# Electronic Supplementary Material (ESI) for CrystEngComm # 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_dy-fe _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 Dy Fe N11 O3, 3(H2 O)' _chemical_formula_sum 'C27 H33 Dy Fe N11 O6' _chemical_formula_weight 825.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.411(3) _cell_length_b 13.323(3) _cell_length_c 15.828(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.087(3) _cell_angle_gamma 90.00 _cell_volume 3426.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.73 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 2.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6927 _exptl_absorpt_correction_T_max 0.7781 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23626 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6687 _reflns_number_gt 5907 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+4.0130P] 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 6687 _refine_ls_number_parameters 449 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4469(2) 0.7807(3) 1.0913(2) 0.0524(9) Uani 1 1 d . . . H1 H 0.4173 0.7223 1.0763 0.063 Uiso 1 1 calc R . . C2 C 0.5258(2) 0.7720(3) 1.1335(2) 0.0606(10) Uani 1 1 d . . . H2 H 0.5488 0.7093 1.1474 0.073 Uiso 1 1 calc R . . C3 C 0.5697(2) 0.8588(4) 1.1548(3) 0.0714(13) Uani 1 1 d . . . H3 H 0.6239 0.8553 1.1814 0.086 Uiso 1 1 calc R . . C4 C 0.5341(2) 0.9477(4) 1.1371(3) 0.0683(12) Uani 1 1 d . . . H4 H 0.5633 1.0061 1.1532 0.082 Uiso 1 1 calc R . . C5 C 0.45445(19) 0.9545(3) 1.0951(2) 0.0487(9) Uani 1 1 d . . . C6 C 0.4116(2) 1.0522(3) 1.0750(2) 0.0483(8) Uani 1 1 d . . . C7 C 0.4484(3) 1.1439(4) 1.1017(3) 0.0812(15) Uani 1 1 d . . . H7 H 0.5016 1.1457 1.1310 0.097 Uiso 1 1 calc R . . C8 C 0.4048(4) 1.2305(4) 1.0839(4) 0.0937(17) Uani 1 1 d . . . H8 H 0.4280 1.2917 1.1023 0.112 Uiso 1 1 calc R . . C9 C 0.3273(3) 1.2277(3) 1.0392(3) 0.0730(13) Uani 1 1 d . . . H9 H 0.2977 1.2867 1.0268 0.088 Uiso 1 1 calc R . . C10 C 0.2933(2) 1.1351(2) 1.0126(2) 0.0487(9) Uani 1 1 d . . . C11 C 0.2101(2) 1.1268(3) 0.9646(2) 0.0489(9) Uani 1 1 d . . . C12 C 0.1659(3) 1.2112(3) 0.9313(3) 0.0760(13) Uani 1 1 d . . . H12 H 0.1890 1.2749 0.9384 0.091 Uiso 1 1 calc R . . C13 C 0.0884(4) 1.1990(5) 0.8885(3) 0.0950(19) Uani 1 1 d . . . H13 H 0.0581 1.2543 0.8662 0.114 Uiso 1 1 calc R . . C14 C 0.0564(3) 1.1064(4) 0.8789(3) 0.0927(18) Uani 1 1 d . . . H14 H 0.0033 1.0970 0.8506 0.111 Uiso 1 1 calc R . . C15 C 0.1026(3) 1.0252(4) 0.9114(3) 0.0755(13) Uani 1 1 d . . . H15 H 0.0798 0.9614 0.9036 0.091 Uiso 1 1 calc R . . C16 C 0.27282(16) 0.5553(2) 1.28442(18) 0.0292(6) Uani 1 1 d . . . C17 C 0.22920(18) 0.3864(2) 1.19657(19) 0.0351(7) Uani 1 1 d . . . C18 C 0.20503(17) 0.4917(2) 1.04713(18) 0.0329(6) Uani 1 1 d . . . C19 C 0.25435(16) 0.6614(2) 1.12755(17) 0.0298(6) Uani 1 1 d . . . C20 C 0.12901(18) 0.5602(2) 1.18189(18) 0.0360(7) Uani 1 1 d . . . C21 C 0.35463(18) 0.5030(2) 1.15028(19) 0.0368(7) Uani 1 1 d . . . C22 C 0.0996(2) 0.7381(3) 0.9654(2) 0.0487(7) Uani 1 1 d U A . H22 H 0.1220 0.6970 1.0102 0.058 Uiso 1 1 calc R . . C23 C -0.0111(3) 0.7705(4) 0.8559(3) 0.1057(16) Uani 1 1 d U . . H23A H -0.0376 0.8285 0.8757 0.159 Uiso 1 1 calc R . . H23B H -0.0514 0.7293 0.8223 0.159 Uiso 1 1 calc R . . H23C H 0.0297 0.7915 0.8216 0.159 Uiso 1 1 calc R . . C24 C -0.0206(3) 0.6319(3) 0.9531(3) 0.0686(11) Uani 1 1 d U . . H24A H -0.0273 0.5817 0.9092 0.103 Uiso 1 1 calc R . . H24B H -0.0737 0.6557 0.9629 0.103 Uiso 1 1 calc R . . H24C H 0.0076 0.6033 1.0048 0.103 Uiso 1 1 calc R . . C25A C 0.3259(3) 0.6519(4) 0.9278(4) 0.0474(15) Uani 0.659(7) 1 d P A 1 H25 H 0.3093 0.6121 0.9705 0.057 Uiso 0.659(7) 1 calc PR A 1 C26A C 0.3838(4) 0.6544(7) 0.7971(4) 0.070(2) Uani 0.659(7) 1 d P A 1 H26A H 0.3517 0.6316 0.7452 0.105 Uiso 0.659(7) 1 calc PR A 1 H26B H 0.4408 0.6392 0.7958 0.105 Uiso 0.659(7) 1 calc PR A 1 H26C H 0.3772 0.7256 0.8025 0.105 Uiso 0.659(7) 1 calc PR A 1 C27A C 0.3646(5) 0.4922(5) 0.8715(7) 0.101(3) Uani 0.659(7) 1 d P A 1 H27D H 0.4211 0.4728 0.8726 0.151 Uiso 0.659(7) 1 calc PR A 1 H27E H 0.3318 0.4624 0.8229 0.151 Uiso 0.659(7) 1 calc PR A 1 H27F H 0.3452 0.4698 0.9227 0.151 Uiso 0.659(7) 1 calc PR A 1 C25B C 0.3271(5) 0.7032(8) 0.8704(6) 0.041(3) Uani 0.341(7) 1 d P A 2 H25A H 0.3135 0.7385 0.8197 0.049 Uiso 0.341(7) 1 calc PR A 2 C26B C 0.3760(8) 0.5787(12) 0.7777(7) 0.065(4) Uani 0.341(7) 1 d P A 2 H26D H 0.3471 0.5182 0.7594 0.098 Uiso 0.341(7) 1 calc PR A 2 H26E H 0.4341 0.5683 0.7796 0.098 Uiso 0.341(7) 1 calc PR A 2 H26F H 0.3584 0.6319 0.7383 0.098 Uiso 0.341(7) 1 calc PR A 2 C27B C 0.3839(8) 0.5498(10) 0.9354(8) 0.066(4) Uani 0.341(7) 1 d P A 2 H27A H 0.4425 0.5557 0.9494 0.100 Uiso 0.341(7) 1 calc PR A 2 H27B H 0.3695 0.4809 0.9236 0.100 Uiso 0.341(7) 1 calc PR A 2 H27C H 0.3580 0.5727 0.9827 0.100 Uiso 0.341(7) 1 calc PR A 2 Dy1 Dy 0.266983(8) 0.880793(9) 0.998592(8) 0.02708(5) Uani 1 1 d . . . Fe1 Fe 0.24092(2) 0.52583(3) 1.16542(2) 0.02549(9) Uani 1 1 d . . . N1 N 0.41112(15) 0.8684(2) 1.07070(17) 0.0395(6) Uani 1 1 d . . . N2 N 0.33551(16) 1.04821(19) 1.03129(16) 0.0381(6) Uani 1 1 d . . . N3 N 0.17869(18) 1.0341(2) 0.95360(18) 0.0486(7) Uani 1 1 d . . . N4 N 0.26160(15) 0.73901(19) 1.09753(15) 0.0360(6) Uani 1 1 d . . . N5 N 0.28894(16) 0.5702(2) 1.35635(16) 0.0381(6) Uani 1 1 d . . . N6 N 0.22467(19) 0.3035(2) 1.2130(2) 0.0544(8) Uani 1 1 d . . . N7 N 0.18326(17) 0.4725(2) 0.97707(17) 0.0479(7) Uani 1 1 d . . . N8 N 0.42155(18) 0.4914(3) 1.1397(2) 0.0659(9) Uani 1 1 d . . . N9 N 0.06350(18) 0.5828(3) 1.1912(2) 0.0584(8) Uani 1 1 d . . . N10 N 0.35761(18) 0.6069(2) 0.8653(2) 0.0491(7) Uani 1 1 d . . . N11 N 0.02714(16) 0.7149(2) 0.92676(19) 0.0500(6) Uani 1 1 d U . . O1 O 0.31728(16) 0.74244(18) 0.93257(15) 0.0520(6) Uani 1 1 d . . . O2 O 0.14146(14) 0.81015(19) 0.94777(16) 0.0547(6) Uani 1 1 d . . . O3 O 0.21898(16) 0.93552(17) 1.12093(15) 0.0532(6) Uani 1 1 d . . . H3A H 0.2357 0.9917 1.1422 0.064 Uiso 1 1 d R A . H3B H 0.1855 0.8999 1.1443 0.064 Uiso 1 1 d R . . O4 O 0.1526(2) 0.8335(3) 0.2424(2) 0.0999(12) Uani 1 1 d . . . H4A H 0.1154 0.7918 0.2321 0.120 Uiso 1 1 d R . . H4B H 0.1358 0.8845 0.2711 0.120 Uiso 1 1 d R . . O5 O 0.2016(3) 0.0987(2) 0.2033(3) 0.1158(17) Uani 1 1 d . . . H5A H 0.1703 0.0771 0.2378 0.139 Uiso 1 1 d R . . H5B H 0.2063 0.1619 0.2092 0.139 Uiso 1 1 d R . . O6 O 0.10168(14) 0.0132(2) 0.31038(14) 0.0552(6) Uani 1 1 d . . . H6A H 0.1272 0.0216 0.3631 0.066 Uiso 1 1 d R . . H6B H 0.0532 0.0379 0.3118 0.066 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0380(17) 0.052(2) 0.065(2) -0.0051(18) -0.0011(16) 0.0011(16) C2 0.0426(19) 0.072(3) 0.064(2) 0.002(2) -0.0015(17) 0.0152(19) C3 0.0351(18) 0.112(4) 0.063(2) -0.007(3) -0.0060(17) -0.003(2) C4 0.046(2) 0.093(4) 0.064(2) -0.013(2) 0.0008(18) -0.019(2) C5 0.0393(17) 0.068(3) 0.0396(17) -0.0106(17) 0.0098(13) -0.0176(16) C6 0.0533(19) 0.048(2) 0.0471(19) -0.0136(16) 0.0186(15) -0.0210(16) C7 0.070(3) 0.073(3) 0.101(4) -0.031(3) 0.012(3) -0.038(3) C8 0.108(4) 0.045(3) 0.132(5) -0.036(3) 0.034(4) -0.032(3) C9 0.094(3) 0.032(2) 0.100(3) -0.012(2) 0.038(3) -0.010(2) C10 0.074(2) 0.0258(18) 0.053(2) -0.0055(15) 0.0341(18) -0.0076(16) C11 0.075(2) 0.032(2) 0.0443(18) 0.0024(14) 0.0222(17) 0.0123(16) C12 0.118(4) 0.038(2) 0.076(3) 0.011(2) 0.027(3) 0.026(2) C13 0.126(5) 0.085(4) 0.069(3) 0.008(3) -0.001(3) 0.064(4) C14 0.097(4) 0.083(4) 0.088(4) -0.010(3) -0.024(3) 0.047(3) C15 0.070(3) 0.064(3) 0.084(3) -0.007(2) -0.021(2) 0.024(2) C16 0.0319(13) 0.0209(14) 0.0351(15) 0.0019(11) 0.0059(11) 0.0026(11) C17 0.0373(15) 0.0302(18) 0.0377(15) -0.0003(13) 0.0045(12) -0.0030(12) C18 0.0351(14) 0.0278(16) 0.0355(16) -0.0003(12) 0.0043(12) -0.0037(12) C19 0.0330(14) 0.0284(16) 0.0275(13) -0.0012(12) 0.0021(11) 0.0003(12) C20 0.0357(16) 0.0392(18) 0.0332(15) 0.0004(13) 0.0045(12) -0.0031(13) C21 0.0364(16) 0.0334(17) 0.0407(16) 0.0059(13) 0.0058(12) 0.0002(13) C22 0.0414(13) 0.0419(16) 0.0586(16) 0.0041(14) -0.0072(12) -0.0111(12) C23 0.077(3) 0.121(3) 0.105(3) 0.045(2) -0.036(2) -0.031(2) C24 0.057(2) 0.057(2) 0.089(3) -0.0003(19) 0.0024(19) -0.0268(17) C25A 0.052(3) 0.037(3) 0.056(3) -0.001(3) 0.019(2) -0.001(2) C26A 0.075(4) 0.093(6) 0.044(3) -0.014(4) 0.021(3) 0.006(4) C27A 0.096(5) 0.036(4) 0.186(10) -0.030(5) 0.072(6) -0.004(4) C25B 0.042(5) 0.046(6) 0.034(5) -0.002(5) 0.003(4) 0.005(4) C26B 0.075(8) 0.083(11) 0.035(6) -0.019(6) -0.004(5) 0.022(7) C27B 0.087(9) 0.051(8) 0.067(8) 0.013(6) 0.033(7) 0.027(6) Dy1 0.03064(7) 0.02073(8) 0.02968(7) 0.00078(5) 0.00362(5) -0.00386(5) Fe1 0.02790(18) 0.0208(2) 0.02769(19) 0.00066(15) 0.00350(14) -0.00169(15) N1 0.0311(12) 0.0397(16) 0.0466(15) -0.0033(12) 0.0019(11) -0.0044(11) N2 0.0472(14) 0.0308(15) 0.0390(13) -0.0056(11) 0.0150(11) -0.0110(11) N3 0.0570(17) 0.0384(17) 0.0498(16) 0.0029(13) 0.0048(13) 0.0106(13) N4 0.0423(14) 0.0295(15) 0.0357(13) 0.0032(11) 0.0042(10) -0.0020(11) N5 0.0481(15) 0.0328(15) 0.0330(14) -0.0003(11) 0.0041(11) 0.0038(11) N6 0.0661(19) 0.0284(17) 0.069(2) 0.0063(14) 0.0109(15) -0.0074(13) N7 0.0548(16) 0.0514(19) 0.0367(15) -0.0059(13) 0.0030(12) -0.0116(14) N8 0.0386(16) 0.080(3) 0.082(2) 0.0122(19) 0.0176(15) 0.0094(16) N9 0.0388(16) 0.081(2) 0.0555(18) -0.0038(17) 0.0089(13) 0.0077(15) N10 0.0483(16) 0.0434(18) 0.0575(18) -0.0155(14) 0.0140(13) 0.0047(13) N11 0.0394(12) 0.0494(14) 0.0587(14) 0.0010(11) -0.0020(10) -0.0145(10) O1 0.0780(17) 0.0322(14) 0.0465(14) -0.0047(11) 0.0114(12) 0.0113(12) O2 0.0411(12) 0.0516(16) 0.0664(16) 0.0154(12) -0.0095(11) -0.0187(11) O3 0.0809(17) 0.0307(13) 0.0557(14) -0.0008(11) 0.0360(13) -0.0030(12) O4 0.139(3) 0.064(2) 0.114(3) 0.006(2) 0.078(2) 0.000(2) O5 0.205(4) 0.0252(15) 0.148(3) -0.0112(18) 0.135(3) -0.0085(19) O6 0.0427(12) 0.083(2) 0.0402(12) -0.0029(12) 0.0086(10) 0.0056(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.328(4) . ? C1 C2 1.375(5) . ? C1 H1 0.9300 . ? C2 C3 1.379(6) . ? C2 H2 0.9300 . ? C3 C4 1.333(6) . ? C3 H3 0.9300 . ? C4 C5 1.384(5) . ? C4 H4 0.9300 . ? C5 N1 1.376(4) . ? C5 C6 1.493(5) . ? C6 N2 1.341(4) . ? C6 C7 1.401(5) . ? C7 C8 1.366(7) . ? C7 H7 0.9300 . ? C8 C9 1.365(7) . ? C8 H8 0.9300 . ? C9 C10 1.395(5) . ? C9 H9 0.9300 . ? C10 N2 1.360(4) . ? C10 C11 1.470(6) . ? C11 N3 1.341(4) . ? C11 C12 1.401(5) . ? C12 C13 1.363(7) . ? C12 H12 0.9300 . ? C13 C14 1.341(8) . ? C13 H13 0.9300 . ? C14 C15 1.379(6) . ? C14 H14 0.9300 . ? C15 N3 1.335(5) . ? C15 H15 0.9300 . ? C16 N5 1.149(4) . ? C16 Fe1 1.923(3) . ? C17 N6 1.139(4) . ? C17 Fe1 1.939(3) . ? C18 N7 1.145(4) . ? C18 Fe1 1.936(3) . ? C19 N4 1.151(4) . ? C19 Fe1 1.926(3) . ? C20 N9 1.145(4) . ? C20 Fe1 1.946(3) . ? C21 N8 1.145(4) . ? C21 Fe1 1.939(3) . ? C22 O2 1.235(4) . ? C22 N11 1.296(4) . ? C22 H22 0.9300 . ? C23 N11 1.416(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N11 1.450(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25A O1 1.218(6) . ? C25A N10 1.324(6) . ? C25A H25 0.9300 . ? C26A N10 1.372(7) . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A N10 1.534(7) . ? C27A H27D 0.9600 . ? C27A H27E 0.9600 . ? C27A H27F 0.9600 . ? C25B O1 1.146(9) . ? C25B N10 1.384(10) . ? C25B H25A 0.9300 . ? C26B N10 1.507(11) . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B N10 1.364(11) . ? C27B H27A 0.9600 . ? C27B H27B 0.9600 . ? C27B H27C 0.9600 . ? Dy1 O2 2.304(2) . ? Dy1 O3 2.309(2) . ? Dy1 O1 2.327(2) . ? Dy1 N5 2.420(3) 4_575 ? Dy1 N4 2.463(3) . ? Dy1 N1 2.483(2) . ? Dy1 N2 2.519(3) . ? Dy1 N3 2.547(3) . ? N5 Dy1 2.419(3) 4_576 ? O3 H3A 0.8499 . ? O3 H3B 0.8499 . ? O4 H4A 0.8251 . ? O4 H4B 0.8831 . ? O5 H5A 0.8500 . ? O5 H5B 0.8501 . ? O6 H6A 0.8862 . ? O6 H6B 0.8636 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.2(4) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.2(4) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.0(4) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N1 C5 C4 119.8(4) . . ? N1 C5 C6 117.3(3) . . ? C4 C5 C6 123.0(4) . . ? N2 C6 C7 121.4(4) . . ? N2 C6 C5 116.8(3) . . ? C7 C6 C5 121.7(4) . . ? C8 C7 C6 118.9(4) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C9 120.4(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C10 118.9(4) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N2 C10 C9 121.2(4) . . ? N2 C10 C11 117.1(3) . . ? C9 C10 C11 121.7(4) . . ? N3 C11 C12 121.4(4) . . ? N3 C11 C10 116.6(3) . . ? C12 C11 C10 121.9(4) . . ? C13 C12 C11 119.3(5) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 119.3(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 119.5(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N3 C15 C14 122.9(5) . . ? N3 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? N5 C16 Fe1 176.8(3) . . ? N6 C17 Fe1 177.3(3) . . ? N7 C18 Fe1 179.3(3) . . ? N4 C19 Fe1 173.8(2) . . ? N9 C20 Fe1 178.4(3) . . ? N8 C21 Fe1 178.2(3) . . ? O2 C22 N11 125.6(3) . . ? O2 C22 H22 117.2 . . ? N11 C22 H22 117.2 . . ? N11 C23 H23A 109.5 . . ? N11 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N11 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N11 C24 H24A 109.5 . . ? N11 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N11 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25A N10 123.9(5) . . ? O1 C25A H25 118.1 . . ? N10 C25A H25 118.1 . . ? N10 C26A H26A 109.5 . . ? N10 C26A H26B 109.5 . . ? N10 C26A H26C 109.5 . . ? N10 C27A H27D 109.5 . . ? N10 C27A H27E 109.5 . . ? N10 C27A H27F 109.5 . . ? O1 C25B N10 124.6(8) . . ? O1 C25B H25A 117.7 . . ? N10 C25B H25A 117.7 . . ? N10 C26B H26D 109.5 . . ? N10 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? N10 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? N10 C27B H27A 109.5 . . ? N10 C27B H27B 109.5 . . ? H27A C27B H27B 109.5 . . ? N10 C27B H27C 109.5 . . ? H27A C27B H27C 109.5 . . ? H27B C27B H27C 109.5 . . ? O2 Dy1 O3 91.61(10) . . ? O2 Dy1 O1 82.87(10) . . ? O3 Dy1 O1 144.22(8) . . ? O2 Dy1 N5 91.62(9) . 4_575 ? O3 Dy1 N5 143.92(9) . 4_575 ? O1 Dy1 N5 71.78(9) . 4_575 ? O2 Dy1 N4 78.38(8) . . ? O3 Dy1 N4 70.25(8) . . ? O1 Dy1 N4 74.02(9) . . ? N5 Dy1 N4 145.29(9) 4_575 . ? O2 Dy1 N1 151.68(9) . . ? O3 Dy1 N1 92.91(9) . . ? O1 Dy1 N1 77.21(9) . . ? N5 Dy1 N1 100.88(9) 4_575 . ? N4 Dy1 N1 76.93(8) . . ? O2 Dy1 N2 141.70(9) . . ? O3 Dy1 N2 75.12(8) . . ? O1 Dy1 N2 128.13(9) . . ? N5 Dy1 N2 80.29(8) 4_575 . ? N4 Dy1 N2 127.11(8) . . ? N1 Dy1 N2 66.14(9) . . ? O2 Dy1 N3 77.55(9) . . ? O3 Dy1 N3 74.54(9) . . ? O1 Dy1 N3 137.18(9) . . ? N5 Dy1 N3 71.13(9) 4_575 . ? N4 Dy1 N3 136.29(9) . . ? N1 Dy1 N3 130.50(9) . . ? N2 Dy1 N3 64.37(10) . . ? C16 Fe1 C19 94.92(12) . . ? C16 Fe1 C18 177.32(12) . . ? C19 Fe1 C18 87.23(12) . . ? C16 Fe1 C21 91.09(12) . . ? C19 Fe1 C21 87.38(12) . . ? C18 Fe1 C21 90.62(12) . . ? C16 Fe1 C17 88.28(12) . . ? C19 Fe1 C17 176.32(12) . . ? C18 Fe1 C17 89.63(12) . . ? C21 Fe1 C17 90.74(13) . . ? C16 Fe1 C20 87.28(12) . . ? C19 Fe1 C20 88.40(12) . . ? C18 Fe1 C20 91.17(12) . . ? C21 Fe1 C20 175.33(14) . . ? C17 Fe1 C20 93.58(13) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Dy1 122.1(2) . . ? C5 N1 Dy1 119.7(2) . . ? C6 N2 C10 119.1(3) . . ? C6 N2 Dy1 119.9(2) . . ? C10 N2 Dy1 120.7(2) . . ? C15 N3 C11 117.5(3) . . ? C15 N3 Dy1 121.6(3) . . ? C11 N3 Dy1 120.6(2) . . ? C19 N4 Dy1 165.1(2) . . ? C16 N5 Dy1 157.6(2) . 4_576 ? C25A N10 C27B 76.0(6) . . ? C25A N10 C26A 125.3(5) . . ? C27B N10 C26A 143.1(7) . . ? C25A N10 C25B 49.7(5) . . ? C27B N10 C25B 123.0(7) . . ? C26A N10 C25B 76.9(5) . . ? C25A N10 C26B 161.8(6) . . ? C27B N10 C26B 121.9(7) . . ? C26A N10 C26B 42.7(6) . . ? C25B N10 C26B 113.9(7) . . ? C25A N10 C27A 116.0(5) . . ? C27B N10 C27A 51.8(7) . . ? C26A N10 C27A 118.7(5) . . ? C25B N10 C27A 160.7(5) . . ? C26B N10 C27A 77.8(7) . . ? C22 N11 C23 121.6(3) . . ? C22 N11 C24 122.9(3) . . ? C23 N11 C24 115.5(3) . . ? C25B O1 C25A 57.5(6) . . ? C25B O1 Dy1 148.1(5) . . ? C25A O1 Dy1 149.8(3) . . ? C22 O2 Dy1 137.5(2) . . ? Dy1 O3 H3A 118.8 . . ? Dy1 O3 H3B 120.4 . . ? H3A O3 H3B 120.8 . . ? H4A O4 H4B 110.0 . . ? H5A O5 H5B 108.5 . . ? H6A O6 H6B 104.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.991 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 896256' ####################################################################### # # 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_2-dyco _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H27 Co Dy N11 O3, 3(H2 O)' _chemical_formula_sum 'C27 H33 Co Dy N11 O6' _chemical_formula_weight 829.07 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' Co Co 0.3494 0.9721 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.362(2) _cell_length_b 13.2326(17) _cell_length_c 15.670(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.246(2) _cell_angle_gamma 90.00 _cell_volume 3357.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2830 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 21.99 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 2.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7331 _exptl_absorpt_correction_T_max 0.8095 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19942 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6588 _reflns_number_gt 4219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+0.1285P] 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 6588 _refine_ls_number_parameters 449 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4462(4) 0.7795(6) 1.0953(4) 0.063(2) Uani 1 1 d . . . H1 H 0.4153 0.7212 1.0818 0.076 Uiso 1 1 calc R . . C2 C 0.5247(4) 0.7670(6) 1.1357(4) 0.073(2) Uani 1 1 d U . . H2 H 0.5465 0.7032 1.1499 0.087 Uiso 1 1 calc R . . C3 C 0.5704(5) 0.8536(7) 1.1546(5) 0.089(3) Uani 1 1 d U . . H3 H 0.6254 0.8487 1.1793 0.107 Uiso 1 1 calc R . . C4 C 0.5363(5) 0.9449(8) 1.1378(5) 0.092(3) Uani 1 1 d . . . H4 H 0.5673 1.0025 1.1537 0.110 Uiso 1 1 calc R . . C5 C 0.4530(4) 0.9550(7) 1.0957(4) 0.069(2) Uani 1 1 d . . . C6 C 0.4099(5) 1.0538(6) 1.0761(5) 0.064(2) Uani 1 1 d . . . C7 C 0.4484(6) 1.1449(7) 1.1030(6) 0.102(3) Uani 1 1 d . . . H7 H 0.5021 1.1461 1.1320 0.122 Uiso 1 1 calc R . . C8 C 0.4053(7) 1.2312(8) 1.0855(7) 0.119(4) Uani 1 1 d . . . H8 H 0.4285 1.2929 1.1040 0.142 Uiso 1 1 calc R . . C9 C 0.3270(7) 1.2274(6) 1.0401(6) 0.096(3) Uani 1 1 d . . . H9 H 0.2974 1.2867 1.0270 0.115 Uiso 1 1 calc R . . C10 C 0.2925(5) 1.1356(5) 1.0142(4) 0.0592(19) Uani 1 1 d . . . C11 C 0.2095(5) 1.1266(6) 0.9654(4) 0.064(2) Uani 1 1 d . . . C12 C 0.1634(7) 1.2106(6) 0.9312(6) 0.092(3) Uani 1 1 d . . . H12 H 0.1856 1.2754 0.9374 0.111 Uiso 1 1 calc R . . C13 C 0.0873(7) 1.1960(9) 0.8897(6) 0.116(4) Uani 1 1 d . . . H13 H 0.0560 1.2514 0.8677 0.139 Uiso 1 1 calc R . . C14 C 0.0549(6) 1.1026(8) 0.8790(6) 0.109(4) Uani 1 1 d . . . H14 H 0.0019 1.0922 0.8500 0.131 Uiso 1 1 calc R . . C15 C 0.1029(5) 1.0236(7) 0.9122(5) 0.095(3) Uani 1 1 d . . . H15 H 0.0808 0.9590 0.9040 0.114 Uiso 1 1 calc R . . C16 C 0.2720(3) 0.5589(4) 1.2851(4) 0.0357(14) Uani 1 1 d . . . C17 C 0.2286(3) 0.3917(5) 1.1982(4) 0.0434(15) Uani 1 1 d . . . C18 C 0.2052(3) 0.4944(4) 1.0510(4) 0.0412(15) Uani 1 1 d . . . C19 C 0.2536(3) 0.6619(5) 1.1328(3) 0.0372(14) Uani 1 1 d . . . C20 C 0.1301(4) 0.5592(5) 1.1830(4) 0.0423(16) Uani 1 1 d . . . C21 C 0.3510(4) 0.5049(4) 1.1532(4) 0.0444(16) Uani 1 1 d . . . C22 C 0.0993(4) 0.7394(6) 0.9667(5) 0.0713(15) Uani 1 1 d U A . H22 H 0.1214 0.6982 1.0123 0.086 Uiso 1 1 calc R . . C23 C -0.0114(5) 0.7741(6) 0.8597(5) 0.109(2) Uani 1 1 d U . . H23A H -0.0110 0.8434 0.8778 0.164 Uiso 1 1 calc R . . H23B H -0.0674 0.7519 0.8440 0.164 Uiso 1 1 calc R . . H23C H 0.0176 0.7679 0.8109 0.164 Uiso 1 1 calc R . . C24 C -0.0196(5) 0.6316(5) 0.9530(5) 0.0872(19) Uani 1 1 d U . . H24A H -0.0264 0.5815 0.9083 0.131 Uiso 1 1 calc R . . H24B H -0.0728 0.6552 0.9632 0.131 Uiso 1 1 calc R . . H24C H 0.0090 0.6025 1.0050 0.131 Uiso 1 1 calc R . . C25A C 0.3270(7) 0.6543(12) 0.9332(9) 0.067(5) Uani 0.626(16) 1 d P A 1 H25 H 0.3127 0.6154 0.9782 0.081 Uiso 0.626(16) 1 calc PR A 1 C26A C 0.3838(12) 0.6495(16) 0.8030(11) 0.108(7) Uani 0.626(16) 1 d P A 1 H26A H 0.3453 0.6338 0.7525 0.161 Uiso 0.626(16) 1 calc PR A 1 H26B H 0.4377 0.6255 0.7956 0.161 Uiso 0.626(16) 1 calc PR A 1 H26C H 0.3856 0.7214 0.8115 0.161 Uiso 0.626(16) 1 calc PR A 1 C27A C 0.3676(10) 0.4882(10) 0.8833(15) 0.116(7) Uani 0.626(16) 1 d P A 1 H27D H 0.4242 0.4710 0.9030 0.174 Uiso 0.626(16) 1 calc PR A 1 H27E H 0.3499 0.4556 0.8290 0.174 Uiso 0.626(16) 1 calc PR A 1 H27F H 0.3337 0.4660 0.9248 0.174 Uiso 0.626(16) 1 calc PR A 1 C25B C 0.3242(11) 0.7033(17) 0.8734(12) 0.054(7) Uani 0.374(16) 1 d P A 2 H25A H 0.3089 0.7375 0.8217 0.065 Uiso 0.374(16) 1 calc PR A 2 C26B C 0.375(2) 0.575(3) 0.7799(17) 0.115(14) Uani 0.374(16) 1 d P A 2 H26D H 0.3254 0.5470 0.7488 0.172 Uiso 0.374(16) 1 calc PR A 2 H26E H 0.4186 0.5265 0.7835 0.172 Uiso 0.374(16) 1 calc PR A 2 H26F H 0.3902 0.6345 0.7504 0.172 Uiso 0.374(16) 1 calc PR A 2 C27B C 0.3928(16) 0.553(2) 0.9420(15) 0.089(10) Uani 0.374(16) 1 d P A 2 H27A H 0.4504 0.5690 0.9555 0.133 Uiso 0.374(16) 1 calc PR A 2 H27B H 0.3868 0.4815 0.9307 0.133 Uiso 0.374(16) 1 calc PR A 2 H27C H 0.3650 0.5701 0.9899 0.133 Uiso 0.374(16) 1 calc PR A 2 Dy1 Dy 0.266697(17) 0.88032(2) 1.001568(17) 0.03424(9) Uani 1 1 d . . . Co1 Co 0.24036(5) 0.52907(6) 1.16850(5) 0.0346(2) Uani 1 1 d . . . N1 N 0.4094(3) 0.8663(4) 1.0732(3) 0.0472(13) Uani 1 1 d . . . N2 N 0.3342(3) 1.0484(4) 1.0321(3) 0.0458(13) Uani 1 1 d . . . N3 N 0.1778(4) 1.0318(4) 0.9548(3) 0.0566(15) Uani 1 1 d . . . N4 N 0.2606(3) 0.7399(4) 1.1020(3) 0.0426(13) Uani 1 1 d . . . N5 N 0.2878(3) 0.5734(4) 1.3583(3) 0.0476(14) Uani 1 1 d . . . N6 N 0.2235(3) 0.3091(4) 1.2142(4) 0.0630(17) Uani 1 1 d . . . N7 N 0.1842(3) 0.4737(4) 0.9816(3) 0.0605(16) Uani 1 1 d . . . N8 N 0.4184(4) 0.4923(5) 1.1430(4) 0.0761(19) Uani 1 1 d . . . N9 N 0.0641(4) 0.5810(5) 1.1908(3) 0.0679(18) Uani 1 1 d . . . N10 N 0.3596(3) 0.6048(5) 0.8719(4) 0.0618(16) Uani 1 1 d . . . N11 N 0.0272(4) 0.7145(5) 0.9271(4) 0.0733(13) Uani 1 1 d U . . O1 O 0.3144(3) 0.7411(4) 0.9368(3) 0.0681(15) Uani 1 1 d . . . O2 O 0.1416(3) 0.8112(3) 0.9506(3) 0.0651(13) Uani 1 1 d . . . O3 O 0.2189(3) 0.9375(3) 1.1243(3) 0.0673(14) Uani 1 1 d . . . H3A H 0.2356 0.9936 1.1455 0.081 Uiso 1 1 d R A . H3B H 0.1852 0.9019 1.1479 0.081 Uiso 1 1 d R . . O4 O 0.1525(4) 0.8340(4) 0.2450(4) 0.140(3) Uani 1 1 d . . . H4A H 0.1139 0.7903 0.2323 0.168 Uiso 1 1 d R . . H4B H 0.1344 0.8830 0.2712 0.168 Uiso 1 1 d R . . O5 O 0.2047(4) 0.1019(3) 0.2066(4) 0.124(3) Uani 1 1 d . . . H5A H 0.1734 0.0803 0.2410 0.149 Uiso 1 1 d R . . H5B H 0.2094 0.1651 0.2125 0.149 Uiso 1 1 d R . . O6 O 0.1024(3) 0.0174(4) 0.3124(3) 0.0753(15) Uani 1 1 d . . . H6A H 0.1272 0.0217 0.3631 0.090 Uiso 1 1 d R . . H6B H 0.0533 0.0380 0.3119 0.090 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.055(5) 0.065(6) 0.068(5) -0.003(4) 0.001(4) 0.001(4) C2 0.049(5) 0.096(7) 0.070(5) -0.001(5) -0.001(4) -0.006(4) C3 0.045(5) 0.121(8) 0.096(6) -0.006(6) -0.008(4) 0.014(5) C4 0.051(6) 0.131(9) 0.093(6) -0.022(6) 0.005(5) -0.028(5) C5 0.054(5) 0.109(7) 0.045(4) -0.007(5) 0.014(4) -0.023(5) C6 0.081(6) 0.048(5) 0.066(5) -0.009(4) 0.024(4) -0.011(4) C7 0.110(8) 0.077(7) 0.123(8) -0.038(7) 0.030(6) -0.043(6) C8 0.140(11) 0.070(8) 0.155(10) -0.046(8) 0.051(8) -0.044(7) C9 0.134(9) 0.044(6) 0.122(8) -0.017(5) 0.055(7) -0.029(6) C10 0.084(6) 0.031(5) 0.069(5) -0.002(4) 0.031(4) -0.001(4) C11 0.093(6) 0.047(5) 0.060(4) 0.005(4) 0.035(4) 0.011(5) C12 0.146(10) 0.047(6) 0.088(7) 0.014(5) 0.033(6) 0.032(6) C13 0.142(11) 0.120(10) 0.081(7) 0.015(7) 0.000(7) 0.068(9) C14 0.116(8) 0.094(8) 0.107(8) -0.015(7) -0.023(6) 0.048(7) C15 0.085(7) 0.089(7) 0.100(7) -0.005(5) -0.020(5) 0.038(5) C16 0.040(4) 0.028(4) 0.039(3) 0.001(3) 0.007(3) 0.003(3) C17 0.043(4) 0.039(4) 0.048(4) -0.008(3) 0.004(3) -0.007(3) C18 0.042(4) 0.039(4) 0.044(4) -0.002(3) 0.011(3) -0.004(3) C19 0.041(4) 0.037(4) 0.033(3) -0.003(3) 0.003(3) 0.001(3) C20 0.047(4) 0.044(4) 0.036(3) 0.003(3) 0.002(3) -0.009(3) C21 0.050(4) 0.040(4) 0.042(4) 0.009(3) 0.005(3) -0.001(3) C22 0.060(3) 0.072(3) 0.077(3) 0.009(3) -0.008(2) -0.015(3) C23 0.092(4) 0.115(4) 0.108(4) 0.030(3) -0.032(3) -0.024(4) C24 0.080(4) 0.076(4) 0.101(4) 0.002(4) 0.001(4) -0.026(3) C25A 0.067(9) 0.080(12) 0.058(9) -0.004(9) 0.019(7) 0.004(7) C26A 0.109(13) 0.16(2) 0.055(11) 0.001(12) 0.029(10) 0.021(14) C27A 0.131(15) 0.034(9) 0.19(2) -0.009(11) 0.059(14) 0.018(8) C25B 0.079(14) 0.067(16) 0.014(10) 0.001(11) -0.001(9) -0.007(12) C26B 0.12(2) 0.17(4) 0.047(16) -0.032(19) -0.008(14) 0.07(2) C27B 0.14(2) 0.07(2) 0.065(16) 0.035(15) 0.037(15) 0.054(17) Dy1 0.04044(16) 0.02900(17) 0.03302(14) 0.00071(15) 0.00440(10) -0.00412(14) Co1 0.0389(5) 0.0316(5) 0.0330(4) 0.0004(4) 0.0045(3) -0.0026(3) N1 0.036(3) 0.047(4) 0.058(3) 0.002(3) 0.002(2) -0.005(3) N2 0.053(4) 0.044(4) 0.043(3) -0.004(3) 0.016(3) -0.007(3) N3 0.064(4) 0.050(4) 0.055(4) -0.001(3) 0.006(3) 0.008(3) N4 0.054(3) 0.037(3) 0.038(3) 0.004(3) 0.011(2) -0.001(2) N5 0.060(4) 0.042(3) 0.041(3) -0.001(3) 0.004(3) 0.003(3) N6 0.077(4) 0.033(4) 0.080(4) -0.001(3) 0.014(3) -0.008(3) N7 0.076(4) 0.067(4) 0.038(3) -0.013(3) 0.007(3) -0.016(3) N8 0.046(4) 0.090(5) 0.094(5) 0.016(4) 0.017(4) 0.009(3) N9 0.045(4) 0.097(5) 0.062(4) -0.003(3) 0.011(3) 0.005(3) N10 0.058(4) 0.065(5) 0.065(4) -0.022(4) 0.014(3) 0.000(3) N11 0.062(3) 0.075(3) 0.078(3) 0.007(3) -0.007(2) -0.018(2) O1 0.112(4) 0.039(4) 0.055(4) -0.002(3) 0.016(3) 0.018(3) O2 0.057(3) 0.063(3) 0.070(3) 0.016(3) -0.006(2) -0.019(2) O3 0.103(4) 0.042(3) 0.065(3) 0.002(2) 0.039(3) -0.010(3) O4 0.188(7) 0.100(5) 0.157(6) 0.004(5) 0.107(5) 0.000(4) O5 0.221(7) 0.032(3) 0.150(5) -0.008(3) 0.133(5) -0.001(4) O6 0.056(3) 0.122(4) 0.049(3) 0.003(3) 0.008(2) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.319(7) . ? C1 C2 1.359(8) . ? C1 H1 0.9300 . ? C2 C3 1.377(10) . ? C2 H2 0.9300 . ? C3 C4 1.340(11) . ? C3 H3 0.9300 . ? C4 C5 1.433(9) . ? C4 H4 0.9300 . ? C5 N1 1.392(8) . ? C5 C6 1.496(10) . ? C6 N2 1.331(8) . ? C6 C7 1.397(10) . ? C7 C8 1.349(12) . ? C7 H7 0.9300 . ? C8 C9 1.374(12) . ? C8 H8 0.9300 . ? C9 C10 1.376(9) . ? C9 H9 0.9300 . ? C10 N2 1.349(8) . ? C10 C11 1.465(10) . ? C11 N3 1.359(8) . ? C11 C12 1.406(10) . ? C12 C13 1.333(12) . ? C12 H12 0.9300 . ? C13 C14 1.346(12) . ? C13 H13 0.9300 . ? C14 C15 1.364(10) . ? C14 H14 0.9300 . ? C15 N3 1.314(9) . ? C15 H15 0.9300 . ? C16 N5 1.155(6) . ? C16 Co1 1.869(6) . ? C17 N6 1.126(7) . ? C17 Co1 1.893(7) . ? C18 N7 1.127(7) . ? C18 Co1 1.904(6) . ? C19 N4 1.152(6) . ? C19 Co1 1.867(6) . ? C20 N9 1.141(7) . ? C20 Co1 1.893(7) . ? C21 N8 1.149(7) . ? C21 Co1 1.887(7) . ? C22 O2 1.222(7) . ? C22 N11 1.295(8) . ? C22 H22 0.9300 . ? C23 N11 1.393(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N11 1.430(8) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25A O1 1.170(14) . ? C25A N10 1.335(14) . ? C25A H25 0.9300 . ? C26A N10 1.340(17) . ? C26A H26A 0.9600 . ? C26A H26B 0.9600 . ? C26A H26C 0.9600 . ? C27A N10 1.557(13) . ? C27A H27D 0.9600 . ? C27A H27E 0.9600 . ? C27A H27F 0.9600 . ? C25B O1 1.144(18) . ? C25B N10 1.43(2) . ? C25B H25A 0.9300 . ? C26B N10 1.55(2) . ? C26B H26D 0.9600 . ? C26B H26E 0.9600 . ? C26B H26F 0.9600 . ? C27B N10 1.345(19) . ? C27B H27A 0.9600 . ? C27B H27B 0.9600 . ? C27B H27C 0.9600 . ? Dy1 O2 2.279(4) . ? Dy1 O1 2.293(5) . ? Dy1 O3 2.304(4) . ? Dy1 N5 2.399(5) 4_575 ? Dy1 N4 2.447(5) . ? Dy1 N1 2.449(5) . ? Dy1 N2 2.498(5) . ? Dy1 N3 2.523(5) . ? N5 Dy1 2.400(5) 4_576 ? O3 H3A 0.8437 . ? O3 H3B 0.8501 . ? O4 H4A 0.8580 . ? O4 H4B 0.8443 . ? O5 H5A 0.8452 . ? O5 H5B 0.8442 . ? O6 H6A 0.8416 . ? O6 H6B 0.8471 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 126.4(7) . . ? N1 C1 H1 116.8 . . ? C2 C1 H1 116.8 . . ? C1 C2 C3 116.5(8) . . ? C1 C2 H2 121.8 . . ? C3 C2 H2 121.8 . . ? C4 C3 C2 120.7(8) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 121.1(8) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N1 C5 C4 117.2(8) . . ? N1 C5 C6 118.4(6) . . ? C4 C5 C6 124.4(8) . . ? N2 C6 C7 123.3(8) . . ? N2 C6 C5 115.8(6) . . ? C7 C6 C5 120.9(8) . . ? C8 C7 C6 118.0(10) . . ? C8 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? C7 C8 C9 119.7(9) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 119.8(9) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 121.4(8) . . ? N2 C10 C11 116.2(6) . . ? C9 C10 C11 122.4(8) . . ? N3 C11 C12 120.6(8) . . ? N3 C11 C10 116.6(7) . . ? C12 C11 C10 122.8(8) . . ? C13 C12 C11 119.0(9) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 121.1(10) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 117.5(10) . . ? C13 C14 H14 121.3 . . ? C15 C14 H14 121.3 . . ? N3 C15 C14 125.1(9) . . ? N3 C15 H15 117.5 . . ? C14 C15 H15 117.5 . . ? N5 C16 Co1 175.8(5) . . ? N6 C17 Co1 177.7(6) . . ? N7 C18 Co1 179.7(6) . . ? N4 C19 Co1 172.7(5) . . ? N9 C20 Co1 177.4(6) . . ? N8 C21 Co1 178.5(6) . . ? O2 C22 N11 127.1(7) . . ? O2 C22 H22 116.4 . . ? N11 C22 H22 116.4 . . ? N11 C23 H23A 109.5 . . ? N11 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N11 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N11 C24 H24A 109.5 . . ? N11 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N11 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25A N10 127.4(14) . . ? O1 C25A H25 116.3 . . ? N10 C25A H25 116.3 . . ? N10 C26A H26A 109.5 . . ? N10 C26A H26B 109.5 . . ? N10 C26A H26C 109.5 . . ? N10 C27A H27D 109.5 . . ? N10 C27A H27E 109.5 . . ? N10 C27A H27F 109.5 . . ? O1 C25B N10 121.4(17) . . ? O1 C25B H25A 119.3 . . ? N10 C25B H25A 119.3 . . ? N10 C26B H26D 109.5 . . ? N10 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? N10 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? N10 C27B H27A 109.5 . . ? N10 C27B H27B 109.5 . . ? H27A C27B H27B 109.5 . . ? N10 C27B H27C 109.5 . . ? H27A C27B H27C 109.5 . . ? H27B C27B H27C 109.5 . . ? O2 Dy1 O1 82.41(18) . . ? O2 Dy1 O3 91.66(16) . . ? O1 Dy1 O3 144.14(17) . . ? O2 Dy1 N5 90.96(16) . 4_575 ? O1 Dy1 N5 71.76(18) . 4_575 ? O3 Dy1 N5 143.95(16) . 4_575 ? O2 Dy1 N4 78.64(15) . . ? O1 Dy1 N4 73.88(18) . . ? O3 Dy1 N4 70.29(15) . . ? N5 Dy1 N4 145.11(16) 4_575 . ? O2 Dy1 N1 151.61(17) . . ? O1 Dy1 N1 77.25(18) . . ? O3 Dy1 N1 93.32(17) . . ? N5 Dy1 N1 101.10(17) 4_575 . ? N4 Dy1 N1 76.83(16) . . ? O2 Dy1 N2 140.75(17) . . ? O1 Dy1 N2 129.08(18) . . ? O3 Dy1 N2 75.04(15) . . ? N5 Dy1 N2 80.39(16) 4_575 . ? N4 Dy1 N2 127.66(16) . . ? N1 Dy1 N2 67.25(18) . . ? O2 Dy1 N3 76.44(18) . . ? O1 Dy1 N3 136.74(18) . . ? O3 Dy1 N3 74.39(16) . . ? N5 Dy1 N3 71.34(17) 4_575 . ? N4 Dy1 N3 135.65(17) . . ? N1 Dy1 N3 131.73(19) . . ? N2 Dy1 N3 64.5(2) . . ? C19 Co1 C16 93.8(2) . . ? C19 Co1 C21 88.1(2) . . ? C16 Co1 C21 91.4(2) . . ? C19 Co1 C20 89.5(2) . . ? C16 Co1 C20 88.5(2) . . ? C21 Co1 C20 177.6(3) . . ? C19 Co1 C17 176.5(2) . . ? C16 Co1 C17 89.2(2) . . ? C21 Co1 C17 90.1(2) . . ? C20 Co1 C17 92.3(3) . . ? C19 Co1 C18 88.2(2) . . ? C16 Co1 C18 177.6(2) . . ? C21 Co1 C18 89.9(3) . . ? C20 Co1 C18 90.3(2) . . ? C17 Co1 C18 88.8(2) . . ? C1 N1 C5 118.0(6) . . ? C1 N1 Dy1 123.7(4) . . ? C5 N1 Dy1 118.2(5) . . ? C6 N2 C10 117.8(6) . . ? C6 N2 Dy1 120.0(5) . . ? C10 N2 Dy1 121.7(5) . . ? C15 N3 C11 116.8(6) . . ? C15 N3 Dy1 122.7(5) . . ? C11 N3 Dy1 120.2(5) . . ? C19 N4 Dy1 165.0(4) . . ? C16 N5 Dy1 158.5(5) . 4_576 ? C25A N10 C26A 123.8(11) . . ? C25A N10 C27B 79.7(11) . . ? C26A N10 C27B 138.9(14) . . ? C25A N10 C25B 48.4(8) . . ? C26A N10 C25B 77.1(11) . . ? C27B N10 C25B 124.9(13) . . ? C25A N10 C26B 158.1(14) . . ? C26A N10 C26B 41.8(14) . . ? C27B N10 C26B 122.1(15) . . ? C25B N10 C26B 111.4(15) . . ? C25A N10 C27A 116.1(11) . . ? C26A N10 C27A 120.0(10) . . ? C27B N10 C27A 51.7(11) . . ? C25B N10 C27A 158.6(11) . . ? C26B N10 C27A 80.5(13) . . ? C22 N11 C23 120.1(7) . . ? C22 N11 C24 123.2(7) . . ? C23 N11 C24 116.5(6) . . ? C25B O1 C25A 58.8(11) . . ? C25B O1 Dy1 146.6(13) . . ? C25A O1 Dy1 152.1(9) . . ? C22 O2 Dy1 138.3(5) . . ? Dy1 O3 H3A 119.3 . . ? Dy1 O3 H3B 120.1 . . ? H3A O3 H3B 120.6 . . ? H4A O4 H4B 109.4 . . ? H5A O5 H5B 108.6 . . ? H6A O6 H6B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.120 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.122 _database_code_depnum_ccdc_archive 'CCDC 896257' ####################################################################### # # 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_3-HoFe _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H64 Fe2 Ho2 N20 O14' _chemical_formula_weight 1610.77 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2315(17) _cell_length_b 13.364(2) _cell_length_c 13.475(2) _cell_angle_alpha 94.491(2) _cell_angle_beta 111.353(2) _cell_angle_gamma 101.917(2) _cell_volume 1655.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9991 _cell_measurement_theta_min 2.466 _cell_measurement_theta_max 27.517 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 802 _exptl_absorpt_coefficient_mu 2.867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5979 _exptl_absorpt_correction_T_max 0.7248 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11485 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5605 _reflns_number_gt 5189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+1.4052P] 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 5605 _refine_ls_number_parameters 408 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O7 O 0.559(2) 0.7855(16) 0.5125(19) 0.049(6) Uiso 0.242(4) 1 d PD A 1 H7B H 0.5001 0.8114 0.4657 0.059 Uiso 0.242(4) 1 d PR A 1 C25 C 0.523(3) 0.6824(16) 0.483(2) 0.058(7) Uiso 0.242(4) 1 d PD A 1 H25A H 0.5988 0.6617 0.4674 0.087 Uiso 0.242(4) 1 d PR A 1 H25B H 0.5094 0.6501 0.5406 0.087 Uiso 0.242(4) 1 d PR A 1 H25C H 0.4342 0.6613 0.4193 0.087 Uiso 0.242(4) 1 d PR A 1 O8 O 0.5715(16) 0.8182(11) 0.5143(13) 0.073(5) Uiso 0.467(12) 1 d PD B 2 H8B H 0.4960 0.8010 0.4560 0.088 Uiso 0.467(12) 1 d PR B 2 C26 C 0.622(3) 0.9204(16) 0.565(2) 0.108(8) Uiso 0.467(12) 1 d PD B 2 H26A H 0.7126 0.9504 0.5599 0.162 Uiso 0.467(12) 1 d PR B 2 H26B H 0.5526 0.9585 0.5310 0.162 Uiso 0.467(12) 1 d PR B 2 H26C H 0.6360 0.9234 0.6398 0.162 Uiso 0.467(12) 1 d PR B 2 C27 C 0.682(3) 0.996(3) 0.587(3) 0.091(10) Uiso 0.291(12) 1 d PD C 3 H27A H 0.7139 1.0699 0.6091 0.136 Uiso 0.291(12) 1 d PR C 3 H27B H 0.6104 0.9794 0.5144 0.136 Uiso 0.291(12) 1 d PR C 3 H27C H 0.6410 0.9653 0.6346 0.136 Uiso 0.291(12) 1 d PR C 3 O9 O 0.798(3) 0.957(2) 0.599(2) 0.111(9) Uiso 0.291(12) 1 d PD C 3 H9B H 0.8607 0.9688 0.6632 0.133 Uiso 0.291(12) 1 d PR C 3 C1 C 0.1714(6) 0.5380(4) 0.6239(5) 0.0435(13) Uani 1 1 d . . . H1 H 0.1607 0.4843 0.6625 0.052 Uiso 1 1 calc R . . C2 C 0.1913(7) 0.5182(6) 0.5319(5) 0.0598(18) Uani 1 1 d . . . H2 H 0.1985 0.4524 0.5105 0.072 Uiso 1 1 calc R . . C3 C 0.2009(9) 0.5915(8) 0.4695(6) 0.074(2) Uani 1 1 d . . . H3 H 0.2072 0.5758 0.4032 0.089 Uiso 1 1 calc R . . C4 C 0.2011(8) 0.6857(7) 0.5057(6) 0.068(2) Uani 1 1 d . . . H4 H 0.2114 0.7383 0.4657 0.082 Uiso 1 1 calc R . . C5 C 0.1865(7) 0.7073(5) 0.6008(5) 0.0517(15) Uani 1 1 d . . . C6 C 0.1993(7) 0.8168(5) 0.6519(6) 0.0531(16) Uani 1 1 d . . . C7 C 0.1785(9) 0.8957(7) 0.5903(8) 0.080(2) Uani 1 1 d . . . H7 H 0.1575 0.8830 0.5166 0.096 Uiso 1 1 calc R . . C8 C 0.1895(10) 0.9911(8) 0.6399(8) 0.087(3) Uani 1 1 d . . . H8 H 0.1750 1.0445 0.6001 0.105 Uiso 1 1 calc R . . C9 C 0.2207(10) 1.0082(6) 0.7451(8) 0.078(2) Uani 1 1 d . . . H9 H 0.2274 1.0735 0.7792 0.093 Uiso 1 1 calc R . . C10 C 0.2438(7) 0.9271(5) 0.8054(6) 0.0526(16) Uani 1 1 d . . . C11 C 0.2911(7) 0.9407(4) 0.9268(6) 0.0498(15) Uani 1 1 d . . . C12 C 0.3303(8) 1.0353(5) 0.9923(9) 0.076(3) Uani 1 1 d . . . H12 H 0.3204 1.0948 0.9618 0.091 Uiso 1 1 calc R . . C13 C 0.3829(9) 1.0416(7) 1.1006(9) 0.086(3) Uani 1 1 d . . . H13 H 0.4137 1.1054 1.1458 0.103 Uiso 1 1 calc R . . C14 C 0.3898(8) 0.9548(7) 1.1409(7) 0.072(2) Uani 1 1 d . . . H14 H 0.4236 0.9571 1.2154 0.087 Uiso 1 1 calc R . . C15 C 0.3475(8) 0.8623(5) 1.0740(6) 0.0600(18) Uani 1 1 d . . . H15 H 0.3535 0.8030 1.1054 0.072 Uiso 1 1 calc R . . C16 C 0.0455(5) 0.4143(4) 0.8228(4) 0.0311(10) Uani 1 1 d . . . C17 C -0.1963(6) 0.2472(4) 0.7385(4) 0.0361(12) Uani 1 1 d . . . C18 C -0.0290(6) 0.1223(4) 0.8409(5) 0.0388(12) Uani 1 1 d . . . C19 C 0.2050(6) 0.2864(4) 0.9290(4) 0.0326(11) Uani 1 1 d . . . C20 C -0.0361(5) 0.2971(4) 0.9557(4) 0.0280(10) Uani 1 1 d . . . C21 C 0.0612(6) 0.2447(4) 0.7091(5) 0.0378(12) Uani 1 1 d . . . C22 C 0.2950(7) 0.5692(5) 1.0639(5) 0.0492(14) Uani 1 1 d . . . H22 H 0.1993 0.5301 1.0386 0.059 Uiso 1 1 calc R . . C23 C 0.5339(9) 0.6167(11) 1.2016(9) 0.120(5) Uani 1 1 d . . . H23A H 0.5397 0.6853 1.1841 0.180 Uiso 1 1 calc R . . H23B H 0.5884 0.5829 1.1714 0.180 Uiso 1 1 calc R . . H23C H 0.5732 0.6210 1.2787 0.180 Uiso 1 1 calc R . . C24 C 0.3366(11) 0.4914(7) 1.2236(7) 0.084(3) Uani 1 1 d . . . H24A H 0.2386 0.4516 1.1832 0.125 Uiso 1 1 calc R . . H24B H 0.3413 0.5331 1.2867 0.125 Uiso 1 1 calc R . . H24C H 0.3986 0.4453 1.2450 0.125 Uiso 1 1 calc R . . Fe1 Fe 0.00675(7) 0.26817(5) 0.83111(5) 0.02572(16) Uani 1 1 d . . . Ho1 Ho 0.19103(2) 0.681835(14) 0.848164(16) 0.02588(10) Uani 1 1 d . . . N1 N 0.1665(5) 0.6305(4) 0.6617(4) 0.0410(10) Uani 1 1 d . . . N2 N 0.2285(5) 0.8304(4) 0.7548(4) 0.0421(11) Uani 1 1 d . . . N3 N 0.2990(5) 0.8509(4) 0.9682(4) 0.0432(11) Uani 1 1 d . . . N4 N 0.0734(5) 0.5006(3) 0.8180(4) 0.0391(10) Uani 1 1 d . . . N5 N -0.3147(6) 0.2338(5) 0.6846(5) 0.0636(16) Uani 1 1 d . . . N6 N -0.0509(7) 0.0355(4) 0.8466(6) 0.0659(17) Uani 1 1 d . . . N7 N 0.3198(6) 0.2964(5) 0.9908(5) 0.0582(14) Uani 1 1 d . . . N8 N 0.0979(6) 0.2353(5) 0.6395(4) 0.0581(14) Uani 1 1 d . . . N9 N -0.0610(5) 0.3144(3) 1.0315(4) 0.0386(10) Uani 1 1 d . . . N10 N 0.3836(6) 0.5576(4) 1.1573(4) 0.0556(13) Uani 1 1 d . . . O1 O -0.0395(4) 0.7055(3) 0.7481(3) 0.0408(9) Uani 1 1 d . . . H1B H -0.0456 0.7220 0.6866 0.049 Uiso 1 1 d R . . H1A H -0.0621 0.7516 0.7817 0.049 Uiso 1 1 d R . . O2 O 0.4161(4) 0.6823(3) 0.8470(3) 0.0470(10) Uani 1 1 d . . . H2B H 0.4419 0.7035 0.7978 0.056 Uiso 1 1 d R . . H2A H 0.4696 0.6567 0.8994 0.056 Uiso 1 1 d R . . O3 O 0.3286(4) 0.6288(3) 1.0055(3) 0.0486(10) Uani 1 1 d . . . O4 O 0.5468(5) 0.7364(4) 0.7079(4) 0.0679(13) Uani 1 1 d . . . H4B H 0.6373 0.7648 0.7572 0.082 Uiso 1 1 d R . . H4A H 0.5487 0.7748 0.6653 0.082 Uiso 1 1 d R . . O5 O 0.8340(6) 0.7552(6) 0.5480(4) 0.0859(19) Uani 1 1 d . . . H5C H 0.7724 0.7953 0.5554 0.103 Uiso 1 1 d R . . H5B H 0.8592 0.7531 0.4945 0.103 Uiso 1 1 d R . . O6 O 0.8440(5) 0.8268(3) 0.8482(3) 0.0478(10) Uani 1 1 d . . . H6A H 0.8716 0.8908 0.8460 0.057 Uiso 1 1 d R . . H6B H 0.8612 0.8179 0.9130 0.057 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.046(3) 0.044(3) 0.037(3) 0.003(2) 0.015(3) 0.010(2) C2 0.057(4) 0.088(5) 0.041(4) 0.000(3) 0.025(3) 0.025(4) C3 0.084(5) 0.106(6) 0.038(4) 0.011(4) 0.031(4) 0.027(5) C4 0.068(5) 0.106(6) 0.040(4) 0.028(4) 0.023(4) 0.031(4) C5 0.046(3) 0.069(4) 0.043(4) 0.022(3) 0.017(3) 0.016(3) C6 0.047(3) 0.067(4) 0.052(4) 0.027(3) 0.022(3) 0.015(3) C7 0.081(5) 0.081(6) 0.094(6) 0.058(5) 0.039(5) 0.032(4) C8 0.084(6) 0.102(7) 0.093(7) 0.066(6) 0.039(5) 0.031(5) C9 0.094(6) 0.056(4) 0.099(7) 0.038(4) 0.043(6) 0.032(4) C10 0.048(3) 0.041(3) 0.079(5) 0.025(3) 0.031(4) 0.015(3) C11 0.046(3) 0.041(3) 0.060(4) 0.000(3) 0.024(3) 0.005(3) C12 0.059(4) 0.034(3) 0.129(8) -0.003(4) 0.035(5) 0.011(3) C13 0.057(5) 0.078(6) 0.103(8) -0.046(6) 0.033(5) -0.004(4) C14 0.054(4) 0.073(5) 0.076(5) -0.023(4) 0.035(4) -0.016(4) C15 0.067(4) 0.052(4) 0.053(4) 0.000(3) 0.031(4) -0.010(3) C16 0.035(3) 0.036(3) 0.023(3) 0.006(2) 0.013(2) 0.009(2) C17 0.033(3) 0.047(3) 0.029(3) 0.011(2) 0.014(3) 0.006(2) C18 0.042(3) 0.035(3) 0.043(3) 0.008(2) 0.020(3) 0.009(2) C19 0.031(3) 0.040(3) 0.030(3) 0.009(2) 0.014(2) 0.011(2) C20 0.027(2) 0.035(2) 0.021(2) 0.0071(19) 0.008(2) 0.0074(19) C21 0.038(3) 0.042(3) 0.037(3) 0.008(2) 0.017(3) 0.013(2) C22 0.053(4) 0.053(3) 0.037(3) 0.015(3) 0.010(3) 0.015(3) C23 0.051(5) 0.214(13) 0.091(7) 0.098(8) 0.011(5) 0.027(6) C24 0.114(7) 0.092(6) 0.072(5) 0.051(5) 0.049(5) 0.045(5) Fe1 0.0289(3) 0.0270(3) 0.0235(4) 0.0067(3) 0.0122(3) 0.0074(3) Ho1 0.02817(15) 0.02686(14) 0.02451(15) 0.00727(9) 0.01169(10) 0.00727(9) N1 0.044(3) 0.048(3) 0.033(3) 0.008(2) 0.014(2) 0.019(2) N2 0.035(2) 0.047(3) 0.047(3) 0.024(2) 0.017(2) 0.0093(19) N3 0.050(3) 0.037(2) 0.035(3) 0.002(2) 0.017(2) -0.003(2) N4 0.054(3) 0.028(2) 0.034(2) 0.0057(18) 0.019(2) 0.0035(19) N5 0.043(3) 0.089(4) 0.054(4) 0.026(3) 0.012(3) 0.013(3) N6 0.069(4) 0.039(3) 0.101(5) 0.024(3) 0.042(4) 0.016(3) N7 0.040(3) 0.076(4) 0.060(4) 0.021(3) 0.016(3) 0.021(3) N8 0.067(4) 0.076(4) 0.037(3) 0.005(3) 0.027(3) 0.018(3) N9 0.041(2) 0.045(2) 0.036(3) 0.014(2) 0.019(2) 0.014(2) N10 0.063(3) 0.064(3) 0.042(3) 0.022(3) 0.017(3) 0.024(3) O1 0.036(2) 0.060(2) 0.031(2) 0.0140(18) 0.0111(17) 0.0219(18) O2 0.0306(19) 0.069(3) 0.049(2) 0.029(2) 0.0175(19) 0.0182(18) O3 0.047(2) 0.068(3) 0.037(2) 0.028(2) 0.0157(19) 0.022(2) O4 0.054(3) 0.094(4) 0.050(3) 0.013(3) 0.022(2) 0.004(3) O5 0.078(4) 0.162(6) 0.046(3) 0.043(3) 0.033(3) 0.064(4) O6 0.061(3) 0.040(2) 0.049(3) 0.0135(18) 0.025(2) 0.0176(18) _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 O7 C25 1.338(18) . ? O7 H7B 0.8501 . ? O7 H8B 0.8705 . ? C25 H25A 0.9600 . ? C25 H25B 0.9601 . ? C25 H25C 0.9600 . ? O8 C26 1.381(17) . ? O8 H7B 0.7658 . ? O8 H8B 0.8500 . ? C26 H26A 0.9601 . ? C26 H26B 0.9600 . ? C26 H26C 0.9601 . ? C26 H27B 1.0795 . ? C26 H27C 1.0031 . ? C27 O9 1.353(18) . ? C27 H26A 0.8530 . ? C27 H26B 1.2308 . ? C27 H26C 1.3533 . ? C27 H27A 0.9601 . ? C27 H27B 0.9600 . ? C27 H27C 0.9599 . ? O9 H26A 0.8215 . ? O9 H9B 0.8500 . ? C1 N1 1.317(7) . ? C1 C2 1.343(8) . ? C1 H1 0.9300 . ? C2 C3 1.352(11) . ? C2 H2 0.9300 . ? C3 C4 1.313(12) . ? C3 H3 0.9300 . ? C4 C5 1.360(10) . ? C4 H4 0.9300 . ? C5 N1 1.391(8) . ? C5 C6 1.526(10) . ? C6 N2 1.297(8) . ? C6 C7 1.395(9) . ? C7 C8 1.356(13) . ? C7 H7 0.9300 . ? C8 C9 1.323(13) . ? C8 H8 0.9300 . ? C9 C10 1.413(9) . ? C9 H9 0.9300 . ? C10 N2 1.363(8) . ? C10 C11 1.512(10) . ? C11 N3 1.367(8) . ? C11 C12 1.377(9) . ? C12 C13 1.347(14) . ? C12 H12 0.9300 . ? C13 C14 1.323(14) . ? C13 H13 0.9300 . ? C14 C15 1.360(10) . ? C14 H14 0.9300 . ? C15 N3 1.312(9) . ? C15 H15 0.9300 . ? C16 N4 1.142(7) . ? C16 Fe1 1.932(5) . ? C17 N5 1.130(8) . ? C17 Fe1 1.941(6) . ? C18 N6 1.149(7) . ? C18 Fe1 1.932(5) . ? C19 N7 1.138(7) . ? C19 Fe1 1.927(5) . ? C20 N9 1.157(7) . ? C20 Fe1 1.915(5) . ? C21 N8 1.138(7) . ? C21 Fe1 1.941(5) . ? C22 O3 1.247(7) . ? C22 N10 1.299(8) . ? C22 H22 0.9300 . ? C23 N10 1.450(11) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N10 1.440(9) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? Ho1 O2 2.307(4) . ? Ho1 O3 2.335(4) . ? Ho1 O1 2.354(4) . ? Ho1 N4 2.402(4) . ? Ho1 N9 2.447(4) 2_567 ? Ho1 N3 2.457(5) . ? Ho1 N1 2.460(5) . ? Ho1 N2 2.470(4) . ? N9 Ho1 2.447(4) 2_567 ? O1 H1B 0.8572 . ? O1 H1A 0.8543 . ? O2 H2B 0.8459 . ? O2 H2A 0.8643 . ? O4 H4B 0.8999 . ? O4 H4A 0.8017 . ? O5 H5C 0.9333 . ? O5 H5B 0.8499 . ? O6 H6A 0.8500 . ? O6 H6B 0.8499 . ? 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 C25 O7 H7B 109.3 . . ? C25 O7 H8B 99.0 . . ? H7B O7 H8B 11.2 . . ? O7 C25 H25A 109.7 . . ? O7 C25 H25B 108.7 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 110.0 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 O8 H7B 109.5 . . ? C26 O8 H8B 119.1 . . ? H7B O8 H8B 10.4 . . ? O8 C26 H26A 109.5 . . ? O8 C26 H26B 109.7 . . ? H26A C26 H26B 109.5 . . ? O8 C26 H26C 109.2 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O8 C26 H27B 117.5 . . ? H26A C26 H27B 69.4 . . ? H26B C26 H27B 40.7 . . ? H26C C26 H27B 130.7 . . ? O8 C26 H27C 141.6 . . ? H26A C26 H27C 96.7 . . ? H26B C26 H27C 86.2 . . ? H26C C26 H27C 33.3 . . ? H27B C26 H27C 97.6 . . ? O9 C27 H26A 35.3 . . ? O9 C27 H26B 130.2 . . ? H26A C27 H26B 95.9 . . ? O9 C27 H26C 90.1 . . ? H26A C27 H26C 87.5 . . ? H26B C27 H26C 74.5 . . ? O9 C27 H27A 109.4 . . ? H26A C27 H27A 135.2 . . ? H26B C27 H27A 117.3 . . ? H26C C27 H27A 128.2 . . ? O9 C27 H27B 113.0 . . ? H26A C27 H27B 79.8 . . ? H26B C27 H27B 35.6 . . ? H26C C27 H27B 105.3 . . ? H27A C27 H27B 109.5 . . ? O9 C27 H27C 105.9 . . ? H26A C27 H27C 107.9 . . ? H26B C27 H27C 74.4 . . ? H26C C27 H27C 20.4 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C27 O9 H26A 36.9 . . ? C27 O9 H9B 114.0 . . ? H26A O9 H9B 145.7 . . ? N1 C1 C2 122.6(6) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 121.6(7) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C4 C3 C2 117.8(7) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 120.8(7) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 N1 121.6(7) . . ? C4 C5 C6 123.2(6) . . ? N1 C5 C6 115.1(5) . . ? N2 C6 C7 122.9(7) . . ? N2 C6 C5 115.6(5) . . ? C7 C6 C5 121.5(7) . . ? C8 C7 C6 118.8(9) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 120.0(8) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.7(8) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? N2 C10 C9 120.1(7) . . ? N2 C10 C11 116.0(5) . . ? C9 C10 C11 123.8(7) . . ? N3 C11 C12 121.9(7) . . ? N3 C11 C10 114.2(5) . . ? C12 C11 C10 123.8(7) . . ? C13 C12 C11 120.0(8) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 118.3(7) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 120.3(9) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? N3 C15 C14 124.5(8) . . ? N3 C15 H15 117.7 . . ? C14 C15 H15 117.7 . . ? N4 C16 Fe1 177.4(5) . . ? N5 C17 Fe1 179.2(6) . . ? N6 C18 Fe1 179.7(5) . . ? N7 C19 Fe1 176.6(5) . . ? N9 C20 Fe1 179.5(5) . . ? N8 C21 Fe1 176.8(5) . . ? O3 C22 N10 124.9(6) . . ? O3 C22 H22 117.6 . . ? N10 C22 H22 117.6 . . ? N10 C23 H23A 109.5 . . ? N10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N10 C24 H24A 109.5 . . ? N10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 Fe1 C19 87.2(2) . . ? C20 Fe1 C18 90.4(2) . . ? C19 Fe1 C18 88.9(2) . . ? C20 Fe1 C16 89.6(2) . . ? C19 Fe1 C16 90.2(2) . . ? C18 Fe1 C16 179.1(3) . . ? C20 Fe1 C21 176.6(2) . . ? C19 Fe1 C21 90.0(2) . . ? C18 Fe1 C21 91.5(2) . . ? C16 Fe1 C21 88.4(2) . . ? C20 Fe1 C17 90.1(2) . . ? C19 Fe1 C17 176.9(2) . . ? C18 Fe1 C17 89.6(2) . . ? C16 Fe1 C17 91.3(2) . . ? C21 Fe1 C17 92.7(2) . . ? O2 Ho1 O3 70.84(14) . . ? O2 Ho1 O1 144.81(14) . . ? O3 Ho1 O1 144.16(13) . . ? O2 Ho1 N4 103.54(15) . . ? O3 Ho1 N4 77.60(16) . . ? O1 Ho1 N4 86.60(16) . . ? O2 Ho1 N9 142.49(16) . 2_567 ? O3 Ho1 N9 73.76(15) . 2_567 ? O1 Ho1 N9 71.96(14) . 2_567 ? N4 Ho1 N9 80.31(15) . 2_567 ? O2 Ho1 N3 88.88(16) . . ? O3 Ho1 N3 80.77(16) . . ? O1 Ho1 N3 99.09(16) . . ? N4 Ho1 N3 149.73(15) . . ? N9 Ho1 N3 73.44(16) 2_567 . ? O2 Ho1 N1 70.56(15) . . ? O3 Ho1 N1 128.53(15) . . ? O1 Ho1 N1 78.49(14) . . ? N4 Ho1 N1 79.73(15) . . ? N9 Ho1 N1 145.06(16) 2_567 . ? N3 Ho1 N1 130.53(15) . . ? O2 Ho1 N2 79.59(14) . . ? O3 Ho1 N2 135.40(15) . . ? O1 Ho1 N2 72.88(14) . . ? N4 Ho1 N2 143.11(16) . . ? N9 Ho1 N2 119.66(15) 2_567 . ? N3 Ho1 N2 65.72(16) . . ? N1 Ho1 N2 66.52(16) . . ? C1 N1 C5 115.4(5) . . ? C1 N1 Ho1 123.4(4) . . ? C5 N1 Ho1 119.0(4) . . ? C6 N2 C10 118.3(5) . . ? C6 N2 Ho1 121.2(4) . . ? C10 N2 Ho1 118.3(4) . . ? C15 N3 C11 115.0(5) . . ? C15 N3 Ho1 123.8(4) . . ? C11 N3 Ho1 120.5(4) . . ? C16 N4 Ho1 164.5(5) . . ? C20 N9 Ho1 161.5(4) . 2_567 ? C22 N10 C24 122.3(7) . . ? C22 N10 C23 120.4(6) . . ? C24 N10 C23 117.2(7) . . ? Ho1 O1 H1B 111.7 . . ? Ho1 O1 H1A 112.6 . . ? H1B O1 H1A 108.7 . . ? Ho1 O2 H2B 122.3 . . ? Ho1 O2 H2A 114.3 . . ? H2B O2 H2A 123.4 . . ? C22 O3 Ho1 132.5(4) . . ? H4B O4 H4A 97.0 . . ? H5C O5 H5B 122.5 . . ? H6A O6 H6B 110.1 . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.420 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.169 _database_code_depnum_ccdc_archive 'CCDC 896258' ####################################################################### # # 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_4-hoco _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H66 Co2 Ho2 N20 O15' _chemical_formula_weight 1634.95 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' 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' Co Co 0.3494 0.9721 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.179(2) _cell_length_b 13.196(3) _cell_length_c 13.425(3) _cell_angle_alpha 93.782(4) _cell_angle_beta 111.077(2) _cell_angle_gamma 102.158(3) _cell_volume 1624.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9986 _cell_measurement_theta_min 2.466 _cell_measurement_theta_max 27.580 _exptl_crystal_description needle _exptl_crystal_colour whitish-red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 814 _exptl_absorpt_coefficient_mu 2.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5866 _exptl_absorpt_correction_T_max 0.7158 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11548 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5621 _reflns_number_gt 5273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5621 _refine_ls_number_parameters 428 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_restrained_S_all 1.234 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1684(5) 0.5363(4) 0.6213(4) 0.0211(10) Uani 1 1 d . . . H1 H 0.1576 0.4827 0.6616 0.025 Uiso 1 1 calc R . . C2 C 0.1852(6) 0.5128(5) 0.5253(4) 0.0300(12) Uani 1 1 d . . . H2 H 0.1879 0.4455 0.5024 0.036 Uiso 1 1 calc R . . C3 C 0.1978(6) 0.5928(5) 0.4636(4) 0.0349(14) Uani 1 1 d . . . H3 H 0.2074 0.5793 0.3980 0.042 Uiso 1 1 calc R . . C4 C 0.1960(6) 0.6888(5) 0.5000(4) 0.0309(12) Uani 1 1 d . . . H4 H 0.2019 0.7421 0.4586 0.037 Uiso 1 1 calc R . . C5 C 0.1854(5) 0.7099(4) 0.5986(4) 0.0226(10) Uani 1 1 d . . . C6 C 0.1958(6) 0.8189(4) 0.6464(4) 0.0258(11) Uani 1 1 d . . . C7 C 0.1752(6) 0.8989(5) 0.5831(5) 0.0342(13) Uani 1 1 d . . . H7 H 0.1549 0.8873 0.5094 0.041 Uiso 1 1 calc R . . C8 C 0.1867(7) 0.9963(5) 0.6358(5) 0.0385(14) Uani 1 1 d . . . H8 H 0.1710 1.0510 0.5964 0.046 Uiso 1 1 calc R . . C9 C 0.2200(6) 1.0131(5) 0.7428(5) 0.0324(13) Uani 1 1 d . . . H9 H 0.2273 1.0788 0.7772 0.039 Uiso 1 1 calc R . . C10 C 0.2437(6) 0.9310(4) 0.8018(4) 0.0245(11) Uani 1 1 d . . . C11 C 0.2925(6) 0.9434(4) 0.9215(4) 0.0225(10) Uani 1 1 d . . . C12 C 0.3344(6) 1.0409(4) 0.9856(5) 0.0321(13) Uani 1 1 d . . . H12 H 0.3271 1.1012 0.9540 0.038 Uiso 1 1 calc R . . C13 C 0.3866(6) 1.0470(5) 1.0959(5) 0.0351(14) Uani 1 1 d . . . H13 H 0.4171 1.1114 1.1404 0.042 Uiso 1 1 calc R . . C14 C 0.3927(6) 0.9564(4) 1.1389(5) 0.0318(13) Uani 1 1 d . . . H14 H 0.4265 0.9589 1.2135 0.038 Uiso 1 1 calc R . . C15 C 0.3497(6) 0.8628(4) 1.0734(4) 0.0270(12) Uani 1 1 d . . . H15 H 0.3550 0.8023 1.1048 0.032 Uiso 1 1 calc R . . C16 C 0.0434(5) 0.4109(4) 0.8235(3) 0.0154(9) Uani 1 1 d . . . C17 C -0.1923(5) 0.2444(4) 0.7440(4) 0.0187(10) Uani 1 1 d . . . C18 C -0.0264(5) 0.1222(4) 0.8444(4) 0.0176(10) Uani 1 1 d . . . C19 C 0.2032(5) 0.2870(4) 0.9314(4) 0.0168(10) Uani 1 1 d . . . C20 C -0.0367(5) 0.2961(4) 0.9566(4) 0.0162(9) Uani 1 1 d . . . C21 C 0.0634(5) 0.2459(4) 0.7151(4) 0.0180(10) Uani 1 1 d . . . C22 C 0.2972(6) 0.5675(4) 1.0635(4) 0.0226(11) Uani 1 1 d . . . H22 H 0.2022 0.5265 1.0395 0.027 Uiso 1 1 calc R . . C23 C 0.5356(7) 0.6195(7) 1.2040(6) 0.056(2) Uani 1 1 d . . . H23A H 0.5581 0.6568 1.1508 0.084 Uiso 1 1 calc R . . H23B H 0.5980 0.5730 1.2263 0.084 Uiso 1 1 calc R . . H23C H 0.5503 0.6686 1.2654 0.084 Uiso 1 1 calc R . . C24 C 0.3377(7) 0.4895(5) 1.2257(5) 0.0381(14) Uani 1 1 d . . . H24A H 0.2378 0.4522 1.1867 0.057 Uiso 1 1 calc R . . H24B H 0.3467 0.5303 1.2908 0.057 Uiso 1 1 calc R . . H24C H 0.3968 0.4404 1.2435 0.057 Uiso 1 1 calc R . . Co1 Co 0.00809(7) 0.26760(5) 0.83534(5) 0.01282(15) Uani 1 1 d . . . Ho1 Ho 0.19196(2) 0.681870(14) 0.846637(14) 0.01254(10) Uani 1 1 d . . . N1 N 0.1671(5) 0.6329(3) 0.6592(3) 0.0216(9) Uani 1 1 d . . . N2 N 0.2284(4) 0.8339(3) 0.7521(3) 0.0197(9) Uani 1 1 d . . . N3 N 0.2994(5) 0.8537(3) 0.9645(3) 0.0198(9) Uani 1 1 d . . . N4 N 0.0709(5) 0.4996(3) 0.8168(3) 0.0216(9) Uani 1 1 d . . . N5 N -0.3134(5) 0.2295(4) 0.6905(3) 0.0296(10) Uani 1 1 d . . . N6 N -0.0504(5) 0.0326(4) 0.8471(4) 0.0297(10) Uani 1 1 d . . . N7 N 0.3192(5) 0.2985(4) 0.9947(4) 0.0281(10) Uani 1 1 d . . . N8 N 0.1014(5) 0.2379(4) 0.6456(3) 0.0286(10) Uani 1 1 d . . . N9 N -0.0608(4) 0.3152(3) 1.0334(3) 0.0172(8) Uani 1 1 d . . . N10 N 0.3861(5) 0.5596(4) 1.1582(3) 0.0273(10) Uani 1 1 d . . . O1 O -0.0406(4) 0.7040(3) 0.7456(3) 0.0210(7) Uani 1 1 d . . . H1B H -0.0466 0.7205 0.6842 0.025 Uiso 1 1 d R . . H1A H -0.0632 0.7501 0.7793 0.025 Uiso 1 1 d R . . O2 O 0.4181(4) 0.6813(3) 0.8425(3) 0.0221(7) Uani 1 1 d . . . H2B H 0.4438 0.7025 0.7933 0.026 Uiso 1 1 d R . . H2A H 0.4715 0.6558 0.8948 0.026 Uiso 1 1 d R . . O3 O 0.3294(4) 0.6258(3) 1.0020(3) 0.0229(7) Uani 1 1 d . . . O4 O 0.5403(5) 0.7468(4) 0.6965(3) 0.0429(11) Uani 1 1 d . . . H4D H 0.5379 0.7301 0.6336 0.051 Uiso 1 1 d R . . H4E H 0.6287 0.7689 0.7396 0.051 Uiso 1 1 d R . . O5 O 0.8277(5) 0.7495(4) 0.5420(3) 0.0385(10) Uani 1 1 d . . . H5C H 0.8420 0.7498 0.4834 0.046 Uiso 1 1 d R . . H5D H 0.7442 0.7095 0.5290 0.046 Uiso 1 1 d R . . O6 O 0.8314(4) 0.8204(3) 0.8422(3) 0.0243(8) Uani 1 1 d . . . H6B H 0.8425 0.8070 0.9053 0.029 Uiso 1 1 d R . . H6A H 0.8650 0.8852 0.8424 0.029 Uiso 1 1 d R . . O7 O 0.5615(9) 0.8045(8) 0.5095(6) 0.046(2) Uani 0.50 1 d P A 1 H7A H 0.5078 0.7651 0.4498 0.056 Uiso 0.50 1 d PR A 1 C25 C 0.5081(14) 0.8947(12) 0.5171(9) 0.048(4) Uani 0.50 1 d P A 1 H25A H 0.5534 0.9311 0.5900 0.072 Uiso 0.50 1 calc PR A 1 H25B H 0.4046 0.8736 0.4970 0.072 Uiso 0.50 1 calc PR A 1 H25C H 0.5302 0.9403 0.4693 0.072 Uiso 0.50 1 calc PR A 1 O8 O 0.8049(10) 0.9438(7) 0.6031(7) 0.042(2) Uani 0.50 1 d P B 2 H8A H 0.7842 0.8785 0.5801 0.051 Uiso 0.50 1 d PR B 2 C26 C 0.7070(18) 0.9991(10) 0.6136(11) 0.056(4) Uani 0.50 1 d P B 2 H26A H 0.6671 0.9710 0.6637 0.084 Uiso 0.50 1 calc PR B 2 H26B H 0.6299 0.9927 0.5445 0.084 Uiso 0.50 1 calc PR B 2 H26C H 0.7565 1.0718 0.6397 0.084 Uiso 0.50 1 calc PR B 2 O9 O 0.5461(16) 0.6207(13) 0.5169(12) 0.108(5) Uani 0.50 1 d PU C 2 H9A H 0.4785 0.6206 0.4570 0.130 Uiso 0.50 1 d PR C 2 H9B H 0.5488 0.5584 0.5281 0.130 Uiso 0.50 1 d PR 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 C1 0.018(3) 0.022(3) 0.020(2) -0.0006(19) 0.006(2) 0.001(2) C2 0.026(3) 0.040(3) 0.024(3) -0.001(2) 0.012(2) 0.008(2) C3 0.029(3) 0.060(4) 0.019(3) 0.007(3) 0.014(2) 0.008(3) C4 0.030(3) 0.044(3) 0.018(2) 0.007(2) 0.011(2) 0.005(3) C5 0.018(3) 0.025(3) 0.023(2) 0.006(2) 0.007(2) 0.002(2) C6 0.022(3) 0.035(3) 0.023(3) 0.010(2) 0.011(2) 0.007(2) C7 0.031(3) 0.035(3) 0.036(3) 0.016(2) 0.012(3) 0.005(3) C8 0.031(3) 0.041(3) 0.043(3) 0.023(3) 0.012(3) 0.009(3) C9 0.035(3) 0.027(3) 0.040(3) 0.009(2) 0.017(3) 0.009(2) C10 0.021(3) 0.022(3) 0.036(3) 0.010(2) 0.017(2) 0.007(2) C11 0.019(3) 0.023(3) 0.028(3) 0.001(2) 0.013(2) 0.004(2) C12 0.025(3) 0.021(3) 0.052(4) 0.003(2) 0.017(3) 0.005(2) C13 0.025(3) 0.035(3) 0.041(3) -0.014(3) 0.016(3) 0.000(2) C14 0.024(3) 0.033(3) 0.035(3) -0.008(2) 0.018(3) -0.009(2) C15 0.026(3) 0.027(3) 0.024(3) 0.000(2) 0.011(2) -0.004(2) C16 0.013(2) 0.019(3) 0.012(2) 0.0007(17) 0.0033(18) 0.0009(19) C17 0.020(3) 0.021(2) 0.015(2) 0.0047(19) 0.009(2) 0.000(2) C18 0.016(2) 0.021(3) 0.016(2) 0.0018(18) 0.0070(19) 0.0026(19) C19 0.016(3) 0.016(2) 0.019(2) 0.0027(18) 0.011(2) -0.0002(19) C20 0.012(2) 0.016(2) 0.018(2) 0.0032(18) 0.0032(19) 0.0027(18) C21 0.016(2) 0.023(2) 0.013(2) 0.0019(18) 0.0037(19) 0.003(2) C22 0.022(3) 0.021(2) 0.022(2) 0.001(2) 0.007(2) 0.003(2) C23 0.027(4) 0.095(6) 0.042(4) 0.032(4) 0.008(3) 0.009(4) C24 0.049(4) 0.044(4) 0.029(3) 0.020(3) 0.020(3) 0.014(3) Co1 0.0124(3) 0.0140(3) 0.0116(3) 0.0013(2) 0.0056(2) 0.0008(2) Ho1 0.01213(14) 0.01327(14) 0.01201(14) 0.00208(8) 0.00564(10) 0.00090(9) N1 0.021(2) 0.031(2) 0.0124(19) 0.0012(16) 0.0044(17) 0.0088(18) N2 0.012(2) 0.027(2) 0.018(2) 0.0053(17) 0.0061(16) 0.0005(17) N3 0.019(2) 0.019(2) 0.020(2) 0.0012(16) 0.0093(17) -0.0023(17) N4 0.024(2) 0.022(2) 0.019(2) 0.0028(17) 0.0099(18) 0.0029(19) N5 0.020(3) 0.044(3) 0.019(2) 0.0072(19) 0.006(2) -0.001(2) N6 0.029(3) 0.027(3) 0.037(3) 0.008(2) 0.015(2) 0.008(2) N7 0.018(3) 0.035(3) 0.029(2) 0.0047(19) 0.006(2) 0.007(2) N8 0.028(3) 0.039(3) 0.021(2) 0.0029(19) 0.013(2) 0.006(2) N9 0.018(2) 0.022(2) 0.0125(19) 0.0023(15) 0.0075(17) 0.0027(17) N10 0.028(3) 0.033(2) 0.024(2) 0.0118(18) 0.010(2) 0.010(2) O1 0.0178(18) 0.0318(19) 0.0161(16) 0.0071(14) 0.0074(14) 0.0089(15) O2 0.0146(18) 0.031(2) 0.0199(17) 0.0079(14) 0.0065(14) 0.0043(15) O3 0.0215(19) 0.0278(19) 0.0213(17) 0.0095(14) 0.0086(15) 0.0080(15) O4 0.028(2) 0.061(3) 0.034(2) -0.0085(19) 0.0151(19) -0.002(2) O5 0.032(2) 0.065(3) 0.026(2) 0.0156(19) 0.0176(18) 0.014(2) O6 0.031(2) 0.0202(18) 0.0292(18) 0.0112(14) 0.0175(16) 0.0089(16) O7 0.035(5) 0.084(7) 0.019(4) 0.009(4) 0.009(4) 0.013(5) C25 0.027(7) 0.073(10) 0.019(6) -0.010(6) -0.003(5) -0.011(7) O8 0.043(5) 0.035(5) 0.039(5) 0.001(4) 0.012(4) -0.002(4) C26 0.076(11) 0.031(7) 0.037(7) 0.002(6) 0.005(7) -0.007(7) O9 0.081(8) 0.136(9) 0.091(8) -0.038(6) 0.042(6) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.346(6) . ? C1 C2 1.383(7) . ? C1 H1 0.9300 . ? C2 C3 1.396(8) . ? C2 H2 0.9300 . ? C3 C4 1.334(9) . ? C3 H3 0.9300 . ? C4 C5 1.381(7) . ? C4 H4 0.9300 . ? C5 N1 1.367(6) . ? C5 C6 1.502(7) . ? C6 N2 1.326(6) . ? C6 C7 1.401(8) . ? C7 C8 1.387(9) . ? C7 H7 0.9300 . ? C8 C9 1.343(8) . ? C8 H8 0.9300 . ? C9 C10 1.395(8) . ? C9 H9 0.9300 . ? C10 N2 1.357(7) . ? C10 C11 1.487(7) . ? C11 N3 1.355(7) . ? C11 C12 1.391(7) . ? C12 C13 1.372(9) . ? C12 H12 0.9300 . ? C13 C14 1.364(9) . ? C13 H13 0.9300 . ? C14 C15 1.358(8) . ? C14 H14 0.9300 . ? C15 N3 1.351(6) . ? C15 H15 0.9300 . ? C16 N4 1.162(6) . ? C16 Co1 1.878(5) . ? C17 N5 1.147(7) . ? C17 Co1 1.910(5) . ? C18 N6 1.161(7) . ? C18 Co1 1.896(5) . ? C19 N7 1.151(6) . ? C19 Co1 1.890(5) . ? C20 N9 1.165(6) . ? C20 Co1 1.878(5) . ? C21 N8 1.137(6) . ? C21 Co1 1.915(5) . ? C22 O3 1.246(6) . ? C22 N10 1.295(7) . ? C22 H22 0.9300 . ? C23 N10 1.441(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N10 1.468(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? Ho1 O3 2.323(3) . ? Ho1 O2 2.324(3) . ? Ho1 O1 2.359(3) . ? Ho1 N4 2.394(4) . ? Ho1 N9 2.437(4) 2_567 ? Ho1 N1 2.464(4) . ? Ho1 N3 2.466(4) . ? Ho1 N2 2.477(4) . ? N9 Ho1 2.437(4) 2_567 ? O1 H1B 0.8511 . ? O1 H1A 0.8510 . ? O2 H2B 0.8377 . ? O2 H2A 0.8585 . ? O4 H4D 0.8501 . ? O4 H4E 0.8500 . ? O5 H5C 0.8499 . ? O5 H5D 0.8501 . ? O6 H6B 0.8500 . ? O6 H6A 0.8505 . ? O7 C25 1.421(17) . ? O7 H7A 0.8501 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? O8 C26 1.393(18) . ? O8 H8A 0.8499 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? O9 H9A 0.8499 . ? O9 H9B 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.2(5) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.3(5) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.1(5) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.7(5) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 121.8(5) . . ? N1 C5 C6 116.1(4) . . ? C4 C5 C6 122.1(5) . . ? N2 C6 C7 123.0(5) . . ? N2 C6 C5 115.3(4) . . ? C7 C6 C5 121.7(5) . . ? C8 C7 C6 116.7(5) . . ? C8 C7 H7 121.7 . . ? C6 C7 H7 121.7 . . ? C9 C8 C7 121.2(5) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.3(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 120.9(5) . . ? N2 C10 C11 115.5(4) . . ? C9 C10 C11 123.5(5) . . ? N3 C11 C12 122.0(5) . . ? N3 C11 C10 115.5(4) . . ? C12 C11 C10 122.4(5) . . ? C13 C12 C11 119.2(5) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 118.6(5) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C15 C14 C13 120.3(6) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? N3 C15 C14 122.9(5) . . ? N3 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? N4 C16 Co1 177.3(4) . . ? N5 C17 Co1 178.7(4) . . ? N6 C18 Co1 178.1(5) . . ? N7 C19 Co1 176.0(4) . . ? N9 C20 Co1 178.2(4) . . ? N8 C21 Co1 176.5(5) . . ? O3 C22 N10 125.0(5) . . ? O3 C22 H22 117.5 . . ? N10 C22 H22 117.5 . . ? N10 C23 H23A 109.5 . . ? N10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N10 C24 H24A 109.5 . . ? N10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 Co1 C16 89.90(19) . . ? C20 Co1 C19 87.65(19) . . ? C16 Co1 C19 90.5(2) . . ? C20 Co1 C18 91.49(19) . . ? C16 Co1 C18 178.62(19) . . ? C19 Co1 C18 89.6(2) . . ? C20 Co1 C17 89.9(2) . . ? C16 Co1 C17 91.4(2) . . ? C19 Co1 C17 176.90(19) . . ? C18 Co1 C17 88.6(2) . . ? C20 Co1 C21 176.5(2) . . ? C16 Co1 C21 87.52(19) . . ? C19 Co1 C21 90.06(19) . . ? C18 Co1 C21 91.1(2) . . ? C17 Co1 C21 92.5(2) . . ? O3 Ho1 O2 70.87(12) . . ? O3 Ho1 O1 144.48(12) . . ? O2 Ho1 O1 144.20(11) . . ? O3 Ho1 N4 77.82(14) . . ? O2 Ho1 N4 103.90(14) . . ? O1 Ho1 N4 85.07(14) . . ? O3 Ho1 N9 74.55(13) . 2_567 ? O2 Ho1 N9 143.34(12) . 2_567 ? O1 Ho1 N9 71.94(12) . 2_567 ? N4 Ho1 N9 79.94(14) . 2_567 ? O3 Ho1 N1 128.35(13) . . ? O2 Ho1 N1 70.11(13) . . ? O1 Ho1 N1 77.67(12) . . ? N4 Ho1 N1 80.14(14) . . ? N9 Ho1 N1 144.79(14) 2_567 . ? O3 Ho1 N3 81.94(13) . . ? O2 Ho1 N3 89.64(13) . . ? O1 Ho1 N3 99.45(13) . . ? N4 Ho1 N3 150.20(13) . . ? N9 Ho1 N3 73.69(13) 2_567 . ? N1 Ho1 N3 129.66(14) . . ? O3 Ho1 N2 135.80(13) . . ? O2 Ho1 N2 79.95(12) . . ? O1 Ho1 N2 72.97(12) . . ? N4 Ho1 N2 142.77(13) . . ? N9 Ho1 N2 119.10(13) 2_567 . ? N1 Ho1 N2 66.22(14) . . ? N3 Ho1 N2 65.07(13) . . ? C1 N1 C5 116.7(4) . . ? C1 N1 Ho1 122.2(3) . . ? C5 N1 Ho1 119.4(3) . . ? C6 N2 C10 118.9(4) . . ? C6 N2 Ho1 120.1(3) . . ? C10 N2 Ho1 118.7(3) . . ? C15 N3 C11 117.0(4) . . ? C15 N3 Ho1 122.2(3) . . ? C11 N3 Ho1 120.3(3) . . ? C16 N4 Ho1 163.0(4) . . ? C20 N9 Ho1 160.5(4) . 2_567 ? C22 N10 C23 122.4(5) . . ? C22 N10 C24 121.1(5) . . ? C23 N10 C24 116.5(5) . . ? Ho1 O1 H1B 111.7 . . ? Ho1 O1 H1A 111.8 . . ? H1B O1 H1A 109.3 . . ? Ho1 O2 H2B 122.9 . . ? Ho1 O2 H2A 113.9 . . ? H2B O2 H2A 123.2 . . ? C22 O3 Ho1 133.3(3) . . ? H4D O4 H4E 108.4 . . ? H5C O5 H5D 108.5 . . ? H6B O6 H6A 112.0 . . ? C25 O7 H7A 109.2 . . ? C26 O8 H8A 125.5 . . ? O8 C26 H26A 109.5 . . ? O8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? H9A O9 H9B 110.7 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.500 _refine_diff_density_min -1.232 _refine_diff_density_rms 0.274 _database_code_depnum_ccdc_archive 'CCDC 896259'