032(6) 0.033(6) 0.022(5) C6 0.050(7) 0.072(8) 0.071(9) 0.027(7) 0.034(7) 0.024(6) O4 0.026(3) 0.063(5) 0.050(5) 0.015(4) 0.019(3) 0.011(3) O5 0.033(4) 0.045(4) 0.054(5) -0.005(3) 0.023(3) -0.001(3) O6 0.031(4) 0.038(4) 0.054(5) 0.002(3) 0.027(3) -0.005(3) C7 0.030(5) 0.039(6) 0.048(6) 0.001(5) 0.024(5) -0.002(4) C8 0.024(5) 0.046(6) 0.042(6) 0.003(5) 0.016(4) -0.005(4) C9 0.068(8) 0.063(8) 0.103(11) -0.011(8) 0.064(9) -0.008(7) C10 0.084(10) 0.080(10) 0.133(14) -0.012(10) 0.088(10) -0.011(8) C11 0.064(8) 0.072(9) 0.093(11) 0.001(8) 0.050(8) -0.014(7) C12 0.054(6) 0.053(7) 0.065(8) 0.004(7) 0.015(6) -0.004(6) C13 0.042(6) 0.049(7) 0.057(7) -0.006(5) 0.024(5) -0.007(5) O7 0.039(4) 0.049(4) 0.042(4) -0.011(3) 0.019(3) 0.002(3) O8 0.038(4) 0.052(5) 0.043(4) -0.010(3) 0.019(3) 0.001(3) C14 0.045(6) 0.058(7) 0.040(6) 0.000(6) 0.023(5) -0.005(6) C15 0.042(6) 0.063(7) 0.036(6) -0.013(5) 0.023(5) -0.003(5) C16 0.047(6) 0.079(9) 0.047(7) -0.021(6) 0.023(6) -0.012(6) C17 0.059(8) 0.127(13) 0.054(9) -0.037(9) 0.017(7) -0.001(8) C18 0.083(10) 0.128(14) 0.050(9) -0.039(9) 0.033(8) -0.025(10) C19 0.080(10) 0.128(13) 0.052(9) -0.049(9) 0.035(8) -0.016(9) C20 0.057(7) 0.083(9) 0.057(8) -0.016(7) 0.028(6) -0.001(7) O9 0.056(5) 0.033(3) 0.068(6) -0.003(3) 0.039(5) -0.001(3) O10 0.045(4) 0.034(4) 0.060(5) -0.004(4) 0.032(4) 0.003(3) C21 0.043(6) 0.035(6) 0.056(7) 0.004(5) 0.024(6) 0.002(4) C22 0.056(7) 0.044(7) 0.070(8) -0.003(6) 0.039(7) 0.005(5) C23 0.079(9) 0.055(8) 0.090(11) -0.012(7) 0.038(8) -0.014(7) C24 0.126(14) 0.069(10) 0.156(18) -0.046(11) 0.083(14) -0.033(10) C25 0.096(12) 0.061(9) 0.128(16) -0.030(10) 0.045(11) -0.022(9) C26 0.140(15) 0.079(11) 0.132(16) -0.055(11) 0.088(13) -0.024(10) C27 0.091(10) 0.067(9) 0.107(12) -0.041(9) 0.060(10) -0.021(7) N31 0.154(13) 0.068(8) 0.077(9) 0.002(7) 0.072(9) 0.008(8) C31 0.085(10) 0.069(9) 0.069(10) -0.001(8) 0.043(8) -0.001(8) C32 0.084(10) 0.096(13) 0.133(15) -0.001(10) 0.066(11) 0.010(8) N32 0.137(18) 0.082(13) 0.085(14) 0.000 0.040(13) 0.000 C33 0.071(13) 0.080(16) 0.090(17) 0.000 0.019(12) 0.000 C34 0.22(4) 0.058(16) 0.21(4) 0.000 0.02(3) 0.000 _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 Tb1 O2 2.333(7) . ? Tb1 O3 2.364(5) . ? Tb1 O1 2.397(6) . ? Tb1 O9 2.415(6) . ? Tb1 O6 2.428(6) . ? Tb1 O8 2.430(7) 7_556 ? Tb1 O4 2.467(6) . ? Tb1 O10 2.569(6) . ? Tb1 N1 2.620(8) . ? Fe1 O2 1.940(7) . ? Fe1 O3 1.963(7) 7_556 ? Fe1 O7 1.993(7) . ? Fe1 O5 2.000(6) . ? Fe1 O1 2.056(6) . ? Fe1 O1 2.071(6) 7_556 ? O1 Fe1 2.071(6) 7_556 ? O1 H1 1.0000 . ? N1 C5 1.477(12) . ? N1 C3 1.500(12) . ? N1 C1 1.512(13) . ? C1 C2 1.525(15) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.404(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.498(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.418(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.963(7) 7_556 ? C5 C6 1.505(15) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.436(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.9500 . ? O5 C7 1.300(11) . ? O6 C7 1.238(11) . ? C7 C8 1.509(12) . ? C8 C13 1.390(14) . ? C8 C9 1.396(15) . ? C9 C10 1.413(16) . ? C9 H9A 0.9500 . ? C10 C11 1.398(18) . ? C10 H10A 0.9500 . ? C11 C12 1.377(17) . ? C11 H11A 0.9500 . ? C12 C13 1.413(15) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O7 C14 1.291(12) . ? O8 C14 1.256(11) . ? O8 Tb1 2.430(7) 7_556 ? C14 C15 1.501(14) . ? C15 C16 1.373(15) . ? C15 C20 1.379(15) . ? C16 C17 1.415(16) . ? C16 H16A 0.9500 . ? C17 C18 1.40(2) . ? C17 H17A 0.9500 . ? C18 C19 1.38(2) . ? C18 H18A 0.9500 . ? C19 C20 1.404(17) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? O9 C21 1.276(12) . ? O10 C21 1.287(11) . ? C21 C22 1.467(14) . ? C22 C27 1.358(17) . ? C22 C23 1.396(16) . ? C23 C24 1.415(19) . ? C23 H23A 0.9500 . ? C24 C25 1.34(2) . ? C24 H24A 0.9500 . ? C25 C26 1.37(2) . ? C25 H25A 0.9500 . ? C26 C27 1.390(17) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N31 C31 1.118(16) . ? C31 C32 1.458(19) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32 C33 1.08(2) . ? C33 C34 1.41(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 O2 Tb1 O3 81.7(2) . . ? O2 Tb1 O1 68.1(2) . . ? O3 Tb1 O1 68.4(2) . . ? O2 Tb1 O9 141.7(2) . . ? O3 Tb1 O9 85.9(2) . . ? O1 Tb1 O9 138.5(2) . . ? O2 Tb1 O6 76.6(2) . . ? O3 Tb1 O6 140.1(2) . . ? O1 Tb1 O6 72.5(2) . . ? O9 Tb1 O6 130.7(2) . . ? O2 Tb1 O8 137.0(2) . 7_556 ? O3 Tb1 O8 73.5(2) . 7_556 ? O1 Tb1 O8 70.3(2) . 7_556 ? O9 Tb1 O8 71.5(2) . 7_556 ? O6 Tb1 O8 100.8(2) . 7_556 ? O2 Tb1 O4 83.8(2) . . ? O3 Tb1 O4 132.0(2) . . ? O1 Tb1 O4 143.2(2) . . ? O9 Tb1 O4 78.0(2) . . ? O6 Tb1 O4 78.4(2) . . ? O8 Tb1 O4 138.5(2) 7_556 . ? O2 Tb1 O10 146.9(2) . . ? O3 Tb1 O10 130.9(2) . . ? O1 Tb1 O10 123.8(2) . . ? O9 Tb1 O10 52.7(2) . . ? O6 Tb1 O10 78.6(2) . . ? O8 Tb1 O10 69.2(2) 7_556 . ? O4 Tb1 O10 70.0(2) . . ? O2 Tb1 N1 67.1(2) . . ? O3 Tb1 N1 67.9(2) . . ? O1 Tb1 N1 120.3(2) . . ? O9 Tb1 N1 74.6(3) . . ? O6 Tb1 N1 129.6(2) . . ? O8 Tb1 N1 129.7(2) 7_556 . ? O4 Tb1 N1 64.3(2) . . ? O10 Tb1 N1 115.4(2) . . ? O2 Fe1 O3 175.4(3) . 7_556 ? O2 Fe1 O7 91.4(3) . . ? O3 Fe1 O7 91.6(3) 7_556 . ? O2 Fe1 O5 90.5(3) . . ? O3 Fe1 O5 92.3(3) 7_556 . ? O7 Fe1 O5 101.7(3) . . ? O2 Fe1 O1 82.9(3) . . ? O3 Fe1 O1 93.5(3) 7_556 . ? O7 Fe1 O1 167.5(3) . . ? O5 Fe1 O1 89.6(3) . . ? O2 Fe1 O1 93.3(3) . 7_556 ? O3 Fe1 O1 83.1(2) 7_556 7_556 ? O7 Fe1 O1 92.2(3) . 7_556 ? O5 Fe1 O1 165.5(3) . 7_556 ? O1 Fe1 O1 77.1(3) . 7_556 ? Fe1 O1 Fe1 102.9(3) . 7_556 ? Fe1 O1 Tb1 100.8(2) . . ? Fe1 O1 Tb1 101.3(2) 7_556 . ? Fe1 O1 H1 116.4 . . ? Fe1 O1 H1 116.4 7_556 . ? Tb1 O1 H1 116.4 . . ? C5 N1 C3 110.0(8) . . ? C5 N1 C1 110.8(8) . . ? C3 N1 C1 111.0(8) . . ? C5 N1 Tb1 108.6(6) . . ? C3 N1 Tb1 104.6(6) . . ? C1 N1 Tb1 111.6(6) . . ? N1 C1 C2 111.5(8) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? O2 C2 C1 109.4(9) . . ? O2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C2 O2 Fe1 133.4(6) . . ? C2 O2 Tb1 119.7(6) . . ? Fe1 O2 Tb1 106.8(3) . . ? C4 C3 N1 111.0(8) . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? N1 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 109.5(8) . . ? O3 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O3 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C4 O3 Fe1 122.2(5) . 7_556 ? C4 O3 Tb1 122.5(5) . . ? Fe1 O3 Tb1 105.9(3) 7_556 . ? N1 C5 C6 110.4(8) . . ? N1 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N1 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? O4 C6 C5 108.3(9) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C6 O4 Tb1 124.2(5) . . ? C6 O4 H4 117.9 . . ? Tb1 O4 H4 117.9 . . ? C7 O5 Fe1 128.3(6) . . ? C7 O6 Tb1 134.8(6) . . ? O6 C7 O5 126.3(9) . . ? O6 C7 C8 120.1(9) . . ? O5 C7 C8 113.6(8) . . ? C13 C8 C9 121.6(10) . . ? C13 C8 C7 119.7(9) . . ? C9 C8 C7 118.6(9) . . ? C8 C9 C10 118.8(12) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C11 C10 C9 120.1(13) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C10 119.9(12) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 121.2(12) . . ? C11 C12 H12A 119.4 . . ? C13 C12 H12A 119.4 . . ? C8 C13 C12 118.3(11) . . ? C8 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C14 O7 Fe1 124.4(6) . . ? C14 O8 Tb1 138.8(6) . 7_556 ? O8 C14 O7 126.2(9) . . ? O8 C14 C15 117.9(9) . . ? O7 C14 C15 115.9(9) . . ? C16 C15 C20 120.8(10) . . ? C16 C15 C14 120.2(10) . . ? C20 C15 C14 119.0(10) . . ? C15 C16 C17 119.2(11) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C18 C17 C16 120.3(13) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C19 C18 C17 119.1(13) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? C18 C19 C20 120.6(14) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C15 C20 C19 119.8(13) . . ? C15 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C21 O9 Tb1 96.7(6) . . ? C21 O10 Tb1 89.3(6) . . ? O9 C21 O10 119.8(9) . . ? O9 C21 C22 118.8(9) . . ? O10 C21 C22 121.4(10) . . ? O9 C21 Tb1 57.0(5) . . ? O10 C21 Tb1 64.0(5) . . ? C22 C21 Tb1 167.8(8) . . ? C27 C22 C23 118.7(12) . . ? C27 C22 C21 122.8(11) . . ? C23 C22 C21 118.5(11) . . ? C22 C23 C24 120.3(14) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 119.7(15) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 119.8(15) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C25 C26 C27 121.7(15) . . ? C25 C26 H26A 119.1 . . ? C27 C26 H26A 119.1 . . ? C22 C27 C26 119.7(14) . . ? C22 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? N31 C31 C32 178.7(16) . . ? 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 . . ? N32 C33 C34 180.0 . . ? 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 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N31 1.00 1.98 2.965(13) 166.9 . O4 H4 O10 0.95 1.81 2.684(9) 151.6 5_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.688 _refine_diff_density_min -1.665 _refine_diff_density_rms 0.163 data_a16ho2 _database_code_depnum_ccdc_archive 'CCDC 918954' #TrackingRef 'fe2ln2_monster_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H58 Fe2 Ho2 N2 O20, 3(C2 H3 N)' _chemical_formula_sum 'C60 H67 Fe2 Ho2 N5 O20' _chemical_formula_weight 1619.75 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.8104(15) _cell_length_b 15.9239(13) _cell_length_c 22.0043(17) _cell_angle_alpha 90.00 _cell_angle_beta 110.339(1) _cell_angle_gamma 90.00 _cell_volume 6180.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6449 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.14 _exptl_crystal_description block _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 3.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.588 _exptl_absorpt_correction_T_max 0.854 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14199 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_unetI/netI 0.0529 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.73 _reflns_number_total 6430 _reflns_number_gt 5642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. O-H distances were restrained: DFIX 0.92 0.04 O1 H1 O4 H4 ; _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^)+(0.0405P)^2^+18.4827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6430 _refine_ls_number_parameters 410 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 Ho1 Ho 0.155072(14) 0.405458(15) 0.495562(11) 0.02641(9) Uani 1 1 d . . . Fe1 Fe 0.17362(4) 0.19784(5) 0.46288(4) 0.02634(17) Uani 1 1 d . . . O1 O 0.2193(2) 0.2784(2) 0.53959(17) 0.0264(8) Uani 1 1 d D . . H1 H 0.223(3) 0.261(3) 0.5797(19) 0.032 Uiso 1 1 d D . . N1 N 0.1539(3) 0.4621(3) 0.3826(2) 0.0357(11) Uani 1 1 d . . . C1 C 0.1352(4) 0.3947(4) 0.3340(3) 0.0399(14) Uani 1 1 d . . . H1A H 0.1825 0.3740 0.3290 0.048 Uiso 1 1 calc R . . H1B H 0.1026 0.4178 0.2917 0.048 Uiso 1 1 calc R . . C2 C 0.0944(3) 0.3213(4) 0.3520(3) 0.0377(13) Uani 1 1 d . . . H2A H 0.0409 0.3364 0.3443 0.045 Uiso 1 1 calc R . . H2B H 0.0951 0.2717 0.3250 0.045 Uiso 1 1 calc R . . O2 O 0.1320(2) 0.3025(2) 0.41801(17) 0.0320(8) Uani 1 1 d . . . C3 C 0.2317(3) 0.4944(4) 0.3966(3) 0.0377(13) Uani 1 1 d . . . H3A H 0.2390 0.5457 0.4234 0.045 Uiso 1 1 calc R . . H3B H 0.2388 0.5096 0.3554 0.045 Uiso 1 1 calc R . . C4 C 0.2904(3) 0.4295(4) 0.4320(3) 0.0340(13) Uani 1 1 d . . . H4A H 0.2884 0.3815 0.4029 0.041 Uiso 1 1 calc R . . H4B H 0.3417 0.4545 0.4451 0.041 Uiso 1 1 calc R . . O3 O 0.2758(2) 0.4012(2) 0.48744(17) 0.0289(8) Uani 1 1 d . . . C5 C 0.0997(4) 0.5324(4) 0.3642(3) 0.0435(15) Uani 1 1 d . . . H5A H 0.0945 0.5521 0.3203 0.052 Uiso 1 1 calc R . . H5B H 0.1192 0.5796 0.3948 0.052 Uiso 1 1 calc R . . C6 C 0.0234(4) 0.5063(4) 0.3651(3) 0.0470(16) Uani 1 1 d . . . H6A H -0.0086 0.5564 0.3627 0.056 Uiso 1 1 calc R . . H6B H -0.0023 0.4699 0.3274 0.056 Uiso 1 1 calc R . . O4 O 0.0340(2) 0.4615(3) 0.42396(19) 0.0382(10) Uani 1 1 d D . . H4 H -0.003(3) 0.474(4) 0.439(3) 0.046 Uiso 1 1 d D . . O5 O 0.0829(2) 0.1844(2) 0.4892(2) 0.0363(9) Uani 1 1 d . . . O6 O 0.0661(2) 0.3148(2) 0.52066(19) 0.0337(9) Uani 1 1 d . . . C7 C 0.0500(3) 0.2388(4) 0.5128(3) 0.0306(12) Uani 1 1 d . . . C8 C -0.0115(3) 0.2045(4) 0.5349(3) 0.0314(12) Uani 1 1 d . . . C9 C -0.0468(4) 0.2552(4) 0.5664(4) 0.0502(17) Uani 1 1 d . . . H9A H -0.0332 0.3128 0.5732 0.060 Uiso 1 1 calc R . . C10 C -0.1023(5) 0.2227(5) 0.5883(4) 0.068(2) Uani 1 1 d . . . H10A H -0.1258 0.2576 0.6108 0.081 Uiso 1 1 calc R . . C11 C -0.1229(4) 0.1389(5) 0.5770(4) 0.061(2) Uani 1 1 d . . . H11A H -0.1616 0.1170 0.5910 0.073 Uiso 1 1 calc R . . C12 C -0.0888(4) 0.0880(4) 0.5464(3) 0.0501(17) Uani 1 1 d . . . H12A H -0.1026 0.0304 0.5395 0.060 Uiso 1 1 calc R . . C13 C -0.0329(4) 0.1212(4) 0.5248(3) 0.0416(14) Uani 1 1 d . . . H13A H -0.0092 0.0857 0.5028 0.050 Uiso 1 1 calc R . . O7 O 0.1443(2) 0.1334(3) 0.38006(18) 0.0335(9) Uani 1 1 d . . . O8 O 0.2558(2) 0.0695(2) 0.39588(18) 0.0345(9) Uani 1 1 d . . . C14 C 0.1883(3) 0.0847(4) 0.3629(3) 0.0336(12) Uani 1 1 d . . . C15 C 0.1553(4) 0.0452(4) 0.2971(3) 0.0392(14) Uani 1 1 d . . . C16 C 0.0912(4) 0.0758(5) 0.2516(3) 0.0459(16) Uani 1 1 d . . . H16A H 0.0661 0.1224 0.2620 0.055 Uiso 1 1 calc R . . C17 C 0.0621(5) 0.0408(6) 0.1909(4) 0.068(2) Uani 1 1 d . . . H17A H 0.0171 0.0627 0.1598 0.082 Uiso 1 1 calc R . . C18 C 0.0986(5) -0.0261(7) 0.1757(4) 0.081(3) Uani 1 1 d . . . H18A H 0.0790 -0.0505 0.1338 0.097 Uiso 1 1 calc R . . C19 C 0.1639(5) -0.0584(6) 0.2211(4) 0.071(2) Uani 1 1 d . . . H19A H 0.1891 -0.1049 0.2105 0.085 Uiso 1 1 calc R . . C20 C 0.1918(4) -0.0226(5) 0.2815(4) 0.0532(18) Uani 1 1 d . . . H20A H 0.2366 -0.0445 0.3129 0.064 Uiso 1 1 calc R . . O9 O 0.1757(2) 0.5528(3) 0.5112(2) 0.0389(10) Uani 1 1 d . . . O10 O 0.0989(2) 0.5052(2) 0.5588(2) 0.0369(9) Uani 1 1 d . . . C21 C 0.1398(3) 0.5631(4) 0.5494(3) 0.0336(12) Uani 1 1 d . . . C22 C 0.1505(4) 0.6442(4) 0.5854(3) 0.0403(14) Uani 1 1 d . . . C23 C 0.1920(5) 0.7081(5) 0.5707(4) 0.061(2) Uani 1 1 d . . . H23A H 0.2133 0.7003 0.5378 0.073 Uiso 1 1 calc R . . C24 C 0.2023(6) 0.7835(5) 0.6042(5) 0.077(3) Uani 1 1 d . . . H24A H 0.2316 0.8266 0.5945 0.093 Uiso 1 1 calc R . . C25 C 0.1723(5) 0.7963(5) 0.6491(5) 0.081(3) Uani 1 1 d . . . H25A H 0.1785 0.8494 0.6701 0.097 Uiso 1 1 calc R . . C26 C 0.1319(6) 0.7340(6) 0.6662(5) 0.088(3) Uani 1 1 d . . . H26A H 0.1117 0.7431 0.6997 0.105 Uiso 1 1 calc R . . C27 C 0.1215(5) 0.6580(5) 0.6338(4) 0.068(2) Uani 1 1 d . . . H27A H 0.0937 0.6147 0.6453 0.081 Uiso 1 1 calc R . . N31 N 0.2156(5) 0.2515(5) 0.6731(4) 0.083(2) Uani 1 1 d . . . C31 C 0.1897(5) 0.3065(5) 0.6890(3) 0.0557(19) Uani 1 1 d . . . C32 C 0.1579(6) 0.3807(6) 0.7066(5) 0.084(3) Uani 1 1 d . . . H32A H 0.1429 0.4200 0.6701 0.126 Uiso 1 1 calc R . . H32B H 0.1958 0.4073 0.7441 0.126 Uiso 1 1 calc R . . H32C H 0.1133 0.3654 0.7175 0.126 Uiso 1 1 calc R . . N32 N 0.0000 0.3177(7) 0.7500 0.088(3) Uani 1 2 d S . . C33 C 0.0000 0.2491(9) 0.7500 0.074(3) Uani 1 2 d S . . C34 C 0.0000 0.1569(10) 0.7500 0.157(9) Uani 1 2 d S . . H34A H 0.0062 0.1364 0.7101 0.236 Uiso 0.50 1 calc PR . . H34B H -0.0481 0.1364 0.7522 0.236 Uiso 0.50 1 calc PR . . H34C H 0.0420 0.1364 0.7876 0.236 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.02756(14) 0.02617(14) 0.02970(13) 0.00134(10) 0.01525(10) 0.00293(11) Fe1 0.0246(4) 0.0277(4) 0.0291(4) -0.0033(3) 0.0124(3) 0.0004(3) O1 0.0290(19) 0.0284(19) 0.0261(18) 0.0010(15) 0.0152(15) 0.0000(15) N1 0.042(3) 0.037(3) 0.034(2) 0.010(2) 0.021(2) 0.005(2) C1 0.046(4) 0.052(4) 0.024(3) 0.008(2) 0.014(2) 0.010(3) C2 0.036(3) 0.045(4) 0.033(3) 0.004(3) 0.013(3) 0.004(3) O2 0.032(2) 0.038(2) 0.0272(18) 0.0048(16) 0.0115(16) 0.0088(17) C3 0.044(3) 0.038(3) 0.039(3) 0.009(3) 0.025(3) 0.001(3) C4 0.032(3) 0.039(3) 0.039(3) 0.001(2) 0.023(3) 0.003(2) O3 0.031(2) 0.0264(19) 0.0350(19) 0.0007(16) 0.0183(16) -0.0008(16) C5 0.050(4) 0.039(4) 0.047(4) 0.021(3) 0.025(3) 0.017(3) C6 0.042(4) 0.051(4) 0.048(4) 0.018(3) 0.017(3) 0.021(3) O4 0.033(2) 0.050(3) 0.038(2) 0.0112(19) 0.0190(18) 0.0135(19) O5 0.036(2) 0.033(2) 0.049(2) -0.0072(18) 0.026(2) -0.0039(18) O6 0.031(2) 0.033(2) 0.044(2) 0.0036(17) 0.0222(18) 0.0038(17) C7 0.023(3) 0.040(3) 0.031(3) 0.001(2) 0.011(2) 0.001(2) C8 0.025(3) 0.034(3) 0.037(3) 0.004(2) 0.013(2) 0.001(2) C9 0.048(4) 0.038(4) 0.076(5) -0.003(3) 0.036(4) -0.003(3) C10 0.063(5) 0.072(6) 0.095(6) -0.009(5) 0.060(5) -0.004(4) C11 0.051(4) 0.064(5) 0.083(5) 0.003(4) 0.044(4) -0.017(4) C12 0.047(4) 0.043(4) 0.062(4) 0.001(3) 0.022(3) -0.015(3) C13 0.038(3) 0.039(3) 0.051(4) 0.003(3) 0.020(3) -0.005(3) O7 0.028(2) 0.040(2) 0.033(2) -0.0109(17) 0.0110(16) -0.0007(17) O8 0.033(2) 0.039(2) 0.034(2) -0.0061(17) 0.0152(18) 0.0041(17) C14 0.031(3) 0.035(3) 0.037(3) -0.003(2) 0.015(2) -0.004(2) C15 0.040(3) 0.052(4) 0.032(3) -0.013(3) 0.020(3) -0.005(3) C16 0.043(4) 0.060(4) 0.037(3) -0.009(3) 0.016(3) -0.009(3) C17 0.053(5) 0.108(7) 0.041(4) -0.017(4) 0.013(4) -0.003(5) C18 0.065(6) 0.139(9) 0.045(4) -0.042(5) 0.026(4) -0.023(6) C19 0.069(6) 0.089(6) 0.068(5) -0.041(5) 0.039(5) -0.007(5) C20 0.049(4) 0.058(5) 0.058(4) -0.025(4) 0.027(4) -0.008(3) O9 0.046(3) 0.030(2) 0.050(2) 0.0005(18) 0.029(2) -0.0014(18) O10 0.037(2) 0.032(2) 0.049(2) 0.0002(18) 0.023(2) 0.0014(18) C21 0.032(3) 0.031(3) 0.037(3) 0.001(2) 0.011(2) 0.006(2) C22 0.041(4) 0.032(3) 0.049(4) 0.000(3) 0.016(3) 0.005(3) C23 0.061(5) 0.049(4) 0.080(5) -0.006(4) 0.034(4) -0.009(4) C24 0.091(7) 0.035(4) 0.124(8) -0.019(5) 0.060(6) -0.016(4) C25 0.078(6) 0.049(5) 0.113(8) -0.039(5) 0.029(6) -0.010(4) C26 0.094(7) 0.083(7) 0.104(7) -0.049(6) 0.057(6) -0.024(6) C27 0.073(6) 0.057(5) 0.091(6) -0.022(4) 0.051(5) -0.019(4) N31 0.146(8) 0.061(5) 0.067(5) 0.000(4) 0.068(5) -0.005(5) C31 0.070(5) 0.063(5) 0.043(4) 0.000(3) 0.031(4) -0.004(4) C32 0.073(6) 0.101(7) 0.094(7) 0.010(6) 0.050(6) 0.023(5) N32 0.105(9) 0.060(7) 0.092(8) 0.000 0.027(7) 0.000 C33 0.071(8) 0.068(8) 0.087(9) 0.000 0.035(7) 0.000 C34 0.17(2) 0.069(11) 0.19(2) 0.000 0.005(17) 0.000 _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 Ho1 O2 2.297(4) . ? Ho1 O3 2.341(4) . ? Ho1 O9 2.383(4) . ? Ho1 O1 2.383(4) . ? Ho1 O6 2.415(4) . ? Ho1 O8 2.427(4) 7_556 ? Ho1 O4 2.443(4) . ? Ho1 O10 2.569(4) . ? Ho1 N1 2.637(4) . ? Fe1 O2 1.956(4) . ? Fe1 O3 1.966(4) 7_556 ? Fe1 O7 1.995(4) . ? Fe1 O5 1.996(4) . ? Fe1 O1 2.056(4) . ? Fe1 O1 2.068(4) 7_556 ? O1 Fe1 2.068(4) 7_556 ? O1 H1 0.91(3) . ? N1 C1 1.470(8) . ? N1 C5 1.473(7) . ? N1 C3 1.479(8) . ? C1 C2 1.524(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.410(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.515(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.413(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.966(4) 7_556 ? C5 C6 1.500(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.429(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.90(3) . ? O5 C7 1.275(6) . ? O6 C7 1.245(7) . ? C7 C8 1.504(7) . ? C8 C9 1.374(8) . ? C8 C13 1.382(8) . ? C9 C10 1.394(9) . ? C9 H9A 0.9500 . ? C10 C11 1.388(11) . ? C10 H10A 0.9500 . ? C11 C12 1.350(10) . ? C11 H11A 0.9500 . ? C12 C13 1.398(8) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O7 C14 1.282(7) . ? O8 C14 1.248(7) . ? O8 Ho1 2.427(4) 7_556 ? C14 C15 1.500(8) . ? C15 C16 1.362(9) . ? C15 C20 1.386(9) . ? C16 C17 1.372(9) . ? C16 H16A 0.9500 . ? C17 C18 1.371(12) . ? C17 H17A 0.9500 . ? C18 C19 1.385(13) . ? C18 H18A 0.9500 . ? C19 C20 1.371(10) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? O9 C21 1.260(6) . ? O10 C21 1.264(7) . ? C21 C22 1.491(8) . ? C22 C27 1.373(9) . ? C22 C23 1.388(9) . ? C23 C24 1.387(10) . ? C23 H23A 0.9500 . ? C24 C25 1.312(12) . ? C24 H24A 0.9500 . ? C25 C26 1.379(13) . ? C25 H25A 0.9500 . ? C26 C27 1.383(11) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N31 C31 1.116(10) . ? C31 C32 1.437(11) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32 C33 1.093(15) . ? C33 C34 1.47(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 O2 Ho1 O3 81.97(13) . . ? O2 Ho1 O9 142.11(13) . . ? O3 Ho1 O9 85.76(13) . . ? O2 Ho1 O1 68.53(12) . . ? O3 Ho1 O1 68.77(12) . . ? O9 Ho1 O1 138.00(14) . . ? O2 Ho1 O6 77.06(13) . . ? O3 Ho1 O6 140.20(12) . . ? O9 Ho1 O6 130.27(13) . . ? O1 Ho1 O6 72.15(12) . . ? O2 Ho1 O8 137.39(13) . 7_556 ? O3 Ho1 O8 73.93(12) . 7_556 ? O9 Ho1 O8 70.99(14) . 7_556 ? O1 Ho1 O8 70.14(13) . 7_556 ? O6 Ho1 O8 99.78(13) . 7_556 ? O2 Ho1 O4 83.62(14) . . ? O3 Ho1 O4 132.29(12) . . ? O9 Ho1 O4 78.55(15) . . ? O1 Ho1 O4 143.11(14) . . ? O6 Ho1 O4 78.54(13) . . ? O8 Ho1 O4 138.12(13) 7_556 . ? O2 Ho1 O10 146.81(13) . . ? O3 Ho1 O10 130.72(13) . . ? O9 Ho1 O10 52.44(12) . . ? O1 Ho1 O10 123.41(12) . . ? O6 Ho1 O10 78.29(13) . . ? O8 Ho1 O10 68.83(13) 7_556 . ? O4 Ho1 O10 69.92(13) . . ? O2 Ho1 N1 66.82(14) . . ? O3 Ho1 N1 68.17(14) . . ? O9 Ho1 N1 75.32(15) . . ? O1 Ho1 N1 120.69(13) . . ? O6 Ho1 N1 129.84(15) . . ? O8 Ho1 N1 130.37(15) 7_556 . ? O4 Ho1 N1 64.32(14) . . ? O10 Ho1 N1 115.41(14) . . ? O2 Fe1 O3 174.53(16) . 7_556 ? O2 Fe1 O7 92.42(16) . . ? O3 Fe1 O7 91.25(16) 7_556 . ? O2 Fe1 O5 90.29(16) . . ? O3 Fe1 O5 92.87(16) 7_556 . ? O7 Fe1 O5 102.57(16) . . ? O2 Fe1 O1 82.10(15) . . ? O3 Fe1 O1 93.48(15) 7_556 . ? O7 Fe1 O1 167.18(15) . . ? O5 Fe1 O1 89.10(15) . . ? O2 Fe1 O1 93.07(15) . 7_556 ? O3 Fe1 O1 82.76(15) 7_556 7_556 ? O7 Fe1 O1 91.85(15) . 7_556 ? O5 Fe1 O1 165.05(15) . 7_556 ? O1 Fe1 O1 76.95(14) . 7_556 ? Fe1 O1 Fe1 103.05(14) . 7_556 ? Fe1 O1 Ho1 100.82(15) . . ? Fe1 O1 Ho1 101.25(14) 7_556 . ? Fe1 O1 H1 118(4) . . ? Fe1 O1 H1 109(4) 7_556 . ? Ho1 O1 H1 122(4) . . ? C1 N1 C5 112.8(5) . . ? C1 N1 C3 112.0(5) . . ? C5 N1 C3 109.5(5) . . ? C1 N1 Ho1 111.0(3) . . ? C5 N1 Ho1 107.2(3) . . ? C3 N1 Ho1 103.9(3) . . ? N1 C1 C2 112.7(4) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C1 108.3(5) . . ? O2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C2 O2 Fe1 132.1(4) . . ? C2 O2 Ho1 120.8(3) . . ? Fe1 O2 Ho1 107.10(16) . . ? N1 C3 C4 111.1(5) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 109.7(4) . . ? O3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 O3 Fe1 122.3(3) . 7_556 ? C4 O3 Ho1 122.7(3) . . ? Fe1 O3 Ho1 106.00(14) 7_556 . ? N1 C5 C6 111.1(5) . . ? N1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O4 C6 C5 108.5(5) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C6 O4 Ho1 124.9(3) . . ? C6 O4 H4 110(4) . . ? Ho1 O4 H4 122(4) . . ? C7 O5 Fe1 129.1(4) . . ? C7 O6 Ho1 134.8(3) . . ? O6 C7 O5 125.9(5) . . ? O6 C7 C8 119.0(5) . . ? O5 C7 C8 115.0(5) . . ? C9 C8 C13 118.7(5) . . ? C9 C8 C7 120.6(5) . . ? C13 C8 C7 120.6(5) . . ? C8 C9 C10 120.5(6) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 119.4(7) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C12 C11 C10 121.0(6) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 119.1(6) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C8 C13 C12 121.3(6) . . ? C8 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C14 O7 Fe1 125.3(4) . . ? C14 O8 Ho1 139.1(3) . 7_556 ? O8 C14 O7 125.2(5) . . ? O8 C14 C15 118.4(5) . . ? O7 C14 C15 116.4(5) . . ? C16 C15 C20 118.9(6) . . ? C16 C15 C14 121.6(6) . . ? C20 C15 C14 119.5(6) . . ? C15 C16 C17 121.6(7) . . ? C15 C16 H16A 119.2 . . ? C17 C16 H16A 119.2 . . ? C18 C17 C16 119.2(8) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 120.5(7) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C20 C19 C18 119.3(8) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C19 C20 C15 120.5(8) . . ? C19 C20 H20A 119.7 . . ? C15 C20 H20A 119.7 . . ? C21 O9 Ho1 97.3(3) . . ? C21 O10 Ho1 88.5(3) . . ? O9 C21 O10 120.8(5) . . ? O9 C21 C22 117.6(5) . . ? O10 C21 C22 121.5(5) . . ? C27 C22 C23 118.1(6) . . ? C27 C22 C21 122.3(6) . . ? C23 C22 C21 119.6(6) . . ? C24 C23 C22 119.8(7) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C25 C24 C23 121.2(8) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C24 C25 C26 121.0(8) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C27 118.8(8) . . ? C25 C26 H26A 120.6 . . ? C27 C26 H26A 120.6 . . ? C22 C27 C26 121.1(8) . . ? C22 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? N31 C31 C32 176.1(8) . . ? 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 . . ? N32 C33 C34 180.0 . . ? 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 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N31 0.91(3) 2.11(4) 2.993(7) 163(5) . O4 H4 O10 0.90(3) 1.84(4) 2.708(5) 161(6) 5_566 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.709 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.127 data_amer16er _database_code_depnum_ccdc_archive 'CCDC 918955' #TrackingRef 'fe2ln2_monster_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C54 H58 Er2 Fe2 N2 O20), 3(C2 H3 N)' _chemical_formula_sum 'C60 H67 Er2 Fe2 N5 O20' _chemical_formula_weight 1624.41 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.6735(7) _cell_length_b 15.9092(6) _cell_length_c 21.8407(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.428(1) _cell_angle_gamma 90.00 _cell_volume 6080.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9453 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.01 _exptl_crystal_description block _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3240 _exptl_absorpt_coefficient_mu 3.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_T_max 0.485 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22580 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_unetI/netI 0.0326 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.10 _reflns_number_total 6896 _reflns_number_gt 6098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. O-H distances were restrained: DFIX 0.92 0.04 O1 H1 O4 H4 ; _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^)+(0.0385P)^2^+5.3585P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6896 _refine_ls_number_parameters 411 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Er1 Er 0.155592(8) 0.405650(9) 0.495554(7) 0.01726(6) Uani 1 1 d . . . Fe1 Fe 0.17280(3) 0.19852(3) 0.46198(2) 0.01738(10) Uani 1 1 d . . . O1 O 0.21915(12) 0.27876(14) 0.53954(11) 0.0176(4) Uani 1 1 d D . . H1 H 0.221(2) 0.261(2) 0.5782(15) 0.021 Uiso 1 1 d D . . N1 N 0.15541(16) 0.46319(18) 0.38353(14) 0.0229(6) Uani 1 1 d . . . C1 C 0.1358(2) 0.3957(2) 0.33293(17) 0.0255(7) Uani 1 1 d . . . H1A H 0.1833 0.3746 0.3279 0.031 Uiso 1 1 calc R . . H1B H 0.1033 0.4197 0.2905 0.031 Uiso 1 1 calc R . . C2 C 0.09382(19) 0.3225(2) 0.35063(16) 0.0237(7) Uani 1 1 d . . . H2A H 0.0400 0.3381 0.3428 0.028 Uiso 1 1 calc R . . H2B H 0.0942 0.2729 0.3234 0.028 Uiso 1 1 calc R . . O2 O 0.13177(13) 0.30361(14) 0.41746(11) 0.0202(5) Uani 1 1 d . . . C3 C 0.23396(19) 0.4943(2) 0.39756(17) 0.0248(7) Uani 1 1 d . . . H3A H 0.2419 0.5456 0.4248 0.030 Uiso 1 1 calc R . . H3B H 0.2410 0.5095 0.3561 0.030 Uiso 1 1 calc R . . C4 C 0.29239(19) 0.4288(2) 0.43281(16) 0.0220(7) Uani 1 1 d . . . H4A H 0.2899 0.3808 0.4034 0.026 Uiso 1 1 calc R . . H4B H 0.3444 0.4532 0.4462 0.026 Uiso 1 1 calc R . . O3 O 0.27707(13) 0.40106(13) 0.48847(11) 0.0200(5) Uani 1 1 d . . . C5 C 0.1007(2) 0.5337(2) 0.36415(18) 0.0275(8) Uani 1 1 d . . . H5A H 0.0955 0.5528 0.3197 0.033 Uiso 1 1 calc R . . H5B H 0.1202 0.5814 0.3945 0.033 Uiso 1 1 calc R . . C6 C 0.0237(2) 0.5073(2) 0.36517(18) 0.0285(8) Uani 1 1 d . . . H6A H -0.0084 0.5574 0.3633 0.034 Uiso 1 1 calc R . . H6B H -0.0026 0.4715 0.3268 0.034 Uiso 1 1 calc R . . O4 O 0.03455(13) 0.46155(15) 0.42396(12) 0.0240(5) Uani 1 1 d D . . H4 H -0.0027(19) 0.472(2) 0.4367(19) 0.029 Uiso 1 1 d D . . O5 O 0.08145(13) 0.18498(14) 0.48831(12) 0.0226(5) Uani 1 1 d . . . O6 O 0.06556(12) 0.31651(14) 0.52039(11) 0.0209(5) Uani 1 1 d . . . C7 C 0.04868(18) 0.2402(2) 0.51234(16) 0.0204(7) Uani 1 1 d . . . C8 C -0.01335(18) 0.2060(2) 0.53454(16) 0.0217(7) Uani 1 1 d . . . C9 C -0.0474(2) 0.2567(2) 0.5677(2) 0.0324(9) Uani 1 1 d . . . H9A H -0.0326 0.3139 0.5757 0.039 Uiso 1 1 calc R . . C10 C -0.1036(3) 0.2242(3) 0.5896(2) 0.0425(11) Uani 1 1 d . . . H10A H -0.1269 0.2593 0.6125 0.051 Uiso 1 1 calc R . . C11 C -0.1255(2) 0.1412(3) 0.5779(2) 0.0378(10) Uani 1 1 d . . . H11A H -0.1640 0.1194 0.5926 0.045 Uiso 1 1 calc R . . C12 C -0.0921(2) 0.0903(2) 0.54539(19) 0.0304(8) Uani 1 1 d . . . H12A H -0.1072 0.0331 0.5377 0.036 Uiso 1 1 calc R . . C13 C -0.03582(19) 0.1222(2) 0.52342(17) 0.0247(7) Uani 1 1 d . . . H13A H -0.0127 0.0866 0.5007 0.030 Uiso 1 1 calc R . . O7 O 0.14304(13) 0.13472(15) 0.37808(11) 0.0224(5) Uani 1 1 d . . . O8 O 0.25557(13) 0.06952(15) 0.39543(11) 0.0219(5) Uani 1 1 d . . . C14 C 0.18783(19) 0.0855(2) 0.36178(16) 0.0211(7) Uani 1 1 d . . . C15 C 0.1546(2) 0.0452(2) 0.29547(17) 0.0254(7) Uani 1 1 d . . . C16 C 0.0896(2) 0.0769(3) 0.24923(18) 0.0316(8) Uani 1 1 d . . . H16A H 0.0648 0.1241 0.2596 0.038 Uiso 1 1 calc R . . C17 C 0.0599(2) 0.0411(3) 0.1877(2) 0.0414(10) Uani 1 1 d . . . H17A H 0.0147 0.0630 0.1562 0.050 Uiso 1 1 calc R . . C18 C 0.0967(2) -0.0270(3) 0.1727(2) 0.0473(12) Uani 1 1 d . . . H18A H 0.0771 -0.0517 0.1305 0.057 Uiso 1 1 calc R . . C19 C 0.1622(2) -0.0593(3) 0.2190(2) 0.0443(11) Uani 1 1 d . . . H19A H 0.1870 -0.1064 0.2087 0.053 Uiso 1 1 calc R . . C20 C 0.1912(2) -0.0229(2) 0.28011(19) 0.0322(9) Uani 1 1 d . . . H20A H 0.2364 -0.0447 0.3117 0.039 Uiso 1 1 calc R . . O9 O 0.17627(14) 0.55204(15) 0.51099(12) 0.0243(5) Uani 1 1 d . . . O10 O 0.09917(12) 0.50420(14) 0.55934(12) 0.0224(5) Uani 1 1 d . . . C21 C 0.14071(19) 0.5624(2) 0.54998(17) 0.0233(7) Uani 1 1 d . . . C22 C 0.1506(2) 0.6435(2) 0.58572(18) 0.0262(7) Uani 1 1 d . . . C23 C 0.1914(2) 0.7084(2) 0.5704(2) 0.0349(9) Uani 1 1 d . . . H23A H 0.2123 0.7007 0.5369 0.042 Uiso 1 1 calc R . . C24 C 0.2019(3) 0.7839(3) 0.6034(2) 0.0463(11) Uani 1 1 d . . . H24A H 0.2304 0.8275 0.5928 0.056 Uiso 1 1 calc R . . C25 C 0.1719(3) 0.7964(3) 0.6506(2) 0.0483(12) Uani 1 1 d . . . H25A H 0.1783 0.8492 0.6723 0.058 Uiso 1 1 calc R . . C26 C 0.1320(3) 0.7330(3) 0.6677(2) 0.0495(12) Uani 1 1 d . . . H26A H 0.1117 0.7418 0.7015 0.059 Uiso 1 1 calc R . . C27 C 0.1217(2) 0.6568(3) 0.6356(2) 0.0399(10) Uani 1 1 d . . . H27A H 0.0947 0.6131 0.6477 0.048 Uiso 1 1 calc R . . N31 N 0.2159(2) 0.2514(2) 0.67360(18) 0.0444(9) Uani 1 1 d . . . C31 C 0.1900(2) 0.3083(3) 0.68867(19) 0.0349(9) Uani 1 1 d . . . C32 C 0.1582(3) 0.3836(3) 0.7069(2) 0.0437(10) Uani 1 1 d . . . H32A H 0.1392 0.4211 0.6690 0.065 Uiso 1 1 calc R . . H32B H 0.1980 0.4125 0.7423 0.065 Uiso 1 1 calc R . . H32C H 0.1161 0.3681 0.7215 0.065 Uiso 1 1 calc R . . N32 N 0.0000 0.3179(4) 0.7500 0.0525(14) Uani 1 2 d S . . C33 C 0.0000 0.2472(4) 0.7500 0.0421(14) Uani 1 2 d S . . C34 C 0.0000 0.1561(5) 0.7500 0.088(3) Uani 1 2 d S . . H34A H 0.0327 0.1355 0.7265 0.133 Uiso 0.50 1 calc PR . . H34B H -0.0523 0.1355 0.7283 0.133 Uiso 0.50 1 calc PR . . H34C H 0.0196 0.1355 0.7951 0.133 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01828(8) 0.01795(8) 0.01834(8) 0.00065(6) 0.00992(6) 0.00103(6) Fe1 0.0165(2) 0.0195(2) 0.0179(2) -0.00249(18) 0.00819(18) -0.00070(17) O1 0.0176(11) 0.0212(11) 0.0161(11) -0.0001(9) 0.0088(9) -0.0011(9) N1 0.0248(15) 0.0243(15) 0.0235(15) 0.0063(12) 0.0132(12) 0.0031(12) C1 0.0265(18) 0.034(2) 0.0161(16) 0.0043(14) 0.0081(14) 0.0062(15) C2 0.0221(17) 0.0302(18) 0.0187(17) 0.0017(14) 0.0069(13) 0.0044(14) O2 0.0219(11) 0.0232(12) 0.0164(11) 0.0012(9) 0.0077(9) 0.0026(9) C3 0.0294(18) 0.0273(18) 0.0239(18) 0.0053(14) 0.0171(15) -0.0001(14) C4 0.0213(16) 0.0288(18) 0.0213(17) 0.0011(14) 0.0141(14) -0.0020(14) O3 0.0215(11) 0.0213(12) 0.0210(12) 0.0017(9) 0.0122(9) -0.0001(9) C5 0.0322(19) 0.0260(18) 0.030(2) 0.0092(15) 0.0177(16) 0.0082(15) C6 0.0275(18) 0.033(2) 0.0268(19) 0.0099(15) 0.0114(15) 0.0115(15) O4 0.0204(12) 0.0314(13) 0.0236(13) 0.0068(10) 0.0120(10) 0.0071(10) O5 0.0218(12) 0.0205(11) 0.0307(13) -0.0047(10) 0.0159(10) -0.0013(9) O6 0.0204(11) 0.0214(12) 0.0251(12) 0.0016(10) 0.0132(10) -0.0011(9) C7 0.0177(16) 0.0262(17) 0.0186(16) -0.0001(13) 0.0081(13) -0.0030(13) C8 0.0166(15) 0.0266(18) 0.0221(17) 0.0017(14) 0.0069(13) -0.0016(13) C9 0.035(2) 0.0276(19) 0.042(2) -0.0021(17) 0.0229(18) -0.0038(16) C10 0.046(2) 0.042(2) 0.057(3) -0.007(2) 0.039(2) -0.006(2) C11 0.031(2) 0.045(2) 0.047(2) 0.005(2) 0.0251(19) -0.0069(18) C12 0.0275(19) 0.0275(19) 0.036(2) 0.0024(16) 0.0102(16) -0.0083(15) C13 0.0201(17) 0.0252(17) 0.0290(19) 0.0023(14) 0.0086(14) -0.0013(13) O7 0.0199(11) 0.0260(12) 0.0227(12) -0.0059(10) 0.0092(10) 0.0006(9) O8 0.0213(12) 0.0245(12) 0.0211(12) -0.0046(10) 0.0091(10) -0.0002(10) C14 0.0231(17) 0.0225(17) 0.0210(17) -0.0007(13) 0.0117(14) -0.0018(13) C15 0.0241(17) 0.0311(19) 0.0244(18) -0.0071(15) 0.0128(15) -0.0056(14) C16 0.0270(19) 0.043(2) 0.026(2) -0.0058(16) 0.0109(15) -0.0005(16) C17 0.030(2) 0.067(3) 0.026(2) -0.009(2) 0.0085(17) -0.004(2) C18 0.039(2) 0.078(3) 0.029(2) -0.027(2) 0.0170(19) -0.012(2) C19 0.039(2) 0.059(3) 0.042(2) -0.025(2) 0.023(2) -0.005(2) C20 0.029(2) 0.039(2) 0.031(2) -0.0102(17) 0.0139(16) -0.0003(16) O9 0.0286(13) 0.0216(12) 0.0289(13) 0.0003(10) 0.0178(11) -0.0018(10) O10 0.0202(12) 0.0212(12) 0.0289(13) 0.0015(10) 0.0123(10) 0.0007(9) C21 0.0236(17) 0.0236(17) 0.0227(17) 0.0024(14) 0.0078(14) 0.0051(14) C22 0.0239(18) 0.0234(18) 0.0306(19) -0.0010(15) 0.0084(15) 0.0040(14) C23 0.040(2) 0.028(2) 0.040(2) -0.0004(17) 0.0170(18) -0.0049(17) C24 0.051(3) 0.029(2) 0.063(3) -0.008(2) 0.025(2) -0.0113(19) C25 0.046(3) 0.034(2) 0.061(3) -0.020(2) 0.013(2) -0.0071(19) C26 0.054(3) 0.046(3) 0.060(3) -0.026(2) 0.034(2) -0.011(2) C27 0.042(2) 0.037(2) 0.050(3) -0.0107(19) 0.027(2) -0.0084(18) N31 0.070(3) 0.039(2) 0.034(2) -0.0029(16) 0.0318(19) 0.0002(19) C31 0.041(2) 0.044(2) 0.0240(19) 0.0007(17) 0.0169(17) -0.0026(19) C32 0.040(2) 0.052(3) 0.047(3) 0.004(2) 0.025(2) 0.008(2) N32 0.066(4) 0.039(3) 0.047(3) 0.000 0.013(3) 0.000 C33 0.041(3) 0.042(4) 0.049(4) 0.000 0.022(3) 0.000 C34 0.087(7) 0.042(4) 0.115(8) 0.000 0.008(6) 0.000 _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 Er1 O2 2.283(2) . ? Er1 O3 2.328(2) . ? Er1 O9 2.366(2) . ? Er1 O1 2.369(2) . ? Er1 O6 2.402(2) . ? Er1 O8 2.413(2) 7_556 ? Er1 O4 2.424(2) . ? Er1 O10 2.556(2) . ? Er1 N1 2.611(3) . ? Er1 C21 2.817(3) . ? Er1 Fe1 3.4153(5) . ? Er1 Fe1 3.4353(5) 7_556 ? Fe1 O2 1.951(2) . ? Fe1 O3 1.962(2) 7_556 ? Fe1 O5 1.993(2) . ? Fe1 O7 1.997(2) . ? Fe1 O1 2.055(2) . ? Fe1 O1 2.062(2) 7_556 ? Fe1 Er1 3.4353(5) 7_556 ? O1 Fe1 2.061(2) 7_556 ? O1 H1 0.88(3) . ? N1 C3 1.475(4) . ? N1 C5 1.477(4) . ? N1 C1 1.491(4) . ? C1 C2 1.527(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.415(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.510(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.413(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.962(2) 7_556 ? C5 C6 1.505(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.427(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.85(3) . ? O5 C7 1.283(4) . ? O6 C7 1.251(4) . ? C7 C8 1.505(4) . ? C8 C9 1.380(5) . ? C8 C13 1.393(5) . ? C9 C10 1.395(5) . ? C9 H9A 0.9500 . ? C10 C11 1.380(6) . ? C10 H10A 0.9500 . ? C11 C12 1.364(5) . ? C11 H11A 0.9500 . ? C12 C13 1.395(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O7 C14 1.283(4) . ? O8 C14 1.247(4) . ? O8 Er1 2.413(2) 7_556 ? C14 C15 1.505(5) . ? C15 C16 1.374(5) . ? C15 C20 1.384(5) . ? C16 C17 1.385(5) . ? C16 H16A 0.9500 . ? C17 C18 1.383(6) . ? C17 H17A 0.9500 . ? C18 C19 1.384(7) . ? C18 H18A 0.9500 . ? C19 C20 1.381(5) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? O9 C21 1.260(4) . ? O10 C21 1.269(4) . ? C21 C22 1.487(5) . ? C22 C23 1.392(5) . ? C22 C27 1.391(5) . ? C23 C24 1.379(6) . ? C23 H23A 0.9500 . ? C24 C25 1.348(6) . ? C24 H24A 0.9500 . ? C25 C26 1.380(6) . ? C25 H25A 0.9500 . ? C26 C27 1.380(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N31 C31 1.128(5) . ? C31 C32 1.453(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32 C33 1.126(8) . ? C33 C34 1.449(10) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 O2 Er1 O3 82.43(8) . . ? O2 Er1 O9 141.82(8) . . ? O3 Er1 O9 85.76(8) . . ? O2 Er1 O1 68.68(8) . . ? O3 Er1 O1 68.80(7) . . ? O9 Er1 O1 138.38(8) . . ? O2 Er1 O6 77.27(8) . . ? O3 Er1 O6 140.50(7) . . ? O9 Er1 O6 129.90(8) . . ? O1 Er1 O6 72.32(7) . . ? O2 Er1 O8 137.84(8) . 7_556 ? O3 Er1 O8 73.76(8) . 7_556 ? O9 Er1 O8 71.12(8) . 7_556 ? O1 Er1 O8 70.41(8) . 7_556 ? O6 Er1 O8 99.68(8) . 7_556 ? O2 Er1 O4 83.36(8) . . ? O3 Er1 O4 132.79(8) . . ? O9 Er1 O4 78.45(9) . . ? O1 Er1 O4 142.80(8) . . ? O6 Er1 O4 78.10(8) . . ? O8 Er1 O4 137.87(8) 7_556 . ? O2 Er1 O10 146.45(8) . . ? O3 Er1 O10 130.70(7) . . ? O9 Er1 O10 52.86(7) . . ? O1 Er1 O10 123.04(7) . . ? O6 Er1 O10 77.58(7) . . ? O8 Er1 O10 68.53(7) 7_556 . ? O4 Er1 O10 69.98(8) . . ? O2 Er1 N1 67.24(8) . . ? O3 Er1 N1 68.37(8) . . ? O9 Er1 N1 74.64(9) . . ? O1 Er1 N1 121.02(8) . . ? O6 Er1 N1 130.28(9) . . ? O8 Er1 N1 130.01(8) 7_556 . ? O4 Er1 N1 64.60(8) . . ? O10 Er1 N1 115.45(8) . . ? O2 Fe1 O3 174.48(10) . 7_556 ? O2 Fe1 O5 90.55(10) . . ? O3 Fe1 O5 92.59(10) 7_556 . ? O2 Fe1 O7 92.48(10) . . ? O3 Fe1 O7 91.27(10) 7_556 . ? O5 Fe1 O7 102.58(9) . . ? O2 Fe1 O1 81.82(9) . . ? O3 Fe1 O1 93.68(9) 7_556 . ? O5 Fe1 O1 89.19(9) . . ? O7 Fe1 O1 167.01(9) . . ? O2 Fe1 O1 93.33(9) . 7_556 ? O3 Fe1 O1 82.49(9) 7_556 7_556 ? O5 Fe1 O1 164.75(9) . 7_556 ? O7 Fe1 O1 91.99(9) . 7_556 ? O1 Fe1 O1 76.79(9) . 7_556 ? Fe1 O1 Fe1 103.21(9) . 7_556 ? Fe1 O1 Er1 100.82(9) . . ? Fe1 O1 Er1 101.46(9) 7_556 . ? Fe1 O1 H1 117(2) . . ? Fe1 O1 H1 111(2) 7_556 . ? Er1 O1 H1 121(2) . . ? C3 N1 C5 110.1(3) . . ? C3 N1 C1 111.4(3) . . ? C5 N1 C1 111.6(3) . . ? C3 N1 Er1 104.29(19) . . ? C5 N1 Er1 108.0(2) . . ? C1 N1 Er1 111.21(19) . . ? N1 C1 C2 112.1(3) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O2 C2 C1 107.9(3) . . ? O2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C2 O2 Fe1 131.6(2) . . ? C2 O2 Er1 121.11(19) . . ? Fe1 O2 Er1 107.26(10) . . ? N1 C3 C4 111.3(3) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 109.1(3) . . ? O3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? O3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C4 O3 Fe1 121.74(19) . 7_556 ? C4 O3 Er1 122.80(19) . . ? Fe1 O3 Er1 106.08(9) 7_556 . ? N1 C5 C6 110.6(3) . . ? N1 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? O4 C6 C5 108.6(3) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? C6 O4 Er1 125.09(19) . . ? C6 O4 H4 108(3) . . ? Er1 O4 H4 123(3) . . ? C7 O5 Fe1 128.5(2) . . ? C7 O6 Er1 134.7(2) . . ? O6 C7 O5 126.1(3) . . ? O6 C7 C8 119.4(3) . . ? O5 C7 C8 114.5(3) . . ? C9 C8 C13 119.0(3) . . ? C9 C8 C7 120.4(3) . . ? C13 C8 C7 120.6(3) . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C8 C13 C12 120.4(3) . . ? C8 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C14 O7 Fe1 124.4(2) . . ? C14 O8 Er1 139.0(2) . 7_556 ? O8 C14 O7 125.9(3) . . ? O8 C14 C15 118.2(3) . . ? O7 C14 C15 115.9(3) . . ? C16 C15 C20 119.5(3) . . ? C16 C15 C14 120.8(3) . . ? C20 C15 C14 119.6(3) . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C18 C17 C16 119.2(4) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C20 C19 C18 119.9(4) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C15 120.1(4) . . ? C19 C20 H20A 119.9 . . ? C15 C20 H20A 119.9 . . ? C21 O9 Er1 97.3(2) . . ? C21 O10 Er1 88.17(19) . . ? O9 C21 O10 120.6(3) . . ? O9 C21 C22 118.0(3) . . ? O10 C21 C22 121.3(3) . . ? C23 C22 C27 118.1(3) . . ? C23 C22 C21 119.8(3) . . ? C27 C22 C21 122.2(3) . . ? C24 C23 C22 120.7(4) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C27 C26 C25 119.8(4) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C22 120.5(4) . . ? C26 C27 H27A 119.7 . . ? C22 C27 H27A 119.7 . . ? N31 C31 C32 177.8(4) . . ? 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 . . ? N32 C33 C34 180.0 . . ? 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 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N31 0.88(3) 2.13(3) 2.982(4) 165(3) . O4 H4 O10 0.85(3) 1.87(3) 2.702(3) 165(4) 5_566 _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.747 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.115 data_am16y _database_code_depnum_ccdc_archive 'CCDC 918956' #TrackingRef 'fe2ln2_monster_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C54 H58 Fe2 N2 O20 Y2), 3(C2 H3 N)' _chemical_formula_sum 'C60 H67 Fe2 N5 O20 Y2' _chemical_formula_weight 1467.71 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.7266(16) _cell_length_b 15.8981(11) _cell_length_c 22.0196(18) _cell_angle_alpha 90.00 _cell_angle_beta 110.230(6) _cell_angle_gamma 90.00 _cell_volume 6151.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8223 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 27.02 _exptl_crystal_description block _exptl_crystal_colour yellow-brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 2.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7138 _exptl_absorpt_correction_T_max 0.8306 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18535 _diffrn_reflns_av_R_equivalents 0.0924 _diffrn_reflns_av_unetI/netI 0.1027 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5632 _reflns_number_gt 3515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. O-H distances were restrained: DFIX 0.92 0.04 O1 H1 O4 H4 ; _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^)+(0.0142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5632 _refine_ls_number_parameters 410 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 Y1 Y 0.15482(2) 0.40542(3) 0.49528(2) 0.03645(11) Uani 1 1 d . . . Fe1 Fe 0.17356(3) 0.19769(4) 0.46284(3) 0.03714(17) Uani 1 1 d . . . O1 O 0.21932(16) 0.27875(18) 0.53910(14) 0.0351(7) Uani 1 1 d D . . H1 H 0.212(2) 0.267(3) 0.5732(17) 0.042 Uiso 1 1 d D . . N1 N 0.15422(19) 0.4623(2) 0.38317(17) 0.0415(9) Uani 1 1 d . . . C1 C 0.1355(2) 0.3946(3) 0.3338(2) 0.0504(12) Uani 1 1 d . . . H1A H 0.1830 0.3740 0.3287 0.060 Uiso 1 1 calc R . . H1B H 0.1026 0.4177 0.2917 0.060 Uiso 1 1 calc R . . C2 C 0.0951(3) 0.3216(3) 0.3523(2) 0.0480(12) Uani 1 1 d . . . H2A H 0.0414 0.3368 0.3445 0.058 Uiso 1 1 calc R . . H2B H 0.0956 0.2720 0.3252 0.058 Uiso 1 1 calc R . . O2 O 0.13183(15) 0.30186(19) 0.41798(14) 0.0414(7) Uani 1 1 d . . . C3 C 0.2320(2) 0.4940(3) 0.3967(2) 0.0469(12) Uani 1 1 d . . . H3A H 0.2394 0.5458 0.4232 0.056 Uiso 1 1 calc R . . H3B H 0.2391 0.5087 0.3554 0.056 Uiso 1 1 calc R . . C4 C 0.2905(2) 0.4296(3) 0.4321(2) 0.0451(12) Uani 1 1 d . . . H4A H 0.2886 0.3813 0.4032 0.054 Uiso 1 1 calc R . . H4B H 0.3420 0.4546 0.4451 0.054 Uiso 1 1 calc R . . O3 O 0.27582(14) 0.40161(19) 0.48764(13) 0.0392(7) Uani 1 1 d . . . C5 C 0.0996(3) 0.5320(3) 0.3637(2) 0.0522(13) Uani 1 1 d . . . H5A H 0.0950 0.5511 0.3197 0.063 Uiso 1 1 calc R . . H5B H 0.1184 0.5798 0.3939 0.063 Uiso 1 1 calc R . . C6 C 0.0228(3) 0.5051(3) 0.3642(2) 0.0554(13) Uani 1 1 d . . . H6A H -0.0101 0.5548 0.3608 0.066 Uiso 1 1 calc R . . H6B H -0.0021 0.4675 0.3270 0.066 Uiso 1 1 calc R . . O4 O 0.03421(17) 0.4616(2) 0.42376(16) 0.0493(9) Uani 1 1 d D . . H4 H -0.005(2) 0.462(3) 0.434(2) 0.059 Uiso 1 1 d D . . O5 O 0.08290(15) 0.18370(18) 0.48960(15) 0.0438(8) Uani 1 1 d . . . O6 O 0.06568(15) 0.31514(19) 0.52022(15) 0.0420(7) Uani 1 1 d . . . C7 C 0.0496(2) 0.2385(3) 0.5131(2) 0.0406(11) Uani 1 1 d . . . C8 C -0.0119(2) 0.2040(3) 0.5351(2) 0.0383(11) Uani 1 1 d . . . C9 C -0.0477(3) 0.2554(3) 0.5662(3) 0.0569(14) Uani 1 1 d . . . H9A H -0.0342 0.3131 0.5730 0.068 Uiso 1 1 calc R . . C10 C -0.1037(3) 0.2227(4) 0.5876(3) 0.0739(18) Uani 1 1 d . . . H10A H -0.1274 0.2576 0.6101 0.089 Uiso 1 1 calc R . . C11 C -0.1246(3) 0.1396(4) 0.5762(3) 0.0639(15) Uani 1 1 d . . . H11A H -0.1644 0.1180 0.5893 0.077 Uiso 1 1 calc R . . C12 C -0.0889(2) 0.0880(4) 0.5463(2) 0.0549(13) Uani 1 1 d . . . H12A H -0.1022 0.0301 0.5400 0.066 Uiso 1 1 calc R . . C13 C -0.0329(2) 0.1207(3) 0.5251(2) 0.0463(12) Uani 1 1 d . . . H13A H -0.0087 0.0852 0.5034 0.056 Uiso 1 1 calc R . . O7 O 0.14435(15) 0.13344(18) 0.38015(14) 0.0427(8) Uani 1 1 d . . . O8 O 0.25611(16) 0.06916(18) 0.39649(14) 0.0435(8) Uani 1 1 d . . . C14 C 0.1887(2) 0.0848(3) 0.3634(2) 0.0417(11) Uani 1 1 d . . . C15 C 0.1566(3) 0.0446(3) 0.2975(2) 0.0462(12) Uani 1 1 d . . . C16 C 0.0915(3) 0.0746(3) 0.2523(2) 0.0520(13) Uani 1 1 d . . . H16A H 0.0656 0.1204 0.2629 0.062 Uiso 1 1 calc R . . C17 C 0.0627(3) 0.0392(4) 0.1912(3) 0.0718(17) Uani 1 1 d . . . H17A H 0.0178 0.0611 0.1598 0.086 Uiso 1 1 calc R . . C18 C 0.0996(3) -0.0273(4) 0.1766(3) 0.0780(19) Uani 1 1 d . . . H18A H 0.0802 -0.0519 0.1348 0.094 Uiso 1 1 calc R . . C19 C 0.1646(3) -0.0594(4) 0.2216(3) 0.0725(17) Uani 1 1 d . . . H19A H 0.1894 -0.1065 0.2111 0.087 Uiso 1 1 calc R . . C20 C 0.1938(3) -0.0230(3) 0.2822(3) 0.0602(14) Uani 1 1 d . . . H20A H 0.2392 -0.0443 0.3133 0.072 Uiso 1 1 calc R . . O9 O 0.17512(16) 0.55329(18) 0.51012(15) 0.0474(8) Uani 1 1 d . . . O10 O 0.09850(16) 0.50476(19) 0.55841(15) 0.0444(8) Uani 1 1 d . . . C21 C 0.1394(2) 0.5631(3) 0.5487(2) 0.0406(11) Uani 1 1 d . . . C22 C 0.1491(3) 0.6434(3) 0.5841(2) 0.0488(12) Uani 1 1 d . . . C23 C 0.1919(3) 0.7081(3) 0.5696(3) 0.0673(16) Uani 1 1 d . . . H23A H 0.2138 0.7003 0.5370 0.081 Uiso 1 1 calc R . . C24 C 0.2019(4) 0.7845(4) 0.6038(4) 0.090(2) Uani 1 1 d . . . H24A H 0.2311 0.8281 0.5944 0.108 Uiso 1 1 calc R . . C25 C 0.1704(4) 0.7967(4) 0.6498(4) 0.086(2) Uani 1 1 d . . . H25A H 0.1759 0.8496 0.6709 0.103 Uiso 1 1 calc R . . C26 C 0.1317(4) 0.7354(4) 0.6661(4) 0.093(2) Uani 1 1 d . . . H26A H 0.1121 0.7438 0.7001 0.111 Uiso 1 1 calc R . . C27 C 0.1201(3) 0.6580(4) 0.6326(3) 0.0777(18) Uani 1 1 d . . . H27A H 0.0916 0.6151 0.6439 0.093 Uiso 1 1 calc R . . N31 N 0.2153(3) 0.2522(3) 0.6715(2) 0.0826(16) Uani 1 1 d . . . C31 C 0.1883(3) 0.3062(4) 0.6875(3) 0.0689(16) Uani 1 1 d . . . C32 C 0.1576(4) 0.3800(4) 0.7071(4) 0.104(2) Uani 1 1 d . . . H32A H 0.1444 0.4216 0.6721 0.155 Uiso 1 1 calc R . . H32B H 0.1956 0.4039 0.7459 0.155 Uiso 1 1 calc R . . H32C H 0.1119 0.3648 0.7166 0.155 Uiso 1 1 calc R . . N32 N 0.0000 0.3188(5) 0.7500 0.087(2) Uani 1 2 d S . . C33 C 0.0000 0.2491(6) 0.7500 0.080(3) Uani 1 2 d S . . C34 C 0.0000 0.1590(6) 0.7500 0.134(5) Uani 1 2 d S . . H34A H -0.0494 0.1384 0.7211 0.201 Uiso 0.50 1 calc PR . . H34B H 0.0092 0.1384 0.7940 0.201 Uiso 0.50 1 calc PR . . H34C H 0.0403 0.1384 0.7349 0.201 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0372(2) 0.0371(2) 0.0384(2) 0.0015(3) 0.01726(18) 0.0019(2) Fe1 0.0352(3) 0.0399(4) 0.0383(4) -0.0038(3) 0.0152(3) -0.0023(3) O1 0.0384(17) 0.0392(19) 0.0298(18) -0.0034(15) 0.0145(14) -0.0020(13) N1 0.044(2) 0.043(2) 0.041(2) 0.0048(19) 0.0194(18) 0.0095(18) C1 0.052(3) 0.059(3) 0.041(3) 0.006(3) 0.017(2) 0.004(3) C2 0.050(3) 0.054(3) 0.039(3) -0.002(2) 0.013(2) 0.002(2) O2 0.0490(18) 0.0425(17) 0.0351(19) 0.0019(15) 0.0176(15) 0.0013(15) C3 0.053(3) 0.044(3) 0.054(3) 0.006(2) 0.031(2) 0.001(2) C4 0.044(3) 0.049(3) 0.047(3) 0.002(2) 0.022(2) 0.000(2) O3 0.0416(16) 0.0440(16) 0.0388(17) 0.0023(16) 0.0225(14) 0.0017(15) C5 0.057(3) 0.058(3) 0.049(3) 0.012(3) 0.027(3) 0.013(3) C6 0.054(3) 0.064(3) 0.049(3) 0.015(3) 0.019(3) 0.016(3) O4 0.0402(18) 0.063(2) 0.049(2) 0.0133(18) 0.0217(16) 0.0118(16) O5 0.0365(16) 0.044(2) 0.055(2) -0.0013(16) 0.0207(15) -0.0014(14) O6 0.0406(17) 0.0426(19) 0.047(2) -0.0003(15) 0.0207(14) -0.0018(14) C7 0.038(3) 0.045(3) 0.042(3) 0.005(2) 0.017(2) 0.004(2) C8 0.033(2) 0.045(3) 0.039(3) 0.003(2) 0.014(2) 0.001(2) C9 0.055(3) 0.052(3) 0.074(4) -0.008(3) 0.035(3) -0.005(2) C10 0.080(4) 0.075(4) 0.096(5) -0.009(4) 0.068(4) -0.008(3) C11 0.054(3) 0.067(4) 0.084(4) 0.006(3) 0.041(3) -0.013(3) C12 0.049(3) 0.054(3) 0.061(3) 0.001(3) 0.017(2) -0.012(3) C13 0.043(3) 0.046(3) 0.052(3) -0.008(2) 0.019(2) -0.003(2) O7 0.0410(17) 0.0449(18) 0.0440(19) -0.0108(15) 0.0168(15) -0.0001(14) O8 0.0410(17) 0.047(2) 0.0453(19) -0.0058(15) 0.0178(15) 0.0025(14) C14 0.043(3) 0.043(3) 0.041(3) -0.004(2) 0.018(2) -0.005(2) C15 0.051(3) 0.054(3) 0.041(3) -0.012(2) 0.026(2) -0.011(2) C16 0.047(3) 0.068(4) 0.042(3) -0.012(3) 0.017(2) -0.003(2) C17 0.054(3) 0.109(5) 0.053(4) -0.023(3) 0.018(3) -0.010(3) C18 0.066(4) 0.123(6) 0.049(4) -0.037(4) 0.025(3) -0.020(4) C19 0.076(4) 0.083(4) 0.070(4) -0.039(4) 0.040(4) -0.009(3) C20 0.064(3) 0.067(4) 0.055(3) -0.014(3) 0.027(3) -0.002(3) O9 0.053(2) 0.0415(17) 0.055(2) -0.0009(16) 0.0283(18) 0.0002(14) O10 0.0419(17) 0.0413(18) 0.055(2) 0.0008(16) 0.0228(15) 0.0022(14) C21 0.041(3) 0.034(3) 0.047(3) 0.005(2) 0.015(2) 0.009(2) C22 0.049(3) 0.047(3) 0.054(3) 0.000(3) 0.023(3) 0.005(2) C23 0.069(4) 0.056(4) 0.081(4) -0.007(3) 0.031(3) -0.009(3) C24 0.101(5) 0.053(4) 0.118(6) -0.019(4) 0.041(5) -0.026(3) C25 0.090(5) 0.063(4) 0.111(6) -0.034(4) 0.042(4) -0.009(4) C26 0.098(5) 0.079(5) 0.124(6) -0.045(4) 0.067(5) -0.026(4) C27 0.081(4) 0.070(4) 0.095(5) -0.017(4) 0.046(4) -0.018(3) N31 0.134(5) 0.063(3) 0.070(4) -0.001(3) 0.061(4) 0.006(3) C31 0.083(4) 0.074(4) 0.051(4) 0.003(3) 0.025(3) -0.006(4) C32 0.087(5) 0.119(6) 0.114(6) 0.011(5) 0.047(4) 0.026(4) N32 0.103(6) 0.073(5) 0.076(5) 0.000 0.018(4) 0.000 C33 0.090(7) 0.068(6) 0.092(7) 0.000 0.044(6) 0.000 C34 0.159(11) 0.069(7) 0.151(11) 0.000 0.023(9) 0.000 _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 Y1 O2 2.299(3) . ? Y1 O3 2.330(3) . ? Y1 O1 2.375(3) . ? Y1 O9 2.386(3) . ? Y1 O6 2.405(3) . ? Y1 O8 2.424(3) 7_556 ? Y1 O4 2.433(3) . ? Y1 O10 2.560(3) . ? Y1 N1 2.625(4) . ? Fe1 O2 1.948(3) . ? Fe1 O3 1.966(3) 7_556 ? Fe1 O5 1.993(3) . ? Fe1 O7 1.992(3) . ? Fe1 O1 2.054(3) . ? Fe1 O1 2.056(3) 7_556 ? O1 Fe1 2.056(3) 7_556 ? O1 H1 0.83(3) . ? N1 C5 1.468(5) . ? N1 C3 1.472(5) . ? N1 C1 1.483(6) . ? C1 C2 1.515(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.406(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.506(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.414(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.966(3) 7_556 ? C5 C6 1.503(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.432(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.84(3) . ? O5 C7 1.281(5) . ? O6 C7 1.251(5) . ? C7 C8 1.499(6) . ? C8 C13 1.378(6) . ? C8 C9 1.379(6) . ? C9 C10 1.390(7) . ? C9 H9A 0.9500 . ? C10 C11 1.376(7) . ? C10 H10A 0.9500 . ? C11 C12 1.363(7) . ? C11 H11A 0.9500 . ? C12 C13 1.388(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O7 C14 1.280(5) . ? O8 C14 1.245(5) . ? O8 Y1 2.424(3) 7_556 ? C14 C15 1.507(6) . ? C15 C16 1.366(6) . ? C15 C20 1.383(6) . ? C16 C17 1.384(6) . ? C16 H16A 0.9500 . ? C17 C18 1.361(8) . ? C17 H17A 0.9500 . ? C18 C19 1.374(7) . ? C18 H18A 0.9500 . ? C19 C20 1.382(7) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? O9 C21 1.260(5) . ? O10 C21 1.267(5) . ? C21 C22 1.473(6) . ? C22 C27 1.377(7) . ? C22 C23 1.405(7) . ? C23 C24 1.407(8) . ? C23 H23A 0.9500 . ? C24 C25 1.350(8) . ? C24 H24A 0.9500 . ? C25 C26 1.336(8) . ? C25 H25A 0.9500 . ? C26 C27 1.411(7) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N31 C31 1.114(7) . ? C31 C32 1.436(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32 C33 1.108(10) . ? C33 C34 1.432(12) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 O2 Y1 O3 82.29(10) . . ? O2 Y1 O1 68.42(10) . . ? O3 Y1 O1 68.69(10) . . ? O2 Y1 O9 141.93(11) . . ? O3 Y1 O9 85.56(10) . . ? O1 Y1 O9 138.19(10) . . ? O2 Y1 O6 76.97(11) . . ? O3 Y1 O6 140.36(10) . . ? O1 Y1 O6 72.35(10) . . ? O9 Y1 O6 130.33(11) . . ? O2 Y1 O8 137.41(10) . 7_556 ? O3 Y1 O8 73.71(10) . 7_556 ? O1 Y1 O8 70.21(10) . 7_556 ? O9 Y1 O8 71.23(10) . 7_556 ? O6 Y1 O8 99.84(10) . 7_556 ? O2 Y1 O4 83.66(11) . . ? O3 Y1 O4 132.15(10) . . ? O1 Y1 O4 143.35(11) . . ? O9 Y1 O4 78.18(11) . . ? O6 Y1 O4 78.74(10) . . ? O8 Y1 O4 138.10(10) 7_556 . ? O2 Y1 O10 146.82(10) . . ? O3 Y1 O10 130.45(10) . . ? O1 Y1 O10 123.35(10) . . ? O9 Y1 O10 52.68(10) . . ? O6 Y1 O10 78.19(10) . . ? O8 Y1 O10 68.65(9) 7_556 . ? O4 Y1 O10 70.14(10) . . ? O2 Y1 N1 67.15(11) . . ? O3 Y1 N1 68.23(10) . . ? O1 Y1 N1 120.68(10) . . ? O9 Y1 N1 74.82(11) . . ? O6 Y1 N1 130.00(11) . . ? O8 Y1 N1 130.15(11) 7_556 . ? O4 Y1 N1 64.14(11) . . ? O10 Y1 N1 115.44(10) . . ? O2 Fe1 O3 174.76(12) . 7_556 ? O2 Fe1 O5 90.66(12) . . ? O3 Fe1 O5 92.47(11) 7_556 . ? O2 Fe1 O7 92.13(12) . . ? O3 Fe1 O7 91.29(12) 7_556 . ? O5 Fe1 O7 102.72(12) . . ? O2 Fe1 O1 82.07(12) . . ? O3 Fe1 O1 93.76(11) 7_556 . ? O5 Fe1 O1 89.18(12) . . ? O7 Fe1 O1 166.87(12) . . ? O2 Fe1 O1 93.31(12) . 7_556 ? O3 Fe1 O1 82.58(11) 7_556 7_556 ? O5 Fe1 O1 164.55(12) . 7_556 ? O7 Fe1 O1 92.05(12) . 7_556 ? O1 Fe1 O1 76.61(13) . 7_556 ? Fe1 O1 Fe1 103.39(13) . 7_556 ? Fe1 O1 Y1 100.96(11) . . ? Fe1 O1 Y1 101.53(12) 7_556 . ? Fe1 O1 H1 116(3) . . ? Fe1 O1 H1 122(3) 7_556 . ? Y1 O1 H1 110(3) . . ? C5 N1 C3 110.0(3) . . ? C5 N1 C1 111.7(4) . . ? C3 N1 C1 111.3(3) . . ? C5 N1 Y1 108.1(3) . . ? C3 N1 Y1 104.2(3) . . ? C1 N1 Y1 111.2(3) . . ? N1 C1 C2 111.9(4) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O2 C2 C1 109.6(4) . . ? O2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C2 O2 Fe1 132.8(3) . . ? C2 O2 Y1 120.1(3) . . ? Fe1 O2 Y1 107.08(13) . . ? N1 C3 C4 111.3(4) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 109.7(4) . . ? O3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 O3 Fe1 122.1(2) . 7_556 ? C4 O3 Y1 122.6(2) . . ? Fe1 O3 Y1 105.98(12) 7_556 . ? N1 C5 C6 110.8(4) . . ? N1 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? O4 C6 C5 107.7(4) . . ? O4 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O4 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 O4 Y1 125.5(3) . . ? C6 O4 H4 112(3) . . ? Y1 O4 H4 122(3) . . ? C7 O5 Fe1 128.8(3) . . ? C7 O6 Y1 135.1(3) . . ? O6 C7 O5 125.7(4) . . ? O6 C7 C8 119.6(4) . . ? O5 C7 C8 114.7(4) . . ? C13 C8 C9 119.1(4) . . ? C13 C8 C7 120.6(4) . . ? C9 C8 C7 120.3(4) . . ? C8 C9 C10 120.0(5) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 119.9(5) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C12 C11 C10 120.6(5) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 119.4(5) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C8 C13 C12 121.0(5) . . ? C8 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C14 O7 Fe1 125.0(3) . . ? C14 O8 Y1 139.1(3) . 7_556 ? O8 C14 O7 125.4(4) . . ? O8 C14 C15 117.7(4) . . ? O7 C14 C15 116.8(4) . . ? C16 C15 C20 119.4(5) . . ? C16 C15 C14 120.8(4) . . ? C20 C15 C14 119.8(5) . . ? C15 C16 C17 121.1(5) . . ? C15 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? C18 C17 C16 119.0(5) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C19 121.0(5) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C18 C19 C20 119.7(5) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C19 C20 C15 119.7(5) . . ? C19 C20 H20A 120.1 . . ? C15 C20 H20A 120.1 . . ? C21 O9 Y1 96.8(3) . . ? C21 O10 Y1 88.5(3) . . ? O9 C21 O10 121.0(4) . . ? O9 C21 C22 117.8(4) . . ? O10 C21 C22 121.2(4) . . ? C27 C22 C23 117.5(5) . . ? C27 C22 C21 123.1(5) . . ? C23 C22 C21 119.4(5) . . ? C22 C23 C24 119.4(6) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C25 C24 C23 120.9(6) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C26 C25 C24 121.0(6) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C25 C26 C27 119.7(7) . . ? C25 C26 H26A 120.2 . . ? C27 C26 H26A 120.2 . . ? C22 C27 C26 121.4(6) . . ? C22 C27 H27A 119.3 . . ? C26 C27 H27A 119.3 . . ? N31 C31 C32 175.6(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 . . ? N32 C33 C34 180.0 . . ? 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 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N31 0.83(3) 2.16(3) 2.971(6) 167(4) . O4 H4 O10 0.84(3) 1.89(3) 2.700(4) 162(5) 5_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.290 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.061