# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1883 data_xr93 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C69 H76 K N2 Ni2 O9 P3 Pb0' _chemical_formula_weight 1326.75 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'K' 'K' 0.2009 0.2494 '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2760(10) _cell_length_b 25.750(2) _cell_length_c 19.392(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.46 _cell_angle_gamma 90.00 _cell_volume 6627.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method ? _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10369 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8561 _reflns_number_observed 6092 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+14.5582P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8561 _refine_ls_number_parameters 679 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_obs 0.0526 _refine_ls_wR_factor_all 0.1352 _refine_ls_wR_factor_obs 0.1167 _refine_ls_goodness_of_fit_all 1.004 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 1.004 _refine_ls_restrained_S_obs 1.043 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.11407(5) 0.24116(2) 0.50329(3) 0.0263(2) Uani 1 d . . Ni2 Ni 0.18556(5) 0.21188(2) 0.39219(3) 0.0275(2) Uani 1 d . . K1 K -0.32311(9) 0.50255(5) 0.24013(6) 0.0380(3) Uani 1 d . . P1 P -0.03622(10) 0.27544(5) 0.50652(7) 0.0283(3) Uani 1 d . . P2 P 0.30106(10) 0.15230(5) 0.39102(7) 0.0307(3) Uani 1 d . . P3 P 0.24001(10) 0.28135(5) 0.45072(7) 0.0273(3) Uani 1 d . . O1 O 0.1533(3) 0.2130(2) 0.6460(2) 0.0580(12) Uani 1 d . . O2 O 0.0941(4) 0.2208(2) 0.2554(2) 0.0667(14) Uani 1 d . . O3 O 0.0406(3) 0.1414(2) 0.4507(2) 0.0473(10) Uani 1 d . . O4 O -0.1794(4) 0.4491(2) 0.3235(2) 0.0637(13) Uani 1 d . . O5 O -0.1198(3) 0.5023(2) 0.2096(3) 0.097(2) Uani 1 d . . O6 O -0.4034(4) 0.5648(2) 0.3447(3) 0.083(2) Uani 1 d . . O7 O -0.3574(5) 0.6075(2) 0.2205(3) 0.102(2) Uani 1 d . . O8 O -0.4757(4) 0.4235(2) 0.2390(3) 0.081(2) Uani 1 d . . O9 O -0.3820(4) 0.4554(2) 0.1183(3) 0.083(2) Uani 1 d . . N1 N -0.3852(4) 0.4549(2) 0.3714(3) 0.0585(15) Uani 1 d . . N2 N -0.2603(4) 0.5487(2) 0.1101(3) 0.0570(15) Uani 1 d . . C1 C -0.0512(3) 0.34339(11) 0.5342(2) 0.0356(13) Uani 1 d G . C2 C 0.0350(2) 0.37402(15) 0.5352(2) 0.056(2) Uani 1 d G . H2 H 0.0970(3) 0.3594(2) 0.5253(3) 0.067 Uiso 1 calc R . C3 C 0.0286(3) 0.42654(14) 0.5510(2) 0.077(2) Uani 1 d G . H3 H 0.0863(4) 0.4470(2) 0.5517(3) 0.093 Uiso 1 calc R . C4 C -0.0641(4) 0.44843(11) 0.5658(2) 0.068(2) Uani 1 d G . H4 H -0.0684(5) 0.48357(12) 0.5765(3) 0.082 Uiso 1 calc R . C5 C -0.1503(3) 0.4178(2) 0.5648(2) 0.061(2) Uani 1 d G . H5 H -0.2123(3) 0.4325(2) 0.5747(3) 0.073 Uiso 1 calc R . C6 C -0.1439(2) 0.36529(15) 0.5490(2) 0.051(2) Uani 1 d G . H6 H -0.2016(3) 0.3448(2) 0.5483(3) 0.061 Uiso 1 calc R . C7 C -0.1155(2) 0.27705(15) 0.42732(14) 0.0324(13) Uani 1 d G . C8 C -0.2180(2) 0.2661(2) 0.4256(2) 0.045(2) Uani 1 d G . H8 H -0.2501(3) 0.2569(2) 0.4659(2) 0.054 Uiso 1 calc R . C9 C -0.2727(2) 0.2688(2) 0.3636(2) 0.058(2) Uani 1 d G . H9 H -0.3413(2) 0.2614(2) 0.3624(3) 0.069 Uiso 1 calc R . C10 C -0.2248(3) 0.2825(2) 0.3033(2) 0.069(2) Uani 1 d G . H10 H -0.2614(4) 0.2843(3) 0.2619(2) 0.083 Uiso 1 calc R . C11 C -0.1223(3) 0.2935(2) 0.30507(14) 0.065(2) Uani 1 d G . H11 H -0.0902(4) 0.3026(3) 0.2647(2) 0.078 Uiso 1 calc R . C12 C -0.0676(2) 0.2908(2) 0.3671(2) 0.050(2) Uani 1 d G . H12 H 0.0010(2) 0.2981(2) 0.3682(3) 0.061 Uiso 1 calc R . C13 C -0.1157(2) 0.23858(12) 0.56623(15) 0.0300(12) Uani 1 d G . C14 C -0.1449(3) 0.25784(11) 0.6296(2) 0.045(2) Uani 1 d G . H14 H -0.1285(4) 0.29167(13) 0.6424(2) 0.055 Uiso 1 calc R . C15 C -0.1987(3) 0.2265(2) 0.67402(14) 0.056(2) Uani 1 d G . H15 H -0.2182(4) 0.2394(2) 0.7164(2) 0.067 Uiso 1 calc R . C16 C -0.2232(3) 0.17595(15) 0.6550(2) 0.056(2) Uani 1 d G . H16 H -0.2592(4) 0.1550(2) 0.6847(2) 0.067 Uiso 1 calc R . C17 C -0.1940(3) 0.15669(11) 0.5916(2) 0.048(2) Uani 1 d G . H17 H -0.2105(4) 0.12286(12) 0.5789(3) 0.057 Uiso 1 calc R . C18 C -0.1403(3) 0.18801(13) 0.54721(14) 0.0391(14) Uani 1 d G . H18 H -0.1207(4) 0.1751(2) 0.5048(2) 0.047 Uiso 1 calc R . C19 C 0.3768(2) 0.14251(14) 0.47074(14) 0.0339(13) Uani 1 d G . C20 C 0.4808(2) 0.14865(15) 0.4748(2) 0.0431(15) Uani 1 d G . H20 H 0.5160(3) 0.1570(2) 0.4354(2) 0.052 Uiso 1 calc R . C21 C 0.5321(2) 0.1423(2) 0.5376(2) 0.056(2) Uani 1 d G . H21 H 0.6017(2) 0.1464(2) 0.5403(3) 0.067 Uiso 1 calc R . C22 C 0.4794(3) 0.1299(2) 0.5964(2) 0.056(2) Uani 1 d G . H22 H 0.5137(4) 0.1256(2) 0.6384(2) 0.068 Uiso 1 calc R . C23 C 0.3754(3) 0.1237(2) 0.59233(14) 0.054(2) Uani 1 d G . H23 H 0.3402(4) 0.1154(2) 0.6317(2) 0.065 Uiso 1 calc R . C24 C 0.3241(2) 0.13005(15) 0.5295(2) 0.0432(15) Uani 1 d G . H24 H 0.2545(2) 0.1259(2) 0.5268(3) 0.052 Uiso 1 calc R . C25 C 0.3966(2) 0.16216(13) 0.3245(2) 0.0340(13) Uani 1 d G . C26 C 0.4298(3) 0.12251(11) 0.2820(2) 0.054(2) Uani 1 d G . H26 H 0.4029(4) 0.08933(12) 0.2858(3) 0.064 Uiso 1 calc R . C27 C 0.5033(3) 0.13246(15) 0.2340(2) 0.068(2) Uani 1 d G . H27 H 0.5255(5) 0.1059(2) 0.2056(3) 0.081 Uiso 1 calc R . C28 C 0.5436(3) 0.1821(2) 0.2284(2) 0.056(2) Uani 1 d G . H28 H 0.5928(4) 0.1887(2) 0.1962(2) 0.067 Uiso 1 calc R . C29 C 0.5104(3) 0.22170(13) 0.2708(2) 0.053(2) Uani 1 d G . H29 H 0.5374(4) 0.25489(15) 0.2671(3) 0.064 Uiso 1 calc R . C30 C 0.4369(3) 0.21175(12) 0.3189(2) 0.0447(15) Uani 1 d G . H30 H 0.4147(4) 0.23828(15) 0.3472(2) 0.054 Uiso 1 calc R . C31 C 0.2592(3) 0.08511(10) 0.3725(2) 0.0368(14) Uani 1 d G . C32 C 0.3152(2) 0.04196(14) 0.3932(2) 0.0429(15) Uani 1 d G . H32 H 0.3726(3) 0.0461(2) 0.4210(3) 0.052 Uiso 1 calc R . C33 C 0.2852(3) -0.00742(11) 0.3722(2) 0.053(2) Uani 1 d G . H33 H 0.3227(4) -0.03629(14) 0.3860(3) 0.063 Uiso 1 calc R . C34 C 0.1993(3) -0.01366(12) 0.3305(2) 0.062(2) Uani 1 d G . H34 H 0.1793(5) -0.04670(13) 0.3165(3) 0.074 Uiso 1 calc R . C35 C 0.1434(3) 0.0295(2) 0.3098(2) 0.068(2) Uani 1 d G . H35 H 0.0859(3) 0.0253(2) 0.2820(3) 0.081 Uiso 1 calc R . C36 C 0.1733(3) 0.07886(13) 0.3308(2) 0.055(2) Uani 1 d G . H36 H 0.1358(4) 0.1077(2) 0.3170(3) 0.066 Uiso 1 calc R . C37 C 0.2332(3) 0.34665(9) 0.4104(2) 0.0272(12) Uani 1 d G . C38 C 0.2639(3) 0.39054(12) 0.44705(13) 0.0344(13) Uani 1 d G . H38 H 0.2907(4) 0.3872(2) 0.49162(15) 0.041 Uiso 1 calc R . C39 C 0.2546(3) 0.43938(10) 0.4170(2) 0.0429(15) Uani 1 d G . H39 H 0.2751(4) 0.46874(12) 0.4415(2) 0.051 Uiso 1 calc R . C40 C 0.2146(3) 0.44433(10) 0.3504(2) 0.045(2) Uani 1 d G . H40 H 0.2084(4) 0.47701(11) 0.3303(2) 0.054 Uiso 1 calc R . C41 C 0.1840(3) 0.40044(13) 0.31380(13) 0.045(2) Uani 1 d G . H41 H 0.1572(4) 0.4038(2) 0.2692(2) 0.054 Uiso 1 calc R . C42 C 0.1933(3) 0.35160(11) 0.3438(2) 0.0352(13) Uani 1 d G . H42 H 0.1727(4) 0.32224(13) 0.3193(2) 0.042 Uiso 1 calc R . C43 C 0.3652(2) 0.28477(13) 0.4959(2) 0.0292(12) Uani 1 d G . C44 C 0.3784(2) 0.26318(13) 0.5612(2) 0.0357(13) Uani 1 d G . H44 H 0.3239(3) 0.2486(2) 0.5833(2) 0.043 Uiso 1 calc R . C45 C 0.4731(3) 0.26342(14) 0.59348(14) 0.0418(14) Uani 1 d G . H45 H 0.4820(4) 0.2490(2) 0.6372(2) 0.050 Uiso 1 calc R . C46 C 0.5546(2) 0.28525(15) 0.5604(2) 0.047(2) Uani 1 d G . H46 H 0.6180(2) 0.2854(2) 0.5820(3) 0.057 Uiso 1 calc R . C47 C 0.5414(2) 0.30684(14) 0.4951(2) 0.048(2) Uani 1 d G . H47 H 0.5959(3) 0.3215(2) 0.4730(3) 0.058 Uiso 1 calc R . C48 C 0.4467(2) 0.30660(14) 0.46288(14) 0.0394(14) Uani 1 d G . H48 H 0.4378(3) 0.3211(2) 0.4192(2) 0.047 Uiso 1 calc R . C49 C 0.1413(4) 0.2223(2) 0.5882(3) 0.0325(13) Uani 1 d . . C50 C 0.1301(4) 0.2190(2) 0.3099(3) 0.0391(14) Uani 1 d . . C51 C 0.0886(4) 0.1794(2) 0.4483(3) 0.0303(12) Uani 1 d . . C52 C -0.3058(7) 0.4220(5) 0.3976(5) 0.143(5) Uani 1 d . . H52A H -0.3113(7) 0.4221(5) 0.4474(5) 0.171 Uiso 1 calc R . H52B H -0.3225(7) 0.3871(5) 0.3825(5) 0.171 Uiso 1 calc R . C53 C -0.2065(6) 0.4287(3) 0.3849(4) 0.089(3) Uani 1 d . . H53A H -0.1783(6) 0.4508(3) 0.4210(4) 0.107 Uiso 1 calc R . H53B H -0.1740(6) 0.3951(3) 0.3897(4) 0.107 Uiso 1 calc R . C54 C -0.0831(6) 0.4563(5) 0.3112(5) 0.126(4) Uani 1 d . . H54A H -0.0488(6) 0.4236(5) 0.3205(5) 0.151 Uiso 1 calc R . H54B H -0.0573(6) 0.4811(5) 0.3448(5) 0.151 Uiso 1 calc R . C55 C -0.0540(5) 0.4730(3) 0.2469(4) 0.065(2) Uani 1 d . . H55A H 0.0078(5) 0.4928(3) 0.2530(4) 0.078 Uiso 1 calc R . H55B H -0.0381(5) 0.4426(3) 0.2197(4) 0.078 Uiso 1 calc R . C56 C -0.0900(5) 0.5185(3) 0.1445(4) 0.064(2) Uani 1 d . . H56A H -0.0811(5) 0.4881(3) 0.1158(4) 0.077 Uiso 1 calc R . H56B H -0.0250(5) 0.5355(3) 0.1495(4) 0.077 Uiso 1 calc R . C57 C -0.1572(8) 0.5526(7) 0.1102(8) 0.265(12) Uani 1 d . . H57A H -0.1413(8) 0.5870(7) 0.1277(8) 0.318 Uiso 1 calc R . H57B H -0.1386(8) 0.5524(7) 0.0622(8) 0.318 Uiso 1 calc R . C58 C -0.4085(13) 0.4929(4) 0.4190(6) 0.220(9) Uani 1 d . . H58A H -0.4609(13) 0.4783(4) 0.4471(6) 0.265 Uiso 1 calc R . H58B H -0.3493(13) 0.4964(4) 0.4491(6) 0.265 Uiso 1 calc R . C59 C -0.4387(8) 0.5425(4) 0.4038(4) 0.107(3) Uani 1 d . . H59A H -0.4189(8) 0.5645(4) 0.4423(4) 0.128 Uiso 1 calc R . H59B H -0.5118(8) 0.5427(4) 0.4006(4) 0.128 Uiso 1 calc R . C60 C -0.4280(11) 0.6136(3) 0.3303(5) 0.160(6) Uani 1 d . . H60A H -0.4142(11) 0.6343(3) 0.3713(5) 0.191 Uiso 1 calc R . H60B H -0.5002(11) 0.6149(3) 0.3213(5) 0.191 Uiso 1 calc R . C61 C -0.3805(7) 0.6377(3) 0.2747(5) 0.091(3) Uani 1 d . . H61A H -0.4239(7) 0.6655(3) 0.2578(5) 0.109 Uiso 1 calc R . H61B H -0.3187(7) 0.6536(3) 0.2922(5) 0.109 Uiso 1 calc R . C62 C -0.3224(6) 0.6312(3) 0.1611(5) 0.084(3) Uani 1 d . . H62A H -0.3735(6) 0.6554(3) 0.1445(5) 0.100 Uiso 1 calc R . H62B H -0.2630(6) 0.6514(3) 0.1737(5) 0.100 Uiso 1 calc R . C63 C -0.2980(14) 0.5984(4) 0.1066(5) 0.214(9) Uani 1 d . . H63A H -0.3590(14) 0.5959(4) 0.0782(5) 0.257 Uiso 1 calc R . H63B H -0.2503(14) 0.6178(4) 0.0796(5) 0.257 Uiso 1 calc R . C64 C -0.4690(10) 0.4261(5) 0.3605(5) 0.180(7) Uani 1 d . . H64A H -0.5242(10) 0.4492(5) 0.3711(5) 0.216 Uiso 1 calc R . H64B H -0.4670(10) 0.4003(5) 0.3968(5) 0.216 Uiso 1 calc R . C65 C -0.5008(7) 0.3999(3) 0.3029(5) 0.093(3) Uani 1 d . . H65A H -0.5735(7) 0.3962(3) 0.3041(5) 0.111 Uiso 1 calc R . H65B H -0.4720(7) 0.3653(3) 0.3045(5) 0.111 Uiso 1 calc R . C66 C -0.4589(6) 0.3907(3) 0.1871(4) 0.088(3) Uani 1 d . . H66A H -0.5118(6) 0.3647(3) 0.1861(4) 0.106 Uiso 1 calc R . H66B H -0.3956(6) 0.3729(3) 0.1965(4) 0.106 Uiso 1 calc R . C67 C -0.4549(5) 0.4147(3) 0.1195(4) 0.071(2) Uani 1 d . . H67A H -0.4381(5) 0.3886(3) 0.0856(4) 0.085 Uiso 1 calc R . H67B H -0.5207(5) 0.4286(3) 0.1069(4) 0.085 Uiso 1 calc R . C68 C -0.3781(6) 0.4826(3) 0.0588(4) 0.073(2) Uani 1 d . . H68A H -0.4416(6) 0.5008(3) 0.0523(4) 0.088 Uiso 1 calc R . H68B H -0.3727(6) 0.4581(3) 0.0212(4) 0.088 Uiso 1 calc R . C69 C -0.2995(12) 0.5192(5) 0.0536(4) 0.206(8) Uani 1 d . . H69A H -0.3213(12) 0.5440(5) 0.0187(4) 0.247 Uiso 1 calc R . H69B H -0.2428(12) 0.5007(5) 0.0347(4) 0.247 Uiso 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 0.0256(4) 0.0273(4) 0.0259(4) 0.0033(3) -0.0002(3) -0.0012(3) Ni2 0.0273(4) 0.0272(4) 0.0281(4) 0.0007(3) -0.0008(3) -0.0004(3) K1 0.0396(7) 0.0348(7) 0.0399(7) 0.0004(6) 0.0045(6) -0.0001(6) P1 0.0304(8) 0.0294(8) 0.0249(7) -0.0004(6) -0.0010(6) 0.0023(6) P2 0.0306(8) 0.0294(8) 0.0321(8) -0.0011(6) 0.0025(6) 0.0024(6) P3 0.0263(7) 0.0265(7) 0.0292(8) 0.0032(6) -0.0011(6) -0.0019(6) O1 0.071(3) 0.075(3) 0.028(2) 0.012(2) -0.005(2) -0.008(3) O2 0.072(3) 0.094(4) 0.033(3) 0.005(2) -0.018(2) -0.009(3) O3 0.047(3) 0.041(2) 0.054(3) -0.007(2) 0.011(2) -0.019(2) O4 0.063(3) 0.084(3) 0.044(3) 0.024(2) 0.002(2) 0.016(3) O5 0.042(3) 0.136(5) 0.114(4) 0.080(4) 0.015(3) 0.018(3) O6 0.117(4) 0.059(3) 0.075(4) -0.005(3) 0.048(3) 0.019(3) O7 0.203(7) 0.036(3) 0.070(4) 0.004(3) 0.026(4) 0.032(4) O8 0.088(4) 0.068(3) 0.089(4) -0.018(3) 0.007(3) -0.023(3) O9 0.079(4) 0.117(5) 0.052(3) -0.020(3) 0.001(3) -0.027(3) N1 0.058(4) 0.057(4) 0.060(4) 0.008(3) 0.013(3) -0.004(3) N2 0.058(4) 0.052(3) 0.061(4) 0.018(3) 0.006(3) 0.009(3) C1 0.048(4) 0.034(3) 0.025(3) 0.004(2) 0.001(3) 0.007(3) C2 0.068(5) 0.040(4) 0.061(4) -0.007(3) 0.030(4) -0.002(3) C3 0.101(6) 0.043(4) 0.090(6) -0.016(4) 0.052(5) -0.024(4) C4 0.108(6) 0.033(4) 0.065(5) -0.004(3) 0.020(4) 0.014(4) C5 0.068(5) 0.051(4) 0.064(5) -0.014(4) -0.004(4) 0.019(4) C6 0.049(4) 0.044(4) 0.060(4) -0.008(3) -0.010(3) 0.016(3) C7 0.033(3) 0.037(3) 0.027(3) 0.001(2) -0.004(2) 0.010(3) C8 0.042(4) 0.055(4) 0.039(3) -0.004(3) -0.008(3) 0.009(3) C9 0.048(4) 0.073(5) 0.051(4) -0.007(4) -0.020(3) 0.009(3) C10 0.083(6) 0.078(5) 0.044(4) -0.009(4) -0.031(4) 0.031(4) C11 0.074(5) 0.089(5) 0.032(4) 0.005(4) 0.000(3) 0.016(4) C12 0.055(4) 0.063(4) 0.034(4) 0.009(3) 0.000(3) 0.016(3) C13 0.024(3) 0.042(3) 0.025(3) 0.003(2) 0.000(2) -0.001(3) C14 0.043(4) 0.057(4) 0.036(3) -0.010(3) 0.005(3) -0.005(3) C15 0.057(4) 0.074(5) 0.038(4) -0.010(3) 0.020(3) -0.012(4) C16 0.044(4) 0.081(5) 0.043(4) 0.013(4) 0.011(3) -0.013(4) C17 0.049(4) 0.045(4) 0.049(4) 0.005(3) 0.008(3) -0.008(3) C18 0.045(4) 0.037(3) 0.036(3) -0.007(3) 0.008(3) 0.001(3) C19 0.038(3) 0.032(3) 0.032(3) -0.001(2) 0.002(3) 0.007(3) C20 0.038(4) 0.048(4) 0.044(4) -0.002(3) 0.003(3) 0.006(3) C21 0.042(4) 0.061(4) 0.063(5) -0.007(4) -0.011(4) 0.008(3) C22 0.067(5) 0.055(4) 0.046(4) 0.002(3) -0.022(4) 0.010(4) C23 0.075(5) 0.051(4) 0.036(4) 0.008(3) 0.002(3) 0.006(4) C24 0.047(4) 0.038(3) 0.044(4) 0.008(3) 0.005(3) 0.009(3) C25 0.032(3) 0.042(3) 0.027(3) 0.002(3) -0.003(2) 0.003(3) C26 0.072(5) 0.041(4) 0.049(4) 0.006(3) 0.024(4) 0.008(3) C27 0.082(5) 0.066(5) 0.057(5) 0.010(4) 0.034(4) 0.027(4) C28 0.050(4) 0.078(5) 0.040(4) 0.019(4) 0.008(3) -0.004(4) C29 0.050(4) 0.068(5) 0.042(4) 0.007(3) -0.001(3) -0.024(3) C30 0.042(4) 0.052(4) 0.040(3) -0.009(3) 0.004(3) -0.011(3) C31 0.038(3) 0.031(3) 0.041(3) -0.006(3) 0.014(3) -0.001(3) C32 0.048(4) 0.035(4) 0.047(4) 0.000(3) 0.017(3) 0.005(3) C33 0.064(5) 0.031(4) 0.064(4) 0.005(3) 0.024(4) 0.005(3) C34 0.075(5) 0.039(4) 0.073(5) -0.012(3) 0.020(4) -0.016(4) C35 0.074(5) 0.050(4) 0.079(5) -0.017(4) -0.011(4) -0.018(4) C36 0.059(4) 0.041(4) 0.065(4) -0.008(3) -0.009(4) -0.005(3) C37 0.025(3) 0.030(3) 0.026(3) 0.003(2) 0.007(2) 0.001(2) C38 0.036(3) 0.033(3) 0.034(3) -0.002(3) 0.003(3) -0.002(3) C39 0.048(4) 0.029(3) 0.052(4) -0.002(3) 0.004(3) 0.005(3) C40 0.054(4) 0.028(3) 0.055(4) 0.015(3) 0.017(3) 0.016(3) C41 0.058(4) 0.042(4) 0.035(3) 0.005(3) 0.006(3) 0.010(3) C42 0.042(3) 0.033(3) 0.031(3) 0.001(3) 0.008(3) 0.002(3) C43 0.030(3) 0.023(3) 0.034(3) -0.004(2) 0.002(2) -0.001(2) C44 0.032(3) 0.038(3) 0.037(3) 0.001(3) -0.002(3) -0.005(3) C45 0.041(4) 0.036(3) 0.047(4) -0.004(3) -0.007(3) 0.004(3) C46 0.027(3) 0.046(4) 0.070(5) -0.014(3) -0.012(3) 0.003(3) C47 0.032(3) 0.044(4) 0.068(5) 0.004(3) 0.001(3) -0.004(3) C48 0.031(3) 0.041(3) 0.046(4) 0.004(3) 0.000(3) -0.003(3) C49 0.029(3) 0.034(3) 0.034(4) 0.004(3) 0.000(3) -0.005(2) C50 0.035(3) 0.043(4) 0.040(4) 0.003(3) 0.004(3) -0.004(3) C51 0.024(3) 0.033(3) 0.034(3) -0.001(3) 0.000(2) -0.001(3) C52 0.080(7) 0.240(14) 0.108(8) 0.117(9) 0.029(6) 0.057(8) C53 0.074(6) 0.099(7) 0.094(7) 0.041(5) 0.008(5) 0.017(5) C54 0.050(6) 0.186(11) 0.142(9) 0.087(8) 0.011(6) 0.023(6) C55 0.048(4) 0.083(5) 0.063(5) -0.006(4) -0.008(4) 0.004(4) C56 0.045(4) 0.074(5) 0.072(5) 0.009(4) 0.012(4) -0.013(4) C57 0.070(7) 0.446(26) 0.282(18) 0.308(20) 0.080(9) 0.067(11) C58 0.447(25) 0.076(7) 0.149(10) 0.035(7) 0.221(14) 0.063(11) C59 0.157(9) 0.087(7) 0.079(6) -0.011(5) 0.054(6) 0.016(6) C60 0.319(18) 0.043(6) 0.119(9) -0.005(5) 0.074(10) 0.052(8) C61 0.108(7) 0.033(4) 0.132(8) -0.006(5) 0.026(6) 0.009(4) C62 0.092(6) 0.041(4) 0.118(7) 0.037(5) 0.005(5) 0.005(4) C63 0.470(27) 0.103(9) 0.075(7) 0.052(6) 0.111(11) 0.107(13) C64 0.202(13) 0.239(15) 0.096(8) 0.068(9) -0.056(8) -0.176(12) C65 0.100(7) 0.081(6) 0.099(7) 0.015(5) 0.030(6) -0.049(5) C66 0.074(6) 0.104(7) 0.088(7) -0.031(6) 0.020(5) -0.022(5) C67 0.061(5) 0.078(5) 0.073(5) -0.038(4) -0.008(4) -0.016(4) C68 0.067(5) 0.081(6) 0.071(6) -0.015(5) -0.013(4) 0.003(4) C69 0.370(21) 0.226(14) 0.024(5) -0.008(6) 0.027(8) -0.183(15) _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 C49 1.746(6) . ? Ni1 C51 1.940(5) . ? Ni1 P1 2.1842(15) . ? Ni1 P3 2.2344(14) . ? Ni1 Ni2 2.4930(9) . ? Ni2 C50 1.749(6) . ? Ni2 C51 1.901(5) . ? Ni2 P2 2.1696(15) . ? Ni2 P3 2.2290(15) . ? K1 O9 2.752(5) . ? K1 O7 2.765(5) . ? K1 O5 2.778(5) . ? K1 O6 2.815(5) . ? K1 O4 2.826(4) . ? K1 O8 2.871(5) . ? K1 N2 2.928(5) . ? K1 N1 2.962(5) . ? K1 C66 3.537(8) . ? P1 C1 1.842(3) . ? P1 C7 1.840(3) . ? P1 C13 1.848(3) . ? P2 C19 1.840(3) . ? P2 C31 1.850(3) . ? P2 C25 1.850(3) . ? P3 C37 1.855(3) . ? P3 C43 1.861(3) . ? O1 C49 1.152(6) . ? O2 C50 1.149(6) . ? O3 C51 1.168(6) . ? O4 C54 1.320(9) . ? O4 C53 1.359(8) . ? O5 C55 1.350(8) . ? O5 C56 1.396(8) . ? O6 C60 1.327(9) . ? O6 C59 1.374(9) . ? O7 C61 1.349(9) . ? O7 C62 1.395(8) . ? O8 C66 1.337(8) . ? O8 C65 1.429(9) . ? O9 C68 1.352(9) . ? O9 C67 1.427(8) . ? N1 C64 1.347(10) . ? N1 C58 1.388(11) . ? N1 C52 1.435(9) . ? N2 C57 1.372(11) . ? N2 C63 1.375(11) . ? N2 C69 1.421(10) . ? C1 C2 1.39 . ? C1 C6 1.39 . ? C2 C3 1.39 . ? C3 C4 1.39 . ? C4 C5 1.39 . ? C5 C6 1.39 . ? C7 C8 1.39 . ? C7 C12 1.39 . ? C8 C9 1.39 . ? C9 C10 1.39 . ? C10 C11 1.39 . ? C11 C12 1.39 . ? C13 C14 1.39 . ? C13 C18 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C16 C17 1.39 . ? C17 C18 1.39 . ? C19 C20 1.39 . ? C19 C24 1.39 . ? C20 C21 1.39 . ? C21 C22 1.39 . ? C22 C23 1.39 . ? C23 C24 1.39 . ? C25 C26 1.39 . ? C25 C30 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? C28 C29 1.39 . ? C29 C30 1.39 . ? C31 C32 1.39 . ? C31 C36 1.39 . ? C32 C33 1.39 . ? C33 C34 1.39 . ? C34 C35 1.39 . ? C35 C36 1.39 . ? C37 C38 1.39 . ? C37 C42 1.39 . ? C38 C39 1.39 . ? C39 C40 1.39 . ? C40 C41 1.39 . ? C41 C42 1.39 . ? C43 C44 1.39 . ? C43 C48 1.39 . ? C44 C45 1.39 . ? C45 C46 1.39 . ? C46 C47 1.39 . ? C47 C48 1.39 . ? C52 C53 1.359(11) . ? C54 C55 1.384(10) . ? C56 C57 1.407(11) . ? C58 C59 1.368(12) . ? C60 C61 1.408(12) . ? C62 C63 1.397(12) . ? C64 C65 1.363(12) . ? C66 C67 1.453(10) . ? C68 C69 1.412(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C49 Ni1 C51 108.6(2) . . ? C49 Ni1 P1 104.6(2) . . ? C51 Ni1 P1 101.6(2) . . ? C49 Ni1 P3 114.8(2) . . ? C51 Ni1 P3 104.6(2) . . ? P1 Ni1 P3 121.38(6) . . ? C49 Ni1 Ni2 131.0(2) . . ? C51 Ni1 Ni2 48.9(2) . . ? P1 Ni1 Ni2 121.01(5) . . ? P3 Ni1 Ni2 55.94(4) . . ? C50 Ni2 C51 107.0(2) . . ? C50 Ni2 P2 110.2(2) . . ? C51 Ni2 P2 100.6(2) . . ? C50 Ni2 P3 120.3(2) . . ? C51 Ni2 P3 106.1(2) . . ? P2 Ni2 P3 110.65(6) . . ? C50 Ni2 Ni1 126.6(2) . . ? C51 Ni2 Ni1 50.2(2) . . ? P2 Ni2 Ni1 120.50(5) . . ? P3 Ni2 Ni1 56.15(4) . . ? O9 K1 O7 105.7(2) . . ? O9 K1 O5 94.1(2) . . ? O7 K1 O5 97.5(2) . . ? O9 K1 O6 139.9(2) . . ? O7 K1 O6 58.6(2) . . ? O5 K1 O6 122.9(2) . . ? O9 K1 O4 116.7(2) . . ? O7 K1 O4 131.4(2) . . ? O5 K1 O4 58.36(14) . . ? O6 K1 O4 97.4(2) . . ? O9 K1 O8 59.7(2) . . ? O7 K1 O8 125.3(2) . . ? O5 K1 O8 133.3(2) . . ? O6 K1 O8 97.4(2) . . ? O4 K1 O8 97.2(2) . . ? O9 K1 N2 61.4(2) . . ? O7 K1 N2 62.3(2) . . ? O5 K1 N2 61.17(15) . . ? O6 K1 N2 120.7(2) . . ? O4 K1 N2 119.15(15) . . ? O8 K1 N2 119.8(2) . . ? O9 K1 N1 118.4(2) . . ? O7 K1 N1 118.4(2) . . ? O5 K1 N1 118.4(2) . . ? O6 K1 N1 59.9(2) . . ? O4 K1 N1 60.37(14) . . ? O8 K1 N1 60.1(2) . . ? N2 K1 N1 179.4(2) . . ? O9 K1 C66 42.2(2) . . ? O7 K1 C66 132.5(2) . . ? O5 K1 C66 115.2(2) . . ? O6 K1 C66 118.2(2) . . ? O4 K1 C66 95.8(2) . . ? O8 K1 C66 21.0(2) . . ? N2 K1 C66 103.6(2) . . ? N1 K1 C66 76.2(2) . . ? C1 P1 C7 99.1(2) . . ? C1 P1 C13 103.8(2) . . ? C7 P1 C13 102.2(2) . . ? C1 P1 Ni1 119.85(14) . . ? C7 P1 Ni1 119.25(13) . . ? C13 P1 Ni1 110.29(13) . . ? C19 P2 C31 101.0(2) . . ? C19 P2 C25 103.6(2) . . ? C31 P2 C25 101.6(2) . . ? C19 P2 Ni2 117.34(13) . . ? C31 P2 Ni2 117.04(13) . . ? C25 P2 Ni2 114.06(13) . . ? C37 P3 C43 100.9(2) . . ? C37 P3 Ni2 120.09(12) . . ? C43 P3 Ni2 123.51(13) . . ? C37 P3 Ni1 125.66(13) . . ? C43 P3 Ni1 118.46(12) . . ? Ni2 P3 Ni1 67.91(4) . . ? C54 O4 C53 119.4(6) . . ? C54 O4 K1 118.2(5) . . ? C53 O4 K1 120.0(4) . . ? C55 O5 C56 117.2(6) . . ? C55 O5 K1 120.4(4) . . ? C56 O5 K1 119.4(4) . . ? C60 O6 C59 118.9(7) . . ? C60 O6 K1 118.9(5) . . ? C59 O6 K1 120.4(4) . . ? C61 O7 C62 118.5(6) . . ? C61 O7 K1 119.8(5) . . ? C62 O7 K1 119.0(4) . . ? C66 O8 C65 115.5(7) . . ? C66 O8 K1 108.9(5) . . ? C65 O8 K1 118.4(4) . . ? C68 O9 C67 115.7(6) . . ? C68 O9 K1 119.2(5) . . ? C67 O9 K1 119.3(4) . . ? C64 N1 C58 107.2(10) . . ? C64 N1 C52 109.1(9) . . ? C58 N1 C52 110.8(9) . . ? C64 N1 K1 109.8(5) . . ? C58 N1 K1 110.5(5) . . ? C52 N1 K1 109.3(4) . . ? C57 N2 C63 107.1(11) . . ? C57 N2 C69 112.7(11) . . ? C63 N2 C69 109.5(10) . . ? C57 N2 K1 109.5(5) . . ? C63 N2 K1 108.0(5) . . ? C69 N2 K1 109.9(5) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 116.6(2) . . ? C6 C1 P1 123.2(2) . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 123.7(2) . . ? C12 C7 P1 116.3(2) . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 P1 123.2(2) . . ? C18 C13 P1 116.7(2) . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 P2 123.5(2) . . ? C24 C19 P2 116.4(2) . . ? C19 C20 C21 120.0 . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 P2 123.1(2) . . ? C30 C25 P2 116.9(2) . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P2 122.4(2) . . ? C36 C31 P2 117.3(2) . . ? C31 C32 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C38 C37 C42 120.0 . . ? C38 C37 P3 120.8(2) . . ? C42 C37 P3 119.2(2) . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C37 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 P3 120.1(2) . . ? C48 C43 P3 119.9(2) . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? O1 C49 Ni1 174.0(5) . . ? O2 C50 Ni2 176.4(5) . . ? O3 C51 Ni2 140.3(4) . . ? O3 C51 Ni1 138.8(4) . . ? Ni2 C51 Ni1 80.9(2) . . ? C53 C52 N1 124.7(8) . . ? O4 C53 C52 119.2(7) . . ? O4 C54 C55 120.0(8) . . ? O5 C55 C54 117.7(7) . . ? O5 C56 C57 115.0(7) . . ? N2 C57 C56 125.2(9) . . ? C59 C58 N1 125.7(10) . . ? C58 C59 O6 117.8(7) . . ? O6 C60 C61 117.8(9) . . ? O7 C61 C60 117.2(7) . . ? C63 C62 O7 116.6(7) . . ? N2 C63 C62 128.1(8) . . ? N1 C64 C65 129.7(10) . . ? C64 C65 O8 115.1(7) . . ? O8 C66 C67 114.9(8) . . ? O8 C66 K1 50.2(4) . . ? C67 C66 K1 83.4(4) . . ? O9 C67 C66 111.5(6) . . ? O9 C68 C69 116.8(7) . . ? C68 C69 N2 123.9(8) . . ? _refine_diff_density_max 0.536 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.069 data_xr103 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C72 H114 K2 N8 Ni2 O18 P2' _chemical_formula_weight 1637.27 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'P' 'P' 0.1023 0.0942 '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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.211(4) _cell_length_b 13.861(2) _cell_length_c 13.942(2) _cell_angle_alpha 76.55 _cell_angle_beta 82.76 _cell_angle_gamma 80.78 _cell_volume 2071.0(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method ? _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8572 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 26.08 _reflns_number_total 7228 _reflns_number_observed 6350 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+8.5143P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7228 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_obs 0.0691 _refine_ls_wR_factor_all 0.1778 _refine_ls_wR_factor_obs 0.1735 _refine_ls_goodness_of_fit_all 1.257 _refine_ls_goodness_of_fit_obs 1.313 _refine_ls_restrained_S_all 1.257 _refine_ls_restrained_S_obs 1.313 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group K K 0.17053(10) 0.26621(8) 0.14678(8) 0.0302(3) Uani 1 d . . Ni Ni -0.38718(6) 0.53800(5) 0.41282(5) 0.0241(2) Uani 1 d . . P1 P -0.42573(11) 0.39495(9) 0.52568(9) 0.0224(3) Uani 1 d . . C1 C -0.3882(5) 0.5184(4) 0.2933(4) 0.0335(12) Uani 1 d . . O1 O -0.3863(4) 0.5001(4) 0.2169(3) 0.0535(12) Uani 1 d . . C2 C -0.2613(5) 0.5816(4) 0.4417(4) 0.0366(13) Uani 1 d . . O2 O -0.1739(4) 0.6044(4) 0.4606(5) 0.072(2) Uani 1 d . . C10 C -0.6879(4) 0.6619(3) 0.3845(3) 0.0241(10) Uani 1 d . . H10 H -0.6314(4) 0.6305(3) 0.4293(3) 0.029 Uiso 1 calc R . C11 C -0.6514(5) 0.7129(4) 0.2898(4) 0.0382(13) Uani 1 d . . H11 H -0.5690(5) 0.7132(4) 0.2702(4) 0.046 Uiso 1 calc R . C12 C -0.8956(5) 0.7090(4) 0.3446(5) 0.0411(14) Uani 1 d . . H12 H -0.9780(5) 0.7062(4) 0.3625(5) 0.049 Uiso 1 calc R . C13 C -0.8109(5) 0.6593(4) 0.4101(4) 0.0313(11) Uani 1 d . . H13 H -0.8372(5) 0.6237(4) 0.4722(4) 0.038 Uiso 1 calc R . C14 C -0.8568(6) 0.7627(5) 0.2528(5) 0.047(2) Uani 1 d . . H14 H -0.9134(6) 0.7986(5) 0.2099(5) 0.056 Uiso 1 calc R . C15 C -0.7351(6) 0.7634(5) 0.2241(4) 0.051(2) Uani 1 d . . H15 H -0.7091(6) 0.7975(5) 0.1611(4) 0.062 Uiso 1 calc R . C16 C -0.5006(5) 0.2975(4) 0.3955(4) 0.0341(12) Uani 1 d . . H16 H -0.5499(5) 0.3581(4) 0.3768(4) 0.041 Uiso 1 calc R . C17 C -0.3510(5) 0.1955(4) 0.4938(4) 0.0280(11) Uani 1 d . . H17 H -0.2980(5) 0.1859(4) 0.5425(4) 0.034 Uiso 1 calc R . C18 C -0.4236(4) 0.2869(3) 0.4693(3) 0.0224(10) Uani 1 d . . H18 H -0.4209(4) 0.3388(3) 0.5006(3) 0.027 Uiso 1 calc R . C19 C -0.3555(5) 0.1181(4) 0.4476(4) 0.0389(13) Uani 1 d . . H19 H -0.3058(5) 0.0575(4) 0.4654(4) 0.047 Uiso 1 calc R . C20 C -0.4331(6) 0.1303(5) 0.3753(5) 0.047(2) Uani 1 d . . H20 H -0.4363(6) 0.0784(5) 0.3442(5) 0.056 Uiso 1 calc R . C21 C -0.5057(6) 0.2204(5) 0.3496(5) 0.0456(15) Uani 1 d . . H21 H -0.5586(6) 0.2295(5) 0.3009(5) 0.055 Uiso 1 calc R . O3 O 0.1103(4) 0.1217(3) 0.3208(3) 0.0413(9) Uani 1 d . . O4 O 0.3622(3) 0.3746(3) 0.1456(3) 0.0370(9) Uani 1 d . . O5 O 0.3033(4) 0.0699(3) 0.1868(3) 0.0424(10) Uani 1 d . . O6 O 0.1264(3) 0.4395(3) 0.2255(3) 0.0423(10) Uani 1 d . . O7 O -0.0492(4) 0.3017(4) 0.0550(4) 0.0622(14) Uani 1 d . . O8 O 0.1738(5) 0.3039(4) -0.0612(3) 0.0572(13) Uani 1 d . . N1 N -0.0602(4) 0.3052(4) 0.2654(4) 0.0456(13) Uani 1 d . . N2 N 0.4041(4) 0.2224(4) 0.0279(3) 0.0428(12) Uani 1 d . . C30 C 0.4265(6) 0.0565(5) 0.1462(5) 0.049(2) Uani 1 d . . H30A H 0.4539(6) -0.0141(5) 0.1493(5) 0.059 Uiso 1 calc R . H30B H 0.4775(6) 0.0805(5) 0.1843(5) 0.059 Uiso 1 calc R . C31 C 0.4998(5) 0.2649(5) 0.0614(5) 0.048(2) Uani 1 d . . H31A H 0.5708(5) 0.2628(5) 0.0139(5) 0.057 Uiso 1 calc R . H31B H 0.5226(5) 0.2233(5) 0.1243(5) 0.057 Uiso 1 calc R . C32 C 0.2896(6) 0.0154(5) 0.2857(5) 0.049(2) Uani 1 d . . H32A H 0.3316(6) 0.0432(5) 0.3275(5) 0.059 Uiso 1 calc R . H32B H 0.3248(6) -0.0539(5) 0.2895(5) 0.059 Uiso 1 calc R . C33 C 0.4632(6) 0.3699(5) 0.0734(5) 0.051(2) Uani 1 d . . H33A H 0.5306(6) 0.3939(5) 0.0937(5) 0.061 Uiso 1 calc R . H33B H 0.4419(6) 0.4126(5) 0.0106(5) 0.061 Uiso 1 calc R . C34 C -0.0551(6) 0.2377(5) 0.3633(5) 0.059(2) Uani 1 d . . H34A H -0.1354(6) 0.2423(5) 0.3985(5) 0.071 Uiso 1 calc R . H34B H -0.0015(6) 0.2603(5) 0.4005(5) 0.071 Uiso 1 calc R . C35 C 0.1581(6) 0.0208(4) 0.3207(5) 0.0452(15) Uani 1 d . . H35A H 0.1155(6) -0.0045(4) 0.2774(5) 0.054 Uiso 1 calc R . H35B H 0.1474(6) -0.0201(4) 0.3871(5) 0.054 Uiso 1 calc R . C36 C 0.4363(6) 0.1136(5) 0.0402(5) 0.055(2) Uani 1 d . . H36A H 0.5190(6) 0.0996(5) 0.0116(5) 0.066 Uiso 1 calc R . H36B H 0.3837(6) 0.0894(5) 0.0035(5) 0.066 Uiso 1 calc R . C37 C -0.0120(6) 0.1307(5) 0.3607(6) 0.058(2) Uani 1 d . . H37A H -0.0191(6) 0.0895(5) 0.4271(6) 0.069 Uiso 1 calc R . H37B H -0.0614(6) 0.1080(5) 0.3203(6) 0.069 Uiso 1 calc R . C38 C 0.2333(6) 0.4698(5) 0.2482(6) 0.057(2) Uani 1 d . . H38A H 0.2644(6) 0.4233(5) 0.3058(6) 0.069 Uiso 1 calc R . H38B H 0.2141(6) 0.5357(5) 0.2634(6) 0.069 Uiso 1 calc R . C39 C 0.0323(6) 0.4417(5) 0.3040(5) 0.051(2) Uani 1 d . . H39A H 0.0132(6) 0.5088(5) 0.3162(5) 0.061 Uiso 1 calc R . H39B H 0.0588(6) 0.3967(5) 0.3641(5) 0.061 Uiso 1 calc R . C40 C 0.3270(6) 0.4724(5) 0.1620(6) 0.054(2) Uani 1 d . . H40A H 0.2944(6) 0.5160(5) 0.1034(6) 0.064 Uiso 1 calc R . H40B H 0.3970(6) 0.4987(5) 0.1752(6) 0.064 Uiso 1 calc R . C41 C -0.0410(9) 0.3523(7) -0.0453(6) 0.088(3) Uani 1 d . . H41A H -0.0282(9) 0.4210(7) -0.0507(6) 0.106 Uiso 1 calc R . H41B H -0.1157(9) 0.3530(7) -0.0739(6) 0.106 Uiso 1 calc R . C42 C -0.0787(5) 0.4102(5) 0.2761(5) 0.050(2) Uani 1 d . . H42A H -0.1451(5) 0.4188(5) 0.3265(5) 0.059 Uiso 1 calc R . H42B H -0.1017(5) 0.4536(5) 0.2141(5) 0.059 Uiso 1 calc R . C43 C -0.1576(7) 0.3398(7) 0.1074(7) 0.083(3) Uani 1 d . . H43A H -0.2279(7) 0.3277(7) 0.0802(7) 0.099 Uiso 1 calc R . H43B H -0.1610(7) 0.4115(7) 0.1001(7) 0.099 Uiso 1 calc R . C44 C -0.1593(6) 0.2895(7) 0.2141(7) 0.073(3) Uani 1 d . . H44A H -0.2356(6) 0.3131(7) 0.2478(7) 0.087 Uiso 1 calc R . H44B H -0.1567(6) 0.2181(7) 0.2198(7) 0.087 Uiso 1 calc R . C45 C 0.2736(8) 0.2549(7) -0.1127(5) 0.068(2) Uani 1 d . . H45A H 0.2737(8) 0.2827(7) -0.1834(5) 0.082 Uiso 1 calc R . H45B H 0.2672(8) 0.1841(7) -0.1010(5) 0.082 Uiso 1 calc R . C46 C 0.0627(8) 0.2990(6) -0.0988(5) 0.070(2) Uani 1 d . . H46A H 0.0511(8) 0.2296(6) -0.0904(5) 0.085 Uiso 1 calc R . H46B H 0.0662(8) 0.3295(6) -0.1689(5) 0.085 Uiso 1 calc R . C47 C 0.3903(7) 0.2692(7) -0.0767(5) 0.071(2) Uani 1 d . . H47A H 0.4583(7) 0.2416(7) -0.1169(5) 0.085 Uiso 1 calc R . H47B H 0.3936(7) 0.3404(7) -0.0867(5) 0.085 Uiso 1 calc R . NS1 N -0.2597(5) 0.8774(4) 0.3593(4) 0.0507(13) Uani 1 d . . CS1 C -0.2033(9) 0.9284(7) 0.2756(8) 0.080(3) Uani 1 d . . CS2 C -0.3767(7) 0.8518(5) 0.3539(7) 0.070(2) Uani 1 d . . HS2A H -0.4062(7) 0.8161(5) 0.4178(7) 0.105 Uiso 1 calc R . HS2B H -0.3708(7) 0.8104(5) 0.3066(7) 0.105 Uiso 1 calc R . HS2C H -0.4317(7) 0.9118(5) 0.3336(7) 0.105 Uiso 1 calc R . CS3 C -0.2030(11) 0.8515(7) 0.4495(8) 0.108(4) Uani 1 d . . HS3A H -0.2549(11) 0.8158(7) 0.5011(8) 0.162 Uiso 1 calc R . HS3B H -0.1890(11) 0.9114(7) 0.4673(8) 0.162 Uiso 1 calc R . HS3C H -0.1270(11) 0.8099(7) 0.4409(8) 0.162 Uiso 1 calc R . OS1 O -0.1084(10) 0.9576(10) 0.2593(10) 0.085(4) Uani 0.50 d P . OS1' O -0.2286(27) 0.9496(16) 0.1995(15) 0.205(14) Uani 0.50 d P . SN1 N 0.0582(11) 0.0362(9) 0.0596(10) 0.058(3) Uani 0.50 d P . SC2 C 0.0512(12) -0.0128(11) 0.0049(11) 0.052(4) Uani 0.50 d P . HC2A H 0.0062(12) 0.0299(11) -0.0479(11) 0.062 Uiso 0.50 calc PR . HC2B H 0.0000(12) -0.0626(11) 0.0396(11) 0.062 Uiso 0.50 calc PR . SN3 N 0.2531(11) -0.0597(10) -0.0199(10) 0.064(3) Uani 0.50 d P . SC4 C 0.1387(26) -0.0577(14) -0.0351(12) 0.108(9) Uani 0.50 d P . HC4A H 0.1341(26) -0.0331(14) -0.1058(12) 0.129 Uiso 0.50 calc PR . HC4B H 0.1245(26) -0.1270(14) -0.0207(12) 0.129 Uiso 0.50 calc PR . 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 K 0.0319(6) 0.0310(6) 0.0282(6) -0.0075(5) -0.0038(5) -0.0034(5) Ni 0.0240(3) 0.0212(3) 0.0249(3) -0.0043(2) 0.0023(2) -0.0010(2) P1 0.0229(6) 0.0196(6) 0.0237(6) -0.0048(5) -0.0012(5) -0.0008(5) C1 0.035(3) 0.028(3) 0.033(3) -0.003(2) 0.000(2) 0.003(2) O1 0.061(3) 0.067(3) 0.033(2) -0.018(2) -0.010(2) 0.002(2) C2 0.034(3) 0.028(3) 0.046(3) -0.009(2) 0.002(3) -0.001(2) O2 0.046(3) 0.070(3) 0.113(5) -0.028(3) -0.020(3) -0.023(3) C10 0.026(2) 0.023(2) 0.024(2) -0.008(2) -0.007(2) 0.002(2) C11 0.034(3) 0.046(3) 0.030(3) -0.001(2) -0.004(2) -0.003(3) C12 0.029(3) 0.045(3) 0.053(4) -0.018(3) -0.010(3) -0.001(2) C13 0.029(3) 0.033(3) 0.033(3) -0.013(2) 0.002(2) -0.003(2) C14 0.045(4) 0.050(4) 0.048(4) -0.012(3) -0.025(3) 0.006(3) C15 0.055(4) 0.067(4) 0.025(3) 0.005(3) -0.010(3) -0.004(3) C16 0.036(3) 0.030(3) 0.035(3) -0.008(2) -0.011(2) 0.004(2) C17 0.028(3) 0.024(3) 0.031(3) -0.005(2) -0.002(2) -0.002(2) C18 0.023(2) 0.021(2) 0.023(2) -0.006(2) 0.001(2) -0.004(2) C19 0.044(3) 0.026(3) 0.046(3) -0.012(2) -0.005(3) 0.003(2) C20 0.062(4) 0.036(3) 0.051(4) -0.022(3) -0.010(3) -0.008(3) C21 0.048(4) 0.047(4) 0.049(4) -0.020(3) -0.021(3) -0.004(3) O3 0.041(2) 0.041(2) 0.039(2) -0.001(2) 0.007(2) -0.012(2) O4 0.036(2) 0.031(2) 0.047(2) -0.011(2) -0.003(2) -0.008(2) O5 0.036(2) 0.034(2) 0.050(2) -0.001(2) -0.001(2) 0.001(2) O6 0.030(2) 0.046(2) 0.060(3) -0.030(2) -0.011(2) 0.002(2) O7 0.051(3) 0.072(3) 0.068(3) -0.029(3) -0.035(2) 0.020(2) O8 0.088(4) 0.061(3) 0.028(2) -0.008(2) -0.014(2) -0.024(3) N1 0.023(2) 0.061(3) 0.059(3) -0.032(3) 0.004(2) -0.001(2) N2 0.041(3) 0.062(3) 0.032(3) -0.019(2) 0.013(2) -0.024(2) C30 0.036(3) 0.044(4) 0.070(5) -0.026(3) 0.004(3) 0.004(3) C31 0.032(3) 0.063(4) 0.055(4) -0.029(3) 0.010(3) -0.014(3) C32 0.044(4) 0.032(3) 0.064(4) 0.004(3) -0.013(3) 0.000(3) C33 0.047(4) 0.059(4) 0.051(4) -0.014(3) 0.006(3) -0.029(3) C34 0.053(4) 0.068(5) 0.053(4) -0.025(4) 0.036(3) -0.016(3) C35 0.050(4) 0.034(3) 0.044(3) 0.009(3) -0.006(3) -0.010(3) C36 0.047(4) 0.069(5) 0.062(4) -0.045(4) 0.020(3) -0.016(3) C37 0.052(4) 0.054(4) 0.060(4) -0.007(3) 0.023(3) -0.018(3) C38 0.037(3) 0.061(4) 0.091(5) -0.049(4) -0.023(3) 0.005(3) C39 0.047(4) 0.056(4) 0.058(4) -0.034(3) -0.013(3) 0.008(3) C40 0.035(3) 0.034(3) 0.100(6) -0.024(3) -0.020(3) -0.002(3) C41 0.106(7) 0.091(6) 0.075(6) -0.035(5) -0.068(5) 0.038(5) C42 0.032(3) 0.062(4) 0.060(4) -0.036(3) 0.001(3) 0.008(3) C43 0.046(4) 0.107(7) 0.118(8) -0.076(6) -0.047(5) 0.028(4) C44 0.024(3) 0.089(6) 0.122(8) -0.063(6) -0.008(4) 0.002(3) C45 0.093(6) 0.098(6) 0.021(3) -0.014(3) 0.003(3) -0.044(5) C46 0.099(6) 0.068(5) 0.048(4) -0.017(4) -0.043(4) 0.012(4) C47 0.078(5) 0.116(7) 0.029(3) -0.019(4) 0.020(3) -0.056(5) NS1 0.050(3) 0.041(3) 0.062(4) -0.017(3) 0.001(3) -0.005(2) CS1 0.081(6) 0.077(6) 0.095(7) -0.046(6) 0.029(6) -0.040(5) CS2 0.050(4) 0.044(4) 0.104(6) 0.003(4) 0.001(4) -0.008(3) CS3 0.179(11) 0.052(5) 0.100(7) -0.026(5) -0.069(8) 0.023(6) OS1 0.050(6) 0.096(9) 0.104(10) -0.011(7) 0.009(6) -0.029(6) OS1' 0.372(36) 0.176(19) 0.105(13) -0.083(14) 0.139(19) -0.197(22) SN1 0.055(7) 0.053(7) 0.063(8) 0.012(6) -0.015(6) -0.024(6) SC2 0.051(7) 0.040(8) 0.035(7) 0.023(6) 0.028(7) 0.009(7) SN3 0.045(7) 0.083(9) 0.066(8) -0.020(7) -0.005(6) -0.007(6) SC4 0.222(28) 0.073(12) 0.047(10) 0.026(9) -0.060(14) -0.094(16) _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 K O4 2.808(4) . ? K O6 2.816(4) . ? K O8 2.821(4) . ? K O7 2.839(4) . ? K O3 2.848(4) . ? K O5 2.852(4) . ? K N1 2.933(5) . ? K N2 2.973(5) . ? Ni C2 1.746(6) . ? Ni C1 1.751(6) . ? Ni P1 2.2905(14) . ? Ni P1 2.3002(15) 2_466 ? P1 C18 1.842(5) . ? P1 C10 1.853(5) 2_466 ? P1 Ni 2.3002(15) 2_466 ? C1 O1 1.148(7) . ? C2 O2 1.155(7) . ? C10 C13 1.384(7) . ? C10 C11 1.390(7) . ? C10 P1 1.853(5) 2_466 ? C11 C15 1.385(8) . ? C12 C14 1.379(9) . ? C12 C13 1.389(8) . ? C14 C15 1.374(9) . ? C16 C21 1.379(8) . ? C16 C18 1.392(7) . ? C17 C19 1.384(7) . ? C17 C18 1.387(7) . ? C19 C20 1.377(8) . ? C20 C21 1.375(9) . ? O3 C37 1.410(7) . ? O3 C35 1.416(7) . ? O4 C40 1.413(7) . ? O4 C33 1.421(7) . ? O5 C32 1.413(7) . ? O5 C30 1.425(7) . ? O6 C39 1.424(8) . ? O6 C38 1.424(7) . ? O7 C41 1.410(10) . ? O7 C43 1.429(9) . ? O8 C45 1.418(9) . ? O8 C46 1.427(9) . ? N1 C44 1.464(8) . ? N1 C34 1.467(9) . ? N1 C42 1.477(8) . ? N2 C47 1.468(8) . ? N2 C36 1.469(8) . ? N2 C31 1.474(7) . ? C30 C36 1.504(10) . ? C31 C33 1.490(9) . ? C32 C35 1.490(9) . ? C34 C37 1.491(9) . ? C38 C40 1.491(10) . ? C39 C42 1.505(9) . ? C41 C46 1.489(11) . ? C43 C44 1.488(13) . ? C45 C47 1.515(10) . ? NS1 CS1 1.355(11) . ? NS1 CS3 1.426(10) . ? NS1 CS2 1.427(9) . ? CS1 OS1' 1.09(3) . ? CS1 OS1 1.176(13) . ? OS1 OS1' 1.70(3) . ? SN1 SC2 1.15(2) . ? SC2 SC4 1.22(3) . ? SN3 SC4 1.32(3) . ? 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 O4 K O6 60.38(11) . . ? O4 K O8 95.09(13) . . ? O6 K O8 114.35(14) . . ? O4 K O7 136.13(14) . . ? O6 K O7 96.07(13) . . ? O8 K O7 59.3(2) . . ? O4 K O3 118.67(12) . . ? O6 K O3 99.44(13) . . ? O8 K O3 141.29(13) . . ? O7 K O3 100.38(15) . . ? O4 K O5 98.05(12) . . ? O6 K O5 139.22(13) . . ? O8 K O5 100.86(14) . . ? O7 K O5 120.15(14) . . ? O3 K O5 58.65(12) . . ? O4 K N1 120.49(13) . . ? O6 K N1 61.40(13) . . ? O8 K N1 119.1(2) . . ? O7 K N1 61.02(15) . . ? O3 K N1 60.99(14) . . ? O5 K N1 118.47(14) . . ? O4 K N2 60.34(12) . . ? O6 K N2 119.57(13) . . ? O8 K N2 61.18(15) . . ? O7 K N2 119.04(15) . . ? O3 K N2 118.02(14) . . ? O5 K N2 60.45(13) . . ? N1 K N2 178.9(2) . . ? C2 Ni C1 118.7(3) . . ? C2 Ni P1 110.1(2) . . ? C1 Ni P1 108.9(2) . . ? C2 Ni P1 116.5(2) . 2_466 ? C1 Ni P1 112.5(2) . 2_466 ? P1 Ni P1 84.59(5) . 2_466 ? C18 P1 C10 98.4(2) . 2_466 ? C18 P1 Ni 113.5(2) . . ? C10 P1 Ni 117.4(2) 2_466 . ? C18 P1 Ni 116.2(2) . 2_466 ? C10 P1 Ni 117.3(2) 2_466 2_466 ? Ni P1 Ni 95.41(5) . 2_466 ? O1 C1 Ni 176.2(5) . . ? O2 C2 Ni 175.6(5) . . ? C13 C10 C11 117.9(5) . . ? C13 C10 P1 121.8(4) . 2_466 ? C11 C10 P1 120.2(4) . 2_466 ? C15 C11 C10 121.5(5) . . ? C14 C12 C13 119.5(5) . . ? C10 C13 C12 121.1(5) . . ? C15 C14 C12 120.6(5) . . ? C14 C15 C11 119.3(6) . . ? C21 C16 C18 121.7(5) . . ? C19 C17 C18 121.5(5) . . ? C17 C18 C16 116.9(5) . . ? C17 C18 P1 125.4(4) . . ? C16 C18 P1 117.7(4) . . ? C20 C19 C17 120.4(5) . . ? C21 C20 C19 119.1(5) . . ? C20 C21 C16 120.4(5) . . ? C37 O3 C35 111.6(5) . . ? C37 O3 K 116.6(4) . . ? C35 O3 K 116.4(3) . . ? C40 O4 C33 112.0(5) . . ? C40 O4 K 115.3(3) . . ? C33 O4 K 119.6(3) . . ? C32 O5 C30 111.1(5) . . ? C32 O5 K 115.9(3) . . ? C30 O5 K 118.3(3) . . ? C39 O6 C38 111.4(5) . . ? C39 O6 K 116.6(3) . . ? C38 O6 K 113.8(3) . . ? C41 O7 C43 111.0(6) . . ? C41 O7 K 115.0(5) . . ? C43 O7 K 118.1(4) . . ? C45 O8 C46 110.7(5) . . ? C45 O8 K 117.0(4) . . ? C46 O8 K 116.0(4) . . ? C44 N1 C34 111.4(6) . . ? C44 N1 C42 108.8(5) . . ? C34 N1 C42 109.7(5) . . ? C44 N1 K 109.0(4) . . ? C34 N1 K 108.7(3) . . ? C42 N1 K 109.4(3) . . ? C47 N2 C36 110.1(5) . . ? C47 N2 C31 109.0(5) . . ? C36 N2 C31 110.0(5) . . ? C47 N2 K 108.9(4) . . ? C36 N2 K 109.4(3) . . ? C31 N2 K 109.4(3) . . ? O5 C30 C36 109.3(5) . . ? N2 C31 C33 113.8(5) . . ? O5 C32 C35 109.2(5) . . ? O4 C33 C31 110.1(5) . . ? N1 C34 C37 114.2(5) . . ? O3 C35 C32 109.0(5) . . ? N2 C36 C30 114.2(5) . . ? O3 C37 C34 109.0(5) . . ? O6 C38 C40 109.8(5) . . ? O6 C39 C42 109.3(5) . . ? O4 C40 C38 109.4(5) . . ? O7 C41 C46 108.2(6) . . ? N1 C42 C39 113.1(5) . . ? O7 C43 C44 109.5(6) . . ? N1 C44 C43 115.4(7) . . ? O8 C45 C47 109.1(6) . . ? O8 C46 C41 110.1(6) . . ? N2 C47 C45 114.4(5) . . ? CS1 NS1 CS3 120.2(8) . . ? CS1 NS1 CS2 117.9(7) . . ? CS3 NS1 CS2 121.8(8) . . ? OS1' CS1 OS1 97.1(15) . . ? OS1' CS1 NS1 130.8(15) . . ? OS1 CS1 NS1 131.9(13) . . ? CS1 OS1 OS1' 39.6(8) . . ? CS1 OS1' OS1 43.3(13) . . ? SN1 SC2 SC4 123.9(20) . . ? SC2 SC4 SN3 125.4(17) . . ? _refine_diff_density_max 0.525 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.084