data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 N6 Ni O9' _chemical_formula_weight 681.34 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' 'Ni' 'Ni' 0.3393 1.1124 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.1673(10) _cell_length_b 19.8159(10) _cell_length_c 20.9173(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6286.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3596 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 24.1 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8759 _exptl_absorpt_correction_T_max 0.9048 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32240 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5852 _reflns_number_gt 3587 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+5.7688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5852 _refine_ls_number_parameters 437 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.38841(3) 0.31875(3) 0.47584(2) 0.03460(16) Uani 1 1 d . . . O1 O 0.31342(16) 0.38237(13) 0.41522(12) 0.0377(7) Uani 1 1 d . . . O2 O 0.50782(16) 0.35226(14) 0.44032(12) 0.0387(7) Uani 1 1 d . . . O3 O 0.1446(2) 0.55333(17) 0.29231(19) 0.0759(11) Uani 1 1 d D . . O4 O 0.03107(19) 0.48526(15) 0.21905(14) 0.0550(8) Uani 1 1 d . . . O5 O 0.79751(18) 0.54298(17) 0.51524(15) 0.0555(9) Uani 1 1 d D . . O6 O 0.87200(18) 0.50500(16) 0.40998(14) 0.0548(8) Uani 1 1 d . . . O7 O 0.9110(3) 0.6147(3) 0.15256(18) 0.1070(16) Uani 1 1 d DU . . O8 O 0.1226(5) 0.7415(4) 0.2448(4) 0.181(3) Uani 1 1 d DU . . N1 N 0.2977(2) 0.28403(17) 0.35732(15) 0.0403(8) Uani 1 1 d . . . N2 N 0.3488(2) 0.25882(17) 0.40616(15) 0.0367(8) Uani 1 1 d . . . N3 N 0.4452(2) 0.22592(17) 0.50286(15) 0.0380(8) Uani 1 1 d . . . N4 N 0.5124(2) 0.41035(16) 0.53587(15) 0.0381(8) Uani 1 1 d . . . N5 N 0.4311(2) 0.38038(16) 0.54299(14) 0.0343(8) Uani 1 1 d . . . N6 N 0.2846(2) 0.31396(17) 0.54332(15) 0.0395(8) Uani 1 1 d . . . C1 C 0.2183(2) 0.3827(2) 0.32488(18) 0.0353(9) Uani 1 1 d . . . C2 C 0.2113(3) 0.4525(2) 0.32559(19) 0.0419(10) Uani 1 1 d . . . H2 H 0.2497 0.4776 0.3508 0.050 Uiso 1 1 calc R . . C3 C 0.1487(3) 0.4853(2) 0.2897(2) 0.0433(10) Uani 1 1 d . . . C4 C 0.0909(3) 0.4479(2) 0.25194(19) 0.0418(10) Uani 1 1 d . . . C5 C 0.0975(3) 0.3792(2) 0.2509(2) 0.0458(11) Uani 1 1 d . . . H5A H 0.0587 0.3541 0.2259 0.055 Uiso 1 1 calc R . . C6 C 0.1615(3) 0.3462(2) 0.28688(19) 0.0418(10) Uani 1 1 d . . . H6 H 0.1659 0.2994 0.2853 0.050 Uiso 1 1 calc R . . C7 C 0.2810(2) 0.3486(2) 0.36863(19) 0.0366(10) Uani 1 1 d . . . C8 C 0.3737(3) 0.1973(2) 0.4062(2) 0.0447(11) Uani 1 1 d . . . H8A H 0.3584 0.1675 0.3736 0.054 Uiso 1 1 calc R . . C9 C 0.4271(3) 0.1767(2) 0.46006(19) 0.0400(10) Uani 1 1 d . . . C10 C 0.4591(3) 0.1120(2) 0.4670(2) 0.0547(12) Uani 1 1 d . . . H10 H 0.4444 0.0787 0.4376 0.066 Uiso 1 1 calc R . . C11 C 0.5128(3) 0.0975(2) 0.5178(3) 0.0595(13) Uani 1 1 d . . . H11 H 0.5360 0.0544 0.5231 0.071 Uiso 1 1 calc R . . C12 C 0.5316(3) 0.1472(3) 0.5606(2) 0.0600(13) Uani 1 1 d . . . H12 H 0.5676 0.1383 0.5956 0.072 Uiso 1 1 calc R . . C13 C 0.4971(3) 0.2107(2) 0.5518(2) 0.0503(12) Uani 1 1 d . . . H13 H 0.5106 0.2442 0.5814 0.060 Uiso 1 1 calc R . . C14 C -0.0349(3) 0.4505(3) 0.1836(2) 0.0643(14) Uani 1 1 d . . . H14A H -0.0074 0.4228 0.1516 0.096 Uiso 1 1 calc R . . H14B H -0.0732 0.4826 0.1634 0.096 Uiso 1 1 calc R . . H14C H -0.0687 0.4225 0.2120 0.096 Uiso 1 1 calc R . . C15 C 0.6329(2) 0.4203(2) 0.46226(18) 0.0354(9) Uani 1 1 d . . . C16 C 0.6747(2) 0.46881(19) 0.49899(18) 0.0365(10) Uani 1 1 d . . . H16 H 0.6481 0.4836 0.5365 0.044 Uiso 1 1 calc R . . C17 C 0.7544(3) 0.4955(2) 0.48126(19) 0.0371(9) Uani 1 1 d . . . C18 C 0.7941(3) 0.4740(2) 0.4242(2) 0.0426(10) Uani 1 1 d . . . C19 C 0.7529(3) 0.4266(2) 0.3876(2) 0.0533(12) Uani 1 1 d . . . H19 H 0.7788 0.4125 0.3496 0.064 Uiso 1 1 calc R . . C20 C 0.6731(3) 0.3994(2) 0.4062(2) 0.0481(11) Uani 1 1 d . . . H20 H 0.6462 0.3668 0.3809 0.058 Uiso 1 1 calc R . . C21 C 0.5455(2) 0.3915(2) 0.47937(19) 0.0356(9) Uani 1 1 d . . . C22 C 0.3831(3) 0.3919(2) 0.59188(19) 0.0403(10) Uani 1 1 d . . . H22 H 0.4000 0.4214 0.6241 0.048 Uiso 1 1 calc R . . C23 C 0.2996(3) 0.3552(2) 0.59349(19) 0.0378(10) Uani 1 1 d . . . C24 C 0.2397(3) 0.3619(2) 0.6428(2) 0.0509(12) Uani 1 1 d . . . H24 H 0.2513 0.3907 0.6768 0.061 Uiso 1 1 calc R . . C25 C 0.1622(3) 0.3253(3) 0.6409(2) 0.0610(13) Uani 1 1 d . . . H25 H 0.1209 0.3292 0.6736 0.073 Uiso 1 1 calc R . . C26 C 0.1473(3) 0.2834(2) 0.5904(2) 0.0565(13) Uani 1 1 d . . . H26 H 0.0956 0.2584 0.5880 0.068 Uiso 1 1 calc R . . C27 C 0.2101(3) 0.2785(2) 0.5427(2) 0.0494(12) Uani 1 1 d . . . H27 H 0.1999 0.2492 0.5087 0.059 Uiso 1 1 calc R . . C28 C 0.9089(3) 0.4918(3) 0.3484(2) 0.0689(15) Uani 1 1 d . . . H28A H 0.8655 0.5008 0.3161 0.103 Uiso 1 1 calc R . . H28B H 0.9268 0.4454 0.3460 0.103 Uiso 1 1 calc R . . H28C H 0.9591 0.5204 0.3418 0.103 Uiso 1 1 calc R . . C29 C 0.8334(4) 0.6425(4) 0.1499(3) 0.110(2) Uani 1 1 d . . . H29A H 0.8067 0.6414 0.1915 0.164 Uiso 1 1 calc R . . H29B H 0.7971 0.6181 0.1203 0.164 Uiso 1 1 calc R . . H29C H 0.8391 0.6885 0.1360 0.164 Uiso 1 1 calc R . . C30 C 0.1331(6) 0.7865(4) 0.1966(4) 0.138(3) Uani 1 1 d U . . H30A H 0.1137 0.7666 0.1572 0.207 Uiso 1 1 calc R . . H30B H 0.1942 0.7985 0.1932 0.207 Uiso 1 1 calc R . . H30C H 0.0988 0.8261 0.2054 0.207 Uiso 1 1 calc R . . O9 O 0.0189(3) 0.6361(2) 0.25465(18) 0.0789(11) Uani 1 1 d GD . . H3 H 0.102(3) 0.573(3) 0.273(3) 0.118 Uiso 1 1 d D . . H5 H 0.764(3) 0.561(3) 0.543(2) 0.118 Uiso 1 1 d D . . H7 H 0.935(4) 0.606(3) 0.1166(15) 0.118 Uiso 1 1 d D . . H8 H 0.174(2) 0.726(4) 0.249(4) 0.118 Uiso 1 1 d D . . H9A H -0.010(4) 0.621(3) 0.2225(18) 0.118 Uiso 1 1 d D . . H9B H 0.041(4) 0.6759(15) 0.248(3) 0.118 Uiso 1 1 d 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 Ni1 0.0344(3) 0.0379(3) 0.0315(3) -0.0032(2) -0.0029(2) -0.0020(2) O1 0.0423(16) 0.0364(16) 0.0345(15) -0.0060(13) -0.0074(13) -0.0010(12) O2 0.0381(15) 0.0462(17) 0.0317(15) -0.0098(13) 0.0012(13) -0.0061(13) O3 0.075(2) 0.044(2) 0.109(3) -0.001(2) -0.050(2) 0.0025(18) O4 0.0480(18) 0.059(2) 0.0578(19) -0.0055(16) -0.0231(16) 0.0052(15) O5 0.0412(17) 0.065(2) 0.060(2) -0.0267(18) 0.0111(16) -0.0158(16) O6 0.0394(16) 0.068(2) 0.057(2) -0.0112(16) 0.0191(15) -0.0147(15) O7 0.066(3) 0.194(5) 0.061(3) -0.014(3) -0.002(2) 0.046(3) O8 0.267(7) 0.161(6) 0.115(4) 0.039(4) -0.045(6) -0.074(6) N1 0.047(2) 0.037(2) 0.037(2) -0.0060(16) -0.0145(17) 0.0056(16) N2 0.0366(18) 0.041(2) 0.0322(19) -0.0022(16) -0.0047(16) 0.0002(16) N3 0.0347(18) 0.043(2) 0.0367(19) -0.0007(16) -0.0025(16) 0.0011(16) N4 0.0324(17) 0.045(2) 0.037(2) -0.0051(16) 0.0040(15) -0.0094(15) N5 0.0343(18) 0.0389(19) 0.0296(18) -0.0013(15) 0.0005(15) -0.0010(15) N6 0.0383(19) 0.042(2) 0.038(2) 0.0014(17) -0.0043(15) -0.0046(17) C1 0.034(2) 0.038(3) 0.033(2) -0.0030(18) 0.0025(18) -0.0018(19) C2 0.038(2) 0.048(3) 0.040(2) -0.003(2) -0.007(2) -0.006(2) C3 0.043(2) 0.038(3) 0.048(3) 0.000(2) -0.008(2) -0.002(2) C4 0.038(2) 0.052(3) 0.036(2) -0.001(2) -0.0048(19) 0.002(2) C5 0.044(3) 0.051(3) 0.042(3) -0.010(2) -0.011(2) -0.004(2) C6 0.044(2) 0.040(2) 0.041(2) -0.005(2) -0.007(2) 0.004(2) C7 0.031(2) 0.045(3) 0.033(2) -0.001(2) -0.0004(19) -0.0043(19) C8 0.047(3) 0.039(3) 0.049(3) -0.010(2) -0.009(2) 0.005(2) C9 0.034(2) 0.041(2) 0.045(3) 0.000(2) -0.0012(19) 0.004(2) C10 0.049(3) 0.045(3) 0.070(3) -0.004(2) -0.005(3) 0.009(2) C11 0.049(3) 0.052(3) 0.077(4) 0.008(3) -0.005(3) 0.017(2) C12 0.050(3) 0.066(3) 0.064(3) 0.016(3) -0.015(3) 0.013(3) C13 0.048(3) 0.060(3) 0.042(3) -0.004(2) -0.011(2) -0.002(2) C14 0.057(3) 0.075(4) 0.061(3) -0.016(3) -0.029(3) 0.011(3) C15 0.034(2) 0.041(2) 0.032(2) -0.0023(18) 0.0032(17) -0.0014(18) C16 0.036(2) 0.040(2) 0.033(2) -0.0060(19) 0.0052(18) 0.0002(19) C17 0.034(2) 0.040(2) 0.037(2) -0.006(2) 0.001(2) 0.0000(18) C18 0.037(2) 0.046(3) 0.045(3) -0.003(2) 0.006(2) 0.000(2) C19 0.046(3) 0.070(3) 0.044(3) -0.020(2) 0.017(2) -0.006(2) C20 0.048(3) 0.058(3) 0.039(2) -0.016(2) 0.004(2) -0.011(2) C21 0.037(2) 0.036(2) 0.034(2) 0.0037(19) -0.004(2) 0.0016(18) C22 0.040(2) 0.047(3) 0.033(2) -0.0040(19) -0.002(2) -0.004(2) C23 0.036(2) 0.042(3) 0.035(2) 0.002(2) -0.004(2) 0.0017(19) C24 0.046(3) 0.066(3) 0.041(3) -0.006(2) 0.011(2) -0.002(2) C25 0.046(3) 0.075(4) 0.062(3) 0.005(3) 0.016(3) 0.000(3) C26 0.036(2) 0.063(3) 0.071(3) 0.009(3) 0.000(3) -0.007(2) C27 0.042(3) 0.051(3) 0.055(3) -0.001(2) -0.007(2) -0.008(2) C28 0.059(3) 0.088(4) 0.060(3) -0.011(3) 0.028(3) -0.013(3) C29 0.078(4) 0.117(6) 0.134(6) -0.032(5) -0.006(4) 0.042(4) C30 0.182(7) 0.123(6) 0.108(5) 0.021(5) -0.025(5) -0.002(5) O9 0.080(3) 0.079(3) 0.078(3) -0.003(2) -0.018(2) 0.011(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 Ni1 N5 1.971(3) . ? Ni1 N2 1.974(3) . ? Ni1 O2 2.067(3) . ? Ni1 N3 2.109(3) . ? Ni1 N6 2.117(3) . ? Ni1 O1 2.119(3) . ? O1 C7 1.280(4) . ? O2 C21 1.264(4) . ? O3 C3 1.351(5) . ? O3 H3 0.850(11) . ? O4 C4 1.359(5) . ? O4 C14 1.423(5) . ? O5 C17 1.349(5) . ? O5 H5 0.846(11) . ? O6 C18 1.365(5) . ? O6 C28 1.428(5) . ? O7 C29 1.301(6) . ? O7 H7 0.852(11) . ? O8 C30 1.355(9) . ? O8 H8 0.848(11) . ? N1 C7 1.326(5) . ? N1 N2 1.376(4) . ? N2 C8 1.276(5) . ? N3 C13 1.326(5) . ? N3 C9 1.352(5) . ? N4 C21 1.338(5) . ? N4 N5 1.376(4) . ? N5 C22 1.276(5) . ? N6 C27 1.330(5) . ? N6 C23 1.349(5) . ? C1 C6 1.377(5) . ? C1 C2 1.388(5) . ? C1 C7 1.483(5) . ? C2 C3 1.372(5) . ? C2 H2 0.9300 . ? C3 C4 1.394(6) . ? C4 C5 1.365(6) . ? C5 C6 1.391(5) . ? C5 H5A 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.446(6) . ? C8 H8A 0.9300 . ? C9 C10 1.379(6) . ? C10 C11 1.370(6) . ? C10 H10 0.9300 . ? C11 C12 1.361(7) . ? C11 H11 0.9300 . ? C12 C13 1.375(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.384(5) . ? C15 C20 1.386(5) . ? C15 C21 1.488(5) . ? C16 C17 1.370(5) . ? C16 H16 0.9300 . ? C17 C18 1.403(5) . ? C18 C19 1.362(6) . ? C19 C20 1.381(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C23 1.460(5) . ? C22 H22 0.9300 . ? C23 C24 1.381(5) . ? C24 C25 1.381(6) . ? C24 H24 0.9300 . ? C25 C26 1.363(6) . ? C25 H25 0.9300 . ? C26 C27 1.383(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? O9 H9B 0.870(11) . ? O9 H9A 0.854(10) . ? O9 H9B 0.870(11) . ? 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 N5 Ni1 N2 177.72(13) . . ? N5 Ni1 O2 76.66(11) . . ? N2 Ni1 O2 101.20(12) . . ? N5 Ni1 N3 102.44(13) . . ? N2 Ni1 N3 78.30(13) . . ? O2 Ni1 N3 91.06(12) . . ? N5 Ni1 N6 78.28(13) . . ? N2 Ni1 N6 103.84(13) . . ? O2 Ni1 N6 154.94(12) . . ? N3 Ni1 N6 94.95(13) . . ? N5 Ni1 O1 103.53(12) . . ? N2 Ni1 O1 75.69(12) . . ? O2 Ni1 O1 93.67(10) . . ? N3 Ni1 O1 154.00(12) . . ? N6 Ni1 O1 91.51(11) . . ? C7 O1 Ni1 110.5(2) . . ? C21 O2 Ni1 111.2(2) . . ? C3 O3 H3 118(4) . . ? C4 O4 C14 118.0(4) . . ? C17 O5 H5 112(4) . . ? C18 O6 C28 116.9(3) . . ? C29 O7 H7 116(4) . . ? C30 O8 H8 102(6) . . ? C7 N1 N2 109.0(3) . . ? C8 N2 N1 120.9(3) . . ? C8 N2 Ni1 119.0(3) . . ? N1 N2 Ni1 120.1(2) . . ? C13 N3 C9 118.0(4) . . ? C13 N3 Ni1 130.4(3) . . ? C9 N3 Ni1 111.6(3) . . ? C21 N4 N5 108.2(3) . . ? C22 N5 N4 121.4(3) . . ? C22 N5 Ni1 119.6(3) . . ? N4 N5 Ni1 119.0(2) . . ? C27 N6 C23 118.1(4) . . ? C27 N6 Ni1 130.4(3) . . ? C23 N6 Ni1 111.5(3) . . ? C6 C1 C2 118.8(4) . . ? C6 C1 C7 121.3(4) . . ? C2 C1 C7 119.7(4) . . ? C3 C2 C1 121.2(4) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? O3 C3 C2 118.8(4) . . ? O3 C3 C4 121.6(4) . . ? C2 C3 C4 119.6(4) . . ? O4 C4 C5 125.7(4) . . ? O4 C4 C3 114.7(4) . . ? C5 C4 C3 119.6(4) . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 120.1(4) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? O1 C7 N1 124.5(4) . . ? O1 C7 C1 118.6(4) . . ? N1 C7 C1 116.9(4) . . ? N2 C8 C9 115.8(4) . . ? N2 C8 H8A 122.1 . . ? C9 C8 H8A 122.1 . . ? N3 C9 C10 121.9(4) . . ? N3 C9 C8 115.3(4) . . ? C10 C9 C8 122.8(4) . . ? C11 C10 C9 119.2(4) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C12 C11 C10 118.8(4) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C13 119.7(4) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? N3 C13 C12 122.4(4) . . ? N3 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 118.5(4) . . ? C16 C15 C21 122.8(3) . . ? C20 C15 C21 118.7(4) . . ? C17 C16 C15 121.4(4) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? O5 C17 C16 123.7(4) . . ? O5 C17 C18 116.9(4) . . ? C16 C17 C18 119.5(4) . . ? C19 C18 O6 125.8(4) . . ? C19 C18 C17 119.3(4) . . ? O6 C18 C17 114.8(4) . . ? C18 C19 C20 120.9(4) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 120.4(4) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? O2 C21 N4 125.0(4) . . ? O2 C21 C15 118.9(4) . . ? N4 C21 C15 116.1(3) . . ? N5 C22 C23 115.1(4) . . ? N5 C22 H22 122.4 . . ? C23 C22 H22 122.4 . . ? N6 C23 C24 121.9(4) . . ? N6 C23 C22 115.5(4) . . ? C24 C23 C22 122.7(4) . . ? C23 C24 C25 119.2(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 118.8(4) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C27 119.3(4) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? N6 C27 C26 122.7(4) . . ? N6 C27 H27 118.6 . . ? C26 C27 H27 118.6 . . ? O6 C28 H28A 109.5 . . ? O6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O7 C29 H29A 109.5 . . ? O7 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O7 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O8 C30 H30A 109.5 . . ? O8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H9B O9 H9A 112(3) . . ? H9B O9 H9B 0(7) . . ? H9A O9 H9B 112(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 N2 0.848(11) 3.38(9) 3.421(8) 86(6) 8_665 O8 H8 N1 0.848(11) 2.58(9) 2.778(8) 94(7) 8_665 O7 H7 N5 0.852(11) 2.57(4) 3.316(5) 147(6) 2_664 O7 H7 N4 0.852(11) 1.897(12) 2.749(5) 178(7) 2_664 O3 H3 O9 0.850(11) 1.83(3) 2.636(5) 159(6) . O9 H9A O7 0.854(10) 1.90(2) 2.724(5) 163(6) 1_455 O5 H5 O1 0.846(11) 1.85(2) 2.671(4) 164(6) 5_666 O9 H9B O8 0.870(11) 1.79(2) 2.621(8) 158(6) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.523 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.063