# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1458 # CIF for componds 3 and 4 only data_Compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H38 Cl2 N10 Ni2 O8' _chemical_formula_weight 1059.19 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.739(3) _cell_length_b 14.266(3) _cell_length_c 14.699(3) _cell_angle_alpha 77.00(3) _cell_angle_beta 84.61(3) _cell_angle_gamma 63.04(3) _cell_volume 2319.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description rod _exptl_crystal_colour crimson _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6922 _exptl_absorpt_correction_T_max 0.9072 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator beta-filter _diffrn_measurement_device_type CAD-4 _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% .7 _diffrn_reflns_number 3603 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 22.46 _reflns_number_total 3391 _reflns_number_gt 3391 _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 w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+1.7669P] 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 3391 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.007 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.15496(6) 0.30687(5) 0.35855(4) 0.0424(2) Uani 1 d . . . Ni2 Ni 0.05401(6) 0.16359(5) 0.31432(4) 0.0414(2) Uani 1 d . . . O1 O 0.1439(3) 0.0160(3) 0.2873(2) 0.0482(9) Uani 1 d . . . O2 O 0.2491(3) 0.2794(3) 0.4735(2) 0.0459(9) Uani 1 d . . . O3 O 0.3263(4) 0.0053(4) 0.0331(3) 0.0886(15) Uani 1 d . . . O4 O 0.0520(5) 0.2845(4) 0.7175(3) 0.0825(14) Uani 1 d . . . O1' O -0.1187(3) 0.2124(3) 0.2920(2) 0.0480(9) Uani 1 d . . . O2' O 0.1608(3) 0.4373(3) 0.2757(2) 0.0480(9) Uani 1 d . . . O3' O -0.3243(4) 0.2736(4) 0.5308(3) 0.0859(15) Uani 1 d . . . O4' O 0.3947(4) 0.3689(3) 0.0520(3) 0.0797(14) Uani 1 d . . . N1 N -0.0124(4) 0.3586(3) 0.2764(3) 0.0478(11) Uani 1 d . . . N2 N 0.1043(4) 0.1968(4) 0.1862(3) 0.0466(11) Uani 1 d . . . N3 N 0.1814(4) 0.1101(4) 0.1493(3) 0.0513(12) Uani 1 d . . . N4 N 0.0283(4) 0.3601(3) 0.4480(3) 0.0451(11) Uani 1 d . . . N5 N 0.0641(4) 0.3385(3) 0.5385(3) 0.0473(11) Uani 1 d . . . N1' N 0.2158(4) 0.1148(3) 0.4046(3) 0.0431(11) Uani 1 d . . . N2' N -0.0023(4) 0.1471(3) 0.4424(3) 0.0412(11) Uani 1 d . . . N3' N -0.1226(4) 0.1906(3) 0.4532(3) 0.0437(11) Uani 1 d . . . N4' N 0.2840(4) 0.2392(3) 0.2749(3) 0.0427(11) Uani 1 d . . . N5' N 0.2998(4) 0.3087(3) 0.2000(3) 0.0470(11) Uani 1 d . . . C1 C -0.0224(5) 0.3742(4) 0.1837(4) 0.0514(15) Uani 1 d . . . C2 C -0.1207(6) 0.4584(5) 0.1342(5) 0.0696(18) Uani 1 d . . . C3 C -0.2112(7) 0.5214(5) 0.1832(6) 0.078(2) Uani 1 d . . . C4 C -0.2023(6) 0.5039(5) 0.2779(6) 0.0699(19) Uani 1 d . . . C5 C -0.1015(5) 0.4245(4) 0.3249(4) 0.0486(14) Uani 1 d . . . C6 C 0.0656(5) 0.2923(5) 0.1360(4) 0.0504(14) Uani 1 d . . . C7 C -0.0814(5) 0.4098(4) 0.4244(4) 0.0497(15) Uani 1 d . . . C8 C 0.1014(7) 0.3171(5) 0.0372(4) 0.081(2) Uani 1 d . . . C9 C -0.1787(5) 0.4502(5) 0.4909(5) 0.0693(18) Uani 1 d . . . C10 C 0.1945(5) 0.0195(4) 0.2092(4) 0.0485(14) Uani 1 d . . . C11 C 0.2739(5) -0.0818(5) 0.1793(4) 0.0520(15) Uani 1 d . . . C12 C 0.2899(6) -0.1781(5) 0.2364(5) 0.0704(18) Uani 1 d . . . C13 C 0.3610(7) -0.2746(6) 0.2107(6) 0.092(2) Uani 1 d . . . C14 C 0.4186(7) -0.2750(7) 0.1288(7) 0.100(3) Uani 1 d . . . C15 C 0.4066(7) -0.1835(7) 0.0707(5) 0.088(2) Uani 1 d . . . C16 C 0.3347(5) -0.0840(6) 0.0945(4) 0.0668(19) Uani 1 d . . . C17 C 0.1806(5) 0.2956(4) 0.5436(4) 0.0459(14) Uani 1 d . . . C18 C 0.2325(5) 0.2639(4) 0.6389(4) 0.0460(14) Uani 1 d . . . C19 C 0.3498(5) 0.2386(4) 0.6477(4) 0.0551(15) Uani 1 d . . . C20 C 0.4034(6) 0.2065(5) 0.7350(5) 0.0735(19) Uani 1 d . . . C21 C 0.3383(8) 0.1963(6) 0.8132(5) 0.087(2) Uani 1 d . . . C22 C 0.2219(8) 0.2218(6) 0.8055(5) 0.081(2) Uani 1 d . . . C23 C 0.1669(7) 0.2575(5) 0.7193(4) 0.0629(17) Uani 1 d . . . C1' C 0.1920(5) 0.0652(4) 0.4881(4) 0.0438(13) Uani 1 d . . . C2' C 0.2805(6) -0.0233(4) 0.5426(4) 0.0570(15) Uani 1 d . . . C3' C 0.3914(6) -0.0654(5) 0.5085(5) 0.0642(17) Uani 1 d . . . C4' C 0.4158(5) -0.0174(4) 0.4225(4) 0.0559(16) Uani 1 d . . . C5' C 0.3282(5) 0.0741(4) 0.3734(4) 0.0462(14) Uani 1 d . . . C6' C 0.0666(5) 0.1049(4) 0.5136(4) 0.0441(13) Uani 1 d . . . C7' C 0.3529(5) 0.1380(4) 0.2875(4) 0.0473(14) Uani 1 d . . . C8' C 0.0283(5) 0.0917(5) 0.6127(4) 0.0596(16) Uani 1 d . . . C9' C 0.4534(6) 0.0899(5) 0.2258(5) 0.077(2) Uani 1 d . . . C10' C -0.1739(5) 0.2250(4) 0.3687(4) 0.0414(13) Uani 1 d . . . C11' C -0.3032(5) 0.2853(4) 0.3666(4) 0.0471(14) Uani 1 d . . . C12' C -0.3616(6) 0.3239(6) 0.2806(5) 0.0703(18) Uani 1 d . . . C13' C -0.4817(7) 0.3835(7) 0.2733(6) 0.094(2) Uani 1 d . . . C14' C -0.5461(6) 0.4053(7) 0.3517(7) 0.094(2) Uani 1 d . . . C15' C -0.4935(6) 0.3688(6) 0.4379(5) 0.078(2) Uani 1 d . . . C16' C -0.3715(5) 0.3084(5) 0.4454(4) 0.0595(16) Uani 1 d . . . C17' C 0.2301(5) 0.4106(4) 0.2078(4) 0.0434(13) Uani 1 d . . . C18' C 0.2387(5) 0.4944(4) 0.1322(4) 0.0447(13) Uani 1 d . . . C19' C 0.1651(6) 0.6003(5) 0.1332(4) 0.0641(17) Uani 1 d . . . C20' C 0.1706(7) 0.6815(5) 0.0647(5) 0.084(2) Uani 1 d . . . C21' C 0.2542(7) 0.6557(6) -0.0048(5) 0.083(2) Uani 1 d . . . C22' C 0.3269(6) 0.5528(6) -0.0069(4) 0.0704(19) Uani 1 d . . . C23' C 0.3209(5) 0.4702(5) 0.0602(4) 0.0556(16) Uani 1 d . . . Cl1 Cl 0.7458(3) 0.0743(3) 0.1774(2) 0.1489(11) Uani 1 d . . . Cl2A Cl 0.9641(7) 0.0408(7) 0.1166(5) 0.147(2) Uani 0.50 d P . . Cl2B Cl 0.9824(7) -0.0524(8) 0.1357(5) 0.185(4) Uani 0.50 d P . . C24 C 0.8629(11) 0.0131(14) 0.1031(12) 0.211(7) Uani 1 d . . . H3O H 0.2885 0.0608 0.0597 0.050 Uiso 1 d . . . H4O H 0.0228 0.3128 0.6489 0.050 Uiso 1 d . . . H2 H -0.1240 0.4712 0.0675 0.080 Uiso 1 d . . . H3 H -0.2818 0.5787 0.1508 0.080 Uiso 1 d . . . H4 H -0.2674 0.5475 0.3128 0.080 Uiso 1 d . . . H81 H 0.1599 0.2512 0.0200 0.080 Uiso 1 d . . . H82 H 0.0339 0.3467 -0.0034 0.080 Uiso 1 d . . . H83 H 0.1336 0.3667 0.0307 0.080 Uiso 1 d . . . H91 H -0.1482 0.4322 0.5522 0.080 Uiso 1 d . . . H92 H -0.2233 0.5264 0.4716 0.080 Uiso 1 d . . . H93 H -0.2306 0.4169 0.4902 0.080 Uiso 1 d . . . H12 H 0.2491 -0.1777 0.2948 0.080 Uiso 1 d . . . H13 H 0.3717 -0.3418 0.2521 0.080 Uiso 1 d . . . H14 H 0.4689 -0.3415 0.1111 0.080 Uiso 1 d . . . H15 H 0.4483 -0.1855 0.0121 0.080 Uiso 1 d . . . H19 H 0.3949 0.2430 0.5932 0.080 Uiso 1 d . . . H20 H 0.4834 0.1917 0.7401 0.080 Uiso 1 d . . . H21 H 0.3755 0.1708 0.8735 0.080 Uiso 1 d . . . H22 H 0.1793 0.2147 0.8608 0.080 Uiso 1 d . . . H3O' H -0.2331 0.2232 0.5304 0.050 Uiso 1 d . . . H4O' H 0.3817 0.3225 0.1101 0.050 Uiso 1 d . . . H2' H 0.2634 -0.0544 0.6040 0.080 Uiso 1 d . . . H3' H 0.4528 -0.1287 0.5440 0.080 Uiso 1 d . . . H4' H 0.4928 -0.0482 0.3971 0.080 Uiso 1 d . . . H81' H -0.0563 0.1226 0.6150 0.080 Uiso 1 d . . . H82' H 0.0607 0.0167 0.6413 0.080 Uiso 1 d . . . H83' H 0.0552 0.1275 0.6460 0.080 Uiso 1 d . . . H91' H 0.4533 0.1460 0.1736 0.080 Uiso 1 d . . . H92' H 0.5263 0.0586 0.2589 0.080 Uiso 1 d . . . H93' H 0.4455 0.0366 0.2012 0.080 Uiso 1 d . . . H12 H -0.3166 0.3083 0.2253 0.080 Uiso 1 d . . . H13 H -0.5190 0.4084 0.2143 0.080 Uiso 1 d . . . H14 H -0.6293 0.4465 0.3462 0.080 Uiso 1 d . . . H15 H -0.5402 0.3843 0.4920 0.080 Uiso 1 d . . . H19 H 0.1093 0.6188 0.1822 0.080 Uiso 1 d . . . H20 H 0.1158 0.7549 0.0638 0.080 Uiso 1 d . . . H21 H 0.2605 0.7117 -0.0512 0.080 Uiso 1 d . . . H22 H 0.3837 0.5364 -0.0555 0.080 Uiso 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 Ni1 0.0413(4) 0.0439(4) 0.0434(4) -0.0141(3) 0.0126(3) -0.0200(3) Ni2 0.0410(4) 0.0418(4) 0.0409(4) -0.0118(3) 0.0090(3) -0.0181(3) O1 0.055(2) 0.043(2) 0.046(2) -0.0148(17) 0.0143(18) -0.0221(18) O2 0.041(2) 0.054(2) 0.044(2) -0.0183(17) 0.0123(17) -0.0217(18) O3 0.096(4) 0.105(4) 0.054(3) -0.029(3) 0.027(2) -0.034(3) O4 0.084(4) 0.123(4) 0.056(3) -0.035(3) 0.028(2) -0.057(3) O1' 0.042(2) 0.058(2) 0.045(2) -0.0147(17) 0.0053(18) -0.0217(18) O2' 0.051(2) 0.042(2) 0.050(2) -0.0158(17) 0.0177(19) -0.0210(18) O3' 0.057(3) 0.108(4) 0.061(3) -0.014(3) 0.015(2) -0.014(3) O4' 0.090(3) 0.069(3) 0.064(3) -0.017(2) 0.041(2) -0.028(3) N1 0.044(3) 0.041(3) 0.057(3) -0.008(2) 0.002(2) -0.020(2) N2 0.047(3) 0.050(3) 0.046(3) -0.013(2) 0.011(2) -0.025(2) N3 0.056(3) 0.054(3) 0.043(3) -0.015(2) 0.012(2) -0.023(2) N4 0.045(3) 0.041(2) 0.048(3) -0.014(2) 0.012(2) -0.018(2) N5 0.042(3) 0.046(3) 0.051(3) -0.015(2) 0.014(2) -0.018(2) N1' 0.039(3) 0.043(3) 0.049(3) -0.013(2) 0.006(2) -0.019(2) N2' 0.043(3) 0.039(2) 0.041(3) -0.010(2) 0.003(2) -0.018(2) N3' 0.037(3) 0.048(3) 0.043(3) -0.008(2) 0.008(2) -0.018(2) N4' 0.044(3) 0.042(3) 0.044(3) -0.015(2) 0.011(2) -0.020(2) N5' 0.052(3) 0.043(3) 0.047(3) -0.014(2) 0.013(2) -0.022(2) C1 0.053(4) 0.048(3) 0.052(4) 0.000(3) -0.006(3) -0.025(3) C2 0.079(5) 0.046(4) 0.079(5) 0.002(3) -0.020(4) -0.027(4) C3 0.080(5) 0.045(4) 0.092(6) -0.005(4) -0.031(4) -0.011(4) C4 0.053(4) 0.043(4) 0.110(6) -0.024(4) -0.006(4) -0.012(3) C5 0.041(4) 0.035(3) 0.069(4) -0.011(3) 0.000(3) -0.016(3) C6 0.055(4) 0.052(4) 0.047(3) -0.003(3) -0.001(3) -0.029(3) C7 0.039(4) 0.032(3) 0.074(4) -0.016(3) 0.012(3) -0.011(3) C8 0.119(6) 0.070(4) 0.049(4) 0.001(3) 0.006(4) -0.046(4) C9 0.052(4) 0.059(4) 0.093(5) -0.029(3) 0.024(3) -0.019(3) C10 0.049(4) 0.058(4) 0.044(3) -0.021(3) 0.012(3) -0.026(3) C11 0.048(4) 0.057(4) 0.048(3) -0.020(3) 0.003(3) -0.016(3) C12 0.057(4) 0.066(4) 0.077(5) -0.028(4) 0.012(3) -0.015(3) C13 0.093(6) 0.062(5) 0.106(6) -0.036(4) 0.007(5) -0.014(4) C14 0.086(6) 0.081(6) 0.121(7) -0.068(6) 0.006(5) -0.005(5) C15 0.070(5) 0.103(6) 0.077(5) -0.059(5) 0.013(4) -0.010(5) C16 0.050(4) 0.093(5) 0.052(4) -0.038(4) 0.004(3) -0.017(4) C17 0.061(4) 0.039(3) 0.047(3) -0.020(2) 0.019(3) -0.028(3) C18 0.062(5) 0.036(3) 0.043(3) -0.016(2) 0.009(3) -0.023(3) C19 0.052(4) 0.043(3) 0.061(4) -0.016(3) 0.001(3) -0.011(3) C20 0.072(5) 0.053(4) 0.077(5) -0.014(3) -0.014(4) -0.010(3) C21 0.110(7) 0.064(5) 0.060(5) -0.014(4) -0.010(5) -0.014(5) C22 0.113(7) 0.076(5) 0.049(4) -0.023(3) 0.012(4) -0.036(5) C23 0.086(6) 0.062(4) 0.047(4) -0.024(3) 0.013(4) -0.034(4) C1' 0.049(4) 0.041(3) 0.044(3) -0.008(3) -0.002(3) -0.023(3) C2' 0.059(4) 0.045(3) 0.061(4) 0.000(3) -0.009(3) -0.021(3) C3' 0.050(4) 0.044(3) 0.082(5) 0.000(3) -0.010(3) -0.011(3) C4' 0.046(4) 0.044(3) 0.073(4) -0.013(3) 0.000(3) -0.016(3) C5' 0.037(4) 0.041(3) 0.067(4) -0.022(3) 0.002(3) -0.018(3) C6' 0.049(4) 0.040(3) 0.046(3) -0.010(2) 0.006(3) -0.022(3) C7' 0.039(3) 0.042(3) 0.059(4) -0.016(3) 0.012(3) -0.017(3) C8' 0.061(4) 0.074(4) 0.048(3) -0.006(3) 0.008(3) -0.037(3) C9' 0.061(4) 0.063(4) 0.086(5) -0.024(4) 0.030(4) -0.011(3) C10' 0.041(4) 0.038(3) 0.049(4) -0.011(2) 0.008(3) -0.022(3) C11' 0.041(4) 0.048(3) 0.057(4) -0.011(3) 0.006(3) -0.025(3) C12' 0.044(4) 0.089(5) 0.072(4) -0.019(4) -0.005(3) -0.022(4) C13' 0.053(5) 0.135(7) 0.085(5) -0.025(5) -0.008(4) -0.031(5) C14' 0.039(4) 0.099(6) 0.120(7) -0.014(5) -0.007(5) -0.013(4) C15' 0.040(4) 0.079(5) 0.092(5) -0.014(4) 0.026(4) -0.013(4) C16' 0.054(4) 0.061(4) 0.055(4) -0.007(3) 0.012(3) -0.023(3) C17' 0.041(3) 0.054(4) 0.043(3) -0.015(3) 0.007(3) -0.028(3) C18' 0.047(3) 0.052(3) 0.043(3) -0.012(3) 0.007(3) -0.029(3) C19' 0.069(4) 0.054(4) 0.063(4) -0.015(3) 0.019(3) -0.025(3) C20' 0.107(6) 0.051(4) 0.081(5) -0.002(4) 0.013(4) -0.032(4) C21' 0.110(6) 0.075(5) 0.069(5) 0.000(4) 0.020(4) -0.056(5) C22' 0.083(5) 0.086(5) 0.049(4) -0.012(3) 0.020(3) -0.047(4) C23' 0.058(4) 0.063(4) 0.049(4) -0.016(3) 0.014(3) -0.031(3) Cl1 0.112(2) 0.187(3) 0.130(2) -0.021(2) 0.0084(16) -0.057(2) Cl2A 0.132(6) 0.160(6) 0.159(6) -0.028(5) -0.018(4) -0.071(5) Cl2B 0.126(6) 0.209(8) 0.140(6) -0.060(6) 0.001(4) 0.005(6) C24 0.086(9) 0.265(18) 0.264(18) -0.043(14) -0.022(10) -0.065(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 Ni1 N4 1.962(4) . ? Ni1 N4' 1.965(4) . ? Ni1 O2' 2.010(3) . ? Ni1 O2 2.026(4) . ? Ni1 N1 2.281(5) . ? Ni1 N1' 2.430(4) . ? Ni2 N1 2.454(4) . ? Ni2 N2' 1.953(4) . ? Ni2 N2 1.956(4) . ? Ni2 O1 2.002(3) . ? Ni2 O1' 2.019(4) . ? Ni2 N1' 2.300(4) . ? O1 C10 1.266(6) . ? O2 C17 1.277(6) . ? O3 C16 1.351(8) . ? O4 C23 1.335(8) . ? O1' C10' 1.276(6) . ? O2' C17' 1.273(6) . ? O3' C16' 1.332(7) . ? O4' C23' 1.346(7) . ? N1 C1 1.340(7) . ? N1 C5 1.364(7) . ? N2 C6 1.285(7) . ? N2 N3 1.375(6) . ? N3 C10 1.340(7) . ? N4 C7 1.288(7) . ? N4 N5 1.369(6) . ? N5 C17 1.327(7) . ? N1' C1' 1.354(6) . ? N1' C5' 1.357(7) . ? N2' C6' 1.279(6) . ? N2' N3' 1.377(6) . ? N3' C10' 1.340(7) . ? N4' C7' 1.284(6) . ? N4' N5' 1.373(6) . ? N5' C17' 1.342(7) . ? C1 C2 1.398(8) . ? C1 C6 1.466(8) . ? C2 C3 1.361(10) . ? C3 C4 1.365(10) . ? C4 C5 1.380(8) . ? C5 C7 1.460(8) . ? C6 C8 1.494(8) . ? C7 C9 1.484(8) . ? C10 C11 1.477(8) . ? C11 C12 1.376(9) . ? C11 C16 1.403(8) . ? C12 C13 1.377(9) . ? C13 C14 1.349(12) . ? C14 C15 1.341(11) . ? C15 C16 1.401(9) . ? C17 C18 1.491(8) . ? C18 C19 1.381(8) . ? C18 C23 1.393(8) . ? C19 C20 1.392(9) . ? C20 C21 1.373(10) . ? C21 C22 1.367(11) . ? C22 C23 1.381(9) . ? C1' C2' 1.389(7) . ? C1' C6' 1.475(8) . ? C2' C3' 1.357(9) . ? C3' C4' 1.375(8) . ? C4' C5' 1.370(8) . ? C5' C7' 1.481(8) . ? C6' C8' 1.491(7) . ? C7' C9' 1.483(8) . ? C10' C11' 1.471(7) . ? C11' C16' 1.389(8) . ? C11' C12' 1.395(8) . ? C12' C13' 1.373(9) . ? C13' C14' 1.360(11) . ? C14' C15' 1.369(11) . ? C15' C16' 1.394(9) . ? C17' C18' 1.475(7) . ? C18' C19' 1.373(8) . ? C18' C23' 1.402(7) . ? C19' C20' 1.376(9) . ? C20' C21' 1.387(10) . ? C21' C22' 1.340(9) . ? C22' C23' 1.382(8) . ? Cl1 C24 1.767(16) . ? Cl2A Cl2B 1.209(10) . ? Cl2A C24 1.549(15) . ? Cl2B C24 1.438(13) . ? 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 N4 Ni1 N4' 174.34(18) . . ? N4 Ni1 O2' 106.31(16) . . ? N4' Ni1 O2' 79.35(16) . . ? N4 Ni1 O2 79.06(17) . . ? N4' Ni1 O2 99.86(16) . . ? O2' Ni1 O2 104.37(15) . . ? N4 Ni1 N1 76.14(18) . . ? N4' Ni1 N1 104.64(17) . . ? O2' Ni1 N1 84.49(15) . . ? O2 Ni1 N1 155.14(15) . . ? N4 Ni1 N1' 100.53(16) . . ? N4' Ni1 N1' 73.81(16) . . ? O2' Ni1 N1' 153.05(14) . . ? O2 Ni1 N1' 82.80(15) . . ? N1 Ni1 N1' 99.88(15) . . ? N2' Ni2 N2 173.70(17) . . ? N2' Ni2 O1 107.14(16) . . ? N2 Ni2 O1 79.10(17) . . ? N2' Ni2 O1' 79.06(17) . . ? N2 Ni2 O1' 100.08(17) . . ? O1 Ni2 O1' 108.04(15) . . ? N2' Ni2 N1' 75.80(17) . . ? N2 Ni2 N1' 104.37(17) . . ? N1 Ni2 N2 73.92(16) . . ? N1 Ni2 N2 99.80(16) . . ? N1 Ni2 N1 98.64(17) . . ? N1 Ni2 O1 152.73(17) . . ? N1 Ni2 O1 80.86(16) . . ? Ni2 N1 Ni1 89.74(13) . . ? O1 Ni2 N1' 84.17(15) . . ? O1' Ni2 N1' 154.41(15) . . ? C10 O1 Ni2 110.6(3) . . ? C17 O2 Ni1 109.4(3) . . ? C10' O1' Ni2 109.3(3) . . ? C17' O2' Ni1 110.2(3) . . ? C1 N1 C5 119.6(5) . . ? C1 N1 Ni1 126.7(4) . . ? C5 N1 Ni1 105.2(3) . . ? C6 N2 N3 120.2(4) . . ? C6 N2 Ni2 123.8(4) . . ? N3 N2 Ni2 116.0(3) . . ? C10 N3 N2 109.0(4) . . ? C7 N4 N5 121.8(4) . . ? C7 N4 Ni1 122.7(4) . . ? N5 N4 Ni1 115.4(3) . . ? C17 N5 N4 110.3(4) . . ? C1' N1' C5' 118.4(4) . . ? C1' N1' Ni2 103.5(3) . . ? C5' N1' Ni2 123.9(3) . . ? C1' N1' Ni1 124.6(3) . . ? C5' N1' Ni1 101.6(3) . . ? Ni2 N1' Ni1 80.73(14) . . ? C6' N2' N3' 120.8(4) . . ? C6' N2' Ni2 122.9(4) . . ? N3' N2' Ni2 116.2(3) . . ? C10' N3' N2' 108.9(4) . . ? C7' N4' N5' 120.1(4) . . ? C7' N4' Ni1 124.6(4) . . ? N5' N4' Ni1 115.2(3) . . ? C17' N5' N4' 110.0(4) . . ? N1 C1 C2 121.8(6) . . ? N1 C1 C6 118.0(5) . . ? C2 C1 C6 119.7(5) . . ? C3 C2 C1 118.3(6) . . ? C2 C3 C4 119.8(6) . . ? C3 C4 C5 120.9(6) . . ? N1 C5 C4 119.4(6) . . ? N1 C5 C7 117.1(5) . . ? C4 C5 C7 123.4(6) . . ? N2 C6 C1 113.1(5) . . ? N2 C6 C8 123.7(5) . . ? C1 C6 C8 123.1(5) . . ? N4 C7 C5 113.5(5) . . ? N4 C7 C9 123.7(6) . . ? C5 C7 C9 122.8(5) . . ? O1 C10 N3 124.7(5) . . ? O1 C10 C11 119.4(5) . . ? N3 C10 C11 116.0(5) . . ? C12 C11 C16 118.3(6) . . ? C12 C11 C10 119.3(5) . . ? C16 C11 C10 122.5(6) . . ? C11 C12 C13 121.4(6) . . ? C14 C13 C12 119.4(7) . . ? C15 C14 C13 121.6(7) . . ? C14 C15 C16 120.5(7) . . ? O3 C16 C15 117.7(6) . . ? O3 C16 C11 123.6(6) . . ? C15 C16 C11 118.8(7) . . ? O2 C17 N5 124.7(5) . . ? O2 C17 C18 119.1(5) . . ? N5 C17 C18 116.2(5) . . ? C19 C18 C23 118.9(6) . . ? C19 C18 C17 119.0(5) . . ? C23 C18 C17 122.1(6) . . ? C18 C19 C20 121.4(6) . . ? C21 C20 C19 118.6(7) . . ? C22 C21 C20 120.6(7) . . ? C21 C22 C23 121.2(7) . . ? O4 C23 C22 117.8(6) . . ? O4 C23 C18 123.0(6) . . ? C22 C23 C18 119.2(7) . . ? N1' C1' C2' 121.3(5) . . ? N1' C1' C6' 116.1(5) . . ? C2' C1' C6' 122.4(5) . . ? C3' C2' C1' 119.2(5) . . ? C2' C3' C4' 119.8(5) . . ? C5' C4' C3' 119.5(5) . . ? N1' C5' C4' 121.6(5) . . ? N1' C5' C7' 116.5(5) . . ? C4' C5' C7' 121.8(5) . . ? N2' C6' C1' 112.9(5) . . ? N2' C6' C8' 125.1(5) . . ? C1' C6' C8' 121.9(5) . . ? N4' C7' C5' 113.8(5) . . ? N4' C7' C9' 123.4(5) . . ? C5' C7' C9' 122.6(5) . . ? O1' C10' N3' 124.8(5) . . ? O1' C10' C11' 119.1(5) . . ? N3' C10' C11' 116.1(5) . . ? C16' C11' C12' 117.3(5) . . ? C16' C11' C10' 123.9(5) . . ? C12' C11' C10' 118.7(5) . . ? C13' C12' C11' 121.8(6) . . ? C14' C13' C12' 119.4(7) . . ? C13' C14' C15' 121.3(6) . . ? C14' C15' C16' 119.3(6) . . ? O3' C16' C11' 122.0(5) . . ? O3' C16' C15' 117.2(6) . . ? C11' C16' C15' 120.9(6) . . ? O2' C17' N5' 124.2(5) . . ? O2' C17' C18' 119.9(5) . . ? N5' C17' C18' 115.9(4) . . ? C19' C18' C23' 118.6(5) . . ? C19' C18' C17' 118.9(5) . . ? C23' C18' C17' 122.5(5) . . ? C18' C19' C20' 121.1(6) . . ? C19' C20' C21' 119.3(6) . . ? C22' C21' C20' 120.5(6) . . ? C21' C22' C23' 121.0(6) . . ? O4' C23' C22' 117.5(5) . . ? O4' C23' C18' 122.9(5) . . ? C22' C23' C18' 119.5(6) . . ? Cl2B Cl2A C24 61.4(8) . . ? Cl2A Cl2B C24 71.1(8) . . ? Cl2B C24 Cl2A 47.6(6) . . ? Cl2B C24 Cl1 122.8(11) . . ? Cl2A C24 Cl1 108.7(11) . . ? _diffrn_measured_fraction_theta_max 0.561 _diffrn_reflns_theta_full 22.46 _diffrn_measured_fraction_theta_full 0.561 _refine_diff_density_max 0.693 _refine_diff_density_min -0.456 _refine_diff_density_rms 0.060 data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28.50 H25 Cl N6 Ni O4' _chemical_formula_weight 609.70 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 '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 (No 15)' 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 20.993(4) _cell_length_b 20.649(4) _cell_length_c 16.821(3) _cell_angle_alpha 90.00 _cell_angle_beta 122.32(2) _cell_angle_gamma 90.00 _cell_volume 6162.0(20) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2696 _exptl_absorpt_coefficient_mu 2.135 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet P3' _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 51 _diffrn_reflns_number 2791 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 6.23 _diffrn_reflns_theta_max 57.42 _reflns_number_total 2791 _reflns_number_observed 2772 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.3265P)^2^+68.8911P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2791 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_obs 0.1232 _refine_ls_wR_factor_all 0.3253 _refine_ls_wR_factor_obs 0.3245 _refine_ls_goodness_of_fit_all 0.826 _refine_ls_goodness_of_fit_obs 0.827 _refine_ls_restrained_S_all 0.826 _refine_ls_restrained_S_obs 0.827 _refine_ls_shift/esd_max 1.651 _refine_ls_shift/esd_mean 0.620 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.5000 0.05830(14) 0.2500 0.0662(13) Uani 1 d S . Ni2 Ni 0.5000 0.27670(14) 0.2500 0.0679(13) Uani 1 d S . O1 O 0.4175(6) -0.0110(4) 0.2278(8) 0.073(3) Uani 1 d . . O2 O 0.2902(7) -0.0815(6) -0.0446(10) 0.106(4) Uani 1 d . . O3 O 0.5158(5) 0.2805(5) 0.1407(7) 0.072(3) Uani 1 d . . O4 O 0.3256(6) 0.2307(7) -0.1209(8) 0.098(4) Uani 1 d . . N1 N 0.4462(6) 0.1248(5) 0.2968(8) 0.064(3) Uani 1 d . . N2 N 0.4416(6) 0.0458(6) 0.1112(9) 0.070(3) Uani 1 d . . N3 N 0.3813(6) 0.0029(6) 0.0725(9) 0.072(3) Uani 1 d . . N4 N 0.5830(7) 0.3512(6) 0.3153(9) 0.083(4) Uani 1 d . . N5 N 0.4135(7) 0.2141(5) 0.1466(9) 0.067(3) Uani 1 d . . N6 N 0.3992(6) 0.2283(6) 0.0575(9) 0.066(3) Uani 1 d . . C1 C 0.4693(8) 0.1133(6) 0.3880(10) 0.063(4) Uani 1 d . . C2 C 0.4305(10) 0.1364(8) 0.4251(11) 0.077(4) Uani 1 d . . C3 C 0.3656(9) 0.1694(7) 0.3738(13) 0.079(4) Uani 1 d . . C4 C 0.3408(9) 0.1816(7) 0.2808(16) 0.080(5) Uani 1 d . . C5 C 0.3840(8) 0.1610(6) 0.2445(11) 0.063(4) Uani 1 d . . C6 C 0.5392(8) 0.0732(6) 0.4426(10) 0.063(3) Uani 1 d . . C7 C 0.5775(10) 0.0652(8) 0.5451(12) 0.086(5) Uani 1 d . . C8 C 0.3768(9) -0.0238(7) 0.1419(12) 0.072(4) Uani 1 d . . C9 C 0.3177(8) -0.0750(7) 0.1117(12) 0.073(4) Uani 1 d . . C10 C 0.2791(10) -0.0996(8) 0.0192(14) 0.077(5) Uani 1 d . . C11 C 0.2263(10) -0.1486(9) -0.0047(16) 0.109(6) Uani 1 d . . C12 C 0.2127(11) -0.1735(9) 0.0584(21) 0.119(7) Uani 1 d . . C13 C 0.2524(13) -0.1518(11) 0.1510(19) 0.113(7) Uani 1 d . . C14 C 0.3026(10) -0.1008(9) 0.1749(14) 0.092(5) Uani 1 d . . C15 C 0.5748(13) 0.4008(9) 0.3622(16) 0.111(7) Uani 1 d . . C16 C 0.6208(18) 0.4536(10) 0.3897(20) 0.133(9) Uani 1 d . . C17 C 0.6755(16) 0.4558(13) 0.3728(20) 0.148(10) Uani 1 d . . C18 C 0.6869(12) 0.4057(12) 0.3281(16) 0.123(7) Uani 1 d . . C19 C 0.6395(10) 0.3535(9) 0.3020(14) 0.099(6) Uani 1 d . . C20 C 0.4563(8) 0.2631(6) 0.0640(11) 0.066(4) Uani 1 d . . C21 C 0.4463(8) 0.2817(7) -0.0256(11) 0.071(4) Uani 1 d . . C22 C 0.3817(9) 0.2663(8) -0.1144(12) 0.078(4) Uani 1 d . . C23 C 0.3762(10) 0.2866(10) -0.1971(13) 0.095(5) Uani 1 d . . C24 C 0.4301(12) 0.3236(10) -0.1924(13) 0.108(6) Uani 1 d . . C25 C 0.4949(12) 0.3406(10) -0.1056(15) 0.103(6) Uani 1 d . . C26 C 0.5015(9) 0.3212(9) -0.0249(12) 0.085(5) Uani 1 d . . C27 C 0.3654(7) 0.1773(6) 0.1512(10) 0.062(3) Uani 1 d . . C28 C 0.2935(10) 0.1550(9) 0.0671(13) 0.091(5) Uani 1 d . . C29 C 0.5000 0.1598(16) 0.7500 0.217(15) Uani 1 d S . Cl3A Cl 0.4340(6) 0.2023(5) 0.6446(7) 0.102(3) Uani 0.50 d P . Cl3B Cl 0.4761(6) 0.1745(5) 0.6609(7) 0.144(3) Uani 0.50 d P . Cl1 Cl 0.5946(7) 0.4746(8) 0.0904(10) 0.146(5) Uani 0.50 d P . Cl2 Cl 0.7288(7) 0.5456(5) 0.2188(11) 0.152(5) Uani 0.50 d P . C30 C 0.6413(81) 0.5402(52) 0.1251(47) 0.311(90) Uani 0.50 d P . H2 H 0.4469 0.1365 0.4769 0.023 Uiso 1 d . . H3 H 0.3374 0.1858 0.3986 0.080 Uiso 1 d . . H4 H 0.3109 0.1975 0.2455 0.080 Uiso 1 d . . H71 H 0.5364 0.0482 0.5483 0.080 Uiso 1 d . . H72 H 0.5879 0.1055 0.5806 0.149 Uiso 1 d . . H73 H 0.6149 0.0276 0.5759 0.155 Uiso 1 d . . H11 H 0.1942 -0.1631 -0.0668 0.080 Uiso 1 d . . H12 H 0.1625 -0.2079 0.0393 0.170 Uiso 1 d . . H13 H 0.2408 -0.1540 0.2056 0.102 Uiso 1 d . . H14 H 0.3351 -0.0869 0.2450 0.020 Uiso 1 d . . H15 H 0.5420 0.3941 0.3857 0.111 Uiso 1 d . . H16 H 0.6078 0.4925 0.4078 0.054 Uiso 1 d . . H17 H 0.7082 0.4924 0.3896 0.080 Uiso 1 d . . H18 H 0.7248 0.4077 0.3145 0.096 Uiso 1 d . . H19 H 0.6526 0.3359 0.2755 0.150 Uiso 1 d . . H25 H 0.3343 0.2799 -0.2584 0.063 Uiso 1 d . . H26 H 0.4230 0.3363 -0.2563 0.053 Uiso 1 d . . H27 H 0.5434 0.3650 -0.0882 0.129 Uiso 1 d . . H28 H 0.5527 0.3306 0.0547 0.067 Uiso 1 d . . H301 H 0.2730 0.2023 0.0325 0.109 Uiso 1 d . . H302 H 0.2602 0.1463 0.0790 0.107 Uiso 1 d . . H303 H 0.3095 0.1198 0.0316 0.099 Uiso 1 d . . H2O H 0.3159 -0.0459 -0.0438 0.224 Uiso 1 d . . H4O H 0.3293 0.2227 -0.0698 0.042 Uiso 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 Ni1 0.062(2) 0.053(2) 0.073(2) 0.000 0.029(2) 0.000 Ni2 0.059(2) 0.053(2) 0.075(2) 0.000 0.024(2) 0.000 O1 0.083(6) 0.068(6) 0.067(7) -0.006(5) 0.039(6) -0.011(5) O2 0.099(9) 0.083(8) 0.107(10) -0.012(7) 0.036(8) -0.001(6) O3 0.057(6) 0.071(6) 0.075(7) 0.002(5) 0.028(6) -0.007(5) O4 0.076(7) 0.121(10) 0.072(7) 0.000(6) 0.023(6) -0.014(7) N1 0.064(7) 0.052(6) 0.074(8) -0.004(5) 0.035(6) -0.002(5) N2 0.059(7) 0.062(7) 0.075(8) 0.000(6) 0.027(6) -0.003(6) N3 0.065(7) 0.058(7) 0.087(9) -0.007(7) 0.037(7) -0.001(6) N4 0.066(8) 0.065(8) 0.088(9) 0.006(7) 0.020(7) -0.001(6) N5 0.066(8) 0.053(6) 0.078(9) -0.003(6) 0.035(7) 0.004(6) N6 0.061(7) 0.058(7) 0.069(8) -0.006(6) 0.028(6) 0.002(5) C1 0.074(8) 0.051(7) 0.073(10) -0.009(6) 0.045(8) -0.010(6) C2 0.109(12) 0.069(9) 0.064(10) -0.003(8) 0.053(10) 0.001(9) C3 0.077(9) 0.067(9) 0.108(12) -0.003(8) 0.059(9) 0.009(7) C4 0.072(10) 0.055(8) 0.115(17) -0.004(9) 0.051(11) 0.004(7) C5 0.067(8) 0.048(7) 0.085(11) 0.000(7) 0.048(8) 0.000(6) C6 0.074(9) 0.044(6) 0.069(9) -0.007(6) 0.036(8) -0.004(6) C7 0.099(12) 0.085(11) 0.081(12) 0.004(9) 0.053(11) 0.006(9) C8 0.080(10) 0.058(8) 0.077(11) 0.014(7) 0.041(9) 0.013(7) C9 0.066(9) 0.057(8) 0.085(11) -0.004(8) 0.032(9) -0.003(7) C10 0.081(12) 0.063(9) 0.084(12) 0.017(9) 0.042(10) 0.011(8) C11 0.083(11) 0.079(11) 0.121(16) -0.011(10) 0.024(11) -0.011(9) C12 0.093(12) 0.083(12) 0.167(23) 0.021(13) 0.061(15) -0.001(9) C13 0.101(15) 0.102(15) 0.135(20) 0.008(14) 0.062(15) -0.021(13) C14 0.079(12) 0.087(11) 0.103(14) 0.015(10) 0.043(11) -0.008(10) C15 0.135(18) 0.067(10) 0.112(16) -0.010(11) 0.054(14) 0.000(11) C16 0.150(24) 0.068(12) 0.163(25) -0.040(13) 0.073(20) -0.044(14) C17 0.133(20) 0.124(19) 0.141(22) -0.022(16) 0.043(17) -0.081(16) C18 0.113(15) 0.096(15) 0.129(16) -0.014(13) 0.043(13) -0.049(13) C19 0.069(11) 0.094(11) 0.109(15) 0.017(10) 0.031(11) -0.018(9) C20 0.056(8) 0.053(7) 0.073(10) -0.010(7) 0.024(8) 0.007(6) C21 0.071(9) 0.075(9) 0.063(9) 0.012(7) 0.034(8) 0.012(7) C22 0.067(9) 0.080(9) 0.078(11) -0.007(8) 0.032(9) 0.001(7) C23 0.077(11) 0.119(14) 0.072(12) 0.019(10) 0.028(10) 0.008(10) C24 0.106(15) 0.141(16) 0.070(11) 0.014(10) 0.042(11) -0.002(12) C25 0.106(15) 0.108(15) 0.098(15) 0.015(11) 0.057(13) -0.014(11) C26 0.074(10) 0.092(13) 0.089(11) 0.014(9) 0.043(9) -0.004(9) C27 0.052(7) 0.056(7) 0.075(9) -0.008(6) 0.033(7) -0.009(6) C28 0.074(11) 0.093(13) 0.089(11) -0.002(9) 0.032(9) -0.015(9) C29 0.231(33) 0.097(22) 0.131(25) 0.000 -0.032(20) 0.000 Cl3A 0.086(6) 0.090(6) 0.120(7) 0.007(5) 0.049(5) 0.014(5) Cl3B 0.161(6) 0.151(6) 0.125(7) -0.019(5) 0.081(5) -0.042(5) Cl1 0.094(7) 0.132(10) 0.144(11) 0.011(8) 0.018(7) -0.023(7) Cl2 0.122(8) 0.082(6) 0.198(13) 0.017(7) 0.050(8) -0.042(6) C30 0.498(180) 0.193(102) 0.114(47) 0.048(57) 0.079(78) 0.254(130) _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 N2 1.990(12) . ? Ni1 N2 1.990(12) 2_655 ? Ni1 O1 2.120(10) . ? Ni1 O1 2.120(10) 2_655 ? Ni1 N1 2.175(11) 2_655 ? Ni1 N1 2.175(11) . ? Ni2 O3 2.036(10) . ? Ni2 O3 2.036(10) 2_655 ? Ni2 N4 2.136(13) . ? Ni2 N4 2.136(13) 2_655 ? Ni2 N5 2.148(12) . ? Ni2 N5 2.148(12) 2_655 ? O1 C8 1.25(2) . ? O2 C10 1.27(2) . ? O3 C20 1.28(2) . ? O4 C22 1.34(2) . ? N1 C5 1.34(2) . ? N1 C1 1.36(2) . ? N2 C6 1.30(2) 2_655 ? N2 N3 1.39(2) . ? N3 C8 1.34(2) . ? N4 C19 1.32(2) . ? N4 C15 1.36(2) . ? N5 C27 1.30(2) . ? N5 N6 1.39(2) . ? N6 C20 1.35(2) . ? C1 C2 1.35(2) . ? C1 C6 1.50(2) . ? C2 C3 1.35(2) . ? C3 C4 1.38(2) . ? C4 C5 1.40(2) . ? C5 C27 1.44(2) . ? C6 N2 1.30(2) 2_655 ? C6 C7 1.47(2) . ? C8 C9 1.50(2) . ? C9 C14 1.37(2) . ? C9 C10 1.41(2) . ? C10 C11 1.39(2) . ? C11 C12 1.34(3) . ? C12 C13 1.39(3) . ? C13 C14 1.39(3) . ? C15 C16 1.36(3) . ? C16 C17 1.32(4) . ? C17 C18 1.37(4) . ? C18 C19 1.37(3) . ? C20 C21 1.46(2) . ? C21 C26 1.41(2) . ? C21 C22 1.42(2) . ? C22 C23 1.40(2) . ? C23 C24 1.33(3) . ? C24 C25 1.41(3) . ? C25 C26 1.35(3) . ? C27 C28 1.49(2) . ? C29 Cl3B 1.337(12) . ? C29 Cl3B 1.337(12) 2_656 ? C29 Cl3A 1.79(2) 2_656 ? C29 Cl3A 1.79(2) . ? Cl3A Cl3B 0.965(11) . ? Cl1 C30 1.59(16) . ? Cl2 C30 1.67(12) . ? 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 N2 Ni1 N2 165.1(7) . 2_655 ? N2 Ni1 O1 76.9(4) . . ? N2 Ni1 O1 93.0(4) 2_655 . ? N2 Ni1 O1 93.0(4) . 2_655 ? N2 Ni1 O1 76.9(4) 2_655 2_655 ? O1 Ni1 O1 95.1(5) . 2_655 ? N2 Ni1 N1 76.7(5) . 2_655 ? N2 Ni1 N1 113.1(5) 2_655 2_655 ? O1 Ni1 N1 153.6(4) . 2_655 ? O1 Ni1 N1 87.5(4) 2_655 2_655 ? N2 Ni1 N1 113.1(5) . . ? N2 Ni1 N1 76.7(5) 2_655 . ? O1 Ni1 N1 87.5(4) . . ? O1 Ni1 N1 153.6(4) 2_655 . ? N1 Ni1 N1 101.7(6) 2_655 . ? O3 Ni2 O3 175.6(6) . 2_655 ? O3 Ni2 N4 87.4(5) . . ? O3 Ni2 N4 89.4(5) 2_655 . ? O3 Ni2 N4 89.4(5) . 2_655 ? O3 Ni2 N4 87.4(5) 2_655 2_655 ? N4 Ni2 N4 87.9(7) . 2_655 ? O3 Ni2 N5 76.5(4) . . ? O3 Ni2 N5 106.2(4) 2_655 . ? N4 Ni2 N5 162.5(5) . . ? N4 Ni2 N5 85.0(4) 2_655 . ? O3 Ni2 N5 106.2(4) . 2_655 ? O3 Ni2 N5 76.5(4) 2_655 2_655 ? N4 Ni2 N5 85.0(4) . 2_655 ? N4 Ni2 N5 162.5(5) 2_655 2_655 ? N5 Ni2 N5 106.0(6) . 2_655 ? C8 O1 Ni1 109.5(9) . . ? C20 O3 Ni2 110.9(9) . . ? C5 N1 C1 118.1(12) . . ? C5 N1 Ni1 128.6(10) . . ? C1 N1 Ni1 111.0(8) . . ? C6 N2 N3 119.6(13) 2_655 . ? C6 N2 Ni1 122.3(10) 2_655 . ? N3 N2 Ni1 117.9(10) . . ? C8 N3 N2 109.0(12) . . ? C19 N4 C15 118.4(16) . . ? C19 N4 Ni2 119.9(13) . . ? C15 N4 Ni2 121.3(13) . . ? C27 N5 N6 117.4(12) . . ? C27 N5 Ni2 130.6(10) . . ? N6 N5 Ni2 110.3(8) . . ? C20 N6 N5 110.6(11) . . ? C2 C1 N1 121.4(13) . . ? C2 C1 C6 123.2(14) . . ? N1 C1 C6 115.4(12) . . ? C1 C2 C3 122.4(15) . . ? C2 C3 C4 117.3(14) . . ? C3 C4 C5 119.8(15) . . ? N1 C5 C4 120.7(15) . . ? N1 C5 C27 116.5(12) . . ? C4 C5 C27 122.8(14) . . ? N2 C6 C7 126.1(13) 2_655 . ? N2 C6 C1 112.4(13) 2_655 . ? C7 C6 C1 121.5(13) . . ? O1 C8 N3 126.6(14) . . ? O1 C8 C9 118.0(14) . . ? N3 C8 C9 115.3(15) . . ? C14 C9 C10 118.7(16) . . ? C14 C9 C8 120.4(16) . . ? C10 C9 C8 120.8(15) . . ? O2 C10 C11 116.5(19) . . ? O2 C10 C9 124.7(16) . . ? C11 C10 C9 118.8(18) . . ? C12 C11 C10 121.6(20) . . ? C11 C12 C13 120.6(19) . . ? C14 C13 C12 118.5(21) . . ? C13 C14 C9 121.7(20) . . ? C16 C15 N4 120.9(24) . . ? C15 C16 C17 119.6(24) . . ? C16 C17 C18 121.1(20) . . ? C19 C18 C17 117.3(22) . . ? N4 C19 C18 122.6(22) . . ? O3 C20 N6 125.4(15) . . ? O3 C20 C21 119.5(13) . . ? N6 C20 C21 115.2(13) . . ? C26 C21 C22 117.2(14) . . ? C26 C21 C20 118.7(14) . . ? C22 C21 C20 124.0(14) . . ? O4 C22 C23 118.8(15) . . ? O4 C22 C21 120.8(15) . . ? C23 C22 C21 120.4(15) . . ? C24 C23 C22 119.9(17) . . ? C23 C24 C25 121.6(18) . . ? C26 C25 C24 119.4(18) . . ? C25 C26 C21 121.4(16) . . ? N5 C27 C5 115.8(12) . . ? N5 C27 C28 123.4(14) . . ? C5 C27 C28 120.7(12) . . ? Cl3B C29 Cl3B 153.8(28) . 2_656 ? Cl3B C29 Cl3A 128.8(19) . 2_656 ? Cl3B C29 Cl3A 31.9(6) 2_656 2_656 ? Cl3B C29 Cl3A 31.9(6) . . ? Cl3B C29 Cl3A 128.8(19) 2_656 . ? Cl3A C29 Cl3A 121.2(19) 2_656 . ? Cl3B Cl3A C29 47.1(9) . . ? Cl3A Cl3B C29 101.0(13) . . ? Cl1 C30 Cl2 123.7(35) . . ? _refine_diff_density_max 0.838 _refine_diff_density_min -1.328 _refine_diff_density_rms 0.122