# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers # 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_H6L _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common C102H108N6O12(Me2SO)11(H2O)3 _chemical_melting_point ? _chemical_formula_moiety C124H180N6O26S11 _chemical_formula_sum 'C124 H180 N6 O26 S11' _chemical_formula_weight 2523.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 24.1319(10) _cell_length_b 24.1319(10) _cell_length_c 43.5952(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21986.3(16) _cell_formula_units_Z 6 _cell_measurement_temperature 120 _cell_measurement_reflns_used 39568 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8100 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9143 _exptl_absorpt_correction_T_max 0.9865 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39568 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8570 _reflns_number_gt 6674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2009)' _computing_data_reduction 'APEX2 (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ORTEP-3 _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^)+(0.0534P)^2^+145.2930P] 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 8570 _refine_ls_number_parameters 999 _refine_ls_number_restraints 1210 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.2262 _refine_ls_wR_factor_gt 0.2112 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.099 _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 0.39963(19) 0.69206(19) 0.36891(9) 0.0550(10) Uani 1 1 d . . . C2 C 0.35827(19) 0.62600(19) 0.36902(9) 0.0548(10) Uani 1 1 d . . . H1 H 0.3755 0.5982 0.3692 0.066 Uiso 1 1 calc R . . C3 C 0.35317(16) 0.62093(16) 0.21145(7) 0.0396(8) Uani 1 1 d . . . C4 C 0.39802(16) 0.68608(16) 0.21149(7) 0.0407(8) Uani 1 1 d . . . H2 H 0.4423 0.6994 0.2115 0.049 Uiso 1 1 calc R . . C5 C 0.47070(19) 0.71956(19) 0.36950(9) 0.0556(10) Uani 1 1 d . . . C6 C 0.50150(19) 0.69332(19) 0.35245(9) 0.0538(9) Uani 1 1 d . . . C7 C 0.56769(19) 0.7199(2) 0.35462(9) 0.0560(10) Uani 1 1 d . . . C8 C 0.6040(2) 0.7750(2) 0.37269(9) 0.0591(10) Uani 1 1 d . . . H3 H 0.6491 0.7931 0.3737 0.071 Uiso 1 1 calc R . . C9 C 0.5755(2) 0.8034(2) 0.38890(10) 0.0590(10) Uani 1 1 d . . . C10 C 0.5084(2) 0.7738(2) 0.38720(9) 0.0579(10) Uani 1 1 d . . . H4 H 0.4877 0.7917 0.3987 0.069 Uiso 1 1 calc R . . O1 O 0.46626(13) 0.64262(14) 0.33402(7) 0.0602(7) Uani 1 1 d . . . H5 H 0.4906 0.6332 0.3244 0.090 Uiso 1 1 calc R . . C11 C 0.6126(2) 0.8636(2) 0.40849(11) 0.0705(13) Uani 1 1 d . . . C12 C 0.5980(3) 0.9152(2) 0.39687(15) 0.0912(17) Uani 1 1 d . . . H6 H 0.6213 0.9540 0.4094 0.137 Uiso 1 1 calc R . . H7 H 0.5519 0.8993 0.3985 0.137 Uiso 1 1 calc R . . H8 H 0.6114 0.9253 0.3754 0.137 Uiso 1 1 calc R . . C13 C 0.5917(2) 0.8475(3) 0.44199(11) 0.0904(18) Uani 1 1 d . . . H9 H 0.6150 0.8860 0.4546 0.136 Uiso 1 1 calc R . . H10 H 0.6011 0.8146 0.4492 0.136 Uiso 1 1 calc R . . H11 H 0.5457 0.8315 0.4436 0.136 Uiso 1 1 calc R . . C14 C 0.6847(2) 0.8899(2) 0.40645(12) 0.0775(14) Uani 1 1 d . . . H12 H 0.7071 0.9284 0.4191 0.116 Uiso 1 1 calc R . . H13 H 0.6986 0.9005 0.3851 0.116 Uiso 1 1 calc R . . H14 H 0.6947 0.8575 0.4138 0.116 Uiso 1 1 calc R . . C15 C 0.60065(19) 0.6921(2) 0.33859(9) 0.0558(10) Uani 1 1 d . A . H15 H 0.6456 0.7109 0.3409 0.067 Uiso 1 1 calc R . . N1 N 0.57042(15) 0.64232(16) 0.32118(7) 0.0528(8) Uani 1 1 d . . . C16 C 0.60292(17) 0.61390(17) 0.30724(9) 0.0498(6) Uani 0.50 1 d PDU A 1 C17 C 0.6582(4) 0.6181(5) 0.3202(3) 0.0626(15) Uani 0.50 1 d PDU A 1 H16 H 0.6736 0.6388 0.3394 0.075 Uiso 0.50 1 calc PR A 1 C18 C 0.6898(4) 0.5924(5) 0.3052(2) 0.0629(15) Uani 0.50 1 d PDU A 1 C19 C 0.6678(5) 0.5618(6) 0.2772(2) 0.0695(15) Uani 0.50 1 d PDU A 1 C20 C 0.6134(5) 0.5571(7) 0.2642(3) 0.0663(18) Uani 0.50 1 d PDU A 1 H17 H 0.5991 0.5376 0.2447 0.080 Uiso 0.50 1 calc PR A 1 C21 C 0.57940(17) 0.58107(17) 0.27987(9) 0.0471(6) Uani 0.50 1 d PDU A 1 O2 O 0.7429(4) 0.5916(6) 0.3165(2) 0.083(2) Uani 0.50 1 d PDU A 1 C22 C 0.7740(6) 0.6333(7) 0.3419(3) 0.099(4) Uani 0.50 1 d PDU A 1 H18 H 0.8104 0.6290 0.3484 0.149 Uiso 0.50 1 calc PR A 1 H19 H 0.7436 0.6219 0.3589 0.149 Uiso 0.50 1 calc PR A 1 H20 H 0.7891 0.6777 0.3357 0.149 Uiso 0.50 1 calc PR A 1 O3 O 0.7049(4) 0.5397(5) 0.2642(2) 0.106(2) Uani 0.50 1 d PDU A 1 C23 C 0.6835(8) 0.5084(9) 0.2349(3) 0.144(5) Uani 0.50 1 d PDU A 1 H21 H 0.7103 0.4904 0.2288 0.215 Uiso 0.50 1 calc PR A 1 H22 H 0.6869 0.5396 0.2195 0.215 Uiso 0.50 1 calc PR A 1 H23 H 0.6389 0.4740 0.2366 0.215 Uiso 0.50 1 calc PR A 1 C24 C 0.60292(17) 0.61390(17) 0.30724(9) 0.0498(6) Uani 0.50 1 d PDU A 2 C25 C 0.6543(4) 0.6126(5) 0.3219(3) 0.0556(14) Uani 0.50 1 d PDU A 2 H24 H 0.6695 0.6341 0.3409 0.067 Uiso 0.50 1 calc PR A 2 C26 C 0.6829(4) 0.5811(5) 0.3094(2) 0.0572(12) Uani 0.50 1 d PDU A 2 C27 C 0.6601(4) 0.5487(5) 0.2818(2) 0.0613(13) Uani 0.50 1 d PDU A 2 C28 C 0.6095(5) 0.5494(5) 0.2672(3) 0.0539(14) Uani 0.50 1 d PDU A 2 H25 H 0.5948 0.5279 0.2481 0.065 Uiso 0.50 1 calc PR A 2 C29 C 0.57940(17) 0.58107(17) 0.27987(9) 0.0471(6) Uani 0.50 1 d PDU A 2 O4 O 0.7340(4) 0.5780(5) 0.3216(3) 0.0777(18) Uani 0.50 1 d PDU A 2 C30 C 0.7575(7) 0.6062(7) 0.3510(3) 0.098(4) Uani 0.50 1 d PDU A 2 H26 H 0.7924 0.5990 0.3572 0.148 Uiso 0.50 1 calc PR A 2 H27 H 0.7228 0.5866 0.3661 0.148 Uiso 0.50 1 calc PR A 2 H28 H 0.7733 0.6523 0.3499 0.148 Uiso 0.50 1 calc PR A 2 O5 O 0.6907(4) 0.5179(4) 0.2706(2) 0.091(2) Uani 0.50 1 d PDU A 2 C31 C 0.6569(7) 0.4710(7) 0.2464(4) 0.123(4) Uani 0.50 1 d PDU A 2 H29 H 0.6826 0.4521 0.2399 0.184 Uiso 0.50 1 calc PR A 2 H30 H 0.6499 0.4923 0.2289 0.184 Uiso 0.50 1 calc PR A 2 H31 H 0.6156 0.4374 0.2542 0.184 Uiso 0.50 1 calc PR A 2 N2 N 0.52525(13) 0.57884(14) 0.26578(7) 0.0443(7) Uani 1 1 d . . . C32 C 0.48760(17) 0.52948(17) 0.24954(8) 0.0457(8) Uani 1 1 d . A . H32 H 0.4945 0.4940 0.2493 0.055 Uiso 1 1 calc R . . C33 C 0.43536(16) 0.52574(16) 0.23173(8) 0.0426(8) Uani 1 1 d . . . C34 C 0.42225(16) 0.57621(16) 0.23072(7) 0.0404(8) Uani 1 1 d . A . C35 C 0.37232(16) 0.57108(16) 0.21214(7) 0.0403(8) Uani 1 1 d . . . C36 C 0.33721(16) 0.51525(16) 0.19501(8) 0.0424(8) Uani 1 1 d . A . H33 H 0.3043 0.5123 0.1820 0.051 Uiso 1 1 calc R . . C37 C 0.34799(18) 0.46339(17) 0.19606(8) 0.0476(9) Uani 1 1 d . . . C38 C 0.39741(17) 0.46984(17) 0.21464(8) 0.0479(9) Uani 1 1 d . A . H34 H 0.4060 0.4355 0.2159 0.057 Uiso 1 1 calc R . . O6 O 0.45622(12) 0.62910(11) 0.24820(5) 0.0466(6) Uani 1 1 d . . . H35 H 0.4820 0.6243 0.2592 0.070 Uiso 1 1 calc R A . C39 C 0.3065(2) 0.40334(18) 0.17681(9) 0.0580(10) Uani 1 1 d . A . C40 C 0.3152(4) 0.3477(2) 0.18726(17) 0.162(4) Uani 1 1 d . . . H36 H 0.2884 0.3099 0.1747 0.243 Uiso 1 1 calc R A . H37 H 0.3027 0.3380 0.2088 0.243 Uiso 1 1 calc R . . H38 H 0.3602 0.3595 0.1850 0.243 Uiso 1 1 calc R . . C41 C 0.3274(2) 0.4178(2) 0.14391(10) 0.0699(12) Uani 1 1 d . . . H39 H 0.3014 0.3799 0.1313 0.105 Uiso 1 1 calc R A . H40 H 0.3725 0.4299 0.1422 0.105 Uiso 1 1 calc R . . H41 H 0.3219 0.4533 0.1367 0.105 Uiso 1 1 calc R . . C42 C 0.2361(2) 0.3854(3) 0.17836(14) 0.099(2) Uani 1 1 d . . . H42 H 0.2104 0.3470 0.1660 0.148 Uiso 1 1 calc R A . H43 H 0.2315 0.4208 0.1704 0.148 Uiso 1 1 calc R . . H44 H 0.2215 0.3770 0.1997 0.148 Uiso 1 1 calc R . . S1 S 0.28629(7) 0.45845(7) 0.30268(4) 0.0675(4) Uani 0.75 1 d PDU B 1 O7 O 0.2940(3) 0.4106(3) 0.28168(17) 0.126(2) Uani 0.75 1 d PDU B 1 C43 C 0.3654(3) 0.5052(4) 0.3160(2) 0.106(3) Uani 0.75 1 d PDU B 1 H45 H 0.3773 0.4782 0.3278 0.158 Uiso 0.75 1 calc PR B 1 H46 H 0.3685 0.5396 0.3291 0.158 Uiso 0.75 1 calc PR B 1 H47 H 0.3944 0.5237 0.2985 0.158 Uiso 0.75 1 calc PR B 1 C44 C 0.2783(4) 0.5119(4) 0.2810(2) 0.126(3) Uani 0.75 1 d PDU B 1 H48 H 0.2350 0.4916 0.2724 0.189 Uiso 0.75 1 calc PR B 1 H49 H 0.3097 0.5267 0.2643 0.189 Uiso 0.75 1 calc PR B 1 H50 H 0.2856 0.5485 0.2937 0.189 Uiso 0.75 1 calc PR B 1 S2 S 0.3457(3) 0.4849(3) 0.29129(15) 0.0533(14) Uani 0.15 1 d PDU C 2 O8 O 0.2918(8) 0.4388(8) 0.2701(4) 0.055(3) Uani 0.15 1 d PDU C 2 C45 C 0.3135(10) 0.5413(8) 0.2904(5) 0.047(3) Uani 0.15 1 d PDU C 2 H51 H 0.3051 0.5480 0.2691 0.071 Uiso 0.15 1 calc PR C 2 H52 H 0.3449 0.5824 0.2994 0.071 Uiso 0.15 1 calc PR C 2 H53 H 0.2736 0.5231 0.3022 0.071 Uiso 0.15 1 calc PR C 2 C46 C 0.3335(12) 0.4689(11) 0.3291(3) 0.050(4) Uani 0.15 1 d PDU C 2 H54 H 0.3667 0.4610 0.3373 0.075 Uiso 0.15 1 calc PR C 2 H55 H 0.2913 0.4309 0.3323 0.075 Uiso 0.15 1 calc PR C 2 H56 H 0.3352 0.5055 0.3398 0.075 Uiso 0.15 1 calc PR C 2 S3 S 0.3172(7) 0.4715(7) 0.2811(4) 0.086(2) Uani 0.10 1 d PDU D 3 O9 O 0.2899(16) 0.4075(10) 0.2968(7) 0.076(3) Uani 0.10 1 d PDU D 3 C47 C 0.358(2) 0.5242(17) 0.3124(9) 0.076(4) Uani 0.10 1 d PDU D 3 H57 H 0.3923 0.5176 0.3195 0.114 Uiso 0.10 1 calc PR D 3 H58 H 0.3272 0.5152 0.3292 0.114 Uiso 0.10 1 calc PR D 3 H59 H 0.3752 0.5686 0.3057 0.114 Uiso 0.10 1 calc PR D 3 C48 C 0.2572(15) 0.4874(18) 0.2752(13) 0.080(5) Uani 0.10 1 d PDU D 3 H60 H 0.2317 0.4631 0.2574 0.119 Uiso 0.10 1 calc PR D 3 H61 H 0.2753 0.5333 0.2713 0.119 Uiso 0.10 1 calc PR D 3 H62 H 0.2297 0.4752 0.2934 0.119 Uiso 0.10 1 calc PR D 3 S4 S 0.4769(2) 0.5624(2) 0.42894(9) 0.1013(9) Uani 0.45 1 d PDU E 1 O10 O 0.4116(4) 0.5537(6) 0.4288(3) 0.120(3) Uani 0.45 1 d PDU E 1 C49 C 0.5270(8) 0.6477(6) 0.4327(4) 0.099(4) Uani 0.45 1 d PDU E 1 H63 H 0.5210 0.6610 0.4531 0.148 Uiso 0.45 1 calc PR E 1 H64 H 0.5154 0.6691 0.4169 0.148 Uiso 0.45 1 calc PR E 1 H65 H 0.5719 0.6594 0.4301 0.148 Uiso 0.45 1 calc PR E 1 C50 C 0.4979(8) 0.5546(8) 0.3918(3) 0.109(4) Uani 0.45 1 d PDU E 1 H66 H 0.4739 0.5096 0.3856 0.164 Uiso 0.45 1 calc PR E 1 H67 H 0.5438 0.5698 0.3909 0.164 Uiso 0.45 1 calc PR E 1 H68 H 0.4877 0.5802 0.3778 0.164 Uiso 0.45 1 calc PR E 1 S5 S 0.4746(3) 0.5919(4) 0.41128(18) 0.148(2) Uani 0.30 1 d PDU F 2 O11 O 0.4342(8) 0.5602(9) 0.4398(4) 0.135(4) Uani 0.30 1 d PDU F 2 C51 C 0.5083(15) 0.5431(14) 0.4011(8) 0.206(9) Uani 0.30 1 d PDU F 2 H69 H 0.4756 0.5040 0.3911 0.309 Uiso 0.30 1 calc PR F 2 H70 H 0.5234 0.5318 0.4196 0.309 Uiso 0.30 1 calc PR F 2 H71 H 0.5442 0.5667 0.3870 0.309 Uiso 0.30 1 calc PR F 2 C52 C 0.5393(11) 0.6549(11) 0.4285(7) 0.117(7) Uani 0.30 1 d PDU F 2 H72 H 0.5275 0.6862 0.4355 0.176 Uiso 0.30 1 calc PR F 2 H73 H 0.5745 0.6753 0.4137 0.176 Uiso 0.30 1 calc PR F 2 H74 H 0.5530 0.6394 0.4461 0.176 Uiso 0.30 1 calc PR F 2 S6 S 0.5183(8) 0.5571(11) 0.4253(5) 0.135(3) Uani 0.10 1 d PDU G 3 O12 O 0.5847(11) 0.571(2) 0.4340(9) 0.127(8) Uani 0.10 1 d PDU G 3 C53 C 0.471(2) 0.482(2) 0.4439(13) 0.158(11) Uani 0.10 1 d PDU G 3 H75 H 0.4692 0.4887 0.4659 0.236 Uiso 0.10 1 calc PR G 3 H76 H 0.4895 0.4546 0.4404 0.236 Uiso 0.10 1 calc PR G 3 H77 H 0.4272 0.4610 0.4355 0.236 Uiso 0.10 1 calc PR G 3 C54 C 0.512(3) 0.535(3) 0.3875(6) 0.125(13) Uani 0.10 1 d PDU G 3 H78 H 0.5387 0.5728 0.3749 0.188 Uiso 0.10 1 calc PR G 3 H79 H 0.4671 0.5162 0.3809 0.188 Uiso 0.10 1 calc PR G 3 H80 H 0.5258 0.5036 0.3850 0.188 Uiso 0.10 1 calc PR G 3 S7 S 0.6047(3) 0.3688(3) 0.30475(17) 0.1356(17) Uani 0.33 1 d PDU H -2 O13 O 0.6538(8) 0.3560(8) 0.2904(4) 0.169(4) Uani 0.33 1 d PDU H -2 C55 C 0.5556(12) 0.2978(8) 0.3256(6) 0.144(7) Uani 0.33 1 d PDU H -2 H81 H 0.5302 0.2629 0.3112 0.216 Uiso 0.33 1 calc PR H -2 H82 H 0.5270 0.3045 0.3390 0.216 Uiso 0.33 1 calc PR H -2 H83 H 0.5825 0.2868 0.3380 0.216 Uiso 0.33 1 calc PR H -2 C56 C 0.6446(10) 0.4210(10) 0.3341(5) 0.134(5) Uani 0.33 1 d PDU H -2 H84 H 0.6748 0.4631 0.3256 0.201 Uiso 0.33 1 calc PR H -2 H85 H 0.6681 0.4050 0.3461 0.201 Uiso 0.33 1 calc PR H -2 H86 H 0.6138 0.4246 0.3474 0.201 Uiso 0.33 1 calc PR H -2 S8 S 0.5526(13) 0.3294(13) 0.2799(7) 0.213(5) Uani 0.10 1 d PDU I -3 O14 O 0.5579(19) 0.341(3) 0.2456(7) 0.198(7) Uani 0.10 1 d PDU I -3 C57 C 0.590(3) 0.4106(19) 0.2931(15) 0.189(10) Uani 0.10 1 d PDU I -3 H87 H 0.6360 0.4313 0.2900 0.283 Uiso 0.10 1 calc PR I -3 H88 H 0.5805 0.4111 0.3149 0.283 Uiso 0.10 1 calc PR I -3 H89 H 0.5727 0.4336 0.2815 0.283 Uiso 0.10 1 calc PR I -3 C58 C 0.4750(17) 0.301(4) 0.2896(15) 0.189(9) Uani 0.10 1 d PDU I -3 H90 H 0.4630 0.3333 0.2851 0.284 Uiso 0.10 1 calc PR I -3 H91 H 0.4693 0.2906 0.3115 0.284 Uiso 0.10 1 calc PR I -3 H92 H 0.4477 0.2621 0.2777 0.284 Uiso 0.10 1 calc PR I -3 S9 S 0.4720(3) 0.4340(3) 0.49447(13) 0.0993(14) Uani 0.30 1 d PDU J -1 O15 O 0.5028(7) 0.3942(6) 0.4942(3) 0.116(3) Uani 0.30 1 d PDU J -1 C59 C 0.5375(9) 0.5151(7) 0.4930(5) 0.119(5) Uani 0.30 1 d PDU J -1 H93 H 0.5609 0.5259 0.5125 0.179 Uiso 0.30 1 calc PR J -1 H94 H 0.5209 0.5442 0.4894 0.179 Uiso 0.30 1 calc PR J -1 H95 H 0.5665 0.5193 0.4762 0.179 Uiso 0.30 1 calc PR J -1 C60 C 0.4392(10) 0.4267(10) 0.4589(4) 0.121(6) Uani 0.30 1 d PDU J -1 H96 H 0.4024 0.3836 0.4565 0.182 Uiso 0.30 1 calc PR J -1 H97 H 0.4712 0.4341 0.4432 0.182 Uiso 0.30 1 calc PR J -1 H98 H 0.4253 0.4583 0.4566 0.182 Uiso 0.30 1 calc PR J -1 S10 S 0.6018(13) 0.4178(14) 0.5080(6) 0.216(3) Uani 0.10 1 d PDU K 5 O16 O 0.5432(18) 0.422(2) 0.5016(10) 0.158(4) Uani 0.10 1 d PDU K 5 C61 C 0.580(3) 0.343(2) 0.4896(12) 0.150(8) Uani 0.10 1 d PDU K 5 H99 H 0.5733 0.3459 0.4677 0.224 Uiso 0.10 1 calc PR K 5 H100 H 0.5408 0.3087 0.4989 0.224 Uiso 0.10 1 calc PR K 5 H101 H 0.6148 0.3332 0.4924 0.224 Uiso 0.10 1 calc PR K 5 C62 C 0.601(4) 0.399(4) 0.5458(7) 0.215(14) Uani 0.10 1 d PDU K 5 H102 H 0.6167 0.4384 0.5582 0.322 Uiso 0.10 1 calc PR K 5 H103 H 0.6288 0.3811 0.5490 0.322 Uiso 0.10 1 calc PR K 5 H104 H 0.5572 0.3683 0.5520 0.322 Uiso 0.10 1 calc PR K 5 S11 S 0.6980(8) 0.4029(7) 0.5424(4) 0.193(3) Uani 0.18 1 d PDU L -1 O17 O 0.6970(11) 0.3428(11) 0.5521(5) 0.157(4) Uani 0.18 1 d PDU L -1 C63 C 0.7343(19) 0.420(2) 0.5053(7) 0.172(9) Uani 0.18 1 d PDU L -1 H105 H 0.7801 0.4353 0.5074 0.258 Uiso 0.18 1 calc PR L -1 H106 H 0.7284 0.4534 0.4955 0.258 Uiso 0.18 1 calc PR L -1 H107 H 0.7143 0.3813 0.4927 0.258 Uiso 0.18 1 calc PR L -1 C64 C 0.6205(12) 0.378(2) 0.5340(11) 0.202(11) Uani 0.18 1 d PDU L -1 H108 H 0.5952 0.3653 0.5529 0.303 Uiso 0.18 1 calc PR L -1 H109 H 0.6040 0.3414 0.5199 0.303 Uiso 0.18 1 calc PR L -1 H110 H 0.6175 0.4130 0.5242 0.303 Uiso 0.18 1 calc PR L -1 S12 S 0.6777(2) 0.5240(3) 0.44369(14) 0.1452(15) Uani 0.45 1 d PDU M 1 O18 O 0.7163(4) 0.5809(3) 0.4248(2) 0.0925(19) Uani 0.45 1 d PDU M 1 C65 C 0.7105(9) 0.5413(11) 0.4796(3) 0.157(5) Uani 0.45 1 d PDU M 1 H111 H 0.7539 0.5478 0.4787 0.235 Uiso 0.45 1 calc PR M 1 H112 H 0.6843 0.5056 0.4934 0.235 Uiso 0.45 1 calc PR M 1 H113 H 0.7120 0.5802 0.4871 0.235 Uiso 0.45 1 calc PR M 1 C66 C 0.6013(6) 0.5094(10) 0.4436(5) 0.180(7) Uani 0.45 1 d PDU M 1 H114 H 0.5846 0.5004 0.4226 0.270 Uiso 0.45 1 calc PR M 1 H115 H 0.6003 0.5470 0.4514 0.270 Uiso 0.45 1 calc PR M 1 H116 H 0.5748 0.4724 0.4566 0.270 Uiso 0.45 1 calc PR M 1 S13 S 0.6740(7) 0.5131(6) 0.4141(3) 0.125(3) Uani 0.15 1 d PDU N 2 O19 O 0.6907(14) 0.5818(7) 0.4202(6) 0.111(7) Uani 0.15 1 d PDU N 2 C67 C 0.6304(13) 0.4889(14) 0.3806(4) 0.093(8) Uani 0.15 1 d PDU N 2 H117 H 0.6571 0.5147 0.3635 0.140 Uiso 0.15 1 calc PR N 2 H118 H 0.5930 0.4945 0.3824 0.140 Uiso 0.15 1 calc PR N 2 H119 H 0.6161 0.4437 0.3769 0.140 Uiso 0.15 1 calc PR N 2 C68 C 0.6351(17) 0.4597(9) 0.4412(4) 0.097(8) Uani 0.15 1 d PDU N 2 H120 H 0.6581 0.4749 0.4606 0.145 Uiso 0.15 1 calc PR N 2 H121 H 0.6320 0.4189 0.4356 0.145 Uiso 0.15 1 calc PR N 2 H122 H 0.5919 0.4537 0.4433 0.145 Uiso 0.15 1 calc PR N 2 S14 S 0.7343(8) 0.5524(9) 0.4794(4) 0.109(3) Uani 0.10 1 d PDU O 3 O20 O 0.7442(19) 0.5628(18) 0.4455(5) 0.121(6) Uani 0.10 1 d PDU O 3 C69 C 0.741(2) 0.4827(19) 0.4862(14) 0.152(8) Uani 0.10 1 d PDU O 3 H123 H 0.7356 0.4729 0.5082 0.228 Uiso 0.10 1 calc PR O 3 H124 H 0.7827 0.4906 0.4794 0.228 Uiso 0.10 1 calc PR O 3 H125 H 0.7070 0.4465 0.4748 0.228 Uiso 0.10 1 calc PR O 3 C70 C 0.6532(11) 0.520(2) 0.4853(9) 0.089(9) Uani 0.10 1 d PDU O 3 H126 H 0.6420 0.5540 0.4826 0.134 Uiso 0.10 1 calc PR O 3 H127 H 0.6423 0.5034 0.5062 0.134 Uiso 0.10 1 calc PR O 3 H128 H 0.6294 0.4860 0.4706 0.134 Uiso 0.10 1 calc PR O 3 S15 S 0.6381(8) 0.5197(8) 0.4138(4) 0.107(2) Uani 0.10 1 d PDU P 4 O21 O 0.6678(14) 0.5660(15) 0.4405(7) 0.097(4) Uani 0.10 1 d PDU P 4 C71 C 0.5613(13) 0.515(2) 0.4118(13) 0.108(3) Uani 0.10 1 d PDU P 4 H129 H 0.5660 0.5532 0.4016 0.163 Uiso 0.10 1 calc PR P 4 H130 H 0.5445 0.5120 0.4325 0.163 Uiso 0.10 1 calc PR P 4 H131 H 0.5316 0.4768 0.4000 0.163 Uiso 0.10 1 calc PR P 4 C72 C 0.620(2) 0.4465(13) 0.4272(13) 0.112(6) Uani 0.10 1 d PDU P 4 H132 H 0.5956 0.4142 0.4115 0.168 Uiso 0.10 1 calc PR P 4 H133 H 0.5934 0.4370 0.4458 0.168 Uiso 0.10 1 calc PR P 4 H134 H 0.6591 0.4462 0.4321 0.168 Uiso 0.10 1 calc PR P 4 O22 O 0.6700(2) 0.6580(3) 0.39639(12) 0.0861(15) Uani 0.67 1 d PD . . H135 H 0.686(2) 0.637(2) 0.4037(19) 0.129 Uiso 0.67 1 d PD . . H136 H 0.699(2) 0.6896(11) 0.3900(15) 0.129 Uiso 0.67 1 d PD . . O23 O 0.6667 0.3333 0.2252(4) 0.291(9) Uani 1 3 d SD . . H137 H 0.662(6) 0.339(6) 0.2446(10) 0.436 Uiso 0.33 1 d PD . . H138 H 0.666(5) 0.298(3) 0.227(3) 0.436 Uiso 0.33 1 d PD . . 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 0.057(2) 0.060(2) 0.047(2) -0.0039(17) 0.0008(17) 0.0286(19) C2 0.057(2) 0.058(2) 0.052(2) -0.0045(18) -0.0030(18) 0.0308(19) C3 0.0485(18) 0.0449(18) 0.0261(16) 0.0006(13) 0.0012(13) 0.0239(15) C4 0.0443(18) 0.0483(19) 0.0285(16) 0.0004(13) -0.0007(13) 0.0225(15) C5 0.058(2) 0.057(2) 0.052(2) -0.0004(18) -0.0009(18) 0.0288(19) C6 0.059(2) 0.059(2) 0.046(2) -0.0045(17) -0.0057(17) 0.0315(19) C7 0.059(2) 0.064(2) 0.048(2) -0.0040(18) -0.0043(18) 0.033(2) C8 0.056(2) 0.067(3) 0.051(2) -0.0048(19) -0.0046(18) 0.029(2) C9 0.057(2) 0.060(2) 0.055(2) -0.0036(19) 0.0017(19) 0.026(2) C10 0.059(2) 0.059(2) 0.055(2) -0.0032(18) 0.0046(19) 0.028(2) O1 0.0573(15) 0.0693(17) 0.0578(17) -0.0138(13) -0.0067(13) 0.0344(14) C11 0.061(3) 0.067(3) 0.069(3) -0.014(2) 0.008(2) 0.021(2) C12 0.072(3) 0.061(3) 0.130(5) -0.015(3) 0.016(3) 0.025(3) C13 0.064(3) 0.097(4) 0.070(3) -0.032(3) 0.004(2) 0.011(3) C14 0.064(3) 0.074(3) 0.076(3) -0.019(2) 0.005(2) 0.021(2) C15 0.054(2) 0.063(2) 0.051(2) -0.0015(18) -0.0060(18) 0.0302(19) N1 0.0544(18) 0.0587(19) 0.0483(18) -0.0013(15) -0.0051(14) 0.0304(15) C16 0.0437(11) 0.0479(17) 0.0547(15) 0.0024(12) 0.0000(12) 0.0207(11) C17 0.0523(17) 0.071(4) 0.065(3) -0.006(3) -0.010(2) 0.032(2) C18 0.0373(17) 0.071(4) 0.076(2) 0.000(3) -0.003(2) 0.024(2) C19 0.0575(16) 0.092(4) 0.071(3) -0.005(3) 0.000(2) 0.047(2) C20 0.0541(18) 0.085(5) 0.066(4) -0.015(3) -0.005(2) 0.039(2) C21 0.0409(12) 0.0427(17) 0.0540(15) 0.0047(12) 0.0010(11) 0.0182(12) O2 0.049(2) 0.099(6) 0.105(4) -0.008(4) -0.015(3) 0.040(3) C22 0.068(6) 0.128(10) 0.099(7) -0.011(5) -0.030(4) 0.047(6) O3 0.086(3) 0.157(6) 0.111(4) -0.032(4) -0.008(4) 0.087(3) C23 0.136(10) 0.216(11) 0.126(7) -0.067(7) -0.010(6) 0.123(9) C24 0.0437(11) 0.0479(17) 0.0547(15) 0.0024(12) 0.0000(12) 0.0207(11) C25 0.0476(19) 0.048(3) 0.068(3) -0.005(3) -0.010(2) 0.0217(19) C26 0.0509(19) 0.039(3) 0.080(2) 0.001(2) -0.010(2) 0.0220(18) C27 0.0522(19) 0.050(3) 0.085(3) -0.009(3) -0.007(2) 0.0288(18) C28 0.051(2) 0.042(4) 0.068(3) -0.002(3) -0.003(2) 0.023(2) C29 0.0409(12) 0.0427(17) 0.0540(15) 0.0047(12) 0.0010(11) 0.0182(12) O4 0.056(3) 0.071(5) 0.112(3) -0.018(4) -0.024(3) 0.036(3) C30 0.091(7) 0.102(9) 0.124(6) -0.033(6) -0.052(5) 0.064(6) O5 0.074(3) 0.086(4) 0.132(5) -0.037(4) -0.021(3) 0.056(3) C31 0.119(9) 0.126(7) 0.165(10) -0.077(6) -0.046(7) 0.093(6) N2 0.0427(15) 0.0444(16) 0.0424(16) 0.0050(13) 0.0007(13) 0.0192(13) C32 0.0490(19) 0.0431(19) 0.046(2) 0.0078(15) 0.0045(16) 0.0238(16) C33 0.0448(18) 0.0405(18) 0.0394(18) 0.0087(14) 0.0039(15) 0.0190(15) C34 0.0411(17) 0.0430(18) 0.0332(17) 0.0041(14) 0.0042(14) 0.0180(15) C35 0.0432(18) 0.0444(18) 0.0314(16) 0.0046(13) 0.0052(14) 0.0205(15) C36 0.0436(18) 0.0444(18) 0.0348(17) 0.0042(14) 0.0015(14) 0.0186(15) C37 0.053(2) 0.0417(19) 0.0403(19) 0.0072(15) 0.0020(16) 0.0179(16) C38 0.055(2) 0.0374(18) 0.048(2) 0.0074(15) 0.0003(16) 0.0199(16) O6 0.0513(14) 0.0480(13) 0.0424(13) -0.0053(11) -0.0077(11) 0.0263(11) C39 0.068(2) 0.045(2) 0.056(2) -0.0034(17) -0.0166(19) 0.0244(19) C40 0.264(8) 0.042(3) 0.164(6) -0.035(3) -0.148(6) 0.065(4) C41 0.068(3) 0.082(3) 0.062(3) -0.026(2) -0.016(2) 0.039(2) C42 0.064(3) 0.081(4) 0.098(4) -0.028(3) 0.010(3) -0.004(3) S1 0.0567(8) 0.0595(8) 0.0659(9) -0.0005(6) 0.0101(7) 0.0139(7) O7 0.088(3) 0.080(3) 0.176(5) -0.062(3) 0.005(3) 0.016(2) C43 0.073(2) 0.124(6) 0.092(5) -0.042(4) -0.016(3) 0.028(3) C44 0.113(5) 0.172(5) 0.127(7) 0.072(4) 0.054(4) 0.097(4) S2 0.041(2) 0.049(3) 0.046(2) 0.002(2) 0.007(2) 0.004(2) O8 0.053(5) 0.052(3) 0.043(3) -0.006(4) 0.003(4) 0.012(4) C45 0.041(5) 0.047(4) 0.029(6) -0.004(4) -0.003(5) 0.003(4) C46 0.049(7) 0.049(6) 0.043(2) -0.004(4) 0.003(4) 0.018(5) S3 0.075(3) 0.075(3) 0.090(5) 0.002(3) 0.020(6) 0.025(3) O9 0.075(5) 0.079(3) 0.072(7) -0.002(4) 0.004(6) 0.039(4) C47 0.078(4) 0.071(5) 0.081(6) 0.010(5) 0.008(5) 0.039(4) C48 0.093(6) 0.063(8) 0.071(9) 0.003(6) -0.002(5) 0.030(5) S4 0.1055(18) 0.1107(19) 0.092(2) 0.0074(19) -0.001(2) 0.0573(17) O10 0.081(2) 0.100(6) 0.150(7) 0.019(6) 0.005(5) 0.025(3) C49 0.076(5) 0.116(2) 0.077(7) 0.022(5) -0.009(7) 0.028(4) C50 0.121(9) 0.117(8) 0.074(4) 0.028(5) -0.001(5) 0.049(8) S5 0.100(3) 0.145(4) 0.143(4) 0.066(3) -0.049(2) 0.020(3) O11 0.099(4) 0.126(9) 0.191(8) 0.044(5) 0.015(7) 0.065(5) C51 0.182(14) 0.208(4) 0.151(18) -0.040(11) 0.048(13) 0.040(7) C52 0.097(10) 0.152(9) 0.081(14) 0.030(8) -0.021(7) 0.045(6) S6 0.083(3) 0.192(5) 0.126(4) 0.026(7) 0.012(8) 0.065(7) O12 0.111(4) 0.146(17) 0.146(7) -0.017(16) -0.035(8) 0.080(8) C53 0.144(13) 0.168(13) 0.146(6) 0.014(12) 0.007(19) 0.067(11) C54 0.11(2) 0.12(2) 0.137(5) 0.008(8) -0.031(10) 0.059(16) S7 0.116(3) 0.128(3) 0.178(5) 0.027(3) 0.000(3) 0.072(2) O13 0.157(5) 0.165(6) 0.221(9) 0.043(6) 0.031(7) 0.108(5) C55 0.149(12) 0.103(5) 0.176(15) 0.004(6) 0.004(9) 0.060(8) C56 0.100(12) 0.105(8) 0.203(12) 0.031(7) -0.018(8) 0.055(7) S8 0.207(3) 0.209(4) 0.215(3) -0.024(10) 0.011(12) 0.099(11) O14 0.181(7) 0.201(9) 0.222(4) -0.003(8) 0.003(8) 0.103(14) C57 0.186(9) 0.185(10) 0.207(18) 0.014(14) 0.01(2) 0.102(10) C58 0.199(7) 0.184(12) 0.189(13) 0.004(11) -0.007(9) 0.098(7) S9 0.091(2) 0.096(3) 0.095(3) 0.016(3) -0.007(3) 0.0346(18) O15 0.138(4) 0.109(3) 0.104(8) 0.005(7) -0.006(7) 0.063(3) C59 0.122(8) 0.092(2) 0.110(12) 0.002(9) -0.017(9) 0.028(3) C60 0.123(12) 0.116(13) 0.102(7) -0.003(9) -0.028(8) 0.043(9) S10 0.236(3) 0.224(4) 0.190(4) 0.018(7) 0.045(13) 0.117(7) O16 0.168(4) 0.145(6) 0.101(9) -0.016(11) 0.033(13) 0.033(7) C61 0.14(2) 0.178(10) 0.120(7) 0.048(10) -0.031(18) 0.073(12) C62 0.22(2) 0.23(2) 0.182(5) -0.019(9) -0.010(16) 0.098(17) S11 0.209(3) 0.152(3) 0.195(4) -0.049(7) 0.001(7) 0.072(6) O17 0.188(3) 0.198(6) 0.075(7) -0.036(9) -0.046(10) 0.089(8) C63 0.191(4) 0.143(19) 0.201(10) 0.021(12) 0.005(10) 0.097(13) C64 0.227(5) 0.19(2) 0.25(2) -0.033(16) 0.029(9) 0.148(13) S12 0.104(2) 0.133(3) 0.181(3) 0.042(3) 0.003(3) 0.046(2) O18 0.057(3) 0.057(3) 0.155(4) -0.017(3) -0.030(4) 0.022(3) C65 0.172(4) 0.154(14) 0.142(5) 0.007(6) 0.033(6) 0.080(10) C66 0.106(3) 0.181(15) 0.233(14) 0.047(13) 0.059(5) 0.056(6) S13 0.170(8) 0.138(3) 0.098(4) 0.016(4) -0.006(5) 0.100(5) O19 0.093(17) 0.087(3) 0.089(8) 0.007(5) -0.007(13) -0.003(7) C67 0.050(12) 0.071(12) 0.114(5) -0.003(7) 0.024(7) -0.003(11) C68 0.110(18) 0.044(5) 0.093(7) -0.054(6) -0.006(10) 0.007(10) S14 0.110(3) 0.076(3) 0.098(3) -0.018(7) 0.029(7) 0.015(5) O20 0.136(6) 0.103(5) 0.099(4) -0.014(8) 0.034(8) 0.041(11) C69 0.159(3) 0.153(10) 0.16(2) 0.008(14) 0.016(19) 0.089(8) C70 0.104(5) 0.087(19) 0.052(16) -0.007(16) -0.004(10) 0.028(10) S15 0.100(2) 0.107(3) 0.101(5) -0.003(4) 0.017(7) 0.043(4) O21 0.091(4) 0.111(3) 0.112(9) -0.016(6) 0.017(5) 0.066(6) C71 0.110(3) 0.106(4) 0.106(5) -0.001(3) 0.001(3) 0.052(3) C72 0.114(10) 0.108(4) 0.119(13) -0.015(6) 0.001(10) 0.059(7) O22 0.091(3) 0.109(4) 0.061(3) -0.027(3) -0.034(3) 0.052(3) O23 0.239(10) 0.239(10) 0.39(3) 0.000 0.000 0.119(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. ; 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 C2 1.387(5) 2_665 ? C1 C2 1.395(5) . ? C1 C5 1.498(6) . ? C2 C1 1.387(6) 3_565 ? C2 H1 0.9500 . ? C3 C4 1.393(5) . ? C3 C4 1.400(5) 3_565 ? C3 C35 1.489(5) . ? C4 C3 1.400(5) 2_665 ? C4 H2 0.9500 . ? C5 C10 1.395(6) . ? C5 C6 1.406(6) . ? C6 O1 1.351(5) . ? C6 C7 1.395(6) . ? C7 C8 1.411(6) . ? C7 C15 1.451(6) . ? C8 C9 1.382(6) . ? C8 H3 0.9500 . ? C9 C10 1.408(6) . ? C9 C11 1.531(6) . ? C10 H4 0.9500 . ? O1 H5 0.8400 . ? C11 C14 1.527(6) . ? C11 C13 1.531(7) . ? C11 C12 1.540(8) . ? C12 H6 0.9800 . ? C12 H7 0.9800 . ? C12 H8 0.9800 . ? C13 H9 0.9800 . ? C13 H10 0.9800 . ? C13 H11 0.9800 . ? C14 H12 0.9800 . ? C14 H13 0.9800 . ? C14 H14 0.9800 . ? C15 N1 1.294(5) . ? C15 H15 0.9500 . ? N1 C16 1.411(5) . ? C16 C21 1.387(5) . ? C16 C17 1.404(10) . ? C17 C18 1.367(11) . ? C17 H16 0.9500 . ? C18 O2 1.381(10) . ? C18 C19 1.387(11) . ? C19 O3 1.371(11) . ? C19 C20 1.381(11) . ? C20 C21 1.395(11) . ? C20 H17 0.9500 . ? C21 N2 1.420(5) . ? O2 C22 1.431(12) . ? C22 H18 0.9800 . ? C22 H19 0.9800 . ? C22 H20 0.9800 . ? O3 C23 1.442(13) . ? C23 H21 0.9800 . ? C23 H22 0.9800 . ? C23 H23 0.9800 . ? C25 C26 1.367(11) . ? C25 H24 0.9500 . ? C26 O4 1.380(10) . ? C26 C27 1.389(11) . ? C27 O5 1.372(10) . ? C27 C28 1.387(11) . ? C28 H25 0.9500 . ? O4 C30 1.428(12) . ? C30 H26 0.9800 . ? C30 H27 0.9800 . ? C30 H28 0.9800 . ? O5 C31 1.461(12) . ? C31 H29 0.9800 . ? C31 H30 0.9800 . ? C31 H31 0.9800 . ? N2 C32 1.290(4) . ? C32 C33 1.444(5) . ? C32 H32 0.9500 . ? C33 C34 1.404(5) . ? C33 C38 1.406(5) . ? C34 O6 1.355(4) . ? C34 C35 1.405(5) . ? C35 C36 1.396(5) . ? C36 C37 1.401(5) . ? C36 H33 0.9500 . ? C37 C38 1.384(5) . ? C37 C39 1.535(5) . ? C38 H34 0.9500 . ? O6 H35 0.8400 . ? C39 C41 1.503(6) . ? C39 C40 1.529(7) . ? C39 C42 1.530(7) . ? C40 H36 0.9800 . ? C40 H37 0.9800 . ? C40 H38 0.9800 . ? C41 H39 0.9800 . ? C41 H40 0.9800 . ? C41 H41 0.9800 . ? C42 H42 0.9800 . ? C42 H43 0.9800 . ? C42 H44 0.9800 . ? S1 O7 1.555(5) . ? S1 C44 1.687(7) . ? S1 C43 1.760(6) . ? C43 H45 0.9800 . ? C43 H46 0.9800 . ? C43 H47 0.9800 . ? C44 H48 0.9800 . ? C44 H49 0.9800 . ? C44 H50 0.9800 . ? S2 O8 1.529(13) . ? S2 C46 1.687(14) . ? S2 C45 1.876(15) . ? C45 H51 0.9800 . ? C45 H52 0.9800 . ? C45 H53 0.9800 . ? C46 H54 0.9800 . ? C46 H55 0.9800 . ? C46 H56 0.9800 . ? S3 O9 1.506(16) . ? S3 C48 1.695(17) . ? S3 C47 1.787(17) . ? C47 H57 0.9800 . ? C47 H58 0.9800 . ? C47 H59 0.9800 . ? C48 H60 0.9800 . ? C48 H61 0.9800 . ? C48 H62 0.9800 . ? S4 O10 1.481(10) . ? S4 C50 1.735(12) . ? S4 C49 1.799(12) . ? C49 H63 0.9800 . ? C49 H64 0.9800 . ? C49 H65 0.9800 . ? C50 H66 0.9800 . ? C50 H67 0.9800 . ? C50 H68 0.9800 . ? S5 O11 1.530(13) . ? S5 C52 1.715(15) . ? S5 C51 1.788(17) . ? C51 H69 0.9800 . ? C51 H70 0.9800 . ? C51 H71 0.9800 . ? C52 H72 0.9800 . ? C52 H73 0.9800 . ? C52 H74 0.9800 . ? S6 O12 1.509(16) . ? S6 C54 1.716(17) . ? S6 C53 1.783(18) . ? C53 H75 0.9800 . ? C53 H76 0.9800 . ? C53 H77 0.9800 . ? C54 H78 0.9800 . ? C54 H79 0.9800 . ? C54 H80 0.9800 . ? S7 O13 1.503(11) . ? S7 C56 1.714(15) . ? S7 C55 1.769(15) . ? C55 H81 0.9800 . ? C55 H82 0.9800 . ? C55 H83 0.9800 . ? C56 H84 0.9800 . ? C56 H85 0.9800 . ? C56 H86 0.9800 . ? S8 O14 1.514(17) . ? S8 C58 1.694(18) . ? S8 C57 1.793(18) . ? C57 H87 0.9800 . ? C57 H88 0.9800 . ? C57 H89 0.9800 . ? C58 H90 0.9800 . ? C58 H91 0.9800 . ? C58 H92 0.9800 . ? S9 O15 1.481(12) . ? S9 C60 1.710(13) . ? S9 C59 1.800(13) . ? C59 H93 0.9800 . ? C59 H94 0.9800 . ? C59 H95 0.9800 . ? C60 H96 0.9800 . ? C60 H97 0.9800 . ? C60 H98 0.9800 . ? S10 O16 1.490(17) . ? S10 C62 1.707(18) . ? S10 C61 1.801(18) . ? C61 H99 0.9800 . ? C61 H100 0.9800 . ? C61 H101 0.9800 . ? C62 H102 0.9800 . ? C62 H103 0.9800 . ? C62 H104 0.9800 . ? S11 O17 1.501(16) . ? S11 C64 1.694(17) . ? S11 C63 1.784(17) . ? C63 H105 0.9800 . ? C63 H106 0.9800 . ? C63 H107 0.9800 . ? C64 H108 0.9800 . ? C64 H109 0.9800 . ? C64 H110 0.9800 . ? S12 O18 1.467(9) . ? S12 C66 1.695(13) . ? S12 C65 1.707(14) . ? C65 H111 0.9800 . ? C65 H112 0.9800 . ? C65 H113 0.9800 . ? C66 H114 0.9800 . ? C66 H115 0.9800 . ? C66 H116 0.9800 . ? S13 O19 1.522(12) . ? S13 C68 1.651(12) . ? S13 C67 1.722(12) . ? C67 H117 0.9800 . ? C67 H118 0.9800 . ? C67 H119 0.9800 . ? C68 H120 0.9800 . ? C68 H121 0.9800 . ? C68 H122 0.9800 . ? S14 O20 1.495(16) . ? S14 C70 1.727(17) . ? S14 C69 1.787(17) . ? C69 H123 0.9800 . ? C69 H124 0.9800 . ? C69 H125 0.9800 . ? C70 H126 0.9800 . ? C70 H127 0.9800 . ? C70 H128 0.9800 . ? S15 O21 1.520(16) . ? S15 C72 1.692(17) . ? S15 C71 1.800(17) . ? C71 H129 0.9800 . ? C71 H130 0.9800 . ? C71 H131 0.9800 . ? C72 H132 0.9800 . ? C72 H133 0.9800 . ? C72 H134 0.9800 . ? O22 H135 0.843(17) . ? O22 H136 0.79(2) . ? O23 H137 0.871(19) . ? O23 H138 0.85(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C2 119.0(4) 2_665 . ? C2 C1 C5 120.1(4) 2_665 . ? C2 C1 C5 120.8(4) . . ? C1 C2 C1 121.0(4) 3_565 . ? C1 C2 H1 119.5 3_565 . ? C1 C2 H1 119.5 . . ? C4 C3 C4 118.7(4) . 3_565 ? C4 C3 C35 122.1(3) . . ? C4 C3 C35 119.2(3) 3_565 . ? C3 C4 C3 121.3(4) . 2_665 ? C3 C4 H2 119.4 . . ? C3 C4 H2 119.4 2_665 . ? C10 C5 C6 118.1(4) . . ? C10 C5 C1 119.4(4) . . ? C6 C5 C1 122.5(4) . . ? O1 C6 C7 120.9(4) . . ? O1 C6 C5 119.2(4) . . ? C7 C6 C5 119.9(4) . . ? C6 C7 C8 119.9(4) . . ? C6 C7 C15 121.4(4) . . ? C8 C7 C15 118.7(4) . . ? C9 C8 C7 121.7(4) . . ? C9 C8 H3 119.2 . . ? C7 C8 H3 119.2 . . ? C8 C9 C10 116.9(4) . . ? C8 C9 C11 123.8(4) . . ? C10 C9 C11 119.3(4) . . ? C5 C10 C9 123.4(4) . . ? C5 C10 H4 118.3 . . ? C9 C10 H4 118.3 . . ? C6 O1 H5 109.5 . . ? C14 C11 C9 111.4(4) . . ? C14 C11 C13 108.8(4) . . ? C9 C11 C13 109.2(4) . . ? C14 C11 C12 108.7(4) . . ? C9 C11 C12 108.8(4) . . ? C13 C11 C12 109.9(4) . . ? C11 C12 H6 109.5 . . ? C11 C12 H7 109.5 . . ? H6 C12 H7 109.5 . . ? C11 C12 H8 109.5 . . ? H6 C12 H8 109.5 . . ? H7 C12 H8 109.5 . . ? C11 C13 H9 109.5 . . ? C11 C13 H10 109.5 . . ? H9 C13 H10 109.5 . . ? C11 C13 H11 109.5 . . ? H9 C13 H11 109.5 . . ? H10 C13 H11 109.5 . . ? C11 C14 H12 109.5 . . ? C11 C14 H13 109.5 . . ? H12 C14 H13 109.5 . . ? C11 C14 H14 109.5 . . ? H12 C14 H14 109.5 . . ? H13 C14 H14 109.5 . . ? N1 C15 C7 121.8(4) . . ? N1 C15 H15 119.1 . . ? C7 C15 H15 119.1 . . ? C15 N1 C16 120.7(3) . . ? C21 C16 C17 119.3(6) . . ? C21 C16 N1 118.7(3) . . ? C17 C16 N1 122.0(6) . . ? C18 C17 C16 120.1(10) . . ? C18 C17 H16 120.0 . . ? C16 C17 H16 120.0 . . ? C17 C18 O2 124.7(9) . . ? C17 C18 C19 120.7(9) . . ? O2 C18 C19 114.6(9) . . ? O3 C19 C20 125.3(9) . . ? O3 C19 C18 114.8(9) . . ? C20 C19 C18 119.9(9) . . ? C19 C20 C21 119.9(9) . . ? C19 C20 H17 120.1 . . ? C21 C20 H17 120.1 . . ? C16 C21 C20 120.0(6) . . ? C16 C21 N2 120.0(3) . . ? C20 C21 N2 119.6(6) . . ? C18 O2 C22 115.3(11) . . ? O2 C22 H18 109.5 . . ? O2 C22 H19 109.5 . . ? H18 C22 H19 109.5 . . ? O2 C22 H20 109.5 . . ? H18 C22 H20 109.5 . . ? H19 C22 H20 109.5 . . ? C19 O3 C23 115.9(10) . . ? O3 C23 H21 109.5 . . ? O3 C23 H22 109.5 . . ? H21 C23 H22 109.5 . . ? O3 C23 H23 109.5 . . ? H21 C23 H23 109.5 . . ? H22 C23 H23 109.5 . . ? C26 C25 H24 119.2 . . ? C25 C26 O4 126.1(9) . . ? C25 C26 C27 119.4(9) . . ? O4 C26 C27 114.5(9) . . ? O5 C27 C28 124.0(9) . . ? O5 C27 C26 116.5(8) . . ? C28 C27 C26 119.5(9) . . ? C27 C28 H25 119.2 . . ? C26 O4 C30 118.2(10) . . ? O4 C30 H26 109.5 . . ? O4 C30 H27 109.5 . . ? H26 C30 H27 109.5 . . ? O4 C30 H28 109.5 . . ? H26 C30 H28 109.5 . . ? H27 C30 H28 109.5 . . ? C27 O5 C31 115.7(9) . . ? O5 C31 H29 109.5 . . ? O5 C31 H30 109.5 . . ? H29 C31 H30 109.5 . . ? O5 C31 H31 109.5 . . ? H29 C31 H31 109.5 . . ? H30 C31 H31 109.5 . . ? C32 N2 C21 118.8(3) . . ? N2 C32 C33 122.8(3) . . ? N2 C32 H32 118.6 . . ? C33 C32 H32 118.6 . . ? C34 C33 C38 119.6(3) . . ? C34 C33 C32 122.1(3) . . ? C38 C33 C32 118.3(3) . . ? O6 C34 C33 120.4(3) . . ? O6 C34 C35 119.7(3) . . ? C33 C34 C35 119.8(3) . . ? C36 C35 C34 118.2(3) . . ? C36 C35 C3 119.0(3) . . ? C34 C35 C3 122.6(3) . . ? C35 C36 C37 123.4(3) . . ? C35 C36 H33 118.3 . . ? C37 C36 H33 118.3 . . ? C38 C37 C36 116.9(3) . . ? C38 C37 C39 123.0(3) . . ? C36 C37 C39 120.1(3) . . ? C37 C38 C33 121.9(3) . . ? C37 C38 H34 119.0 . . ? C33 C38 H34 119.0 . . ? C34 O6 H35 109.5 . . ? C41 C39 C40 108.2(5) . . ? C41 C39 C42 107.6(4) . . ? C40 C39 C42 111.0(5) . . ? C41 C39 C37 108.5(3) . . ? C40 C39 C37 110.8(3) . . ? C42 C39 C37 110.5(4) . . ? C39 C40 H36 109.5 . . ? C39 C40 H37 109.5 . . ? H36 C40 H37 109.5 . . ? C39 C40 H38 109.5 . . ? H36 C40 H38 109.5 . . ? H37 C40 H38 109.5 . . ? C39 C41 H39 109.5 . . ? C39 C41 H40 109.5 . . ? H39 C41 H40 109.5 . . ? C39 C41 H41 109.5 . . ? H39 C41 H41 109.5 . . ? H40 C41 H41 109.5 . . ? C39 C42 H42 109.5 . . ? C39 C42 H43 109.5 . . ? H42 C42 H43 109.5 . . ? C39 C42 H44 109.5 . . ? H42 C42 H44 109.5 . . ? H43 C42 H44 109.5 . . ? O7 S1 C44 109.8(5) . . ? O7 S1 C43 100.2(4) . . ? C44 S1 C43 101.4(4) . . ? S1 C43 H45 109.5 . . ? S1 C43 H46 109.5 . . ? H45 C43 H46 109.5 . . ? S1 C43 H47 109.5 . . ? H45 C43 H47 109.5 . . ? H46 C43 H47 109.5 . . ? S1 C44 H48 109.5 . . ? S1 C44 H49 109.5 . . ? H48 C44 H49 109.5 . . ? S1 C44 H50 109.5 . . ? H48 C44 H50 109.5 . . ? H49 C44 H50 109.5 . . ? O8 S2 C46 116.0(11) . . ? O8 S2 C45 90.3(10) . . ? C46 S2 C45 95.6(10) . . ? S2 C45 H51 109.5 . . ? S2 C45 H52 109.5 . . ? H51 C45 H52 109.5 . . ? S2 C45 H53 109.5 . . ? H51 C45 H53 109.5 . . ? H52 C45 H53 109.5 . . ? S2 C46 H54 109.5 . . ? S2 C46 H55 109.5 . . ? H54 C46 H55 109.5 . . ? S2 C46 H56 109.5 . . ? H54 C46 H56 109.5 . . ? H55 C46 H56 109.5 . . ? O9 S3 C48 108.5(17) . . ? O9 S3 C47 100.7(16) . . ? C48 S3 C47 100.2(16) . . ? S3 C47 H57 109.5 . . ? S3 C47 H58 109.5 . . ? H57 C47 H58 109.5 . . ? S3 C47 H59 109.5 . . ? H57 C47 H59 109.5 . . ? H58 C47 H59 109.5 . . ? S3 C48 H60 109.5 . . ? S3 C48 H61 109.5 . . ? H60 C48 H61 109.5 . . ? S3 C48 H62 109.5 . . ? H60 C48 H62 109.5 . . ? H61 C48 H62 109.5 . . ? O10 S4 C50 109.1(8) . . ? O10 S4 C49 102.8(8) . . ? C50 S4 C49 98.2(8) . . ? S4 C49 H63 109.5 . . ? S4 C49 H64 109.5 . . ? H63 C49 H64 109.5 . . ? S4 C49 H65 109.5 . . ? H63 C49 H65 109.5 . . ? H64 C49 H65 109.5 . . ? S4 C50 H66 109.5 . . ? S4 C50 H67 109.5 . . ? H66 C50 H67 109.5 . . ? S4 C50 H68 109.5 . . ? H66 C50 H68 109.5 . . ? H67 C50 H68 109.5 . . ? O11 S5 C52 99.0(12) . . ? O11 S5 C51 105.0(13) . . ? C52 S5 C51 100.4(14) . . ? S5 C51 H69 109.5 . . ? S5 C51 H70 109.5 . . ? H69 C51 H70 109.5 . . ? S5 C51 H71 109.5 . . ? H69 C51 H71 109.5 . . ? H70 C51 H71 109.5 . . ? S5 C52 H72 109.5 . . ? S5 C52 H73 109.5 . . ? H72 C52 H73 109.5 . . ? S5 C52 H74 109.5 . . ? H72 C52 H74 109.5 . . ? H73 C52 H74 109.5 . . ? O12 S6 C54 103.6(19) . . ? O12 S6 C53 100.9(18) . . ? C54 S6 C53 102.0(18) . . ? S6 C53 H75 109.5 . . ? S6 C53 H76 109.5 . . ? H75 C53 H76 109.5 . . ? S6 C53 H77 109.5 . . ? H75 C53 H77 109.5 . . ? H76 C53 H77 109.5 . . ? S6 C54 H78 109.5 . . ? S6 C54 H79 109.5 . . ? H78 C54 H79 109.5 . . ? S6 C54 H80 109.5 . . ? H78 C54 H80 109.5 . . ? H79 C54 H80 109.5 . . ? O13 S7 C56 104.4(10) . . ? O13 S7 C55 103.2(11) . . ? C56 S7 C55 100.7(13) . . ? S7 C55 H81 109.5 . . ? S7 C55 H82 109.5 . . ? H81 C55 H82 109.5 . . ? S7 C55 H83 109.5 . . ? H81 C55 H83 109.5 . . ? H82 C55 H83 109.5 . . ? S7 C56 H84 109.5 . . ? S7 C56 H85 109.5 . . ? H84 C56 H85 109.5 . . ? S7 C56 H86 109.5 . . ? H84 C56 H86 109.5 . . ? H85 C56 H86 109.5 . . ? O14 S8 C58 107(2) . . ? O14 S8 C57 99.5(19) . . ? C58 S8 C57 102.2(19) . . ? S8 C57 H87 109.5 . . ? S8 C57 H88 109.5 . . ? H87 C57 H88 109.5 . . ? S8 C57 H89 109.5 . . ? H87 C57 H89 109.5 . . ? H88 C57 H89 109.5 . . ? S8 C58 H90 109.5 . . ? S8 C58 H91 109.5 . . ? H90 C58 H91 109.5 . . ? S8 C58 H92 109.5 . . ? H90 C58 H92 109.5 . . ? H91 C58 H92 109.5 . . ? O15 S9 C60 106.4(10) . . ? O15 S9 C59 104.6(10) . . ? C60 S9 C59 100.9(10) . . ? S9 C59 H93 109.5 . . ? S9 C59 H94 109.5 . . ? H93 C59 H94 109.5 . . ? S9 C59 H95 109.5 . . ? H93 C59 H95 109.5 . . ? H94 C59 H95 109.5 . . ? S9 C60 H96 109.5 . . ? S9 C60 H97 109.5 . . ? H96 C60 H97 109.5 . . ? S9 C60 H98 109.5 . . ? H96 C60 H98 109.5 . . ? H97 C60 H98 109.5 . . ? O16 S10 C62 108(2) . . ? O16 S10 C61 100.1(18) . . ? C62 S10 C61 102.0(19) . . ? S10 C61 H99 109.5 . . ? S10 C61 H100 109.5 . . ? H99 C61 H100 109.5 . . ? S10 C61 H101 109.5 . . ? H99 C61 H101 109.5 . . ? H100 C61 H101 109.5 . . ? S10 C62 H102 109.5 . . ? S10 C62 H103 109.5 . . ? H102 C62 H103 109.5 . . ? S10 C62 H104 109.5 . . ? H102 C62 H104 109.5 . . ? H103 C62 H104 109.5 . . ? O17 S11 C64 103.7(16) . . ? O17 S11 C63 104.6(15) . . ? C64 S11 C63 102.3(17) . . ? S11 C63 H105 109.5 . . ? S11 C63 H106 109.5 . . ? H105 C63 H106 109.5 . . ? S11 C63 H107 109.5 . . ? H105 C63 H107 109.5 . . ? H106 C63 H107 109.5 . . ? S11 C64 H108 109.5 . . ? S11 C64 H109 109.5 . . ? H108 C64 H109 109.5 . . ? S11 C64 H110 109.5 . . ? H108 C64 H110 109.5 . . ? H109 C64 H110 109.5 . . ? O18 S12 C66 108.0(8) . . ? O18 S12 C65 106.7(9) . . ? C66 S12 C65 112.2(11) . . ? S12 C65 H111 109.5 . . ? S12 C65 H112 109.5 . . ? H111 C65 H112 109.5 . . ? S12 C65 H113 109.5 . . ? H111 C65 H113 109.5 . . ? H112 C65 H113 109.5 . . ? S12 C66 H114 109.5 . . ? S12 C66 H115 109.5 . . ? H114 C66 H115 109.5 . . ? S12 C66 H116 109.5 . . ? H114 C66 H116 109.5 . . ? H115 C66 H116 109.5 . . ? O19 S13 C68 117.5(13) . . ? O19 S13 C67 107.6(12) . . ? C68 S13 C67 109.2(12) . . ? S13 C67 H117 109.5 . . ? S13 C67 H118 109.5 . . ? H117 C67 H118 109.5 . . ? S13 C67 H119 109.5 . . ? H117 C67 H119 109.5 . . ? H118 C67 H119 109.5 . . ? S13 C68 H120 109.5 . . ? S13 C68 H121 109.5 . . ? H120 C68 H121 109.5 . . ? S13 C68 H122 109.5 . . ? H120 C68 H122 109.5 . . ? H121 C68 H122 109.5 . . ? O20 S14 C70 105.9(18) . . ? O20 S14 C69 103.9(19) . . ? C70 S14 C69 99.6(16) . . ? S14 C69 H123 109.5 . . ? S14 C69 H124 109.5 . . ? H123 C69 H124 109.5 . . ? S14 C69 H125 109.5 . . ? H123 C69 H125 109.5 . . ? H124 C69 H125 109.5 . . ? S14 C70 H126 109.5 . . ? S14 C70 H127 109.5 . . ? H126 C70 H127 109.5 . . ? S14 C70 H128 109.5 . . ? H126 C70 H128 109.5 . . ? H127 C70 H128 109.5 . . ? O21 S15 C72 106.6(19) . . ? O21 S15 C71 100.3(17) . . ? C72 S15 C71 102.9(17) . . ? S15 C71 H129 109.5 . . ? S15 C71 H130 109.5 . . ? H129 C71 H130 109.5 . . ? S15 C71 H131 109.5 . . ? H129 C71 H131 109.5 . . ? H130 C71 H131 109.5 . . ? S15 C72 H132 109.5 . . ? S15 C72 H133 109.5 . . ? H132 C72 H133 109.5 . . ? S15 C72 H134 109.5 . . ? H132 C72 H134 109.5 . . ? H133 C72 H134 109.5 . . ? H135 O22 H136 105(3) . . ? H137 O23 H138 98(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 C2 C1 C2 C1 0.6(8) 2_665 . . 3_565 ? C5 C1 C2 C1 179.1(3) . . . 3_565 ? C4 C3 C4 C3 -0.2(6) 3_565 . . 2_665 ? C35 C3 C4 C3 -178.7(2) . . . 2_665 ? C2 C1 C5 C10 37.9(6) 2_665 . . . ? C2 C1 C5 C10 -140.5(4) . . . . ? C2 C1 C5 C6 -141.1(4) 2_665 . . . ? C2 C1 C5 C6 40.4(6) . . . . ? C10 C5 C6 O1 -176.9(4) . . . . ? C1 C5 C6 O1 2.2(6) . . . . ? C10 C5 C6 C7 2.8(6) . . . . ? C1 C5 C6 C7 -178.1(4) . . . . ? O1 C6 C7 C8 176.5(4) . . . . ? C5 C6 C7 C8 -3.3(6) . . . . ? O1 C6 C7 C15 -3.5(6) . . . . ? C5 C6 C7 C15 176.8(4) . . . . ? C6 C7 C8 C9 1.0(6) . . . . ? C15 C7 C8 C9 -179.1(4) . . . . ? C7 C8 C9 C10 1.6(6) . . . . ? C7 C8 C9 C11 -179.2(4) . . . . ? C6 C5 C10 C9 -0.1(6) . . . . ? C1 C5 C10 C9 -179.2(4) . . . . ? C8 C9 C10 C5 -2.1(6) . . . . ? C11 C9 C10 C5 178.7(4) . . . . ? C8 C9 C11 C14 2.8(7) . . . . ? C10 C9 C11 C14 -177.9(4) . . . . ? C8 C9 C11 C13 -117.4(5) . . . . ? C10 C9 C11 C13 61.8(6) . . . . ? C8 C9 C11 C12 122.7(5) . . . . ? C10 C9 C11 C12 -58.1(5) . . . . ? C6 C7 C15 N1 1.3(6) . . . . ? C8 C7 C15 N1 -178.6(4) . . . . ? C7 C15 N1 C16 -176.3(4) . . . . ? C15 N1 C16 C21 -152.6(4) . . . . ? C15 N1 C16 C17 27.2(7) . . . . ? C21 C16 C17 C18 2.8(11) . . . . ? N1 C16 C17 C18 -177.0(7) . . . . ? C16 C17 C18 O2 -177.2(10) . . . . ? C16 C17 C18 C19 -0.2(13) . . . . ? C17 C18 C19 O3 178.3(10) . . . . ? O2 C18 C19 O3 -4.4(15) . . . . ? C17 C18 C19 C20 0.0(17) . . . . ? O2 C18 C19 C20 177.2(11) . . . . ? O3 C19 C20 C21 179.5(11) . . . . ? C18 C19 C20 C21 -2.3(19) . . . . ? C17 C16 C21 C20 -5.2(10) . . . . ? N1 C16 C21 C20 174.6(8) . . . . ? C17 C16 C21 N2 -177.2(6) . . . . ? N1 C16 C21 N2 2.6(5) . . . . ? C19 C20 C21 C16 5.0(16) . . . . ? C19 C20 C21 N2 177.0(9) . . . . ? C17 C18 O2 C22 -14.9(16) . . . . ? C19 C18 O2 C22 168.0(11) . . . . ? C20 C19 O3 C23 -1(2) . . . . ? C18 C19 O3 C23 -179.3(13) . . . . ? C25 C26 C27 O5 -179.7(9) . . . . ? O4 C26 C27 O5 0.4(14) . . . . ? C25 C26 C27 C28 0.9(15) . . . . ? O4 C26 C27 C28 -178.9(10) . . . . ? C25 C26 O4 C30 4.6(16) . . . . ? C27 C26 O4 C30 -175.6(11) . . . . ? C28 C27 O5 C31 -15.9(17) . . . . ? C26 C27 O5 C31 164.8(11) . . . . ? C16 C21 N2 C32 -150.0(3) . . . . ? C20 C21 N2 C32 38.0(8) . . . . ? C21 N2 C32 C33 -173.3(3) . . . . ? N2 C32 C33 C34 0.5(5) . . . . ? N2 C32 C33 C38 179.6(3) . . . . ? C38 C33 C34 O6 176.7(3) . . . . ? C32 C33 C34 O6 -4.2(5) . . . . ? C38 C33 C34 C35 -1.4(5) . . . . ? C32 C33 C34 C35 177.6(3) . . . . ? O6 C34 C35 C36 -178.4(3) . . . . ? C33 C34 C35 C36 -0.3(5) . . . . ? O6 C34 C35 C3 -2.0(5) . . . . ? C33 C34 C35 C3 176.1(3) . . . . ? C4 C3 C35 C36 -142.3(3) . . . . ? C4 C3 C35 C36 39.3(4) 3_565 . . . ? C4 C3 C35 C34 41.4(5) . . . . ? C4 C3 C35 C34 -137.1(3) 3_565 . . . ? C34 C35 C36 C37 1.9(5) . . . . ? C3 C35 C36 C37 -174.6(3) . . . . ? C35 C36 C37 C38 -1.7(5) . . . . ? C35 C36 C37 C39 179.1(3) . . . . ? C36 C37 C38 C33 -0.1(5) . . . . ? C39 C37 C38 C33 179.1(3) . . . . ? C34 C33 C38 C37 1.6(5) . . . . ? C32 C33 C38 C37 -177.5(3) . . . . ? C38 C37 C39 C41 -103.8(4) . . . . ? C36 C37 C39 C41 75.3(5) . . . . ? C38 C37 C39 C40 14.8(6) . . . . ? C36 C37 C39 C40 -166.1(5) . . . . ? C38 C37 C39 C42 138.4(4) . . . . ? C36 C37 C39 C42 -42.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.532 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.061 _database_code_depnum_ccdc_archive 'CCDC 963501' ####################################################################### # # 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_LNi3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[LNi3]_3DMSO_H2O_5DCM_4cyclohex' _chemical_melting_point ? _chemical_formula_moiety C137H180Cl10N6Ni3O16S3 _chemical_formula_sum 'C137 H180 Cl10 N6 Ni3 O16 S3' _chemical_formula_weight 2793.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.1680(6) _cell_length_b 19.0600(7) _cell_length_c 25.3558(9) _cell_angle_alpha 67.974(2) _cell_angle_beta 83.133(2) _cell_angle_gamma 82.959(2) _cell_volume 7608.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 52060 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2948 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8561 _exptl_absorpt_correction_T_max 0.9386 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 52060 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 26699 _reflns_number_gt 15452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2009)' _computing_data_reduction 'APEX2 (Bruker AXS, 2009)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ORTEP-3 _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^)+(0.0213P)^2^+37.6268P] 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 26699 _refine_ls_number_parameters 2492 _refine_ls_number_restraints 1156 _refine_ls_R_factor_all 0.1560 _refine_ls_R_factor_gt 0.0987 _refine_ls_wR_factor_ref 0.2444 _refine_ls_wR_factor_gt 0.2088 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.094 _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 0.33598(5) 0.48053(4) 0.08946(3) 0.0486(2) Uani 1 1 d . . . Ni2 Ni 0.14895(5) 0.07991(4) 0.30996(4) 0.0582(3) Uani 1 1 d . . . Ni3 Ni 0.14765(6) 0.43982(4) 0.41864(3) 0.0531(2) Uani 1 1 d . . . C1 C 0.0936(4) 0.3913(3) 0.1781(2) 0.0402(14) Uani 1 1 d . . . C2 C 0.0619(3) 0.3274(3) 0.2187(2) 0.0376(14) Uani 1 1 d . . . H1 H 0.0604 0.2839 0.2092 0.045 Uiso 1 1 calc R . . C3 C 0.0323(4) 0.3251(3) 0.2727(2) 0.0402(14) Uani 1 1 d . . . C4 C 0.0354(4) 0.3891(3) 0.2861(2) 0.0455(15) Uani 1 1 d . . . H2 H 0.0158 0.3882 0.3230 0.055 Uiso 1 1 calc R . . C5 C 0.0663(4) 0.4540(3) 0.2467(2) 0.0416(15) Uani 1 1 d . . . C6 C 0.0964(4) 0.4542(3) 0.1933(2) 0.0434(15) Uani 1 1 d . . . H3 H 0.1193 0.4980 0.1666 0.052 Uiso 1 1 calc R . . C7 C 0.3883(4) 0.3468(3) 0.2789(3) 0.0511(17) Uani 1 1 d . . . C8 C 0.3905(4) 0.2901(3) 0.2561(3) 0.0525(17) Uani 1 1 d . . . H4 H 0.4122 0.2988 0.2182 0.063 Uiso 1 1 calc R . . C9 C 0.3605(4) 0.2207(3) 0.2892(3) 0.0537(17) Uani 1 1 d . . . C10 C 0.3273(4) 0.2100(3) 0.3438(3) 0.0598(19) Uani 1 1 d . . . H5 H 0.3059 0.1631 0.3659 0.072 Uiso 1 1 calc R . . C11 C 0.3242(4) 0.2657(3) 0.3673(3) 0.0573(18) Uani 1 1 d . . . C12 C 0.3559(4) 0.3348(3) 0.3329(3) 0.0567(18) Uani 1 1 d . . . H6 H 0.3545 0.3739 0.3478 0.068 Uiso 1 1 calc R . . C13 C 0.1183(4) 0.3960(3) 0.1185(2) 0.0435(15) Uani 1 1 d . . . C14 C 0.1891(4) 0.4267(3) 0.0890(2) 0.0442(15) Uani 1 1 d . . . C15 C 0.2005(4) 0.4409(3) 0.0304(2) 0.0514(17) Uani 1 1 d . . . C16 C 0.1457(4) 0.4192(4) 0.0028(3) 0.0587(19) Uani 1 1 d . . . H7 H 0.1552 0.4289 -0.0369 0.070 Uiso 1 1 calc R . . C17 C 0.0791(4) 0.3846(3) 0.0318(2) 0.0543(18) Uani 1 1 d . . . C18 C 0.0662(4) 0.3754(3) 0.0898(2) 0.0495(16) Uani 1 1 d . . . H8 H 0.0195 0.3540 0.1104 0.059 Uiso 1 1 calc R . . O1 O 0.2409(3) 0.4383(2) 0.11773(16) 0.0491(11) Uani 1 1 d D . . C19 C 0.0192(5) 0.3588(4) 0.0034(3) 0.066(2) Uani 1 1 d . . . C20 C -0.0634(6) 0.3779(8) 0.0238(5) 0.163(5) Uani 1 1 d . . . H9 H -0.0724 0.4329 0.0143 0.245 Uiso 1 1 calc R . . H10 H -0.0711 0.3518 0.0652 0.245 Uiso 1 1 calc R . . H11 H -0.1006 0.3616 0.0051 0.245 Uiso 1 1 calc R . . C21 C 0.0338(7) 0.2767(5) 0.0170(5) 0.154(5) Uani 1 1 d . . . H12 H 0.0878 0.2650 0.0033 0.231 Uiso 1 1 calc R . . H13 H -0.0032 0.2602 -0.0017 0.231 Uiso 1 1 calc R . . H14 H 0.0265 0.2501 0.0584 0.231 Uiso 1 1 calc R . . C22 C 0.0231(7) 0.4018(6) -0.0602(3) 0.124(4) Uani 1 1 d . . . H15 H 0.0133 0.4563 -0.0680 0.187 Uiso 1 1 calc R . . H16 H -0.0170 0.3856 -0.0767 0.187 Uiso 1 1 calc R . . H17 H 0.0754 0.3913 -0.0773 0.187 Uiso 1 1 calc R . . C23 C 0.2628(4) 0.4839(3) -0.0050(2) 0.0519(17) Uani 1 1 d . . . H18 H 0.2646 0.4951 -0.0449 0.062 Uiso 1 1 calc R . . N1 N 0.3167(3) 0.5086(3) 0.0134(2) 0.0472(13) Uani 1 1 d . . . C24 C 0.3735(4) 0.5569(3) -0.0244(3) 0.0506(17) Uani 1 1 d . . . C25 C 0.3707(4) 0.5907(3) -0.0838(3) 0.0535(17) Uani 1 1 d . . . H19 H 0.3306 0.5806 -0.1021 0.064 Uiso 1 1 calc R . . C26 C 0.4276(4) 0.6390(3) -0.1153(3) 0.0556(18) Uani 1 1 d . . . C27 C 0.4866(4) 0.6524(3) -0.0877(3) 0.0556(18) Uani 1 1 d . . . C28 C 0.4898(4) 0.6187(3) -0.0298(3) 0.0530(17) Uani 1 1 d . . . H20 H 0.5312 0.6273 -0.0117 0.064 Uiso 1 1 calc R . . C29 C 0.4311(4) 0.5715(3) 0.0024(3) 0.0479(16) Uani 1 1 d . . . O2 O 0.4311(3) 0.6762(3) -0.17249(19) 0.0669(14) Uani 1 1 d . . . C30 C 0.3718(5) 0.6656(4) -0.2020(3) 0.078(2) Uani 1 1 d . . . H21 H 0.3808 0.6953 -0.2428 0.118 Uiso 1 1 calc R . . H22 H 0.3203 0.6823 -0.1875 0.118 Uiso 1 1 calc R . . H23 H 0.3732 0.6116 -0.1962 0.118 Uiso 1 1 calc R . . O3 O 0.5397(3) 0.7006(2) -0.1235(2) 0.0695(14) Uani 1 1 d . . . C31 C 0.6035(5) 0.7151(4) -0.0984(3) 0.078(2) Uani 1 1 d . . . H24 H 0.6370 0.7501 -0.1282 0.116 Uiso 1 1 calc R . . H25 H 0.6346 0.6672 -0.0796 0.116 Uiso 1 1 calc R . . H26 H 0.5825 0.7378 -0.0702 0.116 Uiso 1 1 calc R . . N2 N 0.4241(3) 0.5358(2) 0.0624(2) 0.0468(13) Uani 1 1 d . . . C32 C 0.4703(4) 0.5476(3) 0.0941(3) 0.0541(18) Uani 1 1 d . . . H27 H 0.5079 0.5835 0.0753 0.065 Uiso 1 1 calc R . . C33 C 0.4707(4) 0.5125(3) 0.1541(3) 0.0539(17) Uani 1 1 d . . . C34 C 0.4184(4) 0.4558(3) 0.1858(3) 0.0507(16) Uani 1 1 d . . . C35 C 0.4307(4) 0.4161(3) 0.2446(3) 0.0505(17) Uani 1 1 d . . . C36 C 0.4837(4) 0.4401(3) 0.2697(3) 0.0552(18) Uani 1 1 d . . . H28 H 0.4888 0.4144 0.3095 0.066 Uiso 1 1 calc R . . C37 C 0.5310(4) 0.5011(3) 0.2394(3) 0.0579(18) Uani 1 1 d . . . C38 C 0.5250(4) 0.5337(3) 0.1827(3) 0.0580(19) Uani 1 1 d . . . H29 H 0.5584 0.5725 0.1608 0.070 Uiso 1 1 calc R . . O4 O 0.3620(3) 0.4393(2) 0.16393(17) 0.0522(11) Uani 1 1 d . . . C39 C 0.5871(5) 0.5240(4) 0.2717(3) 0.067(2) Uani 1 1 d . . . C40 C 0.6366(5) 0.5879(4) 0.2311(4) 0.089(3) Uani 1 1 d . . . H30 H 0.6672 0.5709 0.2022 0.134 Uiso 1 1 calc R . . H31 H 0.6724 0.6005 0.2529 0.134 Uiso 1 1 calc R . . H32 H 0.6016 0.6329 0.2122 0.134 Uiso 1 1 calc R . . C41 C 0.5398(6) 0.5514(5) 0.3159(4) 0.095(3) Uani 1 1 d . . . H33 H 0.5034 0.5951 0.2968 0.142 Uiso 1 1 calc R . . H34 H 0.5756 0.5664 0.3364 0.142 Uiso 1 1 calc R . . H35 H 0.5098 0.5104 0.3430 0.142 Uiso 1 1 calc R . . C42 C 0.6430(5) 0.4568(4) 0.3009(4) 0.088(3) Uani 1 1 d . . . H36 H 0.6735 0.4392 0.2724 0.133 Uiso 1 1 calc R . . H37 H 0.6130 0.4158 0.3281 0.133 Uiso 1 1 calc R . . H38 H 0.6788 0.4718 0.3214 0.133 Uiso 1 1 calc R . . C43 C -0.0094(4) 0.2589(3) 0.3133(2) 0.0412(15) Uani 1 1 d . . . C44 C 0.0231(4) 0.1837(3) 0.3218(2) 0.0417(15) Uani 1 1 d . . . C45 C -0.0266(4) 0.1240(3) 0.3536(2) 0.0442(15) Uani 1 1 d . . . C46 C -0.0997(4) 0.1399(3) 0.3793(2) 0.0473(16) Uani 1 1 d . . . H39 H -0.1308 0.0989 0.4005 0.057 Uiso 1 1 calc R . . C47 C -0.1285(4) 0.2117(3) 0.3752(3) 0.0521(17) Uani 1 1 d . A . C48 C -0.0807(4) 0.2708(3) 0.3402(2) 0.0462(16) Uani 1 1 d . . . H40 H -0.0996 0.3217 0.3353 0.055 Uiso 1 1 calc R . . O5 O 0.0946(3) 0.1713(2) 0.30330(17) 0.0483(11) Uani 1 1 d D . . C49 C -0.2069(5) 0.2293(4) 0.4045(3) 0.0699(14) Uani 1 1 d U . . C50 C -0.247(2) 0.1607(16) 0.4465(13) 0.126(5) Uani 0.441(13) 1 d PU A 1 H41 H -0.2384 0.1192 0.4320 0.189 Uiso 0.441(13) 1 calc PR A 1 H42 H -0.3037 0.1746 0.4510 0.189 Uiso 0.441(13) 1 calc PR A 1 H43 H -0.2250 0.1444 0.4836 0.189 Uiso 0.441(13) 1 calc PR A 1 C51 C -0.2665(16) 0.2621(16) 0.3467(11) 0.122(5) Uani 0.441(13) 1 d PU A 1 H44 H -0.2682 0.2216 0.3320 0.183 Uiso 0.441(13) 1 calc PR A 1 H45 H -0.2445 0.3062 0.3164 0.183 Uiso 0.441(13) 1 calc PR A 1 H46 H -0.3199 0.2769 0.3595 0.183 Uiso 0.441(13) 1 calc PR A 1 C52 C -0.2127(14) 0.2988(12) 0.4200(11) 0.097(6) Uani 0.441(13) 1 d PU A 1 H47 H -0.2651 0.3052 0.4386 0.145 Uiso 0.441(13) 1 calc PR A 1 H48 H -0.2042 0.3437 0.3853 0.145 Uiso 0.441(13) 1 calc PR A 1 H49 H -0.1726 0.2929 0.4461 0.145 Uiso 0.441(13) 1 calc PR A 1 C53 C -0.2561(11) 0.1639(11) 0.4231(8) 0.082(4) Uani 0.559(13) 1 d PU A 2 H50 H -0.2269 0.1183 0.4478 0.124 Uiso 0.559(13) 1 calc PR A 2 H51 H -0.2693 0.1554 0.3896 0.124 Uiso 0.559(13) 1 calc PR A 2 H52 H -0.3047 0.1750 0.4442 0.124 Uiso 0.559(13) 1 calc PR A 2 C54 C -0.2501(11) 0.2944(10) 0.3699(10) 0.122(5) Uani 0.559(13) 1 d PU A 2 H53 H -0.2184 0.3380 0.3577 0.183 Uiso 0.559(13) 1 calc PR A 2 H54 H -0.2985 0.3045 0.3916 0.183 Uiso 0.559(13) 1 calc PR A 2 H55 H -0.2637 0.2862 0.3363 0.183 Uiso 0.559(13) 1 calc PR A 2 C55 C -0.1859(11) 0.2406(13) 0.4598(9) 0.114(5) Uani 0.559(13) 1 d PU A 2 H56 H -0.1558 0.1948 0.4835 0.171 Uiso 0.559(13) 1 calc PR A 2 H57 H -0.2345 0.2498 0.4816 0.171 Uiso 0.559(13) 1 calc PR A 2 H58 H -0.1543 0.2842 0.4485 0.171 Uiso 0.559(13) 1 calc PR A 2 C56 C -0.0046(4) 0.0484(3) 0.3583(2) 0.0459(16) Uani 1 1 d . . . H59 H -0.0414 0.0121 0.3781 0.055 Uiso 1 1 calc R . . N3 N 0.0611(3) 0.0241(2) 0.3381(2) 0.0511(14) Uani 1 1 d . . . C57 C 0.0771(5) -0.0520(3) 0.3418(3) 0.0605(19) Uani 1 1 d . . . C58 C 0.0217(4) -0.1061(3) 0.3598(3) 0.0562(18) Uani 1 1 d . . . H60 H -0.0319 -0.0931 0.3695 0.067 Uiso 1 1 calc R . . C59 C 0.0475(5) -0.1790(4) 0.3630(3) 0.069(2) Uani 1 1 d . . . C60 C 0.1254(6) -0.2001(4) 0.3525(4) 0.096(3) Uani 1 1 d . B . C61 C 0.1808(5) -0.1466(4) 0.3338(4) 0.103(3) Uani 1 1 d . . . H61 H 0.2346 -0.1605 0.3257 0.123 Uiso 1 1 calc R . . C62 C 0.1541(5) -0.0710(4) 0.3272(4) 0.081(3) Uani 1 1 d . . . N4 N 0.2025(4) -0.0085(3) 0.3063(3) 0.079(2) Uani 1 1 d . . . O6 O -0.0020(4) -0.2368(2) 0.3784(2) 0.0767(16) Uani 1 1 d . . . C63 C -0.0837(5) -0.2140(4) 0.3792(4) 0.084(3) Uani 1 1 d . . . H62 H -0.1134 -0.2588 0.3905 0.125 Uiso 1 1 calc R . . H63 H -0.0965 -0.1791 0.3410 0.125 Uiso 1 1 calc R . . H64 H -0.0976 -0.1885 0.4065 0.125 Uiso 1 1 calc R . . O7 O 0.1432(4) -0.2745(3) 0.3602(4) 0.126(2) Uani 1 1 d U . . C64 C 0.2252(13) -0.3087(11) 0.3775(10) 0.110(5) Uani 0.50 1 d PU B 1 H65 H 0.2309 -0.3624 0.3819 0.165 Uiso 0.50 1 calc PR B 1 H66 H 0.2331 -0.3045 0.4139 0.165 Uiso 0.50 1 calc PR B 1 H67 H 0.2645 -0.2814 0.3480 0.165 Uiso 0.50 1 calc PR B 1 C65 C 0.2190(12) -0.2943(9) 0.3356(9) 0.093(4) Uani 0.50 1 d PU B 2 H68 H 0.2253 -0.3492 0.3439 0.140 Uiso 0.50 1 calc PR B 2 H69 H 0.2608 -0.2803 0.3520 0.140 Uiso 0.50 1 calc PR B 2 H70 H 0.2222 -0.2670 0.2942 0.140 Uiso 0.50 1 calc PR B 2 C66 C 0.2727(5) -0.0141(4) 0.2819(4) 0.096(3) Uani 1 1 d . . . H71 H 0.2889 -0.0596 0.2750 0.116 Uiso 1 1 calc R . . C67 C 0.3271(5) 0.0423(4) 0.2646(4) 0.081(3) Uani 1 1 d . . . C68 C 0.3080(4) 0.1099(3) 0.2766(3) 0.067(2) Uani 1 1 d . . . C69 C 0.3711(4) 0.1573(3) 0.2674(3) 0.0577(18) Uani 1 1 d . . . C70 C 0.4419(4) 0.1405(4) 0.2413(3) 0.067(2) Uani 1 1 d . . . H72 H 0.4818 0.1740 0.2341 0.080 Uiso 1 1 calc R . . C71 C 0.4600(5) 0.0772(4) 0.2244(4) 0.078(2) Uani 1 1 d . C . C72 C 0.4011(5) 0.0277(4) 0.2395(4) 0.091(3) Uani 1 1 d . . . H73 H 0.4117 -0.0183 0.2325 0.109 Uiso 1 1 calc R . . O8 O 0.2380(3) 0.1314(2) 0.2936(2) 0.0656(14) Uani 1 1 d . . . C73 C 0.5383(5) 0.0620(5) 0.1940(4) 0.0920(15) Uani 1 1 d U . . C74 C 0.5727(13) -0.0122(11) 0.2231(10) 0.100(5) Uani 0.501(13) 1 d PU C 2 H74 H 0.5323 -0.0484 0.2345 0.150 Uiso 0.501(13) 1 calc PR C 2 H75 H 0.5954 -0.0135 0.2572 0.150 Uiso 0.501(13) 1 calc PR C 2 H76 H 0.6143 -0.0260 0.1978 0.150 Uiso 0.501(13) 1 calc PR C 2 C75 C 0.5193(15) 0.0652(16) 0.1307(10) 0.130(4) Uani 0.501(13) 1 d PU C 2 H77 H 0.4954 0.1159 0.1090 0.195 Uiso 0.501(13) 1 calc PR C 2 H78 H 0.4827 0.0272 0.1356 0.195 Uiso 0.501(13) 1 calc PR C 2 H79 H 0.5683 0.0545 0.1099 0.195 Uiso 0.501(13) 1 calc PR C 2 C76 C 0.5881(13) 0.1273(12) 0.1688(12) 0.124(6) Uani 0.501(13) 1 d PU C 2 H80 H 0.5552 0.1736 0.1492 0.186 Uiso 0.501(13) 1 calc PR C 2 H81 H 0.6290 0.1172 0.1415 0.186 Uiso 0.501(13) 1 calc PR C 2 H82 H 0.6130 0.1340 0.1993 0.186 Uiso 0.501(13) 1 calc PR C 2 C77 C 0.5557(18) -0.0166(13) 0.1931(13) 0.147(6) Uani 0.499(13) 1 d PU C 1 H83 H 0.5538 -0.0538 0.2323 0.220 Uiso 0.499(13) 1 calc PR C 1 H84 H 0.6083 -0.0211 0.1741 0.220 Uiso 0.499(13) 1 calc PR C 1 H85 H 0.5164 -0.0264 0.1722 0.220 Uiso 0.499(13) 1 calc PR C 1 C78 C 0.5409(14) 0.1152(14) 0.1348(9) 0.111(5) Uani 0.499(13) 1 d PU C 1 H86 H 0.5283 0.1671 0.1340 0.167 Uiso 0.499(13) 1 calc PR C 1 H87 H 0.5024 0.1032 0.1145 0.167 Uiso 0.499(13) 1 calc PR C 1 H88 H 0.5938 0.1109 0.1163 0.167 Uiso 0.499(13) 1 calc PR C 1 C79 C 0.6042(12) 0.0864(15) 0.2246(12) 0.131(7) Uani 0.499(13) 1 d PU C 1 H89 H 0.6050 0.0523 0.2646 0.197 Uiso 0.499(13) 1 calc PR C 1 H90 H 0.5905 0.1388 0.2226 0.197 Uiso 0.499(13) 1 calc PR C 1 H91 H 0.6562 0.0828 0.2047 0.197 Uiso 0.499(13) 1 calc PR C 1 C80 C 0.0595(4) 0.5249(3) 0.2600(2) 0.0486(16) Uani 1 1 d . . . C81 C 0.0796(4) 0.5206(3) 0.3143(2) 0.0492(17) Uani 1 1 d . . . C82 C 0.0567(4) 0.5859(3) 0.3285(2) 0.0564(19) Uani 1 1 d . . . C83 C 0.0266(5) 0.6534(3) 0.2879(3) 0.065(2) Uani 1 1 d . . . H92 H 0.0139 0.6967 0.2983 0.077 Uiso 1 1 calc R . . C84 C 0.0148(5) 0.6597(3) 0.2339(3) 0.065(2) Uani 1 1 d . . . C85 C 0.0308(4) 0.5923(3) 0.2225(3) 0.0574(19) Uani 1 1 d . . . H93 H 0.0207 0.5942 0.1859 0.069 Uiso 1 1 calc R . . O9 O 0.1164(3) 0.4595(2) 0.34708(16) 0.0505(11) Uani 1 1 d . . . C86 C -0.0139(7) 0.7333(4) 0.1877(3) 0.093(3) Uani 1 1 d . . . C87 C -0.0315(8) 0.7990(4) 0.2107(4) 0.127(5) Uani 1 1 d . . . H94 H -0.0496 0.8455 0.1800 0.191 Uiso 1 1 calc R . . H95 H 0.0166 0.8073 0.2241 0.191 Uiso 1 1 calc R . . H96 H -0.0725 0.7857 0.2423 0.191 Uiso 1 1 calc R . . C88 C -0.0912(7) 0.7215(5) 0.1686(4) 0.113(4) Uani 1 1 d . . . H97 H -0.1101 0.7685 0.1388 0.170 Uiso 1 1 calc R . . H98 H -0.1306 0.7081 0.2013 0.170 Uiso 1 1 calc R . . H99 H -0.0821 0.6805 0.1536 0.170 Uiso 1 1 calc R . . C89 C 0.0497(7) 0.7547(4) 0.1377(3) 0.114(4) Uani 1 1 d . . . H100 H 0.0318 0.8020 0.1077 0.172 Uiso 1 1 calc R . . H101 H 0.0597 0.7140 0.1223 0.172 Uiso 1 1 calc R . . H102 H 0.0984 0.7616 0.1511 0.172 Uiso 1 1 calc R . . C90 C 0.0637(4) 0.5838(3) 0.3847(2) 0.0551(18) Uani 1 1 d . . . H103 H 0.0443 0.6278 0.3928 0.066 Uiso 1 1 calc R . . N5 N 0.0945(3) 0.5263(3) 0.4255(2) 0.0517(14) Uani 1 1 d . . . C91 C 0.0953(4) 0.5289(3) 0.4815(2) 0.0524(18) Uani 1 1 d . . . C92 C 0.0608(4) 0.5877(3) 0.4985(3) 0.0557(18) Uani 1 1 d . . . H104 H 0.0335 0.6307 0.4725 0.067 Uiso 1 1 calc R . . C93 C 0.0667(4) 0.5829(4) 0.5538(3) 0.0583(19) Uani 1 1 d . . . C94 C 0.1078(4) 0.5185(4) 0.5914(3) 0.062(2) Uani 1 1 d . . . C95 C 0.1410(4) 0.4599(4) 0.5750(3) 0.062(2) Uani 1 1 d . . . H105 H 0.1679 0.4164 0.6009 0.074 Uiso 1 1 calc R . . C96 C 0.1341(4) 0.4661(4) 0.5183(3) 0.0569(18) Uani 1 1 d . . . O10 O 0.0361(3) 0.6359(3) 0.57534(19) 0.0667(14) Uani 1 1 d . . . C97 C -0.0084(5) 0.6999(4) 0.5395(3) 0.069(2) Uani 1 1 d . . . H106 H -0.0273 0.7340 0.5600 0.104 Uiso 1 1 calc R . . H107 H -0.0536 0.6831 0.5284 0.104 Uiso 1 1 calc R . . H108 H 0.0247 0.7268 0.5052 0.104 Uiso 1 1 calc R . . O11 O 0.1113(3) 0.5191(3) 0.64508(19) 0.0732(15) Uani 1 1 d . . . C98 C 0.1511(5) 0.4542(5) 0.6845(3) 0.083(3) Uani 1 1 d . . . H109 H 0.1501 0.4608 0.7211 0.124 Uiso 1 1 calc R . . H110 H 0.2058 0.4482 0.6695 0.124 Uiso 1 1 calc R . . H111 H 0.1247 0.4089 0.6901 0.124 Uiso 1 1 calc R . . N6 N 0.1673(3) 0.4119(3) 0.4946(2) 0.0545(15) Uani 1 1 d . . . C99 C 0.2025(4) 0.3485(3) 0.5247(3) 0.0563(18) Uani 1 1 d . . . H112 H 0.2041 0.3388 0.5641 0.068 Uiso 1 1 calc R . . C100 C 0.2387(4) 0.2922(3) 0.5047(3) 0.0585(19) Uani 1 1 d . . . C101 C 0.2485(4) 0.3048(3) 0.4449(3) 0.0531(17) Uani 1 1 d . . . C102 C 0.2978(5) 0.2506(3) 0.4283(3) 0.064(2) Uani 1 1 d . . . C103 C 0.3256(6) 0.1838(4) 0.4692(3) 0.084(3) Uani 1 1 d . . . H113 H 0.3568 0.1471 0.4570 0.101 Uiso 1 1 calc R . . C104 C 0.3096(6) 0.1675(4) 0.5284(3) 0.091(3) Uani 1 1 d . D . C105 C 0.2698(5) 0.2237(4) 0.5444(3) 0.073(2) Uani 1 1 d . . . H114 H 0.2629 0.2163 0.5838 0.088 Uiso 1 1 calc R . . O12 O 0.2132(3) 0.3626(2) 0.40705(17) 0.0562(12) Uani 1 1 d . . . C106 C 0.3372(8) 0.0904(5) 0.5716(4) 0.1143(16) Uani 1 1 d U . . C107 C 0.3545(15) 0.0270(9) 0.5510(9) 0.130(3) Uani 0.573(11) 1 d PU D 1 H115 H 0.3054 0.0137 0.5424 0.195 Uiso 0.573(11) 1 calc PR D 1 H116 H 0.3789 -0.0171 0.5806 0.195 Uiso 0.573(11) 1 calc PR D 1 H117 H 0.3906 0.0422 0.5165 0.195 Uiso 0.573(11) 1 calc PR D 1 C108 C 0.4202(14) 0.0981(12) 0.5813(10) 0.139(6) Uani 0.573(11) 1 d PU D 1 H118 H 0.4201 0.1394 0.5955 0.209 Uiso 0.573(11) 1 calc PR D 1 H119 H 0.4531 0.1097 0.5452 0.209 Uiso 0.573(11) 1 calc PR D 1 H120 H 0.4414 0.0505 0.6093 0.209 Uiso 0.573(11) 1 calc PR D 1 C109 C 0.2935(13) 0.0788(10) 0.6321(6) 0.115(5) Uani 0.573(11) 1 d PU D 1 H121 H 0.2879 0.1269 0.6384 0.173 Uiso 0.573(11) 1 calc PR D 1 H122 H 0.3242 0.0404 0.6616 0.173 Uiso 0.573(11) 1 calc PR D 1 H123 H 0.2413 0.0618 0.6340 0.173 Uiso 0.573(11) 1 calc PR D 1 C110 C 0.270(2) 0.0344(13) 0.5738(12) 0.141(5) Uani 0.427(11) 1 d PU D 2 H124 H 0.2604 0.0407 0.5348 0.211 Uiso 0.427(11) 1 calc PR D 2 H125 H 0.2206 0.0478 0.5932 0.211 Uiso 0.427(11) 1 calc PR D 2 H126 H 0.2881 -0.0186 0.5947 0.211 Uiso 0.427(11) 1 calc PR D 2 C111 C 0.424(2) 0.055(2) 0.5480(15) 0.174(6) Uani 0.427(11) 1 d PU D 2 H127 H 0.4206 0.0573 0.5092 0.261 Uiso 0.427(11) 1 calc PR D 2 H128 H 0.4360 0.0027 0.5733 0.261 Uiso 0.427(11) 1 calc PR D 2 H129 H 0.4661 0.0860 0.5478 0.261 Uiso 0.427(11) 1 calc PR D 2 C112 C 0.354(2) 0.0842(18) 0.6257(13) 0.137(7) Uani 0.427(11) 1 d PU D 2 H130 H 0.3711 0.0312 0.6478 0.205 Uiso 0.427(11) 1 calc PR D 2 H131 H 0.3069 0.1005 0.6454 0.205 Uiso 0.427(11) 1 calc PR D 2 H132 H 0.3963 0.1164 0.6220 0.205 Uiso 0.427(11) 1 calc PR D 2 O13 O 0.1432(5) 0.2468(4) 0.3766(3) 0.068(2) Uani 0.65 1 d PD E 1 H133 H 0.137(4) 0.225(4) 0.354(2) 0.101 Uiso 0.65 1 d PD F 1 H134 H 0.169(5) 0.284(3) 0.357(3) 0.101 Uiso 0.65 1 d PD G 1 O14 O 0.2424(8) 0.2731(7) 0.1893(5) 0.060(4) Uani 0.35 1 d PD H 3 H135 H 0.247(9) 0.3209(17) 0.173(4) 0.090 Uiso 0.35 1 d PD I 3 H136 H 0.260(8) 0.261(5) 0.221(3) 0.090 Uiso 0.35 1 d PD J 3 S1 S 0.3285(4) 0.5944(3) 0.2285(3) 0.0970(15) Uani 0.40 1 d PDU K 1 O15 O 0.3231(15) 0.6715(8) 0.2286(11) 0.158(5) Uani 0.40 1 d PDU K 1 C113 C 0.2807(19) 0.548(2) 0.2992(10) 0.122(11) Uani 0.40 1 d PDU K 1 H137 H 0.3173 0.5400 0.3281 0.184 Uiso 0.40 1 calc PR K 1 H138 H 0.2652 0.4985 0.3023 0.184 Uiso 0.40 1 calc PR K 1 H139 H 0.2339 0.5796 0.3054 0.184 Uiso 0.40 1 calc PR K 1 C114 C 0.2559(17) 0.6029(19) 0.1790(14) 0.139(8) Uani 0.40 1 d PDU K 1 H140 H 0.2782 0.6272 0.1397 0.209 Uiso 0.40 1 calc PR K 1 H141 H 0.2088 0.6337 0.1862 0.209 Uiso 0.40 1 calc PR K 1 H142 H 0.2416 0.5522 0.1845 0.209 Uiso 0.40 1 calc PR K 1 S2 S 0.2325(5) 0.6246(3) 0.2343(4) 0.0993(17) Uani 0.35 1 d PDU L 2 O16 O 0.2745(15) 0.6952(10) 0.2149(11) 0.143(7) Uani 0.35 1 d PDU L 2 C115 C 0.3056(18) 0.5583(18) 0.2801(12) 0.097(6) Uani 0.35 1 d PDU L 2 H143 H 0.3066 0.5701 0.3144 0.145 Uiso 0.35 1 calc PR L 2 H144 H 0.3577 0.5633 0.2592 0.145 Uiso 0.35 1 calc PR L 2 H145 H 0.2914 0.5062 0.2911 0.145 Uiso 0.35 1 calc PR L 2 C116 C 0.261(2) 0.5803(18) 0.1819(13) 0.094(7) Uani 0.35 1 d PDU L 2 H146 H 0.2306 0.6057 0.1486 0.140 Uiso 0.35 1 calc PR L 2 H147 H 0.2515 0.5265 0.1988 0.140 Uiso 0.35 1 calc PR L 2 H148 H 0.3175 0.5849 0.1699 0.140 Uiso 0.35 1 calc PR L 2 S3 S -0.2708(3) 0.7289(2) 0.2880(2) 0.1056(11) Uani 0.65 1 d PDU M 1 O17 O -0.2252(6) 0.7254(5) 0.3339(4) 0.106(2) Uani 0.65 1 d PDU M 1 C117 C -0.3759(7) 0.7341(12) 0.3225(8) 0.184(4) Uani 0.65 1 d PDU M 1 H149 H -0.3863 0.6845 0.3518 0.277 Uiso 0.65 1 calc PR M 1 H150 H -0.4134 0.7478 0.2932 0.277 Uiso 0.65 1 calc PR M 1 H151 H -0.3816 0.7726 0.3399 0.277 Uiso 0.65 1 calc PR M 1 C118 C -0.2797(14) 0.8247(10) 0.2412(10) 0.194(8) Uani 0.65 1 d PDU M 1 H152 H -0.2302 0.8371 0.2175 0.290 Uiso 0.65 1 calc PR M 1 H153 H -0.2913 0.8576 0.2635 0.290 Uiso 0.65 1 calc PR M 1 H154 H -0.3225 0.8325 0.2167 0.290 Uiso 0.65 1 calc PR M 1 S4 S -0.2856(10) 0.7814(11) 0.2960(7) 0.118(3) Uani 0.15 1 d PDU N 2 O18 O -0.2252(6) 0.7254(5) 0.3339(4) 0.106(2) Uani 0.15 1 d PDU N 2 C119 C -0.3759(7) 0.7341(12) 0.3225(8) 0.184(4) Uani 0.15 1 d PDU N 2 H155 H -0.3924 0.7340 0.3608 0.277 Uiso 0.15 1 calc PR N 2 H156 H -0.3666 0.6816 0.3239 0.277 Uiso 0.15 1 calc PR N 2 H157 H -0.4172 0.7611 0.2969 0.277 Uiso 0.15 1 calc PR N 2 C120 C -0.2755(18) 0.771(3) 0.2271(8) 0.114(4) Uani 0.15 1 d PDU N 2 H158 H -0.2280 0.7932 0.2051 0.171 Uiso 0.15 1 calc PR N 2 H159 H -0.3217 0.7961 0.2062 0.171 Uiso 0.15 1 calc PR N 2 H160 H -0.2713 0.7164 0.2330 0.171 Uiso 0.15 1 calc PR N 2 S5 S -0.15305(18) 0.43484(18) 0.15135(11) 0.0727(7) Uani 0.70 1 d PDU O 1 O19 O -0.2374(4) 0.4651(4) 0.1394(3) 0.0894(16) Uani 0.70 1 d PDU O 1 C121 C -0.1530(10) 0.3393(7) 0.1947(7) 0.074(4) Uani 0.70 1 d PDU O 1 H161 H -0.1646 0.3101 0.1724 0.111 Uiso 0.70 1 calc PR O 1 H162 H -0.1933 0.3331 0.2266 0.111 Uiso 0.70 1 calc PR O 1 H163 H -0.1012 0.3210 0.2095 0.111 Uiso 0.70 1 calc PR O 1 C122 C -0.1333(7) 0.4720(7) 0.2019(4) 0.079(2) Uani 0.70 1 d PDU O 1 H164 H -0.1297 0.5269 0.1834 0.118 Uiso 0.70 1 calc PR O 1 H165 H -0.0834 0.4478 0.2180 0.118 Uiso 0.70 1 calc PR O 1 H166 H -0.1759 0.4620 0.2326 0.118 Uiso 0.70 1 calc PR O 1 S6 S -0.1941(11) 0.4415(13) 0.1921(7) 0.085(3) Uani 0.10 1 d PDU P 2 O20 O -0.2374(4) 0.4651(4) 0.1394(3) 0.0894(16) Uani 0.10 1 d PDU P 2 C123 C -0.136(3) 0.3514(17) 0.198(3) 0.096(10) Uani 0.10 1 d PDU P 2 H167 H -0.1709 0.3118 0.2048 0.145 Uiso 0.10 1 calc PR P 2 H168 H -0.1026 0.3364 0.2305 0.145 Uiso 0.10 1 calc PR P 2 H169 H -0.1019 0.3581 0.1630 0.145 Uiso 0.10 1 calc PR P 2 C124 C -0.109(2) 0.497(2) 0.176(2) 0.103(9) Uani 0.10 1 d PDU P 2 H170 H -0.1273 0.5497 0.1728 0.155 Uiso 0.10 1 calc PR P 2 H171 H -0.0808 0.4975 0.1404 0.155 Uiso 0.10 1 calc PR P 2 H172 H -0.0742 0.4751 0.2073 0.155 Uiso 0.10 1 calc PR P 2 S7 S 0.1268(4) 0.1137(2) 0.50775(16) 0.1211(11) Uani 0.65 1 d PDU Q 1 O21 O 0.1358(7) 0.0571(5) 0.5660(4) 0.112(2) Uani 0.65 1 d PDU Q 1 C125 C 0.1681(15) 0.0704(12) 0.4571(8) 0.164(4) Uani 0.65 1 d PDU Q 1 H173 H 0.2257 0.0661 0.4560 0.245 Uiso 0.65 1 calc PR Q 1 H174 H 0.1514 0.1019 0.4191 0.245 Uiso 0.65 1 calc PR Q 1 H175 H 0.1497 0.0197 0.4687 0.245 Uiso 0.65 1 calc PR Q 1 C126 C 0.0317(11) 0.1056(15) 0.4898(11) 0.161(6) Uani 0.65 1 d PDU Q 1 H176 H -0.0089 0.1257 0.5123 0.241 Uiso 0.65 1 calc PR Q 1 H177 H 0.0250 0.0521 0.4981 0.241 Uiso 0.65 1 calc PR Q 1 H178 H 0.0268 0.1347 0.4490 0.241 Uiso 0.65 1 calc PR Q 1 Cl1 Cl 0.3016(10) 0.5412(7) 0.3031(5) 0.107(3) Uani 0.25 1 d PDU R 3 Cl2 Cl 0.2378(13) 0.6035(9) 0.1880(7) 0.136(6) Uani 0.25 1 d PDU R 3 C127 C 0.2547(17) 0.5231(13) 0.2511(10) 0.099(7) Uani 0.25 1 d PDU R 3 H179 H 0.2876 0.4833 0.2405 0.119 Uiso 0.25 1 calc PR R 3 H180 H 0.2035 0.5028 0.2686 0.119 Uiso 0.25 1 calc PR R 3 Cl3 Cl -0.2211(19) 0.702(2) 0.3316(17) 0.104(7) Uani 0.08 1 d PDU S 3 Cl4 Cl -0.3720(15) 0.762(2) 0.2788(15) 0.107(9) Uani 0.08 1 d PDU S 3 C128 C -0.2671(19) 0.755(8) 0.267(2) 0.088(4) Uani 0.08 1 d PDU S 3 H181 H -0.2507 0.7308 0.2391 0.105 Uiso 0.08 1 calc PR S 3 H182 H -0.2492 0.8072 0.2513 0.105 Uiso 0.08 1 calc PR S 3 Cl5 Cl -0.3143(10) 0.7050(8) 0.3180(7) 0.058(3) Uani 0.12 1 d PDU T 4 Cl6 Cl -0.244(2) 0.8338(17) 0.2225(15) 0.174(10) Uani 0.12 1 d PDU T 4 C129 C -0.327(2) 0.8020(17) 0.272(2) 0.075(11) Uani 0.12 1 d PDU T 4 H183 H -0.3378 0.8339 0.2958 0.090 Uiso 0.12 1 calc PR T 4 H184 H -0.3739 0.8093 0.2506 0.090 Uiso 0.12 1 calc PR T 4 Cl7 Cl -0.1868(5) 0.5120(5) 0.1674(3) 0.0633(19) Uani 0.20 1 d PDU U 3 Cl8 Cl -0.1422(10) 0.3548(6) 0.1763(8) 0.081(4) Uani 0.20 1 d PDU U 3 C130 C -0.1087(13) 0.4372(11) 0.1816(15) 0.051(4) Uani 0.20 1 d PDU U 3 H185 H -0.0628 0.4540 0.1538 0.061 Uiso 0.20 1 calc PR U 3 H186 H -0.0921 0.4246 0.2204 0.061 Uiso 0.20 1 calc PR U 3 Cl9 Cl 0.0561(5) 0.1028(5) 0.5016(4) 0.114(2) Uani 0.30 1 d PDU V 2 Cl10 Cl 0.1638(7) 0.0121(4) 0.4536(3) 0.124(3) Uani 0.30 1 d PDU V 2 C131 C 0.1362(15) 0.1091(11) 0.4492(11) 0.091(6) Uani 0.30 1 d PDU V 2 H187 H 0.1807 0.1309 0.4574 0.110 Uiso 0.30 1 calc PR V 2 H188 H 0.1200 0.1414 0.4107 0.110 Uiso 0.30 1 calc PR V 2 Cl11 Cl 0.0561(5) 0.1028(5) 0.5016(4) 0.114(2) Uani 0.05 1 d PDU W 3 Cl12 Cl 0.2250(13) 0.062(2) 0.472(2) 0.092(9) Uani 0.05 1 d PDU W 3 C132 C 0.126(2) 0.036(4) 0.483(6) 0.109(5) Uani 0.05 1 d PDU W 3 H189 H 0.1228 -0.0144 0.5136 0.131 Uiso 0.05 1 calc PR W 3 H190 H 0.1109 0.0322 0.4475 0.131 Uiso 0.05 1 calc PR W 3 Cl13 Cl 0.2622(6) 0.1553(5) 0.1119(6) 0.155(4) Uani 0.33 1 d PDU X 1 Cl14 Cl 0.1015(3) 0.1517(3) 0.1675(2) 0.1405(14) Uani 0.33 1 d PDU X 1 C133 C 0.1828(10) 0.2048(11) 0.1336(12) 0.100(5) Uani 0.33 1 d PDU X 1 H191 H 0.1651 0.2483 0.0998 0.120 Uiso 0.33 1 calc PR X 1 H192 H 0.2001 0.2257 0.1601 0.120 Uiso 0.33 1 calc PR X 1 Cl15 Cl 0.2349(5) 0.2034(7) 0.0847(4) 0.140(4) Uani 0.33 1 d PDU Y 2 Cl16 Cl 0.1015(3) 0.1517(3) 0.1675(2) 0.1405(14) Uani 0.33 1 d PDU Y 2 C134 C 0.1959(14) 0.185(2) 0.1560(10) 0.143(4) Uani 0.33 1 d PDU Y 2 H193 H 0.2316 0.1473 0.1825 0.171 Uiso 0.33 1 calc PR Y 2 H194 H 0.1922 0.2328 0.1640 0.171 Uiso 0.33 1 calc PR Y 2 Cl17 Cl 0.4038(6) 0.0023(5) 0.4165(5) 0.227(4) Uani 0.50 1 d PDU Z 1 Cl18 Cl 0.3574(6) -0.1328(4) 0.4092(3) 0.178(3) Uani 0.50 1 d PDU Z 1 C135 C 0.3270(13) -0.0447(11) 0.4185(10) 0.171(6) Uani 0.50 1 d PDU Z 1 H195 H 0.2929 -0.0127 0.3880 0.205 Uiso 0.50 1 calc PR Z 1 H196 H 0.2957 -0.0547 0.4556 0.205 Uiso 0.50 1 calc PR Z 1 Cl19 Cl 0.4147(5) -0.2078(5) 0.2853(4) 0.257(2) Uani 0.45 1 d PDU A 1 Cl20 Cl 0.4988(9) -0.2001(6) 0.1808(5) 0.228(3) Uani 0.45 1 d PDU A 1 C136 C 0.4153(19) -0.234(2) 0.2250(12) 0.274(6) Uani 0.45 1 d PDU A 1 H197 H 0.4169 -0.2895 0.2370 0.329 Uiso 0.45 1 calc PR A 1 H198 H 0.3673 -0.2107 0.2047 0.329 Uiso 0.45 1 calc PR A 1 Cl21 Cl 0.4147(5) -0.2078(5) 0.2853(4) 0.257(2) Uani 0.15 1 d PDU B 2 Cl22 Cl 0.4746(15) -0.2367(17) 0.1792(9) 0.202(7) Uani 0.15 1 d PDU B 2 C137 C 0.413(4) -0.265(3) 0.2439(19) 0.219(9) Uani 0.15 1 d PDU B 2 H199 H 0.4298 -0.3180 0.2672 0.263 Uiso 0.15 1 calc PR B 2 H200 H 0.3584 -0.2632 0.2347 0.263 Uiso 0.15 1 calc PR B 2 Cl23 Cl 0.4147(5) -0.2078(5) 0.2853(4) 0.257(2) Uani 0.15 1 d PDU C 3 Cl24 Cl 0.4133(16) -0.1441(14) 0.3747(8) 0.212(4) Uani 0.15 1 d PDU C 3 C138 C 0.360(3) -0.192(4) 0.345(2) 0.244(12) Uani 0.15 1 d PDU C 3 H201 H 0.3095 -0.1617 0.3328 0.293 Uiso 0.15 1 calc PR C 3 H202 H 0.3467 -0.2416 0.3746 0.293 Uiso 0.15 1 calc PR C 3 Cl25 Cl 0.3019(14) -0.084(3) 0.159(2) 0.344(17) Uani 0.15 1 d PDU D 4 Cl26 Cl 0.1292(14) -0.0677(15) 0.1891(11) 0.171(6) Uani 0.15 1 d PDU D 4 C139 C 0.2064(17) -0.101(4) 0.148(3) 0.135(11) Uani 0.15 1 d PDU D 4 H203 H 0.2040 -0.1559 0.1585 0.162 Uiso 0.15 1 calc PR D 4 H204 H 0.1975 -0.0752 0.1074 0.162 Uiso 0.15 1 calc PR D 4 Cl27 Cl 0.1938(16) -0.1243(19) 0.1837(14) 0.133(8) Uani 0.10 1 d PDU E 5 Cl28 Cl 0.3643(18) -0.155(3) 0.209(2) 0.222(12) Uani 0.10 1 d PDU E 5 C140 C 0.293(2) -0.106(9) 0.158(3) 0.164(14) Uani 0.10 1 d PDU E 5 H205 H 0.2979 -0.0509 0.1451 0.197 Uiso 0.10 1 calc PR E 5 H206 H 0.3062 -0.1207 0.1240 0.197 Uiso 0.10 1 calc PR E 5 Cl29 Cl 0.1101(18) -0.039(2) 0.120(2) 0.322(12) Uani 0.15 1 d PDU F 6 C141 C 0.206(4) -0.026(3) 0.134(5) 0.338(13) Uani 0.15 1 d PDU F 6 H207 H 0.2390 -0.0077 0.0980 0.405 Uiso 0.15 1 calc PR F 6 H208 H 0.2014 0.0129 0.1518 0.405 Uiso 0.15 1 calc PR F 6 Cl30 Cl 0.253(2) -0.1119(17) 0.1812(16) 0.261(13) Uani 0.15 1 d PDU F 6 Cl31 Cl 0.6002(4) 0.1541(3) 0.3229(2) 0.1349(18) Uani 0.50 1 d PDU G 1 Cl32 Cl 0.5319(5) 0.1488(7) 0.4306(4) 0.208(4) Uani 0.50 1 d PDU G 1 C142 C 0.5301(17) 0.2025(13) 0.3590(8) 0.194(8) Uani 0.50 1 d PDU G 1 H209 H 0.5450 0.2543 0.3510 0.233 Uiso 0.50 1 calc PR G 1 H210 H 0.4768 0.2065 0.3464 0.233 Uiso 0.50 1 calc PR G 1 Cl33 Cl 0.5235(4) 0.2663(4) 0.4258(3) 0.1019(17) Uani 0.35 1 d PDU H 2 Cl34 Cl 0.5259(12) 0.1341(7) 0.3921(10) 0.289(8) Uani 0.35 1 d PDU H 2 C143 C 0.532(2) 0.2282(12) 0.3747(10) 0.126(5) Uani 0.35 1 d PDU H 2 H211 H 0.4904 0.2552 0.3484 0.151 Uiso 0.35 1 calc PR H 2 H212 H 0.5830 0.2408 0.3526 0.151 Uiso 0.35 1 calc PR H 2 Cl35 Cl 0.5131(11) 0.3500(9) 0.4358(5) 0.182(5) Uani 0.25 1 d PDU I 3 Cl36 Cl 0.4867(19) 0.3100(16) 0.5593(7) 0.292(9) Uani 0.25 1 d PDU I 3 C144 C 0.454(2) 0.304(2) 0.4973(9) 0.136(10) Uani 0.25 1 d PDU I 3 H213 H 0.4543 0.2503 0.5023 0.163 Uiso 0.25 1 calc PR I 3 H214 H 0.3995 0.3275 0.4926 0.163 Uiso 0.25 1 calc PR I 3 Cl37 Cl 0.531(3) 0.273(3) 0.525(2) 0.245(9) Uani 0.10 1 d PDU J 4 Cl38 Cl 0.425(2) 0.3996(19) 0.4548(17) 0.174(11) Uani 0.10 1 d PDU J 4 C145 C 0.476(7) 0.310(4) 0.463(4) 0.199(17) Uani 0.10 1 d PDU J 4 H215 H 0.5125 0.3144 0.4290 0.239 Uiso 0.10 1 calc PR J 4 H216 H 0.4379 0.2732 0.4666 0.239 Uiso 0.10 1 calc PR J 4 Cl39 Cl 0.3892(5) 0.2956(5) -0.0570(4) 0.131(2) Uani 0.40 1 d PDU K 1 Cl40 Cl 0.2385(5) 0.2916(6) -0.1004(5) 0.215(3) Uani 0.40 1 d PDU K 1 C146 C 0.2927(11) 0.3345(13) -0.0677(10) 0.122(5) Uani 0.40 1 d PDU K 1 H217 H 0.2935 0.3892 -0.0915 0.146 Uiso 0.40 1 calc PR K 1 H218 H 0.2650 0.3307 -0.0302 0.146 Uiso 0.40 1 calc PR K 1 Cl41 Cl 0.3507(14) 0.3597(17) -0.0601(13) 0.126(6) Uani 0.10 1 d PDU L 2 Cl42 Cl 0.2385(5) 0.2916(6) -0.1004(5) 0.215(3) Uani 0.10 1 d PDU L 2 C147 C 0.293(4) 0.282(3) -0.0417(18) 0.161(12) Uani 0.10 1 d PDU L 2 H219 H 0.2560 0.2791 -0.0081 0.193 Uiso 0.10 1 calc PR L 2 H220 H 0.3274 0.2336 -0.0318 0.193 Uiso 0.10 1 calc PR L 2 C148 C 0.4084(12) 0.1723(10) -0.0280(10) 0.167(3) Uani 0.50 1 d PDU M 3 H221 H 0.3839 0.1626 0.0112 0.200 Uiso 0.50 1 calc PR M 3 H222 H 0.4606 0.1433 -0.0251 0.200 Uiso 0.50 1 calc PR M 3 C149 C 0.3552(13) 0.1434(11) -0.0611(13) 0.212(6) Uani 0.50 1 d PDU M 3 H223 H 0.3802 0.1508 -0.0998 0.254 Uiso 0.50 1 calc PR M 3 H224 H 0.3490 0.0886 -0.0406 0.254 Uiso 0.50 1 calc PR M 3 C150 C 0.2730(12) 0.1894(11) -0.0653(12) 0.189(6) Uani 0.50 1 d PDU M 3 H225 H 0.2411 0.1759 -0.0895 0.227 Uiso 0.50 1 calc PR M 3 H226 H 0.2450 0.1762 -0.0268 0.227 Uiso 0.50 1 calc PR M 3 C151 C 0.2826(13) 0.2751(11) -0.0909(13) 0.194(4) Uani 0.50 1 d PDU M 3 H227 H 0.3078 0.2882 -0.1302 0.232 Uiso 0.50 1 calc PR M 3 H228 H 0.2298 0.3031 -0.0932 0.232 Uiso 0.50 1 calc PR M 3 C152 C 0.3312(13) 0.3005(10) -0.0567(12) 0.147(5) Uani 0.50 1 d PDU M 3 H229 H 0.3074 0.2875 -0.0170 0.177 Uiso 0.50 1 calc PR M 3 H230 H 0.3346 0.3561 -0.0740 0.177 Uiso 0.50 1 calc PR M 3 C153 C 0.4187(11) 0.2558(11) -0.0575(13) 0.161(7) Uani 0.50 1 d PDU M 3 H231 H 0.4414 0.2667 -0.0972 0.193 Uiso 0.50 1 calc PR M 3 H232 H 0.4544 0.2720 -0.0371 0.193 Uiso 0.50 1 calc PR M 3 C154 C 0.3559(16) 0.4348(11) 0.5511(7) 0.215(5) Uani 0.60 1 d PDU N 1 H233 H 0.3790 0.4052 0.5878 0.258 Uiso 0.60 1 calc PR N 1 H234 H 0.3011 0.4215 0.5547 0.258 Uiso 0.60 1 calc PR N 1 C155 C 0.3554(16) 0.5200(11) 0.5394(8) 0.210(4) Uani 0.60 1 d PDU N 1 H235 H 0.4100 0.5335 0.5365 0.252 Uiso 0.60 1 calc PR N 1 H236 H 0.3255 0.5317 0.5714 0.252 Uiso 0.60 1 calc PR N 1 C156 C 0.3167(15) 0.5678(11) 0.4826(9) 0.214(6) Uani 0.60 1 d PDU N 1 H237 H 0.2615 0.5559 0.4854 0.257 Uiso 0.60 1 calc PR N 1 H238 H 0.3171 0.6227 0.4746 0.257 Uiso 0.60 1 calc PR N 1 C157 C 0.366(2) 0.5467(11) 0.4345(8) 0.229(9) Uani 0.60 1 d PDU N 1 H239 H 0.3411 0.5743 0.3981 0.275 Uiso 0.60 1 calc PR N 1 H240 H 0.4193 0.5633 0.4299 0.275 Uiso 0.60 1 calc PR N 1 C158 C 0.3719(15) 0.4621(11) 0.4463(8) 0.188(5) Uani 0.60 1 d PDU N 1 H241 H 0.4071 0.4519 0.4156 0.226 Uiso 0.60 1 calc PR N 1 H242 H 0.3191 0.4472 0.4448 0.226 Uiso 0.60 1 calc PR N 1 C159 C 0.4030(14) 0.4128(11) 0.5038(10) 0.213(6) Uani 0.60 1 d PDU N 1 H243 H 0.3983 0.3586 0.5112 0.255 Uiso 0.60 1 calc PR N 1 H244 H 0.4593 0.4199 0.5031 0.255 Uiso 0.60 1 calc PR N 1 C160 C 0.353(2) 0.4892(11) 0.5127(10) 0.170(6) Uani 0.40 1 d PDU O 2 H245 H 0.4083 0.4706 0.5192 0.204 Uiso 0.40 1 calc PR O 2 H246 H 0.3199 0.4456 0.5306 0.204 Uiso 0.40 1 calc PR O 2 C161 C 0.326(2) 0.5518(16) 0.5393(10) 0.226(4) Uani 0.40 1 d PDU O 2 H247 H 0.2708 0.5720 0.5310 0.271 Uiso 0.40 1 calc PR O 2 H248 H 0.3281 0.5294 0.5812 0.271 Uiso 0.40 1 calc PR O 2 C162 C 0.381(2) 0.6169(15) 0.5130(11) 0.236(8) Uani 0.40 1 d PDU O 2 H249 H 0.4367 0.5963 0.5190 0.284 Uiso 0.40 1 calc PR O 2 H250 H 0.3682 0.6548 0.5314 0.284 Uiso 0.40 1 calc PR O 2 C163 C 0.370(3) 0.6550(12) 0.4478(12) 0.255(8) Uani 0.40 1 d PDU O 2 H251 H 0.3150 0.6754 0.4418 0.306 Uiso 0.40 1 calc PR O 2 H252 H 0.4044 0.6975 0.4300 0.306 Uiso 0.40 1 calc PR O 2 C164 C 0.393(2) 0.5948(16) 0.4201(10) 0.201(5) Uani 0.40 1 d PDU O 2 H253 H 0.4493 0.5769 0.4243 0.241 Uiso 0.40 1 calc PR O 2 H254 H 0.3854 0.6182 0.3788 0.241 Uiso 0.40 1 calc PR O 2 C165 C 0.342(3) 0.5260(17) 0.4480(11) 0.205(10) Uani 0.40 1 d PDU O 2 H255 H 0.2862 0.5432 0.4419 0.247 Uiso 0.40 1 calc PR O 2 H256 H 0.3586 0.4881 0.4299 0.247 Uiso 0.40 1 calc PR O 2 C166 C -0.1788(13) 0.0654(10) 0.2669(8) 0.126(3) Uani 0.50 1 d PDU P 1 H257 H -0.2348 0.0670 0.2817 0.152 Uiso 0.50 1 calc PR P 1 H258 H -0.1464 0.0445 0.3000 0.152 Uiso 0.50 1 calc PR P 1 C167 C -0.1655(12) 0.0130(10) 0.2330(10) 0.145(4) Uani 0.50 1 d PDU P 1 H259 H -0.2044 0.0292 0.2039 0.175 Uiso 0.50 1 calc PR P 1 H260 H -0.1750 -0.0393 0.2592 0.175 Uiso 0.50 1 calc PR P 1 C168 C -0.0829(14) 0.0126(9) 0.2033(10) 0.146(6) Uani 0.50 1 d PDU P 1 H261 H -0.0807 -0.0162 0.1777 0.175 Uiso 0.50 1 calc PR P 1 H262 H -0.0448 -0.0137 0.2324 0.175 Uiso 0.50 1 calc PR P 1 C169 C -0.0589(13) 0.0926(9) 0.1685(9) 0.136(4) Uani 0.50 1 d PDU P 1 H263 H -0.0026 0.0894 0.1548 0.163 Uiso 0.50 1 calc PR P 1 H264 H -0.0898 0.1148 0.1346 0.163 Uiso 0.50 1 calc PR P 1 C170 C -0.0716(12) 0.1444(10) 0.2019(9) 0.139(5) Uani 0.50 1 d PDU P 1 H265 H -0.0608 0.1966 0.1760 0.167 Uiso 0.50 1 calc PR P 1 H266 H -0.0338 0.1274 0.2318 0.167 Uiso 0.50 1 calc PR P 1 C171 C -0.1579(12) 0.1457(9) 0.2308(9) 0.123(5) Uani 0.50 1 d PDU P 1 H267 H -0.1622 0.1764 0.2552 0.148 Uiso 0.50 1 calc PR P 1 H268 H -0.1954 0.1696 0.2010 0.148 Uiso 0.50 1 calc PR P 1 C172 C -0.072(2) 0.015(2) 0.2331(13) 0.165(3) Uani 0.25 1 d PDU Q 2 H269 H -0.0504 -0.0383 0.2430 0.198 Uiso 0.25 1 calc PR Q 2 H270 H -0.0353 0.0427 0.2438 0.198 Uiso 0.25 1 calc PR Q 2 C173 C -0.082(2) 0.052(2) 0.1680(12) 0.178(5) Uani 0.25 1 d PDU Q 2 H271 H -0.0300 0.0492 0.1465 0.213 Uiso 0.25 1 calc PR Q 2 H272 H -0.1183 0.0244 0.1572 0.213 Uiso 0.25 1 calc PR Q 2 C174 C -0.114(2) 0.136(2) 0.1530(13) 0.173(5) Uani 0.25 1 d PDU Q 2 H273 H -0.0752 0.1642 0.1613 0.208 Uiso 0.25 1 calc PR Q 2 H274 H -0.1214 0.1593 0.1117 0.208 Uiso 0.25 1 calc PR Q 2 C175 C -0.192(2) 0.143(2) 0.1871(14) 0.167(7) Uani 0.25 1 d PDU Q 2 H275 H -0.2328 0.1209 0.1747 0.200 Uiso 0.25 1 calc PR Q 2 H276 H -0.2091 0.1973 0.1786 0.200 Uiso 0.25 1 calc PR Q 2 C176 C -0.187(2) 0.102(2) 0.2516(13) 0.159(9) Uani 0.25 1 d PDU Q 2 H277 H -0.2400 0.1040 0.2716 0.191 Uiso 0.25 1 calc PR Q 2 H278 H -0.1526 0.1291 0.2653 0.191 Uiso 0.25 1 calc PR Q 2 C177 C -0.153(2) 0.0186(19) 0.2658(13) 0.163(11) Uani 0.25 1 d PDU Q 2 H279 H -0.1478 -0.0061 0.3074 0.195 Uiso 0.25 1 calc PR Q 2 H280 H -0.1898 -0.0092 0.2552 0.195 Uiso 0.25 1 calc PR Q 2 C178 C -0.147(3) 0.0521(15) 0.2674(9) 0.129(6) Uani 0.25 1 d PDU R 3 H281 H -0.1259 0.0328 0.3054 0.155 Uiso 0.25 1 calc PR R 3 H282 H -0.2051 0.0573 0.2732 0.155 Uiso 0.25 1 calc PR R 3 C179 C -0.122(2) -0.0052(12) 0.2386(11) 0.119(6) Uani 0.25 1 d PDU R 3 H283 H -0.1468 -0.0530 0.2607 0.143 Uiso 0.25 1 calc PR R 3 H284 H -0.0643 -0.0166 0.2383 0.143 Uiso 0.25 1 calc PR R 3 C180 C -0.146(2) 0.0249(14) 0.1770(11) 0.124(6) Uani 0.25 1 d PDU R 3 H285 H -0.1248 -0.0117 0.1586 0.149 Uiso 0.25 1 calc PR R 3 H286 H -0.2042 0.0292 0.1776 0.149 Uiso 0.25 1 calc PR R 3 C181 C -0.116(3) 0.1023(14) 0.1419(9) 0.130(9) Uani 0.25 1 d PDU R 3 H287 H -0.1373 0.1217 0.1040 0.156 Uiso 0.25 1 calc PR R 3 H288 H -0.0579 0.0963 0.1360 0.156 Uiso 0.25 1 calc PR R 3 C182 C -0.139(3) 0.1602(12) 0.1707(11) 0.121(7) Uani 0.25 1 d PDU R 3 H289 H -0.1970 0.1736 0.1699 0.146 Uiso 0.25 1 calc PR R 3 H290 H -0.1129 0.2070 0.1489 0.146 Uiso 0.25 1 calc PR R 3 C183 C -0.118(3) 0.1301(15) 0.2326(12) 0.131(9) Uani 0.25 1 d PDU R 3 H291 H -0.0599 0.1268 0.2330 0.157 Uiso 0.25 1 calc PR R 3 H292 H -0.1409 0.1665 0.2509 0.157 Uiso 0.25 1 calc PR R 3 C184 C -0.3311(15) 0.2710(12) -0.0401(12) 0.254(3) Uani 0.60 1 d PDU S 1 H293 H -0.3786 0.2856 -0.0190 0.305 Uiso 0.60 1 calc PR S 1 H294 H -0.3376 0.2974 -0.0814 0.305 Uiso 0.60 1 calc PR S 1 C185 C -0.3264(17) 0.1851(13) -0.0260(15) 0.279(4) Uani 0.60 1 d PDU S 1 H295 H -0.3805 0.1689 -0.0159 0.335 Uiso 0.60 1 calc PR S 1 H296 H -0.3062 0.1754 -0.0610 0.335 Uiso 0.60 1 calc PR S 1 C186 C -0.2775(16) 0.1365(10) 0.0202(12) 0.254(6) Uani 0.60 1 d PDU S 1 H297 H -0.2555 0.0918 0.0106 0.305 Uiso 0.60 1 calc PR S 1 H298 H -0.3131 0.1175 0.0553 0.305 Uiso 0.60 1 calc PR S 1 C187 C -0.2110(17) 0.1675(13) 0.0346(15) 0.318(10) Uani 0.60 1 d PDU S 1 H299 H -0.1655 0.1695 0.0063 0.382 Uiso 0.60 1 calc PR S 1 H300 H -0.1945 0.1337 0.0727 0.382 Uiso 0.60 1 calc PR S 1 C188 C -0.2369(19) 0.2505(15) 0.0348(12) 0.301(6) Uani 0.60 1 d PDU S 1 H301 H -0.2825 0.2495 0.0628 0.361 Uiso 0.60 1 calc PR S 1 H302 H -0.1930 0.2713 0.0447 0.361 Uiso 0.60 1 calc PR S 1 C189 C -0.2589(16) 0.2984(10) -0.0255(11) 0.229(7) Uani 0.60 1 d PDU S 1 H303 H -0.2137 0.2956 -0.0531 0.275 Uiso 0.60 1 calc PR S 1 H304 H -0.2703 0.3521 -0.0291 0.275 Uiso 0.60 1 calc PR S 1 C190 C -0.2500(16) 0.222(2) -0.0634(12) 0.251(4) Uani 0.40 1 d PDU T 2 H305 H -0.2451 0.1669 -0.0540 0.301 Uiso 0.40 1 calc PR T 2 H306 H -0.2254 0.2465 -0.1025 0.301 Uiso 0.40 1 calc PR T 2 C191 C -0.3388(16) 0.251(2) -0.0619(11) 0.250(9) Uani 0.40 1 d PDU T 2 H307 H -0.3657 0.2357 -0.0877 0.300 Uiso 0.40 1 calc PR T 2 H308 H -0.3446 0.3072 -0.0750 0.300 Uiso 0.40 1 calc PR T 2 C192 C -0.3767(14) 0.216(2) 0.0005(13) 0.270(5) Uani 0.40 1 d PDU T 2 H309 H -0.4328 0.2356 0.0023 0.323 Uiso 0.40 1 calc PR T 2 H310 H -0.3741 0.1602 0.0127 0.323 Uiso 0.40 1 calc PR T 2 C193 C -0.3317(17) 0.238(2) 0.0405(12) 0.233(9) Uani 0.40 1 d PDU T 2 H311 H -0.3359 0.2941 0.0286 0.280 Uiso 0.40 1 calc PR T 2 H312 H -0.3561 0.2168 0.0799 0.280 Uiso 0.40 1 calc PR T 2 C194 C -0.2456(17) 0.209(3) 0.0394(11) 0.286(11) Uani 0.40 1 d PDU T 2 H313 H -0.2410 0.1529 0.0538 0.343 Uiso 0.40 1 calc PR T 2 H314 H -0.2185 0.2251 0.0648 0.343 Uiso 0.40 1 calc PR T 2 C195 C -0.2056(14) 0.240(2) -0.0219(13) 0.216(9) Uani 0.40 1 d PDU T 2 H315 H -0.2039 0.2957 -0.0343 0.259 Uiso 0.40 1 calc PR T 2 H316 H -0.1508 0.2169 -0.0222 0.259 Uiso 0.40 1 calc PR T 2 C196 C 0.0722(12) 0.0428(14) -0.0206(12) 0.272(10) Uani 0.60 1 d PDU . 1 H317 H 0.1130 0.0057 0.0015 0.327 Uiso 0.60 1 calc PR . 1 H318 H 0.0976 0.0891 -0.0457 0.327 Uiso 0.60 1 calc PR . 1 C197 C 0.0075(17) 0.0626(11) 0.0201(10) 0.228(9) Uani 0.60 1 d PDU U 1 H319 H 0.0310 0.0826 0.0449 0.273 Uiso 0.60 1 calc PR U 1 H320 H -0.0311 0.1024 -0.0022 0.273 Uiso 0.60 1 calc PR U 1 C198 C -0.0343(19) -0.0084(17) 0.0571(9) 0.292(16) Uani 0.60 1 d PDU . 1 H321 H -0.0757 0.0050 0.0832 0.351 Uiso 0.60 1 calc PR . 1 H322 H 0.0042 -0.0471 0.0807 0.351 Uiso 0.60 1 calc PR . 1 C199 C 0.108(3) 0.011(2) -0.0587(14) 0.188(3) Uani 0.20 1 d PDU V 2 H323 H 0.1341 -0.0189 -0.0817 0.226 Uiso 0.20 1 calc PR V 2 H324 H 0.0640 0.0436 -0.0795 0.226 Uiso 0.20 1 calc PR V 2 C200 C 0.167(2) 0.060(2) -0.0526(16) 0.181(3) Uani 0.20 1 d PDU V 2 H325 H 0.1836 0.0973 -0.0906 0.217 Uiso 0.20 1 calc PR V 2 H326 H 0.2147 0.0283 -0.0361 0.217 Uiso 0.20 1 calc PR V 2 C201 C 0.130(3) 0.1036(19) -0.0133(17) 0.174(4) Uani 0.20 1 d PDU V 2 H327 H 0.1695 0.1335 -0.0080 0.208 Uiso 0.20 1 calc PR V 2 H328 H 0.0854 0.1393 -0.0316 0.208 Uiso 0.20 1 calc PR V 2 C202 C 0.100(3) 0.048(2) 0.0449(14) 0.201(4) Uani 0.20 1 d PDU V 2 H329 H 0.0748 0.0762 0.0687 0.241 Uiso 0.20 1 calc PR V 2 H330 H 0.1455 0.0150 0.0645 0.241 Uiso 0.20 1 calc PR V 2 C203 C 0.041(3) -0.003(2) 0.0390(17) 0.190(8) Uani 0.20 1 d PDU V 2 H331 H -0.0074 0.0291 0.0240 0.228 Uiso 0.20 1 calc PR V 2 H332 H 0.0260 -0.0405 0.0771 0.228 Uiso 0.20 1 calc PR V 2 C204 C 0.075(3) -0.044(2) -0.0011(19) 0.177(10) Uani 0.20 1 d PDU V 2 H333 H 0.1179 -0.0829 0.0172 0.212 Uiso 0.20 1 calc PR V 2 H334 H 0.0337 -0.0714 -0.0075 0.212 Uiso 0.20 1 calc PR V 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 0.0645(5) 0.0376(4) 0.0374(4) -0.0023(3) 0.0069(4) -0.0288(4) Ni2 0.0706(6) 0.0349(4) 0.0776(6) -0.0304(4) 0.0210(5) -0.0301(4) Ni3 0.0921(7) 0.0405(4) 0.0348(4) -0.0143(3) -0.0037(4) -0.0359(4) C1 0.053(4) 0.037(3) 0.035(3) -0.015(2) 0.003(3) -0.021(3) C2 0.051(4) 0.031(3) 0.037(3) -0.015(2) 0.001(3) -0.021(3) C3 0.059(4) 0.031(3) 0.034(3) -0.011(2) 0.002(3) -0.024(3) C4 0.071(4) 0.038(3) 0.034(3) -0.017(2) 0.004(3) -0.027(3) C5 0.068(4) 0.032(3) 0.031(3) -0.013(2) -0.003(3) -0.023(3) C6 0.065(4) 0.032(3) 0.035(3) -0.008(2) 0.000(3) -0.031(3) C7 0.065(4) 0.035(3) 0.046(4) 0.001(3) -0.011(3) -0.023(3) C8 0.060(4) 0.043(3) 0.048(4) -0.004(3) 0.003(3) -0.027(3) C9 0.063(4) 0.039(3) 0.054(4) -0.006(3) -0.001(3) -0.022(3) C10 0.081(5) 0.034(3) 0.056(4) -0.003(3) 0.007(4) -0.029(3) C11 0.078(5) 0.035(3) 0.048(4) 0.001(3) -0.003(4) -0.020(3) C12 0.081(5) 0.035(3) 0.050(4) -0.004(3) -0.006(4) -0.027(3) C13 0.067(4) 0.035(3) 0.033(3) -0.012(2) 0.003(3) -0.026(3) C14 0.067(4) 0.036(3) 0.033(3) -0.013(2) 0.007(3) -0.028(3) C15 0.073(5) 0.047(3) 0.034(3) -0.012(3) 0.011(3) -0.031(3) C16 0.088(5) 0.066(4) 0.027(3) -0.017(3) 0.015(3) -0.041(4) C17 0.083(5) 0.055(4) 0.034(3) -0.022(3) 0.006(3) -0.033(3) C18 0.075(5) 0.045(3) 0.036(3) -0.018(3) 0.009(3) -0.033(3) O1 0.067(3) 0.046(2) 0.033(2) -0.0071(18) 0.007(2) -0.034(2) C19 0.097(6) 0.080(5) 0.039(4) -0.032(3) 0.008(4) -0.050(4) C20 0.093(8) 0.317(15) 0.171(10) -0.186(11) -0.024(8) -0.027(9) C21 0.204(11) 0.067(6) 0.221(12) -0.049(7) -0.126(10) -0.035(7) C22 0.208(11) 0.123(7) 0.061(5) -0.022(5) -0.036(6) -0.097(8) C23 0.074(5) 0.048(3) 0.028(3) -0.005(3) 0.009(3) -0.026(3) N1 0.059(3) 0.040(3) 0.038(3) -0.006(2) 0.007(2) -0.021(2) C24 0.065(4) 0.035(3) 0.040(3) -0.001(3) 0.016(3) -0.018(3) C25 0.063(4) 0.044(3) 0.044(4) -0.006(3) 0.009(3) -0.018(3) C26 0.068(5) 0.044(3) 0.039(4) 0.000(3) 0.014(3) -0.013(3) C27 0.062(4) 0.038(3) 0.052(4) -0.000(3) 0.010(3) -0.015(3) C28 0.061(4) 0.037(3) 0.048(4) -0.002(3) 0.012(3) -0.018(3) C29 0.054(4) 0.034(3) 0.043(4) -0.001(3) 0.011(3) -0.017(3) O2 0.076(3) 0.064(3) 0.041(3) 0.004(2) 0.013(2) -0.027(3) C30 0.090(6) 0.082(5) 0.042(4) 0.004(4) 0.011(4) -0.030(5) O3 0.079(3) 0.055(3) 0.056(3) 0.002(2) 0.017(3) -0.033(3) C31 0.074(5) 0.061(4) 0.073(5) 0.009(4) 0.009(4) -0.039(4) N2 0.059(3) 0.028(2) 0.042(3) 0.002(2) 0.009(3) -0.023(2) C32 0.063(4) 0.040(3) 0.052(4) -0.002(3) 0.003(3) -0.033(3) C33 0.068(5) 0.036(3) 0.049(4) -0.001(3) 0.002(3) -0.026(3) C34 0.059(4) 0.040(3) 0.050(4) -0.009(3) 0.002(3) -0.024(3) C35 0.063(4) 0.037(3) 0.047(4) -0.006(3) 0.002(3) -0.025(3) C36 0.070(5) 0.042(3) 0.049(4) -0.008(3) -0.003(3) -0.023(3) C37 0.072(5) 0.042(3) 0.057(4) -0.008(3) -0.003(4) -0.030(3) C38 0.065(4) 0.041(3) 0.063(4) -0.006(3) 0.001(4) -0.033(3) O4 0.066(3) 0.042(2) 0.042(2) 0.0003(18) -0.005(2) -0.028(2) C39 0.082(5) 0.054(4) 0.063(5) -0.009(3) -0.009(4) -0.037(4) C40 0.096(6) 0.075(5) 0.088(6) -0.002(4) -0.017(5) -0.058(5) C41 0.121(8) 0.086(6) 0.094(6) -0.038(5) -0.005(6) -0.055(5) C42 0.090(6) 0.075(5) 0.090(6) -0.003(5) -0.026(5) -0.041(5) C43 0.066(4) 0.033(3) 0.031(3) -0.016(2) 0.007(3) -0.027(3) C44 0.062(4) 0.038(3) 0.031(3) -0.015(2) 0.007(3) -0.026(3) C45 0.066(4) 0.035(3) 0.038(3) -0.016(2) 0.005(3) -0.025(3) C46 0.068(4) 0.036(3) 0.036(3) -0.009(3) 0.014(3) -0.029(3) C47 0.068(4) 0.043(3) 0.044(4) -0.012(3) 0.009(3) -0.024(3) C48 0.069(4) 0.033(3) 0.039(3) -0.014(3) 0.005(3) -0.020(3) O5 0.062(3) 0.036(2) 0.054(3) -0.0226(19) 0.012(2) -0.0269(19) C49 0.075(3) 0.048(2) 0.077(2) -0.018(2) 0.024(3) -0.014(2) C50 0.115(12) 0.089(4) 0.137(5) -0.011(5) 0.066(9) -0.041(6) C51 0.128(8) 0.143(8) 0.111(7) -0.062(6) -0.017(6) -0.005(11) C52 0.103(13) 0.100(5) 0.109(11) -0.071(6) 0.032(9) -0.020(8) C53 0.049(6) 0.086(3) 0.111(9) -0.037(6) 0.022(8) -0.027(4) C54 0.088(8) 0.086(5) 0.143(7) -0.006(7) 0.030(7) 0.024(5) C55 0.094(11) 0.155(12) 0.128(7) -0.097(8) 0.037(7) -0.042(9) C56 0.068(4) 0.033(3) 0.040(3) -0.012(3) 0.005(3) -0.028(3) N3 0.072(4) 0.029(2) 0.060(3) -0.023(2) 0.015(3) -0.029(2) C57 0.093(6) 0.035(3) 0.062(4) -0.024(3) 0.008(4) -0.030(3) C58 0.082(5) 0.037(3) 0.062(4) -0.030(3) 0.011(4) -0.031(3) C59 0.095(6) 0.047(4) 0.080(5) -0.038(4) 0.015(4) -0.038(4) C60 0.105(7) 0.043(4) 0.159(9) -0.064(5) 0.027(6) -0.029(4) C61 0.096(6) 0.054(4) 0.179(9) -0.075(5) 0.043(6) -0.034(4) C62 0.085(6) 0.044(4) 0.133(7) -0.055(4) 0.024(5) -0.033(4) N4 0.072(4) 0.049(3) 0.125(6) -0.048(3) 0.033(4) -0.032(3) O6 0.116(4) 0.041(2) 0.088(4) -0.036(2) 0.012(3) -0.045(3) C63 0.102(7) 0.058(4) 0.106(6) -0.038(4) 0.007(5) -0.048(5) O7 0.108(2) 0.055(3) 0.240(8) -0.089(4) 0.028(3) -0.028(3) C64 0.139(5) 0.080(8) 0.122(10) -0.051(7) 0.002(8) -0.020(7) C65 0.108(6) 0.052(7) 0.128(9) -0.046(7) -0.003(6) -0.005(6) C66 0.096(7) 0.054(4) 0.157(9) -0.064(5) 0.038(6) -0.035(4) C67 0.082(6) 0.048(4) 0.117(7) -0.042(4) 0.039(5) -0.026(4) C68 0.062(5) 0.038(3) 0.101(6) -0.029(4) 0.020(4) -0.018(3) C69 0.068(5) 0.038(3) 0.058(4) -0.007(3) 0.009(4) -0.020(3) C70 0.065(5) 0.045(4) 0.081(5) -0.012(4) 0.008(4) -0.017(3) C71 0.079(6) 0.051(4) 0.090(6) -0.014(4) 0.018(5) -0.012(4) C72 0.086(6) 0.048(4) 0.136(8) -0.042(5) 0.037(6) -0.019(4) O8 0.064(3) 0.039(2) 0.102(4) -0.038(2) 0.023(3) -0.027(2) C73 0.074(3) 0.073(2) 0.115(2) -0.028(2) 0.023(3) -0.011(2) C74 0.087(10) 0.082(3) 0.123(7) -0.040(6) 0.015(8) 0.007(5) C75 0.118(7) 0.136(10) 0.122(5) -0.037(7) 0.002(8) -0.010(10) C76 0.100(11) 0.098(5) 0.159(15) -0.039(9) 0.046(10) -0.036(6) C77 0.153(12) 0.095(3) 0.180(13) -0.062(4) 0.049(11) 0.014(9) C78 0.102(9) 0.117(5) 0.101(4) -0.037(5) 0.020(7) 0.009(11) C79 0.075(10) 0.160(14) 0.152(12) -0.051(11) -0.015(9) 0.003(10) C80 0.084(5) 0.033(3) 0.035(3) -0.014(3) 0.004(3) -0.031(3) C81 0.087(5) 0.033(3) 0.031(3) -0.008(3) -0.002(3) -0.030(3) C82 0.109(6) 0.036(3) 0.033(3) -0.014(3) -0.001(3) -0.038(3) C83 0.126(7) 0.034(3) 0.043(4) -0.018(3) -0.005(4) -0.032(4) C84 0.131(7) 0.036(3) 0.036(4) -0.013(3) -0.013(4) -0.020(4) C85 0.111(6) 0.037(3) 0.031(3) -0.015(3) -0.000(3) -0.028(3) O9 0.085(3) 0.040(2) 0.038(2) -0.0185(18) -0.012(2) -0.027(2) C86 0.192(10) 0.044(4) 0.049(4) -0.021(3) -0.023(6) -0.009(5) C87 0.282(15) 0.039(4) 0.065(5) -0.020(4) -0.042(7) 0.004(6) C88 0.203(12) 0.070(5) 0.079(6) -0.040(5) -0.060(7) 0.029(6) C89 0.240(13) 0.049(4) 0.046(5) -0.004(4) 0.005(6) -0.040(6) C90 0.102(5) 0.035(3) 0.037(3) -0.015(3) -0.003(3) -0.036(3) N5 0.092(4) 0.042(3) 0.032(3) -0.016(2) -0.009(3) -0.036(3) C91 0.092(5) 0.040(3) 0.034(3) -0.014(3) -0.003(3) -0.039(3) C92 0.091(5) 0.048(3) 0.035(3) -0.014(3) -0.002(3) -0.040(3) C93 0.087(5) 0.052(4) 0.046(4) -0.020(3) -0.001(4) -0.039(4) C94 0.089(5) 0.070(4) 0.045(4) -0.033(3) 0.002(4) -0.046(4) C95 0.095(5) 0.055(4) 0.041(4) -0.011(3) -0.011(4) -0.040(4) C96 0.090(5) 0.051(4) 0.045(4) -0.026(3) -0.005(4) -0.039(4) O10 0.104(4) 0.065(3) 0.048(3) -0.034(2) 0.002(3) -0.032(3) C97 0.104(6) 0.067(4) 0.049(4) -0.031(4) 0.001(4) -0.025(4) O11 0.114(4) 0.079(3) 0.042(3) -0.029(2) -0.013(3) -0.033(3) C98 0.122(7) 0.090(6) 0.051(4) -0.035(4) -0.022(5) -0.022(5) N6 0.088(4) 0.042(3) 0.038(3) -0.008(2) -0.016(3) -0.034(3) C99 0.092(5) 0.049(4) 0.038(3) -0.015(3) -0.016(3) -0.033(4) C100 0.098(5) 0.038(3) 0.039(4) -0.003(3) -0.008(4) -0.036(3) C101 0.072(5) 0.035(3) 0.057(4) -0.014(3) -0.007(4) -0.031(3) C102 0.093(6) 0.034(3) 0.056(4) -0.001(3) -0.000(4) -0.031(4) C103 0.127(8) 0.043(4) 0.066(5) -0.000(4) 0.001(5) -0.015(4) C104 0.149(9) 0.045(4) 0.057(5) 0.011(4) -0.005(5) -0.020(5) C105 0.119(7) 0.049(4) 0.047(4) -0.004(3) -0.007(4) -0.031(4) O12 0.085(3) 0.043(2) 0.038(2) -0.0037(19) -0.011(2) -0.030(2) C106 0.155(2) 0.074(2) 0.084(2) 0.004(3) -0.015(2) 0.001(3) C107 0.169(7) 0.049(4) 0.128(5) 0.008(4) -0.018(6) 0.025(7) C108 0.150(3) 0.115(11) 0.113(12) 0.003(9) -0.015(5) -0.003(8) C109 0.150(8) 0.078(8) 0.064(4) 0.037(5) -0.027(6) 0.009(9) C110 0.199(3) 0.072(6) 0.128(10) -0.001(9) -0.051(11) -0.008(6) C111 0.184(5) 0.176(11) 0.146(9) -0.056(11) -0.009(11) 0.033(8) C112 0.163(17) 0.130(16) 0.107(7) -0.031(10) -0.027(8) 0.002(12) O13 0.094(6) 0.065(4) 0.056(4) -0.028(4) 0.005(4) -0.044(4) O14 0.051(8) 0.064(8) 0.046(8) 0.001(6) -0.003(6) -0.005(7) S1 0.113(4) 0.076(2) 0.110(3) -0.038(3) 0.016(3) -0.044(3) O15 0.199(9) 0.065(3) 0.203(12) -0.041(4) 0.018(12) -0.046(9) C113 0.10(2) 0.138(18) 0.109(4) -0.004(14) -0.004(8) -0.058(19) C114 0.167(16) 0.133(19) 0.136(8) -0.095(14) -0.061(12) 0.114(14) S2 0.134(4) 0.057(2) 0.114(3) -0.034(3) -0.009(4) -0.028(3) O16 0.206(17) 0.075(3) 0.173(11) -0.052(4) -0.035(15) -0.061(6) C115 0.104(11) 0.106(7) 0.087(5) -0.047(8) 0.013(8) -0.015(11) C116 0.101(17) 0.081(10) 0.118(9) -0.048(8) -0.021(10) -0.030(12) S3 0.131(2) 0.087(2) 0.130(3) -0.068(2) -0.063(2) 0.018(2) O17 0.1651(19) 0.079(6) 0.094(2) -0.041(3) -0.050(3) -0.013(4) C117 0.1543(17) 0.263(11) 0.177(5) -0.113(7) -0.000(3) -0.077(7) C118 0.189(13) 0.166(6) 0.119(9) 0.027(8) 0.019(9) 0.095(11) S4 0.128(7) 0.125(9) 0.103(5) -0.035(6) -0.033(7) -0.011(6) O18 0.1651(19) 0.079(6) 0.094(2) -0.041(3) -0.050(3) -0.013(4) C119 0.1543(17) 0.263(11) 0.177(5) -0.113(7) -0.000(3) -0.077(7) C120 0.123(7) 0.121(9) 0.107(3) -0.037(5) -0.059(3) -0.010(7) S5 0.0780(15) 0.1028(16) 0.0422(13) -0.0281(12) 0.0096(13) -0.0348(15) O19 0.0889(19) 0.117(4) 0.054(3) -0.015(3) -0.011(3) -0.028(3) C121 0.058(8) 0.1026(19) 0.065(9) -0.025(3) -0.001(6) -0.039(4) C122 0.082(5) 0.113(5) 0.053(5) -0.038(4) 0.011(4) -0.040(6) S6 0.084(4) 0.140(4) 0.040(6) -0.045(8) 0.005(5) -0.009(5) O20 0.0889(19) 0.117(4) 0.054(3) -0.015(3) -0.011(3) -0.028(3) C123 0.089(13) 0.114(3) 0.09(2) -0.034(9) -0.023(13) -0.019(7) C124 0.111(10) 0.117(10) 0.10(2) -0.051(16) -0.037(10) -0.012(10) S7 0.221(3) 0.082(2) 0.0648(18) -0.0173(14) 0.009(2) -0.079(2) O21 0.167(5) 0.082(5) 0.073(2) -0.005(3) 0.027(4) -0.068(5) C125 0.230(4) 0.178(11) 0.099(5) -0.067(7) 0.020(9) -0.056(11) C126 0.212(4) 0.170(15) 0.127(11) -0.077(10) -0.022(6) -0.032(8) Cl1 0.134(7) 0.049(5) 0.126(5) -0.031(4) 0.043(6) -0.019(6) Cl2 0.166(16) 0.085(7) 0.146(8) -0.024(7) 0.014(8) -0.058(10) C127 0.049(19) 0.065(17) 0.168(19) -0.035(7) 0.025(17) -0.005(15) Cl3 0.142(4) 0.075(18) 0.112(6) -0.034(12) -0.051(7) -0.040(14) Cl4 0.091(3) 0.111(19) 0.117(18) -0.042(16) 0.005(7) -0.008(14) C128 0.089(3) 0.088(5) 0.087(5) -0.032(3) -0.007(3) -0.008(3) Cl5 0.058(8) 0.061(4) 0.068(8) -0.035(5) -0.012(6) -0.007(6) Cl6 0.177(6) 0.141(17) 0.150(18) -0.007(12) 0.069(13) -0.047(16) C129 0.059(16) 0.082(9) 0.072(19) -0.009(12) -0.028(12) 0.003(17) Cl7 0.066(4) 0.086(3) 0.027(4) -0.017(4) 0.000(4) 0.014(4) Cl8 0.065(7) 0.082(3) 0.109(11) -0.047(6) 0.018(7) -0.041(5) C130 0.050(7) 0.057(5) 0.049(8) -0.019(6) -0.013(6) -0.009(4) Cl9 0.117(3) 0.065(3) 0.132(5) -0.007(4) 0.026(4) -0.030(4) Cl10 0.223(8) 0.082(3) 0.088(5) -0.049(3) -0.086(5) 0.044(5) C131 0.109(12) 0.090(6) 0.117(13) -0.083(10) 0.000(8) -0.025(10) Cl11 0.117(3) 0.065(3) 0.132(5) -0.007(4) 0.026(4) -0.030(4) Cl12 0.115(3) 0.079(17) 0.079(18) -0.025(14) 0.004(10) -0.022(8) C132 0.106(6) 0.110(7) 0.108(9) -0.036(6) -0.008(6) -0.012(5) Cl13 0.151(3) 0.091(5) 0.236(12) -0.073(6) -0.015(5) -0.017(5) Cl14 0.198(2) 0.119(3) 0.111(3) -0.043(3) 0.017(3) -0.062(3) C133 0.112(6) 0.064(11) 0.144(16) -0.041(10) -0.070(7) -0.011(5) Cl15 0.094(5) 0.187(11) 0.126(3) -0.032(7) -0.037(3) -0.025(6) Cl16 0.198(2) 0.119(3) 0.111(3) -0.043(3) 0.017(3) -0.062(3) C134 0.141(5) 0.137(8) 0.145(5) -0.050(6) -0.012(6) -0.001(5) Cl17 0.187(4) 0.176(3) 0.341(13) -0.126(6) -0.050(8) 0.029(5) Cl18 0.241(9) 0.149(3) 0.121(6) -0.014(4) -0.017(6) -0.036(5) C135 0.237(15) 0.173(10) 0.101(15) -0.034(11) -0.066(15) -0.009(10) Cl19 0.202(6) 0.246(3) 0.292(3) -0.071(4) 0.014(4) -0.032(5) Cl20 0.320(5) 0.155(8) 0.232(5) -0.081(7) -0.032(6) -0.067(8) C136 0.239(14) 0.260(10) 0.297(9) -0.073(9) -0.041(14) 0.004(17) Cl21 0.202(6) 0.246(3) 0.292(3) -0.071(4) 0.014(4) -0.032(5) Cl22 0.111(10) 0.198(14) 0.194(8) 0.040(9) -0.003(12) -0.002(18) C137 0.17(2) 0.220(7) 0.203(13) -0.021(9) 0.027(14) -0.003(19) Cl23 0.202(6) 0.246(3) 0.292(3) -0.071(4) 0.014(4) -0.032(5) Cl24 0.154(8) 0.297(13) 0.102(11) 0.056(8) -0.050(12) -0.100(15) C138 0.24(2) 0.24(2) 0.250(15) -0.083(17) -0.041(12) -0.026(16) Cl25 0.210(2) 0.57(3) 0.42(5) -0.34(4) -0.000(11) -0.16(2) Cl26 0.223(5) 0.164(15) 0.178(17) -0.115(14) -0.047(12) -0.011(17) C139 0.154(12) 0.13(2) 0.12(2) -0.028(17) -0.043(14) -0.021(15) Cl27 0.181(2) 0.128(18) 0.118(18) -0.066(14) -0.006(6) -0.055(14) Cl28 0.199(5) 0.25(3) 0.240(15) -0.085(19) -0.056(11) -0.07(2) C140 0.175(8) 0.15(2) 0.17(2) -0.065(16) 0.010(12) -0.032(18) Cl29 0.284(3) 0.21(2) 0.48(3) -0.153(19) 0.111(16) -0.106(18) C141 0.344(13) 0.344(14) 0.34(2) -0.140(15) -0.023(17) -0.036(16) Cl30 0.27(2) 0.158(18) 0.36(4) -0.157(18) 0.176(18) -0.058(19) Cl31 0.157(5) 0.094(3) 0.113(3) 0.031(3) -0.058(3) -0.038(3) Cl32 0.099(5) 0.299(12) 0.220(3) -0.092(5) 0.012(5) -0.030(7) C142 0.144(16) 0.116(14) 0.274(6) -0.012(10) -0.025(13) -0.017(12) Cl33 0.063(4) 0.123(2) 0.088(3) 0.004(3) -0.008(3) -0.026(4) Cl34 0.29(2) 0.130(3) 0.464(16) -0.128(6) -0.15(2) 0.086(10) C143 0.103(9) 0.132(4) 0.121(7) -0.022(5) -0.011(7) -0.006(7) Cl35 0.248(9) 0.186(12) 0.138(3) -0.068(7) 0.043(9) -0.149(10) Cl36 0.446(16) 0.31(2) 0.131(5) -0.062(13) 0.021(15) -0.17(2) C144 0.111(18) 0.13(2) 0.147(12) -0.040(13) 0.024(11) -0.020(16) Cl37 0.203(7) 0.268(14) 0.291(10) -0.13(2) -0.081(17) 0.02(3) Cl38 0.232(19) 0.151(10) 0.13(3) -0.03(2) -0.01(3) -0.070(18) C145 0.19(3) 0.21(2) 0.20(2) -0.069(18) -0.009(17) -0.031(18) Cl39 0.159(2) 0.115(5) 0.108(5) -0.023(4) 0.023(4) -0.062(4) Cl40 0.192(3) 0.262(6) 0.195(4) -0.062(6) 0.002(5) -0.123(6) C146 0.164(6) 0.115(11) 0.077(12) -0.034(10) 0.052(9) -0.038(8) Cl41 0.129(7) 0.136(10) 0.14(2) -0.094(14) 0.015(13) 0.006(12) Cl42 0.192(3) 0.262(6) 0.195(4) -0.062(6) 0.002(5) -0.123(6) C147 0.16(2) 0.15(2) 0.175(17) -0.060(17) 0.004(14) -0.019(16) C148 0.178(3) 0.142(3) 0.167(7) -0.030(7) -0.022(8) -0.043(4) C149 0.190(4) 0.231(3) 0.226(16) -0.078(9) -0.029(13) -0.070(6) C150 0.199(6) 0.171(3) 0.178(15) -0.019(8) -0.040(10) -0.074(7) C151 0.204(3) 0.186(3) 0.167(8) -0.013(9) 0.000(9) -0.114(6) C152 0.131(4) 0.152(6) 0.143(13) -0.035(10) 0.027(10) -0.046(6) C153 0.187(8) 0.120(5) 0.16(2) -0.045(8) -0.004(11) 0.006(8) C154 0.226(14) 0.250(2) 0.200(3) -0.084(3) -0.068(9) -0.079(9) C155 0.206(12) 0.247(3) 0.191(3) -0.073(5) -0.019(9) -0.093(11) C156 0.210(14) 0.259(4) 0.179(8) -0.084(5) -0.002(9) -0.043(11) C157 0.29(2) 0.231(3) 0.211(4) -0.126(5) -0.026(13) -0.022(15) C158 0.162(14) 0.214(4) 0.197(4) -0.069(7) 0.016(12) -0.094(12) C159 0.19(2) 0.241(9) 0.234(12) -0.085(7) -0.040(12) -0.086(13) C160 0.142(17) 0.190(3) 0.181(3) -0.068(3) -0.032(6) -0.008(8) C161 0.259(7) 0.257(6) 0.200(4) -0.124(3) -0.026(14) -0.028(9) C162 0.27(2) 0.222(8) 0.257(3) -0.146(6) 0.008(15) -0.014(12) C163 0.31(2) 0.222(3) 0.254(6) -0.120(5) 0.019(11) -0.020(12) C164 0.215(8) 0.192(10) 0.192(7) -0.076(6) 0.010(17) -0.010(12) C165 0.23(3) 0.237(15) 0.165(6) -0.087(7) -0.005(15) -0.048(17) C166 0.139(5) 0.124(3) 0.113(5) -0.031(4) -0.030(6) -0.020(6) C167 0.150(3) 0.133(3) 0.171(12) -0.063(5) -0.038(8) -0.030(6) C168 0.177(9) 0.104(2) 0.153(13) -0.042(5) -0.016(10) -0.012(7) C169 0.181(9) 0.095(3) 0.139(9) -0.055(6) -0.006(7) -0.006(7) C170 0.187(4) 0.130(8) 0.117(13) -0.063(8) 0.017(9) -0.040(9) C171 0.168(10) 0.114(5) 0.086(12) -0.035(6) -0.016(9) -0.008(10) C172 0.166(4) 0.155(6) 0.175(3) -0.058(4) -0.036(8) -0.001(10) C173 0.195(7) 0.169(4) 0.162(3) -0.055(13) -0.004(8) -0.019(13) C174 0.174(5) 0.172(7) 0.157(4) -0.042(8) -0.017(9) -0.010(14) C175 0.131(15) 0.184(8) 0.178(4) -0.050(11) -0.043(13) -0.013(14) C176 0.15(2) 0.158(5) 0.168(5) -0.055(17) -0.011(11) -0.020(13) C177 0.186(14) 0.166(12) 0.146(12) -0.068(12) -0.027(13) -0.004(19) C178 0.138(17) 0.131(3) 0.117(3) -0.030(2) -0.023(12) -0.041(10) C179 0.099(18) 0.120(3) 0.125(4) -0.024(3) -0.011(10) -0.033(14) C180 0.125(16) 0.120(3) 0.127(8) -0.041(6) -0.017(14) -0.016(11) C181 0.15(3) 0.098(4) 0.127(3) -0.029(4) -0.012(15) 0.008(13) C182 0.13(2) 0.120(6) 0.111(5) -0.038(4) 0.004(13) -0.025(16) C183 0.14(3) 0.118(9) 0.121(10) -0.024(8) -0.015(17) -0.023(16) C184 0.261(3) 0.220(2) 0.287(7) -0.121(4) 0.015(8) 0.015(7) C185 0.291(4) 0.219(3) 0.335(10) -0.105(6) -0.021(9) -0.041(9) C186 0.277(4) 0.218(3) 0.231(14) -0.068(6) 0.071(10) -0.021(7) C187 0.327(16) 0.249(3) 0.36(2) -0.093(4) -0.081(15) 0.043(10) C188 0.305(18) 0.258(9) 0.337(6) -0.113(11) -0.033(12) -0.001(12) C189 0.252(15) 0.173(9) 0.273(11) -0.126(10) 0.068(14) -0.003(10) C190 0.246(3) 0.256(10) 0.270(3) -0.109(9) -0.015(4) -0.053(8) C191 0.253(3) 0.27(2) 0.230(4) -0.080(7) -0.048(6) -0.032(10) C192 0.289(3) 0.278(9) 0.264(7) -0.126(9) 0.012(5) -0.052(17) C193 0.258(3) 0.22(2) 0.221(8) -0.086(14) 0.000(7) -0.002(13) C194 0.254(7) 0.33(3) 0.238(4) -0.087(11) 0.015(10) 0.006(13) C195 0.215(8) 0.18(2) 0.236(11) -0.052(14) -0.007(7) -0.06(2) C196 0.274(5) 0.246(18) 0.243(16) -0.048(9) 0.012(13) 0.012(17) C197 0.305(11) 0.142(12) 0.20(2) -0.039(14) -0.036(15) 0.046(14) C198 0.28(2) 0.28(2) 0.28(3) -0.072(19) 0.020(18) -0.06(2) C199 0.220(5) 0.192(4) 0.166(3) -0.079(3) -0.019(8) -0.022(8) C200 0.199(7) 0.165(6) 0.181(3) -0.067(5) -0.024(8) -0.005(8) C201 0.181(8) 0.189(10) 0.164(6) -0.074(5) -0.042(11) -0.005(10) C202 0.221(6) 0.181(4) 0.202(9) -0.079(6) 0.006(11) -0.021(12) C203 0.19(2) 0.199(7) 0.179(9) -0.074(11) -0.006(12) -0.008(13) C204 0.18(2) 0.147(19) 0.192(12) -0.056(9) -0.023(15) 0.016(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O4 1.840(4) . ? Ni1 O1 1.854(4) . ? Ni1 N1 1.857(5) . ? Ni1 N2 1.863(5) . ? Ni2 O5 1.832(4) . ? Ni2 O8 1.840(4) . ? Ni2 N4 1.848(6) . ? Ni2 N3 1.867(5) . ? Ni3 O12 1.832(5) . ? Ni3 N5 1.841(5) . ? Ni3 O9 1.842(4) . ? Ni3 N6 1.858(5) . ? C1 C2 1.389(7) . ? C1 C6 1.398(7) . ? C1 C13 1.491(8) . ? C2 C3 1.389(8) . ? C2 H1 0.9500 . ? C3 C4 1.393(7) . ? C3 C43 1.496(7) . ? C4 C5 1.385(7) . ? C4 H2 0.9500 . ? C5 C6 1.387(8) . ? C5 C80 1.500(7) . ? C6 H3 0.9500 . ? C7 C12 1.361(9) . ? C7 C8 1.399(9) . ? C7 C35 1.501(7) . ? C8 C9 1.396(8) . ? C8 H4 0.9500 . ? C9 C10 1.381(9) . ? C9 C69 1.491(9) . ? C10 C11 1.392(9) . ? C10 H5 0.9500 . ? C11 C12 1.412(8) . ? C11 C102 1.486(9) . ? C12 H6 0.9500 . ? C13 C18 1.393(8) . ? C13 C14 1.417(8) . ? C14 O1 1.302(7) . ? C14 C15 1.401(8) . ? C15 C16 1.418(9) . ? C15 C23 1.434(8) . ? C16 C17 1.380(9) . ? C16 H7 0.9500 . ? C17 C18 1.407(8) . ? C17 C19 1.544(9) . ? C18 H8 0.9500 . ? C19 C21 1.465(11) . ? C19 C20 1.500(12) . ? C19 C22 1.508(10) . ? C20 H9 0.9800 . ? C20 H10 0.9800 . ? C20 H11 0.9800 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C23 N1 1.292(8) . ? C23 H18 0.9500 . ? N1 C24 1.432(7) . ? C24 C29 1.373(9) . ? C24 C25 1.403(8) . ? C25 C26 1.386(8) . ? C25 H19 0.9500 . ? C26 O2 1.353(7) . ? C26 C27 1.394(10) . ? C27 C28 1.370(9) . ? C27 O3 1.372(7) . ? C28 C29 1.403(8) . ? C28 H20 0.9500 . ? C29 N2 1.413(7) . ? O2 C30 1.408(9) . ? C30 H21 0.9800 . ? C30 H22 0.9800 . ? C30 H23 0.9800 . ? O3 C31 1.433(9) . ? C31 H24 0.9800 . ? C31 H25 0.9800 . ? C31 H26 0.9800 . ? N2 C32 1.286(8) . ? C32 C33 1.415(9) . ? C32 H27 0.9500 . ? C33 C38 1.426(9) . ? C33 C34 1.426(8) . ? C34 O4 1.296(7) . ? C34 C35 1.424(9) . ? C35 C36 1.380(9) . ? C36 C37 1.420(8) . ? C36 H28 0.9500 . ? C37 C38 1.345(9) . ? C37 C39 1.532(9) . ? C38 H29 0.9500 . ? C39 C42 1.506(11) . ? C39 C41 1.518(11) . ? C39 C40 1.538(9) . ? C40 H30 0.9800 . ? C40 H31 0.9800 . ? C40 H32 0.9800 . ? C41 H33 0.9800 . ? C41 H34 0.9800 . ? C41 H35 0.9800 . ? C42 H36 0.9800 . ? C42 H37 0.9800 . ? C42 H38 0.9800 . ? C43 C48 1.365(8) . ? C43 C44 1.419(8) . ? C44 O5 1.287(7) . ? C44 C45 1.433(7) . ? C45 C46 1.397(8) . ? C45 C56 1.408(8) . ? C46 C47 1.368(8) . ? C46 H39 0.9500 . ? C47 C48 1.425(8) . ? C47 C49 1.521(10) . ? C48 H40 0.9500 . ? C49 C54 1.406(18) . ? C49 C53 1.487(19) . ? C49 C52 1.507(19) . ? C49 C50 1.52(3) . ? C49 C55 1.584(19) . ? C49 C51 1.76(3) . ? C50 H41 0.9800 . ? C50 H42 0.9800 . ? C50 H43 0.9800 . ? C51 H44 0.9800 . ? C51 H45 0.9800 . ? C51 H46 0.9800 . ? C52 H47 0.9800 . ? C52 H48 0.9800 . ? C52 H49 0.9800 . ? C53 H50 0.9800 . ? C53 H51 0.9800 . ? C53 H52 0.9800 . ? C54 H53 0.9800 . ? C54 H54 0.9800 . ? C54 H55 0.9800 . ? C55 H56 0.9800 . ? C55 H57 0.9800 . ? C55 H58 0.9800 . ? C56 N3 1.287(8) . ? C56 H59 0.9500 . ? N3 C57 1.412(7) . ? C57 C62 1.373(10) . ? C57 C58 1.400(8) . ? C58 C59 1.381(9) . ? C58 H60 0.9500 . ? C59 C60 1.372(11) . ? C59 O6 1.384(7) . ? C60 O7 1.357(8) . ? C60 C61 1.391(10) . ? C61 C62 1.412(9) . ? C61 H61 0.9500 . ? C62 N4 1.432(8) . ? N4 C66 1.298(10) . ? O6 C63 1.416(9) . ? C63 H62 0.9800 . ? C63 H63 0.9800 . ? C63 H64 0.9800 . ? O7 C65 1.445(19) . ? O7 C64 1.52(2) . ? C64 H65 0.9800 . ? C64 H66 0.9800 . ? C64 H67 0.9800 . ? C65 H68 0.9800 . ? C65 H69 0.9800 . ? C65 H70 0.9800 . ? C66 C67 1.421(10) . ? C66 H71 0.9500 . ? C67 C72 1.396(10) . ? C67 C68 1.424(9) . ? C68 O8 1.300(8) . ? C68 C69 1.436(9) . ? C69 C70 1.374(10) . ? C70 C71 1.414(10) . ? C70 H72 0.9500 . ? C71 C72 1.389(10) . ? C71 C73 1.519(11) . ? C72 H73 0.9500 . ? C73 C74 1.42(2) . ? C73 C78 1.46(2) . ? C73 C76 1.49(2) . ? C73 C77 1.50(2) . ? C73 C79 1.65(2) . ? C73 C75 1.65(3) . ? C74 H74 0.9800 . ? C74 H75 0.9800 . ? C74 H76 0.9800 . ? C75 H77 0.9800 . ? C75 H78 0.9800 . ? C75 H79 0.9800 . ? C76 H80 0.9800 . ? C76 H81 0.9800 . ? C76 H82 0.9800 . ? C77 H83 0.9800 . ? C77 H84 0.9800 . ? C77 H85 0.9800 . ? C78 H86 0.9800 . ? C78 H87 0.9800 . ? C78 H88 0.9800 . ? C79 H89 0.9800 . ? C79 H90 0.9800 . ? C79 H91 0.9800 . ? C80 C85 1.357(8) . ? C80 C81 1.429(8) . ? C81 O9 1.291(7) . ? C81 C82 1.420(8) . ? C82 C83 1.397(9) . ? C82 C90 1.429(8) . ? C83 C84 1.368(8) . ? C83 H92 0.9500 . ? C84 C85 1.407(8) . ? C84 C86 1.522(10) . ? C85 H93 0.9500 . ? C86 C88 1.533(14) . ? C86 C89 1.536(13) . ? C86 C87 1.553(10) . ? C87 H94 0.9800 . ? C87 H95 0.9800 . ? C87 H96 0.9800 . ? C88 H97 0.9800 . ? C88 H98 0.9800 . ? C88 H99 0.9800 . ? C89 H100 0.9800 . ? C89 H101 0.9800 . ? C89 H102 0.9800 . ? C90 N5 1.300(8) . ? C90 H103 0.9500 . ? N5 C91 1.439(7) . ? C91 C96 1.365(9) . ? C91 C92 1.390(9) . ? C92 C93 1.387(8) . ? C92 H104 0.9500 . ? C93 O10 1.346(8) . ? C93 C94 1.407(10) . ? C94 C95 1.372(10) . ? C94 O11 1.374(7) . ? C95 C96 1.415(9) . ? C95 H105 0.9500 . ? C96 N6 1.411(8) . ? O10 C97 1.415(8) . ? C97 H106 0.9800 . ? C97 H107 0.9800 . ? C97 H108 0.9800 . ? O11 C98 1.423(9) . ? C98 H109 0.9800 . ? C98 H110 0.9800 . ? C98 H111 0.9800 . ? N6 C99 1.283(8) . ? C99 C100 1.401(9) . ? C99 H112 0.9500 . ? C100 C105 1.404(9) . ? C100 C101 1.437(9) . ? C101 O12 1.299(7) . ? C101 C102 1.410(10) . ? C102 C103 1.379(10) . ? C103 C104 1.414(11) . ? C103 H113 0.9500 . ? C104 C105 1.364(11) . ? C104 C106 1.527(11) . ? C105 H114 0.9500 . ? C106 C112 1.40(3) . ? C106 C107 1.47(2) . ? C106 C108 1.51(2) . ? C106 C109 1.57(2) . ? C106 C110 1.65(3) . ? C106 C111 1.70(4) . ? C107 H115 0.9800 . ? C107 H116 0.9800 . ? C107 H117 0.9800 . ? C108 H118 0.9800 . ? C108 H119 0.9800 . ? C108 H120 0.9800 . ? C109 H121 0.9800 . ? C109 H122 0.9800 . ? C109 H123 0.9800 . ? C110 H124 0.9800 . ? C110 H125 0.9800 . ? C110 H126 0.9800 . ? C111 H127 0.9800 . ? C111 H128 0.9800 . ? C111 H129 0.9800 . ? C112 H130 0.9800 . ? C112 H131 0.9800 . ? C112 H132 0.9800 . ? O13 H133 0.851(17) . ? O13 H134 0.83(2) . ? O14 H135 0.855(19) . ? O14 H136 0.84(2) . ? S1 O15 1.461(14) . ? S1 C113 1.819(18) . ? S1 C114 1.825(19) . ? C113 H137 0.9800 . ? C113 H138 0.9800 . ? C113 H139 0.9800 . ? C114 H140 0.9800 . ? C114 H141 0.9800 . ? C114 H142 0.9800 . ? S2 O16 1.493(14) . ? S2 C116 1.818(18) . ? S2 C115 1.838(19) . ? C115 H143 0.9800 . ? C115 H144 0.9800 . ? C115 H145 0.9800 . ? C116 H146 0.9800 . ? C116 H147 0.9800 . ? C116 H148 0.9800 . ? S3 O17 1.456(9) . ? S3 C118 1.764(15) . ? S3 C117 1.916(12) . ? C117 H149 0.9800 . ? C117 H150 0.9800 . ? C117 H151 0.9800 . ? C118 H152 0.9800 . ? C118 H153 0.9800 . ? C118 H154 0.9800 . ? S4 C120 1.820(19) . ? C120 H158 0.9800 . ? C120 H159 0.9800 . ? C120 H160 0.9800 . ? S5 O19 1.514(7) . ? S5 C121 1.738(11) . ? S5 C122 1.762(10) . ? C121 H161 0.9800 . ? C121 H162 0.9800 . ? C121 H163 0.9800 . ? C122 H164 0.9800 . ? C122 H165 0.9800 . ? C122 H166 0.9800 . ? S6 C124 1.828(19) . ? S6 C123 1.84(2) . ? C123 H167 0.9800 . ? C123 H168 0.9800 . ? C123 H169 0.9800 . ? C124 H170 0.9800 . ? C124 H171 0.9800 . ? C124 H172 0.9800 . ? S7 O21 1.478(9) . ? S7 C126 1.786(16) . ? S7 C125 1.808(15) . ? C125 H173 0.9800 . ? C125 H174 0.9800 . ? C125 H175 0.9800 . ? C126 H176 0.9800 . ? C126 H177 0.9800 . ? C126 H178 0.9800 . ? Cl1 C127 1.779(19) . ? Cl2 C127 1.776(18) . ? C127 H179 0.9900 . ? C127 H180 0.9900 . ? Cl3 C128 1.78(2) . ? Cl4 C128 1.78(2) . ? C128 H181 0.9900 . ? C128 H182 0.9900 . ? Cl5 C129 1.78(2) . ? Cl6 C129 1.79(2) . ? C129 H183 0.9900 . ? C129 H184 0.9900 . ? Cl7 C130 1.795(17) . ? Cl8 C130 1.793(18) . ? C130 H185 0.9900 . ? C130 H186 0.9900 . ? Cl9 C131 1.776(18) . ? Cl10 C131 1.817(16) . ? C131 H187 0.9900 . ? C131 H188 0.9900 . ? Cl12 C132 1.79(2) . ? C132 H189 0.9900 . ? C132 H190 0.9900 . ? Cl13 C133 1.717(17) . ? Cl14 C133 1.765(16) . ? C133 H191 0.9900 . ? C133 H192 0.9900 . ? Cl15 C134 1.771(19) . ? C134 H193 0.9900 . ? C134 H194 0.9900 . ? Cl17 C135 1.667(17) . ? Cl18 C135 1.789(17) . ? C135 H195 0.9900 . ? C135 H196 0.9900 . ? Cl19 C136 1.772(19) . ? Cl20 C136 1.739(19) . ? C136 H197 0.9900 . ? C136 H198 0.9900 . ? Cl22 C137 1.78(2) . ? C137 H199 0.9900 . ? C137 H200 0.9900 . ? Cl24 C138 1.77(2) . ? C138 H201 0.9900 . ? C138 H202 0.9900 . ? Cl25 C139 1.77(2) . ? Cl26 C139 1.78(2) . ? C139 H203 0.9900 . ? C139 H204 0.9900 . ? Cl27 C140 1.78(2) . ? Cl28 C140 1.79(2) . ? C140 H205 0.9900 . ? C140 H206 0.9900 . ? Cl29 C141 1.79(2) . ? C141 Cl30 1.78(2) . ? C141 H207 0.9900 . ? C141 H208 0.9900 . ? Cl31 C142 1.801(18) . ? Cl32 C142 1.718(17) . ? C142 H209 0.9900 . ? C142 H210 0.9900 . ? Cl33 C143 1.691(18) . ? Cl34 C143 1.691(17) . ? C143 H211 0.9900 . ? C143 H212 0.9900 . ? Cl35 C144 1.741(19) . ? Cl36 C144 1.773(19) . ? C144 H213 0.9900 . ? C144 H214 0.9900 . ? Cl37 C145 1.78(2) . ? Cl38 C145 1.78(2) . ? C145 H215 0.9900 . ? C145 H216 0.9900 . ? Cl39 C146 1.740(17) . ? Cl40 C146 1.762(17) . ? C146 H217 0.9900 . ? C146 H218 0.9900 . ? Cl41 C147 1.78(2) . ? C147 H219 0.9900 . ? C147 H220 0.9900 . ? C148 C153 1.506(17) . ? C148 C149 1.579(17) . ? C148 H221 0.9900 . ? C148 H222 0.9900 . ? C149 C150 1.559(17) . ? C149 H223 0.9900 . ? C149 H224 0.9900 . ? C150 C151 1.537(17) . ? C150 H225 0.9900 . ? C150 H226 0.9900 . ? C151 C152 1.508(18) . ? C151 H227 0.9900 . ? C151 H228 0.9900 . ? C152 C153 1.635(17) . ? C152 H229 0.9900 . ? C152 H230 0.9900 . ? C153 H231 0.9900 . ? C153 H232 0.9900 . ? C154 C159 1.526(17) . ? C154 C155 1.536(16) . ? C154 H233 0.9900 . ? C154 H234 0.9900 . ? C155 C156 1.562(17) . ? C155 H235 0.9900 . ? C155 H236 0.9900 . ? C156 C157 1.549(18) . ? C156 H237 0.9900 . ? C156 H238 0.9900 . ? C157 C158 1.517(16) . ? C157 H239 0.9900 . ? C157 H240 0.9900 . ? C158 C159 1.527(17) . ? C158 H241 0.9900 . ? C158 H242 0.9900 . ? C159 H243 0.9900 . ? C159 H244 0.9900 . ? C160 C165 1.545(19) . ? C160 C161 1.577(18) . ? C160 H245 0.9900 . ? C160 H246 0.9900 . ? C161 C162 1.554(19) . ? C161 H247 0.9900 . ? C161 H248 0.9900 . ? C162 C163 1.560(19) . ? C162 H249 0.9900 . ? C162 H250 0.9900 . ? C163 C164 1.546(18) . ? C163 H251 0.9900 . ? C163 H252 0.9900 . ? C164 C165 1.553(19) . ? C164 H253 0.9900 . ? C164 H254 0.9900 . ? C165 H255 0.9900 . ? C165 H256 0.9900 . ? C166 C171 1.521(15) . ? C166 C167 1.525(17) . ? C166 H257 0.9900 . ? C166 H258 0.9900 . ? C167 C168 1.525(16) . ? C167 H259 0.9900 . ? C167 H260 0.9900 . ? C168 C169 1.526(16) . ? C168 H261 0.9900 . ? C168 H262 0.9900 . ? C169 C170 1.508(16) . ? C169 H263 0.9900 . ? C169 H264 0.9900 . ? C170 C171 1.574(16) . ? C170 H265 0.9900 . ? C170 H266 0.9900 . ? C171 H267 0.9900 . ? C171 H268 0.9900 . ? C172 C177 1.54(2) . ? C172 C173 1.551(19) . ? C172 H269 0.9900 . ? C172 H270 0.9900 . ? C173 C174 1.546(19) . ? C173 H271 0.9900 . ? C173 H272 0.9900 . ? C174 C175 1.528(19) . ? C174 H273 0.9900 . ? C174 H274 0.9900 . ? C175 C176 1.535(19) . ? C175 H275 0.9900 . ? C175 H276 0.9900 . ? C176 C177 1.553(19) . ? C176 H277 0.9900 . ? C176 H278 0.9900 . ? C177 H279 0.9900 . ? C177 H280 0.9900 . ? C178 C179 1.523(19) . ? C178 C183 1.527(19) . ? C178 H281 0.9900 . ? C178 H282 0.9900 . ? C179 C180 1.537(19) . ? C179 H283 0.9900 . ? C179 H284 0.9900 . ? C180 C181 1.525(19) . ? C180 H285 0.9900 . ? C180 H286 0.9900 . ? C181 C182 1.530(19) . ? C181 H287 0.9900 . ? C181 H288 0.9900 . ? C182 C183 1.532(19) . ? C182 H289 0.9900 . ? C182 H290 0.9900 . ? C183 H291 0.9900 . ? C183 H292 0.9900 . ? C184 C185 1.531(16) . ? C184 C189 1.537(17) . ? C184 H293 0.9900 . ? C184 H294 0.9900 . ? C185 C186 1.470(17) . ? C185 H295 0.9900 . ? C185 H296 0.9900 . ? C186 C187 1.489(17) . ? C186 H297 0.9900 . ? C186 H298 0.9900 . ? C187 C188 1.592(18) . ? C187 H299 0.9900 . ? C187 H300 0.9900 . ? C188 C189 1.523(18) . ? C188 H301 0.9900 . ? C188 H302 0.9900 . ? C189 H303 0.9900 . ? C189 H304 0.9900 . ? C190 C195 1.522(19) . ? C190 C191 1.556(19) . ? C190 H305 0.9900 . ? C190 H306 0.9900 . ? C191 C192 1.561(19) . ? C191 H307 0.9900 . ? C191 H308 0.9900 . ? C192 C193 1.545(19) . ? C192 H309 0.9900 . ? C192 H310 0.9900 . ? C193 C194 1.513(19) . ? C193 H311 0.9900 . ? C193 H312 0.9900 . ? C194 C195 1.546(19) . ? C194 H313 0.9900 . ? C194 H314 0.9900 . ? C195 H315 0.9900 . ? C195 H316 0.9900 . ? C196 C197 1.536(18) . ? C196 C198 1.553(18) 2 ? C196 H317 0.9900 . ? C196 H318 0.9900 . ? C197 C198 1.533(18) . ? C197 H319 0.9900 . ? C197 H320 0.9900 . ? C198 C196 1.553(18) 2 ? C198 H321 0.9900 . ? C198 H322 0.9900 . ? C199 C200 1.530(19) . ? C199 C204 1.532(19) . ? C199 H323 0.9900 . ? C199 H324 0.9900 . ? C200 C201 1.553(19) . ? C200 H325 0.9900 . ? C200 H326 0.9900 . ? C201 C202 1.534(19) . ? C201 H327 0.9900 . ? C201 H328 0.9900 . ? C202 C203 1.54(2) . ? C202 H329 0.9900 . ? C202 H330 0.9900 . ? C203 C204 1.54(2) . ? C203 H331 0.9900 . ? C203 H332 0.9900 . ? C204 H333 0.9900 . ? C204 H334 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ni1 O1 85.65(18) . . ? O4 Ni1 N1 171.4(2) . . ? O1 Ni1 N1 94.6(2) . . ? O4 Ni1 N2 94.7(2) . . ? O1 Ni1 N2 171.5(2) . . ? N1 Ni1 N2 86.3(2) . . ? O5 Ni2 O8 85.75(19) . . ? O5 Ni2 N4 172.3(3) . . ? O8 Ni2 N4 94.2(2) . . ? O5 Ni2 N3 94.7(2) . . ? O8 Ni2 N3 171.3(2) . . ? N4 Ni2 N3 86.5(2) . . ? O12 Ni3 N5 171.3(2) . . ? O12 Ni3 O9 85.54(19) . . ? N5 Ni3 O9 94.6(2) . . ? O12 Ni3 N6 95.0(2) . . ? N5 Ni3 N6 86.1(2) . . ? O9 Ni3 N6 172.1(2) . . ? C2 C1 C6 117.9(5) . . ? C2 C1 C13 121.7(5) . . ? C6 C1 C13 120.2(5) . . ? C1 C2 C3 122.1(5) . . ? C1 C2 H1 119.0 . . ? C3 C2 H1 119.0 . . ? C2 C3 C4 118.4(5) . . ? C2 C3 C43 120.9(5) . . ? C4 C3 C43 120.4(5) . . ? C5 C4 C3 121.2(5) . . ? C5 C4 H2 119.4 . . ? C3 C4 H2 119.4 . . ? C4 C5 C6 119.1(5) . . ? C4 C5 C80 119.6(5) . . ? C6 C5 C80 121.0(5) . . ? C5 C6 C1 121.3(5) . . ? C5 C6 H3 119.4 . . ? C1 C6 H3 119.4 . . ? C12 C7 C8 120.0(5) . . ? C12 C7 C35 121.9(6) . . ? C8 C7 C35 117.8(6) . . ? C9 C8 C7 119.9(6) . . ? C9 C8 H4 120.1 . . ? C7 C8 H4 120.1 . . ? C10 C9 C8 119.1(6) . . ? C10 C9 C69 120.9(5) . . ? C8 C9 C69 119.7(6) . . ? C9 C10 C11 122.0(5) . . ? C9 C10 H5 119.0 . . ? C11 C10 H5 119.0 . . ? C10 C11 C12 117.4(6) . . ? C10 C11 C102 121.9(5) . . ? C12 C11 C102 120.4(6) . . ? C7 C12 C11 121.5(6) . . ? C7 C12 H6 119.2 . . ? C11 C12 H6 119.2 . . ? C18 C13 C14 119.4(5) . . ? C18 C13 C1 118.2(5) . . ? C14 C13 C1 122.2(5) . . ? O1 C14 C15 123.4(5) . . ? O1 C14 C13 118.7(5) . . ? C15 C14 C13 117.9(5) . . ? C14 C15 C16 120.5(5) . . ? C14 C15 C23 121.9(6) . . ? C16 C15 C23 117.3(5) . . ? C17 C16 C15 122.2(6) . . ? C17 C16 H7 118.9 . . ? C15 C16 H7 118.9 . . ? C16 C17 C18 116.2(6) . . ? C16 C17 C19 123.5(5) . . ? C18 C17 C19 120.3(6) . . ? C13 C18 C17 123.5(6) . . ? C13 C18 H8 118.3 . . ? C17 C18 H8 118.3 . . ? C14 O1 Ni1 127.4(4) . . ? C21 C19 C20 110.3(9) . . ? C21 C19 C22 111.3(8) . . ? C20 C19 C22 104.1(9) . . ? C21 C19 C17 109.1(7) . . ? C20 C19 C17 110.5(6) . . ? C22 C19 C17 111.5(6) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? N1 C23 C15 124.9(6) . . ? N1 C23 H18 117.6 . . ? C15 C23 H18 117.6 . . ? C23 N1 C24 122.4(5) . . ? C23 N1 Ni1 125.4(4) . . ? C24 N1 Ni1 112.1(4) . . ? C29 C24 C25 120.9(5) . . ? C29 C24 N1 114.5(5) . . ? C25 C24 N1 124.5(6) . . ? C26 C25 C24 118.8(6) . . ? C26 C25 H19 120.6 . . ? C24 C25 H19 120.6 . . ? O2 C26 C25 124.9(7) . . ? O2 C26 C27 115.3(6) . . ? C25 C26 C27 119.7(6) . . ? C28 C27 O3 124.2(7) . . ? C28 C27 C26 121.5(6) . . ? O3 C27 C26 114.3(6) . . ? C27 C28 C29 118.9(7) . . ? C27 C28 H20 120.6 . . ? C29 C28 H20 120.6 . . ? C24 C29 C28 120.1(6) . . ? C24 C29 N2 114.2(5) . . ? C28 C29 N2 125.7(6) . . ? C26 O2 C30 117.3(5) . . ? O2 C30 H21 109.5 . . ? O2 C30 H22 109.5 . . ? H21 C30 H22 109.5 . . ? O2 C30 H23 109.5 . . ? H21 C30 H23 109.5 . . ? H22 C30 H23 109.5 . . ? C27 O3 C31 117.5(5) . . ? O3 C31 H24 109.5 . . ? O3 C31 H25 109.5 . . ? H24 C31 H25 109.5 . . ? O3 C31 H26 109.5 . . ? H24 C31 H26 109.5 . . ? H25 C31 H26 109.5 . . ? C32 N2 C29 121.9(5) . . ? C32 N2 Ni1 124.9(4) . . ? C29 N2 Ni1 112.9(4) . . ? N2 C32 C33 126.5(5) . . ? N2 C32 H27 116.7 . . ? C33 C32 H27 116.7 . . ? C32 C33 C38 119.2(5) . . ? C32 C33 C34 120.7(6) . . ? C38 C33 C34 120.1(6) . . ? O4 C34 C35 119.8(5) . . ? O4 C34 C33 123.6(6) . . ? C35 C34 C33 116.6(6) . . ? C36 C35 C34 119.8(5) . . ? C36 C35 C7 119.7(6) . . ? C34 C35 C7 120.4(5) . . ? C35 C36 C37 123.4(6) . . ? C35 C36 H28 118.3 . . ? C37 C36 H28 118.3 . . ? C38 C37 C36 116.6(6) . . ? C38 C37 C39 124.1(5) . . ? C36 C37 C39 119.2(6) . . ? C37 C38 C33 122.8(5) . . ? C37 C38 H29 118.6 . . ? C33 C38 H29 118.6 . . ? C34 O4 Ni1 127.9(4) . . ? C42 C39 C41 109.5(7) . . ? C42 C39 C37 109.8(6) . . ? C41 C39 C37 109.4(7) . . ? C42 C39 C40 107.8(7) . . ? C41 C39 C40 108.8(6) . . ? C37 C39 C40 111.5(6) . . ? C39 C40 H30 109.5 . . ? C39 C40 H31 109.5 . . ? H30 C40 H31 109.5 . . ? C39 C40 H32 109.5 . . ? H30 C40 H32 109.5 . . ? H31 C40 H32 109.5 . . ? C39 C41 H33 109.5 . . ? C39 C41 H34 109.5 . . ? H33 C41 H34 109.5 . . ? C39 C41 H35 109.5 . . ? H33 C41 H35 109.5 . . ? H34 C41 H35 109.5 . . ? C39 C42 H36 109.5 . . ? C39 C42 H37 109.5 . . ? H36 C42 H37 109.5 . . ? C39 C42 H38 109.5 . . ? H36 C42 H38 109.5 . . ? H37 C42 H38 109.5 . . ? C48 C43 C44 119.9(5) . . ? C48 C43 C3 119.9(5) . . ? C44 C43 C3 120.1(5) . . ? O5 C44 C43 120.4(5) . . ? O5 C44 C45 123.1(5) . . ? C43 C44 C45 116.5(6) . . ? C46 C45 C56 118.0(5) . . ? C46 C45 C44 120.6(5) . . ? C56 C45 C44 121.4(6) . . ? C47 C46 C45 122.9(5) . . ? C47 C46 H39 118.5 . . ? C45 C46 H39 118.5 . . ? C46 C47 C48 115.5(6) . . ? C46 C47 C49 123.3(5) . . ? C48 C47 C49 121.1(6) . . ? C43 C48 C47 124.1(6) . . ? C43 C48 H40 118.0 . . ? C47 C48 H40 118.0 . . ? C44 O5 Ni2 128.0(3) . . ? C54 C49 C53 108.8(13) . . ? C54 C49 C52 63.0(13) . . ? C53 C49 C52 132.0(12) . . ? C54 C49 C47 113.1(9) . . ? C53 C49 C47 110.8(9) . . ? C52 C49 C47 115.7(10) . . ? C54 C49 C50 121.7(16) . . ? C53 C49 C50 23.4(16) . . ? C52 C49 C50 117.2(16) . . ? C47 C49 C50 115.8(13) . . ? C54 C49 C55 110.4(14) . . ? C53 C49 C55 108.0(11) . . ? C52 C49 C55 48.4(11) . . ? C47 C49 C55 105.7(9) . . ? C50 C49 C55 84.9(15) . . ? C54 C49 C51 37.6(12) . . ? C53 C49 C51 81.9(12) . . ? C52 C49 C51 100.5(14) . . ? C47 C49 C51 100.5(10) . . ? C50 C49 C51 103.0(17) . . ? C55 C49 C51 146.0(13) . . ? C49 C50 H41 109.5 . . ? C49 C50 H42 109.5 . . ? H41 C50 H42 109.5 . . ? C49 C50 H43 109.5 . . ? H41 C50 H43 109.5 . . ? H42 C50 H43 109.5 . . ? C49 C51 H44 109.5 . . ? C49 C51 H45 109.5 . . ? H44 C51 H45 109.5 . . ? C49 C51 H46 109.5 . . ? H44 C51 H46 109.5 . . ? H45 C51 H46 109.5 . . ? C49 C52 H47 109.5 . . ? C49 C52 H48 109.5 . . ? H47 C52 H48 109.5 . . ? C49 C52 H49 109.5 . . ? H47 C52 H49 109.5 . . ? H48 C52 H49 109.5 . . ? C49 C53 H50 109.5 . . ? C49 C53 H51 109.5 . . ? H50 C53 H51 109.5 . . ? C49 C53 H52 109.5 . . ? H50 C53 H52 109.5 . . ? H51 C53 H52 109.5 . . ? C49 C54 H53 109.5 . . ? C49 C54 H54 109.5 . . ? H53 C54 H54 109.5 . . ? C49 C54 H55 109.5 . . ? H53 C54 H55 109.5 . . ? H54 C54 H55 109.5 . . ? C49 C55 H56 109.5 . . ? C49 C55 H57 109.5 . . ? H56 C55 H57 109.5 . . ? C49 C55 H58 109.5 . . ? H56 C55 H58 109.5 . . ? H57 C55 H58 109.5 . . ? N3 C56 C45 125.8(5) . . ? N3 C56 H59 117.1 . . ? C45 C56 H59 117.1 . . ? C56 N3 C57 122.4(5) . . ? C56 N3 Ni2 124.6(4) . . ? C57 N3 Ni2 112.5(5) . . ? C62 C57 C58 120.8(6) . . ? C62 C57 N3 114.3(5) . . ? C58 C57 N3 124.9(7) . . ? C59 C58 C57 117.7(7) . . ? C59 C58 H60 121.1 . . ? C57 C58 H60 121.1 . . ? C60 C59 C58 122.1(6) . . ? C60 C59 O6 114.8(6) . . ? C58 C59 O6 123.1(7) . . ? O7 C60 C59 115.9(7) . . ? O7 C60 C61 123.5(8) . . ? C59 C60 C61 120.6(7) . . ? C60 C61 C62 117.7(8) . . ? C60 C61 H61 121.2 . . ? C62 C61 H61 121.2 . . ? C57 C62 C61 120.9(6) . . ? C57 C62 N4 114.2(6) . . ? C61 C62 N4 124.9(7) . . ? C66 N4 C62 121.6(6) . . ? C66 N4 Ni2 125.6(5) . . ? C62 N4 Ni2 112.3(5) . . ? C59 O6 C63 115.8(6) . . ? O6 C63 H62 109.5 . . ? O6 C63 H63 109.5 . . ? H62 C63 H63 109.5 . . ? O6 C63 H64 109.5 . . ? H62 C63 H64 109.5 . . ? H63 C63 H64 109.5 . . ? C60 O7 C65 116.8(9) . . ? C60 O7 C64 117.1(9) . . ? C65 O7 C64 39.7(10) . . ? O7 C64 H65 109.5 . . ? O7 C64 H66 109.5 . . ? H65 C64 H66 109.5 . . ? O7 C64 H67 109.5 . . ? H65 C64 H67 109.5 . . ? H66 C64 H67 109.5 . . ? O7 C65 H68 109.5 . . ? O7 C65 H69 109.5 . . ? H68 C65 H69 109.5 . . ? O7 C65 H70 109.5 . . ? H68 C65 H70 109.5 . . ? H69 C65 H70 109.5 . . ? N4 C66 C67 125.3(7) . . ? N4 C66 H71 117.4 . . ? C67 C66 H71 117.4 . . ? C72 C67 C66 118.8(7) . . ? C72 C67 C68 121.0(7) . . ? C66 C67 C68 120.1(7) . . ? O8 C68 C67 124.3(6) . . ? O8 C68 C69 119.2(6) . . ? C67 C68 C69 116.5(7) . . ? C70 C69 C68 119.0(6) . . ? C70 C69 C9 121.1(6) . . ? C68 C69 C9 119.8(6) . . ? C69 C70 C71 125.2(7) . . ? C69 C70 H72 117.4 . . ? C71 C70 H72 117.4 . . ? C72 C71 C70 114.6(7) . . ? C72 C71 C73 121.9(7) . . ? C70 C71 C73 123.5(7) . . ? C71 C72 C67 123.1(7) . . ? C71 C72 H73 118.5 . . ? C67 C72 H73 118.5 . . ? C68 O8 Ni2 127.3(4) . . ? C74 C73 C78 135.4(14) . . ? C74 C73 C76 120.4(15) . . ? C78 C73 C76 54.3(13) . . ? C74 C73 C77 35.1(14) . . ? C78 C73 C77 107.5(16) . . ? C76 C73 C77 128.2(15) . . ? C74 C73 C71 111.1(11) . . ? C78 C73 C71 108.7(11) . . ? C76 C73 C71 115.8(11) . . ? C77 C73 C71 116.0(13) . . ? C74 C73 C79 82.8(14) . . ? C78 C73 C79 106.0(15) . . ? C76 C73 C79 51.8(13) . . ? C77 C73 C79 113.5(17) . . ? C71 C73 C79 104.6(11) . . ? C74 C73 C75 106.8(14) . . ? C78 C73 C75 41.1(12) . . ? C76 C73 C75 92.9(15) . . ? C77 C73 C75 72.2(15) . . ? C71 C73 C75 106.9(11) . . ? C79 C73 C75 140.7(14) . . ? C73 C74 H74 109.5 . . ? C73 C74 H75 109.5 . . ? H74 C74 H75 109.5 . . ? C73 C74 H76 109.5 . . ? H74 C74 H76 109.5 . . ? H75 C74 H76 109.5 . . ? C73 C75 H77 109.5 . . ? C73 C75 H78 109.5 . . ? H77 C75 H78 109.5 . . ? C73 C75 H79 109.5 . . ? H77 C75 H79 109.5 . . ? H78 C75 H79 109.5 . . ? C73 C76 H80 109.5 . . ? C73 C76 H81 109.5 . . ? H80 C76 H81 109.5 . . ? C73 C76 H82 109.5 . . ? H80 C76 H82 109.5 . . ? H81 C76 H82 109.5 . . ? C73 C77 H83 109.5 . . ? C73 C77 H84 109.5 . . ? H83 C77 H84 109.5 . . ? C73 C77 H85 109.5 . . ? H83 C77 H85 109.5 . . ? H84 C77 H85 109.5 . . ? C73 C78 H86 109.5 . . ? C73 C78 H87 109.5 . . ? H86 C78 H87 109.5 . . ? C73 C78 H88 109.5 . . ? H86 C78 H88 109.5 . . ? H87 C78 H88 109.5 . . ? C73 C79 H89 109.5 . . ? C73 C79 H90 109.5 . . ? H89 C79 H90 109.5 . . ? C73 C79 H91 109.5 . . ? H89 C79 H91 109.5 . . ? H90 C79 H91 109.5 . . ? C85 C80 C81 119.5(5) . . ? C85 C80 C5 121.0(5) . . ? C81 C80 C5 119.5(5) . . ? O9 C81 C82 124.1(5) . . ? O9 C81 C80 119.7(5) . . ? C82 C81 C80 116.2(6) . . ? C83 C82 C81 120.8(5) . . ? C83 C82 C90 118.7(6) . . ? C81 C82 C90 120.6(6) . . ? C84 C83 C82 122.6(6) . . ? C84 C83 H92 118.7 . . ? C82 C83 H92 118.7 . . ? C83 C84 C85 115.6(6) . . ? C83 C84 C86 124.0(6) . . ? C85 C84 C86 120.4(6) . . ? C80 C85 C84 124.7(6) . . ? C80 C85 H93 117.7 . . ? C84 C85 H93 117.7 . . ? C81 O9 Ni3 127.8(4) . . ? C84 C86 C88 108.7(7) . . ? C84 C86 C89 108.9(8) . . ? C88 C86 C89 111.2(7) . . ? C84 C86 C87 111.4(6) . . ? C88 C86 C87 107.3(9) . . ? C89 C86 C87 109.4(7) . . ? C86 C87 H94 109.5 . . ? C86 C87 H95 109.5 . . ? H94 C87 H95 109.5 . . ? C86 C87 H96 109.5 . . ? H94 C87 H96 109.5 . . ? H95 C87 H96 109.5 . . ? C86 C88 H97 109.5 . . ? C86 C88 H98 109.5 . . ? H97 C88 H98 109.5 . . ? C86 C88 H99 109.5 . . ? H97 C88 H99 109.5 . . ? H98 C88 H99 109.5 . . ? C86 C89 H100 109.5 . . ? C86 C89 H101 109.5 . . ? H100 C89 H101 109.5 . . ? C86 C89 H102 109.5 . . ? H100 C89 H102 109.5 . . ? H101 C89 H102 109.5 . . ? N5 C90 C82 125.2(6) . . ? N5 C90 H103 117.4 . . ? C82 C90 H103 117.4 . . ? C90 N5 C91 120.6(5) . . ? C90 N5 Ni3 126.1(4) . . ? C91 N5 Ni3 113.1(4) . . ? C96 C91 C92 121.3(6) . . ? C96 C91 N5 113.2(6) . . ? C92 C91 N5 125.5(6) . . ? C93 C92 C91 119.4(6) . . ? C93 C92 H104 120.3 . . ? C91 C92 H104 120.3 . . ? O10 C93 C92 125.0(7) . . ? O10 C93 C94 116.0(6) . . ? C92 C93 C94 119.1(6) . . ? C95 C94 O11 123.3(7) . . ? C95 C94 C93 121.8(6) . . ? O11 C94 C93 114.9(6) . . ? C94 C95 C96 118.1(7) . . ? C94 C95 H105 121.0 . . ? C96 C95 H105 121.0 . . ? C91 C96 N6 114.9(5) . . ? C91 C96 C95 120.4(6) . . ? N6 C96 C95 124.7(6) . . ? C93 O10 C97 117.5(5) . . ? O10 C97 H106 109.5 . . ? O10 C97 H107 109.5 . . ? H106 C97 H107 109.5 . . ? O10 C97 H108 109.5 . . ? H106 C97 H108 109.5 . . ? H107 C97 H108 109.5 . . ? C94 O11 C98 116.4(6) . . ? O11 C98 H109 109.5 . . ? O11 C98 H110 109.5 . . ? H109 C98 H110 109.5 . . ? O11 C98 H111 109.5 . . ? H109 C98 H111 109.5 . . ? H110 C98 H111 109.5 . . ? C99 N6 C96 122.1(5) . . ? C99 N6 Ni3 125.1(5) . . ? C96 N6 Ni3 112.7(4) . . ? N6 C99 C100 126.1(6) . . ? N6 C99 H112 116.9 . . ? C100 C99 H112 116.9 . . ? C99 C100 C105 118.5(6) . . ? C99 C100 C101 121.5(6) . . ? C105 C100 C101 119.9(7) . . ? O12 C101 C102 120.4(6) . . ? O12 C101 C100 122.4(6) . . ? C102 C101 C100 117.2(6) . . ? C103 C102 C101 119.8(7) . . ? C103 C102 C11 118.9(7) . . ? C101 C102 C11 121.2(6) . . ? C102 C103 C104 123.0(8) . . ? C102 C103 H113 118.5 . . ? C104 C103 H113 118.5 . . ? C105 C104 C103 116.9(7) . . ? C105 C104 C106 122.5(8) . . ? C103 C104 C106 120.5(9) . . ? C104 C105 C100 122.4(7) . . ? C104 C105 H114 118.8 . . ? C100 C105 H114 118.8 . . ? C101 O12 Ni3 127.9(4) . . ? C112 C106 C107 122.4(17) . . ? C112 C106 C108 60.9(16) . . ? C107 C106 C108 98.0(15) . . ? C112 C106 C104 120.1(16) . . ? C107 C106 C104 117.0(11) . . ? C108 C106 C104 105.2(11) . . ? C112 C106 C109 40.7(15) . . ? C107 C106 C109 121.3(12) . . ? C108 C106 C109 101.5(14) . . ? C104 C106 C109 110.1(10) . . ? C112 C106 C110 112.9(19) . . ? C107 C106 C110 57.5(13) . . ? C108 C106 C110 148.4(15) . . ? C104 C106 C110 104.0(12) . . ? C109 C106 C110 79.3(14) . . ? C112 C106 C111 101(2) . . ? C107 C106 C111 50.0(15) . . ? C108 C106 C111 50.1(15) . . ? C104 C106 C111 111.3(14) . . ? C109 C106 C111 134.7(15) . . ? C110 C106 C111 107.3(19) . . ? C106 C107 H115 109.5 . . ? C106 C107 H116 109.5 . . ? H115 C107 H116 109.5 . . ? C106 C107 H117 109.5 . . ? H115 C107 H117 109.5 . . ? H116 C107 H117 109.5 . . ? C106 C108 H118 109.5 . . ? C106 C108 H119 109.5 . . ? H118 C108 H119 109.5 . . ? C106 C108 H120 109.5 . . ? H118 C108 H120 109.5 . . ? H119 C108 H120 109.5 . . ? C106 C109 H121 109.5 . . ? C106 C109 H122 109.5 . . ? H121 C109 H122 109.5 . . ? C106 C109 H123 109.5 . . ? H121 C109 H123 109.5 . . ? H122 C109 H123 109.5 . . ? C106 C110 H124 109.5 . . ? C106 C110 H125 109.5 . . ? H124 C110 H125 109.5 . . ? C106 C110 H126 109.5 . . ? H124 C110 H126 109.5 . . ? H125 C110 H126 109.5 . . ? C106 C111 H127 109.5 . . ? C106 C111 H128 109.5 . . ? H127 C111 H128 109.5 . . ? C106 C111 H129 109.5 . . ? H127 C111 H129 109.5 . . ? H128 C111 H129 109.5 . . ? C106 C112 H130 109.5 . . ? C106 C112 H131 109.5 . . ? H130 C112 H131 109.5 . . ? C106 C112 H132 109.5 . . ? H130 C112 H132 109.5 . . ? H131 C112 H132 109.5 . . ? H133 O13 H134 106(3) . . ? H135 O14 H136 105(3) . . ? O15 S1 C113 98.6(18) . . ? O15 S1 C114 102.0(15) . . ? C113 S1 C114 105.1(17) . . ? S1 C113 H137 109.5 . . ? S1 C113 H138 109.5 . . ? H137 C113 H138 109.5 . . ? S1 C113 H139 109.5 . . ? H137 C113 H139 109.5 . . ? H138 C113 H139 109.5 . . ? S1 C114 H140 109.5 . . ? S1 C114 H141 109.5 . . ? H140 C114 H141 109.5 . . ? S1 C114 H142 109.5 . . ? H140 C114 H142 109.5 . . ? H141 C114 H142 109.5 . . ? O16 S2 C116 106.6(17) . . ? O16 S2 C115 98.9(16) . . ? C116 S2 C115 88.8(17) . . ? S2 C115 H143 109.5 . . ? S2 C115 H144 109.5 . . ? H143 C115 H144 109.5 . . ? S2 C115 H145 109.5 . . ? H143 C115 H145 109.5 . . ? H144 C115 H145 109.5 . . ? S2 C116 H146 109.5 . . ? S2 C116 H147 109.5 . . ? H146 C116 H147 109.5 . . ? S2 C116 H148 109.5 . . ? H146 C116 H148 109.5 . . ? H147 C116 H148 109.5 . . ? O17 S3 C118 107.0(11) . . ? O17 S3 C117 100.9(7) . . ? C118 S3 C117 93.3(10) . . ? S3 C117 H149 109.5 . . ? S3 C117 H150 109.5 . . ? H149 C117 H150 109.5 . . ? S3 C117 H151 109.5 . . ? H149 C117 H151 109.5 . . ? H150 C117 H151 109.5 . . ? S3 C118 H152 109.5 . . ? S3 C118 H153 109.5 . . ? H152 C118 H153 109.5 . . ? S3 C118 H154 109.5 . . ? H152 C118 H154 109.5 . . ? H153 C118 H154 109.5 . . ? S4 C120 H158 109.5 . . ? S4 C120 H159 109.5 . . ? H158 C120 H159 109.5 . . ? S4 C120 H160 109.5 . . ? H158 C120 H160 109.5 . . ? H159 C120 H160 109.5 . . ? O19 S5 C121 107.8(7) . . ? O19 S5 C122 103.2(5) . . ? C121 S5 C122 99.3(8) . . ? S5 C121 H161 109.5 . . ? S5 C121 H162 109.5 . . ? H161 C121 H162 109.5 . . ? S5 C121 H163 109.5 . . ? H161 C121 H163 109.5 . . ? H162 C121 H163 109.5 . . ? S5 C122 H164 109.5 . . ? S5 C122 H165 109.5 . . ? H164 C122 H165 109.5 . . ? S5 C122 H166 109.5 . . ? H164 C122 H166 109.5 . . ? H165 C122 H166 109.5 . . ? C124 S6 C123 95.2(13) . . ? S6 C123 H167 109.5 . . ? S6 C123 H168 109.5 . . ? H167 C123 H168 109.5 . . ? S6 C123 H169 109.5 . . ? H167 C123 H169 109.5 . . ? H168 C123 H169 109.5 . . ? S6 C124 H170 109.5 . . ? S6 C124 H171 109.5 . . ? H170 C124 H171 109.5 . . ? S6 C124 H172 109.5 . . ? H170 C124 H172 109.5 . . ? H171 C124 H172 109.5 . . ? O21 S7 C126 106.3(10) . . ? O21 S7 C125 108.3(9) . . ? C126 S7 C125 87.6(12) . . ? S7 C125 H173 109.5 . . ? S7 C125 H174 109.5 . . ? H173 C125 H174 109.5 . . ? S7 C125 H175 109.5 . . ? H173 C125 H175 109.5 . . ? H174 C125 H175 109.5 . . ? S7 C126 H176 109.5 . . ? S7 C126 H177 109.5 . . ? H176 C126 H177 109.5 . . ? S7 C126 H178 109.5 . . ? H176 C126 H178 109.5 . . ? H177 C126 H178 109.5 . . ? Cl2 C127 Cl1 114.8(13) . . ? Cl2 C127 H179 108.6 . . ? Cl1 C127 H179 108.6 . . ? Cl2 C127 H180 108.6 . . ? Cl1 C127 H180 108.6 . . ? H179 C127 H180 107.6 . . ? Cl3 C128 Cl4 112.1(18) . . ? Cl3 C128 H181 109.2 . . ? Cl4 C128 H181 109.2 . . ? Cl3 C128 H182 109.2 . . ? Cl4 C128 H182 109.2 . . ? H181 C128 H182 107.9 . . ? Cl5 C129 Cl6 113.5(16) . . ? Cl5 C129 H183 108.9 . . ? Cl6 C129 H183 108.9 . . ? Cl5 C129 H184 108.9 . . ? Cl6 C129 H184 108.9 . . ? H183 C129 H184 107.7 . . ? Cl8 C130 Cl7 109.5(12) . . ? Cl8 C130 H185 109.8 . . ? Cl7 C130 H185 109.8 . . ? Cl8 C130 H186 109.8 . . ? Cl7 C130 H186 109.8 . . ? H185 C130 H186 108.2 . . ? Cl9 C131 Cl10 105.2(11) . . ? Cl9 C131 H187 110.7 . . ? Cl10 C131 H187 110.7 . . ? Cl9 C131 H188 110.7 . . ? Cl10 C131 H188 110.7 . . ? H187 C131 H188 108.8 . . ? Cl12 C132 H189 108.9 . . ? Cl12 C132 H190 108.9 . . ? H189 C132 H190 107.7 . . ? Cl13 C133 Cl14 115.2(11) . . ? Cl13 C133 H191 108.5 . . ? Cl14 C133 H191 108.5 . . ? Cl13 C133 H192 108.5 . . ? Cl14 C133 H192 108.5 . . ? H191 C133 H192 107.5 . . ? Cl15 C134 H193 109.5 . . ? Cl15 C134 H194 109.5 . . ? H193 C134 H194 108.1 . . ? Cl17 C135 Cl18 111.8(12) . . ? Cl17 C135 H195 109.3 . . ? Cl18 C135 H195 109.3 . . ? Cl17 C135 H196 109.3 . . ? Cl18 C135 H196 109.3 . . ? H195 C135 H196 107.9 . . ? Cl20 C136 Cl19 107.1(14) . . ? Cl20 C136 H197 110.3 . . ? Cl19 C136 H197 110.3 . . ? Cl20 C136 H198 110.3 . . ? Cl19 C136 H198 110.3 . . ? H197 C136 H198 108.6 . . ? Cl22 C137 H199 108.7 . . ? Cl22 C137 H200 108.7 . . ? H199 C137 H200 107.6 . . ? Cl24 C138 H201 109.4 . . ? Cl24 C138 H202 109.4 . . ? H201 C138 H202 108.0 . . ? Cl25 C139 Cl26 114.1(18) . . ? Cl25 C139 H203 108.7 . . ? Cl26 C139 H203 108.7 . . ? Cl25 C139 H204 108.7 . . ? Cl26 C139 H204 108.7 . . ? H203 C139 H204 107.6 . . ? Cl27 C140 Cl28 114.6(19) . . ? Cl27 C140 H205 108.6 . . ? Cl28 C140 H205 108.6 . . ? Cl27 C140 H206 108.6 . . ? Cl28 C140 H206 108.6 . . ? H205 C140 H206 107.6 . . ? Cl30 C141 Cl29 112.3(18) . . ? Cl30 C141 H207 109.1 . . ? Cl29 C141 H207 109.1 . . ? Cl30 C141 H208 109.1 . . ? Cl29 C141 H208 109.1 . . ? H207 C141 H208 107.9 . . ? Cl32 C142 Cl31 106.1(11) . . ? Cl32 C142 H209 110.5 . . ? Cl31 C142 H209 110.5 . . ? Cl32 C142 H210 110.5 . . ? Cl31 C142 H210 110.5 . . ? H209 C142 H210 108.7 . . ? Cl34 C143 Cl33 120.9(16) . . ? Cl34 C143 H211 107.1 . . ? Cl33 C143 H211 107.1 . . ? Cl34 C143 H212 107.1 . . ? Cl33 C143 H212 107.1 . . ? H211 C143 H212 106.8 . . ? Cl35 C144 Cl36 112.6(15) . . ? Cl35 C144 H213 109.1 . . ? Cl36 C144 H213 109.1 . . ? Cl35 C144 H214 109.1 . . ? Cl36 C144 H214 109.1 . . ? H213 C144 H214 107.8 . . ? Cl38 C145 Cl37 112.8(18) . . ? Cl38 C145 H215 109.0 . . ? Cl37 C145 H215 109.0 . . ? Cl38 C145 H216 109.0 . . ? Cl37 C145 H216 109.0 . . ? H215 C145 H216 107.8 . . ? Cl39 C146 Cl40 114.8(12) . . ? Cl39 C146 H217 108.6 . . ? Cl40 C146 H217 108.6 . . ? Cl39 C146 H218 108.6 . . ? Cl40 C146 H218 108.6 . . ? H217 C146 H218 107.5 . . ? Cl41 C147 H219 109.7 . . ? Cl41 C147 H220 109.7 . . ? H219 C147 H220 108.2 . . ? C153 C148 C149 111.8(14) . . ? C153 C148 H221 109.3 . . ? C149 C148 H221 109.3 . . ? C153 C148 H222 109.3 . . ? C149 C148 H222 109.3 . . ? H221 C148 H222 107.9 . . ? C150 C149 C148 108.8(14) . . ? C150 C149 H223 109.9 . . ? C148 C149 H223 109.9 . . ? C150 C149 H224 109.9 . . ? C148 C149 H224 109.9 . . ? H223 C149 H224 108.3 . . ? C151 C150 C149 110.3(14) . . ? C151 C150 H225 109.6 . . ? C149 C150 H225 109.6 . . ? C151 C150 H226 109.6 . . ? C149 C150 H226 109.6 . . ? H225 C150 H226 108.1 . . ? C152 C151 C150 113.0(16) . . ? C152 C151 H227 109.0 . . ? C150 C151 H227 109.0 . . ? C152 C151 H228 109.0 . . ? C150 C151 H228 109.0 . . ? H227 C151 H228 107.8 . . ? C151 C152 C153 106.4(14) . . ? C151 C152 H229 110.4 . . ? C153 C152 H229 110.4 . . ? C151 C152 H230 110.4 . . ? C153 C152 H230 110.4 . . ? H229 C152 H230 108.6 . . ? C148 C153 C152 106.7(14) . . ? C148 C153 H231 110.4 . . ? C152 C153 H231 110.4 . . ? C148 C153 H232 110.4 . . ? C152 C153 H232 110.4 . . ? H231 C153 H232 108.6 . . ? C159 C154 C155 112.1(14) . . ? C159 C154 H233 109.2 . . ? C155 C154 H233 109.2 . . ? C159 C154 H234 109.2 . . ? C155 C154 H234 109.2 . . ? H233 C154 H234 107.9 . . ? C154 C155 C156 110.1(14) . . ? C154 C155 H235 109.6 . . ? C156 C155 H235 109.6 . . ? C154 C155 H236 109.6 . . ? C156 C155 H236 109.6 . . ? H235 C155 H236 108.1 . . ? C157 C156 C155 107.1(14) . . ? C157 C156 H237 110.3 . . ? C155 C156 H237 110.3 . . ? C157 C156 H238 110.3 . . ? C155 C156 H238 110.3 . . ? H237 C156 H238 108.6 . . ? C158 C157 C156 112.8(15) . . ? C158 C157 H239 109.0 . . ? C156 C157 H239 109.0 . . ? C158 C157 H240 109.0 . . ? C156 C157 H240 109.0 . . ? H239 C157 H240 107.8 . . ? C157 C158 C159 113.9(14) . . ? C157 C158 H241 108.8 . . ? C159 C158 H241 108.8 . . ? C157 C158 H242 108.8 . . ? C159 C158 H242 108.8 . . ? H241 C158 H242 107.7 . . ? C154 C159 C158 109.7(14) . . ? C154 C159 H243 109.7 . . ? C158 C159 H243 109.7 . . ? C154 C159 H244 109.7 . . ? C158 C159 H244 109.7 . . ? H243 C159 H244 108.2 . . ? C165 C160 C161 107.5(15) . . ? C165 C160 H245 110.2 . . ? C161 C160 H245 110.2 . . ? C165 C160 H246 110.2 . . ? C161 C160 H246 110.2 . . ? H245 C160 H246 108.5 . . ? C162 C161 C160 108.8(16) . . ? C162 C161 H247 109.9 . . ? C160 C161 H247 109.9 . . ? C162 C161 H248 109.9 . . ? C160 C161 H248 109.9 . . ? H247 C161 H248 108.3 . . ? C161 C162 C163 108.2(17) . . ? C161 C162 H249 110.1 . . ? C163 C162 H249 110.1 . . ? C161 C162 H250 110.1 . . ? C163 C162 H250 110.1 . . ? H249 C162 H250 108.4 . . ? C164 C163 C162 108.7(16) . . ? C164 C163 H251 109.9 . . ? C162 C163 H251 109.9 . . ? C164 C163 H252 109.9 . . ? C162 C163 H252 109.9 . . ? H251 C163 H252 108.3 . . ? C163 C164 C165 111.4(17) . . ? C163 C164 H253 109.4 . . ? C165 C164 H253 109.4 . . ? C163 C164 H254 109.4 . . ? C165 C164 H254 109.4 . . ? H253 C164 H254 108.0 . . ? C160 C165 C164 110.2(17) . . ? C160 C165 H255 109.6 . . ? C164 C165 H255 109.6 . . ? C160 C165 H256 109.6 . . ? C164 C165 H256 109.6 . . ? H255 C165 H256 108.1 . . ? C171 C166 C167 112.1(13) . . ? C171 C166 H257 109.2 . . ? C167 C166 H257 109.2 . . ? C171 C166 H258 109.2 . . ? C167 C166 H258 109.2 . . ? H257 C166 H258 107.9 . . ? C166 C167 C168 113.4(14) . . ? C166 C167 H259 108.9 . . ? C168 C167 H259 108.9 . . ? C166 C167 H260 108.9 . . ? C168 C167 H260 108.9 . . ? H259 C167 H260 107.7 . . ? C167 C168 C169 112.4(13) . . ? C167 C168 H261 109.1 . . ? C169 C168 H261 109.1 . . ? C167 C168 H262 109.1 . . ? C169 C168 H262 109.1 . . ? H261 C168 H262 107.9 . . ? C170 C169 C168 113.0(13) . . ? C170 C169 H263 109.0 . . ? C168 C169 H263 109.0 . . ? C170 C169 H264 109.0 . . ? C168 C169 H264 109.0 . . ? H263 C169 H264 107.8 . . ? C169 C170 C171 112.2(13) . . ? C169 C170 H265 109.2 . . ? C171 C170 H265 109.2 . . ? C169 C170 H266 109.2 . . ? C171 C170 H266 109.2 . . ? H265 C170 H266 107.9 . . ? C166 C171 C170 110.5(13) . . ? C166 C171 H267 109.6 . . ? C170 C171 H267 109.6 . . ? C166 C171 H268 109.6 . . ? C170 C171 H268 109.6 . . ? H267 C171 H268 108.1 . . ? C177 C172 C173 109.2(17) . . ? C177 C172 H269 109.8 . . ? C173 C172 H269 109.8 . . ? C177 C172 H270 109.8 . . ? C173 C172 H270 109.8 . . ? H269 C172 H270 108.3 . . ? C174 C173 C172 109.2(17) . . ? C174 C173 H271 109.8 . . ? C172 C173 H271 109.8 . . ? C174 C173 H272 109.8 . . ? C172 C173 H272 109.8 . . ? H271 C173 H272 108.3 . . ? C175 C174 C173 111.3(18) . . ? C175 C174 H273 109.4 . . ? C173 C174 H273 109.4 . . ? C175 C174 H274 109.4 . . ? C173 C174 H274 109.4 . . ? H273 C174 H274 108.0 . . ? C174 C175 C176 112.5(18) . . ? C174 C175 H275 109.1 . . ? C176 C175 H275 109.1 . . ? C174 C175 H276 109.1 . . ? C176 C175 H276 109.1 . . ? H275 C175 H276 107.8 . . ? C175 C176 C177 110.5(18) . . ? C175 C176 H277 109.6 . . ? C177 C176 H277 109.6 . . ? C175 C176 H278 109.6 . . ? C177 C176 H278 109.6 . . ? H277 C176 H278 108.1 . . ? C172 C177 C176 110.2(18) . . ? C172 C177 H279 109.6 . . ? C176 C177 H279 109.6 . . ? C172 C177 H280 109.6 . . ? C176 C177 H280 109.6 . . ? H279 C177 H280 108.1 . . ? C179 C178 C183 112.5(18) . . ? C179 C178 H281 109.1 . . ? C183 C178 H281 109.1 . . ? C179 C178 H282 109.1 . . ? C183 C178 H282 109.1 . . ? H281 C178 H282 107.8 . . ? C178 C179 C180 111.7(17) . . ? C178 C179 H283 109.3 . . ? C180 C179 H283 109.3 . . ? C178 C179 H284 109.3 . . ? C180 C179 H284 109.3 . . ? H283 C179 H284 107.9 . . ? C181 C180 C179 111.9(17) . . ? C181 C180 H285 109.2 . . ? C179 C180 H285 109.2 . . ? C181 C180 H286 109.2 . . ? C179 C180 H286 109.2 . . ? H285 C180 H286 107.9 . . ? C180 C181 C182 112.5(17) . . ? C180 C181 H287 109.1 . . ? C182 C181 H287 109.1 . . ? C180 C181 H288 109.1 . . ? C182 C181 H288 109.1 . . ? H287 C181 H288 107.8 . . ? C181 C182 C183 112.4(17) . . ? C181 C182 H289 109.1 . . ? C183 C182 H289 109.1 . . ? C181 C182 H290 109.1 . . ? C183 C182 H290 109.1 . . ? H289 C182 H290 107.9 . . ? C178 C183 C182 112.6(18) . . ? C178 C183 H291 109.1 . . ? C182 C183 H291 109.1 . . ? C178 C183 H292 109.1 . . ? C182 C183 H292 109.1 . . ? H291 C183 H292 107.8 . . ? C185 C184 C189 114.2(13) . . ? C185 C184 H293 108.7 . . ? C189 C184 H293 108.7 . . ? C185 C184 H294 108.7 . . ? C189 C184 H294 108.7 . . ? H293 C184 H294 107.6 . . ? C186 C185 C184 117.3(14) . . ? C186 C185 H295 108.0 . . ? C184 C185 H295 108.0 . . ? C186 C185 H296 108.0 . . ? C184 C185 H296 108.0 . . ? H295 C185 H296 107.2 . . ? C185 C186 C187 120.1(15) . . ? C185 C186 H297 107.3 . . ? C187 C186 H297 107.3 . . ? C185 C186 H298 107.3 . . ? C187 C186 H298 107.3 . . ? H297 C186 H298 106.9 . . ? C186 C187 C188 110.2(15) . . ? C186 C187 H299 109.6 . . ? C188 C187 H299 109.6 . . ? C186 C187 H300 109.6 . . ? C188 C187 H300 109.6 . . ? H299 C187 H300 108.1 . . ? C189 C188 C187 105.7(15) . . ? C189 C188 H301 110.6 . . ? C187 C188 H301 110.6 . . ? C189 C188 H302 110.6 . . ? C187 C188 H302 110.6 . . ? H301 C188 H302 108.7 . . ? C188 C189 C184 111.6(15) . . ? C188 C189 H303 109.3 . . ? C184 C189 H303 109.3 . . ? C188 C189 H304 109.3 . . ? C184 C189 H304 109.3 . . ? H303 C189 H304 108.0 . . ? C195 C190 C191 112.8(17) . . ? C195 C190 H305 109.0 . . ? C191 C190 H305 109.0 . . ? C195 C190 H306 109.0 . . ? C191 C190 H306 109.0 . . ? H305 C190 H306 107.8 . . ? C190 C191 C192 109.1(16) . . ? C190 C191 H307 109.9 . . ? C192 C191 H307 109.9 . . ? C190 C191 H308 109.9 . . ? C192 C191 H308 109.9 . . ? H307 C191 H308 108.3 . . ? C193 C192 C191 109.0(17) . . ? C193 C192 H309 109.9 . . ? C191 C192 H309 109.9 . . ? C193 C192 H310 109.9 . . ? C191 C192 H310 109.9 . . ? H309 C192 H310 108.3 . . ? C194 C193 C192 111.8(18) . . ? C194 C193 H311 109.3 . . ? C192 C193 H311 109.3 . . ? C194 C193 H312 109.3 . . ? C192 C193 H312 109.3 . . ? H311 C193 H312 107.9 . . ? C193 C194 C195 110.8(18) . . ? C193 C194 H313 109.5 . . ? C195 C194 H313 109.5 . . ? C193 C194 H314 109.5 . . ? C195 C194 H314 109.5 . . ? H313 C194 H314 108.1 . . ? C190 C195 C194 111.1(17) . . ? C190 C195 H315 109.4 . . ? C194 C195 H315 109.4 . . ? C190 C195 H316 109.4 . . ? C194 C195 H316 109.4 . . ? H315 C195 H316 108.0 . . ? C197 C196 C198 108.7(16) . 2 ? C197 C196 H317 110.0 . . ? C198 C196 H317 110.0 2 . ? C197 C196 H318 110.0 . . ? C198 C196 H318 110.0 2 . ? H317 C196 H318 108.3 . . ? C198 C197 C196 109.9(16) . . ? C198 C197 H319 109.7 . . ? C196 C197 H319 109.7 . . ? C198 C197 H320 109.7 . . ? C196 C197 H320 109.7 . . ? H319 C197 H320 108.2 . . ? C197 C198 C196 112.1(17) . 2 ? C197 C198 H321 109.2 . . ? C196 C198 H321 109.2 2 . ? C197 C198 H322 109.2 . . ? C196 C198 H322 109.2 2 . ? H321 C198 H322 107.9 . . ? C200 C199 C204 113.0(18) . . ? C200 C199 H323 109.0 . . ? C204 C199 H323 109.0 . . ? C200 C199 H324 109.0 . . ? C204 C199 H324 109.0 . . ? H323 C199 H324 107.8 . . ? C199 C200 C201 110.3(17) . . ? C199 C200 H325 109.6 . . ? C201 C200 H325 109.6 . . ? C199 C200 H326 109.6 . . ? C201 C200 H326 109.6 . . ? H325 C200 H326 108.1 . . ? C202 C201 C200 110.4(17) . . ? C202 C201 H327 109.6 . . ? C200 C201 H327 109.6 . . ? C202 C201 H328 109.6 . . ? C200 C201 H328 109.6 . . ? H327 C201 H328 108.1 . . ? C201 C202 C203 111.8(18) . . ? C201 C202 H329 109.3 . . ? C203 C202 H329 109.3 . . ? C201 C202 H330 109.3 . . ? C203 C202 H330 109.3 . . ? H329 C202 H330 107.9 . . ? C202 C203 C204 111.5(18) . . ? C202 C203 H331 109.3 . . ? C204 C203 H331 109.3 . . ? C202 C203 H332 109.3 . . ? C204 C203 H332 109.3 . . ? H331 C203 H332 108.0 . . ? C199 C204 C203 111.6(18) . . ? C199 C204 H333 109.3 . . ? C203 C204 H333 109.3 . . ? C199 C204 H334 109.3 . . ? C203 C204 H334 109.3 . . ? H333 C204 H334 108.0 . . ? 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 1.0(9) . . . . ? C13 C1 C2 C3 -174.2(6) . . . . ? C1 C2 C3 C4 -0.3(9) . . . . ? C1 C2 C3 C43 173.2(6) . . . . ? C2 C3 C4 C5 0.6(10) . . . . ? C43 C3 C4 C5 -173.0(6) . . . . ? C3 C4 C5 C6 -1.5(10) . . . . ? C3 C4 C5 C80 172.4(6) . . . . ? C4 C5 C6 C1 2.2(10) . . . . ? C80 C5 C6 C1 -171.7(6) . . . . ? C2 C1 C6 C5 -1.9(9) . . . . ? C13 C1 C6 C5 173.3(6) . . . . ? C12 C7 C8 C9 -1.1(10) . . . . ? C35 C7 C8 C9 172.1(6) . . . . ? C7 C8 C9 C10 1.6(10) . . . . ? C7 C8 C9 C69 -173.0(6) . . . . ? C8 C9 C10 C11 -1.3(11) . . . . ? C69 C9 C10 C11 173.2(7) . . . . ? C9 C10 C11 C12 0.6(11) . . . . ? C9 C10 C11 C102 -172.1(7) . . . . ? C8 C7 C12 C11 0.4(11) . . . . ? C35 C7 C12 C11 -172.6(6) . . . . ? C10 C11 C12 C7 -0.1(11) . . . . ? C102 C11 C12 C7 172.7(7) . . . . ? C2 C1 C13 C18 47.9(8) . . . . ? C6 C1 C13 C18 -127.1(6) . . . . ? C2 C1 C13 C14 -137.7(6) . . . . ? C6 C1 C13 C14 47.2(9) . . . . ? C18 C13 C14 O1 -173.0(5) . . . . ? C1 C13 C14 O1 12.7(9) . . . . ? C18 C13 C14 C15 5.2(9) . . . . ? C1 C13 C14 C15 -169.1(6) . . . . ? O1 C14 C15 C16 173.0(6) . . . . ? C13 C14 C15 C16 -5.1(9) . . . . ? O1 C14 C15 C23 -13.2(10) . . . . ? C13 C14 C15 C23 168.7(6) . . . . ? C14 C15 C16 C17 0.8(11) . . . . ? C23 C15 C16 C17 -173.3(6) . . . . ? C15 C16 C17 C18 3.3(10) . . . . ? C15 C16 C17 C19 -178.7(7) . . . . ? C14 C13 C18 C17 -1.2(9) . . . . ? C1 C13 C18 C17 173.4(6) . . . . ? C16 C17 C18 C13 -3.1(10) . . . . ? C19 C17 C18 C13 178.8(6) . . . . ? C15 C14 O1 Ni1 4.2(8) . . . . ? C13 C14 O1 Ni1 -177.8(4) . . . . ? O4 Ni1 O1 C14 -163.3(5) . . . . ? N1 Ni1 O1 C14 8.0(5) . . . . ? N2 Ni1 O1 C14 104.0(14) . . . . ? C16 C17 C19 C21 100.6(9) . . . . ? C18 C17 C19 C21 -81.4(10) . . . . ? C16 C17 C19 C20 -137.9(9) . . . . ? C18 C17 C19 C20 40.0(10) . . . . ? C16 C17 C19 C22 -22.7(11) . . . . ? C18 C17 C19 C22 155.3(8) . . . . ? C14 C15 C23 N1 5.2(11) . . . . ? C16 C15 C23 N1 179.2(6) . . . . ? C15 C23 N1 C24 -174.4(6) . . . . ? C15 C23 N1 Ni1 11.1(10) . . . . ? O4 Ni1 N1 C23 75.9(16) . . . . ? O1 Ni1 N1 C23 -15.3(6) . . . . ? N2 Ni1 N1 C23 173.1(6) . . . . ? O4 Ni1 N1 C24 -99.1(13) . . . . ? O1 Ni1 N1 C24 169.7(4) . . . . ? N2 Ni1 N1 C24 -1.9(4) . . . . ? C23 N1 C24 C29 -173.7(6) . . . . ? Ni1 N1 C24 C29 1.4(7) . . . . ? C23 N1 C24 C25 9.1(10) . . . . ? Ni1 N1 C24 C25 -175.8(5) . . . . ? C29 C24 C25 C26 0.3(10) . . . . ? N1 C24 C25 C26 177.3(6) . . . . ? C24 C25 C26 O2 -178.7(6) . . . . ? C24 C25 C26 C27 0.7(10) . . . . ? O2 C26 C27 C28 179.6(6) . . . . ? C25 C26 C27 C28 0.0(10) . . . . ? O2 C26 C27 O3 -1.0(9) . . . . ? C25 C26 C27 O3 179.5(6) . . . . ? O3 C27 C28 C29 178.8(6) . . . . ? C26 C27 C28 C29 -1.8(10) . . . . ? C25 C24 C29 C28 -2.0(10) . . . . ? N1 C24 C29 C28 -179.3(5) . . . . ? C25 C24 C29 N2 177.5(6) . . . . ? N1 C24 C29 N2 0.2(8) . . . . ? C27 C28 C29 C24 2.7(10) . . . . ? C27 C28 C29 N2 -176.7(6) . . . . ? C25 C26 O2 C30 0.6(10) . . . . ? C27 C26 O2 C30 -178.9(6) . . . . ? C28 C27 O3 C31 1.4(10) . . . . ? C26 C27 O3 C31 -178.0(6) . . . . ? C24 C29 N2 C32 -175.4(6) . . . . ? C28 C29 N2 C32 4.1(10) . . . . ? C24 C29 N2 Ni1 -1.7(7) . . . . ? C28 C29 N2 Ni1 177.8(5) . . . . ? O4 Ni1 N2 C32 -13.1(6) . . . . ? O1 Ni1 N2 C32 78.9(15) . . . . ? N1 Ni1 N2 C32 175.4(6) . . . . ? O4 Ni1 N2 C29 173.5(4) . . . . ? O1 Ni1 N2 C29 -94.5(14) . . . . ? N1 Ni1 N2 C29 2.0(4) . . . . ? C29 N2 C32 C33 -177.0(6) . . . . ? Ni1 N2 C32 C33 10.1(10) . . . . ? N2 C32 C33 C38 -178.5(7) . . . . ? N2 C32 C33 C34 2.5(11) . . . . ? C32 C33 C34 O4 -8.7(11) . . . . ? C38 C33 C34 O4 172.3(6) . . . . ? C32 C33 C34 C35 171.3(6) . . . . ? C38 C33 C34 C35 -7.7(10) . . . . ? O4 C34 C35 C36 -171.5(6) . . . . ? C33 C34 C35 C36 8.5(10) . . . . ? O4 C34 C35 C7 10.6(10) . . . . ? C33 C34 C35 C7 -169.4(6) . . . . ? C12 C7 C35 C36 44.8(10) . . . . ? C8 C7 C35 C36 -128.3(7) . . . . ? C12 C7 C35 C34 -137.3(7) . . . . ? C8 C7 C35 C34 49.6(9) . . . . ? C34 C35 C36 C37 -3.3(11) . . . . ? C7 C35 C36 C37 174.6(7) . . . . ? C35 C36 C37 C38 -3.2(11) . . . . ? C35 C36 C37 C39 179.0(7) . . . . ? C36 C37 C38 C33 4.0(11) . . . . ? C39 C37 C38 C33 -178.3(7) . . . . ? C32 C33 C38 C37 -177.6(7) . . . . ? C34 C33 C38 C37 1.4(11) . . . . ? C35 C34 O4 Ni1 -178.5(5) . . . . ? C33 C34 O4 Ni1 1.6(10) . . . . ? O1 Ni1 O4 C34 -163.9(5) . . . . ? N1 Ni1 O4 C34 104.2(14) . . . . ? N2 Ni1 O4 C34 7.6(6) . . . . ? C38 C37 C39 C42 -120.3(8) . . . . ? C36 C37 C39 C42 57.3(9) . . . . ? C38 C37 C39 C41 119.5(8) . . . . ? C36 C37 C39 C41 -62.9(9) . . . . ? C38 C37 C39 C40 -1.0(11) . . . . ? C36 C37 C39 C40 176.7(7) . . . . ? C2 C3 C43 C48 -130.5(6) . . . . ? C4 C3 C43 C48 42.9(9) . . . . ? C2 C3 C43 C44 46.5(8) . . . . ? C4 C3 C43 C44 -140.0(6) . . . . ? C48 C43 C44 O5 -170.3(5) . . . . ? C3 C43 C44 O5 12.7(8) . . . . ? C48 C43 C44 C45 7.4(8) . . . . ? C3 C43 C44 C45 -169.6(5) . . . . ? O5 C44 C45 C46 171.3(6) . . . . ? C43 C44 C45 C46 -6.4(8) . . . . ? O5 C44 C45 C56 -10.8(9) . . . . ? C43 C44 C45 C56 171.6(5) . . . . ? C56 C45 C46 C47 -176.9(6) . . . . ? C44 C45 C46 C47 1.1(9) . . . . ? C45 C46 C47 C48 3.2(9) . . . . ? C45 C46 C47 C49 -178.0(6) . . . . ? C44 C43 C48 C47 -3.4(9) . . . . ? C3 C43 C48 C47 173.6(6) . . . . ? C46 C47 C48 C43 -2.0(9) . . . . ? C49 C47 C48 C43 179.1(6) . . . . ? C43 C44 O5 Ni2 179.3(4) . . . . ? C45 C44 O5 Ni2 1.7(8) . . . . ? O8 Ni2 O5 C44 -161.9(5) . . . . ? N4 Ni2 O5 C44 107.9(17) . . . . ? N3 Ni2 O5 C44 9.4(5) . . . . ? C46 C47 C49 C54 -138.5(14) . . . . ? C48 C47 C49 C54 40.3(15) . . . . ? C46 C47 C49 C53 -16.2(13) . . . . ? C48 C47 C49 C53 162.6(10) . . . . ? C46 C47 C49 C52 151.5(13) . . . . ? C48 C47 C49 C52 -29.7(15) . . . . ? C46 C47 C49 C50 8.7(19) . . . . ? C48 C47 C49 C50 -172.5(16) . . . . ? C46 C47 C49 C55 100.6(11) . . . . ? C48 C47 C49 C55 -80.6(11) . . . . ? C46 C47 C49 C51 -101.3(12) . . . . ? C48 C47 C49 C51 77.4(12) . . . . ? C46 C45 C56 N3 -178.6(6) . . . . ? C44 C45 C56 N3 3.4(10) . . . . ? C45 C56 N3 C57 -176.4(6) . . . . ? C45 C56 N3 Ni2 12.0(9) . . . . ? O5 Ni2 N3 C56 -15.9(6) . . . . ? O8 Ni2 N3 C56 76.7(16) . . . . ? N4 Ni2 N3 C56 171.7(6) . . . . ? O5 Ni2 N3 C57 171.7(4) . . . . ? O8 Ni2 N3 C57 -95.7(14) . . . . ? N4 Ni2 N3 C57 -0.7(5) . . . . ? C56 N3 C57 C62 -169.2(7) . . . . ? Ni2 N3 C57 C62 3.4(8) . . . . ? C56 N3 C57 C58 9.4(10) . . . . ? Ni2 N3 C57 C58 -178.0(6) . . . . ? C62 C57 C58 C59 0.8(11) . . . . ? N3 C57 C58 C59 -177.7(7) . . . . ? C57 C58 C59 C60 4.0(12) . . . . ? C57 C58 C59 O6 -177.9(7) . . . . ? C58 C59 C60 O7 176.5(8) . . . . ? O6 C59 C60 O7 -1.8(12) . . . . ? C58 C59 C60 C61 -5.1(15) . . . . ? O6 C59 C60 C61 176.7(8) . . . . ? O7 C60 C61 C62 179.6(9) . . . . ? C59 C60 C61 C62 1.2(15) . . . . ? C58 C57 C62 C61 -4.6(13) . . . . ? N3 C57 C62 C61 174.1(8) . . . . ? C58 C57 C62 N4 176.2(7) . . . . ? N3 C57 C62 N4 -5.1(11) . . . . ? C60 C61 C62 C57 3.5(15) . . . . ? C60 C61 C62 N4 -177.4(9) . . . . ? C57 C62 N4 C66 -168.3(9) . . . . ? C61 C62 N4 C66 12.5(15) . . . . ? C57 C62 N4 Ni2 4.4(10) . . . . ? C61 C62 N4 Ni2 -174.7(8) . . . . ? O5 Ni2 N4 C66 71(2) . . . . ? O8 Ni2 N4 C66 -18.3(9) . . . . ? N3 Ni2 N4 C66 170.4(9) . . . . ? O5 Ni2 N4 C62 -101.1(17) . . . . ? O8 Ni2 N4 C62 169.3(6) . . . . ? N3 Ni2 N4 C62 -2.0(6) . . . . ? C60 C59 O6 C63 -168.7(8) . . . . ? C58 C59 O6 C63 13.0(10) . . . . ? C59 C60 O7 C65 164.1(12) . . . . ? C61 C60 O7 C65 -14.3(17) . . . . ? C59 C60 O7 C64 -151.0(12) . . . . ? C61 C60 O7 C64 30.6(17) . . . . ? C62 N4 C66 C67 -174.0(9) . . . . ? Ni2 N4 C66 C67 14.3(15) . . . . ? N4 C66 C67 C72 179.1(10) . . . . ? N4 C66 C67 C68 3.7(16) . . . . ? C72 C67 C68 O8 171.7(9) . . . . ? C66 C67 C68 O8 -13.0(14) . . . . ? C72 C67 C68 C69 -6.5(13) . . . . ? C66 C67 C68 C69 168.8(8) . . . . ? O8 C68 C69 C70 -170.3(7) . . . . ? C67 C68 C69 C70 8.0(11) . . . . ? O8 C68 C69 C9 13.4(11) . . . . ? C67 C68 C69 C9 -168.3(7) . . . . ? C10 C9 C69 C70 -131.0(8) . . . . ? C8 C9 C69 C70 43.5(10) . . . . ? C10 C9 C69 C68 45.2(10) . . . . ? C8 C9 C69 C68 -140.3(7) . . . . ? C68 C69 C70 C71 -2.8(12) . . . . ? C9 C69 C70 C71 173.4(7) . . . . ? C69 C70 C71 C72 -4.2(13) . . . . ? C69 C70 C71 C73 178.1(8) . . . . ? C70 C71 C72 C67 5.9(14) . . . . ? C73 C71 C72 C67 -176.4(9) . . . . ? C66 C67 C72 C71 -176.0(9) . . . . ? C68 C67 C72 C71 -0.6(15) . . . . ? C67 C68 O8 Ni2 3.5(12) . . . . ? C69 C68 O8 Ni2 -178.4(5) . . . . ? O5 Ni2 O8 C68 -162.5(7) . . . . ? N4 Ni2 O8 C68 9.8(7) . . . . ? N3 Ni2 O8 C68 104.2(15) . . . . ? C72 C71 C73 C74 -51.3(16) . . . . ? C70 C71 C73 C74 126.3(13) . . . . ? C72 C71 C73 C78 108.0(15) . . . . ? C70 C71 C73 C78 -74.4(16) . . . . ? C72 C71 C73 C76 166.7(16) . . . . ? C70 C71 C73 C76 -15.8(19) . . . . ? C72 C71 C73 C77 -13(2) . . . . ? C70 C71 C73 C77 164.3(17) . . . . ? C72 C71 C73 C79 -139.1(13) . . . . ? C70 C71 C73 C79 38.5(14) . . . . ? C72 C71 C73 C75 64.8(14) . . . . ? C70 C71 C73 C75 -117.6(13) . . . . ? C4 C5 C80 C85 -129.2(7) . . . . ? C6 C5 C80 C85 44.6(9) . . . . ? C4 C5 C80 C81 47.3(9) . . . . ? C6 C5 C80 C81 -138.9(6) . . . . ? C85 C80 C81 O9 -170.9(6) . . . . ? C5 C80 C81 O9 12.6(9) . . . . ? C85 C80 C81 C82 9.0(9) . . . . ? C5 C80 C81 C82 -167.5(6) . . . . ? O9 C81 C82 C83 171.2(6) . . . . ? C80 C81 C82 C83 -8.6(10) . . . . ? O9 C81 C82 C90 -9.1(10) . . . . ? C80 C81 C82 C90 171.0(6) . . . . ? C81 C82 C83 C84 2.5(11) . . . . ? C90 C82 C83 C84 -177.2(7) . . . . ? C82 C83 C84 C85 3.4(12) . . . . ? C82 C83 C84 C86 -176.7(8) . . . . ? C81 C80 C85 C84 -3.4(11) . . . . ? C5 C80 C85 C84 173.1(7) . . . . ? C83 C84 C85 C80 -3.0(12) . . . . ? C86 C84 C85 C80 177.1(8) . . . . ? C82 C81 O9 Ni3 0.8(9) . . . . ? C80 C81 O9 Ni3 -179.3(4) . . . . ? O12 Ni3 O9 C81 -162.8(5) . . . . ? N5 Ni3 O9 C81 8.4(5) . . . . ? N6 Ni3 O9 C81 103.2(17) . . . . ? C83 C84 C86 C88 -120.6(9) . . . . ? C85 C84 C86 C88 59.3(11) . . . . ? C83 C84 C86 C89 118.1(9) . . . . ? C85 C84 C86 C89 -62.0(10) . . . . ? C83 C84 C86 C87 -2.6(14) . . . . ? C85 C84 C86 C87 177.3(9) . . . . ? C83 C82 C90 N5 -176.1(7) . . . . ? C81 C82 C90 N5 4.2(11) . . . . ? C82 C90 N5 C91 -177.2(6) . . . . ? C82 C90 N5 Ni3 8.6(10) . . . . ? O12 Ni3 N5 C90 77.7(15) . . . . ? O9 Ni3 N5 C90 -12.9(5) . . . . ? N6 Ni3 N5 C90 175.1(5) . . . . ? O12 Ni3 N5 C91 -97.0(13) . . . . ? O9 Ni3 N5 C91 172.5(4) . . . . ? N6 Ni3 N5 C91 0.4(4) . . . . ? C90 N5 C91 C96 -176.1(6) . . . . ? Ni3 N5 C91 C96 -1.2(7) . . . . ? C90 N5 C91 C92 4.2(9) . . . . ? Ni3 N5 C91 C92 179.2(5) . . . . ? C96 C91 C92 C93 0.8(10) . . . . ? N5 C91 C92 C93 -179.6(6) . . . . ? C91 C92 C93 O10 179.9(6) . . . . ? C91 C92 C93 C94 0.2(9) . . . . ? O10 C93 C94 C95 179.2(6) . . . . ? C92 C93 C94 C95 -1.1(10) . . . . ? O10 C93 C94 O11 -0.4(9) . . . . ? C92 C93 C94 O11 179.3(6) . . . . ? O11 C94 C95 C96 -179.4(6) . . . . ? C93 C94 C95 C96 1.0(10) . . . . ? C92 C91 C96 N6 -178.9(6) . . . . ? N5 C91 C96 N6 1.5(8) . . . . ? C92 C91 C96 C95 -0.9(10) . . . . ? N5 C91 C96 C95 179.4(6) . . . . ? C94 C95 C96 C91 -0.0(10) . . . . ? C94 C95 C96 N6 177.7(6) . . . . ? C92 C93 O10 C97 2.9(9) . . . . ? C94 C93 O10 C97 -177.4(6) . . . . ? C95 C94 O11 C98 -0.8(10) . . . . ? C93 C94 O11 C98 178.8(6) . . . . ? C91 C96 N6 C99 -176.9(6) . . . . ? C95 C96 N6 C99 5.3(10) . . . . ? C91 C96 N6 Ni3 -1.1(7) . . . . ? C95 C96 N6 Ni3 -179.0(5) . . . . ? O12 Ni3 N6 C99 -12.7(6) . . . . ? N5 Ni3 N6 C99 176.0(6) . . . . ? O9 Ni3 N6 C99 80.7(19) . . . . ? O12 Ni3 N6 C96 171.6(4) . . . . ? N5 Ni3 N6 C96 0.3(4) . . . . ? O9 Ni3 N6 C96 -95.0(16) . . . . ? C96 N6 C99 C100 -178.4(6) . . . . ? Ni3 N6 C99 C100 6.4(10) . . . . ? N6 C99 C100 C105 -175.6(7) . . . . ? N6 C99 C100 C101 8.0(11) . . . . ? C99 C100 C101 O12 -12.1(10) . . . . ? C105 C100 C101 O12 171.6(6) . . . . ? C99 C100 C101 C102 168.8(6) . . . . ? C105 C100 C101 C102 -7.6(9) . . . . ? O12 C101 C102 C103 -170.3(7) . . . . ? C100 C101 C102 C103 8.8(10) . . . . ? O12 C101 C102 C11 12.9(9) . . . . ? C100 C101 C102 C11 -167.9(6) . . . . ? C10 C11 C102 C103 44.3(11) . . . . ? C12 C11 C102 C103 -128.2(8) . . . . ? C10 C11 C102 C101 -138.9(7) . . . . ? C12 C11 C102 C101 48.6(10) . . . . ? C101 C102 C103 C104 -2.8(13) . . . . ? C11 C102 C103 C104 174.1(8) . . . . ? C102 C103 C104 C105 -4.9(14) . . . . ? C102 C103 C104 C106 175.8(9) . . . . ? C103 C104 C105 C100 6.2(13) . . . . ? C106 C104 C105 C100 -174.5(9) . . . . ? C99 C100 C105 C104 -176.5(8) . . . . ? C101 C100 C105 C104 -0.0(12) . . . . ? C102 C101 O12 Ni3 -179.5(4) . . . . ? C100 C101 O12 Ni3 1.4(8) . . . . ? N5 Ni3 O12 C101 105.7(13) . . . . ? O9 Ni3 O12 C101 -163.1(5) . . . . ? N6 Ni3 O12 C101 9.0(5) . . . . ? C105 C104 C106 C112 -28(2) . . . . ? C103 C104 C106 C112 151(2) . . . . ? C105 C104 C106 C107 159.7(14) . . . . ? C103 C104 C106 C107 -21.0(19) . . . . ? C105 C104 C106 C108 -92.8(15) . . . . ? C103 C104 C106 C108 86.5(15) . . . . ? C105 C104 C106 C109 15.8(17) . . . . ? C103 C104 C106 C109 -164.9(12) . . . . ? C105 C104 C106 C110 99.4(16) . . . . ? C103 C104 C106 C110 -81.3(16) . . . . ? C105 C104 C106 C111 -145.4(19) . . . . ? C103 C104 C106 C111 34(2) . . . . ? C153 C148 C149 C150 -59(3) . . . . ? C148 C149 C150 C151 53(3) . . . . ? C149 C150 C151 C152 -59(3) . . . . ? C150 C151 C152 C153 62(2) . . . . ? C149 C148 C153 C152 63(2) . . . . ? C151 C152 C153 C148 -63(2) . . . . ? C159 C154 C155 C156 61(2) . . . . ? C154 C155 C156 C157 -59(2) . . . . ? C155 C156 C157 C158 56(3) . . . . ? C156 C157 C158 C159 -54(3) . . . . ? C155 C154 C159 C158 -55(3) . . . . ? C157 C158 C159 C154 51(3) . . . . ? C165 C160 C161 C162 -63(3) . . . . ? C160 C161 C162 C163 64(3) . . . . ? C161 C162 C163 C164 -61(3) . . . . ? C162 C163 C164 C165 58(3) . . . . ? C161 C160 C165 C164 59(3) . . . . ? C163 C164 C165 C160 -58(3) . . . . ? C171 C166 C167 C168 53(3) . . . . ? C166 C167 C168 C169 -51(3) . . . . ? C167 C168 C169 C170 51(3) . . . . ? C168 C169 C170 C171 -53(3) . . . . ? C167 C166 C171 C170 -54(2) . . . . ? C169 C170 C171 C166 54(2) . . . . ? C177 C172 C173 C174 61(3) . . . . ? C172 C173 C174 C175 -57(4) . . . . ? C173 C174 C175 C176 54(4) . . . . ? C174 C175 C176 C177 -54(4) . . . . ? C173 C172 C177 C176 -61(3) . . . . ? C175 C176 C177 C172 57(4) . . . . ? C183 C178 C179 C180 -53(4) . . . . ? C178 C179 C180 C181 54(4) . . . . ? C179 C180 C181 C182 -53(4) . . . . ? C180 C181 C182 C183 52(4) . . . . ? C179 C178 C183 C182 52(4) . . . . ? C181 C182 C183 C178 -51(4) . . . . ? C189 C184 C185 C186 27(4) . . . . ? C184 C185 C186 C187 -26(5) . . . . ? C185 C186 C187 C188 43(4) . . . . ? C186 C187 C188 C189 -61(3) . . . . ? C187 C188 C189 C184 65(3) . . . . ? C185 C184 C189 C188 -49(3) . . . . ? C195 C190 C191 C192 -56(3) . . . . ? C190 C191 C192 C193 57(3) . . . . ? C191 C192 C193 C194 -60(3) . . . . ? C192 C193 C194 C195 58(4) . . . . ? C191 C190 C195 C194 54(4) . . . . ? C193 C194 C195 C190 -54(4) . . . . ? C198 C196 C197 C198 57(3) 2 . . . ? C196 C197 C198 C196 -59(3) . . . 2 ? C204 C199 C200 C201 -55(4) . . . . ? C199 C200 C201 C202 56(4) . . . . ? C200 C201 C202 C203 -57(4) . . . . ? C201 C202 C203 C204 55(4) . . . . ? C200 C199 C204 C203 53(4) . . . . ? C202 C203 C204 C199 -52(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.333 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.091 _database_code_depnum_ccdc_archive 'CCDC 963502' ####################################################################### # # 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_LNi3Gu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[LNi3]_2(CH6N3Cl)_1.5CHCl3_1.8DMSO_6.3EtOAc_4H2O' _chemical_melting_point ? _chemical_formula_moiety C134.30H184.70Cl6.50N12Ni3O30.40S1.80 _chemical_formula_sum 'C134.30 H184.70 Cl6.50 N12 Ni3 O30.40 S1.80' _chemical_formula_weight 2917.90 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 17.831(3) _cell_length_b 21.045(4) _cell_length_c 24.615(4) _cell_angle_alpha 106.808(3) _cell_angle_beta 108.969(3) _cell_angle_gamma 91.349(3) _cell_volume 8291(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 39722 _cell_measurement_theta_min 4.08 _cell_measurement_theta_max 25.00 _exptl_crystal_description prismatic _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3082 _exptl_absorpt_coefficient_mu 0.530 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8363 _exptl_absorpt_correction_T_max 0.9343 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator 'multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39722 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.2044 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 28652 _reflns_number_gt 13018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2009)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2009)' _computing_data_reduction 'APEX2 (Bruker AXS, 2009)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP-3 _computing_publication_material ORTEP-3 _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^)+(0.0559P)^2^+6.8730P] 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 28652 _refine_ls_number_parameters 2263 _refine_ls_number_restraints 1218 _refine_ls_R_factor_all 0.2038 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2134 _refine_ls_wR_factor_gt 0.1769 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.191 _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 0.06368(4) 0.10941(5) 0.13199(4) 0.0304(3) Uani 1 1 d . . . Ni2 Ni 0.42061(4) 0.35083(4) 0.41467(4) 0.0313(3) Uani 1 1 d . . . Ni3 Ni 0.15019(4) 0.05287(4) 0.45293(4) 0.0280(2) Uani 1 1 d . . . C1 C 0.3901(3) 0.1143(3) 0.3633(3) 0.0291(17) Uani 1 1 d . . . C2 C 0.3411(3) 0.0620(3) 0.3632(3) 0.0265(17) Uani 1 1 d . . . H1 H 0.3481 0.0529 0.4001 0.032 Uiso 1 1 calc R . . C3 C 0.2819(3) 0.0225(3) 0.3104(3) 0.0301(18) Uani 1 1 d . . . C4 C 0.2732(3) 0.0376(3) 0.2565(3) 0.0278(17) Uani 1 1 d . . . H2 H 0.2326 0.0116 0.2201 0.033 Uiso 1 1 calc R . . C5 C 0.3214(3) 0.0886(4) 0.2551(3) 0.0295(18) Uani 1 1 d . . . C6 C 0.3814(3) 0.1261(3) 0.3088(3) 0.0306(18) Uani 1 1 d . . . H3 H 0.4168 0.1602 0.3081 0.037 Uiso 1 1 calc R . . C7 C 0.1383(3) 0.3179(3) 0.3532(3) 0.0317(18) Uani 1 1 d . . . C8 C 0.1629(3) 0.3134(3) 0.4122(3) 0.0290(17) Uani 1 1 d . . . H4 H 0.2053 0.3446 0.4436 0.035 Uiso 1 1 calc R . . C9 C 0.1257(3) 0.2638(3) 0.4248(3) 0.0283(17) Uani 1 1 d . . . C10 C 0.0620(3) 0.2191(3) 0.3792(3) 0.0297(17) Uani 1 1 d . . . H5 H 0.0357 0.1860 0.3884 0.036 Uiso 1 1 calc R . . C11 C 0.0365(3) 0.2224(3) 0.3205(3) 0.0282(17) Uani 1 1 d . . . C12 C 0.0752(3) 0.2718(3) 0.3079(3) 0.0294(18) Uani 1 1 d . . . H6 H 0.0584 0.2743 0.2679 0.035 Uiso 1 1 calc R . . C13 C 0.3102(3) 0.1016(4) 0.1963(3) 0.0320(18) Uani 1 1 d . . . C14 C 0.2322(3) 0.1050(3) 0.1570(3) 0.0305(18) Uani 1 1 d . . . C15 C 0.2247(3) 0.1034(4) 0.0971(3) 0.038(2) Uani 1 1 d . . . C16 C 0.2921(3) 0.1033(4) 0.0795(3) 0.044(2) Uani 1 1 d . . . H7 H 0.2848 0.1014 0.0390 0.053 Uiso 1 1 calc R . . C17 C 0.3686(4) 0.1059(4) 0.1187(3) 0.050(2) Uani 1 1 d . . . C18 C 0.3744(4) 0.1036(4) 0.1770(3) 0.045(2) Uani 1 1 d . . . H8 H 0.4260 0.1035 0.2046 0.054 Uiso 1 1 calc R . . O1 O 0.1714(2) 0.1121(2) 0.17702(18) 0.0330(12) Uani 1 1 d . . . C19 C 0.4438(4) 0.1057(6) 0.1001(3) 0.073(3) Uani 1 1 d . . . C20 C 0.4806(5) 0.0386(6) 0.1033(4) 0.105(4) Uani 1 1 d . . . H9 H 0.4419 0.0002 0.0741 0.157 Uiso 1 1 calc R . . H10 H 0.4930 0.0354 0.1442 0.157 Uiso 1 1 calc R . . H11 H 0.5297 0.0385 0.0936 0.157 Uiso 1 1 calc R . . C21 C 0.5044(5) 0.1641(7) 0.1450(4) 0.123(5) Uani 1 1 d . . . H12 H 0.5525 0.1644 0.1341 0.184 Uiso 1 1 calc R . . H13 H 0.5183 0.1599 0.1857 0.184 Uiso 1 1 calc R . . H14 H 0.4816 0.2059 0.1445 0.184 Uiso 1 1 calc R . . C22 C 0.4241(4) 0.1100(7) 0.0368(4) 0.129(6) Uani 1 1 d . . . H15 H 0.3863 0.0709 0.0078 0.194 Uiso 1 1 calc R . . H16 H 0.4732 0.1108 0.0271 0.194 Uiso 1 1 calc R . . H17 H 0.4001 0.1509 0.0344 0.194 Uiso 1 1 calc R . . C23 C 0.1485(3) 0.0963(3) 0.0516(3) 0.0355(19) Uani 1 1 d . . . H18 H 0.1483 0.0941 0.0125 0.043 Uiso 1 1 calc R . . N1 N 0.0795(3) 0.0926(3) 0.0580(2) 0.0294(14) Uani 1 1 d . . . C24 C 0.0068(3) 0.0811(3) 0.0080(3) 0.0282(17) Uani 1 1 d . . . C25 C -0.0000(3) 0.0718(3) -0.0524(3) 0.0292(17) Uani 1 1 d . . . H19 H 0.0462 0.0705 -0.0637 0.035 Uiso 1 1 calc R . . C26 C -0.0749(4) 0.0646(4) -0.0949(3) 0.0348(19) Uani 1 1 d . . . C27 C -0.1442(3) 0.0688(4) -0.0776(3) 0.0327(18) Uani 1 1 d . . . C28 C -0.1365(3) 0.0757(3) -0.0187(3) 0.0328(18) Uani 1 1 d . . . H20 H -0.1826 0.0763 -0.0072 0.039 Uiso 1 1 calc R . . C29 C -0.0607(3) 0.0818(3) 0.0239(3) 0.0274(17) Uani 1 1 d . . . O2 O -0.0911(2) 0.0548(3) -0.15546(18) 0.0399(13) Uani 1 1 d . . . C30 C -0.0261(4) 0.0480(4) -0.1770(3) 0.043(2) Uani 1 1 d . . . H21 H -0.0457 0.0417 -0.2205 0.065 Uiso 1 1 calc R . . H22 H -0.0006 0.0092 -0.1695 0.065 Uiso 1 1 calc R . . H23 H 0.0129 0.0885 -0.1558 0.065 Uiso 1 1 calc R . . O3 O -0.2146(2) 0.0652(3) -0.12294(18) 0.0417(14) Uani 1 1 d . . . C31 C -0.2851(3) 0.0699(4) -0.1069(3) 0.050(2) Uani 1 1 d . . . H24 H -0.3314 0.0687 -0.1423 0.075 Uiso 1 1 calc R . . H25 H -0.2786 0.1120 -0.0746 0.075 Uiso 1 1 calc R . . H26 H -0.2937 0.0322 -0.0928 0.075 Uiso 1 1 calc R . . N2 N -0.0447(3) 0.0918(3) 0.0863(2) 0.0318(15) Uani 1 1 d . . . C32 C -0.1006(3) 0.0796(4) 0.1063(3) 0.0352(19) Uani 1 1 d . . . H27 H -0.1496 0.0549 0.0773 0.042 Uiso 1 1 calc R . . C33 C -0.0944(3) 0.1002(3) 0.1680(3) 0.0312(18) Uani 1 1 d . . . C34 C -0.0230(3) 0.1391(3) 0.2149(3) 0.0315(18) Uani 1 1 d . . . C35 C -0.0295(3) 0.1727(3) 0.2722(3) 0.0290(18) Uani 1 1 d . . . C36 C -0.0995(3) 0.1600(4) 0.2822(3) 0.0332(18) Uani 1 1 d . . . H28 H -0.1021 0.1819 0.3210 0.040 Uiso 1 1 calc R . . C37 C -0.1674(3) 0.1164(4) 0.2383(3) 0.0328(18) Uani 1 1 d . . . C38 C -0.1640(3) 0.0892(4) 0.1821(3) 0.036(2) Uani 1 1 d . . . H29 H -0.2098 0.0617 0.1510 0.043 Uiso 1 1 calc R . . O4 O 0.0458(2) 0.1416(2) 0.20522(18) 0.0288(11) Uani 1 1 d . . . C39 C -0.2443(3) 0.1059(4) 0.2527(3) 0.039(2) Uani 1 1 d . . . C40 C -0.3039(4) 0.0484(4) 0.2036(3) 0.058(2) Uani 1 1 d . . . H30 H -0.3513 0.0431 0.2145 0.087 Uiso 1 1 calc R . . H31 H -0.2792 0.0069 0.1996 0.087 Uiso 1 1 calc R . . H32 H -0.3195 0.0579 0.1650 0.087 Uiso 1 1 calc R . . C41 C -0.2825(4) 0.1708(4) 0.2593(4) 0.058(2) Uani 1 1 d . . . H33 H -0.2445 0.2074 0.2919 0.087 Uiso 1 1 calc R . . H34 H -0.3309 0.1651 0.2690 0.087 Uiso 1 1 calc R . . H35 H -0.2967 0.1813 0.2212 0.087 Uiso 1 1 calc R . . C42 C -0.2243(4) 0.0888(4) 0.3122(3) 0.054(2) Uani 1 1 d . . . H36 H -0.1885 0.1260 0.3456 0.081 Uiso 1 1 calc R . . H37 H -0.1978 0.0482 0.3089 0.081 Uiso 1 1 calc R . . H38 H -0.2737 0.0812 0.3200 0.081 Uiso 1 1 calc R . . C43 C 0.4536(3) 0.1571(4) 0.4207(3) 0.0301(18) Uani 1 1 d . . . C44 C 0.4648(3) 0.2274(4) 0.4362(3) 0.0298(18) Uani 1 1 d . . . C45 C 0.5355(3) 0.2624(4) 0.4855(3) 0.0323(18) Uani 1 1 d . . . C46 C 0.5843(3) 0.2273(4) 0.5223(3) 0.0325(18) Uani 1 1 d . . . H39 H 0.6296 0.2517 0.5559 0.039 Uiso 1 1 calc R . . C47 C 0.5686(3) 0.1604(4) 0.5113(3) 0.0320(18) Uani 1 1 d . . . C48 C 0.5034(3) 0.1262(3) 0.4585(3) 0.0270(17) Uani 1 1 d . . . H40 H 0.4932 0.0789 0.4481 0.032 Uiso 1 1 calc R . . O5 O 0.4111(2) 0.2600(2) 0.40813(18) 0.0319(12) Uani 1 1 d . . . C49 C 0.6181(3) 0.1197(4) 0.5500(3) 0.037(2) Uani 1 1 d . . . C50 C 0.6564(4) 0.0674(4) 0.5132(3) 0.051(2) Uani 1 1 d . . . H41 H 0.6878 0.0425 0.5387 0.076 Uiso 1 1 calc R . . H42 H 0.6914 0.0900 0.4991 0.076 Uiso 1 1 calc R . . H43 H 0.6143 0.0364 0.4783 0.076 Uiso 1 1 calc R . . C51 C 0.5638(4) 0.0857(4) 0.5738(3) 0.045(2) Uani 1 1 d . . . H44 H 0.5952 0.0599 0.5985 0.068 Uiso 1 1 calc R . . H45 H 0.5200 0.0557 0.5396 0.068 Uiso 1 1 calc R . . H46 H 0.5418 0.1199 0.5986 0.068 Uiso 1 1 calc R . . C52 C 0.6856(4) 0.1661(4) 0.6059(3) 0.051(2) Uani 1 1 d . . . H47 H 0.7165 0.1393 0.6296 0.077 Uiso 1 1 calc R . . H48 H 0.6623 0.1988 0.6308 0.077 Uiso 1 1 calc R . . H49 H 0.7209 0.1896 0.5926 0.077 Uiso 1 1 calc R . . C53 C 0.5641(3) 0.3284(3) 0.4929(3) 0.0333(19) Uani 1 1 d . . . H50 H 0.6138 0.3475 0.5244 0.040 Uiso 1 1 calc R . . N3 N 0.5290(3) 0.3658(3) 0.4607(2) 0.0299(14) Uani 1 1 d . . . C54 C 0.5674(3) 0.4271(3) 0.4645(3) 0.0292(17) Uani 1 1 d . . . C55 C 0.6505(3) 0.4475(3) 0.4902(3) 0.0308(18) Uani 1 1 d . . . H51 H 0.6854 0.4202 0.5084 0.037 Uiso 1 1 calc R . . C56 C 0.6803(3) 0.5068(4) 0.4884(3) 0.0347(18) Uani 1 1 d . . . C57 C 0.6287(4) 0.5487(3) 0.4622(3) 0.0328(18) Uani 1 1 d . . . C58 C 0.5473(3) 0.5278(4) 0.4359(3) 0.0341(18) Uani 1 1 d . . . H52 H 0.5125 0.5551 0.4176 0.041 Uiso 1 1 calc R . . C59 C 0.5169(3) 0.4665(3) 0.4363(3) 0.0296(17) Uani 1 1 d . . . O6 O 0.7602(2) 0.5308(2) 0.5091(2) 0.0456(14) Uani 1 1 d . . . C60 C 0.8150(4) 0.4894(4) 0.5342(4) 0.056(2) Uani 1 1 d . . . H53 H 0.8700 0.5107 0.5466 0.084 Uiso 1 1 calc R . . H54 H 0.8075 0.4456 0.5037 0.084 Uiso 1 1 calc R . . H55 H 0.8050 0.4835 0.5694 0.084 Uiso 1 1 calc R . . O7 O 0.6662(2) 0.6070(2) 0.4642(2) 0.0419(13) Uani 1 1 d . . . C61 C 0.6173(4) 0.6510(4) 0.4393(4) 0.053(2) Uani 1 1 d . . . H56 H 0.6510 0.6908 0.4434 0.080 Uiso 1 1 calc R . . H57 H 0.5799 0.6644 0.4610 0.080 Uiso 1 1 calc R . . H58 H 0.5872 0.6282 0.3964 0.080 Uiso 1 1 calc R . . N4 N 0.4355(3) 0.4360(3) 0.4088(2) 0.0337(15) Uani 1 1 d . . . C62 C 0.3802(3) 0.4650(4) 0.3781(3) 0.0345(19) Uani 1 1 d . . . H59 H 0.3970 0.5056 0.3732 0.041 Uiso 1 1 calc R . . C63 C 0.2973(3) 0.4405(4) 0.3516(3) 0.0330(18) Uani 1 1 d . . . C64 C 0.2649(3) 0.3828(3) 0.3586(3) 0.0286(17) Uani 1 1 d . . . C65 C 0.1792(3) 0.3699(3) 0.3392(3) 0.0303(17) Uani 1 1 d . . . C66 C 0.1340(3) 0.4085(3) 0.3076(3) 0.0330(18) Uani 1 1 d . . . H60 H 0.0775 0.3980 0.2933 0.040 Uiso 1 1 calc R . . C67 C 0.1650(3) 0.4619(4) 0.2950(3) 0.039(2) Uani 1 1 d . . . C68 C 0.2474(4) 0.4790(4) 0.3189(3) 0.040(2) Uani 1 1 d . . . H61 H 0.2708 0.5167 0.3136 0.048 Uiso 1 1 calc R . . O8 O 0.3093(2) 0.3409(2) 0.38078(19) 0.0315(12) Uani 1 1 d . . . C69 C 0.1080(4) 0.5005(4) 0.2576(3) 0.048(2) Uani 1 1 d . . . C70 C 0.1521(4) 0.5591(4) 0.2516(4) 0.059(3) Uani 1 1 d . . . H62 H 0.1901 0.5428 0.2312 0.089 Uiso 1 1 calc R . . H63 H 0.1812 0.5905 0.2920 0.089 Uiso 1 1 calc R . . H64 H 0.1137 0.5819 0.2279 0.089 Uiso 1 1 calc R . . C71 C 0.0474(4) 0.5268(4) 0.2886(4) 0.065(3) Uani 1 1 d . . . H65 H 0.0177 0.4891 0.2918 0.098 Uiso 1 1 calc R . . H66 H 0.0100 0.5500 0.2646 0.098 Uiso 1 1 calc R . . H67 H 0.0760 0.5579 0.3292 0.098 Uiso 1 1 calc R . . C72 C 0.0628(5) 0.4510(4) 0.1933(4) 0.071(3) Uani 1 1 d . . . H68 H 0.1014 0.4339 0.1739 0.107 Uiso 1 1 calc R . . H69 H 0.0258 0.4742 0.1690 0.107 Uiso 1 1 calc R . . H70 H 0.0326 0.4135 0.1966 0.107 Uiso 1 1 calc R . . C73 C 0.2273(3) -0.0331(4) 0.3081(3) 0.0248(17) Uani 1 1 d . . . C74 C 0.1854(3) -0.0253(4) 0.3504(3) 0.0278(18) Uani 1 1 d . . . C75 C 0.1399(3) -0.0839(3) 0.3459(3) 0.0249(17) Uani 1 1 d . . . C76 C 0.1274(3) -0.1430(4) 0.2974(3) 0.0323(19) Uani 1 1 d . . . H71 H 0.0928 -0.1799 0.2943 0.039 Uiso 1 1 calc R . . C77 C 0.1626(3) -0.1505(4) 0.2540(3) 0.0330(19) Uani 1 1 d . A . C78 C 0.2137(3) -0.0935(4) 0.2625(3) 0.0291(18) Uani 1 1 d . . . H72 H 0.2410 -0.0968 0.2346 0.035 Uiso 1 1 calc R . . O9 O 0.1900(2) 0.0337(2) 0.3897(2) 0.0297(12) Uani 1 1 d . . . C79 C 0.1487(4) -0.2158(4) 0.2031(3) 0.0397(19) Uani 1 1 d U . . C80 C 0.2051(8) -0.2170(7) 0.1678(6) 0.075(4) Uani 0.713(11) 1 d PU A 1 H73 H 0.2012 -0.1781 0.1533 0.112 Uiso 0.713(11) 1 calc PR A 1 H74 H 0.1903 -0.2581 0.1332 0.112 Uiso 0.713(11) 1 calc PR A 1 H75 H 0.2602 -0.2157 0.1942 0.112 Uiso 0.713(11) 1 calc PR A 1 C81 C 0.0642(7) -0.2244(7) 0.1576(6) 0.077(4) Uani 0.713(11) 1 d PU A 1 H76 H 0.0574 -0.1859 0.1423 0.115 Uiso 0.713(11) 1 calc PR A 1 H77 H 0.0252 -0.2272 0.1774 0.115 Uiso 0.713(11) 1 calc PR A 1 H78 H 0.0557 -0.2655 0.1237 0.115 Uiso 0.713(11) 1 calc PR A 1 C82 C 0.1573(8) -0.2746(6) 0.2267(5) 0.059(4) Uani 0.713(11) 1 d PU A 1 H79 H 0.1494 -0.3158 0.1931 0.089 Uiso 0.713(11) 1 calc PR A 1 H80 H 0.1171 -0.2770 0.2456 0.089 Uiso 0.713(11) 1 calc PR A 1 H81 H 0.2109 -0.2692 0.2567 0.089 Uiso 0.713(11) 1 calc PR A 1 C83 C 0.132(2) -0.2071(18) 0.1414(12) 0.069(9) Uani 0.287(11) 1 d PU A 2 H82 H 0.1246 -0.2510 0.1111 0.103 Uiso 0.287(11) 1 calc PR A 2 H83 H 0.1772 -0.1789 0.1423 0.103 Uiso 0.287(11) 1 calc PR A 2 H84 H 0.0834 -0.1857 0.1310 0.103 Uiso 0.287(11) 1 calc PR A 2 C84 C 0.0737(17) -0.2631(18) 0.1938(16) 0.075(10) Uani 0.287(11) 1 d PU A 2 H85 H 0.0782 -0.2707 0.2321 0.113 Uiso 0.287(11) 1 calc PR A 2 H86 H 0.0706 -0.3060 0.1632 0.113 Uiso 0.287(11) 1 calc PR A 2 H87 H 0.0254 -0.2424 0.1801 0.113 Uiso 0.287(11) 1 calc PR A 2 C85 C 0.2227(19) -0.2560(18) 0.2208(16) 0.086(11) Uani 0.287(11) 1 d PU A 2 H88 H 0.2286 -0.2633 0.2594 0.129 Uiso 0.287(11) 1 calc PR A 2 H89 H 0.2715 -0.2300 0.2246 0.129 Uiso 0.287(11) 1 calc PR A 2 H90 H 0.2134 -0.2992 0.1892 0.129 Uiso 0.287(11) 1 calc PR A 2 C86 C 0.1108(3) -0.0860(4) 0.3932(3) 0.0290(18) Uani 1 1 d . . . H91 H 0.0804 -0.1263 0.3881 0.035 Uiso 1 1 calc R . . N5 N 0.1232(3) -0.0364(3) 0.4431(3) 0.0321(16) Uani 1 1 d . . . C87 C 0.1014(3) -0.0456(4) 0.4918(3) 0.0281(17) Uani 1 1 d . . . C88 C 0.0810(3) -0.1077(4) 0.4965(3) 0.0303(17) Uani 1 1 d . . . H92 H 0.0811 -0.1477 0.4663 0.036 Uiso 1 1 calc R . . C89 C 0.0605(3) -0.1104(4) 0.5454(3) 0.0330(19) Uani 1 1 d . . . C90 C 0.0599(3) -0.0493(4) 0.5901(3) 0.0291(18) Uani 1 1 d . . . C91 C 0.0814(3) 0.0110(4) 0.5852(3) 0.0302(17) Uani 1 1 d . . . H93 H 0.0812 0.0515 0.6149 0.036 Uiso 1 1 calc R . . C92 C 0.1038(3) 0.0127(4) 0.5358(3) 0.0284(18) Uani 1 1 d . . . O10 O 0.0403(2) -0.1674(3) 0.5553(2) 0.0392(13) Uani 1 1 d . . . C93 C 0.0371(4) -0.2297(4) 0.5103(4) 0.045(2) Uani 1 1 d . . . H94 H 0.0211 -0.2669 0.5225 0.067 Uiso 1 1 calc R . . H95 H 0.0899 -0.2341 0.5066 0.067 Uiso 1 1 calc R . . H96 H -0.0021 -0.2308 0.4713 0.067 Uiso 1 1 calc R . . O11 O 0.0365(2) -0.0598(3) 0.6342(2) 0.0380(13) Uani 1 1 d . . . C94 C 0.0444(4) -0.0032(4) 0.6854(4) 0.042(2) Uani 1 1 d . . . H97 H 0.0256 -0.0172 0.7138 0.063 Uiso 1 1 calc R . . H98 H 0.0124 0.0303 0.6721 0.063 Uiso 1 1 calc R . . H99 H 0.1007 0.0162 0.7053 0.063 Uiso 1 1 calc R . . N6 N 0.1273(3) 0.0716(3) 0.5247(3) 0.0283(15) Uani 1 1 d . . . C95 C 0.1400(3) 0.1301(4) 0.5638(3) 0.0304(18) Uani 1 1 d . . . H100 H 0.1383 0.1319 0.6023 0.037 Uiso 1 1 calc R . . C96 C 0.1564(3) 0.1925(4) 0.5555(3) 0.0281(17) Uani 1 1 d . . . C97 C 0.1546(3) 0.1942(4) 0.4971(3) 0.0310(18) Uani 1 1 d . . . C98 C 0.1502(3) 0.2588(4) 0.4889(3) 0.0284(17) Uani 1 1 d . . . C99 C 0.1632(3) 0.3152(4) 0.5373(3) 0.0334(19) Uani 1 1 d . . . H101 H 0.1644 0.3574 0.5306 0.040 Uiso 1 1 calc R . . C100 C 0.1749(4) 0.3145(4) 0.5969(3) 0.040(2) Uani 1 1 d . B . C101 C 0.1663(3) 0.2517(4) 0.6029(3) 0.0359(19) Uani 1 1 d . . . H102 H 0.1671 0.2487 0.6408 0.043 Uiso 1 1 calc R . . O12 O 0.1585(2) 0.1412(3) 0.4544(2) 0.0310(12) Uani 1 1 d . . . C102 C 0.1891(5) 0.3777(4) 0.6493(4) 0.053(2) Uani 1 1 d U . . C103 C 0.1929(10) 0.3655(7) 0.7092(6) 0.062(4) Uani 0.639(14) 1 d PU B 1 H103 H 0.2355 0.3381 0.7203 0.092 Uiso 0.639(14) 1 calc PR B 1 H104 H 0.1416 0.3421 0.7038 0.092 Uiso 0.639(14) 1 calc PR B 1 H105 H 0.2041 0.4085 0.7413 0.092 Uiso 0.639(14) 1 calc PR B 1 C104 C 0.1264(11) 0.4244(9) 0.6367(7) 0.094(6) Uani 0.639(14) 1 d PU B 1 H106 H 0.1261 0.4369 0.6012 0.141 Uiso 0.639(14) 1 calc PR B 1 H107 H 0.1392 0.4647 0.6718 0.141 Uiso 0.639(14) 1 calc PR B 1 H108 H 0.0736 0.4016 0.6288 0.141 Uiso 0.639(14) 1 calc PR B 1 C105 C 0.2746(10) 0.4138(9) 0.6644(7) 0.091(6) Uani 0.639(14) 1 d PU B 1 H109 H 0.3146 0.3843 0.6754 0.136 Uiso 0.639(14) 1 calc PR B 1 H110 H 0.2852 0.4552 0.6983 0.136 Uiso 0.639(14) 1 calc PR B 1 H111 H 0.2775 0.4245 0.6289 0.136 Uiso 0.639(14) 1 calc PR B 1 C106 C 0.1110(16) 0.3896(17) 0.6650(16) 0.097(10) Uani 0.361(14) 1 d PU B 2 H112 H 0.0687 0.3951 0.6302 0.145 Uiso 0.361(14) 1 calc PR B 2 H113 H 0.1217 0.4300 0.6999 0.145 Uiso 0.361(14) 1 calc PR B 2 H114 H 0.0939 0.3510 0.6748 0.145 Uiso 0.361(14) 1 calc PR B 2 C107 C 0.2139(16) 0.4406(12) 0.6389(11) 0.063(7) Uani 0.361(14) 1 d PU B 2 H115 H 0.1831 0.4394 0.5975 0.095 Uiso 0.361(14) 1 calc PR B 2 H116 H 0.2711 0.4439 0.6446 0.095 Uiso 0.361(14) 1 calc PR B 2 H117 H 0.2038 0.4795 0.6677 0.095 Uiso 0.361(14) 1 calc PR B 2 C108 C 0.255(2) 0.3729(16) 0.7031(13) 0.101(11) Uani 0.361(14) 1 d PU B 2 H118 H 0.2651 0.4148 0.7364 0.152 Uiso 0.361(14) 1 calc PR B 2 H119 H 0.3031 0.3648 0.6930 0.152 Uiso 0.361(14) 1 calc PR B 2 H120 H 0.2388 0.3358 0.7153 0.152 Uiso 0.361(14) 1 calc PR B 2 C109 C 0.2149(3) 0.1715(4) 0.3364(3) 0.0315(18) Uani 1 1 d . . . N7 N 0.2578(3) 0.1899(3) 0.3959(2) 0.0358(15) Uani 1 1 d . . . H121 H 0.2963 0.2238 0.4121 0.043 Uiso 1 1 calc R . . H122 H 0.2474 0.1679 0.4187 0.043 Uiso 1 1 calc R . . N8 N 0.1575(3) 0.1208(3) 0.3138(2) 0.0324(15) Uani 1 1 d . . . H123 H 0.1285 0.1080 0.2750 0.039 Uiso 1 1 calc R . . H124 H 0.1482 0.0995 0.3374 0.039 Uiso 1 1 calc R . . N9 N 0.2303(3) 0.2042(3) 0.3025(2) 0.0353(15) Uani 1 1 d . . . H125 H 0.2020 0.1923 0.2636 0.042 Uiso 1 1 calc R . . H126 H 0.2689 0.2380 0.3185 0.042 Uiso 1 1 calc R . . C110 C 0.2142(6) 0.2012(6) 0.8395(4) 0.084(3) Uani 1 1 d . . . N10 N 0.1554(4) 0.1530(4) 0.8153(3) 0.085(3) Uani 1 1 d . . . H127 H 0.1194 0.1490 0.7798 0.103 Uiso 1 1 calc R . . H128 H 0.1515 0.1244 0.8345 0.103 Uiso 1 1 calc R . . N11 N 0.2216(5) 0.2451(5) 0.8117(4) 0.128(4) Uani 1 1 d . . . H129 H 0.1861 0.2418 0.7761 0.153 Uiso 1 1 calc R . . H130 H 0.2619 0.2775 0.8288 0.153 Uiso 1 1 calc R . . N12 N 0.2690(5) 0.2075(5) 0.8936(4) 0.135(4) Uani 1 1 d . . . H131 H 0.2650 0.1788 0.9127 0.162 Uiso 1 1 calc R . . H132 H 0.3090 0.2402 0.9100 0.162 Uiso 1 1 calc R . . Cl1 Cl 0.07189(11) 0.18429(12) 0.69114(9) 0.0582(6) Uani 1 1 d . . . Cl2 Cl 0.19816(11) 0.08163(12) -0.08252(9) 0.0634(7) Uani 1 1 d . . . Cl3 Cl -0.13520(13) 0.32488(15) 0.38802(13) 0.0986(10) Uani 0.787(7) 1 d PD C 1 Cl4 Cl 0.00063(17) 0.40787(16) 0.48495(16) 0.0720(12) Uani 0.787(7) 1 d PD C 1 Cl5 Cl -0.04564(19) 0.4314(2) 0.37038(18) 0.0873(16) Uani 0.787(7) 1 d PD C 1 C111 C -0.0422(5) 0.3707(5) 0.4073(5) 0.057(3) Uani 0.787(7) 1 d PD C 1 H133 H -0.0063 0.3384 0.3945 0.068 Uiso 0.787(7) 1 calc PR C 1 Cl6 Cl -0.13520(13) 0.32488(15) 0.38802(13) 0.0986(10) Uani 0.213(7) 1 d PDU C 2 Cl7 Cl -0.0939(13) 0.3790(12) 0.3173(11) 0.162(8) Uani 0.213(7) 1 d PDU C 2 Cl8 Cl -0.0177(13) 0.4261(13) 0.4426(12) 0.193(10) Uani 0.213(7) 1 d PDU C 2 C112 C -0.0506(15) 0.3552(17) 0.3801(13) 0.134(8) Uani 0.213(7) 1 d PDU C 2 H134 H -0.0107 0.3231 0.3767 0.161 Uiso 0.213(7) 1 calc PR C 2 Cl9 Cl 0.5060(9) 0.0150(10) 0.7681(9) 0.129(5) Uani 0.20 1 d PDU D 2 Cl10 Cl 0.5787(14) 0.1058(12) 0.7354(11) 0.162(8) Uani 0.20 1 d PDU D 2 Cl11 Cl 0.4494(13) 0.0101(13) 0.6485(9) 0.182(8) Uani 0.20 1 d PDU D 2 C113 C 0.5347(19) 0.0249(18) 0.7108(12) 0.143(11) Uani 0.20 1 d PDU D 2 H135 H 0.5732 -0.0070 0.7021 0.172 Uiso 0.20 1 calc PR D 2 Cl12 Cl -0.2975(15) 0.3182(15) 0.1824(15) 0.173(9) Uani 0.15 1 d PDU E 2 Cl13 Cl -0.1690(18) 0.4055(14) 0.1924(16) 0.196(11) Uani 0.15 1 d PDU E 2 Cl14 Cl -0.1421(16) 0.2806(15) 0.2110(13) 0.141(8) Uani 0.15 1 d PDU E 2 C114 C -0.2081(18) 0.3230(18) 0.171(2) 0.131(11) Uani 0.15 1 d PDU E 2 H136 H -0.2176 0.3021 0.1269 0.157 Uiso 0.15 1 calc PR E 2 Cl15 Cl -0.3685(17) 0.3202(15) 0.1727(13) 0.179(9) Uani 0.15 1 d PDU F 3 Cl16 Cl -0.368(2) 0.3448(19) 0.0698(14) 0.250(13) Uani 0.15 1 d PDU F 3 Cl17 Cl -0.279(2) 0.4339(17) 0.1809(16) 0.251(13) Uani 0.15 1 d PDU F 3 C115 C -0.369(3) 0.383(2) 0.1414(18) 0.252(16) Uani 0.15 1 d PDU F 3 H137 H -0.4162 0.4087 0.1413 0.302 Uiso 0.15 1 calc PR F 3 S1 S 0.62779(19) 0.34292(19) 0.68034(17) 0.0905(12) Uani 0.80 1 d PDU G 1 O13 O 0.5961(8) 0.3997(8) 0.6574(5) 0.081(3) Uani 0.80 1 d PDU G 1 C116 C 0.5489(7) 0.2924(6) 0.6707(7) 0.096(4) Uani 0.80 1 d PDU G 1 H138 H 0.5218 0.2691 0.6275 0.145 Uiso 0.80 1 calc PR G 1 H139 H 0.5120 0.3186 0.6871 0.145 Uiso 0.80 1 calc PR G 1 H140 H 0.5662 0.2595 0.6920 0.145 Uiso 0.80 1 calc PR G 1 C117 C 0.6440(10) 0.3688(9) 0.7583(6) 0.135(5) Uani 0.80 1 d PDU G 1 H141 H 0.6919 0.4020 0.7799 0.202 Uiso 0.80 1 calc PR G 1 H142 H 0.6516 0.3300 0.7731 0.202 Uiso 0.80 1 calc PR G 1 H143 H 0.5977 0.3888 0.7655 0.202 Uiso 0.80 1 calc PR G 1 S2 S 0.5656(12) 0.3864(14) 0.7058(13) 0.179(8) Uani 0.20 1 d PDU H 2 O14 O 0.584(3) 0.393(3) 0.6529(18) 0.098(9) Uani 0.20 1 d PDU H 2 C118 C 0.523(3) 0.439(3) 0.743(2) 0.191(13) Uani 0.20 1 d PDU H 2 H144 H 0.4686 0.4394 0.7163 0.286 Uiso 0.20 1 calc PR H 2 H145 H 0.5534 0.4832 0.7575 0.286 Uiso 0.20 1 calc PR H 2 H146 H 0.5204 0.4251 0.7771 0.286 Uiso 0.20 1 calc PR H 2 C119 C 0.660(2) 0.430(4) 0.764(2) 0.162(13) Uani 0.20 1 d PDU H 2 H147 H 0.7037 0.4055 0.7572 0.242 Uiso 0.20 1 calc PR H 2 H148 H 0.6579 0.4332 0.8037 0.242 Uiso 0.20 1 calc PR H 2 H149 H 0.6684 0.4753 0.7613 0.242 Uiso 0.20 1 calc PR H 2 S3 S 0.712(3) 0.169(2) 1.0748(18) 0.220(13) Uani 0.15 1 d PDU I 2 O15 O 0.663(4) 0.102(3) 1.048(4) 0.178(17) Uani 0.15 1 d PDU I 2 C120 C 0.753(5) 0.189(5) 1.031(4) 0.19(2) Uani 0.15 1 d PDU I 2 H150 H 0.8060 0.1734 1.0388 0.281 Uiso 0.15 1 calc PR I 2 H151 H 0.7589 0.2373 1.0401 0.281 Uiso 0.15 1 calc PR I 2 H152 H 0.7195 0.1669 0.9891 0.281 Uiso 0.15 1 calc PR I 2 C121 C 0.636(4) 0.222(3) 1.054(4) 0.151(18) Uani 0.15 1 d PDU I 2 H153 H 0.5878 0.2067 1.0604 0.226 Uiso 0.15 1 calc PR I 2 H154 H 0.6237 0.2189 1.0120 0.226 Uiso 0.15 1 calc PR I 2 H155 H 0.6557 0.2682 1.0801 0.226 Uiso 0.15 1 calc PR I 2 S4 S 0.4451(8) 0.3363(8) 0.8776(7) 0.186(6) Uani 0.35 1 d PDU J 1 O16 O 0.3645(15) 0.3168(18) 0.8766(15) 0.193(10) Uani 0.35 1 d PDU J 1 C122 C 0.450(2) 0.353(2) 0.8187(14) 0.150(11) Uani 0.35 1 d PDU J 1 H156 H 0.4189 0.3165 0.7822 0.225 Uiso 0.35 1 calc PR J 1 H157 H 0.5062 0.3570 0.8211 0.225 Uiso 0.35 1 calc PR J 1 H158 H 0.4288 0.3949 0.8171 0.225 Uiso 0.35 1 calc PR J 1 C123 C 0.449(3) 0.4271(13) 0.911(2) 0.223(13) Uani 0.35 1 d PDU J 1 H159 H 0.4623 0.4381 0.9551 0.334 Uiso 0.35 1 calc PR J 1 H160 H 0.3962 0.4406 0.8938 0.334 Uiso 0.35 1 calc PR J 1 H161 H 0.4891 0.4510 0.9028 0.334 Uiso 0.35 1 calc PR J 1 S5 S 0.3918(11) 0.4037(11) 0.8523(10) 0.209(8) Uani 0.30 1 d PDU K 2 O17 O 0.3337(19) 0.366(2) 0.8679(16) 0.189(11) Uani 0.30 1 d PDU K 2 C124 C 0.431(3) 0.359(3) 0.805(2) 0.221(18) Uani 0.30 1 d PDU K 2 H162 H 0.3988 0.3585 0.7637 0.331 Uiso 0.30 1 calc PR K 2 H163 H 0.4306 0.3136 0.8069 0.331 Uiso 0.30 1 calc PR K 2 H164 H 0.4856 0.3793 0.8151 0.331 Uiso 0.30 1 calc PR K 2 C125 C 0.484(2) 0.391(4) 0.908(2) 0.232(14) Uani 0.30 1 d PDU K 2 H165 H 0.4837 0.4136 0.9494 0.348 Uiso 0.30 1 calc PR K 2 H166 H 0.5307 0.4107 0.9035 0.348 Uiso 0.30 1 calc PR K 2 H167 H 0.4856 0.3434 0.9023 0.348 Uiso 0.30 1 calc PR K 2 C126 C 0.4238(5) 0.2852(5) 0.2650(4) 0.083(3) Uani 1 1 d D . . H168 H 0.3931 0.2432 0.2595 0.125 Uiso 1 1 calc R . . H169 H 0.4168 0.2903 0.2254 0.125 Uiso 1 1 calc R . . H170 H 0.4047 0.3228 0.2888 0.125 Uiso 1 1 calc R . . C127 C 0.5107(5) 0.2842(5) 0.2977(4) 0.076(3) Uani 1 1 d D . . O18 O 0.5404(4) 0.2377(4) 0.3143(3) 0.098(2) Uani 1 1 d D . . O19 O 0.5555(3) 0.3409(3) 0.3064(3) 0.0712(18) Uani 1 1 d D . . C128 C 0.6406(5) 0.3437(5) 0.3365(5) 0.082(3) Uani 1 1 d D . . H171 H 0.6621 0.3063 0.3137 0.098 Uiso 1 1 calc R . . H172 H 0.6522 0.3414 0.3780 0.098 Uiso 1 1 calc R . . C129 C 0.6759(5) 0.4093(5) 0.3379(5) 0.093(4) Uani 1 1 d D . . H173 H 0.7341 0.4148 0.3577 0.140 Uiso 1 1 calc R . . H174 H 0.6537 0.4456 0.3606 0.140 Uiso 1 1 calc R . . H175 H 0.6631 0.4107 0.2965 0.140 Uiso 1 1 calc R . . C130 C 0.7072(6) 0.1986(5) 0.4304(4) 0.077(3) Uani 1 1 d . . . H176 H 0.7224 0.1593 0.4430 0.115 Uiso 1 1 calc R . . H177 H 0.7234 0.1977 0.3958 0.115 Uiso 1 1 calc R . . H178 H 0.6491 0.1982 0.4188 0.115 Uiso 1 1 calc R . . C131 C 0.7466(5) 0.2588(6) 0.4800(5) 0.071(3) Uani 1 1 d . . . O20 O 0.7403(3) 0.3171(4) 0.4797(3) 0.090(2) Uani 1 1 d . . . O21 O 0.7927(3) 0.2477(3) 0.5308(3) 0.0670(17) Uani 1 1 d . . . C132 C 0.8343(6) 0.3057(6) 0.5820(5) 0.089(3) Uani 1 1 d . . . H179 H 0.7954 0.3305 0.5977 0.107 Uiso 1 1 calc R . . H180 H 0.8638 0.3359 0.5694 0.107 Uiso 1 1 calc R . . C133 C 0.8909(6) 0.2834(5) 0.6296(4) 0.078(3) Uani 1 1 d . . . H181 H 0.9191 0.3224 0.6647 0.117 Uiso 1 1 calc R . . H182 H 0.9298 0.2595 0.6140 0.117 Uiso 1 1 calc R . . H183 H 0.8614 0.2534 0.6418 0.117 Uiso 1 1 calc R . . C134 C 0.2021(8) 0.2886(7) 0.1841(5) 0.096(4) Uani 0.75 1 d PDU L 7 H184 H 0.1440 0.2760 0.1688 0.144 Uiso 0.75 1 calc PR L 7 H185 H 0.2160 0.3330 0.2146 0.144 Uiso 0.75 1 calc PR L 7 H186 H 0.2285 0.2558 0.2024 0.144 Uiso 0.75 1 calc PR L 7 C135 C 0.2285(9) 0.2902(9) 0.1346(6) 0.126(5) Uani 0.75 1 d PDU L 7 O22 O 0.2962(7) 0.3012(9) 0.1328(6) 0.187(5) Uani 0.75 1 d PDU L 7 O23 O 0.1650(6) 0.2662(5) 0.0801(4) 0.120(3) Uani 0.75 1 d PDU L 7 C136 C 0.1865(9) 0.2611(9) 0.0264(6) 0.132(6) Uani 0.75 1 d PDU L 7 H187 H 0.2157 0.3041 0.0312 0.158 Uiso 0.75 1 calc PR L 7 H188 H 0.2215 0.2257 0.0210 0.158 Uiso 0.75 1 calc PR L 7 C137 C 0.1135(8) 0.2449(7) -0.0254(5) 0.105(5) Uani 0.75 1 d PDU L 7 H189 H 0.1262 0.2417 -0.0618 0.157 Uiso 0.75 1 calc PR L 7 H190 H 0.0791 0.2801 -0.0194 0.157 Uiso 0.75 1 calc PR L 7 H191 H 0.0855 0.2020 -0.0300 0.157 Uiso 0.75 1 calc PR L 7 C138 C 0.5696(10) 0.2058(10) 0.8218(8) 0.151(5) Uani 0.80 1 d PU M 1 H192 H 0.5556 0.1852 0.8488 0.227 Uiso 0.80 1 calc PR M 1 H193 H 0.5363 0.2414 0.8159 0.227 Uiso 0.80 1 calc PR M 1 H194 H 0.6261 0.2249 0.8398 0.227 Uiso 0.80 1 calc PR M 1 C139 C 0.5554(8) 0.1541(11) 0.7622(9) 0.103(4) Uani 0.80 1 d PU M 1 O24 O 0.5720(7) 0.1627(7) 0.7233(5) 0.141(4) Uani 0.80 1 d PU M 1 O25 O 0.5263(7) 0.0940(7) 0.7594(5) 0.122(3) Uani 0.80 1 d PU M 1 C140 C 0.5156(7) 0.0377(9) 0.7020(7) 0.101(4) Uani 0.80 1 d PU M 1 H195 H 0.5684 0.0238 0.7024 0.122 Uiso 0.80 1 calc PR M 1 H196 H 0.4932 0.0539 0.6668 0.122 Uiso 0.80 1 calc PR M 1 C141 C 0.4588(8) -0.0239(7) 0.6950(7) 0.097(3) Uani 0.80 1 d PU M 1 H197 H 0.4530 -0.0593 0.6574 0.145 Uiso 0.80 1 calc PR M 1 H198 H 0.4062 -0.0105 0.6940 0.145 Uiso 0.80 1 calc PR M 1 H199 H 0.4813 -0.0407 0.7294 0.145 Uiso 0.80 1 calc PR M 1 C142 C 0.4466(8) 0.1212(8) 0.8842(6) 0.118(5) Uani 0.75 1 d PDU N 1 H200 H 0.4641 0.0770 0.8734 0.177 Uiso 0.75 1 calc PR N 1 H201 H 0.4375 0.1396 0.8506 0.177 Uiso 0.75 1 calc PR N 1 H202 H 0.3968 0.1171 0.8925 0.177 Uiso 0.75 1 calc PR N 1 C143 C 0.5089(9) 0.1662(8) 0.9387(6) 0.112(5) Uani 0.75 1 d PDU N 1 O26 O 0.4999(11) 0.2226(7) 0.9615(6) 0.205(6) Uani 0.75 1 d PDU N 1 O27 O 0.5665(5) 0.1346(6) 0.9659(4) 0.115(3) Uani 0.75 1 d PDU N 1 C144 C 0.6287(7) 0.1703(8) 1.0247(6) 0.103(4) Uani 0.75 1 d PDU N 1 H203 H 0.6667 0.2011 1.0195 0.124 Uiso 0.75 1 calc PR N 1 H204 H 0.6041 0.1968 1.0532 0.124 Uiso 0.75 1 calc PR N 1 C145 C 0.6704(8) 0.1192(9) 1.0480(8) 0.095(5) Uani 0.75 1 d PDU N 1 H205 H 0.7124 0.1410 1.0872 0.142 Uiso 0.75 1 calc PR N 1 H206 H 0.6944 0.0934 1.0194 0.142 Uiso 0.75 1 calc PR N 1 H207 H 0.6321 0.0891 1.0530 0.142 Uiso 0.75 1 calc PR N 1 C146 C 0.288(2) 0.0986(16) 0.7018(15) 0.082(8) Uani 0.50 1 d PDU O 1 H208 H 0.2543 0.0671 0.6629 0.124 Uiso 0.50 1 calc PR O 1 H209 H 0.2550 0.1183 0.7254 0.124 Uiso 0.50 1 calc PR O 1 H210 H 0.3271 0.0748 0.7241 0.124 Uiso 0.50 1 calc PR O 1 C147 C 0.331(2) 0.1525(14) 0.6911(11) 0.072(5) Uani 0.50 1 d PDU O 1 O28 O 0.3715(8) 0.2051(8) 0.7287(7) 0.106(5) Uani 0.50 1 d PDU O 1 O29 O 0.3308(16) 0.1322(9) 0.6333(9) 0.061(5) Uani 0.50 1 d PDU O 1 C148 C 0.372(3) 0.1783(12) 0.6153(12) 0.063(8) Uani 0.50 1 d PDU O 1 H211 H 0.4299 0.1867 0.6401 0.076 Uiso 0.50 1 calc PR O 1 H212 H 0.3504 0.2215 0.6221 0.076 Uiso 0.50 1 calc PR O 1 C149 C 0.3623(17) 0.1497(15) 0.5514(9) 0.057(6) Uani 0.50 1 d PDU O 1 H213 H 0.3887 0.1816 0.5390 0.085 Uiso 0.50 1 calc PR O 1 H214 H 0.3052 0.1404 0.5271 0.085 Uiso 0.50 1 calc PR O 1 H215 H 0.3864 0.1080 0.5453 0.085 Uiso 0.50 1 calc PR O 1 C150 C 0.356(3) 0.1411(19) 0.5565(13) 0.095(10) Uani 0.50 1 d PDU P 2 H216 H 0.3471 0.0927 0.5489 0.142 Uiso 0.50 1 calc PR P 2 H217 H 0.4069 0.1533 0.5531 0.142 Uiso 0.50 1 calc PR P 2 H218 H 0.3123 0.1538 0.5268 0.142 Uiso 0.50 1 calc PR P 2 C151 C 0.356(3) 0.1767(13) 0.6184(15) 0.084(7) Uani 0.50 1 d PDU P 2 O30 O 0.3757(9) 0.2369(9) 0.6469(7) 0.116(5) Uani 0.50 1 d PDU P 2 O31 O 0.325(2) 0.1345(12) 0.6399(11) 0.089(7) Uani 0.50 1 d PDU P 2 C152 C 0.321(3) 0.1611(16) 0.7009(13) 0.096(11) Uani 0.50 1 d PDU P 2 H219 H 0.2871 0.1975 0.7026 0.115 Uiso 0.50 1 calc PR P 2 H220 H 0.3757 0.1796 0.7305 0.115 Uiso 0.50 1 calc PR P 2 C153 C 0.288(3) 0.106(2) 0.7154(17) 0.099(11) Uani 0.50 1 d PDU P 2 H221 H 0.2890 0.1222 0.7572 0.148 Uiso 0.50 1 calc PR P 2 H222 H 0.3204 0.0692 0.7110 0.148 Uiso 0.50 1 calc PR P 2 H223 H 0.2329 0.0906 0.6878 0.148 Uiso 0.50 1 calc PR P 2 C154 C -0.0377(10) 0.2605(8) 0.0760(10) 0.130(5) Uani 0.65 1 d PDU Q 1 H224 H 0.0046 0.2897 0.1119 0.196 Uiso 0.65 1 calc PR Q 1 H225 H -0.0500 0.2809 0.0436 0.196 Uiso 0.65 1 calc PR Q 1 H226 H -0.0197 0.2169 0.0626 0.196 Uiso 0.65 1 calc PR Q 1 C155 C -0.1100(11) 0.2512(10) 0.0909(9) 0.141(6) Uani 0.65 1 d PDU Q 1 O32 O -0.1773(8) 0.2171(8) 0.0623(7) 0.169(6) Uani 0.65 1 d PDU Q 1 O33 O -0.0877(8) 0.2798(8) 0.1518(7) 0.155(5) Uani 0.65 1 d PDU Q 1 C156 C -0.1537(13) 0.2710(12) 0.1737(11) 0.149(7) Uani 0.65 1 d PDU Q 1 H227 H -0.2059 0.2725 0.1437 0.178 Uiso 0.65 1 calc PR Q 1 H228 H -0.1551 0.2279 0.1823 0.178 Uiso 0.65 1 calc PR Q 1 C157 C -0.135(2) 0.3274(18) 0.2289(13) 0.248(14) Uani 0.65 1 d PDU Q 1 H229 H -0.1761 0.3252 0.2472 0.372 Uiso 0.65 1 calc PR Q 1 H230 H -0.1343 0.3694 0.2193 0.372 Uiso 0.65 1 calc PR Q 1 H231 H -0.0827 0.3255 0.2575 0.372 Uiso 0.65 1 calc PR Q 1 C158 C 0.129(3) 0.312(2) 0.894(3) 0.114(15) Uani 0.15 1 d PDU R 1 H232 H 0.1773 0.3008 0.8849 0.171 Uiso 0.15 1 calc PR R 1 H233 H 0.0838 0.2779 0.8665 0.171 Uiso 0.15 1 calc PR R 1 H234 H 0.1372 0.3141 0.9360 0.171 Uiso 0.15 1 calc PR R 1 C159 C 0.111(2) 0.3773(18) 0.8867(15) 0.131(13) Uani 0.15 1 d PDU R 1 O34 O 0.060(2) 0.413(2) 0.897(2) 0.117(12) Uani 0.15 1 d PDU R 1 O35 O 0.161(2) 0.4038(18) 0.8644(18) 0.127(12) Uani 0.15 1 d PDU R 1 C160 C 0.139(2) 0.4685(19) 0.8589(19) 0.099(12) Uani 0.15 1 d PDU R 1 H235 H 0.0822 0.4616 0.8319 0.119 Uiso 0.15 1 calc PR R 1 H236 H 0.1420 0.4979 0.8992 0.119 Uiso 0.15 1 calc PR R 1 C161 C 0.186(3) 0.503(3) 0.836(3) 0.095(17) Uani 0.15 1 d PDU R 1 H237 H 0.1643 0.5445 0.8325 0.143 Uiso 0.15 1 calc PR R 1 H238 H 0.1836 0.4744 0.7961 0.143 Uiso 0.15 1 calc PR R 1 H239 H 0.2413 0.5132 0.8638 0.143 Uiso 0.15 1 calc PR R 1 C162 C 0.101(2) 0.514(3) 1.076(3) 0.171(14) Uani 0.20 1 d PDU S 1 H240 H 0.0914 0.5577 1.0694 0.257 Uiso 0.20 1 calc PR S 1 H241 H 0.0877 0.5134 1.1117 0.257 Uiso 0.20 1 calc PR S 1 H242 H 0.0663 0.4784 1.0405 0.257 Uiso 0.20 1 calc PR S 1 C163 C 0.185(2) 0.505(2) 1.0863(14) 0.160(12) Uani 0.20 1 d PDU S 1 O36 O 0.223(2) 0.458(2) 1.094(2) 0.158(11) Uani 0.20 1 d PDU S 1 O37 O 0.220(3) 0.5626(19) 1.0859(15) 0.195(12) Uani 0.20 1 d PDU S 1 C164 C 0.305(3) 0.571(3) 1.095(2) 0.205(16) Uani 0.20 1 d PDU S 1 H243 H 0.3172 0.5372 1.0626 0.246 Uiso 0.20 1 calc PR S 1 H244 H 0.3377 0.5680 1.1347 0.246 Uiso 0.20 1 calc PR S 1 C165 C 0.319(4) 0.638(3) 1.091(3) 0.19(2) Uani 0.20 1 d PDU S 1 H245 H 0.3759 0.6497 1.0994 0.279 Uiso 0.20 1 calc PR S 1 H246 H 0.3024 0.6707 1.1215 0.279 Uiso 0.20 1 calc PR S 1 H247 H 0.2877 0.6397 1.0509 0.279 Uiso 0.20 1 calc PR S 1 O38 O 0.5310(18) 0.5214(14) 0.7373(10) 0.162(10) Uani 0.40 1 d PU T 1 O39 O 0.4829(16) 0.5221(15) 0.7715(15) 0.186(11) Uani 0.40 1 d PU U 3 O40 O 0.0804(7) 0.3635(8) 0.8216(7) 0.115(5) Uani 0.50 1 d PU V 2 O41 O 0.178(2) 0.554(2) 0.850(2) 0.189(17) Uani 0.25 1 d PU W 4 O42 O 0.401(2) 0.381(2) 1.0459(18) 0.256(16) Uani 0.40 1 d PU X 1 O43 O 0.424(3) 0.317(2) 1.086(2) 0.33(2) Uani 0.40 1 d PU Y 2 O44 O 0.040(3) 0.555(2) 1.0705(17) 0.208(16) Uani 0.30 1 d PU Z 2 O45 O 0.028(4) 0.589(3) 1.005(3) 0.21(2) Uani 0.20 1 d PU A 3 O46 O 0.330(7) 0.503(6) 1.055(5) 0.30(5) Uani 0.15 1 d PU B 5 O47 O 0.547(2) 0.537(2) 0.8024(16) 0.115(13) Uani 0.20 1 d PU C 4 O48 O 0.405(2) 0.303(2) 0.956(2) 0.179(16) Uani 0.25 1 d PU D 3 O49 O -0.102(2) 0.2552(19) 0.0130(18) 0.155(14) Uani 0.25 1 d PU E 2 O50 O 0.295(2) 0.694(2) 1.0273(19) 0.205(15) Uani 0.30 1 d PU F 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 0.0182(4) 0.0488(7) 0.0223(5) 0.0137(5) 0.0029(3) -0.0016(4) Ni2 0.0210(4) 0.0377(6) 0.0335(5) 0.0147(5) 0.0044(4) -0.0029(4) Ni3 0.0233(4) 0.0368(6) 0.0230(5) 0.0099(5) 0.0068(4) -0.0018(4) C1 0.026(3) 0.035(5) 0.027(4) 0.013(4) 0.009(3) 0.005(3) C2 0.026(3) 0.038(5) 0.018(3) 0.011(4) 0.009(3) 0.004(3) C3 0.021(3) 0.042(5) 0.032(4) 0.018(4) 0.010(3) 0.005(3) C4 0.022(3) 0.037(5) 0.024(4) 0.009(4) 0.008(3) 0.004(3) C5 0.021(3) 0.050(5) 0.022(4) 0.016(4) 0.008(3) 0.005(3) C6 0.023(3) 0.041(5) 0.030(4) 0.015(4) 0.008(3) 0.005(3) C7 0.022(3) 0.036(5) 0.039(4) 0.015(4) 0.010(3) 0.008(3) C8 0.021(3) 0.034(5) 0.029(4) 0.009(4) 0.006(3) 0.000(3) C9 0.023(3) 0.035(5) 0.025(4) 0.009(4) 0.004(3) 0.005(3) C10 0.020(3) 0.039(5) 0.030(4) 0.011(4) 0.008(3) -0.001(3) C11 0.018(3) 0.037(5) 0.028(4) 0.011(4) 0.007(3) 0.005(3) C12 0.016(3) 0.042(5) 0.029(4) 0.017(4) 0.002(3) 0.001(3) C13 0.028(3) 0.047(5) 0.017(4) 0.008(4) 0.005(3) -0.001(3) C14 0.029(3) 0.041(5) 0.025(4) 0.011(4) 0.013(3) 0.003(3) C15 0.023(3) 0.068(6) 0.031(4) 0.023(4) 0.011(3) 0.003(3) C16 0.030(3) 0.078(6) 0.028(4) 0.023(5) 0.008(3) 0.002(4) C17 0.028(3) 0.093(7) 0.035(4) 0.028(5) 0.014(3) 0.004(4) C18 0.023(3) 0.082(7) 0.028(4) 0.025(5) 0.001(3) -0.005(4) O1 0.020(2) 0.051(3) 0.028(3) 0.015(3) 0.0057(19) 0.002(2) C19 0.025(4) 0.163(10) 0.039(5) 0.045(6) 0.013(4) -0.002(5) C20 0.057(5) 0.204(14) 0.073(7) 0.054(9) 0.037(5) 0.051(7) C21 0.036(4) 0.265(17) 0.074(7) 0.077(10) 0.011(5) -0.040(7) C22 0.029(4) 0.327(18) 0.061(6) 0.100(10) 0.020(4) 0.011(7) C23 0.029(3) 0.053(5) 0.028(4) 0.017(4) 0.010(3) 0.006(3) N1 0.020(2) 0.044(4) 0.025(3) 0.012(3) 0.007(2) 0.004(2) C24 0.022(3) 0.038(5) 0.026(4) 0.012(4) 0.009(3) 0.006(3) C25 0.022(3) 0.043(5) 0.025(4) 0.015(4) 0.008(3) 0.001(3) C26 0.033(3) 0.049(5) 0.018(4) 0.006(4) 0.007(3) 0.005(3) C27 0.025(3) 0.045(5) 0.026(4) 0.011(4) 0.006(3) 0.003(3) C28 0.024(3) 0.043(5) 0.032(4) 0.012(4) 0.010(3) 0.001(3) C29 0.030(3) 0.033(5) 0.016(4) 0.004(4) 0.007(3) 0.005(3) O2 0.027(2) 0.073(4) 0.019(3) 0.014(3) 0.009(2) 0.004(2) C30 0.037(4) 0.071(6) 0.024(4) 0.012(4) 0.015(3) 0.014(4) O3 0.022(2) 0.072(4) 0.024(3) 0.014(3) -0.0006(19) 0.003(2) C31 0.024(3) 0.089(7) 0.031(4) 0.014(5) 0.005(3) 0.009(4) N2 0.022(3) 0.050(4) 0.025(3) 0.014(3) 0.009(2) -0.004(3) C32 0.020(3) 0.056(5) 0.024(4) 0.014(4) 0.001(3) 0.000(3) C33 0.022(3) 0.047(5) 0.023(4) 0.012(4) 0.005(3) -0.000(3) C34 0.023(3) 0.045(5) 0.033(4) 0.021(4) 0.009(3) 0.005(3) C35 0.018(3) 0.046(5) 0.026(4) 0.015(4) 0.008(3) 0.007(3) C36 0.025(3) 0.052(5) 0.023(4) 0.013(4) 0.009(3) 0.005(3) C37 0.025(3) 0.049(5) 0.030(4) 0.016(4) 0.013(3) 0.004(3) C38 0.018(3) 0.059(6) 0.032(4) 0.020(4) 0.007(3) -0.002(3) O4 0.0173(19) 0.042(3) 0.025(2) 0.009(3) 0.0063(18) -0.0033(19) C39 0.016(3) 0.075(6) 0.029(4) 0.019(4) 0.010(3) 0.003(3) C40 0.033(4) 0.091(8) 0.041(5) 0.010(5) 0.013(4) -0.018(4) C41 0.032(4) 0.086(7) 0.061(6) 0.021(6) 0.024(4) 0.010(4) C42 0.032(4) 0.092(7) 0.043(5) 0.028(5) 0.016(3) -0.009(4) C43 0.018(3) 0.049(5) 0.022(4) 0.011(4) 0.006(3) 0.001(3) C44 0.023(3) 0.041(5) 0.029(4) 0.018(4) 0.008(3) 0.003(3) C45 0.025(3) 0.038(5) 0.030(4) 0.010(4) 0.004(3) -0.002(3) C46 0.022(3) 0.048(5) 0.024(4) 0.014(4) 0.002(3) -0.002(3) C47 0.021(3) 0.047(5) 0.030(4) 0.019(4) 0.006(3) 0.001(3) C48 0.024(3) 0.024(4) 0.026(4) 0.002(4) 0.006(3) -0.006(3) O5 0.0197(19) 0.038(3) 0.034(3) 0.015(3) 0.0016(19) -0.004(2) C49 0.025(3) 0.042(5) 0.031(4) 0.011(4) -0.006(3) -0.001(3) C50 0.038(4) 0.058(6) 0.051(5) 0.020(5) 0.004(4) 0.016(4) C51 0.040(4) 0.049(5) 0.040(4) 0.024(5) -0.001(3) -0.003(4) C52 0.043(4) 0.051(6) 0.042(5) 0.016(5) -0.010(4) 0.001(4) C53 0.020(3) 0.043(5) 0.030(4) 0.012(4) -0.000(3) 0.002(3) N3 0.021(2) 0.029(4) 0.040(3) 0.013(3) 0.009(2) -0.001(2) C54 0.027(3) 0.030(5) 0.027(4) 0.003(4) 0.010(3) 0.002(3) C55 0.021(3) 0.036(5) 0.032(4) 0.011(4) 0.006(3) -0.006(3) C56 0.022(3) 0.046(5) 0.031(4) 0.007(4) 0.008(3) -0.005(3) C57 0.037(4) 0.026(5) 0.034(4) 0.005(4) 0.015(3) -0.003(3) C58 0.026(3) 0.042(5) 0.032(4) 0.011(4) 0.007(3) -0.001(3) C59 0.022(3) 0.034(5) 0.032(4) 0.009(4) 0.010(3) -0.008(3) O6 0.026(2) 0.046(4) 0.057(3) 0.017(3) 0.004(2) -0.006(2) C60 0.027(3) 0.051(6) 0.078(6) 0.016(5) 0.009(4) -0.003(4) O7 0.033(2) 0.043(3) 0.050(3) 0.017(3) 0.014(2) -0.004(2) C61 0.039(4) 0.047(6) 0.077(6) 0.030(5) 0.017(4) -0.004(4) N4 0.024(3) 0.047(4) 0.029(3) 0.013(3) 0.007(2) -0.003(3) C62 0.029(3) 0.038(5) 0.038(4) 0.015(4) 0.011(3) -0.001(3) C63 0.027(3) 0.040(5) 0.034(4) 0.015(4) 0.010(3) 0.002(3) C64 0.024(3) 0.034(5) 0.025(4) 0.008(4) 0.006(3) 0.000(3) C65 0.028(3) 0.034(5) 0.029(4) 0.009(4) 0.009(3) 0.000(3) C66 0.024(3) 0.033(5) 0.037(4) 0.009(4) 0.006(3) 0.001(3) C67 0.030(3) 0.043(5) 0.040(4) 0.019(4) 0.002(3) -0.000(3) C68 0.035(3) 0.045(5) 0.040(4) 0.021(4) 0.006(3) -0.003(3) O8 0.0206(19) 0.033(3) 0.042(3) 0.018(3) 0.0076(19) -0.0030(19) C69 0.037(4) 0.046(6) 0.057(5) 0.025(5) 0.004(4) -0.001(4) C70 0.048(4) 0.069(6) 0.072(6) 0.049(6) 0.013(4) 0.008(4) C71 0.044(4) 0.064(7) 0.100(7) 0.045(6) 0.023(5) 0.016(4) C72 0.073(5) 0.070(7) 0.052(6) 0.026(6) -0.008(5) 0.003(5) C73 0.022(3) 0.031(5) 0.018(4) 0.007(4) 0.004(3) -0.003(3) C74 0.014(3) 0.045(5) 0.029(4) 0.021(4) 0.006(3) 0.001(3) C75 0.015(3) 0.028(5) 0.027(4) 0.005(4) 0.006(3) -0.005(3) C76 0.022(3) 0.029(5) 0.031(4) 0.005(4) -0.005(3) -0.009(3) C77 0.029(3) 0.048(6) 0.023(4) 0.012(4) 0.010(3) 0.001(3) C78 0.024(3) 0.040(5) 0.022(4) 0.009(4) 0.006(3) 0.002(3) O9 0.029(2) 0.030(3) 0.029(3) 0.007(3) 0.010(2) 0.002(2) C79 0.043(3) 0.043(5) 0.028(4) 0.005(4) 0.012(3) -0.004(3) C80 0.099(7) 0.065(9) 0.064(8) -0.003(7) 0.057(6) -0.020(7) C81 0.063(4) 0.079(10) 0.053(8) 0.007(7) -0.014(4) -0.007(6) C82 0.086(9) 0.048(7) 0.046(7) 0.015(6) 0.026(6) 0.004(6) C83 0.090(17) 0.089(18) 0.030(10) 0.012(13) 0.030(11) 0.006(12) C84 0.069(10) 0.074(18) 0.079(18) -0.000(14) 0.044(14) -0.023(9) C85 0.066(10) 0.087(19) 0.081(18) 0.009(14) 0.006(12) 0.027(11) C86 0.019(3) 0.037(5) 0.023(4) 0.006(4) 0.000(3) -0.005(3) N5 0.017(2) 0.050(4) 0.034(4) 0.023(4) 0.007(2) -0.005(3) C87 0.020(3) 0.037(5) 0.024(4) 0.009(4) 0.005(3) -0.001(3) C88 0.026(3) 0.036(5) 0.025(4) 0.007(4) 0.008(3) -0.005(3) C89 0.017(3) 0.039(5) 0.036(4) 0.014(4) 0.001(3) -0.006(3) C90 0.022(3) 0.035(5) 0.025(4) 0.008(4) 0.004(3) -0.005(3) C91 0.022(3) 0.037(5) 0.025(4) 0.004(4) 0.005(3) 0.001(3) C92 0.017(3) 0.042(5) 0.026(4) 0.016(4) 0.004(3) 0.000(3) O10 0.038(2) 0.043(4) 0.041(3) 0.017(3) 0.017(2) -0.008(2) C93 0.040(4) 0.043(6) 0.057(5) 0.022(5) 0.020(4) -0.006(4) O11 0.035(2) 0.053(4) 0.033(3) 0.018(3) 0.018(2) 0.001(2) C94 0.044(4) 0.053(6) 0.042(5) 0.024(5) 0.023(4) 0.005(4) N6 0.017(2) 0.033(4) 0.032(3) 0.012(4) 0.004(2) -0.005(3) C95 0.026(3) 0.036(5) 0.026(4) 0.010(4) 0.005(3) -0.005(3) C96 0.025(3) 0.036(5) 0.027(4) 0.010(4) 0.012(3) -0.006(3) C97 0.022(3) 0.042(5) 0.028(4) 0.008(4) 0.010(3) 0.000(3) C98 0.018(3) 0.031(5) 0.029(4) 0.004(4) 0.003(3) -0.008(3) C99 0.031(3) 0.030(5) 0.037(4) 0.010(4) 0.010(3) -0.007(3) C100 0.038(4) 0.043(6) 0.033(4) 0.004(5) 0.013(3) -0.007(4) C101 0.038(4) 0.039(5) 0.027(4) 0.006(4) 0.010(3) -0.004(4) O12 0.026(2) 0.043(4) 0.026(3) 0.012(3) 0.011(2) -0.001(2) C102 0.066(4) 0.053(6) 0.036(4) 0.005(5) 0.024(4) -0.007(3) C103 0.093(9) 0.053(9) 0.037(6) 0.001(7) 0.034(7) -0.011(7) C104 0.140(9) 0.076(12) 0.065(10) 0.013(8) 0.040(9) 0.043(9) C105 0.103(6) 0.085(12) 0.073(10) 0.002(9) 0.040(8) -0.050(7) C106 0.089(10) 0.095(19) 0.116(19) 0.012(14) 0.068(11) -0.007(11) C107 0.076(14) 0.046(11) 0.063(14) 0.004(11) 0.031(11) -0.009(9) C108 0.114(13) 0.080(17) 0.077(15) 0.022(13) -0.007(10) 0.008(15) C109 0.020(3) 0.039(5) 0.034(4) 0.009(4) 0.010(3) 0.004(3) N7 0.031(3) 0.043(4) 0.029(3) 0.011(3) 0.005(3) -0.006(3) N8 0.026(3) 0.045(4) 0.025(3) 0.014(3) 0.006(2) 0.000(3) N9 0.026(3) 0.050(4) 0.029(3) 0.017(3) 0.004(2) -0.003(3) C110 0.074(6) 0.110(10) 0.067(7) 0.041(7) 0.013(6) -0.021(6) N10 0.077(5) 0.105(7) 0.055(5) 0.021(5) 0.005(4) -0.041(5) N11 0.124(7) 0.141(10) 0.088(7) 0.056(7) -0.014(6) -0.057(7) N12 0.105(7) 0.169(11) 0.092(7) 0.061(8) -0.030(6) -0.052(7) Cl1 0.0515(11) 0.0741(17) 0.0545(13) 0.0184(13) 0.0279(10) -0.0041(11) Cl2 0.0562(11) 0.0878(19) 0.0409(12) 0.0173(14) 0.0129(10) 0.0022(11) Cl3 0.0639(14) 0.106(2) 0.108(2) 0.036(2) 0.0060(14) -0.0022(14) Cl4 0.0660(17) 0.062(2) 0.076(2) 0.016(2) 0.0149(16) 0.0005(15) Cl5 0.081(2) 0.095(3) 0.101(3) 0.053(3) 0.031(2) 0.017(2) C111 0.048(6) 0.034(8) 0.075(8) 0.004(7) 0.014(6) 0.001(5) Cl6 0.0639(14) 0.106(2) 0.108(2) 0.036(2) 0.0060(14) -0.0022(14) Cl7 0.186(15) 0.177(16) 0.184(12) 0.106(12) 0.098(11) 0.068(12) Cl8 0.158(14) 0.154(14) 0.211(14) 0.032(13) 0.019(13) -0.072(9) C112 0.144(18) 0.153(19) 0.133(15) 0.064(10) 0.070(14) -0.013(16) Cl9 0.102(9) 0.137(13) 0.158(10) 0.045(11) 0.061(9) 0.010(9) Cl10 0.183(14) 0.180(14) 0.156(14) 0.093(12) 0.068(11) 0.016(10) Cl11 0.173(13) 0.213(16) 0.156(10) 0.051(13) 0.059(11) 0.036(11) C113 0.15(2) 0.155(16) 0.141(15) 0.037(19) 0.077(9) 0.042(16) Cl12 0.166(11) 0.181(18) 0.194(19) 0.068(15) 0.083(14) 0.053(11) Cl13 0.210(18) 0.154(13) 0.21(2) 0.085(16) 0.026(14) 0.006(12) Cl14 0.146(12) 0.164(15) 0.111(14) 0.070(14) 0.015(12) 0.022(13) C114 0.136(16) 0.136(15) 0.12(2) 0.053(19) 0.033(14) 0.035(14) Cl15 0.157(15) 0.180(16) 0.166(15) -0.009(14) 0.067(14) 0.030(12) Cl16 0.27(2) 0.25(2) 0.217(15) 0.091(14) 0.052(14) 0.049(16) Cl17 0.27(2) 0.239(19) 0.234(18) 0.087(15) 0.066(16) 0.005(14) C115 0.24(2) 0.26(2) 0.26(2) 0.071(14) 0.092(19) 0.020(18) S1 0.083(2) 0.100(3) 0.099(3) 0.049(3) 0.030(2) 0.0041(19) O13 0.081(7) 0.078(6) 0.083(6) 0.032(6) 0.022(5) -0.013(4) C116 0.100(6) 0.083(8) 0.157(9) 0.065(8) 0.085(7) 0.030(4) C117 0.159(11) 0.171(13) 0.108(3) 0.081(6) 0.057(7) 0.011(9) S2 0.125(11) 0.231(17) 0.206(14) 0.111(12) 0.052(9) 0.044(10) O14 0.09(2) 0.034(16) 0.152(13) 0.057(13) -0.009(11) 0.011(14) C118 0.194(13) 0.188(15) 0.189(14) 0.066(6) 0.059(8) 0.021(7) C119 0.195(11) 0.18(2) 0.119(16) 0.049(18) 0.058(15) 0.021(17) S3 0.25(2) 0.207(17) 0.21(2) 0.119(17) 0.040(13) 0.025(12) O15 0.17(2) 0.197(15) 0.16(3) 0.070(19) 0.039(17) 0.053(14) C120 0.16(2) 0.18(3) 0.20(3) 0.042(19) 0.06(2) 0.040(17) C121 0.15(2) 0.15(2) 0.16(3) 0.052(19) 0.067(17) -0.023(19) S4 0.155(8) 0.184(10) 0.190(10) 0.084(9) 0.004(8) -0.043(9) O16 0.171(13) 0.240(18) 0.181(19) 0.097(16) 0.052(14) 0.004(14) C122 0.097(18) 0.17(2) 0.181(15) 0.059(13) 0.037(16) 0.017(15) C123 0.24(2) 0.214(11) 0.21(2) 0.035(15) 0.090(18) -0.004(14) S5 0.170(11) 0.218(16) 0.192(14) 0.024(11) 0.042(9) -0.028(10) O17 0.221(14) 0.17(2) 0.159(19) 0.054(16) 0.051(13) 0.008(14) C124 0.19(3) 0.24(3) 0.237(16) 0.075(16) 0.074(17) 0.034(18) C125 0.215(13) 0.23(3) 0.237(18) 0.067(19) 0.069(14) 0.044(18) C126 0.078(6) 0.088(8) 0.075(7) 0.027(7) 0.016(5) -0.005(6) C127 0.079(6) 0.090(9) 0.072(7) 0.037(7) 0.033(6) 0.013(6) O18 0.089(5) 0.094(6) 0.124(6) 0.055(6) 0.035(4) 0.008(4) O19 0.075(4) 0.073(5) 0.070(4) 0.031(4) 0.025(3) -0.000(4) C128 0.076(6) 0.078(8) 0.083(7) 0.019(7) 0.023(6) 0.004(6) C129 0.092(7) 0.086(9) 0.104(9) 0.033(8) 0.033(6) 0.005(6) C130 0.094(7) 0.077(8) 0.056(6) 0.011(7) 0.031(6) 0.010(6) C131 0.055(5) 0.097(10) 0.098(8) 0.060(8) 0.045(6) 0.033(6) O20 0.075(4) 0.091(6) 0.106(6) 0.038(5) 0.029(4) 0.021(4) O21 0.063(3) 0.066(5) 0.072(4) 0.013(4) 0.032(3) -0.006(3) C132 0.090(7) 0.091(10) 0.080(8) 0.017(8) 0.030(6) 0.013(7) C133 0.120(8) 0.059(7) 0.053(6) 0.020(6) 0.025(6) 0.013(6) C134 0.145(9) 0.058(9) 0.078(5) 0.025(7) 0.025(6) 0.014(8) C135 0.114(6) 0.165(14) 0.091(5) 0.058(10) 0.011(5) -0.010(10) O22 0.130(6) 0.259(15) 0.159(10) 0.048(11) 0.049(6) -0.013(9) O23 0.144(6) 0.117(8) 0.077(4) 0.035(6) 0.009(4) 0.007(6) C136 0.149(10) 0.149(14) 0.092(5) 0.069(9) 0.010(5) -0.018(10) C137 0.140(10) 0.088(11) 0.076(5) 0.031(8) 0.021(6) 0.012(8) C138 0.151(12) 0.162(8) 0.138(9) 0.021(7) 0.068(10) 0.037(10) C139 0.071(8) 0.146(7) 0.097(7) 0.044(6) 0.031(7) 0.011(8) O24 0.148(9) 0.182(10) 0.114(7) 0.072(7) 0.050(7) 0.005(7) O25 0.138(8) 0.135(7) 0.130(7) 0.060(5) 0.077(7) 0.040(6) C140 0.052(6) 0.141(7) 0.105(8) 0.048(5) 0.010(7) 0.026(6) C141 0.115(9) 0.122(7) 0.113(9) 0.064(6) 0.090(8) 0.059(6) C142 0.097(8) 0.172(10) 0.084(8) 0.059(7) 0.014(5) 0.025(8) C143 0.128(9) 0.140(9) 0.074(8) 0.047(7) 0.032(5) 0.015(7) O26 0.318(14) 0.130(8) 0.148(10) 0.053(7) 0.047(10) 0.044(9) O27 0.074(5) 0.192(9) 0.077(6) 0.043(6) 0.023(4) 0.014(5) C144 0.082(7) 0.144(11) 0.084(8) 0.032(8) 0.034(5) -0.011(8) C145 0.053(6) 0.178(13) 0.065(8) 0.043(10) 0.033(5) 0.000(8) C146 0.082(14) 0.104(13) 0.071(13) 0.053(13) 0.016(9) 0.025(9) C147 0.051(11) 0.088(11) 0.078(9) 0.026(8) 0.022(11) 0.021(8) O28 0.089(9) 0.123(11) 0.088(8) -0.000(7) 0.039(8) -0.009(7) O29 0.041(10) 0.074(9) 0.062(7) 0.036(6) -0.002(7) 0.012(7) C148 0.056(17) 0.052(12) 0.065(8) 0.010(9) 0.008(9) -0.003(9) C149 0.026(11) 0.076(13) 0.063(8) 0.027(8) 0.005(8) 0.018(9) C150 0.061(16) 0.122(17) 0.104(13) 0.030(10) 0.038(13) -0.000(13) C151 0.046(14) 0.107(10) 0.097(12) 0.032(8) 0.022(11) 0.012(11) O30 0.129(11) 0.108(9) 0.102(10) 0.032(8) 0.031(9) 0.000(9) O31 0.053(12) 0.115(11) 0.091(11) 0.020(9) 0.027(11) -0.004(10) C152 0.09(2) 0.102(17) 0.079(11) 0.024(11) 0.021(12) 0.004(13) C153 0.081(16) 0.117(18) 0.093(17) 0.023(14) 0.035(14) -0.004(12) C154 0.147(9) 0.045(10) 0.190(13) 0.028(11) 0.054(10) 0.020(9) C155 0.125(9) 0.109(14) 0.177(8) 0.039(11) 0.039(7) 0.045(9) O32 0.117(8) 0.166(13) 0.197(11) 0.023(9) 0.046(8) 0.038(8) O33 0.156(9) 0.141(11) 0.168(8) 0.070(9) 0.039(7) 0.012(8) C156 0.151(14) 0.126(14) 0.182(13) 0.076(11) 0.048(11) 0.043(12) C157 0.27(2) 0.23(2) 0.226(18) 0.018(13) 0.095(15) 0.054(18) C158 0.11(2) 0.120(16) 0.11(2) 0.037(18) 0.032(17) -0.005(15) C159 0.140(19) 0.117(17) 0.13(2) 0.038(16) 0.045(16) 0.001(13) O34 0.123(17) 0.115(19) 0.11(2) 0.044(17) 0.031(15) -0.005(15) O35 0.14(2) 0.086(16) 0.15(2) 0.026(16) 0.059(16) 0.006(12) C160 0.092(14) 0.105(12) 0.096(13) 0.026(8) 0.031(7) 0.018(6) C161 0.10(2) 0.08(2) 0.10(3) 0.015(19) 0.042(16) 0.022(16) C162 0.186(12) 0.19(2) 0.15(3) 0.058(19) 0.061(18) 0.050(12) C163 0.170(13) 0.175(15) 0.13(2) 0.059(18) 0.041(17) 0.024(10) O36 0.158(13) 0.159(12) 0.159(13) 0.043(7) 0.062(7) 0.021(6) O37 0.209(15) 0.172(16) 0.20(2) 0.068(18) 0.057(17) 0.018(13) C164 0.219(17) 0.21(2) 0.20(3) 0.078(19) 0.072(19) -0.005(15) C165 0.20(3) 0.18(2) 0.19(3) 0.06(2) 0.08(2) 0.030(15) O38 0.25(2) 0.18(2) 0.107(14) 0.063(15) 0.112(15) 0.042(16) O39 0.142(17) 0.21(2) 0.22(2) 0.129(18) 0.021(15) 0.048(16) O40 0.074(8) 0.140(13) 0.143(12) 0.068(11) 0.031(8) 0.013(8) O41 0.14(2) 0.17(2) 0.23(3) 0.06(2) 0.018(18) 0.04(2) O42 0.28(2) 0.25(2) 0.26(2) 0.09(2) 0.107(19) 0.021(19) O43 0.38(3) 0.26(3) 0.35(3) 0.14(2) 0.10(2) 0.08(2) O44 0.28(3) 0.20(2) 0.14(2) 0.05(2) 0.066(19) 0.05(2) O45 0.25(3) 0.19(3) 0.21(3) 0.10(2) 0.08(2) 0.01(2) O46 0.31(5) 0.30(5) 0.30(5) 0.10(3) 0.10(3) 0.06(3) O47 0.084(17) 0.15(2) 0.072(19) -0.028(17) 0.028(15) 0.059(18) O48 0.14(2) 0.18(3) 0.19(3) 0.04(2) 0.054(19) -0.033(19) O49 0.18(2) 0.12(2) 0.15(2) 0.041(19) 0.040(18) -0.003(18) O50 0.20(2) 0.22(3) 0.22(2) 0.10(2) 0.077(19) -0.019(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 N2 1.858(4) . ? Ni1 O4 1.868(4) . ? Ni1 N1 1.868(5) . ? Ni1 O1 1.870(3) . ? Ni2 N4 1.858(5) . ? Ni2 N3 1.860(4) . ? Ni2 O8 1.865(3) . ? Ni2 O5 1.869(4) . ? Ni3 O12 1.851(5) . ? Ni3 N5 1.855(6) . ? Ni3 O9 1.860(5) . ? Ni3 N6 1.875(6) . ? C1 C2 1.388(8) . ? C1 C6 1.396(8) . ? C1 C43 1.507(9) . ? C2 C3 1.391(8) . ? C2 H1 0.9500 . ? C3 C4 1.412(8) . ? C3 C73 1.481(8) . ? C4 C5 1.376(8) . ? C4 H2 0.9500 . ? C5 C6 1.396(8) . ? C5 C13 1.501(8) . ? C6 H3 0.9500 . ? C7 C12 1.399(9) . ? C7 C8 1.407(8) . ? C7 C65 1.480(8) . ? C8 C9 1.383(8) . ? C8 H4 0.9500 . ? C9 C10 1.394(8) . ? C9 C98 1.532(8) . ? C10 C11 1.390(8) . ? C10 H5 0.9500 . ? C11 C12 1.394(8) . ? C11 C35 1.484(9) . ? C12 H6 0.9500 . ? C13 C18 1.378(9) . ? C13 C14 1.431(7) . ? C14 O1 1.323(7) . ? C14 C15 1.428(9) . ? C15 C16 1.402(9) . ? C15 C23 1.423(7) . ? C16 C17 1.381(8) . ? C16 H7 0.9500 . ? C17 C18 1.419(9) . ? C17 C19 1.551(10) . ? C18 H8 0.9500 . ? C19 C21 1.508(14) . ? C19 C22 1.513(10) . ? C19 C20 1.584(14) . ? C20 H9 0.9800 . ? C20 H10 0.9800 . ? C20 H11 0.9800 . ? C21 H12 0.9800 . ? C21 H13 0.9800 . ? C21 H14 0.9800 . ? C22 H15 0.9800 . ? C22 H16 0.9800 . ? C22 H17 0.9800 . ? C23 N1 1.293(7) . ? C23 H18 0.9500 . ? N1 C24 1.425(6) . ? C24 C29 1.381(8) . ? C24 C25 1.406(8) . ? C25 C26 1.375(7) . ? C25 H19 0.9500 . ? C26 O2 1.374(7) . ? C26 C27 1.428(9) . ? C27 O3 1.365(6) . ? C27 C28 1.375(9) . ? C28 C29 1.393(7) . ? C28 H20 0.9500 . ? C29 N2 1.416(8) . ? O2 C30 1.417(7) . ? C30 H21 0.9800 . ? C30 H22 0.9800 . ? C30 H23 0.9800 . ? O3 C31 1.433(7) . ? C31 H24 0.9800 . ? C31 H25 0.9800 . ? C31 H26 0.9800 . ? N2 C32 1.296(7) . ? C32 C33 1.421(9) . ? C32 H27 0.9500 . ? C33 C38 1.424(8) . ? C33 C34 1.439(8) . ? C34 O4 1.326(7) . ? C34 C35 1.428(9) . ? C35 C36 1.382(8) . ? C36 C37 1.414(9) . ? C36 H28 0.9500 . ? C37 C38 1.358(9) . ? C37 C39 1.549(8) . ? C38 H29 0.9500 . ? C39 C40 1.521(10) . ? C39 C41 1.530(10) . ? C39 C42 1.542(8) . ? C40 H30 0.9800 . ? C40 H31 0.9800 . ? C40 H32 0.9800 . ? C41 H33 0.9800 . ? C41 H34 0.9800 . ? C41 H35 0.9800 . ? C42 H36 0.9800 . ? C42 H37 0.9800 . ? C42 H38 0.9800 . ? C43 C48 1.385(7) . ? C43 C44 1.407(9) . ? C44 O5 1.321(6) . ? C44 C45 1.431(8) . ? C45 C53 1.408(9) . ? C45 C46 1.423(7) . ? C46 C47 1.360(9) . ? C46 H39 0.9500 . ? C47 C48 1.413(8) . ? C47 C49 1.541(7) . ? C48 H40 0.9500 . ? C49 C50 1.536(10) . ? C49 C51 1.541(9) . ? C49 C52 1.545(9) . ? C50 H41 0.9800 . ? C50 H42 0.9800 . ? C50 H43 0.9800 . ? C51 H44 0.9800 . ? C51 H45 0.9800 . ? C51 H46 0.9800 . ? C52 H47 0.9800 . ? C52 H48 0.9800 . ? C52 H49 0.9800 . ? C53 N3 1.305(6) . ? C53 H50 0.9500 . ? N3 C54 1.410(8) . ? C54 C59 1.394(7) . ? C54 C55 1.408(8) . ? C55 C56 1.363(9) . ? C55 H51 0.9500 . ? C56 O6 1.375(7) . ? C56 C57 1.420(8) . ? C57 O7 1.365(7) . ? C57 C58 1.384(8) . ? C58 C59 1.393(8) . ? C58 H52 0.9500 . ? C59 N4 1.428(7) . ? O6 C60 1.434(7) . ? C60 H53 0.9800 . ? C60 H54 0.9800 . ? C60 H55 0.9800 . ? O7 C61 1.418(7) . ? C61 H56 0.9800 . ? C61 H57 0.9800 . ? C61 H58 0.9800 . ? N4 C62 1.316(6) . ? C62 C63 1.421(8) . ? C62 H59 0.9500 . ? C63 C64 1.411(8) . ? C63 C68 1.428(7) . ? C64 O8 1.316(6) . ? C64 C65 1.440(8) . ? C65 C66 1.380(7) . ? C66 C67 1.395(9) . ? C66 H60 0.9500 . ? C67 C68 1.387(8) . ? C67 C69 1.551(8) . ? C68 H61 0.9500 . ? C69 C70 1.515(9) . ? C69 C71 1.541(11) . ? C69 C72 1.554(11) . ? C70 H62 0.9800 . ? C70 H63 0.9800 . ? C70 H64 0.9800 . ? C71 H65 0.9800 . ? C71 H66 0.9800 . ? C71 H67 0.9800 . ? C72 H68 0.9800 . ? C72 H69 0.9800 . ? C72 H70 0.9800 . ? C73 C78 1.385(9) . ? C73 C74 1.445(9) . ? C74 O9 1.316(8) . ? C74 C75 1.416(9) . ? C75 C76 1.407(9) . ? C75 C86 1.431(9) . ? C76 C77 1.379(9) . ? C76 H71 0.9500 . ? C77 C78 1.410(9) . ? C77 C79 1.518(10) . ? C78 H72 0.9500 . ? C79 C82 1.502(11) . ? C79 C83 1.52(3) . ? C79 C80 1.525(13) . ? C79 C81 1.527(11) . ? C79 C84 1.56(3) . ? C79 C85 1.59(3) . ? C80 H73 0.9800 . ? C80 H74 0.9800 . ? C80 H75 0.9800 . ? C81 H76 0.9800 . ? C81 H77 0.9800 . ? C81 H78 0.9800 . ? C82 H79 0.9800 . ? C82 H80 0.9800 . ? C82 H81 0.9800 . ? C83 H82 0.9800 . ? C83 H83 0.9800 . ? C83 H84 0.9800 . ? C84 H85 0.9800 . ? C84 H86 0.9800 . ? C84 H87 0.9800 . ? C85 H88 0.9800 . ? C85 H89 0.9800 . ? C85 H90 0.9800 . ? C86 N5 1.311(8) . ? C86 H91 0.9500 . ? N5 C87 1.433(8) . ? C87 C92 1.369(9) . ? C87 C88 1.394(9) . ? C88 C89 1.383(9) . ? C88 H92 0.9500 . ? C89 O10 1.352(7) . ? C89 C90 1.434(9) . ? C90 O11 1.354(7) . ? C90 C91 1.367(9) . ? C91 C92 1.407(8) . ? C91 H93 0.9500 . ? C92 N6 1.425(8) . ? O10 C93 1.437(9) . ? C93 H94 0.9800 . ? C93 H95 0.9800 . ? C93 H96 0.9800 . ? O11 C94 1.426(8) . ? C94 H97 0.9800 . ? C94 H98 0.9800 . ? C94 H99 0.9800 . ? N6 C95 1.286(8) . ? C95 C96 1.423(9) . ? C95 H100 0.9500 . ? C96 C101 1.400(9) . ? C96 C97 1.439(9) . ? C97 O12 1.315(8) . ? C97 C98 1.431(9) . ? C98 C99 1.368(9) . ? C99 C100 1.415(9) . ? C99 H101 0.9500 . ? C100 C101 1.381(9) . ? C100 C102 1.510(11) . ? C101 H102 0.9500 . ? C102 C108 1.49(2) . ? C102 C107 1.50(2) . ? C102 C104 1.520(15) . ? C102 C103 1.548(13) . ? C102 C105 1.567(15) . ? C102 C106 1.57(3) . ? C103 H103 0.9800 . ? C103 H104 0.9800 . ? C103 H105 0.9800 . ? C104 H106 0.9800 . ? C104 H107 0.9800 . ? C104 H108 0.9800 . ? C105 H109 0.9800 . ? C105 H110 0.9800 . ? C105 H111 0.9800 . ? C106 H112 0.9800 . ? C106 H113 0.9800 . ? C106 H114 0.9800 . ? C107 H115 0.9800 . ? C107 H116 0.9800 . ? C107 H117 0.9800 . ? C108 H118 0.9800 . ? C108 H119 0.9800 . ? C108 H120 0.9800 . ? C109 N9 1.312(8) . ? C109 N8 1.315(8) . ? C109 N7 1.346(8) . ? N7 H121 0.8800 . ? N7 H122 0.8800 . ? N8 H123 0.8800 . ? N8 H124 0.8800 . ? N9 H125 0.8800 . ? N9 H126 0.8800 . ? C110 N10 1.294(11) . ? C110 N11 1.325(11) . ? C110 N12 1.339(10) . ? N10 H127 0.8800 . ? N10 H128 0.8800 . ? N11 H129 0.8800 . ? N11 H130 0.8800 . ? N12 H131 0.8800 . ? N12 H132 0.8800 . ? Cl3 C111 1.748(10) . ? Cl4 C111 1.734(12) . ? Cl5 C111 1.761(10) . ? C111 H133 1.0000 . ? Cl7 C112 1.71(2) . ? Cl8 C112 1.73(2) . ? C112 H134 1.0000 . ? Cl9 C113 1.71(2) . ? Cl10 C113 1.71(2) . ? Cl11 C113 1.72(2) . ? C113 H135 1.0000 . ? Cl12 C114 1.71(2) . ? Cl13 C114 1.72(2) . ? Cl14 C114 1.72(2) . ? C114 H136 1.0000 . ? Cl15 C115 1.72(2) . ? Cl16 C115 1.72(2) . ? Cl17 C115 1.73(2) . ? C115 H137 1.0000 . ? S1 O13 1.509(14) . ? S1 C116 1.653(11) . ? S1 C117 1.759(14) . ? C116 H138 0.9800 . ? C116 H139 0.9800 . ? C116 H140 0.9800 . ? C117 H141 0.9800 . ? C117 H142 0.9800 . ? C117 H143 0.9800 . ? S2 O14 1.48(2) . ? S2 C118 1.59(2) . ? S2 C119 1.82(2) . ? C118 H144 0.9800 . ? C118 H145 0.9800 . ? C118 H146 0.9800 . ? C119 H147 0.9800 . ? C119 H148 0.9800 . ? C119 H149 0.9800 . ? S3 O15 1.50(2) . ? S3 C120 1.61(2) . ? S3 C121 1.81(2) . ? C120 H150 0.9800 . ? C120 H151 0.9800 . ? C120 H152 0.9800 . ? C121 H153 0.9800 . ? C121 H154 0.9800 . ? C121 H155 0.9800 . ? S4 O16 1.477(18) . ? S4 C122 1.61(2) . ? S4 C123 1.84(2) . ? C122 H156 0.9800 . ? C122 H157 0.9800 . ? C122 H158 0.9800 . ? C123 H159 0.9800 . ? C123 H160 0.9800 . ? C123 H161 0.9800 . ? S5 O17 1.501(19) . ? S5 C124 1.62(2) . ? S5 C125 1.85(2) . ? C124 H162 0.9800 . ? C124 H163 0.9800 . ? C124 H164 0.9800 . ? C125 H165 0.9800 . ? C125 H166 0.9800 . ? C125 H167 0.9800 . ? C126 C127 1.500(9) . ? C126 H168 0.9800 . ? C126 H169 0.9800 . ? C126 H170 0.9800 . ? C127 O18 1.233(9) . ? C127 O19 1.343(9) . ? O19 C128 1.447(8) . ? C128 C129 1.490(10) . ? C128 H171 0.9900 . ? C128 H172 0.9900 . ? C129 H173 0.9800 . ? C129 H174 0.9800 . ? C129 H175 0.9800 . ? C130 C131 1.446(13) . ? C130 H176 0.9800 . ? C130 H177 0.9800 . ? C130 H178 0.9800 . ? C131 O20 1.238(11) . ? C131 O21 1.342(9) . ? O21 C132 1.444(11) . ? C132 C133 1.479(10) . ? C132 H179 0.9900 . ? C132 H180 0.9900 . ? C133 H181 0.9800 . ? C133 H182 0.9800 . ? C133 H183 0.9800 . ? C134 C135 1.449(13) . ? C134 H184 0.9800 . ? C134 H185 0.9800 . ? C134 H186 0.9800 . ? C135 O22 1.242(13) . ? C135 O23 1.390(12) . ? O23 C136 1.469(13) . ? C136 C137 1.444(12) . ? C136 H187 0.9900 . ? C136 H188 0.9900 . ? C137 H189 0.9800 . ? C137 H190 0.9800 . ? C137 H191 0.9800 . ? C138 C139 1.49(2) . ? C138 H192 0.9800 . ? C138 H193 0.9800 . ? C138 H194 0.9800 . ? C139 O24 1.149(18) . ? C139 O25 1.33(2) . ? O25 C140 1.511(18) . ? C140 C141 1.561(18) . ? C140 H195 0.9900 . ? C140 H196 0.9900 . ? C141 H197 0.9800 . ? C141 H198 0.9800 . ? C141 H199 0.9800 . ? C142 C143 1.475(14) . ? C142 H200 0.9800 . ? C142 H201 0.9800 . ? C142 H202 0.9800 . ? C143 O26 1.196(13) . ? C143 O27 1.339(12) . ? O27 C144 1.476(12) . ? C144 C145 1.467(15) . ? C144 H203 0.9900 . ? C144 H204 0.9900 . ? C145 H205 0.9800 . ? C145 H206 0.9800 . ? C145 H207 0.9800 . ? C146 C147 1.487(15) . ? C146 H208 0.9800 . ? C146 H209 0.9800 . ? C146 H210 0.9800 . ? C147 O28 1.237(16) . ? C147 O29 1.360(15) . ? O29 C148 1.453(15) . ? C148 C149 1.459(16) . ? C148 H211 0.9900 . ? C148 H212 0.9900 . ? C149 H213 0.9800 . ? C149 H214 0.9800 . ? C149 H215 0.9800 . ? C150 C151 1.484(16) . ? C150 H216 0.9800 . ? C150 H217 0.9800 . ? C150 H218 0.9800 . ? C151 O30 1.234(16) . ? C151 O31 1.355(15) . ? O31 C152 1.464(15) . ? C152 C153 1.469(16) . ? C152 H219 0.9900 . ? C152 H220 0.9900 . ? C153 H221 0.9800 . ? C153 H222 0.9800 . ? C153 H223 0.9800 . ? C154 C155 1.473(15) . ? C154 H224 0.9800 . ? C154 H225 0.9800 . ? C154 H226 0.9800 . ? C155 O32 1.252(14) . ? C155 O33 1.359(15) . ? O33 C156 1.473(15) . ? C156 C157 1.457(17) . ? C156 H227 0.9900 . ? C156 H228 0.9900 . ? C157 H229 0.9800 . ? C157 H230 0.9800 . ? C157 H231 0.9800 . ? C158 C159 1.462(17) . ? C158 H232 0.9800 . ? C158 H233 0.9800 . ? C158 H234 0.9800 . ? C159 O34 1.240(17) . ? C159 O35 1.367(17) . ? O35 C160 1.461(17) . ? C160 C161 1.432(18) . ? C160 H235 0.9900 . ? C160 H236 0.9900 . ? C161 H237 0.9800 . ? C161 H238 0.9800 . ? C161 H239 0.9800 . ? C162 C163 1.480(17) . ? C162 H240 0.9800 . ? C162 H241 0.9800 . ? C162 H242 0.9800 . ? C163 O36 1.236(16) . ? C163 O37 1.352(17) . ? O37 C164 1.455(17) . ? C164 C165 1.460(18) . ? C164 H243 0.9900 . ? C164 H244 0.9900 . ? C165 H245 0.9800 . ? C165 H246 0.9800 . ? C165 H247 0.9800 . ? 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 N2 Ni1 O4 93.4(2) . . ? N2 Ni1 N1 85.5(2) . . ? O4 Ni1 N1 169.8(2) . . ? N2 Ni1 O1 170.5(2) . . ? O4 Ni1 O1 87.77(17) . . ? N1 Ni1 O1 94.98(19) . . ? N4 Ni2 N3 85.8(2) . . ? N4 Ni2 O8 94.88(18) . . ? N3 Ni2 O8 170.5(2) . . ? N4 Ni2 O5 169.6(2) . . ? N3 Ni2 O5 93.62(19) . . ? O8 Ni2 O5 87.37(16) . . ? O12 Ni3 N5 169.90(17) . . ? O12 Ni3 O9 87.0(2) . . ? N5 Ni3 O9 94.0(2) . . ? O12 Ni3 N6 94.7(2) . . ? N5 Ni3 N6 85.9(3) . . ? O9 Ni3 N6 170.51(16) . . ? C2 C1 C6 119.2(6) . . ? C2 C1 C43 121.2(5) . . ? C6 C1 C43 119.6(6) . . ? C1 C2 C3 121.5(5) . . ? C1 C2 H1 119.3 . . ? C3 C2 H1 119.3 . . ? C2 C3 C4 117.6(6) . . ? C2 C3 C73 123.6(5) . . ? C4 C3 C73 118.8(6) . . ? C5 C4 C3 122.2(6) . . ? C5 C4 H2 118.9 . . ? C3 C4 H2 118.9 . . ? C4 C5 C6 118.6(5) . . ? C4 C5 C13 119.8(5) . . ? C6 C5 C13 121.6(6) . . ? C1 C6 C5 120.9(6) . . ? C1 C6 H3 119.6 . . ? C5 C6 H3 119.6 . . ? C12 C7 C8 118.7(6) . . ? C12 C7 C65 120.7(5) . . ? C8 C7 C65 120.6(6) . . ? C9 C8 C7 120.3(6) . . ? C9 C8 H4 119.8 . . ? C7 C8 H4 119.8 . . ? C8 C9 C10 120.0(5) . . ? C8 C9 C98 121.3(5) . . ? C10 C9 C98 118.7(5) . . ? C11 C10 C9 120.9(6) . . ? C11 C10 H5 119.6 . . ? C9 C10 H5 119.6 . . ? C10 C11 C12 118.8(6) . . ? C10 C11 C35 119.9(6) . . ? C12 C11 C35 121.3(5) . . ? C11 C12 C7 121.3(5) . . ? C11 C12 H6 119.4 . . ? C7 C12 H6 119.4 . . ? C18 C13 C14 119.3(5) . . ? C18 C13 C5 119.7(5) . . ? C14 C13 C5 120.7(6) . . ? O1 C14 C15 122.6(5) . . ? O1 C14 C13 120.5(5) . . ? C15 C14 C13 116.8(6) . . ? C16 C15 C23 117.4(6) . . ? C16 C15 C14 121.0(5) . . ? C23 C15 C14 121.4(6) . . ? C17 C16 C15 122.6(6) . . ? C17 C16 H7 118.7 . . ? C15 C16 H7 118.7 . . ? C16 C17 C18 115.6(6) . . ? C16 C17 C19 123.3(6) . . ? C18 C17 C19 120.9(5) . . ? C13 C18 C17 124.4(5) . . ? C13 C18 H8 117.8 . . ? C17 C18 H8 117.8 . . ? C14 O1 Ni1 127.5(4) . . ? C21 C19 C22 110.2(8) . . ? C21 C19 C17 108.5(8) . . ? C22 C19 C17 112.0(6) . . ? C21 C19 C20 108.6(7) . . ? C22 C19 C20 109.2(9) . . ? C17 C19 C20 108.3(7) . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? N1 C23 C15 126.9(6) . . ? N1 C23 H18 116.5 . . ? C15 C23 H18 116.5 . . ? C23 N1 C24 121.7(5) . . ? C23 N1 Ni1 124.9(4) . . ? C24 N1 Ni1 113.1(4) . . ? C29 C24 C25 120.4(5) . . ? C29 C24 N1 113.4(5) . . ? C25 C24 N1 126.1(5) . . ? C26 C25 C24 118.7(6) . . ? C26 C25 H19 120.6 . . ? C24 C25 H19 120.6 . . ? O2 C26 C25 125.5(6) . . ? O2 C26 C27 113.9(5) . . ? C25 C26 C27 120.6(5) . . ? O3 C27 C28 124.9(6) . . ? O3 C27 C26 115.4(5) . . ? C28 C27 C26 119.7(5) . . ? C27 C28 C29 119.3(6) . . ? C27 C28 H20 120.3 . . ? C29 C28 H20 120.3 . . ? C24 C29 C28 121.0(5) . . ? C24 C29 N2 114.2(5) . . ? C28 C29 N2 124.7(6) . . ? C26 O2 C30 117.7(4) . . ? O2 C30 H21 109.5 . . ? O2 C30 H22 109.5 . . ? H21 C30 H22 109.5 . . ? O2 C30 H23 109.5 . . ? H21 C30 H23 109.5 . . ? H22 C30 H23 109.5 . . ? C27 O3 C31 116.7(5) . . ? O3 C31 H24 109.5 . . ? O3 C31 H25 109.5 . . ? H24 C31 H25 109.5 . . ? O3 C31 H26 109.5 . . ? H24 C31 H26 109.5 . . ? H25 C31 H26 109.5 . . ? C32 N2 C29 121.6(5) . . ? C32 N2 Ni1 124.4(4) . . ? C29 N2 Ni1 113.3(4) . . ? N2 C32 C33 125.4(6) . . ? N2 C32 H27 117.3 . . ? C33 C32 H27 117.3 . . ? C32 C33 C38 118.4(5) . . ? C32 C33 C34 121.1(6) . . ? C38 C33 C34 119.9(6) . . ? O4 C34 C35 122.1(5) . . ? O4 C34 C33 121.0(6) . . ? C35 C34 C33 116.9(5) . . ? C36 C35 C34 119.2(6) . . ? C36 C35 C11 119.6(6) . . ? C34 C35 C11 121.1(5) . . ? C35 C36 C37 124.2(6) . . ? C35 C36 H28 117.9 . . ? C37 C36 H28 117.9 . . ? C38 C37 C36 116.7(6) . . ? C38 C37 C39 122.1(6) . . ? C36 C37 C39 121.0(6) . . ? C37 C38 C33 122.5(6) . . ? C37 C38 H29 118.8 . . ? C33 C38 H29 118.8 . . ? C34 O4 Ni1 128.1(4) . . ? C40 C39 C41 109.8(5) . . ? C40 C39 C42 106.8(6) . . ? C41 C39 C42 109.0(7) . . ? C40 C39 C37 112.0(6) . . ? C41 C39 C37 108.5(6) . . ? C42 C39 C37 110.6(5) . . ? C39 C40 H30 109.5 . . ? C39 C40 H31 109.5 . . ? H30 C40 H31 109.5 . . ? C39 C40 H32 109.5 . . ? H30 C40 H32 109.5 . . ? H31 C40 H32 109.5 . . ? C39 C41 H33 109.5 . . ? C39 C41 H34 109.5 . . ? H33 C41 H34 109.5 . . ? C39 C41 H35 109.5 . . ? H33 C41 H35 109.5 . . ? H34 C41 H35 109.5 . . ? C39 C42 H36 109.5 . . ? C39 C42 H37 109.5 . . ? H36 C42 H37 109.5 . . ? C39 C42 H38 109.5 . . ? H36 C42 H38 109.5 . . ? H37 C42 H38 109.5 . . ? C48 C43 C44 119.3(5) . . ? C48 C43 C1 118.7(6) . . ? C44 C43 C1 121.9(5) . . ? O5 C44 C43 121.6(5) . . ? O5 C44 C45 121.1(6) . . ? C43 C44 C45 117.2(5) . . ? C53 C45 C46 118.6(5) . . ? C53 C45 C44 121.0(5) . . ? C46 C45 C44 119.7(6) . . ? C47 C46 C45 122.7(6) . . ? C47 C46 H39 118.7 . . ? C45 C46 H39 118.7 . . ? C46 C47 C48 115.9(5) . . ? C46 C47 C49 125.3(5) . . ? C48 C47 C49 118.7(6) . . ? C43 C48 C47 124.2(6) . . ? C43 C48 H40 117.9 . . ? C47 C48 H40 117.9 . . ? C44 O5 Ni2 127.9(4) . . ? C50 C49 C51 110.7(6) . . ? C50 C49 C47 111.0(5) . . ? C51 C49 C47 109.3(5) . . ? C50 C49 C52 108.2(5) . . ? C51 C49 C52 106.9(6) . . ? C47 C49 C52 110.8(6) . . ? C49 C50 H41 109.5 . . ? C49 C50 H42 109.5 . . ? H41 C50 H42 109.5 . . ? C49 C50 H43 109.5 . . ? H41 C50 H43 109.5 . . ? H42 C50 H43 109.5 . . ? C49 C51 H44 109.5 . . ? C49 C51 H45 109.5 . . ? H44 C51 H45 109.5 . . ? C49 C51 H46 109.5 . . ? H44 C51 H46 109.5 . . ? H45 C51 H46 109.5 . . ? C49 C52 H47 109.5 . . ? C49 C52 H48 109.5 . . ? H47 C52 H48 109.5 . . ? C49 C52 H49 109.5 . . ? H47 C52 H49 109.5 . . ? H48 C52 H49 109.5 . . ? N3 C53 C45 126.2(5) . . ? N3 C53 H50 116.9 . . ? C45 C53 H50 116.9 . . ? C53 N3 C54 122.5(5) . . ? C53 N3 Ni2 123.8(4) . . ? C54 N3 Ni2 113.1(3) . . ? C59 C54 C55 120.0(6) . . ? C59 C54 N3 114.6(5) . . ? C55 C54 N3 125.2(5) . . ? C56 C55 C54 119.2(5) . . ? C56 C55 H51 120.4 . . ? C54 C55 H51 120.4 . . ? C55 C56 O6 124.9(5) . . ? C55 C56 C57 121.0(5) . . ? O6 C56 C57 114.1(6) . . ? O7 C57 C58 125.3(5) . . ? O7 C57 C56 115.0(5) . . ? C58 C57 C56 119.6(6) . . ? C57 C58 C59 119.5(5) . . ? C57 C58 H52 120.3 . . ? C59 C58 H52 120.3 . . ? C58 C59 C54 120.5(5) . . ? C58 C59 N4 126.8(5) . . ? C54 C59 N4 112.6(5) . . ? C56 O6 C60 116.4(5) . . ? O6 C60 H53 109.5 . . ? O6 C60 H54 109.5 . . ? H53 C60 H54 109.5 . . ? O6 C60 H55 109.5 . . ? H53 C60 H55 109.5 . . ? H54 C60 H55 109.5 . . ? C57 O7 C61 117.2(5) . . ? O7 C61 H56 109.5 . . ? O7 C61 H57 109.5 . . ? H56 C61 H57 109.5 . . ? O7 C61 H58 109.5 . . ? H56 C61 H58 109.5 . . ? H57 C61 H58 109.5 . . ? C62 N4 C59 120.8(5) . . ? C62 N4 Ni2 125.4(4) . . ? C59 N4 Ni2 113.5(3) . . ? N4 C62 C63 125.2(6) . . ? N4 C62 H59 117.4 . . ? C63 C62 H59 117.4 . . ? C64 C63 C62 122.4(5) . . ? C64 C63 C68 121.3(5) . . ? C62 C63 C68 116.3(6) . . ? O8 C64 C63 123.0(5) . . ? O8 C64 C65 119.9(5) . . ? C63 C64 C65 117.1(5) . . ? C66 C65 C64 118.4(6) . . ? C66 C65 C7 119.3(5) . . ? C64 C65 C7 122.3(5) . . ? C65 C66 C67 125.0(5) . . ? C65 C66 H60 117.5 . . ? C67 C66 H60 117.5 . . ? C68 C67 C66 116.8(5) . . ? C68 C67 C69 123.0(6) . . ? C66 C67 C69 120.2(5) . . ? C67 C68 C63 120.7(6) . . ? C67 C68 H61 119.6 . . ? C63 C68 H61 119.6 . . ? C64 O8 Ni2 127.5(4) . . ? C70 C69 C71 108.9(7) . . ? C70 C69 C67 112.5(5) . . ? C71 C69 C67 108.9(6) . . ? C70 C69 C72 108.8(6) . . ? C71 C69 C72 109.6(6) . . ? C67 C69 C72 108.1(6) . . ? C69 C70 H62 109.5 . . ? C69 C70 H63 109.5 . . ? H62 C70 H63 109.5 . . ? C69 C70 H64 109.5 . . ? H62 C70 H64 109.5 . . ? H63 C70 H64 109.5 . . ? C69 C71 H65 109.5 . . ? C69 C71 H66 109.5 . . ? H65 C71 H66 109.5 . . ? C69 C71 H67 109.5 . . ? H65 C71 H67 109.5 . . ? H66 C71 H67 109.5 . . ? C69 C72 H68 109.5 . . ? C69 C72 H69 109.5 . . ? H68 C72 H69 109.5 . . ? C69 C72 H70 109.5 . . ? H68 C72 H70 109.5 . . ? H69 C72 H70 109.5 . . ? C78 C73 C74 119.0(6) . . ? C78 C73 C3 118.9(6) . . ? C74 C73 C3 122.0(7) . . ? O9 C74 C75 123.8(6) . . ? O9 C74 C73 120.2(6) . . ? C75 C74 C73 116.0(7) . . ? C76 C75 C74 121.0(6) . . ? C76 C75 C86 118.2(6) . . ? C74 C75 C86 120.6(7) . . ? C77 C76 C75 123.8(7) . . ? C77 C76 H71 118.1 . . ? C75 C76 H71 118.1 . . ? C76 C77 C78 114.2(7) . . ? C76 C77 C79 121.8(7) . . ? C78 C77 C79 123.9(6) . . ? C73 C78 C77 125.4(7) . . ? C73 C78 H72 117.3 . . ? C77 C78 H72 117.3 . . ? C74 O9 Ni3 127.1(4) . . ? C82 C79 C83 134.8(15) . . ? C82 C79 C77 111.2(7) . . ? C83 C79 C77 113.9(14) . . ? C82 C79 C80 108.9(9) . . ? C83 C79 C80 50.9(13) . . ? C77 C79 C80 112.6(7) . . ? C82 C79 C81 108.6(9) . . ? C83 C79 C81 57.3(13) . . ? C77 C79 C81 109.2(7) . . ? C80 C79 C81 106.1(8) . . ? C82 C79 C84 59.0(14) . . ? C83 C79 C84 103.3(19) . . ? C77 C79 C84 113.0(14) . . ? C80 C79 C84 133.9(15) . . ? C81 C79 C84 51.8(13) . . ? C82 C79 C85 49.0(14) . . ? C83 C79 C85 112(2) . . ? C77 C79 C85 108.5(13) . . ? C80 C79 C85 65.3(16) . . ? C81 C79 C85 141.6(15) . . ? C84 C79 C85 105(2) . . ? C79 C80 H73 109.5 . . ? C79 C80 H74 109.5 . . ? H73 C80 H74 109.5 . . ? C79 C80 H75 109.5 . . ? H73 C80 H75 109.5 . . ? H74 C80 H75 109.5 . . ? C79 C81 H76 109.5 . . ? C79 C81 H77 109.5 . . ? H76 C81 H77 109.5 . . ? C79 C81 H78 109.5 . . ? H76 C81 H78 109.5 . . ? H77 C81 H78 109.5 . . ? C79 C82 H79 109.5 . . ? C79 C82 H80 109.5 . . ? H79 C82 H80 109.5 . . ? C79 C82 H81 109.5 . . ? H79 C82 H81 109.5 . . ? H80 C82 H81 109.5 . . ? C79 C83 H82 109.5 . . ? C79 C83 H83 109.5 . . ? H82 C83 H83 109.5 . . ? C79 C83 H84 109.5 . . ? H82 C83 H84 109.5 . . ? H83 C83 H84 109.5 . . ? C79 C84 H85 109.5 . . ? C79 C84 H86 109.5 . . ? H85 C84 H86 109.5 . . ? C79 C84 H87 109.5 . . ? H85 C84 H87 109.5 . . ? H86 C84 H87 109.5 . . ? C79 C85 H88 109.5 . . ? C79 C85 H89 109.5 . . ? H88 C85 H89 109.5 . . ? C79 C85 H90 109.5 . . ? H88 C85 H90 109.5 . . ? H89 C85 H90 109.5 . . ? N5 C86 C75 124.8(6) . . ? N5 C86 H91 117.6 . . ? C75 C86 H91 117.6 . . ? C86 N5 C87 121.2(6) . . ? C86 N5 Ni3 124.9(4) . . ? C87 N5 Ni3 112.9(5) . . ? C92 C87 C88 121.1(6) . . ? C92 C87 N5 114.4(6) . . ? C88 C87 N5 124.5(7) . . ? C89 C88 C87 119.5(7) . . ? C89 C88 H92 120.3 . . ? C87 C88 H92 120.3 . . ? O10 C89 C88 125.1(7) . . ? O10 C89 C90 115.7(6) . . ? C88 C89 C90 119.3(6) . . ? O11 C90 C91 127.0(7) . . ? O11 C90 C89 112.7(6) . . ? C91 C90 C89 120.4(6) . . ? C90 C91 C92 119.5(7) . . ? C90 C91 H93 120.3 . . ? C92 C91 H93 120.3 . . ? C87 C92 C91 120.2(6) . . ? C87 C92 N6 114.0(6) . . ? C91 C92 N6 125.7(7) . . ? C89 O10 C93 117.5(6) . . ? O10 C93 H94 109.5 . . ? O10 C93 H95 109.5 . . ? H94 C93 H95 109.5 . . ? O10 C93 H96 109.5 . . ? H94 C93 H96 109.5 . . ? H95 C93 H96 109.5 . . ? C90 O11 C94 117.3(5) . . ? O11 C94 H97 109.5 . . ? O11 C94 H98 109.5 . . ? H97 C94 H98 109.5 . . ? O11 C94 H99 109.5 . . ? H97 C94 H99 109.5 . . ? H98 C94 H99 109.5 . . ? C95 N6 C92 122.4(6) . . ? C95 N6 Ni3 124.3(5) . . ? C92 N6 Ni3 112.8(5) . . ? N6 C95 C96 127.1(6) . . ? N6 C95 H100 116.5 . . ? C96 C95 H100 116.5 . . ? C101 C96 C95 119.1(6) . . ? C101 C96 C97 120.9(6) . . ? C95 C96 C97 119.7(7) . . ? O12 C97 C98 121.7(6) . . ? O12 C97 C96 123.2(6) . . ? C98 C97 C96 115.0(7) . . ? C99 C98 C97 120.6(6) . . ? C99 C98 C9 120.2(6) . . ? C97 C98 C9 119.1(7) . . ? C98 C99 C100 124.0(6) . . ? C98 C99 H101 118.0 . . ? C100 C99 H101 118.0 . . ? C101 C100 C99 115.3(7) . . ? C101 C100 C102 121.9(6) . . ? C99 C100 C102 122.6(6) . . ? C100 C101 C96 122.8(6) . . ? C100 C101 H102 118.6 . . ? C96 C101 H102 118.6 . . ? C97 O12 Ni3 127.2(4) . . ? C108 C102 C107 105.6(17) . . ? C108 C102 C100 109.9(14) . . ? C107 C102 C100 115.0(12) . . ? C108 C102 C104 136.3(16) . . ? C107 C102 C104 62.6(11) . . ? C100 C102 C104 113.1(8) . . ? C108 C102 C103 45.3(14) . . ? C107 C102 C103 129.5(13) . . ? C100 C102 C103 114.1(8) . . ? C104 C102 C103 107.2(11) . . ? C108 C102 C105 61.8(15) . . ? C107 C102 C105 49.8(10) . . ? C100 C102 C105 107.9(9) . . ? C104 C102 C105 110.6(12) . . ? C103 C102 C105 103.6(9) . . ? C108 C102 C106 110(2) . . ? C107 C102 C106 105.9(17) . . ? C100 C102 C106 110.6(14) . . ? C104 C102 C106 46.9(12) . . ? C103 C102 C106 66.2(14) . . ? C105 C102 C106 141.0(15) . . ? C102 C103 H103 109.5 . . ? C102 C103 H104 109.5 . . ? H103 C103 H104 109.5 . . ? C102 C103 H105 109.5 . . ? H103 C103 H105 109.5 . . ? H104 C103 H105 109.5 . . ? C102 C104 H106 109.5 . . ? C102 C104 H107 109.5 . . ? H106 C104 H107 109.5 . . ? C102 C104 H108 109.5 . . ? H106 C104 H108 109.5 . . ? H107 C104 H108 109.5 . . ? C102 C105 H109 109.5 . . ? C102 C105 H110 109.5 . . ? H109 C105 H110 109.5 . . ? C102 C105 H111 109.5 . . ? H109 C105 H111 109.5 . . ? H110 C105 H111 109.5 . . ? C102 C106 H112 109.5 . . ? C102 C106 H113 109.5 . . ? H112 C106 H113 109.5 . . ? C102 C106 H114 109.5 . . ? H112 C106 H114 109.5 . . ? H113 C106 H114 109.5 . . ? C102 C107 H115 109.5 . . ? C102 C107 H116 109.5 . . ? H115 C107 H116 109.5 . . ? C102 C107 H117 109.5 . . ? H115 C107 H117 109.5 . . ? H116 C107 H117 109.5 . . ? C102 C108 H118 109.5 . . ? C102 C108 H119 109.5 . . ? H118 C108 H119 109.5 . . ? C102 C108 H120 109.5 . . ? H118 C108 H120 109.5 . . ? H119 C108 H120 109.5 . . ? N9 C109 N8 121.5(6) . . ? N9 C109 N7 120.1(6) . . ? N8 C109 N7 118.4(6) . . ? C109 N7 H121 120.0 . . ? C109 N7 H122 120.0 . . ? H121 N7 H122 120.0 . . ? C109 N8 H123 120.0 . . ? C109 N8 H124 120.0 . . ? H123 N8 H124 120.0 . . ? C109 N9 H125 120.0 . . ? C109 N9 H126 120.0 . . ? H125 N9 H126 120.0 . . ? N10 C110 N11 121.3(9) . . ? N10 C110 N12 120.0(9) . . ? N11 C110 N12 118.7(10) . . ? C110 N10 H127 120.0 . . ? C110 N10 H128 120.0 . . ? H127 N10 H128 120.0 . . ? C110 N11 H129 120.0 . . ? C110 N11 H130 120.0 . . ? H129 N11 H130 120.0 . . ? C110 N12 H131 120.0 . . ? C110 N12 H132 120.0 . . ? H131 N12 H132 120.0 . . ? Cl4 C111 Cl3 111.1(6) . . ? Cl4 C111 Cl5 110.0(6) . . ? Cl3 C111 Cl5 113.5(5) . . ? Cl4 C111 H133 107.3 . . ? Cl3 C111 H133 107.3 . . ? Cl5 C111 H133 107.3 . . ? Cl7 C112 Cl8 109(2) . . ? Cl7 C112 H134 115.4 . . ? Cl8 C112 H134 115.4 . . ? Cl10 C113 Cl9 105.8(18) . . ? Cl10 C113 Cl11 112(2) . . ? Cl9 C113 Cl11 106.9(18) . . ? Cl10 C113 H135 110.7 . . ? Cl9 C113 H135 110.7 . . ? Cl11 C113 H135 110.7 . . ? Cl12 C114 Cl14 111(2) . . ? Cl12 C114 Cl13 110(2) . . ? Cl14 C114 Cl13 110(2) . . ? Cl12 C114 H136 108.8 . . ? Cl14 C114 H136 108.8 . . ? Cl13 C114 H136 108.8 . . ? Cl15 C115 Cl16 105(2) . . ? Cl15 C115 Cl17 107(2) . . ? Cl16 C115 Cl17 106(2) . . ? Cl15 C115 H137 112.7 . . ? Cl16 C115 H137 112.7 . . ? Cl17 C115 H137 112.7 . . ? O13 S1 C116 106.5(7) . . ? O13 S1 C117 106.8(8) . . ? C116 S1 C117 87.8(7) . . ? S1 C116 H138 109.5 . . ? S1 C116 H139 109.5 . . ? H138 C116 H139 109.5 . . ? S1 C116 H140 109.5 . . ? H138 C116 H140 109.5 . . ? H139 C116 H140 109.5 . . ? S1 C117 H141 109.5 . . ? S1 C117 H142 109.5 . . ? H141 C117 H142 109.5 . . ? S1 C117 H143 109.5 . . ? H141 C117 H143 109.5 . . ? H142 C117 H143 109.5 . . ? O14 S2 C118 124(3) . . ? O14 S2 C119 97(2) . . ? C118 S2 C119 86.8(19) . . ? S2 C118 H144 109.5 . . ? S2 C118 H145 109.5 . . ? H144 C118 H145 109.5 . . ? S2 C118 H146 109.5 . . ? H144 C118 H146 109.5 . . ? H145 C118 H146 109.5 . . ? S2 C119 H147 109.5 . . ? S2 C119 H148 109.5 . . ? H147 C119 H148 109.5 . . ? S2 C119 H149 109.5 . . ? H147 C119 H149 109.5 . . ? H148 C119 H149 109.5 . . ? O15 S3 C120 115(3) . . ? O15 S3 C121 100(2) . . ? C120 S3 C121 89.3(19) . . ? S3 C120 H150 109.5 . . ? S3 C120 H151 109.5 . . ? H150 C120 H151 109.5 . . ? S3 C120 H152 109.5 . . ? H150 C120 H152 109.5 . . ? H151 C120 H152 109.5 . . ? S3 C121 H153 109.5 . . ? S3 C121 H154 109.5 . . ? H153 C121 H154 109.5 . . ? S3 C121 H155 109.5 . . ? H153 C121 H155 109.5 . . ? H154 C121 H155 109.5 . . ? O16 S4 C122 116.8(18) . . ? O16 S4 C123 96.9(17) . . ? C122 S4 C123 86.5(17) . . ? S4 C122 H156 109.5 . . ? S4 C122 H157 109.5 . . ? H156 C122 H157 109.5 . . ? S4 C122 H158 109.5 . . ? H156 C122 H158 109.5 . . ? H157 C122 H158 109.5 . . ? S4 C123 H159 109.5 . . ? S4 C123 H160 109.5 . . ? H159 C123 H160 109.5 . . ? S4 C123 H161 109.5 . . ? H159 C123 H161 109.5 . . ? H160 C123 H161 109.5 . . ? O17 S5 C124 116(2) . . ? O17 S5 C125 96.7(18) . . ? C124 S5 C125 82.4(17) . . ? S5 C124 H162 109.5 . . ? S5 C124 H163 109.5 . . ? H162 C124 H163 109.5 . . ? S5 C124 H164 109.5 . . ? H162 C124 H164 109.5 . . ? H163 C124 H164 109.5 . . ? S5 C125 H165 109.5 . . ? S5 C125 H166 109.5 . . ? H165 C125 H166 109.5 . . ? S5 C125 H167 109.5 . . ? H165 C125 H167 109.5 . . ? H166 C125 H167 109.5 . . ? C127 C126 H168 109.5 . . ? C127 C126 H169 109.5 . . ? H168 C126 H169 109.5 . . ? C127 C126 H170 109.5 . . ? H168 C126 H170 109.5 . . ? H169 C126 H170 109.5 . . ? O18 C127 O19 121.9(8) . . ? O18 C127 C126 126.2(9) . . ? O19 C127 C126 111.9(7) . . ? C127 O19 C128 115.7(6) . . ? O19 C128 C129 104.7(7) . . ? O19 C128 H171 110.8 . . ? C129 C128 H171 110.8 . . ? O19 C128 H172 110.8 . . ? C129 C128 H172 110.8 . . ? H171 C128 H172 108.9 . . ? C128 C129 H173 109.5 . . ? C128 C129 H174 109.5 . . ? H173 C129 H174 109.5 . . ? C128 C129 H175 109.5 . . ? H173 C129 H175 109.5 . . ? H174 C129 H175 109.5 . . ? C131 C130 H176 109.5 . . ? C131 C130 H177 109.5 . . ? H176 C130 H177 109.5 . . ? C131 C130 H178 109.5 . . ? H176 C130 H178 109.5 . . ? H177 C130 H178 109.5 . . ? O20 C131 O21 119.1(11) . . ? O20 C131 C130 126.4(9) . . ? O21 C131 C130 114.4(9) . . ? C131 O21 C132 117.3(8) . . ? O21 C132 C133 109.0(8) . . ? O21 C132 H179 109.9 . . ? C133 C132 H179 109.9 . . ? O21 C132 H180 109.9 . . ? C133 C132 H180 109.9 . . ? H179 C132 H180 108.3 . . ? C132 C133 H181 109.5 . . ? C132 C133 H182 109.5 . . ? H181 C133 H182 109.5 . . ? C132 C133 H183 109.5 . . ? H181 C133 H183 109.5 . . ? H182 C133 H183 109.5 . . ? C135 C134 H184 109.5 . . ? C135 C134 H185 109.5 . . ? H184 C134 H185 109.5 . . ? C135 C134 H186 109.5 . . ? H184 C134 H186 109.5 . . ? H185 C134 H186 109.5 . . ? O22 C135 O23 118.1(13) . . ? O22 C135 C134 131.5(13) . . ? O23 C135 C134 109.8(12) . . ? C135 O23 C136 114.3(10) . . ? C137 C136 O23 107.9(11) . . ? C137 C136 H187 110.1 . . ? O23 C136 H187 110.1 . . ? C137 C136 H188 110.1 . . ? O23 C136 H188 110.1 . . ? H187 C136 H188 108.4 . . ? C136 C137 H189 109.5 . . ? C136 C137 H190 109.5 . . ? H189 C137 H190 109.5 . . ? C136 C137 H191 109.5 . . ? H189 C137 H191 109.5 . . ? H190 C137 H191 109.5 . . ? C139 C138 H192 109.5 . . ? C139 C138 H193 109.5 . . ? H192 C138 H193 109.5 . . ? C139 C138 H194 109.5 . . ? H192 C138 H194 109.5 . . ? H193 C138 H194 109.5 . . ? O24 C139 O25 122(2) . . ? O24 C139 C138 125(2) . . ? O25 C139 C138 113.1(17) . . ? C139 O25 C140 116.4(15) . . ? O25 C140 C141 111.7(13) . . ? O25 C140 H195 109.3 . . ? C141 C140 H195 109.3 . . ? O25 C140 H196 109.3 . . ? C141 C140 H196 109.3 . . ? H195 C140 H196 107.9 . . ? C140 C141 H197 109.5 . . ? C140 C141 H198 109.5 . . ? H197 C141 H198 109.5 . . ? C140 C141 H199 109.5 . . ? H197 C141 H199 109.5 . . ? H198 C141 H199 109.5 . . ? C143 C142 H200 109.5 . . ? C143 C142 H201 109.5 . . ? H200 C142 H201 109.5 . . ? C143 C142 H202 109.5 . . ? H200 C142 H202 109.5 . . ? H201 C142 H202 109.5 . . ? O26 C143 O27 123.5(14) . . ? O26 C143 C142 121.6(14) . . ? O27 C143 C142 113.5(12) . . ? C143 O27 C144 121.0(11) . . ? C145 C144 O27 106.9(12) . . ? C145 C144 H203 110.3 . . ? O27 C144 H203 110.3 . . ? C145 C144 H204 110.3 . . ? O27 C144 H204 110.3 . . ? H203 C144 H204 108.6 . . ? C144 C145 H205 109.5 . . ? C144 C145 H206 109.5 . . ? H205 C145 H206 109.5 . . ? C144 C145 H207 109.5 . . ? H205 C145 H207 109.5 . . ? H206 C145 H207 109.5 . . ? C147 C146 H208 109.5 . . ? C147 C146 H209 109.5 . . ? H208 C146 H209 109.5 . . ? C147 C146 H210 109.5 . . ? H208 C146 H210 109.5 . . ? H209 C146 H210 109.5 . . ? O28 C147 O29 121.8(17) . . ? O28 C147 C146 128.1(19) . . ? O29 C147 C146 109.6(16) . . ? C147 O29 C148 117.1(14) . . ? O29 C148 C149 109.6(16) . . ? O29 C148 H211 109.7 . . ? C149 C148 H211 109.7 . . ? O29 C148 H212 109.7 . . ? C149 C148 H212 109.7 . . ? H211 C148 H212 108.2 . . ? C148 C149 H213 109.5 . . ? C148 C149 H214 109.5 . . ? H213 C149 H214 109.5 . . ? C148 C149 H215 109.5 . . ? H213 C149 H215 109.5 . . ? H214 C149 H215 109.5 . . ? C151 C150 H216 109.5 . . ? C151 C150 H217 109.5 . . ? H216 C150 H217 109.5 . . ? C151 C150 H218 109.5 . . ? H216 C150 H218 109.5 . . ? H217 C150 H218 109.5 . . ? O30 C151 O31 121.2(19) . . ? O30 C151 C150 128(2) . . ? O31 C151 C150 110.3(17) . . ? C151 O31 C152 117.8(16) . . ? O31 C152 C153 108.2(18) . . ? O31 C152 H219 110.1 . . ? C153 C152 H219 110.1 . . ? O31 C152 H220 110.1 . . ? C153 C152 H220 110.1 . . ? H219 C152 H220 108.4 . . ? C152 C153 H221 109.5 . . ? C152 C153 H222 109.5 . . ? H221 C153 H222 109.5 . . ? C152 C153 H223 109.5 . . ? H221 C153 H223 109.5 . . ? H222 C153 H223 109.5 . . ? C155 C154 H224 109.5 . . ? C155 C154 H225 109.5 . . ? H224 C154 H225 109.5 . . ? C155 C154 H226 109.5 . . ? H224 C154 H226 109.5 . . ? H225 C154 H226 109.5 . . ? O32 C155 O33 119.2(17) . . ? O32 C155 C154 134.1(18) . . ? O33 C155 C154 105.7(15) . . ? C155 O33 C156 111.6(14) . . ? C157 C156 O33 103.7(17) . . ? C157 C156 H227 111.0 . . ? O33 C156 H227 111.0 . . ? C157 C156 H228 111.0 . . ? O33 C156 H228 111.0 . . ? H227 C156 H228 109.0 . . ? C156 C157 H229 109.5 . . ? C156 C157 H230 109.5 . . ? H229 C157 H230 109.5 . . ? C156 C157 H231 109.5 . . ? H229 C157 H231 109.5 . . ? H230 C157 H231 109.5 . . ? C159 C158 H232 109.5 . . ? C159 C158 H233 109.5 . . ? H232 C158 H233 109.5 . . ? C159 C158 H234 109.5 . . ? H232 C158 H234 109.5 . . ? H233 C158 H234 109.5 . . ? O34 C159 O35 114(2) . . ? O34 C159 C158 132(3) . . ? O35 C159 C158 114(2) . . ? C159 O35 C160 109(2) . . ? C161 C160 O35 116(3) . . ? C161 C160 H235 108.3 . . ? O35 C160 H235 108.3 . . ? C161 C160 H236 108.3 . . ? O35 C160 H236 108.3 . . ? H235 C160 H236 107.4 . . ? C160 C161 H237 109.5 . . ? C160 C161 H238 109.5 . . ? H237 C161 H238 109.5 . . ? C160 C161 H239 109.5 . . ? H237 C161 H239 109.5 . . ? H238 C161 H239 109.5 . . ? C163 C162 H240 109.5 . . ? C163 C162 H241 109.5 . . ? H240 C162 H241 109.5 . . ? C163 C162 H242 109.5 . . ? H240 C162 H242 109.5 . . ? H241 C162 H242 109.5 . . ? O36 C163 O37 123(2) . . ? O36 C163 C162 132(3) . . ? O37 C163 C162 105(2) . . ? C163 O37 C164 120(2) . . ? O37 C164 C165 104(2) . . ? O37 C164 H243 111.0 . . ? C165 C164 H243 111.0 . . ? O37 C164 H244 111.0 . . ? C165 C164 H244 111.0 . . ? H243 C164 H244 109.0 . . ? C164 C165 H245 109.5 . . ? C164 C165 H246 109.5 . . ? H245 C165 H246 109.5 . . ? C164 C165 H247 109.5 . . ? H245 C165 H247 109.5 . . ? H246 C165 H247 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 C6 C1 C2 C3 -2.0(9) . . . . ? C43 C1 C2 C3 179.5(6) . . . . ? C1 C2 C3 C4 -0.2(9) . . . . ? C1 C2 C3 C73 -179.0(6) . . . . ? C2 C3 C4 C5 0.9(9) . . . . ? C73 C3 C4 C5 179.7(6) . . . . ? C3 C4 C5 C6 0.6(10) . . . . ? C3 C4 C5 C13 178.9(6) . . . . ? C2 C1 C6 C5 3.6(9) . . . . ? C43 C1 C6 C5 -177.9(6) . . . . ? C4 C5 C6 C1 -2.9(10) . . . . ? C13 C5 C6 C1 178.8(6) . . . . ? C12 C7 C8 C9 0.7(9) . . . . ? C65 C7 C8 C9 -178.6(6) . . . . ? C7 C8 C9 C10 -1.8(9) . . . . ? C7 C8 C9 C98 -178.7(6) . . . . ? C8 C9 C10 C11 1.8(10) . . . . ? C98 C9 C10 C11 178.8(6) . . . . ? C9 C10 C11 C12 -0.8(9) . . . . ? C9 C10 C11 C35 177.9(6) . . . . ? C10 C11 C12 C7 -0.4(9) . . . . ? C35 C11 C12 C7 -179.0(6) . . . . ? C8 C7 C12 C11 0.4(9) . . . . ? C65 C7 C12 C11 179.6(6) . . . . ? C4 C5 C13 C18 -126.2(7) . . . . ? C6 C5 C13 C18 52.0(10) . . . . ? C4 C5 C13 C14 47.4(9) . . . . ? C6 C5 C13 C14 -134.3(7) . . . . ? C18 C13 C14 O1 -170.9(7) . . . . ? C5 C13 C14 O1 15.4(10) . . . . ? C18 C13 C14 C15 6.4(10) . . . . ? C5 C13 C14 C15 -167.3(7) . . . . ? O1 C14 C15 C16 172.8(7) . . . . ? C13 C14 C15 C16 -4.4(11) . . . . ? O1 C14 C15 C23 -12.4(11) . . . . ? C13 C14 C15 C23 170.3(6) . . . . ? C23 C15 C16 C17 -176.1(7) . . . . ? C14 C15 C16 C17 -1.2(12) . . . . ? C15 C16 C17 C18 4.6(12) . . . . ? C15 C16 C17 C19 179.9(9) . . . . ? C14 C13 C18 C17 -3.1(12) . . . . ? C5 C13 C18 C17 170.6(7) . . . . ? C16 C17 C18 C13 -2.5(12) . . . . ? C19 C17 C18 C13 -177.9(8) . . . . ? C15 C14 O1 Ni1 9.3(10) . . . . ? C13 C14 O1 Ni1 -173.5(5) . . . . ? N2 Ni1 O1 C14 93.8(14) . . . . ? O4 Ni1 O1 C14 -169.0(5) . . . . ? N1 Ni1 O1 C14 1.2(6) . . . . ? C16 C17 C19 C21 128.0(9) . . . . ? C18 C17 C19 C21 -57.0(11) . . . . ? C16 C17 C19 C22 6.2(14) . . . . ? C18 C17 C19 C22 -178.7(9) . . . . ? C16 C17 C19 C20 -114.3(8) . . . . ? C18 C17 C19 C20 60.8(11) . . . . ? C16 C15 C23 N1 177.1(7) . . . . ? C14 C15 C23 N1 2.2(12) . . . . ? C15 C23 N1 C24 -175.8(7) . . . . ? C15 C23 N1 Ni1 10.4(10) . . . . ? N2 Ni1 N1 C23 178.8(6) . . . . ? O4 Ni1 N1 C23 94.6(10) . . . . ? O1 Ni1 N1 C23 -10.7(6) . . . . ? N2 Ni1 N1 C24 4.6(4) . . . . ? O4 Ni1 N1 C24 -79.7(11) . . . . ? O1 Ni1 N1 C24 175.1(4) . . . . ? C23 N1 C24 C29 -177.2(6) . . . . ? Ni1 N1 C24 C29 -2.7(7) . . . . ? C23 N1 C24 C25 0.9(10) . . . . ? Ni1 N1 C24 C25 175.4(5) . . . . ? C29 C24 C25 C26 1.2(10) . . . . ? N1 C24 C25 C26 -176.8(6) . . . . ? C24 C25 C26 O2 -179.7(7) . . . . ? C24 C25 C26 C27 2.1(10) . . . . ? O2 C26 C27 O3 -2.5(9) . . . . ? C25 C26 C27 O3 175.9(6) . . . . ? O2 C26 C27 C28 177.3(6) . . . . ? C25 C26 C27 C28 -4.3(11) . . . . ? O3 C27 C28 C29 -177.1(6) . . . . ? C26 C27 C28 C29 3.2(10) . . . . ? C25 C24 C29 C28 -2.3(10) . . . . ? N1 C24 C29 C28 175.9(6) . . . . ? C25 C24 C29 N2 -179.9(6) . . . . ? N1 C24 C29 N2 -1.7(8) . . . . ? C27 C28 C29 C24 0.1(10) . . . . ? C27 C28 C29 N2 177.4(6) . . . . ? C25 C26 O2 C30 3.6(10) . . . . ? C27 C26 O2 C30 -178.1(6) . . . . ? C28 C27 O3 C31 0.8(10) . . . . ? C26 C27 O3 C31 -179.4(6) . . . . ? C24 C29 N2 C32 -165.0(6) . . . . ? C28 C29 N2 C32 17.5(10) . . . . ? C24 C29 N2 Ni1 5.4(7) . . . . ? C28 C29 N2 Ni1 -172.1(5) . . . . ? O4 Ni1 N2 C32 -25.6(6) . . . . ? N1 Ni1 N2 C32 164.6(6) . . . . ? O1 Ni1 N2 C32 71.2(16) . . . . ? O4 Ni1 N2 C29 164.3(4) . . . . ? N1 Ni1 N2 C29 -5.5(5) . . . . ? O1 Ni1 N2 C29 -98.9(13) . . . . ? C29 N2 C32 C33 -166.9(6) . . . . ? Ni1 N2 C32 C33 23.9(10) . . . . ? N2 C32 C33 C38 173.3(6) . . . . ? N2 C32 C33 C34 1.5(10) . . . . ? C32 C33 C34 O4 -18.7(9) . . . . ? C38 C33 C34 O4 169.6(5) . . . . ? C32 C33 C34 C35 163.2(6) . . . . ? C38 C33 C34 C35 -8.5(8) . . . . ? O4 C34 C35 C36 -170.2(5) . . . . ? C33 C34 C35 C36 7.9(8) . . . . ? O4 C34 C35 C11 11.6(9) . . . . ? C33 C34 C35 C11 -170.4(5) . . . . ? C10 C11 C35 C36 49.1(8) . . . . ? C12 C11 C35 C36 -132.3(6) . . . . ? C10 C11 C35 C34 -132.6(6) . . . . ? C12 C11 C35 C34 46.0(8) . . . . ? C34 C35 C36 C37 -1.7(9) . . . . ? C11 C35 C36 C37 176.6(5) . . . . ? C35 C36 C37 C38 -4.2(9) . . . . ? C35 C36 C37 C39 -178.7(5) . . . . ? C36 C37 C38 C33 3.6(9) . . . . ? C39 C37 C38 C33 178.0(6) . . . . ? C32 C33 C38 C37 -169.2(6) . . . . ? C34 C33 C38 C37 2.7(9) . . . . ? C35 C34 O4 Ni1 -172.5(4) . . . . ? C33 C34 O4 Ni1 9.5(8) . . . . ? N2 Ni1 O4 C34 9.4(5) . . . . ? N1 Ni1 O4 C34 93.0(11) . . . . ? O1 Ni1 O4 C34 -161.1(5) . . . . ? C38 C37 C39 C40 15.9(9) . . . . ? C36 C37 C39 C40 -169.9(6) . . . . ? C38 C37 C39 C41 -105.5(8) . . . . ? C36 C37 C39 C41 68.7(7) . . . . ? C38 C37 C39 C42 134.9(7) . . . . ? C36 C37 C39 C42 -50.9(9) . . . . ? C2 C1 C43 C48 46.8(9) . . . . ? C6 C1 C43 C48 -131.7(6) . . . . ? C2 C1 C43 C44 -134.9(6) . . . . ? C6 C1 C43 C44 46.6(9) . . . . ? C48 C43 C44 O5 -167.8(5) . . . . ? C1 C43 C44 O5 13.8(10) . . . . ? C48 C43 C44 C45 9.7(9) . . . . ? C1 C43 C44 C45 -168.7(6) . . . . ? O5 C44 C45 C53 -21.6(10) . . . . ? C43 C44 C45 C53 160.9(6) . . . . ? O5 C44 C45 C46 167.8(6) . . . . ? C43 C44 C45 C46 -9.7(9) . . . . ? C53 C45 C46 C47 -168.0(7) . . . . ? C44 C45 C46 C47 2.8(10) . . . . ? C45 C46 C47 C48 4.0(10) . . . . ? C45 C46 C47 C49 -178.9(6) . . . . ? C44 C43 C48 C47 -2.9(9) . . . . ? C1 C43 C48 C47 175.5(6) . . . . ? C46 C47 C48 C43 -4.1(10) . . . . ? C49 C47 C48 C43 178.7(6) . . . . ? C43 C44 O5 Ni2 -171.1(5) . . . . ? C45 C44 O5 Ni2 11.5(8) . . . . ? N4 Ni2 O5 C44 94.9(10) . . . . ? N3 Ni2 O5 C44 8.2(5) . . . . ? O8 Ni2 O5 C44 -162.4(5) . . . . ? C46 C47 C49 C50 -116.5(8) . . . . ? C48 C47 C49 C50 60.4(8) . . . . ? C46 C47 C49 C51 121.2(7) . . . . ? C48 C47 C49 C51 -61.9(8) . . . . ? C46 C47 C49 C52 3.7(10) . . . . ? C48 C47 C49 C52 -179.4(6) . . . . ? C46 C45 C53 N3 175.9(6) . . . . ? C44 C45 C53 N3 5.2(11) . . . . ? C45 C53 N3 C54 -169.5(7) . . . . ? C45 C53 N3 Ni2 20.1(10) . . . . ? N4 Ni2 N3 C53 167.1(6) . . . . ? O8 Ni2 N3 C53 72.4(14) . . . . ? O5 Ni2 N3 C53 -23.3(6) . . . . ? N4 Ni2 N3 C54 -4.0(5) . . . . ? O8 Ni2 N3 C54 -98.7(12) . . . . ? O5 Ni2 N3 C54 165.5(5) . . . . ? C53 N3 C54 C59 -168.0(6) . . . . ? Ni2 N3 C54 C59 3.3(7) . . . . ? C53 N3 C54 C55 16.7(10) . . . . ? Ni2 N3 C54 C55 -172.0(5) . . . . ? C59 C54 C55 C56 1.8(10) . . . . ? N3 C54 C55 C56 176.9(7) . . . . ? C54 C55 C56 O6 -176.6(6) . . . . ? C54 C55 C56 C57 1.1(11) . . . . ? C55 C56 C57 O7 179.2(7) . . . . ? O6 C56 C57 O7 -2.9(9) . . . . ? C55 C56 C57 C58 -2.6(11) . . . . ? O6 C56 C57 C58 175.4(6) . . . . ? O7 C57 C58 C59 179.1(7) . . . . ? C56 C57 C58 C59 1.1(10) . . . . ? C57 C58 C59 C54 1.8(10) . . . . ? C57 C58 C59 N4 -176.7(7) . . . . ? C55 C54 C59 C58 -3.3(10) . . . . ? N3 C54 C59 C58 -178.9(6) . . . . ? C55 C54 C59 N4 175.5(6) . . . . ? N3 C54 C59 N4 -0.2(8) . . . . ? C55 C56 O6 C60 -0.2(10) . . . . ? C57 C56 O6 C60 -178.0(6) . . . . ? C58 C57 O7 C61 2.7(10) . . . . ? C56 C57 O7 C61 -179.1(6) . . . . ? C58 C59 N4 C62 1.4(10) . . . . ? C54 C59 N4 C62 -177.2(6) . . . . ? C58 C59 N4 Ni2 175.5(6) . . . . ? C54 C59 N4 Ni2 -3.1(7) . . . . ? N3 Ni2 N4 C62 177.8(6) . . . . ? O8 Ni2 N4 C62 -11.6(6) . . . . ? O5 Ni2 N4 C62 90.4(11) . . . . ? N3 Ni2 N4 C59 4.0(5) . . . . ? O8 Ni2 N4 C59 174.5(5) . . . . ? O5 Ni2 N4 C59 -83.4(10) . . . . ? C59 N4 C62 C63 -176.8(7) . . . . ? Ni2 N4 C62 C63 9.8(10) . . . . ? N4 C62 C63 C64 3.4(11) . . . . ? N4 C62 C63 C68 -178.7(6) . . . . ? C62 C63 C64 O8 -12.0(11) . . . . ? C68 C63 C64 O8 170.2(6) . . . . ? C62 C63 C64 C65 169.0(6) . . . . ? C68 C63 C64 C65 -8.8(10) . . . . ? O8 C64 C65 C66 -170.0(6) . . . . ? C63 C64 C65 C66 9.0(10) . . . . ? O8 C64 C65 C7 11.4(10) . . . . ? C63 C64 C65 C7 -169.6(7) . . . . ? C12 C7 C65 C66 49.6(9) . . . . ? C8 C7 C65 C66 -131.2(6) . . . . ? C12 C7 C65 C64 -131.7(7) . . . . ? C8 C7 C65 C64 47.5(10) . . . . ? C64 C65 C66 C67 -3.1(11) . . . . ? C7 C65 C66 C67 175.6(7) . . . . ? C65 C66 C67 C68 -3.5(11) . . . . ? C65 C66 C67 C69 178.5(7) . . . . ? C66 C67 C68 C63 3.8(11) . . . . ? C69 C67 C68 C63 -178.3(7) . . . . ? C64 C63 C68 C67 2.4(11) . . . . ? C62 C63 C68 C67 -175.5(7) . . . . ? C63 C64 O8 Ni2 6.8(9) . . . . ? C65 C64 O8 Ni2 -174.3(5) . . . . ? N4 Ni2 O8 C64 3.7(5) . . . . ? N3 Ni2 O8 C64 97.7(13) . . . . ? O5 Ni2 O8 C64 -166.1(5) . . . . ? C68 C67 C69 C70 -1.2(11) . . . . ? C66 C67 C69 C70 176.7(7) . . . . ? C68 C67 C69 C71 -122.1(8) . . . . ? C66 C67 C69 C71 55.8(9) . . . . ? C68 C67 C69 C72 119.0(8) . . . . ? C66 C67 C69 C72 -63.1(9) . . . . ? C2 C3 C73 C78 -134.5(6) . . . . ? C4 C3 C73 C78 46.7(7) . . . . ? C2 C3 C73 C74 48.0(8) . . . . ? C4 C3 C73 C74 -130.8(6) . . . . ? C78 C73 C74 O9 -172.0(4) . . . . ? C3 C73 C74 O9 5.4(7) . . . . ? C78 C73 C74 C75 7.1(6) . . . . ? C3 C73 C74 C75 -175.4(4) . . . . ? O9 C74 C75 C76 170.2(4) . . . . ? C73 C74 C75 C76 -8.9(7) . . . . ? O9 C74 C75 C86 -14.9(7) . . . . ? C73 C74 C75 C86 166.0(4) . . . . ? C74 C75 C76 C77 5.3(7) . . . . ? C86 C75 C76 C77 -169.8(5) . . . . ? C75 C76 C77 C78 0.6(7) . . . . ? C75 C76 C77 C79 178.7(5) . . . . ? C74 C73 C78 C77 -1.6(7) . . . . ? C3 C73 C78 C77 -179.1(5) . . . . ? C76 C77 C78 C73 -2.4(7) . . . . ? C79 C77 C78 C73 179.5(5) . . . . ? C75 C74 O9 Ni3 7.9(6) . . . . ? C73 C74 O9 Ni3 -173.0(3) . . . . ? O12 Ni3 O9 C74 -161.9(4) . . . . ? N5 Ni3 O9 C74 8.1(4) . . . . ? N6 Ni3 O9 C74 97.2(15) . . . . ? C76 C77 C79 C82 -46.7(9) . . . . ? C78 C77 C79 C82 131.2(8) . . . . ? C76 C77 C79 C83 135.0(16) . . . . ? C78 C77 C79 C83 -47.1(17) . . . . ? C76 C77 C79 C80 -169.2(7) . . . . ? C78 C77 C79 C80 8.7(9) . . . . ? C76 C77 C79 C81 73.2(9) . . . . ? C78 C77 C79 C81 -108.9(8) . . . . ? C76 C77 C79 C84 17.5(16) . . . . ? C78 C77 C79 C84 -164.6(15) . . . . ? C76 C77 C79 C85 -98.9(18) . . . . ? C78 C77 C79 C85 79.0(18) . . . . ? C76 C75 C86 N5 174.8(5) . . . . ? C74 C75 C86 N5 -0.3(8) . . . . ? C75 C86 N5 C87 -171.4(4) . . . . ? C75 C86 N5 Ni3 21.0(7) . . . . ? O12 Ni3 N5 C86 73.9(16) . . . . ? O9 Ni3 N5 C86 -21.9(5) . . . . ? N6 Ni3 N5 C86 167.6(5) . . . . ? O12 Ni3 N5 C87 -94.6(14) . . . . ? O9 Ni3 N5 C87 169.6(3) . . . . ? N6 Ni3 N5 C87 -0.9(3) . . . . ? C86 N5 C87 C92 -168.4(5) . . . . ? Ni3 N5 C87 C92 0.6(5) . . . . ? C86 N5 C87 C88 13.1(7) . . . . ? Ni3 N5 C87 C88 -178.0(4) . . . . ? C92 C87 C88 C89 1.9(8) . . . . ? N5 C87 C88 C89 -179.6(5) . . . . ? C87 C88 C89 O10 -179.4(5) . . . . ? C87 C88 C89 C90 0.6(7) . . . . ? O10 C89 C90 O11 -1.8(6) . . . . ? C88 C89 C90 O11 178.2(4) . . . . ? O10 C89 C90 C91 178.3(5) . . . . ? C88 C89 C90 C91 -1.7(7) . . . . ? O11 C90 C91 C92 -179.6(5) . . . . ? C89 C90 C91 C92 0.2(7) . . . . ? C88 C87 C92 C91 -3.4(7) . . . . ? N5 C87 C92 C91 178.0(4) . . . . ? C88 C87 C92 N6 178.8(4) . . . . ? N5 C87 C92 N6 0.2(6) . . . . ? C90 C91 C92 C87 2.3(7) . . . . ? C90 C91 C92 N6 179.8(5) . . . . ? C88 C89 O10 C93 -2.4(7) . . . . ? C90 C89 O10 C93 177.6(5) . . . . ? C91 C90 O11 C94 -8.7(7) . . . . ? C89 C90 O11 C94 171.4(4) . . . . ? C87 C92 N6 C95 -173.4(5) . . . . ? C91 C92 N6 C95 9.0(8) . . . . ? C87 C92 N6 Ni3 -0.9(5) . . . . ? C91 C92 N6 Ni3 -178.5(4) . . . . ? O12 Ni3 N6 C95 -16.8(4) . . . . ? N5 Ni3 N6 C95 173.3(4) . . . . ? O9 Ni3 N6 C95 83.4(15) . . . . ? O12 Ni3 N6 C92 170.9(3) . . . . ? N5 Ni3 N6 C92 1.0(3) . . . . ? O9 Ni3 N6 C92 -88.9(15) . . . . ? C92 N6 C95 C96 -173.8(5) . . . . ? Ni3 N6 C95 C96 14.6(8) . . . . ? N6 C95 C96 C101 178.0(5) . . . . ? N6 C95 C96 C97 4.3(9) . . . . ? C101 C96 C97 O12 168.6(5) . . . . ? C95 C96 C97 O12 -17.8(8) . . . . ? C101 C96 C97 C98 -9.8(8) . . . . ? C95 C96 C97 C98 163.8(5) . . . . ? O12 C97 C98 C99 -166.0(5) . . . . ? C96 C97 C98 C99 12.4(8) . . . . ? O12 C97 C98 C9 17.8(8) . . . . ? C96 C97 C98 C9 -163.8(5) . . . . ? C8 C9 C98 C99 44.0(9) . . . . ? C10 C9 C98 C99 -133.0(6) . . . . ? C8 C9 C98 C97 -139.8(6) . . . . ? C10 C9 C98 C97 43.3(8) . . . . ? C97 C98 C99 C100 -5.4(9) . . . . ? C9 C98 C99 C100 170.8(6) . . . . ? C98 C99 C100 C101 -4.8(9) . . . . ? C98 C99 C100 C102 -180.0(6) . . . . ? C99 C100 C101 C96 7.5(9) . . . . ? C102 C100 C101 C96 -177.3(6) . . . . ? C95 C96 C101 C100 -173.8(6) . . . . ? C97 C96 C101 C100 -0.2(9) . . . . ? C98 C97 O12 Ni3 -170.7(4) . . . . ? C96 C97 O12 Ni3 11.0(8) . . . . ? N5 Ni3 O12 C97 97.5(15) . . . . ? O9 Ni3 O12 C97 -166.1(4) . . . . ? N6 Ni3 O12 C97 4.5(4) . . . . ? C101 C100 C102 C108 48.9(19) . . . . ? C99 C100 C102 C108 -136.3(18) . . . . ? C101 C100 C102 C107 167.9(13) . . . . ? C99 C100 C102 C107 -17.3(15) . . . . ? C101 C100 C102 C104 -122.8(11) . . . . ? C99 C100 C102 C104 51.9(12) . . . . ? C101 C100 C102 C103 0.1(12) . . . . ? C99 C100 C102 C103 174.8(9) . . . . ? C101 C100 C102 C105 114.6(10) . . . . ? C99 C100 C102 C105 -70.6(10) . . . . ? C101 C100 C102 C106 -72.2(16) . . . . ? C99 C100 C102 C106 102.6(16) . . . . ? O18 C127 O19 C128 0.1(14) . . . . ? C126 C127 O19 C128 -178.7(8) . . . . ? C127 O19 C128 C129 177.6(9) . . . . ? O20 C131 O21 C132 -1.7(12) . . . . ? C130 C131 O21 C132 179.6(8) . . . . ? C131 O21 C132 C133 -171.4(7) . . . . ? O22 C135 O23 C136 -4(2) . . . . ? C134 C135 O23 C136 -175.9(13) . . . . ? C135 O23 C136 C137 -171.9(13) . . . . ? O24 C139 O25 C140 -1(2) . . . . ? C138 C139 O25 C140 -176.0(11) . . . . ? C139 O25 C140 C141 -162.8(11) . . . . ? O26 C143 O27 C144 -6(3) . . . . ? C142 C143 O27 C144 -173.1(12) . . . . ? C143 O27 C144 C145 167.4(13) . . . . ? O28 C147 O29 C148 -6(5) . . . . ? C146 C147 O29 C148 -179(3) . . . . ? C147 O29 C148 C149 -177(3) . . . . ? O30 C151 O31 C152 -6(7) . . . . ? C150 C151 O31 C152 179(4) . . . . ? C151 O31 C152 C153 -178(4) . . . . ? O32 C155 O33 C156 -6(3) . . . . ? C154 C155 O33 C156 -176.9(15) . . . . ? C155 O33 C156 C157 -154(2) . . . . ? O34 C159 O35 C160 0.2(7) . . . . ? C158 C159 O35 C160 -179.9(4) . . . . ? C159 O35 C160 C161 179.9(4) . . . . ? O36 C163 O37 C164 0.2(8) . . . . ? C162 C163 O37 C164 -180.0(4) . . . . ? C163 O37 C164 C165 179.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.959 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 963503'