data_joef040 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H96 N6 Ni O12' _chemical_formula_weight 1392.34 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' '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 Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.752(3) _cell_length_b 14.752(3) _cell_length_c 32.249(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7018(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1013 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.32 _exptl_crystal_description block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 0.345 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9035 _exptl_absorpt_correction_T_max 0.9373 _exptl_absorpt_process_details 'SADABS, Sheldrick (2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 120(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 AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 79762 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8472 _reflns_number_gt 7770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2002)' _computing_cell_refinement 'SHELXTL, Sheldrick (2001)' _computing_data_reduction 'SHELXTL, Sheldrick (2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Sheldrick (2001)' _computing_publication_material 'SHELXTL, Sheldrick (2001)' _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^)+(0.0575P)^2^+4.0015P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(12) _refine_ls_number_reflns 8472 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Ni Ni 0.824462(18) 0.824462(18) 1.0000 0.01349(9) Uani 1 2 d S . . N1 N 0.91214(13) 0.86374(13) 1.03623(6) 0.0158(4) Uani 1 1 d . . . N2 N 0.61434(12) 0.66803(14) 1.04816(5) 0.0155(4) Uani 1 1 d . . . H2A H 0.6566 0.6901 1.0318 0.019 Uiso 1 1 calc R . . N3 N 0.54112(12) 0.80024(13) 0.99459(6) 0.0163(4) Uani 1 1 d . . . H3A H 0.5564 0.8113 0.9687 0.020 Uiso 1 1 calc R . . O1 O 0.76926(11) 0.74923(11) 1.03761(5) 0.0168(3) Uani 1 1 d . . . O2 O 0.58789(11) 0.60852(12) 1.11206(5) 0.0228(4) Uani 1 1 d . . . O3 O 0.55039(13) 0.84903(12) 1.06126(5) 0.0235(4) Uani 1 1 d . . . O4 O 0.57218(12) 0.93936(12) 0.93682(5) 0.0218(4) Uani 1 1 d . . . O5 O 0.29093(13) 0.79922(16) 0.95949(7) 0.0395(5) Uani 1 1 d . . . O6 O 0.42105(12) 0.78550(13) 0.92399(5) 0.0230(4) Uani 1 1 d . . . C1 C 1.09827(18) 1.04172(19) 1.01501(9) 0.0293(6) Uani 1 1 d . . . H1A H 1.1349 1.0825 1.0327 0.035 Uiso 1 1 calc R . . H1B H 1.1404 1.0027 0.9991 0.035 Uiso 1 1 calc R . . C2 C 1.03781(17) 0.98238(18) 1.04241(8) 0.0253(5) Uani 1 1 d . . . H2B H 1.0758 0.9441 1.0607 0.030 Uiso 1 1 calc R . . H2C H 0.9990 1.0211 1.0601 0.030 Uiso 1 1 calc R . . C3 C 0.97930(15) 0.92298(16) 1.01510(7) 0.0176(5) Uani 1 1 d . . . H3B H 1.0204 0.8833 0.9984 0.021 Uiso 1 1 calc R . . C4 C 0.92295(16) 0.83927(15) 1.07420(7) 0.0172(4) Uani 1 1 d . . . H4A H 0.9740 0.8626 1.0886 0.021 Uiso 1 1 calc R . . C5 C 0.86338(16) 0.77911(15) 1.09641(7) 0.0171(4) Uani 1 1 d . . . C6 C 0.88313(17) 0.76062(17) 1.13807(7) 0.0198(5) Uani 1 1 d . . . H6A H 0.9355 0.7866 1.1504 0.024 Uiso 1 1 calc R . . C7 C 0.82775(18) 0.70522(17) 1.16151(7) 0.0219(5) Uani 1 1 d . . . H7A H 0.8426 0.6916 1.1895 0.026 Uiso 1 1 calc R . . C8 C 0.75009(16) 0.66975(17) 1.14351(7) 0.0190(4) Uani 1 1 d . . . H8A H 0.7110 0.6333 1.1599 0.023 Uiso 1 1 calc R . . C9 C 0.72742(15) 0.68574(15) 1.10217(7) 0.0151(4) Uani 1 1 d . . . C10 C 0.78615(15) 0.73910(15) 1.07722(7) 0.0143(4) Uani 1 1 d . . . C11 C 0.63774(15) 0.64934(14) 1.08810(6) 0.0156(4) Uani 1 1 d . . . C12 C 0.52788(15) 0.65469(15) 1.03116(7) 0.0155(4) Uani 1 1 d . . . C13 C 0.47791(17) 0.57668(16) 1.04002(7) 0.0198(5) Uani 1 1 d . . . H13A H 0.5025 0.5321 1.0580 0.024 Uiso 1 1 calc R . . C14 C 0.39304(18) 0.56360(17) 1.02287(8) 0.0236(5) Uani 1 1 d . . . H14A H 0.3592 0.5108 1.0295 0.028 Uiso 1 1 calc R . . C15 C 0.35757(16) 0.62727(17) 0.99606(8) 0.0239(5) Uani 1 1 d . . . H15A H 0.2990 0.6186 0.9845 0.029 Uiso 1 1 calc R . . C16 C 0.40760(16) 0.70424(17) 0.98600(7) 0.0200(5) Uani 1 1 d . . . C17 C 0.49254(15) 0.71955(15) 1.00376(7) 0.0163(4) Uani 1 1 d . . . C18 C 0.56499(16) 0.86159(16) 1.02461(7) 0.0181(5) Uani 1 1 d . . . C19 C 0.61300(16) 0.94555(15) 1.00986(7) 0.0177(5) Uani 1 1 d . . . C20 C 0.65731(18) 0.99785(17) 1.03999(8) 0.0242(5) Uani 1 1 d . . . H20A H 0.6573 0.9777 1.0680 0.029 Uiso 1 1 calc R . . C21 C 0.70111(19) 1.07802(17) 1.03015(8) 0.0259(6) Uani 1 1 d . . . H21A H 0.7310 1.1117 1.0512 0.031 Uiso 1 1 calc R . . C22 C 0.70148(17) 1.10945(17) 0.98927(8) 0.0225(5) Uani 1 1 d . . . H22A H 0.7315 1.1643 0.9823 0.027 Uiso 1 1 calc R . . C23 C 0.65758(16) 1.05953(16) 0.95933(7) 0.0191(5) Uani 1 1 d . . . C24 C 0.61424(16) 0.97918(16) 0.96967(7) 0.0176(5) Uani 1 1 d . . . C25 C 0.58010(18) 1.00093(17) 0.90135(7) 0.0222(5) Uani 1 1 d . . . H25A H 0.5197 1.0248 0.8937 0.027 Uiso 1 1 calc R . . H25B H 0.6055 0.9683 0.8772 0.027 Uiso 1 1 calc R . . C26 C 0.64314(18) 1.07903(17) 0.91394(8) 0.0226(5) Uani 1 1 d . . . H26A H 0.7021 1.0733 0.8988 0.027 Uiso 1 1 calc R . . C27 C 0.60278(19) 1.17231(19) 0.90586(8) 0.0289(6) Uani 1 1 d . . . H27A H 0.6426 1.2189 0.9176 0.043 Uiso 1 1 calc R . . H27B H 0.5429 1.1763 0.9189 0.043 Uiso 1 1 calc R . . H27C H 0.5969 1.1818 0.8759 0.043 Uiso 1 1 calc R . . C28 C 0.36583(17) 0.76850(18) 0.95609(8) 0.0234(5) Uani 1 1 d . . . C29 C 0.38477(18) 0.84537(18) 0.89229(8) 0.0256(5) Uani 1 1 d . . . H29A H 0.3898 0.9092 0.9015 0.031 Uiso 1 1 calc R . . H29B H 0.3199 0.8316 0.8875 0.031 Uiso 1 1 calc R . . C30 C 0.43744(19) 0.83177(19) 0.85302(8) 0.0283(5) Uani 1 1 d . . . H30A H 0.4350 0.7671 0.8449 0.034 Uiso 1 1 calc R . . H30B H 0.5017 0.8481 0.8578 0.034 Uiso 1 1 calc R . . C31 C 0.3991(2) 0.8897(2) 0.81808(9) 0.0356(7) Uani 1 1 d . . . H31A H 0.4033 0.9543 0.8262 0.043 Uiso 1 1 calc R . . H31B H 0.3341 0.8749 0.8145 0.043 Uiso 1 1 calc R . . C32 C 0.4473(2) 0.8769(2) 0.77668(9) 0.0376(7) Uani 1 1 d . . . H32A H 0.4534 0.8112 0.7710 0.045 Uiso 1 1 calc R . . H32B H 0.5091 0.9028 0.7787 0.045 Uiso 1 1 calc R . . C33 C 0.3975(2) 0.9216(2) 0.74036(9) 0.0394(7) Uani 1 1 d . . . H33A H 0.3784 0.9831 0.7490 0.047 Uiso 1 1 calc R . . H33B H 0.4406 0.9285 0.7171 0.047 Uiso 1 1 calc R . . C34 C 0.3142(2) 0.8703(2) 0.72474(10) 0.0398(7) Uani 1 1 d . . . H34A H 0.2750 0.9128 0.7092 0.048 Uiso 1 1 calc R . . H34B H 0.2793 0.8481 0.7489 0.048 Uiso 1 1 calc R . . C35 C 0.3372(2) 0.7896(2) 0.69668(10) 0.0407(7) Uani 1 1 d . . . H35A H 0.3889 0.7563 0.7089 0.049 Uiso 1 1 calc R . . H35B H 0.2846 0.7479 0.6962 0.049 Uiso 1 1 calc R . . C36 C 0.3607(3) 0.8149(3) 0.65306(10) 0.0472(8) Uani 1 1 d . . . H36A H 0.4104 0.8599 0.6537 0.057 Uiso 1 1 calc R . . H36B H 0.3073 0.8442 0.6402 0.057 Uiso 1 1 calc R . . C37 C 0.3896(3) 0.7357(3) 0.62617(11) 0.0497(8) Uani 1 1 d . . . H37A H 0.3445 0.6864 0.6292 0.060 Uiso 1 1 calc R . . H37B H 0.3890 0.7553 0.5968 0.060 Uiso 1 1 calc R . . C38 C 0.4810(2) 0.6991(2) 0.63616(11) 0.0425(8) Uani 1 1 d . . . H38A H 0.4812 0.6800 0.6656 0.051 Uiso 1 1 calc R . . H38B H 0.5257 0.7489 0.6333 0.051 Uiso 1 1 calc R . . C39 C 0.5128(3) 0.6196(3) 0.60982(12) 0.0539(9) Uani 1 1 d . . . H39A H 0.4712 0.5679 0.6144 0.065 Uiso 1 1 calc R . . H39B H 0.5083 0.6369 0.5802 0.065 Uiso 1 1 calc R . . C40 C 0.6093(3) 0.5884(3) 0.61860(13) 0.0609(11) Uani 1 1 d . . . H40A H 0.6202 0.5304 0.6047 0.091 Uiso 1 1 calc R . . H40B H 0.6175 0.5810 0.6486 0.091 Uiso 1 1 calc R . . H40C H 0.6521 0.6338 0.6082 0.091 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 Ni 0.01457(12) 0.01457(12) 0.01132(17) 0.00142(11) -0.00142(11) -0.00424(15) N1 0.0164(9) 0.0145(9) 0.0166(9) 0.0010(7) -0.0015(7) -0.0028(7) N2 0.0157(9) 0.0183(9) 0.0126(8) 0.0024(7) 0.0019(7) -0.0047(7) N3 0.0171(9) 0.0181(9) 0.0136(9) 0.0001(7) 0.0018(7) -0.0017(7) O1 0.0181(8) 0.0198(8) 0.0124(7) 0.0027(6) -0.0010(6) -0.0060(6) O2 0.0204(8) 0.0309(10) 0.0170(8) 0.0062(7) 0.0021(7) -0.0047(7) O3 0.0325(10) 0.0232(9) 0.0148(8) -0.0017(7) 0.0053(7) -0.0038(7) O4 0.0298(10) 0.0216(9) 0.0141(8) 0.0011(7) 0.0004(7) -0.0068(7) O5 0.0219(9) 0.0522(13) 0.0444(12) 0.0169(10) 0.0042(9) 0.0103(9) O6 0.0200(8) 0.0303(9) 0.0188(8) 0.0035(7) -0.0026(7) 0.0023(7) C1 0.0227(13) 0.0295(14) 0.0356(15) 0.0097(12) -0.0087(11) -0.0129(11) C2 0.0233(13) 0.0260(13) 0.0266(12) 0.0052(10) -0.0085(10) -0.0098(10) C3 0.0166(11) 0.0175(11) 0.0186(11) 0.0044(9) -0.0016(9) -0.0036(9) C4 0.0173(10) 0.0152(11) 0.0192(10) -0.0012(9) -0.0053(8) -0.0009(8) C5 0.0186(11) 0.0162(11) 0.0165(10) -0.0010(8) -0.0005(9) -0.0002(8) C6 0.0209(11) 0.0215(11) 0.0169(11) -0.0015(9) -0.0039(9) -0.0007(9) C7 0.0270(12) 0.0260(12) 0.0127(10) 0.0033(9) -0.0027(10) -0.0002(11) C8 0.0213(11) 0.0199(11) 0.0158(10) 0.0026(9) 0.0032(8) 0.0013(10) C9 0.0173(10) 0.0146(10) 0.0134(10) -0.0001(8) 0.0014(8) -0.0002(8) C10 0.0167(10) 0.0138(10) 0.0124(10) -0.0019(8) -0.0014(8) 0.0010(8) C11 0.0187(11) 0.0140(10) 0.0142(10) -0.0006(8) 0.0022(8) 0.0016(8) C12 0.0160(10) 0.0176(11) 0.0130(10) -0.0027(8) 0.0035(8) -0.0027(8) C13 0.0250(12) 0.0184(11) 0.0159(11) -0.0009(9) 0.0038(9) -0.0047(9) C14 0.0244(13) 0.0225(12) 0.0241(12) -0.0013(10) 0.0023(10) -0.0110(10) C15 0.0187(11) 0.0292(13) 0.0237(12) -0.0028(10) 0.0003(10) -0.0066(9) C16 0.0174(11) 0.0250(12) 0.0177(11) -0.0026(9) 0.0020(9) -0.0008(9) C17 0.0162(10) 0.0185(11) 0.0144(10) -0.0012(9) 0.0032(9) -0.0021(8) C18 0.0184(11) 0.0175(11) 0.0184(11) -0.0014(9) 0.0010(9) -0.0002(9) C19 0.0191(11) 0.0164(10) 0.0177(11) 0.0004(8) 0.0005(8) -0.0018(9) C20 0.0299(15) 0.0220(12) 0.0206(11) 0.0020(10) -0.0046(10) -0.0028(10) C21 0.0334(14) 0.0194(12) 0.0250(12) -0.0015(10) -0.0083(10) -0.0042(10) C22 0.0225(12) 0.0170(11) 0.0281(13) 0.0008(9) -0.0015(10) -0.0040(9) C23 0.0175(12) 0.0179(11) 0.0218(11) 0.0008(9) 0.0025(9) -0.0005(9) C24 0.0164(11) 0.0174(11) 0.0189(11) -0.0014(9) 0.0019(9) 0.0001(9) C25 0.0276(13) 0.0207(12) 0.0182(11) 0.0028(9) 0.0001(10) -0.0051(10) C26 0.0258(12) 0.0216(12) 0.0204(12) 0.0033(9) 0.0027(9) -0.0028(10) C27 0.0361(14) 0.0232(12) 0.0276(13) 0.0065(11) -0.0044(11) -0.0051(12) C28 0.0211(12) 0.0260(13) 0.0230(12) -0.0008(10) -0.0035(10) -0.0036(10) C29 0.0261(13) 0.0250(13) 0.0258(12) 0.0063(10) -0.0059(10) -0.0006(10) C30 0.0343(14) 0.0262(13) 0.0243(12) 0.0011(11) -0.0046(10) 0.0000(11) C31 0.0393(17) 0.0377(16) 0.0299(15) 0.0063(12) -0.0026(12) 0.0043(13) C32 0.0418(17) 0.0418(17) 0.0290(15) 0.0040(13) -0.0030(12) -0.0052(14) C33 0.055(2) 0.0326(15) 0.0311(16) 0.0044(12) -0.0044(13) -0.0036(14) C34 0.0388(17) 0.0412(17) 0.0394(16) 0.0078(13) 0.0001(14) -0.0019(14) C35 0.0402(18) 0.0357(16) 0.0462(17) 0.0030(13) -0.0074(14) -0.0039(14) C36 0.051(2) 0.051(2) 0.0394(17) 0.0075(16) -0.0030(15) 0.0016(17) C37 0.054(2) 0.051(2) 0.0446(19) -0.0018(16) -0.0098(16) -0.0057(17) C38 0.0414(18) 0.0388(18) 0.0474(18) -0.0067(15) -0.0002(15) -0.0111(14) C39 0.064(2) 0.054(2) 0.0436(19) -0.0143(17) 0.0033(18) -0.0037(19) C40 0.040(2) 0.084(3) 0.059(2) -0.029(2) 0.0134(17) -0.010(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 Ni O1 1.8346(16) . ? Ni O1 1.8347(16) 7_557 ? Ni N1 1.8368(19) . ? Ni N1 1.8368(19) 7_557 ? N1 C4 1.287(3) . ? N1 C3 1.486(3) . ? N2 C11 1.362(3) . ? N2 C12 1.402(3) . ? N3 C18 1.371(3) . ? N3 C17 1.421(3) . ? O1 C10 1.310(3) . ? O2 C11 1.225(3) . ? O3 C18 1.216(3) . ? O4 C24 1.361(3) . ? O4 C25 1.465(3) . ? O5 C28 1.199(3) . ? O6 C28 1.341(3) . ? O6 C29 1.453(3) . ? C1 C1 1.526(5) 7_557 ? C1 C2 1.530(4) . ? C2 C3 1.513(3) . ? C3 C3 1.526(4) 7_557 ? C4 C5 1.440(3) . ? C5 C6 1.402(3) . ? C5 C10 1.425(3) . ? C6 C7 1.381(3) . ? C7 C8 1.387(3) . ? C8 C9 1.395(3) . ? C9 C10 1.420(3) . ? C9 C11 1.498(3) . ? C12 C13 1.396(3) . ? C12 C17 1.403(3) . ? C13 C14 1.382(3) . ? C14 C15 1.380(4) . ? C15 C16 1.392(3) . ? C16 C17 1.396(3) . ? C16 C28 1.486(3) . ? C18 C19 1.504(3) . ? C19 C24 1.388(3) . ? C19 C20 1.402(3) . ? C20 C21 1.384(4) . ? C21 C22 1.398(4) . ? C22 C23 1.376(3) . ? C23 C24 1.387(3) . ? C23 C26 1.507(3) . ? C25 C26 1.535(3) . ? C26 C27 1.522(4) . ? C29 C30 1.499(4) . ? C30 C31 1.523(4) . ? C31 C32 1.524(4) . ? C32 C33 1.531(4) . ? C33 C34 1.528(4) . ? C34 C35 1.533(5) . ? C35 C36 1.496(4) . ? C36 C37 1.515(5) . ? C37 C38 1.488(5) . ? C38 C39 1.523(5) . ? C39 C40 1.522(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni O1 84.27(10) . 7_557 ? O1 Ni N1 94.75(8) . . ? O1 Ni N1 170.58(8) 7_557 . ? O1 Ni N1 170.58(8) . 7_557 ? O1 Ni N1 94.75(8) 7_557 7_557 ? N1 Ni N1 87.73(12) . 7_557 ? C4 N1 C3 121.25(19) . . ? C4 N1 Ni 127.17(16) . . ? C3 N1 Ni 111.30(14) . . ? C11 N2 C12 124.88(19) . . ? C18 N3 C17 122.38(19) . . ? C10 O1 Ni 129.00(14) . . ? C24 O4 C25 107.68(18) . . ? C28 O6 C29 115.7(2) . . ? C1 C1 C2 111.1(2) 7_557 . ? C3 C2 C1 109.1(2) . . ? N1 C3 C2 117.00(19) . . ? N1 C3 C3 104.47(14) . 7_557 ? C2 C3 C3 111.52(17) . 7_557 ? N1 C4 C5 124.8(2) . . ? C6 C5 C10 120.1(2) . . ? C6 C5 C4 118.0(2) . . ? C10 C5 C4 121.8(2) . . ? C7 C6 C5 121.1(2) . . ? C6 C7 C8 118.9(2) . . ? C7 C8 C9 122.3(2) . . ? C8 C9 C10 119.3(2) . . ? C8 C9 C11 116.1(2) . . ? C10 C9 C11 124.46(19) . . ? O1 C10 C9 120.0(2) . . ? O1 C10 C5 121.9(2) . . ? C9 C10 C5 118.1(2) . . ? O2 C11 N2 123.0(2) . . ? O2 C11 C9 121.0(2) . . ? N2 C11 C9 115.96(19) . . ? C13 C12 N2 121.1(2) . . ? C13 C12 C17 119.7(2) . . ? N2 C12 C17 119.2(2) . . ? C14 C13 C12 120.8(2) . . ? C15 C14 C13 119.9(2) . . ? C14 C15 C16 120.0(2) . . ? C15 C16 C17 120.8(2) . . ? C15 C16 C28 116.8(2) . . ? C17 C16 C28 122.4(2) . . ? C16 C17 C12 118.8(2) . . ? C16 C17 N3 120.2(2) . . ? C12 C17 N3 121.0(2) . . ? O3 C18 N3 122.7(2) . . ? O3 C18 C19 121.1(2) . . ? N3 C18 C19 116.2(2) . . ? C24 C19 C20 116.4(2) . . ? C24 C19 C18 126.6(2) . . ? C20 C19 C18 117.0(2) . . ? C21 C20 C19 121.9(2) . . ? C20 C21 C22 120.1(2) . . ? C23 C22 C21 118.8(2) . . ? C22 C23 C24 120.4(2) . . ? C22 C23 C26 130.2(2) . . ? C24 C23 C26 109.3(2) . . ? O4 C24 C23 113.1(2) . . ? O4 C24 C19 124.5(2) . . ? C23 C24 C19 122.4(2) . . ? O4 C25 C26 107.88(19) . . ? C23 C26 C27 113.2(2) . . ? C23 C26 C25 101.50(19) . . ? C27 C26 C25 113.3(2) . . ? O5 C28 O6 124.0(2) . . ? O5 C28 C16 124.3(2) . . ? O6 C28 C16 111.6(2) . . ? O6 C29 C30 108.8(2) . . ? C29 C30 C31 110.9(2) . . ? C30 C31 C32 113.9(3) . . ? C31 C32 C33 113.2(3) . . ? C34 C33 C32 115.1(3) . . ? C33 C34 C35 113.7(3) . . ? C36 C35 C34 114.4(3) . . ? C35 C36 C37 114.3(3) . . ? C38 C37 C36 114.2(3) . . ? C37 C38 C39 116.0(3) . . ? C40 C39 C38 114.6(3) . . ? 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 O1 Ni N1 C4 0.8(2) . . . . ? O1 Ni N1 C4 -82.8(5) 7_557 . . . ? N1 Ni N1 C4 171.7(3) 7_557 . . . ? O1 Ni N1 C3 174.63(15) . . . . ? O1 Ni N1 C3 91.0(5) 7_557 . . . ? N1 Ni N1 C3 -14.47(11) 7_557 . . . ? O1 Ni O1 C10 176.6(2) 7_557 . . . ? N1 Ni O1 C10 6.0(2) . . . . ? N1 Ni O1 C10 -99.0(5) 7_557 . . . ? C1 C1 C2 C3 56.8(4) 7_557 . . . ? C4 N1 C3 C2 -23.7(3) . . . . ? Ni N1 C3 C2 162.09(18) . . . . ? C4 N1 C3 C3 -147.5(2) . . . 7_557 ? Ni N1 C3 C3 38.3(3) . . . 7_557 ? C1 C2 C3 N1 -176.8(2) . . . . ? C1 C2 C3 C3 -56.7(3) . . . 7_557 ? C3 N1 C4 C5 -177.2(2) . . . . ? Ni N1 C4 C5 -4.0(3) . . . . ? N1 C4 C5 C6 -178.5(2) . . . . ? N1 C4 C5 C10 1.3(4) . . . . ? C10 C5 C6 C7 -1.3(4) . . . . ? C4 C5 C6 C7 178.5(2) . . . . ? C5 C6 C7 C8 -1.8(4) . . . . ? C6 C7 C8 C9 2.1(4) . . . . ? C7 C8 C9 C10 0.9(3) . . . . ? C7 C8 C9 C11 -175.1(2) . . . . ? Ni O1 C10 C9 171.62(15) . . . . ? Ni O1 C10 C5 -9.4(3) . . . . ? C8 C9 C10 O1 175.0(2) . . . . ? C11 C9 C10 O1 -9.3(3) . . . . ? C8 C9 C10 C5 -4.0(3) . . . . ? C11 C9 C10 C5 171.7(2) . . . . ? C6 C5 C10 O1 -174.8(2) . . . . ? C4 C5 C10 O1 5.4(3) . . . . ? C6 C5 C10 C9 4.2(3) . . . . ? C4 C5 C10 C9 -175.6(2) . . . . ? C12 N2 C11 O2 9.1(4) . . . . ? C12 N2 C11 C9 -168.1(2) . . . . ? C8 C9 C11 O2 0.4(3) . . . . ? C10 C9 C11 O2 -175.4(2) . . . . ? C8 C9 C11 N2 177.6(2) . . . . ? C10 C9 C11 N2 1.8(3) . . . . ? C11 N2 C12 C13 -42.1(3) . . . . ? C11 N2 C12 C17 140.1(2) . . . . ? N2 C12 C13 C14 -179.4(2) . . . . ? C17 C12 C13 C14 -1.6(3) . . . . ? C12 C13 C14 C15 1.2(4) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? C14 C15 C16 C17 -2.1(4) . . . . ? C14 C15 C16 C28 178.5(2) . . . . ? C15 C16 C17 C12 1.7(3) . . . . ? C28 C16 C17 C12 -178.9(2) . . . . ? C15 C16 C17 N3 -177.3(2) . . . . ? C28 C16 C17 N3 2.2(3) . . . . ? C13 C12 C17 C16 0.1(3) . . . . ? N2 C12 C17 C16 178.0(2) . . . . ? C13 C12 C17 N3 179.1(2) . . . . ? N2 C12 C17 N3 -3.0(3) . . . . ? C18 N3 C17 C16 119.3(3) . . . . ? C18 N3 C17 C12 -59.6(3) . . . . ? C17 N3 C18 O3 3.8(4) . . . . ? C17 N3 C18 C19 -177.6(2) . . . . ? O3 C18 C19 C24 -162.8(2) . . . . ? N3 C18 C19 C24 18.6(4) . . . . ? O3 C18 C19 C20 13.7(4) . . . . ? N3 C18 C19 C20 -164.8(2) . . . . ? C24 C19 C20 C21 -0.9(4) . . . . ? C18 C19 C20 C21 -177.8(2) . . . . ? C19 C20 C21 C22 0.5(4) . . . . ? C20 C21 C22 C23 0.2(4) . . . . ? C21 C22 C23 C24 -0.4(4) . . . . ? C21 C22 C23 C26 176.6(3) . . . . ? C25 O4 C24 C23 -5.3(3) . . . . ? C25 O4 C24 C19 173.2(2) . . . . ? C22 C23 C24 O4 178.4(2) . . . . ? C26 C23 C24 O4 0.9(3) . . . . ? C22 C23 C24 C19 -0.1(4) . . . . ? C26 C23 C24 C19 -177.6(2) . . . . ? C20 C19 C24 O4 -177.6(2) . . . . ? C18 C19 C24 O4 -1.0(4) . . . . ? C20 C19 C24 C23 0.7(4) . . . . ? C18 C19 C24 C23 177.3(2) . . . . ? C24 O4 C25 C26 7.4(3) . . . . ? C22 C23 C26 C27 -51.8(4) . . . . ? C24 C23 C26 C27 125.4(2) . . . . ? C22 C23 C26 C25 -173.6(3) . . . . ? C24 C23 C26 C25 3.6(3) . . . . ? O4 C25 C26 C23 -6.5(3) . . . . ? O4 C25 C26 C27 -128.3(2) . . . . ? C29 O6 C28 O5 0.2(4) . . . . ? C29 O6 C28 C16 178.0(2) . . . . ? C15 C16 C28 O5 51.8(4) . . . . ? C17 C16 C28 O5 -127.7(3) . . . . ? C15 C16 C28 O6 -126.0(2) . . . . ? C17 C16 C28 O6 54.5(3) . . . . ? C28 O6 C29 C30 -160.1(2) . . . . ? O6 C29 C30 C31 177.2(2) . . . . ? C29 C30 C31 C32 -177.9(3) . . . . ? C30 C31 C32 C33 169.3(3) . . . . ? C31 C32 C33 C34 -76.7(4) . . . . ? C32 C33 C34 C35 -78.9(3) . . . . ? C33 C34 C35 C36 -78.6(4) . . . . ? C34 C35 C36 C37 176.0(3) . . . . ? C35 C36 C37 C38 -72.3(4) . . . . ? C36 C37 C38 C39 -179.9(3) . . . . ? C37 C38 C39 C40 175.6(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 N2 H2A O1 0.88 1.89 2.603(2) 137.4 . N3 H3A O4 0.88 2.16 2.809(3) 129.8 . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.596 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.063