# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2020 data_ninl11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ni(C34 H50 N4 O4).2NO3.CH2Cl2' _chemical_formula_sum 'C35 H52 Cl2 N6 Ni O10' _chemical_formula_weight 846.44 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.5599(16) _cell_length_b 14.2742(14) _cell_length_c 16.7199(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.773(7) _cell_angle_gamma 90.00 _cell_volume 3950.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_crystal_description block _exptl_crystal_colour Red _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.51 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.6 _diffrn_reflns_number 8568 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.07 _reflns_number_total 6972 _reflns_number_gt 4296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _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^)+(0.0471P)^2^+2.3549P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric, except H on morpholine N placed on difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6972 _refine_ls_number_parameters 506 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.019 _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 Ni1 Ni 0.20045(3) 0.00544(4) 0.04242(3) 0.02742(15) Uani 1 1 d . . . C1A C 0.0990(2) -0.1463(3) -0.0048(2) 0.0291(9) Uani 1 1 d . . . O1A O 0.16300(15) -0.09514(18) -0.01880(15) 0.0337(7) Uani 1 1 d . . . C2A C 0.0369(2) -0.1185(3) 0.0460(2) 0.0288(9) Uani 1 1 d . . . C21A C 0.0416(2) -0.0338(3) 0.0908(2) 0.0309(9) Uani 1 1 d . . . H211 H -0.0046 -0.0146 0.1177 0.037 Uiso 1 1 calc R . . N2A N 0.10527(18) 0.0184(2) 0.09666(17) 0.0297(8) Uani 1 1 d . . . C22A C 0.1040(2) 0.1019(3) 0.1488(2) 0.0353(10) Uani 1 1 d . . . H221 H 0.0669 0.0926 0.1927 0.042 Uiso 1 1 calc R . . H222 H 0.0869 0.1574 0.1182 0.042 Uiso 1 1 calc R . . C3A C -0.0305(2) -0.1768(3) 0.0574(2) 0.0344(10) Uani 1 1 d . . . H3A H -0.0722 -0.1550 0.0895 0.041 Uiso 1 1 calc R . . C4A C -0.0378(2) -0.2646(3) 0.0231(2) 0.0359(10) Uani 1 1 d . A . C41A C -0.1111(2) -0.3272(3) 0.0401(2) 0.0390(10) Uani 1 1 d D . . C42A C -0.1172(6) -0.3419(7) 0.1289(4) 0.071(2) Uani 0.62 1 d PD A 1 H421 H -0.0668 -0.3674 0.1503 0.107 Uiso 0.62 1 calc PR A 1 H422 H -0.1608 -0.3853 0.1389 0.107 Uiso 0.62 1 calc PR A 1 H423 H -0.1280 -0.2825 0.1546 0.107 Uiso 0.62 1 calc PR A 1 C43A C -0.1015(5) -0.4282(5) 0.0018(5) 0.063(2) Uani 0.62 1 d PD A 1 H431 H -0.0533 -0.4580 0.0242 0.094 Uiso 0.62 1 calc PR A 1 H432 H -0.0970 -0.4224 -0.0557 0.094 Uiso 0.62 1 calc PR A 1 H433 H -0.1484 -0.4661 0.0134 0.094 Uiso 0.62 1 calc PR A 1 C44A C -0.1868(4) -0.2874(6) 0.0018(5) 0.059(2) Uani 0.62 1 d PD A 1 H441 H -0.1796 -0.2800 -0.0552 0.089 Uiso 0.62 1 calc PR A 1 H442 H -0.1981 -0.2269 0.0253 0.089 Uiso 0.62 1 calc PR A 1 H443 H -0.2316 -0.3296 0.0105 0.089 Uiso 0.62 1 calc PR A 1 C45A C -0.0840(7) -0.4004(9) 0.0983(8) 0.059(2) Uani 0.38 1 d PD A 2 H451 H -0.0580 -0.3708 0.1446 0.089 Uiso 0.38 1 calc PR A 2 H452 H -0.0460 -0.4420 0.0733 0.089 Uiso 0.38 1 calc PR A 2 H453 H -0.1303 -0.4361 0.1152 0.089 Uiso 0.38 1 calc PR A 2 C46A C -0.1761(7) -0.2652(8) 0.0857(8) 0.063(2) Uani 0.38 1 d PD A 2 H461 H -0.1527 -0.2437 0.1363 0.094 Uiso 0.38 1 calc PR A 2 H462 H -0.2236 -0.3028 0.0953 0.094 Uiso 0.38 1 calc PR A 2 H463 H -0.1913 -0.2116 0.0529 0.094 Uiso 0.38 1 calc PR A 2 C47A C -0.1506(9) -0.3557(11) -0.0362(6) 0.071(2) Uani 0.38 1 d PD A 2 H471 H -0.1617 -0.3006 -0.0687 0.107 Uiso 0.38 1 calc PR A 2 H472 H -0.2009 -0.3876 -0.0257 0.107 Uiso 0.38 1 calc PR A 2 H473 H -0.1152 -0.3976 -0.0644 0.107 Uiso 0.38 1 calc PR A 2 C5A C 0.0247(2) -0.2922(3) -0.0256(2) 0.0348(10) Uani 1 1 d . . . H5A H 0.0217 -0.3517 -0.0497 0.042 Uiso 1 1 calc R A . C6A C 0.0911(2) -0.2362(3) -0.0404(2) 0.0307(9) Uani 1 1 d . A . C61A C 0.1578(2) -0.2731(3) -0.0903(2) 0.0349(10) Uani 1 1 d . . . H611 H 0.1647 -0.3401 -0.0794 0.042 Uiso 1 1 calc R A . H612 H 0.2083 -0.2416 -0.0741 0.042 Uiso 1 1 calc R . . N62A N 0.14318(19) -0.2594(2) -0.17938(19) 0.0303(8) Uani 1 1 d . A . H62A H 0.092(2) -0.291(3) -0.191(2) 0.032(10) Uiso 1 1 d . . . C63A C 0.1371(3) -0.1595(3) -0.2036(3) 0.0401(11) Uani 1 1 d . . . H631 H 0.1857 -0.1259 -0.1850 0.048 Uiso 1 1 calc R A . H632 H 0.0904 -0.1307 -0.1786 0.048 Uiso 1 1 calc R . . C64A C 0.1278(3) -0.1512(3) -0.2942(3) 0.0500(12) Uani 1 1 d . A . H641 H 0.0774 -0.1814 -0.3125 0.060 Uiso 1 1 calc R . . H642 H 0.1251 -0.0850 -0.3094 0.060 Uiso 1 1 calc R . . O65A O 0.19475(17) -0.1949(2) -0.33153(17) 0.0488(8) Uani 1 1 d . . . C66A C 0.1949(3) -0.2918(3) -0.3130(3) 0.0470(12) Uani 1 1 d . A . H661 H 0.2376 -0.3232 -0.3423 0.056 Uiso 1 1 calc R . . H662 H 0.1430 -0.3195 -0.3301 0.056 Uiso 1 1 calc R . . C67A C 0.2089(2) -0.3072(3) -0.2242(3) 0.0438(11) Uani 1 1 d . . . H671 H 0.2088 -0.3744 -0.2124 0.053 Uiso 1 1 calc R A . H672 H 0.2616 -0.2816 -0.2072 0.053 Uiso 1 1 calc R . . C1B C 0.3536(2) 0.0599(3) -0.0144(2) 0.0295(9) Uani 1 1 d . . . O1B O 0.29196(14) 0.00139(19) -0.01871(14) 0.0328(6) Uani 1 1 d . . . C2B C 0.3667(2) 0.1264(3) 0.0471(2) 0.0330(10) Uani 1 1 d . . . C21B C 0.3098(2) 0.1376(3) 0.1089(2) 0.0360(10) Uani 1 1 d . . . H212 H 0.3235 0.1794 0.1506 0.043 Uiso 1 1 calc R . . N2B N 0.24173(18) 0.0955(2) 0.11211(18) 0.0314(8) Uani 1 1 d . . . C22B C 0.1890(2) 0.1129(3) 0.1805(2) 0.0385(11) Uani 1 1 d . . . H223 H 0.1977 0.1762 0.2017 0.046 Uiso 1 1 calc R . . H224 H 0.2005 0.0677 0.2235 0.046 Uiso 1 1 calc R . . C3B C 0.4340(2) 0.1857(3) 0.0472(2) 0.0350(10) Uani 1 1 d . . . H3B H 0.4406 0.2291 0.0892 0.042 Uiso 1 1 calc R . . C4B C 0.4915(2) 0.1836(3) -0.0116(2) 0.0313(10) Uani 1 1 d . . . C41B C 0.5600(2) 0.2547(3) -0.0122(2) 0.0349(10) Uani 1 1 d . . . C42B C 0.5227(3) 0.3518(3) -0.0294(3) 0.0495(12) Uani 1 1 d . . . H424 H 0.5652 0.3984 -0.0302 0.074 Uiso 1 1 calc R . . H425 H 0.4852 0.3673 0.0120 0.074 Uiso 1 1 calc R . . H426 H 0.4941 0.3506 -0.0810 0.074 Uiso 1 1 calc R . . C43B C 0.6217(3) 0.2327(3) -0.0761(3) 0.0566(14) Uani 1 1 d . . . H434 H 0.6640 0.2797 -0.0744 0.085 Uiso 1 1 calc R . . H435 H 0.5949 0.2329 -0.1285 0.085 Uiso 1 1 calc R . . H436 H 0.6452 0.1714 -0.0658 0.085 Uiso 1 1 calc R . . C44B C 0.6058(3) 0.2581(3) 0.0689(3) 0.0495(12) Uani 1 1 d . . . H444 H 0.6489 0.3039 0.0667 0.074 Uiso 1 1 calc R . . H445 H 0.6285 0.1969 0.0809 0.074 Uiso 1 1 calc R . . H446 H 0.5689 0.2756 0.1103 0.074 Uiso 1 1 calc R . . C5B C 0.4782(2) 0.1158(3) -0.0719(2) 0.0319(10) Uani 1 1 d . . . H5B H 0.5159 0.1108 -0.1125 0.038 Uiso 1 1 calc R . . C6B C 0.4125(2) 0.0566(3) -0.0741(2) 0.0292(9) Uani 1 1 d . . . C61B C 0.4009(2) -0.0109(3) -0.1430(2) 0.0325(9) Uani 1 1 d . . . H613 H 0.4535 -0.0370 -0.1566 0.039 Uiso 1 1 calc R . . H614 H 0.3666 -0.0628 -0.1263 0.039 Uiso 1 1 calc R . . N62B N 0.36302(19) 0.0344(2) -0.21638(19) 0.0301(8) Uani 1 1 d . . . H62B H 0.399(3) 0.083(3) -0.232(3) 0.055(14) Uiso 1 1 d . . . C63B C 0.3558(3) -0.0354(3) -0.2829(2) 0.0414(11) Uani 1 1 d . . . H633 H 0.3241 -0.0893 -0.2656 0.050 Uiso 1 1 calc R . . H634 H 0.4097 -0.0579 -0.2962 0.050 Uiso 1 1 calc R . . C64B C 0.3154(3) 0.0084(4) -0.3561(3) 0.0559(13) Uani 1 1 d . . . H643 H 0.3492 0.0594 -0.3757 0.067 Uiso 1 1 calc R . . H644 H 0.3096 -0.0386 -0.3986 0.067 Uiso 1 1 calc R . . O65B O 0.23801(19) 0.0442(2) -0.33781(19) 0.0594(9) Uani 1 1 d . . . C66B C 0.2466(3) 0.1149(3) -0.2785(3) 0.0483(12) Uani 1 1 d . . . H663 H 0.1936 0.1424 -0.2687 0.058 Uiso 1 1 calc R . . H664 H 0.2817 0.1647 -0.2980 0.058 Uiso 1 1 calc R . . C67B C 0.2820(2) 0.0764(3) -0.2016(2) 0.0369(10) Uani 1 1 d . . . H673 H 0.2876 0.1267 -0.1619 0.044 Uiso 1 1 calc R . . H674 H 0.2460 0.0285 -0.1805 0.044 Uiso 1 1 calc R . . C1D C 0.3990(3) 0.0026(4) 0.3278(3) 0.0568(12) Uani 1 1 d . . . H1D1 H 0.4244 0.0641 0.3219 0.068 Uiso 1 1 calc R . . H1D2 H 0.4397 -0.0402 0.3509 0.068 Uiso 1 1 calc R . . Cl1D Cl 0.36740(8) -0.03862(10) 0.23371(8) 0.0678(4) Uani 1 1 d . . . Cl2D Cl 0.31822(8) 0.01213(10) 0.39315(9) 0.0717(4) Uani 1 1 d . . . N1S N -0.0156(3) -0.3948(3) -0.2324(2) 0.0488(10) Uani 1 1 d . . . O1S1 O 0.0513(2) -0.4289(3) -0.2137(2) 0.0748(11) Uani 1 1 d . . . O1S2 O -0.0243(2) -0.3094(3) -0.2242(2) 0.0652(10) Uani 1 1 d . . . O1S3 O -0.0702(2) -0.4447(3) -0.2606(2) 0.0681(11) Uani 1 1 d . . . N2S N 0.4523(2) 0.2494(3) -0.2459(2) 0.0458(10) Uani 1 1 d . . . O2S1 O 0.3891(2) 0.2640(2) -0.2102(2) 0.0616(9) Uani 1 1 d . . . O2S2 O 0.5032(2) 0.3119(2) -0.2535(2) 0.0704(11) Uani 1 1 d . . . O2S3 O 0.46409(19) 0.1691(2) -0.27677(19) 0.0552(9) 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 Ni1 0.0287(2) 0.0298(3) 0.0241(2) -0.0017(2) 0.00665(18) -0.0028(2) C1A 0.029(2) 0.035(2) 0.023(2) 0.0028(18) -0.0009(17) -0.0034(18) O1A 0.0309(15) 0.0373(16) 0.0336(16) -0.0072(13) 0.0105(12) -0.0068(13) C2A 0.029(2) 0.035(2) 0.022(2) 0.0039(18) 0.0017(16) 0.0021(18) C21A 0.027(2) 0.038(2) 0.028(2) 0.0065(18) 0.0067(16) 0.0027(18) N2A 0.0348(18) 0.030(2) 0.0247(17) -0.0001(14) 0.0076(14) 0.0018(15) C22A 0.043(2) 0.033(2) 0.030(2) -0.0012(19) 0.0139(19) 0.0020(19) C3A 0.030(2) 0.048(3) 0.025(2) 0.006(2) 0.0028(17) -0.003(2) C4A 0.035(2) 0.046(3) 0.026(2) 0.013(2) -0.0046(19) -0.011(2) C41A 0.034(2) 0.047(3) 0.036(2) 0.009(2) -0.0004(19) -0.011(2) C42A 0.081(6) 0.090(6) 0.043(4) 0.011(4) 0.007(4) -0.045(5) C43A 0.055(4) 0.045(4) 0.089(6) -0.001(4) 0.005(4) -0.024(4) C44A 0.049(4) 0.060(5) 0.067(5) 0.025(4) 0.002(4) -0.013(4) C45A 0.049(4) 0.060(5) 0.067(5) 0.025(4) 0.002(4) -0.013(4) C46A 0.055(4) 0.045(4) 0.089(6) -0.001(4) 0.005(4) -0.024(4) C47A 0.081(6) 0.090(6) 0.043(4) 0.011(4) 0.007(4) -0.045(5) C5A 0.043(2) 0.031(2) 0.030(2) 0.0027(19) -0.0044(19) -0.0054(19) C6A 0.030(2) 0.035(2) 0.027(2) 0.0001(19) -0.0014(17) -0.0006(18) C61A 0.036(2) 0.033(2) 0.036(2) -0.0064(19) -0.0023(19) 0.0006(19) N62A 0.0244(17) 0.032(2) 0.0345(19) -0.0074(16) 0.0022(14) -0.0027(15) C63A 0.041(2) 0.033(2) 0.047(3) -0.004(2) 0.005(2) 0.005(2) C64A 0.049(3) 0.053(3) 0.049(3) 0.005(2) 0.013(2) 0.008(2) O65A 0.0495(19) 0.051(2) 0.0466(19) -0.0002(16) 0.0164(15) 0.0021(16) C66A 0.050(3) 0.048(3) 0.044(3) -0.013(2) 0.015(2) -0.002(2) C67A 0.038(2) 0.040(3) 0.054(3) -0.012(2) 0.010(2) 0.009(2) C1B 0.026(2) 0.030(2) 0.033(2) 0.0046(19) 0.0042(17) -0.0036(18) O1B 0.0328(14) 0.0342(15) 0.0322(15) -0.0078(14) 0.0104(11) -0.0070(14) C2B 0.034(2) 0.036(2) 0.029(2) -0.0020(19) 0.0049(18) -0.0058(19) C21B 0.041(2) 0.039(3) 0.028(2) -0.0061(19) 0.0021(19) -0.007(2) N2B 0.0339(19) 0.036(2) 0.0244(18) -0.0021(15) 0.0047(14) -0.0037(16) C22B 0.047(3) 0.039(3) 0.030(2) -0.014(2) 0.016(2) -0.008(2) C3B 0.038(2) 0.036(2) 0.030(2) -0.0034(19) 0.0005(18) -0.0051(19) C4B 0.028(2) 0.037(2) 0.029(2) 0.0047(19) -0.0008(18) -0.0006(18) C41B 0.035(2) 0.035(2) 0.035(2) 0.003(2) 0.0054(18) -0.0064(19) C42B 0.043(3) 0.043(3) 0.062(3) 0.008(2) 0.001(2) -0.006(2) C43B 0.046(3) 0.055(3) 0.071(3) -0.007(3) 0.025(2) -0.018(2) C44B 0.041(3) 0.052(3) 0.055(3) 0.011(2) -0.012(2) -0.017(2) C5B 0.030(2) 0.035(2) 0.031(2) 0.0061(19) 0.0078(17) 0.0019(19) C6B 0.034(2) 0.024(2) 0.030(2) 0.0028(18) 0.0044(17) 0.0051(18) C61B 0.035(2) 0.026(2) 0.037(2) 0.0032(19) 0.0102(17) 0.0029(18) N62B 0.0298(18) 0.0279(19) 0.0329(19) -0.0047(15) 0.0078(15) -0.0016(15) C63B 0.047(3) 0.038(3) 0.040(3) -0.015(2) 0.007(2) 0.000(2) C64B 0.061(3) 0.066(3) 0.040(3) -0.020(3) -0.001(2) 0.006(3) O65B 0.053(2) 0.068(2) 0.056(2) -0.0159(19) -0.0138(17) 0.0029(17) C66B 0.045(3) 0.047(3) 0.053(3) -0.005(2) -0.003(2) 0.009(2) C67B 0.030(2) 0.035(2) 0.045(3) -0.007(2) 0.0074(19) 0.0023(19) C1D 0.047(3) 0.059(3) 0.065(3) 0.005(3) 0.002(2) -0.001(3) Cl1D 0.0617(8) 0.0764(10) 0.0658(9) -0.0076(7) 0.0093(7) -0.0022(7) Cl2D 0.0722(9) 0.0708(10) 0.0731(9) -0.0088(8) 0.0165(7) 0.0208(8) N1S 0.053(3) 0.060(3) 0.034(2) -0.006(2) 0.0116(19) -0.021(2) O1S1 0.063(2) 0.070(3) 0.091(3) -0.014(2) -0.003(2) -0.005(2) O1S2 0.083(3) 0.048(2) 0.064(2) -0.0065(19) -0.0083(19) -0.0093(19) O1S3 0.058(2) 0.080(3) 0.067(2) -0.028(2) 0.0230(18) -0.043(2) N2S 0.058(3) 0.045(3) 0.034(2) 0.0120(19) -0.0048(19) -0.012(2) O2S1 0.063(2) 0.050(2) 0.072(2) -0.0022(19) 0.0096(19) -0.0029(18) O2S2 0.090(3) 0.056(2) 0.065(2) 0.0035(18) 0.006(2) -0.040(2) O2S3 0.070(2) 0.040(2) 0.057(2) -0.0003(17) 0.0164(17) -0.0055(17) _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 N2B 1.852(3) . ? Ni1 N2A 1.852(3) . ? Ni1 O1B 1.855(2) . ? Ni1 O1A 1.859(3) . ? C1A O1A 1.313(4) . ? C1A C2A 1.412(5) . ? C1A C6A 1.419(5) . ? C2A C3A 1.410(5) . ? C2A C21A 1.423(5) . ? C21A N2A 1.293(5) . ? N2A C22A 1.477(5) . ? C22A C22B 1.497(5) . ? C3A C4A 1.381(6) . ? C4A C5A 1.394(5) . ? C4A C41A 1.541(5) . ? C41A C47A 1.472(10) . ? C41A C45A 1.488(10) . ? C41A C44A 1.502(7) . ? C41A C42A 1.505(7) . ? C41A C43A 1.588(7) . ? C41A C46A 1.604(10) . ? C5A C6A 1.388(5) . ? C6A C61A 1.501(5) . ? C61A N62A 1.514(5) . ? N62A C63A 1.485(5) . ? N62A C67A 1.503(5) . ? C63A C64A 1.522(6) . ? C64A O65A 1.432(5) . ? O65A C66A 1.418(5) . ? C66A C67A 1.512(6) . ? C1B O1B 1.319(4) . ? C1B C2B 1.411(5) . ? C1B C6B 1.418(5) . ? C2B C3B 1.399(5) . ? C2B C21B 1.428(5) . ? C21B N2B 1.280(5) . ? N2B C22B 1.481(4) . ? C3B C4B 1.391(5) . ? C4B C5B 1.409(5) . ? C4B C41B 1.522(5) . ? C41B C44B 1.533(5) . ? C41B C43B 1.534(5) . ? C41B C42B 1.540(6) . ? C5B C6B 1.377(5) . ? C6B C61B 1.509(5) . ? C61B N62B 1.506(5) . ? N62B C63B 1.496(5) . ? N62B C67B 1.497(5) . ? C63B C64B 1.513(6) . ? C64B O65B 1.421(5) . ? O65B C66B 1.419(5) . ? C66B C67B 1.501(6) . ? C1D Cl1D 1.744(5) . ? C1D Cl2D 1.759(4) . ? N1S O1S3 1.233(4) . ? N1S O1S2 1.235(5) . ? N1S O1S1 1.241(5) . ? N2S O2S2 1.236(4) . ? N2S O2S1 1.239(4) . ? N2S O2S3 1.274(5) . ? 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 N2B Ni1 N2A 85.73(13) . . ? N2B Ni1 O1B 94.38(12) . . ? N2A Ni1 O1B 174.40(13) . . ? N2B Ni1 O1A 173.36(14) . . ? N2A Ni1 O1A 94.16(12) . . ? O1B Ni1 O1A 86.38(11) . . ? O1A C1A C2A 123.9(4) . . ? O1A C1A C6A 119.6(3) . . ? C2A C1A C6A 116.5(3) . . ? C1A O1A Ni1 126.1(2) . . ? C3A C2A C1A 120.7(4) . . ? C3A C2A C21A 117.4(3) . . ? C1A C2A C21A 121.8(3) . . ? N2A C21A C2A 124.1(3) . . ? C21A N2A C22A 118.9(3) . . ? C21A N2A Ni1 127.6(3) . . ? C22A N2A Ni1 113.4(2) . . ? N2A C22A C22B 105.3(3) . . ? C4A C3A C2A 122.6(4) . . ? C3A C4A C5A 116.3(4) . . ? C3A C4A C41A 120.6(4) . . ? C5A C4A C41A 123.1(4) . . ? C47A C41A C45A 119.4(9) . . ? C47A C41A C44A 52.6(7) . . ? C45A C41A C44A 140.9(6) . . ? C47A C41A C42A 140.7(6) . . ? C45A C41A C42A 44.4(6) . . ? C44A C41A C42A 113.1(5) . . ? C47A C41A C4A 109.4(6) . . ? C45A C41A C4A 107.7(6) . . ? C44A C41A C4A 110.7(4) . . ? C42A C41A C4A 109.9(4) . . ? C47A C41A C43A 56.4(7) . . ? C45A C41A C43A 66.1(7) . . ? C44A C41A C43A 105.3(5) . . ? C42A C41A C43A 106.4(5) . . ? C4A C41A C43A 111.3(4) . . ? C47A C41A C46A 106.1(8) . . ? C45A C41A C46A 105.7(7) . . ? C44A C41A C46A 55.3(6) . . ? C42A C41A C46A 62.8(6) . . ? C4A C41A C46A 108.1(5) . . ? C43A C41A C46A 140.3(6) . . ? C6A C5A C4A 123.2(4) . . ? C5A C6A C1A 120.7(4) . . ? C5A C6A C61A 119.9(4) . . ? C1A C6A C61A 119.3(3) . . ? C6A C61A N62A 113.8(3) . . ? C63A N62A C67A 110.1(3) . . ? C63A N62A C61A 113.5(3) . . ? C67A N62A C61A 109.6(3) . . ? N62A C63A C64A 110.5(3) . . ? O65A C64A C63A 110.2(4) . . ? C66A O65A C64A 109.0(3) . . ? O65A C66A C67A 110.8(4) . . ? N62A C67A C66A 109.5(3) . . ? O1B C1B C2B 124.5(3) . . ? O1B C1B C6B 119.2(3) . . ? C2B C1B C6B 116.2(3) . . ? C1B O1B Ni1 126.5(2) . . ? C3B C2B C1B 120.8(3) . . ? C3B C2B C21B 118.3(4) . . ? C1B C2B C21B 120.8(3) . . ? N2B C21B C2B 125.4(4) . . ? C21B N2B C22B 119.7(3) . . ? C21B N2B Ni1 127.4(3) . . ? C22B N2B Ni1 112.8(2) . . ? N2B C22B C22A 106.2(3) . . ? C4B C3B C2B 123.3(4) . . ? C3B C4B C5B 115.1(4) . . ? C3B C4B C41B 121.1(4) . . ? C5B C4B C41B 123.6(3) . . ? C4B C41B C44B 111.3(3) . . ? C4B C41B C43B 112.3(3) . . ? C44B C41B C43B 107.5(4) . . ? C4B C41B C42B 107.9(3) . . ? C44B C41B C42B 108.8(4) . . ? C43B C41B C42B 109.0(3) . . ? C6B C5B C4B 123.2(3) . . ? C5B C6B C1B 121.3(4) . . ? C5B C6B C61B 119.6(3) . . ? C1B C6B C61B 119.0(3) . . ? N62B C61B C6B 112.8(3) . . ? C63B N62B C67B 109.8(3) . . ? C63B N62B C61B 109.9(3) . . ? C67B N62B C61B 113.0(3) . . ? N62B C63B C64B 110.4(3) . . ? O65B C64B C63B 110.7(4) . . ? C66B O65B C64B 109.5(3) . . ? O65B C66B C67B 111.5(4) . . ? N62B C67B C66B 109.5(3) . . ? Cl1D C1D Cl2D 112.0(3) . . ? O1S3 N1S O1S2 121.7(5) . . ? O1S3 N1S O1S1 120.5(5) . . ? O1S2 N1S O1S1 117.7(4) . . ? O2S2 N2S O2S1 121.1(4) . . ? O2S2 N2S O2S3 119.6(4) . . ? O2S1 N2S O2S3 119.2(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.277 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.062 data_hmcylg _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [C38H56N4O4].?0.5C6H14 _chemical_formula_sum 'C41 H63 N4 O4' _chemical_formula_weight 675.95 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 24.786(3) _cell_length_b 12.9082(15) _cell_length_c 26.542(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.715(18) _cell_angle_gamma 90.00 _cell_volume 8488(2) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 87 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.8237 _exptl_absorpt_correction_T_max 0.8699 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -3 _diffrn_reflns_number 8611 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 69.73 _reflns_number_total 7339 _reflns_number_gt 3727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _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^)+(0.1108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7339 _refine_ls_number_parameters 434 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1320 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2058 _refine_ls_wR_factor_gt 0.1762 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.151 _refine_ls_shift/su_mean 0.005 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 C1A C 0.01474(12) 0.9501(2) 0.41351(11) 0.0499(7) Uani 1 1 d . . . O1A O -0.01544(8) 1.01531(17) 0.38399(8) 0.0610(6) Uani 1 1 d . . . H1A H 0.0038 1.0412 0.3622 0.092 Uiso 1 1 calc R . . C2A C 0.07011(12) 0.9378(2) 0.40567(11) 0.0506(7) Uani 1 1 d . . . C21A C 0.09689(13) 0.9920(2) 0.36550(12) 0.0530(8) Uani 1 1 d . . . H21A H 0.1343 0.9835 0.3625 0.064 Uiso 1 1 calc R . . N2A N 0.07170(10) 1.0504(2) 0.33430(10) 0.0534(6) Uani 1 1 d . . . C22A C 0.10283(12) 1.1040(2) 0.29639(12) 0.0537(8) Uani 1 1 d . . . H22A H 0.1417 1.0905 0.3029 0.064 Uiso 1 1 calc R . . C23A C 0.09235(15) 1.2205(3) 0.30014(14) 0.0703(10) Uani 1 1 d . . . H231 H 0.0535 1.2335 0.2965 0.084 Uiso 1 1 calc R . . H232 H 0.1044 1.2452 0.3335 0.084 Uiso 1 1 calc R . . C24A C 0.12158(17) 1.2809(3) 0.25986(15) 0.0794(11) Uani 1 1 d . . . H241 H 0.1125 1.3546 0.2624 0.095 Uiso 1 1 calc R . . H242 H 0.1607 1.2738 0.2655 0.095 Uiso 1 1 calc R . . C3A C 0.10046(13) 0.8731(2) 0.43809(12) 0.0537(8) Uani 1 1 d . . . H3A H 0.1375 0.8642 0.4326 0.064 Uiso 1 1 calc R . . C4A C 0.07764(12) 0.8222(2) 0.47767(12) 0.0548(8) Uani 1 1 d . A . C41A C 0.11081(14) 0.7536(3) 0.51419(13) 0.0661(9) Uani 1 1 d D . . C42A C 0.1726(2) 0.7637(6) 0.5068(3) 0.106(2) Uani 0.70 1 d PD A 1 H421 H 0.1918 0.7192 0.5306 0.159 Uiso 0.70 1 calc PR A 1 H422 H 0.1835 0.8351 0.5123 0.159 Uiso 0.70 1 calc PR A 1 H423 H 0.1809 0.7433 0.4727 0.159 Uiso 0.70 1 calc PR A 1 C43A C 0.1005(3) 0.7843(6) 0.5684(2) 0.105(2) Uani 0.70 1 d PD A 1 H431 H 0.1217 0.7406 0.5912 0.157 Uiso 0.70 1 calc PR A 1 H432 H 0.0625 0.7758 0.5750 0.157 Uiso 0.70 1 calc PR A 1 H433 H 0.1107 0.8562 0.5736 0.157 Uiso 0.70 1 calc PR A 1 C44A C 0.0962(3) 0.6405(4) 0.5064(3) 0.102(2) Uani 0.70 1 d PD A 1 H441 H 0.1176 0.5980 0.5295 0.153 Uiso 0.70 1 calc PR A 1 H442 H 0.1034 0.6206 0.4720 0.153 Uiso 0.70 1 calc PR A 1 H443 H 0.0581 0.6306 0.5126 0.153 Uiso 0.70 1 calc PR A 1 C45A C 0.0779(6) 0.6737(15) 0.5395(7) 0.106(2) Uani 0.30 1 d P A 2 H451 H 0.1010 0.6324 0.5617 0.159 Uiso 0.30 1 calc PR A 2 H452 H 0.0606 0.6294 0.5143 0.159 Uiso 0.30 1 calc PR A 2 H453 H 0.0505 0.7075 0.5591 0.159 Uiso 0.30 1 calc PR A 2 C46A C 0.1540(8) 0.6999(15) 0.4880(6) 0.105(2) Uani 0.30 1 d P A 2 H461 H 0.1745 0.6575 0.5119 0.157 Uiso 0.30 1 calc PR A 2 H462 H 0.1776 0.7504 0.4732 0.157 Uiso 0.30 1 calc PR A 2 H463 H 0.1383 0.6561 0.4617 0.157 Uiso 0.30 1 calc PR A 2 C47A C 0.1351(8) 0.8256(11) 0.5526(7) 0.102(2) Uani 0.30 1 d P A 2 H471 H 0.1572 0.7864 0.5767 0.153 Uiso 0.30 1 calc PR A 2 H472 H 0.1066 0.8607 0.5701 0.153 Uiso 0.30 1 calc PR A 2 H473 H 0.1574 0.8763 0.5361 0.153 Uiso 0.30 1 calc PR A 2 C5A C 0.02235(13) 0.8359(2) 0.48384(12) 0.0570(8) Uani 1 1 d . . . H5A H 0.0060 0.8012 0.5105 0.068 Uiso 1 1 calc R A . C6A C -0.00971(12) 0.8986(2) 0.45237(12) 0.0549(8) Uani 1 1 d . A . C61A C -0.06895(13) 0.9145(3) 0.46063(14) 0.0659(9) Uani 1 1 d . . . H611 H -0.0736 0.9775 0.4807 0.079 Uiso 1 1 calc R A . H612 H -0.0874 0.9253 0.4279 0.079 Uiso 1 1 calc R . . N62A N -0.09447(10) 0.8283(2) 0.48613(11) 0.0617(7) Uani 1 1 d . A . C63A C -0.10007(15) 0.7395(3) 0.45288(17) 0.0839(12) Uani 1 1 d . . . H631 H -0.0645 0.7177 0.4418 0.101 Uiso 1 1 calc R A . H632 H -0.1222 0.7581 0.4230 0.101 Uiso 1 1 calc R . . C64A C -0.12637(19) 0.6524(3) 0.4807(2) 0.1166(18) Uani 1 1 d . A . H641 H -0.1293 0.5915 0.4587 0.140 Uiso 1 1 calc R . . H642 H -0.1038 0.6336 0.5102 0.140 Uiso 1 1 calc R . . O65A O -0.17823(13) 0.6805(3) 0.49644(17) 0.1298(13) Uani 1 1 d . . . C66A C -0.1742(2) 0.7691(4) 0.5280(2) 0.1231(19) Uani 1 1 d . A . H661 H -0.1529 0.7516 0.5585 0.148 Uiso 1 1 calc R . . H662 H -0.2104 0.7894 0.5381 0.148 Uiso 1 1 calc R . . C67A C -0.14830(15) 0.8581(3) 0.50222(17) 0.0854(12) Uani 1 1 d . . . H671 H -0.1706 0.8790 0.4728 0.102 Uiso 1 1 calc R A . H672 H -0.1454 0.9172 0.5253 0.102 Uiso 1 1 calc R . . C1B C 0.12132(12) 0.7384(2) 0.22016(12) 0.0556(8) Uani 1 1 d . . . O1B O 0.16254(8) 0.79106(17) 0.24380(9) 0.0664(6) Uani 1 1 d . . . H1B H 0.1530 0.8516 0.2491 0.100 Uiso 1 1 calc R . . C2B C 0.07234(12) 0.7874(2) 0.20827(12) 0.0513(8) Uani 1 1 d . . . C21B C 0.06345(13) 0.8966(2) 0.21850(12) 0.0540(8) Uani 1 1 d . . . H21B H 0.0296 0.9255 0.2097 0.065 Uiso 1 1 calc R . . N2B N 0.09968(10) 0.9555(2) 0.23902(10) 0.0528(6) Uani 1 1 d . . . C22B C 0.08671(12) 1.0654(2) 0.24366(11) 0.0513(8) Uani 1 1 d . . . H22B H 0.0474 1.0751 0.2380 0.062 Uiso 1 1 calc R . . C23B C 0.11655(14) 1.1263(3) 0.20409(13) 0.0655(9) Uani 1 1 d . . . H233 H 0.1049 1.1023 0.1705 0.079 Uiso 1 1 calc R . . H234 H 0.1554 1.1131 0.2082 0.079 Uiso 1 1 calc R . . C24B C 0.10618(16) 1.2424(3) 0.20816(15) 0.0784(11) Uani 1 1 d . . . H243 H 0.1272 1.2792 0.1831 0.094 Uiso 1 1 calc R . . H244 H 0.0679 1.2566 0.2010 0.094 Uiso 1 1 calc R . . C3B C 0.03063(12) 0.7305(3) 0.18515(12) 0.0563(8) Uani 1 1 d . . . H3B H -0.0023 0.7638 0.1773 0.068 Uiso 1 1 calc R . . C4B C 0.03624(12) 0.6264(2) 0.17337(12) 0.0553(8) Uani 1 1 d . B . C41B C -0.01023(12) 0.5628(3) 0.14967(13) 0.0605(9) Uani 1 1 d D . . C42B C -0.0279(3) 0.4808(5) 0.1863(2) 0.0894(18) Uani 0.70 1 d PD B 1 H424 H -0.0574 0.4410 0.1711 0.134 Uiso 0.70 1 calc PR B 1 H425 H -0.0399 0.5136 0.2169 0.134 Uiso 0.70 1 calc PR B 1 H426 H 0.0022 0.4350 0.1944 0.134 Uiso 0.70 1 calc PR B 1 C43B C 0.0078(3) 0.5146(6) 0.1007(2) 0.098(2) Uani 0.70 1 d PD B 1 H434 H -0.0216 0.4746 0.0856 0.147 Uiso 0.70 1 calc PR B 1 H435 H 0.0385 0.4695 0.1076 0.147 Uiso 0.70 1 calc PR B 1 H436 H 0.0181 0.5689 0.0777 0.147 Uiso 0.70 1 calc PR B 1 C44B C -0.0601(2) 0.6303(5) 0.1370(3) 0.0890(18) Uani 0.70 1 d PD B 1 H444 H -0.0885 0.5874 0.1221 0.134 Uiso 0.70 1 calc PR B 1 H445 H -0.0504 0.6840 0.1133 0.134 Uiso 0.70 1 calc PR B 1 H446 H -0.0728 0.6620 0.1676 0.134 Uiso 0.70 1 calc PR B 1 C45B C -0.0114(7) 0.5679(12) 0.0933(4) 0.0894(18) Uani 0.30 1 d PD B 2 H454 H -0.0414 0.5270 0.0799 0.134 Uiso 0.30 1 calc PR B 2 H455 H 0.0221 0.5406 0.0808 0.134 Uiso 0.30 1 calc PR B 2 H456 H -0.0158 0.6393 0.0826 0.134 Uiso 0.30 1 calc PR B 2 C46B C -0.0640(5) 0.5997(13) 0.1689(6) 0.098(2) Uani 0.30 1 d PD B 2 H464 H -0.0929 0.5588 0.1536 0.147 Uiso 0.30 1 calc PR B 2 H465 H -0.0692 0.6721 0.1603 0.147 Uiso 0.30 1 calc PR B 2 H466 H -0.0642 0.5917 0.2053 0.147 Uiso 0.30 1 calc PR B 2 C47B C -0.0048(6) 0.4466(8) 0.1631(6) 0.0890(18) Uani 0.30 1 d PD B 2 H474 H -0.0347 0.4085 0.1476 0.134 Uiso 0.30 1 calc PR B 2 H475 H -0.0053 0.4382 0.1994 0.134 Uiso 0.30 1 calc PR B 2 H476 H 0.0289 0.4200 0.1507 0.134 Uiso 0.30 1 calc PR B 2 C5B C 0.08604(12) 0.5815(3) 0.18468(13) 0.0602(9) Uani 1 1 d . . . H5B H 0.0911 0.5115 0.1761 0.072 Uiso 1 1 calc R B . C6B C 0.12886(12) 0.6344(3) 0.20800(13) 0.0574(8) Uani 1 1 d . B . C61B C 0.18146(14) 0.5796(3) 0.22032(14) 0.0688(10) Uani 1 1 d . . . H613 H 0.2099 0.6312 0.2262 0.083 Uiso 1 1 calc R B . H614 H 0.1778 0.5396 0.2514 0.083 Uiso 1 1 calc R . . N62B N 0.19707(10) 0.5105(2) 0.18008(11) 0.0614(7) Uani 1 1 d . B . C63B C 0.21593(15) 0.5670(3) 0.13623(15) 0.0779(11) Uani 1 1 d . . . H633 H 0.2476 0.6087 0.1461 0.093 Uiso 1 1 calc R B . H634 H 0.1875 0.6140 0.1238 0.093 Uiso 1 1 calc R . . C64B C 0.23050(17) 0.4936(4) 0.09518(16) 0.0918(13) Uani 1 1 d . B . H643 H 0.1983 0.4548 0.0840 0.110 Uiso 1 1 calc R . . H644 H 0.2433 0.5330 0.0663 0.110 Uiso 1 1 calc R . . O65B O 0.27120(10) 0.4231(3) 0.11162(12) 0.0937(9) Uani 1 1 d . . . C66B C 0.25439(15) 0.3683(3) 0.15451(18) 0.0856(12) Uani 1 1 d . B . H663 H 0.2834 0.3217 0.1661 0.103 Uiso 1 1 calc R . . H664 H 0.2229 0.3258 0.1452 0.103 Uiso 1 1 calc R . . C67B C 0.24016(13) 0.4400(3) 0.19680(15) 0.0698(10) Uani 1 1 d . . . H673 H 0.2283 0.3994 0.2256 0.084 Uiso 1 1 calc R B . H674 H 0.2721 0.4799 0.2076 0.084 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 C1A 0.0519(17) 0.0484(18) 0.0489(17) -0.0025(15) -0.0071(14) 0.0040(15) O1A 0.0565(12) 0.0648(14) 0.0615(14) 0.0104(12) -0.0029(10) 0.0063(11) C2A 0.0582(18) 0.0458(18) 0.0475(17) -0.0059(15) -0.0033(14) 0.0016(14) C21A 0.0568(18) 0.0514(19) 0.0508(18) -0.0042(16) -0.0003(14) 0.0050(15) N2A 0.0596(15) 0.0476(15) 0.0530(15) -0.0013(13) 0.0024(12) 0.0054(13) C22A 0.0554(18) 0.0469(18) 0.0588(19) -0.0004(16) 0.0037(15) 0.0030(15) C23A 0.088(3) 0.050(2) 0.074(2) -0.0051(19) 0.007(2) -0.0007(18) C24A 0.103(3) 0.052(2) 0.084(3) -0.002(2) 0.018(2) -0.009(2) C3A 0.0589(18) 0.0462(18) 0.0557(19) -0.0039(16) -0.0031(15) 0.0059(15) C4A 0.0597(19) 0.0492(19) 0.055(2) -0.0017(16) -0.0085(15) 0.0020(15) C41A 0.078(2) 0.064(2) 0.056(2) 0.0068(18) -0.0084(17) 0.0070(18) C42A 0.082(4) 0.124(6) 0.109(5) 0.045(5) -0.027(3) 0.004(4) C43A 0.130(5) 0.127(6) 0.057(3) 0.015(4) -0.008(3) 0.052(5) C44A 0.144(6) 0.058(3) 0.099(5) 0.004(3) -0.059(4) 0.009(4) C45A 0.082(4) 0.124(6) 0.109(5) 0.045(5) -0.027(3) 0.004(4) C46A 0.130(5) 0.127(6) 0.057(3) 0.015(4) -0.008(3) 0.052(5) C47A 0.144(6) 0.058(3) 0.099(5) 0.004(3) -0.059(4) 0.009(4) C5A 0.066(2) 0.0503(19) 0.0544(19) 0.0045(16) 0.0015(15) -0.0062(16) C6A 0.0546(18) 0.0525(19) 0.057(2) -0.0037(16) -0.0007(15) -0.0023(15) C61A 0.066(2) 0.059(2) 0.073(2) -0.0001(19) 0.0044(17) -0.0024(17) N62A 0.0555(16) 0.0615(17) 0.0684(18) -0.0105(15) 0.0061(13) -0.0117(14) C63A 0.069(2) 0.069(3) 0.113(3) -0.028(2) -0.001(2) -0.004(2) C64A 0.088(3) 0.073(3) 0.187(6) -0.004(3) -0.020(3) -0.015(3) O65A 0.086(2) 0.098(2) 0.206(4) 0.001(3) 0.013(2) -0.0341(19) C66A 0.097(3) 0.125(4) 0.149(5) -0.018(4) 0.041(3) -0.040(3) C67A 0.071(2) 0.084(3) 0.102(3) -0.018(2) 0.020(2) -0.017(2) C1B 0.0506(17) 0.052(2) 0.064(2) -0.0012(17) -0.0028(15) -0.0055(15) O1B 0.0585(13) 0.0564(14) 0.0833(17) -0.0139(12) -0.0164(11) -0.0007(11) C2B 0.0493(17) 0.0494(19) 0.0554(19) -0.0003(15) 0.0048(14) -0.0030(14) C21B 0.0545(17) 0.055(2) 0.0525(18) 0.0037(16) 0.0044(14) 0.0032(15) N2B 0.0547(15) 0.0497(16) 0.0540(15) -0.0014(13) 0.0033(12) 0.0013(12) C22B 0.0541(17) 0.0465(18) 0.0533(18) 0.0005(16) 0.0028(14) 0.0047(14) C23B 0.079(2) 0.064(2) 0.054(2) 0.0030(18) 0.0049(17) -0.0015(18) C24B 0.098(3) 0.057(2) 0.081(3) 0.016(2) 0.016(2) 0.004(2) C3B 0.0474(17) 0.062(2) 0.060(2) 0.0061(17) 0.0018(14) -0.0021(15) C4B 0.0551(18) 0.050(2) 0.060(2) 0.0037(16) -0.0010(15) -0.0075(15) C41B 0.0589(19) 0.057(2) 0.066(2) 0.0029(18) -0.0032(16) -0.0120(16) C42B 0.095(4) 0.087(4) 0.085(4) 0.011(3) -0.009(3) -0.039(3) C43B 0.084(4) 0.111(5) 0.099(5) -0.031(4) -0.005(3) -0.018(3) C44B 0.080(4) 0.080(4) 0.105(5) 0.014(3) -0.033(3) -0.024(3) C45B 0.095(4) 0.087(4) 0.085(4) 0.011(3) -0.009(3) -0.039(3) C46B 0.084(4) 0.111(5) 0.099(5) -0.031(4) -0.005(3) -0.018(3) C47B 0.080(4) 0.080(4) 0.105(5) 0.014(3) -0.033(3) -0.024(3) C5B 0.061(2) 0.051(2) 0.068(2) -0.0028(17) -0.0059(16) -0.0006(16) C6B 0.0559(19) 0.0509(19) 0.065(2) 0.0012(17) -0.0094(15) 0.0004(15) C61B 0.068(2) 0.063(2) 0.073(2) -0.006(2) -0.0160(17) 0.0088(18) N62B 0.0572(15) 0.0519(16) 0.0743(19) 0.0008(15) -0.0105(13) 0.0042(13) C63B 0.074(2) 0.076(3) 0.083(3) 0.012(2) -0.009(2) 0.002(2) C64B 0.079(3) 0.115(4) 0.081(3) 0.000(3) -0.002(2) 0.018(3) O65B 0.0622(15) 0.120(2) 0.099(2) -0.012(2) -0.0022(14) 0.0176(16) C66B 0.065(2) 0.076(3) 0.116(4) -0.011(3) -0.006(2) 0.014(2) C67B 0.060(2) 0.060(2) 0.088(3) 0.005(2) -0.0105(18) 0.0049(17) _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 C1A O1A 1.359(3) . ? C1A C6A 1.382(4) . ? C1A C2A 1.403(4) . ? C2A C3A 1.402(4) . ? C2A C21A 1.452(4) . ? C21A N2A 1.271(4) . ? N2A C22A 1.460(4) . ? C22A C22B 1.527(4) . ? C22A C23A 1.531(4) . ? C23A C24A 1.524(5) . ? C24A C24B 1.498(5) . ? C3A C4A 1.375(4) . ? C4A C5A 1.396(4) . ? C4A C41A 1.534(4) . ? C41A C46A 1.466(16) . ? C41A C47A 1.494(15) . ? C41A C45A 1.488(16) . ? C41A C44A 1.517(6) . ? C41A C43A 1.522(6) . ? C41A C42A 1.555(6) . ? C5A C6A 1.394(4) . ? C6A C61A 1.505(4) . ? C61A N62A 1.456(4) . ? N62A C63A 1.451(4) . ? N62A C67A 1.464(4) . ? C63A C64A 1.505(6) . ? C64A O65A 1.411(5) . ? O65A C66A 1.420(6) . ? C66A C67A 1.492(6) . ? C1B O1B 1.364(4) . ? C1B C6B 1.394(4) . ? C1B C2B 1.397(4) . ? C2B C3B 1.395(4) . ? C2B C21B 1.454(4) . ? C21B N2B 1.285(4) . ? N2B C22B 1.460(4) . ? C22B C23B 1.521(4) . ? C23B C24B 1.525(5) . ? C3B C4B 1.387(4) . ? C4B C5B 1.389(4) . ? C4B C41B 1.534(4) . ? C41B C45B 1.498(11) . ? C41B C42B 1.511(6) . ? C41B C46B 1.518(10) . ? C41B C43B 1.520(6) . ? C41B C44B 1.542(6) . ? C41B C47B 1.547(10) . ? C5B C6B 1.392(4) . ? C6B C61B 1.511(4) . ? C61B N62B 1.453(4) . ? N62B C63B 1.462(4) . ? N62B C67B 1.463(4) . ? C63B C64B 1.496(5) . ? C64B O65B 1.418(5) . ? O65B C66B 1.413(5) . ? C66B C67B 1.505(5) . ? 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 O1A C1A C6A 118.8(3) . . ? O1A C1A C2A 120.6(3) . . ? C6A C1A C2A 120.6(3) . . ? C3A C2A C1A 119.0(3) . . ? C3A C2A C21A 119.3(3) . . ? C1A C2A C21A 121.7(3) . . ? N2A C21A C2A 122.6(3) . . ? C21A N2A C22A 118.1(3) . . ? N2A C22A C22B 110.4(2) . . ? N2A C22A C23A 109.1(2) . . ? C22B C22A C23A 109.9(3) . . ? C24A C23A C22A 111.8(3) . . ? C24B C24A C23A 111.1(3) . . ? C4A C3A C2A 121.9(3) . . ? C3A C4A C5A 117.2(3) . . ? C3A C4A C41A 122.3(3) . . ? C5A C4A C41A 120.5(3) . . ? C46A C41A C47A 109.4(11) . . ? C46A C41A C45A 107.7(11) . . ? C47A C41A C45A 109.7(11) . . ? C46A C41A C44A 69.8(9) . . ? C47A C41A C44A 141.5(7) . . ? C45A C41A C44A 42.5(8) . . ? C46A C41A C43A 135.8(7) . . ? C47A C41A C43A 42.9(8) . . ? C45A C41A C43A 69.1(9) . . ? C44A C41A C43A 109.5(5) . . ? C46A C41A C4A 111.0(6) . . ? C47A C41A C4A 105.7(6) . . ? C45A C41A C4A 113.3(6) . . ? C44A C41A C4A 110.4(3) . . ? C43A C41A C4A 110.2(3) . . ? C46A C41A C42A 41.0(8) . . ? C47A C41A C42A 69.9(9) . . ? C45A C41A C42A 132.2(7) . . ? C44A C41A C42A 107.2(5) . . ? C43A C41A C42A 107.0(5) . . ? C4A C41A C42A 112.5(3) . . ? C6A C5A C4A 123.2(3) . . ? C1A C6A C5A 118.1(3) . . ? C1A C6A C61A 119.6(3) . . ? C5A C6A C61A 122.2(3) . . ? N62A C61A C6A 113.7(3) . . ? C63A N62A C61A 110.8(3) . . ? C63A N62A C67A 108.3(3) . . ? C61A N62A C67A 110.3(3) . . ? N62A C63A C64A 109.1(4) . . ? O65A C64A C63A 111.4(4) . . ? C64A O65A C66A 109.4(3) . . ? O65A C66A C67A 112.0(4) . . ? N62A C67A C66A 109.8(4) . . ? O1B C1B C6B 118.8(3) . . ? O1B C1B C2B 120.8(3) . . ? C6B C1B C2B 120.4(3) . . ? C3B C2B C1B 119.2(3) . . ? C3B C2B C21B 118.6(3) . . ? C1B C2B C21B 122.2(3) . . ? N2B C21B C2B 123.0(3) . . ? C21B N2B C22B 117.2(3) . . ? N2B C22B C23B 109.3(2) . . ? N2B C22B C22A 110.0(3) . . ? C23B C22B C22A 110.2(3) . . ? C22B C23B C24B 111.8(3) . . ? C24A C24B C23B 110.6(3) . . ? C4B C3B C2B 122.1(3) . . ? C3B C4B C5B 116.8(3) . . ? C3B C4B C41B 122.1(3) . . ? C5B C4B C41B 121.1(3) . . ? C45B C41B C42B 132.5(7) . . ? C45B C41B C46B 109.3(9) . . ? C42B C41B C46B 74.3(7) . . ? C45B C41B C43B 33.0(6) . . ? C42B C41B C43B 111.2(4) . . ? C46B C41B C43B 134.4(7) . . ? C45B C41B C4B 112.3(6) . . ? C42B C41B C4B 109.9(3) . . ? C46B C41B C4B 110.5(6) . . ? C43B C41B C4B 109.4(3) . . ? C45B C41B C44B 76.4(7) . . ? C42B C41B C44B 106.9(4) . . ? C46B C41B C44B 35.9(6) . . ? C43B C41B C44B 107.4(4) . . ? C4B C41B C44B 112.0(3) . . ? C45B C41B C47B 105.8(8) . . ? C42B C41B C47B 36.6(6) . . ? C46B C41B C47B 107.3(8) . . ? C43B C41B C47B 77.0(7) . . ? C4B C41B C47B 111.5(6) . . ? C44B C41B C47B 131.5(6) . . ? C4B C5B C6B 123.5(3) . . ? C5B C6B C1B 118.0(3) . . ? C5B C6B C61B 120.5(3) . . ? C1B C6B C61B 121.5(3) . . ? N62B C61B C6B 112.1(3) . . ? C61B N62B C63B 112.2(3) . . ? C61B N62B C67B 111.6(3) . . ? C63B N62B C67B 107.7(3) . . ? N62B C63B C64B 110.8(3) . . ? O65B C64B C63B 111.5(3) . . ? C66B O65B C64B 110.2(3) . . ? O65B C66B C67B 112.0(3) . . ? N62B C67B C66B 110.0(3) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 69.73 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.242 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.047 data_hmcyni _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Ni(LCy)](SO4).2CHCl3 _chemical_formula_sum 'C80 H116 Cl12 N8 Ni2 O16 S2' _chemical_formula_weight 2052.75 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' 'S' 'S' 0.3331 0.5567 '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' 'Ni' 'Ni' -3.0029 0.5091 '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 11.108(5) _cell_length_b 14.319(7) _cell_length_c 16.230(11) _cell_angle_alpha 99.26(3) _cell_angle_beta 107.95(3) _cell_angle_gamma 98.71(3) _cell_volume 2368(2) _cell_formula_units_Z 1 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 4.555 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.396 _exptl_absorpt_correction_T_max 0.509 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 10618 _diffrn_reflns_av_R_equivalents 0.1161 _diffrn_reflns_av_sigmaI/netI 0.1511 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 60.17 _reflns_number_total 6928 _reflns_number_gt 3543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _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. Attempts to model the solvent region with discrete CHCl3 molecules led to the development of very large Uij's for the Cl-atoms. Difference maps implied the presence of positional disorder, while the low angle data were generally rather poorly modelled. The solvent was treated in the manner described by van der Sluis and Spek, amounting to 224 e/cell. This corresponds to ca 2CHCl3 per formula unit, and this was taken into account in calculating F(000), density etc. ; _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^)+(0.1721P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00025(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6928 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1724 _refine_ls_R_factor_gt 0.1119 _refine_ls_wR_factor_ref 0.3271 _refine_ls_wR_factor_gt 0.2884 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.004 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.74615(12) 0.46983(10) 1.00936(9) 0.0267(4) Uani 1 1 d . . . O1 O 0.8559(5) 0.4108(4) 1.0852(4) 0.0416(16) Uani 1 1 d . . . C1 C 0.9714(7) 0.4527(7) 1.1441(6) 0.034(2) Uani 1 1 d . . . C2 C 1.0236(8) 0.4044(6) 1.2095(6) 0.033(2) Uani 1 1 d . . . C1A C 0.9551(8) 0.3095(7) 1.2178(7) 0.039(2) Uani 1 1 d . . . H1A1 H 1.0192 0.2714 1.2405 0.047 Uiso 1 1 calc R . . H1A2 H 0.8971 0.2731 1.1588 0.047 Uiso 1 1 calc R . . N2A N 0.8766(7) 0.3225(6) 1.2796(5) 0.043(2) Uani 1 1 d . . . H2A H 0.8327 0.2617 1.2772 0.052 Uiso 1 1 calc R . . C3A C 0.9599(9) 0.3642(7) 1.3752(7) 0.046(2) Uani 1 1 d . . . H3A1 H 1.0221 0.3234 1.3939 0.055 Uiso 1 1 calc R . . H3A2 H 1.0092 0.4289 1.3802 0.055 Uiso 1 1 calc R . . C4A C 0.8846(12) 0.3711(9) 1.4350(9) 0.069(4) Uani 1 1 d . . . H4A1 H 0.8392 0.3062 1.4333 0.083 Uiso 1 1 calc R . . H4A2 H 0.9430 0.3994 1.4960 0.083 Uiso 1 1 calc R . . O5A O 0.7907(10) 0.4314(7) 1.4081(7) 0.085(3) Uani 1 1 d . . . C6A C 0.7045(13) 0.3842(12) 1.3185(11) 0.088(5) Uani 1 1 d . . . H6A1 H 0.6363 0.4202 1.2997 0.106 Uiso 1 1 calc R . . H6A2 H 0.6632 0.3184 1.3179 0.106 Uiso 1 1 calc R . . C7A C 0.7800(10) 0.3797(8) 1.2540(8) 0.055(3) Uani 1 1 d . . . H7A1 H 0.7204 0.3505 1.1935 0.066 Uiso 1 1 calc R . . H7A2 H 0.8222 0.4453 1.2549 0.066 Uiso 1 1 calc R . . C3 C 1.1492(8) 0.4440(7) 1.2693(6) 0.039(2) Uani 1 1 d . . . H3 H 1.1872 0.4085 1.3104 0.047 Uiso 1 1 calc R . . C4 C 1.2211(7) 0.5339(6) 1.2708(6) 0.033(2) Uani 1 1 d . . . C41 C 1.3553(9) 0.5767(7) 1.3425(6) 0.039(2) Uani 1 1 d . . . C42 C 1.3331(11) 0.5930(9) 1.4331(8) 0.069(3) Uani 1 1 d . . . H42A H 1.4153 0.6205 1.4804 0.103 Uiso 1 1 calc R . . H42B H 1.2952 0.5315 1.4421 0.103 Uiso 1 1 calc R . . H42C H 1.2749 0.6371 1.4333 0.103 Uiso 1 1 calc R . . C43 C 1.4161(10) 0.6757(8) 1.3348(8) 0.061(3) Uani 1 1 d . . . H43A H 1.4997 0.6994 1.3816 0.092 Uiso 1 1 calc R . . H43B H 1.3600 0.7203 1.3405 0.092 Uiso 1 1 calc R . . H43C H 1.4274 0.6708 1.2774 0.092 Uiso 1 1 calc R . . C44 C 1.4452(9) 0.5089(10) 1.3421(8) 0.070(4) Uani 1 1 d . . . H44A H 1.5286 0.5376 1.3879 0.105 Uiso 1 1 calc R . . H44B H 1.4564 0.4968 1.2846 0.105 Uiso 1 1 calc R . . H44C H 1.4091 0.4482 1.3534 0.105 Uiso 1 1 calc R . . C5 C 1.1660(8) 0.5799(7) 1.2070(7) 0.043(2) Uani 1 1 d . . . H5 H 1.2127 0.6400 1.2061 0.052 Uiso 1 1 calc R . . C6 C 1.0428(8) 0.5428(6) 1.1417(6) 0.035(2) Uani 1 1 d . . . C7 C 0.9910(8) 0.5980(7) 1.0805(6) 0.038(2) Uani 1 1 d . . . H7 H 1.0452 0.6558 1.0818 0.045 Uiso 1 1 calc R . . N8 N 0.8748(7) 0.5761(5) 1.0225(5) 0.0390(19) Uani 1 1 d . . . C9 C 0.8239(8) 0.6351(8) 0.9595(7) 0.044(2) Uani 1 1 d . . . H9 H 0.8161 0.6005 0.8996 0.053 Uiso 1 1 calc R . . C10 C 0.9058(9) 0.7387(7) 0.9775(8) 0.049(3) Uani 1 1 d . . . H10A H 0.9202 0.7733 1.0381 0.059 Uiso 1 1 calc R . . H10B H 0.9904 0.7351 0.9717 0.059 Uiso 1 1 calc R . . C11 C 0.8348(10) 0.7928(8) 0.9111(8) 0.057(3) Uani 1 1 d . . . H11A H 0.8318 0.7625 0.8517 0.068 Uiso 1 1 calc R . . H11B H 0.8839 0.8597 0.9258 0.068 Uiso 1 1 calc R . . C12 C 0.6973(9) 0.7940(8) 0.9093(9) 0.062(3) Uani 1 1 d . . . H12A H 0.6997 0.8318 0.9660 0.074 Uiso 1 1 calc R . . H12B H 0.6546 0.8252 0.8621 0.074 Uiso 1 1 calc R . . C13 C 0.6220(9) 0.6938(7) 0.8933(7) 0.043(2) Uani 1 1 d . . . H13A H 0.6096 0.6591 0.8331 0.051 Uiso 1 1 calc R . . H13B H 0.5362 0.6966 0.8972 0.051 Uiso 1 1 calc R . . C14 C 0.6902(8) 0.6369(7) 0.9609(9) 0.052(3) Uani 1 1 d . . . H14 H 0.6963 0.6694 1.0212 0.063 Uiso 1 1 calc R . . N15 N 0.6331(7) 0.5333(5) 0.9455(6) 0.0422(19) Uani 1 1 d . . . C16 C 0.5115(9) 0.4980(7) 0.8965(7) 0.043(2) Uani 1 1 d . . . H16 H 0.4619 0.5414 0.8733 0.051 Uiso 1 1 calc R . . C17 C 0.4493(8) 0.3988(6) 0.8758(6) 0.036(2) Uani 1 1 d . . . C18 C 0.3257(8) 0.3657(6) 0.8074(6) 0.033(2) Uani 1 1 d . . . H18 H 0.2863 0.4108 0.7786 0.039 Uiso 1 1 calc R . . C19 C 0.2627(8) 0.2709(7) 0.7824(7) 0.044(2) Uani 1 1 d . . . C191 C 0.1320(8) 0.2308(7) 0.7093(6) 0.041(2) Uani 1 1 d . . . C192 C 0.1444(13) 0.1607(11) 0.6380(10) 0.091(5) Uani 1 1 d . . . H19A H 0.2086 0.1909 0.6158 0.136 Uiso 1 1 calc R . . H19B H 0.0615 0.1389 0.5902 0.136 Uiso 1 1 calc R . . H19C H 0.1712 0.1057 0.6606 0.136 Uiso 1 1 calc R . . C193 C 0.0793(12) 0.3130(10) 0.6644(11) 0.096(5) Uani 1 1 d . . . H19D H 0.0664 0.3614 0.7082 0.145 Uiso 1 1 calc R . . H19E H -0.0025 0.2851 0.6167 0.145 Uiso 1 1 calc R . . H19F H 0.1415 0.3431 0.6405 0.145 Uiso 1 1 calc R . . C194 C 0.0302(10) 0.1817(11) 0.7450(9) 0.081(4) Uani 1 1 d . . . H19G H 0.0204 0.2284 0.7916 0.121 Uiso 1 1 calc R . . H19H H 0.0589 0.1277 0.7688 0.121 Uiso 1 1 calc R . . H19I H -0.0522 0.1582 0.6971 0.121 Uiso 1 1 calc R . . C20 C 0.3238(8) 0.2046(7) 0.8298(6) 0.039(2) Uani 1 1 d . . . H20 H 0.2814 0.1391 0.8155 0.046 Uiso 1 1 calc R . . C21 C 0.4457(8) 0.2359(6) 0.8970(6) 0.034(2) Uani 1 1 d . . . C1B C 0.5099(9) 0.1653(6) 0.9428(6) 0.039(2) Uani 1 1 d . . . H1B1 H 0.4435 0.1143 0.9467 0.047 Uiso 1 1 calc R . . H1B2 H 0.5651 0.1985 1.0034 0.047 Uiso 1 1 calc R . . N2B N 0.5938(7) 0.1179(5) 0.8942(5) 0.0395(18) Uani 1 1 d . . . H2B H 0.5448 0.0588 0.8596 0.047 Uiso 1 1 calc R . . C3B C 0.6396(11) 0.1699(9) 0.8388(9) 0.063(3) Uani 1 1 d . . . H3B1 H 0.6855 0.2351 0.8735 0.076 Uiso 1 1 calc R . . H3B2 H 0.5648 0.1765 0.7905 0.076 Uiso 1 1 calc R . . C4B C 0.7279(12) 0.1250(10) 0.7991(9) 0.071(4) Uani 1 1 d . . . H4B1 H 0.6783 0.0651 0.7555 0.085 Uiso 1 1 calc R . . H4B2 H 0.7625 0.1694 0.7678 0.085 Uiso 1 1 calc R . . O5B O 0.8281(6) 0.1046(6) 0.8618(6) 0.062(2) Uani 1 1 d . . . C6B C 0.7921(12) 0.0507(10) 0.9165(10) 0.078(4) Uani 1 1 d . . . H6B1 H 0.8697 0.0443 0.9626 0.093 Uiso 1 1 calc R . . H6B2 H 0.7451 -0.0144 0.8818 0.093 Uiso 1 1 calc R . . C7B C 0.7030(11) 0.0997(12) 0.9617(9) 0.082(4) Uani 1 1 d . . . H7B1 H 0.6715 0.0570 0.9956 0.098 Uiso 1 1 calc R . . H7B2 H 0.7533 0.1609 1.0030 0.098 Uiso 1 1 calc R . . C22 C 0.5128(7) 0.3326(6) 0.9208(6) 0.032(2) Uani 1 1 d . . . O22 O 0.6257(5) 0.3573(4) 0.9846(4) 0.0394(15) Uani 1 1 d . . . S1' S 0.6699(3) 0.0964(2) 1.19660(19) 0.0581(8) Uani 1 1 d . . . O1' O 0.6293(10) 0.1696(7) 1.1464(7) 0.093(3) Uani 1 1 d . . . O2' O 0.5597(9) 0.0427(7) 1.2159(6) 0.095(3) Uani 1 1 d . . . O3' O 0.7240(9) 0.0280(7) 1.1499(6) 0.086(3) Uani 1 1 d . . . O4' O 0.7681(7) 0.1488(6) 1.2826(5) 0.073(2) 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 Ni1 0.0212(7) 0.0297(8) 0.0289(8) 0.0115(6) 0.0068(6) 0.0026(5) O1 0.025(3) 0.037(4) 0.054(4) 0.014(3) 0.001(3) 0.002(3) C1 0.018(4) 0.047(5) 0.037(5) 0.006(4) 0.008(4) 0.019(4) C2 0.031(5) 0.039(5) 0.035(5) 0.009(4) 0.020(4) 0.006(4) C1A 0.031(5) 0.041(5) 0.053(6) 0.015(5) 0.019(5) 0.016(4) N2A 0.041(4) 0.054(5) 0.050(5) 0.028(4) 0.028(4) 0.014(4) C3A 0.047(5) 0.046(6) 0.045(6) 0.010(5) 0.019(5) 0.006(4) C4A 0.080(8) 0.076(8) 0.081(9) 0.037(7) 0.057(8) 0.018(7) O5A 0.110(7) 0.093(7) 0.091(7) 0.036(6) 0.072(7) 0.044(6) C6A 0.070(8) 0.114(12) 0.113(13) 0.026(10) 0.056(9) 0.063(8) C7A 0.063(7) 0.052(6) 0.080(8) 0.029(6) 0.050(7) 0.032(5) C3 0.035(5) 0.053(6) 0.035(5) 0.016(5) 0.012(4) 0.015(4) C4 0.022(4) 0.038(5) 0.039(5) 0.002(4) 0.018(4) 0.001(4) C41 0.045(5) 0.041(5) 0.031(5) 0.010(4) 0.010(4) 0.014(4) C42 0.061(7) 0.073(8) 0.048(7) -0.014(6) 0.009(6) -0.012(6) C43 0.045(6) 0.061(7) 0.054(7) 0.009(6) -0.007(5) -0.007(5) C44 0.030(5) 0.118(11) 0.060(8) 0.027(7) 0.007(5) 0.021(6) C5 0.024(4) 0.051(6) 0.056(6) 0.026(5) 0.010(5) 0.003(4) C6 0.040(5) 0.030(5) 0.033(5) 0.006(4) 0.013(4) -0.002(4) C7 0.026(5) 0.061(6) 0.024(5) 0.017(4) 0.004(4) 0.006(4) N8 0.032(4) 0.035(4) 0.049(5) 0.019(4) 0.008(4) 0.006(3) C9 0.032(5) 0.068(7) 0.045(6) 0.036(5) 0.014(5) 0.019(5) C10 0.033(5) 0.048(6) 0.066(7) 0.017(5) 0.019(5) -0.004(4) C11 0.052(6) 0.041(6) 0.080(8) 0.021(6) 0.023(6) 0.008(5) C12 0.043(6) 0.050(7) 0.084(9) 0.009(6) 0.016(6) 0.004(5) C13 0.044(5) 0.035(5) 0.054(6) 0.024(5) 0.012(5) 0.018(4) C14 0.018(4) 0.031(5) 0.093(9) 0.012(5) 0.002(5) -0.001(4) N15 0.035(4) 0.038(5) 0.053(5) 0.020(4) 0.011(4) 0.004(3) C16 0.042(6) 0.032(5) 0.059(7) 0.014(5) 0.021(5) 0.011(4) C17 0.035(5) 0.031(5) 0.042(6) 0.019(4) 0.006(4) 0.010(4) C18 0.034(5) 0.044(5) 0.029(5) 0.005(4) 0.020(4) 0.014(4) C19 0.021(4) 0.044(6) 0.062(7) 0.000(5) 0.017(5) -0.004(4) C191 0.030(5) 0.043(6) 0.032(5) 0.004(4) -0.007(4) -0.001(4) C192 0.078(9) 0.097(11) 0.071(10) -0.018(8) 0.014(8) 0.005(8) C193 0.051(7) 0.086(10) 0.115(13) 0.051(9) -0.031(7) -0.004(6) C194 0.031(6) 0.135(12) 0.071(9) 0.037(8) 0.016(6) -0.010(6) C20 0.036(5) 0.038(5) 0.041(6) 0.010(4) 0.013(4) 0.008(4) C21 0.028(4) 0.034(5) 0.045(6) 0.014(4) 0.015(4) 0.015(4) C1B 0.051(5) 0.024(5) 0.040(6) 0.007(4) 0.014(5) 0.006(4) N2B 0.035(4) 0.036(4) 0.053(5) 0.017(4) 0.018(4) 0.010(3) C3B 0.072(7) 0.074(8) 0.077(8) 0.048(7) 0.046(7) 0.038(6) C4B 0.065(8) 0.090(9) 0.079(9) 0.022(7) 0.039(7) 0.045(7) O5B 0.035(4) 0.075(5) 0.073(6) 0.010(4) 0.017(4) 0.011(3) C6B 0.073(8) 0.086(9) 0.109(11) 0.052(9) 0.041(8) 0.063(7) C7B 0.046(7) 0.135(13) 0.067(9) 0.043(9) 0.006(6) 0.034(7) C22 0.011(4) 0.040(5) 0.042(5) 0.013(4) 0.005(4) 0.004(3) O22 0.028(3) 0.046(4) 0.046(4) 0.021(3) 0.010(3) 0.006(3) S1' 0.0583(17) 0.0573(18) 0.0521(17) 0.0125(14) 0.0183(14) -0.0062(13) O1' 0.114(8) 0.083(7) 0.080(7) 0.032(6) 0.015(6) 0.036(6) O2' 0.089(6) 0.096(7) 0.073(6) -0.009(5) 0.034(5) -0.040(5) O3' 0.104(7) 0.078(6) 0.086(7) 0.003(5) 0.059(6) 0.011(5) O4' 0.057(5) 0.082(6) 0.056(5) 0.025(4) -0.007(4) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N15 1.824(8) . ? Ni1 O22 1.832(6) . ? Ni1 O1 1.854(6) . ? Ni1 N8 1.859(7) . ? O1 C1 1.321(10) . ? C1 C2 1.385(12) . ? C1 C6 1.422(12) . ? C2 C3 1.399(13) . ? C2 C1A 1.502(12) . ? C1A N2A 1.527(10) . ? N2A C7A 1.448(12) . ? N2A C3A 1.507(13) . ? C3A C4A 1.465(13) . ? C4A O5A 1.462(14) . ? O5A C6A 1.454(18) . ? C6A C7A 1.530(15) . ? C3 C4 1.400(12) . ? C4 C5 1.355(13) . ? C4 C41 1.541(12) . ? C41 C44 1.496(14) . ? C41 C43 1.517(14) . ? C41 C42 1.552(14) . ? C5 C6 1.408(13) . ? C6 C7 1.407(13) . ? C7 N8 1.298(11) . ? N8 C9 1.464(11) . ? C9 C14 1.497(12) . ? C9 C10 1.549(13) . ? C10 C11 1.521(15) . ? C11 C12 1.522(14) . ? C12 C13 1.487(13) . ? C13 C14 1.550(14) . ? C14 N15 1.470(11) . ? N15 C16 1.309(12) . ? C16 C17 1.419(12) . ? C17 C22 1.428(12) . ? C17 C18 1.427(12) . ? C18 C19 1.362(12) . ? C19 C20 1.436(14) . ? C19 C191 1.520(13) . ? C191 C192 1.460(16) . ? C191 C194 1.550(13) . ? C191 C193 1.576(15) . ? C20 C21 1.405(13) . ? C21 C22 1.399(12) . ? C21 C1B 1.489(12) . ? C1B N2B 1.557(11) . ? N2B C3B 1.415(12) . ? N2B C7B 1.452(13) . ? C3B C4B 1.496(14) . ? C4B O5B 1.363(14) . ? O5B C6B 1.374(14) . ? C6B C7B 1.582(16) . ? C22 O22 1.311(10) . ? S1' O3' 1.455(9) . ? S1' O1' 1.468(9) . ? S1' O4' 1.475(8) . ? S1' O2' 1.489(8) . ? 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 N15 Ni1 O22 94.9(3) . . ? N15 Ni1 O1 173.5(3) . . ? O22 Ni1 O1 85.2(3) . . ? N15 Ni1 N8 86.2(3) . . ? O22 Ni1 N8 172.5(3) . . ? O1 Ni1 N8 94.6(3) . . ? C1 O1 Ni1 126.4(6) . . ? O1 C1 C2 117.3(8) . . ? O1 C1 C6 122.8(8) . . ? C2 C1 C6 119.9(8) . . ? C1 C2 C3 118.5(8) . . ? C1 C2 C1A 123.7(8) . . ? C3 C2 C1A 117.8(8) . . ? C2 C1A N2A 112.4(7) . . ? C7A N2A C3A 108.7(8) . . ? C7A N2A C1A 114.3(7) . . ? C3A N2A C1A 113.1(7) . . ? C4A C3A N2A 112.9(9) . . ? O5A C4A C3A 109.9(9) . . ? C6A O5A C4A 107.2(10) . . ? O5A C6A C7A 110.5(10) . . ? N2A C7A C6A 109.4(9) . . ? C4 C3 C2 123.3(9) . . ? C5 C4 C3 116.4(8) . . ? C5 C4 C41 122.8(8) . . ? C3 C4 C41 120.8(8) . . ? C44 C41 C43 110.5(9) . . ? C44 C41 C4 111.3(8) . . ? C43 C41 C4 112.9(8) . . ? C44 C41 C42 109.5(9) . . ? C43 C41 C42 105.7(9) . . ? C4 C41 C42 106.5(7) . . ? C4 C5 C6 123.8(8) . . ? C5 C6 C7 119.7(8) . . ? C5 C6 C1 118.0(9) . . ? C7 C6 C1 122.2(8) . . ? N8 C7 C6 125.7(8) . . ? C7 N8 C9 124.4(8) . . ? C7 N8 Ni1 125.9(7) . . ? C9 N8 Ni1 109.7(6) . . ? N8 C9 C14 105.0(7) . . ? N8 C9 C10 115.9(8) . . ? C14 C9 C10 111.7(8) . . ? C11 C10 C9 109.3(8) . . ? C10 C11 C12 113.6(9) . . ? C13 C12 C11 110.6(9) . . ? C12 C13 C14 112.3(9) . . ? N15 C14 C9 102.1(8) . . ? N15 C14 C13 117.3(8) . . ? C9 C14 C13 110.5(8) . . ? C16 N15 C14 120.7(8) . . ? C16 N15 Ni1 127.2(7) . . ? C14 N15 Ni1 111.9(6) . . ? N15 C16 C17 124.7(9) . . ? C16 C17 C22 119.9(8) . . ? C16 C17 C18 119.3(8) . . ? C22 C17 C18 120.7(8) . . ? C19 C18 C17 122.2(9) . . ? C18 C19 C20 117.4(9) . . ? C18 C19 C191 124.8(9) . . ? C20 C19 C191 117.8(8) . . ? C192 C191 C19 110.4(9) . . ? C192 C191 C194 109.2(10) . . ? C19 C191 C194 111.7(8) . . ? C192 C191 C193 105.3(11) . . ? C19 C191 C193 111.1(8) . . ? C194 C191 C193 108.9(9) . . ? C21 C20 C19 121.1(8) . . ? C22 C21 C20 121.7(8) . . ? C22 C21 C1B 117.9(8) . . ? C20 C21 C1B 120.3(8) . . ? C21 C1B N2B 112.7(7) . . ? C3B N2B C7B 109.5(9) . . ? C3B N2B C1B 117.1(7) . . ? C7B N2B C1B 107.2(8) . . ? N2B C3B C4B 115.0(10) . . ? O5B C4B C3B 112.0(11) . . ? C4B O5B C6B 114.8(9) . . ? O5B C6B C7B 111.2(10) . . ? N2B C7B C6B 109.8(10) . . ? O22 C22 C21 118.7(8) . . ? O22 C22 C17 124.4(8) . . ? C21 C22 C17 116.8(8) . . ? C22 O22 Ni1 126.0(6) . . ? O3' S1' O1' 111.9(6) . . ? O3' S1' O4' 110.0(6) . . ? O1' S1' O4' 107.0(6) . . ? O3' S1' O2' 109.4(6) . . ? O1' S1' O2' 111.1(6) . . ? O4' S1' O2' 107.3(5) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 60.17 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.577 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.103 data_n1nl12 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety NiL _chemical_formula_sum 'C34 H48 N4 Ni O4' _chemical_formula_weight 635.47 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3052(5) _cell_length_b 15.1256(14) _cell_length_c 15.6704(14) _cell_angle_alpha 72.470(3) _cell_angle_beta 87.161(5) _cell_angle_gamma 81.267(4) _cell_volume 1631.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.637 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Kappa CCD' _diffrn_measurement_method Omega-phi _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23521 _diffrn_reflns_av_R_equivalents 0.1733 _diffrn_reflns_av_sigmaI/netI 0.1968 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 26.31 _reflns_number_total 6557 _reflns_number_gt 3256 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR92 _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^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6557 _refine_ls_number_parameters 385 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1630 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.34097(7) 0.42750(4) 0.51199(3) 0.02740(18) Uani 1 1 d . . . C1A C 0.2791(5) 0.5269(3) 0.3282(3) 0.0267(10) Uani 1 1 d . . . O1A O 0.3470(3) 0.44987(18) 0.38929(16) 0.0282(7) Uani 1 1 d . . . C2A C 0.1960(5) 0.6088(3) 0.3472(3) 0.0258(9) Uani 1 1 d . . . C21A C 0.1713(5) 0.6131(3) 0.4369(3) 0.0285(10) Uani 1 1 d . . . H21A H 0.1167 0.6710 0.4453 0.034 Uiso 1 1 calc R . . N2A N 0.2178(4) 0.5439(2) 0.5074(2) 0.0257(8) Uani 1 1 d . . . C22A C 0.1895(7) 0.5625(3) 0.5946(3) 0.0545(13) Uani 1 1 d . . . H22A H 0.0602 0.5919 0.5990 0.065 Uiso 1 1 calc R . . H22B H 0.2728 0.6068 0.5991 0.065 Uiso 1 1 calc R . . C3A C 0.1306(5) 0.6892(3) 0.2768(3) 0.0326(11) Uani 1 1 d . . . H3A H 0.0787 0.7444 0.2913 0.039 Uiso 1 1 calc R . . C4A C 0.1382(5) 0.6916(3) 0.1887(3) 0.0339(11) Uani 1 1 d . . . C41A C 0.0738(6) 0.7773(3) 0.1098(3) 0.0398(11) Uani 1 1 d . . . C42A C 0.0048(6) 0.8632(3) 0.1416(3) 0.0527(13) Uani 1 1 d . . . H42A H -0.0342 0.9172 0.0898 0.079 Uiso 1 1 calc R . . H42B H 0.1050 0.8770 0.1727 0.079 Uiso 1 1 calc R . . H42C H -0.1004 0.8503 0.1824 0.079 Uiso 1 1 calc R . . C43A C -0.0847(6) 0.7582(3) 0.0604(3) 0.0529(13) Uani 1 1 d . . . H43A H -0.1244 0.8136 0.0100 0.079 Uiso 1 1 calc R . . H43B H -0.1891 0.7442 0.1016 0.079 Uiso 1 1 calc R . . H43C H -0.0420 0.7047 0.0380 0.079 Uiso 1 1 calc R . . C44A C 0.2351(6) 0.7999(3) 0.0442(3) 0.0574(14) Uani 1 1 d . . . H44A H 0.1936 0.8553 -0.0060 0.086 Uiso 1 1 calc R . . H44B H 0.2774 0.7465 0.0216 0.086 Uiso 1 1 calc R . . H44C H 0.3372 0.8125 0.0750 0.086 Uiso 1 1 calc R . . C5A C 0.2126(5) 0.6074(3) 0.1715(3) 0.0340(11) Uani 1 1 d . . . H5A H 0.2126 0.6057 0.1114 0.041 Uiso 1 1 calc R . . C6A C 0.2861(5) 0.5267(3) 0.2365(3) 0.0271(10) Uani 1 1 d . . . C61A C 0.3653(5) 0.4399(3) 0.2134(2) 0.0320(10) Uani 1 1 d . . . H61A H 0.3465 0.3850 0.2649 0.038 Uiso 1 1 calc R . . H61B H 0.2954 0.4364 0.1622 0.038 Uiso 1 1 calc R . . N62A N 0.5650(4) 0.4333(2) 0.1900(2) 0.0317(8) Uani 1 1 d . . . C63A C 0.6244(6) 0.3445(3) 0.1707(3) 0.0481(12) Uani 1 1 d . . . H63A H 0.5466 0.3405 0.1223 0.058 Uiso 1 1 calc R . . H63B H 0.6066 0.2920 0.2247 0.058 Uiso 1 1 calc R . . C64A C 0.8254(6) 0.3355(3) 0.1424(3) 0.0610(14) Uani 1 1 d . . . H64A H 0.9040 0.3365 0.1917 0.073 Uiso 1 1 calc R . . H64B H 0.8616 0.2749 0.1298 0.073 Uiso 1 1 calc R . . O65A O 0.8545(4) 0.4102(2) 0.0646(2) 0.0619(9) Uani 1 1 d . . . C66A C 0.8046(6) 0.4965(3) 0.0845(3) 0.0495(13) Uani 1 1 d . . . H66A H 0.8263 0.5488 0.0310 0.059 Uiso 1 1 calc R . . H66B H 0.8848 0.4979 0.1331 0.059 Uiso 1 1 calc R . . C67A C 0.6052(5) 0.5105(3) 0.1128(3) 0.0375(11) Uani 1 1 d . . . H67A H 0.5780 0.5701 0.1281 0.045 Uiso 1 1 calc R . . H67B H 0.5243 0.5150 0.0624 0.045 Uiso 1 1 calc R . . O1B O 0.4809(3) 0.31426(18) 0.51547(16) 0.0279(7) Uani 1 1 d . . . C1B C 0.5160(5) 0.2404(3) 0.5849(3) 0.0257(9) Uani 1 1 d . . . C2B C 0.4586(5) 0.2376(3) 0.6726(3) 0.0270(10) Uani 1 1 d . . . C21B C 0.3690(5) 0.3198(3) 0.6920(3) 0.0303(10) Uani 1 1 d . . . H21B H 0.3432 0.3151 0.7531 0.036 Uiso 1 1 calc R . . N2B N 0.3199(4) 0.3999(2) 0.6343(2) 0.0229(7) Uani 1 1 d . . . C22B C 0.2276(5) 0.4748(3) 0.6690(3) 0.0364(11) Uani 1 1 d . . . H22C H 0.3076 0.4842 0.7138 0.044 Uiso 1 1 calc R . . H22D H 0.1100 0.4574 0.6987 0.044 Uiso 1 1 calc R . . C3B C 0.4895(5) 0.1520(3) 0.7427(3) 0.0353(11) Uani 1 1 d . . . H3B H 0.4529 0.1517 0.8018 0.042 Uiso 1 1 calc R . . C4B C 0.5707(5) 0.0693(3) 0.7283(3) 0.0356(11) Uani 1 1 d . A . C41B C 0.5887(5) -0.0269(3) 0.8002(3) 0.0435(12) Uani 1 1 d D . . C42B C 0.5097(14) -0.0216(8) 0.8911(5) 0.041(3) Uiso 0.50 1 d PD A 1 H42D H 0.5255 -0.0845 0.9341 0.061 Uiso 0.50 1 calc PR A 1 H42E H 0.3776 0.0035 0.8849 0.061 Uiso 0.50 1 calc PR A 1 H42F H 0.5754 0.0195 0.9124 0.061 Uiso 0.50 1 calc PR A 1 C43B C 0.4866(13) -0.0924(7) 0.7686(7) 0.044(3) Uiso 0.50 1 d PD A 1 H43D H 0.4976 -0.1538 0.8140 0.066 Uiso 0.50 1 calc PR A 1 H43E H 0.5412 -0.0994 0.7122 0.066 Uiso 0.50 1 calc PR A 1 H43F H 0.3556 -0.0659 0.7594 0.066 Uiso 0.50 1 calc PR A 1 C44B C 0.7976(9) -0.0675(8) 0.8086(8) 0.046(4) Uiso 0.50 1 d PD A 1 H44D H 0.8140 -0.1289 0.8542 0.069 Uiso 0.50 1 calc PR A 1 H44E H 0.8662 -0.0249 0.8261 0.069 Uiso 0.50 1 calc PR A 1 H44F H 0.8443 -0.0745 0.7509 0.069 Uiso 0.50 1 calc PR A 1 C45B C 0.5569(14) -0.0156(8) 0.8949(5) 0.034(3) Uiso 0.50 1 d PD A 2 H45A H 0.5695 -0.0775 0.9395 0.051 Uiso 0.50 1 calc PR A 2 H45B H 0.4322 0.0177 0.8987 0.051 Uiso 0.50 1 calc PR A 2 H45C H 0.6488 0.0203 0.9066 0.051 Uiso 0.50 1 calc PR A 2 C46B C 0.4350(13) -0.0786(8) 0.7810(8) 0.059(4) Uiso 0.50 1 d PD A 2 H46A H 0.4411 -0.1405 0.8254 0.088 Uiso 0.50 1 calc PR A 2 H46B H 0.4532 -0.0860 0.7210 0.088 Uiso 0.50 1 calc PR A 2 H46C H 0.3135 -0.0421 0.7843 0.088 Uiso 0.50 1 calc PR A 2 C47B C 0.7783(10) -0.0849(8) 0.8006(9) 0.054(4) Uiso 0.50 1 d PD A 2 H47A H 0.7820 -0.1449 0.8478 0.081 Uiso 0.50 1 calc PR A 2 H47B H 0.8738 -0.0508 0.8119 0.081 Uiso 0.50 1 calc PR A 2 H47C H 0.8012 -0.0964 0.7425 0.081 Uiso 0.50 1 calc PR A 2 C5B C 0.6334(5) 0.0750(3) 0.6403(3) 0.0334(10) Uani 1 1 d . . . H5B H 0.6913 0.0194 0.6283 0.040 Uiso 1 1 calc R A . C6B C 0.6146(5) 0.1570(3) 0.5714(3) 0.0279(10) Uani 1 1 d . A . C61B C 0.6928(5) 0.1598(3) 0.4810(3) 0.0287(10) Uani 1 1 d . . . H61C H 0.7007 0.0969 0.4729 0.034 Uiso 1 1 calc R A . H61D H 0.6085 0.2041 0.4347 0.034 Uiso 1 1 calc R . . N62B N 0.8790(4) 0.1892(2) 0.4688(2) 0.0375(9) Uani 1 1 d . A . C63B C 1.0114(5) 0.1199(3) 0.5309(4) 0.0592(15) Uani 1 1 d . . . H63C H 1.0066 0.0568 0.5254 0.071 Uiso 1 1 calc R A . H63D H 0.9781 0.1189 0.5932 0.071 Uiso 1 1 calc R . . C64B C 1.2050(7) 0.1446(4) 0.5099(5) 0.098(2) Uani 1 1 d . A . H64C H 1.2108 0.2056 0.5201 0.118 Uiso 1 1 calc R . . H64D H 1.2933 0.0966 0.5514 0.118 Uiso 1 1 calc R . . O65B O 1.2598(5) 0.1501(4) 0.4209(5) 0.116(2) Uani 1 1 d . . . C66B C 1.1391(8) 0.2222(4) 0.3648(5) 0.093(2) Uani 1 1 d . A . H66C H 1.1777 0.2305 0.3018 0.111 Uiso 1 1 calc R . . H66D H 1.1454 0.2815 0.3784 0.111 Uiso 1 1 calc R . . C67B C 0.9390(6) 0.2005(3) 0.3771(3) 0.0580(14) Uani 1 1 d . . . H67C H 0.8561 0.2522 0.3363 0.070 Uiso 1 1 calc R A . H67D H 0.9315 0.1423 0.3616 0.070 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 Ni1 0.0309(3) 0.0254(3) 0.0258(3) -0.0083(2) 0.0009(2) -0.0024(2) C1A 0.022(2) 0.028(3) 0.028(3) -0.005(2) 0.0021(18) -0.0044(18) O1A 0.0345(15) 0.0257(17) 0.0241(16) -0.0085(14) 0.0001(12) -0.0012(13) C2A 0.025(2) 0.025(3) 0.024(3) -0.005(2) 0.0019(18) -0.0016(18) C21A 0.028(2) 0.023(3) 0.034(3) -0.010(2) 0.0058(19) -0.0018(18) N2A 0.0295(18) 0.024(2) 0.023(2) -0.0081(18) 0.0038(15) -0.0001(15) C22A 0.084(4) 0.045(3) 0.034(3) -0.019(3) 0.021(3) -0.001(3) C3A 0.028(2) 0.030(3) 0.040(3) -0.011(2) 0.001(2) -0.0037(19) C4A 0.032(2) 0.035(3) 0.033(3) -0.006(2) 0.002(2) -0.009(2) C41A 0.046(3) 0.030(3) 0.034(3) 0.002(2) 0.000(2) -0.002(2) C42A 0.061(3) 0.040(3) 0.046(3) 0.002(3) -0.004(2) 0.001(2) C43A 0.050(3) 0.059(4) 0.036(3) 0.004(3) -0.006(2) -0.001(2) C44A 0.052(3) 0.051(3) 0.051(3) 0.011(3) 0.005(2) -0.010(3) C5A 0.033(2) 0.046(3) 0.023(3) -0.005(2) 0.0008(19) -0.014(2) C6A 0.030(2) 0.026(3) 0.024(2) -0.005(2) 0.0006(18) -0.0060(19) C61A 0.037(2) 0.033(3) 0.023(2) -0.005(2) -0.0014(19) -0.006(2) N62A 0.042(2) 0.029(2) 0.023(2) -0.0080(17) 0.0093(16) -0.0047(16) C63A 0.063(3) 0.037(3) 0.044(3) -0.014(2) 0.018(2) -0.008(2) C64A 0.074(4) 0.045(3) 0.060(4) -0.018(3) 0.029(3) -0.001(3) O65A 0.082(2) 0.056(2) 0.047(2) -0.022(2) 0.0333(18) -0.0082(19) C66A 0.059(3) 0.052(4) 0.037(3) -0.014(3) 0.022(2) -0.012(3) C67A 0.047(3) 0.042(3) 0.027(3) -0.014(2) 0.006(2) -0.011(2) O1B 0.0356(16) 0.0230(17) 0.0223(16) -0.0063(14) 0.0040(12) 0.0018(12) C1B 0.031(2) 0.020(2) 0.025(3) -0.005(2) -0.0017(19) -0.0036(18) C2B 0.035(2) 0.024(3) 0.022(3) -0.007(2) 0.0014(18) -0.0029(19) C21B 0.035(2) 0.036(3) 0.021(2) -0.009(2) 0.0044(19) -0.006(2) N2B 0.0293(18) 0.021(2) 0.020(2) -0.0096(17) 0.0027(14) 0.0001(15) C22B 0.041(2) 0.039(3) 0.033(3) -0.019(2) -0.001(2) 0.001(2) C3B 0.047(3) 0.037(3) 0.022(3) -0.008(2) 0.005(2) -0.007(2) C4B 0.048(3) 0.028(3) 0.028(3) -0.006(2) -0.005(2) 0.000(2) C41B 0.069(3) 0.031(3) 0.029(3) -0.006(2) 0.001(2) -0.005(2) C5B 0.041(2) 0.025(3) 0.034(3) -0.011(2) -0.005(2) 0.0023(19) C6B 0.030(2) 0.025(3) 0.029(3) -0.008(2) -0.0022(18) -0.0029(19) C61B 0.027(2) 0.024(2) 0.034(3) -0.008(2) 0.0005(18) 0.0002(18) N62B 0.0328(19) 0.030(2) 0.053(3) -0.0188(19) 0.0092(18) -0.0064(16) C63B 0.034(3) 0.051(3) 0.099(4) -0.031(3) -0.012(3) -0.007(2) C64B 0.040(4) 0.073(5) 0.198(8) -0.065(5) -0.020(4) -0.001(3) O65B 0.041(2) 0.084(4) 0.251(7) -0.095(4) 0.045(3) -0.021(2) C66B 0.085(5) 0.073(5) 0.150(7) -0.072(5) 0.078(4) -0.045(4) C67B 0.062(3) 0.051(3) 0.070(4) -0.031(3) 0.039(3) -0.021(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2A 1.834(3) . ? Ni1 N2B 1.838(3) . ? Ni1 O1B 1.844(3) . ? Ni1 O1A 1.849(2) . ? C1A O1A 1.311(4) . ? C1A C2A 1.404(5) . ? C1A C6A 1.436(5) . ? C2A C3A 1.411(5) . ? C2A C21A 1.429(5) . ? C21A N2A 1.290(4) . ? N2A C22A 1.474(5) . ? C22A C22B 1.478(5) . ? C3A C4A 1.369(5) . ? C4A C5A 1.405(5) . ? C4A C41A 1.528(5) . ? C41A C43A 1.533(5) . ? C41A C42A 1.535(6) . ? C41A C44A 1.534(5) . ? C5A C6A 1.386(5) . ? C6A C61A 1.492(5) . ? C61A N62A 1.483(4) . ? N62A C67A 1.460(5) . ? N62A C63A 1.462(5) . ? C63A C64A 1.511(5) . ? C64A O65A 1.424(5) . ? O65A C66A 1.424(5) . ? C66A C67A 1.503(5) . ? O1B C1B 1.306(4) . ? C1B C2B 1.406(5) . ? C1B C6B 1.423(5) . ? C2B C3B 1.419(5) . ? C2B C21B 1.424(5) . ? C21B N2B 1.286(4) . ? N2B C22B 1.462(5) . ? C3B C4B 1.378(5) . ? C4B C5B 1.413(5) . ? C4B C41B 1.540(5) . ? C41B C47B 1.522(6) . ? C41B C43B 1.528(6) . ? C41B C42B 1.531(6) . ? C41B C45B 1.547(6) . ? C41B C46B 1.551(6) . ? C41B C44B 1.552(6) . ? C5B C6B 1.371(5) . ? C6B C61B 1.492(5) . ? C61B N62B 1.481(4) . ? N62B C67B 1.449(5) . ? N62B C63B 1.467(5) . ? C63B C64B 1.512(6) . ? C64B O65B 1.414(7) . ? O65B C66B 1.395(7) . ? C66B C67B 1.537(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 N2A Ni1 N2B 86.22(14) . . ? N2A Ni1 O1B 175.75(12) . . ? N2B Ni1 O1B 94.42(13) . . ? N2A Ni1 O1A 94.77(13) . . ? N2B Ni1 O1A 175.46(12) . . ? O1B Ni1 O1A 84.92(11) . . ? O1A C1A C2A 124.0(4) . . ? O1A C1A C6A 118.1(4) . . ? C2A C1A C6A 117.9(4) . . ? C1A O1A Ni1 127.3(3) . . ? C1A C2A C3A 120.1(4) . . ? C1A C2A C21A 121.7(4) . . ? C3A C2A C21A 118.2(4) . . ? N2A C21A C2A 124.7(4) . . ? C21A N2A C22A 117.1(3) . . ? C21A N2A Ni1 127.4(3) . . ? C22A N2A Ni1 115.1(3) . . ? N2A C22A C22B 110.8(4) . . ? C4A C3A C2A 123.3(4) . . ? C3A C4A C5A 115.8(4) . . ? C3A C4A C41A 125.4(4) . . ? C5A C4A C41A 118.8(4) . . ? C4A C41A C43A 110.4(3) . . ? C4A C41A C42A 111.1(4) . . ? C43A C41A C42A 108.3(3) . . ? C4A C41A C44A 109.7(3) . . ? C43A C41A C44A 108.7(4) . . ? C42A C41A C44A 108.6(4) . . ? C6A C5A C4A 124.3(4) . . ? C5A C6A C1A 118.5(4) . . ? C5A C6A C61A 121.5(4) . . ? C1A C6A C61A 119.9(3) . . ? N62A C61A C6A 114.8(3) . . ? C67A N62A C63A 109.3(3) . . ? C67A N62A C61A 112.4(3) . . ? C63A N62A C61A 108.9(3) . . ? N62A C63A C64A 111.4(4) . . ? O65A C64A C63A 110.4(4) . . ? C64A O65A C66A 108.7(3) . . ? O65A C66A C67A 112.2(4) . . ? N62A C67A C66A 111.2(3) . . ? C1B O1B Ni1 127.6(3) . . ? O1B C1B C2B 123.9(4) . . ? O1B C1B C6B 118.4(4) . . ? C2B C1B C6B 117.7(4) . . ? C1B C2B C3B 119.8(4) . . ? C1B C2B C21B 120.8(4) . . ? C3B C2B C21B 119.4(4) . . ? N2B C21B C2B 125.9(4) . . ? C21B N2B C22B 116.8(3) . . ? C21B N2B Ni1 126.4(3) . . ? C22B N2B Ni1 116.6(2) . . ? N2B C22B C22A 109.6(3) . . ? C4B C3B C2B 122.5(4) . . ? C3B C4B C5B 116.3(4) . . ? C3B C4B C41B 124.3(4) . . ? C5B C4B C41B 119.4(4) . . ? C47B C41B C43B 94.5(6) . . ? C47B C41B C42B 116.6(7) . . ? C43B C41B C42B 108.7(6) . . ? C47B C41B C4B 113.1(6) . . ? C43B C41B C4B 109.0(5) . . ? C42B C41B C4B 113.0(5) . . ? C47B C41B C45B 106.9(6) . . ? C43B C41B C45B 121.4(7) . . ? C42B C41B C45B 14.2(6) . . ? C4B C41B C45B 110.9(5) . . ? C47B C41B C46B 110.6(6) . . ? C43B C41B C46B 17.3(6) . . ? C42B C41B C46B 94.9(6) . . ? C4B C41B C46B 106.7(5) . . ? C45B C41B C46B 108.6(6) . . ? C47B C41B C44B 13.8(7) . . ? C43B C41B C44B 108.3(6) . . ? C42B C41B C44B 110.3(6) . . ? C4B C41B C44B 107.3(5) . . ? C45B C41B C44B 98.6(6) . . ? C46B C41B C44B 124.2(7) . . ? C6B C5B C4B 123.2(4) . . ? C5B C6B C1B 120.1(4) . . ? C5B C6B C61B 120.8(4) . . ? C1B C6B C61B 119.1(4) . . ? N62B C61B C6B 111.8(3) . . ? C67B N62B C63B 110.5(4) . . ? C67B N62B C61B 109.3(3) . . ? C63B N62B C61B 110.5(3) . . ? N62B C63B C64B 109.8(4) . . ? O65B C64B C63B 112.7(5) . . ? C66B O65B C64B 107.2(5) . . ? O65B C66B C67B 111.0(5) . . ? N62B C67B C66B 110.3(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.494 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.079 data_ninlio _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [NiL].3.75MeOH _chemical_formula_sum 'C37.75 H65 N4 Ni O11.75 S' _chemical_formula_weight 847.70 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' 'S' 'S' 0.1246 0.1234 '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 P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 18.9754(4) _cell_length_b 12.8666(3) _cell_length_c 19.7197(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.5710(10) _cell_angle_gamma 90.00 _cell_volume 4228.25(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1818 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type sortav _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'EPSRC Nonius Kappa CCD' _diffrn_measurement_method 'Phi + omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8643 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.38 _reflns_number_total 8643 _reflns_number_gt 6055 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR92 _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. Solvent treated by van der Sluis + spek method (270.1 e/cell). ; _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^)+(0.0815P)^2^+0.5276P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric (NH visible in diff. map)' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8643 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0736 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.697430(19) 0.00406(2) 0.096164(18) 0.02143(12) Uani 1 1 d . . . O1A O 0.62144(10) 0.10842(14) 0.06605(10) 0.0254(4) Uani 1 1 d . . . C1A C 0.56097(15) 0.1126(2) 0.08169(15) 0.0235(6) Uani 1 1 d . . . C2A C 0.53301(16) 0.0259(2) 0.10633(16) 0.0259(6) Uani 1 1 d . . . C21A C 0.56831(16) -0.0750(2) 0.11355(15) 0.0262(6) Uani 1 1 d . . . H21A H 0.5425 -0.1327 0.1224 0.031 Uiso 1 1 calc R . . N2A N 0.63266(13) -0.09232(16) 0.10887(12) 0.0236(5) Uani 1 1 d . . . C22A C 0.66102(16) -0.2002(2) 0.11387(16) 0.0271(6) Uani 1 1 d . . . H22A H 0.6425 -0.2294 0.0616 0.033 Uiso 1 1 calc R . . H22B H 0.6405 -0.2445 0.1417 0.033 Uiso 1 1 calc R . . C3A C 0.46835(16) 0.0367(2) 0.12243(15) 0.0264(6) Uani 1 1 d . . . H3A H 0.4501 -0.0229 0.1379 0.032 Uiso 1 1 calc R . . C4A C 0.43077(15) 0.1306(2) 0.11644(14) 0.0241(6) Uani 1 1 d . . . C41A C 0.36098(16) 0.1459(2) 0.13404(15) 0.0285(6) Uani 1 1 d . . . C42A C 0.33910(19) 0.0450(2) 0.1595(2) 0.0409(8) Uani 1 1 d . . . H42A H 0.2945 0.0575 0.1703 0.061 Uiso 1 1 calc R . . H42B H 0.3856 0.0194 0.2063 0.061 Uiso 1 1 calc R . . H42C H 0.3231 -0.0068 0.1184 0.061 Uiso 1 1 calc R . . C43A C 0.28740(17) 0.1858(3) 0.06121(16) 0.0380(7) Uani 1 1 d . . . H43A H 0.2428 0.1962 0.0723 0.057 Uiso 1 1 calc R . . H43B H 0.2719 0.1347 0.0196 0.057 Uiso 1 1 calc R . . H43C H 0.3005 0.2519 0.0452 0.057 Uiso 1 1 calc R . . C44A C 0.38372(17) 0.2265(2) 0.19857(16) 0.0313(6) Uani 1 1 d . . . H44A H 0.3387 0.2360 0.2091 0.047 Uiso 1 1 calc R . . H44B H 0.3963 0.2928 0.1824 0.047 Uiso 1 1 calc R . . H44C H 0.4307 0.2020 0.2454 0.047 Uiso 1 1 calc R . . C5A C 0.45780(15) 0.2155(2) 0.09016(15) 0.0256(6) Uani 1 1 d . . . H5A H 0.4320 0.2808 0.0842 0.031 Uiso 1 1 calc R . . C6A C 0.52028(15) 0.2087(2) 0.07257(14) 0.0236(5) Uani 1 1 d . . . C61A C 0.54002(15) 0.2995(2) 0.03696(15) 0.0259(6) Uani 1 1 d . . . H61A H 0.4909 0.3417 0.0084 0.031 Uiso 1 1 calc R . . H61B H 0.5556 0.2727 -0.0011 0.031 Uiso 1 1 calc R . . N62A N 0.60638(12) 0.36958(16) 0.09315(12) 0.0247(5) Uani 1 1 d . . . H62A H 0.6170 0.4173 0.0638 0.030 Uiso 1 1 calc R . . C63A C 0.58213(17) 0.4307(2) 0.14305(18) 0.0365(7) Uani 1 1 d . . . H63A H 0.5696 0.3831 0.1753 0.044 Uiso 1 1 calc R . . H63B H 0.5335 0.4721 0.1104 0.044 Uiso 1 1 calc R . . C64A C 0.6507(2) 0.5027(2) 0.1944(2) 0.0461(8) Uani 1 1 d . . . H64A H 0.6601 0.5534 0.1619 0.055 Uiso 1 1 calc R . . H64B H 0.6357 0.5418 0.2288 0.055 Uiso 1 1 calc R . . O65A O 0.72243(12) 0.44594(17) 0.23988(11) 0.0402(5) Uani 1 1 d . . . C66A C 0.74685(17) 0.3910(2) 0.19145(17) 0.0340(7) Uani 1 1 d . . . H66A H 0.7979 0.3541 0.2237 0.041 Uiso 1 1 calc R . . H66B H 0.7557 0.4408 0.1580 0.041 Uiso 1 1 calc R . . C67A C 0.68274(16) 0.3137(2) 0.14205(15) 0.0281(6) Uani 1 1 d . . . H67A H 0.6998 0.2752 0.1089 0.034 Uiso 1 1 calc R . . H67B H 0.6747 0.2629 0.1754 0.034 Uiso 1 1 calc R . . O1B O 0.76114(10) 0.10088(14) 0.08130(10) 0.0245(4) Uani 1 1 d . . . C1B C 0.83549(15) 0.0893(2) 0.09376(14) 0.0230(5) Uani 1 1 d . . . C2B C 0.87980(16) -0.0038(2) 0.12123(15) 0.0244(6) Uani 1 1 d . . . C21B C 0.84610(16) -0.0940(2) 0.13843(15) 0.0266(6) Uani 1 1 d . . . H21B H 0.8788 -0.1543 0.1563 0.032 Uiso 1 1 calc R . . N2B N 0.77524(13) -0.09934(17) 0.13142(12) 0.0250(5) Uani 1 1 d . . . C22B C 0.75160(16) -0.1951(2) 0.15755(16) 0.0285(6) Uani 1 1 d . . . H22C H 0.7707 -0.1922 0.2138 0.034 Uiso 1 1 calc R . . H22D H 0.7751 -0.2572 0.1463 0.034 Uiso 1 1 calc R . . C3B C 0.95967(16) -0.0106(2) 0.13418(15) 0.0251(6) Uani 1 1 d . . . H3B H 0.9876 -0.0746 0.1519 0.030 Uiso 1 1 calc R . . C4B C 0.99839(15) 0.0719(2) 0.12205(14) 0.0243(6) Uani 1 1 d . . . C41B C 1.08499(16) 0.0671(2) 0.13574(16) 0.0301(6) Uani 1 1 d . . . C42B C 1.11947(19) -0.0420(3) 0.1567(2) 0.0437(8) Uani 1 1 d . . . H42D H 1.0862 -0.0901 0.1150 0.066 Uiso 1 1 calc R . . H42E H 1.1201 -0.0640 0.2046 0.066 Uiso 1 1 calc R . . H42F H 1.1743 -0.0424 0.1640 0.066 Uiso 1 1 calc R . . C43B C 1.08827(18) 0.1014(3) 0.06272(17) 0.0393(7) Uani 1 1 d . . . H43D H 1.0550 0.0548 0.0199 0.059 Uiso 1 1 calc R . . H43E H 1.1439 0.0986 0.0722 0.059 Uiso 1 1 calc R . . H43F H 1.0681 0.1727 0.0494 0.059 Uiso 1 1 calc R . . C44B C 1.13659(18) 0.1409(3) 0.20219(18) 0.0457(8) Uani 1 1 d . . . H44D H 1.1144 0.2113 0.1895 0.069 Uiso 1 1 calc R . . H44E H 1.1916 0.1410 0.2101 0.069 Uiso 1 1 calc R . . H44F H 1.1367 0.1174 0.2495 0.069 Uiso 1 1 calc R . . C5B C 0.95390(15) 0.1648(2) 0.09589(14) 0.0260(6) Uani 1 1 d . . . H5B H 0.9792 0.2236 0.0877 0.031 Uiso 1 1 calc R . . C6B C 0.87562(16) 0.1745(2) 0.08153(14) 0.0239(6) Uani 1 1 d . . . C61B C 0.83292(15) 0.2773(2) 0.05703(14) 0.0242(6) Uani 1 1 d . . . H61C H 0.8728 0.3335 0.0817 0.029 Uiso 1 1 calc R . . H61D H 0.7939 0.2820 0.0768 0.029 Uiso 1 1 calc R . . N62B N 0.78886(13) 0.29632(16) -0.02903(12) 0.0253(5) Uani 1 1 d . . . H62B H 0.7589 0.3566 -0.0369 0.030 Uiso 1 1 calc R . . C63B C 0.73083(18) 0.2118(2) -0.07391(16) 0.0344(7) Uani 1 1 d . . . H63C H 0.6923 0.2011 -0.0540 0.041 Uiso 1 1 calc R . . H63D H 0.7601 0.1459 -0.0681 0.041 Uiso 1 1 calc R . . C64B C 0.6864(2) 0.2425(3) -0.15786(17) 0.0429(8) Uani 1 1 d . . . H64C H 0.6474 0.1874 -0.1878 0.052 Uiso 1 1 calc R . . H64D H 0.6561 0.3075 -0.1634 0.052 Uiso 1 1 calc R . . O65B O 0.73986(14) 0.25768(17) -0.18777(12) 0.0447(6) Uani 1 1 d . . . C66B C 0.7940(2) 0.3401(3) -0.14775(19) 0.0557(10) Uani 1 1 d . . . H66C H 0.7634 0.4050 -0.1543 0.067 Uiso 1 1 calc R . . H66D H 0.8304 0.3512 -0.1700 0.067 Uiso 1 1 calc R . . C67B C 0.8432(2) 0.3153(3) -0.06235(18) 0.0430(8) Uani 1 1 d . . . H67C H 0.8765 0.2529 -0.0554 0.052 Uiso 1 1 calc R . . H67D H 0.8794 0.3741 -0.0353 0.052 Uiso 1 1 calc R . . S1 S 0.65814(4) 0.49916(5) -0.03783(4) 0.03034(18) Uani 1 1 d . . . O1 O 0.6361(2) 0.5421(2) 0.01808(15) 0.0782(9) Uani 1 1 d . . . O2 O 0.74306(14) 0.5095(2) -0.01666(18) 0.0742(9) Uani 1 1 d . . . O3 O 0.64395(14) 0.38659(17) -0.03756(14) 0.0500(6) Uani 1 1 d . . . O4 O 0.60837(12) 0.54469(16) -0.11327(11) 0.0387(5) 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 Ni1 0.01938(19) 0.0225(2) 0.0252(2) 0.00185(13) 0.01300(15) 0.00049(13) O1A 0.0213(9) 0.0263(10) 0.0340(10) 0.0022(8) 0.0176(8) 0.0020(8) C1A 0.0186(13) 0.0281(14) 0.0261(14) -0.0043(11) 0.0125(11) -0.0033(11) C2A 0.0225(14) 0.0263(14) 0.0322(15) -0.0033(11) 0.0157(12) -0.0034(11) C21A 0.0248(14) 0.0264(14) 0.0313(15) 0.0000(11) 0.0166(12) -0.0062(11) N2A 0.0243(12) 0.0209(11) 0.0273(12) -0.0006(9) 0.0136(10) -0.0001(9) C22A 0.0269(15) 0.0215(14) 0.0365(15) 0.0002(11) 0.0180(12) -0.0015(11) C3A 0.0226(14) 0.0277(14) 0.0319(15) -0.0040(11) 0.0154(12) -0.0045(11) C4A 0.0195(13) 0.0308(15) 0.0242(13) -0.0054(11) 0.0122(11) -0.0044(11) C41A 0.0229(14) 0.0344(16) 0.0327(15) -0.0021(12) 0.0169(12) -0.0014(12) C42A 0.0373(18) 0.0350(17) 0.067(2) -0.0043(15) 0.0383(17) -0.0055(14) C43A 0.0234(15) 0.058(2) 0.0331(16) -0.0084(14) 0.0142(13) -0.0020(14) C44A 0.0270(15) 0.0412(17) 0.0304(15) 0.0003(12) 0.0176(13) 0.0041(13) C5A 0.0206(13) 0.0283(14) 0.0272(14) -0.0021(11) 0.0109(11) 0.0009(11) C6A 0.0188(13) 0.0291(14) 0.0234(13) -0.0027(10) 0.0106(11) -0.0031(11) C61A 0.0200(13) 0.0326(15) 0.0253(14) 0.0009(11) 0.0111(11) 0.0001(11) N62A 0.0226(12) 0.0255(12) 0.0304(12) 0.0049(9) 0.0161(10) 0.0003(9) C63A 0.0279(16) 0.0317(16) 0.0512(19) -0.0115(13) 0.0199(14) 0.0015(13) C64A 0.0348(18) 0.0354(18) 0.066(2) -0.0183(16) 0.0227(17) -0.0035(14) O65A 0.0335(12) 0.0494(14) 0.0367(12) -0.0143(10) 0.0159(10) -0.0019(10) C66A 0.0246(15) 0.0365(16) 0.0402(17) -0.0072(13) 0.0149(13) 0.0019(12) C67A 0.0218(14) 0.0325(15) 0.0300(14) -0.0030(11) 0.0124(12) 0.0037(11) O1B 0.0204(9) 0.0256(10) 0.0324(10) 0.0069(8) 0.0165(8) 0.0038(7) C1B 0.0216(13) 0.0283(14) 0.0227(13) 0.0008(10) 0.0136(11) 0.0015(11) C2B 0.0226(13) 0.0285(14) 0.0243(13) 0.0020(11) 0.0130(11) -0.0002(11) C21B 0.0232(14) 0.0269(14) 0.0297(14) 0.0031(11) 0.0127(12) 0.0048(11) N2B 0.0239(12) 0.0255(12) 0.0268(12) 0.0029(9) 0.0130(10) -0.0002(9) C22B 0.0264(15) 0.0271(15) 0.0316(15) 0.0087(11) 0.0136(12) -0.0007(11) C3B 0.0201(13) 0.0312(15) 0.0247(14) 0.0047(11) 0.0113(11) 0.0041(11) C4B 0.0181(13) 0.0323(15) 0.0215(13) -0.0006(11) 0.0088(11) -0.0002(11) C41B 0.0215(14) 0.0395(17) 0.0318(15) 0.0034(12) 0.0148(12) 0.0024(12) C42B 0.0285(16) 0.0464(19) 0.062(2) 0.0122(16) 0.0266(16) 0.0129(15) C43B 0.0263(15) 0.058(2) 0.0401(17) 0.0041(15) 0.0212(14) -0.0022(14) C44B 0.0256(16) 0.066(2) 0.0415(18) -0.0131(16) 0.0130(14) -0.0023(15) C5B 0.0222(14) 0.0304(15) 0.0262(14) -0.0001(11) 0.0123(11) -0.0031(11) C6B 0.0248(14) 0.0254(14) 0.0238(13) 0.0004(10) 0.0135(11) 0.0031(11) C61B 0.0212(13) 0.0246(14) 0.0276(14) -0.0022(11) 0.0124(11) -0.0028(11) N62B 0.0285(12) 0.0206(11) 0.0289(12) 0.0028(9) 0.0154(10) 0.0039(9) C63B 0.0334(16) 0.0335(16) 0.0320(15) 0.0000(12) 0.0121(13) -0.0077(13) C64B 0.049(2) 0.0423(19) 0.0321(17) -0.0016(13) 0.0153(15) -0.0016(15) O65B 0.0627(15) 0.0415(13) 0.0315(11) -0.0020(9) 0.0237(11) 0.0055(11) C66B 0.070(3) 0.065(2) 0.0391(19) 0.0068(17) 0.0323(19) -0.008(2) C67B 0.0438(19) 0.050(2) 0.0465(19) 0.0056(15) 0.0306(16) -0.0081(15) S1 0.0272(4) 0.0307(4) 0.0348(4) 0.0068(3) 0.0162(3) 0.0061(3) O1 0.120(3) 0.0662(18) 0.0539(16) 0.0090(14) 0.0457(17) 0.0442(19) O2 0.0226(12) 0.084(2) 0.099(2) 0.0477(16) 0.0162(13) -0.0037(12) O3 0.0496(14) 0.0384(13) 0.0611(15) 0.0206(11) 0.0258(12) 0.0019(11) O4 0.0348(12) 0.0372(12) 0.0391(12) 0.0100(9) 0.0135(10) 0.0020(10) _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 N2A 1.846(2) . ? Ni1 O1A 1.8482(17) . ? Ni1 O1B 1.8542(17) . ? Ni1 N2B 1.858(2) . ? O1A C1A 1.324(3) . ? C1A C2A 1.417(4) . ? C1A C6A 1.423(4) . ? C2A C3A 1.414(3) . ? C2A C21A 1.436(4) . ? C21A N2A 1.287(3) . ? N2A C22A 1.475(3) . ? C22A C22B 1.511(4) . ? C3A C4A 1.379(4) . ? C4A C5A 1.408(4) . ? C4A C41A 1.534(3) . ? C41A C42A 1.520(4) . ? C41A C44A 1.534(4) . ? C41A C43A 1.535(4) . ? C5A C6A 1.388(3) . ? C6A C61A 1.499(4) . ? C61A N62A 1.514(3) . ? N62A C67A 1.487(3) . ? N62A C63A 1.494(3) . ? C63A C64A 1.521(4) . ? C64A O65A 1.422(4) . ? O65A C66A 1.431(3) . ? C66A C67A 1.512(4) . ? O1B C1B 1.320(3) . ? C1B C2B 1.414(4) . ? C1B C6B 1.420(4) . ? C2B C3B 1.414(4) . ? C2B C21B 1.442(4) . ? C21B N2B 1.286(3) . ? N2B C22B 1.485(3) . ? C3B C4B 1.376(4) . ? C4B C5B 1.411(4) . ? C4B C41B 1.534(4) . ? C41B C42B 1.521(4) . ? C41B C44B 1.533(4) . ? C41B C43B 1.536(4) . ? C5B C6B 1.378(4) . ? C6B C61B 1.505(4) . ? C61B N62B 1.510(3) . ? N62B C67B 1.484(3) . ? N62B C63B 1.499(4) . ? C63B C64B 1.508(4) . ? C64B O65B 1.410(4) . ? O65B C66B 1.424(4) . ? C66B C67B 1.518(5) . ? S1 O4 1.451(2) . ? S1 O1 1.462(3) . ? S1 O2 1.465(2) . ? S1 O3 1.474(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2A Ni1 O1A 93.67(8) . . ? N2A Ni1 O1B 178.86(9) . . ? O1A Ni1 O1B 85.90(7) . . ? N2A Ni1 N2B 85.97(9) . . ? O1A Ni1 N2B 177.20(8) . . ? O1B Ni1 N2B 94.51(8) . . ? C1A O1A Ni1 125.75(16) . . ? O1A C1A C2A 123.8(2) . . ? O1A C1A C6A 118.9(2) . . ? C2A C1A C6A 117.3(2) . . ? C3A C2A C1A 120.5(2) . . ? C3A C2A C21A 118.7(2) . . ? C1A C2A C21A 120.8(2) . . ? N2A C21A C2A 124.3(2) . . ? C21A N2A C22A 119.1(2) . . ? C21A N2A Ni1 127.55(18) . . ? C22A N2A Ni1 113.33(16) . . ? N2A C22A C22B 106.0(2) . . ? C4A C3A C2A 122.4(2) . . ? C3A C4A C5A 116.6(2) . . ? C3A C4A C41A 124.1(2) . . ? C5A C4A C41A 119.3(2) . . ? C42A C41A C4A 111.5(2) . . ? C42A C41A C44A 108.4(2) . . ? C4A C41A C44A 110.1(2) . . ? C42A C41A C43A 108.9(2) . . ? C4A C41A C43A 109.2(2) . . ? C44A C41A C43A 108.6(2) . . ? C6A C5A C4A 123.2(2) . . ? C5A C6A C1A 120.0(2) . . ? C5A C6A C61A 120.2(2) . . ? C1A C6A C61A 119.6(2) . . ? C6A C61A N62A 115.3(2) . . ? C67A N62A C63A 109.8(2) . . ? C67A N62A C61A 113.4(2) . . ? C63A N62A C61A 112.7(2) . . ? N62A C63A C64A 108.9(2) . . ? O65A C64A C63A 111.3(2) . . ? C64A O65A C66A 110.5(2) . . ? O65A C66A C67A 109.7(2) . . ? N62A C67A C66A 109.5(2) . . ? C1B O1B Ni1 127.92(16) . . ? O1B C1B C2B 123.6(2) . . ? O1B C1B C6B 119.6(2) . . ? C2B C1B C6B 116.8(2) . . ? C3B C2B C1B 120.8(2) . . ? C3B C2B C21B 117.7(2) . . ? C1B C2B C21B 121.5(2) . . ? N2B C21B C2B 125.2(2) . . ? C21B N2B C22B 118.7(2) . . ? C21B N2B Ni1 127.23(19) . . ? C22B N2B Ni1 113.95(16) . . ? N2B C22B C22A 106.8(2) . . ? C4B C3B C2B 122.4(2) . . ? C3B C4B C5B 116.2(2) . . ? C3B C4B C41B 123.7(2) . . ? C5B C4B C41B 120.1(2) . . ? C42B C41B C44B 108.9(3) . . ? C42B C41B C4B 111.7(2) . . ? C44B C41B C4B 108.6(2) . . ? C42B C41B C43B 108.4(2) . . ? C44B C41B C43B 109.2(2) . . ? C4B C41B C43B 110.1(2) . . ? C6B C5B C4B 123.4(2) . . ? C5B C6B C1B 120.5(2) . . ? C5B C6B C61B 120.5(2) . . ? C1B C6B C61B 118.9(2) . . ? C6B C61B N62B 115.3(2) . . ? C67B N62B C63B 109.1(2) . . ? C67B N62B C61B 113.3(2) . . ? C63B N62B C61B 113.7(2) . . ? N62B C63B C64B 109.0(2) . . ? O65B C64B C63B 111.0(3) . . ? C64B O65B C66B 110.1(2) . . ? O65B C66B C67B 110.8(3) . . ? N62B C67B C66B 109.7(3) . . ? O4 S1 O1 109.86(14) . . ? O4 S1 O2 110.08(14) . . ? O1 S1 O2 115.1(2) . . ? O4 S1 O3 111.72(13) . . ? O1 S1 O3 104.48(16) . . ? O2 S1 O3 105.47(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.234 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.074