Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'D.Fenton' 'Harry Adams' 'Scott Clunas' 'Sharon E. Spey' _publ_contact_author_name 'Prof D Fenton' _publ_contact_author_address ; Chemistry Department The University of Sheffield Dainton Building Brook Hill Sheffield S3 7H U.K. ; _publ_contact_author_email 'D.FENTON@SHEFFIELD.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Dinuclear Nickel(II) Complexes of Reduced Asymmetric Compartmental Ligands ; data_ifn227a _database_code_CSD 194355 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H70 B N4 Ni2 O9' _chemical_formula_weight 1035.36 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' 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 11.2426(17) _cell_length_b 13.318(2) _cell_length_c 18.752(3) _cell_angle_alpha 71.951(3) _cell_angle_beta 82.185(3) _cell_angle_gamma 88.779(3) _cell_volume 2644.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 82 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.7186 _exptl_absorpt_correction_T_max 0.8739 _exptl_absorpt_process_details sadabs _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16878 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.1029 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.27 _reflns_number_total 11960 _reflns_number_gt 6036 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1325P)^2^+0.0000P] 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 11960 _refine_ls_number_parameters 673 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1452 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.2507 _refine_ls_wR_factor_gt 0.2128 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.25305(6) 0.62679(5) 0.30317(4) 0.0502(2) Uani 1 1 d . A . Ni2 Ni 0.08140(8) 0.81992(6) 0.34818(4) 0.0690(3) Uani 1 1 d D . . O1 O 0.1930(3) 0.7762(3) 0.27028(19) 0.0516(8) Uani 1 1 d . A . O2 O -0.0258(4) 0.6925(4) 0.3707(2) 0.0749(12) Uani 1 1 d . A . O3 O 0.0969(4) 0.5561(3) 0.36951(19) 0.0570(9) Uani 1 1 d . . . O4 O 0.1752(5) 0.7463(4) 0.4349(2) 0.0897(15) Uani 1 1 d . A . O5 O 0.3200(4) 0.6553(3) 0.3928(2) 0.0711(12) Uani 1 1 d . . . O6 O 0.3306(4) 0.4737(3) 0.3365(2) 0.0753(12) Uani 1 1 d . . . O7 O -0.0417(7) 0.8301(5) 0.4593(3) 0.122(2) Uani 1 1 d . A . N1 N -0.0243(4) 0.9108(4) 0.2666(2) 0.0610(12) Uani 1 1 d . A . N3 N 0.2038(3) 0.5985(3) 0.2088(2) 0.0409(9) Uani 1 1 d . . . N4 N 0.4144(4) 0.6730(3) 0.2307(3) 0.0600(12) Uani 1 1 d . . . B1 B 0.6857(4) 0.2984(4) 0.1881(3) 0.0393(11) Uani 1 1 d . . . C1 C 0.2133(4) 0.8333(4) 0.1964(3) 0.0447(11) Uani 1 1 d . . . C2 C 0.3286(4) 0.8428(4) 0.1573(3) 0.0542(13) Uani 1 1 d . A . C3 C 0.3505(5) 0.9030(4) 0.0807(3) 0.0559(13) Uani 1 1 d . . . H3A H 0.4295 0.9072 0.0542 0.067 Uiso 1 1 calc R A . C4 C 0.2582(5) 0.9572(4) 0.0424(3) 0.0485(12) Uani 1 1 d . A . C5 C 0.1440(4) 0.9475(4) 0.0830(3) 0.0445(11) Uani 1 1 d . . . H5A H 0.0804 0.9849 0.0586 0.053 Uiso 1 1 calc R A . C6 C 0.1191(4) 0.8844(4) 0.1590(3) 0.0432(11) Uani 1 1 d . A . C7 C -0.0067(4) 0.8719(4) 0.1989(3) 0.0486(12) Uani 1 1 d . . . H7A H -0.0306 0.7962 0.2154 0.058 Uiso 1 1 calc R A . H7B H -0.0608 0.9107 0.1627 0.058 Uiso 1 1 calc R . . C8 C 0.0166(6) 1.0242(4) 0.2456(3) 0.0639(15) Uani 1 1 d D . . H8A H -0.0495 1.0708 0.2265 0.077 Uiso 0.612(9) 1 calc PR A 1 H8B H 0.0852 1.0383 0.2045 0.077 Uiso 0.612(9) 1 calc PR A 1 H8C H -0.0291 1.0580 0.2807 0.077 Uiso 0.388(9) 1 d PR A 2 H8D H -0.0010 1.0621 0.1938 0.077 Uiso 0.388(9) 1 d PR A 2 C9A C 0.0538(10) 1.0493(8) 0.3126(5) 0.070(2) Uani 0.612(9) 1 d PDU A 1 H9AA H -0.0134 1.0360 0.3546 0.084 Uiso 0.612(9) 1 calc PR A 1 H9AB H 0.0815 1.1238 0.2985 0.084 Uiso 0.612(9) 1 calc PR A 1 C20A C 0.2717(12) 0.9963(14) 0.2889(9) 0.110(4) Uiso 0.612(9) 1 d PDU A 1 H20A H 0.3002 1.0658 0.2879 0.165 Uiso 0.612(9) 1 calc PR A 1 H20B H 0.2628 0.9974 0.2374 0.165 Uiso 0.612(9) 1 calc PR A 1 H20C H 0.3300 0.9428 0.3093 0.165 Uiso 0.612(9) 1 calc PR A 1 N2A N 0.1598(9) 0.9713(5) 0.3353(4) 0.108(3) Uani 0.612(9) 1 d PDU A 1 C9B C 0.1484(9) 1.0313(12) 0.2517(8) 0.071(3) Uani 0.388(9) 1 d PDU A 2 H9BA H 0.1739 1.1061 0.2395 0.085 Uiso 0.388(9) 1 calc PR A 2 H9BB H 0.1965 1.0007 0.2155 0.085 Uiso 0.388(9) 1 calc PR A 2 N2B N 0.1688(16) 0.9679(7) 0.3355(4) 0.108(3) Uani 0.388(9) 1 d PDU A 2 C20B C 0.2937(17) 0.963(2) 0.3139(16) 0.114(5) Uiso 0.388(9) 1 d PDU A 2 H20D H 0.3304 1.0333 0.3007 0.171 Uiso 0.388(9) 1 calc PR A 2 H20E H 0.3077 0.9368 0.2700 0.171 Uiso 0.388(9) 1 calc PR A 2 H20F H 0.3295 0.9146 0.3561 0.171 Uiso 0.388(9) 1 calc PR A 2 C10 C 0.0908(4) 0.5833(3) 0.1968(3) 0.0405(10) Uani 1 1 d . A . H10A H 0.0274 0.5766 0.2372 0.049 Uiso 1 1 calc R . . C11 C 0.0627(4) 0.5770(4) 0.1290(3) 0.0436(11) Uani 1 1 d . . . H11A H -0.0178 0.5654 0.1226 0.052 Uiso 1 1 calc R A . C12 C 0.1559(5) 0.5881(4) 0.0704(3) 0.0509(12) Uani 1 1 d . A . H12A H 0.1406 0.5833 0.0229 0.061 Uiso 1 1 calc R . . C13 C 0.2696(5) 0.6058(4) 0.0816(3) 0.0539(13) Uani 1 1 d . . . H13A H 0.3337 0.6160 0.0412 0.065 Uiso 1 1 calc R A . C14 C 0.2921(4) 0.6090(4) 0.1515(3) 0.0490(12) Uani 1 1 d . A . C15 C 0.4171(5) 0.6245(5) 0.1697(4) 0.0694(18) Uani 1 1 d . A . H15A H 0.4560 0.5551 0.1850 0.083 Uiso 1 1 calc R . . H15B H 0.4661 0.6700 0.1235 0.083 Uiso 1 1 calc R . . C16 C 0.4316(5) 0.7897(4) 0.1986(4) 0.0694(17) Uani 1 1 d . A . H16A H 0.5074 0.8059 0.1631 0.083 Uiso 1 1 calc R . . H16B H 0.4394 0.8193 0.2402 0.083 Uiso 1 1 calc R . . C17 C 0.2822(5) 1.0270(4) -0.0391(3) 0.0602(14) Uani 1 1 d . . . H17A H 0.2069 1.0579 -0.0557 0.090 Uiso 1 1 calc R A . H17B H 0.3156 0.9846 -0.0712 0.090 Uiso 1 1 calc R . . H17C H 0.3396 1.0835 -0.0433 0.090 Uiso 1 1 calc R . . C18 C -0.1517(6) 0.8983(6) 0.3002(3) 0.0780(19) Uani 1 1 d . . . H18A H -0.1614 0.9303 0.3417 0.094 Uiso 1 1 calc R A . H18B H -0.1699 0.8218 0.3234 0.094 Uiso 1 1 calc R . . C19 C -0.2466(5) 0.9450(5) 0.2483(3) 0.0761(18) Uani 1 1 d . A . H19A H -0.3268 0.9305 0.2778 0.114 Uiso 1 1 calc R . . H19B H -0.2408 0.9129 0.2075 0.114 Uiso 1 1 calc R . . H19C H -0.2330 1.0215 0.2265 0.114 Uiso 1 1 calc R . . C21 C 0.1688(9) 0.9949(8) 0.4057(7) 0.156(5) Uani 1 1 d D . . H21A H 0.2056 1.0653 0.3938 0.234 Uiso 1 1 calc R A 1 H21B H 0.2186 0.9421 0.4365 0.234 Uiso 1 1 calc R A 1 H21C H 0.0884 0.9930 0.4339 0.234 Uiso 1 1 calc R A 1 C22 C -0.0045(6) 0.5970(5) 0.3869(3) 0.0648(16) Uani 1 1 d . A . C23 C -0.1068(6) 0.5209(7) 0.4301(5) 0.107(3) Uani 1 1 d . . . H23A H -0.1779 0.5608 0.4403 0.161 Uiso 1 1 calc R A . H23B H -0.0833 0.4761 0.4781 0.161 Uiso 1 1 calc R . . H23C H -0.1254 0.4765 0.3998 0.161 Uiso 1 1 calc R . . C24 C 0.2678(7) 0.6981(5) 0.4406(4) 0.0780(19) Uani 1 1 d . A . C25 C 0.3308(9) 0.6851(7) 0.5095(5) 0.120(3) Uani 1 1 d . . . H25A H 0.2849 0.7200 0.5430 0.180 Uiso 1 1 calc R A . H25B H 0.4116 0.7171 0.4932 0.180 Uiso 1 1 calc R . . H25C H 0.3367 0.6098 0.5367 0.180 Uiso 1 1 calc R . . C26 C -0.1756(12) 0.8115(11) 0.4872(6) 0.172(5) Uani 1 1 d . . . H26A H -0.1943 0.8264 0.5355 0.258 Uiso 1 1 calc R A . H26B H -0.1972 0.7379 0.4943 0.258 Uiso 1 1 calc R . . H26C H -0.2214 0.8584 0.4498 0.258 Uiso 1 1 calc R . . C27 C 0.3804(7) 0.4260(6) 0.4030(4) 0.096(2) Uani 1 1 d . A . H27A H 0.4087 0.3557 0.4033 0.144 Uiso 1 1 calc R . . H27B H 0.3193 0.4192 0.4469 0.144 Uiso 1 1 calc R . . H27C H 0.4481 0.4695 0.4054 0.144 Uiso 1 1 calc R . . C28 C 0.6943(4) 0.4208(4) 0.1916(3) 0.0428(11) Uani 1 1 d . . . C29 C 0.7291(4) 0.5068(4) 0.1267(3) 0.0469(11) Uani 1 1 d . . . H29A H 0.7445 0.4940 0.0792 0.056 Uiso 1 1 calc R . . C30 C 0.7422(4) 0.6087(4) 0.1281(4) 0.0620(15) Uani 1 1 d . . . H30A H 0.7642 0.6640 0.0822 0.074 Uiso 1 1 calc R . . C31 C 0.7236(5) 0.6308(5) 0.1953(5) 0.0721(19) Uani 1 1 d . . . H31A H 0.7345 0.7008 0.1965 0.086 Uiso 1 1 calc R . . C32 C 0.6891(5) 0.5506(6) 0.2609(4) 0.0731(19) Uani 1 1 d . . . H32A H 0.6754 0.5653 0.3077 0.088 Uiso 1 1 calc R . . C33 C 0.6737(5) 0.4462(5) 0.2595(3) 0.0574(14) Uani 1 1 d . . . H33A H 0.6489 0.3920 0.3056 0.069 Uiso 1 1 calc R . . C34 C 0.6677(5) 0.2167(4) 0.2743(3) 0.0517(12) Uani 1 1 d . . . C35 C 0.5535(7) 0.1871(7) 0.3151(3) 0.098(3) Uani 1 1 d . . . H35A H 0.4851 0.2114 0.2904 0.118 Uiso 1 1 calc R . . C36 C 0.5360(9) 0.1228(9) 0.3912(4) 0.131(4) Uani 1 1 d . . . H36A H 0.4572 0.1056 0.4176 0.157 Uiso 1 1 calc R . . C37 C 0.6335(11) 0.0854(7) 0.4265(4) 0.120(3) Uani 1 1 d . . . H37A H 0.6223 0.0412 0.4777 0.144 Uiso 1 1 calc R . . C38 C 0.7484(8) 0.1111(6) 0.3889(4) 0.093(2) Uani 1 1 d . . . H38A H 0.8163 0.0844 0.4133 0.112 Uiso 1 1 calc R . . C39 C 0.7621(6) 0.1767(5) 0.3146(3) 0.0652(16) Uani 1 1 d . . . H39A H 0.8415 0.1956 0.2896 0.078 Uiso 1 1 calc R . . C40 C 0.8123(4) 0.2738(3) 0.1405(2) 0.0369(10) Uani 1 1 d . . . C41 C 0.9227(4) 0.3169(4) 0.1452(3) 0.0442(11) Uani 1 1 d . . . H41A H 0.9238 0.3620 0.1758 0.053 Uiso 1 1 calc R . . C42 C 1.0315(4) 0.2961(4) 0.1067(3) 0.0511(12) Uani 1 1 d . . . H42A H 1.1044 0.3269 0.1113 0.061 Uiso 1 1 calc R . . C43 C 1.0324(4) 0.2310(4) 0.0623(3) 0.0509(12) Uani 1 1 d . . . H43A H 1.1060 0.2164 0.0362 0.061 Uiso 1 1 calc R . . C44 C 0.9266(4) 0.1875(4) 0.0558(3) 0.0463(11) Uani 1 1 d . . . H44A H 0.9267 0.1419 0.0255 0.056 Uiso 1 1 calc R . . C45 C 0.8184(4) 0.2101(3) 0.0938(2) 0.0389(10) Uani 1 1 d . . . H45A H 0.7459 0.1807 0.0873 0.047 Uiso 1 1 calc R . . C46 C 0.5720(4) 0.2838(4) 0.1443(2) 0.0396(10) Uani 1 1 d . . . C47 C 0.5330(4) 0.1807(4) 0.1489(3) 0.0497(12) Uani 1 1 d . . . H47A H 0.5692 0.1212 0.1804 0.060 Uiso 1 1 calc R . . C48 C 0.4444(5) 0.1642(5) 0.1092(4) 0.0605(14) Uani 1 1 d . . . H48A H 0.4211 0.0941 0.1136 0.073 Uiso 1 1 calc R . . C49 C 0.3887(5) 0.2499(5) 0.0625(3) 0.0630(15) Uani 1 1 d . . . H49A H 0.3284 0.2388 0.0346 0.076 Uiso 1 1 calc R . . C50 C 0.4228(4) 0.3493(4) 0.0578(3) 0.0536(13) Uani 1 1 d . . . H50A H 0.3855 0.4082 0.0266 0.064 Uiso 1 1 calc R . . C51 C 0.5111(4) 0.3661(4) 0.0980(3) 0.0431(11) Uani 1 1 d . . . H51A H 0.5312 0.4367 0.0939 0.052 Uiso 1 1 calc R . . O1S O 0.0612(7) 0.3477(5) 0.3894(4) 0.064(2) Uani 0.577(7) 1 d PD B 1 H1S H 0.0765 0.4126 0.3783 0.096 Uiso 0.577(7) 1 calc PR B 1 C1S C -0.0195(14) 0.3329(10) 0.3480(7) 0.114(6) Uani 0.577(7) 1 d PD B 1 H1S1 H -0.0608 0.2646 0.3733 0.171 Uiso 0.577(7) 1 calc PR B 1 H1S2 H 0.0209 0.3338 0.2981 0.171 Uiso 0.577(7) 1 calc PR B 1 H1S3 H -0.0781 0.3895 0.3420 0.171 Uiso 0.577(7) 1 calc PR B 1 O2S O 0.5549(8) 0.6249(9) 0.4027(6) 0.082(4) Uani 0.423(7) 1 d PD B 2 H2S H 0.5776 0.5838 0.4421 0.123 Uiso 0.423(7) 1 calc PR B 2 C2S C 0.6033(12) 0.7199(10) 0.3884(8) 0.068(4) Uani 0.423(7) 1 d PD B 2 H2S1 H 0.5714 0.7498 0.4285 0.102 Uiso 0.423(7) 1 calc PR B 2 H2S2 H 0.5837 0.7659 0.3396 0.102 Uiso 0.423(7) 1 calc PR B 2 H2S3 H 0.6907 0.7146 0.3864 0.102 Uiso 0.423(7) 1 calc PR B 2 O3S O 0.2637(12) 0.3212(8) 0.2380(7) 0.235(5) Uani 1 1 d D . . H3SH H 0.2759 0.2688 0.2213 0.353 Uiso 0.506(11) 1 d PR C 1 H3SG H 0.2152 0.3653 0.2150 0.353 Uiso 0.494(11) 1 d PR C 2 C3SA C 0.3615(11) 0.3620(10) 0.2542(7) 0.064(2) Uani 0.506(11) 1 d PDU C 1 H3SA H 0.4146 0.3962 0.2072 0.096 Uiso 0.506(11) 1 calc PR C 1 H3SB H 0.4044 0.3053 0.2872 0.096 Uiso 0.506(11) 1 calc PR C 1 H3SC H 0.3367 0.4142 0.2801 0.096 Uiso 0.506(11) 1 calc PR C 1 C3SB C 0.2490(11) 0.2982(10) 0.3138(6) 0.064(2) Uani 0.494(11) 1 d PDU C 2 H3SD H 0.1730 0.2588 0.3353 0.097 Uiso 0.494(11) 1 calc PR C 2 H3SE H 0.2475 0.3638 0.3271 0.097 Uiso 0.494(11) 1 calc PR C 2 H3SF H 0.3156 0.2551 0.3342 0.097 Uiso 0.494(11) 1 calc PR C 2 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 0.0483(4) 0.0464(4) 0.0533(4) -0.0030(3) -0.0276(3) 0.0017(3) Ni2 0.1049(7) 0.0632(5) 0.0462(4) -0.0163(3) -0.0407(4) 0.0217(4) O1 0.056(2) 0.0494(19) 0.048(2) -0.0063(15) -0.0246(16) 0.0026(16) O2 0.089(3) 0.080(3) 0.044(2) -0.002(2) -0.007(2) 0.009(2) O3 0.071(3) 0.054(2) 0.0403(19) -0.0019(16) -0.0176(17) -0.0069(18) O4 0.146(4) 0.070(3) 0.066(3) -0.019(2) -0.068(3) 0.038(3) O5 0.074(3) 0.064(2) 0.076(3) -0.007(2) -0.050(2) 0.005(2) O6 0.084(3) 0.064(2) 0.071(3) 0.001(2) -0.041(2) 0.018(2) O7 0.181(6) 0.122(4) 0.072(3) -0.036(3) -0.050(4) 0.076(4) N1 0.073(3) 0.073(3) 0.037(2) -0.013(2) -0.018(2) 0.019(2) N3 0.0317(19) 0.039(2) 0.045(2) -0.0025(16) -0.0070(16) 0.0038(15) N4 0.044(2) 0.053(3) 0.080(3) -0.008(2) -0.027(2) 0.0020(19) B1 0.035(3) 0.045(3) 0.034(3) -0.007(2) -0.004(2) 0.006(2) C1 0.047(3) 0.038(2) 0.049(3) -0.006(2) -0.021(2) -0.001(2) C2 0.047(3) 0.044(3) 0.067(3) -0.002(2) -0.027(2) -0.006(2) C3 0.040(3) 0.051(3) 0.074(4) -0.011(3) -0.015(2) -0.007(2) C4 0.056(3) 0.040(3) 0.047(3) -0.006(2) -0.014(2) -0.009(2) C5 0.052(3) 0.041(2) 0.044(3) -0.013(2) -0.021(2) 0.008(2) C6 0.052(3) 0.042(3) 0.040(2) -0.013(2) -0.022(2) 0.005(2) C7 0.055(3) 0.056(3) 0.035(2) -0.012(2) -0.015(2) 0.010(2) C8 0.094(4) 0.049(3) 0.053(3) -0.015(3) -0.029(3) 0.027(3) C9A 0.090(6) 0.061(5) 0.071(5) -0.026(4) -0.039(5) 0.030(5) N2A 0.180(7) 0.055(3) 0.116(5) -0.028(4) -0.112(5) 0.033(4) C9B 0.093(7) 0.060(5) 0.072(6) -0.027(5) -0.041(5) 0.028(5) N2B 0.180(7) 0.055(4) 0.116(5) -0.028(4) -0.113(6) 0.033(4) C10 0.038(2) 0.039(2) 0.041(3) -0.0074(19) -0.0088(19) 0.0030(19) C11 0.043(3) 0.041(2) 0.047(3) -0.011(2) -0.013(2) 0.005(2) C12 0.067(3) 0.045(3) 0.042(3) -0.013(2) -0.010(2) 0.012(2) C13 0.050(3) 0.052(3) 0.051(3) -0.008(2) 0.003(2) 0.013(2) C14 0.046(3) 0.038(3) 0.055(3) -0.002(2) -0.010(2) 0.008(2) C15 0.034(3) 0.065(4) 0.088(4) 0.006(3) -0.008(3) 0.012(2) C16 0.048(3) 0.060(3) 0.086(4) 0.008(3) -0.030(3) -0.016(3) C17 0.065(3) 0.055(3) 0.053(3) -0.004(3) -0.011(3) -0.006(3) C18 0.075(4) 0.109(5) 0.042(3) -0.011(3) -0.011(3) 0.028(4) C19 0.067(4) 0.092(5) 0.058(4) -0.007(3) -0.009(3) 0.026(3) C21 0.133(8) 0.151(9) 0.252(14) -0.150(10) -0.060(8) 0.037(7) C22 0.074(4) 0.080(4) 0.033(3) 0.000(3) -0.022(3) -0.010(3) C23 0.076(5) 0.115(6) 0.093(5) 0.027(5) -0.015(4) -0.028(4) C24 0.113(6) 0.062(4) 0.076(4) -0.027(3) -0.056(4) 0.004(4) C25 0.168(8) 0.111(6) 0.101(6) -0.028(5) -0.102(6) 0.017(6) C26 0.175(12) 0.229(14) 0.086(7) -0.020(8) 0.000(7) 0.022(10) C27 0.121(6) 0.080(5) 0.089(5) -0.011(4) -0.058(5) 0.033(4) C28 0.032(2) 0.051(3) 0.049(3) -0.018(2) -0.0130(19) 0.012(2) C29 0.034(2) 0.048(3) 0.058(3) -0.015(2) -0.004(2) 0.004(2) C30 0.033(3) 0.053(3) 0.101(5) -0.022(3) -0.015(3) 0.005(2) C31 0.045(3) 0.066(4) 0.130(6) -0.055(4) -0.041(3) 0.022(3) C32 0.069(4) 0.095(5) 0.088(5) -0.062(4) -0.049(3) 0.045(4) C33 0.057(3) 0.071(4) 0.057(3) -0.032(3) -0.029(3) 0.028(3) C34 0.056(3) 0.056(3) 0.037(3) -0.009(2) -0.001(2) 0.004(2) C35 0.081(5) 0.149(7) 0.042(3) 0.002(4) 0.001(3) -0.040(5) C36 0.126(7) 0.186(10) 0.051(4) 0.004(5) 0.004(5) -0.083(7) C37 0.182(10) 0.114(7) 0.040(4) 0.014(4) -0.017(5) -0.027(6) C38 0.130(7) 0.089(5) 0.044(4) 0.002(3) -0.017(4) 0.029(5) C39 0.085(4) 0.066(4) 0.034(3) -0.004(2) -0.006(3) 0.029(3) C40 0.037(2) 0.035(2) 0.035(2) -0.0033(18) -0.0108(18) 0.0054(18) C41 0.038(2) 0.044(3) 0.052(3) -0.015(2) -0.010(2) 0.005(2) C42 0.031(2) 0.051(3) 0.069(3) -0.012(3) -0.014(2) 0.001(2) C43 0.039(3) 0.053(3) 0.057(3) -0.015(2) -0.003(2) 0.008(2) C44 0.049(3) 0.047(3) 0.043(3) -0.014(2) -0.011(2) 0.008(2) C45 0.041(2) 0.040(2) 0.035(2) -0.0073(19) -0.0110(18) 0.0020(19) C46 0.030(2) 0.044(2) 0.040(2) -0.008(2) -0.0009(18) 0.0000(18) C47 0.042(3) 0.043(3) 0.059(3) -0.010(2) -0.003(2) 0.000(2) C48 0.043(3) 0.057(3) 0.086(4) -0.028(3) -0.008(3) -0.003(2) C49 0.044(3) 0.081(4) 0.073(4) -0.034(3) -0.016(3) -0.004(3) C50 0.047(3) 0.062(3) 0.047(3) -0.008(2) -0.014(2) 0.003(2) C51 0.041(2) 0.043(2) 0.043(3) -0.008(2) -0.006(2) 0.000(2) O1S 0.094(5) 0.040(3) 0.060(4) -0.013(3) -0.023(4) 0.008(3) C1S 0.202(17) 0.076(8) 0.067(8) -0.025(7) -0.017(9) -0.046(9) O2S 0.042(5) 0.140(10) 0.080(7) -0.058(7) -0.002(5) -0.010(6) C2S 0.054(8) 0.065(9) 0.068(9) -0.001(7) 0.009(7) -0.025(7) O3S 0.265(14) 0.191(9) 0.224(12) -0.060(9) 0.040(10) 0.022(9) C3SA 0.073(6) 0.070(6) 0.055(5) -0.024(4) -0.016(4) 0.006(5) C3SB 0.073(6) 0.073(6) 0.052(5) -0.022(4) -0.018(4) 0.003(5) _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. The atoms N2, C9 and C20 were found to be disordered and refined with a 61.5 : 38.5 % occupancy. The two methanol molecules were also found to be disordered and refined with 57.8 : 42.2 % and 50.5 : 49.5 % occupancies respectively. ; 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 O1 2.023(3) . ? Ni1 N3 2.066(4) . ? Ni1 O3 2.066(4) . ? Ni1 O5 2.070(4) . ? Ni1 N4 2.092(5) . ? Ni1 O6 2.142(4) . ? Ni1 Ni2 3.4268(11) . ? Ni2 O2 2.004(5) . ? Ni2 O1 2.011(4) . ? Ni2 O4 2.038(4) . ? Ni2 N1 2.122(4) . ? Ni2 N2A 2.149(6) . ? Ni2 N2B 2.152(7) . ? Ni2 O7 2.379(6) . ? O1 C1 1.348(6) . ? O2 C22 1.238(7) . ? O3 C22 1.298(7) . ? O4 C24 1.211(8) . ? O5 C24 1.278(8) . ? O6 C27 1.399(7) . ? O7 C26 1.524(13) . ? N1 C18 1.475(8) . ? N1 C7 1.500(6) . ? N1 C8 1.504(7) . ? N3 C14 1.335(6) . ? N3 C10 1.351(5) . ? N4 C15 1.473(8) . ? N4 C16 1.490(7) . ? B1 C34 1.634(7) . ? B1 C46 1.655(7) . ? B1 C40 1.657(6) . ? B1 C28 1.658(7) . ? C1 C2 1.388(7) . ? C1 C6 1.398(6) . ? C2 C3 1.402(7) . ? C2 C16 1.521(7) . ? C3 C4 1.400(7) . ? C4 C5 1.387(7) . ? C4 C17 1.514(7) . ? C5 C6 1.404(6) . ? C6 C7 1.495(7) . ? C8 C9A 1.508(9) . ? C8 C9B 1.508(10) . ? C9A N2A 1.578(10) . ? C20A N2A 1.411(11) . ? N2A C21 1.466(12) . ? C9B N2B 1.581(10) . ? N2B C20B 1.414(12) . ? N2B C21 1.469(12) . ? C10 C11 1.380(6) . ? C11 C12 1.386(7) . ? C12 C13 1.359(7) . ? C13 C14 1.383(7) . ? C14 C15 1.523(7) . ? C18 C19 1.533(8) . ? C22 C23 1.515(8) . ? C24 C25 1.518(8) . ? C28 C29 1.404(7) . ? C28 C33 1.405(7) . ? C29 C30 1.376(7) . ? C30 C31 1.369(9) . ? C31 C32 1.370(9) . ? C32 C33 1.413(9) . ? C34 C39 1.387(7) . ? C34 C35 1.398(8) . ? C35 C36 1.408(9) . ? C36 C37 1.363(13) . ? C37 C38 1.380(12) . ? C38 C39 1.386(8) . ? C40 C45 1.392(6) . ? C40 C41 1.404(6) . ? C41 C42 1.401(7) . ? C42 C43 1.375(7) . ? C43 C44 1.371(7) . ? C44 C45 1.400(6) . ? C46 C51 1.402(6) . ? C46 C47 1.425(7) . ? C47 C48 1.381(8) . ? C48 C49 1.401(8) . ? C49 C50 1.360(8) . ? C50 C51 1.385(7) . ? O1S C1S 1.326(11) . ? O2S C2S 1.323(11) . ? O3S C3SB 1.346(12) . ? O3S C3SA 1.348(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 O1 Ni1 N3 91.55(14) . . ? O1 Ni1 O3 97.39(15) . . ? N3 Ni1 O3 92.00(14) . . ? O1 Ni1 O5 90.21(15) . . ? N3 Ni1 O5 174.28(16) . . ? O3 Ni1 O5 93.17(16) . . ? O1 Ni1 N4 91.04(15) . . ? N3 Ni1 N4 81.53(17) . . ? O3 Ni1 N4 169.53(17) . . ? O5 Ni1 N4 93.00(18) . . ? O1 Ni1 O6 175.50(15) . . ? N3 Ni1 O6 90.19(15) . . ? O3 Ni1 O6 86.70(16) . . ? O5 Ni1 O6 87.67(16) . . ? N4 Ni1 O6 85.11(17) . . ? O1 Ni1 Ni2 31.74(10) . . ? N3 Ni1 Ni2 110.82(10) . . ? O3 Ni1 Ni2 72.10(11) . . ? O5 Ni1 Ni2 73.18(12) . . ? N4 Ni1 Ni2 117.87(13) . . ? O6 Ni1 Ni2 150.14(12) . . ? O2 Ni2 O1 92.42(16) . . ? O2 Ni2 O4 91.72(19) . . ? O1 Ni2 O4 94.23(18) . . ? O2 Ni2 N1 91.48(18) . . ? O1 Ni2 N1 92.81(15) . . ? O4 Ni2 N1 172.13(18) . . ? O2 Ni2 N2A 166.6(3) . . ? O1 Ni2 N2A 100.1(3) . . ? O4 Ni2 N2A 92.2(3) . . ? N1 Ni2 N2A 83.1(3) . . ? O2 Ni2 N2B 169.2(5) . . ? O1 Ni2 N2B 98.1(4) . . ? O4 Ni2 N2B 90.2(4) . . ? N1 Ni2 N2B 85.4(4) . . ? N2A Ni2 N2B 2.9(7) . . ? O2 Ni2 O7 79.5(2) . . ? O1 Ni2 O7 166.20(16) . . ? O4 Ni2 O7 75.0(2) . . ? N1 Ni2 O7 98.54(18) . . ? N2A Ni2 O7 89.1(3) . . ? N2B Ni2 O7 90.7(4) . . ? O2 Ni2 Ni1 72.77(13) . . ? O1 Ni2 Ni1 31.95(9) . . ? O4 Ni2 Ni1 70.32(14) . . ? N1 Ni2 Ni1 117.52(13) . . ? N2A Ni2 Ni1 120.6(3) . . ? N2B Ni2 Ni1 117.8(5) . . ? O7 Ni2 Ni1 134.26(13) . . ? C1 O1 Ni2 123.8(3) . . ? C1 O1 Ni1 119.0(3) . . ? Ni2 O1 Ni1 116.31(16) . . ? C22 O2 Ni2 132.0(4) . . ? C22 O3 Ni1 130.5(4) . . ? C24 O4 Ni2 135.3(5) . . ? C24 O5 Ni1 128.5(4) . . ? C27 O6 Ni1 127.2(4) . . ? C26 O7 Ni2 133.2(6) . . ? C18 N1 C7 109.9(5) . . ? C18 N1 C8 110.4(5) . . ? C7 N1 C8 111.1(4) . . ? C18 N1 Ni2 108.9(3) . . ? C7 N1 Ni2 108.9(3) . . ? C8 N1 Ni2 107.6(3) . . ? C14 N3 C10 117.9(4) . . ? C14 N3 Ni1 115.3(3) . . ? C10 N3 Ni1 126.3(3) . . ? C15 N4 C16 110.7(5) . . ? C15 N4 Ni1 108.0(3) . . ? C16 N4 Ni1 113.3(4) . . ? C34 B1 C46 109.6(4) . . ? C34 B1 C40 110.1(4) . . ? C46 B1 C40 108.9(4) . . ? C34 B1 C28 109.1(4) . . ? C46 B1 C28 110.9(4) . . ? C40 B1 C28 108.3(4) . . ? O1 C1 C2 120.0(4) . . ? O1 C1 C6 120.5(4) . . ? C2 C1 C6 119.5(4) . . ? C1 C2 C3 120.3(4) . . ? C1 C2 C16 119.5(5) . . ? C3 C2 C16 120.3(5) . . ? C4 C3 C2 121.3(5) . . ? C5 C4 C3 117.3(4) . . ? C5 C4 C17 121.0(4) . . ? C3 C4 C17 121.6(5) . . ? C4 C5 C6 122.4(4) . . ? C1 C6 C5 119.1(4) . . ? C1 C6 C7 120.6(4) . . ? C5 C6 C7 120.3(4) . . ? C6 C7 N1 114.2(4) . . ? N1 C8 C9A 111.3(6) . . ? N1 C8 C9B 110.5(7) . . ? C9A C8 C9B 60.7(8) . . ? C8 C9A N2A 103.5(6) . . ? C20A N2A C21 108.0(10) . . ? C20A N2A C9A 117.3(9) . . ? C21 N2A C9A 94.9(7) . . ? C20A N2A Ni2 116.1(9) . . ? C21 N2A Ni2 115.8(7) . . ? C9A N2A Ni2 102.9(6) . . ? C8 C9B N2B 108.3(12) . . ? C20B N2B C21 100.2(14) . . ? C20B N2B C9B 92.0(15) . . ? C21 N2B C9B 134.9(11) . . ? C20B N2B Ni2 110.3(14) . . ? C21 N2B Ni2 115.4(7) . . ? C9B N2B Ni2 100.1(6) . . ? N3 C10 C11 123.3(4) . . ? C10 C11 C12 117.7(4) . . ? C13 C12 C11 119.3(5) . . ? C12 C13 C14 120.2(5) . . ? N3 C14 C13 121.6(5) . . ? N3 C14 C15 114.8(5) . . ? C13 C14 C15 123.6(5) . . ? N4 C15 C14 112.5(4) . . ? N4 C16 C2 112.7(4) . . ? N1 C18 C19 118.2(5) . . ? N2A C21 N2B 4.3(10) . . ? O2 C22 O3 126.1(5) . . ? O2 C22 C23 117.0(7) . . ? O3 C22 C23 116.9(6) . . ? O4 C24 O5 125.6(6) . . ? O4 C24 C25 119.4(7) . . ? O5 C24 C25 114.9(7) . . ? C29 C28 C33 114.7(5) . . ? C29 C28 B1 122.1(4) . . ? C33 C28 B1 123.0(4) . . ? C30 C29 C28 123.6(5) . . ? C31 C30 C29 120.4(6) . . ? C30 C31 C32 119.1(6) . . ? C31 C32 C33 120.7(6) . . ? C28 C33 C32 121.5(6) . . ? C39 C34 C35 114.7(5) . . ? C39 C34 B1 123.6(5) . . ? C35 C34 B1 121.5(5) . . ? C34 C35 C36 122.5(7) . . ? C37 C36 C35 119.2(8) . . ? C36 C37 C38 120.8(7) . . ? C37 C38 C39 118.4(7) . . ? C38 C39 C34 124.4(6) . . ? C45 C40 C41 115.0(4) . . ? C45 C40 B1 123.6(4) . . ? C41 C40 B1 121.3(4) . . ? C42 C41 C40 122.6(5) . . ? C43 C42 C41 119.8(5) . . ? C44 C43 C42 119.6(5) . . ? C43 C44 C45 119.9(5) . . ? C40 C45 C44 123.0(4) . . ? C51 C46 C47 114.5(4) . . ? C51 C46 B1 125.6(4) . . ? C47 C46 B1 119.8(4) . . ? C48 C47 C46 122.2(5) . . ? C47 C48 C49 120.5(5) . . ? C50 C49 C48 118.5(5) . . ? C49 C50 C51 121.1(5) . . ? C50 C51 C46 123.1(5) . . ? C3SB O3S C3SA 74.3(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 Ni2 O2 125.5(2) . . . . ? N3 Ni1 Ni2 O2 69.53(16) . . . . ? O3 Ni1 Ni2 O2 -15.67(15) . . . . ? O5 Ni1 Ni2 O2 -114.78(17) . . . . ? N4 Ni1 Ni2 O2 160.84(18) . . . . ? O6 Ni1 Ni2 O2 -62.5(3) . . . . ? N3 Ni1 Ni2 O1 -56.0(2) . . . . ? O3 Ni1 Ni2 O1 -141.2(2) . . . . ? O5 Ni1 Ni2 O1 119.7(2) . . . . ? N4 Ni1 Ni2 O1 35.3(2) . . . . ? O6 Ni1 Ni2 O1 172.0(3) . . . . ? O1 Ni1 Ni2 O4 -136.2(2) . . . . ? N3 Ni1 Ni2 O4 167.8(2) . . . . ? O3 Ni1 Ni2 O4 82.6(2) . . . . ? O5 Ni1 Ni2 O4 -16.5(2) . . . . ? N4 Ni1 Ni2 O4 -100.9(2) . . . . ? O6 Ni1 Ni2 O4 35.8(3) . . . . ? O1 Ni1 Ni2 N1 43.0(2) . . . . ? N3 Ni1 Ni2 N1 -12.94(19) . . . . ? O3 Ni1 Ni2 N1 -98.14(19) . . . . ? O5 Ni1 Ni2 N1 162.7(2) . . . . ? N4 Ni1 Ni2 N1 78.4(2) . . . . ? O6 Ni1 Ni2 N1 -145.0(3) . . . . ? O1 Ni1 Ni2 N2A -55.7(3) . . . . ? N3 Ni1 Ni2 N2A -111.7(3) . . . . ? O3 Ni1 Ni2 N2A 163.1(3) . . . . ? O5 Ni1 Ni2 N2A 64.0(3) . . . . ? N4 Ni1 Ni2 N2A -20.3(3) . . . . ? O6 Ni1 Ni2 N2A 116.3(3) . . . . ? O1 Ni1 Ni2 N2B -56.9(3) . . . . ? N3 Ni1 Ni2 N2B -112.9(3) . . . . ? O3 Ni1 Ni2 N2B 161.9(3) . . . . ? O5 Ni1 Ni2 N2B 62.8(3) . . . . ? N4 Ni1 Ni2 N2B -21.6(3) . . . . ? O6 Ni1 Ni2 N2B 115.1(3) . . . . ? O1 Ni1 Ni2 O7 -179.1(3) . . . . ? N3 Ni1 Ni2 O7 124.9(3) . . . . ? O3 Ni1 Ni2 O7 39.7(3) . . . . ? O5 Ni1 Ni2 O7 -59.4(3) . . . . ? N4 Ni1 Ni2 O7 -143.8(3) . . . . ? O6 Ni1 Ni2 O7 -7.1(4) . . . . ? O2 Ni2 O1 C1 117.8(3) . . . . ? O4 Ni2 O1 C1 -150.3(4) . . . . ? N1 Ni2 O1 C1 26.2(4) . . . . ? N2A Ni2 O1 C1 -57.3(4) . . . . ? N2B Ni2 O1 C1 -59.5(5) . . . . ? O7 Ni2 O1 C1 171.6(8) . . . . ? Ni1 Ni2 O1 C1 168.9(4) . . . . ? O2 Ni2 O1 Ni1 -51.10(19) . . . . ? O4 Ni2 O1 Ni1 40.8(2) . . . . ? N1 Ni2 O1 Ni1 -142.7(2) . . . . ? N2A Ni2 O1 Ni1 133.8(3) . . . . ? N2B Ni2 O1 Ni1 131.6(4) . . . . ? O7 Ni2 O1 Ni1 2.7(9) . . . . ? N3 Ni1 O1 C1 -40.3(3) . . . . ? O3 Ni1 O1 C1 -132.5(3) . . . . ? O5 Ni1 O1 C1 134.3(3) . . . . ? N4 Ni1 O1 C1 41.3(3) . . . . ? O6 Ni1 O1 C1 72(2) . . . . ? Ni2 Ni1 O1 C1 -169.5(4) . . . . ? N3 Ni1 O1 Ni2 129.21(18) . . . . ? O3 Ni1 O1 Ni2 36.99(19) . . . . ? O5 Ni1 O1 Ni2 -56.2(2) . . . . ? N4 Ni1 O1 Ni2 -149.2(2) . . . . ? O6 Ni1 O1 Ni2 -118.1(19) . . . . ? O1 Ni2 O2 C22 51.4(5) . . . . ? O4 Ni2 O2 C22 -42.9(5) . . . . ? N1 Ni2 O2 C22 144.3(5) . . . . ? N2A Ni2 O2 C22 -149.7(10) . . . . ? N2B Ni2 O2 C22 -142.8(16) . . . . ? O7 Ni2 O2 C22 -117.3(5) . . . . ? Ni1 Ni2 O2 C22 25.8(5) . . . . ? O1 Ni1 O3 C22 -3.1(4) . . . . ? N3 Ni1 O3 C22 -94.9(4) . . . . ? O5 Ni1 O3 C22 87.5(4) . . . . ? N4 Ni1 O3 C22 -146.5(8) . . . . ? O6 Ni1 O3 C22 175.0(4) . . . . ? Ni2 Ni1 O3 C22 16.3(4) . . . . ? O2 Ni2 O4 C24 96.3(7) . . . . ? O1 Ni2 O4 C24 3.8(7) . . . . ? N1 Ni2 O4 C24 -149.6(13) . . . . ? N2A Ni2 O4 C24 -96.5(7) . . . . ? N2B Ni2 O4 C24 -94.3(8) . . . . ? O7 Ni2 O4 C24 175.0(7) . . . . ? Ni1 Ni2 O4 C24 25.3(6) . . . . ? O1 Ni1 O5 C24 47.7(5) . . . . ? N3 Ni1 O5 C24 155.7(13) . . . . ? O3 Ni1 O5 C24 -49.7(5) . . . . ? N4 Ni1 O5 C24 138.8(5) . . . . ? O6 Ni1 O5 C24 -136.2(5) . . . . ? Ni2 Ni1 O5 C24 20.5(5) . . . . ? O1 Ni1 O6 C27 72(2) . . . . ? N3 Ni1 O6 C27 -175.3(5) . . . . ? O3 Ni1 O6 C27 -83.3(5) . . . . ? O5 Ni1 O6 C27 10.0(6) . . . . ? N4 Ni1 O6 C27 103.2(6) . . . . ? Ni2 Ni1 O6 C27 -39.3(7) . . . . ? O2 Ni2 O7 C26 -40.8(8) . . . . ? O1 Ni2 O7 C26 -95.9(10) . . . . ? O4 Ni2 O7 C26 -135.5(8) . . . . ? N1 Ni2 O7 C26 49.1(8) . . . . ? N2A Ni2 O7 C26 132.1(8) . . . . ? N2B Ni2 O7 C26 134.6(9) . . . . ? Ni1 Ni2 O7 C26 -93.9(8) . . . . ? O2 Ni2 N1 C18 49.5(4) . . . . ? O1 Ni2 N1 C18 142.0(4) . . . . ? O4 Ni2 N1 C18 -64.6(16) . . . . ? N2A Ni2 N1 C18 -118.2(5) . . . . ? N2B Ni2 N1 C18 -120.1(6) . . . . ? O7 Ni2 N1 C18 -30.2(5) . . . . ? Ni1 Ni2 N1 C18 120.8(4) . . . . ? O2 Ni2 N1 C7 -70.4(4) . . . . ? O1 Ni2 N1 C7 22.1(3) . . . . ? O4 Ni2 N1 C7 175.6(14) . . . . ? N2A Ni2 N1 C7 121.9(4) . . . . ? N2B Ni2 N1 C7 120.0(5) . . . . ? O7 Ni2 N1 C7 -150.0(4) . . . . ? Ni1 Ni2 N1 C7 0.9(4) . . . . ? O2 Ni2 N1 C8 169.1(3) . . . . ? O1 Ni2 N1 C8 -98.4(3) . . . . ? O4 Ni2 N1 C8 55.1(16) . . . . ? N2A Ni2 N1 C8 1.4(4) . . . . ? N2B Ni2 N1 C8 -0.5(5) . . . . ? O7 Ni2 N1 C8 89.5(4) . . . . ? Ni1 Ni2 N1 C8 -119.6(3) . . . . ? O1 Ni1 N3 C14 97.8(3) . . . . ? O3 Ni1 N3 C14 -164.7(3) . . . . ? O5 Ni1 N3 C14 -10.1(16) . . . . ? N4 Ni1 N3 C14 7.0(3) . . . . ? O6 Ni1 N3 C14 -78.0(3) . . . . ? Ni2 Ni1 N3 C14 123.7(3) . . . . ? O1 Ni1 N3 C10 -73.8(4) . . . . ? O3 Ni1 N3 C10 23.6(4) . . . . ? O5 Ni1 N3 C10 178.3(13) . . . . ? N4 Ni1 N3 C10 -164.6(4) . . . . ? O6 Ni1 N3 C10 110.3(4) . . . . ? Ni2 Ni1 N3 C10 -48.0(4) . . . . ? O1 Ni1 N4 C15 -111.8(3) . . . . ? N3 Ni1 N4 C15 -20.4(3) . . . . ? O3 Ni1 N4 C15 31.9(10) . . . . ? O5 Ni1 N4 C15 157.9(3) . . . . ? O6 Ni1 N4 C15 70.5(3) . . . . ? Ni2 Ni1 N4 C15 -129.5(3) . . . . ? O1 Ni1 N4 C16 11.3(4) . . . . ? N3 Ni1 N4 C16 102.7(4) . . . . ? O3 Ni1 N4 C16 155.0(7) . . . . ? O5 Ni1 N4 C16 -79.0(4) . . . . ? O6 Ni1 N4 C16 -166.4(4) . . . . ? Ni2 Ni1 N4 C16 -6.4(4) . . . . ? Ni2 O1 C1 C2 139.6(4) . . . . ? Ni1 O1 C1 C2 -51.7(5) . . . . ? Ni2 O1 C1 C6 -39.6(6) . . . . ? Ni1 O1 C1 C6 129.0(4) . . . . ? O1 C1 C2 C3 -179.3(5) . . . . ? C6 C1 C2 C3 0.0(7) . . . . ? O1 C1 C2 C16 -1.0(7) . . . . ? C6 C1 C2 C16 178.3(5) . . . . ? C1 C2 C3 C4 1.7(8) . . . . ? C16 C2 C3 C4 -176.6(5) . . . . ? C2 C3 C4 C5 -0.9(7) . . . . ? C2 C3 C4 C17 176.8(5) . . . . ? C3 C4 C5 C6 -1.5(7) . . . . ? C17 C4 C5 C6 -179.2(5) . . . . ? O1 C1 C6 C5 177.0(4) . . . . ? C2 C1 C6 C5 -2.3(7) . . . . ? O1 C1 C6 C7 -3.3(7) . . . . ? C2 C1 C6 C7 177.4(5) . . . . ? C4 C5 C6 C1 3.1(7) . . . . ? C4 C5 C6 C7 -176.6(4) . . . . ? C1 C6 C7 N1 61.3(6) . . . . ? C5 C6 C7 N1 -119.0(5) . . . . ? C18 N1 C7 C6 178.0(4) . . . . ? C8 N1 C7 C6 55.6(5) . . . . ? Ni2 N1 C7 C6 -62.7(5) . . . . ? C18 N1 C8 C9A 84.2(6) . . . . ? C7 N1 C8 C9A -153.7(6) . . . . ? Ni2 N1 C8 C9A -34.6(6) . . . . ? C18 N1 C8 C9B 149.6(7) . . . . ? C7 N1 C8 C9B -88.3(7) . . . . ? Ni2 N1 C8 C9B 30.9(7) . . . . ? N1 C8 C9A N2A 60.1(8) . . . . ? C9B C8 C9A N2A -42.2(7) . . . . ? C8 C9A N2A C20A 75.4(12) . . . . ? C8 C9A N2A C21 -171.4(8) . . . . ? C8 C9A N2A Ni2 -53.5(7) . . . . ? O2 Ni2 N2A C20A -167.8(10) . . . . ? O1 Ni2 N2A C20A -9.2(9) . . . . ? O4 Ni2 N2A C20A 85.5(9) . . . . ? N1 Ni2 N2A C20A -100.9(9) . . . . ? N2B Ni2 N2A C20A 39(2) . . . . ? O7 Ni2 N2A C20A 160.4(9) . . . . ? Ni1 Ni2 N2A C20A 17.2(10) . . . . ? O2 Ni2 N2A C21 63.9(14) . . . . ? O1 Ni2 N2A C21 -137.5(7) . . . . ? O4 Ni2 N2A C21 -42.8(8) . . . . ? N1 Ni2 N2A C21 130.8(8) . . . . ? N2B Ni2 N2A C21 -90(2) . . . . ? O7 Ni2 N2A C21 32.1(8) . . . . ? Ni1 Ni2 N2A C21 -111.2(7) . . . . ? O2 Ni2 N2A C9A -38.2(12) . . . . ? O1 Ni2 N2A C9A 120.4(5) . . . . ? O4 Ni2 N2A C9A -144.9(5) . . . . ? N1 Ni2 N2A C9A 28.7(5) . . . . ? N2B Ni2 N2A C9A 168(2) . . . . ? O7 Ni2 N2A C9A -70.0(5) . . . . ? Ni1 Ni2 N2A C9A 146.8(4) . . . . ? N1 C8 C9B N2B -57.8(11) . . . . ? C9A C8 C9B N2B 45.7(10) . . . . ? C8 C9B N2B C20B 162.6(14) . . . . ? C8 C9B N2B C21 -90.8(18) . . . . ? C8 C9B N2B Ni2 51.6(12) . . . . ? O2 Ni2 N2B C20B 163.6(18) . . . . ? O1 Ni2 N2B C20B -30.7(14) . . . . ? O4 Ni2 N2B C20B 63.6(14) . . . . ? N1 Ni2 N2B C20B -122.9(14) . . . . ? N2A Ni2 N2B C20B -163(3) . . . . ? O7 Ni2 N2B C20B 138.6(14) . . . . ? Ni1 Ni2 N2B C20B -4.1(14) . . . . ? O2 Ni2 N2B C21 51(3) . . . . ? O1 Ni2 N2B C21 -143.4(11) . . . . ? O4 Ni2 N2B C21 -49.1(11) . . . . ? N1 Ni2 N2B C21 124.5(12) . . . . ? N2A Ni2 N2B C21 84.0(19) . . . . ? O7 Ni2 N2B C21 25.9(11) . . . . ? Ni1 Ni2 N2B C21 -116.8(11) . . . . ? O2 Ni2 N2B C9B -100.4(12) . . . . ? O1 Ni2 N2B C9B 65.3(10) . . . . ? O4 Ni2 N2B C9B 159.5(10) . . . . ? N1 Ni2 N2B C9B -26.9(10) . . . . ? N2A Ni2 N2B C9B -67(3) . . . . ? O7 Ni2 N2B C9B -125.5(10) . . . . ? Ni1 Ni2 N2B C9B 91.9(10) . . . . ? C14 N3 C10 C11 0.7(6) . . . . ? Ni1 N3 C10 C11 172.2(3) . . . . ? N3 C10 C11 C12 -0.7(7) . . . . ? C10 C11 C12 C13 -0.8(7) . . . . ? C11 C12 C13 C14 2.2(7) . . . . ? C10 N3 C14 C13 0.7(7) . . . . ? Ni1 N3 C14 C13 -171.6(4) . . . . ? C10 N3 C14 C15 -179.3(4) . . . . ? Ni1 N3 C14 C15 8.4(5) . . . . ? C12 C13 C14 N3 -2.3(7) . . . . ? C12 C13 C14 C15 177.7(5) . . . . ? C16 N4 C15 C14 -94.4(5) . . . . ? Ni1 N4 C15 C14 30.3(5) . . . . ? N3 C14 C15 N4 -26.5(6) . . . . ? C13 C14 C15 N4 153.5(5) . . . . ? C15 N4 C16 C2 65.6(6) . . . . ? Ni1 N4 C16 C2 -56.0(6) . . . . ? C1 C2 C16 N4 60.4(8) . . . . ? C3 C2 C16 N4 -121.3(6) . . . . ? C7 N1 C18 C19 -52.8(7) . . . . ? C8 N1 C18 C19 70.1(7) . . . . ? Ni2 N1 C18 C19 -172.0(5) . . . . ? C20A N2A C21 N2B -42(2) . . . . ? C9A N2A C21 N2B -163(2) . . . . ? Ni2 N2A C21 N2B 90(2) . . . . ? C20B N2B C21 N2A 157(3) . . . . ? C9B N2B C21 N2A 54(3) . . . . ? Ni2 N2B C21 N2A -84.6(19) . . . . ? Ni2 O2 C22 O3 -24.8(8) . . . . ? Ni2 O2 C22 C23 156.1(5) . . . . ? Ni1 O3 C22 O2 -5.9(8) . . . . ? Ni1 O3 C22 C23 173.2(4) . . . . ? Ni2 O4 C24 O5 -20.1(12) . . . . ? Ni2 O4 C24 C25 159.9(6) . . . . ? Ni1 O5 C24 O4 -13.2(10) . . . . ? Ni1 O5 C24 C25 166.8(5) . . . . ? C34 B1 C28 C29 169.4(4) . . . . ? C46 B1 C28 C29 -69.8(5) . . . . ? C40 B1 C28 C29 49.6(5) . . . . ? C34 B1 C28 C33 -7.2(6) . . . . ? C46 B1 C28 C33 113.6(5) . . . . ? C40 B1 C28 C33 -127.0(4) . . . . ? C33 C28 C29 C30 -0.3(7) . . . . ? B1 C28 C29 C30 -177.1(4) . . . . ? C28 C29 C30 C31 1.4(7) . . . . ? C29 C30 C31 C32 -1.5(8) . . . . ? C30 C31 C32 C33 0.5(8) . . . . ? C29 C28 C33 C32 -0.8(7) . . . . ? B1 C28 C33 C32 176.0(4) . . . . ? C31 C32 C33 C28 0.7(8) . . . . ? C46 B1 C34 C39 152.4(5) . . . . ? C40 B1 C34 C39 32.7(7) . . . . ? C28 B1 C34 C39 -86.0(6) . . . . ? C46 B1 C34 C35 -31.9(7) . . . . ? C40 B1 C34 C35 -151.7(6) . . . . ? C28 B1 C34 C35 89.7(7) . . . . ? C39 C34 C35 C36 0.6(11) . . . . ? B1 C34 C35 C36 -175.4(8) . . . . ? C34 C35 C36 C37 -1.6(15) . . . . ? C35 C36 C37 C38 0.9(16) . . . . ? C36 C37 C38 C39 0.7(14) . . . . ? C37 C38 C39 C34 -1.8(11) . . . . ? C35 C34 C39 C38 1.1(10) . . . . ? B1 C34 C39 C38 177.0(6) . . . . ? C34 B1 C40 C45 95.3(5) . . . . ? C46 B1 C40 C45 -24.9(5) . . . . ? C28 B1 C40 C45 -145.6(4) . . . . ? C34 B1 C40 C41 -84.6(5) . . . . ? C46 B1 C40 C41 155.3(4) . . . . ? C28 B1 C40 C41 34.6(5) . . . . ? C45 C40 C41 C42 -1.0(6) . . . . ? B1 C40 C41 C42 178.9(4) . . . . ? C40 C41 C42 C43 -0.1(7) . . . . ? C41 C42 C43 C44 0.3(7) . . . . ? C42 C43 C44 C45 0.5(7) . . . . ? C41 C40 C45 C44 1.9(6) . . . . ? B1 C40 C45 C44 -178.0(4) . . . . ? C43 C44 C45 C40 -1.7(7) . . . . ? C34 B1 C46 C51 137.1(4) . . . . ? C40 B1 C46 C51 -102.4(5) . . . . ? C28 B1 C46 C51 16.7(6) . . . . ? C34 B1 C46 C47 -46.4(6) . . . . ? C40 B1 C46 C47 74.1(5) . . . . ? C28 B1 C46 C47 -166.9(4) . . . . ? C51 C46 C47 C48 1.5(7) . . . . ? B1 C46 C47 C48 -175.3(5) . . . . ? C46 C47 C48 C49 -0.2(8) . . . . ? C47 C48 C49 C50 -0.8(8) . . . . ? C48 C49 C50 C51 0.3(8) . . . . ? C49 C50 C51 C46 1.1(8) . . . . ? C47 C46 C51 C50 -2.0(7) . . . . ? B1 C46 C51 C50 174.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 0.939 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.090 data_ifn308m _database_code_CSD 194356 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H43 F6 N4 Ni2 O7 P' _chemical_formula_weight 786.03 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' O O 0.0106 0.0060 '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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.771(2) _cell_length_b 16.086(3) _cell_length_c 17.687(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.915(4) _cell_angle_gamma 90.00 _cell_volume 3250.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1696 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.291 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7302 _exptl_absorpt_correction_T_max 0.7644 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20456 _diffrn_reflns_av_R_equivalents 0.1327 _diffrn_reflns_av_sigmaI/netI 0.2407 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.41 _reflns_number_total 7829 _reflns_number_gt 2867 _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. F1, F2, F3 and F4 were found to be disordered and refined to an occupancy of 32%-68%. ; _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^)+(0.0558P)^2^+0.0000P] 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 7829 _refine_ls_number_parameters 415 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1892 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.833 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.79781(7) 0.26178(5) 0.48421(4) 0.0269(2) Uani 1 1 d . . . Ni2 Ni 0.56609(7) 0.14473(5) 0.52688(5) 0.0272(2) Uani 1 1 d . . . P1 P 0.09688(16) 0.04359(12) 0.28081(11) 0.0364(5) Uani 1 1 d D . . O1 O 0.6250(3) 0.2406(2) 0.4709(2) 0.0256(10) Uani 1 1 d . . . O2 O 0.8544(3) 0.2511(3) 0.6073(2) 0.0317(11) Uani 1 1 d . . . O3 O 0.9814(3) 0.2607(3) 0.5356(2) 0.0313(10) Uani 1 1 d . . . O4 O 0.8190(3) 0.1347(3) 0.4791(2) 0.0327(11) Uani 1 1 d . . . O5 O 0.6584(4) 0.0591(2) 0.4789(2) 0.0291(10) Uani 1 1 d . . . O6 O 0.5046(4) 0.0465(3) 0.5886(2) 0.0326(11) Uani 1 1 d . . . H5A H 0.4805 -0.0045 0.5624 0.039 Uiso 1 1 calc R . . O7 O 0.7002(3) 0.1470(2) 0.6268(2) 0.0298(10) Uani 1 1 d . . . H5B H 0.6997 0.1112 0.6658 0.036 Uiso 1 1 d R . . H5C H 0.7591 0.1837 0.6312 0.036 Uiso 1 1 d R . . N1 N 0.7767(4) 0.3934(3) 0.4840(3) 0.0283(13) Uani 1 1 d . . . N2 N 0.8040(4) 0.2754(3) 0.3682(3) 0.0338(14) Uani 1 1 d . . . N3 N 0.4140(4) 0.1326(3) 0.4391(3) 0.0303(13) Uani 1 1 d . . . H40A H 0.4011 0.0760 0.4297 0.036 Uiso 1 1 calc R . . N4 N 0.4621(4) 0.2262(3) 0.5680(3) 0.0275(12) Uani 1 1 d . . . F1 F 0.1707(14) 0.0132(9) 0.3626(7) 0.074(3) Uiso 0.326(6) 1 d PDU A 1 F1' F 0.0767(7) 0.0259(4) 0.3646(4) 0.071(2) Uiso 0.674(6) 1 d PDU A 2 F2 F 0.2281(9) 0.0285(8) 0.2646(9) 0.055(3) Uiso 0.326(6) 1 d PDU A 1 F2' F 0.2298(5) 0.0169(4) 0.3138(4) 0.0583(19) Uiso 0.674(6) 1 d PDU A 2 F3 F 0.0593(14) 0.0719(9) 0.1910(6) 0.061(3) Uiso 0.326(6) 1 d PDU A 1 F3' F 0.1182(7) 0.0598(4) 0.1982(4) 0.062(2) Uiso 0.674(6) 1 d PDU A 2 F4 F -0.0307(10) 0.0545(9) 0.2876(9) 0.059(3) Uiso 0.326(6) 1 d PDU A 1 F4' F -0.0352(5) 0.0718(4) 0.2481(4) 0.0586(19) Uiso 0.674(6) 1 d PDU A 2 F5 F 0.0665(4) -0.0497(2) 0.2563(3) 0.0712(14) Uani 1 1 d . A . F6 F 0.1321(4) 0.1368(2) 0.3041(2) 0.0604(13) Uani 1 1 d . A . C1 C 0.2883(6) 0.4636(4) 0.2931(4) 0.049(2) Uani 1 1 d . . . H1A H 0.3120 0.5211 0.3068 0.073 Uiso 1 1 calc R . . H1B H 0.2121 0.4530 0.3044 0.073 Uiso 1 1 calc R . . H1C H 0.2825 0.4547 0.2375 0.073 Uiso 1 1 calc R . . C2 C 0.3782(6) 0.4048(4) 0.3402(4) 0.0339(17) Uani 1 1 d . . . C3 C 0.3643(6) 0.3188(4) 0.3316(4) 0.0367(17) Uani 1 1 d . . . H3A H 0.2982 0.2976 0.2948 0.044 Uiso 1 1 calc R . . C4 C 0.4448(5) 0.2632(4) 0.3756(3) 0.0278(15) Uani 1 1 d . . . C5 C 0.5441(5) 0.2939(4) 0.4293(4) 0.0286(15) Uani 1 1 d . . . C6 C 0.5582(5) 0.3805(4) 0.4394(4) 0.0289(15) Uani 1 1 d . . . C7 C 0.4764(5) 0.4327(4) 0.3945(4) 0.0317(16) Uani 1 1 d . . . H7B H 0.4877 0.4910 0.4010 0.038 Uiso 1 1 calc R . . C8 C 0.6601(5) 0.4131(4) 0.4985(4) 0.0321(16) Uani 1 1 d . . . H8A H 0.6571 0.3904 0.5500 0.039 Uiso 1 1 calc R . . H8B H 0.6525 0.4743 0.5011 0.039 Uiso 1 1 calc R . . C9 C 0.8670(5) 0.4323(4) 0.5473(4) 0.0338(16) Uani 1 1 d . . . H9A H 0.9449 0.4136 0.5421 0.041 Uiso 1 1 calc R . . H9B H 0.8565 0.4112 0.5977 0.041 Uiso 1 1 calc R . . C10 C 0.8672(6) 0.5285(4) 0.5502(4) 0.0405(18) Uani 1 1 d . . . H10A H 0.9297 0.5475 0.5940 0.061 Uiso 1 1 calc R . . H10B H 0.7915 0.5482 0.5571 0.061 Uiso 1 1 calc R . . H10C H 0.8804 0.5506 0.5015 0.061 Uiso 1 1 calc R . . C11 C 0.7877(6) 0.4224(4) 0.4056(4) 0.0349(17) Uani 1 1 d . . . H11A H 0.7388 0.4726 0.3906 0.042 Uiso 1 1 calc R . . H11B H 0.8700 0.4379 0.4087 0.042 Uiso 1 1 calc R . . C13 C 0.7421(6) 0.2107(4) 0.3148(4) 0.047(2) Uani 1 1 d . . . H13A H 0.7496 0.2224 0.2618 0.070 Uiso 1 1 calc R . . H13B H 0.6592 0.2105 0.3156 0.070 Uiso 1 1 calc R . . H13C H 0.7765 0.1563 0.3315 0.070 Uiso 1 1 calc R . . C12 C 0.7508(6) 0.3574(4) 0.3443(4) 0.0364(17) Uani 1 1 d . . . H12A H 0.6645 0.3519 0.3320 0.044 Uiso 1 1 calc R . . H12B H 0.7730 0.3754 0.2964 0.044 Uiso 1 1 calc R . . C14 C 0.9276(6) 0.2743(4) 0.3628(4) 0.0399(18) Uani 1 1 d . . . H14A H 0.9307 0.2807 0.3083 0.060 Uiso 1 1 calc R . . H14B H 0.9636 0.2214 0.3830 0.060 Uiso 1 1 calc R . . H14C H 0.9701 0.3202 0.3936 0.060 Uiso 1 1 calc R . . C15 C 0.4272(6) 0.1709(4) 0.3661(4) 0.0324(16) Uani 1 1 d . . . H15A H 0.3564 0.1596 0.3242 0.039 Uiso 1 1 calc R . . H15B H 0.4951 0.1458 0.3507 0.039 Uiso 1 1 calc R . . C16 C 0.3125(5) 0.1658(4) 0.4657(4) 0.0337(17) Uani 1 1 d . . . H16A H 0.2703 0.1191 0.4831 0.040 Uiso 1 1 calc R . . H16B H 0.2580 0.1933 0.4214 0.040 Uiso 1 1 calc R . . C17 C 0.3487(5) 0.2266(4) 0.5310(3) 0.0265(15) Uani 1 1 d . . . C18 C 0.2676(6) 0.2771(4) 0.5536(4) 0.0361(17) Uani 1 1 d . . . H18A H 0.1873 0.2751 0.5268 0.043 Uiso 1 1 calc R . . C19 C 0.3053(6) 0.3303(4) 0.6154(4) 0.0402(18) Uani 1 1 d . . . H19A H 0.2509 0.3647 0.6325 0.048 Uiso 1 1 calc R . . C20 C 0.4226(6) 0.3332(4) 0.6524(4) 0.0369(17) Uani 1 1 d . . . H20A H 0.4508 0.3710 0.6940 0.044 Uiso 1 1 calc R . . C21 C 0.4979(6) 0.2799(4) 0.6277(4) 0.0358(17) Uani 1 1 d . . . H21A H 0.5786 0.2809 0.6537 0.043 Uiso 1 1 calc R . . C22 C 0.9607(5) 0.2427(4) 0.6009(4) 0.0309(16) Uani 1 1 d . . . C23 C 1.0535(5) 0.2151(4) 0.6678(4) 0.0368(17) Uani 1 1 d . . . H23A H 1.0960 0.2636 0.6938 0.055 Uiso 1 1 calc R . . H23B H 1.1078 0.1785 0.6495 0.055 Uiso 1 1 calc R . . H23C H 1.0184 0.1848 0.7046 0.055 Uiso 1 1 calc R . . C24 C 0.7632(6) 0.0697(4) 0.4674(4) 0.0309(16) Uani 1 1 d . . . C25 C 0.8196(6) -0.0033(4) 0.4367(4) 0.048(2) Uani 1 1 d . . . H25A H 0.8971 0.0129 0.4305 0.072 Uiso 1 1 calc R . . H25B H 0.7705 -0.0205 0.3862 0.072 Uiso 1 1 calc R . . H25C H 0.8276 -0.0497 0.4735 0.072 Uiso 1 1 calc R . . C26 C 0.4987(6) 0.0554(4) 0.6687(4) 0.047(2) Uani 1 1 d . . . H26A H 0.4684 0.0040 0.6862 0.071 Uiso 1 1 calc R . . H26B H 0.4465 0.1017 0.6732 0.071 Uiso 1 1 calc R . . H26C H 0.5771 0.0667 0.7012 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0197(4) 0.0311(5) 0.0306(5) 0.0024(4) 0.0071(4) -0.0023(4) Ni2 0.0227(5) 0.0288(5) 0.0311(5) -0.0009(4) 0.0083(4) -0.0026(4) P1 0.0325(11) 0.0353(11) 0.0393(11) -0.0003(9) 0.0042(9) -0.0017(9) O1 0.019(2) 0.028(2) 0.029(2) 0.007(2) 0.0032(19) 0.0025(19) O2 0.022(2) 0.037(3) 0.036(3) -0.002(2) 0.007(2) -0.002(2) O3 0.027(2) 0.035(3) 0.032(2) 0.001(2) 0.008(2) -0.002(2) O4 0.024(3) 0.031(3) 0.042(3) -0.006(2) 0.004(2) -0.008(2) O5 0.030(3) 0.026(3) 0.033(2) -0.004(2) 0.012(2) -0.007(2) O6 0.043(3) 0.027(3) 0.031(2) -0.005(2) 0.014(2) -0.005(2) O7 0.028(3) 0.034(3) 0.027(2) 0.001(2) 0.008(2) -0.009(2) N1 0.026(3) 0.027(3) 0.033(3) 0.002(3) 0.010(3) -0.003(2) N2 0.031(3) 0.039(4) 0.034(3) 0.003(3) 0.014(3) 0.000(3) N3 0.029(3) 0.030(3) 0.032(3) -0.001(3) 0.008(3) -0.002(2) N4 0.034(3) 0.023(3) 0.026(3) -0.006(2) 0.009(3) -0.008(2) F5 0.068(3) 0.035(3) 0.108(4) -0.011(3) 0.015(3) -0.017(2) F6 0.056(3) 0.033(2) 0.077(3) -0.018(2) -0.015(2) 0.006(2) C1 0.045(5) 0.055(5) 0.047(5) 0.012(4) 0.013(4) 0.014(4) C2 0.028(4) 0.043(5) 0.032(4) 0.006(3) 0.011(3) 0.008(3) C3 0.022(4) 0.051(5) 0.036(4) 0.005(4) 0.005(3) 0.005(3) C4 0.018(3) 0.046(4) 0.019(3) 0.003(3) 0.002(3) 0.002(3) C5 0.016(3) 0.043(4) 0.029(4) 0.001(3) 0.010(3) 0.000(3) C6 0.020(4) 0.030(4) 0.037(4) -0.001(3) 0.006(3) 0.001(3) C7 0.028(4) 0.036(4) 0.034(4) 0.007(3) 0.012(3) 0.005(3) C8 0.029(4) 0.033(4) 0.037(4) 0.001(3) 0.015(3) -0.001(3) C9 0.028(4) 0.037(4) 0.036(4) 0.005(3) 0.006(3) -0.004(3) C10 0.034(4) 0.033(4) 0.056(5) -0.002(4) 0.014(4) -0.007(3) C11 0.031(4) 0.038(4) 0.040(4) 0.016(4) 0.017(3) 0.001(3) C13 0.055(5) 0.053(5) 0.031(4) -0.008(4) 0.011(4) -0.018(4) C12 0.029(4) 0.050(5) 0.034(4) 0.008(4) 0.013(3) -0.002(4) C14 0.042(4) 0.041(4) 0.041(4) -0.002(4) 0.018(4) 0.003(4) C15 0.028(4) 0.042(4) 0.028(4) -0.004(3) 0.008(3) -0.004(3) C16 0.025(4) 0.040(4) 0.036(4) -0.004(3) 0.007(3) -0.012(3) C17 0.026(4) 0.027(4) 0.029(4) 0.006(3) 0.014(3) -0.004(3) C18 0.019(4) 0.047(5) 0.046(4) 0.005(4) 0.015(3) 0.006(3) C19 0.040(5) 0.040(4) 0.044(4) -0.001(4) 0.018(4) 0.005(4) C20 0.050(5) 0.026(4) 0.039(4) -0.003(3) 0.020(4) 0.002(3) C21 0.035(4) 0.043(5) 0.031(4) 0.000(3) 0.010(3) 0.001(3) C22 0.025(4) 0.027(4) 0.035(4) 0.001(3) -0.003(3) -0.012(3) C23 0.027(4) 0.041(4) 0.040(4) 0.004(3) 0.004(3) 0.000(3) C24 0.026(4) 0.041(4) 0.027(4) -0.007(3) 0.009(3) -0.001(3) C25 0.047(5) 0.054(5) 0.049(5) -0.006(4) 0.024(4) -0.001(4) C26 0.048(5) 0.051(5) 0.048(5) -0.007(4) 0.022(4) -0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.019(4) . ? Ni1 O4 2.065(4) . ? Ni1 N2 2.082(5) . ? Ni1 O2 2.125(4) . ? Ni1 N1 2.131(5) . ? Ni1 O3 2.134(4) . ? Ni1 C22 2.476(6) . ? Ni1 Ni2 3.5419(12) . ? Ni2 O1 2.042(4) . ? Ni2 N4 2.042(5) . ? Ni2 O5 2.060(4) . ? Ni2 O7 2.067(4) . ? Ni2 N3 2.078(5) . ? Ni2 O6 2.143(4) . ? P1 F4 1.545(10) . ? P1 F3' 1.562(6) . ? P1 F1 1.575(11) . ? P1 F5 1.579(4) . ? P1 F1' 1.583(6) . ? P1 F6 1.584(4) . ? P1 F4' 1.589(6) . ? P1 F2' 1.592(6) . ? P1 F3 1.608(11) . ? P1 F2 1.655(10) . ? O1 C5 1.360(7) . ? O2 C22 1.290(7) . ? O3 C22 1.270(7) . ? O4 C24 1.225(7) . ? O5 C24 1.309(7) . ? O6 C26 1.443(7) . ? N1 C9 1.485(7) . ? N1 C8 1.490(7) . ? N1 C11 1.498(7) . ? N2 C13 1.475(8) . ? N2 C12 1.477(8) . ? N2 C14 1.480(7) . ? N3 C15 1.471(7) . ? N3 C16 1.485(7) . ? N4 C17 1.338(7) . ? N4 C21 1.350(8) . ? C1 C2 1.511(8) . ? C2 C7 1.387(8) . ? C2 C3 1.397(9) . ? C3 C4 1.397(8) . ? C4 C5 1.406(8) . ? C4 C15 1.503(8) . ? C5 C6 1.409(8) . ? C6 C7 1.377(8) . ? C6 C8 1.483(8) . ? C9 C10 1.547(8) . ? C11 C12 1.493(8) . ? C16 C17 1.495(8) . ? C17 C18 1.383(8) . ? C18 C19 1.375(9) . ? C19 C20 1.380(9) . ? C20 C21 1.379(8) . ? C22 C23 1.472(8) . ? C24 C25 1.513(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O4 87.53(16) . . ? O1 Ni1 N2 100.14(18) . . ? O4 Ni1 N2 91.62(19) . . ? O1 Ni1 O2 99.48(15) . . ? O4 Ni1 O2 87.32(16) . . ? N2 Ni1 O2 160.28(18) . . ? O1 Ni1 N1 93.06(17) . . ? O4 Ni1 N1 177.32(18) . . ? N2 Ni1 N1 85.7(2) . . ? O2 Ni1 N1 95.15(18) . . ? O1 Ni1 O3 159.52(16) . . ? O4 Ni1 O3 83.69(16) . . ? N2 Ni1 O3 98.57(18) . . ? O2 Ni1 O3 61.74(15) . . ? N1 Ni1 O3 96.58(18) . . ? O1 Ni1 C22 129.24(19) . . ? O4 Ni1 C22 80.57(18) . . ? N2 Ni1 C22 129.1(2) . . ? O2 Ni1 C22 31.39(17) . . ? N1 Ni1 C22 101.0(2) . . ? O3 Ni1 C22 30.86(17) . . ? O1 Ni1 Ni2 29.48(11) . . ? O4 Ni1 Ni2 65.80(12) . . ? N2 Ni1 Ni2 118.51(15) . . ? O2 Ni1 Ni2 78.86(11) . . ? N1 Ni1 Ni2 115.65(13) . . ? O3 Ni1 Ni2 131.14(12) . . ? C22 Ni1 Ni2 103.78(15) . . ? O1 Ni2 N4 89.47(18) . . ? O1 Ni2 O5 91.80(16) . . ? N4 Ni2 O5 175.16(18) . . ? O1 Ni2 O7 97.01(15) . . ? N4 Ni2 O7 94.84(18) . . ? O5 Ni2 O7 89.64(16) . . ? O1 Ni2 N3 92.36(18) . . ? N4 Ni2 N3 81.0(2) . . ? O5 Ni2 N3 94.25(18) . . ? O7 Ni2 N3 169.74(18) . . ? O1 Ni2 O6 178.27(16) . . ? N4 Ni2 O6 89.25(17) . . ? O5 Ni2 O6 89.58(16) . . ? O7 Ni2 O6 81.94(16) . . ? N3 Ni2 O6 88.58(18) . . ? O1 Ni2 Ni1 29.12(11) . . ? N4 Ni2 Ni1 107.04(14) . . ? O5 Ni2 Ni1 76.02(11) . . ? O7 Ni2 Ni1 72.76(11) . . ? N3 Ni2 Ni1 117.40(14) . . ? O6 Ni2 Ni1 150.72(12) . . ? F4 P1 F3' 115.6(6) . . ? F4 P1 F1 107.2(8) . . ? F3' P1 F1 137.1(7) . . ? F4 P1 F5 88.2(5) . . ? F3' P1 F5 88.7(3) . . ? F1 P1 F5 89.7(5) . . ? F4 P1 F1' 65.2(6) . . ? F3' P1 F1' 179.0(4) . . ? F1 P1 F1' 42.1(6) . . ? F5 P1 F1' 90.6(3) . . ? F4 P1 F6 94.1(5) . . ? F3' P1 F6 89.7(3) . . ? F1 P1 F6 90.2(5) . . ? F5 P1 F6 177.6(3) . . ? F1' P1 F6 90.9(3) . . ? F4 P1 F4' 27.3(5) . . ? F3' P1 F4' 88.6(4) . . ? F1 P1 F4' 134.3(7) . . ? F5 P1 F4' 91.9(3) . . ? F1' P1 F4' 92.2(4) . . ? F6 P1 F4' 89.8(3) . . ? F4 P1 F2' 152.9(6) . . ? F3' P1 F2' 91.3(4) . . ? F1 P1 F2' 45.8(6) . . ? F5 P1 F2' 89.0(3) . . ? F1' P1 F2' 87.9(4) . . ? F6 P1 F2' 89.3(3) . . ? F4' P1 F2' 179.1(4) . . ? F4 P1 F3 90.2(8) . . ? F3' P1 F3 25.5(6) . . ? F1 P1 F3 162.6(9) . . ? F5 P1 F3 90.4(6) . . ? F1' P1 F3 155.3(6) . . ? F6 P1 F3 88.9(5) . . ? F4' P1 F3 63.1(6) . . ? F2' P1 F3 116.8(6) . . ? F4 P1 F2 174.3(7) . . ? F3' P1 F2 59.8(5) . . ? F1 P1 F2 77.4(7) . . ? F5 P1 F2 88.4(5) . . ? F1' P1 F2 119.5(6) . . ? F6 P1 F2 89.3(5) . . ? F4' P1 F2 148.3(6) . . ? F2' P1 F2 31.5(5) . . ? F3 P1 F2 85.3(7) . . ? C5 O1 Ni1 120.8(3) . . ? C5 O1 Ni2 117.6(3) . . ? Ni1 O1 Ni2 121.40(19) . . ? C22 O2 Ni1 89.5(4) . . ? C22 O3 Ni1 89.6(4) . . ? C24 O4 Ni1 141.9(4) . . ? C24 O5 Ni2 125.9(4) . . ? C26 O6 Ni2 121.9(4) . . ? C9 N1 C8 107.6(5) . . ? C9 N1 C11 111.2(5) . . ? C8 N1 C11 112.4(5) . . ? C9 N1 Ni1 110.9(4) . . ? C8 N1 Ni1 108.9(4) . . ? C11 N1 Ni1 106.0(4) . . ? C13 N2 C12 109.6(5) . . ? C13 N2 C14 106.9(5) . . ? C12 N2 C14 110.4(5) . . ? C13 N2 Ni1 115.3(4) . . ? C12 N2 Ni1 105.2(4) . . ? C14 N2 Ni1 109.3(4) . . ? C15 N3 C16 113.0(5) . . ? C15 N3 Ni2 111.2(4) . . ? C16 N3 Ni2 110.1(4) . . ? C17 N4 C21 117.8(5) . . ? C17 N4 Ni2 116.2(4) . . ? C21 N4 Ni2 126.0(4) . . ? C7 C2 C3 116.9(6) . . ? C7 C2 C1 122.4(6) . . ? C3 C2 C1 120.7(6) . . ? C4 C3 C2 121.9(6) . . ? C3 C4 C5 119.5(6) . . ? C3 C4 C15 120.9(6) . . ? C5 C4 C15 119.6(5) . . ? O1 C5 C4 120.2(6) . . ? O1 C5 C6 120.6(6) . . ? C4 C5 C6 119.2(6) . . ? C7 C6 C5 118.9(6) . . ? C7 C6 C8 121.7(6) . . ? C5 C6 C8 119.3(6) . . ? C6 C7 C2 123.6(6) . . ? C6 C8 N1 115.2(5) . . ? N1 C9 C10 116.3(5) . . ? C12 C11 N1 112.3(5) . . ? N2 C12 C11 112.8(5) . . ? N3 C15 C4 110.9(5) . . ? N3 C16 C17 112.3(5) . . ? N4 C17 C18 122.6(6) . . ? N4 C17 C16 116.1(5) . . ? C18 C17 C16 121.3(6) . . ? C19 C18 C17 118.8(6) . . ? C18 C19 C20 119.6(6) . . ? C21 C20 C19 118.3(6) . . ? N4 C21 C20 122.9(6) . . ? O3 C22 O2 117.2(6) . . ? O3 C22 C23 122.1(6) . . ? O2 C22 C23 120.6(6) . . ? O3 C22 Ni1 59.5(3) . . ? O2 C22 Ni1 59.1(3) . . ? C23 C22 Ni1 169.6(5) . . ? O4 C24 O5 124.9(6) . . ? O4 C24 C25 117.3(6) . . ? O5 C24 C25 117.7(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ni1 Ni2 O1 -134.3(3) . . . . ? N2 Ni1 Ni2 O1 -56.4(3) . . . . ? O2 Ni1 Ni2 O1 133.6(3) . . . . ? N1 Ni1 Ni2 O1 43.2(3) . . . . ? O3 Ni1 Ni2 O1 169.2(3) . . . . ? C22 Ni1 Ni2 O1 152.8(3) . . . . ? O1 Ni1 Ni2 N4 -55.2(3) . . . . ? O4 Ni1 Ni2 N4 170.45(19) . . . . ? N2 Ni1 Ni2 N4 -111.6(2) . . . . ? O2 Ni1 Ni2 N4 78.37(18) . . . . ? N1 Ni1 Ni2 N4 -12.0(2) . . . . ? O3 Ni1 Ni2 N4 114.0(2) . . . . ? C22 Ni1 Ni2 N4 97.6(2) . . . . ? O1 Ni1 Ni2 O5 120.9(3) . . . . ? O4 Ni1 Ni2 O5 -13.44(17) . . . . ? N2 Ni1 Ni2 O5 64.5(2) . . . . ? O2 Ni1 Ni2 O5 -105.52(16) . . . . ? N1 Ni1 Ni2 O5 164.09(19) . . . . ? O3 Ni1 Ni2 O5 -69.89(19) . . . . ? C22 Ni1 Ni2 O5 -86.3(2) . . . . ? O1 Ni1 Ni2 O7 -145.1(3) . . . . ? O4 Ni1 Ni2 O7 80.60(17) . . . . ? N2 Ni1 Ni2 O7 158.5(2) . . . . ? O2 Ni1 Ni2 O7 -11.48(16) . . . . ? N1 Ni1 Ni2 O7 -101.87(19) . . . . ? O3 Ni1 Ni2 O7 24.15(19) . . . . ? C22 Ni1 Ni2 O7 7.8(2) . . . . ? O1 Ni1 Ni2 N3 33.4(3) . . . . ? O4 Ni1 Ni2 N3 -101.0(2) . . . . ? N2 Ni1 Ni2 N3 -23.0(2) . . . . ? O2 Ni1 Ni2 N3 166.9(2) . . . . ? N1 Ni1 Ni2 N3 76.5(2) . . . . ? O3 Ni1 Ni2 N3 -157.4(2) . . . . ? C22 Ni1 Ni2 N3 -173.8(2) . . . . ? O1 Ni1 Ni2 O6 -176.5(3) . . . . ? O4 Ni1 Ni2 O6 49.2(3) . . . . ? N2 Ni1 Ni2 O6 127.1(3) . . . . ? O2 Ni1 Ni2 O6 -42.9(3) . . . . ? N1 Ni1 Ni2 O6 -133.3(3) . . . . ? O3 Ni1 Ni2 O6 -7.2(3) . . . . ? C22 Ni1 Ni2 O6 -23.6(3) . . . . ? O4 Ni1 O1 C5 -144.6(4) . . . . ? N2 Ni1 O1 C5 -53.4(4) . . . . ? O2 Ni1 O1 C5 128.5(4) . . . . ? N1 Ni1 O1 C5 32.8(4) . . . . ? O3 Ni1 O1 C5 150.9(5) . . . . ? C22 Ni1 O1 C5 139.7(4) . . . . ? Ni2 Ni1 O1 C5 174.6(5) . . . . ? O4 Ni1 O1 Ni2 40.8(2) . . . . ? N2 Ni1 O1 Ni2 132.0(2) . . . . ? O2 Ni1 O1 Ni2 -46.1(2) . . . . ? N1 Ni1 O1 Ni2 -141.8(2) . . . . ? O3 Ni1 O1 Ni2 -23.7(6) . . . . ? C22 Ni1 O1 Ni2 -34.9(3) . . . . ? N4 Ni2 O1 C5 -46.5(4) . . . . ? O5 Ni2 O1 C5 128.8(4) . . . . ? O7 Ni2 O1 C5 -141.4(4) . . . . ? N3 Ni2 O1 C5 34.5(4) . . . . ? O6 Ni2 O1 C5 -88(5) . . . . ? Ni1 Ni2 O1 C5 -174.8(5) . . . . ? N4 Ni2 O1 Ni1 128.3(2) . . . . ? O5 Ni2 O1 Ni1 -56.4(2) . . . . ? O7 Ni2 O1 Ni1 33.4(2) . . . . ? N3 Ni2 O1 Ni1 -150.8(2) . . . . ? O6 Ni2 O1 Ni1 86(5) . . . . ? O1 Ni1 O2 C22 163.3(3) . . . . ? O4 Ni1 O2 C22 76.2(4) . . . . ? N2 Ni1 O2 C22 -11.1(7) . . . . ? N1 Ni1 O2 C22 -102.8(4) . . . . ? O3 Ni1 O2 C22 -8.1(3) . . . . ? Ni2 Ni1 O2 C22 142.1(3) . . . . ? O1 Ni1 O3 C22 -17.0(7) . . . . ? O4 Ni1 O3 C22 -82.2(4) . . . . ? N2 Ni1 O3 C22 -172.9(4) . . . . ? O2 Ni1 O3 C22 8.2(3) . . . . ? N1 Ni1 O3 C22 100.5(4) . . . . ? Ni2 Ni1 O3 C22 -32.3(4) . . . . ? O1 Ni1 O4 C24 5.8(7) . . . . ? N2 Ni1 O4 C24 -94.3(7) . . . . ? O2 Ni1 O4 C24 105.4(7) . . . . ? N1 Ni1 O4 C24 -97(4) . . . . ? O3 Ni1 O4 C24 167.3(7) . . . . ? C22 Ni1 O4 C24 136.3(7) . . . . ? Ni2 Ni1 O4 C24 26.4(7) . . . . ? O1 Ni2 O5 C24 38.3(5) . . . . ? N4 Ni2 O5 C24 143(2) . . . . ? O7 Ni2 O5 C24 -58.7(5) . . . . ? N3 Ni2 O5 C24 130.8(5) . . . . ? O6 Ni2 O5 C24 -140.6(5) . . . . ? Ni1 Ni2 O5 C24 13.6(4) . . . . ? O1 Ni2 O6 C26 -5(6) . . . . ? N4 Ni2 O6 C26 -46.8(5) . . . . ? O5 Ni2 O6 C26 137.9(5) . . . . ? O7 Ni2 O6 C26 48.2(4) . . . . ? N3 Ni2 O6 C26 -127.8(5) . . . . ? Ni1 Ni2 O6 C26 78.4(5) . . . . ? O1 Ni1 N1 C9 134.9(4) . . . . ? O4 Ni1 N1 C9 -122(4) . . . . ? N2 Ni1 N1 C9 -125.2(4) . . . . ? O2 Ni1 N1 C9 35.0(4) . . . . ? O3 Ni1 N1 C9 -27.0(4) . . . . ? C22 Ni1 N1 C9 3.9(4) . . . . ? Ni2 Ni1 N1 C9 115.1(3) . . . . ? O1 Ni1 N1 C8 16.7(4) . . . . ? O4 Ni1 N1 C8 119(4) . . . . ? N2 Ni1 N1 C8 116.6(4) . . . . ? O2 Ni1 N1 C8 -83.1(4) . . . . ? O3 Ni1 N1 C8 -145.2(4) . . . . ? C22 Ni1 N1 C8 -114.3(4) . . . . ? Ni2 Ni1 N1 C8 -3.0(4) . . . . ? O1 Ni1 N1 C11 -104.4(4) . . . . ? O4 Ni1 N1 C11 -2(4) . . . . ? N2 Ni1 N1 C11 -4.4(4) . . . . ? O2 Ni1 N1 C11 155.8(4) . . . . ? O3 Ni1 N1 C11 93.7(4) . . . . ? C22 Ni1 N1 C11 124.6(4) . . . . ? Ni2 Ni1 N1 C11 -124.1(3) . . . . ? O1 Ni1 N2 C13 -47.8(5) . . . . ? O4 Ni1 N2 C13 39.9(5) . . . . ? O2 Ni1 N2 C13 126.5(6) . . . . ? N1 Ni1 N2 C13 -140.2(5) . . . . ? O3 Ni1 N2 C13 123.8(4) . . . . ? C22 Ni1 N2 C13 119.1(5) . . . . ? Ni2 Ni1 N2 C13 -23.2(5) . . . . ? O1 Ni1 N2 C12 73.1(4) . . . . ? O4 Ni1 N2 C12 160.9(4) . . . . ? O2 Ni1 N2 C12 -112.5(6) . . . . ? N1 Ni1 N2 C12 -19.2(4) . . . . ? O3 Ni1 N2 C12 -115.2(4) . . . . ? C22 Ni1 N2 C12 -119.9(4) . . . . ? Ni2 Ni1 N2 C12 97.8(4) . . . . ? O1 Ni1 N2 C14 -168.3(4) . . . . ? O4 Ni1 N2 C14 -80.6(4) . . . . ? O2 Ni1 N2 C14 6.0(8) . . . . ? N1 Ni1 N2 C14 99.3(4) . . . . ? O3 Ni1 N2 C14 3.3(4) . . . . ? C22 Ni1 N2 C14 -1.4(5) . . . . ? Ni2 Ni1 N2 C14 -143.7(4) . . . . ? O1 Ni2 N3 C15 19.9(4) . . . . ? N4 Ni2 N3 C15 108.9(4) . . . . ? O5 Ni2 N3 C15 -72.1(4) . . . . ? O7 Ni2 N3 C15 175.8(9) . . . . ? O6 Ni2 N3 C15 -161.6(4) . . . . ? Ni1 Ni2 N3 C15 4.3(4) . . . . ? O1 Ni2 N3 C16 -106.1(4) . . . . ? N4 Ni2 N3 C16 -17.1(4) . . . . ? O5 Ni2 N3 C16 161.9(4) . . . . ? O7 Ni2 N3 C16 49.8(12) . . . . ? O6 Ni2 N3 C16 72.4(4) . . . . ? Ni1 Ni2 N3 C16 -121.7(4) . . . . ? O1 Ni2 N4 C17 101.5(4) . . . . ? O5 Ni2 N4 C17 -4(2) . . . . ? O7 Ni2 N4 C17 -161.5(4) . . . . ? N3 Ni2 N4 C17 9.0(4) . . . . ? O6 Ni2 N4 C17 -79.7(4) . . . . ? Ni1 Ni2 N4 C17 125.0(4) . . . . ? O1 Ni2 N4 C21 -77.3(5) . . . . ? O5 Ni2 N4 C21 177.5(19) . . . . ? O7 Ni2 N4 C21 19.7(5) . . . . ? N3 Ni2 N4 C21 -169.8(5) . . . . ? O6 Ni2 N4 C21 101.5(5) . . . . ? Ni1 Ni2 N4 C21 -53.8(5) . . . . ? C7 C2 C3 C4 0.3(9) . . . . ? C1 C2 C3 C4 -178.7(6) . . . . ? C2 C3 C4 C5 -1.1(9) . . . . ? C2 C3 C4 C15 179.2(6) . . . . ? Ni1 O1 C5 C4 135.6(5) . . . . ? Ni2 O1 C5 C4 -49.6(6) . . . . ? Ni1 O1 C5 C6 -44.6(7) . . . . ? Ni2 O1 C5 C6 130.2(5) . . . . ? C3 C4 C5 O1 -178.1(5) . . . . ? C15 C4 C5 O1 1.6(8) . . . . ? C3 C4 C5 C6 2.1(9) . . . . ? C15 C4 C5 C6 -178.2(6) . . . . ? O1 C5 C6 C7 178.0(5) . . . . ? C4 C5 C6 C7 -2.2(9) . . . . ? O1 C5 C6 C8 -2.5(9) . . . . ? C4 C5 C6 C8 177.3(5) . . . . ? C5 C6 C7 C2 1.4(9) . . . . ? C8 C6 C7 C2 -178.1(6) . . . . ? C3 C2 C7 C6 -0.4(9) . . . . ? C1 C2 C7 C6 178.5(6) . . . . ? C7 C6 C8 N1 -117.3(6) . . . . ? C5 C6 C8 N1 63.2(8) . . . . ? C9 N1 C8 C6 178.6(5) . . . . ? C11 N1 C8 C6 55.9(7) . . . . ? Ni1 N1 C8 C6 -61.2(6) . . . . ? C8 N1 C9 C10 -65.2(6) . . . . ? C11 N1 C9 C10 58.3(7) . . . . ? Ni1 N1 C9 C10 175.9(4) . . . . ? C9 N1 C11 C12 148.6(5) . . . . ? C8 N1 C11 C12 -90.7(6) . . . . ? Ni1 N1 C11 C12 28.1(6) . . . . ? C13 N2 C12 C11 165.7(5) . . . . ? C14 N2 C12 C11 -76.7(6) . . . . ? Ni1 N2 C12 C11 41.1(6) . . . . ? N1 C11 C12 N2 -48.5(7) . . . . ? C16 N3 C15 C4 60.0(6) . . . . ? Ni2 N3 C15 C4 -64.3(6) . . . . ? C3 C4 C15 N3 -117.8(6) . . . . ? C5 C4 C15 N3 62.5(7) . . . . ? C15 N3 C16 C17 -102.5(6) . . . . ? Ni2 N3 C16 C17 22.5(6) . . . . ? C21 N4 C17 C18 -2.7(9) . . . . ? Ni2 N4 C17 C18 178.5(5) . . . . ? C21 N4 C17 C16 -179.5(5) . . . . ? Ni2 N4 C17 C16 1.6(7) . . . . ? N3 C16 C17 N4 -16.4(8) . . . . ? N3 C16 C17 C18 166.7(6) . . . . ? N4 C17 C18 C19 1.4(10) . . . . ? C16 C17 C18 C19 178.2(6) . . . . ? C17 C18 C19 C20 1.2(10) . . . . ? C18 C19 C20 C21 -2.4(10) . . . . ? C17 N4 C21 C20 1.3(9) . . . . ? Ni2 N4 C21 C20 -179.9(5) . . . . ? C19 C20 C21 N4 1.2(10) . . . . ? Ni1 O3 C22 O2 -13.4(5) . . . . ? Ni1 O3 C22 C23 167.9(5) . . . . ? Ni1 O2 C22 O3 13.5(6) . . . . ? Ni1 O2 C22 C23 -167.9(5) . . . . ? O1 Ni1 C22 O3 172.4(3) . . . . ? O4 Ni1 C22 O3 93.5(4) . . . . ? N2 Ni1 C22 O3 9.1(5) . . . . ? O2 Ni1 C22 O3 -166.1(6) . . . . ? N1 Ni1 C22 O3 -84.3(4) . . . . ? Ni2 Ni1 C22 O3 155.5(3) . . . . ? O1 Ni1 C22 O2 -21.5(4) . . . . ? O4 Ni1 C22 O2 -100.4(3) . . . . ? N2 Ni1 C22 O2 175.2(3) . . . . ? N1 Ni1 C22 O2 81.7(3) . . . . ? O3 Ni1 C22 O2 166.1(6) . . . . ? Ni2 Ni1 C22 O2 -38.4(3) . . . . ? O1 Ni1 C22 C23 70(3) . . . . ? O4 Ni1 C22 C23 -9(3) . . . . ? N2 Ni1 C22 C23 -93(3) . . . . ? O2 Ni1 C22 C23 92(3) . . . . ? N1 Ni1 C22 C23 173(3) . . . . ? O3 Ni1 C22 C23 -102(3) . . . . ? Ni2 Ni1 C22 C23 53(3) . . . . ? Ni1 O4 C24 O5 -25.7(11) . . . . ? Ni1 O4 C24 C25 153.7(5) . . . . ? Ni2 O5 C24 O4 -5.0(9) . . . . ? Ni2 O5 C24 C25 175.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.063 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.119 data_ifn253m _database_code_CSD 194357 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H88 F12 N8 Ni4 O15 P2' _chemical_formula_weight 1590.08 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 20.653(6) _cell_length_b 10.707(3) _cell_length_c 31.627(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.049(5) _cell_angle_gamma 90.00 _cell_volume 6989(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 778 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 1.203 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6995 _exptl_absorpt_correction_T_max 0.8892 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43495 _diffrn_reflns_av_R_equivalents 0.1417 _diffrn_reflns_av_sigmaI/netI 0.2919 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.42 _reflns_number_total 16858 _reflns_number_gt 5464 _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^)+(0.0593P)^2^+0.0000P] 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 16858 _refine_ls_number_parameters 857 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.2149 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.80689(4) 0.63576(8) 0.03114(3) 0.0251(2) Uani 1 1 d . . . Ni2 Ni 0.76039(4) 0.39231(8) 0.08839(3) 0.0263(2) Uani 1 1 d . . . O1 O 0.8245(2) 0.5297(4) 0.08027(13) 0.0246(11) Uani 1 1 d . . . O2 O 0.7084(2) 0.6545(4) 0.03662(14) 0.0306(12) Uani 1 1 d . . . O3 O 0.6862(2) 0.5233(4) 0.08997(14) 0.0281(11) Uani 1 1 d . . . O4 O 0.7895(2) 0.5058(4) -0.01245(14) 0.0312(12) Uani 1 1 d . . . O5 O 0.7404(2) 0.3590(4) 0.02581(14) 0.0320(12) Uani 1 1 d . . . O7 O 0.6865(2) 0.2580(4) 0.09829(14) 0.0283(11) Uani 1 1 d . . . H7A H 0.6507 0.2779 0.1156 0.034 Uiso 1 1 d R . . N1 N 0.9030(3) 0.6525(5) 0.01349(17) 0.0297(14) Uani 1 1 d . . . N2 N 0.8231(3) 0.8119(5) 0.05900(17) 0.0280(14) Uani 1 1 d . . . N3 N 0.7793(3) 0.3955(5) 0.15351(16) 0.0251(13) Uani 1 1 d . . . H3 H 0.7395 0.3963 0.1663 0.030 Uiso 1 1 calc R . . N4 N 0.8352(3) 0.2641(5) 0.09232(17) 0.0264(13) Uani 1 1 d . . . C1 C 1.0597(3) 0.5655(7) 0.1772(2) 0.040(2) Uani 1 1 d . . . H1A H 1.0950 0.5798 0.1580 0.060 Uiso 1 1 calc R . . H1B H 1.0688 0.4902 0.1940 0.060 Uiso 1 1 calc R . . H1C H 1.0560 0.6374 0.1962 0.060 Uiso 1 1 calc R . . C2 C 0.9962(4) 0.5485(6) 0.1517(2) 0.0322(18) Uani 1 1 d . . . C3 C 0.9383(3) 0.5272(6) 0.1704(2) 0.0300(17) Uani 1 1 d . . . H3' H 0.9380 0.5166 0.2003 0.036 Uiso 1 1 calc R . . C4 C 0.8803(3) 0.5208(6) 0.1472(2) 0.0249(16) Uani 1 1 d . . . C5 C 0.8803(3) 0.5344(6) 0.1034(2) 0.0212(15) Uani 1 1 d . . . C6 C 0.9392(3) 0.5505(6) 0.0834(2) 0.0215(15) Uani 1 1 d . . . C7 C 0.9948(3) 0.5596(6) 0.1078(2) 0.0287(17) Uani 1 1 d . . . H7 H 1.0344 0.5742 0.0942 0.034 Uiso 1 1 calc R . . C8 C 0.9407(3) 0.5536(6) 0.0363(2) 0.0299(17) Uani 1 1 d . . . H8A H 0.9865 0.5616 0.0285 0.036 Uiso 1 1 calc R . . H8B H 0.9250 0.4718 0.0255 0.036 Uiso 1 1 calc R . . C9 C 0.9279(3) 0.7784(6) 0.0262(2) 0.0337(18) Uani 1 1 d . . . H9A H 0.9206 0.8378 0.0025 0.040 Uiso 1 1 calc R . . H9B H 0.9751 0.7736 0.0325 0.040 Uiso 1 1 calc R . . C10 C 0.8936(3) 0.8255(6) 0.0650(2) 0.0292(17) Uani 1 1 d . . . H10A H 0.9088 0.7775 0.0902 0.035 Uiso 1 1 calc R . . H10B H 0.9046 0.9145 0.0699 0.035 Uiso 1 1 calc R . . C11 C 0.7929(3) 0.8266(6) 0.1003(2) 0.0359(19) Uani 1 1 d . . . H11A H 0.7458 0.8174 0.0966 0.054 Uiso 1 1 calc R . . H11B H 0.8030 0.9096 0.1118 0.054 Uiso 1 1 calc R . . H11C H 0.8097 0.7625 0.1199 0.054 Uiso 1 1 calc R . . C12 C 0.7971(4) 0.9086(6) 0.0299(2) 0.040(2) Uani 1 1 d . . . H12A H 0.7501 0.8979 0.0260 0.061 Uiso 1 1 calc R . . H12B H 0.8175 0.9008 0.0026 0.061 Uiso 1 1 calc R . . H12C H 0.8064 0.9914 0.0419 0.061 Uiso 1 1 calc R . . C13 C 0.9124(3) 0.6322(7) -0.0326(2) 0.0325(18) Uani 1 1 d . . . H13A H 0.9037 0.5433 -0.0394 0.039 Uiso 1 1 calc R . . H13B H 0.9582 0.6494 -0.0388 0.039 Uiso 1 1 calc R . . C14 C 0.8693(4) 0.7129(7) -0.0612(2) 0.044(2) Uani 1 1 d . . . H14A H 0.8778 0.6943 -0.0908 0.066 Uiso 1 1 calc R . . H14B H 0.8786 0.8012 -0.0554 0.066 Uiso 1 1 calc R . . H14C H 0.8238 0.6954 -0.0558 0.066 Uiso 1 1 calc R . . C15 C 0.8152(3) 0.5082(6) 0.1686(2) 0.0267(16) Uani 1 1 d . . . H15A H 0.8229 0.5029 0.1996 0.032 Uiso 1 1 calc R . . H15B H 0.7887 0.5835 0.1625 0.032 Uiso 1 1 calc R . . C16 C 0.8113(3) 0.2768(6) 0.1654(2) 0.0326(18) Uani 1 1 d . . . H16A H 0.7782 0.2113 0.1692 0.039 Uiso 1 1 calc R . . H16B H 0.8361 0.2872 0.1925 0.039 Uiso 1 1 calc R . . C17 C 0.8564(3) 0.2373(6) 0.1313(2) 0.0250(16) Uani 1 1 d . . . C18 C 0.9148(4) 0.1775(6) 0.1396(2) 0.0353(19) Uani 1 1 d . . . H18 H 0.9284 0.1589 0.1679 0.042 Uiso 1 1 calc R . . C19 C 0.9531(4) 0.1451(7) 0.1065(3) 0.040(2) Uani 1 1 d . . . H19 H 0.9937 0.1051 0.1117 0.048 Uiso 1 1 calc R . . C20 C 0.9317(3) 0.1715(6) 0.0661(2) 0.0342(19) Uani 1 1 d . . . H20 H 0.9571 0.1495 0.0428 0.041 Uiso 1 1 calc R . . C21 C 0.8726(3) 0.2307(6) 0.0595(2) 0.0308(17) Uani 1 1 d . . . H21 H 0.8577 0.2485 0.0314 0.037 Uiso 1 1 calc R . . C22 C 0.6715(3) 0.6088(6) 0.0643(2) 0.0268(16) Uani 1 1 d . . . C23 C 0.6052(3) 0.6663(7) 0.0661(3) 0.048(2) Uani 1 1 d . . . H23A H 0.6003 0.7314 0.0445 0.073 Uiso 1 1 calc R . . H23B H 0.5997 0.7031 0.0942 0.073 Uiso 1 1 calc R . . H23C H 0.5722 0.6017 0.0610 0.073 Uiso 1 1 calc R . . C24 C 0.7574(3) 0.4070(6) -0.0082(2) 0.0266(17) Uani 1 1 d . . . C25 C 0.7349(3) 0.3400(7) -0.0487(2) 0.0383(19) Uani 1 1 d . . . H25A H 0.7507 0.3850 -0.0732 0.057 Uiso 1 1 calc R . . H25B H 0.6875 0.3371 -0.0504 0.057 Uiso 1 1 calc R . . H25C H 0.7522 0.2547 -0.0485 0.057 Uiso 1 1 calc R . . C26 C 0.6911(3) 0.1382(6) 0.0789(2) 0.0369(19) Uani 1 1 d . . . H26A H 0.6538 0.0872 0.0864 0.055 Uiso 1 1 calc R . . H26B H 0.7311 0.0971 0.0889 0.055 Uiso 1 1 calc R . . H26C H 0.6914 0.1481 0.0481 0.055 Uiso 1 1 calc R . . Ni1A Ni 0.39696(4) 0.26317(9) 0.09879(3) 0.0316(2) Uani 1 1 d . . . Ni2A Ni 0.53611(4) 0.34731(8) 0.15318(3) 0.0279(2) Uani 1 1 d . . . O1A O 0.4619(2) 0.2254(4) 0.14512(14) 0.0319(12) Uani 1 1 d . . . O2A O 0.4670(2) 0.3070(4) 0.05621(14) 0.0358(13) Uani 1 1 d . . . O3A O 0.5631(2) 0.3207(4) 0.09129(14) 0.0301(12) Uani 1 1 d . . . O4A O 0.3867(2) 0.4474(5) 0.11500(15) 0.0410(13) Uani 1 1 d . . . O5A O 0.4875(2) 0.5041(4) 0.13686(14) 0.0338(12) Uani 1 1 d . . . O6A O 0.3281(2) 0.3327(4) 0.05089(15) 0.0448(14) Uani 1 1 d . . . H1SA H 0.3105 0.2805 0.0314 0.054 Uiso 1 1 d R . . H1SB H 0.3170 0.4140 0.0507 0.054 Uiso 1 1 d R . . O7A O 0.6199(2) 0.4650(4) 0.15993(14) 0.0316(12) Uani 1 1 d . . . H7' H 0.6584 0.4439 0.1454 0.038 Uiso 1 1 d R . . N1A N 0.3184(3) 0.2050(6) 0.13760(19) 0.0422(17) Uani 1 1 d . . . N2A N 0.3892(3) 0.0756(5) 0.07270(18) 0.0346(15) Uani 1 1 d . . . N3A N 0.5968(3) 0.2083(5) 0.17576(18) 0.0298(14) Uani 1 1 d . . . H3A H 0.6363 0.2208 0.1632 0.036 Uiso 1 1 calc R . . N4A N 0.5193(3) 0.3676(5) 0.21556(19) 0.0339(15) Uani 1 1 d . . . C1A C 0.4376(4) -0.2092(7) 0.2480(3) 0.059(3) Uani 1 1 d . . . H1A1 H 0.3927 -0.2166 0.2567 0.089 Uiso 1 1 calc R . . H1A2 H 0.4667 -0.2048 0.2731 0.089 Uiso 1 1 calc R . . H1A3 H 0.4488 -0.2822 0.2310 0.089 Uiso 1 1 calc R . . C2A C 0.4450(4) -0.0910(7) 0.2217(2) 0.040(2) Uani 1 1 d . . . C3A C 0.5038(4) -0.0574(6) 0.2055(2) 0.0346(18) Uani 1 1 d . . . H3A' H 0.5408 -0.1082 0.2115 0.042 Uiso 1 1 calc R . . C4A C 0.5103(3) 0.0500(6) 0.1806(2) 0.0267(16) Uani 1 1 d . . . C5A C 0.4563(3) 0.1269(6) 0.1715(2) 0.0284(17) Uani 1 1 d . . . C6A C 0.3973(3) 0.0979(7) 0.1889(2) 0.0315(18) Uani 1 1 d . . . C7A C 0.3928(4) -0.0111(7) 0.2131(2) 0.039(2) Uani 1 1 d . . . H7A' H 0.3521 -0.0316 0.2243 0.046 Uiso 1 1 calc R . . C8A C 0.3425(3) 0.1843(7) 0.1814(2) 0.040(2) Uani 1 1 d . . . H8A1 H 0.3059 0.1534 0.1978 0.048 Uiso 1 1 calc R . . H8A2 H 0.3553 0.2664 0.1934 0.048 Uiso 1 1 calc R . . C9A C 0.2921(4) 0.0873(8) 0.1177(3) 0.052(2) Uani 1 1 d . . . H9A1 H 0.2617 0.1092 0.0940 0.063 Uiso 1 1 calc R . . H9A2 H 0.2677 0.0403 0.1389 0.063 Uiso 1 1 calc R . . C10A C 0.3451(4) 0.0056(7) 0.1015(3) 0.054(2) Uani 1 1 d . . . H10C H 0.3254 -0.0657 0.0859 0.065 Uiso 1 1 calc R . . H10D H 0.3711 -0.0282 0.1258 0.065 Uiso 1 1 calc R . . C11A C 0.4520(4) 0.0115(7) 0.0721(2) 0.049(2) Uani 1 1 d . . . H11D H 0.4715 0.0093 0.1008 0.073 Uiso 1 1 calc R . . H11E H 0.4807 0.0564 0.0533 0.073 Uiso 1 1 calc R . . H11F H 0.4456 -0.0740 0.0617 0.073 Uiso 1 1 calc R . . C12A C 0.3600(4) 0.0784(8) 0.0306(2) 0.056(2) Uani 1 1 d . . . H12D H 0.3181 0.1214 0.0311 0.084 Uiso 1 1 calc R . . H12E H 0.3534 -0.0072 0.0203 0.084 Uiso 1 1 calc R . . H12F H 0.3885 0.1230 0.0116 0.084 Uiso 1 1 calc R . . C13A C 0.2668(3) 0.3001(8) 0.1376(3) 0.052(2) Uani 1 1 d . . . H13C H 0.2518 0.3144 0.1079 0.062 Uiso 1 1 calc R . . H13D H 0.2860 0.3793 0.1482 0.062 Uiso 1 1 calc R . . C14A C 0.2073(4) 0.2714(10) 0.1636(3) 0.074(3) Uani 1 1 d . . . H14D H 0.1767 0.3412 0.1612 0.111 Uiso 1 1 calc R . . H14E H 0.2208 0.2596 0.1933 0.111 Uiso 1 1 calc R . . H14F H 0.1863 0.1951 0.1528 0.111 Uiso 1 1 calc R . . C15A C 0.5746(3) 0.0818(6) 0.1628(2) 0.0335(18) Uani 1 1 d . . . H15C H 0.6072 0.0194 0.1726 0.040 Uiso 1 1 calc R . . H15D H 0.5711 0.0776 0.1315 0.040 Uiso 1 1 calc R . . C16A C 0.6097(3) 0.2225(7) 0.2221(2) 0.0380(19) Uani 1 1 d . . . H16C H 0.6528 0.2614 0.2271 0.046 Uiso 1 1 calc R . . H16D H 0.6107 0.1389 0.2355 0.046 Uiso 1 1 calc R . . C17A C 0.5589(4) 0.3019(6) 0.2427(2) 0.0338(19) Uani 1 1 d . . . C18A C 0.5566(4) 0.3119(7) 0.2860(2) 0.045(2) Uani 1 1 d . . . H18A H 0.5872 0.2686 0.3037 0.054 Uiso 1 1 calc R . . C19A C 0.5097(5) 0.3852(7) 0.3034(3) 0.052(2) Uani 1 1 d . . . H19A H 0.5064 0.3910 0.3332 0.062 Uiso 1 1 calc R . . C20A C 0.4680(4) 0.4494(8) 0.2769(3) 0.050(2) Uani 1 1 d . . . H20A H 0.4353 0.5010 0.2880 0.061 Uiso 1 1 calc R . . C21A C 0.4741(4) 0.4382(7) 0.2338(2) 0.041(2) Uani 1 1 d . . . H21A H 0.4445 0.4832 0.2159 0.049 Uiso 1 1 calc R . . C22A C 0.5270(4) 0.3181(6) 0.0582(2) 0.0305(18) Uani 1 1 d . . . C23A C 0.5607(4) 0.3347(8) 0.0167(2) 0.051(2) Uani 1 1 d . . . H23D H 0.6075 0.3427 0.0222 0.077 Uiso 1 1 calc R . . H23E H 0.5443 0.4102 0.0024 0.077 Uiso 1 1 calc R . . H23F H 0.5521 0.2619 -0.0015 0.077 Uiso 1 1 calc R . . C24A C 0.4300(4) 0.5262(7) 0.1252(2) 0.038(2) Uani 1 1 d . . . C25A C 0.4116(4) 0.6653(7) 0.1240(3) 0.066(3) Uani 1 1 d . . . H25D H 0.4494 0.7158 0.1326 0.099 Uiso 1 1 calc R . . H25E H 0.3765 0.6805 0.1435 0.099 Uiso 1 1 calc R . . H25F H 0.3971 0.6884 0.0953 0.099 Uiso 1 1 calc R . . C26A C 0.6193(4) 0.5804(9) 0.1873(3) 0.079(3) Uani 1 1 d . . . H26D H 0.6615 0.6220 0.1866 0.119 Uiso 1 1 calc R . . H26E H 0.6105 0.5566 0.2165 0.119 Uiso 1 1 calc R . . H26F H 0.5854 0.6375 0.1767 0.119 Uiso 1 1 calc R . . P1 P 0.75571(10) 0.4245(2) 0.28825(6) 0.0378(5) Uani 1 1 d D . . P2 P 0.10967(10) 0.89036(19) 0.07924(7) 0.0385(5) Uani 1 1 d . . . F1 F 0.7925(9) 0.409(2) 0.3347(4) 0.064(5) Uani 0.488(19) 1 d PDU A 1 F1' F 0.7773(9) 0.477(2) 0.3339(4) 0.062(4) Uani 0.512(19) 1 d PDU A 2 F2 F 0.6864(2) 0.4687(5) 0.30355(16) 0.0761(16) Uani 1 1 d . A . F3 F 0.7269(2) 0.4111(5) 0.24217(13) 0.0627(14) Uani 1 1 d . A . F4 F 0.8252(2) 0.3863(4) 0.27238(13) 0.0549(13) Uani 1 1 d . A . F5 F 0.7373(3) 0.2891(5) 0.29954(18) 0.0873(18) Uani 1 1 d . A . F6 F 0.7816(12) 0.5663(12) 0.2864(7) 0.056(4) Uani 0.488(19) 1 d PDU A 1 F6' F 0.7642(11) 0.5645(12) 0.2687(6) 0.058(4) Uani 0.512(19) 1 d PDU A 2 F7 F 0.1154(2) 1.0034(4) 0.11237(15) 0.0621(14) Uani 1 1 d . . . F8 F 0.0442(2) 0.8467(4) 0.09932(14) 0.0531(12) Uani 1 1 d . . . F9 F 0.1496(2) 0.8040(4) 0.11080(14) 0.0621(14) Uani 1 1 d . . . F10 F 0.1048(2) 0.7780(4) 0.04580(14) 0.0566(13) Uani 1 1 d . . . F11 F 0.1755(2) 0.9354(5) 0.05889(15) 0.0665(15) Uani 1 1 d . . . F12 F 0.0694(2) 0.9781(4) 0.04701(14) 0.0566(13) Uani 1 1 d . . . O1W O 0.2028(8) -0.1204(15) 0.1952(6) 0.191(7) Uiso 0.711(15) 1 d PU B 1 O1W' O 0.234(2) -0.147(4) 0.2334(15) 0.189(7) Uiso 0.289(15) 1 d PU B 2 O2W' O 0.2864(12) 0.575(3) 0.2150(14) 0.254(10) Uiso 0.61(3) 1 d PU C 1 O2W O 0.2899(19) 0.592(4) 0.249(2) 0.253(10) Uiso 0.39(3) 1 d PU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0309(5) 0.0180(5) 0.0265(5) 0.0007(4) 0.0025(4) -0.0003(4) Ni2 0.0313(5) 0.0183(5) 0.0294(5) 0.0003(4) 0.0043(4) -0.0011(4) O1 0.030(3) 0.020(3) 0.024(3) 0.000(2) 0.000(2) -0.002(2) O2 0.038(3) 0.021(3) 0.032(3) 0.007(2) 0.001(2) -0.004(2) O3 0.034(3) 0.018(3) 0.032(3) 0.004(2) 0.007(2) -0.006(2) O4 0.041(3) 0.022(3) 0.031(3) -0.002(2) 0.008(2) -0.008(2) O5 0.044(3) 0.021(3) 0.031(3) 0.001(2) 0.002(2) -0.009(2) O7 0.037(3) 0.012(2) 0.037(3) -0.004(2) 0.011(2) 0.000(2) N1 0.042(4) 0.021(3) 0.026(3) 0.004(3) -0.003(3) -0.003(3) N2 0.036(4) 0.025(3) 0.023(3) 0.006(3) 0.000(3) 0.002(3) N3 0.031(3) 0.010(3) 0.035(3) 0.003(3) 0.012(3) 0.001(3) N4 0.030(3) 0.020(3) 0.029(3) -0.003(3) 0.003(3) -0.005(3) C1 0.035(4) 0.054(5) 0.031(4) 0.003(4) -0.001(4) 0.007(4) C2 0.044(5) 0.019(4) 0.033(4) 0.004(3) -0.006(4) 0.003(4) C3 0.044(5) 0.020(4) 0.026(4) -0.001(3) 0.004(4) 0.000(4) C4 0.032(4) 0.015(4) 0.028(4) 0.001(3) 0.006(3) -0.004(3) C5 0.030(4) 0.011(3) 0.022(4) 0.003(3) 0.000(3) 0.004(3) C6 0.034(4) 0.007(3) 0.024(4) -0.001(3) 0.008(3) 0.000(3) C7 0.037(4) 0.020(4) 0.030(4) 0.001(3) 0.004(4) 0.004(3) C8 0.036(4) 0.024(4) 0.030(4) 0.001(3) 0.010(3) 0.002(4) C9 0.039(4) 0.020(4) 0.042(5) 0.002(3) 0.009(4) -0.005(4) C10 0.036(4) 0.022(4) 0.030(4) 0.000(3) 0.002(3) -0.008(3) C11 0.039(4) 0.023(4) 0.045(5) -0.015(4) 0.000(4) -0.004(4) C12 0.051(5) 0.026(4) 0.044(5) 0.005(4) -0.001(4) -0.002(4) C13 0.039(4) 0.030(4) 0.029(4) 0.003(3) 0.006(3) -0.002(4) C14 0.056(5) 0.043(5) 0.033(5) 0.011(4) -0.004(4) 0.002(4) C15 0.036(4) 0.014(4) 0.030(4) -0.001(3) 0.004(3) -0.005(3) C16 0.053(5) 0.021(4) 0.024(4) 0.007(3) 0.004(4) 0.001(4) C17 0.035(4) 0.013(4) 0.027(4) -0.002(3) 0.002(3) -0.003(3) C18 0.044(5) 0.024(4) 0.038(5) -0.001(4) 0.001(4) 0.003(4) C19 0.033(4) 0.024(4) 0.062(6) -0.003(4) -0.005(4) 0.006(4) C20 0.026(4) 0.026(4) 0.051(5) -0.005(4) 0.006(4) -0.004(3) C21 0.038(4) 0.013(4) 0.041(5) -0.007(3) 0.005(4) -0.008(3) C22 0.038(4) 0.019(4) 0.024(4) 0.001(3) 0.008(3) 0.011(4) C23 0.039(5) 0.047(5) 0.061(6) 0.025(4) 0.024(4) 0.008(4) C24 0.029(4) 0.021(4) 0.030(4) 0.000(3) 0.003(3) 0.002(3) C25 0.047(5) 0.035(5) 0.033(5) -0.004(4) -0.002(4) -0.007(4) C26 0.048(5) 0.021(4) 0.044(5) -0.006(4) 0.018(4) -0.007(4) Ni1A 0.0320(5) 0.0262(5) 0.0363(6) -0.0014(4) -0.0046(4) 0.0024(5) Ni2A 0.0299(5) 0.0210(5) 0.0326(5) 0.0032(4) -0.0016(4) -0.0007(4) O1A 0.033(3) 0.029(3) 0.033(3) 0.006(2) -0.002(2) -0.002(2) O2A 0.041(3) 0.033(3) 0.033(3) 0.001(2) -0.006(3) 0.003(3) O3A 0.029(3) 0.033(3) 0.028(3) -0.002(2) 0.000(2) 0.001(2) O4A 0.043(3) 0.029(3) 0.050(3) -0.006(3) -0.016(3) 0.008(3) O5A 0.043(3) 0.025(3) 0.033(3) 0.008(2) -0.011(2) 0.002(3) O6A 0.051(3) 0.032(3) 0.051(3) -0.009(3) -0.015(3) 0.014(3) O7A 0.032(3) 0.027(3) 0.037(3) -0.001(2) 0.008(2) -0.001(2) N1A 0.031(4) 0.048(4) 0.047(4) -0.011(3) -0.015(3) 0.003(3) N2A 0.038(4) 0.031(4) 0.035(4) 0.001(3) -0.007(3) -0.001(3) N3A 0.027(3) 0.022(3) 0.040(4) 0.006(3) 0.001(3) -0.005(3) N4A 0.030(3) 0.023(4) 0.048(4) -0.003(3) -0.005(3) -0.003(3) C1A 0.080(7) 0.032(5) 0.067(6) 0.015(5) 0.019(5) -0.010(5) C2A 0.051(5) 0.030(5) 0.039(5) 0.006(4) 0.005(4) -0.010(4) C3A 0.044(5) 0.021(4) 0.038(5) -0.001(3) -0.003(4) -0.009(4) C4A 0.033(4) 0.013(4) 0.034(4) -0.001(3) 0.000(3) -0.008(3) C5A 0.038(4) 0.023(4) 0.024(4) 0.002(3) -0.003(3) -0.007(4) C6A 0.025(4) 0.033(5) 0.036(4) -0.004(4) -0.001(3) -0.005(4) C7A 0.045(5) 0.039(5) 0.033(5) -0.004(4) 0.011(4) -0.014(4) C8A 0.032(4) 0.050(5) 0.036(5) -0.002(4) -0.003(4) -0.004(4) C9A 0.033(5) 0.060(6) 0.064(6) -0.013(5) 0.006(4) -0.014(5) C10A 0.074(6) 0.031(5) 0.056(6) 0.003(4) -0.004(5) -0.024(5) C11A 0.054(5) 0.038(5) 0.054(6) -0.009(4) -0.003(4) 0.005(4) C12A 0.084(7) 0.047(6) 0.035(5) -0.005(4) -0.020(5) -0.001(5) C13A 0.030(5) 0.076(7) 0.049(6) -0.008(5) -0.002(4) 0.013(5) C14A 0.041(5) 0.128(10) 0.052(6) -0.004(6) -0.002(5) 0.031(6) C15A 0.040(5) 0.026(4) 0.034(4) -0.002(3) -0.012(4) 0.007(4) C16A 0.038(4) 0.039(5) 0.036(5) 0.004(4) -0.015(4) 0.004(4) C17A 0.052(5) 0.019(4) 0.029(4) 0.001(3) -0.001(4) -0.010(4) C18A 0.064(6) 0.037(5) 0.034(5) 0.000(4) -0.010(4) -0.002(5) C19A 0.101(7) 0.022(5) 0.033(5) 0.004(4) 0.017(5) -0.014(5) C20A 0.066(6) 0.037(5) 0.050(6) -0.003(4) 0.020(5) -0.001(5) C21A 0.049(5) 0.033(5) 0.043(5) -0.001(4) 0.011(4) -0.001(4) C22A 0.035(5) 0.018(4) 0.038(5) -0.003(3) -0.001(4) 0.006(4) C23A 0.052(5) 0.066(6) 0.036(5) 0.003(4) 0.006(4) 0.001(5) C24A 0.048(5) 0.036(5) 0.029(4) -0.003(4) -0.016(4) 0.005(4) C25A 0.090(7) 0.020(5) 0.086(7) -0.006(4) -0.042(6) 0.017(5) C26A 0.062(6) 0.063(7) 0.113(9) 0.009(7) 0.007(6) -0.009(6) P1 0.0416(13) 0.0416(14) 0.0308(12) -0.0041(10) 0.0079(10) -0.0141(11) P2 0.0429(13) 0.0318(12) 0.0411(13) 0.0045(10) 0.0043(10) -0.0044(11) F1 0.044(8) 0.114(14) 0.036(4) -0.016(7) 0.005(4) -0.018(9) F1' 0.043(8) 0.106(14) 0.038(4) -0.036(7) 0.012(4) -0.019(8) F2 0.061(3) 0.089(4) 0.080(4) -0.013(3) 0.038(3) -0.008(3) F3 0.056(3) 0.101(4) 0.031(3) 0.010(3) 0.004(2) -0.018(3) F4 0.047(3) 0.072(3) 0.046(3) 0.008(2) 0.011(2) 0.015(3) F5 0.091(4) 0.055(4) 0.117(5) 0.034(3) 0.019(4) -0.007(3) F6 0.063(11) 0.033(4) 0.073(12) -0.032(6) 0.011(8) -0.029(5) F6' 0.069(11) 0.037(4) 0.070(12) -0.022(6) 0.021(8) -0.027(5) F7 0.074(3) 0.035(3) 0.077(4) -0.012(3) -0.003(3) -0.007(3) F8 0.054(3) 0.048(3) 0.059(3) -0.007(2) 0.022(2) -0.011(2) F9 0.077(3) 0.056(3) 0.052(3) 0.018(2) -0.011(3) 0.019(3) F10 0.069(3) 0.045(3) 0.057(3) -0.013(2) 0.013(3) 0.002(3) F11 0.045(3) 0.068(4) 0.087(4) 0.020(3) 0.014(3) -0.018(3) F12 0.058(3) 0.047(3) 0.063(3) 0.018(2) -0.013(3) 0.002(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 O1 1.948(4) . ? Ni1 O4 1.983(4) . ? Ni1 O2 2.058(5) . ? Ni1 N1 2.089(6) . ? Ni1 N2 2.103(5) . ? Ni1 Ni2 3.3346(14) . ? Ni2 O1 2.001(4) . ? Ni2 O5 2.039(5) . ? Ni2 N4 2.067(6) . ? Ni2 O3 2.079(4) . ? Ni2 N3 2.083(5) . ? Ni2 O7 2.128(4) . ? O1 C5 1.344(7) . ? O2 C22 1.278(7) . ? O3 C22 1.255(7) . ? O4 C24 1.258(7) . ? O5 C24 1.254(7) . ? O7 C26 1.427(7) . ? N1 C8 1.486(8) . ? N1 C9 1.492(8) . ? N1 C13 1.495(8) . ? N2 C10 1.470(8) . ? N2 C12 1.473(8) . ? N2 C11 1.475(8) . ? N3 C16 1.475(8) . ? N3 C15 1.486(7) . ? N4 C17 1.324(8) . ? N4 C21 1.363(8) . ? C1 C2 1.527(9) . ? C2 C3 1.374(9) . ? C2 C7 1.392(9) . ? C3 C4 1.386(9) . ? C4 C5 1.391(8) . ? C4 C15 1.531(9) . ? C5 C6 1.402(9) . ? C6 C7 1.364(8) . ? C6 C8 1.492(8) . ? C9 C10 1.525(9) . ? C13 C14 1.515(9) . ? C16 C17 1.510(9) . ? C17 C18 1.383(9) . ? C18 C19 1.380(9) . ? C19 C20 1.366(10) . ? C20 C21 1.384(9) . ? C22 C23 1.505(9) . ? C24 C25 1.525(9) . ? Ni1A O1A 1.992(4) . ? Ni1A O4A 2.051(5) . ? Ni1A O2A 2.065(5) . ? Ni1A N1A 2.161(6) . ? Ni1A O6A 2.171(5) . ? Ni1A N2A 2.175(6) . ? Ni1A Ni2A 3.4171(14) . ? Ni2A O5A 2.014(5) . ? Ni2A O1A 2.023(5) . ? Ni2A N4A 2.027(6) . ? Ni2A N3A 2.058(5) . ? Ni2A O3A 2.074(5) . ? Ni2A O7A 2.145(4) . ? O1A C5A 1.353(7) . ? O2A C22A 1.244(8) . ? O3A C22A 1.262(8) . ? O4A C24A 1.264(8) . ? O5A C24A 1.253(8) . ? O7A C26A 1.509(10) . ? N1A C8A 1.473(9) . ? N1A C13A 1.474(9) . ? N1A C9A 1.501(9) . ? N2A C12A 1.444(8) . ? N2A C11A 1.467(8) . ? N2A C10A 1.510(9) . ? N3A C15A 1.483(8) . ? N3A C16A 1.488(8) . ? N4A C21A 1.347(9) . ? N4A C17A 1.361(8) . ? C1A C2A 1.526(10) . ? C2A C3A 1.384(10) . ? C2A C7A 1.394(10) . ? C3A C4A 1.403(9) . ? C4A C5A 1.407(9) . ? C4A C15A 1.500(9) . ? C5A C6A 1.390(9) . ? C6A C7A 1.400(9) . ? C6A C8A 1.474(9) . ? C9A C10A 1.505(10) . ? C13A C14A 1.533(10) . ? C16A C17A 1.515(10) . ? C17A C18A 1.375(9) . ? C18A C19A 1.377(11) . ? C19A C20A 1.366(11) . ? C20A C21A 1.377(10) . ? C22A C23A 1.521(10) . ? C24A C25A 1.538(10) . ? P1 F5 1.545(5) . ? P1 F3 1.561(5) . ? P1 F4 1.590(4) . ? P1 F1' 1.598(10) . ? P1 F2 1.600(5) . ? P1 F6 1.611(11) . ? P1 F6' 1.632(11) . ? P1 F1 1.637(11) . ? P2 F9 1.573(4) . ? P2 F8 1.586(4) . ? P2 F12 1.598(4) . ? P2 F11 1.600(5) . ? P2 F7 1.602(5) . ? P2 F10 1.603(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 O1 Ni1 O4 99.74(18) . . ? O1 Ni1 O2 98.42(18) . . ? O4 Ni1 O2 88.37(18) . . ? O1 Ni1 N1 96.40(19) . . ? O4 Ni1 N1 91.4(2) . . ? O2 Ni1 N1 164.99(19) . . ? O1 Ni1 N2 99.57(19) . . ? O4 Ni1 N2 160.5(2) . . ? O2 Ni1 N2 91.2(2) . . ? N1 Ni1 N2 84.1(2) . . ? O1 Ni1 Ni2 32.89(12) . . ? O4 Ni1 Ni2 77.30(13) . . ? O2 Ni1 Ni2 74.08(12) . . ? N1 Ni1 Ni2 120.48(15) . . ? N2 Ni1 Ni2 121.19(15) . . ? O1 Ni2 O5 96.68(17) . . ? O1 Ni2 N4 89.97(19) . . ? O5 Ni2 N4 93.9(2) . . ? O1 Ni2 O3 89.96(17) . . ? O5 Ni2 O3 90.99(18) . . ? N4 Ni2 O3 175.1(2) . . ? O1 Ni2 N3 90.74(18) . . ? O5 Ni2 N3 170.81(19) . . ? N4 Ni2 N3 80.7(2) . . ? O3 Ni2 N3 94.45(19) . . ? O1 Ni2 O7 175.20(17) . . ? O5 Ni2 O7 84.43(17) . . ? N4 Ni2 O7 94.63(19) . . ? O3 Ni2 O7 85.35(16) . . ? N3 Ni2 O7 88.62(19) . . ? O1 Ni2 Ni1 31.92(12) . . ? O5 Ni2 Ni1 70.26(13) . . ? N4 Ni2 Ni1 108.83(15) . . ? O3 Ni2 Ni1 73.32(12) . . ? N3 Ni2 Ni1 118.45(14) . . ? O7 Ni2 Ni1 146.11(12) . . ? C5 O1 Ni1 123.0(4) . . ? C5 O1 Ni2 121.1(4) . . ? Ni1 O1 Ni2 115.2(2) . . ? C22 O2 Ni1 129.5(4) . . ? C22 O3 Ni2 129.6(4) . . ? C24 O4 Ni1 126.8(4) . . ? C24 O5 Ni2 135.1(4) . . ? C26 O7 Ni2 119.1(4) . . ? C8 N1 C9 110.1(5) . . ? C8 N1 C13 106.6(5) . . ? C9 N1 C13 109.8(5) . . ? C8 N1 Ni1 107.2(4) . . ? C9 N1 Ni1 109.1(4) . . ? C13 N1 Ni1 113.9(4) . . ? C10 N2 C12 110.3(5) . . ? C10 N2 C11 108.9(5) . . ? C12 N2 C11 108.7(5) . . ? C10 N2 Ni1 106.6(4) . . ? C12 N2 Ni1 108.7(4) . . ? C11 N2 Ni1 113.6(4) . . ? C16 N3 C15 113.9(5) . . ? C16 N3 Ni2 107.7(4) . . ? C15 N3 Ni2 113.9(4) . . ? C17 N4 C21 118.3(6) . . ? C17 N4 Ni2 114.9(5) . . ? C21 N4 Ni2 124.8(5) . . ? C3 C2 C7 117.2(7) . . ? C3 C2 C1 122.4(6) . . ? C7 C2 C1 120.4(7) . . ? C2 C3 C4 121.9(7) . . ? C3 C4 C5 119.5(6) . . ? C3 C4 C15 121.7(6) . . ? C5 C4 C15 118.7(6) . . ? O1 C5 C4 120.5(6) . . ? O1 C5 C6 119.9(6) . . ? C4 C5 C6 119.6(6) . . ? C7 C6 C5 118.7(6) . . ? C7 C6 C8 121.1(6) . . ? C5 C6 C8 120.2(6) . . ? C6 C7 C2 123.0(7) . . ? N1 C8 C6 118.1(5) . . ? N1 C9 C10 110.5(5) . . ? N2 C10 C9 110.5(5) . . ? N1 C13 C14 113.9(6) . . ? N3 C15 C4 111.4(5) . . ? N3 C16 C17 110.0(5) . . ? N4 C17 C18 122.3(6) . . ? N4 C17 C16 114.4(6) . . ? C18 C17 C16 123.3(6) . . ? C19 C18 C17 119.4(7) . . ? C20 C19 C18 118.8(7) . . ? C19 C20 C21 119.4(7) . . ? N4 C21 C20 121.7(7) . . ? O3 C22 O2 125.9(6) . . ? O3 C22 C23 118.2(6) . . ? O2 C22 C23 115.9(6) . . ? O5 C24 O4 126.9(6) . . ? O5 C24 C25 116.2(6) . . ? O4 C24 C25 116.9(6) . . ? O1A Ni1A O4A 94.84(19) . . ? O1A Ni1A O2A 93.27(19) . . ? O4A Ni1A O2A 91.5(2) . . ? O1A Ni1A N1A 91.3(2) . . ? O4A Ni1A N1A 92.8(2) . . ? O2A Ni1A N1A 173.5(2) . . ? O1A Ni1A O6A 171.63(19) . . ? O4A Ni1A O6A 76.91(18) . . ? O2A Ni1A O6A 85.61(19) . . ? N1A Ni1A O6A 90.5(2) . . ? O1A Ni1A N2A 97.5(2) . . ? O4A Ni1A N2A 167.4(2) . . ? O2A Ni1A N2A 90.3(2) . . ? N1A Ni1A N2A 84.4(2) . . ? O6A Ni1A N2A 90.8(2) . . ? O1A Ni1A Ni2A 31.93(13) . . ? O4A Ni1A Ni2A 73.36(13) . . ? O2A Ni1A Ni2A 70.87(13) . . ? N1A Ni1A Ni2A 115.14(16) . . ? O6A Ni1A Ni2A 141.13(14) . . ? N2A Ni1A Ni2A 118.90(15) . . ? O5A Ni2A O1A 97.86(19) . . ? O5A Ni2A N4A 93.4(2) . . ? O1A Ni2A N4A 92.1(2) . . ? O5A Ni2A N3A 169.7(2) . . ? O1A Ni2A N3A 91.5(2) . . ? N4A Ni2A N3A 82.2(2) . . ? O5A Ni2A O3A 91.20(18) . . ? O1A Ni2A O3A 91.19(18) . . ? N4A Ni2A O3A 174.0(2) . . ? N3A Ni2A O3A 92.7(2) . . ? O5A Ni2A O7A 85.92(18) . . ? O1A Ni2A O7A 175.39(18) . . ? N4A Ni2A O7A 90.3(2) . . ? N3A Ni2A O7A 84.90(19) . . ? O3A Ni2A O7A 86.07(17) . . ? O5A Ni2A Ni1A 71.82(13) . . ? O1A Ni2A Ni1A 31.39(13) . . ? N4A Ni2A Ni1A 110.35(16) . . ? N3A Ni2A Ni1A 118.37(15) . . ? O3A Ni2A Ni1A 74.84(12) . . ? O7A Ni2A Ni1A 149.99(12) . . ? C5A O1A Ni1A 122.8(4) . . ? C5A O1A Ni2A 120.4(4) . . ? Ni1A O1A Ni2A 116.7(2) . . ? C22A O2A Ni1A 135.0(5) . . ? C22A O3A Ni2A 127.8(5) . . ? C24A O4A Ni1A 128.8(5) . . ? C24A O5A Ni2A 133.7(5) . . ? C26A O7A Ni2A 121.0(4) . . ? C8A N1A C13A 109.0(6) . . ? C8A N1A C9A 111.8(6) . . ? C13A N1A C9A 109.2(6) . . ? C8A N1A Ni1A 110.0(4) . . ? C13A N1A Ni1A 111.0(5) . . ? C9A N1A Ni1A 105.8(4) . . ? C12A N2A C11A 109.8(6) . . ? C12A N2A C10A 109.0(6) . . ? C11A N2A C10A 109.2(6) . . ? C12A N2A Ni1A 110.7(5) . . ? C11A N2A Ni1A 112.6(4) . . ? C10A N2A Ni1A 105.5(4) . . ? C15A N3A C16A 114.2(5) . . ? C15A N3A Ni2A 112.7(4) . . ? C16A N3A Ni2A 110.6(4) . . ? C21A N4A C17A 115.5(7) . . ? C21A N4A Ni2A 128.5(5) . . ? C17A N4A Ni2A 116.0(5) . . ? C3A C2A C7A 116.9(7) . . ? C3A C2A C1A 121.5(7) . . ? C7A C2A C1A 121.6(7) . . ? C2A C3A C4A 121.6(7) . . ? C3A C4A C5A 120.2(6) . . ? C3A C4A C15A 120.0(6) . . ? C5A C4A C15A 119.8(6) . . ? O1A C5A C6A 120.9(6) . . ? O1A C5A C4A 119.8(6) . . ? C6A C5A C4A 119.2(6) . . ? C5A C6A C7A 118.6(7) . . ? C5A C6A C8A 118.4(7) . . ? C7A C6A C8A 123.0(7) . . ? C2A C7A C6A 123.5(7) . . ? N1A C8A C6A 118.6(6) . . ? N1A C9A C10A 112.0(6) . . ? C9A C10A N2A 112.3(6) . . ? N1A C13A C14A 117.1(7) . . ? N3A C15A C4A 111.8(6) . . ? N3A C16A C17A 112.3(6) . . ? N4A C17A C18A 123.1(7) . . ? N4A C17A C16A 115.4(6) . . ? C18A C17A C16A 121.3(7) . . ? C17A C18A C19A 119.5(8) . . ? C20A C19A C18A 118.6(8) . . ? C19A C20A C21A 119.1(8) . . ? N4A C21A C20A 124.2(8) . . ? O2A C22A O3A 127.1(7) . . ? O2A C22A C23A 116.9(7) . . ? O3A C22A C23A 116.0(7) . . ? O5A C24A O4A 127.2(7) . . ? O5A C24A C25A 114.9(7) . . ? O4A C24A C25A 117.9(7) . . ? F5 P1 F3 92.3(3) . . ? F5 P1 F4 93.6(3) . . ? F3 P1 F4 90.0(3) . . ? F5 P1 F1' 100.8(8) . . ? F3 P1 F1' 163.7(8) . . ? F4 P1 F1' 98.7(7) . . ? F5 P1 F2 88.7(3) . . ? F3 P1 F2 89.7(3) . . ? F4 P1 F2 177.7(3) . . ? F1' P1 F2 81.1(7) . . ? F5 P1 F6 168.0(8) . . ? F3 P1 F6 99.7(7) . . ? F4 P1 F6 85.8(10) . . ? F1' P1 F6 67.5(9) . . ? F2 P1 F6 91.9(10) . . ? F5 P1 F6' 168.5(7) . . ? F3 P1 F6' 76.9(7) . . ? F4 P1 F6' 90.4(9) . . ? F1' P1 F6' 89.2(8) . . ? F2 P1 F6' 87.3(9) . . ? F6 P1 F6' 23.2(7) . . ? F5 P1 F1 78.9(8) . . ? F3 P1 F1 167.7(8) . . ? F4 P1 F1 82.1(7) . . ? F1' P1 F1 28.5(7) . . ? F2 P1 F1 98.7(7) . . ? F6 P1 F1 89.1(8) . . ? F6' P1 F1 112.3(8) . . ? F9 P2 F8 90.5(3) . . ? F9 P2 F12 179.7(3) . . ? F8 P2 F12 89.8(3) . . ? F9 P2 F11 89.9(3) . . ? F8 P2 F11 179.6(3) . . ? F12 P2 F11 89.8(3) . . ? F9 P2 F7 90.2(3) . . ? F8 P2 F7 90.3(3) . . ? F12 P2 F7 89.9(3) . . ? F11 P2 F7 89.5(3) . . ? F9 P2 F10 89.8(3) . . ? F8 P2 F10 90.5(2) . . ? F12 P2 F10 90.1(3) . . ? F11 P2 F10 89.8(3) . . ? F7 P2 F10 179.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ni1 Ni2 O1 131.9(3) . . . . ? O2 Ni1 Ni2 O1 -136.2(3) . . . . ? N1 Ni1 Ni2 O1 47.8(3) . . . . ? N2 Ni1 Ni2 O1 -54.7(3) . . . . ? O1 Ni1 Ni2 O5 -144.1(3) . . . . ? O4 Ni1 Ni2 O5 -12.18(19) . . . . ? O2 Ni1 Ni2 O5 79.77(19) . . . . ? N1 Ni1 Ni2 O5 -96.3(2) . . . . ? N2 Ni1 Ni2 O5 161.2(2) . . . . ? O1 Ni1 Ni2 N4 -56.7(3) . . . . ? O4 Ni1 Ni2 N4 75.1(2) . . . . ? O2 Ni1 Ni2 N4 167.1(2) . . . . ? N1 Ni1 Ni2 N4 -9.0(2) . . . . ? N2 Ni1 Ni2 N4 -111.4(2) . . . . ? O1 Ni1 Ni2 O3 118.7(3) . . . . ? O4 Ni1 Ni2 O3 -109.46(18) . . . . ? O2 Ni1 Ni2 O3 -17.51(18) . . . . ? N1 Ni1 Ni2 O3 166.4(2) . . . . ? N2 Ni1 Ni2 O3 64.0(2) . . . . ? O1 Ni1 Ni2 N3 32.7(3) . . . . ? O4 Ni1 Ni2 N3 164.6(2) . . . . ? O2 Ni1 Ni2 N3 -103.5(2) . . . . ? N1 Ni1 Ni2 N3 80.5(2) . . . . ? N2 Ni1 Ni2 N3 -22.0(2) . . . . ? O1 Ni1 Ni2 O7 171.9(3) . . . . ? O4 Ni1 Ni2 O7 -56.2(3) . . . . ? O2 Ni1 Ni2 O7 35.8(3) . . . . ? N1 Ni1 Ni2 O7 -140.3(3) . . . . ? N2 Ni1 Ni2 O7 117.2(3) . . . . ? O4 Ni1 O1 C5 122.5(4) . . . . ? O2 Ni1 O1 C5 -147.7(4) . . . . ? N1 Ni1 O1 C5 29.9(5) . . . . ? N2 Ni1 O1 C5 -55.1(5) . . . . ? Ni2 Ni1 O1 C5 170.0(6) . . . . ? O4 Ni1 O1 Ni2 -47.5(2) . . . . ? O2 Ni1 O1 Ni2 42.3(2) . . . . ? N1 Ni1 O1 Ni2 -140.0(2) . . . . ? N2 Ni1 O1 Ni2 134.9(2) . . . . ? O5 Ni2 O1 C5 -136.4(4) . . . . ? N4 Ni2 O1 C5 -42.5(4) . . . . ? O3 Ni2 O1 C5 132.6(4) . . . . ? N3 Ni2 O1 C5 38.2(4) . . . . ? O7 Ni2 O1 C5 121(2) . . . . ? Ni1 Ni2 O1 C5 -170.2(6) . . . . ? O5 Ni2 O1 Ni1 33.8(2) . . . . ? N4 Ni2 O1 Ni1 127.7(2) . . . . ? O3 Ni2 O1 Ni1 -57.2(2) . . . . ? N3 Ni2 O1 Ni1 -151.7(2) . . . . ? O7 Ni2 O1 Ni1 -69(2) . . . . ? O1 Ni1 O2 C22 -0.1(6) . . . . ? O4 Ni1 O2 C22 99.5(6) . . . . ? N1 Ni1 O2 C22 -171.0(7) . . . . ? N2 Ni1 O2 C22 -99.9(6) . . . . ? Ni2 Ni1 O2 C22 22.3(5) . . . . ? O1 Ni2 O3 C22 52.0(6) . . . . ? O5 Ni2 O3 C22 -44.6(6) . . . . ? N4 Ni2 O3 C22 141(2) . . . . ? N3 Ni2 O3 C22 142.8(6) . . . . ? O7 Ni2 O3 C22 -129.0(6) . . . . ? Ni1 Ni2 O3 C22 24.4(5) . . . . ? O1 Ni1 O4 C24 41.3(5) . . . . ? O2 Ni1 O4 C24 -56.9(5) . . . . ? N1 Ni1 O4 C24 138.1(5) . . . . ? N2 Ni1 O4 C24 -145.8(6) . . . . ? Ni2 Ni1 O4 C24 17.1(5) . . . . ? O1 Ni2 O5 C24 -3.2(6) . . . . ? N4 Ni2 O5 C24 -93.6(6) . . . . ? O3 Ni2 O5 C24 86.8(6) . . . . ? N3 Ni2 O5 C24 -146.8(11) . . . . ? O7 Ni2 O5 C24 172.1(6) . . . . ? Ni1 Ni2 O5 C24 15.0(6) . . . . ? O1 Ni2 O7 C26 157.4(19) . . . . ? O5 Ni2 O7 C26 53.8(5) . . . . ? N4 Ni2 O7 C26 -39.6(5) . . . . ? O3 Ni2 O7 C26 145.3(5) . . . . ? N3 Ni2 O7 C26 -120.2(5) . . . . ? Ni1 Ni2 O7 C26 94.9(5) . . . . ? O1 Ni1 N1 C8 15.5(4) . . . . ? O4 Ni1 N1 C8 -84.5(4) . . . . ? O2 Ni1 N1 C8 -173.6(6) . . . . ? N2 Ni1 N1 C8 114.5(4) . . . . ? Ni2 Ni1 N1 C8 -8.4(4) . . . . ? O1 Ni1 N1 C9 -103.8(4) . . . . ? O4 Ni1 N1 C9 156.3(4) . . . . ? O2 Ni1 N1 C9 67.2(9) . . . . ? N2 Ni1 N1 C9 -4.8(4) . . . . ? Ni2 Ni1 N1 C9 -127.6(4) . . . . ? O1 Ni1 N1 C13 133.2(4) . . . . ? O4 Ni1 N1 C13 33.2(4) . . . . ? O2 Ni1 N1 C13 -55.9(10) . . . . ? N2 Ni1 N1 C13 -127.8(4) . . . . ? Ni2 Ni1 N1 C13 109.3(4) . . . . ? O1 Ni1 N2 C10 74.8(4) . . . . ? O4 Ni1 N2 C10 -98.1(7) . . . . ? O2 Ni1 N2 C10 173.5(4) . . . . ? N1 Ni1 N2 C10 -20.7(4) . . . . ? Ni2 Ni1 N2 C10 101.5(4) . . . . ? O1 Ni1 N2 C12 -166.3(4) . . . . ? O4 Ni1 N2 C12 20.8(9) . . . . ? O2 Ni1 N2 C12 -67.5(4) . . . . ? N1 Ni1 N2 C12 98.2(5) . . . . ? Ni2 Ni1 N2 C12 -139.6(4) . . . . ? O1 Ni1 N2 C11 -45.1(4) . . . . ? O4 Ni1 N2 C11 142.0(6) . . . . ? O2 Ni1 N2 C11 53.6(4) . . . . ? N1 Ni1 N2 C11 -140.7(4) . . . . ? Ni2 Ni1 N2 C11 -18.4(5) . . . . ? O1 Ni2 N3 C16 -112.9(4) . . . . ? O5 Ni2 N3 C16 31.0(14) . . . . ? N4 Ni2 N3 C16 -23.0(4) . . . . ? O3 Ni2 N3 C16 157.1(4) . . . . ? O7 Ni2 N3 C16 71.9(4) . . . . ? Ni1 Ni2 N3 C16 -129.4(4) . . . . ? O1 Ni2 N3 C15 14.4(4) . . . . ? O5 Ni2 N3 C15 158.3(11) . . . . ? N4 Ni2 N3 C15 104.3(4) . . . . ? O3 Ni2 N3 C15 -75.6(4) . . . . ? O7 Ni2 N3 C15 -160.8(4) . . . . ? Ni1 Ni2 N3 C15 -2.2(5) . . . . ? O1 Ni2 N4 C17 95.1(5) . . . . ? O5 Ni2 N4 C17 -168.2(5) . . . . ? O3 Ni2 N4 C17 6(3) . . . . ? N3 Ni2 N4 C17 4.3(5) . . . . ? O7 Ni2 N4 C17 -83.5(5) . . . . ? Ni1 Ni2 N4 C17 121.3(4) . . . . ? O1 Ni2 N4 C21 -68.6(5) . . . . ? O5 Ni2 N4 C21 28.1(5) . . . . ? O3 Ni2 N4 C21 -158(2) . . . . ? N3 Ni2 N4 C21 -159.4(5) . . . . ? O7 Ni2 N4 C21 112.8(5) . . . . ? Ni1 Ni2 N4 C21 -42.4(5) . . . . ? C7 C2 C3 C4 -2.0(10) . . . . ? C1 C2 C3 C4 175.3(6) . . . . ? C2 C3 C4 C5 0.9(10) . . . . ? C2 C3 C4 C15 -174.7(6) . . . . ? Ni1 O1 C5 C4 142.2(5) . . . . ? Ni2 O1 C5 C4 -48.4(7) . . . . ? Ni1 O1 C5 C6 -39.2(7) . . . . ? Ni2 O1 C5 C6 130.2(5) . . . . ? C3 C4 C5 O1 -179.4(6) . . . . ? C15 C4 C5 O1 -3.7(9) . . . . ? C3 C4 C5 C6 2.1(9) . . . . ? C15 C4 C5 C6 177.8(6) . . . . ? O1 C5 C6 C7 177.6(6) . . . . ? C4 C5 C6 C7 -3.8(9) . . . . ? O1 C5 C6 C8 -4.2(9) . . . . ? C4 C5 C6 C8 174.4(6) . . . . ? C5 C6 C7 C2 2.8(10) . . . . ? C8 C6 C7 C2 -175.5(6) . . . . ? C3 C2 C7 C6 0.1(10) . . . . ? C1 C2 C7 C6 -177.3(6) . . . . ? C9 N1 C8 C6 61.8(7) . . . . ? C13 N1 C8 C6 -179.1(6) . . . . ? Ni1 N1 C8 C6 -56.8(6) . . . . ? C7 C6 C8 N1 -121.6(7) . . . . ? C5 C6 C8 N1 60.2(8) . . . . ? C8 N1 C9 C10 -88.3(7) . . . . ? C13 N1 C9 C10 154.6(6) . . . . ? Ni1 N1 C9 C10 29.0(6) . . . . ? C12 N2 C10 C9 -75.3(7) . . . . ? C11 N2 C10 C9 165.4(5) . . . . ? Ni1 N2 C10 C9 42.5(6) . . . . ? N1 C9 C10 N2 -48.9(7) . . . . ? C8 N1 C13 C14 171.4(6) . . . . ? C9 N1 C13 C14 -69.4(7) . . . . ? Ni1 N1 C13 C14 53.4(7) . . . . ? C16 N3 C15 C4 65.6(7) . . . . ? Ni2 N3 C15 C4 -58.4(6) . . . . ? C3 C4 C15 N3 -123.0(7) . . . . ? C5 C4 C15 N3 61.4(8) . . . . ? C15 N3 C16 C17 -90.3(6) . . . . ? Ni2 N3 C16 C17 37.0(6) . . . . ? C21 N4 C17 C18 0.2(9) . . . . ? Ni2 N4 C17 C18 -164.6(5) . . . . ? C21 N4 C17 C16 -179.4(5) . . . . ? Ni2 N4 C17 C16 15.8(7) . . . . ? N3 C16 C17 N4 -35.9(8) . . . . ? N3 C16 C17 C18 144.6(6) . . . . ? N4 C17 C18 C19 0.7(10) . . . . ? C16 C17 C18 C19 -179.8(6) . . . . ? C17 C18 C19 C20 -1.0(10) . . . . ? C18 C19 C20 C21 0.5(10) . . . . ? C17 N4 C21 C20 -0.7(9) . . . . ? Ni2 N4 C21 C20 162.4(5) . . . . ? C19 C20 C21 N4 0.4(10) . . . . ? Ni2 O3 C22 O2 -18.6(10) . . . . ? Ni2 O3 C22 C23 162.8(5) . . . . ? Ni1 O2 C22 O3 -14.0(10) . . . . ? Ni1 O2 C22 C23 164.7(5) . . . . ? Ni2 O5 C24 O4 -8.4(11) . . . . ? Ni2 O5 C24 C25 173.5(4) . . . . ? Ni1 O4 C24 O5 -14.5(10) . . . . ? Ni1 O4 C24 C25 163.7(4) . . . . ? O1A Ni1A Ni2A O5A -144.5(3) . . . . ? O4A Ni1A Ni2A O5A -14.3(2) . . . . ? O2A Ni1A Ni2A O5A 83.3(2) . . . . ? N1A Ni1A Ni2A O5A -99.4(2) . . . . ? O6A Ni1A Ni2A O5A 27.4(3) . . . . ? N2A Ni1A Ni2A O5A 162.7(2) . . . . ? O4A Ni1A Ni2A O1A 130.3(3) . . . . ? O2A Ni1A Ni2A O1A -132.1(3) . . . . ? N1A Ni1A Ni2A O1A 45.1(3) . . . . ? O6A Ni1A Ni2A O1A 171.9(3) . . . . ? N2A Ni1A Ni2A O1A -52.8(3) . . . . ? O1A Ni1A Ni2A N4A -57.7(3) . . . . ? O4A Ni1A Ni2A N4A 72.5(2) . . . . ? O2A Ni1A Ni2A N4A 170.1(2) . . . . ? N1A Ni1A Ni2A N4A -12.6(3) . . . . ? O6A Ni1A Ni2A N4A 114.1(3) . . . . ? N2A Ni1A Ni2A N4A -110.5(3) . . . . ? O1A Ni1A Ni2A N3A 34.3(3) . . . . ? O4A Ni1A Ni2A N3A 164.5(2) . . . . ? O2A Ni1A Ni2A N3A -97.9(2) . . . . ? N1A Ni1A Ni2A N3A 79.4(3) . . . . ? O6A Ni1A Ni2A N3A -153.9(3) . . . . ? N2A Ni1A Ni2A N3A -18.5(3) . . . . ? O1A Ni1A Ni2A O3A 119.0(3) . . . . ? O4A Ni1A Ni2A O3A -110.7(2) . . . . ? O2A Ni1A Ni2A O3A -13.09(19) . . . . ? N1A Ni1A Ni2A O3A 164.2(2) . . . . ? O6A Ni1A Ni2A O3A -69.1(2) . . . . ? N2A Ni1A Ni2A O3A 66.3(2) . . . . ? O1A Ni1A Ni2A O7A 171.4(4) . . . . ? O4A Ni1A Ni2A O7A -58.4(3) . . . . ? O2A Ni1A Ni2A O7A 39.2(3) . . . . ? N1A Ni1A Ni2A O7A -143.5(3) . . . . ? O6A Ni1A Ni2A O7A -16.7(3) . . . . ? N2A Ni1A Ni2A O7A 118.6(3) . . . . ? O4A Ni1A O1A C5A 130.0(5) . . . . ? O2A Ni1A O1A C5A -138.2(5) . . . . ? N1A Ni1A O1A C5A 37.1(5) . . . . ? O6A Ni1A O1A C5A 139.7(12) . . . . ? N2A Ni1A O1A C5A -47.4(5) . . . . ? Ni2A Ni1A O1A C5A 177.2(6) . . . . ? O4A Ni1A O1A Ni2A -47.2(3) . . . . ? O2A Ni1A O1A Ni2A 44.6(3) . . . . ? N1A Ni1A O1A Ni2A -140.1(3) . . . . ? O6A Ni1A O1A Ni2A -37.5(14) . . . . ? N2A Ni1A O1A Ni2A 135.3(3) . . . . ? O5A Ni2A O1A C5A -143.5(5) . . . . ? N4A Ni2A O1A C5A -49.8(5) . . . . ? N3A Ni2A O1A C5A 32.4(5) . . . . ? O3A Ni2A O1A C5A 125.1(5) . . . . ? O7A Ni2A O1A C5A 72(2) . . . . ? Ni1A Ni2A O1A C5A -177.3(6) . . . . ? O5A Ni2A O1A Ni1A 33.8(3) . . . . ? N4A Ni2A O1A Ni1A 127.5(3) . . . . ? N3A Ni2A O1A Ni1A -150.3(3) . . . . ? O3A Ni2A O1A Ni1A -57.6(2) . . . . ? O7A Ni2A O1A Ni1A -111(2) . . . . ? O1A Ni1A O2A C22A -5.9(7) . . . . ? O4A Ni1A O2A C22A 89.1(6) . . . . ? N1A Ni1A O2A C22A -140.2(18) . . . . ? O6A Ni1A O2A C22A 165.8(7) . . . . ? N2A Ni1A O2A C22A -103.4(7) . . . . ? Ni2A Ni1A O2A C22A 17.3(6) . . . . ? O5A Ni2A O3A C22A -52.5(6) . . . . ? O1A Ni2A O3A C22A 45.4(6) . . . . ? N4A Ni2A O3A C22A 168.2(18) . . . . ? N3A Ni2A O3A C22A 137.0(6) . . . . ? O7A Ni2A O3A C22A -138.3(6) . . . . ? Ni1A Ni2A O3A C22A 18.3(5) . . . . ? O1A Ni1A O4A C24A 44.1(6) . . . . ? O2A Ni1A O4A C24A -49.4(6) . . . . ? N1A Ni1A O4A C24A 135.6(6) . . . . ? O6A Ni1A O4A C24A -134.5(6) . . . . ? N2A Ni1A O4A C24A -147.6(9) . . . . ? Ni2A Ni1A O4A C24A 20.2(6) . . . . ? O1A Ni2A O5A C24A 0.1(7) . . . . ? N4A Ni2A O5A C24A -92.5(6) . . . . ? N3A Ni2A O5A C24A -156.1(11) . . . . ? O3A Ni2A O5A C24A 91.4(6) . . . . ? O7A Ni2A O5A C24A 177.4(6) . . . . ? Ni1A Ni2A O5A C24A 17.8(6) . . . . ? O5A Ni2A O7A C26A 53.2(5) . . . . ? O1A Ni2A O7A C26A -162(2) . . . . ? N4A Ni2A O7A C26A -40.2(6) . . . . ? N3A Ni2A O7A C26A -122.3(6) . . . . ? O3A Ni2A O7A C26A 144.7(5) . . . . ? Ni1A Ni2A O7A C26A 94.7(6) . . . . ? O1A Ni1A N1A C8A 9.3(5) . . . . ? O4A Ni1A N1A C8A -85.6(5) . . . . ? O2A Ni1A N1A C8A 143.8(17) . . . . ? O6A Ni1A N1A C8A -162.5(5) . . . . ? N2A Ni1A N1A C8A 106.7(5) . . . . ? Ni2A Ni1A N1A C8A -12.7(5) . . . . ? O1A Ni1A N1A C13A 130.0(5) . . . . ? O4A Ni1A N1A C13A 35.1(5) . . . . ? O2A Ni1A N1A C13A -95.5(19) . . . . ? O6A Ni1A N1A C13A -41.8(5) . . . . ? N2A Ni1A N1A C13A -132.6(5) . . . . ? Ni2A Ni1A N1A C13A 108.0(4) . . . . ? O1A Ni1A N1A C9A -111.7(5) . . . . ? O4A Ni1A N1A C9A 153.4(5) . . . . ? O2A Ni1A N1A C9A 23(2) . . . . ? O6A Ni1A N1A C9A 76.5(5) . . . . ? N2A Ni1A N1A C9A -14.3(5) . . . . ? Ni2A Ni1A N1A C9A -133.7(4) . . . . ? O1A Ni1A N2A C12A -162.8(5) . . . . ? O4A Ni1A N2A C12A 29.0(13) . . . . ? O2A Ni1A N2A C12A -69.4(5) . . . . ? N1A Ni1A N2A C12A 106.6(5) . . . . ? O6A Ni1A N2A C12A 16.2(5) . . . . ? Ni2A Ni1A N2A C12A -137.6(5) . . . . ? O1A Ni1A N2A C11A -39.5(5) . . . . ? O4A Ni1A N2A C11A 152.2(9) . . . . ? O2A Ni1A N2A C11A 53.9(5) . . . . ? N1A Ni1A N2A C11A -130.1(5) . . . . ? O6A Ni1A N2A C11A 139.5(5) . . . . ? Ni2A Ni1A N2A C11A -14.4(5) . . . . ? O1A Ni1A N2A C10A 79.5(5) . . . . ? O4A Ni1A N2A C10A -88.8(11) . . . . ? O2A Ni1A N2A C10A 172.9(5) . . . . ? N1A Ni1A N2A C10A -11.1(4) . . . . ? O6A Ni1A N2A C10A -101.5(5) . . . . ? Ni2A Ni1A N2A C10A 104.6(4) . . . . ? O5A Ni2A N3A C15A 177.7(10) . . . . ? O1A Ni2A N3A C15A 21.2(5) . . . . ? N4A Ni2A N3A C15A 113.1(5) . . . . ? O3A Ni2A N3A C15A -70.1(5) . . . . ? O7A Ni2A N3A C15A -155.9(5) . . . . ? Ni1A Ni2A N3A C15A 4.2(5) . . . . ? O5A Ni2A N3A C16A 48.5(14) . . . . ? O1A Ni2A N3A C16A -108.0(4) . . . . ? N4A Ni2A N3A C16A -16.1(4) . . . . ? O3A Ni2A N3A C16A 160.8(4) . . . . ? O7A Ni2A N3A C16A 75.0(4) . . . . ? Ni1A Ni2A N3A C16A -125.0(4) . . . . ? O5A Ni2A N4A C21A 18.3(6) . . . . ? O1A Ni2A N4A C21A -79.7(6) . . . . ? N3A Ni2A N4A C21A -170.9(6) . . . . ? O3A Ni2A N4A C21A 157.5(17) . . . . ? O7A Ni2A N4A C21A 104.3(6) . . . . ? Ni1A Ni2A N4A C21A -53.5(6) . . . . ? O5A Ni2A N4A C17A -161.4(5) . . . . ? O1A Ni2A N4A C17A 100.6(5) . . . . ? N3A Ni2A N4A C17A 9.4(5) . . . . ? O3A Ni2A N4A C17A -22(2) . . . . ? O7A Ni2A N4A C17A -75.4(5) . . . . ? Ni1A Ni2A N4A C17A 126.8(4) . . . . ? C7A C2A C3A C4A -2.0(11) . . . . ? C1A C2A C3A C4A 178.7(7) . . . . ? C2A C3A C4A C5A 0.2(11) . . . . ? C2A C3A C4A C15A -178.5(7) . . . . ? Ni1A O1A C5A C6A -44.0(8) . . . . ? Ni2A O1A C5A C6A 133.1(6) . . . . ? Ni1A O1A C5A C4A 134.0(5) . . . . ? Ni2A O1A C5A C4A -48.9(8) . . . . ? C3A C4A C5A O1A -175.5(6) . . . . ? C15A C4A C5A O1A 3.2(9) . . . . ? C3A C4A C5A C6A 2.5(10) . . . . ? C15A C4A C5A C6A -178.7(6) . . . . ? O1A C5A C6A C7A 174.7(6) . . . . ? C4A C5A C6A C7A -3.4(10) . . . . ? O1A C5A C6A C8A -6.1(10) . . . . ? C4A C5A C6A C8A 175.9(6) . . . . ? C3A C2A C7A C6A 1.1(11) . . . . ? C1A C2A C7A C6A -179.6(7) . . . . ? C5A C6A C7A C2A 1.6(11) . . . . ? C8A C6A C7A C2A -177.6(7) . . . . ? C13A N1A C8A C6A -176.5(6) . . . . ? C9A N1A C8A C6A 62.7(8) . . . . ? Ni1A N1A C8A C6A -54.5(8) . . . . ? C5A C6A C8A N1A 62.1(9) . . . . ? C7A C6A C8A N1A -118.7(8) . . . . ? C8A N1A C9A C10A -81.2(8) . . . . ? C13A N1A C9A C10A 158.1(7) . . . . ? Ni1A N1A C9A C10A 38.6(8) . . . . ? N1A C9A C10A N2A -52.4(9) . . . . ? C12A N2A C10A C9A -83.0(8) . . . . ? C11A N2A C10A C9A 157.1(6) . . . . ? Ni1A N2A C10A C9A 35.8(7) . . . . ? C8A N1A C13A C14A -59.1(9) . . . . ? C9A N1A C13A C14A 63.3(9) . . . . ? Ni1A N1A C13A C14A 179.5(6) . . . . ? C16A N3A C15A C4A 64.1(7) . . . . ? Ni2A N3A C15A C4A -63.2(6) . . . . ? C3A C4A C15A N3A -123.2(7) . . . . ? C5A C4A C15A N3A 58.0(8) . . . . ? C15A N3A C16A C17A -108.2(6) . . . . ? Ni2A N3A C16A C17A 20.1(7) . . . . ? C21A N4A C17A C18A -4.2(10) . . . . ? Ni2A N4A C17A C18A 175.5(6) . . . . ? C21A N4A C17A C16A 180.0(6) . . . . ? Ni2A N4A C17A C16A -0.3(8) . . . . ? N3A C16A C17A N4A -13.5(9) . . . . ? N3A C16A C17A C18A 170.7(6) . . . . ? N4A C17A C18A C19A 4.4(11) . . . . ? C16A C17A C18A C19A 179.9(7) . . . . ? C17A C18A C19A C20A -2.2(11) . . . . ? C18A C19A C20A C21A 0.3(12) . . . . ? C17A N4A C21A C20A 2.2(10) . . . . ? Ni2A N4A C21A C20A -177.5(6) . . . . ? C19A C20A C21A N4A -0.3(12) . . . . ? Ni1A O2A C22A O3A -10.5(11) . . . . ? Ni1A O2A C22A C23A 171.7(5) . . . . ? Ni2A O3A C22A O2A -14.9(10) . . . . ? Ni2A O3A C22A C23A 162.9(5) . . . . ? Ni2A O5A C24A O4A -10.3(12) . . . . ? Ni2A O5A C24A C25A 169.0(5) . . . . ? Ni1A O4A C24A O5A -17.2(11) . . . . ? Ni1A O4A C24A C25A 163.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.109 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.113 data_ifn291m _database_code_CSD 194358 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H88 B2 N6 Ni2 O7' _chemical_formula_weight 1240.48 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' 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 11.728(4) _cell_length_b 14.200(5) _cell_length_c 21.057(7) _cell_angle_alpha 79.907(7) _cell_angle_beta 75.858(7) _cell_angle_gamma 78.937(6) _cell_volume 3306.8(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description green _exptl_crystal_colour prism _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7792 _exptl_absorpt_correction_T_max 0.9459 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18809 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.2628 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.34 _reflns_number_total 14525 _reflns_number_gt 4937 _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. O1W was found to be disordered and refined with a 64.3 : 35.7 % occupancy ; _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^)+(0.1438P)^2^+0.0000P] 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 14525 _refine_ls_number_parameters 766 _refine_ls_number_restraints 480 _refine_ls_R_factor_all 0.2458 _refine_ls_R_factor_gt 0.0955 _refine_ls_wR_factor_ref 0.3084 _refine_ls_wR_factor_gt 0.2402 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.06109(9) 0.37088(7) 0.22433(5) 0.0354(3) Uani 1 1 d . . . Ni2 Ni 0.13845(11) 0.15308(8) 0.22530(6) 0.0532(4) Uani 1 1 d . . . B1 B -0.2522(8) 0.6841(7) 0.3845(4) 0.035(2) Uani 1 1 d . . . B2 B -0.2976(7) 0.2153(6) 0.0385(4) 0.0234(18) Uani 1 1 d . . . N1 N 0.2797(7) 0.0597(5) 0.2580(4) 0.0494(19) Uani 1 1 d . . . N2 N 0.1632(6) 0.0663(4) 0.1522(3) 0.0391(17) Uani 1 1 d . . . N3 N 0.1176(5) 0.4680(5) 0.2668(3) 0.0359(16) Uani 1 1 d . . . H3A H 0.0554 0.5189 0.2751 0.043 Uiso 1 1 calc R . . N4 N 0.1777(5) 0.4206(4) 0.1367(3) 0.0276(14) Uani 1 1 d . . . N5 N -0.1634(6) 0.3840(6) 0.1547(4) 0.063(2) Uani 1 1 d . . . H5A H -0.1160 0.3309 0.1661 0.075 Uiso 1 1 calc R . . H5B H -0.2196 0.3809 0.1344 0.075 Uiso 1 1 calc R . . N6 N -0.2202(6) 0.5478(6) 0.1475(4) 0.056(2) Uani 1 1 d . . . H6B H -0.2106 0.6049 0.1543 0.068 Uiso 1 1 calc R . . H6C H -0.2759 0.5433 0.1272 0.068 Uiso 1 1 calc R . . O1 O 0.1727(5) 0.2603(4) 0.2613(3) 0.0399(14) Uani 1 1 d . . . O2 O 0.0346(4) 0.2577(3) 0.1854(2) 0.0295(12) Uani 1 1 d . . . H2B H -0.0147 0.2564 0.1560 0.035 Uiso 1 1 calc R . . O3 O -0.0708(5) 0.4744(4) 0.1969(3) 0.0452(15) Uani 1 1 d . . . O4 O -0.0023(7) 0.1066(5) 0.2939(4) 0.094(3) Uani 1 1 d . . . H7D H -0.0791 0.1390 0.2936 0.113 Uiso 1 1 d R . . H7E H 0.0101 0.0531 0.3253 0.113 Uiso 1 1 d R . . O5 O -0.0738(7) 0.3357(7) 0.3106(4) 0.104(3) Uani 1 1 d . . . H5AA H -0.1485 0.3780 0.3197 0.124 Uiso 1 1 d R . . H5AB H -0.0588 0.2774 0.3402 0.124 Uiso 1 1 d R . . C1 C 0.4532(8) 0.2754(6) 0.3478(4) 0.0472(12) Uani 1 1 d U . . C2 C 0.3525(8) 0.3475(6) 0.3522(4) 0.0451(12) Uani 1 1 d U . . H2A H 0.3479 0.4000 0.3756 0.054 Uiso 1 1 calc R . . C3 C 0.2593(8) 0.3441(6) 0.3230(4) 0.0427(11) Uani 1 1 d U . . C4 C 0.2615(8) 0.2654(6) 0.2889(4) 0.0427(12) Uani 1 1 d U . . C5 C 0.3653(8) 0.1958(6) 0.2823(4) 0.0444(12) Uani 1 1 d U . . C6 C 0.4555(8) 0.2019(6) 0.3119(4) 0.0463(12) Uani 1 1 d U . . H6A H 0.5235 0.1529 0.3074 0.056 Uiso 1 1 calc R . . C7 C 0.5545(8) 0.2822(7) 0.3796(5) 0.060(2) Uani 1 1 d U . . H7A H 0.6173 0.2264 0.3718 0.091 Uiso 1 1 calc R . . H7B H 0.5243 0.2826 0.4273 0.091 Uiso 1 1 calc R . . H7C H 0.5869 0.3421 0.3602 0.091 Uiso 1 1 calc R . . C8 C 0.3808(8) 0.1150(6) 0.2409(4) 0.0463(15) Uani 1 1 d U . . H8A H 0.3916 0.1432 0.1938 0.056 Uiso 1 1 calc R . . H8B H 0.4543 0.0696 0.2463 0.056 Uiso 1 1 calc R . . C9 C 0.2483(10) 0.0239(7) 0.3291(5) 0.070(3) Uani 1 1 d U . . H9A H 0.1813 -0.0129 0.3368 0.084 Uiso 1 1 calc R . . H9B H 0.2195 0.0804 0.3535 0.084 Uiso 1 1 calc R . . C10 C 0.3478(10) -0.0402(7) 0.3579(5) 0.078(3) Uani 1 1 d U . . H10A H 0.3183 -0.0599 0.4052 0.118 Uiso 1 1 calc R . . H10B H 0.4140 -0.0043 0.3518 0.118 Uiso 1 1 calc R . . H10C H 0.3755 -0.0979 0.3353 0.118 Uiso 1 1 calc R . . C11 C 0.3069(9) -0.0204(7) 0.2183(5) 0.060(2) Uani 1 1 d U . . H11A H 0.3918 -0.0488 0.2143 0.072 Uiso 1 1 calc R . . H11B H 0.2588 -0.0713 0.2417 0.072 Uiso 1 1 calc R . . C12 C 0.2832(9) 0.0091(7) 0.1522(5) 0.063(2) Uani 1 1 d U . . H12A H 0.2910 -0.0495 0.1310 0.076 Uiso 1 1 calc R . . H12B H 0.3439 0.0482 0.1253 0.076 Uiso 1 1 calc R . . C13 C 0.1690(11) 0.1189(7) 0.0846(5) 0.076(3) Uani 1 1 d . . . H13A H 0.1805 0.0724 0.0534 0.114 Uiso 1 1 calc R . . H13B H 0.2358 0.1555 0.0725 0.114 Uiso 1 1 calc R . . H13C H 0.0946 0.1636 0.0831 0.114 Uiso 1 1 calc R . . C14 C 0.0738(9) 0.0008(7) 0.1677(5) 0.069(3) Uani 1 1 d . . . H14A H 0.0882 -0.0389 0.1320 0.104 Uiso 1 1 calc R . . H14B H -0.0060 0.0391 0.1721 0.104 Uiso 1 1 calc R . . H14C H 0.0798 -0.0414 0.2093 0.104 Uiso 1 1 calc R . . C15 C 0.1510(8) 0.4244(6) 0.3310(4) 0.0418(15) Uani 1 1 d U . . H15A H 0.0824 0.3974 0.3611 0.050 Uiso 1 1 calc R . . H15B H 0.1686 0.4759 0.3517 0.050 Uiso 1 1 calc R . . C16 C 0.2170(6) 0.5071(5) 0.2181(4) 0.0307(14) Uani 1 1 d U . . H16A H 0.2926 0.4631 0.2208 0.037 Uiso 1 1 calc R . . H16B H 0.2240 0.5712 0.2279 0.037 Uiso 1 1 calc R . . C17 C 0.1944(7) 0.5168(5) 0.1500(4) 0.0303(14) Uani 1 1 d U . . H17A H 0.1222 0.5649 0.1463 0.036 Uiso 1 1 calc R . . H17B H 0.2626 0.5399 0.1169 0.036 Uiso 1 1 calc R . . C18 C 0.2923(6) 0.3555(5) 0.1238(4) 0.0314(18) Uani 1 1 d . . . H18A H 0.3431 0.3817 0.0828 0.047 Uiso 1 1 calc R . . H18B H 0.2782 0.2913 0.1194 0.047 Uiso 1 1 calc R . . H18C H 0.3317 0.3500 0.1606 0.047 Uiso 1 1 calc R . . C19 C 0.1291(7) 0.4329(6) 0.0771(4) 0.037(2) Uani 1 1 d . . . H19A H 0.1877 0.4559 0.0384 0.056 Uiso 1 1 calc R . . H19B H 0.0559 0.4803 0.0819 0.056 Uiso 1 1 calc R . . H19C H 0.1115 0.3707 0.0712 0.056 Uiso 1 1 calc R . . C20 C -0.1502(7) 0.4678(7) 0.1680(4) 0.043(2) Uani 1 1 d . . . C21 C -0.3078(7) 0.1128(5) 0.0894(4) 0.0330(12) Uani 1 1 d U . . C22 C -0.3668(7) 0.0406(5) 0.0820(4) 0.0364(12) Uani 1 1 d U . . H22A H -0.4037 0.0498 0.0455 0.044 Uiso 1 1 calc R . . C23 C -0.3739(7) -0.0447(5) 0.1261(4) 0.0412(13) Uani 1 1 d U . . H23A H -0.4151 -0.0923 0.1195 0.049 Uiso 1 1 calc R . . C24 C -0.3206(7) -0.0594(6) 0.1795(4) 0.0431(13) Uani 1 1 d U . . H24A H -0.3278 -0.1164 0.2105 0.052 Uiso 1 1 calc R . . C25 C -0.2577(7) 0.0072(5) 0.1880(4) 0.0407(12) Uani 1 1 d U . . H25A H -0.2180 -0.0039 0.2236 0.049 Uiso 1 1 calc R . . C26 C -0.2530(7) 0.0926(5) 0.1430(4) 0.0369(12) Uani 1 1 d U . . H26A H -0.2101 0.1392 0.1494 0.044 Uiso 1 1 calc R . . C27 C -0.3750(6) 0.2265(5) -0.0194(4) 0.0278(11) Uani 1 1 d U . . C28 C -0.3261(7) 0.2428(5) -0.0868(3) 0.0274(11) Uani 1 1 d U . . H28A H -0.2428 0.2432 -0.1015 0.033 Uiso 1 1 calc R . . C29 C -0.3967(6) 0.2587(5) -0.1331(4) 0.0301(11) Uani 1 1 d U . . H29A H -0.3605 0.2687 -0.1788 0.036 Uiso 1 1 calc R . . C30 C -0.5183(7) 0.2603(5) -0.1141(4) 0.0309(11) Uani 1 1 d U . . H30A H -0.5660 0.2724 -0.1461 0.037 Uiso 1 1 calc R . . C31 C -0.5686(7) 0.2438(5) -0.0473(4) 0.0321(11) Uani 1 1 d U . . H31A H -0.6520 0.2440 -0.0327 0.039 Uiso 1 1 calc R . . C32 C -0.4971(6) 0.2269(5) -0.0020(4) 0.0310(11) Uani 1 1 d U . . H32A H -0.5334 0.2148 0.0435 0.037 Uiso 1 1 calc R . . C33 C -0.3608(6) 0.3102(5) 0.0789(3) 0.0250(11) Uani 1 1 d U . . C34 C -0.4083(6) 0.3058(5) 0.1462(3) 0.0255(11) Uani 1 1 d U . . H34A H -0.4037 0.2442 0.1725 0.031 Uiso 1 1 calc R . . C35 C -0.4623(6) 0.3869(5) 0.1772(4) 0.0270(11) Uani 1 1 d U . . H35A H -0.4928 0.3805 0.2236 0.032 Uiso 1 1 calc R . . C36 C -0.4711(6) 0.4778(5) 0.1390(4) 0.0290(11) Uani 1 1 d U . . H36A H -0.5069 0.5339 0.1596 0.035 Uiso 1 1 calc R . . C37 C -0.4285(6) 0.4862(5) 0.0725(4) 0.0272(11) Uani 1 1 d U . . H37A H -0.4353 0.5481 0.0466 0.033 Uiso 1 1 calc R . . C38 C -0.3748(6) 0.4042(5) 0.0425(4) 0.0268(11) Uani 1 1 d U . . H38A H -0.3465 0.4113 -0.0042 0.032 Uiso 1 1 calc R . . C39 C -0.1559(6) 0.2181(5) 0.0052(3) 0.0284(11) Uani 1 1 d U . . C40 C -0.0968(6) 0.2980(5) -0.0038(3) 0.0288(11) Uani 1 1 d U . . H40A H -0.1407 0.3559 0.0120 0.035 Uiso 1 1 calc R . . C41 C 0.0203(6) 0.2969(5) -0.0341(3) 0.0314(12) Uani 1 1 d U . . H41A H 0.0563 0.3528 -0.0378 0.038 Uiso 1 1 calc R . . C42 C 0.0873(7) 0.2144(5) -0.0594(4) 0.0340(12) Uani 1 1 d U . . H42A H 0.1685 0.2137 -0.0813 0.041 Uiso 1 1 calc R . . C43 C 0.0335(6) 0.1336(5) -0.0520(4) 0.0334(12) Uani 1 1 d U . . H43A H 0.0779 0.0764 -0.0687 0.040 Uiso 1 1 calc R . . C44 C -0.0849(6) 0.1358(5) -0.0204(3) 0.0310(12) Uani 1 1 d U . . H44A H -0.1198 0.0792 -0.0158 0.037 Uiso 1 1 calc R . . C45 C -0.2919(10) 0.7841(7) 0.4175(5) 0.0619(16) Uani 1 1 d U . . C46 C -0.3005(10) 0.7897(7) 0.4825(5) 0.0709(17) Uani 1 1 d U . . H46A H -0.2915 0.7309 0.5117 0.085 Uiso 1 1 calc R . . C47 C -0.3220(11) 0.8782(7) 0.5089(5) 0.0776(17) Uani 1 1 d U . . H47A H -0.3185 0.8790 0.5534 0.093 Uiso 1 1 calc R . . C48 C -0.3482(11) 0.9634(8) 0.4682(5) 0.0769(17) Uani 1 1 d U . . H48A H -0.3727 1.0230 0.4858 0.092 Uiso 1 1 calc R . . C49 C -0.3387(10) 0.9613(7) 0.4036(5) 0.0701(17) Uani 1 1 d U . . H49A H -0.3510 1.0201 0.3750 0.084 Uiso 1 1 calc R . . C50 C -0.3110(9) 0.8736(7) 0.3784(5) 0.0643(16) Uani 1 1 d U . . H50A H -0.3047 0.8744 0.3325 0.077 Uiso 1 1 calc R . . C51 C -0.2408(8) 0.5880(6) 0.4406(4) 0.0459(14) Uani 1 1 d U . . C52 C -0.1381(8) 0.5255(7) 0.4473(4) 0.0559(15) Uani 1 1 d U . . H52A H -0.0653 0.5399 0.4190 0.067 Uiso 1 1 calc R . . C53 C -0.1348(9) 0.4417(7) 0.4939(4) 0.0612(16) Uani 1 1 d U . . H53A H -0.0615 0.4003 0.4961 0.073 Uiso 1 1 calc R . . C54 C -0.2389(8) 0.4198(7) 0.5364(4) 0.0569(15) Uani 1 1 d U . . H54A H -0.2381 0.3643 0.5689 0.068 Uiso 1 1 calc R . . C55 C -0.3429(8) 0.4794(6) 0.5309(4) 0.0486(14) Uani 1 1 d U . . H55A H -0.4153 0.4647 0.5595 0.058 Uiso 1 1 calc R . . C56 C -0.3444(8) 0.5600(6) 0.4846(4) 0.0440(14) Uani 1 1 d U . . H56A H -0.4188 0.5992 0.4820 0.053 Uiso 1 1 calc R . . C57 C -0.3511(8) 0.6651(7) 0.3472(4) 0.0492(14) Uani 1 1 d U . . C58 C -0.4650(8) 0.7217(7) 0.3500(4) 0.0519(14) Uani 1 1 d U . . H58A H -0.4837 0.7785 0.3709 0.062 Uiso 1 1 calc R . . C59 C -0.5512(8) 0.6968(7) 0.3228(4) 0.0548(14) Uani 1 1 d U . . H59A H -0.6259 0.7377 0.3245 0.066 Uiso 1 1 calc R . . C60 C -0.5288(8) 0.6147(7) 0.2940(4) 0.0548(14) Uani 1 1 d U . . H60A H -0.5886 0.5973 0.2771 0.066 Uiso 1 1 calc R . . C61 C -0.4184(8) 0.5564(7) 0.2895(4) 0.0556(14) Uani 1 1 d U . . H61A H -0.4018 0.4987 0.2696 0.067 Uiso 1 1 calc R . . C62 C -0.3328(8) 0.5840(7) 0.3148(4) 0.0533(14) Uani 1 1 d U . . H62A H -0.2565 0.5450 0.3096 0.064 Uiso 1 1 calc R . . C63 C -0.1239(7) 0.6983(6) 0.3332(4) 0.0386(12) Uani 1 1 d U . . C64 C -0.1079(7) 0.7153(6) 0.2643(4) 0.0401(13) Uani 1 1 d U . . H64A H -0.1713 0.7104 0.2449 0.048 Uiso 1 1 calc R . . C65 C -0.0020(7) 0.7393(6) 0.2233(4) 0.0431(13) Uani 1 1 d U . . H65A H 0.0054 0.7497 0.1767 0.052 Uiso 1 1 calc R . . C66 C 0.0904(8) 0.7479(6) 0.2486(4) 0.0442(13) Uani 1 1 d U . . H66A H 0.1616 0.7657 0.2202 0.053 Uiso 1 1 calc R . . C67 C 0.0801(8) 0.7307(6) 0.3150(4) 0.0448(13) Uani 1 1 d U . . H67A H 0.1457 0.7346 0.3328 0.054 Uiso 1 1 calc R . . C68 C -0.0252(7) 0.7073(6) 0.3576(4) 0.0425(13) Uani 1 1 d U . . H68A H -0.0304 0.6973 0.4040 0.051 Uiso 1 1 calc R . . O1W O -0.078(4) -0.122(3) 0.499(2) 0.20(2) Uiso 0.357(18) 1 d P A 1 O1W' O -0.0475(11) -0.0665(9) 0.3585(6) 0.096(6) Uiso 0.643(18) 1 d P A 2 O2W O -0.064(3) 0.1904(11) 0.4247(11) 0.369(15) 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 0.0310(6) 0.0359(6) 0.0420(7) -0.0105(5) -0.0056(5) -0.0103(5) Ni2 0.0623(9) 0.0317(7) 0.0691(9) -0.0042(6) -0.0227(7) -0.0071(6) B1 0.033(5) 0.043(6) 0.030(5) -0.001(4) -0.015(4) -0.002(4) B2 0.022(4) 0.020(4) 0.026(5) -0.011(3) 0.000(3) 0.002(3) N1 0.063(5) 0.022(4) 0.061(5) -0.001(3) -0.026(4) 0.009(3) N2 0.045(4) 0.022(4) 0.057(5) -0.004(3) -0.025(4) -0.007(3) N3 0.033(4) 0.034(4) 0.040(4) -0.009(3) -0.007(3) -0.001(3) N4 0.026(3) 0.029(4) 0.029(4) -0.005(3) -0.011(3) -0.001(3) N5 0.045(5) 0.068(6) 0.088(6) -0.029(5) -0.026(4) -0.008(4) N6 0.032(4) 0.069(6) 0.076(6) -0.008(4) -0.023(4) -0.014(4) O1 0.051(4) 0.031(3) 0.043(3) -0.007(3) -0.017(3) -0.011(3) O2 0.033(3) 0.024(3) 0.042(3) -0.003(2) -0.021(2) -0.016(2) O3 0.029(3) 0.050(4) 0.065(4) -0.026(3) -0.015(3) -0.002(3) O4 0.100(6) 0.061(5) 0.110(6) -0.003(4) 0.002(5) -0.024(5) O5 0.090(6) 0.118(7) 0.090(6) 0.018(5) 0.005(5) -0.047(6) C1 0.067(3) 0.036(3) 0.038(3) -0.001(2) -0.019(2) -0.001(2) C2 0.066(3) 0.036(3) 0.035(3) -0.003(2) -0.018(2) -0.003(2) C3 0.063(3) 0.032(2) 0.034(2) -0.0041(19) -0.015(2) -0.003(2) C4 0.064(3) 0.029(2) 0.034(2) -0.002(2) -0.014(2) -0.002(2) C5 0.066(3) 0.030(2) 0.036(2) -0.0021(19) -0.016(2) 0.000(2) C6 0.066(3) 0.033(3) 0.038(3) 0.000(2) -0.017(2) 0.001(2) C7 0.072(4) 0.052(4) 0.060(5) -0.007(4) -0.029(4) 0.002(4) C8 0.067(3) 0.031(3) 0.039(3) -0.005(2) -0.017(3) 0.002(3) C9 0.102(7) 0.031(5) 0.077(6) 0.005(4) -0.035(5) -0.003(4) C10 0.112(7) 0.037(5) 0.086(6) 0.002(4) -0.040(5) 0.005(5) C11 0.073(5) 0.042(4) 0.071(5) -0.028(4) -0.033(4) 0.016(4) C12 0.076(5) 0.045(4) 0.073(5) -0.026(4) -0.032(4) 0.018(4) C13 0.135(10) 0.046(6) 0.054(7) 0.002(5) -0.033(7) -0.021(7) C14 0.074(7) 0.057(7) 0.090(8) -0.008(6) -0.026(6) -0.034(6) C15 0.061(3) 0.033(3) 0.034(3) -0.008(3) -0.014(3) -0.005(2) C16 0.030(3) 0.024(3) 0.041(3) -0.008(3) -0.011(3) -0.004(3) C17 0.030(3) 0.023(3) 0.041(3) -0.007(3) -0.009(3) -0.004(3) C18 0.034(5) 0.023(4) 0.039(5) -0.006(3) -0.008(4) -0.009(3) C19 0.039(5) 0.037(5) 0.043(5) -0.004(4) -0.022(4) -0.009(4) C20 0.027(5) 0.060(6) 0.048(6) -0.022(5) -0.004(4) -0.013(4) C21 0.039(3) 0.018(2) 0.037(3) -0.004(2) -0.003(2) 0.001(2) C22 0.045(3) 0.019(2) 0.042(3) -0.007(2) -0.003(2) 0.000(2) C23 0.049(3) 0.020(2) 0.047(3) -0.005(2) 0.000(2) -0.001(2) C24 0.050(3) 0.022(2) 0.046(3) 0.000(2) 0.001(2) 0.003(2) C25 0.047(3) 0.025(2) 0.042(3) 0.000(2) -0.004(2) 0.005(2) C26 0.042(3) 0.023(2) 0.040(3) -0.002(2) -0.005(2) 0.003(2) C27 0.035(2) 0.017(2) 0.034(2) -0.006(2) -0.008(2) -0.006(2) C28 0.035(2) 0.018(2) 0.032(2) -0.004(2) -0.0102(19) -0.005(2) C29 0.038(2) 0.021(2) 0.032(2) -0.002(2) -0.011(2) -0.002(2) C30 0.038(2) 0.021(2) 0.036(2) -0.004(2) -0.014(2) -0.004(2) C31 0.037(2) 0.023(2) 0.039(2) -0.005(2) -0.011(2) -0.005(2) C32 0.036(2) 0.021(2) 0.037(2) -0.006(2) -0.008(2) -0.005(2) C33 0.023(2) 0.023(2) 0.031(2) -0.0035(19) -0.010(2) -0.005(2) C34 0.023(2) 0.025(2) 0.031(2) -0.0032(19) -0.010(2) -0.006(2) C35 0.024(2) 0.026(2) 0.033(2) -0.0050(19) -0.009(2) -0.005(2) C36 0.025(2) 0.026(2) 0.037(2) -0.006(2) -0.008(2) -0.003(2) C37 0.024(2) 0.022(2) 0.036(2) -0.004(2) -0.009(2) -0.004(2) C38 0.025(2) 0.023(2) 0.033(2) -0.0033(19) -0.008(2) -0.004(2) C39 0.029(2) 0.026(2) 0.029(2) -0.005(2) -0.009(2) 0.0026(19) C40 0.028(2) 0.026(2) 0.032(3) -0.007(2) -0.008(2) 0.0022(19) C41 0.028(2) 0.030(2) 0.036(3) -0.006(2) -0.009(2) 0.000(2) C42 0.028(2) 0.033(2) 0.038(3) -0.004(2) -0.008(2) 0.0042(19) C43 0.031(2) 0.029(2) 0.036(3) -0.005(2) -0.007(2) 0.006(2) C44 0.031(2) 0.025(2) 0.033(3) -0.004(2) -0.007(2) 0.004(2) C45 0.101(4) 0.039(3) 0.049(3) -0.005(2) -0.018(3) -0.019(3) C46 0.117(4) 0.044(3) 0.051(3) -0.008(3) -0.012(3) -0.018(3) C47 0.125(4) 0.047(3) 0.057(3) -0.011(2) -0.007(3) -0.015(3) C48 0.120(4) 0.045(3) 0.061(3) -0.010(3) -0.006(3) -0.014(3) C49 0.108(4) 0.042(3) 0.059(3) -0.006(3) -0.013(3) -0.016(3) C50 0.102(4) 0.040(3) 0.053(3) -0.004(2) -0.017(3) -0.018(3) C51 0.048(3) 0.047(3) 0.045(3) 0.005(2) -0.018(2) -0.013(2) C52 0.052(3) 0.054(3) 0.054(3) 0.014(2) -0.014(3) -0.008(3) C53 0.058(3) 0.057(3) 0.058(3) 0.016(3) -0.012(3) -0.005(3) C54 0.058(3) 0.054(3) 0.053(3) 0.012(3) -0.013(3) -0.011(3) C55 0.052(3) 0.048(3) 0.046(3) 0.005(2) -0.014(3) -0.016(2) C56 0.047(3) 0.046(3) 0.044(3) 0.002(2) -0.018(2) -0.016(2) C57 0.052(3) 0.055(3) 0.047(3) 0.000(2) -0.021(3) -0.020(3) C58 0.054(3) 0.055(3) 0.053(3) 0.002(3) -0.023(3) -0.018(3) C59 0.055(3) 0.059(3) 0.056(3) 0.004(3) -0.025(3) -0.020(3) C60 0.058(3) 0.064(3) 0.052(3) 0.000(3) -0.025(3) -0.024(3) C61 0.060(3) 0.065(3) 0.052(3) -0.006(3) -0.022(3) -0.023(3) C62 0.056(3) 0.061(3) 0.051(3) -0.005(2) -0.021(3) -0.019(3) C63 0.043(3) 0.038(3) 0.035(2) -0.002(2) -0.012(2) -0.005(2) C64 0.046(3) 0.038(3) 0.035(3) -0.002(2) -0.010(2) -0.005(2) C65 0.048(3) 0.039(3) 0.037(3) 0.000(2) -0.007(2) -0.003(2) C66 0.045(3) 0.039(3) 0.043(3) 0.001(2) -0.006(2) -0.004(2) C67 0.044(3) 0.044(3) 0.044(3) 0.002(2) -0.011(2) -0.006(2) C68 0.043(3) 0.044(3) 0.040(3) 0.000(2) -0.013(2) -0.007(2) O2W 0.69(5) 0.095(12) 0.33(2) 0.019(13) -0.17(3) -0.039(19) _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 O1 2.016(5) . ? Ni1 O2 2.032(4) . ? Ni1 O3 2.038(6) . ? Ni1 N3 2.054(6) . ? Ni1 N4 2.110(6) . ? Ni1 O5 2.153(7) . ? Ni1 Ni2 3.0495(18) . ? Ni2 O2 1.940(5) . ? Ni2 O1 1.960(5) . ? Ni2 O4 2.041(7) . ? Ni2 N2 2.069(7) . ? Ni2 N1 2.091(7) . ? B1 C45 1.628(13) . ? B1 C57 1.635(12) . ? B1 C51 1.648(12) . ? B1 C63 1.649(12) . ? B2 C39 1.644(10) . ? B2 C21 1.655(10) . ? B2 C27 1.659(10) . ? B2 C33 1.674(10) . ? N1 C11 1.468(10) . ? N1 C9 1.473(11) . ? N1 C8 1.485(11) . ? N2 C14 1.474(10) . ? N2 C13 1.479(11) . ? N2 C12 1.483(11) . ? N3 C16 1.477(9) . ? N3 C15 1.495(9) . ? N4 C18 1.472(9) . ? N4 C19 1.472(8) . ? N4 C17 1.498(9) . ? N5 C20 1.315(11) . ? N6 C20 1.341(11) . ? O1 C4 1.329(9) . ? O3 C20 1.255(9) . ? C1 C6 1.385(11) . ? C1 C2 1.404(12) . ? C1 C7 1.524(11) . ? C2 C3 1.390(11) . ? C3 C4 1.424(11) . ? C3 C15 1.533(11) . ? C4 C5 1.408(11) . ? C5 C6 1.375(11) . ? C5 C8 1.518(11) . ? C9 C10 1.519(13) . ? C11 C12 1.460(12) . ? C16 C17 1.501(10) . ? C21 C22 1.390(10) . ? C21 C26 1.392(10) . ? C22 C23 1.394(10) . ? C23 C24 1.380(11) . ? C24 C25 1.366(11) . ? C25 C26 1.403(10) . ? C27 C32 1.388(10) . ? C27 C28 1.391(10) . ? C28 C29 1.390(9) . ? C29 C30 1.380(10) . ? C30 C31 1.383(10) . ? C31 C32 1.380(10) . ? C33 C34 1.384(9) . ? C33 C38 1.420(9) . ? C34 C35 1.391(10) . ? C35 C36 1.396(9) . ? C36 C37 1.359(10) . ? C37 C38 1.391(10) . ? C39 C40 1.401(10) . ? C39 C44 1.407(10) . ? C40 C41 1.364(9) . ? C41 C42 1.391(10) . ? C42 C43 1.381(10) . ? C43 C44 1.382(10) . ? C45 C46 1.362(12) . ? C45 C50 1.399(12) . ? C46 C47 1.417(13) . ? C47 C48 1.385(14) . ? C48 C49 1.341(13) . ? C49 C50 1.389(13) . ? C51 C52 1.374(12) . ? C51 C56 1.414(11) . ? C52 C53 1.405(12) . ? C53 C54 1.378(12) . ? C54 C55 1.362(12) . ? C55 C56 1.367(11) . ? C57 C62 1.395(12) . ? C57 C58 1.414(12) . ? C58 C59 1.401(11) . ? C59 C60 1.360(13) . ? C60 C61 1.388(13) . ? C61 C62 1.390(11) . ? C63 C64 1.401(10) . ? C63 C68 1.411(11) . ? C64 C65 1.392(11) . ? C65 C66 1.352(11) . ? C66 C67 1.356(11) . ? C67 C68 1.397(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O2 77.95(19) . . ? O1 Ni1 O3 171.7(2) . . ? O2 Ni1 O3 99.9(2) . . ? O1 Ni1 N3 91.4(2) . . ? O2 Ni1 N3 168.8(2) . . ? O3 Ni1 N3 91.1(2) . . ? O1 Ni1 N4 99.7(2) . . ? O2 Ni1 N4 93.0(2) . . ? O3 Ni1 N4 88.4(2) . . ? N3 Ni1 N4 85.4(2) . . ? O1 Ni1 O5 87.5(3) . . ? O2 Ni1 O5 89.2(3) . . ? O3 Ni1 O5 84.5(3) . . ? N3 Ni1 O5 93.7(3) . . ? N4 Ni1 O5 172.8(3) . . ? O1 Ni1 Ni2 39.24(14) . . ? O2 Ni1 Ni2 38.75(13) . . ? O3 Ni1 Ni2 137.81(15) . . ? N3 Ni1 Ni2 130.64(18) . . ? N4 Ni1 Ni2 99.57(17) . . ? O5 Ni1 Ni2 86.4(3) . . ? O2 Ni2 O1 81.5(2) . . ? O2 Ni2 O4 91.7(3) . . ? O1 Ni2 O4 104.1(3) . . ? O2 Ni2 N2 94.9(2) . . ? O1 Ni2 N2 152.8(2) . . ? O4 Ni2 N2 103.0(3) . . ? O2 Ni2 N1 167.1(2) . . ? O1 Ni2 N1 91.0(3) . . ? O4 Ni2 N1 100.3(3) . . ? N2 Ni2 N1 87.0(3) . . ? O2 Ni2 Ni1 40.96(13) . . ? O1 Ni2 Ni1 40.61(16) . . ? O4 Ni2 Ni1 98.9(2) . . ? N2 Ni2 Ni1 131.10(18) . . ? N1 Ni2 Ni1 131.1(2) . . ? C45 B1 C57 112.4(7) . . ? C45 B1 C51 112.0(7) . . ? C57 B1 C51 103.9(7) . . ? C45 B1 C63 103.7(7) . . ? C57 B1 C63 112.6(7) . . ? C51 B1 C63 112.5(7) . . ? C39 B2 C21 107.8(6) . . ? C39 B2 C27 110.9(6) . . ? C21 B2 C27 112.3(6) . . ? C39 B2 C33 112.2(6) . . ? C21 B2 C33 110.4(6) . . ? C27 B2 C33 103.3(5) . . ? C11 N1 C9 111.0(7) . . ? C11 N1 C8 109.8(7) . . ? C9 N1 C8 112.6(7) . . ? C11 N1 Ni2 104.9(5) . . ? C9 N1 Ni2 112.1(6) . . ? C8 N1 Ni2 106.0(5) . . ? C14 N2 C13 110.1(7) . . ? C14 N2 C12 109.8(7) . . ? C13 N2 C12 106.0(8) . . ? C14 N2 Ni2 111.8(6) . . ? C13 N2 Ni2 115.0(5) . . ? C12 N2 Ni2 103.7(5) . . ? C16 N3 C15 112.4(6) . . ? C16 N3 Ni1 107.8(4) . . ? C15 N3 Ni1 112.5(5) . . ? C18 N4 C19 106.5(6) . . ? C18 N4 C17 111.1(5) . . ? C19 N4 C17 110.1(5) . . ? C18 N4 Ni1 112.6(4) . . ? C19 N4 Ni1 113.8(4) . . ? C17 N4 Ni1 102.8(4) . . ? C4 O1 Ni2 130.5(5) . . ? C4 O1 Ni1 127.7(5) . . ? Ni2 O1 Ni1 100.2(2) . . ? Ni2 O2 Ni1 100.3(2) . . ? C20 O3 Ni1 129.7(6) . . ? C6 C1 C2 116.3(8) . . ? C6 C1 C7 123.5(8) . . ? C2 C1 C7 120.2(8) . . ? C3 C2 C1 121.6(8) . . ? C2 C3 C4 120.9(8) . . ? C2 C3 C15 118.7(7) . . ? C4 C3 C15 120.3(7) . . ? O1 C4 C5 121.3(7) . . ? O1 C4 C3 121.8(8) . . ? C5 C4 C3 116.8(8) . . ? C6 C5 C4 120.3(8) . . ? C6 C5 C8 119.1(8) . . ? C4 C5 C8 120.5(8) . . ? C5 C6 C1 123.9(9) . . ? N1 C8 C5 114.2(7) . . ? N1 C9 C10 115.7(9) . . ? C12 C11 N1 113.4(8) . . ? C11 C12 N2 113.2(8) . . ? N3 C15 C3 112.9(6) . . ? N3 C16 C17 109.4(6) . . ? N4 C17 C16 109.5(6) . . ? O3 C20 N5 121.4(9) . . ? O3 C20 N6 119.9(8) . . ? N5 C20 N6 118.6(8) . . ? C22 C21 C26 115.2(7) . . ? C22 C21 B2 124.3(7) . . ? C26 C21 B2 120.5(6) . . ? C21 C22 C23 122.6(8) . . ? C24 C23 C22 119.6(8) . . ? C25 C24 C23 120.6(8) . . ? C24 C25 C26 118.4(8) . . ? C21 C26 C25 123.7(8) . . ? C32 C27 C28 115.8(7) . . ? C32 C27 B2 120.4(6) . . ? C28 C27 B2 123.6(6) . . ? C29 C28 C27 121.2(7) . . ? C30 C29 C28 121.6(7) . . ? C29 C30 C31 118.1(7) . . ? C32 C31 C30 119.6(7) . . ? C31 C32 C27 123.6(7) . . ? C34 C33 C38 115.1(7) . . ? C34 C33 B2 125.7(6) . . ? C38 C33 B2 119.1(6) . . ? C33 C34 C35 123.5(7) . . ? C34 C35 C36 118.9(7) . . ? C37 C36 C35 120.2(7) . . ? C36 C37 C38 120.0(7) . . ? C37 C38 C33 122.4(7) . . ? C40 C39 C44 114.6(7) . . ? C40 C39 B2 126.2(6) . . ? C44 C39 B2 119.2(6) . . ? C41 C40 C39 123.5(7) . . ? C40 C41 C42 120.2(7) . . ? C43 C42 C41 118.7(7) . . ? C42 C43 C44 120.0(7) . . ? C43 C44 C39 122.9(7) . . ? C46 C45 C50 114.5(9) . . ? C46 C45 B1 124.4(8) . . ? C50 C45 B1 120.9(8) . . ? C45 C46 C47 123.7(10) . . ? C48 C47 C46 118.2(10) . . ? C49 C48 C47 119.7(10) . . ? C48 C49 C50 120.4(10) . . ? C49 C50 C45 123.1(9) . . ? C52 C51 C56 113.9(8) . . ? C52 C51 B1 126.1(8) . . ? C56 C51 B1 119.8(7) . . ? C51 C52 C53 123.6(9) . . ? C54 C53 C52 119.4(9) . . ? C55 C54 C53 118.8(8) . . ? C54 C55 C56 120.8(9) . . ? C55 C56 C51 123.4(8) . . ? C62 C57 C58 114.1(8) . . ? C62 C57 B1 121.3(8) . . ? C58 C57 B1 124.3(8) . . ? C59 C58 C57 122.2(9) . . ? C60 C59 C58 120.6(9) . . ? C59 C60 C61 119.9(9) . . ? C60 C61 C62 118.6(9) . . ? C61 C62 C57 124.6(10) . . ? C64 C63 C68 115.1(7) . . ? C64 C63 B1 124.1(7) . . ? C68 C63 B1 120.3(7) . . ? C65 C64 C63 122.1(8) . . ? C66 C65 C64 121.1(8) . . ? C65 C66 C67 119.1(8) . . ? C66 C67 C68 121.3(8) . . ? C67 C68 C63 121.3(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 Ni2 O2 -176.5(3) . . . . ? O3 Ni1 Ni2 O2 15.4(3) . . . . ? N3 Ni1 Ni2 O2 -175.0(3) . . . . ? N4 Ni1 Ni2 O2 -82.9(3) . . . . ? O5 Ni1 Ni2 O2 93.2(3) . . . . ? O2 Ni1 Ni2 O1 176.5(3) . . . . ? O3 Ni1 Ni2 O1 -168.1(4) . . . . ? N3 Ni1 Ni2 O1 1.5(3) . . . . ? N4 Ni1 Ni2 O1 93.6(3) . . . . ? O5 Ni1 Ni2 O1 -90.4(3) . . . . ? O1 Ni1 Ni2 O4 101.2(3) . . . . ? O2 Ni1 Ni2 O4 -82.3(3) . . . . ? O3 Ni1 Ni2 O4 -66.9(4) . . . . ? N3 Ni1 Ni2 O4 102.7(3) . . . . ? N4 Ni1 Ni2 O4 -165.2(3) . . . . ? O5 Ni1 Ni2 O4 10.9(3) . . . . ? O1 Ni1 Ni2 N2 -142.8(4) . . . . ? O2 Ni1 Ni2 N2 33.7(3) . . . . ? O3 Ni1 Ni2 N2 49.1(4) . . . . ? N3 Ni1 Ni2 N2 -141.3(3) . . . . ? N4 Ni1 Ni2 N2 -49.2(3) . . . . ? O5 Ni1 Ni2 N2 126.8(3) . . . . ? O1 Ni1 Ni2 N1 -10.9(4) . . . . ? O2 Ni1 Ni2 N1 165.6(4) . . . . ? O3 Ni1 Ni2 N1 -179.0(4) . . . . ? N3 Ni1 Ni2 N1 -9.4(4) . . . . ? N4 Ni1 Ni2 N1 82.7(3) . . . . ? O5 Ni1 Ni2 N1 -101.3(4) . . . . ? O2 Ni2 N1 C11 -106.0(12) . . . . ? O1 Ni2 N1 C11 -160.1(6) . . . . ? O4 Ni2 N1 C11 95.4(6) . . . . ? N2 Ni2 N1 C11 -7.2(6) . . . . ? Ni1 Ni2 N1 C11 -153.1(5) . . . . ? O2 Ni2 N1 C9 133.4(11) . . . . ? O1 Ni2 N1 C9 79.3(6) . . . . ? O4 Ni2 N1 C9 -25.2(6) . . . . ? N2 Ni2 N1 C9 -127.8(6) . . . . ? Ni1 Ni2 N1 C9 86.4(6) . . . . ? O2 Ni2 N1 C8 10.2(15) . . . . ? O1 Ni2 N1 C8 -43.9(5) . . . . ? O4 Ni2 N1 C8 -148.4(5) . . . . ? N2 Ni2 N1 C8 109.0(5) . . . . ? Ni1 Ni2 N1 C8 -36.9(6) . . . . ? O2 Ni2 N2 C14 -90.6(6) . . . . ? O1 Ni2 N2 C14 -171.6(6) . . . . ? O4 Ni2 N2 C14 2.2(6) . . . . ? N1 Ni2 N2 C14 102.1(6) . . . . ? Ni1 Ni2 N2 C14 -112.1(5) . . . . ? O2 Ni2 N2 C13 35.8(7) . . . . ? O1 Ni2 N2 C13 -45.1(9) . . . . ? O4 Ni2 N2 C13 128.7(7) . . . . ? N1 Ni2 N2 C13 -131.4(7) . . . . ? Ni1 Ni2 N2 C13 14.4(7) . . . . ? O2 Ni2 N2 C12 151.1(5) . . . . ? O1 Ni2 N2 C12 70.1(8) . . . . ? O4 Ni2 N2 C12 -116.0(6) . . . . ? N1 Ni2 N2 C12 -16.1(6) . . . . ? Ni1 Ni2 N2 C12 129.7(5) . . . . ? O1 Ni1 N3 C16 91.7(5) . . . . ? O2 Ni1 N3 C16 74.4(13) . . . . ? O3 Ni1 N3 C16 -96.2(5) . . . . ? N4 Ni1 N3 C16 -7.9(4) . . . . ? O5 Ni1 N3 C16 179.2(5) . . . . ? Ni2 Ni1 N3 C16 90.7(5) . . . . ? O1 Ni1 N3 C15 -32.8(5) . . . . ? O2 Ni1 N3 C15 -50.0(14) . . . . ? O3 Ni1 N3 C15 139.3(5) . . . . ? N4 Ni1 N3 C15 -132.4(5) . . . . ? O5 Ni1 N3 C15 54.8(6) . . . . ? Ni2 Ni1 N3 C15 -33.7(6) . . . . ? O1 Ni1 N4 C18 8.6(5) . . . . ? O2 Ni1 N4 C18 -69.7(4) . . . . ? O3 Ni1 N4 C18 -169.5(4) . . . . ? N3 Ni1 N4 C18 99.3(5) . . . . ? O5 Ni1 N4 C18 -178(2) . . . . ? Ni2 Ni1 N4 C18 -31.2(4) . . . . ? O1 Ni1 N4 C19 130.0(5) . . . . ? O2 Ni1 N4 C19 51.7(5) . . . . ? O3 Ni1 N4 C19 -48.2(5) . . . . ? N3 Ni1 N4 C19 -139.4(5) . . . . ? O5 Ni1 N4 C19 -56(2) . . . . ? Ni2 Ni1 N4 C19 90.2(5) . . . . ? O1 Ni1 N4 C17 -111.0(4) . . . . ? O2 Ni1 N4 C17 170.7(4) . . . . ? O3 Ni1 N4 C17 70.9(4) . . . . ? N3 Ni1 N4 C17 -20.4(4) . . . . ? O5 Ni1 N4 C17 63(2) . . . . ? Ni2 Ni1 N4 C17 -150.8(4) . . . . ? O2 Ni2 O1 C4 -163.8(7) . . . . ? O4 Ni2 O1 C4 106.5(7) . . . . ? N2 Ni2 O1 C4 -79.7(8) . . . . ? N1 Ni2 O1 C4 5.6(7) . . . . ? Ni1 Ni2 O1 C4 -166.2(8) . . . . ? O2 Ni2 O1 Ni1 2.3(2) . . . . ? O4 Ni2 O1 Ni1 -87.3(3) . . . . ? N2 Ni2 O1 Ni1 86.5(5) . . . . ? N1 Ni2 O1 Ni1 171.8(3) . . . . ? O2 Ni1 O1 C4 164.5(7) . . . . ? O3 Ni1 O1 C4 -119.6(15) . . . . ? N3 Ni1 O1 C4 -12.2(7) . . . . ? N4 Ni1 O1 C4 73.4(7) . . . . ? O5 Ni1 O1 C4 -105.8(7) . . . . ? Ni2 Ni1 O1 C4 166.7(8) . . . . ? O2 Ni1 O1 Ni2 -2.2(2) . . . . ? O3 Ni1 O1 Ni2 73.7(15) . . . . ? N3 Ni1 O1 Ni2 -178.9(3) . . . . ? N4 Ni1 O1 Ni2 -93.3(2) . . . . ? O5 Ni1 O1 Ni2 87.5(3) . . . . ? O1 Ni2 O2 Ni1 -2.3(2) . . . . ? O4 Ni2 O2 Ni1 101.6(3) . . . . ? N2 Ni2 O2 Ni1 -155.2(2) . . . . ? N1 Ni2 O2 Ni1 -57.3(12) . . . . ? O1 Ni1 O2 Ni2 2.3(2) . . . . ? O3 Ni1 O2 Ni2 -169.6(2) . . . . ? N3 Ni1 O2 Ni2 19.9(12) . . . . ? N4 Ni1 O2 Ni2 101.5(2) . . . . ? O5 Ni1 O2 Ni2 -85.3(3) . . . . ? O1 Ni1 O3 C20 -70.3(18) . . . . ? O2 Ni1 O3 C20 4.1(7) . . . . ? N3 Ni1 O3 C20 -177.7(7) . . . . ? N4 Ni1 O3 C20 96.9(7) . . . . ? O5 Ni1 O3 C20 -84.1(7) . . . . ? Ni2 Ni1 O3 C20 -5.6(8) . . . . ? C6 C1 C2 C3 1.3(12) . . . . ? C7 C1 C2 C3 179.2(8) . . . . ? C1 C2 C3 C4 1.6(12) . . . . ? C1 C2 C3 C15 178.8(7) . . . . ? Ni2 O1 C4 C5 15.6(11) . . . . ? Ni1 O1 C4 C5 -147.1(6) . . . . ? Ni2 O1 C4 C3 -168.2(6) . . . . ? Ni1 O1 C4 C3 29.1(11) . . . . ? C2 C3 C4 O1 179.3(7) . . . . ? C15 C3 C4 O1 2.2(12) . . . . ? C2 C3 C4 C5 -4.4(12) . . . . ? C15 C3 C4 C5 178.5(7) . . . . ? O1 C4 C5 C6 -179.3(7) . . . . ? C3 C4 C5 C6 4.4(12) . . . . ? O1 C4 C5 C8 2.5(12) . . . . ? C3 C4 C5 C8 -173.8(7) . . . . ? C4 C5 C6 C1 -1.6(13) . . . . ? C8 C5 C6 C1 176.6(8) . . . . ? C2 C1 C6 C5 -1.3(12) . . . . ? C7 C1 C6 C5 -179.1(8) . . . . ? C11 N1 C8 C5 -176.3(7) . . . . ? C9 N1 C8 C5 -52.1(9) . . . . ? Ni2 N1 C8 C5 70.9(7) . . . . ? C6 C5 C8 N1 129.7(8) . . . . ? C4 C5 C8 N1 -52.1(10) . . . . ? C11 N1 C9 C10 66.2(11) . . . . ? C8 N1 C9 C10 -57.4(10) . . . . ? Ni2 N1 C9 C10 -176.8(7) . . . . ? C9 N1 C11 C12 152.4(9) . . . . ? C8 N1 C11 C12 -82.4(10) . . . . ? Ni2 N1 C11 C12 31.1(10) . . . . ? N1 C11 C12 N2 -49.7(12) . . . . ? C14 N2 C12 C11 -81.1(10) . . . . ? C13 N2 C12 C11 160.1(8) . . . . ? Ni2 N2 C12 C11 38.6(9) . . . . ? C16 N3 C15 C3 -56.7(8) . . . . ? Ni1 N3 C15 C3 65.1(7) . . . . ? C2 C3 C15 N3 129.9(8) . . . . ? C4 C3 C15 N3 -52.9(10) . . . . ? C15 N3 C16 C17 160.1(6) . . . . ? Ni1 N3 C16 C17 35.6(6) . . . . ? C18 N4 C17 C16 -75.0(7) . . . . ? C19 N4 C17 C16 167.2(6) . . . . ? Ni1 N4 C17 C16 45.7(6) . . . . ? N3 C16 C17 N4 -56.6(7) . . . . ? Ni1 O3 C20 N5 4.9(12) . . . . ? Ni1 O3 C20 N6 -172.1(6) . . . . ? C39 B2 C21 C22 -117.8(8) . . . . ? C27 B2 C21 C22 4.6(10) . . . . ? C33 B2 C21 C22 119.3(8) . . . . ? C39 B2 C21 C26 60.4(9) . . . . ? C27 B2 C21 C26 -177.2(6) . . . . ? C33 B2 C21 C26 -62.4(9) . . . . ? C26 C21 C22 C23 1.9(11) . . . . ? B2 C21 C22 C23 -179.7(7) . . . . ? C21 C22 C23 C24 -0.1(12) . . . . ? C22 C23 C24 C25 -2.3(12) . . . . ? C23 C24 C25 C26 2.7(12) . . . . ? C22 C21 C26 C25 -1.4(11) . . . . ? B2 C21 C26 C25 -179.9(7) . . . . ? C24 C25 C26 C21 -0.8(12) . . . . ? C39 B2 C27 C32 -179.4(6) . . . . ? C21 B2 C27 C32 60.0(8) . . . . ? C33 B2 C27 C32 -59.0(8) . . . . ? C39 B2 C27 C28 -4.2(9) . . . . ? C21 B2 C27 C28 -124.8(7) . . . . ? C33 B2 C27 C28 116.2(7) . . . . ? C32 C27 C28 C29 0.2(10) . . . . ? B2 C27 C28 C29 -175.2(6) . . . . ? C27 C28 C29 C30 1.0(10) . . . . ? C28 C29 C30 C31 -1.2(10) . . . . ? C29 C30 C31 C32 0.3(10) . . . . ? C30 C31 C32 C27 0.8(11) . . . . ? C28 C27 C32 C31 -1.1(10) . . . . ? B2 C27 C32 C31 174.5(6) . . . . ? C39 B2 C33 C34 -116.2(7) . . . . ? C21 B2 C33 C34 4.1(9) . . . . ? C27 B2 C33 C34 124.3(7) . . . . ? C39 B2 C33 C38 67.6(8) . . . . ? C21 B2 C33 C38 -172.1(6) . . . . ? C27 B2 C33 C38 -51.9(8) . . . . ? C38 C33 C34 C35 -2.2(10) . . . . ? B2 C33 C34 C35 -178.5(6) . . . . ? C33 C34 C35 C36 0.8(10) . . . . ? C34 C35 C36 C37 0.8(10) . . . . ? C35 C36 C37 C38 -0.7(10) . . . . ? C36 C37 C38 C33 -0.9(10) . . . . ? C34 C33 C38 C37 2.2(10) . . . . ? B2 C33 C38 C37 178.8(6) . . . . ? C21 B2 C39 C40 -136.3(7) . . . . ? C27 B2 C39 C40 100.4(8) . . . . ? C33 B2 C39 C40 -14.6(10) . . . . ? C21 B2 C39 C44 47.2(8) . . . . ? C27 B2 C39 C44 -76.1(8) . . . . ? C33 B2 C39 C44 168.9(6) . . . . ? C44 C39 C40 C41 -0.8(10) . . . . ? B2 C39 C40 C41 -177.5(7) . . . . ? C39 C40 C41 C42 1.6(11) . . . . ? C40 C41 C42 C43 -1.3(11) . . . . ? C41 C42 C43 C44 0.4(11) . . . . ? C42 C43 C44 C39 0.3(11) . . . . ? C40 C39 C44 C43 -0.1(10) . . . . ? B2 C39 C44 C43 176.8(6) . . . . ? C57 B1 C45 C46 124.2(11) . . . . ? C51 B1 C45 C46 7.7(13) . . . . ? C63 B1 C45 C46 -113.9(10) . . . . ? C57 B1 C45 C50 -61.0(12) . . . . ? C51 B1 C45 C50 -177.5(9) . . . . ? C63 B1 C45 C50 60.9(11) . . . . ? C50 C45 C46 C47 -2.5(17) . . . . ? B1 C45 C46 C47 172.6(10) . . . . ? C45 C46 C47 C48 7.1(18) . . . . ? C46 C47 C48 C49 -7.9(18) . . . . ? C47 C48 C49 C50 4.5(18) . . . . ? C48 C49 C50 C45 0.2(18) . . . . ? C46 C45 C50 C49 -1.2(17) . . . . ? B1 C45 C50 C49 -176.5(9) . . . . ? C45 B1 C51 C52 -114.9(10) . . . . ? C57 B1 C51 C52 123.6(10) . . . . ? C63 B1 C51 C52 1.5(12) . . . . ? C45 B1 C51 C56 69.5(10) . . . . ? C57 B1 C51 C56 -52.1(10) . . . . ? C63 B1 C51 C56 -174.2(7) . . . . ? C56 C51 C52 C53 -0.5(14) . . . . ? B1 C51 C52 C53 -176.4(9) . . . . ? C51 C52 C53 C54 -0.9(15) . . . . ? C52 C53 C54 C55 1.5(15) . . . . ? C53 C54 C55 C56 -0.7(14) . . . . ? C54 C55 C56 C51 -0.8(14) . . . . ? C52 C51 C56 C55 1.4(13) . . . . ? B1 C51 C56 C55 177.5(8) . . . . ? C45 B1 C57 C62 178.9(8) . . . . ? C51 B1 C57 C62 -59.8(10) . . . . ? C63 B1 C57 C62 62.2(10) . . . . ? C45 B1 C57 C58 -7.6(12) . . . . ? C51 B1 C57 C58 113.7(9) . . . . ? C63 B1 C57 C58 -124.3(9) . . . . ? C62 C57 C58 C59 0.6(13) . . . . ? B1 C57 C58 C59 -173.3(8) . . . . ? C57 C58 C59 C60 1.8(14) . . . . ? C58 C59 C60 C61 -2.1(14) . . . . ? C59 C60 C61 C62 -0.1(14) . . . . ? C60 C61 C62 C57 2.7(14) . . . . ? C58 C57 C62 C61 -2.9(13) . . . . ? B1 C57 C62 C61 171.2(8) . . . . ? C45 B1 C63 C64 -107.6(9) . . . . ? C57 B1 C63 C64 14.2(11) . . . . ? C51 B1 C63 C64 131.2(8) . . . . ? C45 B1 C63 C68 63.5(9) . . . . ? C57 B1 C63 C68 -174.7(8) . . . . ? C51 B1 C63 C68 -57.7(10) . . . . ? C68 C63 C64 C65 0.0(12) . . . . ? B1 C63 C64 C65 171.5(8) . . . . ? C63 C64 C65 C66 -0.5(13) . . . . ? C64 C65 C66 C67 1.5(13) . . . . ? C65 C66 C67 C68 -2.0(13) . . . . ? C66 C67 C68 C63 1.6(13) . . . . ? C64 C63 C68 C67 -0.6(12) . . . . ? B1 C63 C68 C67 -172.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 1.055 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.111