Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Laurence K. Thompson' 'Craig J. Matthews' 'Liang Zhao' 'Claire Wilson' 'Michael A. Leech' 'Judith A.K. Howard' _publ_contact_author_name 'Laurie K. Thompson' _publ_contact_author_address ; Laurie K. Thompson, University Research Professor, Dept. of Chemistry, Memorial University, St. John's, Newfoundland, A1B 3X7 CANADA ; _publ_contact_author_email 'lthomp@morgan.ucs.mun.ca' data_cjm64cm (1) _database_code_CSD 162087 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H48 N33 Ni3 O33.50' _chemical_formula_weight 1871.38 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 15.211(3) _cell_length_b 15.363(3) _cell_length_c 19.525(4) _cell_angle_alpha 111.999(2) _cell_angle_beta 91.168(3) _cell_angle_gamma 109.541(2) _cell_volume 3931.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 875 _cell_measurement_theta_min 14.86 _cell_measurement_theta_max 22.83 _exptl_crystal_description 'triangular block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1910 _exptl_absorpt_coefficient_mu 0.819 _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 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 'Bruker SMART CCD area detector' _diffrn_measurement_method 'omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48465 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13820 _reflns_number_gt 10510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0828P)^2^+9.3411P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13820 _refine_ls_number_parameters 1096 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.022 _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 0.16160(4) 0.38056(4) 0.08180(3) 0.01773(15) Uani 1 1 d . . . Ni2 Ni 0.30148(4) 0.28456(4) 0.16852(3) 0.01829(15) Uani 1 1 d . . . Ni3 Ni 0.59439(4) 0.10939(4) 0.34089(3) 0.01986(15) Uani 1 1 d . . . O101 O 0.3367(2) 0.0812(3) 0.3980(2) 0.0346(8) Uani 1 1 d . . . N101 N 0.6958(3) 0.2145(3) 0.4351(2) 0.0258(8) Uani 1 1 d . . . C101 C 0.7818(3) 0.2142(4) 0.4518(3) 0.0309(11) Uani 1 1 d . . . H10A H 0.8005 0.1651 0.4179 0.037 Uiso 1 1 calc R . . O102 O 0.0134(2) 0.1286(2) 0.15834(18) 0.0266(7) Uani 1 1 d . . . N102 N 0.5476(3) 0.3603(3) 0.4959(2) 0.0301(9) Uani 1 1 d . . . H10B H 0.4928 0.3582 0.4816 0.036 Uiso 1 1 calc R . . H10C H 0.5848 0.4117 0.5339 0.036 Uiso 1 1 calc R . . C102 C 0.8431(4) 0.2830(4) 0.5165(3) 0.0411(13) Uani 1 1 d . . . H10D H 0.9026 0.2814 0.5260 0.049 Uiso 1 1 calc R . . N103 N 0.5248(2) 0.2026(3) 0.4013(2) 0.0220(8) Uani 1 1 d . . . C103 C 0.8147(4) 0.3549(4) 0.5673(3) 0.0468(15) Uani 1 1 d . . . H10E H 0.8544 0.4010 0.6124 0.056 Uiso 1 1 calc R . . N104 N 0.4409(2) 0.2056(3) 0.3721(2) 0.0225(8) Uani 1 1 d . . . H10F H 0.4456 0.2505 0.3548 0.027 Uiso 1 1 calc R . . C104 C 0.7269(4) 0.3580(4) 0.5512(3) 0.0366(12) Uani 1 1 d . . . H10G H 0.7070 0.4063 0.5847 0.044 Uiso 1 1 calc R . . N105 N 0.3118(2) 0.2100(3) 0.2880(2) 0.0213(8) Uani 1 1 d . . . H10H H 0.3713 0.2448 0.2959 0.026 Uiso 1 1 calc R . . C105 C 0.6693(3) 0.2872(3) 0.4835(3) 0.0232(9) Uani 1 1 d . . . N106 N 0.2533(2) 0.2163(3) 0.24061(19) 0.0202(8) Uani 1 1 d . . . C106 C 0.5748(3) 0.2841(3) 0.4593(2) 0.0211(9) Uani 1 1 d . . . N107 N 0.1572(2) 0.2104(3) 0.12866(19) 0.0176(7) Uani 1 1 d . . . C107 C 0.3547(3) 0.1425(3) 0.3699(2) 0.0199(9) Uani 1 1 d . . . N108 N 0.1153(2) 0.2320(3) 0.07457(19) 0.0173(7) Uani 1 1 d . . . C108 C 0.2786(3) 0.1497(3) 0.3237(2) 0.0182(9) Uani 1 1 d . . . N109 N 0.0937(3) 0.0705(3) -0.0156(2) 0.0221(8) Uani 1 1 d . . . H10I H 0.1128 0.0523 0.0168 0.027 Uiso 1 1 calc R . . H10J H 0.0763 0.0291 -0.0619 0.027 Uiso 1 1 calc R . . C109 C 0.1828(3) 0.0978(3) 0.3174(3) 0.0243(10) Uani 1 1 d . . . H10K H 0.1607 0.0593 0.3449 0.029 Uiso 1 1 calc R . . N110 N 0.0917(2) 0.2982(3) -0.0280(2) 0.0203(8) Uani 1 1 d . . . C110 C 0.1214(3) 0.1052(3) 0.2689(2) 0.0215(9) Uani 1 1 d . . . H11A H 0.0563 0.0736 0.2636 0.026 Uiso 1 1 calc R . . C111 C 0.1607(3) 0.1620(3) 0.2280(2) 0.0169(8) Uani 1 1 d . . . C112 C 0.1025(3) 0.1667(3) 0.1668(2) 0.0178(9) Uani 1 1 d . . . C113 C 0.0909(3) 0.1635(3) 0.0064(2) 0.0174(9) Uani 1 1 d . . . C114 C 0.0644(3) 0.1970(3) -0.0509(2) 0.0184(9) Uani 1 1 d . . . C115 C 0.0170(3) 0.1310(3) -0.1226(2) 0.0235(9) Uani 1 1 d . . . H11B H -0.0006 0.0617 -0.1374 0.028 Uiso 1 1 calc R . . C116 C -0.0041(3) 0.1693(4) -0.1722(3) 0.0303(11) Uani 1 1 d . . . H11C H -0.0372 0.1261 -0.2202 0.036 Uiso 1 1 calc R . . C117 C 0.0250(4) 0.2727(4) -0.1490(3) 0.0343(12) Uani 1 1 d . . . H11D H 0.0126 0.3003 -0.1813 0.041 Uiso 1 1 calc R . . C118 C 0.0728(3) 0.3343(4) -0.0768(3) 0.0276(10) Uani 1 1 d . . . H11E H 0.0928 0.4039 -0.0615 0.033 Uiso 1 1 calc R . . O201 O 0.4675(3) -0.0717(3) 0.10641(18) 0.0358(8) Uani 1 1 d . . . N201 N 0.5408(2) -0.0027(3) 0.38136(19) 0.0207(8) Uani 1 1 d . . . C201 C 0.5838(3) -0.0094(4) 0.4389(3) 0.0269(10) Uani 1 1 d . . . H20A H 0.6362 0.0457 0.4701 0.032 Uiso 1 1 calc R . . O202 O 0.3265(3) 0.2163(2) -0.05490(18) 0.0312(8) Uani 1 1 d . . . N202 N 0.3339(3) -0.1292(3) 0.2389(2) 0.0317(9) Uani 1 1 d . . . H20B H 0.3088 -0.1204 0.2033 0.038 Uiso 1 1 calc R . . H20C H 0.3032 -0.1785 0.2505 0.038 Uiso 1 1 calc R . . C202 C 0.5528(4) -0.0954(4) 0.4536(3) 0.0315(11) Uani 1 1 d . . . H20D H 0.5839 -0.0980 0.4938 0.038 Uiso 1 1 calc R . . N203 N 0.4737(2) 0.0110(3) 0.26411(19) 0.0193(7) Uani 1 1 d . . . C203 C 0.4750(4) -0.1768(4) 0.4075(3) 0.0327(11) Uani 1 1 d . . . H20E H 0.4543 -0.2360 0.4154 0.039 Uiso 1 1 calc R . . N204 N 0.4308(3) 0.0319(3) 0.21028(19) 0.0215(8) Uani 1 1 d . . . H20F H 0.3995 0.0710 0.2253 0.026 Uiso 1 1 calc R . . C204 C 0.4277(4) -0.1700(4) 0.3492(3) 0.0297(11) Uani 1 1 d . . . H20G H 0.3740 -0.2235 0.3184 0.036 Uiso 1 1 calc R . . N205 N 0.3730(2) 0.1167(3) 0.1377(2) 0.0200(8) Uani 1 1 d . . . H20H H 0.3739 0.1305 0.1848 0.024 Uiso 1 1 calc R . . C205 C 0.4628(3) -0.0812(3) 0.3380(2) 0.0209(9) Uani 1 1 d . . . N206 N 0.3468(2) 0.1704(3) 0.1083(2) 0.0196(8) Uani 1 1 d . . . C206 C 0.4194(3) -0.0668(3) 0.2758(2) 0.0201(9) Uani 1 1 d . . . N207 N 0.3207(2) 0.3022(3) 0.0699(2) 0.0194(7) Uani 1 1 d . . . C207 C 0.4360(3) -0.0057(3) 0.1374(2) 0.0202(9) Uani 1 1 d . . . N208 N 0.2901(2) 0.3722(3) 0.0562(2) 0.0197(8) Uani 1 1 d . . . C208 C 0.3979(3) 0.0411(3) 0.0948(2) 0.0194(9) Uani 1 1 d . . . N209 N 0.4487(3) 0.4743(3) 0.0728(2) 0.0302(9) Uani 1 1 d . . . H20I H 0.4684 0.4289 0.0750 0.036 Uiso 1 1 calc R . . H20J H 0.4887 0.5316 0.0769 0.036 Uiso 1 1 calc R . . C209 C 0.3919(3) 0.0118(3) 0.0182(2) 0.0227(9) Uani 1 1 d . . . H20K H 0.4031 -0.0454 -0.0119 0.027 Uiso 1 1 calc R . . N210 N 0.2294(3) 0.5163(3) 0.0707(2) 0.0222(8) Uani 1 1 d . . . C210 C 0.3689(3) 0.0708(3) -0.0116(3) 0.0239(10) Uani 1 1 d . . . H21A H 0.3657 0.0558 -0.0625 0.029 Uiso 1 1 calc R . . C211 C 0.3505(3) 0.1532(3) 0.0361(2) 0.0185(9) Uani 1 1 d . . . C212 C 0.3306(3) 0.2285(3) 0.0127(2) 0.0196(9) Uani 1 1 d . . . C213 C 0.3561(3) 0.4557(3) 0.0630(2) 0.0217(9) Uani 1 1 d . . . C214 C 0.3205(3) 0.5340(3) 0.0607(2) 0.0213(9) Uani 1 1 d . . . C215 C 0.3747(3) 0.6180(3) 0.0491(3) 0.0294(11) Uani 1 1 d . . . H21B H 0.4372 0.6285 0.0425 0.035 Uiso 1 1 calc R . . C216 C 0.3351(4) 0.6862(4) 0.0473(3) 0.0359(12) Uani 1 1 d . . . H21C H 0.3698 0.7420 0.0379 0.043 Uiso 1 1 calc R . . C217 C 0.2430(4) 0.6699(3) 0.0597(3) 0.0303(11) Uani 1 1 d . . . H21D H 0.2154 0.7158 0.0605 0.036 Uiso 1 1 calc R . . C218 C 0.1928(3) 0.5851(3) 0.0709(3) 0.0282(10) Uani 1 1 d . . . H21E H 0.1308 0.5746 0.0791 0.034 Uiso 1 1 calc R . . O301 O 0.6973(2) 0.3959(2) 0.3723(2) 0.0371(8) Uani 1 1 d . . . N301 N 0.6884(3) 0.0441(3) 0.2864(2) 0.0223(8) Uani 1 1 d . . . C301 C 0.7094(3) -0.0302(4) 0.2935(3) 0.0294(10) Uani 1 1 d . . . H30A H 0.6830 -0.0547 0.3283 0.035 Uiso 1 1 calc R . . O302 O 0.3781(2) 0.5948(2) 0.26748(19) 0.0300(7) Uani 1 1 d . . . N302 N 0.7338(3) 0.2014(3) 0.1824(2) 0.0320(9) Uani 1 1 d . . . H30B H 0.7175 0.2483 0.1789 0.038 Uiso 1 1 calc R . . H30C H 0.7712 0.1797 0.1541 0.038 Uiso 1 1 calc R . . C302 C 0.7684(4) -0.0726(4) 0.2518(3) 0.0333(11) Uani 1 1 d . . . H30D H 0.7837 -0.1220 0.2601 0.040 Uiso 1 1 calc R . . N303 N 0.6447(3) 0.1890(3) 0.2769(2) 0.0223(8) Uani 1 1 d . . . C303 C 0.8035(4) -0.0401(4) 0.1983(3) 0.0423(14) Uani 1 1 d . . . H30E H 0.8402 -0.0702 0.1674 0.051 Uiso 1 1 calc R . . N304 N 0.6106(3) 0.2585(3) 0.2676(2) 0.0234(8) Uani 1 1 d . . . H30F H 0.5714 0.2384 0.2275 0.028 Uiso 1 1 calc R . . C304 C 0.7844(4) 0.0377(4) 0.1901(3) 0.0351(12) Uani 1 1 d . . . H30G H 0.8090 0.0617 0.1546 0.042 Uiso 1 1 calc R . . C305 C 0.7276(3) 0.0793(3) 0.2359(3) 0.0246(10) Uani 1 1 d . . . N306 N 0.4955(2) 0.3435(3) 0.2512(2) 0.0216(8) Uani 1 1 d . . . H30H H 0.4859 0.2803 0.2288 0.026 Uiso 1 1 calc R . . C306 C 0.7016(3) 0.1629(3) 0.2309(3) 0.0244(10) Uani 1 1 d . . . N307 N 0.4329(2) 0.3783(3) 0.2355(2) 0.0198(8) Uani 1 1 d . . . C307 C 0.6351(3) 0.3538(3) 0.3167(2) 0.0212(9) Uani 1 1 d . . . C308 C 0.5735(3) 0.4055(3) 0.3016(2) 0.0200(9) Uani 1 1 d . . . N309 N 0.2881(2) 0.4227(3) 0.2218(2) 0.0199(8) Uani 1 1 d . . . C309 C 0.5931(3) 0.5085(3) 0.3385(3) 0.0273(10) Uani 1 1 d . . . H30I H 0.6482 0.5512 0.3729 0.033 Uiso 1 1 calc R . . N310 N 0.2085(2) 0.4364(3) 0.1959(2) 0.0190(7) Uani 1 1 d . . . C310 C 0.5282(3) 0.5446(3) 0.3221(3) 0.0265(10) Uani 1 1 d . . . H31A H 0.5382 0.6130 0.3447 0.032 Uiso 1 1 calc R . . N311 N 0.1459(3) 0.4132(3) 0.2993(2) 0.0279(9) Uani 1 1 d . . . H31B H 0.1978 0.4142 0.3184 0.033 Uiso 1 1 calc R . . H31C H 0.0975 0.4053 0.3217 0.033 Uiso 1 1 calc R . . C311 C 0.4467(3) 0.4761(3) 0.2707(2) 0.0187(9) Uani 1 1 d . . . C312 C 0.3658(3) 0.5042(3) 0.2519(2) 0.0185(9) Uani 1 1 d . . . N312 N 0.0449(3) 0.4070(3) 0.1284(2) 0.0218(8) Uani 1 1 d . . . C313 C 0.1402(3) 0.4241(3) 0.2342(2) 0.0188(9) Uani 1 1 d . . . C314 C 0.0512(3) 0.4243(3) 0.2016(2) 0.0214(9) Uani 1 1 d . . . C315 C -0.0197(3) 0.4419(4) 0.2423(3) 0.0274(10) Uani 1 1 d . . . H31D H -0.0140 0.4532 0.2927 0.033 Uiso 1 1 calc R . . C316 C -0.0986(3) 0.4421(4) 0.2066(3) 0.0326(11) Uani 1 1 d . . . H31E H -0.1464 0.4548 0.2329 0.039 Uiso 1 1 calc R . . C317 C -0.1062(3) 0.4234(4) 0.1312(3) 0.0304(11) Uani 1 1 d . . . H31F H -0.1589 0.4228 0.1058 0.036 Uiso 1 1 calc R . . C318 C -0.0331(3) 0.4056(3) 0.0947(3) 0.0266(10) Uani 1 1 d . . . H31G H -0.0385 0.3919 0.0439 0.032 Uiso 1 1 calc R . . N1 N 0.1833(3) 0.9202(3) 0.0951(2) 0.0268(9) Uani 1 1 d . . . O1 O 0.1700(3) 0.8378(3) 0.0418(2) 0.0529(11) Uani 1 1 d . . . O2 O 0.2172(2) 0.9359(3) 0.1591(2) 0.0403(9) Uani 1 1 d . . . O3 O 0.1601(2) 0.9844(2) 0.0835(2) 0.0322(8) Uani 1 1 d . . . N2 N 0.5998(3) 0.3129(4) 0.1167(3) 0.0365(11) Uani 1 1 d . . . O4 O 0.5569(3) 0.3547(4) 0.0944(3) 0.0723(16) Uani 1 1 d . . . O5 O 0.5653(3) 0.2206(3) 0.1008(2) 0.0505(10) Uani 1 1 d . . . O6 O 0.6808(2) 0.3645(3) 0.1578(2) 0.0412(9) Uani 1 1 d . . . N3 N 0.3051(3) 0.3844(3) 0.4313(2) 0.0458(12) Uani 1 1 d D . . O7 O 0.2154(3) 0.3453(4) 0.4181(3) 0.0516(7) Uiso 0.80 1 d PD . . O8 O 0.3389(3) 0.4410(4) 0.3990(3) 0.0516(7) Uiso 0.80 1 d PD . . O9 O 0.3474(4) 0.3613(4) 0.4711(3) 0.0516(7) Uiso 0.80 1 d PD . . O7A O 0.3908(6) 0.4201(13) 0.4250(11) 0.0516(7) Uiso 0.20 1 d PD . . O8A O 0.2529(10) 0.4266(13) 0.4230(11) 0.0516(7) Uiso 0.20 1 d PD . . O9A O 0.2915(12) 0.3317(13) 0.4684(10) 0.0516(7) Uiso 0.20 1 d PD . . O1W O 0.4582(7) 0.1965(8) 0.2608(6) 0.076(3) Uiso 0.50 1 d P . . O2W O 0.5515(3) 0.8247(3) 0.1569(2) 0.0427(9) Uani 1 1 d . . . O3W O 0.3650(3) 0.3588(3) -0.1140(2) 0.0450(9) Uani 1 1 d . . . O4W O 0.5489(3) 0.7152(3) 0.2386(2) 0.0427(9) Uani 1 1 d . . . O5W O -0.1233(3) 0.1734(3) 0.0984(2) 0.0414(9) Uani 1 1 d . . . O6W O 0.9567(6) 0.0888(7) 0.3933(5) 0.0838(13) Uiso 0.70 1 d P . . O6WA O 0.9967(15) 0.1080(16) 0.4226(12) 0.0838(13) Uiso 0.30 1 d P . . O7W O 0.8303(6) 0.0809(6) 0.6027(5) 0.0838(13) Uiso 0.70 1 d P . . O7WA O 0.9005(14) 0.0932(14) 0.5416(11) 0.0838(13) Uiso 0.30 1 d P . . O8W O 1.1248(6) 0.2206(6) 0.4901(5) 0.0838(13) Uiso 0.70 1 d P . . O8WA O 1.1779(15) 0.2203(15) 0.5060(11) 0.0838(13) Uiso 0.30 1 d P . . O9W O 0.0215(4) 0.0987(4) -0.3499(3) 0.0890(17) Uani 1 1 d . . . O10W O 0.9223(4) 0.2866(4) 0.6843(3) 0.0755(14) Uani 1 1 d . . . O11W O 0.6973(4) 0.7760(4) 0.3530(3) 0.0687(13) Uani 1 1 d . . . O12W O 1.0794(4) 0.3484(4) 0.6109(3) 0.0721(14) Uani 1 1 d . . . O13W O 0.8333(3) 0.7008(4) 0.2913(3) 0.0684(13) Uani 1 1 d . . . O14W O 0.8880(3) 0.4973(4) 0.4360(3) 0.0568(11) Uani 1 1 d . . . O15W O 0.7535(3) 0.5587(3) 0.1510(3) 0.0618(12) Uani 1 1 d . . . O16W O 0.7746(3) 0.3236(3) 0.7560(2) 0.0522(11) Uani 1 1 d . . . O17W O 1.0174(3) 0.4031(3) 0.4093(2) 0.0550(11) Uani 1 1 d . . . O18W O 0.8092(9) -0.0061(10) 0.4547(7) 0.100(4) Uiso 0.50 1 d P . . O19W O 0.7808(7) -0.1034(7) 0.4892(5) 0.063(2) Uiso 0.50 1 d P . . O20W O 0.9512(4) 0.2020(5) 0.3161(4) 0.0939(19) 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 0.0187(3) 0.0163(3) 0.0218(3) 0.0096(2) 0.0043(2) 0.0084(2) Ni2 0.0190(3) 0.0171(3) 0.0214(3) 0.0094(2) 0.0040(2) 0.0080(2) Ni3 0.0210(3) 0.0209(3) 0.0206(3) 0.0088(2) 0.0041(2) 0.0108(2) O101 0.0252(17) 0.047(2) 0.042(2) 0.0339(18) 0.0032(15) 0.0088(16) N101 0.024(2) 0.026(2) 0.028(2) 0.0105(17) 0.0046(16) 0.0116(16) C101 0.025(2) 0.032(3) 0.036(3) 0.012(2) 0.002(2) 0.014(2) O102 0.0164(15) 0.0336(18) 0.0341(18) 0.0219(15) 0.0029(13) 0.0050(13) N102 0.027(2) 0.024(2) 0.033(2) 0.0037(18) -0.0008(17) 0.0103(17) C102 0.025(3) 0.040(3) 0.051(3) 0.009(3) -0.004(2) 0.015(2) N103 0.0196(18) 0.0245(19) 0.0233(19) 0.0091(16) 0.0017(15) 0.0105(16) C103 0.036(3) 0.039(3) 0.043(3) -0.002(3) -0.016(2) 0.008(2) N104 0.0186(18) 0.0244(19) 0.029(2) 0.0129(17) 0.0029(15) 0.0105(16) C104 0.031(3) 0.030(3) 0.037(3) 0.002(2) -0.002(2) 0.012(2) N105 0.0180(18) 0.0263(19) 0.0206(19) 0.0122(16) 0.0027(15) 0.0061(15) C105 0.020(2) 0.022(2) 0.027(2) 0.0096(19) 0.0011(18) 0.0067(18) N106 0.0231(19) 0.0239(19) 0.0175(18) 0.0106(15) 0.0028(15) 0.0107(16) C106 0.023(2) 0.021(2) 0.023(2) 0.0114(19) 0.0065(18) 0.0088(18) N107 0.0201(18) 0.0204(18) 0.0163(17) 0.0104(15) 0.0019(14) 0.0090(15) C107 0.025(2) 0.022(2) 0.015(2) 0.0075(18) 0.0073(17) 0.0115(18) N108 0.0177(17) 0.0208(18) 0.0169(18) 0.0107(15) 0.0019(14) 0.0078(14) C108 0.021(2) 0.020(2) 0.0118(19) 0.0046(17) 0.0024(16) 0.0075(17) N109 0.032(2) 0.0185(18) 0.0176(18) 0.0084(15) -0.0004(15) 0.0106(16) C109 0.026(2) 0.026(2) 0.026(2) 0.018(2) 0.0065(19) 0.0066(19) N110 0.0202(18) 0.0231(19) 0.0234(19) 0.0143(16) 0.0046(15) 0.0095(15) C110 0.016(2) 0.023(2) 0.027(2) 0.0143(19) 0.0039(17) 0.0050(18) C111 0.019(2) 0.0126(19) 0.019(2) 0.0057(17) 0.0053(17) 0.0059(16) C112 0.019(2) 0.014(2) 0.021(2) 0.0071(17) 0.0017(17) 0.0070(17) C113 0.0100(18) 0.019(2) 0.023(2) 0.0089(18) 0.0037(16) 0.0047(16) C114 0.018(2) 0.021(2) 0.020(2) 0.0122(18) 0.0069(17) 0.0080(17) C115 0.021(2) 0.022(2) 0.024(2) 0.0085(19) 0.0025(18) 0.0050(18) C116 0.028(2) 0.036(3) 0.024(2) 0.013(2) -0.0009(19) 0.007(2) C117 0.036(3) 0.043(3) 0.035(3) 0.026(2) 0.001(2) 0.016(2) C118 0.032(3) 0.028(2) 0.030(3) 0.017(2) 0.005(2) 0.013(2) O201 0.063(2) 0.043(2) 0.0227(17) 0.0161(16) 0.0135(16) 0.0418(19) N201 0.0221(18) 0.0266(19) 0.0184(18) 0.0099(16) 0.0058(15) 0.0140(16) C201 0.025(2) 0.037(3) 0.023(2) 0.013(2) 0.0049(19) 0.017(2) O202 0.051(2) 0.0349(19) 0.0241(18) 0.0177(15) 0.0124(15) 0.0290(17) N202 0.033(2) 0.028(2) 0.028(2) 0.0156(18) -0.0070(18) 0.0007(18) C202 0.039(3) 0.046(3) 0.023(2) 0.021(2) 0.007(2) 0.024(2) N203 0.0250(19) 0.0209(18) 0.0171(18) 0.0102(15) 0.0020(15) 0.0117(15) C203 0.049(3) 0.038(3) 0.032(3) 0.026(2) 0.016(2) 0.027(3) N204 0.030(2) 0.0252(19) 0.0188(19) 0.0122(16) 0.0063(15) 0.0174(16) C204 0.039(3) 0.024(2) 0.030(3) 0.013(2) 0.004(2) 0.014(2) N205 0.0265(19) 0.0204(18) 0.0169(18) 0.0086(15) 0.0052(15) 0.0120(15) C205 0.027(2) 0.023(2) 0.016(2) 0.0080(18) 0.0070(18) 0.0142(19) N206 0.0229(18) 0.0188(18) 0.0232(19) 0.0119(15) 0.0051(15) 0.0108(15) C206 0.025(2) 0.019(2) 0.018(2) 0.0059(18) 0.0031(18) 0.0120(18) N207 0.0247(19) 0.0184(18) 0.0245(19) 0.0132(16) 0.0081(15) 0.0141(15) C207 0.024(2) 0.016(2) 0.023(2) 0.0094(18) 0.0043(18) 0.0082(18) N208 0.0244(19) 0.0169(18) 0.0257(19) 0.0135(15) 0.0073(15) 0.0114(15) C208 0.023(2) 0.017(2) 0.024(2) 0.0121(18) 0.0064(18) 0.0096(18) N209 0.021(2) 0.026(2) 0.052(3) 0.024(2) 0.0091(18) 0.0088(17) C209 0.025(2) 0.022(2) 0.025(2) 0.0099(19) 0.0062(18) 0.0132(19) N210 0.0254(19) 0.0174(18) 0.026(2) 0.0090(16) 0.0026(16) 0.0109(15) C210 0.031(2) 0.028(2) 0.021(2) 0.0132(19) 0.0066(19) 0.017(2) C211 0.019(2) 0.021(2) 0.021(2) 0.0111(18) 0.0066(17) 0.0109(17) C212 0.021(2) 0.019(2) 0.022(2) 0.0108(18) 0.0051(17) 0.0082(18) C213 0.026(2) 0.025(2) 0.022(2) 0.0152(19) 0.0079(18) 0.0118(19) C214 0.028(2) 0.019(2) 0.017(2) 0.0069(18) 0.0000(18) 0.0102(18) C215 0.031(3) 0.025(2) 0.038(3) 0.018(2) 0.006(2) 0.010(2) C216 0.048(3) 0.019(2) 0.040(3) 0.017(2) 0.002(2) 0.006(2) C217 0.044(3) 0.021(2) 0.033(3) 0.013(2) 0.001(2) 0.018(2) C218 0.034(3) 0.024(2) 0.030(3) 0.011(2) 0.000(2) 0.015(2) O301 0.0313(19) 0.0277(18) 0.046(2) 0.0115(17) -0.0114(16) 0.0086(15) N301 0.0241(19) 0.0218(19) 0.025(2) 0.0105(16) 0.0060(15) 0.0114(16) C301 0.035(3) 0.028(2) 0.035(3) 0.017(2) 0.008(2) 0.018(2) O302 0.0278(17) 0.0176(16) 0.041(2) 0.0089(14) -0.0053(14) 0.0084(13) N302 0.035(2) 0.040(2) 0.044(3) 0.029(2) 0.0186(19) 0.027(2) C302 0.035(3) 0.034(3) 0.048(3) 0.025(2) 0.014(2) 0.023(2) N303 0.0231(19) 0.0213(19) 0.030(2) 0.0129(16) 0.0049(16) 0.0139(16) C303 0.044(3) 0.046(3) 0.063(4) 0.031(3) 0.031(3) 0.036(3) N304 0.0243(19) 0.0202(19) 0.027(2) 0.0079(16) -0.0004(16) 0.0113(16) C304 0.034(3) 0.042(3) 0.049(3) 0.029(3) 0.025(2) 0.025(2) C305 0.024(2) 0.023(2) 0.032(3) 0.015(2) 0.0062(19) 0.0117(19) N306 0.0186(18) 0.0151(17) 0.029(2) 0.0073(16) 0.0015(15) 0.0062(15) C306 0.019(2) 0.024(2) 0.033(3) 0.015(2) 0.0023(19) 0.0077(18) N307 0.0167(17) 0.0176(18) 0.027(2) 0.0100(16) 0.0042(15) 0.0081(15) C307 0.016(2) 0.021(2) 0.028(2) 0.0138(19) 0.0008(18) 0.0047(18) C308 0.019(2) 0.019(2) 0.026(2) 0.0120(18) 0.0073(18) 0.0081(18) N309 0.0182(18) 0.0173(18) 0.0257(19) 0.0101(15) 0.0038(15) 0.0069(15) C309 0.022(2) 0.020(2) 0.032(3) 0.009(2) -0.0045(19) 0.0015(19) N310 0.0181(18) 0.0164(17) 0.0256(19) 0.0092(15) 0.0037(15) 0.0094(14) C310 0.030(2) 0.015(2) 0.032(3) 0.0060(19) -0.001(2) 0.0089(19) N311 0.0219(19) 0.041(2) 0.027(2) 0.0166(19) 0.0060(16) 0.0153(18) C311 0.022(2) 0.015(2) 0.021(2) 0.0100(18) 0.0063(17) 0.0060(17) C312 0.021(2) 0.018(2) 0.020(2) 0.0090(18) 0.0073(17) 0.0116(18) N312 0.0228(19) 0.0188(18) 0.027(2) 0.0099(16) 0.0030(15) 0.0109(15) C313 0.019(2) 0.014(2) 0.022(2) 0.0040(17) 0.0015(17) 0.0084(17) C314 0.019(2) 0.016(2) 0.029(2) 0.0096(19) 0.0032(18) 0.0068(17) C315 0.022(2) 0.034(3) 0.024(2) 0.009(2) 0.0031(19) 0.012(2) C316 0.023(2) 0.038(3) 0.038(3) 0.012(2) 0.008(2) 0.017(2) C317 0.022(2) 0.040(3) 0.037(3) 0.019(2) 0.004(2) 0.017(2) C318 0.026(2) 0.029(2) 0.025(2) 0.010(2) 0.0010(19) 0.012(2) N1 0.0229(19) 0.027(2) 0.037(2) 0.0188(19) 0.0074(17) 0.0106(17) O1 0.099(3) 0.044(2) 0.038(2) 0.0192(19) 0.016(2) 0.049(2) O2 0.0338(19) 0.053(2) 0.037(2) 0.0264(18) -0.0046(16) 0.0111(17) O3 0.0339(18) 0.0259(17) 0.047(2) 0.0228(16) 0.0070(16) 0.0148(15) N2 0.031(2) 0.063(3) 0.043(3) 0.038(2) 0.020(2) 0.030(2) O4 0.056(3) 0.134(5) 0.105(4) 0.100(4) 0.045(3) 0.067(3) O5 0.043(2) 0.049(3) 0.051(3) 0.014(2) 0.0059(19) 0.013(2) O6 0.0272(19) 0.042(2) 0.057(2) 0.0287(19) 0.0041(17) 0.0066(16) N3 0.067(3) 0.030(2) 0.032(2) 0.010(2) 0.024(2) 0.010(2) O2W 0.045(2) 0.046(2) 0.045(2) 0.0233(19) 0.0102(18) 0.0219(18) O3W 0.051(2) 0.045(2) 0.044(2) 0.0228(19) 0.0123(18) 0.0188(19) O4W 0.046(2) 0.044(2) 0.051(2) 0.0270(19) 0.0185(18) 0.0223(18) O5W 0.036(2) 0.066(3) 0.041(2) 0.031(2) 0.0185(17) 0.0301(19) O9W 0.092(4) 0.085(4) 0.077(4) 0.028(3) 0.007(3) 0.022(3) O10W 0.078(3) 0.084(4) 0.085(4) 0.046(3) 0.018(3) 0.040(3) O11W 0.072(3) 0.074(3) 0.080(3) 0.046(3) 0.024(3) 0.034(3) O12W 0.065(3) 0.077(3) 0.078(3) 0.033(3) 0.016(3) 0.029(3) O13W 0.058(3) 0.069(3) 0.076(3) 0.024(3) 0.010(2) 0.027(2) O14W 0.040(2) 0.071(3) 0.061(3) 0.028(2) 0.004(2) 0.020(2) O15W 0.046(2) 0.050(3) 0.087(3) 0.028(2) 0.017(2) 0.014(2) O16W 0.062(3) 0.036(2) 0.053(3) 0.0210(19) 0.002(2) 0.009(2) O17W 0.048(2) 0.072(3) 0.049(2) 0.027(2) 0.016(2) 0.024(2) O20W 0.061(3) 0.089(4) 0.106(5) 0.013(4) 0.008(3) 0.027(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 N208 2.061(4) . ? Ni1 N310 2.074(4) . ? Ni1 N110 2.075(4) . ? Ni1 N210 2.090(4) . ? Ni1 N108 2.098(3) . ? Ni1 N312 2.101(4) . ? Ni2 N207 2.055(3) . ? Ni2 N206 2.057(3) . ? Ni2 N106 2.062(3) . ? Ni2 N309 2.067(3) . ? Ni2 N107 2.077(3) . ? Ni2 N307 2.083(4) . ? Ni3 N303 2.049(4) . ? Ni3 N203 2.058(4) . ? Ni3 N201 2.088(4) . ? Ni3 N101 2.089(4) . ? Ni3 N103 2.089(4) . ? Ni3 N301 2.099(4) . ? O101 C107 1.219(5) . ? N101 C101 1.343(6) . ? N101 C105 1.352(6) . ? C101 C102 1.369(7) . ? O102 C112 1.262(5) . ? N102 C106 1.327(6) . ? C102 C103 1.381(8) . ? N103 C106 1.301(6) . ? N103 N104 1.408(5) . ? C103 C104 1.387(8) . ? N104 C107 1.333(5) . ? C104 C105 1.391(7) . ? N105 N106 1.322(5) . ? N105 C108 1.335(5) . ? C105 C106 1.485(6) . ? N106 C111 1.335(5) . ? N107 C112 1.314(5) . ? N107 N108 1.417(5) . ? C107 C108 1.512(6) . ? N108 C113 1.300(5) . ? C108 C109 1.384(6) . ? N109 C113 1.345(5) . ? C109 C110 1.378(6) . ? N110 C118 1.337(6) . ? N110 C114 1.353(5) . ? C110 C111 1.397(6) . ? C111 C112 1.510(6) . ? C113 C114 1.494(6) . ? C114 C115 1.383(6) . ? C115 C116 1.389(7) . ? C116 C117 1.380(7) . ? C117 C118 1.382(7) . ? O201 C207 1.224(5) . ? N201 C201 1.342(6) . ? N201 C205 1.347(6) . ? C201 C202 1.387(7) . ? O202 C212 1.258(5) . ? N202 C206 1.319(6) . ? C202 C203 1.377(7) . ? N203 C206 1.309(5) . ? N203 N204 1.414(5) . ? C203 C204 1.390(7) . ? N204 C207 1.336(6) . ? C204 C205 1.392(6) . ? N205 N206 1.317(5) . ? N205 C208 1.332(5) . ? C205 C206 1.491(6) . ? N206 C211 1.339(5) . ? N207 C212 1.315(5) . ? N207 N208 1.410(5) . ? C207 C208 1.501(6) . ? N208 C213 1.295(5) . ? C208 C209 1.383(6) . ? N209 C213 1.335(6) . ? C209 C210 1.371(6) . ? N210 C218 1.347(6) . ? N210 C214 1.354(6) . ? C210 C211 1.383(6) . ? C211 C212 1.504(6) . ? C213 C214 1.489(6) . ? C214 C215 1.382(6) . ? C215 C216 1.382(7) . ? C216 C217 1.382(7) . ? C217 C218 1.373(7) . ? O301 C307 1.230(5) . ? N301 C301 1.336(6) . ? N301 C305 1.352(6) . ? C301 C302 1.385(7) . ? O302 C312 1.254(5) . ? N302 C306 1.317(6) . ? C302 C303 1.365(7) . ? N303 C306 1.309(6) . ? N303 N304 1.398(5) . ? C303 C304 1.384(7) . ? N304 C307 1.331(6) . ? C304 C305 1.388(6) . ? C305 C306 1.499(6) . ? N306 N307 1.319(5) . ? N306 C308 1.333(6) . ? N307 C311 1.335(5) . ? C307 C308 1.501(6) . ? C308 C309 1.391(6) . ? N309 C312 1.318(5) . ? N309 N310 1.412(5) . ? C309 C310 1.368(6) . ? N310 C313 1.296(5) . ? C310 C311 1.392(6) . ? N311 C313 1.347(6) . ? C311 C312 1.513(6) . ? N312 C318 1.334(6) . ? N312 C314 1.348(6) . ? C313 C314 1.486(6) . ? C314 C315 1.391(6) . ? C315 C316 1.378(7) . ? C316 C317 1.385(7) . ? C317 C318 1.381(7) . ? N1 O3 1.242(5) . ? N1 O2 1.246(5) . ? N1 O1 1.249(5) . ? N2 O4 1.227(6) . ? N2 O5 1.245(6) . ? N2 O6 1.274(6) . ? N3 O9 1.218(4) . ? N3 O8A 1.223(5) . ? N3 O8 1.241(4) . ? N3 O9A 1.248(5) . ? N3 O7A 1.263(5) . ? N3 O7 1.269(4) . ? O7 O8A 1.151(16) . ? O7 O9A 1.619(14) . ? O8 O7A 1.122(14) . ? O8 O8A 1.375(14) . ? O9 O9A 0.808(15) . ? O9 O7A 1.516(13) . ? O6W O6WA 0.72(2) . ? O7W O7WA 1.64(2) . ? O8W O8WA 0.86(2) . ? O18W O19W 1.791(16) . ? 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 N208 Ni1 N310 92.34(14) . . ? N208 Ni1 N110 94.38(14) . . ? N310 Ni1 N110 166.85(13) . . ? N208 Ni1 N210 77.48(13) . . ? N310 Ni1 N210 96.16(14) . . ? N110 Ni1 N210 96.33(14) . . ? N208 Ni1 N108 89.80(13) . . ? N310 Ni1 N108 90.59(13) . . ? N110 Ni1 N108 78.15(13) . . ? N210 Ni1 N108 165.79(14) . . ? N208 Ni1 N312 169.17(14) . . ? N310 Ni1 N312 77.29(14) . . ? N110 Ni1 N312 96.40(14) . . ? N210 Ni1 N312 100.29(14) . . ? N108 Ni1 N312 93.38(13) . . ? N207 Ni2 N206 76.51(13) . . ? N207 Ni2 N106 159.70(14) . . ? N206 Ni2 N106 91.12(14) . . ? N207 Ni2 N309 93.60(14) . . ? N206 Ni2 N309 164.49(14) . . ? N106 Ni2 N309 101.52(14) . . ? N207 Ni2 N107 89.54(14) . . ? N206 Ni2 N107 99.16(14) . . ? N106 Ni2 N107 76.42(13) . . ? N309 Ni2 N107 92.59(13) . . ? N207 Ni2 N307 101.98(14) . . ? N206 Ni2 N307 94.33(14) . . ? N106 Ni2 N307 94.86(14) . . ? N309 Ni2 N307 75.84(13) . . ? N107 Ni2 N307 164.02(14) . . ? N303 Ni3 N203 93.90(14) . . ? N303 Ni3 N201 165.55(14) . . ? N203 Ni3 N201 77.50(14) . . ? N303 Ni3 N101 93.51(15) . . ? N203 Ni3 N101 167.36(14) . . ? N201 Ni3 N101 97.14(14) . . ? N303 Ni3 N103 95.08(14) . . ? N203 Ni3 N103 92.17(14) . . ? N201 Ni3 N103 96.82(14) . . ? N101 Ni3 N103 76.99(14) . . ? N303 Ni3 N301 77.40(14) . . ? N203 Ni3 N301 97.54(14) . . ? N201 Ni3 N301 92.08(14) . . ? N101 Ni3 N301 94.05(15) . . ? N103 Ni3 N301 168.06(14) . . ? C101 N101 C105 118.6(4) . . ? C101 N101 Ni3 126.1(3) . . ? C105 N101 Ni3 115.2(3) . . ? N101 C101 C102 122.9(5) . . ? C101 C102 C103 118.5(5) . . ? C106 N103 N104 114.2(3) . . ? C106 N103 Ni3 117.3(3) . . ? N104 N103 Ni3 124.7(3) . . ? C102 C103 C104 119.9(5) . . ? C107 N104 N103 123.6(4) . . ? C103 C104 C105 118.3(5) . . ? N106 N105 C108 120.2(4) . . ? N101 C105 C104 121.7(4) . . ? N101 C105 C106 115.0(4) . . ? C104 C105 C106 123.3(4) . . ? N105 N106 C111 120.1(3) . . ? N105 N106 Ni2 121.9(3) . . ? C111 N106 Ni2 116.8(3) . . ? N103 C106 N102 125.5(4) . . ? N103 C106 C105 114.2(4) . . ? N102 C106 C105 120.3(4) . . ? C112 N107 N108 118.8(3) . . ? C112 N107 Ni2 119.5(3) . . ? N108 N107 Ni2 119.1(2) . . ? O101 C107 N104 125.6(4) . . ? O101 C107 C108 121.7(4) . . ? N104 C107 C108 112.6(4) . . ? C113 N108 N107 116.9(3) . . ? C113 N108 Ni1 114.0(3) . . ? N107 N108 Ni1 119.6(2) . . ? N105 C108 C109 122.3(4) . . ? N105 C108 C107 114.0(4) . . ? C109 C108 C107 123.7(4) . . ? C110 C109 C108 117.6(4) . . ? C118 N110 C114 118.5(4) . . ? C118 N110 Ni1 127.4(3) . . ? C114 N110 Ni1 114.2(3) . . ? C109 C110 C111 117.5(4) . . ? N106 C111 C110 121.8(4) . . ? N106 C111 C112 115.4(3) . . ? C110 C111 C112 122.8(4) . . ? O102 C112 N107 130.2(4) . . ? O102 C112 C111 119.0(4) . . ? N107 C112 C111 110.9(3) . . ? N108 C113 N109 125.4(4) . . ? N108 C113 C114 114.8(4) . . ? N109 C113 C114 119.6(4) . . ? N110 C114 C115 121.7(4) . . ? N110 C114 C113 114.9(4) . . ? C115 C114 C113 123.4(4) . . ? C114 C115 C116 119.3(4) . . ? C117 C116 C115 118.8(4) . . ? C116 C117 C118 118.8(4) . . ? N110 C118 C117 122.9(4) . . ? C201 N201 C205 118.6(4) . . ? C201 N201 Ni3 125.9(3) . . ? C205 N201 Ni3 114.7(3) . . ? N201 C201 C202 122.4(4) . . ? C203 C202 C201 118.8(4) . . ? C206 N203 N204 114.5(3) . . ? C206 N203 Ni3 118.1(3) . . ? N204 N203 Ni3 125.3(3) . . ? C202 C203 C204 119.6(4) . . ? C207 N204 N203 123.7(4) . . ? C203 C204 C205 118.3(5) . . ? N206 N205 C208 120.1(4) . . ? N201 C205 C204 122.2(4) . . ? N201 C205 C206 114.9(4) . . ? C204 C205 C206 122.8(4) . . ? N205 N206 C211 120.3(3) . . ? N205 N206 Ni2 123.2(3) . . ? C211 N206 Ni2 116.5(3) . . ? N203 C206 N202 126.4(4) . . ? N203 C206 C205 113.5(4) . . ? N202 C206 C205 120.1(4) . . ? C212 N207 N208 118.8(3) . . ? C212 N207 Ni2 118.6(3) . . ? N208 N207 Ni2 118.7(2) . . ? O201 C207 N204 125.4(4) . . ? O201 C207 C208 121.8(4) . . ? N204 C207 C208 112.8(4) . . ? C213 N208 N207 115.9(3) . . ? C213 N208 Ni1 116.4(3) . . ? N207 N208 Ni1 119.8(2) . . ? N205 C208 C209 122.2(4) . . ? N205 C208 C207 114.1(4) . . ? C209 C208 C207 123.7(4) . . ? C210 C209 C208 117.2(4) . . ? C218 N210 C214 117.7(4) . . ? C218 N210 Ni1 128.0(3) . . ? C214 N210 Ni1 114.3(3) . . ? C209 C210 C211 118.4(4) . . ? N206 C211 C210 121.1(4) . . ? N206 C211 C212 114.4(4) . . ? C210 C211 C212 124.4(4) . . ? O202 C212 N207 128.4(4) . . ? O202 C212 C211 119.9(4) . . ? N207 C212 C211 111.7(4) . . ? N208 C213 N209 125.0(4) . . ? N208 C213 C214 114.1(4) . . ? N209 C213 C214 120.9(4) . . ? N210 C214 C215 122.0(4) . . ? N210 C214 C213 114.3(4) . . ? C215 C214 C213 123.7(4) . . ? C216 C215 C214 119.4(5) . . ? C215 C216 C217 118.7(4) . . ? C218 C217 C216 119.1(4) . . ? N210 C218 C217 123.0(4) . . ? C301 N301 C305 117.7(4) . . ? C301 N301 Ni3 127.5(3) . . ? C305 N301 Ni3 114.7(3) . . ? N301 C301 C302 123.3(4) . . ? C303 C302 C301 118.4(4) . . ? C306 N303 N304 114.8(4) . . ? C306 N303 Ni3 119.0(3) . . ? N304 N303 Ni3 125.2(3) . . ? C302 C303 C304 119.7(5) . . ? C307 N304 N303 124.1(4) . . ? C303 C304 C305 118.6(5) . . ? N301 C305 C304 122.1(4) . . ? N301 C305 C306 115.0(4) . . ? C304 C305 C306 122.9(4) . . ? N307 N306 C308 120.5(4) . . ? N303 C306 N302 126.0(4) . . ? N303 C306 C305 113.6(4) . . ? N302 C306 C305 120.3(4) . . ? N306 N307 C311 120.2(4) . . ? N306 N307 Ni2 122.9(3) . . ? C311 N307 Ni2 116.4(3) . . ? O301 C307 N304 125.1(4) . . ? O301 C307 C308 121.6(4) . . ? N304 C307 C308 113.2(4) . . ? N306 C308 C309 122.0(4) . . ? N306 C308 C307 114.3(4) . . ? C309 C308 C307 123.7(4) . . ? C312 N309 N310 116.3(3) . . ? C312 N309 Ni2 118.4(3) . . ? N310 N309 Ni2 118.3(3) . . ? C310 C309 C308 117.5(4) . . ? C313 N310 N309 114.1(3) . . ? C313 N310 Ni1 113.2(3) . . ? N309 N310 Ni1 120.0(3) . . ? C309 C310 C311 118.1(4) . . ? N307 C311 C310 121.7(4) . . ? N307 C311 C312 114.6(4) . . ? C310 C311 C312 123.7(4) . . ? O302 C312 N309 129.6(4) . . ? O302 C312 C311 120.3(4) . . ? N309 C312 C311 110.1(3) . . ? C318 N312 C314 117.8(4) . . ? C318 N312 Ni1 128.7(3) . . ? C314 N312 Ni1 113.4(3) . . ? N310 C313 N311 125.0(4) . . ? N310 C313 C314 114.8(4) . . ? N311 C313 C314 120.2(4) . . ? N312 C314 C315 122.2(4) . . ? N312 C314 C313 114.0(4) . . ? C315 C314 C313 123.8(4) . . ? C316 C315 C314 118.8(4) . . ? C315 C316 C317 119.5(4) . . ? C318 C317 C316 118.0(4) . . ? N312 C318 C317 123.7(4) . . ? O3 N1 O2 121.0(4) . . ? O3 N1 O1 119.2(4) . . ? O2 N1 O1 119.8(4) . . ? O4 N2 O5 121.5(5) . . ? O4 N2 O6 119.9(5) . . ? O5 N2 O6 118.6(4) . . ? O9 N3 O8A 150.5(10) . . ? O9 N3 O8 128.0(4) . . ? O8A N3 O8 67.8(8) . . ? O9 N3 O9A 38.2(7) . . ? O8A N3 O9A 124.4(8) . . ? O8 N3 O9A 166.2(8) . . ? O9 N3 O7A 75.3(8) . . ? O8A N3 O7A 118.3(8) . . ? O8 N3 O7A 53.2(7) . . ? O9A N3 O7A 113.0(7) . . ? O9 N3 O7 118.2(4) . . ? O8A N3 O7 55.0(8) . . ? O8 N3 O7 113.7(4) . . ? O9A N3 O7 80.0(8) . . ? O7A N3 O7 163.4(9) . . ? O8A O7 N3 60.5(4) . . ? O8A O7 O9A 103.0(8) . . ? N3 O7 O9A 49.4(4) . . ? O7A O8 N3 64.4(5) . . ? O7A O8 O8A 117.1(7) . . ? N3 O8 O8A 55.5(4) . . ? O9A O9 N3 72.9(6) . . ? O9A O9 O7A 125.9(8) . . ? N3 O9 O7A 53.7(4) . . ? O8 O7A N3 62.4(5) . . ? O8 O7A O9 113.0(5) . . ? N3 O7A O9 51.0(4) . . ? O7 O8A N3 64.5(5) . . ? O7 O8A O8 112.3(9) . . ? N3 O8A O8 56.7(4) . . ? O9 O9A N3 68.9(5) . . ? O9 O9A O7 119.4(6) . . ? N3 O9A O7 50.5(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.299 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.097 #===END data_l2m (2) _database_code_CSD 149292 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H53 B3 F13 N33 Ni2 O10' _chemical_formula_weight 1685.11 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 12.5079(17) _cell_length_b 14.952(2) _cell_length_c 19.463(3) _cell_angle_alpha 96.740(2) _cell_angle_beta 96.966(2) _cell_angle_gamma 108.259(2) _cell_volume 3384.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 17.34 _cell_measurement_theta_max 27.27 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.721 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART-CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33715 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.54 _reflns_number_total 15434 _reflns_number_gt 13936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0364P)^2^+14.5747P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15434 _refine_ls_number_parameters 1221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1485 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.008 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 1.15565(3) 0.96152(3) 0.23206(2) 0.01232(10) Uani 1 1 d . . . Ni2 Ni 0.67052(4) 0.48574(3) 0.23753(2) 0.01281(10) Uani 1 1 d . . . F13 F 0.91200(16) 0.72130(14) 0.22751(10) 0.0159(4) Uani 1 1 d . . . O72 O 0.8834(2) 0.99540(17) 0.09985(12) 0.0163(5) Uani 1 1 d . . . O50 O 0.6982(2) 0.47167(18) 0.01792(13) 0.0188(5) Uani 1 1 d . . . O12 O 1.0999(2) 0.97977(17) 0.43850(13) 0.0203(5) Uani 1 1 d . . . O20 O 0.9054(2) 0.47798(18) 0.39093(13) 0.0230(5) Uani 1 1 d . . . O80 O 0.5308(2) 0.68812(18) 0.28928(13) 0.0192(5) Uani 1 1 d . . . N52 N 0.6690(2) 0.5487(2) 0.14953(14) 0.0138(5) Uani 1 1 d . . . N1 N 1.1181(2) 1.0893(2) 0.22961(15) 0.0145(5) Uani 1 1 d . . . O42 O 1.2643(2) 0.77988(19) 0.12646(14) 0.0206(5) Uani 1 1 d . . . N40 N 1.1252(3) 0.7487(2) 0.19480(15) 0.0151(5) Uani 1 1 d . . . N48 N 0.9731(2) 0.6339(2) 0.08867(15) 0.0146(5) Uani 1 1 d . . . N82 N 0.6978(2) 0.60863(19) 0.30550(15) 0.0143(5) Uani 1 1 d . . . N51 N 0.7654(2) 0.5835(2) 0.11771(15) 0.0146(5) Uani 1 1 d . . . N69 N 1.0407(2) 0.90587(19) 0.13986(14) 0.0130(5) Uani 1 1 d . . . N78 N 0.7318(2) 0.8252(2) 0.19486(14) 0.0142(5) Uani 1 1 d . . . N9 N 1.0364(2) 0.9506(2) 0.29612(14) 0.0141(5) Uani 1 1 d . . . N81 N 0.7150(2) 0.6986(2) 0.28399(15) 0.0137(5) Uani 1 1 d . . . N54 N 0.5587(3) 0.5950(2) 0.06245(16) 0.0193(6) Uani 1 1 d . . . N39 N 1.1794(2) 0.8343(2) 0.24283(15) 0.0139(5) Uani 1 1 d . . . N61 N 1.2606(2) 0.9890(2) 0.15717(15) 0.0153(5) Uani 1 1 d . . . N30 N 0.6720(2) 0.3597(2) 0.17831(15) 0.0154(5) Uani 1 1 d . . . N18 N 1.0006(2) 0.7276(2) 0.39513(15) 0.0159(5) Uani 1 1 d . . . N22 N 0.8393(2) 0.4958(2) 0.25468(14) 0.0146(5) Uani 1 1 d . . . N31 N 1.2809(2) 0.9974(2) 0.32345(15) 0.0167(6) Uani 1 1 d . . . N4 N 1.0229(3) 1.2318(2) 0.21427(16) 0.0206(6) Uani 1 1 d . . . N60 N 0.4977(2) 0.4727(2) 0.20977(15) 0.0160(6) Uani 1 1 d . . . N8 N 0.9008(3) 1.0127(2) 0.33658(16) 0.0187(6) Uani 1 1 d . . . C49 C 0.7749(3) 0.5382(2) 0.05596(17) 0.0148(6) Uani 1 1 d . . . N10 N 1.0065(2) 0.8786(2) 0.33737(15) 0.0143(5) Uani 1 1 d . . . N27 N 0.7062(3) 0.2112(2) 0.09189(16) 0.0194(6) Uani 1 1 d . . . N84 N 0.7047(3) 0.6797(2) 0.42038(17) 0.0238(7) Uani 1 1 d . . . F10 F 0.3692(3) 0.41855(19) 0.39471(14) 0.0430(7) Uani 1 1 d . . . O95 O 0.1656(3) 0.5197(3) 0.35792(17) 0.0364(7) Uani 1 1 d . . . N70 N 0.9231(2) 0.8683(2) 0.13784(15) 0.0142(5) Uani 1 1 d . . . N24 N 0.9689(3) 0.4114(2) 0.24884(18) 0.0209(6) Uani 1 1 d . . . N21 N 0.9229(3) 0.5681(2) 0.30322(15) 0.0154(5) Uani 1 1 d . . . C37 C 1.2485(3) 0.8292(3) 0.29595(18) 0.0179(7) Uani 1 1 d . . . C19 C 0.9374(3) 0.5560(2) 0.37159(18) 0.0174(6) Uani 1 1 d . . . N68 N 1.0192(3) 0.8991(2) 0.01650(16) 0.0176(6) Uani 1 1 d . . . N64 N 1.3814(3) 0.9978(2) 0.04600(17) 0.0216(6) Uani 1 1 d . . . C74 C 0.6445(3) 0.8976(2) 0.11059(18) 0.0167(6) Uani 1 1 d . . . C53 C 0.5744(3) 0.5560(2) 0.11925(17) 0.0142(6) Uani 1 1 d . . . N90 N 0.6462(3) 0.4374(2) 0.33368(15) 0.0167(6) Uani 1 1 d . . . N34 N 1.3832(3) 1.0088(3) 0.46085(17) 0.0252(7) Uani 1 1 d . . . F12 F 0.3129(4) 0.2805(2) 0.43839(14) 0.0553(9) Uani 1 1 d . . . C76 C 0.5307(3) 0.8019(2) 0.18266(19) 0.0170(6) Uani 1 1 d . . . C77 C 0.6291(3) 0.7888(2) 0.21379(17) 0.0148(6) Uani 1 1 d . . . F9 F 0.2917(3) 0.27645(19) 0.32199(13) 0.0539(9) Uani 1 1 d . . . C36 C 1.2974(3) 0.9201(3) 0.34703(18) 0.0169(6) Uani 1 1 d . . . C6 C 1.0283(3) 1.0919(2) 0.26000(17) 0.0148(6) Uani 1 1 d . . . C71 C 0.8552(3) 0.9213(2) 0.12546(16) 0.0134(6) Uani 1 1 d . . . C5 C 0.9809(3) 1.1635(3) 0.25253(19) 0.0203(7) Uani 1 1 d . . . C44 C 1.1067(3) 0.6585(3) 0.00797(19) 0.0186(7) Uani 1 1 d . . . C56 C 0.3764(3) 0.5402(3) 0.14523(19) 0.0235(8) Uani 1 1 d . . . C7 C 0.9843(3) 1.0131(2) 0.30062(17) 0.0148(6) Uani 1 1 d . . . C55 C 0.4773(3) 0.5203(2) 0.15749(17) 0.0163(6) Uani 1 1 d . . . C46 C 0.9098(3) 0.5619(3) -0.03222(18) 0.0174(6) Uani 1 1 d . . . N38 N 1.2738(3) 0.7515(3) 0.3083(2) 0.0305(8) Uani 1 1 d . . . C17 C 0.9947(3) 0.6478(2) 0.42175(18) 0.0191(7) Uani 1 1 d . . . C66 C 1.2064(3) 0.9594(2) 0.09047(18) 0.0144(6) Uani 1 1 d . . . C79 C 0.6202(3) 0.7222(2) 0.26670(17) 0.0148(6) Uani 1 1 d . . . C47 C 0.8914(3) 0.5796(2) 0.03639(17) 0.0145(6) Uani 1 1 d . . . C23 C 0.8679(3) 0.4218(2) 0.23380(17) 0.0157(6) Uani 1 1 d . . . C75 C 0.5381(3) 0.8556(3) 0.12907(19) 0.0176(7) Uani 1 1 d . . . C62 C 1.3742(3) 1.0232(2) 0.16856(19) 0.0183(7) Uani 1 1 d . . . C29 C 0.5888(3) 0.3000(3) 0.12919(19) 0.0186(7) Uani 1 1 d . . . C41 C 1.1663(3) 0.7385(2) 0.13371(18) 0.0156(6) Uani 1 1 d . . . C25 C 0.7748(3) 0.3466(2) 0.18381(17) 0.0153(6) Uani 1 1 d . . . C11 C 1.0531(3) 0.8985(2) 0.40597(18) 0.0158(6) Uani 1 1 d . . . C73 C 0.7380(3) 0.8801(2) 0.14482(17) 0.0132(6) Uani 1 1 d . . . C13 C 1.0447(3) 0.8107(2) 0.43865(18) 0.0184(7) Uani 1 1 d . . . C65 C 1.2676(3) 0.9628(3) 0.03544(19) 0.0180(7) Uani 1 1 d . . . C83 C 0.6892(3) 0.6058(2) 0.37107(18) 0.0169(6) Uani 1 1 d . . . C35 C 1.3484(3) 0.9267(3) 0.4155(2) 0.0228(7) Uani 1 1 d . . . C45 C 1.0190(3) 0.6024(3) -0.04625(19) 0.0200(7) Uani 1 1 d . . . C3 C 1.1111(3) 1.2276(3) 0.18408(19) 0.0192(7) Uani 1 1 d . . . C26 C 0.7892(3) 0.2711(2) 0.14211(18) 0.0172(6) Uani 1 1 d . . . C2 C 1.1592(3) 1.1568(2) 0.19195(19) 0.0186(7) Uani 1 1 d . . . C43 C 1.0787(3) 0.6721(2) 0.07461(18) 0.0150(6) Uani 1 1 d . . . N87 N 0.6204(3) 0.3949(2) 0.46740(17) 0.0275(7) Uani 1 1 d . . . C58 C 0.3136(3) 0.4639(3) 0.2340(2) 0.0268(8) Uani 1 1 d . . . C32 C 1.3174(3) 1.0793(3) 0.36780(19) 0.0204(7) Uani 1 1 d . . . C59 C 0.4144(3) 0.4439(3) 0.24719(19) 0.0212(7) Uani 1 1 d . . . C33 C 1.3689(3) 1.0846(3) 0.4366(2) 0.0239(8) Uani 1 1 d . . . N57 N 0.2940(3) 0.5125(3) 0.18393(18) 0.0283(7) Uani 1 1 d . . . C89 C 0.6231(3) 0.3482(3) 0.3466(2) 0.0222(7) Uani 1 1 d . . . C63 C 1.4344(3) 1.0281(3) 0.1127(2) 0.0199(7) Uani 1 1 d . . . C86 C 0.6444(4) 0.4851(3) 0.4541(2) 0.0245(8) Uani 1 1 d . . . C67 C 1.0789(3) 0.9195(2) 0.08098(17) 0.0134(6) Uani 1 1 d . . . C85 C 0.6591(3) 0.5064(3) 0.38798(18) 0.0193(7) Uani 1 1 d . . . C28 C 0.6064(3) 0.2277(3) 0.08504(19) 0.0197(7) Uani 1 1 d . . . C16 C 1.0330(4) 0.6476(3) 0.4913(2) 0.0318(10) Uani 1 1 d . . . C14 C 1.0864(5) 0.8183(3) 0.5092(2) 0.0346(11) Uani 1 1 d . . . C88 C 0.6105(4) 0.3276(3) 0.4136(2) 0.0260(8) Uani 1 1 d . . . C15 C 1.0800(5) 0.7343(3) 0.5357(2) 0.0428(13) Uani 1 1 d . . . F11 F 0.1829(4) 0.3381(3) 0.3843(3) 0.1034(19) Uani 1 1 d . . . B3 B 0.2880(5) 0.3274(4) 0.3845(3) 0.0328(10) Uani 1 1 d . . . F4 F 0.2177(2) 0.15601(16) 0.04043(12) 0.0279(5) Uani 1 1 d . . . F2 F 0.3890(2) 0.24643(18) 0.01771(12) 0.0288(5) Uani 1 1 d . . . F3 F 0.3251(2) 0.29052(18) 0.11605(12) 0.0310(5) Uani 1 1 d . . . F1 F 0.2405(2) 0.3006(2) 0.00787(16) 0.0428(7) Uani 1 1 d . . . B1 B 0.2934(3) 0.2488(3) 0.0459(2) 0.0191(8) Uani 1 1 d . . . O92 O 0.7959(2) 0.88979(19) 0.43055(14) 0.0214(5) Uani 1 1 d . . . F6 F 0.7570(2) 0.1354(2) 0.32843(15) 0.0390(6) Uani 1 1 d . . . F8 F 0.6062(3) 0.00754(18) 0.27267(14) 0.0444(7) Uani 1 1 d . . . F5 F 0.6269(3) 0.15522(19) 0.24407(15) 0.0425(7) Uani 1 1 d . . . F7 F 0.5785(3) 0.1200(2) 0.34760(18) 0.0486(8) Uani 1 1 d . . . B2 B 0.6425(4) 0.1048(3) 0.2981(2) 0.0230(8) Uani 1 1 d . . . O93 O 0.5890(3) 0.9142(2) 0.39260(18) 0.0309(7) Uani 1 1 d . . . O94 O 0.3927(3) 0.6673(3) 0.39754(17) 0.0347(7) Uani 1 1 d . . . H5 H 1.236(3) 0.936(3) -0.010(2) 0.010(9) Uiso 1 1 d . . . H6 H 1.020(3) 0.453(3) 0.283(2) 0.006(8) Uiso 1 1 d . . . H7 H 1.181(3) 0.686(3) -0.0004(18) 0.004(8) Uiso 1 1 d . . . H8 H 0.224(4) 0.569(3) 0.366(2) 0.012(10) Uiso 1 1 d . . . H9 H 0.954(4) 0.882(3) 0.0105(19) 0.002(8) Uiso 1 1 d . . . H10 H 0.988(4) 0.821(3) 0.312(2) 0.016(10) Uiso 1 1 d . . . H12 H 0.858(4) 0.260(3) 0.147(2) 0.015(10) Uiso 1 1 d . . . H13 H 1.393(4) 1.144(3) 0.469(2) 0.021(11) Uiso 1 1 d . . . H14 H 0.654(3) 0.539(3) 0.494(2) 0.014(10) Uiso 1 1 d . . . H16 H 1.110(4) 0.879(3) 0.539(2) 0.018(10) Uiso 1 1 d . . . H17 H 1.221(4) 1.154(3) 0.170(2) 0.014(10) Uiso 1 1 d . . . H18 H 0.731(4) 0.737(3) 0.414(2) 0.017(10) Uiso 1 1 d . . . H19 H 0.554(4) 0.187(3) 0.049(2) 0.015(10) Uiso 1 1 d . . . H20 H 1.359(4) 0.874(3) 0.433(2) 0.027(12) Uiso 1 1 d . . . H21 H 0.620(4) 0.298(3) 0.313(2) 0.020(11) Uiso 1 1 d . . . H22 H 1.415(3) 1.048(3) 0.219(2) 0.012(9) Uiso 1 1 d . . . H23 H 0.863(4) 1.054(3) 0.333(2) 0.021(11) Uiso 1 1 d . . . H24 H 1.522(4) 1.051(3) 0.121(2) 0.017(10) Uiso 1 1 d . . . H25 H 0.428(4) 0.412(3) 0.284(2) 0.016(10) Uiso 1 1 d . . . H26 H 1.307(4) 1.129(3) 0.354(2) 0.016(10) Uiso 1 1 d . . . H28 H 0.655(3) 0.936(3) 0.075(2) 0.013(9) Uiso 1 1 d . . . H30 H 0.584(4) 0.956(3) 0.427(3) 0.021(11) Uiso 1 1 d . . . H31 H 0.486(4) 0.867(3) 0.105(2) 0.020(11) Uiso 1 1 d . . . H32 H 0.512(4) 0.311(3) 0.122(2) 0.024(11) Uiso 1 1 d . . . H33 H 1.129(4) 1.271(3) 0.156(2) 0.018(10) Uiso 1 1 d . . . H34 H 0.927(4) 0.620(4) 0.298(2) 0.024(12) Uiso 1 1 d . . . H36 H 0.832(4) 0.925(4) 0.468(3) 0.030(13) Uiso 1 1 d . . . H37 H 0.730(5) 0.899(4) 0.424(3) 0.039(14) Uiso 1 1 d . . . H38 H 1.106(5) 0.739(4) 0.582(3) 0.039(14) Uiso 1 1 d . . . H39 H 0.828(5) 0.626(4) 0.146(3) 0.041(14) Uiso 1 1 d . . . H44 H 0.849(4) 0.523(4) -0.069(3) 0.032(13) Uiso 1 1 d . . . H45 H 1.037(4) 0.593(3) -0.095(2) 0.027(12) Uiso 1 1 d . . . H46 H 0.706(5) 0.672(4) 0.466(3) 0.039(14) Uiso 1 1 d . . . H47 H 0.986(4) 0.364(4) 0.238(3) 0.028(12) Uiso 1 1 d . . . H48 H 0.915(4) 1.171(4) 0.273(3) 0.033(13) Uiso 1 1 d . . . H49 H 1.039(5) 0.920(4) -0.016(3) 0.039(15) Uiso 1 1 d . . . H60 H 0.874(4) 0.966(4) 0.364(3) 0.029(12) Uiso 1 1 d . . . H59 H 0.462(5) 0.778(4) 0.197(3) 0.039(14) Uiso 1 1 d . . . H50 H 1.061(5) 0.732(4) 0.195(3) 0.028(13) Uiso 1 1 d . . . H56 H 0.604(5) 0.264(4) 0.424(3) 0.039(14) Uiso 1 1 d . . . H54 H 0.257(4) 0.442(4) 0.267(3) 0.034(13) Uiso 1 1 d . . . H55 H 0.618(5) 0.619(4) 0.043(3) 0.042(15) Uiso 1 1 d . . . H52 H 0.765(4) 0.714(4) 0.261(3) 0.031(13) Uiso 1 1 d . . . H51 H 1.242(5) 0.701(4) 0.278(3) 0.047(16) Uiso 1 1 d . . . H61 H 0.908(5) 0.828(4) 0.165(3) 0.049(17) Uiso 1 1 d . . . H67 H 0.371(5) 0.578(4) 0.109(3) 0.039(14) Uiso 1 1 d . . . H65 H 1.333(5) 0.748(4) 0.343(3) 0.048(16) Uiso 1 1 d . . . H63 H 0.467(8) 0.694(7) 0.384(5) 0.12(3) Uiso 1 1 d . . . H64 H 0.418(6) 0.637(5) 0.438(4) 0.07(2) Uiso 1 1 d . . . H68 H 1.036(6) 0.592(5) 0.505(4) 0.07(2) Uiso 1 1 d . . . H66 H 0.500(6) 0.590(4) 0.043(3) 0.050(18) Uiso 1 1 d . . . H80 H 0.192(6) 0.463(5) 0.385(4) 0.07(2) Uiso 1 1 d . . . H90 H 0.595(8) 0.934(7) 0.367(5) 0.11(4) Uiso 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 0.01032(19) 0.01279(19) 0.0145(2) 0.00506(15) 0.00195(15) 0.00382(15) Ni2 0.0130(2) 0.01254(19) 0.01282(19) 0.00446(15) 0.00422(15) 0.00253(15) F13 0.0140(9) 0.0165(9) 0.0174(9) 0.0058(7) 0.0037(7) 0.0041(7) O72 0.0142(11) 0.0174(11) 0.0184(11) 0.0100(9) 0.0053(9) 0.0035(9) O50 0.0149(12) 0.0195(12) 0.0182(12) 0.0012(9) 0.0026(9) 0.0014(10) O12 0.0262(13) 0.0148(11) 0.0175(12) 0.0037(9) 0.0020(10) 0.0039(10) O20 0.0311(14) 0.0153(12) 0.0200(12) 0.0060(10) -0.0011(11) 0.0050(11) O80 0.0163(12) 0.0222(12) 0.0211(12) 0.0100(10) 0.0084(10) 0.0051(10) N52 0.0100(12) 0.0170(13) 0.0139(13) 0.0054(10) 0.0044(10) 0.0018(10) N1 0.0134(13) 0.0137(13) 0.0170(13) 0.0051(10) 0.0023(10) 0.0046(10) O42 0.0100(11) 0.0237(13) 0.0259(13) 0.0045(10) 0.0042(9) 0.0022(10) N40 0.0126(14) 0.0136(13) 0.0178(14) 0.0036(11) 0.0039(11) 0.0016(11) N48 0.0139(13) 0.0150(13) 0.0160(13) 0.0051(10) 0.0045(10) 0.0044(11) N82 0.0156(13) 0.0128(13) 0.0157(13) 0.0064(10) 0.0054(10) 0.0041(10) N51 0.0100(13) 0.0170(13) 0.0156(13) 0.0050(11) 0.0043(10) 0.0013(11) N69 0.0074(12) 0.0151(13) 0.0165(13) 0.0064(10) 0.0018(10) 0.0023(10) N78 0.0138(13) 0.0138(13) 0.0152(13) 0.0048(10) 0.0033(10) 0.0036(10) N9 0.0156(13) 0.0138(13) 0.0139(13) 0.0072(10) 0.0046(10) 0.0035(11) N81 0.0122(13) 0.0143(13) 0.0159(13) 0.0078(10) 0.0056(11) 0.0033(10) N54 0.0152(15) 0.0279(16) 0.0181(14) 0.0110(12) 0.0047(12) 0.0087(13) N39 0.0122(13) 0.0148(13) 0.0156(13) 0.0054(10) 0.0015(10) 0.0049(10) N61 0.0112(13) 0.0129(13) 0.0213(14) 0.0047(11) 0.0024(11) 0.0027(10) N30 0.0150(13) 0.0161(13) 0.0148(13) 0.0067(10) 0.0047(10) 0.0026(11) N18 0.0171(14) 0.0161(13) 0.0144(13) 0.0044(11) 0.0017(11) 0.0051(11) N22 0.0157(13) 0.0125(13) 0.0143(13) 0.0026(10) 0.0017(10) 0.0029(11) N31 0.0132(13) 0.0189(14) 0.0177(14) 0.0045(11) 0.0020(11) 0.0047(11) N4 0.0248(16) 0.0170(14) 0.0239(15) 0.0093(12) 0.0068(12) 0.0094(12) N60 0.0127(13) 0.0170(13) 0.0157(13) 0.0024(11) 0.0042(10) 0.0006(11) N8 0.0193(15) 0.0201(14) 0.0225(15) 0.0103(12) 0.0099(12) 0.0100(12) C49 0.0138(15) 0.0153(15) 0.0166(15) 0.0069(12) 0.0036(12) 0.0048(12) N10 0.0170(14) 0.0121(13) 0.0146(13) 0.0065(11) 0.0044(11) 0.0036(11) N27 0.0201(15) 0.0157(14) 0.0214(15) 0.0035(11) 0.0050(12) 0.0041(12) N84 0.040(2) 0.0160(15) 0.0146(15) 0.0040(12) 0.0077(13) 0.0068(14) F10 0.0572(18) 0.0306(14) 0.0290(13) -0.0043(11) 0.0156(12) -0.0020(12) O95 0.0262(16) 0.0416(19) 0.0370(17) -0.0009(14) -0.0038(13) 0.0109(15) N70 0.0101(13) 0.0163(13) 0.0173(13) 0.0087(11) 0.0036(10) 0.0032(10) N24 0.0188(15) 0.0166(15) 0.0268(16) -0.0009(12) 0.0001(13) 0.0083(12) N21 0.0181(14) 0.0114(13) 0.0152(13) 0.0042(11) -0.0004(11) 0.0033(11) C37 0.0179(16) 0.0205(17) 0.0181(16) 0.0070(13) 0.0026(13) 0.0089(13) C19 0.0185(16) 0.0166(16) 0.0172(16) 0.0041(13) 0.0014(13) 0.0061(13) N68 0.0105(14) 0.0259(16) 0.0165(14) 0.0091(12) 0.0035(11) 0.0035(12) N64 0.0143(14) 0.0268(16) 0.0282(16) 0.0131(13) 0.0094(12) 0.0077(12) C74 0.0141(15) 0.0183(16) 0.0192(16) 0.0081(13) 0.0053(12) 0.0047(13) C53 0.0129(15) 0.0160(15) 0.0135(15) 0.0026(12) 0.0036(12) 0.0040(12) N90 0.0190(14) 0.0151(13) 0.0173(14) 0.0058(11) 0.0061(11) 0.0050(11) N34 0.0193(15) 0.0355(18) 0.0202(15) 0.0023(13) 0.0006(12) 0.0103(14) F12 0.112(3) 0.0415(16) 0.0217(13) 0.0116(12) 0.0206(15) 0.0321(18) C76 0.0129(15) 0.0160(15) 0.0227(17) 0.0062(13) 0.0076(13) 0.0030(12) C77 0.0149(15) 0.0127(14) 0.0168(15) 0.0042(12) 0.0058(12) 0.0029(12) F9 0.106(3) 0.0226(13) 0.0182(12) 0.0054(10) 0.0062(14) 0.0014(15) C36 0.0123(15) 0.0211(16) 0.0189(16) 0.0065(13) 0.0009(12) 0.0073(13) C6 0.0144(15) 0.0141(15) 0.0154(15) 0.0043(12) 0.0033(12) 0.0032(12) C71 0.0103(14) 0.0167(15) 0.0126(14) 0.0049(12) 0.0017(11) 0.0027(12) C5 0.0226(18) 0.0202(17) 0.0234(17) 0.0091(14) 0.0077(14) 0.0109(14) C44 0.0161(16) 0.0188(16) 0.0220(17) 0.0068(13) 0.0090(13) 0.0039(13) C56 0.0152(16) 0.037(2) 0.0181(17) 0.0063(15) 0.0023(13) 0.0082(15) C7 0.0148(15) 0.0154(15) 0.0128(14) 0.0040(12) 0.0012(12) 0.0027(12) C55 0.0120(15) 0.0197(16) 0.0142(15) 0.0016(12) 0.0028(12) 0.0012(12) C46 0.0152(16) 0.0191(16) 0.0181(16) 0.0041(13) 0.0032(13) 0.0055(13) N38 0.039(2) 0.0234(17) 0.0300(18) 0.0044(14) -0.0098(15) 0.0166(15) C17 0.0234(17) 0.0166(16) 0.0160(16) 0.0046(13) 0.0000(13) 0.0053(13) C66 0.0103(14) 0.0131(14) 0.0214(16) 0.0068(12) 0.0036(12) 0.0043(12) C79 0.0154(15) 0.0136(15) 0.0148(15) 0.0031(12) 0.0035(12) 0.0035(12) C47 0.0128(15) 0.0151(15) 0.0172(15) 0.0063(12) 0.0029(12) 0.0055(12) C23 0.0157(15) 0.0154(15) 0.0152(15) 0.0051(12) 0.0033(12) 0.0029(12) C75 0.0142(16) 0.0187(16) 0.0217(17) 0.0066(13) 0.0025(13) 0.0072(13) C62 0.0124(15) 0.0169(16) 0.0254(18) 0.0069(13) 0.0022(13) 0.0035(13) C29 0.0141(16) 0.0190(16) 0.0199(16) 0.0037(13) 0.0023(13) 0.0017(13) C41 0.0140(15) 0.0148(15) 0.0205(16) 0.0074(12) 0.0038(12) 0.0065(12) C25 0.0146(15) 0.0147(15) 0.0157(15) 0.0062(12) 0.0039(12) 0.0016(12) C11 0.0155(15) 0.0172(16) 0.0163(15) 0.0056(12) 0.0035(12) 0.0063(13) C73 0.0103(14) 0.0150(15) 0.0146(14) 0.0059(12) 0.0040(11) 0.0027(12) C13 0.0226(17) 0.0166(16) 0.0157(16) 0.0070(13) 0.0041(13) 0.0044(13) C65 0.0144(16) 0.0214(17) 0.0217(17) 0.0103(14) 0.0055(13) 0.0075(13) C83 0.0181(16) 0.0183(16) 0.0157(15) 0.0052(12) 0.0034(12) 0.0069(13) C35 0.0192(17) 0.031(2) 0.0205(17) 0.0074(15) 0.0005(14) 0.0113(15) C45 0.0204(17) 0.0222(17) 0.0185(16) 0.0064(13) 0.0087(13) 0.0056(14) C3 0.0204(17) 0.0159(16) 0.0235(17) 0.0090(14) 0.0042(14) 0.0067(13) C26 0.0150(16) 0.0173(16) 0.0198(16) 0.0057(13) 0.0037(13) 0.0047(13) C2 0.0180(16) 0.0168(16) 0.0221(17) 0.0060(13) 0.0067(13) 0.0048(13) C43 0.0112(14) 0.0150(15) 0.0197(16) 0.0052(12) 0.0044(12) 0.0040(12) N87 0.0375(19) 0.0237(16) 0.0205(15) 0.0096(13) 0.0067(14) 0.0061(14) C58 0.0166(17) 0.038(2) 0.0203(18) 0.0018(16) 0.0080(14) 0.0013(16) C32 0.0171(16) 0.0213(17) 0.0217(17) 0.0041(14) 0.0028(13) 0.0046(14) C59 0.0181(17) 0.0250(18) 0.0176(16) 0.0035(14) 0.0072(13) 0.0017(14) C33 0.0183(17) 0.0278(19) 0.0219(18) -0.0012(15) 0.0014(14) 0.0052(15) N57 0.0114(14) 0.050(2) 0.0236(16) 0.0066(15) 0.0058(12) 0.0090(14) C89 0.0284(19) 0.0164(17) 0.0216(17) 0.0042(14) 0.0072(14) 0.0056(14) C63 0.0107(15) 0.0183(16) 0.0331(19) 0.0104(14) 0.0057(14) 0.0051(13) C86 0.030(2) 0.0227(18) 0.0193(17) 0.0052(14) 0.0055(15) 0.0053(15) C67 0.0108(14) 0.0128(14) 0.0182(15) 0.0073(12) 0.0027(12) 0.0046(12) C85 0.0230(17) 0.0177(16) 0.0171(16) 0.0049(13) 0.0046(13) 0.0052(14) C28 0.0185(17) 0.0166(16) 0.0200(17) 0.0024(13) 0.0035(13) 0.0002(13) C16 0.052(3) 0.0188(18) 0.0193(18) 0.0075(15) -0.0063(17) 0.0069(18) C14 0.061(3) 0.0159(18) 0.0163(18) 0.0036(14) -0.0056(18) 0.0030(18) C88 0.032(2) 0.0202(18) 0.0255(19) 0.0106(15) 0.0077(16) 0.0055(16) C15 0.076(4) 0.025(2) 0.0160(19) 0.0073(16) -0.010(2) 0.006(2) F11 0.049(2) 0.066(3) 0.215(6) 0.059(3) 0.047(3) 0.025(2) B3 0.042(3) 0.026(2) 0.031(2) 0.0088(19) 0.012(2) 0.008(2) F4 0.0236(11) 0.0207(11) 0.0320(12) 0.0057(9) -0.0027(9) -0.0009(9) F2 0.0219(11) 0.0409(14) 0.0222(11) 0.0032(10) 0.0035(9) 0.0095(10) F3 0.0218(11) 0.0347(13) 0.0257(12) -0.0033(10) 0.0084(9) -0.0044(10) F1 0.0391(15) 0.0471(16) 0.0582(18) 0.0370(14) 0.0124(13) 0.0250(13) B1 0.0160(18) 0.0197(18) 0.0215(19) 0.0069(15) 0.0018(14) 0.0051(15) O92 0.0227(14) 0.0217(13) 0.0196(13) 0.0039(10) 0.0053(11) 0.0062(11) F6 0.0193(12) 0.0490(16) 0.0460(15) 0.0013(12) -0.0041(11) 0.0133(11) F8 0.068(2) 0.0230(13) 0.0329(14) 0.0002(10) -0.0064(13) 0.0097(13) F5 0.0476(17) 0.0311(14) 0.0423(15) 0.0146(12) -0.0089(12) 0.0070(12) F7 0.0438(17) 0.0399(16) 0.072(2) 0.0144(15) 0.0350(16) 0.0168(13) B2 0.0169(19) 0.025(2) 0.027(2) 0.0030(16) -0.0027(16) 0.0085(16) O93 0.0351(17) 0.0364(17) 0.0234(15) 0.0066(14) 0.0051(13) 0.0143(14) O94 0.0284(16) 0.054(2) 0.0348(16) 0.0257(15) 0.0127(13) 0.0224(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 N9 2.037(3) . ? Ni1 N39 2.046(3) . ? Ni1 N69 2.062(3) . ? Ni1 N61 2.069(3) . ? Ni1 N1 2.110(3) . ? Ni1 N31 2.117(3) . ? Ni2 N82 2.042(3) . ? Ni2 N52 2.050(3) . ? Ni2 N22 2.052(3) . ? Ni2 N30 2.097(3) . ? Ni2 N60 2.105(3) . ? Ni2 N90 2.106(3) . ? O72 C71 1.236(4) . ? O50 C49 1.231(4) . ? O12 C11 1.226(4) . ? O20 C19 1.229(4) . ? O80 C79 1.231(4) . ? N52 C53 1.298(4) . ? N52 N51 1.404(4) . ? N1 C2 1.327(4) . ? N1 C6 1.339(4) . ? O42 C41 1.222(4) . ? N40 C41 1.362(4) . ? N40 N39 1.411(4) . ? N48 C47 1.332(4) . ? N48 C43 1.341(4) . ? N82 C83 1.298(4) . ? N82 N81 1.416(4) . ? N51 C49 1.346(4) . ? N69 C67 1.308(4) . ? N69 N70 1.394(4) . ? N78 C73 1.340(4) . ? N78 C77 1.344(4) . ? N9 C7 1.297(4) . ? N9 N10 1.402(4) . ? N81 C79 1.355(4) . ? N54 C53 1.331(4) . ? N39 C37 1.290(4) . ? N61 C62 1.331(4) . ? N61 C66 1.343(4) . ? N30 C29 1.330(4) . ? N30 C25 1.354(4) . ? N18 C13 1.333(5) . ? N18 C17 1.340(4) . ? N22 C23 1.301(4) . ? N22 N21 1.402(4) . ? N31 C32 1.327(5) . ? N31 C36 1.356(4) . ? N4 C3 1.325(5) . ? N4 C5 1.345(5) . ? N60 C59 1.333(4) . ? N60 C55 1.352(4) . ? N8 C7 1.324(4) . ? C49 C47 1.509(4) . ? N10 C11 1.349(4) . ? N27 C28 1.341(5) . ? N27 C26 1.343(5) . ? N84 C83 1.324(5) . ? F10 B3 1.395(6) . ? N70 C71 1.351(4) . ? N24 C23 1.322(5) . ? N21 C19 1.362(4) . ? C37 N38 1.337(5) . ? C37 C36 1.491(5) . ? C19 C17 1.500(5) . ? N68 C67 1.328(4) . ? N64 C65 1.334(5) . ? N64 C63 1.340(5) . ? C74 C73 1.387(5) . ? C74 C75 1.393(5) . ? C53 C55 1.490(4) . ? N90 C89 1.334(5) . ? N90 C85 1.344(5) . ? N34 C33 1.332(5) . ? N34 C35 1.339(5) . ? F12 B3 1.387(6) . ? C76 C75 1.384(5) . ? C76 C77 1.385(5) . ? C77 C79 1.505(4) . ? F9 B3 1.371(6) . ? C36 C35 1.384(5) . ? C6 C5 1.390(5) . ? C6 C7 1.495(4) . ? C71 C73 1.515(4) . ? C44 C43 1.393(5) . ? C44 C45 1.398(5) . ? C56 N57 1.340(5) . ? C56 C55 1.384(5) . ? C46 C45 1.385(5) . ? C46 C47 1.391(5) . ? C17 C16 1.381(5) . ? C66 C65 1.387(5) . ? C66 C67 1.498(4) . ? C23 C25 1.489(5) . ? C62 C63 1.391(5) . ? C29 C28 1.390(5) . ? C41 C43 1.501(5) . ? C25 C26 1.382(5) . ? C11 C13 1.506(5) . ? C13 C14 1.386(5) . ? C83 C85 1.501(5) . ? C3 C2 1.386(5) . ? N87 C88 1.330(5) . ? N87 C86 1.351(5) . ? C58 N57 1.326(6) . ? C58 C59 1.386(6) . ? C32 C33 1.396(5) . ? C89 C88 1.390(5) . ? C86 C85 1.381(5) . ? C16 C15 1.382(6) . ? C14 C15 1.397(6) . ? F11 B3 1.372(7) . ? F4 B1 1.396(4) . ? F2 B1 1.383(5) . ? F3 B1 1.387(5) . ? F1 B1 1.387(5) . ? F6 B2 1.389(5) . ? F8 B2 1.388(5) . ? F5 B2 1.393(5) . ? F7 B2 1.369(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 N9 Ni1 N39 96.45(11) . . ? N9 Ni1 N69 96.00(11) . . ? N39 Ni1 N69 93.79(11) . . ? N9 Ni1 N61 168.56(11) . . ? N39 Ni1 N61 93.67(11) . . ? N69 Ni1 N61 77.97(11) . . ? N9 Ni1 N1 76.83(11) . . ? N39 Ni1 N1 173.27(11) . . ? N69 Ni1 N1 87.41(11) . . ? N61 Ni1 N1 93.06(11) . . ? N9 Ni1 N31 87.81(11) . . ? N39 Ni1 N31 76.89(11) . . ? N69 Ni1 N31 170.30(11) . . ? N61 Ni1 N31 99.70(11) . . ? N1 Ni1 N31 102.16(11) . . ? N82 Ni2 N52 94.58(11) . . ? N82 Ni2 N22 93.32(11) . . ? N52 Ni2 N22 99.04(11) . . ? N82 Ni2 N30 169.09(11) . . ? N52 Ni2 N30 90.91(11) . . ? N22 Ni2 N30 76.48(11) . . ? N82 Ni2 N60 90.39(11) . . ? N52 Ni2 N60 76.74(11) . . ? N22 Ni2 N60 174.61(11) . . ? N30 Ni2 N60 100.06(11) . . ? N82 Ni2 N90 76.87(11) . . ? N52 Ni2 N90 166.94(11) . . ? N22 Ni2 N90 91.38(11) . . ? N30 Ni2 N90 99.21(11) . . ? N60 Ni2 N90 93.27(11) . . ? C53 N52 N51 116.5(3) . . ? C53 N52 Ni2 119.8(2) . . ? N51 N52 Ni2 123.7(2) . . ? C2 N1 C6 117.7(3) . . ? C2 N1 Ni1 127.2(2) . . ? C6 N1 Ni1 113.9(2) . . ? C41 N40 N39 117.8(3) . . ? C47 N48 C43 118.3(3) . . ? C83 N82 N81 116.1(3) . . ? C83 N82 Ni2 120.3(2) . . ? N81 N82 Ni2 123.3(2) . . ? C49 N51 N52 121.3(3) . . ? C67 N69 N70 118.5(3) . . ? C67 N69 Ni1 117.7(2) . . ? N70 N69 Ni1 123.0(2) . . ? C73 N78 C77 116.9(3) . . ? C7 N9 N10 116.5(3) . . ? C7 N9 Ni1 119.8(2) . . ? N10 N9 Ni1 123.8(2) . . ? C79 N81 N82 116.4(3) . . ? C37 N39 N40 115.9(3) . . ? C37 N39 Ni1 119.8(2) . . ? N40 N39 Ni1 124.2(2) . . ? C62 N61 C66 118.0(3) . . ? C62 N61 Ni1 126.8(2) . . ? C66 N61 Ni1 114.8(2) . . ? C29 N30 C25 117.0(3) . . ? C29 N30 Ni2 127.0(2) . . ? C25 N30 Ni2 115.2(2) . . ? C13 N18 C17 117.8(3) . . ? C23 N22 N21 115.3(3) . . ? C23 N22 Ni2 119.4(2) . . ? N21 N22 Ni2 123.2(2) . . ? C32 N31 C36 117.7(3) . . ? C32 N31 Ni1 126.2(2) . . ? C36 N31 Ni1 113.2(2) . . ? C3 N4 C5 117.1(3) . . ? C59 N60 C55 116.4(3) . . ? C59 N60 Ni2 127.3(3) . . ? C55 N60 Ni2 114.2(2) . . ? O50 C49 N51 125.2(3) . . ? O50 C49 C47 122.4(3) . . ? N51 C49 C47 112.4(3) . . ? C11 N10 N9 118.7(3) . . ? C28 N27 C26 115.8(3) . . ? C71 N70 N69 121.0(3) . . ? C19 N21 N22 118.5(3) . . ? N39 C37 N38 125.9(3) . . ? N39 C37 C36 113.4(3) . . ? N38 C37 C36 120.7(3) . . ? O20 C19 N21 123.7(3) . . ? O20 C19 C17 122.8(3) . . ? N21 C19 C17 113.5(3) . . ? C65 N64 C63 116.8(3) . . ? C73 C74 C75 118.3(3) . . ? N52 C53 N54 127.5(3) . . ? N52 C53 C55 113.1(3) . . ? N54 C53 C55 119.4(3) . . ? C89 N90 C85 117.5(3) . . ? C89 N90 Ni2 127.7(2) . . ? C85 N90 Ni2 114.7(2) . . ? C33 N34 C35 116.9(3) . . ? C75 C76 C77 118.4(3) . . ? N78 C77 C76 123.7(3) . . ? N78 C77 C79 117.0(3) . . ? C76 C77 C79 118.9(3) . . ? N31 C36 C35 120.7(3) . . ? N31 C36 C37 114.9(3) . . ? C35 C36 C37 124.2(3) . . ? N1 C6 C5 120.8(3) . . ? N1 C6 C7 115.4(3) . . ? C5 C6 C7 123.8(3) . . ? O72 C71 N70 124.4(3) . . ? O72 C71 C73 122.3(3) . . ? N70 C71 C73 113.3(3) . . ? N4 C5 C6 121.2(3) . . ? C43 C44 C45 117.4(3) . . ? N57 C56 C55 121.8(4) . . ? N9 C7 N8 126.9(3) . . ? N9 C7 C6 113.0(3) . . ? N8 C7 C6 120.1(3) . . ? N60 C55 C56 121.4(3) . . ? N60 C55 C53 115.0(3) . . ? C56 C55 C53 123.4(3) . . ? C45 C46 C47 117.9(3) . . ? N18 C17 C16 123.5(3) . . ? N18 C17 C19 115.6(3) . . ? C16 C17 C19 120.9(3) . . ? N61 C66 C65 120.7(3) . . ? N61 C66 C67 115.6(3) . . ? C65 C66 C67 123.6(3) . . ? O80 C79 N81 123.1(3) . . ? O80 C79 C77 121.8(3) . . ? N81 C79 C77 115.0(3) . . ? N48 C47 C46 123.3(3) . . ? N48 C47 C49 115.5(3) . . ? C46 C47 C49 121.2(3) . . ? N22 C23 N24 127.2(3) . . ? N22 C23 C25 112.8(3) . . ? N24 C23 C25 119.9(3) . . ? C76 C75 C74 118.9(3) . . ? N61 C62 C63 120.6(3) . . ? N30 C29 C28 121.8(3) . . ? O42 C41 N40 124.1(3) . . ? O42 C41 C43 122.4(3) . . ? N40 C41 C43 113.6(3) . . ? N30 C25 C26 120.6(3) . . ? N30 C25 C23 114.7(3) . . ? C26 C25 C23 124.6(3) . . ? O12 C11 N10 123.8(3) . . ? O12 C11 C13 122.9(3) . . ? N10 C11 C13 113.3(3) . . ? N78 C73 C74 123.7(3) . . ? N78 C73 C71 115.6(3) . . ? C74 C73 C71 120.7(3) . . ? N18 C13 C14 123.2(3) . . ? N18 C13 C11 115.9(3) . . ? C14 C13 C11 120.7(3) . . ? N64 C65 C66 121.9(3) . . ? N82 C83 N84 126.4(3) . . ? N82 C83 C85 112.8(3) . . ? N84 C83 C85 120.8(3) . . ? N34 C35 C36 121.8(4) . . ? C46 C45 C44 119.9(3) . . ? N4 C3 C2 121.8(3) . . ? N27 C26 C25 122.8(3) . . ? N1 C2 C3 121.4(3) . . ? N48 C43 C44 123.2(3) . . ? N48 C43 C41 116.5(3) . . ? C44 C43 C41 120.1(3) . . ? C88 N87 C86 116.7(3) . . ? N57 C58 C59 122.4(3) . . ? N31 C32 C33 120.7(4) . . ? N60 C59 C58 121.6(4) . . ? N34 C33 C32 122.2(4) . . ? C58 N57 C56 116.5(3) . . ? N90 C89 C88 121.0(3) . . ? N64 C63 C62 121.9(3) . . ? N87 C86 C85 121.6(4) . . ? N69 C67 N68 128.1(3) . . ? N69 C67 C66 113.1(3) . . ? N68 C67 C66 118.8(3) . . ? N90 C85 C86 121.1(3) . . ? N90 C85 C83 115.3(3) . . ? C86 C85 C83 123.5(3) . . ? N27 C28 C29 121.9(3) . . ? C17 C16 C15 118.2(4) . . ? C13 C14 C15 118.0(4) . . ? N87 C88 C89 122.1(4) . . ? C16 C15 C14 119.3(4) . . ? F9 B3 F11 110.7(5) . . ? F9 B3 F12 108.6(4) . . ? F11 B3 F12 111.0(4) . . ? F9 B3 F10 109.9(4) . . ? F11 B3 F10 107.6(4) . . ? F12 B3 F10 109.0(4) . . ? F2 B1 F1 108.2(3) . . ? F2 B1 F3 109.9(3) . . ? F1 B1 F3 110.7(3) . . ? F2 B1 F4 109.8(3) . . ? F1 B1 F4 109.0(3) . . ? F3 B1 F4 109.2(3) . . ? F7 B2 F8 108.2(4) . . ? F7 B2 F6 109.6(4) . . ? F8 B2 F6 109.6(3) . . ? F7 B2 F5 108.9(3) . . ? F8 B2 F5 110.4(3) . . ? F6 B2 F5 110.1(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.953 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.086