# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H28 F3 N3 Ni O4, H0.80 O0.40, 1.6(H2 O)' _chemical_formula_sum 'C38 H32 F3 N3 Ni O6' _chemical_formula_weight 742.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.869(2) _cell_length_b 11.874(3) _cell_length_c 14.3120(18) _cell_angle_alpha 74.121(2) _cell_angle_beta 78.329(3) _cell_angle_gamma 79.1460(10) _cell_volume 1880.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3532 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.05 _exptl_crystal_description Rod _exptl_crystal_colour Red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_type multi-scan' _exptl_absorpt_correction_T_min 0.8549 _exptl_absorpt_correction_T_max 0.8834 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 10366 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7258 _reflns_number_gt 5573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0600P)^2^+1.9900P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7258 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 C1 C -0.2061(3) 0.4230(3) 0.1591(2) 0.0346(7) Uani 1 1 d . . . H1A H -0.2551 0.4050 0.1201 0.042 Uiso 1 1 calc R . . H1B H -0.1563 0.4780 0.1153 0.042 Uiso 1 1 calc R . . C2 C -0.2835(3) 0.4836(3) 0.2362(2) 0.0366(7) Uani 1 1 d . . . C3 C -0.2402(3) 0.5577(3) 0.2747(2) 0.0384(7) Uani 1 1 d . . . H3 H -0.1636 0.5716 0.2537 0.046 Uiso 1 1 calc R . . C4 C -0.3103(3) 0.6118(3) 0.3446(3) 0.0459(8) Uani 1 1 d . . . H4 H -0.2805 0.6615 0.3706 0.055 Uiso 1 1 calc R . . C5 C -0.4247(3) 0.5919(3) 0.3758(3) 0.0430(8) Uani 1 1 d . . . H5 H -0.4713 0.6275 0.4233 0.052 Uiso 1 1 calc R . . C6 C -0.4691(3) 0.5201(3) 0.3368(3) 0.0447(8) Uani 1 1 d . . . H6 H -0.5460 0.5069 0.3573 0.054 Uiso 1 1 calc R . . C7 C -0.3979(3) 0.4666(3) 0.2660(3) 0.0403(7) Uani 1 1 d . . . H7 H -0.4284 0.4188 0.2385 0.048 Uiso 1 1 calc R . . C8 C -0.2018(3) 0.2259(3) 0.2744(2) 0.0371(7) Uani 1 1 d . . . H8A H -0.1664 0.1459 0.2721 0.044 Uiso 1 1 calc R . . H8B H -0.2795 0.2378 0.2584 0.044 Uiso 1 1 calc R . . C9 C -0.2084(3) 0.2429(3) 0.3784(2) 0.0373(7) Uani 1 1 d . . . C10 C -0.0611(3) 0.2635(3) 0.1186(2) 0.0364(7) Uani 1 1 d . . . H10A H -0.1077 0.2746 0.0675 0.044 Uiso 1 1 calc R . . H10B H -0.0368 0.1793 0.1420 0.044 Uiso 1 1 calc R . . C11 C 0.0453(3) 0.3263(3) 0.0765(2) 0.0333(7) Uani 1 1 d . . . C12 C -0.1081(3) 0.3189(3) 0.4730(2) 0.0395(7) Uani 1 1 d . . . C13 C -0.2059(3) 0.3447(3) 0.5413(2) 0.0381(7) Uani 1 1 d . . . H13 H -0.2796 0.3382 0.5320 0.046 Uiso 1 1 calc R . . C14 C -0.1923(3) 0.3804(3) 0.6237(3) 0.0432(8) Uani 1 1 d . . . H14 H -0.2578 0.4035 0.6659 0.052 Uiso 1 1 calc R . . C15 C -0.0820(3) 0.3817(3) 0.6432(2) 0.0422(8) Uani 1 1 d . . . H15 H -0.0734 0.4020 0.6995 0.051 Uiso 1 1 calc R . . C16 C 0.0120(3) 0.3530(3) 0.5787(2) 0.0404(7) Uani 1 1 d . . . H16 H 0.0854 0.3549 0.5912 0.049 Uiso 1 1 calc R . . C17 C 0.0033(3) 0.3204(3) 0.4939(2) 0.0373(7) Uani 1 1 d . . . C18 C 0.1098(3) 0.2941(3) 0.4258(2) 0.0363(7) Uani 1 1 d . . . C19 C 0.2210(3) 0.2430(3) 0.4655(3) 0.0383(7) Uani 1 1 d . . . C20 C 0.2221(3) 0.1513(3) 0.5495(3) 0.0422(8) Uani 1 1 d . . . H20 H 0.1526 0.1269 0.5853 0.051 Uiso 1 1 calc R . . C21 C 0.3271(3) 0.0955(3) 0.5806(3) 0.0434(8) Uani 1 1 d . . . H21 H 0.3283 0.0314 0.6352 0.052 Uiso 1 1 calc R . . C22 C 0.4316(3) 0.1371(3) 0.5286(3) 0.0422(8) Uani 1 1 d . . . H22 H 0.5014 0.1034 0.5512 0.051 Uiso 1 1 calc R . . C23 C 0.4306(3) 0.2257(3) 0.4461(3) 0.0412(8) Uani 1 1 d . . . H23 H 0.5002 0.2504 0.4107 0.049 Uiso 1 1 calc R . . C24 C 0.3238(3) 0.2818(3) 0.4126(2) 0.0378(7) Uani 1 1 d . . . H24 H 0.3231 0.3434 0.3562 0.045 Uiso 1 1 calc R . . C25 C 0.1691(3) 0.4339(3) 0.1204(3) 0.0397(7) Uani 1 1 d . . . C26 C 0.1447(3) 0.5546(3) 0.1162(3) 0.0390(7) Uani 1 1 d . . . H26 H 0.0677 0.5900 0.1245 0.047 Uiso 1 1 calc R . . C27 C 0.2333(3) 0.6235(3) 0.0999(2) 0.0398(7) Uani 1 1 d . . . H27 H 0.2156 0.7038 0.0978 0.048 Uiso 1 1 calc R . . C28 C 0.3478(3) 0.5709(3) 0.0869(3) 0.0427(8) Uani 1 1 d . . . H28 H 0.4074 0.6153 0.0785 0.051 Uiso 1 1 calc R . . C29 C 0.3743(3) 0.4517(3) 0.0862(2) 0.0357(7) Uani 1 1 d . . . H29 H 0.4515 0.4185 0.0726 0.043 Uiso 1 1 calc R . . C30 C 0.2865(3) 0.3818(3) 0.1057(2) 0.0342(7) Uani 1 1 d . . . C31 C 0.3207(3) 0.2530(3) 0.1191(2) 0.0380(7) Uani 1 1 d . . . C32 C 0.4125(3) 0.2127(3) 0.0409(2) 0.0361(7) Uani 1 1 d . . . C33 C 0.3835(3) 0.2400(3) -0.0537(3) 0.0447(8) Uani 1 1 d . . . H33 H 0.3120 0.2834 -0.0664 0.054 Uiso 1 1 calc R . . C34 C 0.4629(3) 0.2012(3) -0.1291(3) 0.0411(8) Uani 1 1 d . . . H34 H 0.4445 0.2190 -0.1921 0.049 Uiso 1 1 calc R . . C35 C 0.5712(3) 0.1350(3) -0.1088(3) 0.0483(9) Uani 1 1 d . . . H35 H 0.6240 0.1079 -0.1582 0.058 Uiso 1 1 calc R . . C36 C 0.5974(3) 0.1114(3) -0.0173(3) 0.0435(8) Uani 1 1 d . . . H36 H 0.6695 0.0695 -0.0049 0.052 Uiso 1 1 calc R . . C37 C 0.5200(3) 0.1477(3) 0.0584(3) 0.0388(7) Uani 1 1 d . . . C38 C 0.5562(3) 0.1226(3) 0.1572(3) 0.0436(8) Uani 1 1 d . . . F1 F 0.50459(19) 0.03301(19) 0.22531(16) 0.0568(6) Uani 1 1 d . . . F2 F 0.52475(17) 0.21124(18) 0.20049(15) 0.0464(5) Uani 1 1 d . . . F3 F 0.66787(18) 0.09375(18) 0.15553(15) 0.0494(5) Uani 1 1 d . . . N1 N -0.1317(2) 0.3118(2) 0.2014(2) 0.0368(6) Uani 1 1 d . . . N2 N -0.1172(2) 0.2912(2) 0.38564(19) 0.0358(6) Uani 1 1 d . . . N3 N 0.0752(2) 0.3684(2) 0.1441(2) 0.0390(6) Uani 1 1 d . . . Ni1 Ni -0.01508(4) 0.32972(4) 0.26978(3) 0.03684(13) Uani 1 1 d . . . O1 O -0.2863(2) 0.2035(2) 0.44475(18) 0.0448(6) Uani 1 1 d . . . O2 O 0.09594(19) 0.3299(2) -0.00714(16) 0.0378(5) Uani 1 1 d . . . O3 O 0.10927(19) 0.3094(2) 0.33388(17) 0.0386(5) Uani 1 1 d . . . O4 O 0.2767(2) 0.1823(2) 0.18913(19) 0.0532(7) Uani 1 1 d . . . O1W O 0.9867(5) 0.0548(5) 0.7555(5) 0.0471(15) Uani 0.40 1 d P . . H1WD H 0.9280 0.0729 0.7260 0.056 Uiso 0.40 1 d PR . . H1WB H 1.0071 0.1174 0.7607 0.071 Uiso 0.40 1 d PR . . O2W O 0.1089(5) 0.8975(5) 0.1055(5) 0.0479(15) Uani 0.40 1 d P . . H2WA H 0.1278 0.9668 0.0873 0.072 Uiso 0.40 1 d PR . . H2WB H 0.1103 0.8722 0.0551 0.072 Uiso 0.40 1 d PR . . O3W O 1.0000 0.0000 0.5000 0.0461(10) Uani 0.80 2 d SP . . H3WA H 1.0490 -0.0492 0.4739 0.069 Uiso 0.40 1 d PR . . H3WB H 1.0332 0.0285 0.5339 0.069 Uiso 0.40 1 d PR . . O4W O 0.3131(6) 0.9255(6) 0.3544(5) 0.0535(16) Uani 0.40 1 d P . . H4WA H 0.3813 0.9177 0.3221 0.080 Uiso 0.40 1 d PR . . H4WB H 0.2836 0.9979 0.3413 0.080 Uiso 0.40 1 d PR . . O5W O 0.1776(6) 0.1562(5) 0.8463(5) 0.0509(16) Uani 0.40 1 d P . . H5WA H 0.2123 0.1483 0.8946 0.076 Uiso 0.40 1 d PR . . H5WB H 0.1052 0.1561 0.8667 0.076 Uiso 0.40 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0321(16) 0.0411(17) 0.0320(16) -0.0121(13) -0.0118(13) 0.0033(13) C2 0.0326(16) 0.0410(18) 0.0339(16) -0.0074(14) -0.0059(13) -0.0014(13) C3 0.0362(17) 0.0453(18) 0.0396(17) -0.0149(15) -0.0160(14) -0.0029(14) C4 0.0425(19) 0.047(2) 0.049(2) -0.0190(16) -0.0128(16) 0.0088(16) C5 0.0400(19) 0.0460(19) 0.0398(18) -0.0151(15) -0.0035(15) 0.0054(15) C6 0.0360(18) 0.0390(18) 0.053(2) -0.0143(16) 0.0087(16) -0.0038(14) C7 0.0392(18) 0.0430(18) 0.0418(18) -0.0136(15) -0.0019(15) -0.0132(14) C8 0.0289(15) 0.0454(18) 0.0366(17) -0.0055(14) -0.0037(13) -0.0129(13) C9 0.0319(16) 0.0451(18) 0.0321(16) -0.0017(14) -0.0010(13) -0.0148(14) C10 0.0337(16) 0.0396(17) 0.0377(17) -0.0154(14) -0.0019(13) -0.0053(13) C11 0.0320(16) 0.0340(16) 0.0342(16) -0.0093(13) -0.0051(13) -0.0044(13) C12 0.0341(17) 0.0423(18) 0.0370(17) -0.0075(14) -0.0012(14) -0.0008(14) C13 0.0275(16) 0.0487(19) 0.0311(16) -0.0111(14) 0.0004(13) 0.0086(14) C14 0.0420(19) 0.0392(18) 0.0418(19) -0.0148(15) 0.0105(15) -0.0007(14) C15 0.046(2) 0.0422(18) 0.0345(17) -0.0136(15) -0.0034(15) 0.0071(15) C16 0.0409(18) 0.0439(18) 0.0340(17) -0.0121(14) -0.0046(14) 0.0026(15) C17 0.0360(17) 0.0342(16) 0.0401(17) -0.0105(14) -0.0019(14) -0.0034(13) C18 0.0352(17) 0.0346(16) 0.0396(18) -0.0101(14) -0.0007(14) -0.0104(13) C19 0.0333(17) 0.0354(17) 0.0461(19) -0.0133(14) -0.0022(14) -0.0044(13) C20 0.0380(18) 0.0465(19) 0.0416(18) -0.0060(15) -0.0100(15) -0.0079(15) C21 0.0444(19) 0.0433(19) 0.0416(19) -0.0098(15) -0.0145(16) 0.0034(15) C22 0.0355(18) 0.049(2) 0.0425(19) -0.0113(16) -0.0208(15) 0.0079(15) C23 0.0398(18) 0.0427(18) 0.0391(18) -0.0128(15) -0.0057(14) 0.0021(14) C24 0.0333(17) 0.0441(18) 0.0392(17) -0.0162(15) -0.0074(14) -0.0028(14) C25 0.0314(16) 0.0413(18) 0.0447(19) -0.0089(15) -0.0010(14) -0.0085(14) C26 0.0332(17) 0.0375(17) 0.0442(18) -0.0124(15) -0.0002(14) -0.0027(13) C27 0.0398(18) 0.0456(19) 0.0341(17) -0.0141(15) 0.0046(14) -0.0112(15) C28 0.0327(17) 0.048(2) 0.0464(19) -0.0138(16) 0.0054(14) -0.0120(15) C29 0.0295(15) 0.0400(17) 0.0377(17) -0.0120(14) 0.0081(13) -0.0160(13) C30 0.0329(16) 0.0375(17) 0.0349(16) -0.0152(13) 0.0021(13) -0.0103(13) C31 0.0412(18) 0.0332(16) 0.0392(18) -0.0091(14) -0.0038(14) -0.0067(14) C32 0.0318(16) 0.0334(16) 0.0423(18) -0.0111(14) -0.0012(14) -0.0047(13) C33 0.0416(19) 0.0456(19) 0.0419(19) -0.0111(16) 0.0022(15) -0.0029(15) C34 0.0388(18) 0.0424(18) 0.0404(18) -0.0141(15) 0.0063(15) -0.0091(14) C35 0.051(2) 0.046(2) 0.0394(19) -0.0107(16) 0.0152(16) -0.0094(16) C36 0.0361(18) 0.0454(19) 0.048(2) -0.0160(16) -0.0039(15) 0.0000(14) C37 0.0360(17) 0.0385(17) 0.0447(19) -0.0148(15) -0.0095(15) -0.0017(14) C38 0.046(2) 0.0441(19) 0.0387(18) -0.0144(15) -0.0138(15) 0.0115(15) F1 0.0514(13) 0.0478(12) 0.0499(12) 0.0009(10) -0.0014(10) 0.0187(10) F2 0.0469(11) 0.0479(11) 0.0462(11) -0.0179(9) -0.0167(9) 0.0080(9) F3 0.0446(12) 0.0541(12) 0.0446(11) -0.0127(10) -0.0166(9) 0.0160(9) N1 0.0326(14) 0.0382(14) 0.0401(15) -0.0100(12) -0.0028(12) -0.0091(11) N2 0.0286(13) 0.0416(15) 0.0330(14) -0.0063(12) -0.0001(11) -0.0041(11) N3 0.0348(14) 0.0442(15) 0.0399(15) -0.0132(12) -0.0001(12) -0.0119(12) Ni1 0.0340(2) 0.0378(2) 0.0374(2) -0.00765(18) -0.00160(17) -0.00832(17) O1 0.0393(13) 0.0417(13) 0.0462(14) -0.0017(11) 0.0042(11) -0.0135(10) O2 0.0332(11) 0.0489(13) 0.0315(11) -0.0131(10) 0.0031(9) -0.0105(10) O3 0.0338(12) 0.0460(13) 0.0395(12) -0.0130(10) -0.0032(10) -0.0131(10) O4 0.0480(15) 0.0470(14) 0.0465(14) -0.0029(12) 0.0205(12) -0.0051(12) O1W 0.033(3) 0.034(3) 0.053(4) 0.005(3) 0.011(3) 0.006(2) O2W 0.045(3) 0.040(3) 0.047(4) -0.008(3) 0.018(3) -0.011(3) O3W 0.041(2) 0.045(2) 0.054(3) -0.014(2) -0.015(2) -0.0006(19) O4W 0.058(4) 0.048(4) 0.051(4) -0.014(3) -0.016(3) 0.010(3) O5W 0.044(3) 0.045(3) 0.057(4) -0.008(3) 0.007(3) -0.013(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 C1 N1 1.493(4) . ? C1 C2 1.534(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.374(5) . ? C2 C3 1.376(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9300 . ? C4 C5 1.383(5) . ? C4 H4 0.9300 . ? C5 C6 1.365(5) . ? C5 H5 0.9300 . ? C6 C7 1.395(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.487(4) . ? C8 C9 1.542(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O1 1.241(4) . ? C9 N2 1.350(4) . ? C10 N1 1.492(4) . ? C10 C11 1.521(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O2 1.219(4) . ? C11 N3 1.335(4) . ? C12 C13 1.402(4) . ? C12 N2 1.406(4) . ? C12 C17 1.419(5) . ? C13 C14 1.405(5) . ? C13 H13 0.9300 . ? C14 C15 1.396(5) . ? C14 H14 0.9300 . ? C15 C16 1.352(5) . ? C15 H15 0.9300 . ? C16 C17 1.398(5) . ? C16 H16 0.9300 . ? C17 C18 1.471(4) . ? C18 O3 1.279(4) . ? C18 C19 1.499(5) . ? C19 C20 1.384(5) . ? C19 C24 1.386(5) . ? C20 C21 1.394(5) . ? C20 H20 0.9300 . ? C21 C22 1.412(5) . ? C21 H21 0.9300 . ? C22 C23 1.350(5) . ? C22 H22 0.9300 . ? C23 C24 1.426(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.395(5) . ? C25 N3 1.411(4) . ? C25 C30 1.413(5) . ? C26 C27 1.397(5) . ? C26 H26 0.9300 . ? C27 C28 1.383(5) . ? C27 H27 0.9300 . ? C28 C29 1.394(5) . ? C28 H28 0.9300 . ? C29 C30 1.390(4) . ? C29 H29 0.9300 . ? C30 C31 1.476(4) . ? C31 O4 1.214(4) . ? C31 C32 1.507(5) . ? C32 C37 1.392(5) . ? C32 C33 1.402(5) . ? C33 C34 1.400(5) . ? C33 H33 0.9300 . ? C34 C35 1.414(5) . ? C34 H34 0.9300 . ? C35 C36 1.350(5) . ? C35 H35 0.9300 . ? C36 C37 1.381(5) . ? C36 H36 0.9300 . ? C37 C38 1.497(5) . ? C38 F3 1.302(4) . ? C38 F2 1.321(4) . ? C38 F1 1.376(4) . ? N1 Ni1 1.921(3) . ? N2 Ni1 1.846(3) . ? N3 Ni1 1.884(3) . ? Ni1 O3 1.836(2) . ? O1W H1WD 0.8499 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8499 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? O5W H5WA 0.8499 . ? O5W H5WB 0.8500 . ? 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 N1 C1 C2 114.3(3) . . ? N1 C1 H1A 108.7 . . ? C2 C1 H1A 108.7 . . ? N1 C1 H1B 108.7 . . ? C2 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C7 C2 C3 119.1(3) . . ? C7 C2 C1 120.4(3) . . ? C3 C2 C1 120.5(3) . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 119.4(3) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C2 C7 C6 121.0(3) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? N1 C8 C9 109.7(3) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O1 C9 N2 128.5(3) . . ? O1 C9 C8 119.1(3) . . ? N2 C9 C8 112.1(3) . . ? N1 C10 C11 109.9(2) . . ? N1 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? N1 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? O2 C11 N3 127.2(3) . . ? O2 C11 C10 121.8(3) . . ? N3 C11 C10 110.9(3) . . ? C13 C12 N2 122.3(3) . . ? C13 C12 C17 118.4(3) . . ? N2 C12 C17 119.4(3) . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 121.1(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 118.6(3) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 122.6(3) . . ? C15 C16 H16 118.7 . . ? C17 C16 H16 118.7 . . ? C16 C17 C12 119.3(3) . . ? C16 C17 C18 119.2(3) . . ? C12 C17 C18 121.4(3) . . ? O3 C18 C17 121.8(3) . . ? O3 C18 C19 118.9(3) . . ? C17 C18 C19 119.3(3) . . ? C20 C19 C24 120.5(3) . . ? C20 C19 C18 120.2(3) . . ? C24 C19 C18 119.1(3) . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 119.4(3) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.6(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C19 C24 C23 119.0(3) . . ? C19 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 N3 118.2(3) . . ? C26 C25 C30 118.6(3) . . ? N3 C25 C30 123.1(3) . . ? C25 C26 C27 121.5(3) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 119.2(3) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 120.4(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 120.6(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C25 119.7(3) . . ? C29 C30 C31 117.9(3) . . ? C25 C30 C31 122.3(3) . . ? O4 C31 C30 121.9(3) . . ? O4 C31 C32 121.2(3) . . ? C30 C31 C32 116.8(3) . . ? C37 C32 C33 119.5(3) . . ? C37 C32 C31 124.1(3) . . ? C33 C32 C31 116.4(3) . . ? C34 C33 C32 119.5(3) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 119.7(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 119.5(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C37 121.8(3) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C36 C37 C32 120.0(3) . . ? C36 C37 C38 119.1(3) . . ? C32 C37 C38 120.7(3) . . ? F3 C38 F2 106.2(3) . . ? F3 C38 F1 106.8(3) . . ? F2 C38 F1 102.2(3) . . ? F3 C38 C37 113.6(3) . . ? F2 C38 C37 114.2(3) . . ? F1 C38 C37 112.8(3) . . ? C8 N1 C10 113.3(3) . . ? C8 N1 C1 111.7(3) . . ? C10 N1 C1 108.4(3) . . ? C8 N1 Ni1 104.8(2) . . ? C10 N1 Ni1 102.63(19) . . ? C1 N1 Ni1 115.8(2) . . ? C9 N2 C12 121.6(3) . . ? C9 N2 Ni1 114.7(2) . . ? C12 N2 Ni1 123.5(2) . . ? C11 N3 C25 120.8(3) . . ? C11 N3 Ni1 114.5(2) . . ? C25 N3 Ni1 124.6(2) . . ? O3 Ni1 N2 93.10(11) . . ? O3 Ni1 N3 93.42(11) . . ? N2 Ni1 N3 173.40(12) . . ? O3 Ni1 N1 166.05(11) . . ? N2 Ni1 N1 88.05(12) . . ? N3 Ni1 N1 85.37(12) . . ? C18 O3 Ni1 128.8(2) . . ? H1WD O1W H1WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? H3WA O3W H3WB 109.5 . . ? H4WA O4W H4WB 109.5 . . ? H5WA O5W H5WB 109.5 . . ? 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 N1 C1 C2 C7 -97.9(4) . . . . ? N1 C1 C2 C3 83.6(4) . . . . ? C7 C2 C3 C4 1.8(5) . . . . ? C1 C2 C3 C4 -179.7(3) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? C4 C5 C6 C7 0.4(5) . . . . ? C3 C2 C7 C6 -2.2(5) . . . . ? C1 C2 C7 C6 179.3(3) . . . . ? C5 C6 C7 C2 1.2(5) . . . . ? N1 C8 C9 O1 160.8(3) . . . . ? N1 C8 C9 N2 -25.3(4) . . . . ? N1 C10 C11 O2 -157.2(3) . . . . ? N1 C10 C11 N3 25.9(4) . . . . ? N2 C12 C13 C14 -175.2(3) . . . . ? C17 C12 C13 C14 5.1(5) . . . . ? C12 C13 C14 C15 -5.1(5) . . . . ? C13 C14 C15 C16 2.9(5) . . . . ? C14 C15 C16 C17 -0.9(5) . . . . ? C15 C16 C17 C12 1.0(5) . . . . ? C15 C16 C17 C18 178.0(3) . . . . ? C13 C12 C17 C16 -3.1(5) . . . . ? N2 C12 C17 C16 177.2(3) . . . . ? C13 C12 C17 C18 179.9(3) . . . . ? N2 C12 C17 C18 0.3(5) . . . . ? C16 C17 C18 O3 -152.1(3) . . . . ? C12 C17 C18 O3 24.9(5) . . . . ? C16 C17 C18 C19 30.7(4) . . . . ? C12 C17 C18 C19 -152.3(3) . . . . ? O3 C18 C19 C20 -132.2(3) . . . . ? C17 C18 C19 C20 45.1(4) . . . . ? O3 C18 C19 C24 42.3(4) . . . . ? C17 C18 C19 C24 -140.4(3) . . . . ? C24 C19 C20 C21 -1.3(5) . . . . ? C18 C19 C20 C21 173.2(3) . . . . ? C19 C20 C21 C22 3.1(5) . . . . ? C20 C21 C22 C23 -3.8(5) . . . . ? C21 C22 C23 C24 2.6(5) . . . . ? C20 C19 C24 C23 0.0(5) . . . . ? C18 C19 C24 C23 -174.6(3) . . . . ? C22 C23 C24 C19 -0.7(5) . . . . ? N3 C25 C26 C27 175.5(3) . . . . ? C30 C25 C26 C27 -1.2(5) . . . . ? C25 C26 C27 C28 0.5(5) . . . . ? C26 C27 C28 C29 2.5(5) . . . . ? C27 C28 C29 C30 -4.7(5) . . . . ? C28 C29 C30 C25 3.9(5) . . . . ? C28 C29 C30 C31 -170.8(3) . . . . ? C26 C25 C30 C29 -1.0(5) . . . . ? N3 C25 C30 C29 -177.6(3) . . . . ? C26 C25 C30 C31 173.5(3) . . . . ? N3 C25 C30 C31 -3.1(5) . . . . ? C29 C30 C31 O4 130.1(4) . . . . ? C25 C30 C31 O4 -44.4(5) . . . . ? C29 C30 C31 C32 -50.3(4) . . . . ? C25 C30 C31 C32 135.1(3) . . . . ? O4 C31 C32 C37 -62.0(5) . . . . ? C30 C31 C32 C37 118.4(4) . . . . ? O4 C31 C32 C33 115.6(4) . . . . ? C30 C31 C32 C33 -64.0(4) . . . . ? C37 C32 C33 C34 0.1(5) . . . . ? C31 C32 C33 C34 -177.5(3) . . . . ? C32 C33 C34 C35 0.1(5) . . . . ? C33 C34 C35 C36 -0.9(5) . . . . ? C34 C35 C36 C37 1.6(6) . . . . ? C35 C36 C37 C32 -1.3(6) . . . . ? C35 C36 C37 C38 -177.7(3) . . . . ? C33 C32 C37 C36 0.4(5) . . . . ? C31 C32 C37 C36 177.9(3) . . . . ? C33 C32 C37 C38 176.7(3) . . . . ? C31 C32 C37 C38 -5.8(5) . . . . ? C36 C37 C38 F3 15.8(5) . . . . ? C32 C37 C38 F3 -160.5(3) . . . . ? C36 C37 C38 F2 137.9(3) . . . . ? C32 C37 C38 F2 -38.4(5) . . . . ? C36 C37 C38 F1 -105.9(4) . . . . ? C32 C37 C38 F1 77.8(4) . . . . ? C9 C8 N1 C10 145.0(3) . . . . ? C9 C8 N1 C1 -92.3(3) . . . . ? C9 C8 N1 Ni1 33.9(3) . . . . ? C11 C10 N1 C8 -153.4(3) . . . . ? C11 C10 N1 C1 82.1(3) . . . . ? C11 C10 N1 Ni1 -41.0(3) . . . . ? C2 C1 N1 C8 54.9(3) . . . . ? C2 C1 N1 C10 -179.6(3) . . . . ? C2 C1 N1 Ni1 -65.0(3) . . . . ? O1 C9 N2 C12 -9.4(5) . . . . ? C8 C9 N2 C12 177.4(3) . . . . ? O1 C9 N2 Ni1 176.0(3) . . . . ? C8 C9 N2 Ni1 2.8(4) . . . . ? C13 C12 N2 C9 -26.5(5) . . . . ? C17 C12 N2 C9 153.2(3) . . . . ? C13 C12 N2 Ni1 147.6(3) . . . . ? C17 C12 N2 Ni1 -32.7(4) . . . . ? O2 C11 N3 C25 5.7(5) . . . . ? C10 C11 N3 C25 -177.7(3) . . . . ? O2 C11 N3 Ni1 -173.0(3) . . . . ? C10 C11 N3 Ni1 3.6(3) . . . . ? C26 C25 N3 C11 110.1(4) . . . . ? C30 C25 N3 C11 -73.3(5) . . . . ? C26 C25 N3 Ni1 -71.4(4) . . . . ? C30 C25 N3 Ni1 105.2(4) . . . . ? C9 N2 Ni1 O3 -151.6(2) . . . . ? C12 N2 Ni1 O3 34.0(3) . . . . ? C9 N2 Ni1 N3 19.1(12) . . . . ? C12 N2 Ni1 N3 -155.4(10) . . . . ? C9 N2 Ni1 N1 14.5(2) . . . . ? C12 N2 Ni1 N1 -160.0(3) . . . . ? C11 N3 Ni1 O3 142.6(2) . . . . ? C25 N3 Ni1 O3 -36.0(3) . . . . ? C11 N3 Ni1 N2 -28.0(12) . . . . ? C25 N3 Ni1 N2 153.3(10) . . . . ? C11 N3 Ni1 N1 -23.4(2) . . . . ? C25 N3 Ni1 N1 158.0(3) . . . . ? C8 N1 Ni1 O3 67.8(5) . . . . ? C10 N1 Ni1 O3 -50.8(5) . . . . ? C1 N1 Ni1 O3 -168.6(4) . . . . ? C8 N1 Ni1 N2 -27.2(2) . . . . ? C10 N1 Ni1 N2 -145.8(2) . . . . ? C1 N1 Ni1 N2 96.4(2) . . . . ? C8 N1 Ni1 N3 153.3(2) . . . . ? C10 N1 Ni1 N3 34.8(2) . . . . ? C1 N1 Ni1 N3 -83.1(2) . . . . ? C17 C18 O3 Ni1 -15.9(4) . . . . ? C19 C18 O3 Ni1 161.4(2) . . . . ? N2 Ni1 O3 C18 -10.0(3) . . . . ? N3 Ni1 O3 C18 171.1(3) . . . . ? N1 Ni1 O3 C18 -104.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.325 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.059 _database_code_depnum_ccdc_archive 'CCDC 951881' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H30 F3 N3 Ni O5, H2 O' _chemical_formula_sum 'C39 H32 F3 N3 Ni O6' _chemical_formula_weight 754.39 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' F F 0.0171 0.0103 '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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.648(4) _cell_length_b 13.897(6) _cell_length_c 16.270(7) _cell_angle_alpha 66.870(7) _cell_angle_beta 74.393(7) _cell_angle_gamma 87.648(8) _cell_volume 1927.0(14) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 470 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 17.52 _exptl_crystal_description Rod _exptl_crystal_colour Red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7 _exptl_absorpt_correction_T_max 0.8 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _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 10590 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7415 _reflns_number_gt 4985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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. Rigid bond restraint (DELU in Shelxl) was applied to anisotropic displacement parameters of N(2) and C(18) to treat adp's small elongation. ; _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^)+(0.04P)^2^+0.44P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7415 _refine_ls_number_parameters 488 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 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 C1 C 0.0491(4) -0.0529(3) 0.7456(2) 0.0543(8) Uani 1 1 d . . . H1A H 0.0508 -0.1225 0.7923 0.065 Uiso 1 1 calc R . . H1B H -0.0257 -0.0552 0.7167 0.065 Uiso 1 1 calc R . . C2 C 0.0138(3) 0.0239(2) 0.7921(2) 0.0442(7) Uani 1 1 d . . . C3 C 0.0946(3) 0.1880(2) 0.78333(19) 0.0422(7) Uani 1 1 d . . . C4 C 0.0593(3) 0.1637(2) 0.87855(19) 0.0430(7) Uani 1 1 d . . . H4 H 0.0239 0.0956 0.9196 0.052 Uiso 1 1 calc R . . C5 C 0.0745(3) 0.2353(2) 0.91398(19) 0.0402(7) Uani 1 1 d . . . H5 H 0.0534 0.2150 0.9780 0.048 Uiso 1 1 calc R . . C6 C 0.1203(3) 0.3358(2) 0.8564(2) 0.0468(7) Uani 1 1 d . . . H6 H 0.1259 0.3849 0.8813 0.056 Uiso 1 1 calc R . . C7 C 0.1576(3) 0.3661(2) 0.7638(2) 0.0443(7) Uani 1 1 d . . . H7 H 0.1933 0.4348 0.7253 0.053 Uiso 1 1 calc R . . C8 C 0.1430(3) 0.2932(2) 0.7240(2) 0.0468(7) Uani 1 1 d . . . C9 C 0.1830(3) 0.3330(2) 0.62268(19) 0.0417(7) Uani 1 1 d . . . C10 C 0.1998(3) 0.4441(2) 0.5613(2) 0.0466(7) Uani 1 1 d . . . C11 C 0.1015(3) 0.5134(2) 0.57423(18) 0.0383(6) Uani 1 1 d . . . H11 H 0.0212 0.4877 0.6255 0.046 Uiso 1 1 calc R . . C12 C 0.1110(3) 0.6185(2) 0.5175(2) 0.0480(7) Uani 1 1 d . . . H12 H 0.0394 0.6619 0.5296 0.058 Uiso 1 1 calc R . . C13 C 0.2308(3) 0.6566(2) 0.44238(19) 0.0397(6) Uani 1 1 d . . . C14 C 0.3383(3) 0.5906(2) 0.4246(2) 0.0513(8) Uani 1 1 d . . . H14 H 0.4200 0.6165 0.3744 0.062 Uiso 1 1 calc R . . C15 C 0.3186(4) 0.4840(2) 0.4853(2) 0.0553(9) Uani 1 1 d . . . H15 H 0.3880 0.4390 0.4738 0.066 Uiso 1 1 calc R . . C16 C 0.1688(3) 0.8346(2) 0.3960(2) 0.0438(7) Uani 1 1 d . . . H16A H 0.1070 0.8053 0.4584 0.066 Uiso 1 1 calc R . . H16B H 0.1112 0.8537 0.3529 0.066 Uiso 1 1 calc R . . H16C H 0.2234 0.8958 0.3872 0.066 Uiso 1 1 calc R . . C17 C 0.1935(3) -0.0519(2) 0.5940(2) 0.0459(7) Uani 1 1 d . . . H17A H 0.0969 -0.0547 0.5874 0.055 Uiso 1 1 calc R . . H17B H 0.2309 -0.1203 0.6043 0.055 Uiso 1 1 calc R . . C18 C 0.2899(3) 0.0308(2) 0.50694(19) 0.0386(6) Uani 1 1 d U . . C19 C 0.4001(3) 0.2046(2) 0.44232(19) 0.0436(7) Uani 1 1 d . . . C20 C 0.5243(3) 0.2447(2) 0.4507(2) 0.0457(7) Uani 1 1 d . . . H20 H 0.5520 0.2120 0.5052 0.055 Uiso 1 1 calc R . . C21 C 0.6081(3) 0.3336(2) 0.3785(2) 0.0427(7) Uani 1 1 d . . . H21 H 0.6923 0.3575 0.3842 0.051 Uiso 1 1 calc R . . C22 C 0.5646(3) 0.3835(2) 0.3011(2) 0.0450(7) Uani 1 1 d . . . H22 H 0.6152 0.4451 0.2550 0.054 Uiso 1 1 calc R . . C23 C 0.4480(3) 0.3446(2) 0.2900(2) 0.0472(7) Uani 1 1 d . . . H23 H 0.4253 0.3771 0.2337 0.057 Uiso 1 1 calc R . . C24 C 0.3589(3) 0.2566(2) 0.36035(19) 0.0406(6) Uani 1 1 d . . . C25 C 0.2261(3) 0.2262(2) 0.3438(2) 0.0456(7) Uani 1 1 d . . . C26 C 0.2394(3) 0.2312(2) 0.2485(2) 0.0430(7) Uani 1 1 d . . . C27 C 0.3331(3) 0.1676(2) 0.2188(2) 0.0424(7) Uani 1 1 d . . . H27 H 0.3859 0.1251 0.2577 0.051 Uiso 1 1 calc R . . C28 C 0.3513(3) 0.1643(2) 0.1342(2) 0.0469(7) Uani 1 1 d . . . H28 H 0.4139 0.1188 0.1166 0.056 Uiso 1 1 calc R . . C29 C 0.2756(3) 0.2298(2) 0.0737(2) 0.0474(7) Uani 1 1 d . . . H29 H 0.2876 0.2280 0.0157 0.057 Uiso 1 1 calc R . . C30 C 0.1845(3) 0.2959(2) 0.1001(2) 0.0443(7) Uani 1 1 d . . . H30 H 0.1350 0.3402 0.0597 0.053 Uiso 1 1 calc R . . C31 C 0.1647(3) 0.2976(2) 0.1884(2) 0.0395(6) Uani 1 1 d . . . C32 C 0.0603(3) 0.3687(2) 0.2132(2) 0.0470(7) Uani 1 1 d . . . C33 C 0.3119(3) -0.0704(2) 0.7160(2) 0.0479(7) Uani 1 1 d . . . H33A H 0.2890 -0.1454 0.7492 0.058 Uiso 1 1 calc R . . H33B H 0.3985 -0.0597 0.6655 0.058 Uiso 1 1 calc R . . C34 C 0.3446(3) -0.0282(2) 0.7809(2) 0.0467(7) Uani 1 1 d . . . C35 C 0.2753(3) -0.0760(2) 0.87785(19) 0.0449(7) Uani 1 1 d . . . H35 H 0.2120 -0.1353 0.9018 0.054 Uiso 1 1 calc R . . C36 C 0.3022(3) -0.0345(2) 0.9343(2) 0.0447(7) Uani 1 1 d . . . H36 H 0.2548 -0.0652 0.9974 0.054 Uiso 1 1 calc R . . C37 C 0.3990(3) 0.0532(2) 0.9016(2) 0.0475(7) Uani 1 1 d . . . H37 H 0.4175 0.0811 0.9413 0.057 Uiso 1 1 calc R . . C38 C 0.4650(3) 0.0958(2) 0.8079(2) 0.0449(7) Uani 1 1 d . . . H38 H 0.5311 0.1535 0.7841 0.054 Uiso 1 1 calc R . . C39 C 0.4382(3) 0.0574(2) 0.7484(2) 0.0440(7) Uani 1 1 d . . . H39 H 0.4840 0.0898 0.6852 0.053 Uiso 1 1 calc R . . F1 F -0.06386(19) 0.31927(13) 0.27119(12) 0.0561(5) Uani 1 1 d . . . F2 F 0.10669(18) 0.41662(12) 0.25912(12) 0.0476(4) Uani 1 1 d . . . F3 F 0.02915(17) 0.44379(13) 0.14315(11) 0.0492(4) Uani 1 1 d . . . N1 N 0.1899(3) -0.02307(18) 0.67463(17) 0.0456(6) Uani 1 1 d . . . N2 N 0.3158(3) 0.12017(18) 0.51731(16) 0.0426(6) Uani 1 1 d U . . N3 N 0.0908(3) 0.11421(19) 0.74482(16) 0.0421(6) Uani 1 1 d . . . Ni1 Ni 0.20857(4) 0.12579(3) 0.62935(3) 0.03768(11) Uani 1 1 d . . . O1 O -0.0811(2) -0.00291(15) 0.86659(14) 0.0491(5) Uani 1 1 d . . . O2 O 0.2194(2) 0.27008(15) 0.57982(14) 0.0469(5) Uani 1 1 d . . . O3 O 0.2642(2) 0.75952(15) 0.38058(14) 0.0470(5) Uani 1 1 d . . . O4 O 0.3404(2) 0.01288(15) 0.43629(13) 0.0447(5) Uani 1 1 d . . . O5 O 0.1111(2) 0.20175(15) 0.40381(14) 0.0449(5) Uani 1 1 d . . . O1W O 0.3035(7) 0.6043(5) 0.9572(5) 0.064(2) Uani 0.30 1 d P . . H1WA H 0.3931 0.6233 0.9349 0.096 Uiso 0.30 1 d PR . . H1WB H 0.2551 0.6564 0.9362 0.096 Uiso 0.30 1 d PR . . O2W O 0.2983(6) 0.6808(4) 0.1708(3) 0.0493(13) Uani 0.40 1 d P . . H2WA H 0.3202 0.7441 0.1324 0.074 Uiso 0.40 1 d PR . . H2WC H 0.2147 0.6617 0.1724 0.074 Uiso 0.40 1 d PR . . O3W O 0.4314(7) 0.5858(5) 0.1102(4) 0.0481(17) Uani 0.30 1 d P . . H3WA H 0.4199 0.5990 0.0570 0.072 Uiso 0.30 1 d PR . . H3WB H 0.5191 0.6005 0.1045 0.072 Uiso 0.30 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0528(19) 0.0525(19) 0.0455(18) -0.0178(16) 0.0046(14) -0.0063(15) C2 0.0433(17) 0.0406(16) 0.0376(15) -0.0103(13) -0.0010(13) 0.0009(13) C3 0.0401(16) 0.0477(17) 0.0357(15) -0.0168(14) -0.0051(12) 0.0024(13) C4 0.0416(16) 0.0457(17) 0.0364(15) -0.0137(14) -0.0063(12) 0.0051(13) C5 0.0417(16) 0.0411(16) 0.0358(15) -0.0144(13) -0.0104(12) 0.0128(13) C6 0.0426(17) 0.0558(19) 0.0404(17) -0.0134(15) -0.0154(13) -0.0109(14) C7 0.0421(16) 0.0462(17) 0.0364(15) -0.0052(14) -0.0142(13) -0.0013(13) C8 0.0456(17) 0.0450(17) 0.0359(15) -0.0065(14) -0.0041(13) 0.0036(13) C9 0.0498(17) 0.0306(14) 0.0362(15) -0.0105(12) -0.0019(13) 0.0001(12) C10 0.0527(18) 0.0429(17) 0.0384(16) -0.0113(14) -0.0100(13) -0.0018(14) C11 0.0425(16) 0.0400(15) 0.0306(14) -0.0123(13) -0.0082(12) -0.0075(12) C12 0.0387(16) 0.0401(17) 0.0527(18) -0.0105(14) -0.0045(14) 0.0019(13) C13 0.0419(16) 0.0369(15) 0.0330(14) -0.0067(12) -0.0113(12) 0.0128(12) C14 0.0524(19) 0.0405(17) 0.0458(18) -0.0122(14) 0.0017(14) 0.0111(14) C15 0.058(2) 0.0422(18) 0.0422(17) -0.0052(15) 0.0038(15) 0.0134(15) C16 0.0422(16) 0.0386(15) 0.0392(15) -0.0003(13) -0.0176(13) 0.0117(13) C17 0.0450(17) 0.0483(17) 0.0415(16) -0.0193(14) -0.0038(13) -0.0050(13) C18 0.0400(16) 0.0407(14) 0.0404(16) -0.0185(13) -0.0155(12) 0.0030(12) C19 0.0471(17) 0.0457(17) 0.0328(14) -0.0134(13) -0.0046(13) -0.0043(13) C20 0.0382(16) 0.0418(16) 0.0498(17) -0.0109(14) -0.0131(14) 0.0127(13) C21 0.0354(16) 0.0471(17) 0.0428(16) -0.0175(14) -0.0058(13) -0.0032(13) C22 0.0446(17) 0.0388(16) 0.0482(17) -0.0109(14) -0.0144(14) -0.0145(13) C23 0.0445(17) 0.0453(17) 0.0441(16) -0.0103(14) -0.0088(13) -0.0156(13) C24 0.0348(15) 0.0429(16) 0.0369(15) -0.0115(13) -0.0045(12) -0.0008(12) C25 0.0410(17) 0.0503(18) 0.0389(16) -0.0140(14) -0.0052(13) -0.0060(13) C26 0.0431(17) 0.0407(16) 0.0463(17) -0.0163(14) -0.0156(13) 0.0050(13) C27 0.0357(15) 0.0428(16) 0.0460(17) -0.0145(14) -0.0126(13) 0.0090(13) C28 0.0418(17) 0.0471(17) 0.0513(18) -0.0199(15) -0.0133(14) 0.0174(14) C29 0.0473(17) 0.0441(17) 0.0446(17) -0.0131(14) -0.0112(14) 0.0119(14) C30 0.0446(17) 0.0441(17) 0.0416(16) -0.0148(14) -0.0130(13) 0.0153(13) C31 0.0454(17) 0.0296(14) 0.0425(16) -0.0123(13) -0.0132(13) 0.0007(12) C32 0.0487(18) 0.0455(18) 0.0391(16) -0.0105(14) -0.0105(14) 0.0113(14) C33 0.0548(19) 0.0434(17) 0.0368(15) -0.0104(14) -0.0083(14) 0.0110(14) C34 0.0425(17) 0.0522(19) 0.0397(16) -0.0134(14) -0.0103(13) 0.0073(14) C35 0.0530(18) 0.0356(16) 0.0352(15) -0.0078(13) -0.0044(13) 0.0042(13) C36 0.0440(16) 0.0465(17) 0.0397(16) -0.0155(14) -0.0090(13) 0.0112(14) C37 0.0503(18) 0.0446(17) 0.0456(17) -0.0158(15) -0.0149(14) 0.0130(14) C38 0.0489(17) 0.0457(17) 0.0375(15) -0.0153(14) -0.0113(13) 0.0136(14) C39 0.0429(17) 0.0462(17) 0.0369(15) -0.0097(14) -0.0141(13) 0.0176(14) F1 0.0513(11) 0.0496(11) 0.0518(11) -0.0174(9) 0.0048(9) 0.0130(8) F2 0.0493(10) 0.0425(10) 0.0499(10) -0.0187(8) -0.0136(8) 0.0175(8) F3 0.0428(10) 0.0488(10) 0.0492(10) -0.0118(8) -0.0160(8) 0.0197(8) N1 0.0470(15) 0.0378(13) 0.0444(14) -0.0135(11) -0.0040(11) -0.0037(11) N2 0.0465(14) 0.0339(12) 0.0392(13) -0.0123(11) -0.0027(11) 0.0063(10) N3 0.0440(14) 0.0435(14) 0.0339(13) -0.0125(11) -0.0076(11) 0.0064(11) Ni1 0.0448(2) 0.0345(2) 0.03397(19) -0.01723(15) -0.00552(15) 0.00191(15) O1 0.0427(11) 0.0412(11) 0.0501(12) -0.0188(10) 0.0117(9) -0.0139(9) O2 0.0487(12) 0.0388(11) 0.0464(12) -0.0156(10) -0.0046(10) 0.0051(9) O3 0.0420(12) 0.0327(10) 0.0447(11) 0.0007(9) -0.0025(9) 0.0033(9) O4 0.0458(12) 0.0378(11) 0.0423(12) -0.0145(9) -0.0010(9) 0.0008(9) O5 0.0354(11) 0.0428(11) 0.0496(12) -0.0152(10) -0.0042(9) -0.0060(9) O1W 0.042(4) 0.039(4) 0.077(5) -0.021(4) 0.035(4) 0.001(3) O2W 0.051(3) 0.053(3) 0.041(3) -0.013(3) -0.015(2) -0.004(2) O3W 0.034(4) 0.064(5) 0.039(4) -0.016(3) -0.004(3) -0.005(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 C1 N1 1.475(4) . ? C1 C2 1.515(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O1 1.233(3) . ? C2 N3 1.315(4) . ? C3 N3 1.402(4) . ? C3 C4 1.394(4) . ? C3 C8 1.411(4) . ? C4 C5 1.361(4) . ? C4 H4 0.9300 . ? C5 C6 1.350(4) . ? C5 H5 0.9300 . ? C6 C7 1.342(4) . ? C6 H6 0.9300 . ? C7 C8 1.428(4) . ? C7 H7 0.9300 . ? C8 C9 1.460(4) . ? C9 O2 1.302(3) . ? C9 C10 1.460(4) . ? C10 C11 1.359(4) . ? C10 C15 1.378(4) . ? C11 C12 1.379(4) . ? C11 H11 0.9300 . ? C12 C13 1.376(4) . ? C12 H12 0.9300 . ? C13 O3 1.376(3) . ? C13 C14 1.403(4) . ? C14 C15 1.406(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O3 1.415(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N1 1.507(4) . ? C17 C18 1.513(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 O4 1.238(3) . ? C18 N2 1.359(4) . ? C19 N2 1.395(4) . ? C19 C20 1.402(4) . ? C19 C24 1.401(4) . ? C20 C21 1.411(4) . ? C20 H20 0.9300 . ? C21 C22 1.348(4) . ? C21 H21 0.9300 . ? C22 C23 1.352(4) . ? C22 H22 0.9300 . ? C23 C24 1.415(4) . ? C23 H23 0.9300 . ? C24 C25 1.486(4) . ? C25 O5 1.219(3) . ? C25 C26 1.495(4) . ? C26 C27 1.366(4) . ? C26 C31 1.394(4) . ? C27 C28 1.358(4) . ? C27 H27 0.9300 . ? C28 C29 1.400(4) . ? C28 H28 0.9300 . ? C29 C30 1.357(4) . ? C29 H29 0.9300 . ? C30 C31 1.407(4) . ? C30 H30 0.9300 . ? C31 C32 1.471(4) . ? C32 F3 1.305(3) . ? C32 F1 1.322(3) . ? C32 F2 1.341(4) . ? C33 C34 1.496(4) . ? C33 N1 1.512(4) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C39 1.359(4) . ? C34 C35 1.422(4) . ? C35 C36 1.342(4) . ? C35 H35 0.9300 . ? C36 C37 1.399(4) . ? C36 H36 0.9300 . ? C37 C38 1.371(4) . ? C37 H37 0.9300 . ? C38 C39 1.356(4) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? N1 Ni1 1.902(3) . ? N2 Ni1 1.868(2) . ? N3 Ni1 1.864(2) . ? Ni1 O2 1.839(2) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8499 . ? O2W H2WC 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? 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 N1 C1 C2 111.5(3) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? O1 C2 N3 128.0(3) . . ? O1 C2 C1 118.6(3) . . ? N3 C2 C1 113.4(3) . . ? N3 C3 C4 124.1(3) . . ? N3 C3 C8 119.5(3) . . ? C4 C3 C8 116.4(3) . . ? C5 C4 C3 122.8(3) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 121.1(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 120.4(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C3 C8 C7 119.1(3) . . ? C3 C8 C9 123.9(3) . . ? C7 C8 C9 117.0(3) . . ? O2 C9 C8 121.1(3) . . ? O2 C9 C10 114.4(3) . . ? C8 C9 C10 124.2(3) . . ? C11 C10 C15 116.3(3) . . ? C11 C10 C9 123.1(3) . . ? C15 C10 C9 120.6(3) . . ? C10 C11 C12 125.3(3) . . ? C10 C11 H11 117.3 . . ? C12 C11 H11 117.3 . . ? C13 C12 C11 117.2(3) . . ? C13 C12 H12 121.4 . . ? C11 C12 H12 121.4 . . ? C12 C13 O3 126.2(2) . . ? C12 C13 C14 121.0(3) . . ? O3 C13 C14 112.7(2) . . ? C13 C14 C15 117.9(3) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C10 C15 C14 122.2(3) . . ? C10 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? O3 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 C18 108.0(2) . . ? N1 C17 H17A 110.1 . . ? C18 C17 H17A 110.1 . . ? N1 C17 H17B 110.1 . . ? C18 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? O4 C18 N2 126.1(3) . . ? O4 C18 C17 120.6(3) . . ? N2 C18 C17 113.3(2) . . ? N2 C19 C20 119.7(3) . . ? N2 C19 C24 121.9(3) . . ? C20 C19 C24 118.2(3) . . ? C19 C20 C21 121.6(3) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 119.2(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 122.8(3) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C19 C24 C23 117.7(3) . . ? C19 C24 C25 124.0(3) . . ? C23 C24 C25 118.3(3) . . ? O5 C25 C24 121.9(3) . . ? O5 C25 C26 121.6(3) . . ? C24 C25 C26 116.5(2) . . ? C27 C26 C31 118.7(3) . . ? C27 C26 C25 117.2(3) . . ? C31 C26 C25 124.1(3) . . ? C28 C27 C26 122.0(3) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C29 119.7(3) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 119.7(3) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.1(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C26 C31 C30 119.6(3) . . ? C26 C31 C32 123.4(3) . . ? C30 C31 C32 116.9(2) . . ? F3 C32 F1 106.5(2) . . ? F3 C32 F2 105.5(2) . . ? F1 C32 F2 103.6(2) . . ? F3 C32 C31 115.2(3) . . ? F1 C32 C31 113.0(3) . . ? F2 C32 C31 112.1(2) . . ? C34 C33 N1 116.0(2) . . ? C34 C33 H33A 108.3 . . ? N1 C33 H33A 108.3 . . ? C34 C33 H33B 108.3 . . ? N1 C33 H33B 108.3 . . ? H33A C33 H33B 107.4 . . ? C39 C34 C35 118.8(3) . . ? C39 C34 C33 120.9(3) . . ? C35 C34 C33 120.3(3) . . ? C36 C35 C34 119.2(3) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 122.3(3) . . ? C35 C36 H36 118.8 . . ? C37 C36 H36 118.8 . . ? C38 C37 C36 116.4(3) . . ? C38 C37 H37 121.8 . . ? C36 C37 H37 121.8 . . ? C39 C38 C37 122.9(3) . . ? C39 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? C38 C39 C34 120.3(3) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? C1 N1 C17 112.6(2) . . ? C1 N1 C33 111.6(2) . . ? C17 N1 C33 109.9(2) . . ? C1 N1 Ni1 104.20(18) . . ? C17 N1 Ni1 107.81(18) . . ? C33 N1 Ni1 110.60(19) . . ? C18 N2 C19 119.9(2) . . ? C18 N2 Ni1 114.77(19) . . ? C19 N2 Ni1 124.59(19) . . ? C2 N3 C3 122.2(2) . . ? C2 N3 Ni1 113.3(2) . . ? C3 N3 Ni1 124.14(19) . . ? O2 Ni1 N3 93.67(10) . . ? O2 Ni1 N2 93.03(9) . . ? N3 Ni1 N2 172.54(11) . . ? O2 Ni1 N1 175.95(11) . . ? N3 Ni1 N1 87.90(11) . . ? N2 Ni1 N1 85.21(10) . . ? C9 O2 Ni1 128.69(19) . . ? C13 O3 C16 117.6(2) . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WC 109.5 . . ? H3WA O3W H3WB 109.5 . . ? 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 N1 C1 C2 O1 -162.9(3) . . . . ? N1 C1 C2 N3 17.8(4) . . . . ? N3 C3 C4 C5 174.8(3) . . . . ? C8 C3 C4 C5 -2.2(4) . . . . ? C3 C4 C5 C6 2.6(4) . . . . ? C4 C5 C6 C7 -3.0(4) . . . . ? C5 C6 C7 C8 3.1(4) . . . . ? N3 C3 C8 C7 -175.0(3) . . . . ? C4 C3 C8 C7 2.2(4) . . . . ? N3 C3 C8 C9 3.6(4) . . . . ? C4 C3 C8 C9 -179.3(3) . . . . ? C6 C7 C8 C3 -2.7(4) . . . . ? C6 C7 C8 C9 178.7(3) . . . . ? C3 C8 C9 O2 -21.5(5) . . . . ? C7 C8 C9 O2 157.0(3) . . . . ? C3 C8 C9 C10 164.7(3) . . . . ? C7 C8 C9 C10 -16.7(4) . . . . ? O2 C9 C10 C11 138.5(3) . . . . ? C8 C9 C10 C11 -47.3(5) . . . . ? O2 C9 C10 C15 -40.9(4) . . . . ? C8 C9 C10 C15 133.2(3) . . . . ? C15 C10 C11 C12 0.6(5) . . . . ? C9 C10 C11 C12 -178.8(3) . . . . ? C10 C11 C12 C13 -0.9(5) . . . . ? C11 C12 C13 O3 -176.4(3) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C12 C13 C14 C15 1.0(5) . . . . ? O3 C13 C14 C15 177.8(3) . . . . ? C11 C10 C15 C14 0.5(5) . . . . ? C9 C10 C15 C14 180.0(3) . . . . ? C13 C14 C15 C10 -1.2(5) . . . . ? N1 C17 C18 O4 161.5(3) . . . . ? N1 C17 C18 N2 -16.4(3) . . . . ? N2 C19 C20 C21 -176.5(3) . . . . ? C24 C19 C20 C21 -1.3(4) . . . . ? C19 C20 C21 C22 2.7(5) . . . . ? C20 C21 C22 C23 -4.7(5) . . . . ? C21 C22 C23 C24 5.5(5) . . . . ? N2 C19 C24 C23 176.9(3) . . . . ? C20 C19 C24 C23 1.9(4) . . . . ? N2 C19 C24 C25 -1.7(5) . . . . ? C20 C19 C24 C25 -176.8(3) . . . . ? C22 C23 C24 C19 -4.0(5) . . . . ? C22 C23 C24 C25 174.7(3) . . . . ? C19 C24 C25 O5 42.3(5) . . . . ? C23 C24 C25 O5 -136.3(3) . . . . ? C19 C24 C25 C26 -140.0(3) . . . . ? C23 C24 C25 C26 41.4(4) . . . . ? O5 C25 C26 C27 -120.5(3) . . . . ? C24 C25 C26 C27 61.8(4) . . . . ? O5 C25 C26 C31 60.8(4) . . . . ? C24 C25 C26 C31 -116.9(3) . . . . ? C31 C26 C27 C28 -2.5(5) . . . . ? C25 C26 C27 C28 178.7(3) . . . . ? C26 C27 C28 C29 1.8(5) . . . . ? C27 C28 C29 C30 0.0(5) . . . . ? C28 C29 C30 C31 -0.9(5) . . . . ? C27 C26 C31 C30 1.5(4) . . . . ? C25 C26 C31 C30 -179.7(3) . . . . ? C27 C26 C31 C32 179.4(3) . . . . ? C25 C26 C31 C32 -1.9(5) . . . . ? C29 C30 C31 C26 0.1(5) . . . . ? C29 C30 C31 C32 -177.9(3) . . . . ? C26 C31 C32 F3 162.7(3) . . . . ? C30 C31 C32 F3 -19.4(4) . . . . ? C26 C31 C32 F1 -74.6(4) . . . . ? C30 C31 C32 F1 103.3(3) . . . . ? C26 C31 C32 F2 42.0(4) . . . . ? C30 C31 C32 F2 -140.1(3) . . . . ? N1 C33 C34 C39 -87.9(3) . . . . ? N1 C33 C34 C35 90.6(3) . . . . ? C39 C34 C35 C36 1.0(4) . . . . ? C33 C34 C35 C36 -177.5(3) . . . . ? C34 C35 C36 C37 -1.5(4) . . . . ? C35 C36 C37 C38 0.5(4) . . . . ? C36 C37 C38 C39 1.0(4) . . . . ? C37 C38 C39 C34 -1.4(4) . . . . ? C35 C34 C39 C38 0.4(4) . . . . ? C33 C34 C39 C38 178.9(3) . . . . ? C2 C1 N1 C17 -147.1(3) . . . . ? C2 C1 N1 C33 88.8(3) . . . . ? C2 C1 N1 Ni1 -30.5(3) . . . . ? C18 C17 N1 C1 146.3(3) . . . . ? C18 C17 N1 C33 -88.7(3) . . . . ? C18 C17 N1 Ni1 31.9(3) . . . . ? C34 C33 N1 C1 -68.7(3) . . . . ? C34 C33 N1 C17 165.7(2) . . . . ? C34 C33 N1 Ni1 46.8(3) . . . . ? O4 C18 N2 C19 3.8(4) . . . . ? C17 C18 N2 C19 -178.4(3) . . . . ? O4 C18 N2 Ni1 174.6(2) . . . . ? C17 C18 N2 Ni1 -7.6(3) . . . . ? C20 C19 N2 C18 -122.8(3) . . . . ? C24 C19 N2 C18 62.2(4) . . . . ? C20 C19 N2 Ni1 67.3(4) . . . . ? C24 C19 N2 Ni1 -107.7(3) . . . . ? O1 C2 N3 C3 13.0(5) . . . . ? C1 C2 N3 C3 -167.7(3) . . . . ? O1 C2 N3 Ni1 -173.8(3) . . . . ? C1 C2 N3 Ni1 5.4(3) . . . . ? C4 C3 N3 C2 21.3(4) . . . . ? C8 C3 N3 C2 -161.8(3) . . . . ? C4 C3 N3 Ni1 -151.1(2) . . . . ? C8 C3 N3 Ni1 25.8(4) . . . . ? C2 N3 Ni1 O2 156.5(2) . . . . ? C3 N3 Ni1 O2 -30.6(2) . . . . ? C2 N3 Ni1 N1 -19.8(2) . . . . ? C3 N3 Ni1 N1 153.2(2) . . . . ? C18 N2 Ni1 O2 -154.3(2) . . . . ? C19 N2 Ni1 O2 16.1(2) . . . . ? C18 N2 Ni1 N1 22.1(2) . . . . ? C19 N2 Ni1 N1 -167.5(2) . . . . ? C1 N1 Ni1 N3 27.4(2) . . . . ? C17 N1 Ni1 N3 147.24(19) . . . . ? C33 N1 Ni1 N3 -92.57(19) . . . . ? C1 N1 Ni1 N2 -149.7(2) . . . . ? C17 N1 Ni1 N2 -29.9(2) . . . . ? C33 N1 Ni1 N2 90.28(19) . . . . ? C8 C9 O2 Ni1 8.3(4) . . . . ? C10 C9 O2 Ni1 -177.4(2) . . . . ? N3 Ni1 O2 C9 13.7(3) . . . . ? N2 Ni1 O2 C9 -169.6(3) . . . . ? C12 C13 O3 C16 1.5(4) . . . . ? C14 C13 O3 C16 -175.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.559 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.047 _database_code_depnum_ccdc_archive 'CCDC 951882' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_no8 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H30 F3 N3 O5 Pd' _chemical_formula_sum 'C39 H30 F3 N3 O5 Pd' _chemical_formula_weight 784.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_int_tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9428(2) _cell_length_b 23.9074(4) _cell_length_c 26.1834(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6849.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 74634 _cell_measurement_theta_min 4.75 _cell_measurement_theta_max 68.17 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 4.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7593 _exptl_absorpt_correction_T_max 0.9077 _exptl_absorpt_process_details 'absorption was corrected by abscor' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54186 _diffrn_source 'rotating anode x-ray' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID IP area detector system' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74634 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 4.75 _diffrn_reflns_theta_max 68.17 _reflns_number_total 6252 _reflns_number_gt 4073 _reflns_threshold_expression >2\s(I) _computing_data_collection 'PROCESS-AUTO (Rigaku, 1998)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0662P)^2^+30.6229P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00023(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6252 _refine_ls_number_parameters 461 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 C1 C 0.6722(9) 0.0124(4) 0.6399(3) 0.079(3) Uani 1 1 d . . . H1 H 0.6909 0.0009 0.6069 0.095 Uiso 1 1 calc R . . C2 C 0.7473(13) -0.0035(6) 0.6800(5) 0.116(4) Uani 1 1 d . . . H2 H 0.8160 -0.0254 0.6739 0.139 Uiso 1 1 calc R . . C3 C 0.7193(17) 0.0133(6) 0.7286(5) 0.136(6) Uani 1 1 d . . . H3 H 0.7704 0.0034 0.7555 0.163 Uiso 1 1 calc R . . C4 C 0.6174(18) 0.0445(5) 0.7379(4) 0.137(6) Uani 1 1 d . . . H4 H 0.5986 0.0554 0.7711 0.164 Uiso 1 1 calc R . . C5 C 0.5410(12) 0.0601(4) 0.6973(3) 0.096(3) Uani 1 1 d . . . H5 H 0.4706 0.0807 0.7037 0.115 Uiso 1 1 calc R . . C25 C 1.3682(9) 0.1948(4) 0.3802(3) 0.078(3) Uani 1 1 d . . . H25A H 1.4382 0.2121 0.3646 0.118 Uiso 1 1 calc R . . H25B H 1.3000 0.1969 0.3572 0.118 Uiso 1 1 calc R . . H25C H 1.3862 0.1564 0.3875 0.118 Uiso 1 1 calc R . . C6 C 0.5697(9) 0.0451(3) 0.6482(3) 0.064(2) Uani 1 1 d . . . C7 C 0.4884(8) 0.0602(3) 0.6040(3) 0.063(2) Uani 1 1 d . . . H7A H 0.4057 0.0652 0.6165 0.076 Uiso 1 1 calc R . . H7B H 0.4876 0.0293 0.5800 0.076 Uiso 1 1 calc R . . C8 C 0.5138(7) 0.1641(3) 0.6094(3) 0.063(2) Uani 1 1 d . . . H8A H 0.4485 0.1579 0.6338 0.075 Uiso 1 1 calc R . . H8B H 0.4905 0.1955 0.5881 0.075 Uiso 1 1 calc R . . C9 C 0.6297(8) 0.1789(3) 0.6382(3) 0.0607(19) Uani 1 1 d . . . C10 C 0.4584(7) 0.1155(4) 0.5265(3) 0.062(2) Uani 1 1 d . . . H10A H 0.4533 0.1543 0.5158 0.075 Uiso 1 1 calc R . . H10B H 0.3758 0.1020 0.5317 0.075 Uiso 1 1 calc R . . C11 C 0.5187(7) 0.0814(3) 0.4846(3) 0.0569(18) Uani 1 1 d . . . C12 C 0.8506(7) 0.1631(3) 0.6384(3) 0.0526(17) Uani 1 1 d . . . C13 C 0.8660(9) 0.1716(3) 0.6910(3) 0.067(2) Uani 1 1 d . . . H13 H 0.7976 0.1750 0.7119 0.080 Uiso 1 1 calc R . . C14 C 0.9807(9) 0.1748(4) 0.7123(3) 0.072(2) Uani 1 1 d . . . H14 H 0.9884 0.1812 0.7472 0.086 Uiso 1 1 calc R . . C15 C 1.0849(9) 0.1689(4) 0.6829(3) 0.075(2) Uani 1 1 d . . . H15 H 1.1620 0.1702 0.6977 0.090 Uiso 1 1 calc R . . C16 C 1.0717(8) 0.1610(3) 0.6310(3) 0.062(2) Uani 1 1 d . . . H16 H 1.1414 0.1571 0.6111 0.074 Uiso 1 1 calc R . . C17 C 0.9554(7) 0.1587(3) 0.6070(2) 0.0490(16) Uani 1 1 d . . . C18 C 0.9535(7) 0.1502(3) 0.5515(2) 0.0489(16) Uani 1 1 d . . . C19 C 1.0541(6) 0.1703(3) 0.5187(2) 0.0492(16) Uani 1 1 d . . . C20 C 1.1216(7) 0.2186(3) 0.5293(3) 0.0591(19) Uani 1 1 d . . . H20 H 1.1039 0.2394 0.5583 0.071 Uiso 1 1 calc R . . C21 C 1.2134(7) 0.2355(3) 0.4973(3) 0.062(2) Uani 1 1 d . . . H21 H 1.2569 0.2679 0.5048 0.074 Uiso 1 1 calc R . . C22 C 1.2424(7) 0.2053(3) 0.4541(3) 0.0567(18) Uani 1 1 d . . . C23 C 1.1738(7) 0.1577(3) 0.4420(3) 0.063(2) Uani 1 1 d . . . H23 H 1.1916 0.1372 0.4128 0.076 Uiso 1 1 calc R . . C24 C 1.0804(7) 0.1413(3) 0.4734(3) 0.0590(19) Uani 1 1 d . . . H24 H 1.0334 0.1104 0.4646 0.071 Uiso 1 1 calc R . . C26 C 0.7155(7) 0.0464(3) 0.4573(2) 0.0479(16) Uani 1 1 d . . . C27 C 0.7842(8) 0.0013(3) 0.4724(3) 0.064(2) Uani 1 1 d . . . H27 H 0.7750 -0.0128 0.5053 0.077 Uiso 1 1 calc R . . C28 C 0.8673(10) -0.0235(4) 0.4394(3) 0.084(3) Uani 1 1 d . . . H28 H 0.9145 -0.0535 0.4506 0.100 Uiso 1 1 calc R . . C29 C 0.8800(9) -0.0040(4) 0.3901(3) 0.083(3) Uani 1 1 d . . . H29 H 0.9338 -0.0213 0.3676 0.100 Uiso 1 1 calc R . . C30 C 0.8121(8) 0.0416(3) 0.3745(3) 0.070(2) Uani 1 1 d . . . H30 H 0.8202 0.0545 0.3412 0.084 Uiso 1 1 calc R . . C31 C 0.7319(7) 0.0686(3) 0.4074(3) 0.0534(17) Uani 1 1 d . . . C32 C 0.6786(7) 0.1222(3) 0.3914(3) 0.0592(19) Uani 1 1 d . . . C33 C 0.6555(8) 0.1312(3) 0.3354(3) 0.0601(19) Uani 1 1 d . . . C34 C 0.5697(9) 0.0986(4) 0.3113(4) 0.081(3) Uani 1 1 d . . . H34 H 0.5322 0.0695 0.3290 0.097 Uiso 1 1 calc R . . C35 C 0.5384(11) 0.1088(5) 0.2603(4) 0.107(4) Uani 1 1 d . . . H35 H 0.4797 0.0871 0.2439 0.128 Uiso 1 1 calc R . . C36 C 0.5967(13) 0.1519(6) 0.2347(4) 0.112(4) Uani 1 1 d . . . H36 H 0.5767 0.1591 0.2008 0.134 Uiso 1 1 calc R . . C37 C 0.6823(11) 0.1838(5) 0.2582(4) 0.089(3) Uani 1 1 d . . . H37 H 0.7211 0.2122 0.2401 0.107 Uiso 1 1 calc R . . C38 C 0.7119(8) 0.1746(4) 0.3079(3) 0.066(2) Uani 1 1 d . . . C39 C 0.8097(9) 0.2088(4) 0.3317(4) 0.083(3) Uani 1 1 d . . . O1 O 0.6225(6) 0.2100(3) 0.6754(2) 0.0828(18) Uani 1 1 d . . . O2 O 0.4589(5) 0.0668(2) 0.44668(19) 0.0695(15) Uani 1 1 d . . . O3 O 0.6541(7) 0.1599(2) 0.4213(2) 0.0830(18) Uani 1 1 d . . . O4 O 0.8713(5) 0.1239(2) 0.52880(18) 0.0590(13) Uani 1 1 d . . . O5 O 1.3390(5) 0.2234(2) 0.4265(2) 0.0697(15) Uani 1 1 d . . . N1 N 0.7337(6) 0.1579(3) 0.6173(2) 0.0548(15) Uani 1 1 d . . . N2 N 0.5266(6) 0.1125(2) 0.5761(2) 0.0569(15) Uani 1 1 d . . . N3 N 0.6371(6) 0.0717(2) 0.4937(2) 0.0525(14) Uani 1 1 d . . . F1 F 0.7701(6) 0.2471(3) 0.3655(3) 0.114(2) Uani 1 1 d . . . F2 F 0.8916(5) 0.1780(3) 0.3572(2) 0.1049(18) Uani 1 1 d . . . F3 F 0.8740(6) 0.2379(3) 0.2977(3) 0.134(3) Uani 1 1 d . . . Pd1 Pd 0.70142(5) 0.11339(2) 0.554852(17) 0.0485(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.100(7) 0.077(6) 0.061(5) 0.012(5) -0.005(5) -0.007(5) C2 0.119(9) 0.119(10) 0.110(9) 0.024(8) -0.025(8) -0.013(8) C3 0.220(18) 0.099(10) 0.088(9) 0.019(8) -0.057(11) -0.022(11) C4 0.27(2) 0.091(9) 0.053(6) -0.001(6) -0.020(9) -0.004(11) C5 0.160(10) 0.076(6) 0.052(5) 0.002(4) 0.010(6) 0.006(7) C25 0.087(7) 0.088(6) 0.060(5) 0.009(5) 0.025(5) 0.007(5) C6 0.094(6) 0.054(4) 0.044(4) 0.005(3) 0.015(4) -0.021(4) C7 0.076(5) 0.059(5) 0.053(4) 0.001(4) 0.011(4) -0.012(4) C8 0.070(5) 0.059(5) 0.059(4) -0.012(4) 0.001(4) -0.003(4) C9 0.071(5) 0.059(5) 0.052(4) -0.001(4) 0.011(4) 0.000(4) C10 0.061(5) 0.076(5) 0.049(4) -0.006(4) 0.003(3) 0.007(4) C11 0.064(5) 0.055(4) 0.051(4) 0.003(3) 0.012(4) 0.004(4) C12 0.067(5) 0.049(4) 0.042(4) 0.002(3) 0.001(3) -0.004(4) C13 0.091(6) 0.076(5) 0.034(3) -0.002(4) 0.000(4) -0.006(5) C14 0.103(7) 0.074(6) 0.039(4) -0.004(4) -0.013(4) 0.001(5) C15 0.086(6) 0.086(6) 0.054(5) 0.003(4) -0.017(5) -0.006(5) C16 0.075(5) 0.062(5) 0.049(4) 0.002(4) -0.005(4) 0.001(4) C17 0.059(4) 0.052(4) 0.036(3) -0.007(3) -0.008(3) -0.007(3) C18 0.060(4) 0.041(3) 0.046(4) -0.004(3) -0.004(3) -0.005(3) C19 0.053(4) 0.051(4) 0.043(3) -0.002(3) 0.001(3) 0.001(3) C20 0.070(5) 0.058(4) 0.050(4) -0.006(3) 0.006(4) -0.006(4) C21 0.074(5) 0.050(4) 0.062(4) 0.000(4) 0.007(4) -0.004(4) C22 0.058(4) 0.058(4) 0.054(4) 0.005(3) 0.007(4) -0.001(4) C23 0.074(5) 0.066(5) 0.049(4) -0.002(4) 0.007(4) 0.003(4) C24 0.068(5) 0.061(5) 0.047(4) -0.007(3) 0.006(4) -0.008(4) C26 0.065(5) 0.044(4) 0.035(3) -0.013(3) -0.002(3) -0.003(3) C27 0.086(6) 0.063(5) 0.044(4) 0.012(4) 0.002(4) 0.014(4) C28 0.122(8) 0.070(6) 0.059(5) 0.002(4) 0.008(5) 0.039(6) C29 0.111(8) 0.078(6) 0.061(5) 0.001(4) 0.015(5) 0.035(6) C30 0.101(7) 0.064(5) 0.044(4) -0.003(4) 0.015(4) 0.016(5) C31 0.070(5) 0.047(4) 0.043(4) -0.005(3) 0.008(3) 0.003(3) C32 0.071(5) 0.053(4) 0.053(4) -0.004(3) 0.010(4) 0.013(4) C33 0.075(5) 0.060(4) 0.045(4) 0.001(3) 0.009(4) -0.006(4) C34 0.096(7) 0.067(6) 0.080(6) -0.002(5) 0.009(5) -0.007(5) C35 0.103(9) 0.132(10) 0.086(8) -0.017(7) -0.036(7) 0.005(8) C36 0.143(11) 0.127(10) 0.066(6) 0.023(7) -0.013(7) 0.030(9) C37 0.119(9) 0.089(7) 0.061(6) 0.025(5) 0.007(6) 0.018(6) C38 0.075(6) 0.064(5) 0.060(5) 0.013(4) 0.006(4) 0.012(4) C39 0.076(6) 0.083(6) 0.089(7) 0.022(6) 0.017(5) 0.006(5) O1 0.093(4) 0.092(4) 0.063(3) -0.046(3) 0.014(3) -0.003(3) O2 0.075(4) 0.077(4) 0.056(3) -0.012(3) -0.020(3) -0.001(3) O3 0.137(6) 0.051(3) 0.060(3) 0.000(3) 0.014(4) 0.022(3) O4 0.068(3) 0.062(3) 0.046(3) -0.011(2) 0.000(2) -0.009(3) O5 0.072(3) 0.067(3) 0.071(3) 0.002(3) 0.019(3) -0.006(3) N1 0.060(4) 0.057(4) 0.047(3) 0.001(3) 0.009(3) 0.004(3) N2 0.077(4) 0.045(3) 0.049(3) -0.009(3) 0.001(3) 0.003(3) N3 0.059(4) 0.054(3) 0.044(3) 0.000(3) 0.007(3) 0.002(3) F1 0.112(5) 0.086(4) 0.144(5) -0.026(4) 0.017(4) -0.006(4) F2 0.079(4) 0.113(5) 0.122(5) 0.015(4) -0.001(3) 0.001(3) F3 0.121(5) 0.132(6) 0.148(6) 0.047(5) 0.035(5) -0.034(4) Pd1 0.0587(4) 0.0499(3) 0.0368(3) -0.0039(2) 0.0039(2) -0.0011(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C6 1.385(12) . ? C1 C2 1.387(14) . ? C1 H1 0.9300 . ? C2 C3 1.370(18) . ? C2 H2 0.9300 . ? C3 C4 1.36(2) . ? C3 H3 0.9300 . ? C4 C5 1.404(16) . ? C4 H4 0.9300 . ? C5 C6 1.369(11) . ? C5 H5 0.9300 . ? C25 O5 1.428(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C6 C7 1.504(11) . ? C7 N2 1.507(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N2 1.517(9) . ? C8 C9 1.518(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O1 1.227(8) . ? C9 N1 1.359(9) . ? C10 N2 1.498(9) . ? C10 C11 1.521(10) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O2 1.239(9) . ? C11 N3 1.337(9) . ? C12 N1 1.399(9) . ? C12 C13 1.403(9) . ? C12 C17 1.415(10) . ? C13 C14 1.375(12) . ? C13 H13 0.9300 . ? C14 C15 1.383(12) . ? C14 H14 0.9300 . ? C15 C16 1.378(10) . ? C15 H15 0.9300 . ? C16 C17 1.421(10) . ? C16 H16 0.9300 . ? C17 C18 1.466(8) . ? C18 O4 1.248(8) . ? C18 C19 1.478(9) . ? C19 C20 1.399(10) . ? C19 C24 1.402(9) . ? C20 C21 1.369(10) . ? C20 H20 0.9300 . ? C21 C22 1.378(10) . ? C21 H21 0.9300 . ? C22 O5 1.352(9) . ? C22 C23 1.400(11) . ? C23 C24 1.369(10) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C26 C27 1.373(10) . ? C26 N3 1.418(8) . ? C26 C31 1.421(9) . ? C27 C28 1.388(11) . ? C27 H27 0.9300 . ? C28 C29 1.380(11) . ? C28 H28 0.9300 . ? C29 C30 1.380(11) . ? C29 H29 0.9300 . ? C30 C31 1.390(10) . ? C30 H30 0.9300 . ? C31 C32 1.470(10) . ? C32 O3 1.222(8) . ? C32 C33 1.503(10) . ? C33 C34 1.374(12) . ? C33 C38 1.404(11) . ? C34 C35 1.402(13) . ? C34 H34 0.9300 . ? C35 C36 1.384(16) . ? C35 H35 0.9300 . ? C36 C37 1.355(16) . ? C36 H36 0.9300 . ? C37 C38 1.361(12) . ? C37 H37 0.9300 . ? C38 C39 1.484(13) . ? C39 F3 1.331(10) . ? C39 F2 1.339(10) . ? C39 F1 1.346(11) . ? O4 Pd1 1.996(5) . ? N1 Pd1 1.983(6) . ? N2 Pd1 1.992(7) . ? N3 Pd1 2.012(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 121.0(10) . . ? C6 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 119.4(14) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C4 C3 C2 120.7(13) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.8(12) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.4(12) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? O5 C25 H25A 109.5 . . ? O5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C5 C6 C1 118.8(9) . . ? C5 C6 C7 121.6(9) . . ? C1 C6 C7 119.5(7) . . ? C6 C7 N2 114.1(6) . . ? C6 C7 H7A 108.7 . . ? N2 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? N2 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? N2 C8 C9 113.5(6) . . ? N2 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N2 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? O1 C9 N1 126.7(8) . . ? O1 C9 C8 118.8(7) . . ? N1 C9 C8 114.4(6) . . ? N2 C10 C11 112.5(6) . . ? N2 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? N2 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? O2 C11 N3 127.4(7) . . ? O2 C11 C10 120.0(7) . . ? N3 C11 C10 112.6(7) . . ? N1 C12 C13 120.7(7) . . ? N1 C12 C17 120.3(6) . . ? C13 C12 C17 118.9(7) . . ? C14 C13 C12 121.0(8) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 121.5(7) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 118.4(8) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C15 C16 C17 122.4(8) . . ? C15 C16 H16 118.8 . . ? C17 C16 H16 118.8 . . ? C12 C17 C16 117.7(6) . . ? C12 C17 C18 125.0(6) . . ? C16 C17 C18 117.2(7) . . ? O4 C18 C17 123.6(6) . . ? O4 C18 C19 115.0(6) . . ? C17 C18 C19 121.4(6) . . ? C20 C19 C24 117.8(7) . . ? C20 C19 C18 123.2(6) . . ? C24 C19 C18 119.0(6) . . ? C21 C20 C19 120.7(7) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 121.0(7) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? O5 C22 C21 116.8(7) . . ? O5 C22 C23 124.0(7) . . ? C21 C22 C23 119.2(7) . . ? C24 C23 C22 119.8(7) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 121.3(7) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? C27 C26 N3 118.2(6) . . ? C27 C26 C31 119.2(6) . . ? N3 C26 C31 122.4(6) . . ? C26 C27 C28 121.1(7) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 120.2(8) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.3(8) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C29 C30 C31 121.6(7) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C30 C31 C26 118.5(7) . . ? C30 C31 C32 118.7(6) . . ? C26 C31 C32 122.5(6) . . ? O3 C32 C31 123.2(7) . . ? O3 C32 C33 118.8(7) . . ? C31 C32 C33 118.0(6) . . ? C34 C33 C38 119.0(8) . . ? C34 C33 C32 118.8(7) . . ? C38 C33 C32 122.1(7) . . ? C33 C34 C35 120.4(9) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C36 C35 C34 118.5(11) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C37 C36 C35 121.3(10) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 120.5(10) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C33 120.4(9) . . ? C37 C38 C39 118.9(9) . . ? C33 C38 C39 120.6(8) . . ? F3 C39 F2 105.5(8) . . ? F3 C39 F1 104.8(9) . . ? F2 C39 F1 105.1(9) . . ? F3 C39 C38 112.9(9) . . ? F2 C39 C38 112.9(8) . . ? F1 C39 C38 114.8(8) . . ? C18 O4 Pd1 124.8(4) . . ? C22 O5 C25 118.5(6) . . ? C9 N1 C12 125.0(6) . . ? C9 N1 Pd1 112.4(5) . . ? C12 N1 Pd1 122.4(5) . . ? C10 N2 C7 108.8(6) . . ? C10 N2 C8 114.3(6) . . ? C7 N2 C8 111.7(6) . . ? C10 N2 Pd1 103.7(4) . . ? C7 N2 Pd1 114.2(5) . . ? C8 N2 Pd1 103.9(5) . . ? C11 N3 C26 122.6(6) . . ? C11 N3 Pd1 113.4(5) . . ? C26 N3 Pd1 122.3(5) . . ? N1 Pd1 N2 87.0(2) . . ? N1 Pd1 O4 92.8(2) . . ? N2 Pd1 O4 172.3(2) . . ? N1 Pd1 N3 169.7(2) . . ? N2 Pd1 N3 83.1(2) . . ? O4 Pd1 N3 96.7(2) . . ? 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 C6 C1 C2 C3 0.1(17) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 C6 -1.3(19) . . . . ? C4 C5 C6 C1 2.8(15) . . . . ? C4 C5 C6 C7 178.8(9) . . . . ? C2 C1 C6 C5 -2.2(14) . . . . ? C2 C1 C6 C7 -178.3(9) . . . . ? C5 C6 C7 N2 96.5(9) . . . . ? C1 C6 C7 N2 -87.5(9) . . . . ? N2 C8 C9 O1 -161.5(7) . . . . ? N2 C8 C9 N1 22.0(9) . . . . ? N2 C10 C11 O2 159.9(7) . . . . ? N2 C10 C11 N3 -21.5(9) . . . . ? N1 C12 C13 C14 177.9(7) . . . . ? C17 C12 C13 C14 -0.9(12) . . . . ? C12 C13 C14 C15 -1.2(13) . . . . ? C13 C14 C15 C16 1.7(13) . . . . ? C14 C15 C16 C17 -0.1(13) . . . . ? N1 C12 C17 C16 -176.4(7) . . . . ? C13 C12 C17 C16 2.4(10) . . . . ? N1 C12 C17 C18 1.5(11) . . . . ? C13 C12 C17 C18 -179.6(7) . . . . ? C15 C16 C17 C12 -1.9(11) . . . . ? C15 C16 C17 C18 180.0(7) . . . . ? C12 C17 C18 O4 -30.6(11) . . . . ? C16 C17 C18 O4 147.3(7) . . . . ? C12 C17 C18 C19 152.4(7) . . . . ? C16 C17 C18 C19 -29.7(10) . . . . ? O4 C18 C19 C20 150.3(7) . . . . ? C17 C18 C19 C20 -32.4(10) . . . . ? O4 C18 C19 C24 -26.7(10) . . . . ? C17 C18 C19 C24 150.5(7) . . . . ? C24 C19 C20 C21 -2.5(11) . . . . ? C18 C19 C20 C21 -179.6(7) . . . . ? C19 C20 C21 C22 -0.5(12) . . . . ? C20 C21 C22 O5 -176.3(7) . . . . ? C20 C21 C22 C23 2.3(12) . . . . ? O5 C22 C23 C24 177.5(7) . . . . ? C21 C22 C23 C24 -0.9(12) . . . . ? C22 C23 C24 C19 -2.1(12) . . . . ? C20 C19 C24 C23 3.8(11) . . . . ? C18 C19 C24 C23 -179.0(7) . . . . ? N3 C26 C27 C28 -176.7(8) . . . . ? C31 C26 C27 C28 -1.4(12) . . . . ? C26 C27 C28 C29 -1.5(15) . . . . ? C27 C28 C29 C30 2.0(16) . . . . ? C28 C29 C30 C31 0.6(15) . . . . ? C29 C30 C31 C26 -3.5(13) . . . . ? C29 C30 C31 C32 169.6(8) . . . . ? C27 C26 C31 C30 3.9(11) . . . . ? N3 C26 C31 C30 179.0(7) . . . . ? C27 C26 C31 C32 -169.0(7) . . . . ? N3 C26 C31 C32 6.1(11) . . . . ? C30 C31 C32 O3 -147.0(9) . . . . ? C26 C31 C32 O3 25.8(13) . . . . ? C30 C31 C32 C33 32.0(11) . . . . ? C26 C31 C32 C33 -155.2(7) . . . . ? O3 C32 C33 C34 -115.4(10) . . . . ? C31 C32 C33 C34 65.6(11) . . . . ? O3 C32 C33 C38 59.7(12) . . . . ? C31 C32 C33 C38 -119.3(9) . . . . ? C38 C33 C34 C35 -0.5(14) . . . . ? C32 C33 C34 C35 174.7(9) . . . . ? C33 C34 C35 C36 0.7(17) . . . . ? C34 C35 C36 C37 0.0(19) . . . . ? C35 C36 C37 C38 -0.9(18) . . . . ? C36 C37 C38 C33 1.1(15) . . . . ? C36 C37 C38 C39 177.5(10) . . . . ? C34 C33 C38 C37 -0.4(13) . . . . ? C32 C33 C38 C37 -175.4(8) . . . . ? C34 C33 C38 C39 -176.7(8) . . . . ? C32 C33 C38 C39 8.2(12) . . . . ? C37 C38 C39 F3 -12.3(13) . . . . ? C33 C38 C39 F3 164.1(8) . . . . ? C37 C38 C39 F2 -131.9(9) . . . . ? C33 C38 C39 F2 44.5(12) . . . . ? C37 C38 C39 F1 107.7(10) . . . . ? C33 C38 C39 F1 -75.9(11) . . . . ? C17 C18 O4 Pd1 24.3(10) . . . . ? C19 C18 O4 Pd1 -158.6(5) . . . . ? C21 C22 O5 C25 -177.0(7) . . . . ? C23 C22 O5 C25 4.6(12) . . . . ? O1 C9 N1 C12 7.8(12) . . . . ? C8 C9 N1 C12 -176.0(7) . . . . ? O1 C9 N1 Pd1 -176.5(7) . . . . ? C8 C9 N1 Pd1 -0.3(8) . . . . ? C13 C12 N1 C9 24.3(11) . . . . ? C17 C12 N1 C9 -156.9(7) . . . . ? C13 C12 N1 Pd1 -151.1(6) . . . . ? C17 C12 N1 Pd1 27.8(9) . . . . ? C11 C10 N2 C7 -83.6(8) . . . . ? C11 C10 N2 C8 150.8(7) . . . . ? C11 C10 N2 Pd1 38.3(7) . . . . ? C6 C7 N2 C10 166.8(6) . . . . ? C6 C7 N2 C8 -66.1(9) . . . . ? C6 C7 N2 Pd1 51.5(7) . . . . ? C9 C8 N2 C10 -143.4(7) . . . . ? C9 C8 N2 C7 92.5(8) . . . . ? C9 C8 N2 Pd1 -31.1(7) . . . . ? O2 C11 N3 C26 5.9(12) . . . . ? C10 C11 N3 C26 -172.5(6) . . . . ? O2 C11 N3 Pd1 171.1(6) . . . . ? C10 C11 N3 Pd1 -7.4(8) . . . . ? C27 C26 N3 C11 -128.6(8) . . . . ? C31 C26 N3 C11 56.2(10) . . . . ? C27 C26 N3 Pd1 67.5(8) . . . . ? C31 C26 N3 Pd1 -107.6(7) . . . . ? C9 N1 Pd1 N2 -14.9(5) . . . . ? C12 N1 Pd1 N2 161.0(5) . . . . ? C9 N1 Pd1 O4 157.4(5) . . . . ? C12 N1 Pd1 O4 -26.7(5) . . . . ? C9 N1 Pd1 N3 0.7(16) . . . . ? C12 N1 Pd1 N3 176.5(11) . . . . ? C10 N2 Pd1 N1 144.4(5) . . . . ? C7 N2 Pd1 N1 -97.3(5) . . . . ? C8 N2 Pd1 N1 24.6(5) . . . . ? C10 N2 Pd1 O4 56.4(17) . . . . ? C7 N2 Pd1 O4 174.6(14) . . . . ? C8 N2 Pd1 O4 -63.5(17) . . . . ? C10 N2 Pd1 N3 -32.8(4) . . . . ? C7 N2 Pd1 N3 85.4(5) . . . . ? C8 N2 Pd1 N3 -152.7(5) . . . . ? C18 O4 Pd1 N1 1.3(6) . . . . ? C18 O4 Pd1 N2 88.9(16) . . . . ? C18 O4 Pd1 N3 177.2(6) . . . . ? C11 N3 Pd1 N1 8.7(16) . . . . ? C26 N3 Pd1 N1 173.9(11) . . . . ? C11 N3 Pd1 N2 24.3(5) . . . . ? C26 N3 Pd1 N2 -170.5(5) . . . . ? C11 N3 Pd1 O4 -147.9(5) . . . . ? C26 N3 Pd1 O4 17.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 68.17 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.308 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 951883'