# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Diana Visinescu' _publ_contact_author_email DIANA.VISINESCU@GMAIL.COM _publ_section_title ; [Fe(phen)(CN)4]-: a suitable metalloligand unit to build 3d-4f heterobimetallic complexes with mixed bpym-cyano bridges (phen = 1,10-phenantroline, bpym = 2,2'-bipyrimidine) ; loop_ _publ_author_name 'Diana Visinescu' 'Oscar Fabelo' 'Miguel Julve' 'F Lloret' 'Catalina Ruiz-Perez' # Attachment 'compound_1.cif' data_compound _database_code_depnum_ccdc_archive 'CCDC 764597' #TrackingRef 'compound_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H66 Eu2 Fe4 N30 O20' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Brown _diffrn_ambient_temperature 293(2) _chemical_formula_weight 2198.87 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' O O 0.0106 0.0060 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1400(6) _cell_length_b 15.0630(15) _cell_length_c 16.5770(18) _cell_angle_alpha 94.960(8) _cell_angle_beta 104.473(8) _cell_angle_gamma 92.006(7) _cell_volume 2438.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 1.922 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25218 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 6.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10719 _reflns_number_gt 8818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+2.8244P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10719 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Eu1 Eu 0.707962(17) 0.664650(12) 0.128855(12) 0.02887(7) Uani 1 1 d . . . Fe1 Fe 1.12711(5) 0.45384(4) 0.27035(3) 0.03228(13) Uani 1 1 d . . . Fe2 Fe 0.37264(6) 0.91797(4) 0.20856(4) 0.04037(15) Uani 1 1 d . . . C1 C 0.7923(4) 0.4706(3) 0.0305(3) 0.0398(10) Uani 1 1 d . . . H1 H 0.8786 0.4942 0.0598 0.048 Uiso 1 1 calc R . . C2 C 0.7806(4) 0.3938(3) -0.0206(3) 0.0527(13) Uani 1 1 d . . . H2 H 0.8576 0.3653 -0.0272 0.063 Uiso 1 1 calc R . . C3 C 0.6525(4) 0.3595(3) -0.0620(3) 0.0469(12) Uani 1 1 d . . . H3 H 0.6430 0.3068 -0.0971 0.056 Uiso 1 1 calc R . . C4 C 0.5613(3) 0.4760(2) -0.0040(2) 0.0276(7) Uani 1 1 d . . . C5 C 0.9841(4) 0.5317(3) 0.2326(3) 0.0340(8) Uani 1 1 d . . . C6 C 0.4969(4) 0.8282(3) 0.1985(3) 0.0364(9) Uani 1 1 d . . . C7 C 1.0990(4) 0.4057(3) 0.1572(3) 0.0409(10) Uani 1 1 d . . . C8 C 1.2652(4) 0.5371(3) 0.2524(3) 0.0414(10) Uani 1 1 d . . . C9 C 0.9863(5) 0.3693(3) 0.2834(3) 0.0497(11) Uani 1 1 d . . . C10 C 0.3975(5) 0.8918(4) 0.3227(4) 0.0611(14) Uani 1 1 d . . . C11 C 0.5229(5) 1.0072(3) 0.2427(4) 0.0560(13) Uani 1 1 d . . . C12 C 0.2239(4) 0.8261(3) 0.1721(3) 0.0418(10) Uani 1 1 d . . . C13 C 1.3261(5) 0.3099(3) 0.2706(4) 0.0553(13) Uani 1 1 d . . . H13 H 1.2953 0.3026 0.2125 0.066 Uiso 1 1 calc R . . C14 C 1.4257(6) 0.2557(4) 0.3097(5) 0.0773(19) Uani 1 1 d . . . H14 H 1.4588 0.2118 0.2782 0.093 Uiso 1 1 calc R . . C15 C 1.4745(8) 0.2671(6) 0.3943(6) 0.103(3) Uani 1 1 d . . . H15 H 1.5408 0.2308 0.4208 0.124 Uiso 1 1 calc R . . C16 C 1.4248(7) 0.3342(6) 0.4423(4) 0.089(2) Uani 1 1 d . . . C17 C 1.3215(5) 0.3848(4) 0.3981(3) 0.0585(14) Uani 1 1 d . . . C18 C 1.4697(9) 0.3566(9) 0.5318(6) 0.135(4) Uani 1 1 d . . . H18 H 1.5391 0.3257 0.5633 0.162 Uiso 1 1 calc R . . C19 C 1.4132(10) 0.4209(9) 0.5702(5) 0.139(4) Uani 1 1 d . . . H19 H 1.4431 0.4325 0.6281 0.167 Uiso 1 1 calc R . . C20 C 1.3104(8) 0.4716(6) 0.5262(4) 0.097(2) Uani 1 1 d . . . C21 C 1.2642(5) 0.4523(4) 0.4386(3) 0.0598(14) Uani 1 1 d . . . C22 C 1.1121(6) 0.5637(4) 0.4266(3) 0.0630(14) Uani 1 1 d . . . H22 H 1.0466 0.5961 0.3938 0.076 Uiso 1 1 calc R . . C23 C 1.1507(9) 0.5856(6) 0.5135(4) 0.096(2) Uani 1 1 d . . . H23 H 1.1095 0.6312 0.5378 0.115 Uiso 1 1 calc R . . C24 C 1.2465(9) 0.5411(7) 0.5613(4) 0.114(3) Uani 1 1 d . . . H24 H 1.2716 0.5562 0.6189 0.136 Uiso 1 1 calc R . . C25 C 0.1929(6) 1.0430(4) 0.2781(5) 0.0746(18) Uani 1 1 d . . . H25 H 0.2251 1.0210 0.3297 0.090 Uiso 1 1 calc R . . C26 C 0.0965(7) 1.1086(5) 0.2692(6) 0.087(2) Uani 1 1 d . . . H26 H 0.0665 1.1306 0.3153 0.105 Uiso 1 1 calc R . . C27 C 0.0468(7) 1.1402(4) 0.1939(6) 0.086(2) Uani 1 1 d . . . H27 H -0.0181 1.1829 0.1886 0.104 Uiso 1 1 calc R . . C28 C 0.0927(5) 1.1090(3) 0.1241(5) 0.0684(17) Uani 1 1 d . . . C29 C 0.1904(5) 1.0444(3) 0.1380(4) 0.0527(13) Uani 1 1 d . . . C30 C 0.0489(6) 1.1362(4) 0.0425(6) 0.078(2) Uani 1 1 d . . . H30 H -0.0159 1.1788 0.0327 0.094 Uiso 1 1 calc R . . C31 C 0.0970(6) 1.1032(4) -0.0204(5) 0.0751(19) Uani 1 1 d . . . H31 H 0.0658 1.1237 -0.0728 0.090 Uiso 1 1 calc R . . C32 C 0.1968(5) 1.0363(3) -0.0098(4) 0.0586(14) Uani 1 1 d . . . C33 C 0.2417(4) 1.0092(3) 0.0707(4) 0.0496(12) Uani 1 1 d . . . C34 C 0.3852(5) 0.9112(3) 0.0276(4) 0.0515(12) Uani 1 1 d . . . H34 H 0.4488 0.8680 0.0391 0.062 Uiso 1 1 calc R . . C35 C 0.3461(6) 0.9352(4) -0.0528(4) 0.0623(14) Uani 1 1 d . . . H35 H 0.3845 0.9092 -0.0939 0.075 Uiso 1 1 calc R . . C36 C 0.2503(6) 0.9976(4) -0.0724(4) 0.0660(15) Uani 1 1 d . . . H36 H 0.2220 1.0135 -0.1267 0.079 Uiso 1 1 calc R . . O1A O 0.6358(4) 0.7821(3) 0.0352(2) 0.0605(9) Uani 1 1 d . . . O1W O 0.8948(3) 0.6787(2) 0.06845(18) 0.0398(7) Uani 1 1 d . . . O2A O 0.6301(4) 0.6653(3) -0.0468(3) 0.0698(11) Uani 1 1 d . . . O2W O 0.6184(3) 0.5809(2) 0.2215(2) 0.0529(8) Uani 1 1 d . . . O3A O 0.5777(6) 0.7903(3) -0.0974(3) 0.0900(15) Uani 1 1 d . . . O3W O 0.8594(3) 0.7694(2) 0.2262(2) 0.0629(10) Uani 1 1 d . . . O4W O 0.6213(6) 0.3986(4) 0.2036(4) 0.1141(19) Uani 1 1 d . . . O5W O 0.1065(6) 0.7451(5) 0.3340(5) 0.141(3) Uani 1 1 d . . . O6W O 0.8105(9) 1.1815(5) 0.3712(4) 0.150(3) Uani 1 1 d . . . O7W O 0.8468(9) 0.9336(6) 0.2972(7) 0.214(5) Uani 1 1 d . . . N1 N 0.6818(3) 0.5135(2) 0.0397(2) 0.0309(7) Uani 1 1 d . . . N1A N 0.6123(4) 0.7460(3) -0.0393(3) 0.0564(11) Uani 1 1 d . . . N2 N 0.5406(3) 0.3996(2) -0.0532(2) 0.0347(7) Uani 1 1 d . . . N3 N 0.8956(3) 0.5750(3) 0.2082(2) 0.0416(8) Uani 1 1 d . . . N4 N 0.5672(4) 0.7726(2) 0.1886(2) 0.0417(8) Uani 1 1 d . . . N5 N 1.0850(4) 0.3738(3) 0.0893(3) 0.0608(12) Uani 1 1 d . . . N6 N 1.3525(4) 0.5821(3) 0.2424(3) 0.0621(12) Uani 1 1 d . . . N7 N 0.9016(6) 0.3217(4) 0.2898(4) 0.0901(19) Uani 1 1 d . . . N8 N 0.4109(7) 0.8768(5) 0.3893(4) 0.100(2) Uani 1 1 d . . . N9 N 0.6120(6) 1.0593(4) 0.2625(4) 0.0871(17) Uani 1 1 d . . . N10 N 0.1375(4) 0.7734(3) 0.1477(3) 0.0532(10) Uani 1 1 d . . . N11 N 1.2735(4) 0.3718(3) 0.3133(2) 0.0433(9) Uani 1 1 d . . . N12 N 1.1663(4) 0.4983(3) 0.3903(2) 0.0454(9) Uani 1 1 d . . . N13 N 0.2387(4) 1.0119(3) 0.2127(3) 0.0537(11) Uani 1 1 d . . . N14 N 0.3366(3) 0.9467(2) 0.0897(3) 0.0427(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02009(9) 0.03007(11) 0.03455(12) -0.00479(7) 0.00594(7) 0.00249(6) Fe1 0.0280(3) 0.0418(3) 0.0268(3) 0.0009(2) 0.0066(2) 0.0077(2) Fe2 0.0307(3) 0.0341(3) 0.0531(4) -0.0105(3) 0.0092(3) 0.0043(2) C1 0.0197(17) 0.046(2) 0.045(3) -0.0148(19) -0.0006(16) 0.0077(16) C2 0.0216(19) 0.058(3) 0.069(3) -0.025(2) 0.0034(19) 0.0130(18) C3 0.0284(19) 0.044(2) 0.060(3) -0.023(2) 0.0047(19) 0.0099(17) C4 0.0233(16) 0.0285(18) 0.030(2) -0.0010(15) 0.0064(14) 0.0034(14) C5 0.0269(18) 0.043(2) 0.031(2) -0.0024(17) 0.0065(15) 0.0052(16) C6 0.0295(19) 0.035(2) 0.040(2) -0.0075(17) 0.0038(16) 0.0001(16) C7 0.0283(19) 0.059(3) 0.035(2) 0.001(2) 0.0068(16) 0.0122(18) C8 0.028(2) 0.058(3) 0.037(2) 0.006(2) 0.0041(17) 0.0090(19) C9 0.048(3) 0.050(3) 0.055(3) -0.003(2) 0.023(2) 0.003(2) C10 0.054(3) 0.073(4) 0.052(3) -0.014(3) 0.010(2) 0.011(3) C11 0.046(3) 0.042(3) 0.074(4) -0.010(2) 0.009(2) 0.003(2) C12 0.032(2) 0.040(2) 0.051(3) -0.003(2) 0.0084(18) 0.0089(18) C13 0.049(3) 0.054(3) 0.064(3) 0.009(2) 0.014(2) 0.018(2) C14 0.067(4) 0.071(4) 0.099(5) 0.021(4) 0.022(4) 0.035(3) C15 0.085(5) 0.124(6) 0.112(7) 0.057(5) 0.022(4) 0.067(5) C16 0.072(4) 0.135(6) 0.062(4) 0.047(4) 0.003(3) 0.041(4) C17 0.049(3) 0.083(4) 0.045(3) 0.025(3) 0.008(2) 0.019(3) C18 0.096(6) 0.238(12) 0.070(6) 0.062(7) -0.003(4) 0.067(7) C19 0.117(7) 0.252(13) 0.039(4) 0.016(6) -0.008(4) 0.064(8) C20 0.088(5) 0.162(8) 0.033(3) 0.002(4) 0.001(3) 0.019(5) C21 0.057(3) 0.090(4) 0.029(3) 0.009(3) 0.005(2) 0.008(3) C22 0.079(4) 0.071(4) 0.040(3) -0.008(3) 0.019(3) 0.011(3) C23 0.122(6) 0.118(6) 0.045(4) -0.023(4) 0.027(4) 0.013(5) C24 0.112(6) 0.187(9) 0.031(3) -0.026(5) 0.009(4) 0.015(6) C25 0.066(4) 0.068(4) 0.091(5) -0.020(3) 0.029(3) 0.019(3) C26 0.078(4) 0.073(4) 0.113(6) -0.028(4) 0.039(4) 0.024(4) C27 0.060(4) 0.053(3) 0.147(8) -0.011(4) 0.031(4) 0.020(3) C28 0.041(3) 0.038(3) 0.123(6) -0.005(3) 0.018(3) 0.008(2) C29 0.037(2) 0.029(2) 0.088(4) -0.002(2) 0.012(2) 0.0041(18) C30 0.048(3) 0.047(3) 0.135(7) 0.024(4) 0.008(4) 0.017(2) C31 0.056(3) 0.051(3) 0.115(6) 0.031(3) 0.008(3) 0.010(3) C32 0.041(3) 0.044(3) 0.088(4) 0.021(3) 0.006(3) 0.001(2) C33 0.038(2) 0.030(2) 0.078(4) 0.005(2) 0.010(2) 0.0002(18) C34 0.046(3) 0.045(3) 0.066(3) 0.003(2) 0.017(2) 0.008(2) C35 0.060(3) 0.065(3) 0.067(4) 0.014(3) 0.022(3) 0.005(3) C36 0.062(3) 0.063(3) 0.072(4) 0.024(3) 0.011(3) -0.001(3) O1A 0.067(2) 0.071(2) 0.051(2) 0.0159(19) 0.0233(18) 0.0248(19) O1W 0.0302(14) 0.0520(18) 0.0368(16) -0.0037(13) 0.0115(12) -0.0031(12) O2A 0.061(2) 0.052(2) 0.099(3) 0.008(2) 0.025(2) 0.0113(18) O2W 0.0357(16) 0.075(2) 0.055(2) 0.0236(18) 0.0180(14) 0.0097(15) O3A 0.129(4) 0.093(3) 0.054(3) 0.032(2) 0.021(3) 0.039(3) O3W 0.0379(17) 0.061(2) 0.075(3) -0.0340(19) 0.0011(16) -0.0044(15) O4W 0.114(4) 0.076(3) 0.145(5) 0.016(3) 0.019(4) -0.005(3) O5W 0.095(4) 0.188(7) 0.129(5) 0.052(5) -0.003(4) -0.030(4) O6W 0.205(7) 0.127(5) 0.102(5) -0.002(4) 0.024(5) -0.080(5) O7W 0.143(6) 0.132(6) 0.301(12) -0.105(7) -0.028(7) 0.037(5) N1 0.0212(14) 0.0340(17) 0.0340(18) -0.0048(14) 0.0028(12) 0.0043(12) N1A 0.049(2) 0.067(3) 0.062(3) 0.020(2) 0.024(2) 0.021(2) N2 0.0234(15) 0.0335(17) 0.042(2) -0.0101(14) 0.0036(13) 0.0048(12) N3 0.0306(17) 0.051(2) 0.041(2) -0.0007(17) 0.0070(15) 0.0053(16) N4 0.0363(18) 0.0388(19) 0.047(2) -0.0060(16) 0.0083(16) 0.0059(15) N5 0.044(2) 0.095(3) 0.039(2) -0.012(2) 0.0067(18) 0.020(2) N6 0.041(2) 0.080(3) 0.068(3) 0.025(3) 0.013(2) 0.001(2) N7 0.092(4) 0.068(3) 0.124(5) -0.012(3) 0.064(4) -0.019(3) N8 0.110(5) 0.129(6) 0.059(4) 0.002(4) 0.021(3) 0.019(4) N9 0.074(3) 0.065(3) 0.113(5) -0.019(3) 0.019(3) -0.021(3) N10 0.036(2) 0.052(2) 0.067(3) -0.002(2) 0.0070(19) -0.0001(18) N11 0.0372(18) 0.052(2) 0.040(2) 0.0085(17) 0.0058(15) 0.0144(16) N12 0.051(2) 0.057(2) 0.0273(19) -0.0025(17) 0.0110(16) 0.0024(18) N13 0.042(2) 0.042(2) 0.075(3) -0.014(2) 0.015(2) 0.0080(17) N14 0.0337(18) 0.0328(18) 0.060(3) 0.0028(17) 0.0100(17) 0.0029(14) _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 Eu1 O1W 2.365(3) . ? Eu1 O3W 2.367(3) . ? Eu1 O2W 2.393(3) . ? Eu1 O1A 2.464(4) . ? Eu1 N4 2.501(3) . ? Eu1 N3 2.532(4) . ? Eu1 N1 2.573(3) . ? Eu1 N2 2.627(3) 2_665 ? Eu1 O2A 2.821(5) . ? Eu1 N1A 3.088(5) . ? Fe1 C7 1.899(5) . ? Fe1 C5 1.914(4) . ? Fe1 C8 1.942(5) . ? Fe1 C9 1.944(5) . ? Fe1 N12 1.979(4) . ? Fe1 N11 1.998(3) . ? Fe2 C6 1.905(4) . ? Fe2 C10 1.923(7) . ? Fe2 C11 1.934(5) . ? Fe2 C12 1.952(5) . ? Fe2 N14 2.001(4) . ? Fe2 N13 2.004(4) . ? C1 N1 1.346(4) . ? C1 C2 1.356(6) . ? C1 H1 0.9300 . ? C2 C3 1.368(6) . ? C2 H2 0.9300 . ? C3 N2 1.337(5) . ? C3 H3 0.9300 . ? C4 N2 1.330(5) . ? C4 N1 1.333(5) . ? C4 C4 1.488(6) 2_665 ? C5 N3 1.140(5) . ? C6 N4 1.146(5) . ? C7 N5 1.158(6) . ? C8 N6 1.150(6) . ? C9 N7 1.131(7) . ? C10 N8 1.122(8) . ? C11 N9 1.139(7) . ? C12 N10 1.131(6) . ? C13 N11 1.328(6) . ? C13 C14 1.389(7) . ? C13 H13 0.9300 . ? C14 C15 1.358(11) . ? C14 H14 0.9300 . ? C15 C16 1.417(11) . ? C15 H15 0.9300 . ? C16 C17 1.408(7) . ? C16 C18 1.444(12) . ? C17 N11 1.363(6) . ? C17 C21 1.393(8) . ? C18 C19 1.336(13) . ? C18 H18 0.9300 . ? C19 C20 1.405(12) . ? C19 H19 0.9300 . ? C20 C24 1.409(11) . ? C20 C21 1.412(8) . ? C21 N12 1.361(6) . ? C22 N12 1.318(6) . ? C22 C23 1.402(8) . ? C22 H22 0.9300 . ? C23 C24 1.331(11) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N13 1.336(7) . ? C25 C26 1.406(8) . ? C25 H25 0.9300 . ? C26 C27 1.357(11) . ? C26 H26 0.9300 . ? C27 C28 1.402(10) . ? C27 H27 0.9300 . ? C28 C29 1.405(6) . ? C28 C30 1.415(10) . ? C29 N13 1.354(7) . ? C29 C33 1.415(8) . ? C30 C31 1.325(10) . ? C30 H30 0.9300 . ? C31 C32 1.444(7) . ? C31 H31 0.9300 . ? C32 C36 1.382(9) . ? C32 C33 1.398(8) . ? C33 N14 1.369(5) . ? C34 N14 1.328(6) . ? C34 C35 1.377(8) . ? C34 H34 0.9300 . ? C35 C36 1.375(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O1A N1A 1.266(6) . ? O2A N1A 1.236(5) . ? O3A N1A 1.206(6) . ? N2 Eu1 2.627(3) 2_665 ? 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 O1W Eu1 O3W 77.22(12) . . ? O1W Eu1 O2W 143.11(10) . . ? O3W Eu1 O2W 100.63(14) . . ? O1W Eu1 O1A 78.48(11) . . ? O3W Eu1 O1A 90.39(14) . . ? O2W Eu1 O1A 138.30(11) . . ? O1W Eu1 N4 134.60(11) . . ? O3W Eu1 N4 72.33(12) . . ? O2W Eu1 N4 76.28(12) . . ? O1A Eu1 N4 69.01(13) . . ? O1W Eu1 N3 72.62(11) . . ? O3W Eu1 N3 74.33(13) . . ? O2W Eu1 N3 71.44(11) . . ? O1A Eu1 N3 149.58(12) . . ? N4 Eu1 N3 127.52(12) . . ? O1W Eu1 N1 79.45(10) . . ? O3W Eu1 N1 146.08(10) . . ? O2W Eu1 N1 83.80(12) . . ? O1A Eu1 N1 108.68(12) . . ? N4 Eu1 N1 140.25(11) . . ? N3 Eu1 N1 75.40(11) . . ? O1W Eu1 N2 127.02(10) . 2_665 ? O3W Eu1 N2 150.75(11) . 2_665 ? O2W Eu1 N2 70.30(11) . 2_665 ? O1A Eu1 N2 80.53(12) . 2_665 ? N4 Eu1 N2 78.46(11) . 2_665 ? N3 Eu1 N2 124.87(11) . 2_665 ? N1 Eu1 N2 62.42(9) . 2_665 ? O1W Eu1 O2A 66.48(11) . . ? O3W Eu1 O2A 127.04(14) . . ? O2W Eu1 O2A 131.55(12) . . ? O1A Eu1 O2A 46.64(12) . . ? N4 Eu1 O2A 107.58(12) . . ? N3 Eu1 O2A 124.83(11) . . ? N1 Eu1 O2A 62.30(11) . . ? N2 Eu1 O2A 63.73(11) 2_665 . ? O1W Eu1 N1A 71.05(10) . . ? O3W Eu1 N1A 109.15(14) . . ? O2W Eu1 N1A 140.19(11) . . ? O1A Eu1 N1A 23.05(12) . . ? N4 Eu1 N1A 88.02(12) . . ? N3 Eu1 N1A 141.47(11) . . ? N1 Eu1 N1A 85.76(12) . . ? N2 Eu1 N1A 70.80(12) 2_665 . ? O2A Eu1 N1A 23.60(11) . . ? C7 Fe1 C5 87.82(17) . . ? C7 Fe1 C8 88.20(19) . . ? C5 Fe1 C8 92.45(17) . . ? C7 Fe1 C9 89.5(2) . . ? C5 Fe1 C9 86.90(19) . . ? C8 Fe1 C9 177.7(2) . . ? C7 Fe1 N12 176.11(17) . . ? C5 Fe1 N12 96.07(17) . . ? C8 Fe1 N12 91.61(18) . . ? C9 Fe1 N12 90.67(19) . . ? C7 Fe1 N11 93.71(17) . . ? C5 Fe1 N11 177.91(16) . . ? C8 Fe1 N11 89.03(17) . . ? C9 Fe1 N11 91.68(19) . . ? N12 Fe1 N11 82.40(16) . . ? C6 Fe2 C10 87.0(2) . . ? C6 Fe2 C11 90.13(19) . . ? C10 Fe2 C11 90.3(3) . . ? C6 Fe2 C12 88.47(17) . . ? C10 Fe2 C12 90.5(2) . . ? C11 Fe2 C12 178.3(2) . . ? C6 Fe2 N14 95.60(17) . . ? C10 Fe2 N14 176.97(19) . . ? C11 Fe2 N14 91.3(2) . . ? C12 Fe2 N14 88.00(18) . . ? C6 Fe2 N13 177.06(19) . . ? C10 Fe2 N13 95.8(2) . . ? C11 Fe2 N13 90.78(18) . . ? C12 Fe2 N13 90.58(16) . . ? N14 Fe2 N13 81.59(18) . . ? N1 C1 C2 121.6(4) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 118.2(4) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? N2 C3 C2 121.8(4) . . ? N2 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? N2 C4 N1 126.1(3) . . ? N2 C4 C4 117.3(4) . 2_665 ? N1 C4 C4 116.6(4) . 2_665 ? N3 C5 Fe1 177.0(4) . . ? N4 C6 Fe2 176.5(4) . . ? N5 C7 Fe1 177.4(4) . . ? N6 C8 Fe1 175.7(4) . . ? N7 C9 Fe1 178.0(6) . . ? N8 C10 Fe2 179.4(6) . . ? N9 C11 Fe2 179.5(6) . . ? N10 C12 Fe2 177.2(5) . . ? N11 C13 C14 122.2(6) . . ? N11 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.3(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 116.6(6) . . ? C17 C16 C18 116.7(7) . . ? C15 C16 C18 126.8(7) . . ? N11 C17 C21 116.1(4) . . ? N11 C17 C16 122.1(5) . . ? C21 C17 C16 121.8(6) . . ? C19 C18 C16 121.1(7) . . ? C19 C18 H18 119.4 . . ? C16 C18 H18 119.4 . . ? C18 C19 C20 122.3(7) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C24 126.2(7) . . ? C19 C20 C21 118.4(7) . . ? C24 C20 C21 115.5(7) . . ? N12 C21 C17 117.5(4) . . ? N12 C21 C20 122.8(6) . . ? C17 C21 C20 119.7(5) . . ? N12 C22 C23 121.7(6) . . ? N12 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 119.9(7) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C20 121.2(6) . . ? C23 C24 H24 119.4 . . ? C20 C24 H24 119.4 . . ? N13 C25 C26 120.4(7) . . ? N13 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 120.5(7) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 120.5(6) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C29 115.8(7) . . ? C27 C28 C30 126.0(6) . . ? C29 C28 C30 118.2(6) . . ? N13 C29 C28 123.8(5) . . ? N13 C29 C33 116.9(4) . . ? C28 C29 C33 119.3(6) . . ? C31 C30 C28 122.4(5) . . ? C31 C30 H30 118.8 . . ? C28 C30 H30 118.8 . . ? C30 C31 C32 121.6(6) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C36 C32 C33 118.3(5) . . ? C36 C32 C31 125.2(6) . . ? C33 C32 C31 116.6(6) . . ? N14 C33 C32 122.6(5) . . ? N14 C33 C29 115.5(5) . . ? C32 C33 C29 121.9(4) . . ? N14 C34 C35 123.2(5) . . ? N14 C34 H34 118.4 . . ? C35 C34 H34 118.4 . . ? C36 C35 C34 119.9(6) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C32 118.8(6) . . ? C35 C36 H36 120.6 . . ? C32 C36 H36 120.6 . . ? N1A O1A Eu1 107.3(3) . . ? N1A O2A Eu1 90.4(3) . . ? C4 N1 C1 116.1(3) . . ? C4 N1 Eu1 122.9(2) . . ? C1 N1 Eu1 120.8(2) . . ? O3A N1A O2A 124.1(5) . . ? O3A N1A O1A 120.2(5) . . ? O2A N1A O1A 115.6(4) . . ? O3A N1A Eu1 169.8(4) . . ? O2A N1A Eu1 66.0(3) . . ? O1A N1A Eu1 49.6(2) . . ? C4 N2 C3 116.2(3) . . ? C4 N2 Eu1 120.7(2) . 2_665 ? C3 N2 Eu1 123.2(3) . 2_665 ? C5 N3 Eu1 169.7(3) . . ? C6 N4 Eu1 164.8(4) . . ? C13 N11 C17 119.2(4) . . ? C13 N11 Fe1 128.8(3) . . ? C17 N11 Fe1 112.0(3) . . ? C22 N12 C21 118.9(4) . . ? C22 N12 Fe1 129.2(4) . . ? C21 N12 Fe1 112.0(3) . . ? C25 N13 C29 119.0(5) . . ? C25 N13 Fe2 128.1(4) . . ? C29 N13 Fe2 112.9(3) . . ? C34 N14 C33 117.1(4) . . ? C34 N14 Fe2 129.7(3) . . ? C33 N14 Fe2 113.1(3) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.368 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.102 # Attachment 'compound_2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 764598' #TrackingRef 'compound_2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H74 Fe4 Gd2 N30 O23' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Brown _diffrn_ambient_temperature 150(2) _chemical_formula_weight 2265.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1241(6) _cell_length_b 14.9965(12) _cell_length_c 16.4861(10) _cell_angle_alpha 94.712(7) _cell_angle_beta 104.484(5) _cell_angle_gamma 92.130(5) _cell_volume 2411.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 2.023 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46817 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 6.42 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10868 _reflns_number_gt 10030 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+5.3900P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10868 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 0.706951(13) 0.664815(9) 0.129124(8) 0.01638(5) Uani 1 1 d . . . Fe1 Fe 1.12579(4) 0.45325(3) 0.27057(2) 0.01826(9) Uani 1 1 d . . . Fe2 Fe 0.37330(5) 0.91928(3) 0.20899(3) 0.02337(10) Uani 1 1 d . . . C1 C 0.7935(3) 0.4718(2) 0.0301(2) 0.0237(6) Uani 1 1 d . . . H1 H 0.8799 0.4962 0.0589 0.028 Uiso 1 1 calc R . . C2 C 0.7822(3) 0.3937(2) -0.0210(2) 0.0308(7) Uani 1 1 d . . . H2 H 0.8594 0.3654 -0.0279 0.037 Uiso 1 1 calc R . . C3 C 0.6530(3) 0.3584(2) -0.0619(2) 0.0286(7) Uani 1 1 d . . . H3 H 0.6433 0.3052 -0.0967 0.034 Uiso 1 1 calc R . . C4 C 0.5614(3) 0.47604(18) -0.00384(17) 0.0165(5) Uani 1 1 d . . . C5 C 0.9822(3) 0.5309(2) 0.23250(18) 0.0206(6) Uani 1 1 d . . . C6 C 0.4974(3) 0.8289(2) 0.19939(19) 0.0220(6) Uani 1 1 d . . . C7 C 1.0974(3) 0.4046(2) 0.15645(19) 0.0247(6) Uani 1 1 d . . . C8 C 1.2637(3) 0.5377(2) 0.25203(19) 0.0241(6) Uani 1 1 d . . . C9 C 0.9835(4) 0.3683(2) 0.2833(2) 0.0302(7) Uani 1 1 d . . . C10 C 0.4013(4) 0.8937(3) 0.3239(2) 0.0377(8) Uani 1 1 d . . . C11 C 0.5256(4) 1.0085(2) 0.2420(2) 0.0337(7) Uani 1 1 d . . . C12 C 0.2247(3) 0.8267(2) 0.1732(2) 0.0239(6) Uani 1 1 d . . . C13 C 1.3270(4) 0.3096(2) 0.2708(2) 0.0337(7) Uani 1 1 d . . . H13 H 1.2951 0.3014 0.2125 0.040 Uiso 1 1 calc R . . C14 C 1.4299(5) 0.2566(3) 0.3105(3) 0.0488(11) Uani 1 1 d . . . H14 H 1.4645 0.2134 0.2790 0.059 Uiso 1 1 calc R . . C15 C 1.4794(6) 0.2687(4) 0.3964(4) 0.0700(17) Uani 1 1 d . . . H15 H 1.5475 0.2335 0.4234 0.084 Uiso 1 1 calc R . . C16 C 1.4268(5) 0.3346(4) 0.4432(3) 0.0635(15) Uani 1 1 d . . . C17 C 1.3222(4) 0.3846(3) 0.3983(2) 0.0398(9) Uani 1 1 d . . . C18 C 1.4727(7) 0.3568(7) 0.5333(4) 0.101(3) Uani 1 1 d . . . H18 H 1.5417 0.3252 0.5647 0.122 Uiso 1 1 calc R . . C19 C 1.4173(7) 0.4221(7) 0.5724(3) 0.105(3) Uani 1 1 d . . . H19 H 1.4494 0.4348 0.6304 0.126 Uiso 1 1 calc R . . C20 C 1.3114(6) 0.4722(5) 0.5280(3) 0.0690(17) Uani 1 1 d . . . C21 C 1.2646(4) 0.4529(3) 0.4402(2) 0.0411(9) Uani 1 1 d . . . C22 C 1.1090(4) 0.5620(3) 0.4282(2) 0.0389(8) Uani 1 1 d . . . H22 H 1.0412 0.5930 0.3951 0.047 Uiso 1 1 calc R . . C23 C 1.1483(6) 0.5855(4) 0.5154(3) 0.0592(13) Uani 1 1 d . . . H23 H 1.1059 0.6308 0.5393 0.071 Uiso 1 1 calc R . . C24 C 1.2479(6) 0.5421(5) 0.5643(3) 0.082(2) Uani 1 1 d . . . H24 H 1.2750 0.5581 0.6220 0.099 Uiso 1 1 calc R . . C25 C 0.1948(4) 1.0461(3) 0.2781(3) 0.0435(9) Uani 1 1 d . . . H25 H 0.2288 1.0253 0.3304 0.052 Uiso 1 1 calc R . . C26 C 0.0969(5) 1.1113(3) 0.2699(3) 0.0518(11) Uani 1 1 d . . . H26 H 0.0671 1.1328 0.3163 0.062 Uiso 1 1 calc R . . C27 C 0.0457(4) 1.1432(3) 0.1933(3) 0.0478(11) Uani 1 1 d . . . H27 H -0.0193 1.1860 0.1875 0.057 Uiso 1 1 calc R . . C28 C 0.0922(4) 1.1108(2) 0.1238(3) 0.0381(8) Uani 1 1 d . . . C29 C 0.1906(3) 1.0458(2) 0.1375(2) 0.0312(7) Uani 1 1 d . . . C30 C 0.0470(4) 1.1377(3) 0.0405(3) 0.0442(10) Uani 1 1 d . . . H30 H -0.0177 1.1806 0.0304 0.053 Uiso 1 1 calc R . . C31 C 0.0945(4) 1.1032(3) -0.0233(3) 0.0409(9) Uani 1 1 d . . . H31 H 0.0620 1.1222 -0.0766 0.049 Uiso 1 1 calc R . . C32 C 0.1952(4) 1.0370(2) -0.0106(3) 0.0338(8) Uani 1 1 d . . . C33 C 0.2417(3) 1.0097(2) 0.0703(2) 0.0284(7) Uani 1 1 d . . . C34 C 0.3868(3) 0.9113(2) 0.0278(2) 0.0284(7) Uani 1 1 d . . . H34 H 0.4521 0.8691 0.0402 0.034 Uiso 1 1 calc R . . C35 C 0.3450(4) 0.9345(3) -0.0549(2) 0.0352(8) Uani 1 1 d . . . H35 H 0.3818 0.9075 -0.0964 0.042 Uiso 1 1 calc R . . C36 C 0.2495(4) 0.9973(3) -0.0744(3) 0.0369(8) Uani 1 1 d . . . H36 H 0.2212 1.0133 -0.1291 0.044 Uiso 1 1 calc R . . N1 N 0.6826(2) 0.51394(16) 0.03960(15) 0.0187(5) Uani 1 1 d . . . N1A N 0.6126(3) 0.7474(2) -0.0399(2) 0.0325(6) Uani 1 1 d . . . N2 N 0.5409(2) 0.39875(17) -0.05288(16) 0.0201(5) Uani 1 1 d . . . N3 N 0.8919(3) 0.57392(18) 0.20747(17) 0.0238(5) Uani 1 1 d . . . N4 N 0.5672(3) 0.77236(18) 0.18868(17) 0.0239(5) Uani 1 1 d . . . N5 N 1.0854(3) 0.3725(2) 0.08923(18) 0.0342(7) Uani 1 1 d . . . N6 N 1.3507(3) 0.5835(2) 0.2410(2) 0.0353(7) Uani 1 1 d . . . N7 N 0.8944(4) 0.3212(2) 0.2882(3) 0.0497(9) Uani 1 1 d . . . N8 N 0.4183(5) 0.8792(3) 0.3930(2) 0.0611(11) Uani 1 1 d . . . N9 N 0.6174(4) 1.0600(2) 0.2617(3) 0.0503(9) Uani 1 1 d . . . N10 N 0.1377(3) 0.77263(19) 0.14818(19) 0.0299(6) Uani 1 1 d . . . N11 N 1.2729(3) 0.37124(19) 0.31321(17) 0.0263(5) Uani 1 1 d . . . N12 N 1.1651(3) 0.4973(2) 0.39152(16) 0.0281(6) Uani 1 1 d . . . N13 N 0.2400(3) 1.01341(19) 0.2134(2) 0.0321(6) Uani 1 1 d . . . N14 N 0.3365(3) 0.94743(17) 0.08935(18) 0.0251(5) Uani 1 1 d . . . O1A O 0.6360(3) 0.78328(19) 0.03589(16) 0.0368(6) Uani 1 1 d . . . O1W O 0.8926(2) 0.67956(15) 0.06887(14) 0.0244(4) Uani 1 1 d . . . O2A O 0.6285(3) 0.66553(18) -0.0486(2) 0.0449(7) Uani 1 1 d . . . O3W O 0.8586(2) 0.76564(17) 0.22893(17) 0.0345(6) Uani 1 1 d . . . O3A O 0.5776(4) 0.7934(2) -0.09849(18) 0.0532(8) Uani 1 1 d . . . O2W O 0.6168(2) 0.58029(18) 0.22141(16) 0.0324(5) Uani 1 1 d . . . O7W O 0.8582(5) 0.9389(3) 0.2877(3) 0.0895(15) Uani 1 1 d . . . O6W O 0.7980(6) 1.1862(3) 0.3735(2) 0.0905(16) Uani 1 1 d . . . O4W O 0.6211(4) 0.3976(2) 0.2022(3) 0.0695(11) Uani 1 1 d . . . O8W O 1.0652(6) 0.9896(4) 0.4367(3) 0.0986(15) Uani 1 1 d . . . O5W O 1.1067(4) 0.7312(3) 0.3268(2) 0.0685(11) Uani 1 1 d . . . O9W O 0.7916(9) 1.1588(5) 0.5313(4) 0.0635(19) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.01213(7) 0.01763(8) 0.01826(8) -0.00335(5) 0.00330(5) 0.00136(5) Fe1 0.01665(19) 0.0242(2) 0.01401(19) 0.00033(15) 0.00424(15) 0.00363(15) Fe2 0.0211(2) 0.0198(2) 0.0280(2) -0.00542(17) 0.00600(17) 0.00393(16) C1 0.0135(13) 0.0290(15) 0.0258(15) -0.0056(12) 0.0014(11) 0.0046(11) C2 0.0147(14) 0.0360(17) 0.0369(18) -0.0134(14) 0.0018(12) 0.0084(12) C3 0.0187(14) 0.0273(15) 0.0345(17) -0.0137(13) 0.0019(12) 0.0059(12) C4 0.0138(13) 0.0182(12) 0.0167(12) -0.0006(10) 0.0030(10) 0.0029(10) C5 0.0186(13) 0.0259(14) 0.0172(13) -0.0021(11) 0.0057(11) 0.0011(11) C6 0.0202(14) 0.0225(14) 0.0217(14) -0.0033(11) 0.0044(11) -0.0009(11) C7 0.0173(14) 0.0355(17) 0.0206(14) 0.0001(12) 0.0033(11) 0.0082(12) C8 0.0182(14) 0.0321(16) 0.0211(14) 0.0042(12) 0.0023(11) 0.0055(12) C9 0.0332(18) 0.0298(16) 0.0305(17) -0.0035(13) 0.0155(14) 0.0018(13) C10 0.040(2) 0.041(2) 0.0320(19) -0.0058(15) 0.0107(15) 0.0121(16) C11 0.0331(18) 0.0244(16) 0.0397(19) -0.0062(14) 0.0045(15) 0.0034(13) C12 0.0221(14) 0.0244(14) 0.0256(15) 0.0002(12) 0.0068(12) 0.0088(12) C13 0.0303(17) 0.0355(18) 0.0380(19) 0.0063(15) 0.0113(15) 0.0111(14) C14 0.044(2) 0.051(2) 0.058(3) 0.021(2) 0.019(2) 0.027(2) C15 0.058(3) 0.100(4) 0.065(3) 0.042(3) 0.021(3) 0.052(3) C16 0.050(3) 0.108(4) 0.038(2) 0.030(3) 0.008(2) 0.040(3) C17 0.0339(19) 0.063(3) 0.0241(17) 0.0135(17) 0.0052(14) 0.0152(18) C18 0.075(4) 0.195(9) 0.038(3) 0.040(4) 0.003(3) 0.066(5) C19 0.076(4) 0.210(9) 0.023(2) 0.015(4) -0.003(2) 0.057(5) C20 0.057(3) 0.125(5) 0.0194(19) 0.000(2) 0.0012(19) 0.021(3) C21 0.036(2) 0.068(3) 0.0186(16) 0.0047(16) 0.0036(14) 0.0101(18) C22 0.049(2) 0.044(2) 0.0231(17) -0.0076(15) 0.0123(16) 0.0040(17) C23 0.069(3) 0.078(3) 0.029(2) -0.020(2) 0.018(2) 0.004(3) C24 0.071(4) 0.148(6) 0.018(2) -0.022(3) 0.003(2) 0.014(4) C25 0.046(2) 0.040(2) 0.046(2) -0.0080(17) 0.0154(18) 0.0157(17) C26 0.054(3) 0.042(2) 0.063(3) -0.012(2) 0.026(2) 0.018(2) C27 0.040(2) 0.0304(19) 0.075(3) -0.0032(19) 0.019(2) 0.0151(16) C28 0.0295(18) 0.0209(15) 0.064(3) 0.0014(15) 0.0121(17) 0.0059(13) C29 0.0244(16) 0.0199(14) 0.048(2) -0.0003(13) 0.0077(14) 0.0031(12) C30 0.0310(19) 0.0254(17) 0.075(3) 0.0135(18) 0.0075(19) 0.0094(14) C31 0.0325(19) 0.0300(18) 0.060(3) 0.0178(17) 0.0065(18) 0.0075(15) C32 0.0267(17) 0.0244(16) 0.049(2) 0.0112(15) 0.0055(15) 0.0008(13) C33 0.0217(15) 0.0187(14) 0.0428(19) 0.0028(13) 0.0048(13) 0.0010(11) C34 0.0269(16) 0.0263(15) 0.0333(17) 0.0051(13) 0.0090(13) 0.0051(12) C35 0.0350(19) 0.0359(18) 0.0363(19) 0.0061(15) 0.0110(15) 0.0026(15) C36 0.0346(19) 0.0341(18) 0.042(2) 0.0129(15) 0.0069(16) 0.0005(15) N1 0.0142(11) 0.0206(11) 0.0194(11) -0.0030(9) 0.0021(9) 0.0028(9) N1A 0.0306(15) 0.0382(16) 0.0355(16) 0.0127(13) 0.0167(13) 0.0132(12) N2 0.0142(11) 0.0218(12) 0.0220(12) -0.0052(9) 0.0026(9) 0.0035(9) N3 0.0177(12) 0.0300(13) 0.0228(13) -0.0013(10) 0.0042(10) 0.0038(10) N4 0.0223(12) 0.0236(12) 0.0244(13) -0.0041(10) 0.0051(10) 0.0034(10) N5 0.0265(14) 0.0536(19) 0.0206(13) -0.0061(12) 0.0038(11) 0.0130(13) N6 0.0239(14) 0.0447(17) 0.0384(17) 0.0139(14) 0.0065(12) 0.0012(12) N7 0.056(2) 0.0382(18) 0.063(2) -0.0067(16) 0.035(2) -0.0084(16) N8 0.077(3) 0.073(3) 0.036(2) 0.0032(19) 0.0163(19) 0.027(2) N9 0.046(2) 0.0367(18) 0.061(2) -0.0073(16) 0.0041(17) -0.0086(15) N10 0.0234(14) 0.0296(14) 0.0351(15) -0.0012(12) 0.0055(12) 0.0025(11) N11 0.0238(13) 0.0314(14) 0.0249(13) 0.0070(11) 0.0059(10) 0.0076(11) N12 0.0306(14) 0.0363(15) 0.0165(12) -0.0009(11) 0.0053(11) 0.0007(12) N13 0.0291(15) 0.0251(13) 0.0415(17) -0.0074(12) 0.0106(13) 0.0066(11) N14 0.0219(13) 0.0204(12) 0.0324(14) 0.0016(10) 0.0058(11) 0.0023(10) O1A 0.0383(14) 0.0473(15) 0.0301(13) 0.0105(11) 0.0148(11) 0.0161(12) O1W 0.0192(10) 0.0328(12) 0.0213(10) -0.0034(9) 0.0079(8) -0.0012(8) O2A 0.0412(15) 0.0319(14) 0.067(2) 0.0054(13) 0.0233(14) 0.0074(11) O3W 0.0245(12) 0.0340(13) 0.0382(14) -0.0173(10) 0.0027(10) -0.0015(10) O3A 0.076(2) 0.0582(19) 0.0315(15) 0.0195(13) 0.0171(15) 0.0280(17) O2W 0.0220(11) 0.0453(14) 0.0343(13) 0.0159(11) 0.0109(10) 0.0077(10) O7W 0.088(3) 0.053(2) 0.108(4) -0.024(2) -0.002(3) 0.012(2) O6W 0.133(4) 0.081(3) 0.043(2) -0.0002(18) 0.007(2) -0.064(3) O4W 0.063(2) 0.0458(19) 0.092(3) 0.0125(19) 0.005(2) -0.0052(16) O8W 0.100(4) 0.112(4) 0.086(3) 0.003(3) 0.030(3) 0.006(3) O5W 0.049(2) 0.090(3) 0.060(2) 0.030(2) -0.0037(16) -0.0138(18) O9W 0.083(5) 0.074(5) 0.029(3) -0.003(3) 0.010(3) -0.014(4) _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 O3W 2.347(2) . ? Gd1 O1W 2.347(2) . ? Gd1 O2W 2.383(2) . ? Gd1 O1A 2.455(3) . ? Gd1 N4 2.485(3) . ? Gd1 N3 2.510(3) . ? Gd1 N1 2.566(2) . ? Gd1 N2 2.614(2) 2_665 ? Gd1 O2A 2.838(3) . ? Fe1 C7 1.909(3) . ? Fe1 C5 1.912(3) . ? Fe1 C8 1.948(3) . ? Fe1 C9 1.950(4) . ? Fe1 N12 1.985(3) . ? Fe1 N11 1.995(3) . ? Fe2 C6 1.905(3) . ? Fe2 C10 1.917(4) . ? Fe2 C11 1.942(4) . ? Fe2 C12 1.950(3) . ? Fe2 N14 1.997(3) . ? Fe2 N13 1.998(3) . ? C1 N1 1.345(4) . ? C1 C2 1.368(4) . ? C2 C3 1.376(4) . ? C3 N2 1.341(4) . ? C4 N1 1.336(4) . ? C4 N2 1.336(4) . ? C4 C4 1.486(5) 2_665 ? C5 N3 1.148(4) . ? C6 N4 1.154(4) . ? C7 N5 1.147(4) . ? C8 N6 1.156(4) . ? C9 N7 1.148(5) . ? C10 N8 1.149(6) . ? C11 N9 1.149(5) . ? C12 N10 1.147(4) . ? C13 N11 1.330(4) . ? C13 C14 1.397(5) . ? C14 C15 1.373(8) . ? C15 C16 1.406(8) . ? C16 C17 1.410(5) . ? C16 C18 1.446(8) . ? C17 N11 1.362(5) . ? C17 C21 1.413(6) . ? C18 C19 1.345(11) . ? C19 C20 1.417(8) . ? C20 C21 1.408(5) . ? C20 C24 1.418(9) . ? C21 N12 1.355(5) . ? C22 N12 1.321(5) . ? C22 C23 1.403(5) . ? C23 C24 1.348(8) . ? C25 N13 1.327(5) . ? C25 C26 1.409(6) . ? C26 C27 1.372(7) . ? C27 C28 1.402(6) . ? C28 C29 1.410(5) . ? C28 C30 1.431(6) . ? C29 N13 1.364(5) . ? C29 C33 1.413(5) . ? C30 C31 1.337(7) . ? C31 C32 1.439(5) . ? C32 C33 1.400(5) . ? C32 C36 1.405(6) . ? C33 N14 1.362(4) . ? C34 N14 1.330(4) . ? C34 C35 1.400(5) . ? C35 C36 1.374(5) . ? N1A O3A 1.221(4) . ? N1A O2A 1.245(4) . ? N1A O1A 1.280(4) . ? N2 Gd1 2.614(2) 2_665 ? 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 C7 Fe1 C5 87.87(13) . . ? C7 Fe1 C8 88.24(14) . . ? C5 Fe1 C8 92.35(13) . . ? C7 Fe1 C9 89.25(14) . . ? C5 Fe1 C9 86.34(14) . . ? C8 Fe1 C9 177.22(14) . . ? C7 Fe1 N12 175.90(13) . . ? C5 Fe1 N12 96.21(12) . . ? C8 Fe1 N12 91.88(13) . . ? C9 Fe1 N12 90.71(13) . . ? C7 Fe1 N11 93.36(12) . . ? C5 Fe1 N11 178.17(12) . . ? C8 Fe1 N11 89.04(12) . . ? C9 Fe1 N11 92.32(14) . . ? N12 Fe1 N11 82.55(12) . . ? C6 Fe2 C10 86.39(14) . . ? C6 Fe2 C11 89.68(14) . . ? C10 Fe2 C11 89.94(18) . . ? C6 Fe2 C12 88.22(12) . . ? C10 Fe2 C12 91.04(16) . . ? C11 Fe2 C12 177.62(14) . . ? C6 Fe2 N14 95.66(12) . . ? C10 Fe2 N14 177.67(14) . . ? C11 Fe2 N14 91.18(14) . . ? C12 Fe2 N14 87.92(12) . . ? C6 Fe2 N13 177.42(13) . . ? C10 Fe2 N13 96.03(15) . . ? C11 Fe2 N13 91.20(14) . . ? C12 Fe2 N13 90.85(12) . . ? N14 Fe2 N13 81.90(12) . . ? O3W Gd1 O1W 77.74(8) . . ? O3W Gd1 O2W 99.44(10) . . ? O1W Gd1 O2W 143.29(8) . . ? O3W Gd1 O1A 91.70(10) . . ? O1W Gd1 O1A 78.31(8) . . ? O2W Gd1 O1A 138.29(8) . . ? O3W Gd1 N4 72.70(9) . . ? O1W Gd1 N4 134.40(8) . . ? O2W Gd1 N4 76.40(9) . . ? O1A Gd1 N4 68.83(9) . . ? O3W Gd1 N3 73.54(9) . . ? O1W Gd1 N3 72.83(8) . . ? O2W Gd1 N3 71.36(8) . . ? O1A Gd1 N3 149.71(9) . . ? N4 Gd1 N3 127.87(9) . . ? O3W Gd1 N1 144.91(8) . . ? O1W Gd1 N1 79.11(8) . . ? O2W Gd1 N1 83.94(9) . . ? O1A Gd1 N1 108.98(9) . . ? N4 Gd1 N1 140.75(8) . . ? N3 Gd1 N1 74.63(8) . . ? O3W Gd1 N2 151.04(8) . 2_665 ? O1W Gd1 N2 126.85(8) . 2_665 ? O2W Gd1 N2 70.38(8) . 2_665 ? O1A Gd1 N2 80.54(9) . 2_665 ? N4 Gd1 N2 78.50(8) . 2_665 ? N3 Gd1 N2 124.58(8) . 2_665 ? N1 Gd1 N2 62.88(8) . 2_665 ? O3W Gd1 O2A 128.72(9) . . ? O1W Gd1 O2A 66.47(8) . . ? O2W Gd1 O2A 131.20(9) . . ? O1A Gd1 O2A 47.10(8) . . ? N4 Gd1 O2A 107.68(8) . . ? N3 Gd1 O2A 124.42(8) . . ? N1 Gd1 O2A 62.07(8) . . ? N2 Gd1 O2A 63.40(8) 2_665 . ? N1 C1 C2 121.6(3) . . ? C1 C2 C3 117.9(3) . . ? N2 C3 C2 121.7(3) . . ? N1 C4 N2 125.8(2) . . ? N1 C4 C4 116.9(3) . 2_665 ? N2 C4 C4 117.3(3) . 2_665 ? N3 C5 Fe1 176.6(3) . . ? N4 C6 Fe2 175.7(3) . . ? N5 C7 Fe1 176.6(3) . . ? N6 C8 Fe1 175.9(3) . . ? N7 C9 Fe1 176.2(4) . . ? N8 C10 Fe2 179.4(4) . . ? N9 C11 Fe2 178.7(3) . . ? N10 C12 Fe2 176.7(3) . . ? N11 C13 C14 122.4(4) . . ? C15 C14 C13 119.5(4) . . ? C14 C15 C16 119.7(4) . . ? C15 C16 C17 117.2(4) . . ? C15 C16 C18 125.6(5) . . ? C17 C16 C18 117.2(5) . . ? N11 C17 C16 122.6(4) . . ? N11 C17 C21 116.4(3) . . ? C16 C17 C21 121.0(4) . . ? C19 C18 C16 121.3(5) . . ? C18 C19 C20 121.9(5) . . ? C21 C20 C19 118.5(5) . . ? C21 C20 C24 116.0(5) . . ? C19 C20 C24 125.5(5) . . ? N12 C21 C20 123.3(4) . . ? N12 C21 C17 116.6(3) . . ? C20 C21 C17 120.1(4) . . ? N12 C22 C23 122.3(4) . . ? C24 C23 C22 119.7(5) . . ? C23 C24 C20 120.2(4) . . ? N13 C25 C26 122.0(4) . . ? C27 C26 C25 120.0(4) . . ? C26 C27 C28 119.5(4) . . ? C27 C28 C29 117.0(4) . . ? C27 C28 C30 125.3(4) . . ? C29 C28 C30 117.7(4) . . ? N13 C29 C28 123.4(4) . . ? N13 C29 C33 116.4(3) . . ? C28 C29 C33 120.2(4) . . ? C31 C30 C28 122.2(3) . . ? C30 C31 C32 120.9(4) . . ? C33 C32 C36 117.6(3) . . ? C33 C32 C31 118.1(4) . . ? C36 C32 C31 124.3(4) . . ? N14 C33 C32 123.0(3) . . ? N14 C33 C29 116.1(3) . . ? C32 C33 C29 120.8(3) . . ? N14 C34 C35 122.5(3) . . ? C36 C35 C34 119.7(4) . . ? C35 C36 C32 119.1(4) . . ? C4 N1 C1 116.5(2) . . ? C4 N1 Gd1 122.42(18) . . ? C1 N1 Gd1 120.92(19) . . ? O3A N1A O2A 123.9(3) . . ? O3A N1A O1A 119.9(3) . . ? O2A N1A O1A 116.2(3) . . ? C4 N2 C3 116.4(2) . . ? C4 N2 Gd1 120.47(18) . 2_665 ? C3 N2 Gd1 123.06(19) . 2_665 ? C5 N3 Gd1 170.0(2) . . ? C6 N4 Gd1 165.2(3) . . ? C13 N11 C17 118.6(3) . . ? C13 N11 Fe1 129.4(2) . . ? C17 N11 Fe1 112.0(2) . . ? C22 N12 C21 118.5(3) . . ? C22 N12 Fe1 129.0(3) . . ? C21 N12 Fe1 112.5(2) . . ? C25 N13 C29 118.1(3) . . ? C25 N13 Fe2 129.2(3) . . ? C29 N13 Fe2 112.7(2) . . ? C34 N14 C33 118.1(3) . . ? C34 N14 Fe2 129.0(2) . . ? C33 N14 Fe2 112.9(2) . . ? N1A O1A Gd1 107.3(2) . . ? N1A O2A Gd1 89.4(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.174 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.107 # Attachment 'compound31.cif' data_compound31 _database_code_depnum_ccdc_archive 'CCDC 764599' #TrackingRef 'compound31.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H66 Dy2 Fe4 N30 O20' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Brown _diffrn_ambient_temperature 293(2) _chemical_formula_weight 2219.95 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' O O 0.0106 0.0060 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0660(10) _cell_length_b 15.0110(13) _cell_length_c 16.5870(7) _cell_angle_alpha 94.664(5) _cell_angle_beta 104.432(6) _cell_angle_gamma 92.157(10) _cell_volume 2414.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.189 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48282 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 6.44 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10873 _reflns_number_gt 9647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+2.6588P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10873 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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 Dy1 Dy 0.706791(12) 0.662685(8) 0.128405(8) 0.02593(5) Uani 1 1 d . . . Fe1 Fe 1.12671(4) 0.45350(3) 0.27006(2) 0.02956(9) Uani 1 1 d . . . Fe2 Fe 0.37405(4) 0.91557(3) 0.20791(3) 0.03742(11) Uani 1 1 d . . . C1 C 0.7943(3) 0.4718(2) 0.0304(2) 0.0366(7) Uani 1 1 d . . . H1 H 0.8812 0.4958 0.0594 0.044 Uiso 1 1 calc R . . C2 C 0.7829(3) 0.3941(2) -0.0207(2) 0.0487(9) Uani 1 1 d . . . H2 H 0.8605 0.3656 -0.0274 0.058 Uiso 1 1 calc R . . C3 C 0.6537(3) 0.3596(2) -0.0618(2) 0.0443(8) Uani 1 1 d . . . H3 H 0.6439 0.3068 -0.0967 0.053 Uiso 1 1 calc R . . C4 C 0.5616(3) 0.47620(18) -0.00405(16) 0.0250(5) Uani 1 1 d . . . C5 C 0.9832(3) 0.5315(2) 0.23151(18) 0.0319(6) Uani 1 1 d . . . C6 C 0.4985(3) 0.8255(2) 0.19687(19) 0.0339(6) Uani 1 1 d . . . C7 C 1.0994(3) 0.4047(2) 0.15674(19) 0.0392(7) Uani 1 1 d . . . C8 C 1.2664(3) 0.5374(2) 0.25195(19) 0.0389(7) Uani 1 1 d . . . C9 C 0.9844(4) 0.3684(2) 0.2830(2) 0.0455(8) Uani 1 1 d . . . C10 C 0.3990(4) 0.8879(3) 0.3215(3) 0.0570(10) Uani 1 1 d . . . C11 C 0.5264(4) 1.0052(3) 0.2427(3) 0.0531(9) Uani 1 1 d . . . C12 C 0.2228(3) 0.8241(2) 0.1716(2) 0.0376(7) Uani 1 1 d . . . C13 C 1.3268(4) 0.3087(3) 0.2717(3) 0.0520(9) Uani 1 1 d . . . H13 H 1.2958 0.3007 0.2137 0.062 Uiso 1 1 calc R . . C14 C 1.4282(5) 0.2551(4) 0.3120(4) 0.0757(14) Uani 1 1 d . . . H14 H 1.4635 0.2117 0.2811 0.091 Uiso 1 1 calc R . . C15 C 1.4752(6) 0.2667(5) 0.3970(4) 0.096(2) Uani 1 1 d . . . H15 H 1.5418 0.2305 0.4243 0.115 Uiso 1 1 calc R . . C16 C 1.4237(5) 0.3327(4) 0.4431(3) 0.0815(16) Uani 1 1 d . . . C17 C 1.3203(4) 0.3838(3) 0.3982(2) 0.0530(9) Uani 1 1 d . . . C18 C 1.4668(7) 0.3546(7) 0.5323(4) 0.126(3) Uani 1 1 d . . . H18 H 1.5342 0.3222 0.5642 0.151 Uiso 1 1 calc R . . C19 C 1.4118(8) 0.4209(7) 0.5707(4) 0.133(3) Uani 1 1 d . . . H19 H 1.4434 0.4334 0.6283 0.160 Uiso 1 1 calc R . . C20 C 1.3081(6) 0.4719(5) 0.5264(3) 0.0899(18) Uani 1 1 d . . . C21 C 1.2631(4) 0.4521(3) 0.4386(2) 0.0554(10) Uani 1 1 d . . . C22 C 1.1107(5) 0.5642(3) 0.4257(2) 0.0600(10) Uani 1 1 d . . . H22 H 1.0450 0.5967 0.3924 0.072 Uiso 1 1 calc R . . C23 C 1.1497(7) 0.5867(4) 0.5128(3) 0.0885(17) Uani 1 1 d . . . H23 H 1.1085 0.6328 0.5366 0.106 Uiso 1 1 calc R . . C24 C 1.2453(7) 0.5421(5) 0.5611(3) 0.107(2) Uani 1 1 d . . . H24 H 1.2710 0.5575 0.6185 0.128 Uiso 1 1 calc R . . C25 C 0.1932(5) 1.0403(3) 0.2778(3) 0.0727(13) Uani 1 1 d . . . H25 H 0.2249 1.0175 0.3291 0.087 Uiso 1 1 calc R . . C26 C 0.0965(6) 1.1068(4) 0.2696(5) 0.0895(18) Uani 1 1 d . . . H26 H 0.0662 1.1282 0.3157 0.107 Uiso 1 1 calc R . . C27 C 0.0471(5) 1.1396(3) 0.1942(5) 0.0871(18) Uani 1 1 d . . . H27 H -0.0176 1.1827 0.1888 0.104 Uiso 1 1 calc R . . C28 C 0.0940(4) 1.1083(3) 0.1250(4) 0.0666(13) Uani 1 1 d . . . C29 C 0.1915(4) 1.0435(2) 0.1381(3) 0.0522(9) Uani 1 1 d . . . C30 C 0.0500(5) 1.1365(3) 0.0432(4) 0.0746(15) Uani 1 1 d . . . H30 H -0.0148 1.1795 0.0336 0.090 Uiso 1 1 calc R . . C31 C 0.0988(5) 1.1033(3) -0.0205(4) 0.0728(14) Uani 1 1 d . . . H31 H 0.0673 1.1238 -0.0729 0.087 Uiso 1 1 calc R . . C32 C 0.1984(4) 1.0368(3) -0.0094(3) 0.0571(10) Uani 1 1 d . . . C33 C 0.2435(4) 1.0084(2) 0.0713(3) 0.0478(8) Uani 1 1 d . . . C34 C 0.3866(4) 0.9103(3) 0.0274(2) 0.0487(8) Uani 1 1 d . . . H34 H 0.4508 0.8670 0.0387 0.058 Uiso 1 1 calc R . . C35 C 0.3464(5) 0.9352(3) -0.0531(3) 0.0606(10) Uani 1 1 d . . . H35 H 0.3836 0.9088 -0.0946 0.073 Uiso 1 1 calc R . . C36 C 0.2523(5) 0.9984(3) -0.0721(3) 0.0637(11) Uani 1 1 d . . . H36 H 0.2250 1.0153 -0.1262 0.076 Uiso 1 1 calc R . . O1A O 0.6325(3) 0.7742(2) 0.03321(17) 0.0592(7) Uani 1 1 d . . . O1W O 0.8896(2) 0.67771(15) 0.06751(13) 0.0372(5) Uani 1 1 d . . . O2A O 0.6223(4) 0.6621(2) -0.0562(3) 0.0779(10) Uani 1 1 d . . . O2W O 0.6196(2) 0.58135(18) 0.22032(15) 0.0479(6) Uani 1 1 d . . . O3A O 0.5748(4) 0.7921(3) -0.0977(2) 0.0839(11) Uani 1 1 d . . . O3W O 0.8567(2) 0.76589(18) 0.22356(17) 0.0552(7) Uani 1 1 d . . . O4W O 0.6237(5) 0.3997(3) 0.2081(3) 0.1033(13) Uani 1 1 d . . . O5W O 1.1053(5) 0.7452(5) 0.3333(3) 0.141(2) Uani 1 1 d . . . O6W O 0.8146(7) 1.1790(4) 0.3749(3) 0.138(2) Uani 1 1 d . . . O7W O 0.8479(8) 0.9274(5) 0.3010(7) 0.242(5) Uani 1 1 d . . . N1 N 0.6836(2) 0.51394(16) 0.03965(14) 0.0285(5) Uani 1 1 d . . . N1A N 0.6077(3) 0.7427(2) -0.0431(2) 0.0526(8) Uani 1 1 d . . . N2 N 0.5411(2) 0.39979(16) -0.05326(15) 0.0309(5) Uani 1 1 d . . . N3 N 0.8935(3) 0.57462(19) 0.20620(16) 0.0382(6) Uani 1 1 d . . . N4 N 0.5680(3) 0.76965(18) 0.18611(17) 0.0373(6) Uani 1 1 d . . . N5 N 1.0877(3) 0.3733(3) 0.09014(18) 0.0571(9) Uani 1 1 d . . . N6 N 1.3539(3) 0.5823(3) 0.2421(2) 0.0593(9) Uani 1 1 d . . . N7 N 0.8990(5) 0.3207(3) 0.2901(3) 0.0796(12) Uani 1 1 d . . . N8 N 0.4120(6) 0.8720(4) 0.3883(3) 0.0951(15) Uani 1 1 d . . . N9 N 0.6158(5) 1.0569(3) 0.2634(3) 0.0856(13) Uani 1 1 d . . . N10 N 0.1347(3) 0.7717(2) 0.1469(2) 0.0499(7) Uani 1 1 d . . . N11 N 1.2733(3) 0.3709(2) 0.31350(17) 0.0407(6) Uani 1 1 d . . . N12 N 1.1655(3) 0.4981(2) 0.39013(16) 0.0416(6) Uani 1 1 d . . . N13 N 0.2400(3) 1.0099(2) 0.2128(2) 0.0522(8) Uani 1 1 d . . . N14 N 0.3376(3) 0.94541(18) 0.08934(19) 0.0421(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01868(7) 0.02691(7) 0.03057(7) -0.00451(5) 0.00534(5) 0.00238(4) Fe1 0.0260(2) 0.0391(2) 0.02383(18) 0.00199(16) 0.00622(15) 0.00720(16) Fe2 0.0292(2) 0.0302(2) 0.0500(3) -0.00960(18) 0.00838(19) 0.00432(17) C1 0.0189(13) 0.0421(17) 0.0429(16) -0.0121(13) 0.0013(11) 0.0064(11) C2 0.0225(15) 0.053(2) 0.062(2) -0.0251(17) 0.0024(14) 0.0115(13) C3 0.0273(15) 0.0432(18) 0.0549(19) -0.0219(15) 0.0033(13) 0.0095(13) C4 0.0207(12) 0.0267(13) 0.0266(12) -0.0005(10) 0.0045(10) 0.0038(10) C5 0.0262(14) 0.0400(16) 0.0297(14) -0.0001(11) 0.0079(11) 0.0052(12) C6 0.0266(14) 0.0348(15) 0.0369(15) -0.0065(12) 0.0052(11) -0.0005(11) C7 0.0273(15) 0.058(2) 0.0314(15) -0.0006(13) 0.0051(12) 0.0148(13) C8 0.0289(15) 0.055(2) 0.0328(15) 0.0089(13) 0.0056(12) 0.0106(14) C9 0.0455(19) 0.0446(19) 0.0503(19) -0.0012(15) 0.0208(16) 0.0047(15) C10 0.050(2) 0.064(3) 0.053(2) -0.0152(19) 0.0109(17) 0.0116(18) C11 0.044(2) 0.0398(19) 0.070(2) -0.0112(17) 0.0093(17) 0.0008(15) C12 0.0300(15) 0.0356(16) 0.0463(17) -0.0018(13) 0.0088(13) 0.0083(12) C13 0.044(2) 0.055(2) 0.058(2) 0.0056(17) 0.0122(17) 0.0183(17) C14 0.064(3) 0.073(3) 0.095(4) 0.020(3) 0.020(3) 0.037(2) C15 0.073(3) 0.117(5) 0.108(4) 0.060(4) 0.021(3) 0.055(3) C16 0.067(3) 0.121(5) 0.060(3) 0.042(3) 0.006(2) 0.039(3) C17 0.045(2) 0.075(3) 0.0395(18) 0.0204(18) 0.0053(15) 0.0171(18) C18 0.092(5) 0.214(9) 0.070(4) 0.063(5) -0.005(3) 0.058(5) C19 0.111(5) 0.239(10) 0.039(3) 0.026(4) -0.013(3) 0.055(6) C20 0.080(3) 0.152(6) 0.030(2) 0.004(3) 0.002(2) 0.014(3) C21 0.051(2) 0.085(3) 0.0283(16) 0.0083(17) 0.0036(15) 0.0074(19) C22 0.075(3) 0.067(3) 0.0391(19) -0.0087(17) 0.0202(19) 0.010(2) C23 0.110(4) 0.109(4) 0.044(2) -0.027(3) 0.025(3) 0.009(3) C24 0.106(5) 0.172(7) 0.032(2) -0.024(3) 0.007(3) 0.013(5) C25 0.065(3) 0.064(3) 0.089(3) -0.021(2) 0.025(2) 0.020(2) C26 0.076(3) 0.078(4) 0.117(5) -0.028(3) 0.038(3) 0.025(3) C27 0.059(3) 0.051(3) 0.148(6) -0.016(3) 0.025(3) 0.022(2) C28 0.045(2) 0.0316(18) 0.121(4) -0.003(2) 0.018(2) 0.0099(16) C29 0.0357(18) 0.0282(16) 0.088(3) -0.0017(17) 0.0093(18) 0.0051(13) C30 0.049(2) 0.040(2) 0.131(5) 0.022(3) 0.008(3) 0.0137(18) C31 0.052(2) 0.051(2) 0.113(4) 0.033(3) 0.008(3) 0.0063(19) C32 0.042(2) 0.0381(19) 0.087(3) 0.0190(19) 0.0044(19) -0.0006(15) C33 0.0351(17) 0.0284(15) 0.077(2) 0.0054(15) 0.0079(16) 0.0006(13) C34 0.0442(19) 0.0448(19) 0.059(2) 0.0077(16) 0.0146(16) 0.0073(15) C35 0.059(2) 0.062(3) 0.064(2) 0.013(2) 0.019(2) 0.004(2) C36 0.059(3) 0.058(3) 0.072(3) 0.023(2) 0.009(2) -0.002(2) O1A 0.0569(17) 0.082(2) 0.0476(15) 0.0216(14) 0.0216(12) 0.0247(14) O1W 0.0287(10) 0.0481(13) 0.0349(11) -0.0040(9) 0.0116(8) -0.0032(9) O2A 0.071(2) 0.0506(18) 0.124(3) 0.0124(18) 0.044(2) 0.0150(15) O2W 0.0335(12) 0.0658(16) 0.0507(14) 0.0196(12) 0.0170(10) 0.0104(11) O3A 0.121(3) 0.084(2) 0.0508(17) 0.0285(16) 0.0197(18) 0.036(2) O3W 0.0357(13) 0.0547(15) 0.0636(16) -0.0286(12) 0.0020(11) -0.0014(11) O4W 0.092(3) 0.066(2) 0.143(4) 0.017(2) 0.013(3) -0.003(2) O5W 0.095(3) 0.192(6) 0.122(4) 0.055(4) -0.003(3) -0.031(4) O6W 0.186(5) 0.117(4) 0.094(3) -0.002(3) 0.018(3) -0.069(4) O7W 0.152(6) 0.154(6) 0.349(12) -0.137(7) -0.024(7) 0.047(5) N1 0.0189(10) 0.0313(12) 0.0324(12) -0.0044(9) 0.0029(9) 0.0043(9) N1A 0.0474(18) 0.061(2) 0.059(2) 0.0225(16) 0.0247(15) 0.0191(15) N2 0.0216(11) 0.0308(12) 0.0364(12) -0.0090(10) 0.0036(9) 0.0043(9) N3 0.0278(13) 0.0477(15) 0.0383(14) 0.0008(11) 0.0070(11) 0.0062(11) N4 0.0330(13) 0.0349(13) 0.0418(14) -0.0059(11) 0.0077(11) 0.0070(11) N5 0.0443(17) 0.090(3) 0.0340(15) -0.0102(15) 0.0062(13) 0.0198(16) N6 0.0378(17) 0.078(2) 0.065(2) 0.0222(18) 0.0136(15) 0.0006(16) N7 0.081(3) 0.062(2) 0.107(3) -0.005(2) 0.051(3) -0.014(2) N8 0.108(4) 0.119(4) 0.059(3) 0.002(3) 0.021(2) 0.020(3) N9 0.069(3) 0.062(2) 0.112(3) -0.016(2) 0.009(2) -0.021(2) N10 0.0351(15) 0.0464(17) 0.0634(19) -0.0047(14) 0.0073(13) -0.0008(13) N11 0.0338(14) 0.0482(16) 0.0403(14) 0.0087(12) 0.0071(11) 0.0118(12) N12 0.0445(16) 0.0527(17) 0.0278(12) -0.0007(11) 0.0109(11) 0.0024(13) N13 0.0409(16) 0.0363(15) 0.077(2) -0.0142(14) 0.0154(15) 0.0077(12) N14 0.0318(14) 0.0321(13) 0.0599(17) 0.0021(12) 0.0074(12) 0.0030(10) _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 Dy1 O1W 2.321(2) . ? Dy1 O3W 2.326(2) . ? Dy1 O2W 2.340(2) . ? Dy1 O1A 2.406(3) . ? Dy1 N4 2.456(2) . ? Dy1 N3 2.490(3) . ? Dy1 N1 2.542(2) . ? Dy1 N2 2.597(2) 2_665 ? Fe1 C7 1.910(3) . ? Fe1 C5 1.912(3) . ? Fe1 C9 1.946(4) . ? Fe1 C8 1.947(4) . ? Fe1 N12 1.986(3) . ? Fe1 N11 1.997(3) . ? Fe2 C6 1.906(3) . ? Fe2 C10 1.920(5) . ? Fe2 C11 1.943(4) . ? Fe2 C12 1.954(3) . ? Fe2 N14 2.000(3) . ? Fe2 N13 2.003(3) . ? C1 N1 1.338(3) . ? C1 C2 1.368(4) . ? C1 H1 0.9300 . ? C2 C3 1.370(4) . ? C2 H2 0.9300 . ? C3 N2 1.336(4) . ? C3 H3 0.9300 . ? C4 N2 1.331(3) . ? C4 N1 1.338(3) . ? C4 C4 1.483(5) 2_665 ? C5 N3 1.144(4) . ? C6 N4 1.142(4) . ? C7 N5 1.141(4) . ? C8 N6 1.141(5) . ? C9 N7 1.134(5) . ? C10 N8 1.128(6) . ? C11 N9 1.130(5) . ? C12 N10 1.134(4) . ? C13 N11 1.327(5) . ? C13 C14 1.395(6) . ? C13 H13 0.9300 . ? C14 C15 1.366(8) . ? C14 H14 0.9300 . ? C15 C16 1.397(8) . ? C15 H15 0.9300 . ? C16 C17 1.412(5) . ? C16 C18 1.440(9) . ? C17 N11 1.360(5) . ? C17 C21 1.399(6) . ? C18 C19 1.348(11) . ? C18 H18 0.9300 . ? C19 C20 1.409(9) . ? C19 H19 0.9300 . ? C20 C24 1.404(9) . ? C20 C21 1.416(5) . ? C21 N12 1.354(5) . ? C22 N12 1.322(5) . ? C22 C23 1.409(6) . ? C22 H22 0.9300 . ? C23 C24 1.330(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N13 1.334(6) . ? C25 C26 1.411(7) . ? C25 H25 0.9300 . ? C26 C27 1.365(9) . ? C26 H26 0.9300 . ? C27 C28 1.399(8) . ? C27 H27 0.9300 . ? C28 C29 1.399(5) . ? C28 C30 1.423(8) . ? C29 N13 1.359(6) . ? C29 C33 1.413(6) . ? C30 C31 1.341(8) . ? C30 H30 0.9300 . ? C31 C32 1.431(6) . ? C31 H31 0.9300 . ? C32 C36 1.385(7) . ? C32 C33 1.408(6) . ? C33 N14 1.361(4) . ? C34 N14 1.327(5) . ? C34 C35 1.383(6) . ? C34 H34 0.9300 . ? C35 C36 1.365(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O1A N1A 1.274(4) . ? O2A N1A 1.234(4) . ? O3A N1A 1.207(4) . ? N2 Dy1 2.597(2) 2_665 ? 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 O1W Dy1 O3W 77.52(9) . . ? O1W Dy1 O2W 143.86(8) . . ? O3W Dy1 O2W 100.09(10) . . ? O1W Dy1 O1A 77.70(9) . . ? O3W Dy1 O1A 92.12(11) . . ? O2W Dy1 O1A 138.24(9) . . ? O1W Dy1 N4 133.87(9) . . ? O3W Dy1 N4 72.24(9) . . ? O2W Dy1 N4 76.41(9) . . ? O1A Dy1 N4 69.61(9) . . ? O1W Dy1 N3 73.09(8) . . ? O3W Dy1 N3 74.23(10) . . ? O2W Dy1 N3 71.65(9) . . ? O1A Dy1 N3 149.76(9) . . ? N4 Dy1 N3 127.96(9) . . ? O1W Dy1 N1 78.57(8) . . ? O3W Dy1 N1 145.59(8) . . ? O2W Dy1 N1 85.18(9) . . ? O1A Dy1 N1 106.52(9) . . ? N4 Dy1 N1 141.14(8) . . ? N3 Dy1 N1 75.36(8) . . ? O1W Dy1 N2 126.30(7) . 2_665 ? O3W Dy1 N2 150.57(8) . 2_665 ? O2W Dy1 N2 71.21(8) . 2_665 ? O1A Dy1 N2 78.65(10) . 2_665 ? N4 Dy1 N2 78.36(8) . 2_665 ? N3 Dy1 N2 125.62(9) . 2_665 ? N1 Dy1 N2 63.28(7) . 2_665 ? C7 Fe1 C5 87.91(13) . . ? C7 Fe1 C9 89.47(15) . . ? C5 Fe1 C9 87.05(14) . . ? C7 Fe1 C8 88.13(15) . . ? C5 Fe1 C8 92.29(13) . . ? C9 Fe1 C8 177.54(14) . . ? C7 Fe1 N12 175.88(13) . . ? C5 Fe1 N12 96.21(12) . . ? C9 Fe1 N12 90.70(14) . . ? C8 Fe1 N12 91.73(13) . . ? C7 Fe1 N11 93.45(12) . . ? C5 Fe1 N11 177.95(12) . . ? C9 Fe1 N11 91.42(14) . . ? C8 Fe1 N11 89.29(13) . . ? N12 Fe1 N11 82.43(12) . . ? C6 Fe2 C10 87.06(15) . . ? C6 Fe2 C11 90.26(14) . . ? C10 Fe2 C11 90.28(19) . . ? C6 Fe2 C12 88.77(12) . . ? C10 Fe2 C12 90.22(17) . . ? C11 Fe2 C12 178.89(15) . . ? C6 Fe2 N14 95.37(12) . . ? C10 Fe2 N14 176.97(15) . . ? C11 Fe2 N14 91.52(16) . . ? C12 Fe2 N14 88.02(13) . . ? C6 Fe2 N13 176.92(14) . . ? C10 Fe2 N13 95.89(16) . . ? C11 Fe2 N13 90.62(14) . . ? C12 Fe2 N13 90.32(13) . . ? N14 Fe2 N13 81.66(13) . . ? N1 C1 C2 121.6(3) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C1 C2 C3 117.9(3) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? N2 C3 C2 121.8(3) . . ? N2 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? N2 C4 N1 125.9(2) . . ? N2 C4 C4 117.4(3) . 2_665 ? N1 C4 C4 116.7(3) . 2_665 ? N3 C5 Fe1 176.6(3) . . ? N4 C6 Fe2 176.1(3) . . ? N5 C7 Fe1 177.1(3) . . ? N6 C8 Fe1 175.7(3) . . ? N7 C9 Fe1 178.1(4) . . ? N8 C10 Fe2 179.1(4) . . ? N9 C11 Fe2 179.4(5) . . ? N10 C12 Fe2 176.9(3) . . ? N11 C13 C14 122.0(4) . . ? N11 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 119.5(5) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 117.1(4) . . ? C15 C16 C18 126.3(5) . . ? C17 C16 C18 116.6(6) . . ? N11 C17 C21 116.5(3) . . ? N11 C17 C16 122.1(4) . . ? C21 C17 C16 121.4(4) . . ? C19 C18 C16 121.7(5) . . ? C19 C18 H18 119.2 . . ? C16 C18 H18 119.2 . . ? C18 C19 C20 122.1(5) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C24 C20 C19 126.0(5) . . ? C24 C20 C21 116.3(5) . . ? C19 C20 C21 117.7(6) . . ? N12 C21 C17 117.2(3) . . ? N12 C21 C20 122.3(4) . . ? C17 C21 C20 120.5(4) . . ? N12 C22 C23 121.5(5) . . ? N12 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 120.0(5) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C20 120.8(4) . . ? C23 C24 H24 119.6 . . ? C20 C24 H24 119.6 . . ? N13 C25 C26 120.9(5) . . ? N13 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 120.2(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.0(4) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 116.6(5) . . ? C29 C28 C30 117.9(5) . . ? C27 C28 C30 125.4(4) . . ? N13 C29 C28 123.6(4) . . ? N13 C29 C33 116.3(3) . . ? C28 C29 C33 120.0(4) . . ? C31 C30 C28 122.3(4) . . ? C31 C30 H30 118.8 . . ? C28 C30 H30 118.8 . . ? C30 C31 C32 121.3(5) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C36 C32 C33 118.1(4) . . ? C36 C32 C31 124.8(4) . . ? C33 C32 C31 117.2(5) . . ? N14 C33 C32 122.5(4) . . ? N14 C33 C29 116.2(4) . . ? C32 C33 C29 121.3(3) . . ? N14 C34 C35 122.8(4) . . ? N14 C34 H34 118.6 . . ? C35 C34 H34 118.6 . . ? C36 C35 C34 120.3(4) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C32 118.8(4) . . ? C35 C36 H36 120.6 . . ? C32 C36 H36 120.6 . . ? N1A O1A Dy1 112.5(2) . . ? C1 N1 C4 116.3(2) . . ? C1 N1 Dy1 121.23(18) . . ? C4 N1 Dy1 122.32(17) . . ? O3A N1A O2A 123.8(4) . . ? O3A N1A O1A 119.7(4) . . ? O2A N1A O1A 116.5(3) . . ? C4 N2 C3 116.3(2) . . ? C4 N2 Dy1 120.27(17) . 2_665 ? C3 N2 Dy1 123.39(19) . 2_665 ? C5 N3 Dy1 170.6(2) . . ? C6 N4 Dy1 165.8(3) . . ? C13 N11 C17 119.1(3) . . ? C13 N11 Fe1 129.1(2) . . ? C17 N11 Fe1 111.8(2) . . ? C22 N12 C21 119.1(3) . . ? C22 N12 Fe1 128.8(3) . . ? C21 N12 Fe1 112.1(2) . . ? C25 N13 C29 118.7(4) . . ? C25 N13 Fe2 128.5(3) . . ? C29 N13 Fe2 112.8(2) . . ? C34 N14 C33 117.5(3) . . ? C34 N14 Fe2 129.5(2) . . ? C33 N14 Fe2 112.9(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.220 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.087 # Attachment 'compound41.cif' data_compound41 _database_code_depnum_ccdc_archive 'CCDC 764600' #TrackingRef 'compound41.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H66 Fe4 Ho2 N30 O20' _chemical_melting_point ? _exptl_crystal_description Prism _exptl_crystal_colour Brown _diffrn_ambient_temperature 293(2) _chemical_formula_weight 2224.81 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' O O 0.0106 0.0060 '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' 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0450(9) _cell_length_b 15.0130(10) _cell_length_c 16.6290(15) _cell_angle_alpha 95.024(4) _cell_angle_beta 104.536(4) _cell_angle_gamma 92.254(5) _cell_volume 2413.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1106 _exptl_absorpt_coefficient_mu 2.282 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11811 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.66 _reflns_number_total 11811 _reflns_number_gt 10259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_cell_refinement 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+8.8625P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11811 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.2029 _refine_ls_wR_factor_gt 0.1900 _refine_ls_goodness_of_fit_ref 1.302 _refine_ls_restrained_S_all 1.302 _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 0.70695(3) 0.66328(2) 0.128648(19) 0.02730(12) Uani 1 1 d . . . Fe1 Fe 1.12703(11) 0.45569(7) 0.26945(6) 0.0327(2) Uani 1 1 d . . . Fe2 Fe 0.37547(12) 0.91725(8) 0.20678(8) 0.0409(3) Uani 1 1 d . . . C1 C 0.7957(7) 0.4728(5) 0.0296(5) 0.0386(17) Uani 1 1 d . . . H1 H 0.8831 0.4970 0.0581 0.046 Uiso 1 1 calc R . . C2 C 0.7829(8) 0.3946(6) -0.0218(7) 0.056(3) Uani 1 1 d . . . H2 H 0.8605 0.3660 -0.0283 0.067 Uiso 1 1 calc R . . C3 C 0.6570(8) 0.3606(6) -0.0622(6) 0.047(2) Uani 1 1 d . . . H3 H 0.6481 0.3080 -0.0975 0.056 Uiso 1 1 calc R . . C4 C 0.5628(7) 0.4769(4) -0.0037(4) 0.0278(14) Uani 1 1 d . . . C5 C 0.9823(8) 0.5337(5) 0.2309(5) 0.0357(16) Uani 1 1 d . . . C6 C 0.4991(7) 0.8276(5) 0.1960(5) 0.0351(16) Uani 1 1 d . . . C7 C 1.1008(8) 0.4076(6) 0.1563(5) 0.0397(17) Uani 1 1 d . . . C8 C 1.2675(8) 0.5408(6) 0.2537(5) 0.0407(18) Uani 1 1 d . . . C9 C 0.9828(10) 0.3705(6) 0.2808(6) 0.0457(19) Uani 1 1 d . . . C10 C 0.4011(11) 0.8908(8) 0.3189(7) 0.063(3) Uani 1 1 d . . . C11 C 0.5295(10) 1.0077(6) 0.2426(7) 0.056(2) Uani 1 1 d . . . C12 C 0.2236(8) 0.8257(6) 0.1702(6) 0.0429(19) Uani 1 1 d . . . C13 C 1.3286(10) 0.3111(7) 0.2713(7) 0.056(2) Uani 1 1 d . . . H13 H 1.2983 0.3021 0.2134 0.067 Uiso 1 1 calc R . . C14 C 1.4303(12) 0.2589(8) 0.3122(9) 0.073(3) Uani 1 1 d . . . H14 H 1.4696 0.2172 0.2819 0.088 Uiso 1 1 calc R . . C15 C 1.4720(15) 0.2693(11) 0.3974(11) 0.104(5) Uani 1 1 d . . . H15 H 1.5339 0.2307 0.4249 0.125 Uiso 1 1 calc R . . C16 C 1.4242(13) 0.3359(10) 0.4436(7) 0.082(4) Uani 1 1 d . . . C17 C 1.3188(10) 0.3860(7) 0.3974(6) 0.054(2) Uani 1 1 d . . . C18 C 1.4634(17) 0.3552(16) 0.5292(10) 0.128(7) Uani 1 1 d . . . H18 H 1.5305 0.3223 0.5605 0.153 Uiso 1 1 calc R . . C19 C 1.4079(18) 0.4200(17) 0.5689(9) 0.140(8) Uani 1 1 d . . . H19 H 1.4392 0.4311 0.6266 0.168 Uiso 1 1 calc R . . C20 C 1.3033(15) 0.4719(13) 0.5258(7) 0.099(5) Uani 1 1 d . . . C21 C 1.2604(10) 0.4546(8) 0.4389(5) 0.057(3) Uani 1 1 d . . . C22 C 1.1071(12) 0.5656(8) 0.4247(6) 0.063(3) Uani 1 1 d . . . H22 H 1.0393 0.5967 0.3917 0.075 Uiso 1 1 calc R . . C23 C 1.1488(17) 0.5891(12) 0.5124(7) 0.100(5) Uani 1 1 d . . . H23 H 1.1088 0.6361 0.5358 0.120 Uiso 1 1 calc R . . C24 C 1.2417(17) 0.5463(14) 0.5603(8) 0.115(6) Uani 1 1 d . . . H24 H 1.2689 0.5637 0.6173 0.138 Uiso 1 1 calc R . . C25 C 0.1945(12) 1.0428(8) 0.2759(8) 0.074(3) Uani 1 1 d . . . H25 H 0.2258 1.0214 0.3278 0.089 Uiso 1 1 calc R . . C26 C 0.0950(15) 1.1100(9) 0.2645(12) 0.098(5) Uani 1 1 d . . . H26 H 0.0632 1.1318 0.3099 0.118 Uiso 1 1 calc R . . C27 C 0.0471(14) 1.1420(8) 0.1920(12) 0.092(5) Uani 1 1 d . . . H27 H -0.0165 1.1859 0.1865 0.110 Uiso 1 1 calc R . . C28 C 0.0944(10) 1.1082(7) 0.1233(9) 0.071(3) Uani 1 1 d . . . C29 C 0.1935(9) 1.0444(6) 0.1367(7) 0.051(2) Uani 1 1 d . . . C30 C 0.0487(12) 1.1383(7) 0.0436(10) 0.077(4) Uani 1 1 d . . . H30 H -0.0152 1.1820 0.0350 0.092 Uiso 1 1 calc R . . C31 C 0.0977(12) 1.1037(8) -0.0204(10) 0.081(4) Uani 1 1 d . . . H31 H 0.0649 1.1237 -0.0727 0.097 Uiso 1 1 calc R . . C32 C 0.1994(11) 1.0368(7) -0.0109(8) 0.061(3) Uani 1 1 d . . . C33 C 0.2454(9) 1.0087(6) 0.0695(7) 0.051(2) Uani 1 1 d . . . C34 C 0.3865(10) 0.9103(7) 0.0274(6) 0.053(2) Uani 1 1 d . . . H34 H 0.4499 0.8667 0.0395 0.064 Uiso 1 1 calc R . . C35 C 0.3484(11) 0.9329(7) -0.0550(8) 0.066(3) Uani 1 1 d . . . H35 H 0.3857 0.9063 -0.0963 0.079 Uiso 1 1 calc R . . C36 C 0.2505(12) 0.9981(8) -0.0718(9) 0.072(3) Uani 1 1 d . . . H36 H 0.2210 1.0146 -0.1258 0.086 Uiso 1 1 calc R . . O1A O 0.6305(8) 0.7720(5) 0.0324(4) 0.0642(19) Uani 1 1 d . . . O1W O 0.8885(5) 0.6783(4) 0.0677(3) 0.0404(12) Uani 1 1 d . . . O2A O 0.6165(9) 0.6596(6) -0.0613(6) 0.083(3) Uani 1 1 d . . . O2W O 0.6211(6) 0.5846(5) 0.2209(4) 0.0499(15) Uani 1 1 d . . . O3A O 0.5719(11) 0.7897(6) -0.0974(5) 0.086(3) Uani 1 1 d . . . O3W O 0.8583(7) 0.7666(4) 0.2234(4) 0.0581(17) Uani 1 1 d . . . O4W O 0.6246(10) 0.4028(6) 0.2098(8) 0.104(3) Uani 1 1 d . . . O5W O 1.1065(12) 0.7454(9) 0.3332(8) 0.129(5) Uani 1 1 d . . . O6W O 0.8146(14) 1.1837(8) 0.3732(7) 0.130(5) Uani 1 1 d . . . O7W O 0.8493(17) 0.9292(11) 0.2970(14) 0.230(11) Uani 1 1 d . . . N1 N 0.6855(6) 0.5150(4) 0.0395(4) 0.0314(13) Uani 1 1 d . . . N1A N 0.6033(9) 0.7397(6) -0.0458(5) 0.056(2) Uani 1 1 d . . . N2 N 0.5411(6) 0.3999(4) -0.0536(4) 0.0320(13) Uani 1 1 d . . . N3 N 0.8937(7) 0.5760(5) 0.2052(4) 0.0404(15) Uani 1 1 d . . . N4 N 0.5694(7) 0.7714(4) 0.1855(4) 0.0389(15) Uani 1 1 d . . . N5 N 1.0888(8) 0.3766(6) 0.0889(5) 0.058(2) Uani 1 1 d . . . N6 N 1.3556(8) 0.5859(6) 0.2449(5) 0.060(2) Uani 1 1 d . . . N7 N 0.8964(11) 0.3212(7) 0.2867(7) 0.079(3) Uani 1 1 d . . . N8 N 0.4134(15) 0.8742(10) 0.3861(8) 0.102(4) Uani 1 1 d . . . N9 N 0.6191(11) 1.0595(7) 0.2621(8) 0.092(4) Uani 1 1 d . . . N10 N 0.1337(8) 0.7732(5) 0.1458(5) 0.0511(18) Uani 1 1 d . . . N11 N 1.2734(7) 0.3733(5) 0.3120(4) 0.0410(15) Uani 1 1 d . . . N12 N 1.1637(7) 0.5000(5) 0.3896(4) 0.0425(16) Uani 1 1 d . . . N13 N 0.2414(8) 1.0112(5) 0.2110(6) 0.056(2) Uani 1 1 d . . . N14 N 0.3390(7) 0.9461(4) 0.0886(5) 0.0437(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01958(17) 0.02817(18) 0.03275(18) -0.00350(12) 0.00607(12) 0.00307(11) Fe1 0.0274(5) 0.0435(6) 0.0275(5) 0.0026(4) 0.0069(4) 0.0089(4) Fe2 0.0309(6) 0.0339(6) 0.0553(7) -0.0094(5) 0.0103(5) 0.0050(4) C1 0.020(3) 0.044(4) 0.046(4) -0.011(3) 0.001(3) 0.005(3) C2 0.022(4) 0.055(5) 0.081(7) -0.028(5) 0.004(4) 0.014(4) C3 0.026(4) 0.043(4) 0.064(5) -0.022(4) 0.006(4) 0.007(3) C4 0.022(3) 0.027(3) 0.032(3) -0.003(3) 0.007(3) 0.002(3) C5 0.030(4) 0.043(4) 0.033(4) -0.001(3) 0.008(3) -0.001(3) C6 0.026(3) 0.035(4) 0.042(4) -0.007(3) 0.009(3) 0.001(3) C7 0.026(4) 0.052(5) 0.043(4) 0.005(4) 0.010(3) 0.011(3) C8 0.028(4) 0.057(5) 0.039(4) 0.012(4) 0.008(3) 0.011(4) C9 0.049(5) 0.044(5) 0.047(5) -0.005(4) 0.022(4) -0.003(4) C10 0.050(6) 0.076(7) 0.057(6) -0.020(5) 0.008(5) 0.011(5) C11 0.043(5) 0.037(5) 0.081(7) -0.012(4) 0.012(5) 0.000(4) C12 0.030(4) 0.042(4) 0.055(5) -0.009(4) 0.011(4) 0.008(3) C13 0.046(5) 0.060(6) 0.062(6) 0.002(5) 0.014(4) 0.019(4) C14 0.068(7) 0.065(7) 0.092(9) 0.021(6) 0.021(7) 0.033(6) C15 0.077(9) 0.119(12) 0.125(13) 0.067(10) 0.017(9) 0.062(9) C16 0.066(7) 0.128(11) 0.054(6) 0.039(7) 0.006(5) 0.041(8) C17 0.045(5) 0.076(7) 0.042(5) 0.021(5) 0.006(4) 0.019(5) C18 0.093(11) 0.22(2) 0.074(10) 0.068(12) 0.000(8) 0.060(13) C19 0.102(12) 0.27(3) 0.038(7) 0.031(11) -0.010(7) 0.058(15) C20 0.085(9) 0.167(15) 0.037(6) 0.014(8) 0.001(6) 0.011(10) C21 0.051(5) 0.087(7) 0.028(4) 0.010(4) -0.002(4) 0.003(5) C22 0.076(7) 0.073(7) 0.042(5) -0.006(5) 0.023(5) 0.015(6) C23 0.117(12) 0.136(13) 0.041(6) -0.034(7) 0.025(7) 0.007(10) C24 0.105(12) 0.194(19) 0.036(6) -0.023(9) 0.007(7) 0.024(12) C25 0.065(7) 0.068(7) 0.091(9) -0.014(6) 0.028(6) 0.026(6) C26 0.079(9) 0.074(9) 0.145(15) -0.041(9) 0.050(10) 0.024(7) C27 0.068(8) 0.053(7) 0.150(15) -0.012(8) 0.024(9) 0.026(6) C28 0.034(5) 0.051(6) 0.124(11) -0.006(6) 0.020(6) 0.004(4) C29 0.032(4) 0.031(4) 0.087(7) -0.001(4) 0.011(4) 0.004(3) C30 0.057(7) 0.043(6) 0.128(12) 0.021(7) 0.012(7) 0.016(5) C31 0.055(7) 0.050(6) 0.128(12) 0.032(7) -0.002(7) 0.000(5) C32 0.047(5) 0.045(5) 0.088(8) 0.017(5) 0.012(5) 0.001(4) C33 0.032(4) 0.032(4) 0.086(7) 0.010(4) 0.011(4) 0.003(3) C34 0.048(5) 0.051(5) 0.062(6) 0.005(4) 0.018(4) 0.007(4) C35 0.057(6) 0.062(6) 0.085(8) 0.021(6) 0.023(6) 0.002(5) C36 0.063(7) 0.063(7) 0.091(9) 0.032(6) 0.016(6) -0.004(5) O1A 0.060(4) 0.090(5) 0.052(4) 0.028(4) 0.023(3) 0.029(4) O1W 0.031(3) 0.050(3) 0.040(3) -0.006(2) 0.013(2) -0.001(2) O2A 0.083(6) 0.061(5) 0.121(7) 0.027(5) 0.046(5) 0.019(4) O2W 0.032(3) 0.072(4) 0.052(4) 0.021(3) 0.017(3) 0.010(3) O3A 0.122(8) 0.090(6) 0.052(4) 0.030(4) 0.021(5) 0.039(6) O3W 0.043(3) 0.052(4) 0.067(4) -0.025(3) 0.003(3) -0.006(3) O4W 0.085(7) 0.074(6) 0.145(9) 0.019(6) 0.015(6) -0.004(5) O5W 0.088(7) 0.162(11) 0.124(9) 0.046(8) -0.001(7) -0.036(7) O6W 0.165(12) 0.106(8) 0.100(8) -0.010(6) 0.018(8) -0.063(8) O7W 0.141(13) 0.152(13) 0.33(3) -0.152(16) 0.003(14) 0.019(10) N1 0.020(3) 0.036(3) 0.035(3) -0.005(2) 0.003(2) 0.007(2) N1A 0.052(5) 0.062(5) 0.061(5) 0.018(4) 0.023(4) 0.017(4) N2 0.024(3) 0.034(3) 0.036(3) -0.007(2) 0.007(2) 0.006(2) N3 0.030(3) 0.050(4) 0.042(4) 0.003(3) 0.009(3) 0.009(3) N4 0.035(3) 0.038(3) 0.042(4) -0.006(3) 0.011(3) 0.007(3) N5 0.042(4) 0.092(6) 0.037(4) -0.004(4) 0.006(3) 0.023(4) N6 0.037(4) 0.083(6) 0.062(5) 0.024(4) 0.012(4) 0.001(4) N7 0.073(7) 0.059(6) 0.110(8) -0.011(5) 0.039(6) -0.011(5) N8 0.116(10) 0.127(11) 0.064(7) 0.005(7) 0.023(7) 0.026(8) N9 0.068(7) 0.068(6) 0.124(10) -0.011(6) 0.005(6) -0.025(5) N10 0.037(4) 0.050(4) 0.065(5) 0.000(4) 0.012(4) 0.000(3) N11 0.032(3) 0.052(4) 0.040(4) 0.009(3) 0.007(3) 0.011(3) N12 0.042(4) 0.055(4) 0.030(3) 0.002(3) 0.010(3) 0.003(3) N13 0.042(4) 0.044(4) 0.081(6) -0.018(4) 0.018(4) 0.010(3) N14 0.037(4) 0.032(3) 0.063(5) 0.007(3) 0.013(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O1W 2.310(5) . ? Ho1 O3W 2.321(6) . ? Ho1 O2W 2.323(6) . ? Ho1 O1A 2.399(7) . ? Ho1 N4 2.450(6) . ? Ho1 N3 2.478(7) . ? Ho1 N1 2.534(6) . ? Ho1 N2 2.590(6) 2_665 ? Fe1 C7 1.904(8) . ? Fe1 C5 1.921(8) . ? Fe1 C8 1.948(9) . ? Fe1 C9 1.950(9) . ? Fe1 N12 1.987(7) . ? Fe1 N11 1.991(7) . ? Fe2 C6 1.894(7) . ? Fe2 C10 1.896(12) . ? Fe2 C12 1.951(9) . ? Fe2 C11 1.955(9) . ? Fe2 N14 1.996(8) . ? Fe2 N13 1.997(7) . ? C1 N1 1.335(9) . ? C1 C2 1.372(11) . ? C1 H1 0.9300 . ? C2 C3 1.332(11) . ? C2 H2 0.9300 . ? C3 N2 1.358(9) . ? C3 H3 0.9300 . ? C4 N1 1.337(9) . ? C4 N2 1.341(9) . ? C4 C4 1.489(13) 2_665 ? C5 N3 1.132(10) . ? C6 N4 1.150(10) . ? C7 N5 1.151(11) . ? C8 N6 1.140(11) . ? C9 N7 1.146(12) . ? C10 N8 1.145(16) . ? C11 N9 1.129(13) . ? C12 N10 1.143(11) . ? C13 N11 1.325(12) . ? C13 C14 1.388(14) . ? C13 H13 0.9300 . ? C14 C15 1.36(2) . ? C14 H14 0.9300 . ? C15 C16 1.38(2) . ? C15 H15 0.9300 . ? C16 C18 1.38(2) . ? C16 C17 1.426(13) . ? C17 N11 1.372(11) . ? C17 C21 1.416(15) . ? C18 C19 1.34(3) . ? C18 H18 0.9300 . ? C19 C20 1.42(2) . ? C19 H19 0.9300 . ? C20 C21 1.398(14) . ? C20 C24 1.44(2) . ? C21 N12 1.353(12) . ? C22 N12 1.320(12) . ? C22 C23 1.421(15) . ? C22 H22 0.9300 . ? C23 C24 1.30(2) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 N13 1.339(14) . ? C25 C26 1.440(17) . ? C25 H25 0.9300 . ? C26 C27 1.32(2) . ? C26 H26 0.9300 . ? C27 C28 1.41(2) . ? C27 H27 0.9300 . ? C28 C29 1.400(13) . ? C28 C30 1.410(19) . ? C29 N13 1.354(14) . ? C29 C33 1.422(14) . ? C30 C31 1.35(2) . ? C30 H30 0.9300 . ? C31 C32 1.451(16) . ? C31 H31 0.9300 . ? C32 C36 1.345(17) . ? C32 C33 1.407(15) . ? C33 N14 1.356(11) . ? C34 N14 1.313(12) . ? C34 C35 1.402(15) . ? C34 H34 0.9300 . ? C35 C36 1.411(16) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O1A N1A 1.305(11) . ? O2A N1A 1.226(11) . ? O3A N1A 1.181(11) . ? N2 Ho1 2.590(6) 2_665 ? 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 O1W Ho1 O3W 77.3(2) . . ? O1W Ho1 O2W 144.3(2) . . ? O3W Ho1 O2W 99.6(3) . . ? O1W Ho1 O1A 77.6(2) . . ? O3W Ho1 O1A 93.1(3) . . ? O2W Ho1 O1A 138.0(2) . . ? O1W Ho1 N4 133.2(2) . . ? O3W Ho1 N4 72.3(2) . . ? O2W Ho1 N4 76.5(2) . . ? O1A Ho1 N4 69.5(2) . . ? O1W Ho1 N3 73.1(2) . . ? O3W Ho1 N3 74.2(2) . . ? O2W Ho1 N3 71.9(2) . . ? O1A Ho1 N3 149.9(2) . . ? N4 Ho1 N3 128.5(2) . . ? O1W Ho1 N1 77.95(19) . . ? O3W Ho1 N1 144.9(2) . . ? O2W Ho1 N1 86.4(2) . . ? O1A Ho1 N1 105.5(2) . . ? N4 Ho1 N1 142.0(2) . . ? N3 Ho1 N1 75.0(2) . . ? O1W Ho1 N2 126.10(19) . 2_665 ? O3W Ho1 N2 150.9(2) . 2_665 ? O2W Ho1 N2 71.6(2) . 2_665 ? O1A Ho1 N2 77.9(2) . 2_665 ? N4 Ho1 N2 78.7(2) . 2_665 ? N3 Ho1 N2 125.5(2) . 2_665 ? N1 Ho1 N2 63.69(18) . 2_665 ? C7 Fe1 C5 87.8(3) . . ? C7 Fe1 C8 88.6(4) . . ? C5 Fe1 C8 92.3(3) . . ? C7 Fe1 C9 89.6(4) . . ? C5 Fe1 C9 86.5(4) . . ? C8 Fe1 C9 177.9(4) . . ? C7 Fe1 N12 176.2(3) . . ? C5 Fe1 N12 95.9(3) . . ? C8 Fe1 N12 91.5(3) . . ? C9 Fe1 N12 90.4(3) . . ? C7 Fe1 N11 93.2(3) . . ? C5 Fe1 N11 178.0(3) . . ? C8 Fe1 N11 89.4(3) . . ? C9 Fe1 N11 91.8(4) . . ? N12 Fe1 N11 83.0(3) . . ? C6 Fe2 C10 86.8(4) . . ? C6 Fe2 C12 88.8(3) . . ? C10 Fe2 C12 90.5(4) . . ? C6 Fe2 C11 90.3(4) . . ? C10 Fe2 C11 89.8(5) . . ? C12 Fe2 C11 179.0(4) . . ? C6 Fe2 N14 95.4(3) . . ? C10 Fe2 N14 177.2(4) . . ? C12 Fe2 N14 87.9(3) . . ? C11 Fe2 N14 91.8(4) . . ? C6 Fe2 N13 176.7(4) . . ? C10 Fe2 N13 96.3(4) . . ? C12 Fe2 N13 90.2(3) . . ? C11 Fe2 N13 90.7(4) . . ? N14 Fe2 N13 81.5(3) . . ? N1 C1 C2 121.6(7) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 118.6(7) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 N2 122.5(7) . . ? C2 C3 H3 118.7 . . ? N2 C3 H3 118.7 . . ? N1 C4 N2 126.0(6) . . ? N1 C4 C4 118.1(7) . 2_665 ? N2 C4 C4 115.9(7) . 2_665 ? N3 C5 Fe1 176.4(7) . . ? N4 C6 Fe2 176.4(7) . . ? N5 C7 Fe1 177.5(7) . . ? N6 C8 Fe1 175.2(8) . . ? N7 C9 Fe1 178.8(10) . . ? N8 C10 Fe2 178.4(12) . . ? N9 C11 Fe2 178.9(12) . . ? N10 C12 Fe2 177.3(9) . . ? N11 C13 C14 122.2(10) . . ? N11 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C15 C14 C13 119.3(11) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 121.5(10) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C18 C16 C15 126.6(13) . . ? C18 C16 C17 117.6(13) . . ? C15 C16 C17 115.7(11) . . ? N11 C17 C21 117.1(8) . . ? N11 C17 C16 122.5(10) . . ? C21 C17 C16 120.3(9) . . ? C19 C18 C16 122.2(13) . . ? C19 C18 H18 118.9 . . ? C16 C18 H18 118.9 . . ? C18 C19 C20 122.3(13) . . ? C18 C19 H19 118.9 . . ? C20 C19 H19 118.9 . . ? C21 C20 C19 117.4(15) . . ? C21 C20 C24 114.8(13) . . ? C19 C20 C24 127.6(13) . . ? N12 C21 C20 123.9(11) . . ? N12 C21 C17 116.1(8) . . ? C20 C21 C17 120.1(11) . . ? N12 C22 C23 120.6(12) . . ? N12 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 121.2(14) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C20 120.6(12) . . ? C23 C24 H24 119.7 . . ? C20 C24 H24 119.7 . . ? N13 C25 C26 119.3(13) . . ? N13 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 122.5(13) . . ? C27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C26 C27 C28 118.5(11) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C29 C28 C27 117.6(13) . . ? C29 C28 C30 119.9(12) . . ? C27 C28 C30 122.4(12) . . ? N13 C29 C28 123.6(10) . . ? N13 C29 C33 116.6(8) . . ? C28 C29 C33 119.8(11) . . ? C31 C30 C28 120.0(10) . . ? C31 C30 H30 120.0 . . ? C28 C30 H30 120.0 . . ? C30 C31 C32 122.9(12) . . ? C30 C31 H31 118.6 . . ? C32 C31 H31 118.6 . . ? C36 C32 C33 117.6(10) . . ? C36 C32 C31 126.1(12) . . ? C33 C32 C31 116.3(12) . . ? N14 C33 C32 123.7(10) . . ? N14 C33 C29 115.2(9) . . ? C32 C33 C29 121.1(8) . . ? N14 C34 C35 124.7(10) . . ? N14 C34 H34 117.7 . . ? C35 C34 H34 117.7 . . ? C34 C35 C36 116.5(11) . . ? C34 C35 H35 121.8 . . ? C36 C35 H35 121.8 . . ? C32 C36 C35 120.9(11) . . ? C32 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? N1A O1A Ho1 113.7(6) . . ? C1 N1 C4 116.2(6) . . ? C1 N1 Ho1 122.1(5) . . ? C4 N1 Ho1 121.6(4) . . ? O3A N1A O2A 123.9(10) . . ? O3A N1A O1A 118.1(9) . . ? O2A N1A O1A 118.0(9) . . ? C4 N2 C3 115.1(6) . . ? C4 N2 Ho1 120.7(4) . 2_665 ? C3 N2 Ho1 124.3(5) . 2_665 ? C5 N3 Ho1 171.5(6) . . ? C6 N4 Ho1 166.0(7) . . ? C13 N11 C17 118.5(8) . . ? C13 N11 Fe1 130.4(6) . . ? C17 N11 Fe1 111.1(6) . . ? C22 N12 C21 118.8(8) . . ? C22 N12 Fe1 128.6(7) . . ? C21 N12 Fe1 112.6(6) . . ? C25 N13 C29 118.4(9) . . ? C25 N13 Fe2 128.6(8) . . ? C29 N13 Fe2 113.0(6) . . ? C34 N14 C33 116.7(9) . . ? C34 N14 Fe2 129.5(6) . . ? C33 N14 Fe2 113.7(7) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.66 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.527 _refine_diff_density_min -1.561 _refine_diff_density_rms 0.340