# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email agapie@caltech.edu _publ_contact_author_name T.Agapie loop_ _publ_author_name E.Tsui J.S.Kanady M.W.Day T.Agapie # Attachment '- jsk02.cif' data_jsk02 _database_code_depnum_ccdc_archive 'CCDC 777599' #TrackingRef '- jsk02.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H48 Co3 N6 O9' _chemical_formula_sum 'C63 H48 Co3 N6 O9' _chemical_formula_weight 1209.86 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 20.8675(10) _cell_length_b 20.8675(10) _cell_length_c 10.5670(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3985.0(4) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9893 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.53 _exptl_crystal_description Fragment _exptl_crystal_colour Red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1863 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6512 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 10 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28754 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 30.10 _reflns_number_total 5191 _reflns_number_gt 4777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ad _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(11) _refine_ls_number_reflns 5191 _refine_ls_number_parameters 262 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 2.172 _refine_ls_restrained_S_all 2.172 _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 Co1 Co 0.278103(17) 0.563630(17) 0.93578(3) 0.02626(8) Uani 1 1 d . . . O1 O 0.37802(9) 0.61847(8) 0.84425(17) 0.0234(4) Uani 1 1 d . A . N1 N 0.16277(12) 0.51811(12) 1.0019(2) 0.0326(5) Uani 1 1 d . A . N2 N 0.28078(11) 0.47803(11) 0.83753(19) 0.0263(4) Uani 1 1 d . A . C1 C 0.27595(13) 0.68188(13) 0.5878(2) 0.0260(5) Uani 1 1 d . . . H1 H 0.2366 0.6923 0.5845 0.031 Uiso 1 1 calc R . . C2 C 0.26038(13) 0.60898(13) 0.5902(2) 0.0247(5) Uani 1 1 d . . . C3 C 0.18295(13) 0.54576(13) 0.6017(2) 0.0261(5) Uani 1 1 d . . . C4 C 0.15560(14) 0.49421(14) 0.5044(3) 0.0322(6) Uani 1 1 d . . . H4 H 0.1855 0.5018 0.4319 0.039 Uiso 1 1 calc R . . C5 C 0.08524(14) 0.43141(14) 0.5101(3) 0.0331(6) Uani 1 1 d . . . H5 H 0.0673 0.3968 0.4424 0.040 Uiso 1 1 calc R . . C6 C 0.04172(14) 0.42038(14) 0.6173(3) 0.0332(6) Uani 1 1 d . . . H6 H -0.0060 0.3777 0.6231 0.040 Uiso 1 1 calc R . . C7 C 0.06759(14) 0.47092(14) 0.7141(3) 0.0310(6) Uani 1 1 d . . . H7 H 0.0370 0.4625 0.7859 0.037 Uiso 1 1 calc R . . C8 C 0.13807(13) 0.53498(13) 0.7105(2) 0.0264(5) Uani 1 1 d . . . C9 C 0.16485(12) 0.58965(12) 0.8221(2) 0.0245(5) Uani 1 1 d . . . C10 C 0.12619(15) 0.54753(13) 0.9450(2) 0.0300(6) Uani 1 1 d . . . C11 C 0.06120(14) 0.54018(15) 0.9945(3) 0.0371(6) Uani 1 1 d . A . H11 H 0.0357 0.5608 0.9516 0.044 Uiso 1 1 calc R . . C12 C 0.03420(16) 0.50251(17) 1.1066(3) 0.0478(8) Uani 1 1 d . . . H12 H -0.0102 0.4970 1.1418 0.057 Uiso 1 1 calc R A . C13 C 0.07141(16) 0.47312(18) 1.1669(3) 0.0534(9) Uani 1 1 d . A . H13 H 0.0540 0.4479 1.2452 0.064 Uiso 1 1 calc R . . C14 C 0.13464(16) 0.48079(17) 1.1119(3) 0.0456(8) Uani 1 1 d . . . H14 H 0.1597 0.4590 1.1526 0.055 Uiso 1 1 calc R A . C15 C 0.34798(13) 0.49421(13) 0.7967(2) 0.0268(5) Uani 1 1 d . . . C16 C 0.36095(15) 0.44233(14) 0.7378(3) 0.0375(6) Uani 1 1 d . A . H16 H 0.4092 0.4547 0.7104 0.045 Uiso 1 1 calc R . . C17 C 0.30048(16) 0.37098(15) 0.7201(3) 0.0453(7) Uani 1 1 d . . . H17 H 0.3074 0.3341 0.6801 0.054 Uiso 1 1 calc R A . C18 C 0.23167(16) 0.35448(15) 0.7603(3) 0.0412(7) Uani 1 1 d . A . H18 H 0.1902 0.3064 0.7482 0.049 Uiso 1 1 calc R . . C19 C 0.22372(15) 0.40970(14) 0.8193(3) 0.0336(6) Uani 1 1 d . . . H19 H 0.1760 0.3985 0.8477 0.040 Uiso 1 1 calc R A . O2A O 0.3058(4) 0.5351(4) 1.1064(6) 0.0298(11) Uani 0.727(2) 1 d PD A 1 O3A O 0.2407(2) 0.41094(16) 1.1217(3) 0.0656(10) Uani 0.727(2) 1 d PD A 1 C20A C 0.2883(2) 0.4730(2) 1.1604(4) 0.0406(10) Uani 0.727(2) 1 d PD A 1 C21A C 0.3207(3) 0.4751(3) 1.2899(5) 0.0603(14) Uani 0.727(2) 1 d PD A 1 H21A H 0.2816 0.4396 1.3460 0.090 Uiso 0.727(2) 1 calc PR A 1 H21B H 0.3419 0.5250 1.3254 0.090 Uiso 0.727(2) 1 calc PR A 1 H21C H 0.3596 0.4620 1.2819 0.090 Uiso 0.727(2) 1 calc PR A 1 O2B O 0.2357(13) 0.6902(16) 1.120(2) 0.062(8) Uiso 0.273(2) 1 d PD . -2 O3B O 0.3221(4) 0.6685(6) 1.0502(3) 0.0051(13) Uiso 0.273(2) 1 d PD . -2 C20B C 0.2860(4) 0.6733(4) 1.1391(7) 0.0176(16) Uiso 0.273(2) 1 d PD . -2 C21B C 0.2981(5) 0.6542(6) 1.2685(8) 0.030(2) Uiso 0.273(2) 1 d PD A -2 H21D H 0.2917 0.6044 1.2683 0.045 Uiso 0.273(2) 1 calc PR A -2 H21E H 0.2621 0.6556 1.3264 0.045 Uiso 0.273(2) 1 calc PR A -2 H21F H 0.3483 0.6899 1.2963 0.045 Uiso 0.273(2) 1 calc PR A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02458(17) 0.02192(16) 0.03285(17) 0.00259(15) -0.00080(15) 0.01207(15) O1 0.0247(8) 0.0212(8) 0.0248(9) 0.0000(7) -0.0018(7) 0.0119(7) N1 0.0300(11) 0.0291(11) 0.0301(12) 0.0064(9) -0.0017(10) 0.0084(9) N2 0.0286(10) 0.0248(10) 0.0230(11) 0.0004(8) 0.0004(8) 0.0114(8) C1 0.0274(12) 0.0333(13) 0.0187(12) -0.0007(10) -0.0001(9) 0.0162(10) C2 0.0273(12) 0.0289(12) 0.0154(11) 0.0026(9) 0.0009(9) 0.0123(10) C3 0.0281(12) 0.0282(12) 0.0238(13) -0.0002(10) -0.0044(9) 0.0154(10) C4 0.0378(14) 0.0345(14) 0.0269(14) -0.0025(11) -0.0037(11) 0.0199(12) C5 0.0355(14) 0.0296(13) 0.0343(15) -0.0057(11) -0.0092(11) 0.0162(11) C6 0.0288(13) 0.0252(12) 0.0449(16) -0.0015(11) -0.0103(12) 0.0131(11) C7 0.0288(13) 0.0315(13) 0.0345(14) 0.0047(11) 0.0005(11) 0.0163(11) C8 0.0260(12) 0.0275(12) 0.0286(13) 0.0035(10) -0.0017(10) 0.0155(10) C9 0.0241(12) 0.0258(11) 0.0247(13) 0.0021(9) 0.0013(9) 0.0132(10) C10 0.0281(13) 0.0271(12) 0.0277(14) 0.0007(11) 0.0013(10) 0.0085(11) C11 0.0294(13) 0.0397(15) 0.0336(16) -0.0002(12) 0.0048(11) 0.0109(11) C12 0.0288(14) 0.0572(19) 0.0383(17) 0.0039(15) 0.0065(13) 0.0071(14) C13 0.0337(15) 0.060(2) 0.0317(16) 0.0175(15) 0.0022(13) -0.0027(14) C14 0.0370(16) 0.0430(16) 0.0377(17) 0.0135(13) -0.0056(13) 0.0057(13) C15 0.0309(13) 0.0244(11) 0.0255(13) 0.0025(10) -0.0011(10) 0.0141(10) C16 0.0344(14) 0.0272(13) 0.0465(18) -0.0030(12) 0.0061(12) 0.0122(11) C17 0.0523(18) 0.0297(14) 0.0530(19) -0.0105(13) 0.0042(15) 0.0198(14) C18 0.0381(15) 0.0249(13) 0.0503(19) -0.0059(12) 0.0005(13) 0.0079(12) C19 0.0311(13) 0.0281(13) 0.0353(15) -0.0006(11) 0.0006(11) 0.0099(11) O2A 0.033(2) 0.0308(18) 0.0219(18) 0.0094(15) -0.0019(13) 0.0133(16) O3A 0.102(3) 0.0344(17) 0.051(2) 0.0045(14) 0.0030(19) 0.0272(18) C20A 0.051(2) 0.049(2) 0.035(2) 0.0111(19) 0.0111(18) 0.035(2) C21A 0.065(3) 0.083(4) 0.058(3) 0.001(3) -0.022(3) 0.056(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 Co1 O1 1.9981(16) 3_565 yes Co1 O3B 2.035(6) 2_665 yes Co1 O1 2.0509(17) . yes Co1 O2A 2.070(5) . yes Co1 N2 2.091(2) . yes Co1 O2B 2.15(2) 2_665 yes Co1 N1 2.213(2) . yes Co1 O3B 2.254(9) . ? Co1 C20B 2.377(7) 2_665 ? Co1 O3B 2.404(6) 3_565 ? O1 C9 1.391(3) 2_665 ? O1 Co1 1.9981(16) 2_665 ? N1 C10 1.338(3) . ? N1 C14 1.358(4) . ? N2 C19 1.338(3) . ? N2 C15 1.339(3) . ? C1 C2 1.387(3) 3_565 ? C1 C2 1.388(3) . ? C2 C1 1.387(3) 2_665 ? C2 C3 1.495(3) . ? C3 C4 1.388(3) . ? C3 C8 1.427(3) . ? C4 C5 1.397(4) . ? C5 C6 1.397(4) . ? C6 C7 1.371(4) . ? C7 C8 1.409(3) . ? C8 C9 1.539(3) . ? C9 O1 1.391(3) 3_565 ? C9 C10 1.550(3) . ? C9 C15 1.556(3) 3_565 ? C10 C11 1.388(4) . ? C11 C12 1.377(4) . ? C12 C13 1.364(5) . ? C13 C14 1.376(5) . ? C15 C16 1.388(4) . ? C15 C9 1.556(3) 2_665 ? C16 C17 1.402(4) . ? C17 C18 1.366(4) . ? C18 C19 1.391(4) . ? O2A C20A 1.289(7) . ? O3A C20A 1.243(5) . ? C20A C21A 1.517(6) . ? O2B C20B 1.279(18) . ? O2B Co1 2.15(2) 3_565 ? O3B C20B 1.239(8) . ? O3B Co1 2.035(6) 3_565 ? O3B Co1 2.404(6) 2_665 ? C20B C21B 1.481(10) . ? C20B Co1 2.377(7) 3_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O3B 85.75(19) 3_565 2_665 yes O1 Co1 O1 91.81(9) 3_565 . yes O3B Co1 O1 80.2(3) 2_665 . yes O1 Co1 O2A 148.1(2) 3_565 . ? O3B Co1 O2A 69.2(2) 2_665 . ? O1 Co1 O2A 102.7(2) . . yes O1 Co1 N2 117.83(7) 3_565 . yes O3B Co1 N2 148.0(3) 2_665 . yes O1 Co1 N2 77.79(7) . . yes O2A Co1 N2 93.2(2) . . yes O1 Co1 O2B 142.7(6) 3_565 2_665 ? O3B Co1 O2B 63.2(5) 2_665 2_665 yes O1 Co1 O2B 102.0(8) . 2_665 yes O2A Co1 O2B 6.1(7) . 2_665 yes N2 Co1 O2B 99.0(5) . 2_665 yes O1 Co1 N1 74.91(8) 3_565 . yes O3B Co1 N1 100.7(3) 2_665 . yes O1 Co1 N1 166.53(7) . . yes O2A Co1 N1 90.1(2) . . yes N2 Co1 N1 106.14(8) . . yes O2B Co1 N1 90.2(8) 2_665 . yes O1 Co1 O3B 76.24(14) 3_565 . ? O3B Co1 O3B 10.2(3) 2_665 . ? O1 Co1 O3B 84.50(17) . . ? O2A Co1 O3B 77.0(2) . . ? N2 Co1 O3B 157.42(14) . . ? O2B Co1 O3B 70.9(5) 2_665 . ? N1 Co1 O3B 94.32(17) . . ? O1 Co1 C20B 112.81(18) 3_565 2_665 ? O3B Co1 C20B 31.4(2) 2_665 2_665 ? O1 Co1 C20B 95.19(19) . 2_665 ? O2A Co1 C20B 38.4(3) . 2_665 ? N2 Co1 C20B 128.97(18) . 2_665 ? O2B Co1 C20B 32.3(5) 2_665 2_665 ? N1 Co1 C20B 92.14(19) . 2_665 ? O3B Co1 C20B 38.6(2) . 2_665 ? O1 Co1 O3B 81.8(2) 3_565 3_565 ? O3B Co1 O3B 6.26(13) 2_665 3_565 ? O1 Co1 O3B 75.60(15) . 3_565 ? O2A Co1 O3B 74.6(3) . 3_565 ? N2 Co1 O3B 147.3(2) . 3_565 ? O2B Co1 O3B 68.7(6) 2_665 3_565 ? N1 Co1 O3B 104.16(19) . 3_565 ? O3B Co1 O3B 10.2(2) . 3_565 ? C20B Co1 O3B 37.3(2) 2_665 3_565 ? C9 O1 Co1 118.82(13) 2_665 2_665 ? C9 O1 Co1 113.88(13) 2_665 . ? Co1 O1 Co1 105.73(8) 2_665 . ? C10 N1 C14 117.7(3) . . ? C10 N1 Co1 114.14(17) . . ? C14 N1 Co1 125.58(19) . . ? C19 N2 C15 119.0(2) . . ? C19 N2 Co1 126.32(18) . . ? C15 N2 Co1 114.60(15) . . ? C2 C1 C2 120.5(3) 3_565 . ? C1 C2 C1 119.5(3) 2_665 . ? C1 C2 C3 118.7(2) 2_665 . ? C1 C2 C3 121.7(2) . . ? C4 C3 C8 119.4(2) . . ? C4 C3 C2 117.9(2) . . ? C8 C3 C2 122.6(2) . . ? C3 C4 C5 121.8(2) . . ? C4 C5 C6 118.8(2) . . ? C7 C6 C5 120.3(2) . . ? C6 C7 C8 122.2(3) . . ? C7 C8 C3 117.5(2) . . ? C7 C8 C9 120.2(2) . . ? C3 C8 C9 122.3(2) . . ? O1 C9 C8 113.08(19) 3_565 . ? O1 C9 C10 106.07(19) 3_565 . ? C8 C9 C10 109.20(19) . . ? O1 C9 C15 108.68(18) 3_565 3_565 ? C8 C9 C15 109.75(19) . 3_565 ? C10 C9 C15 109.99(19) . 3_565 ? N1 C10 C11 122.0(3) . . ? N1 C10 C9 112.5(2) . . ? C11 C10 C9 125.5(2) . . ? C12 C11 C10 119.0(3) . . ? C13 C12 C11 119.7(3) . . ? C14 C13 C12 118.6(3) . . ? C13 C14 N1 122.9(3) . . ? N2 C15 C16 122.4(2) . . ? N2 C15 C9 114.8(2) . 2_665 ? C16 C15 C9 122.8(2) . 2_665 ? C15 C16 C17 117.7(3) . . ? C18 C17 C16 120.0(3) . . ? C17 C18 C19 118.4(2) . . ? N2 C19 C18 122.4(2) . . ? C20A O2A Co1 134.0(5) . . ? O3A C20A O2A 125.3(5) . . ? O3A C20A C21A 116.0(4) . . ? O2A C20A C21A 118.2(5) . . ? C20B O2B Co1 83.8(12) . 3_565 ? C20B O3B Co1 89.7(5) . 3_565 ? C20B O3B Co1 121.1(7) . . ? Co1 O3B Co1 97.5(2) 3_565 . ? C20B O3B Co1 150.5(8) . 2_665 ? Co1 O3B Co1 92.9(3) 3_565 2_665 ? Co1 O3B Co1 87.67(17) . 2_665 ? O3B C20B O2B 121.2(12) . . ? O3B C20B C21B 119.0(7) . . ? O2B C20B C21B 119.7(12) . . ? O3B C20B Co1 58.9(4) . 3_565 ? O2B C20B Co1 63.9(11) . 3_565 ? C21B C20B Co1 170.7(6) . 3_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.713 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.070 # Attachment '- jsk08.cif' data_jsk08 _database_code_depnum_ccdc_archive 'CCDC 787163' #TrackingRef '- jsk08.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H48 Mn3 N6 O9' _chemical_formula_sum 'C63 H48 Mn3 N6 O9' _chemical_formula_weight 1197.89 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5708(8) _cell_length_b 19.6592(14) _cell_length_c 20.2109(15) _cell_angle_alpha 71.889(4) _cell_angle_beta 88.967(4) _cell_angle_gamma 75.160(4) _cell_volume 3850.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9864 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 29.80 _exptl_crystal_description Column _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1230 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8655 _exptl_absorpt_correction_T_max 0.9439 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 18 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 159858 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 30.02 _reflns_number_total 22372 _reflns_number_gt 16446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; The solvent area is disordered and contains four chloroforms and one diethylether. Due to the difficulty of not being able to establish a satisfactory solvent model the program SQUEEZE was employed to remove the contribution of solvent from the observed intensities. Solvent area constitutes 37% of the total unit cell volume and SQUEEZE accounted for 430 electrons in a volume that could be expected to contain up to 550 electrons. 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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22372 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 2.775 _refine_ls_restrained_S_all 2.775 _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 Mn1 Mn 0.79301(4) 0.18836(2) 0.591055(19) 0.01318(9) Uani 1 1 d . . . Mn2 Mn 0.86581(4) 0.05922(2) 0.752945(19) 0.01487(9) Uani 1 1 d . . . Mn3 Mn 0.74339(4) 0.24168(2) 0.739032(19) 0.01578(9) Uani 1 1 d . . . O1 O 0.75425(14) 0.08925(9) 0.65917(8) 0.0133(4) Uani 1 1 d . . . O2 O 0.72151(15) 0.13864(9) 0.78719(8) 0.0140(4) Uani 1 1 d . . . O3 O 0.66357(14) 0.25743(9) 0.64025(8) 0.0132(4) Uani 1 1 d . . . O4 O 0.94880(16) 0.16199(9) 0.52882(9) 0.0209(4) Uani 1 1 d . . . O5 O 1.12227(17) 0.18574(10) 0.47184(9) 0.0293(5) Uani 1 1 d . . . O6 O 1.03928(17) 0.05506(10) 0.80419(9) 0.0273(5) Uani 1 1 d . . . O7 O 1.1088(2) -0.06259(11) 0.86932(10) 0.0409(5) Uani 1 1 d . . . O8 O 0.92704(16) 0.26862(9) 0.71534(9) 0.0202(4) Uani 1 1 d . . . O9 O 0.92680(15) 0.17067(9) 0.68207(8) 0.0167(4) Uani 1 1 d . . . N1 N 0.68416(18) 0.14556(11) 0.52645(10) 0.0140(4) Uani 1 1 d . . . N2 N 0.95817(19) -0.02675(11) 0.69668(10) 0.0154(5) Uani 1 1 d . . . N3 N 0.77594(19) -0.00403(11) 0.84673(10) 0.0161(5) Uani 1 1 d . . . N4 N 0.82866(19) 0.20660(12) 0.85416(10) 0.0188(5) Uani 1 1 d . . . N5 N 0.59748(19) 0.35034(11) 0.71330(11) 0.0188(5) Uani 1 1 d . . . N6 N 0.79721(19) 0.31198(11) 0.53684(10) 0.0161(5) Uani 1 1 d . . . C1 C 0.4609(2) 0.14782(14) 0.63219(12) 0.0152(5) Uani 1 1 d . . . H1 H 0.4603 0.1384 0.5889 0.018 Uiso 1 1 calc R . . C2 C 0.4933(2) 0.08821(14) 0.69411(13) 0.0150(5) Uani 1 1 d . . . C3 C 0.4843(2) 0.10277(14) 0.75709(13) 0.0159(5) Uani 1 1 d . . . H3 H 0.5014 0.0626 0.7995 0.019 Uiso 1 1 calc R . . C4 C 0.4506(2) 0.17544(14) 0.75950(13) 0.0158(5) Uani 1 1 d . . . C5 C 0.4215(2) 0.23354(14) 0.69756(13) 0.0158(5) Uani 1 1 d . . . H5 H 0.3955 0.2831 0.6988 0.019 Uiso 1 1 calc R . . C6 C 0.4297(2) 0.22062(14) 0.63314(12) 0.0162(5) Uani 1 1 d . . . C7 C 0.4147(2) 0.28111(14) 0.56552(13) 0.0166(6) Uani 1 1 d . . . C8 C 0.3260(2) 0.28371(14) 0.51319(13) 0.0212(6) Uani 1 1 d . . . H8 H 0.2727 0.2499 0.5240 0.025 Uiso 1 1 calc R . . C9 C 0.3136(2) 0.33358(15) 0.44671(14) 0.0243(6) Uani 1 1 d . . . H9 H 0.2519 0.3342 0.4128 0.029 Uiso 1 1 calc R . . C10 C 0.3914(2) 0.38289(14) 0.42964(13) 0.0227(6) Uani 1 1 d . . . H10 H 0.3838 0.4175 0.3841 0.027 Uiso 1 1 calc R . . C11 C 0.4799(2) 0.38074(14) 0.47997(13) 0.0197(6) Uani 1 1 d . . . H11 H 0.5333 0.4144 0.4678 0.024 Uiso 1 1 calc R . . C12 C 0.4953(2) 0.33146(13) 0.54810(12) 0.0157(5) Uani 1 1 d . . . C13 C 0.5443(2) 0.01011(14) 0.69530(12) 0.0161(5) Uani 1 1 d . . . C14 C 0.4742(3) -0.04055(15) 0.73071(13) 0.0230(6) Uani 1 1 d . . . H14 H 0.3946 -0.0228 0.7499 0.028 Uiso 1 1 calc R . . C15 C 0.5172(3) -0.11517(15) 0.73855(13) 0.0239(6) Uani 1 1 d . . . H15 H 0.4672 -0.1481 0.7624 0.029 Uiso 1 1 calc R . . C16 C 0.6332(2) -0.14165(14) 0.71147(13) 0.0209(6) Uani 1 1 d . . . H16 H 0.6647 -0.1931 0.7172 0.025 Uiso 1 1 calc R . . C17 C 0.7033(2) -0.09240(14) 0.67581(12) 0.0186(6) Uani 1 1 d . . . H17 H 0.7820 -0.1110 0.6563 0.022 Uiso 1 1 calc R . . C18 C 0.6636(2) -0.01703(13) 0.66735(12) 0.0142(5) Uani 1 1 d . . . C19 C 0.4543(2) 0.19046(14) 0.82682(13) 0.0171(6) Uani 1 1 d . . . C20 C 0.3389(2) 0.23496(14) 0.84267(13) 0.0229(6) Uani 1 1 d . . . H20 H 0.2634 0.2522 0.8112 0.028 Uiso 1 1 calc R . . C21 C 0.3325(3) 0.25435(14) 0.90350(14) 0.0242(6) Uani 1 1 d . . . H21 H 0.2535 0.2848 0.9130 0.029 Uiso 1 1 calc R . . C22 C 0.4412(3) 0.22917(14) 0.94995(14) 0.0237(6) Uani 1 1 d . . . H22 H 0.4376 0.2417 0.9918 0.028 Uiso 1 1 calc R . . C23 C 0.5572(2) 0.18485(14) 0.93455(13) 0.0200(6) Uani 1 1 d . . . H23 H 0.6318 0.1675 0.9667 0.024 Uiso 1 1 calc R . . C24 C 0.5663(2) 0.16543(13) 0.87309(12) 0.0144(5) Uani 1 1 d . . . C25 C 0.6025(2) 0.32944(13) 0.60024(12) 0.0138(5) Uani 1 1 d . . . C26 C 0.7511(2) 0.03483(13) 0.62891(12) 0.0128(5) Uani 1 1 d . . . C27 C 0.7015(2) 0.11963(13) 0.85809(12) 0.0148(5) Uani 1 1 d . . . C28 C 0.7110(2) 0.36189(13) 0.56013(12) 0.0145(5) Uani 1 1 d . . . C29 C 0.7253(2) 0.43129(14) 0.55071(12) 0.0181(6) Uani 1 1 d . . . H29 H 0.6637 0.4651 0.5680 0.022 Uiso 1 1 calc R . . C30 C 0.8313(2) 0.45244(14) 0.51529(13) 0.0222(6) Uani 1 1 d . . . H30 H 0.8435 0.5003 0.5088 0.027 Uiso 1 1 calc R . . C31 C 0.9172(2) 0.40229(14) 0.49019(13) 0.0226(6) Uani 1 1 d . . . H31 H 0.9889 0.4153 0.4650 0.027 Uiso 1 1 calc R . . C32 C 0.8978(2) 0.33277(14) 0.50208(13) 0.0210(6) Uani 1 1 d . . . H32 H 0.9579 0.2982 0.4850 0.025 Uiso 1 1 calc R . . C33 C 0.5427(2) 0.37601(13) 0.64776(13) 0.0164(5) Uani 1 1 d . . . C34 C 0.4410(2) 0.44027(14) 0.62515(13) 0.0205(6) Uani 1 1 d . . . H34 H 0.4036 0.4571 0.5786 0.025 Uiso 1 1 calc R . . C35 C 0.3935(3) 0.48018(15) 0.67060(15) 0.0279(7) Uani 1 1 d . . . H35 H 0.3245 0.5245 0.6556 0.034 Uiso 1 1 calc R . . C36 C 0.4495(3) 0.45349(16) 0.73809(15) 0.0327(7) Uani 1 1 d . . . H36 H 0.4197 0.4792 0.7706 0.039 Uiso 1 1 calc R . . C37 C 0.5499(3) 0.38850(15) 0.75750(14) 0.0281(7) Uani 1 1 d . . . H37 H 0.5870 0.3699 0.8042 0.034 Uiso 1 1 calc R . . C38 C 0.6948(2) 0.07219(13) 0.55249(12) 0.0133(5) Uani 1 1 d . . . C39 C 0.6496(2) 0.03524(14) 0.51374(12) 0.0168(6) Uani 1 1 d . . . H39 H 0.6612 -0.0169 0.5318 0.020 Uiso 1 1 calc R . . C40 C 0.5870(2) 0.07530(14) 0.44790(13) 0.0192(6) Uani 1 1 d . . . H40 H 0.5558 0.0510 0.4203 0.023 Uiso 1 1 calc R . . C41 C 0.5709(2) 0.15142(14) 0.42347(13) 0.0187(6) Uani 1 1 d . . . H41 H 0.5250 0.1805 0.3797 0.022 Uiso 1 1 calc R . . C42 C 0.6226(2) 0.18387(14) 0.46370(12) 0.0165(6) Uani 1 1 d . . . H42 H 0.6142 0.2357 0.4462 0.020 Uiso 1 1 calc R . . C43 C 0.8945(2) -0.01489(13) 0.63564(12) 0.0142(5) Uani 1 1 d . . . C44 C 0.9513(2) -0.04640(13) 0.58667(12) 0.0152(5) Uani 1 1 d . . . H44 H 0.9053 -0.0356 0.5432 0.018 Uiso 1 1 calc R . . C45 C 1.0769(2) -0.09419(14) 0.60148(13) 0.0184(6) Uani 1 1 d . . . H45 H 1.1176 -0.1173 0.5688 0.022 Uiso 1 1 calc R . . C46 C 1.1411(2) -0.10716(14) 0.66519(13) 0.0214(6) Uani 1 1 d . . . H46 H 1.2264 -0.1400 0.6774 0.026 Uiso 1 1 calc R . . C47 C 1.0793(2) -0.07165(14) 0.71055(13) 0.0179(6) Uani 1 1 d . . . H47 H 1.1248 -0.0795 0.7535 0.021 Uiso 1 1 calc R . . C48 C 0.7119(2) 0.03641(13) 0.88648(12) 0.0145(5) Uani 1 1 d . . . C49 C 0.6583(2) 0.00313(14) 0.94662(13) 0.0186(6) Uani 1 1 d . . . H49 H 0.6154 0.0316 0.9748 0.022 Uiso 1 1 calc R . . C50 C 0.6672(2) -0.07252(14) 0.96596(13) 0.0221(6) Uani 1 1 d . . . H50 H 0.6311 -0.0961 1.0075 0.027 Uiso 1 1 calc R . . C51 C 0.7291(3) -0.11253(15) 0.92404(13) 0.0237(6) Uani 1 1 d . . . H51 H 0.7342 -0.1639 0.9354 0.028 Uiso 1 1 calc R . . C52 C 0.7833(2) -0.07661(14) 0.86538(13) 0.0212(6) Uani 1 1 d . . . H52 H 0.8277 -0.1044 0.8370 0.025 Uiso 1 1 calc R . . C53 C 0.8109(2) 0.14046(14) 0.89279(13) 0.0178(6) Uani 1 1 d . . . C54 C 0.8833(2) 0.09775(14) 0.95443(13) 0.0195(6) Uani 1 1 d . . . H54 H 0.8685 0.0514 0.9802 0.023 Uiso 1 1 calc R . . C55 C 0.9784(2) 0.12365(15) 0.97828(14) 0.0250(6) Uani 1 1 d . . . H55 H 1.0286 0.0955 1.0210 0.030 Uiso 1 1 calc R . . C56 C 0.9989(3) 0.19040(15) 0.93925(14) 0.0271(7) Uani 1 1 d . . . H56 H 1.0642 0.2089 0.9540 0.032 Uiso 1 1 calc R . . C57 C 0.9221(3) 0.22986(15) 0.87814(14) 0.0254(7) Uani 1 1 d . . . H57 H 0.9362 0.2762 0.8515 0.031 Uiso 1 1 calc R . . C58 C 1.0721(3) 0.14954(14) 0.52309(14) 0.0198(6) Uani 1 1 d . . . C59 C 1.1597(2) 0.08643(14) 0.57969(13) 0.0234(6) Uani 1 1 d . . . H59A H 1.1614 0.0393 0.5721 0.035 Uiso 1 1 calc R . . H59B H 1.1259 0.0861 0.6252 0.035 Uiso 1 1 calc R . . H59C H 1.2487 0.0928 0.5785 0.035 Uiso 1 1 calc R . . C60 C 1.1192(3) 0.00123(15) 0.84826(13) 0.0210(6) Uani 1 1 d . . . C61 C 1.2330(3) 0.02119(18) 0.87434(14) 0.0379(8) Uani 1 1 d . . . H61A H 1.2023 0.0501 0.9060 0.057 Uiso 1 1 calc R . . H61B H 1.2711 0.0507 0.8347 0.057 Uiso 1 1 calc R . . H61C H 1.2997 -0.0243 0.8993 0.057 Uiso 1 1 calc R . . C62 C 0.9843(2) 0.21715(15) 0.69150(12) 0.0204(6) Uani 1 1 d . . . C63 C 1.1241(2) 0.21160(16) 0.67250(15) 0.0337(8) Uani 1 1 d . . . H63A H 1.1531 0.2517 0.6812 0.051 Uiso 1 1 calc R . . H63B H 1.1299 0.2158 0.6230 0.051 Uiso 1 1 calc R . . H63C H 1.1804 0.1636 0.7009 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0121(2) 0.0137(2) 0.0144(2) -0.00490(16) 0.00190(16) -0.00412(17) Mn2 0.0124(2) 0.0180(2) 0.0146(2) -0.00640(17) 0.00095(16) -0.00319(17) Mn3 0.0148(2) 0.0167(2) 0.0158(2) -0.00432(17) 0.00138(16) -0.00525(18) O1 0.0114(9) 0.0147(9) 0.0156(9) -0.0064(7) 0.0007(7) -0.0043(7) O2 0.0126(9) 0.0175(10) 0.0126(9) -0.0049(8) 0.0035(7) -0.0049(8) O3 0.0098(9) 0.0117(9) 0.0150(9) -0.0021(7) 0.0003(7) 0.0003(7) O4 0.0151(10) 0.0275(11) 0.0251(10) -0.0142(9) 0.0076(8) -0.0074(9) O5 0.0250(11) 0.0341(12) 0.0279(11) -0.0046(10) 0.0073(9) -0.0131(10) O6 0.0213(11) 0.0333(12) 0.0266(11) -0.0082(10) -0.0033(9) -0.0070(10) O7 0.0591(16) 0.0298(13) 0.0304(12) -0.0033(10) -0.0026(11) -0.0131(12) O8 0.0167(10) 0.0232(11) 0.0245(10) -0.0126(9) 0.0054(8) -0.0060(8) O9 0.0130(9) 0.0182(10) 0.0206(10) -0.0061(8) 0.0000(7) -0.0070(8) N1 0.0089(11) 0.0164(12) 0.0150(11) -0.0036(9) 0.0019(9) -0.0024(9) N2 0.0111(11) 0.0168(12) 0.0176(11) -0.0056(9) -0.0008(9) -0.0019(9) N3 0.0142(12) 0.0170(12) 0.0162(11) -0.0050(9) 0.0000(9) -0.0030(10) N4 0.0212(13) 0.0220(13) 0.0172(11) -0.0073(10) 0.0023(9) -0.0110(10) N5 0.0178(12) 0.0186(12) 0.0223(12) -0.0101(10) 0.0045(10) -0.0042(10) N6 0.0144(12) 0.0157(12) 0.0193(11) -0.0059(9) 0.0038(9) -0.0059(10) C1 0.0054(13) 0.0237(15) 0.0182(13) -0.0077(12) 0.0025(10) -0.0056(11) C2 0.0039(12) 0.0192(14) 0.0234(14) -0.0065(12) 0.0017(10) -0.0060(11) C3 0.0070(13) 0.0222(15) 0.0191(13) -0.0036(11) 0.0037(10) -0.0085(11) C4 0.0052(13) 0.0232(15) 0.0213(14) -0.0088(12) 0.0033(10) -0.0058(11) C5 0.0062(13) 0.0191(14) 0.0249(14) -0.0101(12) 0.0043(11) -0.0043(11) C6 0.0064(13) 0.0220(15) 0.0177(13) -0.0010(11) -0.0006(10) -0.0060(11) C7 0.0105(13) 0.0178(14) 0.0202(14) -0.0070(11) 0.0030(11) -0.0006(11) C8 0.0109(14) 0.0249(16) 0.0263(15) -0.0058(13) 0.0018(11) -0.0053(12) C9 0.0165(15) 0.0283(17) 0.0260(15) -0.0090(13) -0.0075(12) -0.0011(13) C10 0.0242(16) 0.0201(15) 0.0183(14) -0.0004(12) -0.0037(12) -0.0027(13) C11 0.0186(15) 0.0126(14) 0.0262(15) -0.0054(12) -0.0014(12) -0.0019(12) C12 0.0139(14) 0.0142(14) 0.0180(13) -0.0065(11) 0.0029(11) -0.0005(11) C13 0.0150(14) 0.0185(14) 0.0152(13) -0.0038(11) -0.0019(11) -0.0068(12) C14 0.0227(16) 0.0256(16) 0.0241(15) -0.0081(13) 0.0045(12) -0.0125(13) C15 0.0255(16) 0.0253(16) 0.0239(15) -0.0041(13) 0.0048(12) -0.0164(14) C16 0.0239(16) 0.0140(14) 0.0248(15) -0.0044(12) -0.0016(12) -0.0070(12) C17 0.0163(14) 0.0196(15) 0.0205(14) -0.0066(12) -0.0007(11) -0.0053(12) C18 0.0155(14) 0.0163(14) 0.0128(12) -0.0041(11) -0.0007(10) -0.0084(11) C19 0.0150(14) 0.0183(14) 0.0192(14) -0.0068(11) 0.0068(11) -0.0057(12) C20 0.0153(15) 0.0262(16) 0.0248(15) -0.0064(13) 0.0023(12) -0.0034(12) C21 0.0191(15) 0.0231(16) 0.0290(16) -0.0102(13) 0.0096(13) -0.0014(13) C22 0.0268(17) 0.0254(16) 0.0208(15) -0.0101(13) 0.0096(13) -0.0071(13) C23 0.0181(15) 0.0204(15) 0.0221(14) -0.0061(12) 0.0054(12) -0.0071(12) C24 0.0153(14) 0.0127(13) 0.0156(13) -0.0050(11) 0.0056(11) -0.0042(11) C25 0.0145(14) 0.0114(13) 0.0159(13) -0.0039(11) 0.0027(10) -0.0047(11) C26 0.0112(13) 0.0130(13) 0.0149(12) -0.0046(11) 0.0016(10) -0.0040(11) C27 0.0140(14) 0.0206(14) 0.0117(12) -0.0057(11) 0.0021(10) -0.0072(11) C28 0.0130(13) 0.0165(14) 0.0139(12) -0.0040(11) -0.0012(10) -0.0043(11) C29 0.0156(14) 0.0166(14) 0.0198(14) -0.0053(12) 0.0007(11) -0.0008(12) C30 0.0275(16) 0.0138(14) 0.0264(15) -0.0053(12) 0.0015(12) -0.0089(13) C31 0.0191(15) 0.0241(16) 0.0255(15) -0.0061(13) 0.0093(12) -0.0098(13) C32 0.0178(15) 0.0193(15) 0.0238(15) -0.0054(12) 0.0066(12) -0.0033(12) C33 0.0161(14) 0.0136(14) 0.0200(14) -0.0044(11) 0.0049(11) -0.0061(11) C34 0.0175(15) 0.0178(15) 0.0245(15) -0.0050(12) 0.0037(12) -0.0039(12) C35 0.0212(16) 0.0209(16) 0.0384(18) -0.0103(14) 0.0083(14) 0.0007(13) C36 0.0349(19) 0.0316(18) 0.0349(18) -0.0204(15) 0.0108(15) -0.0026(15) C37 0.0349(18) 0.0274(17) 0.0237(15) -0.0108(13) 0.0029(13) -0.0078(14) C38 0.0081(13) 0.0176(14) 0.0156(13) -0.0064(11) 0.0025(10) -0.0043(11) C39 0.0128(14) 0.0191(14) 0.0205(14) -0.0070(12) 0.0042(11) -0.0066(12) C40 0.0131(14) 0.0260(16) 0.0213(14) -0.0095(12) 0.0021(11) -0.0074(12) C41 0.0128(14) 0.0217(15) 0.0178(14) -0.0036(12) -0.0008(11) -0.0013(12) C42 0.0137(14) 0.0159(14) 0.0183(13) -0.0044(11) 0.0022(11) -0.0026(11) C43 0.0158(14) 0.0111(13) 0.0172(13) -0.0035(11) 0.0022(11) -0.0076(11) C44 0.0156(14) 0.0138(13) 0.0171(13) -0.0061(11) 0.0004(11) -0.0040(11) C45 0.0185(15) 0.0193(14) 0.0190(14) -0.0074(12) 0.0048(11) -0.0065(12) C46 0.0177(15) 0.0179(15) 0.0250(15) -0.0044(12) 0.0006(12) -0.0013(12) C47 0.0167(14) 0.0198(15) 0.0158(13) -0.0050(11) 0.0000(11) -0.0032(12) C48 0.0114(13) 0.0185(14) 0.0139(13) -0.0060(11) -0.0014(10) -0.0032(11) C49 0.0146(14) 0.0215(15) 0.0194(14) -0.0059(12) 0.0040(11) -0.0054(12) C50 0.0155(15) 0.0256(16) 0.0222(14) -0.0017(12) 0.0049(11) -0.0076(13) C51 0.0292(17) 0.0176(15) 0.0253(15) -0.0064(12) -0.0010(13) -0.0079(13) C52 0.0223(15) 0.0173(15) 0.0230(15) -0.0060(12) -0.0010(12) -0.0039(12) C53 0.0135(14) 0.0255(16) 0.0179(14) -0.0113(12) 0.0049(11) -0.0057(12) C54 0.0174(15) 0.0202(15) 0.0202(14) -0.0060(12) 0.0031(11) -0.0042(12) C55 0.0212(16) 0.0331(17) 0.0198(14) -0.0068(13) -0.0029(12) -0.0070(14) C56 0.0263(17) 0.0339(18) 0.0274(16) -0.0112(14) -0.0016(13) -0.0170(14) C57 0.0307(17) 0.0259(16) 0.0248(15) -0.0083(13) 0.0066(13) -0.0164(14) C58 0.0201(16) 0.0203(15) 0.0247(15) -0.0135(12) 0.0046(12) -0.0076(13) C59 0.0265(16) 0.0196(15) 0.0237(15) -0.0065(12) -0.0017(12) -0.0053(13) C60 0.0256(17) 0.0240(16) 0.0121(13) -0.0059(12) 0.0033(12) -0.0039(13) C61 0.0213(17) 0.068(2) 0.0254(16) -0.0160(17) -0.0032(13) -0.0121(17) C62 0.0167(15) 0.0275(16) 0.0157(13) -0.0053(12) -0.0020(11) -0.0054(13) C63 0.0119(15) 0.047(2) 0.056(2) -0.0310(18) 0.0110(14) -0.0129(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 Mn1 O4 2.1110(16) . yes Mn1 O3 2.1314(15) . yes Mn1 O1 2.1402(16) . yes Mn1 O9 2.2247(16) . yes Mn1 N1 2.2292(19) . yes Mn1 N6 2.347(2) . yes Mn2 O1 2.0880(16) . yes Mn2 O6 2.0930(18) . yes Mn2 O2 2.1579(15) . yes Mn2 N3 2.2620(19) . yes Mn2 N2 2.3265(19) . yes Mn2 O9 2.4509(16) . yes Mn3 O2 2.0273(16) . yes Mn3 O3 2.0825(16) . yes Mn3 O8 2.1481(16) . yes Mn3 N5 2.205(2) . yes Mn3 N4 2.337(2) . yes O1 C26 1.395(2) . ? O2 C27 1.391(3) . ? O3 C25 1.383(3) . ? O4 C58 1.273(3) . ? O5 C58 1.255(3) . ? O6 C60 1.269(3) . ? O7 C60 1.227(3) . ? O8 C62 1.266(3) . ? O9 C62 1.280(3) . ? N1 C42 1.336(3) . ? N1 C38 1.348(3) . ? N2 C47 1.333(3) . ? N2 C43 1.342(3) . ? N3 C52 1.339(3) . ? N3 C48 1.355(3) . ? N4 C57 1.344(3) . ? N4 C53 1.351(3) . ? N5 C33 1.344(3) . ? N5 C37 1.349(3) . ? N6 C32 1.344(3) . ? N6 C28 1.352(3) . ? C1 C6 1.390(3) . ? C1 C2 1.398(3) . ? C2 C3 1.385(3) . ? C2 C13 1.484(3) . ? C3 C4 1.397(3) . ? C4 C5 1.382(3) . ? C4 C19 1.483(3) . ? C5 C6 1.399(3) . ? C6 C7 1.486(3) . ? C7 C8 1.406(3) . ? C7 C12 1.426(3) . ? C8 C9 1.380(3) . ? C9 C10 1.388(3) . ? C10 C11 1.378(3) . ? C11 C12 1.400(3) . ? C12 C25 1.546(3) . ? C13 C14 1.403(3) . ? C13 C18 1.417(3) . ? C14 C15 1.378(3) . ? C15 C16 1.379(3) . ? C16 C17 1.386(3) . ? C17 C18 1.388(3) . ? C18 C26 1.570(3) . ? C19 C20 1.404(3) . ? C19 C24 1.404(3) . ? C20 C21 1.391(3) . ? C21 C22 1.381(4) . ? C22 C23 1.402(3) . ? C23 C24 1.403(3) . ? C24 C27 1.563(3) . ? C25 C33 1.545(3) . ? C25 C28 1.549(3) . ? C26 C38 1.544(3) . ? C26 C43 1.561(3) . ? C27 C48 1.531(3) . ? C27 C53 1.564(3) . ? C28 C29 1.365(3) . ? C29 C30 1.402(3) . ? C30 C31 1.375(3) . ? C31 C32 1.381(3) . ? C33 C34 1.387(3) . ? C34 C35 1.393(3) . ? C35 C36 1.382(4) . ? C36 C37 1.386(4) . ? C38 C39 1.384(3) . ? C39 C40 1.394(3) . ? C40 C41 1.388(3) . ? C41 C42 1.373(3) . ? C43 C44 1.376(3) . ? C44 C45 1.391(3) . ? C45 C46 1.386(3) . ? C46 C47 1.378(3) . ? C48 C49 1.378(3) . ? C49 C50 1.393(3) . ? C50 C51 1.377(3) . ? C51 C52 1.376(3) . ? C53 C54 1.377(3) . ? C54 C55 1.391(3) . ? C55 C56 1.374(4) . ? C56 C57 1.380(4) . ? C58 C59 1.508(4) . ? C60 C61 1.508(3) . ? C62 C63 1.506(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O3 155.18(6) . . yes O4 Mn1 O1 110.39(6) . . yes O3 Mn1 O1 93.00(6) . . yes O4 Mn1 O9 93.38(6) . . yes O3 Mn1 O9 81.70(6) . . yes O1 Mn1 O9 81.31(6) . . yes O4 Mn1 N1 83.80(6) . . yes O3 Mn1 N1 111.88(6) . . yes O1 Mn1 N1 73.09(7) . . yes O9 Mn1 N1 151.31(7) . . yes O4 Mn1 N6 85.32(7) . . yes O3 Mn1 N6 70.98(6) . . yes O1 Mn1 N6 163.94(6) . . yes O9 Mn1 N6 94.83(6) . . yes N1 Mn1 N6 113.30(7) . . yes O1 Mn2 O6 148.30(7) . . yes O1 Mn2 O2 90.62(6) . . yes O6 Mn2 O2 102.32(6) . . yes O1 Mn2 N3 113.74(7) . . yes O6 Mn2 N3 97.83(7) . . yes O2 Mn2 N3 71.94(6) . . yes O1 Mn2 N2 72.73(6) . . yes O6 Mn2 N2 97.05(7) . . yes O2 Mn2 N2 160.63(6) . . yes N3 Mn2 N2 105.25(7) . . yes O1 Mn2 O9 77.15(6) . . yes O6 Mn2 O9 75.99(6) . . yes O2 Mn2 O9 82.71(6) . . yes N3 Mn2 O9 152.10(6) . . yes N2 Mn2 O9 102.52(6) . . yes O2 Mn3 O3 98.33(6) . . yes O2 Mn3 O8 125.50(7) . . yes O3 Mn3 O8 101.82(6) . . yes O2 Mn3 N5 129.67(7) . . yes O3 Mn3 N5 76.08(7) . . yes O8 Mn3 N5 104.29(7) . . yes O2 Mn3 N4 73.34(7) . . yes O3 Mn3 N4 171.64(7) . . yes O8 Mn3 N4 83.03(7) . . yes N5 Mn3 N4 109.55(7) . . yes C26 O1 Mn2 119.12(14) . . ? C26 O1 Mn1 115.84(13) . . ? Mn2 O1 Mn1 107.77(7) . . ? C27 O2 Mn3 117.61(13) . . ? C27 O2 Mn2 117.05(14) . . ? Mn3 O2 Mn2 109.09(7) . . ? C25 O3 Mn3 117.26(13) . . ? C25 O3 Mn1 118.03(13) . . ? Mn3 O3 Mn1 110.09(7) . . ? C58 O4 Mn1 145.85(16) . . ? C60 O6 Mn2 130.50(18) . . ? C62 O8 Mn3 100.56(15) . . ? C62 O9 Mn1 126.57(16) . . ? C62 O9 Mn2 137.78(15) . . ? Mn1 O9 Mn2 93.75(6) . . ? C42 N1 C38 119.3(2) . . ? C42 N1 Mn1 126.17(16) . . ? C38 N1 Mn1 114.21(15) . . ? C47 N2 C43 118.7(2) . . ? C47 N2 Mn2 125.29(16) . . ? C43 N2 Mn2 113.79(16) . . ? C52 N3 C48 119.3(2) . . ? C52 N3 Mn2 125.22(16) . . ? C48 N3 Mn2 115.50(15) . . ? C57 N4 C53 117.0(2) . . ? C57 N4 Mn3 127.45(17) . . ? C53 N4 Mn3 111.83(15) . . ? C33 N5 C37 118.2(2) . . ? C33 N5 Mn3 114.40(15) . . ? C37 N5 Mn3 127.07(18) . . ? C32 N6 C28 118.2(2) . . ? C32 N6 Mn1 124.46(16) . . ? C28 N6 Mn1 114.43(15) . . ? C6 C1 C2 120.9(2) . . ? C3 C2 C1 118.8(2) . . ? C3 C2 C13 118.3(2) . . ? C1 C2 C13 122.8(2) . . ? C2 C3 C4 121.3(2) . . ? C5 C4 C3 118.9(2) . . ? C5 C4 C19 120.2(2) . . ? C3 C4 C19 120.8(2) . . ? C4 C5 C6 121.1(2) . . ? C1 C6 C5 118.8(2) . . ? C1 C6 C7 118.2(2) . . ? C5 C6 C7 122.9(2) . . ? C8 C7 C12 118.1(2) . . ? C8 C7 C6 118.0(2) . . ? C12 C7 C6 123.6(2) . . ? C9 C8 C7 122.4(2) . . ? C8 C9 C10 119.8(2) . . ? C11 C10 C9 118.8(2) . . ? C10 C11 C12 123.4(2) . . ? C11 C12 C7 117.6(2) . . ? C11 C12 C25 120.2(2) . . ? C7 C12 C25 122.1(2) . . ? C14 C13 C18 118.4(2) . . ? C14 C13 C2 117.4(2) . . ? C18 C13 C2 124.0(2) . . ? C15 C14 C13 122.1(2) . . ? C14 C15 C16 119.5(2) . . ? C15 C16 C17 119.2(2) . . ? C16 C17 C18 122.8(2) . . ? C17 C18 C13 117.8(2) . . ? C17 C18 C26 119.9(2) . . ? C13 C18 C26 122.2(2) . . ? C20 C19 C24 119.3(2) . . ? C20 C19 C4 116.6(2) . . ? C24 C19 C4 124.0(2) . . ? C21 C20 C19 121.5(2) . . ? C22 C21 C20 119.8(2) . . ? C21 C22 C23 119.2(2) . . ? C22 C23 C24 121.9(2) . . ? C23 C24 C19 118.3(2) . . ? C23 C24 C27 118.5(2) . . ? C19 C24 C27 123.2(2) . . ? O3 C25 C33 110.18(19) . . ? O3 C25 C12 111.32(18) . . ? C33 C25 C12 110.27(19) . . ? O3 C25 C28 106.36(19) . . ? C33 C25 C28 108.61(18) . . ? C12 C25 C28 109.98(19) . . ? O1 C26 C38 109.45(19) . . ? O1 C26 C43 106.80(18) . . ? C38 C26 C43 112.97(18) . . ? O1 C26 C18 112.94(17) . . ? C38 C26 C18 107.56(18) . . ? C43 C26 C18 107.20(19) . . ? O2 C27 C48 109.01(18) . . ? O2 C27 C24 112.05(19) . . ? C48 C27 C24 110.53(18) . . ? O2 C27 C53 106.11(18) . . ? C48 C27 C53 111.7(2) . . ? C24 C27 C53 107.43(18) . . ? N6 C28 C29 122.0(2) . . ? N6 C28 C25 112.2(2) . . ? C29 C28 C25 125.7(2) . . ? C28 C29 C30 119.6(2) . . ? C31 C30 C29 118.4(2) . . ? C30 C31 C32 119.0(2) . . ? N6 C32 C31 122.7(2) . . ? N5 C33 C34 121.6(2) . . ? N5 C33 C25 115.2(2) . . ? C34 C33 C25 123.2(2) . . ? C33 C34 C35 120.1(3) . . ? C36 C35 C34 118.2(3) . . ? C35 C36 C37 118.8(2) . . ? N5 C37 C36 123.2(3) . . ? N1 C38 C39 121.1(2) . . ? N1 C38 C26 115.44(19) . . ? C39 C38 C26 123.3(2) . . ? C38 C39 C40 119.3(2) . . ? C41 C40 C39 118.7(2) . . ? C42 C41 C40 118.7(2) . . ? N1 C42 C41 122.7(2) . . ? N2 C43 C44 122.0(2) . . ? N2 C43 C26 112.68(19) . . ? C44 C43 C26 125.2(2) . . ? C43 C44 C45 119.4(2) . . ? C46 C45 C44 118.2(2) . . ? C47 C46 C45 119.0(2) . . ? N2 C47 C46 122.7(2) . . ? N3 C48 C49 120.6(2) . . ? N3 C48 C27 115.1(2) . . ? C49 C48 C27 124.2(2) . . ? C48 C49 C50 119.7(2) . . ? C51 C50 C49 119.0(2) . . ? C50 C51 C52 118.6(2) . . ? N3 C52 C51 122.6(2) . . ? N4 C53 C54 122.7(2) . . ? N4 C53 C27 111.6(2) . . ? C54 C53 C27 125.7(2) . . ? C53 C54 C55 118.9(2) . . ? C56 C55 C54 119.2(3) . . ? C55 C56 C57 118.3(2) . . ? N4 C57 C56 123.8(3) . . ? O5 C58 O4 123.0(3) . . ? O5 C58 C59 119.4(2) . . ? O4 C58 C59 117.6(2) . . ? O7 C60 O6 124.9(3) . . ? O7 C60 C61 120.7(3) . . ? O6 C60 C61 114.4(2) . . ? O8 C62 O9 122.2(2) . . ? O8 C62 C63 118.5(2) . . ? O9 C62 C63 119.2(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.734 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.086 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.142 0.500 0.000 1415 430 ' ' _platon_squeeze_details ; ; data_eyt28 _database_code_depnum_ccdc_archive 'CCDC 803592' #TrackingRef '- eyt28.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H45 N6 O7 Zn3' _chemical_formula_sum 'C61 H45 N6 O7 Zn3' _chemical_formula_weight 1170.14 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.1063(11) _cell_length_b 18.7848(9) _cell_length_c 36.1295(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12967.2(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9960 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.91 _exptl_crystal_description Fragment _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4792 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7858 _exptl_absorpt_correction_T_max 0.9035 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 5 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 105797 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 26.43 _reflns_number_total 13288 _reflns_number_gt 8098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13288 _refine_ls_number_parameters 696 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0967 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 2.297 _refine_ls_restrained_S_all 2.297 _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 Zn1 Zn 0.31940(3) 0.57471(3) 0.130688(18) 0.02152(17) Uani 1 1 d . . . Zn2 Zn 0.46676(3) 0.65938(3) 0.099890(18) 0.02230(17) Uani 1 1 d . . . Zn3 Zn 0.39574(3) 0.68533(3) 0.184491(18) 0.02210(17) Uani 1 1 d . . . O1 O 0.35964(17) 0.63434(15) 0.09151(9) 0.0175(9) Uani 1 1 d . . . O2 O 0.43380(17) 0.72967(15) 0.13698(9) 0.0191(9) Uani 1 1 d . . . O3 O 0.30444(17) 0.66022(15) 0.16597(9) 0.0181(9) Uani 1 1 d . . . O4 O 0.38023(19) 0.51959(16) 0.16579(10) 0.0240(10) Uani 1 1 d . . . O5 O 0.45859(19) 0.60023(16) 0.18645(10) 0.0253(10) Uani 1 1 d . . . O6 O 0.49913(19) 0.56067(16) 0.10643(10) 0.0280(10) Uani 1 1 d . . . O7 O 0.5696(2) 0.5706(2) 0.05692(12) 0.0448(13) Uani 1 1 d . . . N1 N 0.3387(2) 0.4969(2) 0.08545(13) 0.0271(13) Uani 1 1 d . . . N2 N 0.4520(2) 0.6808(2) 0.04448(12) 0.0210(11) Uani 1 1 d . . . N3 N 0.5652(2) 0.7076(2) 0.12020(13) 0.0280(13) Uani 1 1 d . . . N4 N 0.4181(2) 0.7848(2) 0.20376(12) 0.0200(12) Uani 1 1 d . . . N5 N 0.3457(2) 0.6394(2) 0.23570(13) 0.0246(12) Uani 1 1 d . . . N6 N 0.2147(2) 0.5653(2) 0.14441(12) 0.0233(12) Uani 1 1 d . . . C1 C 0.2209(3) 0.7412(2) 0.11602(16) 0.0208(15) Uani 1 1 d . . . H1 H 0.1796 0.7149 0.1213 0.025 Uiso 1 1 calc R . . C2 C 0.2523(3) 0.7338(3) 0.08158(16) 0.0188(14) Uani 1 1 d . . . C3 C 0.3090(3) 0.7740(2) 0.07240(15) 0.0216(15) Uani 1 1 d . . . H3 H 0.3280 0.7715 0.0481 0.026 Uiso 1 1 calc R . . C4 C 0.3390(3) 0.8190(2) 0.09891(16) 0.0212(14) Uani 1 1 d . . . C5 C 0.3085(3) 0.8264(2) 0.13390(15) 0.0212(14) Uani 1 1 d . . . H5 H 0.3281 0.8583 0.1514 0.025 Uiso 1 1 calc R . . C6 C 0.2484(3) 0.7863(2) 0.14314(17) 0.0213(15) Uani 1 1 d . . . C7 C 0.2262(3) 0.6754(3) 0.05688(15) 0.0227(14) Uani 1 1 d . . . C8 C 0.1548(3) 0.6740(3) 0.04671(17) 0.0365(17) Uani 1 1 d . . . H8 H 0.1254 0.7107 0.0560 0.044 Uiso 1 1 calc R . . C9 C 0.1246(3) 0.6227(3) 0.02410(16) 0.0383(19) Uani 1 1 d . . . H9 H 0.0765 0.6245 0.0175 0.046 Uiso 1 1 calc R . . C10 C 0.1670(3) 0.5702(3) 0.01190(16) 0.0377(17) Uani 1 1 d . . . H10 H 0.1477 0.5338 -0.0033 0.045 Uiso 1 1 calc R . . C11 C 0.2382(3) 0.5674(3) 0.02073(14) 0.0275(15) Uani 1 1 d . . . H11 H 0.2663 0.5302 0.0109 0.033 Uiso 1 1 calc R . . C12 C 0.2690(3) 0.6193(3) 0.04410(15) 0.0227(15) Uani 1 1 d . . . C13 C 0.4072(3) 0.8545(2) 0.08992(15) 0.0208(14) Uani 1 1 d . . . C14 C 0.4085(3) 0.9000(2) 0.05879(15) 0.0255(15) Uani 1 1 d . . . H14 H 0.3667 0.9072 0.0450 0.031 Uiso 1 1 calc R . . C15 C 0.4697(3) 0.9348(3) 0.04776(16) 0.0292(16) Uani 1 1 d . . . H15 H 0.4694 0.9647 0.0266 0.035 Uiso 1 1 calc R . . C16 C 0.5295(3) 0.9256(3) 0.06750(16) 0.0291(16) Uani 1 1 d . . . H16 H 0.5708 0.9505 0.0606 0.035 Uiso 1 1 calc R . . C17 C 0.5309(3) 0.8804(2) 0.09734(16) 0.0254(14) Uani 1 1 d . . . H17 H 0.5736 0.8739 0.1103 0.030 Uiso 1 1 calc R . . C18 C 0.4708(3) 0.8432(2) 0.10940(14) 0.0188(13) Uani 1 1 d . . . C19 C 0.2227(3) 0.7869(3) 0.18214(16) 0.0189(14) Uani 1 1 d . . . C20 C 0.2014(3) 0.8518(3) 0.19731(16) 0.0266(15) Uani 1 1 d . . . H20 H 0.2041 0.8934 0.1825 0.032 Uiso 1 1 calc R . . C21 C 0.1772(3) 0.8576(3) 0.23212(17) 0.0336(17) Uani 1 1 d . . . H21 H 0.1627 0.9025 0.2415 0.040 Uiso 1 1 calc R . . C22 C 0.1734(3) 0.7972(3) 0.25425(16) 0.0380(17) Uani 1 1 d . . . H22 H 0.1562 0.8001 0.2789 0.046 Uiso 1 1 calc R . . C23 C 0.1954(3) 0.7319(3) 0.23957(16) 0.0299(16) Uani 1 1 d . . . H23 H 0.1928 0.6905 0.2546 0.036 Uiso 1 1 calc R . . C24 C 0.2203(3) 0.7258(3) 0.20455(16) 0.0209(15) Uani 1 1 d . . . C25 C 0.3484(3) 0.6107(3) 0.05537(15) 0.0187(14) Uani 1 1 d . . . C26 C 0.4764(3) 0.7890(3) 0.14279(15) 0.0224(15) Uani 1 1 d . . . C27 C 0.2502(3) 0.6518(3) 0.19140(16) 0.0233(15) Uani 1 1 d . . . C28 C 0.3644(3) 0.5288(3) 0.05457(16) 0.0232(15) Uani 1 1 d . . . C29 C 0.3972(3) 0.4935(3) 0.02671(15) 0.0329(17) Uani 1 1 d . . . H29 H 0.4155 0.5183 0.0060 0.040 Uiso 1 1 calc R . . C30 C 0.4029(4) 0.4219(3) 0.02939(17) 0.053(2) Uani 1 1 d . . . H30 H 0.4251 0.3955 0.0103 0.064 Uiso 1 1 calc R . . C31 C 0.3762(4) 0.3870(3) 0.0603(2) 0.065(3) Uani 1 1 d . . . H31 H 0.3791 0.3367 0.0622 0.077 Uiso 1 1 calc R . . C32 C 0.3458(3) 0.4259(3) 0.08780(17) 0.0440(19) Uani 1 1 d . . . H32 H 0.3293 0.4021 0.1093 0.053 Uiso 1 1 calc R . . C33 C 0.3952(3) 0.6514(2) 0.02900(15) 0.0190(14) Uani 1 1 d . . . C34 C 0.3807(3) 0.6606(2) -0.00732(16) 0.0264(15) Uani 1 1 d . . . H34 H 0.3411 0.6382 -0.0182 0.032 Uiso 1 1 calc R . . C35 C 0.4234(3) 0.7025(3) -0.02802(16) 0.0320(16) Uani 1 1 d . . . H35 H 0.4134 0.7102 -0.0535 0.038 Uiso 1 1 calc R . . C36 C 0.4816(3) 0.7338(3) -0.01200(17) 0.0334(17) Uani 1 1 d . . . H36 H 0.5117 0.7635 -0.0261 0.040 Uiso 1 1 calc R . . C37 C 0.4946(3) 0.7213(3) 0.02418(15) 0.0247(15) Uani 1 1 d . . . H37 H 0.5349 0.7417 0.0354 0.030 Uiso 1 1 calc R . . C38 C 0.5526(3) 0.7615(3) 0.14498(16) 0.0243(15) Uani 1 1 d . . . C39 C 0.6053(3) 0.7860(3) 0.16878(15) 0.0278(15) Uani 1 1 d . . . H39 H 0.5955 0.8234 0.1857 0.033 Uiso 1 1 calc R . . C40 C 0.6709(3) 0.7563(3) 0.16768(17) 0.0374(17) Uani 1 1 d . . . H40 H 0.7071 0.7725 0.1836 0.045 Uiso 1 1 calc R . . C41 C 0.6823(3) 0.7017(3) 0.14248(19) 0.046(2) Uani 1 1 d . . . H41 H 0.7270 0.6795 0.1413 0.056 Uiso 1 1 calc R . . C42 C 0.6289(3) 0.6790(3) 0.11890(18) 0.044(2) Uani 1 1 d . . . H42 H 0.6381 0.6422 0.1015 0.053 Uiso 1 1 calc R . . C43 C 0.4540(3) 0.8248(3) 0.18051(15) 0.0225(14) Uani 1 1 d . . . C44 C 0.4663(3) 0.8960(2) 0.18808(15) 0.0243(14) Uani 1 1 d . . . H44 H 0.4936 0.9242 0.1716 0.029 Uiso 1 1 calc R . . C45 C 0.4387(3) 0.9253(3) 0.21957(15) 0.0275(15) Uani 1 1 d . . . H45 H 0.4472 0.9737 0.2256 0.033 Uiso 1 1 calc R . . C46 C 0.3991(3) 0.8837(3) 0.24191(15) 0.0249(15) Uani 1 1 d . . . H46 H 0.3775 0.9031 0.2633 0.030 Uiso 1 1 calc R . . C47 C 0.3905(3) 0.8144(3) 0.23333(14) 0.0222(14) Uani 1 1 d . . . H47 H 0.3633 0.7856 0.2494 0.027 Uiso 1 1 calc R . . C48 C 0.2815(3) 0.6138(3) 0.22583(16) 0.0250(15) Uani 1 1 d . . . C49 C 0.2480(3) 0.5590(3) 0.24521(16) 0.0316(16) Uani 1 1 d . . . H49 H 0.2041 0.5407 0.2373 0.038 Uiso 1 1 calc R . . C50 C 0.2809(4) 0.5327(3) 0.27605(18) 0.0409(19) Uani 1 1 d . . . H50 H 0.2600 0.4955 0.2901 0.049 Uiso 1 1 calc R . . C51 C 0.3454(3) 0.5612(3) 0.28662(17) 0.0373(18) Uani 1 1 d . . . H51 H 0.3678 0.5447 0.3085 0.045 Uiso 1 1 calc R . . C52 C 0.3764(3) 0.6130(3) 0.26551(16) 0.0298(16) Uani 1 1 d . . . H52 H 0.4212 0.6303 0.2725 0.036 Uiso 1 1 calc R . . C53 C 0.1916(3) 0.6069(3) 0.17236(15) 0.0199(14) Uani 1 1 d . . . C54 C 0.1224(3) 0.6097(3) 0.18222(16) 0.0277(15) Uani 1 1 d . . . H54 H 0.1076 0.6380 0.2026 0.033 Uiso 1 1 calc R . . C55 C 0.0752(3) 0.5712(3) 0.16224(16) 0.0336(17) Uani 1 1 d . . . H55 H 0.0271 0.5726 0.1689 0.040 Uiso 1 1 calc R . . C56 C 0.0960(3) 0.5302(3) 0.13258(17) 0.0321(16) Uani 1 1 d . . . H56 H 0.0631 0.5045 0.1181 0.038 Uiso 1 1 calc R . . C57 C 0.1674(3) 0.5278(2) 0.12461(16) 0.0283(16) Uani 1 1 d . . . H57 H 0.1832 0.4990 0.1047 0.034 Uiso 1 1 calc R . . C58 C 0.4369(3) 0.5377(3) 0.18100(16) 0.0260(15) Uani 1 1 d . . . C59 C 0.4826(3) 0.4784(2) 0.19386(16) 0.0371(18) Uani 1 1 d . . . H59A H 0.5137 0.4638 0.1737 0.056 Uiso 1 1 calc R . . H59B H 0.4535 0.4380 0.2014 0.056 Uiso 1 1 calc R . . H59C H 0.5107 0.4945 0.2150 0.056 Uiso 1 1 calc R . . C60 C 0.5426(4) 0.5373(3) 0.0817(2) 0.0391(19) Uani 1 1 d . . . C61 C 0.5586(4) 0.4581(3) 0.08621(19) 0.086(3) Uani 1 1 d . . . H61A H 0.5176 0.4339 0.0966 0.129 Uiso 1 1 calc R . . H61B H 0.5985 0.4521 0.1029 0.129 Uiso 1 1 calc R . . H61C H 0.5699 0.4375 0.0620 0.129 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0250(4) 0.0185(3) 0.0210(4) -0.0011(3) 0.0032(4) -0.0018(3) Zn2 0.0245(4) 0.0197(3) 0.0226(4) -0.0022(3) 0.0026(4) -0.0007(3) Zn3 0.0249(4) 0.0203(3) 0.0212(4) -0.0004(3) 0.0014(4) -0.0022(3) O1 0.022(2) 0.0164(19) 0.014(2) -0.0015(16) -0.0007(19) 0.0006(16) O2 0.020(2) 0.0180(19) 0.019(3) -0.0023(17) 0.0007(19) -0.0046(17) O3 0.020(2) 0.0178(19) 0.016(2) -0.0001(17) 0.0046(19) -0.0023(18) O4 0.029(3) 0.018(2) 0.025(3) 0.0012(17) 0.002(2) 0.0013(19) O5 0.029(2) 0.018(2) 0.029(3) 0.0030(18) 0.004(2) 0.0010(19) O6 0.032(3) 0.016(2) 0.036(3) -0.0020(18) 0.006(2) 0.0043(18) O7 0.051(3) 0.048(3) 0.035(3) 0.002(2) 0.020(3) 0.012(2) N1 0.035(3) 0.016(3) 0.030(4) -0.006(2) 0.001(3) 0.002(2) N2 0.026(3) 0.017(2) 0.020(3) 0.003(2) 0.008(2) 0.003(2) N3 0.021(3) 0.025(3) 0.038(4) 0.000(2) 0.002(3) 0.000(2) N4 0.026(3) 0.021(3) 0.013(3) 0.002(2) 0.000(2) -0.007(2) N5 0.030(3) 0.020(3) 0.024(3) -0.002(2) 0.003(3) 0.002(2) N6 0.028(3) 0.018(3) 0.024(3) 0.001(2) 0.001(3) -0.004(2) C1 0.014(3) 0.013(3) 0.035(4) -0.001(3) -0.012(3) 0.001(3) C2 0.018(4) 0.018(3) 0.021(4) -0.004(3) -0.006(3) 0.003(3) C3 0.027(4) 0.018(3) 0.020(4) 0.000(3) -0.004(3) 0.000(3) C4 0.024(4) 0.012(3) 0.028(4) 0.009(3) 0.003(3) 0.003(3) C5 0.022(4) 0.011(3) 0.031(4) -0.001(3) 0.003(3) 0.002(3) C6 0.017(3) 0.011(3) 0.036(4) 0.002(3) -0.002(3) 0.007(3) C7 0.028(4) 0.023(3) 0.017(4) 0.001(3) -0.004(3) -0.002(3) C8 0.025(4) 0.033(4) 0.051(5) -0.005(3) 0.001(4) 0.014(3) C9 0.029(4) 0.035(4) 0.051(5) -0.027(3) -0.016(4) 0.005(3) C10 0.047(5) 0.036(4) 0.030(4) -0.012(3) -0.018(4) -0.011(4) C11 0.044(4) 0.023(3) 0.015(4) -0.006(3) -0.003(3) -0.002(3) C12 0.029(4) 0.022(3) 0.017(4) 0.006(3) 0.001(3) -0.003(3) C13 0.027(4) 0.018(3) 0.018(4) -0.010(3) 0.004(3) 0.002(3) C14 0.037(4) 0.021(3) 0.018(4) 0.003(3) -0.004(3) 0.007(3) C15 0.037(4) 0.024(3) 0.026(4) 0.006(3) 0.004(4) 0.001(3) C16 0.026(4) 0.028(3) 0.034(4) 0.014(3) 0.015(3) -0.002(3) C17 0.017(3) 0.028(3) 0.031(4) -0.003(3) 0.000(3) 0.001(3) C18 0.029(4) 0.013(3) 0.014(4) -0.001(2) 0.001(3) 0.002(3) C19 0.017(3) 0.022(3) 0.018(4) -0.004(3) 0.002(3) -0.002(3) C20 0.035(4) 0.023(3) 0.021(4) -0.001(3) 0.004(3) -0.001(3) C21 0.045(4) 0.023(3) 0.033(5) -0.009(3) 0.003(4) 0.002(3) C22 0.047(5) 0.043(4) 0.023(4) -0.009(3) 0.015(4) -0.001(4) C23 0.037(4) 0.025(3) 0.028(4) 0.004(3) 0.010(3) -0.002(3) C24 0.021(4) 0.020(3) 0.022(4) -0.009(3) 0.002(3) -0.002(3) C25 0.022(4) 0.016(3) 0.018(4) 0.000(3) 0.001(3) -0.003(3) C26 0.017(4) 0.019(3) 0.030(4) -0.002(3) 0.001(3) -0.005(3) C27 0.026(4) 0.022(3) 0.022(4) -0.003(3) 0.008(3) -0.006(3) C28 0.031(4) 0.021(3) 0.018(4) 0.004(3) 0.001(3) -0.004(3) C29 0.063(5) 0.014(3) 0.021(4) -0.001(3) 0.015(4) 0.009(3) C30 0.096(6) 0.033(4) 0.030(5) -0.003(3) 0.032(4) 0.003(4) C31 0.116(7) 0.014(3) 0.064(6) -0.017(4) 0.036(5) 0.009(4) C32 0.073(5) 0.019(3) 0.040(5) 0.009(3) 0.021(4) -0.004(4) C33 0.024(4) 0.016(3) 0.016(4) 0.002(3) 0.001(3) -0.003(3) C34 0.036(4) 0.020(3) 0.024(4) 0.001(3) 0.002(3) -0.009(3) C35 0.049(5) 0.034(4) 0.012(4) -0.002(3) -0.001(3) 0.008(3) C36 0.040(5) 0.024(3) 0.037(5) 0.004(3) 0.018(4) -0.001(3) C37 0.031(4) 0.026(3) 0.017(4) 0.000(3) 0.005(3) 0.001(3) C38 0.027(4) 0.020(3) 0.026(4) 0.009(3) 0.003(3) 0.000(3) C39 0.023(4) 0.035(4) 0.025(4) 0.002(3) 0.000(3) -0.002(3) C40 0.028(4) 0.047(4) 0.037(5) 0.005(3) -0.009(4) -0.002(4) C41 0.015(4) 0.046(4) 0.079(6) 0.010(4) -0.004(4) 0.009(3) C42 0.030(4) 0.033(4) 0.069(6) -0.007(4) 0.013(4) 0.008(3) C43 0.022(4) 0.024(3) 0.021(4) -0.010(3) -0.008(3) 0.001(3) C44 0.028(4) 0.024(3) 0.022(4) 0.006(3) -0.005(3) -0.008(3) C45 0.034(4) 0.025(3) 0.023(4) -0.016(3) -0.004(3) 0.004(3) C46 0.027(4) 0.034(4) 0.014(4) 0.000(3) 0.007(3) -0.002(3) C47 0.030(4) 0.024(3) 0.012(4) -0.006(3) 0.003(3) -0.003(3) C48 0.038(4) 0.022(3) 0.015(4) 0.001(3) 0.005(3) 0.007(3) C49 0.036(4) 0.030(3) 0.029(4) 0.007(3) 0.001(4) -0.007(3) C50 0.056(5) 0.033(4) 0.033(5) 0.018(3) 0.017(4) 0.008(4) C51 0.043(5) 0.046(4) 0.023(4) 0.003(3) -0.006(4) 0.018(4) C52 0.039(4) 0.033(4) 0.017(4) 0.007(3) 0.001(3) 0.005(3) C53 0.030(4) 0.014(3) 0.015(4) 0.000(3) 0.001(3) -0.001(3) C54 0.026(4) 0.027(3) 0.030(4) -0.006(3) 0.007(3) -0.003(3) C55 0.026(4) 0.031(4) 0.044(5) -0.007(3) 0.012(4) -0.002(3) C56 0.022(4) 0.024(3) 0.050(5) -0.004(3) 0.002(4) -0.008(3) C57 0.040(4) 0.014(3) 0.031(4) -0.003(3) 0.001(4) -0.005(3) C58 0.030(4) 0.027(4) 0.021(4) 0.008(3) 0.002(3) 0.007(3) C59 0.038(4) 0.026(3) 0.047(5) 0.000(3) -0.010(4) 0.002(3) C60 0.038(5) 0.030(4) 0.049(6) -0.018(4) -0.003(4) 0.013(4) C61 0.095(7) 0.035(4) 0.127(8) 0.002(4) 0.044(6) 0.033(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 Zn1 Zn2 3.4199(9) . yes Zn1 Zn3 3.1975(9) . yes Zn2 Zn3 3.3796(9) . yes Zn1 O1 1.962(3) . yes Zn1 O4 2.008(4) . yes Zn1 O3 2.070(3) . yes Zn1 N6 2.069(4) . yes Zn1 N1 2.223(4) . yes Zn2 O6 1.969(3) . yes Zn2 O2 1.984(3) . yes Zn2 N2 2.061(4) . yes Zn2 O1 2.122(3) . yes Zn2 N3 2.212(4) . yes Zn3 O3 1.927(3) . yes Zn3 O5 2.001(3) . yes Zn3 N4 2.039(4) . yes Zn3 O2 2.042(3) . yes Zn3 N5 2.254(4) . yes O1 C25 1.395(6) . ? O2 C26 1.395(5) . ? O3 C27 1.394(6) . ? O4 C58 1.261(6) . ? O5 C58 1.261(6) . ? O6 C60 1.296(7) . ? O7 C60 1.208(7) . ? N1 C32 1.343(6) . ? N1 C28 1.358(6) . ? N2 C33 1.340(6) . ? N2 C37 1.334(6) . ? N3 C42 1.331(6) . ? N3 C38 1.372(6) . ? N4 C47 1.315(6) . ? N4 C43 1.320(6) . ? N5 C52 1.323(6) . ? N5 C48 1.365(7) . ? N6 C53 1.351(6) . ? N6 C57 1.350(6) . ? C1 C2 1.388(7) . ? C1 C6 1.397(7) . ? C2 C3 1.361(7) . ? C2 C7 1.499(7) . ? C3 C4 1.401(7) . ? C4 C5 1.399(7) . ? C4 C13 1.498(7) . ? C5 C6 1.413(7) . ? C6 C19 1.492(7) . ? C7 C8 1.414(7) . ? C7 C12 1.412(7) . ? C8 C9 1.388(7) . ? C9 C10 1.350(7) . ? C10 C11 1.397(7) . ? C11 C12 1.417(7) . ? C12 C25 1.580(7) . ? C13 C14 1.413(6) . ? C13 C18 1.420(7) . ? C14 C15 1.397(7) . ? C15 C16 1.359(7) . ? C16 C17 1.372(6) . ? C17 C18 1.412(7) . ? C18 C26 1.583(7) . ? C19 C20 1.397(6) . ? C19 C24 1.405(7) . ? C20 C21 1.345(7) . ? C21 C22 1.389(7) . ? C22 C23 1.401(7) . ? C23 C24 1.357(7) . ? C24 C27 1.578(6) . ? C25 C28 1.570(6) . ? C25 C33 1.513(7) . ? C26 C38 1.548(7) . ? C26 C43 1.579(7) . ? C27 C53 1.561(7) . ? C27 C48 1.553(7) . ? C28 C29 1.358(7) . ? C29 C30 1.353(6) . ? C30 C31 1.390(8) . ? C31 C32 1.364(7) . ? C33 C34 1.352(7) . ? C34 C35 1.358(7) . ? C35 C36 1.384(7) . ? C36 C37 1.351(7) . ? C38 C39 1.401(7) . ? C39 C40 1.373(7) . ? C40 C41 1.389(7) . ? C41 C42 1.397(8) . ? C43 C44 1.386(6) . ? C44 C45 1.369(7) . ? C45 C46 1.355(6) . ? C46 C47 1.347(6) . ? C48 C49 1.400(7) . ? C49 C50 1.371(7) . ? C50 C51 1.398(8) . ? C51 C52 1.370(7) . ? C53 C54 1.372(7) . ? C54 C55 1.363(7) . ? C55 C56 1.378(7) . ? C56 C57 1.394(7) . ? C58 C59 1.488(6) . ? C60 C61 1.528(7) . ? 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 Zn3 Zn1 Zn2 61.314(19) . . yes Zn3 Zn2 Zn1 56.098(18) . . yes Zn1 Zn3 Zn2 62.588(19) . . yes O1 Zn1 O4 121.55(14) . . yes O1 Zn1 O3 93.17(13) . . yes O4 Zn1 O3 95.23(13) . . yes O1 Zn1 N6 126.93(15) . . yes O4 Zn1 N6 111.36(15) . . yes O3 Zn1 N6 77.61(15) . . yes O1 Zn1 N1 77.29(15) . . yes O4 Zn1 N1 91.70(15) . . yes O3 Zn1 N1 170.21(15) . . yes N6 Zn1 N1 106.25(17) . . yes O1 Zn1 Zn3 83.62(10) . . yes O4 Zn1 Zn3 71.76(10) . . yes O3 Zn1 Zn3 35.37(9) . . yes N6 Zn1 Zn3 110.56(13) . . yes N1 Zn1 Zn3 143.00(12) . . yes O1 Zn1 Zn2 34.62(10) . . yes O4 Zn1 Zn2 88.21(10) . . yes O3 Zn1 Zn2 87.31(9) . . yes N6 Zn1 Zn2 156.07(11) . . yes N1 Zn1 Zn2 86.00(12) . . yes O6 Zn2 O2 130.20(15) . . yes O6 Zn2 N2 110.10(15) . . yes O2 Zn2 N2 118.83(14) . . yes O6 Zn2 O1 96.39(13) . . yes O2 Zn2 O1 86.43(13) . . yes N2 Zn2 O1 76.84(16) . . yes O6 Zn2 N3 94.54(15) . . yes O2 Zn2 N3 76.88(15) . . yes N2 Zn2 N3 111.02(17) . . yes O1 Zn2 N3 163.31(15) . . yes O6 Zn2 Zn3 98.82(11) . . yes O2 Zn2 Zn3 33.45(9) . . yes N2 Zn2 Zn3 142.65(12) . . yes O1 Zn2 Zn3 76.92(9) . . yes N3 Zn2 Zn3 88.97(12) . . yes O6 Zn2 Zn1 77.38(11) . . yes O2 Zn2 Zn1 80.12(9) . . yes N2 Zn2 Zn1 107.09(13) . . yes O1 Zn2 Zn1 31.70(9) . . yes N3 Zn2 Zn1 141.47(12) . . yes O3 Zn3 O5 111.11(14) . . yes O3 Zn3 N4 122.16(15) . . yes O5 Zn3 N4 126.47(16) . . yes O3 Zn3 O2 97.48(14) . . yes O5 Zn3 O2 98.16(13) . . yes N4 Zn3 O2 80.71(15) . . yes O3 Zn3 N5 78.90(16) . . yes O5 Zn3 N5 85.39(15) . . yes N4 Zn3 N5 99.17(16) . . yes O2 Zn3 N5 175.70(16) . . yes O3 Zn3 Zn1 38.45(9) . . yes O5 Zn3 Zn1 77.06(10) . . yes N4 Zn3 Zn1 153.96(12) . . yes O2 Zn3 Zn1 85.21(9) . . yes N5 Zn3 Zn1 93.25(12) . . yes O3 Zn3 Zn2 90.81(10) . . yes O5 Zn3 Zn2 71.08(10) . . yes N4 Zn3 Zn2 110.91(13) . . yes O2 Zn3 Zn2 32.38(8) . . yes N5 Zn3 Zn2 149.02(10) . . yes C25 O1 Zn1 115.7(3) . . ? C25 O1 Zn2 110.6(3) . . ? Zn1 O1 Zn2 113.68(16) . . ? C26 O2 Zn2 116.6(3) . . ? C26 O2 Zn3 114.0(3) . . ? Zn2 O2 Zn3 114.17(14) . . ? C27 O3 Zn3 118.1(3) . . ? C27 O3 Zn1 114.8(3) . . ? Zn3 O3 Zn1 106.18(15) . . ? C58 O4 Zn1 129.3(3) . . ? C58 O5 Zn3 122.8(4) . . ? C60 O6 Zn2 115.9(4) . . ? C32 N1 C28 116.9(5) . . ? C32 N1 Zn1 128.5(4) . . ? C28 N1 Zn1 112.0(3) . . ? C33 N2 C37 120.0(5) . . ? C33 N2 Zn2 115.9(4) . . ? C37 N2 Zn2 124.1(4) . . ? C42 N3 C38 118.7(5) . . ? C42 N3 Zn2 126.8(4) . . ? C38 N3 Zn2 111.7(4) . . ? C47 N4 C43 119.0(4) . . ? C47 N4 Zn3 125.6(4) . . ? C43 N4 Zn3 114.4(4) . . ? C52 N5 C48 118.6(5) . . ? C52 N5 Zn3 128.6(4) . . ? C48 N5 Zn3 107.6(4) . . ? C53 N6 C57 118.7(5) . . ? C53 N6 Zn1 116.4(4) . . ? C57 N6 Zn1 124.4(4) . . ? C2 C1 C6 121.8(5) . . ? C1 C2 C3 120.4(5) . . ? C1 C2 C7 117.6(5) . . ? C3 C2 C7 121.7(5) . . ? C2 C3 C4 119.6(5) . . ? C3 C4 C5 120.4(5) . . ? C3 C4 C13 118.4(5) . . ? C5 C4 C13 121.0(5) . . ? C6 C5 C4 120.0(5) . . ? C5 C6 C1 117.6(6) . . ? C5 C6 C19 119.1(5) . . ? C1 C6 C19 122.9(5) . . ? C8 C7 C12 117.4(5) . . ? C8 C7 C2 119.3(5) . . ? C12 C7 C2 123.3(5) . . ? C9 C8 C7 124.5(5) . . ? C10 C9 C8 116.8(6) . . ? C9 C10 C11 122.4(5) . . ? C10 C11 C12 121.0(5) . . ? C7 C12 C11 117.9(5) . . ? C7 C12 C25 123.2(5) . . ? C11 C12 C25 118.9(5) . . ? C14 C13 C18 118.0(5) . . ? C14 C13 C4 117.2(5) . . ? C18 C13 C4 124.8(5) . . ? C15 C14 C13 121.7(5) . . ? C16 C15 C14 119.7(5) . . ? C15 C16 C17 120.4(6) . . ? C18 C17 C16 122.2(5) . . ? C17 C18 C13 118.0(5) . . ? C17 C18 C26 119.9(5) . . ? C13 C18 C26 122.1(5) . . ? C20 C19 C24 118.5(5) . . ? C20 C19 C6 118.2(5) . . ? C24 C19 C6 123.2(5) . . ? C21 C20 C19 122.5(5) . . ? C20 C21 C22 119.3(5) . . ? C21 C22 C23 118.8(5) . . ? C22 C23 C24 122.1(5) . . ? C23 C24 C19 118.7(5) . . ? C23 C24 C27 118.8(5) . . ? C19 C24 C27 122.4(5) . . ? O1 C25 C28 107.4(4) . . ? O1 C25 C33 109.8(4) . . ? C28 C25 C33 111.6(4) . . ? O1 C25 C12 110.9(4) . . ? C28 C25 C12 106.4(4) . . ? C33 C25 C12 110.7(4) . . ? O2 C26 C38 106.8(4) . . ? O2 C26 C43 108.2(4) . . ? C38 C26 C43 110.7(5) . . ? O2 C26 C18 111.1(4) . . ? C38 C26 C18 108.5(4) . . ? C43 C26 C18 111.4(4) . . ? O3 C27 C53 107.7(4) . . ? O3 C27 C48 107.1(4) . . ? C53 C27 C48 112.4(4) . . ? O3 C27 C24 111.5(4) . . ? C53 C27 C24 110.5(4) . . ? C48 C27 C24 107.6(4) . . ? N1 C28 C29 124.1(5) . . ? N1 C28 C25 110.2(5) . . ? C29 C28 C25 125.6(5) . . ? C28 C29 C30 118.0(5) . . ? C31 C30 C29 119.7(6) . . ? C32 C31 C30 119.3(6) . . ? N1 C32 C31 122.0(6) . . ? N2 C33 C34 121.2(5) . . ? N2 C33 C25 115.0(5) . . ? C34 C33 C25 123.7(5) . . ? C35 C34 C33 119.0(6) . . ? C34 C35 C36 119.9(6) . . ? C35 C36 C37 118.6(6) . . ? N2 C37 C36 121.2(6) . . ? N3 C38 C39 121.2(5) . . ? N3 C38 C26 112.2(5) . . ? C39 C38 C26 126.7(5) . . ? C38 C39 C40 120.2(5) . . ? C41 C40 C39 117.6(6) . . ? C42 C41 C40 120.7(6) . . ? N3 C42 C41 121.6(6) . . ? N4 C43 C44 120.8(5) . . ? N4 C43 C26 116.6(4) . . ? C44 C43 C26 122.4(5) . . ? C43 C44 C45 119.1(5) . . ? C46 C45 C44 118.6(5) . . ? C45 C46 C47 119.2(5) . . ? N4 C47 C46 123.2(5) . . ? N5 C48 C49 122.6(5) . . ? N5 C48 C27 113.2(5) . . ? C49 C48 C27 124.2(6) . . ? C50 C49 C48 117.5(6) . . ? C51 C50 C49 119.2(6) . . ? C50 C51 C52 120.1(6) . . ? N5 C52 C51 121.8(6) . . ? N6 C53 C54 122.1(5) . . ? N6 C53 C27 114.1(5) . . ? C54 C53 C27 123.8(5) . . ? C53 C54 C55 118.7(5) . . ? C56 C55 C54 121.2(6) . . ? C57 C56 C55 117.5(6) . . ? N6 C57 C56 121.9(5) . . ? O4 C58 O5 126.9(5) . . ? O4 C58 C59 116.0(5) . . ? O5 C58 C59 117.1(5) . . ? O7 C60 O6 127.6(6) . . ? O7 C60 C61 119.8(6) . . ? O6 C60 C61 112.6(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.813 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.102 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.740 -0.049 0.250 1980 536 ' ' 2 0.722 0.033 0.750 1980 530 ' ' _platon_squeeze_details ; ; # Attachment '- eyt31.cif' data_eyt31 _database_code_depnum_ccdc_archive 'CCDC 803593' #TrackingRef '- eyt31.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H45 Cu3 N6 O7' _chemical_formula_sum 'C61 H45 Cu3 N6 O7' _chemical_formula_weight 1164.65 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.9118(5) _cell_length_b 19.0501(5) _cell_length_c 36.0732(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12996.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9955 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 24.95 _exptl_crystal_description Fragment _exptl_crystal_colour Green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4768 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8063 _exptl_absorpt_correction_T_max 0.9046 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 4 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 105802 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.40 _reflns_number_total 13264 _reflns_number_gt 9476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13264 _refine_ls_number_parameters 696 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 2.988 _refine_ls_restrained_S_all 2.988 _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 Cu1 Cu 0.31112(3) 0.58005(3) 0.128939(13) 0.02521(14) Uani 1 1 d . . . Cu2 Cu 0.46247(3) 0.65700(3) 0.105172(13) 0.02495(14) Uani 1 1 d . . . Cu3 Cu 0.39213(3) 0.68654(3) 0.183777(13) 0.02435(14) Uani 1 1 d . . . O1 O 0.36047(13) 0.63861(13) 0.09286(6) 0.0203(7) Uani 1 1 d . . . O2 O 0.42657(13) 0.72994(13) 0.13837(6) 0.0207(7) Uani 1 1 d . . . O3 O 0.29845(13) 0.65949(13) 0.16151(6) 0.0207(7) Uani 1 1 d . . . O4 O 0.37038(16) 0.52090(14) 0.16753(7) 0.0294(8) Uani 1 1 d . . . O5 O 0.45713(15) 0.59967(14) 0.17975(7) 0.0303(8) Uani 1 1 d . . . O6 O 0.49511(15) 0.56058(14) 0.09823(8) 0.0328(8) Uani 1 1 d . . . O7 O 0.57210(17) 0.57482(18) 0.05148(9) 0.0523(10) Uani 1 1 d . . . N1 N 0.33350(18) 0.50686(18) 0.09046(9) 0.0276(9) Uani 1 1 d . . . N2 N 0.45202(19) 0.68285(17) 0.04566(9) 0.0258(9) Uani 1 1 d . . . N3 N 0.55538(18) 0.69463(18) 0.12615(9) 0.0273(9) Uani 1 1 d . . . N4 N 0.41426(18) 0.78220(17) 0.20379(9) 0.0239(9) Uani 1 1 d . . . N5 N 0.34804(19) 0.63944(16) 0.22851(9) 0.0242(9) Uani 1 1 d . . . N6 N 0.20947(18) 0.56311(17) 0.14454(9) 0.0244(9) Uani 1 1 d . . . C1 C 0.2196(2) 0.7444(2) 0.11582(11) 0.0220(11) Uani 1 1 d . . . H1 H 0.1773 0.7193 0.1210 0.026 Uiso 1 1 calc R . . C2 C 0.2514(2) 0.7367(2) 0.08162(11) 0.0204(10) Uani 1 1 d . . . C3 C 0.3097(2) 0.77629(19) 0.07344(10) 0.0205(10) Uani 1 1 d . . . H3 H 0.3300 0.7734 0.0494 0.025 Uiso 1 1 calc R . . C4 C 0.3399(2) 0.8207(2) 0.09970(11) 0.0207(10) Uani 1 1 d . . . C5 C 0.3079(2) 0.82825(19) 0.13425(10) 0.0212(10) Uani 1 1 d . . . H5 H 0.3266 0.8603 0.1519 0.025 Uiso 1 1 calc R . . C6 C 0.2480(2) 0.7883(2) 0.14281(11) 0.0204(10) Uani 1 1 d . . . C7 C 0.2263(2) 0.6801(2) 0.05672(11) 0.0230(10) Uani 1 1 d . . . C8 C 0.1556(2) 0.6801(2) 0.04641(11) 0.0387(13) Uani 1 1 d . . . H8 H 0.1266 0.7172 0.0553 0.046 Uiso 1 1 calc R . . C9 C 0.1242(3) 0.6292(3) 0.02392(12) 0.0448(14) Uani 1 1 d . . . H9 H 0.0756 0.6313 0.0174 0.054 Uiso 1 1 calc R . . C10 C 0.1666(3) 0.5768(3) 0.01185(12) 0.0408(13) Uani 1 1 d . . . H10 H 0.1477 0.5416 -0.0040 0.049 Uiso 1 1 calc R . . C11 C 0.2367(2) 0.5735(2) 0.02218(11) 0.0314(12) Uani 1 1 d . . . H11 H 0.2647 0.5355 0.0135 0.038 Uiso 1 1 calc R . . C12 C 0.2682(2) 0.6243(2) 0.04514(10) 0.0231(11) Uani 1 1 d . . . C13 C 0.4093(2) 0.8538(2) 0.09161(10) 0.0222(10) Uani 1 1 d . . . C14 C 0.4142(2) 0.8998(2) 0.06130(11) 0.0269(11) Uani 1 1 d . . . H14 H 0.3729 0.9086 0.0470 0.032 Uiso 1 1 calc R . . C15 C 0.4762(2) 0.9328(2) 0.05140(12) 0.0332(12) Uani 1 1 d . . . H15 H 0.4771 0.9643 0.0310 0.040 Uiso 1 1 calc R . . C16 C 0.5367(2) 0.9199(2) 0.07125(11) 0.0331(12) Uani 1 1 d . . . H16 H 0.5796 0.9426 0.0647 0.040 Uiso 1 1 calc R . . C17 C 0.5350(2) 0.8735(2) 0.10113(11) 0.0272(11) Uani 1 1 d . . . H17 H 0.5770 0.8648 0.1148 0.033 Uiso 1 1 calc R . . C18 C 0.4717(2) 0.8390(2) 0.11131(10) 0.0227(10) Uani 1 1 d . . . C19 C 0.2219(2) 0.7868(2) 0.18149(11) 0.0229(10) Uani 1 1 d . . . C20 C 0.2021(2) 0.8504(2) 0.19788(11) 0.0306(12) Uani 1 1 d . . . H20 H 0.2046 0.8925 0.1838 0.037 Uiso 1 1 calc R . . C21 C 0.1791(2) 0.8531(2) 0.23384(12) 0.0411(13) Uani 1 1 d . . . H21 H 0.1676 0.8971 0.2447 0.049 Uiso 1 1 calc R . . C22 C 0.1726(3) 0.7921(2) 0.25438(11) 0.0396(13) Uani 1 1 d . . . H22 H 0.1550 0.7937 0.2790 0.048 Uiso 1 1 calc R . . C23 C 0.1918(2) 0.7291(2) 0.23867(11) 0.0321(12) Uani 1 1 d . . . H23 H 0.1875 0.6874 0.2529 0.039 Uiso 1 1 calc R . . C24 C 0.2173(2) 0.7244(2) 0.20250(11) 0.0233(11) Uani 1 1 d . . . C25 C 0.3466(2) 0.6138(2) 0.05672(11) 0.0218(10) Uani 1 1 d . . . C26 C 0.4744(2) 0.7857(2) 0.14463(10) 0.0207(10) Uani 1 1 d . . . C27 C 0.2463(2) 0.6510(2) 0.18877(11) 0.0239(10) Uani 1 1 d . . . C28 C 0.3598(2) 0.5343(2) 0.05857(11) 0.0254(11) Uani 1 1 d . . . C29 C 0.3898(2) 0.4926(2) 0.03138(12) 0.0366(13) Uani 1 1 d . . . H29 H 0.4086 0.5129 0.0094 0.044 Uiso 1 1 calc R . . C30 C 0.3919(3) 0.4213(2) 0.03675(13) 0.0500(15) Uani 1 1 d . . . H30 H 0.4115 0.3915 0.0183 0.060 Uiso 1 1 calc R . . C31 C 0.3650(3) 0.3930(2) 0.06942(13) 0.0527(16) Uani 1 1 d . . . H31 H 0.3656 0.3437 0.0734 0.063 Uiso 1 1 calc R . . C32 C 0.3377(2) 0.4369(2) 0.09582(12) 0.0424(14) Uani 1 1 d . . . H32 H 0.3213 0.4176 0.1185 0.051 Uiso 1 1 calc R . . C33 C 0.3956(2) 0.6525(2) 0.03006(11) 0.0229(10) Uani 1 1 d . . . C34 C 0.3813(2) 0.6588(2) -0.00722(11) 0.0277(11) Uani 1 1 d . . . H34 H 0.3415 0.6358 -0.0177 0.033 Uiso 1 1 calc R . . C35 C 0.4249(3) 0.6985(2) -0.02897(12) 0.0355(12) Uani 1 1 d . . . H35 H 0.4157 0.7039 -0.0547 0.043 Uiso 1 1 calc R . . C36 C 0.4829(2) 0.7309(2) -0.01270(13) 0.0355(13) Uani 1 1 d . . . H36 H 0.5138 0.7592 -0.0271 0.043 Uiso 1 1 calc R . . C37 C 0.4949(2) 0.7213(2) 0.02442(12) 0.0301(12) Uani 1 1 d . . . H37 H 0.5352 0.7427 0.0354 0.036 Uiso 1 1 calc R . . C38 C 0.5477(2) 0.7529(2) 0.14727(11) 0.0230(10) Uani 1 1 d . . . C39 C 0.6035(2) 0.7788(2) 0.16805(11) 0.0309(12) Uani 1 1 d . . . H39 H 0.5971 0.8196 0.1828 0.037 Uiso 1 1 calc R . . C40 C 0.6686(2) 0.7455(3) 0.16741(12) 0.0360(13) Uani 1 1 d . . . H40 H 0.7074 0.7628 0.1814 0.043 Uiso 1 1 calc R . . C41 C 0.6748(2) 0.6859(3) 0.14556(12) 0.0413(13) Uani 1 1 d . . . H41 H 0.7185 0.6614 0.1444 0.050 Uiso 1 1 calc R . . C42 C 0.6171(3) 0.6619(2) 0.12529(12) 0.0402(13) Uani 1 1 d . . . H42 H 0.6221 0.6210 0.1105 0.048 Uiso 1 1 calc R . . C43 C 0.4523(2) 0.8220(2) 0.18072(10) 0.0226(10) Uani 1 1 d . . . C44 C 0.4662(2) 0.8908(2) 0.18906(11) 0.0260(11) Uani 1 1 d . . . H44 H 0.4960 0.9181 0.1735 0.031 Uiso 1 1 calc R . . C45 C 0.4362(2) 0.9200(2) 0.22049(11) 0.0280(11) Uani 1 1 d . . . H45 H 0.4449 0.9677 0.2266 0.034 Uiso 1 1 calc R . . C46 C 0.3941(2) 0.8801(2) 0.24268(11) 0.0280(11) Uani 1 1 d . . . H46 H 0.3711 0.8998 0.2636 0.034 Uiso 1 1 calc R . . C47 C 0.3859(2) 0.8106(2) 0.23390(10) 0.0276(11) Uani 1 1 d . . . H47 H 0.3589 0.7816 0.2500 0.033 Uiso 1 1 calc R . . C48 C 0.2824(2) 0.6152(2) 0.22236(11) 0.0222(11) Uani 1 1 d . . . C49 C 0.2515(2) 0.5653(2) 0.24508(11) 0.0299(11) Uani 1 1 d . . . H49 H 0.2057 0.5476 0.2397 0.036 Uiso 1 1 calc R . . C50 C 0.2884(3) 0.5420(2) 0.27552(12) 0.0382(13) Uani 1 1 d . . . H50 H 0.2686 0.5080 0.2917 0.046 Uiso 1 1 calc R . . C51 C 0.3548(3) 0.5691(2) 0.28203(12) 0.0359(13) Uani 1 1 d . . . H51 H 0.3807 0.5545 0.3032 0.043 Uiso 1 1 calc R . . C52 C 0.3834(2) 0.6168(2) 0.25813(11) 0.0283(11) Uani 1 1 d . . . H52 H 0.4297 0.6343 0.2627 0.034 Uiso 1 1 calc R . . C53 C 0.1873(2) 0.6052(2) 0.17242(11) 0.0219(10) Uani 1 1 d . . . C54 C 0.1173(2) 0.6079(2) 0.18299(11) 0.0301(11) Uani 1 1 d . . . H54 H 0.1030 0.6374 0.2028 0.036 Uiso 1 1 calc R . . C55 C 0.0681(2) 0.5670(2) 0.16439(12) 0.0341(12) Uani 1 1 d . . . H55 H 0.0198 0.5674 0.1716 0.041 Uiso 1 1 calc R . . C56 C 0.0907(2) 0.5252(2) 0.13485(12) 0.0328(12) Uani 1 1 d . . . H56 H 0.0580 0.4980 0.1210 0.039 Uiso 1 1 calc R . . C57 C 0.1611(2) 0.5245(2) 0.12638(12) 0.0287(11) Uani 1 1 d . . . H57 H 0.1767 0.4953 0.1067 0.034 Uiso 1 1 calc R . . C58 C 0.4303(3) 0.5370(2) 0.17743(12) 0.0327(12) Uani 1 1 d . . . C59 C 0.4803(2) 0.4790(2) 0.18790(14) 0.0570(16) Uani 1 1 d . . . H59A H 0.5164 0.4739 0.1686 0.085 Uiso 1 1 calc R . . H59B H 0.4540 0.4349 0.1904 0.085 Uiso 1 1 calc R . . H59C H 0.5032 0.4904 0.2115 0.085 Uiso 1 1 calc R . . C60 C 0.5411(3) 0.5393(3) 0.07433(15) 0.0435(14) Uani 1 1 d . . . C61 C 0.5557(3) 0.4634(3) 0.07726(18) 0.103(3) Uani 1 1 d . . . H61A H 0.5215 0.4418 0.0942 0.155 Uiso 1 1 calc R . . H61B H 0.6037 0.4563 0.0868 0.155 Uiso 1 1 calc R . . H61C H 0.5514 0.4417 0.0527 0.155 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0320(3) 0.0188(3) 0.0248(3) -0.0042(3) 0.0073(3) -0.0039(3) Cu2 0.0287(3) 0.0185(3) 0.0276(3) -0.0036(2) 0.0042(3) -0.0007(3) Cu3 0.0316(3) 0.0195(3) 0.0220(3) 0.0000(2) 0.0021(3) -0.0025(3) O1 0.0270(18) 0.0157(17) 0.0180(16) -0.0021(12) 0.0035(13) -0.0002(13) O2 0.0252(17) 0.0186(17) 0.0183(16) 0.0018(12) 0.0030(13) -0.0034(14) O3 0.0230(17) 0.0181(16) 0.0211(15) -0.0024(13) 0.0063(13) -0.0021(14) O4 0.030(2) 0.0227(19) 0.0358(19) 0.0014(14) -0.0038(16) -0.0037(16) O5 0.033(2) 0.0199(18) 0.0376(18) 0.0020(14) 0.0060(16) 0.0033(15) O6 0.037(2) 0.0190(18) 0.043(2) -0.0076(15) 0.0095(16) 0.0018(15) O7 0.054(3) 0.060(3) 0.043(2) -0.0017(19) 0.0201(19) 0.009(2) N1 0.037(3) 0.018(2) 0.028(2) -0.0051(17) 0.0066(19) -0.0044(18) N2 0.034(2) 0.016(2) 0.028(2) -0.0019(17) 0.0109(19) -0.0006(19) N3 0.026(2) 0.022(2) 0.034(2) 0.0007(18) 0.0034(18) 0.0018(18) N4 0.035(2) 0.021(2) 0.016(2) -0.0026(16) -0.0003(17) -0.0053(18) N5 0.033(2) 0.020(2) 0.019(2) 0.0017(16) 0.0052(18) 0.0033(19) N6 0.030(2) 0.019(2) 0.025(2) -0.0010(17) 0.0025(18) -0.0021(18) C1 0.020(3) 0.018(3) 0.028(3) 0.001(2) -0.004(2) 0.000(2) C2 0.022(3) 0.017(3) 0.022(3) -0.0039(19) -0.005(2) 0.006(2) C3 0.031(3) 0.013(2) 0.018(2) 0.0018(19) 0.002(2) 0.006(2) C4 0.027(3) 0.013(2) 0.023(2) 0.0087(19) -0.001(2) 0.004(2) C5 0.028(3) 0.011(2) 0.025(2) -0.0022(19) 0.000(2) 0.003(2) C6 0.025(3) 0.014(2) 0.022(3) -0.0006(19) -0.001(2) 0.010(2) C7 0.021(3) 0.024(3) 0.024(2) 0.000(2) -0.002(2) 0.000(2) C8 0.043(3) 0.033(3) 0.040(3) -0.011(2) -0.005(3) 0.014(3) C9 0.036(3) 0.046(4) 0.052(3) -0.023(3) -0.016(3) 0.007(3) C10 0.053(4) 0.039(3) 0.031(3) -0.013(2) -0.012(3) -0.012(3) C11 0.038(3) 0.030(3) 0.027(3) -0.006(2) 0.006(2) 0.002(3) C12 0.030(3) 0.022(3) 0.017(2) -0.006(2) 0.002(2) -0.007(2) C13 0.031(3) 0.016(2) 0.020(2) -0.0047(19) 0.001(2) 0.000(2) C14 0.035(3) 0.021(3) 0.025(3) 0.001(2) -0.003(2) 0.004(2) C15 0.045(3) 0.029(3) 0.026(3) 0.007(2) 0.004(2) 0.000(3) C16 0.035(3) 0.032(3) 0.033(3) 0.007(2) 0.012(2) -0.008(3) C17 0.033(3) 0.022(3) 0.026(3) 0.000(2) 0.001(2) 0.002(2) C18 0.036(3) 0.013(2) 0.019(2) -0.0032(19) 0.006(2) -0.001(2) C19 0.024(3) 0.020(3) 0.025(3) -0.002(2) -0.003(2) 0.001(2) C20 0.045(3) 0.026(3) 0.021(3) -0.002(2) 0.006(2) 0.003(2) C21 0.056(4) 0.026(3) 0.041(3) -0.012(2) 0.011(3) 0.007(3) C22 0.065(4) 0.031(3) 0.023(3) -0.003(2) 0.016(3) 0.002(3) C23 0.044(3) 0.026(3) 0.027(3) 0.001(2) 0.014(2) 0.002(2) C24 0.027(3) 0.024(3) 0.019(2) -0.007(2) 0.001(2) 0.002(2) C25 0.032(3) 0.015(2) 0.019(2) -0.006(2) 0.008(2) -0.003(2) C26 0.028(3) 0.014(2) 0.020(2) -0.0024(19) 0.001(2) -0.005(2) C27 0.025(3) 0.022(3) 0.024(3) -0.002(2) 0.006(2) -0.006(2) C28 0.029(3) 0.023(3) 0.024(3) -0.006(2) 0.002(2) -0.006(2) C29 0.057(4) 0.018(3) 0.035(3) -0.004(2) 0.018(3) 0.000(3) C30 0.084(4) 0.022(3) 0.044(3) -0.013(2) 0.024(3) 0.000(3) C31 0.094(5) 0.013(3) 0.051(3) -0.006(3) 0.035(3) -0.005(3) C32 0.065(4) 0.023(3) 0.039(3) 0.000(2) 0.020(3) -0.012(3) C33 0.029(3) 0.014(2) 0.026(3) -0.005(2) 0.008(2) 0.000(2) C34 0.040(3) 0.020(3) 0.023(3) -0.003(2) 0.004(2) -0.008(2) C35 0.052(4) 0.029(3) 0.025(3) -0.002(2) 0.005(3) 0.003(3) C36 0.039(3) 0.025(3) 0.042(3) 0.000(2) 0.019(3) 0.000(2) C37 0.031(3) 0.024(3) 0.035(3) -0.005(2) 0.008(2) -0.003(2) C38 0.026(3) 0.020(3) 0.023(3) 0.006(2) 0.003(2) -0.005(2) C39 0.037(3) 0.031(3) 0.025(3) 0.000(2) 0.000(2) 0.000(3) C40 0.031(3) 0.048(4) 0.029(3) 0.005(2) -0.003(2) -0.004(3) C41 0.026(3) 0.040(3) 0.058(3) 0.005(3) 0.003(3) 0.009(3) C42 0.032(3) 0.032(3) 0.057(3) -0.003(3) 0.006(3) 0.003(3) C43 0.030(3) 0.021(3) 0.017(2) 0.000(2) -0.002(2) -0.001(2) C44 0.035(3) 0.020(3) 0.023(3) 0.002(2) 0.000(2) -0.004(2) C45 0.043(3) 0.021(3) 0.021(3) -0.001(2) -0.008(2) -0.002(2) C46 0.035(3) 0.030(3) 0.019(2) -0.002(2) 0.001(2) -0.001(2) C47 0.037(3) 0.023(3) 0.023(2) -0.004(2) 0.003(2) -0.007(2) C48 0.033(3) 0.016(3) 0.018(2) -0.001(2) 0.005(2) 0.007(2) C49 0.032(3) 0.028(3) 0.029(3) 0.003(2) 0.003(2) -0.001(2) C50 0.054(4) 0.028(3) 0.033(3) 0.015(2) 0.014(3) 0.012(3) C51 0.039(3) 0.040(3) 0.028(3) 0.010(2) -0.003(2) 0.016(3) C52 0.032(3) 0.029(3) 0.024(3) 0.001(2) 0.001(2) 0.007(2) C53 0.029(3) 0.014(2) 0.023(3) 0.0039(19) 0.005(2) -0.003(2) C54 0.037(3) 0.021(3) 0.032(3) -0.004(2) 0.004(2) -0.001(2) C55 0.025(3) 0.029(3) 0.049(3) 0.002(2) 0.010(2) -0.007(2) C56 0.038(3) 0.021(3) 0.040(3) -0.004(2) 0.005(2) -0.010(2) C57 0.034(3) 0.019(3) 0.033(3) -0.003(2) 0.005(2) -0.004(2) C58 0.047(4) 0.018(3) 0.033(3) 0.006(2) 0.008(3) 0.008(3) C59 0.045(4) 0.024(3) 0.103(5) 0.005(3) -0.021(3) 0.003(3) C60 0.044(4) 0.026(3) 0.060(4) -0.025(3) 0.001(3) 0.010(3) C61 0.101(6) 0.035(4) 0.174(7) -0.021(4) 0.064(5) 0.018(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 Cu1 Cu2 3.3282(7) . yes Cu1 Cu3 3.2212(7) . yes Cu2 Cu3 3.1822(7) . yes Cu1 O3 1.931(2) . yes Cu1 O1 1.952(2) . yes Cu1 N1 2.012(3) . yes Cu1 N6 2.029(3) . yes Cu1 O4 2.113(3) . yes Cu2 O6 1.954(3) . yes Cu2 O2 1.956(2) . yes Cu2 O1 2.010(3) . yes Cu2 N3 2.043(3) . yes Cu2 N2 2.211(3) . yes Cu3 O2 1.947(2) . yes Cu3 N4 2.004(3) . yes Cu3 O3 2.012(3) . yes Cu3 N5 2.026(3) . yes Cu3 O5 2.067(3) . yes O1 C25 1.411(4) . ? O2 C26 1.413(4) . ? O3 C27 1.403(4) . ? O4 C58 1.226(5) . ? O5 C58 1.300(5) . ? O6 C60 1.290(5) . ? O7 C60 1.217(5) . ? N1 C32 1.350(5) . ? N1 C28 1.358(5) . ? N2 C37 1.334(5) . ? N2 C33 1.338(5) . ? N3 C42 1.324(5) . ? N3 C38 1.355(5) . ? N4 C47 1.327(4) . ? N4 C43 1.337(4) . ? N5 C52 1.332(5) . ? N5 C48 1.343(5) . ? N6 C57 1.344(5) . ? N6 C53 1.353(4) . ? C1 C2 1.381(5) . ? C1 C6 1.392(5) . ? C2 C3 1.368(5) . ? C2 C7 1.481(5) . ? C3 C4 1.393(5) . ? C4 C5 1.392(5) . ? C4 C13 1.485(5) . ? C5 C6 1.399(5) . ? C6 C19 1.481(5) . ? C7 C8 1.389(5) . ? C7 C12 1.390(5) . ? C8 C9 1.397(5) . ? C9 C10 1.352(6) . ? C10 C11 1.379(6) . ? C11 C12 1.407(5) . ? C12 C25 1.553(5) . ? C13 C14 1.405(5) . ? C13 C18 1.406(5) . ? C14 C15 1.378(5) . ? C15 C16 1.371(5) . ? C16 C17 1.395(5) . ? C17 C18 1.414(5) . ? C18 C26 1.575(5) . ? C19 C20 1.400(5) . ? C19 C24 1.412(5) . ? C20 C21 1.369(5) . ? C21 C22 1.384(5) . ? C22 C23 1.377(5) . ? C23 C24 1.394(5) . ? C24 C27 1.580(5) . ? C25 C33 1.524(5) . ? C25 C28 1.537(5) . ? C26 C38 1.522(5) . ? C26 C43 1.533(5) . ? C27 C53 1.534(5) . ? C27 C48 1.549(5) . ? C28 C29 1.385(5) . ? C29 C30 1.372(5) . ? C30 C31 1.392(5) . ? C31 C32 1.368(5) . ? C33 C34 1.377(5) . ? C34 C35 1.367(5) . ? C35 C36 1.388(6) . ? C36 C37 1.371(5) . ? C38 C39 1.386(5) . ? C39 C40 1.385(6) . ? C40 C41 1.387(6) . ? C41 C42 1.391(6) . ? C43 C44 1.370(5) . ? C44 C45 1.385(5) . ? C45 C46 1.360(5) . ? C46 C47 1.369(5) . ? C48 C49 1.384(5) . ? C49 C50 1.375(5) . ? C50 C51 1.376(6) . ? C51 C52 1.366(5) . ? C53 C54 1.378(5) . ? C54 C55 1.387(5) . ? C55 C56 1.397(5) . ? C56 C57 1.366(5) . ? C58 C59 1.504(6) . ? C60 C61 1.476(6) . ? 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 Cu3 Cu1 Cu2 58.111(15) . . yes Cu3 Cu2 Cu1 59.261(15) . . yes Cu2 Cu3 Cu1 62.628(15) . . yes O3 Cu1 O1 90.98(10) . . yes O3 Cu1 N1 171.43(13) . . yes O1 Cu1 N1 80.53(12) . . yes O3 Cu1 N6 80.70(12) . . yes O1 Cu1 N6 136.79(12) . . yes N1 Cu1 N6 106.29(14) . . yes O3 Cu1 O4 94.75(10) . . yes O1 Cu1 O4 119.38(11) . . yes N1 Cu1 O4 88.48(12) . . yes N6 Cu1 O4 103.60(12) . . yes O3 Cu1 Cu3 36.07(8) . . yes O1 Cu1 Cu3 79.75(7) . . yes N1 Cu1 Cu3 139.45(10) . . yes N6 Cu1 Cu3 112.36(9) . . yes O4 Cu1 Cu3 71.27(8) . . yes O3 Cu1 Cu2 85.31(8) . . yes O1 Cu1 Cu2 33.41(7) . . yes N1 Cu1 Cu2 86.94(10) . . yes N6 Cu1 Cu2 163.01(9) . . yes O4 Cu1 Cu2 87.04(8) . . yes O6 Cu2 O2 148.87(11) . . yes O6 Cu2 O1 96.37(11) . . yes O2 Cu2 O1 85.76(10) . . yes O6 Cu2 N3 96.07(13) . . yes O2 Cu2 N3 79.77(12) . . yes O1 Cu2 N3 165.53(12) . . yes O6 Cu2 N2 96.50(12) . . yes O2 Cu2 N2 113.90(11) . . yes O1 Cu2 N2 74.84(12) . . yes N3 Cu2 N2 111.00(13) . . yes O6 Cu2 Cu3 114.37(8) . . yes O2 Cu2 Cu3 35.29(7) . . yes O1 Cu2 Cu3 80.01(7) . . yes N3 Cu2 Cu3 88.13(9) . . yes N2 Cu2 Cu3 142.02(9) . . yes O6 Cu2 Cu1 83.72(8) . . yes O2 Cu2 Cu1 81.76(8) . . yes O1 Cu2 Cu1 32.32(7) . . yes N3 Cu2 Cu1 143.01(9) . . yes N2 Cu2 Cu1 105.74(10) . . yes O2 Cu3 N4 81.20(12) . . yes O2 Cu3 O3 93.87(10) . . yes N4 Cu3 O3 124.08(12) . . yes O2 Cu3 N5 174.79(13) . . yes N4 Cu3 N5 101.64(13) . . yes O3 Cu3 N5 80.92(12) . . yes O2 Cu3 O5 94.70(11) . . yes N4 Cu3 O5 129.00(13) . . yes O3 Cu3 O5 106.89(11) . . yes N5 Cu3 O5 86.91(12) . . yes O2 Cu3 Cu2 35.48(7) . . yes N4 Cu3 Cu2 113.23(10) . . yes O3 Cu3 Cu2 88.11(7) . . yes N5 Cu3 Cu2 143.46(9) . . yes O5 Cu3 Cu2 63.07(7) . . yes O2 Cu3 Cu1 84.83(8) . . yes N4 Cu3 Cu1 153.26(9) . . yes O3 Cu3 Cu1 34.40(7) . . yes N5 Cu3 Cu1 90.83(10) . . yes O5 Cu3 Cu1 74.66(8) . . yes C25 O1 Cu1 109.6(2) . . ? C25 O1 Cu2 116.1(2) . . ? Cu1 O1 Cu2 114.28(12) . . ? C26 O2 Cu3 113.5(2) . . ? C26 O2 Cu2 114.2(2) . . ? Cu3 O2 Cu2 109.24(12) . . ? C27 O3 Cu1 115.1(2) . . ? C27 O3 Cu3 111.7(2) . . ? Cu1 O3 Cu3 109.54(12) . . ? C58 O4 Cu1 123.2(3) . . ? C58 O5 Cu3 120.5(3) . . ? C60 O6 Cu2 126.4(3) . . ? C32 N1 C28 118.7(4) . . ? C32 N1 Cu1 126.7(3) . . ? C28 N1 Cu1 113.2(3) . . ? C37 N2 C33 118.7(4) . . ? C37 N2 Cu2 128.7(3) . . ? C33 N2 Cu2 112.5(3) . . ? C42 N3 C38 119.6(4) . . ? C42 N3 Cu2 125.8(3) . . ? C38 N3 Cu2 113.8(3) . . ? C47 N4 C43 119.7(4) . . ? C47 N4 Cu3 125.6(3) . . ? C43 N4 Cu3 113.9(3) . . ? C52 N5 C48 119.1(4) . . ? C52 N5 Cu3 125.1(3) . . ? C48 N5 Cu3 113.6(3) . . ? C57 N6 C53 118.4(4) . . ? C57 N6 Cu1 126.6(3) . . ? C53 N6 Cu1 113.9(3) . . ? C2 C1 C6 121.3(4) . . ? C3 C2 C1 119.1(4) . . ? C3 C2 C7 121.9(4) . . ? C1 C2 C7 118.7(4) . . ? C2 C3 C4 121.2(4) . . ? C5 C4 C3 119.6(4) . . ? C5 C4 C13 121.1(4) . . ? C3 C4 C13 119.1(4) . . ? C4 C5 C6 119.5(4) . . ? C1 C6 C5 119.1(4) . . ? C1 C6 C19 121.2(4) . . ? C5 C6 C19 119.3(4) . . ? C8 C7 C12 118.0(4) . . ? C8 C7 C2 118.1(4) . . ? C12 C7 C2 123.8(4) . . ? C7 C8 C9 124.4(4) . . ? C10 C9 C8 116.7(4) . . ? C9 C10 C11 121.1(4) . . ? C10 C11 C12 122.3(4) . . ? C7 C12 C11 117.5(4) . . ? C7 C12 C25 124.2(4) . . ? C11 C12 C25 118.3(4) . . ? C14 C13 C18 117.6(4) . . ? C14 C13 C4 118.4(4) . . ? C18 C13 C4 123.9(4) . . ? C15 C14 C13 122.9(4) . . ? C16 C15 C14 119.5(4) . . ? C15 C16 C17 119.9(4) . . ? C16 C17 C18 120.9(4) . . ? C13 C18 C17 119.1(4) . . ? C13 C18 C26 122.9(4) . . ? C17 C18 C26 118.0(4) . . ? C20 C19 C24 119.1(4) . . ? C20 C19 C6 118.0(4) . . ? C24 C19 C6 122.9(4) . . ? C21 C20 C19 121.2(4) . . ? C20 C21 C22 120.2(4) . . ? C23 C22 C21 119.3(4) . . ? C22 C23 C24 122.2(4) . . ? C23 C24 C19 118.0(4) . . ? C23 C24 C27 118.0(4) . . ? C19 C24 C27 123.7(4) . . ? O1 C25 C33 108.0(3) . . ? O1 C25 C28 105.0(3) . . ? C33 C25 C28 113.9(3) . . ? O1 C25 C12 112.5(3) . . ? C33 C25 C12 110.3(3) . . ? C28 C25 C12 107.0(3) . . ? O2 C26 C38 106.5(3) . . ? O2 C26 C43 107.5(3) . . ? C38 C26 C43 112.3(3) . . ? O2 C26 C18 110.0(3) . . ? C38 C26 C18 110.0(3) . . ? C43 C26 C18 110.4(3) . . ? O3 C27 C53 107.9(3) . . ? O3 C27 C48 106.8(3) . . ? C53 C27 C48 111.7(3) . . ? O3 C27 C24 111.2(3) . . ? C53 C27 C24 111.9(3) . . ? C48 C27 C24 107.3(3) . . ? N1 C28 C29 122.0(4) . . ? N1 C28 C25 110.9(4) . . ? C29 C28 C25 127.0(4) . . ? C30 C29 C28 118.7(4) . . ? C29 C30 C31 119.5(4) . . ? C32 C31 C30 119.4(4) . . ? N1 C32 C31 121.7(4) . . ? N2 C33 C34 122.0(4) . . ? N2 C33 C25 115.3(4) . . ? C34 C33 C25 122.6(4) . . ? C35 C34 C33 119.4(4) . . ? C34 C35 C36 118.6(4) . . ? C37 C36 C35 119.0(4) . . ? N2 C37 C36 122.2(4) . . ? N3 C38 C39 120.9(4) . . ? N3 C38 C26 113.5(4) . . ? C39 C38 C26 125.6(4) . . ? C40 C39 C38 120.3(4) . . ? C39 C40 C41 117.4(4) . . ? C40 C41 C42 120.1(4) . . ? N3 C42 C41 121.7(4) . . ? N4 C43 C44 120.7(4) . . ? N4 C43 C26 114.8(3) . . ? C44 C43 C26 124.5(4) . . ? C43 C44 C45 119.0(4) . . ? C46 C45 C44 119.8(4) . . ? C45 C46 C47 118.0(4) . . ? N4 C47 C46 122.5(4) . . ? N5 C48 C49 121.9(4) . . ? N5 C48 C27 112.7(4) . . ? C49 C48 C27 125.4(4) . . ? C50 C49 C48 118.7(4) . . ? C49 C50 C51 118.6(4) . . ? C52 C51 C50 120.2(4) . . ? N5 C52 C51 121.5(4) . . ? N6 C53 C54 121.7(4) . . ? N6 C53 C27 113.5(4) . . ? C54 C53 C27 124.8(4) . . ? C53 C54 C55 119.4(4) . . ? C54 C55 C56 118.8(4) . . ? C57 C56 C55 118.4(4) . . ? N6 C57 C56 123.3(4) . . ? O4 C58 O5 127.6(4) . . ? O4 C58 C59 118.0(4) . . ? O5 C58 C59 114.4(4) . . ? O7 C60 O6 127.1(5) . . ? O7 C60 C61 120.2(5) . . ? O6 C60 C61 112.7(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.760 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.086 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.081 0.371 0.250 2054 482 ' ' 2 0.083 0.625 0.750 2054 482 ' ' _platon_squeeze_details ; ; # Attachment '- eyt46.cif' data_eyt46 _database_code_depnum_ccdc_archive 'CCDC 803594' #TrackingRef '- eyt46.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H48 Fe3 N6 O9' _chemical_formula_sum 'C63 H48 Fe3 N6 O9' _chemical_formula_weight 1200.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6327(4) _cell_length_b 18.9722(8) _cell_length_c 19.6009(8) _cell_angle_alpha 72.453(2) _cell_angle_beta 89.924(2) _cell_angle_gamma 75.857(2) _cell_volume 3644.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9114 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 30.39 _exptl_crystal_description Fragment _exptl_crystal_colour Orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8567 _exptl_absorpt_correction_T_max 0.8618 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 20 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 173889 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 30.60 _reflns_number_total 22216 _reflns_number_gt 16272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22216 _refine_ls_number_parameters 769 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 3.896 _refine_ls_restrained_S_all 3.896 _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 Fe1 Fe 0.30882(4) 0.68002(2) 0.09697(2) 0.02035(10) Uani 1 1 d . A . Fe2 Fe 0.35694(4) 0.54127(3) 0.26280(2) 0.02230(11) Uani 1 1 d . . . Fe3 Fe 0.27040(4) 0.72941(2) 0.24156(2) 0.02067(10) Uani 1 1 d . A . O1 O 0.26013(16) 0.58180(11) 0.16631(10) 0.0199(4) Uani 1 1 d . A . O2 O 0.22915(16) 0.63211(11) 0.29100(10) 0.0188(4) Uani 1 1 d . A . O3 O 0.18051(16) 0.74679(10) 0.14243(9) 0.0173(4) Uani 1 1 d . . . O4 O 0.46269(18) 0.64316(12) 0.04586(11) 0.0326(5) Uani 1 1 d . . . O5 O 0.6418(2) 0.66800(14) -0.00263(14) 0.0483(7) Uani 1 1 d . . . O8 O 0.42257(17) 0.78885(12) 0.20935(11) 0.0275(5) Uani 1 1 d . . . O9 O 0.44609(17) 0.67929(12) 0.18679(11) 0.0294(5) Uani 1 1 d . . . O6A O 0.5226(5) 0.5492(4) 0.3019(4) 0.0247(17) Uani 0.403(9) 1 d P A 3 O7A O 0.6096(9) 0.4295(4) 0.3740(3) 0.040(3) Uani 0.403(9) 1 d P A 3 O6B O 0.5154(4) 0.5055(4) 0.3331(3) 0.0356(16) Uani 0.597(9) 1 d P A 4 O7B O 0.7092(5) 0.4278(3) 0.3722(2) 0.0447(17) Uani 0.597(9) 1 d P A 4 N1 N 0.19593(19) 0.64277(14) 0.02988(12) 0.0207(5) Uani 1 1 d . . . N2 N 0.4515(2) 0.45946(13) 0.20534(12) 0.0211(5) Uani 1 1 d . A . N3 N 0.2608(2) 0.48766(14) 0.35255(12) 0.0220(5) Uani 1 1 d . A . N4 N 0.3579(2) 0.69545(13) 0.35294(13) 0.0232(6) Uani 1 1 d . . . N5 N 0.1278(2) 0.83700(14) 0.22212(13) 0.0247(6) Uani 1 1 d . . . N6 N 0.3132(2) 0.80111(15) 0.03854(13) 0.0274(6) Uani 1 1 d . . . C1 C -0.0310(2) 0.64212(16) 0.13503(15) 0.0198(6) Uani 1 1 d . . . H1 H -0.0307 0.6313 0.0907 0.024 Uiso 1 1 calc R . . C2 C -0.0014(2) 0.58109(15) 0.20003(15) 0.0157(6) Uani 1 1 d . . . C3 C -0.0102(2) 0.59815(16) 0.26394(15) 0.0193(6) Uani 1 1 d . . . H3 H 0.0042 0.5577 0.3080 0.023 Uiso 1 1 calc R . . C4 C -0.0398(2) 0.67386(16) 0.26500(15) 0.0179(6) Uani 1 1 d . . . C5 C -0.0682(2) 0.73199(16) 0.20105(15) 0.0201(6) Uani 1 1 d . . . H5 H -0.0936 0.7835 0.2012 0.024 Uiso 1 1 calc R . . C6 C -0.0601(2) 0.71627(16) 0.13485(15) 0.0180(6) Uani 1 1 d . . . C7 C 0.0498(2) 0.50099(16) 0.20197(14) 0.0187(6) Uani 1 1 d . . . C8 C -0.0185(3) 0.44741(18) 0.23972(15) 0.0270(7) Uani 1 1 d . . . H8 H -0.0963 0.4651 0.2602 0.032 Uiso 1 1 calc R . . C9 C 0.0246(3) 0.37025(17) 0.24756(16) 0.0260(7) Uani 1 1 d . . . H9 H -0.0211 0.3352 0.2746 0.031 Uiso 1 1 calc R . . C10 C 0.1341(3) 0.34498(18) 0.21575(16) 0.0268(7) Uani 1 1 d . . . H10 H 0.1635 0.2922 0.2200 0.032 Uiso 1 1 calc R . . C11 C 0.2023(3) 0.39569(16) 0.17750(15) 0.0226(7) Uani 1 1 d . . . H11 H 0.2767 0.3772 0.1549 0.027 Uiso 1 1 calc R . . C12 C 0.1642(2) 0.47398(16) 0.17129(15) 0.0184(6) Uani 1 1 d . A . C13 C -0.0309(2) 0.69327(15) 0.33193(14) 0.0176(6) Uani 1 1 d . . . C14 C -0.1387(2) 0.74339(16) 0.34864(16) 0.0236(7) Uani 1 1 d . . . H14 H -0.2158 0.7617 0.3174 0.028 Uiso 1 1 calc R . . C15 C -0.1370(3) 0.76683(17) 0.40825(17) 0.0295(8) Uani 1 1 d . . . H15 H -0.2121 0.8008 0.4173 0.035 Uiso 1 1 calc R . . C16 C -0.0288(3) 0.74186(17) 0.45444(16) 0.0286(7) Uani 1 1 d . . . H16 H -0.0271 0.7593 0.4950 0.034 Uiso 1 1 calc R . . C17 C 0.0815(3) 0.68953(17) 0.44149(16) 0.0244(7) Uani 1 1 d . . . H17 H 0.1556 0.6702 0.4751 0.029 Uiso 1 1 calc R . . C18 C 0.0840(2) 0.66580(16) 0.38071(16) 0.0230(7) Uani 1 1 d . A . C19 C -0.0720(2) 0.77772(16) 0.06510(15) 0.0188(6) Uani 1 1 d . A . C20 C -0.1621(2) 0.78048(17) 0.01149(15) 0.0229(7) Uani 1 1 d . . . H20 H -0.2164 0.7461 0.0221 0.027 Uiso 1 1 calc R . . C21 C -0.1734(3) 0.83288(18) -0.05723(16) 0.0280(7) Uani 1 1 d . . . H21 H -0.2343 0.8338 -0.0931 0.034 Uiso 1 1 calc R . . C22 C -0.0949(3) 0.88367(18) -0.07280(16) 0.0315(8) Uani 1 1 d . . . H22 H -0.1039 0.9206 -0.1189 0.038 Uiso 1 1 calc R . . C23 C -0.0040(3) 0.88016(17) -0.02099(16) 0.0248(7) Uani 1 1 d . A . H23 H 0.0513 0.9139 -0.0330 0.030 Uiso 1 1 calc R . . C24 C 0.0099(2) 0.82885(16) 0.04850(15) 0.0193(6) Uani 1 1 d . . . C25 C 0.2532(2) 0.52727(16) 0.13231(15) 0.0173(6) Uani 1 1 d . . . C26 C 0.1991(2) 0.56802(16) 0.05375(15) 0.0168(6) Uani 1 1 d . A . C27 C 0.1505(2) 0.53307(17) 0.01141(15) 0.0210(6) Uani 1 1 d . . . H27 H 0.1560 0.4799 0.0288 0.025 Uiso 1 1 calc R A . C28 C 0.0933(2) 0.57624(17) -0.05697(15) 0.0236(7) Uani 1 1 d . A . H28 H 0.0618 0.5523 -0.0870 0.028 Uiso 1 1 calc R . . C29 C 0.0824(3) 0.65325(18) -0.08094(16) 0.0247(7) Uani 1 1 d . . . H29 H 0.0382 0.6843 -0.1261 0.030 Uiso 1 1 calc R A . C30 C 0.1389(2) 0.68489(17) -0.03630(15) 0.0220(7) Uani 1 1 d . A . H30 H 0.1368 0.7377 -0.0532 0.026 Uiso 1 1 calc R . . C31 C 0.3925(2) 0.47581(16) 0.13988(16) 0.0191(6) Uani 1 1 d . A . C32 C 0.4501(3) 0.44470(17) 0.08828(16) 0.0255(7) Uani 1 1 d . . . H32 H 0.4081 0.4583 0.0417 0.031 Uiso 1 1 calc R A . C33 C 0.5727(3) 0.39248(18) 0.10750(17) 0.0299(8) Uani 1 1 d . A . H33 H 0.6147 0.3696 0.0738 0.036 Uiso 1 1 calc R . . C34 C 0.6311(3) 0.37467(18) 0.17351(17) 0.0322(8) Uani 1 1 d . . . H34 H 0.7135 0.3387 0.1869 0.039 Uiso 1 1 calc R A . C35 C 0.5692(3) 0.40977(18) 0.22201(17) 0.0296(7) Uani 1 1 d . A . H35 H 0.6116 0.3982 0.2682 0.035 Uiso 1 1 calc R . . C36 C 0.2126(2) 0.61489(16) 0.36480(15) 0.0208(6) Uani 1 1 d . . . C37 C 0.2133(2) 0.53008(16) 0.39493(15) 0.0195(6) Uani 1 1 d . A . C38 C 0.1627(2) 0.49831(17) 0.45913(16) 0.0235(7) Uani 1 1 d . . . H38 H 0.1334 0.5284 0.4898 0.028 Uiso 1 1 calc R A . C39 C 0.1550(3) 0.42384(17) 0.47847(17) 0.0262(7) Uani 1 1 d . A . H39 H 0.1198 0.4020 0.5220 0.031 Uiso 1 1 calc R . . C40 C 0.2005(3) 0.38060(18) 0.43235(17) 0.0281(7) Uani 1 1 d . . . H40 H 0.1950 0.3292 0.4432 0.034 Uiso 1 1 calc R A . C41 C 0.2535(3) 0.41533(18) 0.37064(17) 0.0290(7) Uani 1 1 d . A . H41 H 0.2862 0.3862 0.3397 0.035 Uiso 1 1 calc R . . C42 C 0.3270(2) 0.63445(17) 0.39777(16) 0.0230(7) Uani 1 1 d . A . C43 C 0.3922(2) 0.59313(17) 0.46495(16) 0.0239(7) Uani 1 1 d . . . H43 H 0.3699 0.5486 0.4940 0.029 Uiso 1 1 calc R A . C44 C 0.4911(3) 0.61915(18) 0.48826(18) 0.0312(8) Uani 1 1 d . A . H44 H 0.5348 0.5942 0.5347 0.037 Uiso 1 1 calc R . . C45 C 0.5239(3) 0.68164(19) 0.44264(19) 0.0419(9) Uani 1 1 d . . . H45 H 0.5929 0.6994 0.4564 0.050 Uiso 1 1 calc R A . C46 C 0.4549(3) 0.71839(18) 0.37636(18) 0.0356(8) Uani 1 1 d . A . H46 H 0.4775 0.7621 0.3458 0.043 Uiso 1 1 calc R . . C47 C 0.1219(2) 0.82250(16) 0.10346(15) 0.0205(6) Uani 1 1 d . A . C48 C 0.0704(2) 0.86760(16) 0.15522(16) 0.0203(6) Uani 1 1 d . A . C49 C -0.0302(3) 0.93422(17) 0.13646(17) 0.0266(7) Uani 1 1 d . . . H49 H -0.0707 0.9545 0.0890 0.032 Uiso 1 1 calc R A . C50 C -0.0710(3) 0.97054(18) 0.18604(18) 0.0336(8) Uani 1 1 d . A . H50 H -0.1383 1.0166 0.1734 0.040 Uiso 1 1 calc R . . C51 C -0.0117(3) 0.93856(19) 0.25548(19) 0.0398(9) Uani 1 1 d . . . H51 H -0.0382 0.9625 0.2912 0.048 Uiso 1 1 calc R A . C52 C 0.0865(3) 0.87127(18) 0.27199(18) 0.0306(8) Uani 1 1 d . A . H52 H 0.1256 0.8488 0.3197 0.037 Uiso 1 1 calc R . . C53 C 0.2286(3) 0.85543(18) 0.06018(16) 0.0256(7) Uani 1 1 d . A . C54 C 0.2410(3) 0.92869(17) 0.04561(16) 0.0287(7) Uani 1 1 d . . . H54 H 0.1820 0.9650 0.0625 0.034 Uiso 1 1 calc R A . C55 C 0.3423(3) 0.9484(2) 0.00541(18) 0.0415(9) Uani 1 1 d . A . H55 H 0.3547 0.9983 -0.0048 0.050 Uiso 1 1 calc R . . C56 C 0.4241(3) 0.8951(2) -0.01938(19) 0.0465(10) Uani 1 1 d . . . H56 H 0.4913 0.9084 -0.0486 0.056 Uiso 1 1 calc R A . C57 C 0.4083(3) 0.8235(2) -0.00194(17) 0.0347(8) Uani 1 1 d . A . H57 H 0.4667 0.7870 -0.0189 0.042 Uiso 1 1 calc R . . C58 C 0.5875(3) 0.6333(2) 0.04673(19) 0.0350(9) Uani 1 1 d . A . C59 C 0.6648(3) 0.5723(2) 0.11210(19) 0.0407(9) Uani 1 1 d . . . H59A H 0.6692 0.5216 0.1079 0.061 Uiso 1 1 calc R A . H59B H 0.6223 0.5772 0.1554 0.061 Uiso 1 1 calc R . . H59C H 0.7531 0.5788 0.1152 0.061 Uiso 1 1 calc R . . C62 C 0.4873(3) 0.7365(2) 0.18627(16) 0.0284(7) Uani 1 1 d . A . C63 C 0.6182(3) 0.7419(2) 0.15872(18) 0.0388(9) Uani 1 1 d . . . H63A H 0.6871 0.7072 0.1950 0.058 Uiso 1 1 calc R A . H63B H 0.6257 0.7945 0.1487 0.058 Uiso 1 1 calc R . . H63C H 0.6267 0.7276 0.1146 0.058 Uiso 1 1 calc R . . C60A C 0.618(3) 0.4962(14) 0.3441(16) 0.010(3) Uani 0.403(9) 1 d P A 3 C61A C 0.7281(11) 0.5245(9) 0.3624(7) 0.038(3) Uani 0.403(9) 1 d P A 3 H61A H 0.7311 0.5716 0.3247 0.058 Uiso 0.403(9) 1 calc PR A 3 H61B H 0.8099 0.4856 0.3664 0.058 Uiso 0.403(9) 1 calc PR A 3 H61C H 0.7158 0.5351 0.4083 0.058 Uiso 0.403(9) 1 calc PR A 3 C60B C 0.635(3) 0.4905(13) 0.3514(13) 0.041(6) Uani 0.597(9) 1 d P A 4 C61B C 0.6888(9) 0.5603(6) 0.3380(5) 0.051(2) Uani 0.597(9) 1 d P A 4 H61D H 0.6686 0.5917 0.2876 0.076 Uiso 0.597(9) 1 calc PR A 4 H61E H 0.7834 0.5439 0.3489 0.076 Uiso 0.597(9) 1 calc PR A 4 H61F H 0.6491 0.5903 0.3690 0.076 Uiso 0.597(9) 1 calc PR A 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0135(2) 0.0290(3) 0.0248(3) -0.0135(2) 0.00592(17) -0.01027(18) Fe2 0.01138(19) 0.0327(3) 0.0242(3) -0.0146(2) -0.00103(17) -0.00092(18) Fe3 0.01262(19) 0.0255(3) 0.0256(3) -0.0100(2) 0.00020(17) -0.00526(17) O1 0.0114(9) 0.0280(12) 0.0249(12) -0.0135(9) 0.0022(8) -0.0069(8) O2 0.0115(9) 0.0271(11) 0.0203(11) -0.0108(9) 0.0028(8) -0.0054(8) O3 0.0126(9) 0.0190(11) 0.0201(11) -0.0050(9) 0.0005(8) -0.0049(8) O4 0.0213(11) 0.0474(15) 0.0420(14) -0.0285(12) 0.0164(10) -0.0143(10) O5 0.0364(13) 0.0637(18) 0.0682(18) -0.0373(15) 0.0322(13) -0.0345(13) O8 0.0224(11) 0.0354(13) 0.0320(13) -0.0178(11) 0.0052(9) -0.0114(10) O9 0.0114(9) 0.0437(14) 0.0435(14) -0.0271(12) 0.0014(9) -0.0091(9) O6A 0.020(3) 0.026(4) 0.030(4) -0.008(3) -0.006(3) -0.009(3) O7A 0.057(6) 0.027(4) 0.031(4) 0.002(3) -0.006(3) -0.014(4) O6B 0.020(2) 0.061(5) 0.031(3) -0.025(3) -0.0027(19) -0.004(2) O7B 0.036(3) 0.039(3) 0.042(3) -0.005(2) -0.007(2) 0.013(2) N1 0.0115(11) 0.0331(15) 0.0221(14) -0.0128(12) 0.0031(10) -0.0090(10) N2 0.0150(11) 0.0301(15) 0.0214(14) -0.0128(11) 0.0030(10) -0.0058(10) N3 0.0164(11) 0.0267(14) 0.0208(14) -0.0107(11) -0.0083(10) 0.0024(10) N4 0.0184(12) 0.0229(14) 0.0287(15) -0.0080(12) -0.0058(11) -0.0057(11) N5 0.0199(12) 0.0301(15) 0.0308(16) -0.0148(13) 0.0056(11) -0.0120(11) N6 0.0214(13) 0.0382(17) 0.0266(15) -0.0093(13) 0.0055(11) -0.0159(12) C1 0.0084(12) 0.0294(18) 0.0253(17) -0.0118(14) -0.0002(11) -0.0072(12) C2 0.0065(11) 0.0221(16) 0.0209(16) -0.0070(13) 0.0024(11) -0.0079(11) C3 0.0065(12) 0.0282(17) 0.0213(16) -0.0035(13) 0.0008(11) -0.0066(11) C4 0.0080(12) 0.0275(17) 0.0190(16) -0.0072(13) 0.0042(11) -0.0061(11) C5 0.0078(12) 0.0232(16) 0.0289(18) -0.0080(14) 0.0024(11) -0.0036(11) C6 0.0047(11) 0.0265(17) 0.0243(17) -0.0069(13) -0.0007(11) -0.0078(11) C7 0.0156(13) 0.0266(17) 0.0157(15) -0.0061(13) -0.0012(11) -0.0096(12) C8 0.0193(15) 0.040(2) 0.0243(18) -0.0091(15) 0.0016(13) -0.0123(14) C9 0.0282(16) 0.0214(17) 0.0271(18) -0.0021(14) -0.0012(13) -0.0106(13) C10 0.0245(16) 0.0261(18) 0.0293(18) -0.0064(14) 0.0001(13) -0.0083(14) C11 0.0170(14) 0.0222(17) 0.0275(18) -0.0073(14) -0.0043(12) -0.0036(12) C12 0.0134(13) 0.0237(16) 0.0193(16) -0.0072(13) -0.0022(11) -0.0062(12) C13 0.0151(13) 0.0216(16) 0.0183(16) -0.0065(13) 0.0019(11) -0.0082(12) C14 0.0138(13) 0.0254(17) 0.0296(18) -0.0078(14) 0.0005(12) -0.0023(12) C15 0.0236(16) 0.0280(18) 0.035(2) -0.0127(15) 0.0136(14) 0.0009(13) C16 0.0300(17) 0.0332(19) 0.0244(18) -0.0130(15) 0.0064(14) -0.0061(14) C17 0.0219(15) 0.0314(18) 0.0248(18) -0.0156(15) 0.0012(13) -0.0069(13) C18 0.0151(13) 0.0242(17) 0.0288(18) -0.0079(14) 0.0069(12) -0.0040(12) C19 0.0117(12) 0.0257(17) 0.0184(16) -0.0063(13) 0.0033(11) -0.0046(12) C20 0.0160(14) 0.0286(17) 0.0246(17) -0.0074(14) 0.0028(12) -0.0078(12) C21 0.0218(15) 0.036(2) 0.0258(18) -0.0084(15) -0.0051(13) -0.0088(14) C22 0.0296(17) 0.038(2) 0.0214(18) 0.0008(15) 0.0033(14) -0.0103(15) C23 0.0215(15) 0.0294(18) 0.0276(18) -0.0096(15) 0.0027(13) -0.0131(13) C24 0.0134(13) 0.0223(16) 0.0223(17) -0.0090(13) -0.0006(11) -0.0021(12) C25 0.0161(13) 0.0203(16) 0.0202(16) -0.0116(13) 0.0020(11) -0.0067(11) C26 0.0108(12) 0.0193(16) 0.0234(16) -0.0093(13) 0.0036(11) -0.0060(11) C27 0.0156(13) 0.0280(17) 0.0215(17) -0.0094(14) 0.0022(12) -0.0071(12) C28 0.0185(14) 0.038(2) 0.0216(17) -0.0162(15) 0.0032(12) -0.0109(13) C29 0.0181(14) 0.036(2) 0.0208(17) -0.0097(14) 0.0010(12) -0.0078(13) C30 0.0181(14) 0.0233(17) 0.0232(17) -0.0055(14) 0.0040(12) -0.0050(12) C31 0.0123(13) 0.0242(16) 0.0277(17) -0.0171(14) 0.0037(12) -0.0061(12) C32 0.0198(15) 0.0316(18) 0.0268(18) -0.0121(15) 0.0005(13) -0.0057(13) C33 0.0166(14) 0.038(2) 0.036(2) -0.0158(16) 0.0061(14) -0.0021(13) C34 0.0209(15) 0.038(2) 0.034(2) -0.0168(16) 0.0024(14) 0.0052(14) C35 0.0212(15) 0.039(2) 0.0253(18) -0.0124(15) -0.0022(13) 0.0012(14) C36 0.0162(13) 0.0290(17) 0.0206(17) -0.0135(14) -0.0022(12) -0.0044(12) C37 0.0112(13) 0.0239(16) 0.0216(16) -0.0067(13) -0.0049(11) -0.0017(12) C38 0.0138(13) 0.0281(18) 0.0310(18) -0.0160(15) 0.0014(12) -0.0014(12) C39 0.0166(14) 0.0290(18) 0.0301(19) -0.0064(15) -0.0024(13) -0.0044(13) C40 0.0249(16) 0.0252(18) 0.035(2) -0.0108(15) -0.0072(14) -0.0051(13) C41 0.0287(16) 0.0276(19) 0.0302(19) -0.0144(15) -0.0095(14) 0.0006(14) C42 0.0157(14) 0.0287(18) 0.0318(19) -0.0184(15) 0.0025(13) -0.0074(13) C43 0.0176(14) 0.0200(16) 0.0337(19) -0.0104(14) -0.0034(13) -0.0012(12) C44 0.0285(17) 0.0257(18) 0.036(2) -0.0090(16) -0.0137(15) -0.0003(14) C45 0.0310(18) 0.034(2) 0.059(3) -0.0084(19) -0.0219(17) -0.0119(16) C46 0.0361(19) 0.0228(18) 0.046(2) -0.0046(16) -0.0097(16) -0.0123(15) C47 0.0167(14) 0.0228(17) 0.0245(17) -0.0081(13) -0.0002(12) -0.0087(12) C48 0.0158(13) 0.0223(16) 0.0253(17) -0.0074(13) 0.0042(12) -0.0094(12) C49 0.0244(15) 0.0242(17) 0.0292(19) -0.0043(14) 0.0009(13) -0.0075(13) C50 0.0342(18) 0.0218(18) 0.041(2) -0.0095(16) 0.0035(16) -0.0002(14) C51 0.045(2) 0.039(2) 0.042(2) -0.0261(18) 0.0083(17) -0.0062(17) C52 0.0270(16) 0.037(2) 0.034(2) -0.0201(16) -0.0005(14) -0.0074(15) C53 0.0164(14) 0.0320(19) 0.0276(18) -0.0038(15) 0.0005(13) -0.0117(13) C54 0.0233(15) 0.0250(18) 0.037(2) -0.0032(15) 0.0024(14) -0.0126(14) C55 0.0357(19) 0.031(2) 0.052(2) 0.0042(18) -0.0018(17) -0.0200(17) C56 0.0327(19) 0.053(3) 0.049(2) -0.002(2) 0.0192(17) -0.0207(18) C57 0.0243(16) 0.048(2) 0.033(2) -0.0082(17) 0.0126(14) -0.0174(16) C58 0.0245(16) 0.049(2) 0.054(2) -0.041(2) 0.0160(16) -0.0193(16) C59 0.0233(16) 0.048(2) 0.061(3) -0.031(2) 0.0047(17) -0.0098(16) C62 0.0153(14) 0.046(2) 0.0265(18) -0.0146(16) 0.0022(13) -0.0077(14) C63 0.0191(16) 0.058(2) 0.051(2) -0.030(2) 0.0060(15) -0.0160(16) C60A 0.020(8) 0.010(6) 0.002(6) 0.000(4) -0.004(5) -0.010(6) C61A 0.017(5) 0.080(11) 0.024(6) -0.026(7) 0.004(4) -0.010(5) C60B 0.033(8) 0.064(10) 0.022(9) -0.018(7) 0.005(7) -0.002(6) C61B 0.039(6) 0.074(8) 0.054(6) -0.024(5) 0.005(4) -0.035(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Fe2 3.4560(6) . yes Fe1 Fe3 3.2385(6) . yes Fe2 Fe3 3.3557(6) . yes Fe1 O4 2.0071(19) . yes Fe1 O3 2.0230(18) . yes Fe1 O1 2.1283(19) . yes Fe1 N1 2.156(2) . yes Fe1 N6 2.249(2) . yes Fe1 O9 2.2830(19) . yes Fe2 O6A 1.979(6) . yes Fe2 O1 1.9923(18) . yes Fe2 O6B 2.021(4) . yes Fe2 O2 2.1330(18) . yes Fe2 N3 2.144(2) . yes Fe2 N2 2.231(2) . yes Fe3 O2 1.9634(19) . yes Fe3 O3 2.0645(18) . yes Fe3 N5 2.152(2) . yes Fe3 O8 2.1789(18) . yes Fe3 N4 2.216(2) . yes Fe3 O9 2.2997(19) . yes O1 C25 1.405(3) . ? O2 C36 1.405(3) . ? O3 C47 1.392(3) . ? O4 C58 1.293(3) . ? O5 C58 1.227(4) . ? O8 C62 1.265(3) . ? O9 C62 1.264(3) . ? O6A C60A 1.31(3) . ? O7A C60A 1.25(2) . ? O6B C60B 1.26(3) . ? O7B C60B 1.20(3) . ? N1 C26 1.344(3) . ? N1 C30 1.353(3) . ? N2 C35 1.342(3) . ? N2 C31 1.343(3) . ? N3 C41 1.332(4) . ? N3 C37 1.340(3) . ? N4 C42 1.338(4) . ? N4 C46 1.344(3) . ? N5 C48 1.341(3) . ? N5 C52 1.347(4) . ? N6 C57 1.356(3) . ? N6 C53 1.364(4) . ? C1 C6 1.364(4) . ? C1 C2 1.413(4) . ? C2 C3 1.383(4) . ? C2 C7 1.472(4) . ? C3 C4 1.400(4) . ? C4 C5 1.372(4) . ? C4 C13 1.475(4) . ? C5 C6 1.414(4) . ? C6 C19 1.487(4) . ? C7 C12 1.409(4) . ? C7 C8 1.419(4) . ? C8 C9 1.383(4) . ? C9 C10 1.371(4) . ? C10 C11 1.385(4) . ? C11 C12 1.408(4) . ? C12 C25 1.581(4) . ? C13 C14 1.407(4) . ? C13 C18 1.439(4) . ? C14 C15 1.371(4) . ? C15 C16 1.359(4) . ? C16 C17 1.417(4) . ? C17 C18 1.393(4) . ? C18 C36 1.560(4) . ? C19 C20 1.404(4) . ? C19 C24 1.424(4) . ? C20 C21 1.397(4) . ? C21 C22 1.390(4) . ? C22 C23 1.379(4) . ? C23 C24 1.398(4) . ? C24 C47 1.565(4) . ? C25 C26 1.538(4) . ? C25 C31 1.542(3) . ? C26 C27 1.377(4) . ? C27 C28 1.391(4) . ? C28 C29 1.368(4) . ? C29 C30 1.407(4) . ? C31 C32 1.389(4) . ? C32 C33 1.403(4) . ? C33 C34 1.345(4) . ? C34 C35 1.395(4) . ? C36 C37 1.536(4) . ? C36 C42 1.550(4) . ? C37 C38 1.391(4) . ? C38 C39 1.371(4) . ? C39 C40 1.406(4) . ? C40 C41 1.383(4) . ? C42 C43 1.394(4) . ? C43 C44 1.396(4) . ? C44 C45 1.374(4) . ? C45 C46 1.385(4) . ? C47 C48 1.534(4) . ? C47 C53 1.556(4) . ? C48 C49 1.392(4) . ? C49 C50 1.365(4) . ? C50 C51 1.391(4) . ? C51 C52 1.388(4) . ? C53 C54 1.371(4) . ? C54 C55 1.392(4) . ? C55 C56 1.371(5) . ? C56 C57 1.350(4) . ? C58 C59 1.516(5) . ? C62 C63 1.507(4) . ? C60A C61A 1.49(3) . ? C60B C61B 1.52(2) . ? 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 Fe3 Fe1 Fe2 60.062(13) . . yes Fe3 Fe2 Fe1 56.753(12) . . yes Fe1 Fe3 Fe2 63.185(13) . . yes O4 Fe1 O3 160.94(8) . . yes O4 Fe1 O1 107.46(8) . . yes O3 Fe1 O1 89.56(7) . . yes O4 Fe1 N1 86.56(8) . . yes O3 Fe1 N1 106.75(8) . . yes O1 Fe1 N1 74.39(8) . . yes O4 Fe1 N6 89.08(9) . . yes O3 Fe1 N6 73.96(8) . . yes O1 Fe1 N6 163.43(8) . . yes N1 Fe1 N6 108.27(9) . . yes O4 Fe1 O9 89.82(8) . . yes O3 Fe1 O9 81.49(7) . . yes O1 Fe1 O9 89.92(7) . . yes N1 Fe1 O9 161.96(9) . . yes N6 Fe1 O9 89.32(8) . . yes O4 Fe1 Fe3 134.95(6) . . yes O3 Fe1 Fe3 38.05(5) . . yes O1 Fe1 Fe3 80.19(5) . . yes N1 Fe1 Fe3 136.71(6) . . yes N6 Fe1 Fe3 87.57(6) . . yes O9 Fe1 Fe3 45.24(5) . . yes O4 Fe1 Fe2 103.35(7) . . yes O3 Fe1 Fe2 86.48(5) . . yes O1 Fe1 Fe2 31.79(5) . . yes N1 Fe1 Fe2 105.57(7) . . yes N6 Fe1 Fe2 144.53(6) . . yes O9 Fe1 Fe2 58.16(6) . . yes O6A Fe2 O1 134.6(3) . . yes O6A Fe2 O6B 25.68(16) . . yes O1 Fe2 O6B 155.91(16) . . yes O6A Fe2 O2 98.11(18) . . yes O1 Fe2 O2 88.14(7) . . yes O6B Fe2 O2 105.61(14) . . yes O6A Fe2 N3 106.9(2) . . yes O1 Fe2 N3 118.00(8) . . yes O6B Fe2 N3 85.21(18) . . yes O2 Fe2 N3 74.06(8) . . yes O6A Fe2 N2 94.78(18) . . yes O1 Fe2 N2 75.62(8) . . yes O6B Fe2 N2 90.33(14) . . yes O2 Fe2 N2 163.64(8) . . yes N3 Fe2 N2 111.68(9) . . yes O6A Fe2 Fe3 82.2(2) . . yes O1 Fe2 Fe3 78.96(5) . . yes O6B Fe2 Fe3 101.54(18) . . yes O2 Fe2 Fe3 33.37(5) . . yes N3 Fe2 Fe3 106.68(7) . . yes N2 Fe2 Fe3 140.62(6) . . yes O6A Fe2 Fe1 102.1(3) . . yes O1 Fe2 Fe1 34.25(5) . . yes O6B Fe2 Fe1 127.1(2) . . yes O2 Fe2 Fe1 81.41(5) . . yes N3 Fe2 Fe1 144.15(6) . . yes N2 Fe2 Fe1 86.09(6) . . yes O2 Fe3 O3 97.07(7) . . yes O2 Fe3 N5 121.39(8) . . yes O3 Fe3 N5 76.54(8) . . yes O2 Fe3 O8 146.57(7) . . yes O3 Fe3 O8 100.34(7) . . yes N5 Fe3 O8 90.48(8) . . yes O2 Fe3 N4 74.77(8) . . yes O3 Fe3 N4 171.83(8) . . yes N5 Fe3 N4 107.59(9) . . yes O8 Fe3 N4 86.80(8) . . yes O2 Fe3 O9 96.64(8) . . yes O3 Fe3 O9 80.22(7) . . yes N5 Fe3 O9 137.19(9) . . yes O8 Fe3 O9 59.03(7) . . yes N4 Fe3 O9 100.38(8) . . yes O2 Fe3 Fe1 89.76(5) . . yes O3 Fe3 Fe1 37.15(5) . . yes N5 Fe3 Fe1 111.31(7) . . yes O8 Fe3 Fe1 87.21(5) . . yes N4 Fe3 Fe1 140.65(6) . . yes O9 Fe3 Fe1 44.83(5) . . yes O2 Fe3 Fe2 36.69(5) . . yes O3 Fe3 Fe2 88.58(5) . . yes N5 Fe3 Fe2 152.30(6) . . yes O8 Fe3 Fe2 115.40(6) . . yes N4 Fe3 Fe2 84.74(6) . . yes O9 Fe3 Fe2 60.00(6) . . yes C25 O1 Fe2 115.93(16) . . ? C25 O1 Fe1 113.16(16) . . ? Fe2 O1 Fe1 113.97(8) . . ? C36 O2 Fe3 118.01(16) . . ? C36 O2 Fe2 113.72(16) . . ? Fe3 O2 Fe2 109.94(8) . . ? C47 O3 Fe1 120.10(16) . . ? C47 O3 Fe3 115.85(16) . . ? Fe1 O3 Fe3 104.80(8) . . ? C58 O4 Fe1 141.6(2) . . ? C62 O8 Fe3 92.32(18) . . ? C62 O9 Fe1 123.0(2) . . ? C62 O9 Fe3 86.88(16) . . ? Fe1 O9 Fe3 89.93(6) . . ? C60A O6A Fe2 130.4(10) . . ? C60B O6B Fe2 155.2(12) . . ? C26 N1 C30 118.8(2) . . ? C26 N1 Fe1 114.83(18) . . ? C30 N1 Fe1 125.7(2) . . ? C35 N2 C31 118.7(2) . . ? C35 N2 Fe2 127.3(2) . . ? C31 N2 Fe2 112.40(17) . . ? C41 N3 C37 119.3(3) . . ? C41 N3 Fe2 124.7(2) . . ? C37 N3 Fe2 115.86(19) . . ? C42 N4 C46 116.8(3) . . ? C42 N4 Fe3 114.18(18) . . ? C46 N4 Fe3 127.6(2) . . ? C48 N5 C52 119.2(3) . . ? C48 N5 Fe3 115.00(19) . . ? C52 N5 Fe3 125.6(2) . . ? C57 N6 C53 117.0(3) . . ? C57 N6 Fe1 126.3(2) . . ? C53 N6 Fe1 114.80(18) . . ? C6 C1 C2 121.0(3) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 C7 119.0(2) . . ? C1 C2 C7 122.3(3) . . ? C2 C3 C4 121.3(3) . . ? C5 C4 C3 118.9(3) . . ? C5 C4 C13 118.7(3) . . ? C3 C4 C13 122.2(2) . . ? C4 C5 C6 120.9(3) . . ? C1 C6 C5 119.1(3) . . ? C1 C6 C19 118.6(3) . . ? C5 C6 C19 122.0(3) . . ? C12 C7 C8 118.3(3) . . ? C12 C7 C2 124.2(2) . . ? C8 C7 C2 117.4(2) . . ? C9 C8 C7 122.0(3) . . ? C10 C9 C8 119.1(3) . . ? C9 C10 C11 120.5(3) . . ? C10 C11 C12 121.7(3) . . ? C11 C12 C7 118.3(2) . . ? C11 C12 C25 118.9(2) . . ? C7 C12 C25 122.8(2) . . ? C14 C13 C18 117.4(2) . . ? C14 C13 C4 118.8(2) . . ? C18 C13 C4 123.7(2) . . ? C15 C14 C13 122.7(3) . . ? C16 C15 C14 120.6(3) . . ? C15 C16 C17 119.3(3) . . ? C18 C17 C16 121.6(3) . . ? C17 C18 C13 118.4(2) . . ? C17 C18 C36 119.6(2) . . ? C13 C18 C36 121.9(2) . . ? C20 C19 C24 119.1(3) . . ? C20 C19 C6 117.2(2) . . ? C24 C19 C6 123.5(2) . . ? C21 C20 C19 121.1(3) . . ? C22 C21 C20 119.6(3) . . ? C23 C22 C21 119.7(3) . . ? C22 C23 C24 122.5(3) . . ? C23 C24 C19 118.0(3) . . ? C23 C24 C47 120.5(2) . . ? C19 C24 C47 121.2(2) . . ? O1 C25 C26 109.6(2) . . ? O1 C25 C31 105.9(2) . . ? C26 C25 C31 113.2(2) . . ? O1 C25 C12 111.9(2) . . ? C26 C25 C12 109.3(2) . . ? C31 C25 C12 106.9(2) . . ? N1 C26 C27 121.5(3) . . ? N1 C26 C25 114.7(2) . . ? C27 C26 C25 123.7(3) . . ? C26 C27 C28 119.5(3) . . ? C29 C28 C27 120.0(3) . . ? C28 C29 C30 117.6(3) . . ? N1 C30 C29 122.3(3) . . ? N2 C31 C32 122.5(3) . . ? N2 C31 C25 111.9(2) . . ? C32 C31 C25 125.5(3) . . ? C31 C32 C33 117.5(3) . . ? C34 C33 C32 120.3(3) . . ? C33 C34 C35 119.1(3) . . ? N2 C35 C34 121.9(3) . . ? O2 C36 C37 108.6(2) . . ? O2 C36 C42 105.6(2) . . ? C37 C36 C42 113.0(2) . . ? O2 C36 C18 112.3(2) . . ? C37 C36 C18 110.1(2) . . ? C42 C36 C18 107.2(2) . . ? N3 C37 C38 120.8(3) . . ? N3 C37 C36 115.0(2) . . ? C38 C37 C36 124.2(3) . . ? C39 C38 C37 120.4(3) . . ? C38 C39 C40 118.4(3) . . ? C41 C40 C39 117.9(3) . . ? N3 C41 C40 123.1(3) . . ? N4 C42 C43 123.8(2) . . ? N4 C42 C36 111.5(2) . . ? C43 C42 C36 124.7(3) . . ? C42 C43 C44 118.1(3) . . ? C45 C44 C43 118.6(3) . . ? C44 C45 C46 119.2(3) . . ? N4 C46 C45 123.5(3) . . ? O3 C47 C48 109.6(2) . . ? O3 C47 C53 106.9(2) . . ? C48 C47 C53 110.1(2) . . ? O3 C47 C24 111.8(2) . . ? C48 C47 C24 110.6(2) . . ? C53 C47 C24 107.8(2) . . ? N5 C48 C49 121.2(3) . . ? N5 C48 C47 114.9(2) . . ? C49 C48 C47 123.9(3) . . ? C50 C49 C48 120.2(3) . . ? C49 C50 C51 118.5(3) . . ? C52 C51 C50 119.2(3) . . ? N5 C52 C51 121.7(3) . . ? N6 C53 C54 122.7(3) . . ? N6 C53 C47 111.3(2) . . ? C54 C53 C47 126.0(3) . . ? C53 C54 C55 118.1(3) . . ? C56 C55 C54 119.5(3) . . ? C57 C56 C55 119.4(3) . . ? C56 C57 N6 123.2(3) . . ? O5 C58 O4 123.3(3) . . ? O5 C58 C59 121.2(3) . . ? O4 C58 C59 115.4(3) . . ? O9 C62 O8 121.7(3) . . ? O9 C62 C63 119.2(3) . . ? O8 C62 C63 119.1(3) . . ? O7A C60A O6A 122(2) . . ? O7A C60A C61A 122(3) . . ? O6A C60A C61A 114.8(15) . . ? O7B C60B O6B 126(2) . . ? O7B C60B C61B 119(2) . . ? O6B C60B C61B 114.4(18) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.60 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.310 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.093 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.019 0.000 0.500 1229 685 ' ' _platon_squeeze_details ; ; # Attachment '- jsk03.cif' data_jsk03 _database_code_depnum_ccdc_archive 'CCDC 803595' #TrackingRef '- jsk03.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C63 H48 N6 Ni3 O9' _chemical_formula_sum 'C63 H48 N6 Ni3 O9' _chemical_formula_weight 1209.20 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 20.7019(9) _cell_length_b 20.7019(9) _cell_length_c 10.6229(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3942.7(3) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9969 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.90 _exptl_crystal_description Fragment _exptl_crystal_colour 'Pale green' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8137 _exptl_absorpt_correction_T_max 0.8668 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 9 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27943 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 30.16 _reflns_number_total 5180 _reflns_number_gt 4654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _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 matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ad _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(11) _refine_ls_number_reflns 5180 _refine_ls_number_parameters 262 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 2.887 _refine_ls_restrained_S_all 2.887 _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 Ni1 Ni 0.72122(2) 0.43572(2) 0.06433(3) 0.02707(10) Uani 1 1 d . . . O1 O 0.62221(11) 0.37971(11) 0.1598(2) 0.0222(5) Uani 1 1 d . A . N1 N 0.83175(15) 0.47855(15) -0.0042(3) 0.0334(7) Uani 1 1 d . A . N2 N 0.72146(14) 0.51977(14) 0.1645(2) 0.0291(6) Uani 1 1 d . A . C1 C 0.72433(16) 0.31836(17) 0.4128(2) 0.0259(7) Uani 1 1 d . . . H1 H 0.7640 0.3078 0.4146 0.031 Uiso 1 1 calc R . . C2 C 0.74034(17) 0.39129(17) 0.4115(3) 0.0250(7) Uani 1 1 d . . . C3 C 0.81844(17) 0.45569(17) 0.3974(3) 0.0251(7) Uani 1 1 d . . . C4 C 0.84665(18) 0.50738(17) 0.4933(3) 0.0307(8) Uani 1 1 d . . . H4 H 0.8171 0.5000 0.5661 0.037 Uiso 1 1 calc R . . C5 C 0.91750(17) 0.57027(17) 0.4860(3) 0.0338(8) Uani 1 1 d . . . H5 H 0.9361 0.6050 0.5535 0.041 Uiso 1 1 calc R . . C6 C 0.96108(18) 0.58181(18) 0.3780(3) 0.0298(8) Uani 1 1 d . . . H6 H 1.0091 0.6248 0.3706 0.036 Uiso 1 1 calc R . . C7 C 0.93308(17) 0.52996(17) 0.2833(3) 0.0293(8) Uani 1 1 d . . . H7 H 0.9632 0.5377 0.2112 0.035 Uiso 1 1 calc R . . C8 C 0.86205(16) 0.46598(16) 0.2877(3) 0.0264(7) Uani 1 1 d . . . C9 C 0.83307(17) 0.41062(16) 0.1774(3) 0.0259(7) Uani 1 1 d . . . C10 C 0.8709(2) 0.45240(17) 0.0551(3) 0.0339(9) Uani 1 1 d . . . C11 C 0.93827(18) 0.46283(19) 0.0050(3) 0.0401(9) Uani 1 1 d . A . H11 H 0.9657 0.4443 0.0485 0.048 Uiso 1 1 calc R . . C12 C 0.96432(19) 0.5000(2) -0.1072(3) 0.0526(11) Uani 1 1 d . . . H12 H 1.0096 0.5068 -0.1420 0.063 Uiso 1 1 calc R A . C13 C 0.9245(2) 0.5272(2) -0.1688(3) 0.0568(13) Uani 1 1 d . A . H13 H 0.9419 0.5528 -0.2466 0.068 Uiso 1 1 calc R . . C14 C 0.8592(2) 0.5169(2) -0.1163(3) 0.0495(11) Uani 1 1 d . . . H14 H 0.8322 0.5366 -0.1581 0.059 Uiso 1 1 calc R A . C15 C 0.65260(18) 0.50482(16) 0.2024(3) 0.0287(7) Uani 1 1 d . . . C16 C 0.64046(19) 0.55860(17) 0.2571(3) 0.0380(9) Uani 1 1 d . A . H16 H 0.5918 0.5479 0.2806 0.046 Uiso 1 1 calc R . . C17 C 0.7028(2) 0.62951(19) 0.2764(4) 0.0479(10) Uani 1 1 d . . . H17 H 0.6965 0.6672 0.3157 0.057 Uiso 1 1 calc R A . C18 C 0.77261(19) 0.64541(19) 0.2396(3) 0.0425(9) Uani 1 1 d . A . H18 H 0.8149 0.6934 0.2522 0.051 Uiso 1 1 calc R . . C19 C 0.77897(19) 0.58750(18) 0.1824(3) 0.0342(8) Uani 1 1 d . . . H19 H 0.8269 0.5975 0.1553 0.041 Uiso 1 1 calc R A . O2A O 0.6859(3) 0.4648(3) -0.0966(4) 0.0270(9) Uani 0.7406(18) 1 d P A 1 O3A O 0.7563(2) 0.5889(2) -0.1154(4) 0.0724(13) Uani 0.7406(18) 1 d P A 1 C20A C 0.7072(3) 0.5260(3) -0.1553(6) 0.0533(16) Uani 0.7406(18) 1 d P A 1 C21A C 0.6790(3) 0.5265(3) -0.2908(5) 0.0646(19) Uani 0.7406(18) 1 d P A 1 H21A H 0.7213 0.5596 -0.3443 0.097 Uiso 0.7406(18) 1 calc PR A 1 H21B H 0.6432 0.5443 -0.2882 0.097 Uiso 0.7406(18) 1 calc PR A 1 H21C H 0.6547 0.4758 -0.3253 0.097 Uiso 0.7406(18) 1 calc PR A 1 O2B O 0.7666(10) 0.3181(10) -0.1321(15) 0.054(6) Uiso 0.2594(18) 1 d P . -2 O3B O 0.6790(6) 0.3330(10) -0.0520(4) 0.0017(19) Uiso 0.2594(18) 1 d P . -2 C20B C 0.7163(6) 0.3318(6) -0.1391(10) 0.017(2) Uiso 0.2594(18) 1 d P . -2 C21B C 0.7019(6) 0.3471(8) -0.2598(10) 0.030(3) Uiso 0.2594(18) 1 d P A -2 H21D H 0.7080 0.3972 -0.2619 0.045 Uiso 0.2594(18) 1 calc PR A -2 H21E H 0.6507 0.3104 -0.2837 0.045 Uiso 0.2594(18) 1 calc PR A -2 H21F H 0.7369 0.3447 -0.3191 0.045 Uiso 0.2594(18) 1 calc PR A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0281(2) 0.0244(2) 0.0292(2) 0.0026(2) -0.0019(2) 0.0134(2) O1 0.0229(12) 0.0213(12) 0.0230(13) 0.0007(10) 0.0007(10) 0.0116(10) N1 0.0367(17) 0.0293(16) 0.0260(16) 0.0027(13) -0.0046(14) 0.0103(14) N2 0.0299(15) 0.0263(15) 0.0269(16) -0.0025(12) -0.0009(13) 0.0109(13) C1 0.0275(18) 0.0344(18) 0.0201(17) -0.0008(14) -0.0013(13) 0.0186(16) C2 0.0322(18) 0.0256(17) 0.0122(15) 0.0028(13) 0.0021(13) 0.0106(15) C3 0.0287(18) 0.0244(17) 0.0255(18) -0.0004(14) -0.0064(14) 0.0157(14) C4 0.038(2) 0.0333(19) 0.0232(18) -0.0038(15) -0.0064(15) 0.0198(17) C5 0.0322(19) 0.0275(18) 0.040(2) -0.0049(16) -0.0132(16) 0.0135(16) C6 0.0300(18) 0.0257(18) 0.035(2) -0.0009(16) -0.0115(16) 0.0150(16) C7 0.0282(19) 0.0317(19) 0.0281(18) 0.0117(15) 0.0003(15) 0.0150(16) C8 0.0258(18) 0.0252(17) 0.0315(19) 0.0042(15) -0.0019(15) 0.0153(15) C9 0.0316(19) 0.0274(17) 0.0221(18) 0.0042(13) 0.0050(14) 0.0173(15) C10 0.031(2) 0.0298(19) 0.033(2) -0.0048(16) -0.0002(15) 0.0088(17) C11 0.0280(19) 0.043(2) 0.037(2) -0.0029(18) 0.0079(17) 0.0089(17) C12 0.027(2) 0.066(3) 0.038(2) -0.001(2) 0.0068(18) 0.002(2) C13 0.034(2) 0.075(3) 0.024(2) 0.018(2) 0.0031(17) -0.001(2) C14 0.051(3) 0.043(2) 0.031(2) 0.0104(18) -0.0024(19) 0.007(2) C15 0.0331(19) 0.0273(18) 0.0271(19) 0.0012(14) -0.0021(15) 0.0162(16) C16 0.033(2) 0.0266(19) 0.049(2) -0.0003(17) 0.0106(18) 0.0111(17) C17 0.060(3) 0.031(2) 0.054(3) -0.0103(18) 0.004(2) 0.024(2) C18 0.036(2) 0.029(2) 0.059(3) -0.0038(18) 0.0060(18) 0.0134(17) C19 0.0292(19) 0.033(2) 0.032(2) 0.0004(16) -0.0009(16) 0.0092(16) O2A 0.035(2) 0.031(2) 0.019(2) 0.010(2) 0.0018(18) 0.0192(19) O3A 0.106(4) 0.042(2) 0.058(3) -0.001(2) 0.002(2) 0.028(2) C20A 0.056(4) 0.050(4) 0.069(4) 0.019(3) 0.027(3) 0.038(3) C21A 0.077(4) 0.082(4) 0.064(4) -0.019(3) -0.046(3) 0.061(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 Ni1 O1 1.983(2) 3_665 yes Ni1 O3B 2.037(10) 2_655 yes Ni1 N2 2.037(3) . yes Ni1 O1 2.049(2) . yes Ni1 O2A 2.064(4) . yes Ni1 N1 2.127(3) . yes Ni1 O3B 2.226(14) . yes Ni1 O2B 2.303(17) 2_655 yes Ni1 C20B 2.416(10) 2_655 yes O1 C9 1.371(4) 2_655 ? O1 Ni1 1.983(2) 2_655 ? N1 C10 1.337(4) . ? N1 C14 1.386(4) . ? N2 C19 1.323(4) . ? N2 C15 1.360(4) . ? C1 C2 1.374(4) . ? C1 C2 1.392(4) 3_665 ? C2 C1 1.392(4) 2_655 ? C2 C3 1.503(4) . ? C3 C4 1.378(4) . ? C3 C8 1.424(4) . ? C4 C5 1.394(4) . ? C5 C6 1.405(4) . ? C6 C7 1.370(4) . ? C7 C8 1.404(4) . ? C8 C9 1.536(4) . ? C9 O1 1.371(4) 3_665 ? C9 C10 1.540(4) . ? C9 C15 1.568(4) 3_665 ? C10 C11 1.405(4) . ? C11 C12 1.374(5) . ? C12 C13 1.374(5) . ? C13 C14 1.378(5) . ? C15 C16 1.386(4) . ? C15 C9 1.568(4) 2_655 ? C16 C17 1.403(4) . ? C17 C18 1.368(4) . ? C18 C19 1.408(4) . ? O2A C20A 1.277(6) . ? O3A C20A 1.259(6) . ? C20A C21A 1.555(7) . ? O2B C20B 1.210(18) . ? O2B Ni1 2.303(17) 3_665 ? O3B C20B 1.212(11) . ? O3B Ni1 2.037(10) 3_665 ? C20B C21B 1.388(14) . ? C20B Ni1 2.416(10) 3_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 O1 Ni1 O3B 87.8(2) 3_665 2_655 yes O1 Ni1 N2 114.18(9) 3_665 . yes O3B Ni1 N2 149.3(4) 2_655 . yes O1 Ni1 O1 88.78(12) 3_665 . yes O3B Ni1 O1 81.1(4) 2_655 . yes N2 Ni1 O1 78.43(9) . . yes O1 Ni1 O2A 153.73(15) 3_665 . yes O3B Ni1 O2A 69.5(2) 2_655 . yes N2 Ni1 O2A 91.90(16) . . yes O1 Ni1 O2A 100.09(14) . . yes O1 Ni1 N1 76.89(10) 3_665 . yes O3B Ni1 N1 99.2(4) 2_655 . yes N2 Ni1 N1 106.26(10) . . yes O1 Ni1 N1 165.64(9) . . yes O2A Ni1 N1 93.38(14) . . yes O1 Ni1 O3B 78.0(2) 3_665 . yes O3B Ni1 O3B 11.0(4) 2_655 . yes N2 Ni1 O3B 159.7(2) . . yes O1 Ni1 O3B 86.0(3) . . yes O2A Ni1 O3B 78.0(3) . . yes N1 Ni1 O3B 92.0(2) . . yes O1 Ni1 O2B 142.7(4) 3_665 2_655 yes O3B Ni1 O2B 59.3(5) 2_655 2_655 yes N2 Ni1 O2B 103.0(4) . 2_655 yes O1 Ni1 O2B 101.7(5) . 2_655 yes O2A Ni1 O2B 11.1(5) . 2_655 yes N1 Ni1 O2B 90.6(5) . 2_655 yes O3B Ni1 O2B 67.3(5) . 2_655 yes O1 Ni1 C20B 114.7(3) 3_665 2_655 yes O3B Ni1 C20B 30.1(3) 2_655 2_655 yes N2 Ni1 C20B 130.5(3) . 2_655 yes O1 Ni1 C20B 95.1(3) . 2_655 yes O2A Ni1 C20B 40.3(3) . 2_655 yes N1 Ni1 C20B 92.0(3) . 2_655 yes O3B Ni1 C20B 37.7(3) . 2_655 yes O2B Ni1 C20B 29.6(4) 2_655 2_655 yes C9 O1 Ni1 116.94(18) 2_655 2_655 ? C9 O1 Ni1 112.36(17) 2_655 . ? Ni1 O1 Ni1 104.20(10) 2_655 . ? C10 N1 C14 118.7(3) . . ? C10 N1 Ni1 114.5(2) . . ? C14 N1 Ni1 125.4(3) . . ? C19 N2 C15 118.9(3) . . ? C19 N2 Ni1 126.7(2) . . ? C15 N2 Ni1 113.9(2) . . ? C2 C1 C2 121.1(3) . 3_665 ? C1 C2 C1 118.8(3) . 2_655 ? C1 C2 C3 122.5(3) . . ? C1 C2 C3 118.5(3) 2_655 . ? C4 C3 C8 119.9(3) . . ? C4 C3 C2 117.8(3) . . ? C8 C3 C2 122.3(3) . . ? C3 C4 C5 121.6(3) . . ? C4 C5 C6 119.4(3) . . ? C7 C6 C5 118.8(3) . . ? C6 C7 C8 123.3(3) . . ? C7 C8 C3 117.0(3) . . ? C7 C8 C9 120.9(3) . . ? C3 C8 C9 122.1(3) . . ? O1 C9 C8 113.4(2) 3_665 . ? O1 C9 C10 107.3(3) 3_665 . ? C8 C9 C10 109.0(2) . . ? O1 C9 C15 108.1(2) 3_665 3_665 ? C8 C9 C15 109.0(2) . 3_665 ? C10 C9 C15 110.0(2) . 3_665 ? N1 C10 C11 121.0(3) . . ? N1 C10 C9 112.6(3) . . ? C11 C10 C9 126.4(3) . . ? C12 C11 C10 119.8(4) . . ? C13 C12 C11 119.7(4) . . ? C12 C13 C14 119.2(3) . . ? C13 C14 N1 121.7(4) . . ? N2 C15 C16 122.1(3) . . ? N2 C15 C9 114.0(3) . 2_655 ? C16 C15 C9 123.8(3) . 2_655 ? C15 C16 C17 117.4(3) . . ? C18 C17 C16 121.2(3) . . ? C17 C18 C19 117.1(3) . . ? N2 C19 C18 123.2(3) . . ? C20A O2A Ni1 134.2(4) . . ? O3A C20A O2A 124.2(6) . . ? O3A C20A C21A 114.6(5) . . ? O2A C20A C21A 120.9(6) . . ? C20B O2B Ni1 80.4(11) . 3_665 ? C20B O3B Ni1 92.5(8) . 3_665 ? C20B O3B Ni1 119.6(11) . . ? Ni1 O3B Ni1 96.4(3) 3_665 . ? O3B C20B O2B 126.0(13) . . ? O3B C20B C21B 119.3(11) . . ? O2B C20B C21B 114.7(12) . . ? O3B C20B Ni1 57.4(6) . 3_665 ? O2B C20B Ni1 70.0(10) . 3_665 ? C21B C20B Ni1 166.9(9) . 3_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.16 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.125 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.076