# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ql6 _database_code_depnum_ccdc_archive 'CCDC 861395' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H36 Co3 N4 O17' _chemical_formula_sum 'C50 H36 Co3 N4 O17' _chemical_formula_weight 1141.62 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_hall '-c 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.859(4) _cell_length_b 12.2673(18) _cell_length_c 17.083(3) _cell_angle_alpha 90.00 _cell_angle_beta 124.590(2) _cell_angle_gamma 90.00 _cell_volume 4633.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5943 _cell_measurement_theta_min 2.394 _cell_measurement_theta_max 27.433 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2324 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.733 _exptl_absorpt_correction_T_max 0.777 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12417 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4079 _reflns_number_gt 3547 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+8.7497P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4055 _refine_ls_number_parameters 330 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.52716(18) 0.6017(3) 0.4334(3) 0.0496(9) Uani 1 1 d . . . H1 H 0.5530 0.5419 0.4583 0.059 Uiso 1 1 calc R . . C2 C 0.52260(18) 0.6667(3) 0.4942(2) 0.0513(9) Uani 1 1 d . . . H2 H 0.5446 0.6497 0.5586 0.062 Uiso 1 1 calc R . . C3 C 0.48549(14) 0.7577(2) 0.4604(2) 0.0343(7) Uani 1 1 d . . . C4 C 0.45596(15) 0.7784(3) 0.3649(2) 0.0439(8) Uani 1 1 d . . . H4 H 0.4319 0.8403 0.3387 0.053 Uiso 1 1 calc RD . . C5 C 0.46184(16) 0.7081(3) 0.3079(2) 0.0454(8) Uani 1 1 d . . . H5 H 0.4404 0.7234 0.2432 0.054 Uiso 1 1 calc R . . C6 C 0.47669(13) 0.8281(2) 0.5223(2) 0.0326(6) Uani 1 1 d . . . C7 C 0.49745(13) 0.7956(2) 0.6136(2) 0.0343(7) Uani 1 1 d . . . H7 H 0.5204 0.7324 0.6388 0.041 Uiso 1 1 calc R . . C8 C 0.48419(13) 0.8566(2) 0.66724(19) 0.0325(7) Uani 1 1 d . . . C9 C 0.45097(14) 0.9518(2) 0.6335(2) 0.0336(7) Uani 1 1 d . . . H9 H 0.4429 0.9922 0.6712 0.040 Uiso 1 1 calc R . . C10 C 0.42971(13) 0.9863(2) 0.5413(2) 0.0319(6) Uani 1 1 d . . . C11 C 0.44340(14) 0.9244(2) 0.4878(2) 0.0357(7) Uani 1 1 d . . . H11 H 0.4299 0.9479 0.4270 0.043 Uiso 1 1 calc R . . C12 C 0.39026(14) 1.0841(2) 0.4970(2) 0.0330(7) Uani 1 1 d . . . C13 C 0.3809(2) 1.1583(3) 0.5461(3) 0.0684(13) Uani 1 1 d . . . H13 H 0.3989 1.1487 0.6109 0.082 Uiso 1 1 calc R . . C14 C 0.3445(2) 1.2489(4) 0.5002(3) 0.0720(14) Uani 1 1 d . . . H14 H 0.3396 1.2985 0.5365 0.086 Uiso 1 1 calc R . . C15 C 0.3252(2) 1.1941(3) 0.3627(3) 0.0659(13) Uani 1 1 d . . . H15 H 0.3060 1.2040 0.2976 0.079 Uiso 1 1 calc R . . C16 C 0.3601(2) 1.1031(3) 0.4024(3) 0.0650(13) Uani 1 1 d . . . H16 H 0.3632 1.0536 0.3642 0.078 Uiso 1 1 calc R . . C18 C 0.39975(14) 0.3812(2) 0.1786(2) 0.0361(7) Uani 1 1 d . . . C19 C 0.36149(13) 0.2926(2) 0.1101(2) 0.0301(6) Uani 1 1 d . . . C20 C 0.35042(13) 0.2896(2) 0.0207(2) 0.0300(6) Uani 1 1 d . . . H20 H 0.3673 0.3425 0.0034 0.036 Uiso 1 1 calc R . . C21 C 0.31445(12) 0.2085(2) -0.04371(19) 0.0277(6) Uani 1 1 d . . . C22 C 0.28981(13) 0.1291(2) -0.0169(2) 0.0285(6) Uani 1 1 d . . . H22 H 0.2654 0.0748 -0.0599 0.034 Uiso 1 1 calc R . . C23 C 0.30130(13) 0.1301(2) 0.0727(2) 0.0293(6) Uani 1 1 d . . . C24 C 0.33700(13) 0.2128(2) 0.1359(2) 0.0314(6) Uani 1 1 d . . . H24 H 0.3445 0.2144 0.1961 0.038 Uiso 1 1 calc R . . C25 C 0.27622(14) 0.0450(2) 0.1039(2) 0.0332(7) Uani 1 1 d . . . C26 C 0.30239(13) 0.2086(2) -0.1411(2) 0.0305(6) Uani 1 1 d . . . Co1 Co 0.5000 0.51889(4) 0.2500 0.02817(16) Uani 1 2 d S . . Co2 Co 0.242699(19) 0.10031(3) -0.33437(3) 0.03300(14) Uani 1 1 d . . . N1 N 0.49609(12) 0.6202(2) 0.33946(18) 0.0341(6) Uani 1 1 d . . . N2 N 0.31651(12) 1.2687(2) 0.40877(18) 0.038 Uani 1 1 d . . . O1 O 0.43170(11) 0.43383(19) 0.15740(16) 0.0464(6) Uani 1 1 d . . . O2 O 0.39955(13) 0.3999(2) 0.24934(17) 0.0550(7) Uani 1 1 d . . . O3 O 0.32675(11) 0.28085(18) -0.15997(16) 0.0444(6) Uani 1 1 d . . . O4 O 0.26842(10) 0.13401(17) -0.19804(14) 0.0373(5) Uani 1 1 d . . . O5 O 0.29207(12) 0.04414(19) 0.18814(16) 0.0496(6) Uani 1 1 d . . . O6 O 0.23886(10) -0.02478(17) 0.04627(15) 0.0405(5) Uani 1 1 d . . . O7 O 0.5000 0.8060(2) 0.7500 0.0449(8) Uani 1 2 d S . . O1W O 0.16965(12) 0.00876(19) -0.34759(18) 0.0517(6) Uani 1 1 d D . . H1W H 0.1779 -0.0564 -0.3410 0.078 Uiso 1 1 calc RD . . H1WB H 0.1864 0.0170 -0.2935 0.078 Uiso 1 1 d RD . . O2W O 0.31660(10) 0.1952(2) -0.31113(16) 0.0461(6) Uani 1 1 d DU . . H2W3 H 0.3135 0.2615 -0.3010 0.069 Uiso 1 1 d RD . . H2W4 H 0.3312 0.1962 -0.2444 0.069 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.073(2) 0.0394(19) 0.0421(19) 0.0112(16) 0.0365(19) 0.0229(17) C2 0.076(3) 0.046(2) 0.0342(18) 0.0088(16) 0.0326(18) 0.0204(18) C3 0.0389(16) 0.0347(16) 0.0323(15) 0.0010(13) 0.0220(13) 0.0017(13) C4 0.0500(19) 0.0421(19) 0.0350(17) 0.0048(15) 0.0214(15) 0.0189(15) C5 0.0491(19) 0.053(2) 0.0307(16) 0.0021(16) 0.0206(15) 0.0130(16) C6 0.0371(16) 0.0325(16) 0.0319(15) -0.0004(13) 0.0219(13) 0.0005(13) C7 0.0386(16) 0.0304(15) 0.0298(15) 0.0010(13) 0.0170(13) 0.0030(13) C8 0.0397(16) 0.0306(16) 0.0238(15) 0.0008(12) 0.0159(13) -0.0034(13) C9 0.0400(16) 0.0320(16) 0.0311(15) -0.0060(13) 0.0216(14) -0.0030(13) C10 0.0346(15) 0.0298(15) 0.0308(15) -0.0002(12) 0.0183(13) -0.0001(12) C11 0.0461(18) 0.0340(16) 0.0294(15) 0.0054(13) 0.0228(14) 0.0056(14) C12 0.0388(16) 0.0308(16) 0.0303(15) -0.0037(13) 0.0203(13) -0.0029(13) C13 0.104(3) 0.066(3) 0.0348(19) 0.0137(19) 0.039(2) 0.045(3) C14 0.113(4) 0.064(3) 0.046(2) 0.012(2) 0.049(2) 0.049(3) C15 0.088(3) 0.069(3) 0.0301(18) 0.0065(18) 0.0272(19) 0.043(2) C16 0.087(3) 0.061(2) 0.0364(19) 0.0030(18) 0.028(2) 0.040(2) C18 0.0398(17) 0.0284(15) 0.0293(16) 0.0018(13) 0.0131(14) -0.0030(13) C19 0.0326(15) 0.0250(14) 0.0287(14) 0.0003(12) 0.0150(12) -0.0009(12) C20 0.0323(15) 0.0248(14) 0.0312(15) 0.0044(12) 0.0169(13) 0.0008(11) C21 0.0297(14) 0.0255(14) 0.0269(14) 0.0014(11) 0.0155(12) 0.0038(11) C22 0.0316(14) 0.0230(14) 0.0291(14) -0.0020(11) 0.0162(12) -0.0021(11) C23 0.0354(15) 0.0243(14) 0.0319(15) 0.0002(12) 0.0213(13) -0.0014(12) C24 0.0384(16) 0.0295(15) 0.0265(14) -0.0008(12) 0.0185(13) -0.0027(12) C25 0.0432(17) 0.0265(15) 0.0322(16) -0.0019(13) 0.0229(14) -0.0034(13) C26 0.0360(15) 0.0266(15) 0.0291(15) 0.0024(12) 0.0186(13) 0.0037(12) Co1 0.0336(3) 0.0228(3) 0.0259(3) 0.000 0.0156(2) 0.000 Co2 0.0436(3) 0.0271(2) 0.0281(2) 0.00123(16) 0.0203(2) 0.00715(17) N1 0.0415(14) 0.0289(13) 0.0325(13) -0.0013(11) 0.0213(12) 0.0033(11) N2 0.043 0.029 0.035 0.000 0.018 0.007 O1 0.0518(14) 0.0398(13) 0.0381(12) -0.0048(10) 0.0199(11) -0.0195(11) O2 0.0779(18) 0.0475(15) 0.0387(13) -0.0116(11) 0.0325(13) -0.0197(13) O3 0.0652(15) 0.0367(12) 0.0409(12) -0.0025(10) 0.0357(12) -0.0116(11) O4 0.0511(13) 0.0352(12) 0.0280(11) -0.0041(9) 0.0239(10) -0.0066(10) O5 0.0803(17) 0.0409(13) 0.0337(12) -0.0090(10) 0.0360(12) -0.0247(12) O6 0.0529(13) 0.0347(12) 0.0326(11) -0.0030(10) 0.0234(10) -0.0150(10) O7 0.075(2) 0.0315(16) 0.0270(15) 0.000 0.0278(16) 0.000 O1W 0.0693(16) 0.0349(12) 0.0548(15) -0.0056(11) 0.0375(14) -0.0062(11) O2W 0.0513(14) 0.0490(14) 0.0428(13) -0.0024(11) 0.0295(11) -0.0018(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.343(4) . ? C1 C2 1.369(5) . ? C1 H1 0.9300 . ? C2 C3 1.386(4) . ? C2 H2 0.9300 . ? C3 C4 1.373(4) . ? C3 C6 1.484(4) . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 N1 1.317(4) . ? C5 H5 0.9300 . ? C6 C7 1.384(4) . ? C6 C11 1.394(4) . ? C7 C8 1.378(4) . ? C7 H7 0.9300 . ? C8 O7 1.372(3) . ? C8 C9 1.381(4) . ? C9 C10 1.403(4) . ? C9 H9 0.9300 . ? C10 C11 1.389(4) . ? C10 C12 1.491(4) . ? C11 H11 0.9300 . ? C12 C13 1.355(5) . ? C12 C16 1.355(5) . ? C13 C14 1.390(5) . ? C13 H13 0.9300 . ? C14 N2 1.316(4) . ? C14 H14 0.9300 . ? C15 N2 1.312(4) . ? C15 C16 1.365(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 O2 1.233(4) . ? C18 O1 1.280(4) . ? C18 C19 1.497(4) . ? C19 C20 1.381(4) . ? C19 C24 1.383(4) . ? C20 C21 1.388(4) . ? C20 H20 0.9300 . ? C21 C22 1.393(4) . ? C21 C26 1.503(4) . ? C22 C23 1.379(4) . ? C22 H22 0.9300 . ? C23 C24 1.393(4) . ? C23 C25 1.496(4) . ? C24 H24 0.9300 . ? C25 O5 1.247(4) . ? C25 O6 1.260(4) . ? C25 Co2 2.485(3) 6_556 ? C26 O3 1.248(4) . ? C26 O4 1.268(3) . ? Co1 O1 1.914(2) . ? Co1 O1 1.914(2) 2_655 ? Co1 N1 2.018(2) . ? Co1 N1 2.018(2) 2_655 ? Co2 O4 2.060(2) . ? Co2 N2 2.105(3) 7_565 ? Co2 O5 2.114(2) 6 ? Co2 O2W 2.135(2) . ? Co2 O1W 2.158(3) . ? Co2 O6 2.188(2) 6 ? Co2 C25 2.485(3) 6 ? N2 Co2 2.105(3) 7_565 ? O5 Co2 2.114(2) 6_556 ? O6 Co2 2.188(2) 6_556 ? O7 C8 1.372(3) 2_656 ? O1W H1W 0.8200 . ? O1W H1WB 0.7709 . ? O2W H2W3 0.8453 . ? O2W H2W4 0.9730 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.1(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 120.4(3) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 116.0(3) . . ? C4 C3 C6 121.3(3) . . ? C2 C3 C6 122.7(3) . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 123.9(3) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C7 C6 C11 118.2(3) . . ? C7 C6 C3 120.7(3) . . ? C11 C6 C3 121.0(3) . . ? C8 C7 C6 120.1(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? O7 C8 C7 113.2(3) . . ? O7 C8 C9 124.1(3) . . ? C7 C8 C9 122.2(3) . . ? C8 C9 C10 118.5(3) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 C12 118.9(3) . . ? C9 C10 C12 122.1(3) . . ? C10 C11 C6 122.1(3) . . ? C10 C11 H11 119.0 . . ? C6 C11 H11 119.0 . . ? C13 C12 C16 115.3(3) . . ? C13 C12 C10 123.7(3) . . ? C16 C12 C10 121.0(3) . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? N2 C14 C13 124.2(3) . . ? N2 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? N2 C15 C16 125.3(3) . . ? N2 C15 H15 117.4 . . ? C16 C15 H15 117.4 . . ? C12 C16 C15 120.7(3) . . ? C12 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? O2 C18 O1 124.1(3) . . ? O2 C18 C19 121.2(3) . . ? O1 C18 C19 114.7(3) . . ? C20 C19 C24 119.4(3) . . ? C20 C19 C18 120.3(3) . . ? C24 C19 C18 120.3(3) . . ? C19 C20 C21 120.8(3) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C22 119.2(3) . . ? C20 C21 C26 119.5(3) . . ? C22 C21 C26 121.3(3) . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 119.3(3) . . ? C22 C23 C25 121.8(3) . . ? C24 C23 C25 118.9(3) . . ? C19 C24 C23 120.8(3) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? O5 C25 O6 119.7(3) . . ? O5 C25 C23 119.3(3) . . ? O6 C25 C23 121.0(3) . . ? O5 C25 Co2 58.23(15) . 6_556 ? O6 C25 Co2 61.64(15) . 6_556 ? C23 C25 Co2 175.6(2) . 6_556 ? O3 C26 O4 124.6(3) . . ? O3 C26 C21 118.1(3) . . ? O4 C26 C21 117.3(2) . . ? O1 Co1 O1 113.91(15) . 2_655 ? O1 Co1 N1 121.61(11) . . ? O1 Co1 N1 98.48(10) 2_655 . ? O1 Co1 N1 98.48(10) . 2_655 ? O1 Co1 N1 121.61(11) 2_655 2_655 ? N1 Co1 N1 103.97(15) . 2_655 ? O4 Co2 N2 100.54(9) . 7_565 ? O4 Co2 O5 100.92(9) . 6 ? N2 Co2 O5 158.54(9) 7_565 6 ? O4 Co2 O2W 90.03(9) . . ? N2 Co2 O2W 90.00(10) 7_565 . ? O5 Co2 O2W 90.13(10) 6 . ? O4 Co2 O1W 85.66(9) . . ? N2 Co2 O1W 90.21(10) 7_565 . ? O5 Co2 O1W 91.26(10) 6 . ? O2W Co2 O1W 175.65(9) . . ? O4 Co2 O6 161.16(9) . 6 ? N2 Co2 O6 98.09(9) 7_565 6 ? O5 Co2 O6 60.48(8) 6 6 ? O2W Co2 O6 87.20(9) . 6 ? O1W Co2 O6 97.07(10) . 6 ? O4 Co2 C25 130.81(9) . 6 ? N2 Co2 C25 128.52(10) 7_565 6 ? O5 Co2 C25 30.11(9) 6 6 ? O2W Co2 C25 86.99(10) . 6 ? O1W Co2 C25 96.27(10) . 6 ? O6 Co2 C25 30.44(9) 6 6 ? C5 N1 C1 116.3(3) . . ? C5 N1 Co1 121.2(2) . . ? C1 N1 Co1 122.5(2) . . ? C15 N2 C14 114.0(3) . . ? C15 N2 Co2 120.1(2) . 7_565 ? C14 N2 Co2 125.8(2) . 7_565 ? C18 O1 Co1 121.6(2) . . ? C26 O4 Co2 130.22(19) . . ? C25 O5 Co2 91.66(18) . 6_556 ? C25 O6 Co2 87.92(17) . 6_556 ? C8 O7 C8 126.2(3) 2_656 . ? Co2 O1W H1W 109.5 . . ? Co2 O1W H1WB 85.9 . . ? H1W O1W H1WB 91.9 . . ? Co2 O2W H2W3 111.8 . . ? Co2 O2W H2W4 86.4 . . ? H2W3 O2W H2W4 76.6 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.506 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.060 data_ql7 _database_code_depnum_ccdc_archive 'CCDC 861396' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H36 N4 O17 Zn3' _chemical_formula_sum 'C50 H36 N4 O17 Zn3' _chemical_formula_weight 1160.94 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 Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_hall ' -C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.909(5) _cell_length_b 12.170(3) _cell_length_c 17.157(3) _cell_angle_alpha 90.00 _cell_angle_beta 124.694(3) _cell_angle_gamma 90.00 _cell_volume 4619.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1845 _cell_measurement_theta_min 2.878 _cell_measurement_theta_max 22.016 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 1.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.699 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12650 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4066 _reflns_number_gt 2633 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4044 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 C1 C 0.5163(2) 0.8589(4) 0.3334(3) 0.0279(11) Uani 1 1 d . . . C2 C 0.5026(2) 0.7967(3) 0.3865(3) 0.0275(11) Uani 1 1 d . . . H2 H 0.4796 0.7332 0.3612 0.033 Uiso 1 1 calc R . . C3 C 0.52344(19) 0.8298(3) 0.4776(3) 0.0243(10) Uani 1 1 d . . . C4 C 0.5561(2) 0.9254(3) 0.5119(3) 0.0264(11) Uani 1 1 d . . . H4 H 0.5691 0.9492 0.5722 0.032 Uiso 1 1 calc R . . C5 C 0.57074(19) 0.9888(3) 0.4586(3) 0.0248(10) Uani 1 1 d . . . C6 C 0.54965(19) 0.9530(3) 0.3681(3) 0.0272(11) Uani 1 1 d . . . H6 H 0.5583 0.9930 0.3310 0.033 Uiso 1 1 calc R . . C7 C 0.61069(19) 1.0849(3) 0.5038(3) 0.0236(10) Uani 1 1 d . . . C8 C 0.6404(2) 1.1041(4) 0.5982(3) 0.0581(17) Uani 1 1 d . . . H8 H 0.6362 1.0545 0.6354 0.070 Uiso 1 1 calc R . . C9 C 0.6766(2) 1.1955(4) 0.6405(4) 0.0565(16) Uani 1 1 d . . . H9 H 0.6962 1.2045 0.7055 0.068 Uiso 1 1 calc R . . C10 C 0.6574(3) 1.2520(5) 0.5025(4) 0.0593(17) Uani 1 1 d . . . H10 H 0.6625 1.3022 0.4668 0.071 Uiso 1 1 calc R . . C11 C 0.6210(3) 1.1606(4) 0.4563(4) 0.0554(16) Uani 1 1 d . . . H11 H 0.6034 1.1513 0.3918 0.067 Uiso 1 1 calc R . . C12 C 0.5146(2) 0.7574(3) 0.5395(3) 0.0255(11) Uani 1 1 d . . . C13 C 0.4775(2) 0.6671(4) 0.5051(3) 0.0410(13) Uani 1 1 d . . . H13 H 0.4553 0.6507 0.4407 0.049 Uiso 1 1 calc R . . C14 C 0.4732(2) 0.6001(4) 0.5668(3) 0.0401(13) Uani 1 1 d . . . H14 H 0.4480 0.5390 0.5423 0.048 Uiso 1 1 calc R . . C15 C 0.5385(2) 0.7075(4) 0.6918(3) 0.0401(13) Uani 1 1 d . . . H15 H 0.5605 0.7225 0.7564 0.048 Uiso 1 1 calc R . . C16 C 0.5440(2) 0.7788(4) 0.6339(3) 0.0397(13) Uani 1 1 d . . . H16 H 0.5679 0.8414 0.6596 0.048 Uiso 1 1 calc R . . C17 C 0.6006(2) 0.3802(4) 0.8208(3) 0.0340(12) Uani 1 1 d . . . C18 C 0.63894(19) 0.2925(3) 0.8907(3) 0.0261(10) Uani 1 1 d . . . C19 C 0.6643(2) 0.2101(3) 0.8661(3) 0.0320(11) Uani 1 1 d . . . H19 H 0.6573 0.2107 0.8064 0.038 Uiso 1 1 calc R . . C20 C 0.6994(2) 0.1287(3) 0.9294(3) 0.0270(11) Uani 1 1 d . . . C21 C 0.70914(19) 0.1269(3) 1.0180(3) 0.0290(11) Uani 1 1 d . . . H21 H 0.7323 0.0710 1.0606 0.035 Uiso 1 1 calc R . . C22 C 0.68458(19) 0.2079(3) 1.0437(3) 0.0264(11) Uani 1 1 d . . . C23 C 0.64889(18) 0.2887(3) 0.9787(3) 0.0257(10) Uani 1 1 d . . . H23 H 0.6313 0.3416 0.9948 0.031 Uiso 1 1 calc R . . C24 C 0.6961(2) 0.2072(4) 1.1402(3) 0.0306(11) Uani 1 1 d . . . C25 C 0.7268(2) 0.0402(4) 0.9025(4) 0.0376(13) Uani 1 1 d . . . N1 N 0.50378(17) 0.6201(3) 0.6601(2) 0.0303(9) Uani 1 1 d . . . N2 N 0.68491(16) 1.2713(3) 0.5932(3) 0.0310(9) Uani 1 1 d . . . O1 O 0.5000 0.8079(3) 0.2500 0.0383(12) Uani 1 2 d S . . O2 O 0.56798(15) 0.4321(2) 0.8412(2) 0.0438(9) Uani 1 1 d . . . O3 O 0.60098(15) 0.3979(3) 0.7500(2) 0.0486(9) Uani 1 1 d . . . O4 O 0.71200(17) 0.0402(3) 0.8185(3) 0.0557(11) Uani 1 1 d . . . O5 O 0.76237(16) -0.0277(3) 0.9603(2) 0.0477(9) Uani 1 1 d . . . O6 O 0.67248(16) 0.2796(2) 1.1599(2) 0.0460(9) Uani 1 1 d . . . O7 O 0.72890(14) 0.1301(2) 1.1959(2) 0.0390(8) Uani 1 1 d . . . Zn1 Zn 0.5000 0.51823(6) 0.7500 0.0265(2) Uani 1 2 d S . . Zn2 Zn 0.75772(3) -0.09963(5) 0.83014(4) 0.04070(19) Uani 1 1 d . . . O8 O 0.83280(16) -0.0080(3) 0.8464(2) 0.0552(10) Uani 1 1 d . . . H8A H 0.8487 -0.0459 0.8244 0.083 Uiso 1 1 d R . . H8B H 0.8197 0.0522 0.8160 0.083 Uiso 1 1 d R . . O9 O 0.68192(16) -0.1951(2) 0.8116(2) 0.054 Uani 1 1 d . . . H9C H 0.6669 -0.1948 0.7491 0.081 Uiso 1 1 d R . . H9D H 0.6586 -0.2473 0.7815 0.081 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(3) 0.027(3) 0.021(3) -0.001(2) 0.018(2) 0.007(2) C2 0.035(3) 0.022(2) 0.028(3) -0.002(2) 0.019(2) -0.004(2) C3 0.030(3) 0.023(2) 0.023(3) -0.002(2) 0.017(2) -0.002(2) C4 0.038(3) 0.023(3) 0.021(3) -0.005(2) 0.019(2) -0.003(2) C5 0.028(3) 0.023(2) 0.024(3) 0.001(2) 0.015(2) 0.003(2) C6 0.036(3) 0.023(3) 0.026(3) 0.004(2) 0.020(2) 0.003(2) C7 0.030(3) 0.021(2) 0.022(3) 0.003(2) 0.016(2) 0.003(2) C8 0.079(4) 0.049(4) 0.038(3) -0.005(3) 0.028(3) -0.042(3) C9 0.070(4) 0.059(4) 0.029(3) -0.004(3) 0.021(3) -0.032(3) C10 0.084(5) 0.059(4) 0.044(4) -0.002(3) 0.041(4) -0.035(3) C11 0.088(5) 0.053(4) 0.030(3) -0.014(3) 0.036(3) -0.034(3) C12 0.032(3) 0.025(3) 0.024(3) 0.002(2) 0.019(2) -0.001(2) C13 0.062(4) 0.038(3) 0.026(3) -0.012(2) 0.027(3) -0.026(3) C14 0.062(4) 0.027(3) 0.032(3) -0.008(2) 0.027(3) -0.019(3) C15 0.047(3) 0.047(3) 0.024(3) -0.009(2) 0.019(3) -0.020(3) C16 0.049(3) 0.039(3) 0.030(3) -0.003(2) 0.022(3) -0.021(3) C17 0.034(3) 0.027(3) 0.033(3) -0.005(2) 0.014(3) -0.002(2) C18 0.024(3) 0.022(3) 0.027(3) 0.001(2) 0.012(2) 0.001(2) C19 0.037(3) 0.029(3) 0.035(3) 0.000(2) 0.023(3) -0.002(2) C20 0.032(3) 0.018(2) 0.035(3) 0.001(2) 0.022(2) 0.003(2) C21 0.031(3) 0.020(3) 0.032(3) 0.001(2) 0.015(2) 0.005(2) C22 0.025(3) 0.027(3) 0.026(3) -0.002(2) 0.014(2) -0.003(2) C23 0.024(3) 0.022(2) 0.030(3) -0.004(2) 0.015(2) 0.002(2) C24 0.031(3) 0.023(3) 0.036(3) -0.002(2) 0.018(3) -0.006(2) C25 0.051(4) 0.022(3) 0.052(4) -0.004(3) 0.037(3) 0.001(3) N1 0.040(2) 0.026(2) 0.025(2) -0.0016(18) 0.018(2) -0.0039(19) N2 0.038(2) 0.029(2) 0.027(2) 0.0018(18) 0.018(2) -0.0070(19) O1 0.073(4) 0.020(2) 0.029(3) 0.000 0.033(3) 0.000 O2 0.052(2) 0.037(2) 0.038(2) 0.0022(16) 0.0222(19) 0.0185(18) O3 0.067(3) 0.042(2) 0.033(2) 0.0102(18) 0.026(2) 0.0133(19) O4 0.094(3) 0.039(2) 0.055(3) 0.0066(19) 0.055(3) 0.023(2) O5 0.057(2) 0.030(2) 0.049(2) -0.0009(18) 0.027(2) 0.0161(19) O6 0.073(3) 0.032(2) 0.050(2) 0.0026(17) 0.046(2) 0.010(2) O7 0.051(2) 0.034(2) 0.031(2) 0.0055(16) 0.0232(18) 0.0067(18) Zn1 0.0340(5) 0.0208(4) 0.0258(4) 0.000 0.0176(4) 0.000 Zn2 0.0526(4) 0.0305(3) 0.0339(4) 0.0000(3) 0.0216(3) 0.0144(3) O8 0.078(3) 0.032(2) 0.062(3) -0.0052(19) 0.043(2) 0.003(2) O9 0.077 0.029 0.063 -0.003 0.043 0.003 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.365(6) . ? C1 O1 1.383(4) . ? C1 C2 1.385(5) . ? C2 C3 1.385(5) . ? C2 H2 0.9300 . ? C3 C4 1.373(5) . ? C3 C12 1.499(5) . ? C4 C5 1.412(5) . ? C4 H4 0.9300 . ? C5 C6 1.386(5) . ? C5 C7 1.475(6) . ? C6 H6 0.9300 . ? C7 C8 1.358(6) . ? C7 C11 1.359(6) . ? C8 C9 1.381(6) . ? C8 H8 0.9300 . ? C9 N2 1.329(5) . ? C9 H9 0.9300 . ? C10 N2 1.309(6) . ? C10 C11 1.393(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C16 1.363(6) . ? C12 C13 1.372(6) . ? C13 C14 1.392(6) . ? C13 H13 0.9300 . ? C14 N1 1.342(5) . ? C14 H14 0.9300 . ? C15 N1 1.312(5) . ? C15 C16 1.389(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 O3 1.239(5) . ? C17 O2 1.280(5) . ? C17 C18 1.495(6) . ? C18 C23 1.376(5) . ? C18 C19 1.407(5) . ? C19 C20 1.372(6) . ? C19 H19 0.9300 . ? C20 C21 1.390(5) . ? C20 C25 1.517(5) . ? C21 C22 1.391(5) . ? C21 H21 0.9300 . ? C22 C23 1.384(5) . ? C22 C24 1.501(6) . ? C23 H23 0.9300 . ? C24 O6 1.240(5) . ? C24 O7 1.271(5) . ? C25 O5 1.225(5) . ? C25 O4 1.259(5) . ? C25 Zn2 2.511(4) . ? N1 Zn1 2.026(3) . ? N2 Zn2 2.066(4) 4_666 ? O1 C1 1.383(4) 2_655 ? O2 Zn1 1.906(3) . ? O4 Zn2 2.041(3) . ? O5 Zn2 2.334(3) . ? O7 Zn2 2.002(3) 6_556 ? Zn1 O2 1.906(3) 2_656 ? Zn1 N1 2.026(3) 2_656 ? Zn2 O7 2.002(3) 6 ? Zn2 N2 2.066(4) 4_636 ? Zn2 O8 2.183(3) . ? Zn2 O9 2.208(3) . ? O8 H8A 0.8500 . ? O8 H8B 0.8500 . ? O9 H9C 0.9054 . ? O9 H9D 0.8342 . ? 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 C6 C1 O1 124.7(4) . . ? C6 C1 C2 121.8(4) . . ? O1 C1 C2 112.9(4) . . ? C3 C2 C1 119.6(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 118.6(4) . . ? C4 C3 C12 121.0(4) . . ? C2 C3 C12 120.2(4) . . ? C3 C4 C5 122.2(4) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 117.8(4) . . ? C6 C5 C7 123.3(4) . . ? C4 C5 C7 118.8(4) . . ? C1 C6 C5 120.0(4) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C11 114.6(4) . . ? C8 C7 C5 121.4(4) . . ? C11 C7 C5 124.0(4) . . ? C7 C8 C9 121.7(4) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? N2 C9 C8 123.5(5) . . ? N2 C9 H9 118.2 . . ? C8 C9 H9 118.2 . . ? N2 C10 C11 124.0(4) . . ? N2 C10 H10 118.0 . . ? C11 C10 H10 118.0 . . ? C7 C11 C10 121.2(5) . . ? C7 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C16 C12 C13 116.9(4) . . ? C16 C12 C3 120.7(4) . . ? C13 C12 C3 122.4(4) . . ? C12 C13 C14 119.8(4) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? N1 C14 C13 122.7(4) . . ? N1 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? N1 C15 C16 123.4(4) . . ? N1 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C12 C16 C15 120.2(4) . . ? C12 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? O3 C17 O2 124.9(4) . . ? O3 C17 C18 121.5(4) . . ? O2 C17 C18 113.6(4) . . ? C23 C18 C19 118.7(4) . . ? C23 C18 C17 121.3(4) . . ? C19 C18 C17 120.0(4) . . ? C20 C19 C18 120.7(4) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C21 119.6(4) . . ? C19 C20 C25 120.4(4) . . ? C21 C20 C25 120.0(4) . . ? C20 C21 C22 120.5(4) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.1(4) . . ? C23 C22 C24 120.4(4) . . ? C21 C22 C24 120.6(4) . . ? C18 C23 C22 121.4(4) . . ? C18 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? O6 C24 O7 124.4(4) . . ? O6 C24 C22 118.7(4) . . ? O7 C24 C22 116.9(4) . . ? O5 C25 O4 121.3(4) . . ? O5 C25 C20 121.6(4) . . ? O4 C25 C20 117.1(4) . . ? O5 C25 Zn2 67.5(2) . . ? O4 C25 Zn2 53.9(2) . . ? C20 C25 Zn2 170.4(4) . . ? C15 N1 C14 116.7(4) . . ? C15 N1 Zn1 120.9(3) . . ? C14 N1 Zn1 122.3(3) . . ? C10 N2 C9 115.0(4) . . ? C10 N2 Zn2 127.3(3) . 4_666 ? C9 N2 Zn2 117.6(3) . 4_666 ? C1 O1 C1 126.7(5) . 2_655 ? C17 O2 Zn1 122.2(3) . . ? C25 O4 Zn2 96.2(3) . . ? C25 O5 Zn2 83.5(3) . . ? C24 O7 Zn2 130.6(3) . 6_556 ? O2 Zn1 O2 113.3(2) 2_656 . ? O2 Zn1 N1 121.37(14) 2_656 2_656 ? O2 Zn1 N1 98.76(14) . 2_656 ? O2 Zn1 N1 98.76(14) 2_656 . ? O2 Zn1 N1 121.37(14) . . ? N1 Zn1 N1 104.5(2) 2_656 . ? O7 Zn2 O4 102.94(13) 6 . ? O7 Zn2 N2 104.56(13) 6 4_636 ? O4 Zn2 N2 152.41(14) . 4_636 ? O7 Zn2 O8 88.02(12) 6 . ? O4 Zn2 O8 92.81(14) . . ? N2 Zn2 O8 90.30(13) 4_636 . ? O7 Zn2 O9 90.91(12) 6 . ? O4 Zn2 O9 88.22(13) . . ? N2 Zn2 O9 89.18(13) 4_636 . ? O8 Zn2 O9 178.66(11) . . ? O7 Zn2 O5 160.78(13) 6 . ? O4 Zn2 O5 58.84(12) . . ? N2 Zn2 O5 93.59(13) 4_636 . ? O8 Zn2 O5 98.32(12) . . ? O9 Zn2 O5 82.95(12) . . ? O7 Zn2 C25 132.35(16) 6 . ? O4 Zn2 C25 29.89(14) . . ? N2 Zn2 C25 122.56(16) 4_636 . ? O8 Zn2 C25 97.68(14) . . ? O9 Zn2 C25 83.64(13) . . ? O5 Zn2 C25 28.99(13) . . ? Zn2 O8 H8A 109.2 . . ? Zn2 O8 H8B 109.4 . . ? H8A O8 H8B 109.5 . . ? Zn2 O9 H9C 85.5 . . ? Zn2 O9 H9D 142.9 . . ? H9C O9 H9D 66.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.560 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.080 data_ql1 _database_code_depnum_ccdc_archive 'CCDC 893948' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H29 N4 O7 Zn' _chemical_formula_sum 'C44 H29 N4 O7 Zn' _chemical_formula_weight 791.08 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' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' C 2/c ' _symmetry_space_group_name_hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.833(5) _cell_length_b 13.696(3) _cell_length_c 30.322(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.039(5) _cell_angle_gamma 90.00 _cell_volume 7478(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2877 _cell_measurement_theta_min 2.257 _cell_measurement_theta_max 20.990 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3256 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8247 _exptl_absorpt_correction_T_max 0.8584 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20536 _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_av_sigmaI/netI 0.1151 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6541 _reflns_number_gt 3941 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6541 _refine_ls_number_parameters 506 _refine_ls_number_restraints 957 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 0.842 _refine_ls_restrained_S_all 0.895 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1767(2) 1.0060(2) 0.34242(12) 0.0448(9) Uani 1 1 d U . . H1 H 0.1969 1.0367 0.3707 0.054 Uiso 1 1 calc R . . C2 C 0.1421(2) 1.0635(2) 0.30462(12) 0.0446(9) Uani 1 1 d U . . H2 H 0.1393 1.1308 0.3081 0.053 Uiso 1 1 calc R . . C3 C 0.1120(2) 1.0213(2) 0.26187(12) 0.0403(8) Uani 1 1 d U . . C4 C 0.1164(2) 0.9201(2) 0.26029(12) 0.0516(10) Uani 1 1 d U . . H4 H 0.0958 0.8877 0.2325 0.062 Uiso 1 1 calc R . . C5 C 0.1509(2) 0.8673(3) 0.29935(13) 0.0530(10) Uani 1 1 d U . . H5 H 0.1524 0.7996 0.2971 0.064 Uiso 1 1 calc R . . C6 C 0.07947(19) 1.0816(2) 0.21999(11) 0.0381(8) Uani 1 1 d U . . C7 C 0.1011(2) 1.1781(2) 0.21810(13) 0.0474(9) Uani 1 1 d U . . H7 H 0.1358 1.2053 0.2436 0.057 Uiso 1 1 calc R . . C8 C 0.0720(2) 1.2350(2) 0.17889(13) 0.0472(9) Uani 1 1 d U . . C9 C 0.0220(2) 1.1936(2) 0.14068(12) 0.0426(9) Uani 1 1 d U . . H9 H 0.0016 1.2308 0.1144 0.051 Uiso 1 1 calc R . . C10 C 0.00251(19) 1.0971(2) 0.14180(11) 0.0394(8) Uani 1 1 d U . . C11 C 0.02886(19) 1.0408(2) 0.18104(11) 0.0381(8) Uani 1 1 d U . . H11 H 0.0131 0.9766 0.1815 0.046 Uiso 1 1 calc R . . C12 C 0.0941(2) 1.3394(3) 0.17798(14) 0.0575(10) Uani 1 1 d U . . C13 C 0.1612(3) 1.3735(3) 0.20495(16) 0.0752(12) Uani 1 1 d U . . H13 H 0.1957 1.3303 0.2231 0.090 Uiso 1 1 calc R . . C14 C 0.1776(3) 1.4715(4) 0.2052(2) 0.0992(16) Uani 1 1 d U . . H14 H 0.2215 1.4937 0.2259 0.119 Uiso 1 1 calc R . . C15 C 0.0716(4) 1.5035(4) 0.1515(2) 0.1075(17) Uani 1 1 d U . . H15 H 0.0403 1.5480 0.1319 0.129 Uiso 1 1 calc R . . C16 C 0.0476(3) 1.4058(3) 0.15073(16) 0.0866(14) Uani 1 1 d U . . H16 H 0.0010 1.3871 0.1320 0.104 Uiso 1 1 calc R . . C17 C -0.0577(2) 1.0870(2) 0.06025(11) 0.0410(9) Uani 1 1 d U . . C18 C -0.0008(2) 1.1060(2) 0.04281(11) 0.0421(9) Uani 1 1 d U . . H18 H 0.0477 1.0959 0.0611 0.050 Uiso 1 1 calc R . . C19 C -0.0139(2) 1.1408(2) -0.00237(12) 0.0391(8) Uani 1 1 d U . . C20 C -0.0882(2) 1.1557(2) -0.02802(12) 0.0424(9) Uani 1 1 d U . . H20 H -0.0987 1.1819 -0.0575 0.051 Uiso 1 1 calc R . . C21 C -0.1457(2) 1.1325(2) -0.01072(12) 0.0432(9) Uani 1 1 d U . . C22 C -0.1308(2) 1.0964(2) 0.03456(12) 0.0427(9) Uani 1 1 d U . . H22 H -0.1691 1.0795 0.0467 0.051 Uiso 1 1 calc R . . C23 C 0.0473(2) 1.1577(2) -0.02257(12) 0.0387(8) Uani 1 1 d U . . C24 C 0.1224(2) 1.1484(2) 0.00142(13) 0.0488(9) Uani 1 1 d U . . H24 H 0.1362 1.1362 0.0330 0.059 Uiso 1 1 calc R . . C25 C 0.1757(2) 1.1568(2) -0.02027(13) 0.0479(10) Uani 1 1 d U . . H25 H 0.2251 1.1496 -0.0028 0.058 Uiso 1 1 calc R . . C26 C 0.0897(2) 1.1885(3) -0.08852(13) 0.0561(10) Uani 1 1 d U . . H26 H 0.0777 1.2042 -0.1197 0.067 Uiso 1 1 calc R . . C27 C 0.0333(2) 1.1807(3) -0.06896(13) 0.0547(10) Uani 1 1 d U . . H27 H -0.0153 1.1909 -0.0870 0.066 Uiso 1 1 calc R . . C28 C -0.2244(2) 1.1465(3) -0.03886(12) 0.0464(9) Uani 1 1 d U . . C29 C -0.2472(2) 1.2274(3) -0.06660(12) 0.0540(10) Uani 1 1 d U . . H29 H -0.2135 1.2759 -0.0683 0.065 Uiso 1 1 calc R . . C30 C -0.3209(3) 1.2347(3) -0.09173(14) 0.0615(11) Uani 1 1 d U . . H30 H -0.3354 1.2898 -0.1101 0.074 Uiso 1 1 calc R . . C31 C -0.3501(3) 1.0920(3) -0.06543(15) 0.0750(13) Uani 1 1 d U . . H31 H -0.3851 1.0444 -0.0648 0.090 Uiso 1 1 calc R . . C32 C -0.2780(2) 1.0773(3) -0.03888(14) 0.0621(11) Uani 1 1 d U . . H32 H -0.2654 1.0212 -0.0210 0.075 Uiso 1 1 calc R . . C33 C 0.3482(2) 0.9582(3) 0.44676(12) 0.0469(10) Uani 1 1 d U . . C34 C 0.4266(2) 0.9800(2) 0.47343(12) 0.0415(9) Uani 1 1 d U . . C35 C 0.4787(2) 0.9068(2) 0.48749(14) 0.0593(12) Uani 1 1 d U . . H35 H 0.4649 0.8427 0.4792 0.071 Uiso 1 1 calc R . . C36 C 0.4498(2) 1.0738(3) 0.48665(14) 0.0638(13) Uani 1 1 d U . . H36 H 0.4163 1.1250 0.4778 0.077 Uiso 1 1 calc R . . C37 C 0.2116(2) 0.6410(2) 0.36037(13) 0.0467(10) Uani 1 1 d U . . C38 C 0.2387(2) 0.5430(2) 0.34976(12) 0.0414(9) Uani 1 1 d U . . C39 C 0.1889(2) 0.4699(3) 0.33082(13) 0.0539(10) Uani 1 1 d U . . H39 H 0.1381 0.4817 0.3234 0.065 Uiso 1 1 calc R . . C40 C 0.2146(2) 0.3786(3) 0.32275(14) 0.0598(11) Uani 1 1 d U . . H40 H 0.1807 0.3296 0.3098 0.072 Uiso 1 1 calc R . . C41 C 0.2891(2) 0.3595(2) 0.33358(13) 0.0494(10) Uani 1 1 d U . . C42 C 0.3385(2) 0.4321(2) 0.35294(12) 0.0497(10) Uani 1 1 d U . . H42 H 0.3893 0.4196 0.3614 0.060 Uiso 1 1 calc R . . C43 C 0.3130(2) 0.5236(2) 0.35989(12) 0.0481(10) Uani 1 1 d U . . H43 H 0.3471 0.5731 0.3717 0.058 Uiso 1 1 calc R . . C44 C 0.3178(3) 0.2590(3) 0.32692(18) 0.0748(13) Uani 1 1 d U . . N1 N 0.18237(15) 0.90906(19) 0.34049(9) 0.0403(8) Uani 1 1 d . . . N2 N 0.16113(17) 1.17491(18) -0.06550(10) 0.0426(8) Uani 1 1 d . . . N3 N -0.3729(2) 1.1693(3) -0.09170(12) 0.0713(11) Uani 1 1 d . . . N4 N 0.1343(4) 1.5347(3) 0.17778(19) 0.121(2) Uani 1 1 d U . . O1 O -0.04722(14) 1.04996(15) 0.10492(8) 0.0511(7) Uani 1 1 d . . . O2 O 0.33298(14) 0.86942(18) 0.43587(9) 0.0614(8) Uani 1 1 d . . . O3 O 0.30185(16) 1.0237(2) 0.43640(10) 0.0768(10) Uani 1 1 d . . . O4 O 0.26314(15) 0.70153(16) 0.38034(10) 0.0627(8) Uani 1 1 d . . . O5 O 0.14510(17) 0.65913(18) 0.34932(11) 0.0707(9) Uani 1 1 d . . . O6 O 0.2734(2) 0.2025(2) 0.30106(17) 0.1246(16) Uani 1 1 d . . . H6A H 0.2859 0.1460 0.3083 0.187 Uiso 1 1 calc R . . O7 O 0.3817(2) 0.2385(2) 0.34655(14) 0.1314(18) Uani 1 1 d . . . Zn1 Zn 0.23673(2) 0.82908(3) 0.397734(14) 0.03946(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(2) 0.044(2) 0.038(2) -0.0054(16) 0.0094(17) 0.0055(17) C2 0.053(2) 0.0370(17) 0.0405(19) -0.0015(16) 0.0089(17) 0.0046(16) C3 0.043(2) 0.0389(17) 0.0392(18) 0.0023(15) 0.0118(16) 0.0000(15) C4 0.066(2) 0.0421(19) 0.038(2) -0.0002(16) 0.0008(18) -0.0016(18) C5 0.069(2) 0.0377(18) 0.047(2) 0.0014(17) 0.0077(19) 0.0041(18) C6 0.0454(19) 0.0319(16) 0.0365(17) 0.0015(14) 0.0111(15) -0.0003(15) C7 0.054(2) 0.0397(17) 0.0450(19) -0.0023(16) 0.0094(17) -0.0060(16) C8 0.061(2) 0.0332(17) 0.047(2) -0.0010(15) 0.0165(17) -0.0074(16) C9 0.053(2) 0.0333(17) 0.0408(19) 0.0031(15) 0.0125(17) -0.0002(15) C10 0.0424(19) 0.0379(17) 0.0379(18) -0.0040(15) 0.0116(15) -0.0047(15) C11 0.045(2) 0.0293(16) 0.0413(18) 0.0010(14) 0.0147(16) -0.0027(14) C12 0.081(2) 0.0427(19) 0.052(2) -0.0020(17) 0.0230(19) -0.0167(19) C13 0.088(3) 0.058(2) 0.086(3) -0.015(2) 0.036(2) -0.026(2) C14 0.114(4) 0.088(3) 0.107(3) -0.030(3) 0.052(3) -0.049(3) C15 0.154(4) 0.061(3) 0.104(3) 0.013(3) 0.032(3) -0.011(3) C16 0.120(3) 0.048(2) 0.080(3) 0.004(2) 0.009(3) -0.015(2) C17 0.052(2) 0.0347(17) 0.0328(18) -0.0004(14) 0.0072(17) -0.0058(16) C18 0.046(2) 0.0372(17) 0.0365(18) 0.0003(15) 0.0023(16) -0.0019(15) C19 0.048(2) 0.0340(16) 0.0354(17) -0.0050(14) 0.0129(16) 0.0003(15) C20 0.049(2) 0.0427(17) 0.0344(17) 0.0008(15) 0.0107(16) 0.0026(16) C21 0.048(2) 0.0392(17) 0.0409(19) -0.0018(15) 0.0113(17) 0.0024(16) C22 0.049(2) 0.0388(17) 0.0406(19) -0.0006(15) 0.0136(16) -0.0017(16) C23 0.043(2) 0.0334(17) 0.0359(18) -0.0028(14) 0.0062(16) 0.0019(15) C24 0.050(2) 0.058(2) 0.0358(19) 0.0030(17) 0.0094(18) 0.0015(18) C25 0.046(2) 0.053(2) 0.040(2) 0.0011(17) 0.0050(18) 0.0020(18) C26 0.049(2) 0.079(2) 0.040(2) 0.0089(19) 0.0132(19) -0.003(2) C27 0.045(2) 0.070(2) 0.045(2) 0.0071(19) 0.0073(18) -0.0026(19) C28 0.052(2) 0.0495(19) 0.0399(19) 0.0015(16) 0.0164(17) 0.0073(17) C29 0.058(2) 0.056(2) 0.048(2) 0.0022(18) 0.0157(19) 0.0113(19) C30 0.060(3) 0.065(2) 0.060(2) 0.008(2) 0.019(2) 0.021(2) C31 0.060(3) 0.084(3) 0.076(3) 0.015(2) 0.012(2) 0.000(2) C32 0.056(2) 0.067(2) 0.061(2) 0.018(2) 0.012(2) 0.006(2) C33 0.047(2) 0.044(2) 0.043(2) -0.0039(18) 0.0023(19) -0.0055(19) C34 0.044(2) 0.0320(18) 0.045(2) -0.0007(16) 0.0083(18) -0.0030(16) C35 0.050(2) 0.0316(19) 0.080(3) -0.0015(19) -0.007(2) -0.0061(18) C36 0.056(3) 0.037(2) 0.083(3) 0.003(2) -0.005(2) 0.0029(18) C37 0.055(2) 0.0379(19) 0.046(2) 0.0025(17) 0.0142(19) 0.0060(18) C38 0.048(2) 0.0317(17) 0.044(2) 0.0004(15) 0.0123(17) 0.0035(16) C39 0.051(2) 0.047(2) 0.064(2) -0.0078(18) 0.016(2) -0.0027(18) C40 0.066(2) 0.0408(19) 0.070(2) -0.0142(18) 0.015(2) -0.0151(19) C41 0.066(2) 0.0313(18) 0.052(2) 0.0024(16) 0.020(2) 0.0031(18) C42 0.057(2) 0.0392(18) 0.053(2) 0.0011(17) 0.0160(18) 0.0032(17) C43 0.054(2) 0.0366(18) 0.051(2) -0.0030(16) 0.0124(19) -0.0037(17) C44 0.111(3) 0.042(2) 0.083(3) -0.003(2) 0.046(3) -0.001(3) N1 0.047(2) 0.0389(17) 0.0350(17) -0.0022(14) 0.0116(14) 0.0035(14) N2 0.044(2) 0.0403(16) 0.0446(19) 0.0000(14) 0.0144(16) -0.0036(14) N3 0.053(2) 0.087(3) 0.071(3) 0.012(2) 0.013(2) 0.023(2) N4 0.211(6) 0.067(3) 0.110(4) -0.017(3) 0.087(4) -0.072(3) O1 0.0640(19) 0.0482(14) 0.0351(15) 0.0052(11) 0.0051(13) -0.0217(13) O2 0.0512(18) 0.0478(15) 0.0715(19) -0.0034(14) -0.0036(15) -0.0114(13) O3 0.053(2) 0.0672(18) 0.088(2) -0.0181(16) -0.0133(17) 0.0129(15) O4 0.0649(19) 0.0363(14) 0.083(2) -0.0183(14) 0.0159(17) 0.0000(13) O5 0.059(2) 0.0537(17) 0.095(2) -0.0059(15) 0.0154(18) 0.0148(15) O6 0.117(3) 0.0513(19) 0.216(5) -0.054(3) 0.065(3) -0.016(2) O7 0.139(4) 0.080(2) 0.137(3) -0.027(2) -0.019(3) 0.067(2) Zn1 0.0403(3) 0.0345(2) 0.0407(3) -0.00124(19) 0.00756(19) 0.00275(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.335(4) . ? C1 C2 1.385(4) . ? C1 H1 0.9300 . ? C2 C3 1.381(4) . ? C2 H2 0.9300 . ? C3 C4 1.389(4) . ? C3 C6 1.489(4) . ? C4 C5 1.378(4) . ? C4 H4 0.9300 . ? C5 N1 1.342(4) . ? C5 H5 0.9300 . ? C6 C7 1.389(4) . ? C6 C11 1.399(4) . ? C7 C8 1.392(4) . ? C7 H7 0.9300 . ? C8 C9 1.383(4) . ? C8 C12 1.491(5) . ? C9 C10 1.374(4) . ? C9 H9 0.9300 . ? C10 C11 1.382(4) . ? C10 O1 1.390(3) . ? C11 H11 0.9300 . ? C12 C16 1.361(5) . ? C12 C13 1.370(5) . ? C13 C14 1.376(6) . ? C13 H13 0.9300 . ? C14 N4 1.309(6) . ? C14 H14 0.9300 . ? C15 N4 1.288(7) . ? C15 C16 1.410(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.352(5) . ? C17 C22 1.374(4) . ? C17 O1 1.405(4) . ? C18 C19 1.402(5) . ? C18 H18 0.9300 . ? C19 C20 1.403(5) . ? C19 C23 1.472(5) . ? C20 C21 1.373(5) . ? C20 H20 0.9300 . ? C21 C22 1.408(5) . ? C21 C28 1.489(5) . ? C22 H22 0.9300 . ? C23 C27 1.389(5) . ? C23 C24 1.394(5) . ? C24 C25 1.358(5) . ? C24 H24 0.9300 . ? C25 N2 1.341(4) . ? C25 H25 0.9300 . ? C26 N2 1.335(4) . ? C26 C27 1.363(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.381(5) . ? C28 C32 1.385(5) . ? C29 C30 1.378(5) . ? C29 H29 0.9300 . ? C30 N3 1.327(5) . ? C30 H30 0.9300 . ? C31 N3 1.319(5) . ? C31 C32 1.375(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O3 1.226(4) . ? C33 O2 1.271(4) . ? C33 C34 1.492(5) . ? C34 C36 1.377(4) . ? C34 C35 1.379(5) . ? C35 C36 1.371(5) 5_676 ? C35 H35 0.9300 . ? C36 C35 1.371(5) 5_676 ? C36 H36 0.9300 . ? C37 O5 1.223(4) . ? C37 O4 1.285(4) . ? C37 C38 1.504(5) . ? C38 C43 1.367(5) . ? C38 C39 1.377(4) . ? C39 C40 1.389(5) . ? C39 H39 0.9300 . ? C40 C41 1.368(5) . ? C40 H40 0.9300 . ? C41 C42 1.371(5) . ? C41 C44 1.514(5) . ? C42 C43 1.380(5) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 O7 1.209(6) . ? C44 O6 1.236(5) . ? N1 Zn1 2.054(3) . ? N2 Zn1 2.050(3) 6_575 ? O2 Zn1 1.924(2) . ? O4 Zn1 1.932(2) . ? O6 H6A 0.8200 . ? Zn1 N2 2.050(3) 6_576 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.6(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 116.0(3) . . ? C2 C3 C6 121.4(3) . . ? C4 C3 C6 122.6(3) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? N1 C5 C4 122.9(3) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C7 C6 C11 118.8(3) . . ? C7 C6 C3 120.7(3) . . ? C11 C6 C3 120.4(3) . . ? C6 C7 C8 121.4(3) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? C9 C8 C7 119.1(3) . . ? C9 C8 C12 120.2(3) . . ? C7 C8 C12 120.7(3) . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 121.8(3) . . ? C9 C10 O1 123.3(3) . . ? C11 C10 O1 114.9(3) . . ? C10 C11 C6 119.2(3) . . ? C10 C11 H11 120.4 . . ? C6 C11 H11 120.4 . . ? C16 C12 C13 116.8(4) . . ? C16 C12 C8 121.3(4) . . ? C13 C12 C8 121.9(4) . . ? C12 C13 C14 120.2(5) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? N4 C14 C13 123.0(5) . . ? N4 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? N4 C15 C16 123.8(5) . . ? N4 C15 H15 118.1 . . ? C16 C15 H15 118.1 . . ? C12 C16 C15 118.5(5) . . ? C12 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C18 C17 C22 122.5(3) . . ? C18 C17 O1 122.9(3) . . ? C22 C17 O1 114.5(4) . . ? C17 C18 C19 121.0(3) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C20 116.8(4) . . ? C18 C19 C23 121.7(3) . . ? C20 C19 C23 121.4(3) . . ? C21 C20 C19 121.7(3) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 119.9(3) . . ? C20 C21 C28 121.0(3) . . ? C22 C21 C28 119.0(4) . . ? C17 C22 C21 117.8(4) . . ? C17 C22 H22 121.1 . . ? C21 C22 H22 121.1 . . ? C27 C23 C24 114.3(4) . . ? C27 C23 C19 121.2(3) . . ? C24 C23 C19 124.5(3) . . ? C25 C24 C23 121.4(4) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? N2 C25 C24 123.5(4) . . ? N2 C25 H25 118.3 . . ? C24 C25 H25 118.3 . . ? N2 C26 C27 123.8(4) . . ? N2 C26 H26 118.1 . . ? C27 C26 H26 118.1 . . ? C26 C27 C23 121.2(4) . . ? C26 C27 H27 119.4 . . ? C23 C27 H27 119.4 . . ? C29 C28 C32 116.9(4) . . ? C29 C28 C21 122.1(4) . . ? C32 C28 C21 121.0(3) . . ? C28 C29 C30 118.5(4) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? N3 C30 C29 125.1(4) . . ? N3 C30 H30 117.5 . . ? C29 C30 H30 117.5 . . ? N3 C31 C32 124.2(4) . . ? N3 C31 H31 117.9 . . ? C32 C31 H31 117.9 . . ? C31 C32 C28 119.6(4) . . ? C31 C32 H32 120.2 . . ? C28 C32 H32 120.2 . . ? O3 C33 O2 123.0(3) . . ? O3 C33 C34 120.7(3) . . ? O2 C33 C34 116.4(3) . . ? C36 C34 C35 116.8(3) . . ? C36 C34 C33 121.6(3) . . ? C35 C34 C33 121.6(3) . . ? C36 C35 C34 121.7(3) 5_676 . ? C36 C35 H35 119.1 5_676 . ? C34 C35 H35 119.1 . . ? C35 C36 C34 121.5(3) 5_676 . ? C35 C36 H36 119.3 5_676 . ? C34 C36 H36 119.3 . . ? O5 C37 O4 124.7(3) . . ? O5 C37 C38 120.5(3) . . ? O4 C37 C38 114.8(4) . . ? C43 C38 C39 118.7(3) . . ? C43 C38 C37 121.0(3) . . ? C39 C38 C37 120.3(4) . . ? C38 C39 C40 119.8(4) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 121.1(3) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C41 C40 119.0(3) . . ? C42 C41 C44 119.5(4) . . ? C40 C41 C44 121.5(4) . . ? C41 C42 C43 120.0(4) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C38 C43 C42 121.4(3) . . ? C38 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? O7 C44 O6 123.9(5) . . ? O7 C44 C41 119.2(5) . . ? O6 C44 C41 116.8(5) . . ? C1 N1 C5 116.5(3) . . ? C1 N1 Zn1 121.3(2) . . ? C5 N1 Zn1 122.2(2) . . ? C26 N2 C25 115.7(4) . . ? C26 N2 Zn1 118.3(3) . 6_575 ? C25 N2 Zn1 125.7(3) . 6_575 ? C31 N3 C30 115.7(4) . . ? C15 N4 C14 117.5(5) . . ? C10 O1 C17 118.6(3) . . ? C33 O2 Zn1 122.1(2) . . ? C37 O4 Zn1 119.5(3) . . ? C44 O6 H6A 109.5 . . ? O2 Zn1 O4 98.70(11) . . ? O2 Zn1 N2 111.29(12) . 6_576 ? O4 Zn1 N2 113.57(12) . 6_576 ? O2 Zn1 N1 120.22(11) . . ? O4 Zn1 N1 110.85(11) . . ? N2 Zn1 N1 102.72(11) 6_576 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.8(6) . . . . ? C1 C2 C3 C4 2.4(6) . . . . ? C1 C2 C3 C6 -175.5(3) . . . . ? C2 C3 C4 C5 -1.7(6) . . . . ? C6 C3 C4 C5 176.1(4) . . . . ? C3 C4 C5 N1 -0.6(6) . . . . ? C2 C3 C6 C7 23.8(6) . . . . ? C4 C3 C6 C7 -154.0(4) . . . . ? C2 C3 C6 C11 -159.1(4) . . . . ? C4 C3 C6 C11 23.2(6) . . . . ? C11 C6 C7 C8 1.7(6) . . . . ? C3 C6 C7 C8 179.0(4) . . . . ? C6 C7 C8 C9 -1.7(6) . . . . ? C6 C7 C8 C12 178.0(4) . . . . ? C7 C8 C9 C10 -0.8(6) . . . . ? C12 C8 C9 C10 179.5(4) . . . . ? C8 C9 C10 C11 3.2(6) . . . . ? C8 C9 C10 O1 -179.9(3) . . . . ? C9 C10 C11 C6 -3.1(6) . . . . ? O1 C10 C11 C6 179.7(3) . . . . ? C7 C6 C11 C10 0.6(5) . . . . ? C3 C6 C11 C10 -176.6(3) . . . . ? C9 C8 C12 C16 27.6(6) . . . . ? C7 C8 C12 C16 -152.1(4) . . . . ? C9 C8 C12 C13 -153.6(4) . . . . ? C7 C8 C12 C13 26.7(6) . . . . ? C16 C12 C13 C14 2.9(7) . . . . ? C8 C12 C13 C14 -176.0(4) . . . . ? C12 C13 C14 N4 -5.8(9) . . . . ? C13 C12 C16 C15 0.9(7) . . . . ? C8 C12 C16 C15 179.8(5) . . . . ? N4 C15 C16 C12 -2.4(9) . . . . ? C22 C17 C18 C19 2.9(5) . . . . ? O1 C17 C18 C19 178.5(3) . . . . ? C17 C18 C19 C20 0.7(5) . . . . ? C17 C18 C19 C23 -177.2(3) . . . . ? C18 C19 C20 C21 -3.3(5) . . . . ? C23 C19 C20 C21 174.6(3) . . . . ? C19 C20 C21 C22 2.6(5) . . . . ? C19 C20 C21 C28 -178.5(3) . . . . ? C18 C17 C22 C21 -3.6(5) . . . . ? O1 C17 C22 C21 -179.5(3) . . . . ? C20 C21 C22 C17 0.9(5) . . . . ? C28 C21 C22 C17 -178.0(3) . . . . ? C18 C19 C23 C27 172.1(3) . . . . ? C20 C19 C23 C27 -5.7(5) . . . . ? C18 C19 C23 C24 -5.0(5) . . . . ? C20 C19 C23 C24 177.2(3) . . . . ? C27 C23 C24 C25 -3.0(5) . . . . ? C19 C23 C24 C25 174.2(3) . . . . ? C23 C24 C25 N2 0.4(6) . . . . ? N2 C26 C27 C23 0.2(6) . . . . ? C24 C23 C27 C26 2.8(5) . . . . ? C19 C23 C27 C26 -174.6(3) . . . . ? C20 C21 C28 C29 -40.3(5) . . . . ? C22 C21 C28 C29 138.5(4) . . . . ? C20 C21 C28 C32 138.5(4) . . . . ? C22 C21 C28 C32 -42.6(5) . . . . ? C32 C28 C29 C30 0.8(6) . . . . ? C21 C28 C29 C30 179.7(4) . . . . ? C28 C29 C30 N3 -0.2(7) . . . . ? N3 C31 C32 C28 0.0(7) . . . . ? C29 C28 C32 C31 -0.7(6) . . . . ? C21 C28 C32 C31 -179.6(4) . . . . ? O3 C33 C34 C36 -1.0(6) . . . . ? O2 C33 C34 C36 179.2(4) . . . . ? O3 C33 C34 C35 176.6(4) . . . . ? O2 C33 C34 C35 -3.3(6) . . . . ? C36 C34 C35 C36 0.0(7) . . . 5_676 ? C33 C34 C35 C36 -177.7(4) . . . 5_676 ? C35 C34 C36 C35 0.0(7) . . . 5_676 ? C33 C34 C36 C35 177.7(4) . . . 5_676 ? O5 C37 C38 C43 176.7(4) . . . . ? O4 C37 C38 C43 -1.8(5) . . . . ? O5 C37 C38 C39 -5.2(6) . . . . ? O4 C37 C38 C39 176.3(4) . . . . ? C43 C38 C39 C40 0.5(6) . . . . ? C37 C38 C39 C40 -177.6(4) . . . . ? C38 C39 C40 C41 0.4(6) . . . . ? C39 C40 C41 C42 0.4(6) . . . . ? C39 C40 C41 C44 177.2(4) . . . . ? C40 C41 C42 C43 -2.1(6) . . . . ? C44 C41 C42 C43 -179.0(4) . . . . ? C39 C38 C43 C42 -2.2(6) . . . . ? C37 C38 C43 C42 175.9(3) . . . . ? C41 C42 C43 C38 3.0(6) . . . . ? C42 C41 C44 O7 14.3(7) . . . . ? C40 C41 C44 O7 -162.5(5) . . . . ? C42 C41 C44 O6 -165.4(5) . . . . ? C40 C41 C44 O6 17.8(7) . . . . ? C2 C1 N1 C5 -1.6(6) . . . . ? C2 C1 N1 Zn1 178.4(3) . . . . ? C4 C5 N1 C1 2.2(6) . . . . ? C4 C5 N1 Zn1 -177.8(3) . . . . ? C27 C26 N2 C25 -2.9(5) . . . . ? C27 C26 N2 Zn1 171.7(3) . . . 6_575 ? C24 C25 N2 C26 2.6(5) . . . . ? C24 C25 N2 Zn1 -171.5(3) . . . 6_575 ? C32 C31 N3 C30 0.6(7) . . . . ? C29 C30 N3 C31 -0.5(7) . . . . ? C16 C15 N4 C14 -0.2(10) . . . . ? C13 C14 N4 C15 4.3(9) . . . . ? C9 C10 O1 C17 23.9(5) . . . . ? C11 C10 O1 C17 -159.0(3) . . . . ? C18 C17 O1 C10 51.5(5) . . . . ? C22 C17 O1 C10 -132.6(3) . . . . ? O3 C33 O2 Zn1 4.8(6) . . . . ? C34 C33 O2 Zn1 -175.4(2) . . . . ? O5 C37 O4 Zn1 3.3(6) . . . . ? C38 C37 O4 Zn1 -178.2(2) . . . . ? C33 O2 Zn1 O4 162.8(3) . . . . ? C33 O2 Zn1 N2 -77.6(3) . . . 6_576 ? C33 O2 Zn1 N1 42.4(4) . . . . ? C37 O4 Zn1 O2 168.4(3) . . . . ? C37 O4 Zn1 N2 50.5(3) . . . 6_576 ? C37 O4 Zn1 N1 -64.5(3) . . . . ? C1 N1 Zn1 O2 -47.4(3) . . . . ? C5 N1 Zn1 O2 132.6(3) . . . . ? C1 N1 Zn1 O4 -161.5(3) . . . . ? C5 N1 Zn1 O4 18.5(3) . . . . ? C1 N1 Zn1 N2 76.8(3) . . . 6_576 ? C5 N1 Zn1 N2 -103.2(3) . . . 6_576 ? 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 0.500 0.070 0.250 127 29 ' ' 2 0.500 -0.070 0.750 127 29 ' ' 3 0.358 0.125 0.041 8 0 ' ' 4 0.642 0.125 0.459 8 0 ' ' 5 0.000 0.430 0.750 127 29 ' ' 6 1.000 0.570 0.250 127 29 ' ' 7 0.858 0.375 0.541 8 0 ' ' 8 0.142 0.375 0.959 8 0 ' ' 9 0.858 0.625 0.041 8 0 ' ' 10 0.142 0.625 0.459 8 0 ' ' 11 0.358 0.875 0.541 8 0 ' ' 12 0.642 0.875 0.959 8 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.496 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.060 data_2 _database_code_depnum_ccdc_archive 'CCDC 893949' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H36 N4 O12 Zn2' _chemical_formula_sum 'C48 H36 N4 O12 Zn2' _chemical_formula_weight 991.55 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_hall ' -P1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.239(10) _cell_length_b 14.746(6) _cell_length_c 16.5153(16) _cell_angle_alpha 93.9830(15) _cell_angle_beta 101.4790(15) _cell_angle_gamma 105.6240(15) _cell_volume 2333(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2197 _cell_measurement_theta_min 2.391 _cell_measurement_theta_max 20.257 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7493 _exptl_absorpt_correction_T_max 0.7948 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12665 _diffrn_reflns_av_R_equivalents 0.1087 _diffrn_reflns_av_sigmaI/netI 0.1779 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8085 _reflns_number_gt 3639 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8085 _refine_ls_number_parameters 583 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1603 _refine_ls_R_factor_gt 0.0965 _refine_ls_wR_factor_ref 0.2239 _refine_ls_wR_factor_gt 0.2092 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.021 _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 N4 N 0.8890(8) 0.2767(6) 0.3852(4) 0.053(2) Uani 1 1 d . . . N2 N 0.1035(7) 0.8192(5) 0.4584(4) 0.0460(18) Uani 1 1 d D . . C1 C 0.0380(11) 0.2765(7) 0.1679(6) 0.059(3) Uani 1 1 d . . . H1 H -0.0131 0.2252 0.1891 0.071 Uiso 1 1 calc R . . C2 C 0.1703(11) 0.3218(7) 0.2105(6) 0.059(3) Uani 1 1 d . . . H2 H 0.2067 0.3004 0.2591 0.070 Uiso 1 1 calc R . . C3 C 0.2507(9) 0.3979(7) 0.1836(5) 0.050(2) Uani 1 1 d . . . C4 C 0.1862(10) 0.4249(7) 0.1124(6) 0.060(3) Uani 1 1 d . . . H4 H 0.2361 0.4763 0.0908 0.072 Uiso 1 1 calc R . . C5 C 0.0523(10) 0.3797(8) 0.0719(6) 0.066(3) Uani 1 1 d . . . H5 H 0.0114 0.4033 0.0258 0.079 Uiso 1 1 calc R . . C6 C 0.3948(9) 0.4472(7) 0.2245(6) 0.050(2) Uani 1 1 d . . . C7 C 0.4844(9) 0.3972(7) 0.2566(5) 0.049(2) Uani 1 1 d . . . H7 H 0.4508 0.3317 0.2541 0.059 Uiso 1 1 calc R . . C8 C 0.6233(10) 0.4420(7) 0.2924(5) 0.047(2) Uani 1 1 d . . . C9 C 0.6734(9) 0.5380(7) 0.2981(5) 0.047(2) Uani 1 1 d . . . H9 H 0.7667 0.5682 0.3223 0.056 Uiso 1 1 calc R . . C10 C 0.5864(10) 0.5903(6) 0.2682(5) 0.046(2) Uani 1 1 d . . . C11 C 0.4465(9) 0.5465(7) 0.2309(5) 0.052(2) Uani 1 1 d . . . H11 H 0.3883 0.5825 0.2106 0.063 Uiso 1 1 calc R . . C12 C 0.7173(9) 0.3841(6) 0.3257(5) 0.042(2) Uani 1 1 d . . . C13 C 0.6645(10) 0.2977(7) 0.3511(6) 0.054(2) Uani 1 1 d . . . H13 H 0.5695 0.2743 0.3480 0.065 Uiso 1 1 calc R . . C14 C 0.7529(11) 0.2459(7) 0.3813(6) 0.062(3) Uani 1 1 d . . . H14 H 0.7167 0.1880 0.3994 0.074 Uiso 1 1 calc R . . C15 C 0.9422(10) 0.3585(7) 0.3631(6) 0.059(3) Uani 1 1 d . . . H15 H 1.0378 0.3804 0.3679 0.071 Uiso 1 1 calc R . . C16 C 0.8605(10) 0.4127(7) 0.3331(6) 0.061(3) Uani 1 1 d . . . H16 H 0.9015 0.4708 0.3169 0.073 Uiso 1 1 calc R . . C17 C 0.5668(8) 0.7497(6) 0.2676(5) 0.043(2) Uani 1 1 d . . . C18 C 0.6025(9) 0.8217(6) 0.2196(5) 0.049(2) Uani 1 1 d . . . H18 H 0.6659 0.8201 0.1867 0.059 Uiso 1 1 calc R . . C19 C 0.5434(8) 0.8970(6) 0.2205(5) 0.040(2) Uani 1 1 d . . . C20 C 0.4447(9) 0.8949(6) 0.2681(5) 0.046(2) Uani 1 1 d . . . H20 H 0.4051 0.9447 0.2699 0.055 Uiso 1 1 calc R . . C21 C 0.4044(9) 0.8198(7) 0.3128(5) 0.047(2) Uani 1 1 d . . . C22 C 0.4678(9) 0.7458(6) 0.3126(5) 0.044(2) Uani 1 1 d . . . H22 H 0.4426 0.6954 0.3427 0.053 Uiso 1 1 calc R . . C23 C 0.2956(9) 0.8180(7) 0.3636(5) 0.047(2) Uani 1 1 d . . . C24 C 0.2885(9) 0.8987(7) 0.4039(6) 0.052(2) Uani 1 1 d . . . H24 H 0.3498 0.9567 0.3999 0.062 Uiso 1 1 calc R . . C25 C 0.1915(10) 0.8955(7) 0.4507(6) 0.050(2) Uani 1 1 d . . . H25 H 0.1899 0.9522 0.4784 0.060 Uiso 1 1 calc R . . C26 C 0.1028(9) 0.7357(6) 0.4156(5) 0.048(2) Uani 1 1 d . . . H26 H 0.0377 0.6793 0.4194 0.057 Uiso 1 1 calc R . . C27 C 0.1976(9) 0.7348(6) 0.3673(5) 0.046(2) Uani 1 1 d . . . H27 H 0.1954 0.6784 0.3374 0.055 Uiso 1 1 calc R . . C28 C 0.5889(9) 0.9762(6) 0.1749(5) 0.046(2) Uani 1 1 d . . . C29 C 0.6325(13) 0.9645(8) 0.1022(7) 0.084(4) Uani 1 1 d . . . H29 H 0.6212 0.9035 0.0773 0.101 Uiso 1 1 calc R . . C30 C 0.6915(12) 1.0400(8) 0.0662(7) 0.079(4) Uani 1 1 d . . . H30 H 0.7282 1.0291 0.0205 0.095 Uiso 1 1 calc R . . C31 C 0.6456(11) 1.1407(7) 0.1577(6) 0.066(3) Uani 1 1 d . . . H31 H 0.6438 1.2013 0.1762 0.079 Uiso 1 1 calc R . . C32 C 0.5920(12) 1.0683(7) 0.1993(6) 0.068(3) Uani 1 1 d . . . H32 H 0.5568 1.0812 0.2452 0.081 Uiso 1 1 calc R . . C33 C -0.1199(10) 0.2025(8) -0.1116(5) 0.057(3) Uani 1 1 d . . . C34 C -0.0756(10) 0.1355(7) -0.1664(5) 0.051(2) Uani 1 1 d . . . C35 C 0.0101(10) 0.1703(7) -0.2183(5) 0.054(2) Uani 1 1 d . . . H35 H 0.0477 0.2353 -0.2172 0.064 Uiso 1 1 calc R . . C36 C 0.0399(9) 0.1047(8) -0.2737(5) 0.056(3) Uani 1 1 d . . . H36 H 0.0955 0.1276 -0.3103 0.068 Uiso 1 1 calc R . . C37 C -0.0102(9) 0.0096(7) -0.2750(5) 0.045(2) Uani 1 1 d . . . C38 C -0.0913(11) -0.0234(7) -0.2207(6) 0.062(3) Uani 1 1 d . . . H38 H -0.1249 -0.0886 -0.2205 0.074 Uiso 1 1 calc R . . C39 C -0.1248(11) 0.0383(8) -0.1658(6) 0.068(3) Uani 1 1 d . . . H39 H -0.1796 0.0144 -0.1291 0.082 Uiso 1 1 calc R . . C40 C 0.0179(11) -0.0572(8) -0.3366(5) 0.053(3) Uani 1 1 d . . . C45 C -0.3597(10) -0.4906(7) -0.4909(6) 0.055(2) Uani 1 1 d . . . H45 H -0.2656 -0.4855 -0.4845 0.065 Uiso 1 1 calc R . . C46 C -0.4043(9) -0.4110(6) -0.4997(5) 0.044(2) Uani 1 1 d . . . C47 C -0.3080(10) -0.3173(7) -0.4988(6) 0.052(2) Uani 1 1 d . . . C48 C -0.5460(11) -0.4214(7) -0.5086(6) 0.058(3) Uani 1 1 d . . . H48 H -0.5782 -0.3685 -0.5143 0.069 Uiso 1 1 calc R . . N1 N -0.0220(8) 0.3016(5) 0.0975(5) 0.0501(19) Uani 1 1 d . . . N3 N 0.6997(8) 1.1306(6) 0.0933(4) 0.054(2) Uani 1 1 d . . . O1 O 0.1092(7) -0.0289(5) -0.3769(4) 0.0681(19) Uani 1 1 d . . . O2 O -0.0592(8) -0.1413(5) -0.3472(4) 0.0628(19) Uani 1 1 d . . . O3 O -0.0843(8) 0.2878(5) -0.1116(4) 0.076(2) Uani 1 1 d . . . O4 O -0.1921(7) 0.1589(5) -0.0603(4) 0.0631(18) Uani 1 1 d . . . O5 O -0.3565(7) -0.2500(5) -0.5079(5) 0.078(2) Uani 1 1 d . . . O6 O -0.1801(7) -0.3117(4) -0.4881(4) 0.0555(16) Uani 1 1 d . . . O9 O 0.6457(6) 0.6865(5) 0.2712(4) 0.0612(18) Uani 1 1 d . . . O1W O -0.1433(7) -0.1082(5) -0.5211(4) 0.069(2) Uani 1 1 d . . . H1W2 H -0.2197 -0.1069 -0.4960 0.104 Uiso 1 1 d R . . H1W5 H -0.1020 -0.0846 -0.5657 0.104 Uiso 1 1 d R . . Zn1 Zn -0.21739(11) 0.23801(8) 0.03032(6) 0.0475(3) Uani 1 1 d . . . Zn2 Zn -0.02256(11) -0.19408(7) -0.45408(6) 0.0462(3) Uani 1 1 d . . . O3W O 0.9843(11) 0.5652(7) 0.2084(6) 0.139(4) Uani 1 1 d . . . H3W2 H 1.0099 0.6274 0.1916 0.209 Uiso 1 1 d R . . H3W3 H 0.9629 0.5181 0.1608 0.209 Uiso 1 1 d R . . O2W O 0.3791(10) 0.1380(7) 0.3674(7) 0.138(4) Uani 1 1 d . . . H2W1 H 0.2799 0.1105 0.3532 0.207 Uiso 1 1 d R . . H2W2 H 0.4108 0.1518 0.4269 0.207 Uiso 1 1 d R . . O7 O -0.3564(8) 0.3022(6) -0.0002(5) 0.092 Uani 1 1 d . . . C50 C -0.4228(17) 0.4372(10) 0.0218(9) 0.090(5) Uani 1 1 d . . . O8 O -0.2398(8) 0.3963(6) 0.1127(5) 0.090 Uani 1 1 d . . . C49 C -0.3326(16) 0.3727(10) 0.0428(7) 0.102(5) Uani 1 1 d . . . C51 C -0.5367(16) 0.4101(10) -0.0416(8) 0.098(4) Uani 1 1 d . . . H51 H -0.5623 0.3497 -0.0714 0.117 Uiso 1 1 calc R . . C52 C -0.3811(15) 0.5262(13) 0.0638(9) 0.120(6) Uani 1 1 d . . . H52 H -0.3008 0.5457 0.1062 0.144 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 N4 0.043(5) 0.062(6) 0.055(5) 0.006(4) 0.011(4) 0.020(4) N2 0.046(5) 0.044(5) 0.057(5) 0.020(4) 0.015(4) 0.023(4) C1 0.059(7) 0.057(7) 0.065(7) 0.026(5) 0.012(6) 0.020(6) C2 0.066(7) 0.049(7) 0.059(6) 0.023(5) 0.004(6) 0.017(6) C3 0.048(6) 0.061(7) 0.046(5) 0.013(5) 0.010(5) 0.021(5) C4 0.063(7) 0.068(7) 0.042(5) 0.020(5) 0.009(5) 0.007(6) C5 0.050(7) 0.093(9) 0.050(6) 0.027(6) -0.003(5) 0.020(6) C6 0.047(6) 0.053(7) 0.055(6) 0.011(5) 0.013(5) 0.019(5) C7 0.053(6) 0.044(6) 0.052(6) 0.011(5) 0.011(5) 0.017(5) C8 0.054(6) 0.048(6) 0.043(5) 0.007(4) 0.015(5) 0.018(5) C9 0.044(6) 0.049(6) 0.051(5) 0.009(5) 0.016(5) 0.017(5) C10 0.054(6) 0.038(6) 0.048(5) 0.007(4) 0.014(5) 0.013(5) C11 0.044(6) 0.065(7) 0.054(6) 0.021(5) 0.008(5) 0.025(5) C12 0.041(6) 0.043(6) 0.043(5) 0.004(4) 0.004(4) 0.015(5) C13 0.044(6) 0.056(7) 0.062(6) 0.019(5) 0.006(5) 0.016(5) C14 0.070(8) 0.053(7) 0.067(7) 0.027(5) 0.014(6) 0.020(6) C15 0.053(6) 0.066(7) 0.069(7) 0.043(6) 0.025(5) 0.019(6) C16 0.067(7) 0.053(7) 0.071(7) 0.030(5) 0.021(6) 0.023(6) C17 0.035(5) 0.049(6) 0.054(6) 0.016(5) 0.014(4) 0.022(4) C18 0.049(6) 0.052(6) 0.049(6) 0.013(5) 0.016(5) 0.016(5) C19 0.040(5) 0.037(5) 0.040(5) 0.004(4) 0.009(4) 0.006(4) C20 0.058(6) 0.036(5) 0.049(5) 0.012(4) 0.019(5) 0.017(5) C21 0.044(5) 0.058(6) 0.034(5) 0.011(4) 0.002(4) 0.010(5) C22 0.053(6) 0.038(5) 0.046(5) 0.019(4) 0.008(5) 0.019(5) C23 0.046(6) 0.058(7) 0.042(5) 0.014(5) 0.012(4) 0.022(5) C24 0.060(6) 0.043(6) 0.052(6) 0.007(5) 0.019(5) 0.010(5) C25 0.065(7) 0.037(6) 0.050(6) 0.006(4) 0.019(5) 0.013(5) C26 0.053(6) 0.034(6) 0.054(6) 0.020(5) 0.008(5) 0.008(5) C27 0.058(6) 0.041(6) 0.047(5) 0.010(4) 0.021(5) 0.021(5) C28 0.048(6) 0.054(6) 0.039(5) 0.009(4) 0.012(4) 0.015(5) C29 0.142(11) 0.063(8) 0.070(7) 0.017(6) 0.070(8) 0.034(8) C30 0.125(10) 0.065(8) 0.075(8) 0.016(6) 0.065(8) 0.040(7) C31 0.107(9) 0.051(7) 0.056(6) 0.014(5) 0.034(6) 0.034(6) C32 0.106(9) 0.060(7) 0.059(6) 0.013(5) 0.048(6) 0.038(7) C33 0.072(7) 0.062(8) 0.034(5) 0.001(5) 0.013(5) 0.016(6) C34 0.063(6) 0.051(6) 0.046(5) 0.015(5) 0.026(5) 0.015(5) C35 0.072(7) 0.049(6) 0.041(5) 0.003(4) 0.023(5) 0.012(5) C36 0.054(6) 0.090(8) 0.037(5) 0.015(5) 0.018(5) 0.034(6) C37 0.056(6) 0.045(6) 0.037(5) 0.011(4) 0.009(5) 0.019(5) C38 0.092(8) 0.037(6) 0.063(6) 0.012(5) 0.032(6) 0.017(6) C39 0.098(8) 0.068(8) 0.058(6) 0.023(5) 0.049(6) 0.031(7) C40 0.067(7) 0.063(8) 0.031(5) 0.003(5) -0.002(5) 0.032(6) C45 0.048(6) 0.055(7) 0.067(6) 0.014(5) 0.023(5) 0.017(5) C46 0.052(6) 0.039(6) 0.043(5) 0.008(4) 0.014(4) 0.013(5) C47 0.053(7) 0.057(7) 0.054(6) 0.017(5) 0.006(5) 0.032(6) C48 0.077(8) 0.045(6) 0.058(6) 0.012(5) 0.020(6) 0.025(6) N1 0.051(5) 0.046(5) 0.056(5) 0.013(4) 0.015(4) 0.015(4) N3 0.067(5) 0.063(6) 0.039(4) 0.011(4) 0.014(4) 0.027(5) O1 0.075(5) 0.092(6) 0.051(4) 0.014(4) 0.025(4) 0.039(4) O2 0.100(6) 0.056(5) 0.048(4) 0.015(3) 0.028(4) 0.037(4) O3 0.130(7) 0.046(5) 0.061(4) 0.012(4) 0.042(5) 0.024(5) O4 0.087(5) 0.065(5) 0.048(4) 0.007(3) 0.030(4) 0.030(4) O5 0.058(5) 0.060(5) 0.116(6) 0.023(4) 0.013(4) 0.018(4) O6 0.058(4) 0.053(4) 0.061(4) 0.018(3) 0.015(3) 0.021(4) O9 0.046(4) 0.052(5) 0.095(5) 0.019(4) 0.018(4) 0.024(4) O1W 0.070(5) 0.085(5) 0.077(5) 0.042(4) 0.031(4) 0.043(4) Zn1 0.0571(7) 0.0501(7) 0.0432(6) 0.0151(5) 0.0137(5) 0.0249(6) Zn2 0.0512(7) 0.0482(7) 0.0467(6) 0.0130(5) 0.0176(5) 0.0204(6) O3W 0.227(12) 0.103(8) 0.089(6) 0.041(6) 0.055(8) 0.029(8) O2W 0.117(8) 0.114(8) 0.167(10) -0.002(7) 0.054(8) -0.004(6) O7 0.116 0.118 0.074 0.015 0.000 0.103 C50 0.148(13) 0.104(11) 0.080(9) 0.046(8) 0.079(10) 0.094(11) O8 0.111 0.122 0.074 0.016 0.000 0.106 C49 0.195(15) 0.104(10) 0.047(7) 0.034(7) 0.053(9) 0.085(11) C51 0.146(13) 0.102(11) 0.076(9) 0.026(8) 0.027(9) 0.082(10) C52 0.143(13) 0.193(18) 0.089(10) 0.067(11) 0.047(9) 0.133(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 N4 C15 1.293(11) . ? N4 C14 1.331(11) . ? N4 Zn2 2.263(7) 2_655 ? N2 C25 1.270(10) . ? N2 C26 1.374(11) . ? N2 Zn2 2.107(6) 1_566 ? C1 N1 1.329(11) . ? C1 C2 1.357(13) . ? C1 H1 0.9300 . ? C2 C3 1.360(12) . ? C2 H2 0.9300 . ? C3 C4 1.370(12) . ? C3 C6 1.455(13) . ? C4 C5 1.361(13) . ? C4 H4 0.9300 . ? C5 N1 1.345(12) . ? C5 H5 0.9300 . ? C6 C7 1.374(11) . ? C6 C11 1.406(12) . ? C7 C8 1.383(12) . ? C7 H7 0.9300 . ? C8 C9 1.359(12) . ? C8 C12 1.501(11) . ? C9 C10 1.371(11) . ? C9 H9 0.9300 . ? C10 O9 1.377(10) . ? C10 C11 1.394(12) . ? C11 H11 0.9300 . ? C12 C13 1.374(11) . ? C12 C16 1.390(12) . ? C13 C14 1.378(12) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.354(12) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.363(10) . ? C17 C18 1.383(11) . ? C17 O9 1.385(9) . ? C18 C19 1.400(11) . ? C18 H18 0.9300 . ? C19 C20 1.394(11) . ? C19 C28 1.455(11) . ? C20 C21 1.391(11) . ? C20 H20 0.9300 . ? C21 C22 1.412(11) . ? C21 C23 1.518(11) . ? C22 H22 0.9300 . ? C23 C24 1.350(12) . ? C23 C27 1.373(12) . ? C24 C25 1.368(11) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.376(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.377(12) . ? C28 C32 1.381(12) . ? C29 C30 1.353(13) . ? C29 H29 0.9300 . ? C30 N3 1.354(12) . ? C30 H30 0.9300 . ? C31 N3 1.311(10) . ? C31 C32 1.360(13) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O3 1.212(11) . ? C33 O4 1.321(11) . ? C33 C34 1.510(13) . ? C34 C35 1.373(11) . ? C34 C39 1.388(13) . ? C35 C36 1.419(12) . ? C35 H35 0.9300 . ? C36 C37 1.353(13) . ? C36 H36 0.9300 . ? C37 C38 1.366(12) . ? C37 C40 1.490(12) . ? C38 C39 1.395(13) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 O1 1.252(11) . ? C40 O2 1.257(11) . ? C45 C46 1.375(12) . ? C45 C48 1.391(12) 2_444 ? C45 H45 0.9300 . ? C46 C48 1.394(12) . ? C46 C47 1.463(13) . ? C47 O5 1.229(10) . ? C47 O6 1.265(10) . ? C48 C45 1.391(12) 2_444 ? C48 H48 0.9300 . ? N1 Zn1 2.018(8) . ? N3 Zn1 2.041(8) 1_665 ? O2 Zn2 2.022(6) . ? O4 Zn1 1.935(6) . ? O6 Zn2 1.981(7) . ? O1W Zn2 2.202(6) . ? O1W H1W2 0.9600 . ? O1W H1W5 0.9600 . ? Zn1 O7 1.919(6) . ? Zn1 N3 2.041(8) 1_445 ? Zn2 N2 2.107(6) 1_544 ? Zn2 N4 2.263(7) 2_655 ? O3W H3W2 0.9600 . ? O3W H3W3 0.9600 . ? O2W H2W1 0.9600 . ? O2W H2W2 0.9600 . ? O7 C49 1.157(13) . ? C50 C51 1.350(18) . ? C50 C52 1.356(19) . ? C50 C49 1.505(16) . ? O8 C49 1.298(14) . ? C51 C52 1.442(15) 2_465 ? C51 H51 0.9300 . ? C52 C51 1.442(15) 2_465 ? C52 H52 0.9300 . ? 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 C15 N4 C14 120.1(8) . . ? C15 N4 Zn2 122.1(6) . 2_655 ? C14 N4 Zn2 116.7(6) . 2_655 ? C25 N2 C26 118.4(7) . . ? C25 N2 Zn2 125.0(6) . 1_566 ? C26 N2 Zn2 115.9(6) . 1_566 ? N1 C1 C2 123.3(9) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 121.6(9) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C2 C3 C4 114.5(9) . . ? C2 C3 C6 124.3(9) . . ? C4 C3 C6 121.2(9) . . ? C5 C4 C3 122.9(9) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? N1 C5 C4 121.1(9) . . ? N1 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C11 118.3(9) . . ? C7 C6 C3 120.6(9) . . ? C11 C6 C3 121.1(8) . . ? C6 C7 C8 121.7(9) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 119.9(8) . . ? C9 C8 C12 120.4(9) . . ? C7 C8 C12 119.7(8) . . ? C8 C9 C10 120.0(9) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 O9 117.0(8) . . ? C9 C10 C11 121.0(9) . . ? O9 C10 C11 121.8(8) . . ? C10 C11 C6 119.0(8) . . ? C10 C11 H11 120.5 . . ? C6 C11 H11 120.5 . . ? C13 C12 C16 115.6(8) . . ? C13 C12 C8 120.8(8) . . ? C16 C12 C8 123.6(8) . . ? C14 C13 C12 119.7(9) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? N4 C14 C13 121.6(9) . . ? N4 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? N4 C15 C16 120.9(9) . . ? N4 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C12 122.1(9) . . ? C15 C16 H16 119.0 . . ? C12 C16 H16 119.0 . . ? C22 C17 C18 122.0(7) . . ? C22 C17 O9 122.7(7) . . ? C18 C17 O9 115.1(7) . . ? C17 C18 C19 120.2(8) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 118.2(8) . . ? C20 C19 C28 121.7(7) . . ? C18 C19 C28 120.1(8) . . ? C21 C20 C19 121.1(8) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 119.6(8) . . ? C20 C21 C23 120.5(8) . . ? C22 C21 C23 119.8(8) . . ? C17 C22 C21 118.7(8) . . ? C17 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C27 117.7(8) . . ? C24 C23 C21 121.0(9) . . ? C27 C23 C21 121.2(8) . . ? C23 C24 C25 120.2(9) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? N2 C25 C24 123.5(8) . . ? N2 C25 H25 118.3 . . ? C24 C25 H25 118.3 . . ? N2 C26 C27 120.5(8) . . ? N2 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C23 C27 C26 119.5(8) . . ? C23 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C29 C28 C32 114.1(8) . . ? C29 C28 C19 121.9(8) . . ? C32 C28 C19 124.0(8) . . ? C30 C29 C28 121.4(10) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? N3 C30 C29 123.3(9) . . ? N3 C30 H30 118.4 . . ? C29 C30 H30 118.4 . . ? N3 C31 C32 124.2(9) . . ? N3 C31 H31 117.9 . . ? C32 C31 H31 117.9 . . ? C31 C32 C28 121.3(9) . . ? C31 C32 H32 119.3 . . ? C28 C32 H32 119.3 . . ? O3 C33 O4 124.2(9) . . ? O3 C33 C34 122.7(9) . . ? O4 C33 C34 112.9(9) . . ? C35 C34 C39 119.9(8) . . ? C35 C34 C33 120.3(9) . . ? C39 C34 C33 119.8(8) . . ? C34 C35 C36 118.5(9) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C37 C36 C35 122.0(8) . . ? C37 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? C36 C37 C38 118.6(8) . . ? C36 C37 C40 120.5(9) . . ? C38 C37 C40 120.9(9) . . ? C37 C38 C39 121.5(9) . . ? C37 C38 H38 119.2 . . ? C39 C38 H38 119.2 . . ? C34 C39 C38 119.4(9) . . ? C34 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? O1 C40 O2 123.2(9) . . ? O1 C40 C37 121.1(10) . . ? O2 C40 C37 115.7(9) . . ? C46 C45 C48 120.7(9) . 2_444 ? C46 C45 H45 119.7 . . ? C48 C45 H45 119.7 2_444 . ? C45 C46 C48 117.9(8) . . ? C45 C46 C47 122.2(9) . . ? C48 C46 C47 119.9(8) . . ? O5 C47 O6 124.9(10) . . ? O5 C47 C46 118.1(9) . . ? O6 C47 C46 117.0(8) . . ? C45 C48 C46 121.4(8) 2_444 . ? C45 C48 H48 119.3 2_444 . ? C46 C48 H48 119.3 . . ? C1 N1 C5 116.4(9) . . ? C1 N1 Zn1 125.9(7) . . ? C5 N1 Zn1 117.6(6) . . ? C31 N3 C30 115.1(8) . . ? C31 N3 Zn1 125.1(6) . 1_665 ? C30 N3 Zn1 119.7(6) . 1_665 ? C40 O2 Zn2 101.7(6) . . ? C33 O4 Zn1 116.9(6) . . ? C47 O6 Zn2 126.1(6) . . ? C10 O9 C17 121.7(7) . . ? Zn2 O1W H1W2 109.3 . . ? Zn2 O1W H1W5 109.6 . . ? H1W2 O1W H1W5 141.1 . . ? O7 Zn1 O4 115.1(3) . . ? O7 Zn1 N1 124.5(4) . . ? O4 Zn1 N1 104.0(3) . . ? O7 Zn1 N3 106.6(3) . 1_445 ? O4 Zn1 N3 96.8(3) . 1_445 ? N1 Zn1 N3 106.0(3) . 1_445 ? O6 Zn2 O2 101.6(3) . . ? O6 Zn2 N2 109.7(3) . 1_544 ? O2 Zn2 N2 148.7(3) . 1_544 ? O6 Zn2 O1W 92.4(3) . . ? O2 Zn2 O1W 88.2(2) . . ? N2 Zn2 O1W 90.6(2) 1_544 . ? O6 Zn2 N4 90.2(3) . 2_655 ? O2 Zn2 N4 92.2(2) . 2_655 ? N2 Zn2 N4 87.6(2) 1_544 2_655 ? O1W Zn2 N4 177.2(3) . 2_655 ? H3W2 O3W H3W3 109.5 . . ? H2W1 O2W H2W2 109.5 . . ? C49 O7 Zn1 112.0(9) . . ? C51 C50 C52 120.4(12) . . ? C51 C50 C49 120.9(13) . . ? C52 C50 C49 118.5(15) . . ? O7 C49 O8 123.7(11) . . ? O7 C49 C50 118.8(13) . . ? O8 C49 C50 117.2(11) . . ? C50 C51 C52 120.6(13) . 2_465 ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 2_465 . ? C50 C52 C51 119.0(14) . 2_465 ? C50 C52 H52 120.5 . . ? C51 C52 H52 120.5 2_465 . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.920 _refine_diff_density_min -1.622 _refine_diff_density_rms 0.125 data_ql3 _database_code_depnum_ccdc_archive 'CCDC 893950' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H32 Cd N4 O8' _chemical_formula_sum 'C40 H32 Cd N4 O8' _chemical_formula_weight 809.10 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2461(16) _cell_length_b 21.754(3) _cell_length_c 11.6482(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.942(2) _cell_angle_gamma 90.00 _cell_volume 3590.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12407 _cell_measurement_theta_min 2.348 _cell_measurement_theta_max 28.264 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19852 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6275 _reflns_number_gt 5520 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+3.4985P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6275 _refine_ls_number_parameters 472 _refine_ls_number_restraints 919 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1385 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6292(3) 0.4029(2) 1.2640(4) 0.0450(9) Uani 1 1 d U . . H1 H 0.6036 0.3729 1.3083 0.054 Uiso 1 1 calc R . . C2 C 0.7120(3) 0.3900(2) 1.2175(4) 0.0449(9) Uani 1 1 d U . . H2 H 0.7409 0.3519 1.2302 0.054 Uiso 1 1 calc R . . C3 C 0.7522(3) 0.4341(2) 1.1516(4) 0.0379(8) Uani 1 1 d U . . C4 C 0.7066(3) 0.4903(2) 1.1394(4) 0.0421(9) Uani 1 1 d U . . H4 H 0.7321 0.5219 1.0989 0.051 Uiso 1 1 calc R . . C5 C 0.6230(3) 0.4991(2) 1.1875(4) 0.0424(9) Uani 1 1 d U . . H5 H 0.5925 0.5368 1.1767 0.051 Uiso 1 1 calc R . . C6 C 0.8392(3) 0.4217(2) 1.0951(4) 0.0402(8) Uani 1 1 d U . . C7 C 0.9059(3) 0.3797(2) 1.1451(4) 0.0444(9) Uani 1 1 d U . . H7 H 0.8958 0.3608 1.2144 0.053 Uiso 1 1 calc R . . C8 C 0.9867(3) 0.3655(2) 1.0933(4) 0.0478(9) Uani 1 1 d U . . C9 C 1.0024(3) 0.3951(2) 0.9909(4) 0.0454(9) Uani 1 1 d U . . H9 H 1.0563 0.3867 0.9550 0.054 Uiso 1 1 calc R . . C10 C 0.9369(3) 0.4372(2) 0.9434(4) 0.0410(9) Uani 1 1 d U . . C11 C 0.8562(3) 0.4504(2) 0.9922(4) 0.0403(8) Uani 1 1 d U . . H11 H 0.8129 0.4783 0.9570 0.048 Uiso 1 1 calc R . . C12 C 1.0515(3) 0.3179(3) 1.1480(5) 0.0530(10) Uani 1 1 d U . . C13 C 1.0200(4) 0.2726(3) 1.2180(6) 0.0667(12) Uani 1 1 d U . . H13 H 0.9567 0.2715 1.2310 0.080 Uiso 1 1 calc R . . C14 C 1.0811(4) 0.2294(3) 1.2686(6) 0.0769(14) Uani 1 1 d U . . H14 H 1.0575 0.2004 1.3168 0.092 Uiso 1 1 calc R . . C15 C 1.2009(5) 0.2697(4) 1.1898(7) 0.0880(15) Uani 1 1 d U . . H15 H 1.2650 0.2702 1.1806 0.106 Uiso 1 1 calc R . . C16 C 1.1450(4) 0.3161(3) 1.1339(6) 0.0760(13) Uani 1 1 d U . . H16 H 1.1714 0.3450 1.0880 0.091 Uiso 1 1 calc R . . C17 C 0.9638(3) 0.4378(2) 0.7432(4) 0.0422(9) Uani 1 1 d U . . C18 C 0.8970(3) 0.3954(2) 0.6996(4) 0.0439(9) Uani 1 1 d U . . H18 H 0.8459 0.3862 0.7403 0.053 Uiso 1 1 calc R . . C19 C 0.9064(3) 0.3666(2) 0.5943(4) 0.0466(9) Uani 1 1 d U . . C20 C 0.9832(3) 0.3822(3) 0.5345(4) 0.0492(9) Uani 1 1 d U . . H20 H 0.9895 0.3637 0.4637 0.059 Uiso 1 1 calc R . . C21 C 1.0506(3) 0.4248(3) 0.5785(4) 0.0499(9) Uani 1 1 d U . . C22 C 1.0403(3) 0.4527(3) 0.6853(4) 0.0470(9) Uani 1 1 d U . . H22 H 1.0848 0.4810 0.7167 0.056 Uiso 1 1 calc R . . C23 C 0.8385(3) 0.3182(2) 0.5472(4) 0.0499(10) Uani 1 1 d U . . C24 C 0.7461(4) 0.3160(3) 0.5727(6) 0.0648(12) Uani 1 1 d U . . H24 H 0.7226 0.3467 0.6173 0.078 Uiso 1 1 calc R . . C25 C 0.6887(4) 0.2682(3) 0.5322(6) 0.0719(13) Uani 1 1 d U . . H25 H 0.6273 0.2678 0.5524 0.086 Uiso 1 1 calc R . . C26 C 0.8031(4) 0.2256(3) 0.4407(5) 0.0635(12) Uani 1 1 d U . . H26 H 0.8239 0.1948 0.3940 0.076 Uiso 1 1 calc R . . C27 C 0.8656(4) 0.2710(3) 0.4785(5) 0.0570(11) Uani 1 1 d U . . H27 H 0.9269 0.2701 0.4576 0.068 Uiso 1 1 calc R . . C28 C 1.1342(3) 0.4391(3) 0.5167(5) 0.0538(10) Uani 1 1 d U . . C29 C 1.2051(5) 0.4726(3) 0.5579(6) 0.0784(14) Uani 1 1 d U . . H29 H 1.2035 0.4902 0.6304 0.094 Uiso 1 1 calc R . . C30 C 1.2834(5) 0.4834(4) 0.4986(6) 0.0818(15) Uani 1 1 d U . . H30 H 1.3305 0.5089 0.5334 0.098 Uiso 1 1 calc R . . C31 C 1.2182(5) 0.4385(4) 0.3483(6) 0.0847(15) Uani 1 1 d U . . H31 H 1.2188 0.4283 0.2709 0.102 Uiso 1 1 calc R . . C32 C 1.1357(5) 0.4281(4) 0.3989(5) 0.0783(13) Uani 1 1 d U . . H32 H 1.0819 0.4139 0.3548 0.094 Uiso 1 1 calc R . . C33 C 0.4146(3) 0.35416(18) 1.1343(3) 0.0339(8) Uani 1 1 d U . . C34 C 0.4367(3) 0.28700(19) 1.1177(3) 0.0344(8) Uani 1 1 d U . . C35 C 0.4758(4) 0.2525(2) 1.2112(4) 0.0422(9) Uani 1 1 d U . . H35 H 0.4882 0.2710 1.2832 0.051 Uiso 1 1 calc R . . C36 C 0.4966(4) 0.1907(2) 1.1981(4) 0.0433(9) Uani 1 1 d U . . H36 H 0.5226 0.1681 1.2612 0.052 Uiso 1 1 calc R . . C37 C 0.4787(3) 0.16292(18) 1.0919(3) 0.0339(8) Uani 1 1 d U . . C38 C 0.4371(3) 0.19609(19) 0.9990(4) 0.0395(9) Uani 1 1 d U . . H38 H 0.4221 0.1768 0.9282 0.047 Uiso 1 1 calc R . . C39 C 0.4174(3) 0.2583(2) 1.0113(4) 0.0406(9) Uani 1 1 d U . . H39 H 0.3912 0.2808 0.9480 0.049 Uiso 1 1 calc R . . C40 C 0.5086(3) 0.09657(18) 1.0765(3) 0.0334(8) Uani 1 1 d U . . Cd1 Cd 0.434518(19) 0.468440(12) 1.31644(2) 0.02764(14) Uani 1 1 d . . . N1 N 0.5841(3) 0.45591(18) 1.2490(3) 0.0394(8) Uani 1 1 d . . . N2 N 1.1715(4) 0.2264(3) 1.2531(6) 0.094(2) Uani 1 1 d . . . N3 N 0.7142(3) 0.2229(2) 0.4669(5) 0.0701(14) Uani 1 1 d . . . N4 N 1.2947(3) 0.4614(2) 0.4020(4) 0.050 Uani 1 1 d . . . O1 O 0.4064(2) 0.37154(12) 1.2347(2) 0.0382(7) Uani 1 1 d . . . O2 O 0.4064(3) 0.38800(14) 1.0455(3) 0.0498(8) Uani 1 1 d . . . O3 O 0.5341(3) 0.06793(15) 1.1675(3) 0.0576(9) Uani 1 1 d . . . O4 O 0.5108(2) 0.07645(14) 0.9779(3) 0.0452(8) Uani 1 1 d . . . O5 O 0.9533(3) 0.47014(14) 0.8436(3) 0.0457(8) Uani 1 1 d . . . O1W O 0.3602(2) 0.49821(15) 1.1393(3) 0.0447(7) Uani 1 1 d . . . H1W1 H 0.3176 0.4664 1.1096 0.067 Uiso 1 1 d R . . H1W2 H 0.4067 0.5051 1.0866 0.067 Uiso 1 1 d R . . O3W O 0.5853(3) 0.11067(18) 0.4452(3) 0.0646(10) Uani 1 1 d . . . H3WD H 0.5708 0.1311 0.5030 0.078 Uiso 1 1 d R . . H3WB H 0.6394 0.0945 0.4609 0.097 Uiso 1 1 d R . . O2W O 0.7686(3) 0.6270(2) 0.1051(5) 0.0868(14) Uani 1 1 d . . . H2WA H 0.7185 0.6416 0.0696 0.130 Uiso 1 1 d R . . H2WB H 0.8129 0.6532 0.1049 0.130 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(2) 0.050(2) 0.044(2) 0.0075(18) 0.0168(17) 0.0002(18) C2 0.042(2) 0.050(2) 0.043(2) 0.0039(18) 0.0106(17) 0.0054(18) C3 0.0332(17) 0.048(2) 0.0337(18) -0.0009(16) 0.0096(15) 0.0018(16) C4 0.043(2) 0.048(2) 0.0383(19) 0.0045(17) 0.0160(16) -0.0009(18) C5 0.042(2) 0.046(2) 0.042(2) 0.0049(18) 0.0180(17) 0.0041(18) C6 0.0345(17) 0.0495(19) 0.0382(17) -0.0007(16) 0.0119(15) -0.0003(16) C7 0.0378(17) 0.056(2) 0.0410(18) 0.0024(17) 0.0114(15) 0.0005(17) C8 0.0373(18) 0.057(2) 0.0497(19) 0.0003(18) 0.0089(16) 0.0005(17) C9 0.0364(18) 0.055(2) 0.0462(19) -0.0057(17) 0.0132(16) -0.0012(17) C10 0.0392(18) 0.047(2) 0.0387(18) -0.0059(16) 0.0131(15) -0.0067(16) C11 0.0385(18) 0.0475(19) 0.0365(18) -0.0015(16) 0.0115(15) -0.0019(16) C12 0.0407(19) 0.063(2) 0.056(2) 0.002(2) 0.0092(18) 0.0015(18) C13 0.050(2) 0.073(3) 0.078(3) 0.014(2) 0.013(2) 0.004(2) C14 0.059(3) 0.082(3) 0.090(3) 0.021(3) 0.010(2) 0.008(3) C15 0.059(3) 0.099(3) 0.108(3) 0.026(3) 0.015(3) 0.012(3) C16 0.054(2) 0.086(3) 0.091(3) 0.020(2) 0.016(2) 0.007(2) C17 0.0401(18) 0.050(2) 0.0395(18) -0.0035(16) 0.0190(15) -0.0036(16) C18 0.0373(17) 0.052(2) 0.0459(19) -0.0008(17) 0.0193(15) -0.0041(16) C19 0.0394(18) 0.055(2) 0.0474(19) -0.0037(17) 0.0134(16) -0.0061(17) C20 0.0416(18) 0.064(2) 0.0446(19) -0.0096(17) 0.0197(16) -0.0130(17) C21 0.0412(18) 0.067(2) 0.0451(19) -0.0120(18) 0.0230(16) -0.0135(18) C22 0.0400(18) 0.060(2) 0.043(2) -0.0097(18) 0.0176(16) -0.0113(18) C23 0.0413(19) 0.057(2) 0.053(2) -0.0046(18) 0.0145(17) -0.0073(18) C24 0.049(2) 0.064(2) 0.083(3) -0.021(2) 0.018(2) -0.004(2) C25 0.048(2) 0.074(3) 0.095(3) -0.020(3) 0.016(2) -0.012(2) C26 0.056(2) 0.064(3) 0.072(3) -0.018(2) 0.013(2) -0.007(2) C27 0.046(2) 0.065(2) 0.062(2) -0.013(2) 0.0173(19) -0.009(2) C28 0.042(2) 0.070(2) 0.0538(18) -0.0138(19) 0.0239(17) -0.0188(19) C29 0.064(3) 0.113(3) 0.063(3) -0.042(2) 0.030(2) -0.037(2) C30 0.064(3) 0.121(3) 0.066(3) -0.050(3) 0.036(2) -0.041(3) C31 0.070(3) 0.120(3) 0.069(3) -0.035(3) 0.032(2) -0.038(3) C32 0.067(2) 0.112(3) 0.0600(19) -0.029(2) 0.026(2) -0.031(2) C33 0.046(2) 0.0263(18) 0.0299(19) 0.0000(15) 0.0079(16) 0.0020(16) C34 0.050(2) 0.0261(18) 0.0287(17) -0.0018(14) 0.0113(16) 0.0027(16) C35 0.068(2) 0.0309(19) 0.0280(18) -0.0036(15) 0.0050(17) 0.0069(17) C36 0.067(2) 0.0324(19) 0.0305(18) 0.0012(15) 0.0051(17) 0.0065(18) C37 0.049(2) 0.0254(18) 0.0296(17) 0.0005(14) 0.0136(15) 0.0028(16) C38 0.061(2) 0.0291(19) 0.0285(18) -0.0048(15) 0.0064(17) 0.0053(17) C39 0.060(2) 0.0310(19) 0.0305(19) -0.0020(15) 0.0036(17) 0.0082(17) C40 0.046(2) 0.0247(18) 0.0311(19) -0.0018(15) 0.0125(16) -0.0006(16) Cd1 0.0331(2) 0.0231(2) 0.0288(2) -0.00050(9) 0.01349(13) -0.00126(10) N1 0.039(2) 0.044(2) 0.038(2) 0.0029(16) 0.0154(16) 0.0007(16) N2 0.054(3) 0.094(4) 0.134(6) 0.045(4) 0.011(3) 0.010(3) N3 0.054(3) 0.064(3) 0.093(4) -0.017(3) 0.010(2) -0.009(2) N4 0.040 0.059 0.053 -0.012 0.022 -0.006 O1 0.0583(18) 0.0229(14) 0.0355(16) -0.0054(11) 0.0154(13) 0.0015(13) O2 0.084(2) 0.0313(16) 0.0344(16) 0.0006(13) 0.0079(16) 0.0132(16) O3 0.105(3) 0.0289(17) 0.0392(18) 0.0027(13) 0.0103(18) 0.0190(18) O4 0.063(2) 0.0336(17) 0.0400(17) -0.0119(13) 0.0094(14) 0.0059(14) O5 0.060(2) 0.0371(19) 0.0450(18) -0.0032(13) 0.0304(16) -0.0048(14) O1W 0.0555(19) 0.0393(18) 0.0390(17) 0.0008(13) 0.0030(14) 0.0069(14) O3W 0.082(3) 0.054(2) 0.059(2) -0.0096(18) 0.010(2) 0.009(2) O2W 0.070(3) 0.063(3) 0.124(4) -0.006(3) -0.003(3) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.322(6) . ? C1 C2 1.378(6) . ? C1 H1 0.9300 . ? C2 C3 1.389(6) . ? C2 H2 0.9300 . ? C3 C4 1.385(7) . ? C3 C6 1.487(6) . ? C4 C5 1.380(6) . ? C4 H4 0.9300 . ? C5 N1 1.336(6) . ? C5 H5 0.9300 . ? C6 C7 1.401(7) . ? C6 C11 1.394(6) . ? C7 C8 1.388(6) . ? C7 H7 0.9300 . ? C8 C9 1.394(7) . ? C8 C12 1.487(7) . ? C9 C10 1.380(7) . ? C9 H9 0.9300 . ? C10 C11 1.365(6) . ? C10 O5 1.405(6) . ? C11 H11 0.9300 . ? C12 C16 1.359(7) . ? C12 C13 1.383(8) . ? C13 C14 1.373(8) . ? C13 H13 0.9300 . ? C14 N2 1.320(8) . ? C14 H14 0.9300 . ? C15 N2 1.292(9) . ? C15 C16 1.403(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.379(6) . ? C17 C18 1.384(7) . ? C17 O5 1.386(6) . ? C18 C19 1.397(7) . ? C18 H18 0.9300 . ? C19 C20 1.398(6) . ? C19 C23 1.496(7) . ? C20 C21 1.394(7) . ? C20 H20 0.9300 . ? C21 C22 1.405(7) . ? C21 C28 1.487(6) . ? C22 H22 0.9300 . ? C23 C27 1.381(7) . ? C23 C24 1.380(7) . ? C24 C25 1.375(8) . ? C24 H24 0.9300 . ? C25 N3 1.319(8) . ? C25 H25 0.9300 . ? C26 N3 1.334(7) . ? C26 C27 1.373(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.295(8) . ? C28 C32 1.395(8) . ? C29 C30 1.391(8) . ? C29 H29 0.9300 . ? C30 N4 1.249(7) . ? C30 H30 0.9300 . ? C31 N4 1.299(8) . ? C31 C32 1.387(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O1 1.247(5) . ? C33 O2 1.265(5) . ? C33 C34 1.511(6) . ? C34 C35 1.391(6) . ? C34 C39 1.389(6) . ? C35 C36 1.387(6) . ? C35 H35 0.9300 . ? C36 C37 1.377(6) . ? C36 H36 0.9300 . ? C37 C38 1.383(6) . ? C37 C40 1.521(6) . ? C38 C39 1.393(6) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 O4 1.233(5) . ? C40 O3 1.250(5) . ? Cd1 O3 2.214(3) 2_657 ? Cd1 O4 2.291(3) 4_566 ? Cd1 O1W 2.313(3) . ? Cd1 N4 2.322(4) 1_456 ? Cd1 O1 2.330(3) . ? Cd1 N1 2.362(4) . ? N4 Cd1 2.322(4) 1_654 ? O3 Cd1 2.214(3) 2_647 ? O4 Cd1 2.291(3) 4_565 ? O1W H1W1 0.9600 . ? O1W H1W2 0.9600 . ? O3W H3WD 0.8500 . ? O3W H3WB 0.8500 . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.4(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C1 C2 C3 119.6(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 116.8(4) . . ? C2 C3 C6 122.0(4) . . ? C4 C3 C6 121.2(4) . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 122.9(4) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C7 C6 C11 118.6(4) . . ? C7 C6 C3 119.6(4) . . ? C11 C6 C3 121.8(4) . . ? C8 C7 C6 121.4(4) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 118.9(4) . . ? C7 C8 C12 118.3(4) . . ? C9 C8 C12 122.8(4) . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C11 C10 C9 122.4(4) . . ? C11 C10 O5 117.1(4) . . ? C9 C10 O5 120.4(4) . . ? C10 C11 C6 119.5(4) . . ? C10 C11 H11 120.3 . . ? C6 C11 H11 120.3 . . ? C16 C12 C13 115.7(5) . . ? C16 C12 C8 122.8(5) . . ? C13 C12 C8 121.6(4) . . ? C14 C13 C12 120.7(5) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? N2 C14 C13 123.9(6) . . ? N2 C14 H14 118.0 . . ? C13 C14 H14 118.0 . . ? N2 C15 C16 126.0(6) . . ? N2 C15 H15 117.0 . . ? C16 C15 H15 117.0 . . ? C12 C16 C15 118.7(6) . . ? C12 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C22 C17 C18 121.7(4) . . ? C22 C17 O5 117.0(4) . . ? C18 C17 O5 121.1(4) . . ? C17 C18 C19 119.8(4) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 118.6(4) . . ? C18 C19 C23 121.4(4) . . ? C20 C19 C23 119.9(4) . . ? C21 C20 C19 121.6(4) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 118.8(4) . . ? C20 C21 C28 121.1(4) . . ? C22 C21 C28 120.1(4) . . ? C17 C22 C21 119.5(4) . . ? C17 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C27 C23 C24 115.5(5) . . ? C27 C23 C19 121.7(4) . . ? C24 C23 C19 122.8(5) . . ? C25 C24 C23 119.9(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? N3 C25 C24 125.1(5) . . ? N3 C25 H25 117.5 . . ? C24 C25 H25 117.5 . . ? N3 C26 C27 123.9(5) . . ? N3 C26 H26 118.0 . . ? C27 C26 H26 118.0 . . ? C23 C27 C26 120.6(5) . . ? C23 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C29 C28 C32 111.8(5) . . ? C29 C28 C21 124.8(5) . . ? C32 C28 C21 122.3(5) . . ? C28 C29 C30 123.1(6) . . ? C28 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? N4 C30 C29 124.6(6) . . ? N4 C30 H30 117.7 . . ? C29 C30 H30 117.7 . . ? N4 C31 C32 124.4(6) . . ? N4 C31 H31 117.8 . . ? C32 C31 H31 117.8 . . ? C28 C32 C31 119.3(6) . . ? C28 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? O1 C33 O2 125.5(4) . . ? O1 C33 C34 117.0(3) . . ? O2 C33 C34 117.5(3) . . ? C35 C34 C39 118.8(4) . . ? C35 C34 C33 119.6(4) . . ? C39 C34 C33 121.6(4) . . ? C34 C35 C36 120.6(4) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C37 C36 C35 120.2(4) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 119.9(4) . . ? C36 C37 C40 119.7(4) . . ? C38 C37 C40 120.4(4) . . ? C37 C38 C39 120.1(4) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C34 120.4(4) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? O4 C40 O3 125.4(4) . . ? O4 C40 C37 118.7(4) . . ? O3 C40 C37 115.7(3) . . ? O3 Cd1 O4 105.83(13) 2_657 4_566 ? O3 Cd1 O1W 82.62(13) 2_657 . ? O4 Cd1 O1W 170.57(11) 4_566 . ? O3 Cd1 N4 101.69(15) 2_657 1_456 ? O4 Cd1 N4 88.56(15) 4_566 1_456 ? O1W Cd1 N4 93.86(15) . 1_456 ? O3 Cd1 O1 160.63(11) 2_657 . ? O4 Cd1 O1 89.80(11) 4_566 . ? O1W Cd1 O1 81.10(11) . . ? N4 Cd1 O1 89.85(13) 1_456 . ? O3 Cd1 N1 87.68(15) 2_657 . ? O4 Cd1 N1 81.74(13) 4_566 . ? O1W Cd1 N1 94.64(13) . . ? N4 Cd1 N1 168.08(16) 1_456 . ? O1 Cd1 N1 83.24(12) . . ? C1 N1 C5 117.4(4) . . ? C1 N1 Cd1 119.9(3) . . ? C5 N1 Cd1 122.4(3) . . ? C15 N2 C14 114.9(6) . . ? C25 N3 C26 115.0(5) . . ? C30 N4 C31 113.6(5) . . ? C30 N4 Cd1 124.0(4) . 1_654 ? C31 N4 Cd1 122.2(4) . 1_654 ? C33 O1 Cd1 129.0(3) . . ? C40 O3 Cd1 126.7(3) . 2_647 ? C40 O4 Cd1 149.4(3) . 4_565 ? C17 O5 C10 118.7(4) . . ? Cd1 O1W H1W1 109.5 . . ? Cd1 O1W H1W2 109.4 . . ? H1W1 O1W H1W2 109.5 . . ? H3WD O3W H3WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.4(8) . . . . ? C1 C2 C3 C4 1.8(7) . . . . ? C1 C2 C3 C6 -177.3(4) . . . . ? C2 C3 C4 C5 -2.8(7) . . . . ? C6 C3 C4 C5 176.3(4) . . . . ? C3 C4 C5 N1 1.7(7) . . . . ? C2 C3 C6 C7 -29.4(7) . . . . ? C4 C3 C6 C7 151.5(5) . . . . ? C2 C3 C6 C11 149.8(5) . . . . ? C4 C3 C6 C11 -29.2(7) . . . . ? C11 C6 C7 C8 -1.1(7) . . . . ? C3 C6 C7 C8 178.1(4) . . . . ? C6 C7 C8 C9 1.6(7) . . . . ? C6 C7 C8 C12 -176.6(5) . . . . ? C7 C8 C9 C10 -0.6(7) . . . . ? C12 C8 C9 C10 177.6(5) . . . . ? C8 C9 C10 C11 -0.9(7) . . . . ? C8 C9 C10 O5 176.6(4) . . . . ? C9 C10 C11 C6 1.4(7) . . . . ? O5 C10 C11 C6 -176.2(4) . . . . ? C7 C6 C11 C10 -0.4(7) . . . . ? C3 C6 C11 C10 -179.6(4) . . . . ? C7 C8 C12 C16 -154.7(6) . . . . ? C9 C8 C12 C16 27.1(9) . . . . ? C7 C8 C12 C13 24.7(8) . . . . ? C9 C8 C12 C13 -153.5(6) . . . . ? C16 C12 C13 C14 0.0(10) . . . . ? C8 C12 C13 C14 -179.4(6) . . . . ? C12 C13 C14 N2 -1.7(12) . . . . ? C13 C12 C16 C15 0.0(10) . . . . ? C8 C12 C16 C15 179.4(6) . . . . ? N2 C15 C16 C12 1.8(14) . . . . ? C22 C17 C18 C19 0.1(8) . . . . ? O5 C17 C18 C19 175.7(5) . . . . ? C17 C18 C19 C20 -1.0(8) . . . . ? C17 C18 C19 C23 176.8(5) . . . . ? C18 C19 C20 C21 1.1(8) . . . . ? C23 C19 C20 C21 -176.7(5) . . . . ? C19 C20 C21 C22 -0.3(8) . . . . ? C19 C20 C21 C28 177.3(5) . . . . ? C18 C17 C22 C21 0.7(8) . . . . ? O5 C17 C22 C21 -175.1(5) . . . . ? C20 C21 C22 C17 -0.6(8) . . . . ? C28 C21 C22 C17 -178.2(5) . . . . ? C18 C19 C23 C27 -149.8(6) . . . . ? C20 C19 C23 C27 28.0(8) . . . . ? C18 C19 C23 C24 27.6(8) . . . . ? C20 C19 C23 C24 -154.7(6) . . . . ? C27 C23 C24 C25 1.4(9) . . . . ? C19 C23 C24 C25 -176.1(6) . . . . ? C23 C24 C25 N3 -1.2(11) . . . . ? C24 C23 C27 C26 -0.6(9) . . . . ? C19 C23 C27 C26 177.0(5) . . . . ? N3 C26 C27 C23 -0.5(10) . . . . ? C20 C21 C28 C29 -171.7(7) . . . . ? C22 C21 C28 C29 5.8(10) . . . . ? C20 C21 C28 C32 21.7(10) . . . . ? C22 C21 C28 C32 -160.8(7) . . . . ? C32 C28 C29 C30 -14.1(12) . . . . ? C21 C28 C29 C30 178.1(7) . . . . ? C28 C29 C30 N4 -1.6(14) . . . . ? C29 C28 C32 C31 16.3(11) . . . . ? C21 C28 C32 C31 -175.5(7) . . . . ? N4 C31 C32 C28 -4.1(13) . . . . ? O1 C33 C34 C35 -20.3(6) . . . . ? O2 C33 C34 C35 159.4(4) . . . . ? O1 C33 C34 C39 158.6(4) . . . . ? O2 C33 C34 C39 -21.7(6) . . . . ? C39 C34 C35 C36 1.0(7) . . . . ? C33 C34 C35 C36 179.9(4) . . . . ? C34 C35 C36 C37 0.1(8) . . . . ? C35 C36 C37 C38 -2.2(7) . . . . ? C35 C36 C37 C40 175.4(4) . . . . ? C36 C37 C38 C39 3.2(7) . . . . ? C40 C37 C38 C39 -174.4(4) . . . . ? C37 C38 C39 C34 -2.0(7) . . . . ? C35 C34 C39 C38 0.0(7) . . . . ? C33 C34 C39 C38 -178.9(4) . . . . ? C36 C37 C40 O4 -164.8(4) . . . . ? C38 C37 C40 O4 12.8(6) . . . . ? C36 C37 C40 O3 11.5(6) . . . . ? C38 C37 C40 O3 -171.0(4) . . . . ? C2 C1 N1 C5 -1.6(7) . . . . ? C2 C1 N1 Cd1 173.4(4) . . . . ? C4 C5 N1 C1 0.6(7) . . . . ? C4 C5 N1 Cd1 -174.4(4) . . . . ? O3 Cd1 N1 C1 152.8(4) 2_657 . . . ? O4 Cd1 N1 C1 46.4(4) 4_566 . . . ? O1W Cd1 N1 C1 -124.8(4) . . . . ? N4 Cd1 N1 C1 10.6(9) 1_456 . . . ? O1 Cd1 N1 C1 -44.4(4) . . . . ? O3 Cd1 N1 C5 -32.4(4) 2_657 . . . ? O4 Cd1 N1 C5 -138.8(4) 4_566 . . . ? O1W Cd1 N1 C5 50.0(4) . . . . ? N4 Cd1 N1 C5 -174.6(6) 1_456 . . . ? O1 Cd1 N1 C5 130.4(4) . . . . ? C16 C15 N2 C14 -3.3(14) . . . . ? C13 C14 N2 C15 3.2(12) . . . . ? C24 C25 N3 C26 0.1(11) . . . . ? C27 C26 N3 C25 0.8(10) . . . . ? C29 C30 N4 C31 14.7(12) . . . . ? C29 C30 N4 Cd1 -170.8(6) . . . 1_654 ? C32 C31 N4 C30 -11.6(12) . . . . ? C32 C31 N4 Cd1 173.8(6) . . . 1_654 ? O2 C33 O1 Cd1 -27.6(6) . . . . ? C34 C33 O1 Cd1 152.0(3) . . . . ? O3 Cd1 O1 C33 8.1(6) 2_657 . . . ? O4 Cd1 O1 C33 -136.2(4) 4_566 . . . ? O1W Cd1 O1 C33 41.3(4) . . . . ? N4 Cd1 O1 C33 135.2(4) 1_456 . . . ? N1 Cd1 O1 C33 -54.5(4) . . . . ? O4 C40 O3 Cd1 -12.1(7) . . . 2_647 ? C37 C40 O3 Cd1 171.9(3) . . . 2_647 ? O3 C40 O4 Cd1 97.7(7) . . . 4_565 ? C37 C40 O4 Cd1 -86.4(6) . . . 4_565 ? C22 C17 O5 C10 -131.1(5) . . . . ? C18 C17 O5 C10 53.0(6) . . . . ? C11 C10 O5 C17 -121.6(5) . . . . ? C9 C10 O5 C17 60.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.718 _refine_diff_density_min -1.557 _refine_diff_density_rms 0.100 data_4 _database_code_depnum_ccdc_archive 'CCDC 893951' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H30 N4 Ni O7' _chemical_formula_sum 'C40 H30 N4 Ni O7' _chemical_formula_weight 737.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_space_group_name_hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0498(12) _cell_length_b 20.9140(17) _cell_length_c 11.6127(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.684(2) _cell_angle_gamma 90.00 _cell_volume 3400.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10813 _cell_measurement_theta_min 2.394 _cell_measurement_theta_max 28.298 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8434 _exptl_absorpt_correction_T_max 0.8739 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18800 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5990 _reflns_number_gt 4870 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+2.3577P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constra _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5990 _refine_ls_number_parameters 469 _refine_ls_number_restraints 918 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.131 _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 C1 C 0.6196(3) 0.09422(18) 0.7572(3) 0.0331(8) Uani 1 1 d U . . H1 H 0.5953 0.1261 0.8024 0.040 Uiso 1 1 calc R . . C2 C 0.7039(3) 0.10584(19) 0.7086(3) 0.0360(8) Uani 1 1 d U . . H2 H 0.7349 0.1449 0.7204 0.043 Uiso 1 1 calc R . . C3 C 0.7425(3) 0.0590(2) 0.6418(3) 0.0346(8) Uani 1 1 d U . . C4 C 0.6936(3) 0.00160(19) 0.6297(3) 0.0354(8) Uani 1 1 d U . . H4 H 0.7179 -0.0316 0.5876 0.043 Uiso 1 1 calc R . . C5 C 0.6088(3) -0.00627(19) 0.6803(3) 0.0328(8) Uani 1 1 d U . . H5 H 0.5767 -0.0450 0.6705 0.039 Uiso 1 1 calc R . . C6 C 0.8325(3) 0.0716(2) 0.5847(3) 0.0361(7) Uani 1 1 d U . . C7 C 0.8982(3) 0.1151(2) 0.6330(4) 0.0423(8) Uani 1 1 d U . . H7 H 0.8874 0.1340 0.7032 0.051 Uiso 1 1 calc R . . C8 C 0.9803(3) 0.1318(2) 0.5798(4) 0.0455(8) Uani 1 1 d U . . C9 C 0.9979(3) 0.1006(2) 0.4784(4) 0.0425(8) Uani 1 1 d U . . H9 H 1.0532 0.1095 0.4426 0.051 Uiso 1 1 calc R . . C10 C 0.9330(3) 0.0564(2) 0.4304(3) 0.0380(8) Uani 1 1 d U . . C11 C 0.8490(3) 0.0413(2) 0.4809(3) 0.0377(8) Uani 1 1 d U . . H11 H 0.8056 0.0120 0.4467 0.045 Uiso 1 1 calc R . . C12 C 1.0447(3) 0.1819(2) 0.6351(4) 0.0508(9) Uani 1 1 d U . . C13 C 1.0111(4) 0.2262(3) 0.7085(5) 0.0651(11) Uani 1 1 d U . . H13 H 0.9472 0.2252 0.7241 0.078 Uiso 1 1 calc R . . C14 C 1.0702(4) 0.2719(3) 0.7593(6) 0.0764(13) Uani 1 1 d U . . H14 H 1.0449 0.2996 0.8116 0.092 Uiso 1 1 calc R . . C15 C 1.1903(5) 0.2378(4) 0.6692(6) 0.0906(14) Uani 1 1 d U . . H15 H 1.2538 0.2408 0.6528 0.109 Uiso 1 1 calc R . . C16 C 1.1370(4) 0.1884(3) 0.6152(6) 0.0760(12) Uani 1 1 d U . . H16 H 1.1651 0.1604 0.5659 0.091 Uiso 1 1 calc R . . C17 C 0.9634(3) 0.05570(19) 0.2312(3) 0.0362(8) Uani 1 1 d U . . C18 C 0.8948(3) 0.09846(19) 0.1877(3) 0.0379(8) Uani 1 1 d U . . H18 H 0.8415 0.1066 0.2279 0.045 Uiso 1 1 calc R . . C19 C 0.9060(3) 0.12939(19) 0.0833(3) 0.0374(8) Uani 1 1 d U . . C20 C 0.9862(3) 0.11440(19) 0.0245(3) 0.0367(7) Uani 1 1 d U . . H20 H 0.9936 0.1343 -0.0458 0.044 Uiso 1 1 calc R . . C21 C 1.0547(3) 0.07107(19) 0.0669(3) 0.0346(7) Uani 1 1 d U . . C22 C 1.0423(3) 0.04146(19) 0.1737(3) 0.0370(8) Uani 1 1 d U . . H22 H 1.0874 0.0124 0.2050 0.044 Uiso 1 1 calc R . . C23 C 1.1404(3) 0.05697(19) 0.0042(3) 0.0338(8) Uani 1 1 d U . . C24 C 1.2202(3) 0.0262(2) 0.0549(4) 0.0416(9) Uani 1 1 d U . . H24 H 1.2201 0.0121 0.1308 0.050 Uiso 1 1 calc R . . C25 C 1.2994(3) 0.0160(2) -0.0042(3) 0.0392(9) Uani 1 1 d U . . H25 H 1.3508 -0.0060 0.0327 0.047 Uiso 1 1 calc R . . C26 C 1.2290(3) 0.0641(2) -0.1634(4) 0.0432(9) Uani 1 1 d U . . H26 H 1.2306 0.0767 -0.2400 0.052 Uiso 1 1 calc R . . C27 C 1.1469(3) 0.0754(2) -0.1098(4) 0.0449(9) Uani 1 1 d U . . H27 H 1.0954 0.0955 -0.1501 0.054 Uiso 1 1 calc R . . C28 C 0.8362(3) 0.1780(2) 0.0360(4) 0.0398(8) Uani 1 1 d U . . C29 C 0.8631(3) 0.2280(2) -0.0316(4) 0.0460(9) Uani 1 1 d U . . H29 H 0.9259 0.2306 -0.0512 0.055 Uiso 1 1 calc R . . C30 C 0.7987(3) 0.2739(2) -0.0703(4) 0.0522(10) Uani 1 1 d U . . H30 H 0.8195 0.3063 -0.1170 0.063 Uiso 1 1 calc R . . C31 C 0.6824(3) 0.2278(2) 0.0193(5) 0.0605(11) Uani 1 1 d U . . H31 H 0.6196 0.2274 0.0390 0.073 Uiso 1 1 calc R . . C32 C 0.7420(3) 0.1783(2) 0.0605(4) 0.0532(10) Uani 1 1 d U . . H32 H 0.7182 0.1456 0.1043 0.064 Uiso 1 1 calc R . . C33 C 0.4122(3) 0.14318(16) 0.6390(3) 0.0293(7) Uani 1 1 d U . . C34 C 0.4312(3) 0.21333(16) 0.6197(3) 0.0285(7) Uani 1 1 d U . . C35 C 0.4721(3) 0.25089(17) 0.7096(3) 0.0341(8) Uani 1 1 d U . . H35 H 0.4859 0.2328 0.7822 0.041 Uiso 1 1 calc R . . C36 C 0.4082(3) 0.24117(17) 0.5129(3) 0.0318(7) Uani 1 1 d U . . H36 H 0.3797 0.2167 0.4527 0.038 Uiso 1 1 calc R . . C37 C 0.4274(3) 0.30565(16) 0.4951(3) 0.0306(7) Uani 1 1 d U . . H37 H 0.4109 0.3242 0.4235 0.037 Uiso 1 1 calc R . . C38 C 0.4709(3) 0.34210(15) 0.5839(3) 0.0251(7) Uani 1 1 d U . . C39 C 0.4924(3) 0.31442(17) 0.6924(3) 0.0338(8) Uani 1 1 d U . . H39 H 0.5204 0.3389 0.7529 0.041 Uiso 1 1 calc R . . C40 C 0.5036(2) 0.40943(15) 0.5614(3) 0.0234(7) Uani 1 1 d U . . N1 N 0.5706(2) 0.03970(13) 0.7430(3) 0.0280(7) Uani 1 1 d . . . N2 N 1.1610(4) 0.2795(3) 0.7393(6) 0.109(2) Uani 1 1 d . . . N3 N 1.3060(2) 0.03625(13) -0.1124(3) 0.0284(7) Uani 1 1 d . . . N4 N 0.7086(3) 0.2747(2) -0.0451(4) 0.0598(11) Uani 1 1 d . . . Ni1 Ni 0.43572(3) 0.033169(18) 0.81105(3) 0.02068(17) Uani 1 1 d . . . O1 O 0.9520(2) 0.02177(14) 0.3326(2) 0.0448(8) Uani 1 1 d . . . O2 O 0.40900(18) 0.12478(10) 0.74186(19) 0.0279(5) Uani 1 1 d . . . O3 O 0.4036(3) 0.10757(12) 0.5514(2) 0.0491(8) Uani 1 1 d . . . O4 O 0.5351(2) 0.44066(11) 0.6489(2) 0.0315(6) Uani 1 1 d . . . O5 O 0.50257(18) 0.42786(11) 0.4592(2) 0.0289(6) Uani 1 1 d . . . O6 O 0.36827(18) -0.00139(11) 0.6589(2) 0.0294(6) Uani 1 1 d . . . H6A H 0.3573 0.0331 0.6049 0.044 Uiso 1 1 d R . . H6B H 0.3583 -0.0466 0.6658 0.044 Uiso 1 1 d R . . O1W O 0.4186(2) 0.88639(13) 0.5613(2) 0.0486(8) Uani 1 1 d . . . H1WA H 0.4329 0.8470 0.5688 0.058 Uiso 1 1 d R . . H1WB H 0.4685 0.9078 0.5502 0.073 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0354(17) 0.0343(17) 0.0310(16) -0.0040(14) 0.0121(14) -0.0011(15) C2 0.0342(17) 0.0403(18) 0.0349(16) -0.0015(14) 0.0111(15) -0.0032(15) C3 0.0297(16) 0.0469(17) 0.0288(15) 0.0032(14) 0.0115(13) 0.0048(14) C4 0.0354(17) 0.0421(18) 0.0306(16) -0.0044(14) 0.0134(14) 0.0043(15) C5 0.0338(17) 0.0353(17) 0.0303(16) -0.0038(14) 0.0098(15) 0.0006(15) C6 0.0297(15) 0.0468(17) 0.0334(15) 0.0036(14) 0.0132(13) 0.0037(14) C7 0.0345(16) 0.0541(18) 0.0397(16) 0.0012(15) 0.0130(14) 0.0025(15) C8 0.0336(16) 0.0549(18) 0.0496(17) 0.0067(16) 0.0125(15) 0.0036(15) C9 0.0332(16) 0.0509(18) 0.0459(17) 0.0112(15) 0.0190(15) 0.0086(15) C10 0.0363(16) 0.0441(17) 0.0360(16) 0.0096(14) 0.0172(14) 0.0117(15) C11 0.0327(16) 0.0471(17) 0.0351(16) 0.0059(14) 0.0131(14) 0.0064(14) C12 0.0377(17) 0.059(2) 0.0574(19) 0.0052(17) 0.0114(16) 0.0004(16) C13 0.051(2) 0.072(2) 0.074(2) -0.007(2) 0.016(2) -0.008(2) C14 0.063(3) 0.080(3) 0.087(3) -0.014(2) 0.011(2) -0.009(2) C15 0.061(3) 0.100(3) 0.113(3) -0.017(3) 0.015(3) -0.010(3) C16 0.051(2) 0.084(2) 0.094(2) -0.015(2) 0.016(2) -0.005(2) C17 0.0370(16) 0.0393(16) 0.0350(16) 0.0083(14) 0.0192(14) 0.0067(14) C18 0.0344(15) 0.0410(16) 0.0409(16) 0.0033(14) 0.0192(14) 0.0076(14) C19 0.0329(16) 0.0396(16) 0.0416(16) 0.0064(14) 0.0135(14) 0.0085(14) C20 0.0342(15) 0.0428(16) 0.0350(15) 0.0080(14) 0.0151(14) 0.0095(14) C21 0.0309(15) 0.0413(16) 0.0337(15) 0.0057(13) 0.0145(13) 0.0066(14) C22 0.0357(16) 0.0428(17) 0.0346(16) 0.0091(14) 0.0153(14) 0.0115(14) C23 0.0313(16) 0.0399(17) 0.0321(16) 0.0066(14) 0.0142(14) 0.0074(14) C24 0.0385(18) 0.0550(19) 0.0336(17) 0.0179(15) 0.0171(15) 0.0128(16) C25 0.0336(18) 0.049(2) 0.0369(18) 0.0186(16) 0.0162(15) 0.0126(16) C26 0.0397(19) 0.059(2) 0.0331(17) 0.0152(17) 0.0144(16) 0.0127(17) C27 0.0382(18) 0.060(2) 0.0383(17) 0.0157(16) 0.0133(15) 0.0165(17) C28 0.0347(16) 0.0414(17) 0.0449(17) 0.0038(15) 0.0130(15) 0.0072(15) C29 0.0375(18) 0.0468(19) 0.0556(19) 0.0077(17) 0.0143(16) 0.0058(16) C30 0.047(2) 0.049(2) 0.062(2) 0.0182(19) 0.0108(19) 0.0056(18) C31 0.038(2) 0.059(2) 0.086(3) 0.019(2) 0.014(2) 0.0079(19) C32 0.0403(19) 0.050(2) 0.071(2) 0.0187(18) 0.0148(18) 0.0072(17) C33 0.0421(18) 0.0205(15) 0.0260(16) 0.0007(13) 0.0070(14) -0.0042(14) C34 0.0429(18) 0.0187(15) 0.0249(15) 0.0019(12) 0.0095(14) -0.0038(14) C35 0.0545(19) 0.0236(15) 0.0244(15) 0.0033(13) 0.0044(15) -0.0061(15) C36 0.0485(18) 0.0212(15) 0.0258(15) -0.0009(13) 0.0031(14) -0.0075(14) C37 0.0463(18) 0.0216(15) 0.0241(15) 0.0036(13) 0.0041(14) -0.0035(14) C38 0.0369(17) 0.0171(14) 0.0226(14) -0.0003(12) 0.0096(13) -0.0031(13) C39 0.0528(19) 0.0219(15) 0.0266(15) 0.0001(13) 0.0030(15) -0.0066(14) C40 0.0320(16) 0.0166(14) 0.0229(15) 0.0004(12) 0.0106(13) -0.0001(13) N1 0.0314(16) 0.0295(16) 0.0243(15) -0.0020(12) 0.0106(13) -0.0017(13) N2 0.064(3) 0.095(4) 0.166(6) -0.043(4) -0.006(4) -0.014(3) N3 0.0315(17) 0.0263(16) 0.0288(16) 0.0034(12) 0.0106(13) 0.0063(13) N4 0.046(2) 0.050(2) 0.084(3) 0.018(2) 0.008(2) 0.0130(19) Ni1 0.0259(3) 0.0154(3) 0.0220(3) 0.00031(15) 0.00956(18) 0.00082(16) O1 0.0595(19) 0.0417(16) 0.0378(15) 0.0122(12) 0.0316(15) 0.0164(14) O2 0.0423(14) 0.0172(11) 0.0255(12) 0.0037(9) 0.0100(11) -0.0005(11) O3 0.099(3) 0.0218(13) 0.0263(13) -0.0014(11) 0.0073(15) -0.0157(15) O4 0.0504(16) 0.0178(12) 0.0269(12) -0.0010(10) 0.0060(12) -0.0071(11) O5 0.0389(14) 0.0221(12) 0.0268(12) 0.0057(10) 0.0093(11) 0.0000(11) O6 0.0397(14) 0.0199(12) 0.0288(12) 0.0012(10) 0.0042(11) -0.0034(11) O1W 0.065(2) 0.0315(15) 0.0497(17) -0.0067(13) 0.0054(15) 0.0005(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 C1 N1 1.335(5) . ? C1 C2 1.375(5) . ? C1 H1 0.9300 . ? C2 C3 1.386(5) . ? C2 H2 0.9300 . ? C3 C4 1.385(6) . ? C3 C6 1.499(5) . ? C4 C5 1.381(5) . ? C4 H4 0.9300 . ? C5 N1 1.344(5) . ? C5 H5 0.9300 . ? C6 C7 1.383(6) . ? C6 C11 1.398(5) . ? C7 C8 1.395(6) . ? C7 H7 0.9300 . ? C8 C9 1.385(6) . ? C8 C12 1.495(7) . ? C9 C10 1.383(6) . ? C9 H9 0.9300 . ? C10 O1 1.391(5) . ? C10 C11 1.396(5) . ? C11 H11 0.9300 . ? C12 C16 1.342(7) . ? C12 C13 1.369(7) . ? C13 C14 1.369(8) . ? C13 H13 0.9300 . ? C14 N2 1.324(8) . ? C14 H14 0.9300 . ? C15 N2 1.284(8) . ? C15 C16 1.394(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.373(5) . ? C17 C18 1.379(6) . ? C17 O1 1.396(4) . ? C18 C19 1.394(5) . ? C18 H18 0.9300 . ? C19 C20 1.400(5) . ? C19 C28 1.486(6) . ? C20 C21 1.384(5) . ? C20 H20 0.9300 . ? C21 C22 1.409(5) . ? C21 C23 1.486(5) . ? C22 H22 0.9300 . ? C23 C24 1.381(6) . ? C23 C27 1.389(5) . ? C24 C25 1.371(5) . ? C24 H24 0.9300 . ? C25 N3 1.336(5) . ? C25 H25 0.9300 . ? C26 N3 1.325(5) . ? C26 C27 1.376(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C32 1.377(6) . ? C28 C29 1.379(6) . ? C29 C30 1.369(6) . ? C29 H29 0.9300 . ? C30 N4 1.324(6) . ? C30 H30 0.9300 . ? C31 N4 1.304(6) . ? C31 C32 1.390(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 O3 1.258(4) . ? C33 O2 1.259(4) . ? C33 C34 1.512(5) . ? C34 C36 1.384(5) . ? C34 C35 1.393(5) . ? C35 C39 1.377(5) . ? C35 H35 0.9300 . ? C36 C37 1.394(5) . ? C36 H36 0.9300 . ? C37 C38 1.384(5) . ? C37 H37 0.9300 . ? C38 C39 1.397(5) . ? C38 C40 1.511(4) . ? C39 H39 0.9300 . ? C40 O5 1.246(4) . ? C40 O4 1.258(4) . ? N1 Ni1 2.117(3) . ? N3 Ni1 2.093(3) 1_654 ? Ni1 O4 2.024(2) 2_646 ? Ni1 O5 2.060(2) 4_566 ? Ni1 O6 2.066(2) . ? Ni1 N3 2.093(3) 1_456 ? Ni1 O2 2.100(2) . ? O4 Ni1 2.024(2) 2_656 ? O5 Ni1 2.060(2) 4_565 ? O6 H6A 0.9600 . ? O6 H6B 0.9600 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.6(3) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 119.6(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 117.2(3) . . ? C4 C3 C6 122.4(3) . . ? C2 C3 C6 120.4(4) . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 122.8(4) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C7 C6 C11 119.7(4) . . ? C7 C6 C3 119.7(3) . . ? C11 C6 C3 120.5(4) . . ? C6 C7 C8 122.2(4) . . ? C6 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C9 C8 C7 118.0(4) . . ? C9 C8 C12 123.4(4) . . ? C7 C8 C12 118.6(4) . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 O1 120.9(3) . . ? C9 C10 C11 122.2(4) . . ? O1 C10 C11 116.7(4) . . ? C10 C11 C6 117.7(4) . . ? C10 C11 H11 121.1 . . ? C6 C11 H11 121.1 . . ? C16 C12 C13 115.2(5) . . ? C16 C12 C8 123.8(5) . . ? C13 C12 C8 120.9(4) . . ? C12 C13 C14 120.8(5) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? N2 C14 C13 124.6(6) . . ? N2 C14 H14 117.7 . . ? C13 C14 H14 117.7 . . ? N2 C15 C16 126.9(6) . . ? N2 C15 H15 116.5 . . ? C16 C15 H15 116.5 . . ? C12 C16 C15 119.3(6) . . ? C12 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C22 C17 C18 122.1(3) . . ? C22 C17 O1 116.9(3) . . ? C18 C17 O1 120.9(3) . . ? C17 C18 C19 119.6(3) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C19 C20 118.2(4) . . ? C18 C19 C28 121.4(3) . . ? C20 C19 C28 120.4(3) . . ? C21 C20 C19 122.5(3) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 117.9(3) . . ? C20 C21 C23 121.6(3) . . ? C22 C21 C23 120.5(3) . . ? C17 C22 C21 119.7(4) . . ? C17 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C27 114.9(3) . . ? C24 C23 C21 123.1(3) . . ? C27 C23 C21 122.0(4) . . ? C25 C24 C23 121.6(4) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? N3 C25 C24 122.8(4) . . ? N3 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? N3 C26 C27 123.9(4) . . ? N3 C26 H26 118.1 . . ? C27 C26 H26 118.1 . . ? C26 C27 C23 120.4(4) . . ? C26 C27 H27 119.8 . . ? C23 C27 H27 119.8 . . ? C32 C28 C29 115.3(4) . . ? C32 C28 C19 123.0(4) . . ? C29 C28 C19 121.7(4) . . ? C30 C29 C28 120.9(4) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? N4 C30 C29 123.7(4) . . ? N4 C30 H30 118.2 . . ? C29 C30 H30 118.2 . . ? N4 C31 C32 124.6(4) . . ? N4 C31 H31 117.7 . . ? C32 C31 H31 117.7 . . ? C28 C32 C31 119.6(4) . . ? C28 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? O3 C33 O2 125.3(3) . . ? O3 C33 C34 117.4(3) . . ? O2 C33 C34 117.3(3) . . ? C36 C34 C35 119.1(3) . . ? C36 C34 C33 120.7(3) . . ? C35 C34 C33 120.2(3) . . ? C39 C35 C34 120.9(3) . . ? C39 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C34 C36 C37 120.4(3) . . ? C34 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C38 C37 C36 120.1(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 119.6(3) . . ? C37 C38 C40 120.4(3) . . ? C39 C38 C40 119.8(3) . . ? C35 C39 C38 119.9(3) . . ? C35 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? O5 C40 O4 125.8(3) . . ? O5 C40 C38 118.3(3) . . ? O4 C40 C38 115.8(3) . . ? C1 N1 C5 117.0(3) . . ? C1 N1 Ni1 118.5(2) . . ? C5 N1 Ni1 124.4(3) . . ? C15 N2 C14 113.1(6) . . ? C26 N3 C25 116.3(3) . . ? C26 N3 Ni1 122.1(2) . 1_654 ? C25 N3 Ni1 121.3(3) . 1_654 ? C31 N4 C30 115.9(4) . . ? O4 Ni1 O5 96.67(10) 2_646 4_566 ? O4 Ni1 O6 86.11(10) 2_646 . ? O5 Ni1 O6 177.14(9) 4_566 . ? O4 Ni1 N3 95.67(11) 2_646 1_456 ? O5 Ni1 N3 89.22(11) 4_566 1_456 ? O6 Ni1 N3 91.12(11) . 1_456 ? O4 Ni1 O2 170.68(9) 2_646 . ? O5 Ni1 O2 90.79(9) 4_566 . ? O6 Ni1 O2 86.38(9) . . ? N3 Ni1 O2 89.98(10) 1_456 . ? O4 Ni1 N1 88.67(11) 2_646 . ? O5 Ni1 N1 85.71(11) 4_566 . ? O6 Ni1 N1 93.76(11) . . ? N3 Ni1 N1 173.68(11) 1_456 . ? O2 Ni1 N1 86.32(10) . . ? C10 O1 C17 117.9(3) . . ? C33 O2 Ni1 128.5(2) . . ? C40 O4 Ni1 137.2(2) . 2_656 ? C40 O5 Ni1 152.4(2) . 4_565 ? Ni1 O6 H6A 109.5 . . ? Ni1 O6 H6B 109.5 . . ? H6A O6 H6B 141.1 . . ? H1WA O1W H1WB 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.975 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.087