# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Braunstein, Pierre' _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_section_title ; Nuclearity of Nickel and Mixed Sodium-Nickel Complexes: Dependence on the Spacer in Chelating Pyridine-Alcoholate Ligands ; _publ_author_name P.Braunstein # Attachment '- compound2_revised.cif' data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 776753' #TrackingRef '- compound2_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C120 H122 N20 Na10 Ni6 O22' _chemical_formula_sum 'C120 H122 N20 Na10 Ni6 O22' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour green _diffrn_ambient_temperature 173(2) _chemical_formula_weight 2778.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.6401(9) _cell_length_b 18.7399(9) _cell_length_c 28.9389(13) _cell_angle_alpha 98.239(3) _cell_angle_beta 91.523(3) _cell_angle_gamma 97.769(3) _cell_volume 8839.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 100165 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.103 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79012 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.1516 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 25.50 _reflns_number_total 32717 _reflns_number_gt 14378 _reflns_threshold_expression >2sigma(I) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.500 0.635 0.174 3375 1868 ' ' _platon_squeeze_details ; ; _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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. The hydrogen atoms bound to the m-5 oxygen. These were found in the Fo-Fc map and refined isotropically. The O-H bond was constrained to 0.95 \%A, in order to overcome the typical underestimation of O-H bonds lengths by X-ray diffraction. In the crystals, very large voids containing severely disordered solvent molecules were present. None of the atomic positions corresponded to more than a 2.5 e/\%A3 electron density. This disorder affected considerably the model quality and therefore we have chosen to apply a PLATON-SQUEEZE procedure run using the complete molecular model. The calculation estimated a residual electron density of 1868 e/unit cell, total void volume in the unit cell: 3375 \%A3 The modified reflection data were then used for the refinement of the molecular structure, resulting in improved refinement parameters. ; _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^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 32717 _refine_ls_number_parameters 1609 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.018 _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 1.14384(3) 0.45835(3) 0.356568(19) 0.04252(16) Uani 1 1 d . . . Ni2 Ni 0.74970(3) 0.49944(3) 0.433155(19) 0.04479(17) Uani 1 1 d . . . Ni3 Ni 0.90019(4) 0.19796(3) 0.42909(2) 0.05296(19) Uani 1 1 d . . . Ni4 Ni 0.14068(4) 0.30233(3) 0.04328(2) 0.04735(17) Uani 1 1 d . . . Ni5 Ni -0.01270(3) 0.05619(3) 0.164057(18) 0.04188(16) Uani 1 1 d . . . Ni6 Ni 0.27724(3) -0.00155(3) -0.003429(19) 0.04412(17) Uani 1 1 d . . . Na1 Na 1.02726(10) 0.33489(8) 0.40215(5) 0.0438(4) Uani 1 1 d . . . Na2 Na 0.97688(10) 0.48671(8) 0.40479(6) 0.0462(5) Uani 1 1 d . . . Na3 Na 1.13877(10) 0.46379(9) 0.46907(5) 0.0453(5) Uani 1 1 d . . . Na4 Na 0.85697(10) 0.36654(8) 0.44227(6) 0.0483(5) Uani 1 1 d . . . Na5 Na 0.99223(11) 0.31734(9) 0.51039(6) 0.0521(5) Uani 1 1 d . . . Na6 Na 0.05074(10) 0.17157(8) 0.09585(5) 0.0442(4) Uani 1 1 d . . . Na7 Na 0.09111(10) 0.01400(8) 0.07583(5) 0.0424(4) Uani 1 1 d . . . Na8 Na -0.10204(10) 0.04411(8) 0.06251(5) 0.0443(4) Uani 1 1 d . . . Na9 Na 0.16735(10) 0.13063(9) 0.01542(6) 0.0468(5) Uani 1 1 d . . . Na10 Na -0.00382(10) 0.18570(9) -0.00949(6) 0.0460(5) Uani 1 1 d . . . O1 O 1.16086(17) 0.38106(15) 0.39838(9) 0.0455(8) Uani 1 1 d . . . O2 O 1.02570(16) 0.41585(14) 0.34410(9) 0.0429(8) Uani 1 1 d . . . O3 O 1.11567(17) 0.52913(15) 0.41135(9) 0.0445(8) Uani 1 1 d . . . O4 O 0.99368(17) 0.41613(14) 0.46546(9) 0.0422(8) Uani 1 1 d D . . O5 O 0.77448(17) 0.44477(15) 0.48588(10) 0.0457(8) Uani 1 1 d . . . O6 O 0.83091(16) 0.58835(14) 0.46262(10) 0.0442(8) Uani 1 1 d . . . O7 O 0.83186(17) 0.45286(15) 0.39294(10) 0.0486(8) Uani 1 1 d . . . O8 O 0.90012(19) 0.27160(15) 0.38416(10) 0.0489(8) Uani 1 1 d . . . O9 O 1.01892(17) 0.23906(15) 0.44926(10) 0.0487(8) Uani 1 1 d . . . O10 O 0.85899(19) 0.26656(15) 0.48167(10) 0.0542(9) Uani 1 1 d . . . O11 O 1.04792(18) 0.39332(15) 0.58289(11) 0.0547(9) Uani 1 1 d . . . O12 O 0.17564(19) 0.23020(15) 0.08251(10) 0.0514(8) Uani 1 1 d . . . O13 O -0.06322(17) 0.13115(15) 0.13150(9) 0.0438(8) Uani 1 1 d . . . O14 O 0.10031(16) 0.09097(15) 0.14518(9) 0.0414(8) Uani 1 1 d . . . O15 O -0.03308(17) -0.01976(15) 0.10650(9) 0.0431(8) Uani 1 1 d . . . O16 O 0.02871(17) 0.08601(14) 0.02785(9) 0.0405(7) Uani 1 1 d D . . O17 O 0.21241(17) 0.04660(15) -0.04616(10) 0.0463(8) Uani 1 1 d . . . O18 O 0.19124(17) -0.09299(14) -0.01231(10) 0.0467(8) Uani 1 1 d . . . O19 O 0.22622(17) 0.04786(15) 0.05308(10) 0.0466(8) Uani 1 1 d . . . O20 O 0.13669(18) 0.22995(15) -0.01674(10) 0.0472(8) Uani 1 1 d . . . O21 O 0.02179(17) 0.26861(15) 0.05543(9) 0.0474(8) Uani 1 1 d . . . O22 O 0.11256(18) -0.10870(15) 0.05648(10) 0.0474(8) Uani 1 1 d . . . N1 N 0.6707(2) 0.5687(2) 0.46848(13) 0.0490(10) Uani 1 1 d . . . N2 N 0.7229(2) 0.5370(2) 0.36959(13) 0.0524(10) Uani 1 1 d . . . N3 N 0.6584(2) 0.4051(2) 0.41741(15) 0.0496(10) Uani 1 1 d . . . N4 N 0.8742(3) 0.1253(2) 0.47900(14) 0.0664(13) Uani 1 1 d . . . N5 N 1.0323(3) 0.2475(2) 0.57473(15) 0.0679(13) Uani 1 1 d . . . N6 N 0.9610(3) 0.12095(19) 0.38826(14) 0.0533(11) Uani 1 1 d . . . N7 N 0.7862(3) 0.1601(2) 0.39511(17) 0.0657(13) Uani 1 1 d . . . N8 N 1.1425(2) 0.55552(19) 0.32491(13) 0.0466(10) Uani 1 1 d . . . N9 N 1.1509(2) 0.39524(18) 0.29075(12) 0.0431(10) Uani 1 1 d . . . N10 N 1.2716(2) 0.4784(2) 0.36849(12) 0.0463(10) Uani 1 1 d . . . N11 N 0.3269(2) -0.0708(2) -0.05675(12) 0.0490(10) Uani 1 1 d . . . N12 N 0.3452(2) -0.03596(19) 0.04964(12) 0.0456(10) Uani 1 1 d . . . N13 N 0.3597(2) 0.0937(2) -0.00812(14) 0.0487(10) Uani 1 1 d . . . N14 N 0.1198(3) 0.38313(19) 0.09857(12) 0.0520(11) Uani 1 1 d . . . N15 N 0.1241(2) 0.37282(19) -0.00700(13) 0.0505(10) Uani 1 1 d . . . N16 N 0.0213(2) -0.03865(19) 0.18953(12) 0.0441(10) Uani 1 1 d . . . N17 N 0.0849(3) -0.2547(2) 0.05832(14) 0.0573(11) Uani 1 1 d . . . N18 N 0.0302(2) 0.12839(17) 0.22487(11) 0.0400(9) Uani 1 1 d . . . N19 N -0.1329(2) 0.0428(2) 0.18798(12) 0.0462(10) Uani 1 1 d . . . N20 N 0.2685(2) 0.3361(2) 0.04752(15) 0.0548(11) Uani 1 1 d . . . C1 C 0.7967(3) 0.6524(2) 0.47315(17) 0.0550(14) Uani 1 1 d . . . H1A H 0.8067 0.6821 0.4476 0.066 Uiso 1 1 calc R . . H1B H 0.8236 0.6810 0.5022 0.066 Uiso 1 1 calc R . . C2 C 0.7054(3) 0.6380(3) 0.47951(15) 0.0494(13) Uani 1 1 d . . . C3 C 0.5917(3) 0.5551(3) 0.47302(16) 0.0595(14) Uani 1 1 d . . . H3 H 0.5664 0.5059 0.4662 0.071 Uiso 1 1 calc R . . C4 C 0.5440(3) 0.6076(3) 0.48705(18) 0.0667(16) Uani 1 1 d . . . H4 H 0.4870 0.5952 0.4888 0.080 Uiso 1 1 calc R . . C5 C 0.5811(4) 0.6800(3) 0.49872(19) 0.0754(17) Uani 1 1 d . . . H5 H 0.5498 0.7176 0.5089 0.090 Uiso 1 1 calc R . . C6 C 0.6640(3) 0.6954(3) 0.49518(16) 0.0606(15) Uani 1 1 d . . . H6 H 0.6916 0.7436 0.5032 0.073 Uiso 1 1 calc R . . C7 C 0.8179(3) 0.4532(3) 0.34570(17) 0.0616(15) Uani 1 1 d . . . H7A H 0.7987 0.4026 0.3308 0.074 Uiso 1 1 calc R . . H7B H 0.8702 0.4689 0.3322 0.074 Uiso 1 1 calc R . . C8 C 0.7582(3) 0.5005(3) 0.33311(17) 0.0535(13) Uani 1 1 d . . . C9 C 0.6671(3) 0.5807(3) 0.3602(2) 0.0670(15) Uani 1 1 d . . . H9 H 0.6438 0.6075 0.3855 0.080 Uiso 1 1 calc R . . C10 C 0.6437(4) 0.5874(3) 0.3159(2) 0.091(2) Uani 1 1 d . . . H10 H 0.6033 0.6168 0.3102 0.109 Uiso 1 1 calc R . . C11 C 0.6811(4) 0.5495(4) 0.2782(2) 0.102(2) Uani 1 1 d . . . H11 H 0.6668 0.5540 0.2468 0.123 Uiso 1 1 calc R . . C12 C 0.7374(4) 0.5065(3) 0.28739(19) 0.0742(17) Uani 1 1 d . . . H12 H 0.7625 0.4806 0.2624 0.089 Uiso 1 1 calc R . . C13 C 0.6548(3) 0.3656(3) 0.45327(18) 0.0482(13) Uani 1 1 d . . . C14 C 0.7061(3) 0.3987(2) 0.49605(15) 0.0508(13) Uani 1 1 d . . . H14A H 0.6732 0.4268 0.5180 0.061 Uiso 1 1 calc R . . H14B H 0.7237 0.3594 0.5117 0.061 Uiso 1 1 calc R . . C15 C 0.6084(3) 0.2983(3) 0.4481(2) 0.0612(15) Uani 1 1 d . . . H15 H 0.6071 0.2708 0.4733 0.073 Uiso 1 1 calc R . . C16 C 0.5678(3) 0.3107(3) 0.3710(2) 0.0744(18) Uani 1 1 d . . . H16 H 0.5379 0.2928 0.3424 0.089 Uiso 1 1 calc R . . C17 C 0.5633(3) 0.2697(3) 0.4070(2) 0.0761(18) Uani 1 1 d . . . H17 H 0.5305 0.2235 0.4038 0.091 Uiso 1 1 calc R . . C18 C 0.6168(3) 0.3795(3) 0.37683(19) 0.0647(15) Uani 1 1 d . . . H18 H 0.6203 0.4075 0.3519 0.078 Uiso 1 1 calc R . . C19 C 0.8050(3) 0.2287(2) 0.50781(17) 0.0607(15) Uani 1 1 d . . . H19A H 0.7498 0.2234 0.4930 0.073 Uiso 1 1 calc R . . H19B H 0.8044 0.2569 0.5394 0.073 Uiso 1 1 calc R . . C20 C 0.8268(3) 0.1534(3) 0.51214(19) 0.0667(16) Uani 1 1 d . . . C21 C 0.8929(4) 0.0570(3) 0.4799(2) 0.0857(19) Uani 1 1 d . . . H21 H 0.9275 0.0377 0.4572 0.103 Uiso 1 1 calc R . . C22 C 0.8633(4) 0.0149(3) 0.5126(2) 0.097(2) Uani 1 1 d . . . H22 H 0.8766 -0.0329 0.5120 0.117 Uiso 1 1 calc R . . C23 C 0.8144(4) 0.0426(3) 0.5463(2) 0.111(3) Uani 1 1 d . . . H23 H 0.7937 0.0141 0.5691 0.133 Uiso 1 1 calc R . . C24 C 0.7960(4) 0.1121(3) 0.5465(2) 0.093(2) Uani 1 1 d . . . H24 H 0.7627 0.1321 0.5697 0.111 Uiso 1 1 calc R . . C25 C 1.0632(3) 0.3641(2) 0.62343(18) 0.0615(15) Uani 1 1 d . . . H25A H 1.0289 0.3840 0.6481 0.074 Uiso 1 1 calc R . . H25B H 1.1206 0.3806 0.6341 0.074 Uiso 1 1 calc R . . C26 C 1.0480(3) 0.2824(3) 0.61821(19) 0.0622(15) Uani 1 1 d . . . C27 C 1.0188(4) 0.1742(3) 0.5698(2) 0.0833(19) Uani 1 1 d . . . H27 H 1.0085 0.1484 0.5390 0.100 Uiso 1 1 calc R . . C28 C 1.0188(5) 0.1339(3) 0.6060(3) 0.119(3) Uani 1 1 d . . . H28 H 1.0110 0.0822 0.6002 0.143 Uiso 1 1 calc R . . C29 C 1.0303(5) 0.1702(4) 0.6503(2) 0.124(3) Uani 1 1 d . . . H29 H 1.0284 0.1446 0.6764 0.148 Uiso 1 1 calc R . . C30 C 1.0449(4) 0.2449(3) 0.6563(2) 0.107(2) Uani 1 1 d . . . H30 H 1.0531 0.2714 0.6870 0.129 Uiso 1 1 calc R . . C31 C 1.0730(3) 0.1897(2) 0.43814(16) 0.0579(14) Uani 1 1 d . . . H31A H 1.0871 0.1696 0.4666 0.069 Uiso 1 1 calc R . . H31B H 1.1235 0.2157 0.4277 0.069 Uiso 1 1 calc R . . C32 C 1.0400(4) 0.1272(2) 0.40016(17) 0.0570(15) Uani 1 1 d . . . C33 C 0.9304(3) 0.0669(2) 0.35487(17) 0.0599(15) Uani 1 1 d . . . H33 H 0.8742 0.0627 0.3463 0.072 Uiso 1 1 calc R . . C34 C 0.9743(4) 0.0168(3) 0.33188(19) 0.0718(17) Uani 1 1 d . . . H34 H 0.9500 -0.0206 0.3080 0.086 Uiso 1 1 calc R . . C35 C 1.0550(4) 0.0237(3) 0.34528(18) 0.0702(17) Uani 1 1 d . . . H35 H 1.0874 -0.0103 0.3307 0.084 Uiso 1 1 calc R . . C36 C 1.0901(3) 0.0791(3) 0.37949(16) 0.0603(15) Uani 1 1 d . . . H36 H 1.1461 0.0841 0.3886 0.072 Uiso 1 1 calc R . . C37 C 0.7720(3) 0.1957(3) 0.3582(2) 0.0629(16) Uani 1 1 d . . . C38 C 0.8396(3) 0.2552(3) 0.34972(18) 0.0624(15) Uani 1 1 d . . . H38A H 0.8638 0.2397 0.3197 0.075 Uiso 1 1 calc R . . H38B H 0.8156 0.2999 0.3466 0.075 Uiso 1 1 calc R . . C39 C 0.7015(4) 0.1795(3) 0.3302(2) 0.089(2) Uani 1 1 d . . . H39 H 0.6937 0.2062 0.3053 0.107 Uiso 1 1 calc R . . C40 C 0.6568(5) 0.0867(4) 0.3768(3) 0.114(3) Uani 1 1 d . . . H40 H 0.6179 0.0488 0.3845 0.137 Uiso 1 1 calc R . . C41 C 0.6419(4) 0.1239(5) 0.3386(3) 0.112(3) Uani 1 1 d . . . H41 H 0.5932 0.1113 0.3196 0.134 Uiso 1 1 calc R . . C42 C 0.7262(4) 0.1065(3) 0.4013(2) 0.086(2) Uani 1 1 d . . . H42 H 0.7352 0.0800 0.4262 0.103 Uiso 1 1 calc R . . C43 C 1.1454(3) 0.5998(2) 0.40790(15) 0.0470(12) Uani 1 1 d . . . H43A H 1.2015 0.6112 0.4217 0.056 Uiso 1 1 calc R . . H43B H 1.1118 0.6326 0.4260 0.056 Uiso 1 1 calc R . . C44 C 1.1454(3) 0.6139(3) 0.35745(16) 0.0502(13) Uani 1 1 d . . . C45 C 1.1436(4) 0.5645(3) 0.28008(18) 0.0737(17) Uani 1 1 d . . . H45 H 1.1414 0.5227 0.2569 0.088 Uiso 1 1 calc R . . C46 C 1.1479(5) 0.6327(3) 0.2659(2) 0.115(3) Uani 1 1 d . . . H46 H 1.1459 0.6372 0.2336 0.137 Uiso 1 1 calc R . . C47 C 1.1552(4) 0.6934(3) 0.2992(2) 0.103(2) Uani 1 1 d . . . H47 H 1.1629 0.7408 0.2905 0.123 Uiso 1 1 calc R . . C48 C 1.1512(3) 0.6840(3) 0.34542(19) 0.0663(15) Uani 1 1 d . . . H48 H 1.1523 0.7250 0.3690 0.080 Uiso 1 1 calc R . . C49 C 1.0059(3) 0.3890(2) 0.29752(15) 0.0496(13) Uani 1 1 d . . . H49A H 0.9800 0.4256 0.2832 0.059 Uiso 1 1 calc R . . H49B H 0.9656 0.3446 0.2956 0.059 Uiso 1 1 calc R . . C50 C 1.0782(3) 0.3707(2) 0.26931(15) 0.0459(12) Uani 1 1 d . . . C51 C 1.2180(3) 0.3824(2) 0.26682(16) 0.0535(13) Uani 1 1 d . . . H51 H 1.2697 0.3998 0.2819 0.064 Uiso 1 1 calc R . . C52 C 1.2150(3) 0.3452(2) 0.22165(16) 0.0552(14) Uani 1 1 d . . . H52 H 1.2631 0.3379 0.2058 0.066 Uiso 1 1 calc R . . C53 C 1.1379(3) 0.3188(2) 0.20044(16) 0.0530(13) Uani 1 1 d . . . H53 H 1.1327 0.2925 0.1697 0.064 Uiso 1 1 calc R . . C54 C 1.0697(3) 0.3315(2) 0.22471(15) 0.0480(12) Uani 1 1 d . . . H54 H 1.0171 0.3133 0.2109 0.058 Uiso 1 1 calc R . . C55 C 1.2383(3) 0.3625(2) 0.39532(16) 0.0537(13) Uani 1 1 d . . . H55A H 1.2380 0.3207 0.3701 0.064 Uiso 1 1 calc R . . H55B H 1.2544 0.3469 0.4251 0.064 Uiso 1 1 calc R . . C56 C 1.3009(3) 0.4250(3) 0.38534(15) 0.0464(12) Uani 1 1 d . . . C57 C 1.3253(3) 0.5339(3) 0.35867(17) 0.0632(15) Uani 1 1 d . . . H57 H 1.3045 0.5740 0.3484 0.076 Uiso 1 1 calc R . . C58 C 1.4084(4) 0.5367(3) 0.3625(2) 0.0800(18) Uani 1 1 d . . . H58 H 1.4441 0.5760 0.3538 0.096 Uiso 1 1 calc R . . C59 C 1.4368(3) 0.4799(4) 0.3794(2) 0.0834(19) Uani 1 1 d . . . H59 H 1.4936 0.4797 0.3833 0.100 Uiso 1 1 calc R . . C60 C 1.3843(3) 0.4239(3) 0.39070(18) 0.0652(15) Uani 1 1 d . . . H60 H 1.4040 0.3842 0.4021 0.078 Uiso 1 1 calc R . . C61 C 0.2203(3) -0.1558(2) -0.03255(16) 0.0558(14) Uani 1 1 d . . . H61A H 0.1762 -0.1875 -0.0522 0.067 Uiso 1 1 calc R . . H61B H 0.2364 -0.1827 -0.0075 0.067 Uiso 1 1 calc R . . C62 C 0.2916(3) -0.1404(3) -0.06193(16) 0.0536(13) Uani 1 1 d . . . C63 C 0.3925(3) -0.0540(3) -0.08206(16) 0.0602(14) Uani 1 1 d . . . H63 H 0.4170 -0.0046 -0.0787 0.072 Uiso 1 1 calc R . . C64 C 0.4254(3) -0.1043(3) -0.11213(17) 0.0692(17) Uani 1 1 d . . . H64 H 0.4720 -0.0905 -0.1287 0.083 Uiso 1 1 calc R . . C65 C 0.3890(4) -0.1749(3) -0.11749(18) 0.0757(18) Uani 1 1 d . . . H65 H 0.4102 -0.2109 -0.1383 0.091 Uiso 1 1 calc R . . C66 C 0.3208(3) -0.1946(3) -0.09254(17) 0.0640(16) Uani 1 1 d . . . H66 H 0.2950 -0.2436 -0.0963 0.077 Uiso 1 1 calc R . . C67 C 0.2688(3) 0.0480(3) 0.09492(17) 0.0568(14) Uani 1 1 d . . . H67A H 0.2295 0.0360 0.1187 0.068 Uiso 1 1 calc R . . H67B H 0.2970 0.0979 0.1055 0.068 Uiso 1 1 calc R . . C68 C 0.3306(3) -0.0040(2) 0.09302(17) 0.0478(13) Uani 1 1 d . . . C69 C 0.3996(3) -0.0848(3) 0.04733(19) 0.0580(14) Uani 1 1 d . . . H69 H 0.4119 -0.1073 0.0173 0.070 Uiso 1 1 calc R . . C70 C 0.4366(3) -0.1029(3) 0.0847(2) 0.0760(17) Uani 1 1 d . . . H70 H 0.4723 -0.1386 0.0808 0.091 Uiso 1 1 calc R . . C71 C 0.4229(3) -0.0698(3) 0.1291(2) 0.0789(18) Uani 1 1 d . . . H71 H 0.4498 -0.0811 0.1559 0.095 Uiso 1 1 calc R . . C72 C 0.3695(3) -0.0203(3) 0.13313(17) 0.0611(14) Uani 1 1 d . . . H72 H 0.3586 0.0033 0.1631 0.073 Uiso 1 1 calc R . . C73 C 0.3360(3) 0.1287(3) -0.04192(17) 0.0466(12) Uani 1 1 d . . . C74 C 0.2646(3) 0.0896(3) -0.07179(17) 0.0561(14) Uani 1 1 d . . . H74A H 0.2347 0.1255 -0.0842 0.067 Uiso 1 1 calc R . . H74B H 0.2836 0.0582 -0.0986 0.067 Uiso 1 1 calc R . . C75 C 0.3759(3) 0.1979(3) -0.0475(2) 0.0645(15) Uani 1 1 d . . . H75 H 0.3587 0.2216 -0.0721 0.077 Uiso 1 1 calc R . . C76 C 0.4393(3) 0.2313(3) -0.0176(2) 0.0693(16) Uani 1 1 d . . . H76 H 0.4655 0.2785 -0.0208 0.083 Uiso 1 1 calc R . . C77 C 0.4643(3) 0.1951(3) 0.0169(2) 0.0675(16) Uani 1 1 d . . . H77 H 0.5083 0.2167 0.0381 0.081 Uiso 1 1 calc R . . C78 C 0.4237(3) 0.1264(3) 0.02024(17) 0.0562(14) Uani 1 1 d . . . H78 H 0.4421 0.1010 0.0437 0.067 Uiso 1 1 calc R . . C79 C -0.0176(3) 0.3209(2) 0.07918(17) 0.0586(14) Uani 1 1 d . . . H79A H -0.0544 0.2985 0.1011 0.070 Uiso 1 1 calc R . . H79B H -0.0512 0.3408 0.0567 0.070 Uiso 1 1 calc R . . C80 C 0.0414(3) 0.3832(2) 0.10662(16) 0.0549(14) Uani 1 1 d . . . C81 C 0.1738(3) 0.4362(3) 0.12323(17) 0.0621(15) Uani 1 1 d . . . H81 H 0.2300 0.4357 0.1182 0.074 Uiso 1 1 calc R . . C82 C 0.1516(4) 0.4910(3) 0.15516(18) 0.0764(18) Uani 1 1 d . . . H82 H 0.1913 0.5273 0.1719 0.092 Uiso 1 1 calc R . . C83 C 0.0688(5) 0.4917(3) 0.16233(18) 0.0778(18) Uani 1 1 d . . . H83 H 0.0514 0.5295 0.1836 0.093 Uiso 1 1 calc R . . C84 C 0.0126(4) 0.4369(3) 0.13819(17) 0.0675(16) Uani 1 1 d . . . H84 H -0.0439 0.4357 0.1429 0.081 Uiso 1 1 calc R . . C85 C 0.1632(3) 0.2661(2) -0.05343(17) 0.0536(13) Uani 1 1 d . . . H85A H 0.1390 0.2376 -0.0832 0.064 Uiso 1 1 calc R . . H85B H 0.2229 0.2684 -0.0545 0.064 Uiso 1 1 calc R . . C86 C 0.1417(3) 0.3426(2) -0.04966(17) 0.0485(13) Uani 1 1 d . . . C87 C 0.1088(3) 0.4415(3) -0.00054(19) 0.0635(15) Uani 1 1 d . . . H87 H 0.0978 0.4631 0.0300 0.076 Uiso 1 1 calc R . . C88 C 0.1082(3) 0.4828(3) -0.0370(2) 0.0776(18) Uani 1 1 d . . . H88 H 0.0957 0.5312 -0.0318 0.093 Uiso 1 1 calc R . . C89 C 0.1263(3) 0.4517(3) -0.08059(19) 0.0747(17) Uani 1 1 d . . . H89 H 0.1271 0.4785 -0.1061 0.090 Uiso 1 1 calc R . . C90 C 0.1435(3) 0.3801(3) -0.08710(18) 0.0621(15) Uani 1 1 d . . . H90 H 0.1564 0.3577 -0.1170 0.075 Uiso 1 1 calc R . . C91 C -0.0568(3) -0.0884(2) 0.11850(15) 0.0451(12) Uani 1 1 d . . . H91A H -0.0479 -0.1259 0.0921 0.054 Uiso 1 1 calc R . . H91B H -0.1156 -0.0942 0.1241 0.054 Uiso 1 1 calc R . . C92 C -0.0110(3) -0.1002(2) 0.16117(16) 0.0453(12) Uani 1 1 d . . . C93 C 0.0673(3) -0.0438(3) 0.22772(17) 0.0625(15) Uani 1 1 d . . . H93 H 0.0900 -0.0003 0.2473 0.075 Uiso 1 1 calc R . . C94 C 0.0831(4) -0.1106(3) 0.23969(18) 0.0744(17) Uani 1 1 d . . . H94 H 0.1178 -0.1127 0.2659 0.089 Uiso 1 1 calc R . . C95 C 0.0449(4) -0.1755(3) 0.21088(18) 0.0807(19) Uani 1 1 d . . . H95 H 0.0509 -0.2221 0.2186 0.097 Uiso 1 1 calc R . . C96 C -0.0006(3) -0.1689(3) 0.17182(18) 0.0631(15) Uani 1 1 d . . . H96 H -0.0252 -0.2113 0.1519 0.076 Uiso 1 1 calc R . . C97 C 0.1576(3) -0.1352(2) 0.09032(17) 0.0573(14) Uani 1 1 d . . . H97A H 0.1464 -0.1104 0.1216 0.069 Uiso 1 1 calc R . . H97B H 0.2161 -0.1218 0.0855 0.069 Uiso 1 1 calc R . . C98 C 0.1409(3) -0.2167(3) 0.09035(18) 0.0525(13) Uani 1 1 d . . . C99 C 0.0700(3) -0.3269(3) 0.0585(2) 0.0725(17) Uani 1 1 d . . . H99 H 0.0314 -0.3547 0.0359 0.087 Uiso 1 1 calc R . . C100 C 0.1074(5) -0.3636(3) 0.0895(3) 0.098(2) Uani 1 1 d . . . H100 H 0.0944 -0.4148 0.0883 0.117 Uiso 1 1 calc R . . C101 C 0.1636(5) -0.3235(4) 0.1219(2) 0.110(2) Uani 1 1 d . . . H101 H 0.1906 -0.3465 0.1437 0.132 Uiso 1 1 calc R . . C102 C 0.1807(4) -0.2484(3) 0.1223(2) 0.0863(19) Uani 1 1 d . . . H102 H 0.2195 -0.2196 0.1444 0.104 Uiso 1 1 calc R . . C103 C 0.1541(3) 0.1170(2) 0.18302(14) 0.0494(13) Uani 1 1 d . . . H10A H 0.1937 0.1571 0.1750 0.059 Uiso 1 1 calc R . . H10B H 0.1844 0.0775 0.1900 0.059 Uiso 1 1 calc R . . C104 C 0.1105(3) 0.1446(2) 0.22625(14) 0.0416(12) Uani 1 1 d . . . C105 C -0.0100(3) 0.1555(2) 0.26187(15) 0.0456(12) Uani 1 1 d . . . H105 H -0.0675 0.1443 0.2607 0.055 Uiso 1 1 calc R . . C106 C 0.0278(3) 0.1985(2) 0.30120(15) 0.0484(13) Uani 1 1 d . . . H106 H -0.0028 0.2175 0.3262 0.058 Uiso 1 1 calc R . . C107 C 0.1111(3) 0.2130(2) 0.30306(15) 0.0543(14) Uani 1 1 d . . . H107 H 0.1386 0.2416 0.3301 0.065 Uiso 1 1 calc R . . C108 C 0.1561(3) 0.1866(2) 0.26610(15) 0.0529(13) Uani 1 1 d . . . H108 H 0.2137 0.1959 0.2672 0.063 Uiso 1 1 calc R . . C109 C -0.1710(3) 0.0982(3) 0.18136(15) 0.0490(13) Uani 1 1 d . . . C110 C -0.1244(3) 0.1571(2) 0.15702(15) 0.0489(13) Uani 1 1 d . . . H11A H -0.1624 0.1752 0.1360 0.059 Uiso 1 1 calc R . . H11B H -0.1008 0.1986 0.1808 0.059 Uiso 1 1 calc R . . C111 C -0.2511(3) 0.1025(3) 0.19645(19) 0.0741(17) Uani 1 1 d . . . H111 H -0.2777 0.1426 0.1913 0.089 Uiso 1 1 calc R . . C112 C -0.2892(4) 0.0488(4) 0.2183(2) 0.101(2) Uani 1 1 d . . . H112 H -0.3434 0.0501 0.2275 0.121 Uiso 1 1 calc R . . C113 C -0.2478(4) -0.0082(3) 0.2270(2) 0.097(2) Uani 1 1 d . . . H113 H -0.2723 -0.0451 0.2436 0.116 Uiso 1 1 calc R . . C114 C -0.1691(3) -0.0099(3) 0.21074(17) 0.0643(15) Uani 1 1 d . . . H114 H -0.1409 -0.0491 0.2159 0.077 Uiso 1 1 calc R . . C115 C 0.2569(3) 0.2433(3) 0.09732(17) 0.0588(14) Uani 1 1 d . . . H11C H 0.2815 0.1985 0.0880 0.071 Uiso 1 1 calc R . . H11D H 0.2605 0.2537 0.1319 0.071 Uiso 1 1 calc R . . C116 C 0.3062(3) 0.3054(3) 0.07841(17) 0.0503(13) Uani 1 1 d . . . C117 C 0.3128(4) 0.3906(3) 0.0295(2) 0.0765(17) Uani 1 1 d . . . H117 H 0.2876 0.4136 0.0069 0.092 Uiso 1 1 calc R . . C118 C 0.3938(4) 0.4140(3) 0.0428(3) 0.094(2) Uani 1 1 d . . . H118 H 0.4240 0.4519 0.0293 0.113 Uiso 1 1 calc R . . C119 C 0.4299(4) 0.3811(4) 0.0763(2) 0.0843(19) Uani 1 1 d . . . H119 H 0.4849 0.3974 0.0866 0.101 Uiso 1 1 calc R . . C120 C 0.3874(4) 0.3263(3) 0.0942(2) 0.0719(17) Uani 1 1 d . . . H120 H 0.4116 0.3025 0.1167 0.086 Uiso 1 1 calc R . . H4O H 0.974(3) 0.442(2) 0.4900(11) 0.080 Uiso 1 1 d D . . H16O H 0.021(3) 0.063(2) -0.0011(7) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0444(4) 0.0430(4) 0.0416(3) 0.0069(3) 0.0078(3) 0.0093(3) Ni2 0.0410(4) 0.0462(4) 0.0482(4) 0.0050(3) 0.0052(3) 0.0117(3) Ni3 0.0620(5) 0.0378(4) 0.0595(4) 0.0067(3) 0.0181(3) 0.0061(3) Ni4 0.0532(4) 0.0396(4) 0.0493(4) 0.0055(3) 0.0052(3) 0.0073(3) Ni5 0.0455(4) 0.0429(3) 0.0380(3) 0.0038(3) 0.0043(3) 0.0108(3) Ni6 0.0394(4) 0.0471(4) 0.0468(4) 0.0040(3) 0.0035(3) 0.0120(3) Na1 0.0460(11) 0.0390(10) 0.0467(10) 0.0037(8) 0.0100(8) 0.0079(8) Na2 0.0469(11) 0.0431(10) 0.0521(11) 0.0097(9) 0.0121(9) 0.0143(8) Na3 0.0477(12) 0.0465(10) 0.0428(10) 0.0090(8) 0.0086(8) 0.0066(8) Na4 0.0441(11) 0.0428(10) 0.0595(11) 0.0085(9) 0.0109(9) 0.0091(8) Na5 0.0645(13) 0.0434(10) 0.0523(11) 0.0101(9) 0.0162(9) 0.0154(9) Na6 0.0488(12) 0.0432(10) 0.0408(10) 0.0036(8) 0.0032(8) 0.0096(8) Na7 0.0469(11) 0.0422(10) 0.0403(10) 0.0064(8) 0.0037(8) 0.0138(8) Na8 0.0459(11) 0.0440(10) 0.0434(10) 0.0043(8) 0.0001(8) 0.0103(8) Na9 0.0449(11) 0.0437(10) 0.0526(11) 0.0047(9) 0.0072(9) 0.0109(8) Na10 0.0488(12) 0.0455(10) 0.0455(10) 0.0070(8) 0.0016(8) 0.0129(9) O1 0.041(2) 0.0482(18) 0.0492(18) 0.0066(15) 0.0062(15) 0.0121(15) O2 0.0395(19) 0.0434(18) 0.0460(19) 0.0041(15) 0.0029(15) 0.0086(14) O3 0.050(2) 0.0410(19) 0.0453(18) 0.0118(15) 0.0097(15) 0.0093(15) O4 0.0420(19) 0.0405(18) 0.0449(18) 0.0074(15) 0.0080(15) 0.0068(14) O5 0.043(2) 0.0427(18) 0.0521(19) 0.0097(15) 0.0098(15) 0.0032(15) O6 0.0390(19) 0.0390(17) 0.0567(19) 0.0073(15) 0.0059(15) 0.0119(14) O7 0.054(2) 0.0522(19) 0.0419(19) 0.0071(16) 0.0086(16) 0.0161(16) O8 0.048(2) 0.0459(19) 0.0516(19) 0.0062(16) 0.0035(17) 0.0016(16) O9 0.053(2) 0.0422(18) 0.0545(19) 0.0098(15) 0.0148(16) 0.0127(16) O10 0.068(2) 0.0343(17) 0.064(2) 0.0169(16) 0.0278(18) 0.0040(16) O11 0.055(2) 0.0432(19) 0.073(2) 0.0240(18) 0.0139(18) 0.0144(16) O12 0.053(2) 0.0474(19) 0.056(2) 0.0115(16) 0.0008(17) 0.0111(16) O13 0.0421(19) 0.0510(19) 0.0410(17) 0.0065(15) 0.0071(15) 0.0152(15) O14 0.0354(19) 0.0551(19) 0.0336(17) 0.0042(15) 0.0022(14) 0.0089(15) O15 0.048(2) 0.0415(18) 0.0410(17) 0.0057(15) 0.0029(14) 0.0092(15) O16 0.0452(19) 0.0412(18) 0.0370(17) 0.0063(14) 0.0031(15) 0.0125(14) O17 0.042(2) 0.0514(19) 0.0482(18) 0.0119(16) -0.0010(15) 0.0139(16) O18 0.043(2) 0.0393(18) 0.059(2) 0.0059(15) 0.0037(15) 0.0105(15) O19 0.048(2) 0.0455(18) 0.0477(19) 0.0026(15) 0.0032(16) 0.0172(15) O20 0.058(2) 0.0399(18) 0.0461(18) 0.0084(15) 0.0144(16) 0.0106(15) O21 0.052(2) 0.0439(18) 0.0467(18) 0.0028(15) 0.0083(15) 0.0126(15) O22 0.052(2) 0.0434(18) 0.0520(19) 0.0135(16) 0.0029(16) 0.0190(16) N1 0.042(3) 0.049(3) 0.058(3) 0.010(2) 0.011(2) 0.007(2) N2 0.052(3) 0.053(3) 0.054(3) 0.015(2) 0.001(2) 0.008(2) N3 0.035(2) 0.051(3) 0.060(3) -0.004(2) 0.000(2) 0.0108(19) N4 0.079(3) 0.046(3) 0.077(3) 0.014(2) 0.033(3) 0.009(2) N5 0.098(4) 0.044(3) 0.065(3) 0.012(2) 0.016(3) 0.018(2) N6 0.073(3) 0.032(2) 0.057(3) 0.008(2) 0.020(2) 0.008(2) N7 0.065(3) 0.043(3) 0.085(3) -0.003(3) 0.020(3) 0.001(2) N8 0.061(3) 0.041(2) 0.039(2) 0.009(2) 0.0055(19) 0.0056(19) N9 0.046(3) 0.037(2) 0.046(2) 0.0061(18) 0.010(2) 0.0065(19) N10 0.045(3) 0.048(3) 0.049(2) 0.015(2) 0.013(2) 0.008(2) N11 0.041(3) 0.058(3) 0.048(2) 0.003(2) 0.003(2) 0.009(2) N12 0.041(3) 0.045(2) 0.051(2) 0.007(2) -0.0031(19) 0.0069(19) N13 0.039(3) 0.054(3) 0.053(3) 0.008(2) 0.004(2) 0.006(2) N14 0.075(3) 0.038(2) 0.043(2) 0.0072(19) 0.002(2) 0.006(2) N15 0.068(3) 0.033(2) 0.055(3) 0.016(2) 0.012(2) 0.010(2) N16 0.052(3) 0.046(2) 0.037(2) 0.008(2) -0.003(2) 0.014(2) N17 0.067(3) 0.042(3) 0.065(3) 0.009(2) 0.000(2) 0.017(2) N18 0.044(3) 0.037(2) 0.039(2) 0.0069(17) 0.0039(19) 0.0055(18) N19 0.046(3) 0.043(2) 0.048(2) 0.002(2) 0.005(2) 0.005(2) N20 0.054(3) 0.046(3) 0.065(3) 0.011(2) 0.006(2) 0.006(2) C1 0.048(3) 0.047(3) 0.072(3) 0.005(3) 0.007(3) 0.015(2) C2 0.041(3) 0.065(4) 0.048(3) 0.014(3) 0.013(2) 0.020(3) C3 0.045(4) 0.062(3) 0.069(4) 0.002(3) 0.008(3) 0.008(3) C4 0.052(4) 0.077(4) 0.078(4) 0.015(3) 0.015(3) 0.025(3) C5 0.071(4) 0.078(4) 0.091(4) 0.024(3) 0.033(3) 0.038(3) C6 0.060(4) 0.058(3) 0.072(4) 0.015(3) 0.015(3) 0.026(3) C7 0.073(4) 0.060(3) 0.056(3) 0.002(3) 0.005(3) 0.030(3) C8 0.056(3) 0.054(3) 0.049(3) 0.000(3) 0.001(3) 0.012(3) C9 0.070(4) 0.071(4) 0.068(4) 0.019(3) 0.008(3) 0.026(3) C10 0.100(5) 0.109(5) 0.084(5) 0.042(4) 0.013(4) 0.055(4) C11 0.126(6) 0.140(6) 0.064(4) 0.040(4) 0.011(4) 0.071(5) C12 0.089(5) 0.092(4) 0.051(4) 0.025(3) 0.010(3) 0.032(4) C13 0.040(3) 0.047(3) 0.061(3) 0.012(3) 0.011(3) 0.012(3) C14 0.059(4) 0.051(3) 0.046(3) 0.012(3) 0.005(3) 0.013(3) C15 0.041(3) 0.058(4) 0.085(4) 0.012(3) 0.013(3) 0.006(3) C16 0.055(4) 0.079(4) 0.078(4) -0.018(4) -0.008(3) 0.001(3) C17 0.064(4) 0.060(4) 0.096(5) -0.010(4) 0.005(4) -0.002(3) C18 0.050(4) 0.071(4) 0.071(4) 0.000(3) -0.006(3) 0.012(3) C19 0.072(4) 0.044(3) 0.069(3) 0.015(3) 0.026(3) 0.011(3) C20 0.068(4) 0.055(3) 0.082(4) 0.021(3) 0.030(3) 0.008(3) C21 0.114(5) 0.050(4) 0.103(5) 0.022(4) 0.030(4) 0.032(4) C22 0.135(6) 0.051(4) 0.120(5) 0.046(4) 0.052(5) 0.020(4) C23 0.136(6) 0.083(5) 0.136(6) 0.065(4) 0.077(5) 0.032(4) C24 0.122(6) 0.062(4) 0.110(5) 0.046(4) 0.063(4) 0.026(4) C25 0.069(4) 0.047(3) 0.072(4) 0.005(3) 0.019(3) 0.018(3) C26 0.084(4) 0.054(3) 0.055(3) 0.016(3) 0.021(3) 0.022(3) C27 0.121(6) 0.048(4) 0.083(4) 0.010(3) 0.016(4) 0.015(3) C28 0.228(9) 0.057(4) 0.091(5) 0.037(4) 0.039(5) 0.046(5) C29 0.248(10) 0.068(5) 0.071(5) 0.029(4) 0.052(5) 0.051(5) C30 0.190(8) 0.070(5) 0.074(4) 0.026(4) 0.042(5) 0.042(5) C31 0.068(4) 0.052(3) 0.061(3) 0.018(3) 0.021(3) 0.023(3) C32 0.084(4) 0.041(3) 0.051(3) 0.010(3) 0.028(3) 0.018(3) C33 0.091(4) 0.035(3) 0.058(3) 0.013(3) 0.019(3) 0.014(3) C34 0.113(6) 0.041(3) 0.064(4) 0.013(3) 0.013(4) 0.013(3) C35 0.114(6) 0.050(4) 0.055(4) 0.012(3) 0.025(4) 0.033(4) C36 0.086(4) 0.051(3) 0.052(3) 0.016(3) 0.021(3) 0.026(3) C37 0.046(4) 0.052(4) 0.084(4) -0.023(3) 0.012(3) 0.014(3) C38 0.057(4) 0.054(3) 0.078(4) 0.013(3) 0.010(3) 0.010(3) C39 0.064(5) 0.093(5) 0.102(5) -0.011(4) -0.011(4) 0.008(4) C40 0.080(6) 0.102(6) 0.137(7) -0.020(6) 0.016(6) -0.035(5) C41 0.050(5) 0.125(7) 0.140(7) -0.022(6) 0.006(5) -0.015(5) C42 0.080(5) 0.057(4) 0.114(5) 0.004(4) 0.027(4) -0.014(4) C43 0.054(3) 0.043(3) 0.045(3) 0.009(2) 0.014(2) 0.007(2) C44 0.052(3) 0.053(3) 0.047(3) 0.009(3) 0.003(2) 0.011(3) C45 0.121(5) 0.054(4) 0.050(4) 0.015(3) -0.005(3) 0.019(3) C46 0.220(9) 0.067(4) 0.056(4) 0.008(4) -0.012(4) 0.022(5) C47 0.181(8) 0.055(4) 0.075(5) 0.018(4) -0.007(4) 0.022(4) C48 0.098(5) 0.044(3) 0.058(4) 0.009(3) -0.003(3) 0.014(3) C49 0.056(3) 0.046(3) 0.047(3) 0.008(2) 0.000(2) 0.013(2) C50 0.062(4) 0.035(3) 0.042(3) 0.011(2) 0.007(3) 0.008(2) C51 0.055(4) 0.052(3) 0.054(3) 0.011(3) 0.008(3) 0.008(3) C52 0.072(4) 0.050(3) 0.046(3) 0.009(3) 0.016(3) 0.009(3) C53 0.079(4) 0.041(3) 0.041(3) 0.008(2) 0.004(3) 0.015(3) C54 0.060(4) 0.040(3) 0.046(3) 0.010(2) 0.002(3) 0.011(2) C55 0.047(3) 0.059(3) 0.056(3) 0.007(3) 0.012(3) 0.011(3) C56 0.042(3) 0.060(3) 0.035(3) -0.003(2) 0.000(2) 0.010(3) C57 0.052(4) 0.068(4) 0.072(4) 0.009(3) 0.001(3) 0.019(3) C58 0.048(4) 0.093(5) 0.102(5) 0.023(4) 0.010(3) 0.011(3) C59 0.034(4) 0.098(5) 0.117(5) 0.017(4) 0.001(3) 0.005(4) C60 0.044(4) 0.072(4) 0.080(4) 0.004(3) -0.001(3) 0.019(3) C61 0.061(4) 0.045(3) 0.060(3) 0.001(3) 0.002(3) 0.014(3) C62 0.047(3) 0.054(3) 0.057(3) 0.000(3) 0.000(3) 0.006(3) C63 0.047(3) 0.073(4) 0.059(3) 0.007(3) 0.004(3) 0.004(3) C64 0.048(4) 0.098(5) 0.059(3) -0.011(3) 0.010(3) 0.026(3) C65 0.079(5) 0.092(5) 0.057(4) -0.013(3) 0.009(3) 0.037(4) C66 0.066(4) 0.061(3) 0.062(3) -0.016(3) -0.001(3) 0.024(3) C67 0.051(3) 0.062(3) 0.056(3) 0.002(3) -0.006(3) 0.014(3) C68 0.040(3) 0.045(3) 0.057(3) 0.001(3) 0.007(3) 0.004(2) C69 0.038(3) 0.066(4) 0.071(4) 0.005(3) 0.008(3) 0.019(3) C70 0.075(4) 0.085(4) 0.077(4) 0.012(4) -0.011(3) 0.047(3) C71 0.089(5) 0.090(4) 0.072(4) 0.023(3) -0.004(3) 0.053(4) C72 0.065(4) 0.083(4) 0.039(3) 0.013(3) -0.005(3) 0.019(3) C73 0.038(3) 0.049(3) 0.058(3) 0.011(3) 0.007(3) 0.016(3) C74 0.050(3) 0.062(3) 0.058(3) 0.007(3) 0.000(3) 0.017(3) C75 0.043(4) 0.062(4) 0.095(4) 0.014(3) 0.011(3) 0.024(3) C76 0.055(4) 0.055(4) 0.098(5) 0.008(4) -0.005(3) 0.014(3) C77 0.049(4) 0.053(4) 0.092(5) -0.010(3) 0.003(3) 0.001(3) C78 0.047(4) 0.065(4) 0.057(3) -0.002(3) -0.001(3) 0.018(3) C79 0.064(4) 0.051(3) 0.064(3) 0.007(3) 0.012(3) 0.019(3) C80 0.068(4) 0.048(3) 0.050(3) 0.000(3) 0.002(3) 0.020(3) C81 0.087(4) 0.041(3) 0.056(3) 0.008(3) -0.010(3) 0.003(3) C82 0.128(6) 0.045(3) 0.053(4) -0.001(3) -0.033(4) 0.013(4) C83 0.136(6) 0.052(4) 0.050(3) 0.010(3) -0.006(4) 0.031(4) C84 0.101(5) 0.046(3) 0.059(3) 0.003(3) 0.000(3) 0.029(3) C85 0.059(4) 0.041(3) 0.063(3) 0.008(3) 0.007(3) 0.011(2) C86 0.057(3) 0.044(3) 0.049(3) 0.017(3) 0.010(3) 0.009(2) C87 0.074(4) 0.044(3) 0.074(4) 0.008(3) 0.013(3) 0.014(3) C88 0.092(5) 0.055(4) 0.095(5) 0.024(4) 0.024(4) 0.026(3) C89 0.096(5) 0.071(4) 0.070(4) 0.039(3) 0.020(3) 0.027(3) C90 0.078(4) 0.060(4) 0.054(3) 0.014(3) 0.020(3) 0.022(3) C91 0.046(3) 0.048(3) 0.042(3) 0.006(2) -0.001(2) 0.010(2) C92 0.047(3) 0.042(3) 0.047(3) 0.007(3) 0.004(2) 0.008(2) C93 0.080(4) 0.063(4) 0.045(3) 0.002(3) 0.000(3) 0.019(3) C94 0.117(5) 0.071(4) 0.048(3) 0.020(3) -0.002(3) 0.047(4) C95 0.148(6) 0.051(4) 0.051(3) 0.016(3) -0.010(4) 0.036(4) C96 0.078(4) 0.051(3) 0.062(4) 0.006(3) 0.005(3) 0.014(3) C97 0.065(4) 0.044(3) 0.061(3) 0.008(3) 0.005(3) 0.001(3) C98 0.058(4) 0.051(3) 0.054(3) 0.017(3) 0.004(3) 0.016(3) C99 0.076(4) 0.047(4) 0.094(4) 0.004(3) -0.008(3) 0.018(3) C100 0.124(6) 0.052(4) 0.125(6) 0.030(4) 0.003(5) 0.021(4) C101 0.168(8) 0.071(5) 0.102(5) 0.041(4) -0.032(5) 0.035(5) C102 0.111(5) 0.070(4) 0.080(4) 0.021(4) -0.031(4) 0.020(4) C103 0.048(3) 0.057(3) 0.044(3) 0.004(2) 0.004(2) 0.017(2) C104 0.058(4) 0.040(3) 0.029(3) 0.007(2) 0.000(2) 0.015(2) C105 0.058(3) 0.033(3) 0.046(3) 0.005(2) 0.006(3) 0.008(2) C106 0.064(4) 0.046(3) 0.038(3) 0.008(2) 0.008(3) 0.016(3) C107 0.089(5) 0.042(3) 0.032(3) 0.003(2) 0.001(3) 0.011(3) C108 0.064(4) 0.052(3) 0.044(3) 0.010(3) -0.003(3) 0.012(3) C109 0.048(3) 0.055(3) 0.045(3) 0.004(3) 0.004(2) 0.014(3) C110 0.051(3) 0.052(3) 0.044(3) 0.004(2) 0.001(2) 0.010(3) C111 0.057(4) 0.085(4) 0.086(4) 0.013(4) 0.018(3) 0.025(3) C112 0.066(5) 0.100(5) 0.147(6) 0.034(5) 0.055(4) 0.020(4) C113 0.064(5) 0.090(5) 0.140(6) 0.028(4) 0.051(4) 0.003(4) C114 0.064(4) 0.063(4) 0.068(4) 0.018(3) 0.009(3) 0.004(3) C115 0.053(4) 0.067(4) 0.055(3) 0.000(3) -0.007(3) 0.015(3) C116 0.055(4) 0.042(3) 0.051(3) -0.001(3) 0.009(3) 0.006(3) C117 0.073(5) 0.063(4) 0.097(5) 0.031(3) 0.008(4) 0.003(3) C118 0.078(6) 0.068(4) 0.129(6) 0.016(4) 0.012(5) -0.017(4) C119 0.058(4) 0.074(5) 0.115(5) 0.013(4) -0.009(4) -0.007(4) C120 0.054(4) 0.059(4) 0.097(4) 0.001(3) -0.002(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.021(3) . ? Ni1 O3 2.024(2) . ? Ni1 O1 2.058(3) . ? Ni1 N9 2.108(3) . ? Ni1 N10 2.118(4) . ? Ni1 N8 2.155(4) . ? Ni1 Na2 3.2157(16) . ? Ni1 Na3 3.2465(16) . ? Ni1 Na1 3.2638(17) . ? Ni2 O5 2.019(3) . ? Ni2 O7 2.025(3) . ? Ni2 O6 2.062(3) . ? Ni2 N2 2.119(4) . ? Ni2 N1 2.147(3) . ? Ni2 N3 2.156(4) . ? Ni2 Na3 3.2772(18) 2_766 ? Ni2 Na4 3.2900(17) . ? Ni3 O8 2.027(3) . ? Ni3 O10 2.042(3) . ? Ni3 O9 2.058(3) . ? Ni3 N7 2.099(5) . ? Ni3 N6 2.115(3) . ? Ni3 N4 2.136(4) . ? Ni3 Na5 3.2029(18) . ? Ni3 Na1 3.2952(17) . ? Ni3 Na4 3.3054(17) . ? Ni4 O12 2.018(3) . ? Ni4 O20 2.038(3) . ? Ni4 O21 2.049(3) . ? Ni4 N14 2.110(3) . ? Ni4 N20 2.130(4) . ? Ni4 N15 2.137(4) . ? Ni4 Na10 3.2122(18) . ? Ni4 Na6 3.2798(17) . ? Ni4 Na9 3.2956(16) . ? Ni5 O15 2.019(3) . ? Ni5 O14 2.021(3) . ? Ni5 O13 2.055(3) . ? Ni5 N18 2.104(3) . ? Ni5 N19 2.129(4) . ? Ni5 N16 2.156(4) . ? Ni5 Na7 3.1864(15) . ? Ni5 Na8 3.2223(17) . ? Ni5 Na6 3.2253(18) . ? Ni6 O17 2.005(3) . ? Ni6 O19 2.026(2) . ? Ni6 O18 2.059(3) . ? Ni6 N12 2.107(4) . ? Ni6 N13 2.123(4) . ? Ni6 N11 2.129(3) . ? Ni6 Na9 3.2661(16) . ? Ni6 Na8 3.2824(18) 2 ? Na1 O1 2.285(3) . ? Na1 O8 2.289(3) . ? Na1 O4 2.339(3) . ? Na1 O9 2.397(3) . ? Na1 O2 2.421(3) . ? Na2 O2 2.282(3) . ? Na2 O11 2.320(3) 2_766 ? Na2 O3 2.332(3) . ? Na2 O4 2.377(3) . ? Na2 O7 2.413(3) . ? Na2 C7 3.053(6) . ? Na3 O3 2.262(3) . ? Na3 O5 2.304(3) 2_766 ? Na3 O6 2.398(3) 2_766 ? Na3 O1 2.451(3) . ? Na3 O4 2.453(3) . ? Na3 Ni2 3.2772(18) 2_766 ? Na4 O10 2.332(3) . ? Na4 O7 2.375(3) . ? Na4 O4 2.379(3) . ? Na4 O5 2.394(3) . ? Na4 O8 2.462(3) . ? Na4 C14 3.073(5) . ? Na4 H4O 2.50(4) . ? Na5 O9 2.225(3) . ? Na5 O10 2.370(4) . ? Na5 O4 2.408(3) . ? Na5 O11 2.444(4) . ? Na5 N5 2.548(5) . ? Na5 H4O 2.54(5) . ? Na6 O13 2.275(3) . ? Na6 O12 2.285(3) . ? Na6 O16 2.340(3) . ? Na6 O21 2.392(3) . ? Na6 O14 2.427(3) . ? Na7 O14 2.286(3) . ? Na7 O15 2.316(3) . ? Na7 O22 2.365(3) . ? Na7 O16 2.381(3) . ? Na7 O19 2.388(3) . ? Na7 C67 2.960(5) . ? Na8 O15 2.258(3) . ? Na8 O17 2.316(3) 2 ? Na8 O13 2.404(3) . ? Na8 O18 2.406(3) 2 ? Na8 O16 2.497(3) . ? Na8 Ni6 3.2823(18) 2 ? Na9 O20 2.306(3) . ? Na9 O19 2.322(3) . ? Na9 O16 2.400(3) . ? Na9 O17 2.409(3) . ? Na9 O12 2.479(3) . ? Na9 C74 3.095(5) . ? Na9 H16O 2.58(4) . ? Na10 O21 2.251(3) . ? Na10 O20 2.398(3) . ? Na10 O16 2.402(3) . ? Na10 O22 2.410(3) 2 ? Na10 N17 2.527(4) 2 ? Na10 H16O 2.44(5) . ? O1 C55 1.381(5) . ? O2 C49 1.384(5) . ? O3 C43 1.369(5) . ? O4 H4O 0.90(4) . ? O5 C14 1.397(5) . ? O5 Na3 2.304(3) 2_766 ? O6 C1 1.396(4) . ? O6 Na3 2.398(3) 2_766 ? O7 C7 1.382(5) . ? O8 C38 1.370(6) . ? O9 C31 1.387(5) . ? O10 C19 1.379(5) . ? O11 C25 1.395(6) . ? O11 Na2 2.320(3) 2_766 ? O12 C115 1.386(5) . ? O13 C110 1.374(4) . ? O14 C103 1.383(5) . ? O15 C91 1.389(5) . ? O16 H16O 0.883(10) . ? O17 C74 1.404(5) . ? O17 Na8 2.316(3) 2 ? O18 C61 1.391(4) . ? O18 Na8 2.406(3) 2 ? O19 C67 1.386(5) . ? O20 C85 1.390(5) . ? O21 C79 1.367(4) . ? O22 C97 1.403(5) . ? O22 Na10 2.410(3) 2 ? N1 C3 1.319(5) . ? N1 C2 1.337(5) . ? N2 C8 1.363(5) . ? N2 C9 1.367(6) . ? N3 C18 1.339(6) . ? N3 C13 1.357(6) . ? N4 C20 1.351(5) . ? N4 C21 1.361(6) . ? N5 C26 1.334(6) . ? N5 C27 1.349(6) . ? N6 C32 1.336(6) . ? N6 C33 1.331(6) . ? N7 C42 1.352(6) . ? N7 C37 1.370(7) . ? N8 C44 1.332(5) . ? N8 C45 1.332(6) . ? N9 C50 1.338(5) . ? N9 C51 1.360(5) . ? N10 C56 1.318(6) . ? N10 C57 1.344(6) . ? N11 C62 1.341(5) . ? N11 C63 1.359(5) . ? N12 C68 1.354(5) . ? N12 C69 1.369(5) . ? N13 C73 1.333(6) . ? N13 C78 1.348(6) . ? N14 C80 1.330(6) . ? N14 C81 1.352(6) . ? N15 C87 1.335(5) . ? N15 C86 1.339(5) . ? N16 C93 1.350(6) . ? N16 C92 1.353(5) . ? N17 C99 1.342(6) . ? N17 C98 1.350(6) . ? N17 Na10 2.527(4) 2 ? N18 C104 1.328(5) . ? N18 C105 1.351(5) . ? N19 C109 1.321(5) . ? N19 C114 1.348(6) . ? N20 C116 1.319(6) . ? N20 C117 1.353(6) . ? C1 C2 1.527(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C6 1.385(6) . ? C3 C4 1.370(6) . ? C3 H3 0.9500 . ? C4 C5 1.402(7) . ? C4 H4 0.9500 . ? C5 C6 1.381(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.490(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C12 1.382(7) . ? C9 C10 1.358(7) . ? C9 H9 0.9500 . ? C10 C11 1.420(7) . ? C10 H10 0.9500 . ? C11 C12 1.361(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C15 1.372(6) . ? C13 C14 1.492(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C17 1.389(7) . ? C15 H15 0.9500 . ? C16 C17 1.376(7) . ? C16 C18 1.416(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.525(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.411(7) . ? C21 C22 1.377(7) . ? C21 H21 0.9500 . ? C22 C23 1.375(7) . ? C22 H22 0.9500 . ? C23 C24 1.377(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.502(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C30 1.388(7) . ? C27 C28 1.376(8) . ? C27 H27 0.9500 . ? C28 C29 1.358(8) . ? C28 H28 0.9500 . ? C29 C30 1.373(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.519(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C36 1.393(6) . ? C33 C34 1.374(6) . ? C33 H33 0.9500 . ? C34 C35 1.373(7) . ? C34 H34 0.9500 . ? C35 C36 1.382(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C39 1.382(7) . ? C37 C38 1.523(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C41 1.390(8) . ? C39 H39 0.9500 . ? C40 C42 1.319(9) . ? C40 C41 1.423(10) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.520(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C48 1.399(6) . ? C45 C46 1.392(7) . ? C45 H45 0.9500 . ? C46 C47 1.371(7) . ? C46 H46 0.9500 . ? C47 C48 1.376(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.522(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C54 1.384(6) . ? C51 C52 1.387(6) . ? C51 H51 0.9500 . ? C52 C53 1.402(6) . ? C52 H52 0.9500 . ? C53 C54 1.380(6) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.525(6) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C60 1.395(6) . ? C57 C58 1.377(7) . ? C57 H57 0.9500 . ? C58 C59 1.368(8) . ? C58 H58 0.9500 . ? C59 C60 1.356(7) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.498(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C66 1.397(6) . ? C63 C64 1.369(6) . ? C63 H63 0.9500 . ? C64 C65 1.363(7) . ? C64 H64 0.9500 . ? C65 C66 1.397(7) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.506(6) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C72 1.405(6) . ? C69 C70 1.338(7) . ? C69 H69 0.9500 . ? C70 C71 1.384(7) . ? C70 H70 0.9500 . ? C71 C72 1.363(6) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C75 1.407(6) . ? C73 C74 1.491(6) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.367(7) . ? C75 H75 0.9500 . ? C76 C77 1.371(7) . ? C76 H76 0.9500 . ? C77 C78 1.389(6) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.530(6) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C84 1.403(6) . ? C81 C82 1.375(6) . ? C81 H81 0.9500 . ? C82 C83 1.400(7) . ? C82 H82 0.9500 . ? C83 C84 1.385(7) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C86 1.514(6) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C90 1.372(6) . ? C87 C88 1.396(7) . ? C87 H87 0.9500 . ? C88 C89 1.371(7) . ? C88 H88 0.9500 . ? C89 C90 1.396(6) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.493(6) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 C96 1.397(6) . ? C93 C94 1.401(6) . ? C93 H93 0.9500 . ? C94 C95 1.432(7) . ? C94 H94 0.9500 . ? C95 C96 1.373(7) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 C98 1.515(6) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C102 1.369(7) . ? C99 C100 1.387(8) . ? C99 H99 0.9500 . ? C100 C101 1.371(8) . ? C100 H100 0.9500 . ? C101 C102 1.397(8) . ? C101 H101 0.9500 . ? C102 H102 0.9500 . ? C103 C104 1.524(5) . ? C103 H10A 0.9900 . ? C103 H10B 0.9900 . ? C104 C108 1.435(6) . ? C105 C106 1.379(6) . ? C105 H105 0.9500 . ? C106 C107 1.375(6) . ? C106 H106 0.9500 . ? C107 C108 1.393(6) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C111 1.423(6) . ? C109 C110 1.530(6) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.356(7) . ? C111 H111 0.9500 . ? C112 C113 1.396(8) . ? C112 H112 0.9500 . ? C113 C114 1.407(7) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C115 C116 1.508(6) . ? C115 H11C 0.9900 . ? C115 H11D 0.9900 . ? C116 C120 1.400(7) . ? C117 C118 1.388(8) . ? C117 H117 0.9500 . ? C118 C119 1.385(8) . ? C118 H118 0.9500 . ? C119 C120 1.340(7) . ? C119 H119 0.9500 . ? C120 H120 0.9500 . ? 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 O2 Ni1 O3 91.08(11) . . ? O2 Ni1 O1 90.90(12) . . ? O3 Ni1 O1 92.42(11) . . ? O2 Ni1 N9 80.29(13) . . ? O3 Ni1 N9 165.83(14) . . ? O1 Ni1 N9 98.88(12) . . ? O2 Ni1 N10 167.32(13) . . ? O3 Ni1 N10 97.28(12) . . ? O1 Ni1 N10 79.28(14) . . ? N9 Ni1 N10 93.22(14) . . ? O2 Ni1 N8 98.62(13) . . ? O3 Ni1 N8 78.86(12) . . ? O1 Ni1 N8 167.15(13) . . ? N9 Ni1 N8 91.26(13) . . ? N10 Ni1 N8 92.36(15) . . ? O2 Ni1 Na2 44.83(7) . . ? O3 Ni1 Na2 46.27(9) . . ? O1 Ni1 Na2 91.35(8) . . ? N9 Ni1 Na2 124.40(11) . . ? N10 Ni1 Na2 142.31(9) . . ? N8 Ni1 Na2 89.38(10) . . ? O2 Ni1 Na3 94.60(8) . . ? O3 Ni1 Na3 43.59(9) . . ? O1 Ni1 Na3 49.00(7) . . ? N9 Ni1 Na3 147.65(10) . . ? N10 Ni1 Na3 85.05(10) . . ? N8 Ni1 Na3 121.07(10) . . ? Na2 Ni1 Na3 62.31(4) . . ? O2 Ni1 Na1 47.72(9) . . ? O3 Ni1 Na1 85.61(9) . . ? O1 Ni1 Na1 43.99(8) . . ? N9 Ni1 Na1 96.58(10) . . ? N10 Ni1 Na1 123.24(12) . . ? N8 Ni1 Na1 142.79(10) . . ? Na2 Ni1 Na1 56.44(4) . . ? Na3 Ni1 Na1 59.03(4) . . ? O5 Ni2 O7 91.43(11) . . ? O5 Ni2 O6 90.80(12) . . ? O7 Ni2 O6 94.84(11) . . ? O5 Ni2 N2 168.88(13) . . ? O7 Ni2 N2 80.94(14) . . ? O6 Ni2 N2 97.86(13) . . ? O5 Ni2 N1 98.74(13) . . ? O7 Ni2 N1 167.68(14) . . ? O6 Ni2 N1 78.16(13) . . ? N2 Ni2 N1 89.90(15) . . ? O5 Ni2 N3 79.90(15) . . ? O7 Ni2 N3 93.15(12) . . ? O6 Ni2 N3 167.89(14) . . ? N2 Ni2 N3 92.38(16) . . ? N1 Ni2 N3 95.47(14) . . ? O5 Ni2 Na3 44.08(8) . 2_766 ? O7 Ni2 Na3 97.29(9) . 2_766 ? O6 Ni2 Na3 46.86(9) . 2_766 ? N2 Ni2 Na3 144.61(11) . 2_766 ? N1 Ni2 Na3 85.39(11) . 2_766 ? N3 Ni2 Na3 122.97(13) . 2_766 ? O5 Ni2 Na4 46.36(8) . . ? O7 Ni2 Na4 45.84(9) . . ? O6 Ni2 Na4 100.78(8) . . ? N2 Ni2 Na4 124.46(11) . . ? N1 Ni2 Na4 145.04(11) . . ? N3 Ni2 Na4 78.45(11) . . ? Na3 Ni2 Na4 70.28(4) 2_766 . ? O8 Ni3 O10 92.22(11) . . ? O8 Ni3 O9 89.59(12) . . ? O10 Ni3 O9 91.27(12) . . ? O8 Ni3 N7 81.17(17) . . ? O10 Ni3 N7 96.01(14) . . ? O9 Ni3 N7 168.43(16) . . ? O8 Ni3 N6 98.65(13) . . ? O10 Ni3 N6 165.78(16) . . ? O9 Ni3 N6 79.74(15) . . ? N7 Ni3 N6 94.70(16) . . ? O8 Ni3 N4 167.61(14) . . ? O10 Ni3 N4 79.86(13) . . ? O9 Ni3 N4 100.02(15) . . ? N7 Ni3 N4 90.13(19) . . ? N6 Ni3 N4 90.79(14) . . ? O8 Ni3 Na5 92.25(9) . . ? O10 Ni3 Na5 47.65(9) . . ? O9 Ni3 Na5 43.63(7) . . ? N7 Ni3 Na5 143.03(10) . . ? N6 Ni3 Na5 122.26(14) . . ? N4 Ni3 Na5 89.43(12) . . ? O8 Ni3 Na1 43.27(9) . . ? O10 Ni3 Na1 89.85(8) . . ? O9 Ni3 Na1 46.45(9) . . ? N7 Ni3 Na1 124.36(15) . . ? N6 Ni3 Na1 91.81(11) . . ? N4 Ni3 Na1 145.02(13) . . ? Na5 Ni3 Na1 60.12(4) . . ? O8 Ni3 Na4 47.96(8) . . ? O10 Ni3 Na4 44.33(9) . . ? O9 Ni3 Na4 88.73(8) . . ? N7 Ni3 Na4 90.20(12) . . ? N6 Ni3 Na4 145.04(11) . . ? N4 Ni3 Na4 123.85(10) . . ? Na5 Ni3 Na4 60.16(5) . . ? Na1 Ni3 Na4 57.75(4) . . ? O12 Ni4 O20 92.36(12) . . ? O12 Ni4 O21 89.78(12) . . ? O20 Ni4 O21 92.33(11) . . ? O12 Ni4 N14 97.64(13) . . ? O20 Ni4 N14 166.69(15) . . ? O21 Ni4 N14 78.99(14) . . ? O12 Ni4 N20 80.44(16) . . ? O20 Ni4 N20 97.11(13) . . ? O21 Ni4 N20 166.64(15) . . ? N14 Ni4 N20 93.21(15) . . ? O12 Ni4 N15 168.03(13) . . ? O20 Ni4 N15 80.14(13) . . ? O21 Ni4 N15 99.77(13) . . ? N14 Ni4 N15 91.30(14) . . ? N20 Ni4 N15 91.16(17) . . ? O12 Ni4 Na10 92.56(9) . . ? O20 Ni4 Na10 48.23(9) . . ? O21 Ni4 Na10 44.12(8) . . ? N14 Ni4 Na10 122.14(12) . . ? N20 Ni4 Na10 144.62(10) . . ? N15 Ni4 Na10 89.38(11) . . ? O12 Ni4 Na6 43.47(9) . . ? O20 Ni4 Na6 89.11(9) . . ? O21 Ni4 Na6 46.62(9) . . ? N14 Ni4 Na6 92.11(11) . . ? N20 Ni4 Na6 123.85(13) . . ? N15 Ni4 Na6 144.53(11) . . ? Na10 Ni4 Na6 59.36(4) . . ? O12 Ni4 Na9 48.66(8) . . ? O20 Ni4 Na9 43.79(9) . . ? O21 Ni4 Na9 89.22(8) . . ? N14 Ni4 Na9 144.66(11) . . ? N20 Ni4 Na9 91.08(11) . . ? N15 Ni4 Na9 123.68(10) . . ? Na10 Ni4 Na9 60.01(4) . . ? Na6 Ni4 Na9 57.18(4) . . ? O15 Ni5 O14 91.98(11) . . ? O15 Ni5 O13 92.00(11) . . ? O14 Ni5 O13 92.77(11) . . ? O15 Ni5 N18 169.08(13) . . ? O14 Ni5 N18 80.26(12) . . ? O13 Ni5 N18 96.02(12) . . ? O15 Ni5 N19 96.87(12) . . ? O14 Ni5 N19 168.22(13) . . ? O13 Ni5 N19 79.21(14) . . ? N18 Ni5 N19 91.92(13) . . ? O15 Ni5 N16 78.13(13) . . ? O14 Ni5 N16 94.37(13) . . ? O13 Ni5 N16 167.99(13) . . ? N18 Ni5 N16 94.69(14) . . ? N19 Ni5 N16 95.04(15) . . ? O15 Ni5 Na7 46.44(8) . . ? O14 Ni5 Na7 45.60(8) . . ? O13 Ni5 Na7 91.59(8) . . ? N18 Ni5 Na7 125.66(10) . . ? N19 Ni5 Na7 142.21(10) . . ? N16 Ni5 Na7 86.55(9) . . ? O15 Ni5 Na8 44.00(9) . . ? O14 Ni5 Na8 96.77(9) . . ? O13 Ni5 Na8 48.19(8) . . ? N18 Ni5 Na8 144.11(10) . . ? N19 Ni5 Na8 84.38(11) . . ? N16 Ni5 Na8 121.17(10) . . ? Na7 Ni5 Na8 63.22(4) . . ? O15 Ni5 Na6 87.38(9) . . ? O14 Ni5 Na6 48.75(9) . . ? O13 Ni5 Na6 44.52(8) . . ? N18 Ni5 Na6 93.14(10) . . ? N19 Ni5 Na6 123.73(12) . . ? N16 Ni5 Na6 140.11(10) . . ? Na7 Ni5 Na6 57.70(4) . . ? Na8 Ni5 Na6 60.87(4) . . ? O17 Ni6 O19 90.86(12) . . ? O17 Ni6 O18 91.18(12) . . ? O19 Ni6 O18 94.36(11) . . ? O17 Ni6 N12 170.28(12) . . ? O19 Ni6 N12 80.95(13) . . ? O18 Ni6 N12 94.63(13) . . ? O17 Ni6 N13 79.64(15) . . ? O19 Ni6 N13 92.20(12) . . ? O18 Ni6 N13 168.79(15) . . ? N12 Ni6 N13 95.36(16) . . ? O17 Ni6 N11 96.61(13) . . ? O19 Ni6 N11 169.49(14) . . ? O18 Ni6 N11 78.16(13) . . ? N12 Ni6 N11 92.21(14) . . ? N13 Ni6 N11 96.39(14) . . ? O17 Ni6 Na9 47.29(8) . . ? O19 Ni6 Na9 44.87(9) . . ? O18 Ni6 Na9 102.70(8) . . ? N12 Ni6 Na9 123.53(10) . . ? N13 Ni6 Na9 75.81(10) . . ? N11 Ni6 Na9 143.69(11) . . ? O17 Ni6 Na8 44.25(9) . 2 ? O19 Ni6 Na8 92.45(9) . 2 ? O18 Ni6 Na8 46.96(9) . 2 ? N12 Ni6 Na8 140.68(10) . 2 ? N13 Ni6 Na8 123.73(13) . 2 ? N11 Ni6 Na8 87.81(10) . 2 ? Na9 Ni6 Na8 69.07(4) . 2 ? O1 Na1 O8 162.84(11) . . ? O1 Na1 O4 98.94(11) . . ? O8 Na1 O4 97.63(11) . . ? O1 Na1 O9 108.44(12) . . ? O8 Na1 O9 75.75(12) . . ? O4 Na1 O9 90.66(10) . . ? O1 Na1 O2 76.24(11) . . ? O8 Na1 O2 97.34(12) . . ? O4 Na1 O2 96.99(10) . . ? O9 Na1 O2 170.36(11) . . ? O1 Na1 Na2 91.14(9) . . ? O8 Na1 Na2 96.09(9) . . ? O4 Na1 Na2 50.02(8) . . ? O9 Na1 Na2 139.00(8) . . ? O2 Na1 Na2 47.40(7) . . ? O1 Na1 Na4 145.05(9) . . ? O8 Na1 Na4 50.21(8) . . ? O4 Na1 Na4 48.02(8) . . ? O9 Na1 Na4 86.07(8) . . ? O2 Na1 Na4 94.68(8) . . ? Na2 Na1 Na4 60.16(5) . . ? O1 Na1 Na3 49.61(7) . . ? O8 Na1 Na3 147.14(9) . . ? O4 Na1 Na3 49.51(8) . . ? O9 Na1 Na3 101.19(9) . . ? O2 Na1 Na3 88.26(8) . . ? Na2 Na1 Na3 64.39(5) . . ? Na4 Na1 Na3 97.18(5) . . ? O1 Na1 Na5 108.29(9) . . ? O8 Na1 Na5 86.30(9) . . ? O4 Na1 Na5 47.58(8) . . ? O9 Na1 Na5 43.12(7) . . ? O2 Na1 Na5 144.41(8) . . ? Na2 Na1 Na5 97.04(5) . . ? Na4 Na1 Na5 60.84(5) . . ? Na3 Na1 Na5 71.31(5) . . ? O1 Na1 Ni1 38.72(8) . . ? O8 Na1 Ni1 135.05(10) . . ? O4 Na1 Ni1 94.79(8) . . ? O9 Na1 Ni1 147.17(10) . . ? O2 Na1 Ni1 38.15(7) . . ? Na2 Na1 Ni1 60.99(4) . . ? Na4 Na1 Ni1 121.00(6) . . ? Na3 Na1 Ni1 60.22(4) . . ? Na5 Na1 Ni1 131.47(6) . . ? O1 Na1 Ni3 145.11(10) . . ? O8 Na1 Ni3 37.37(8) . . ? O4 Na1 Ni3 93.25(8) . . ? O9 Na1 Ni3 38.47(8) . . ? O2 Na1 Ni3 134.62(9) . . ? Na2 Na1 Ni3 121.09(6) . . ? Na4 Na1 Ni3 61.28(4) . . ? Na3 Na1 Ni3 129.80(6) . . ? Na5 Na1 Ni3 58.54(4) . . ? Ni1 Na1 Ni3 169.98(6) . . ? O2 Na2 O11 133.76(13) . 2_766 ? O2 Na2 O3 77.47(10) . . ? O11 Na2 O3 88.70(12) 2_766 . ? O2 Na2 O4 99.86(11) . . ? O11 Na2 O4 124.26(12) 2_766 . ? O3 Na2 O4 89.62(11) . . ? O2 Na2 O7 102.69(11) . . ? O11 Na2 O7 86.85(11) 2_766 . ? O3 Na2 O7 173.88(13) . . ? O4 Na2 O7 96.36(11) . . ? O2 Na2 C7 84.13(12) . . ? O11 Na2 C7 86.53(13) 2_766 . ? O3 Na2 C7 149.32(14) . . ? O4 Na2 C7 117.85(13) . . ? O7 Na2 C7 26.08(11) . . ? O2 Na2 Na1 51.35(8) . . ? O11 Na2 Na1 171.09(12) 2_766 . ? O3 Na2 Na1 85.63(9) . . ? O4 Na2 Na1 48.95(7) . . ? O7 Na2 Na1 99.28(9) . . ? C7 Na2 Na1 101.82(10) . . ? O2 Na2 Na4 99.03(9) . . ? O11 Na2 Na4 119.45(9) 2_766 . ? O3 Na2 Na4 137.54(10) . . ? O4 Na2 Na4 48.78(8) . . ? O7 Na2 Na4 48.58(8) . . ? C7 Na2 Na4 69.22(11) . . ? Na1 Na2 Na4 61.88(5) . . ? O2 Na2 Ni1 38.64(7) . . ? O11 Na2 Ni1 116.07(9) 2_766 . ? O3 Na2 Ni1 38.84(6) . . ? O4 Na2 Ni1 95.29(8) . . ? O7 Na2 Ni1 141.12(8) . . ? C7 Na2 Ni1 119.34(10) . . ? Na1 Na2 Ni1 62.57(4) . . ? Na4 Na2 Ni1 124.29(6) . . ? O2 Na2 Na3 87.34(9) . . ? O11 Na2 Na3 111.48(11) 2_766 . ? O3 Na2 Na3 42.49(8) . . ? O4 Na2 Na3 47.13(8) . . ? O7 Na2 Na3 143.48(10) . . ? C7 Na2 Na3 160.95(11) . . ? Na1 Na2 Na3 59.88(5) . . ? Na4 Na2 Na3 95.47(6) . . ? Ni1 Na2 Na3 59.30(4) . . ? O2 Na2 Na5 146.09(9) . 2_766 ? O11 Na2 Na5 32.08(9) 2_766 2_766 ? O3 Na2 Na5 72.63(8) . 2_766 ? O4 Na2 Na5 95.64(8) . 2_766 ? O7 Na2 Na5 105.35(8) . 2_766 ? C7 Na2 Na5 114.66(10) . 2_766 ? Na1 Na2 Na5 139.07(7) . 2_766 ? Na4 Na2 Na5 113.76(5) . 2_766 ? Ni1 Na2 Na5 110.23(5) . 2_766 ? Na3 Na2 Na5 81.40(5) . 2_766 ? O2 Na2 Na3 157.60(9) . 2_766 ? O11 Na2 Na3 68.07(9) 2_766 2_766 ? O3 Na2 Na3 112.44(8) . 2_766 ? O4 Na2 Na3 61.47(7) . 2_766 ? O7 Na2 Na3 69.66(7) . 2_766 ? C7 Na2 Na3 93.74(10) . 2_766 ? Na1 Na2 Na3 107.87(6) . 2_766 ? Na4 Na2 Na3 59.76(4) . 2_766 ? Ni1 Na2 Na3 146.45(6) . 2_766 ? Na3 Na2 Na3 87.69(5) . 2_766 ? Na5 Na2 Na3 54.02(4) 2_766 2_766 ? O3 Na3 O5 95.78(12) . 2_766 ? O3 Na3 O6 171.50(12) . 2_766 ? O5 Na3 O6 76.30(11) 2_766 2_766 ? O3 Na3 O1 77.29(10) . . ? O5 Na3 O1 131.16(12) 2_766 . ? O6 Na3 O1 110.19(11) 2_766 . ? O3 Na3 O4 89.40(11) . . ? O5 Na3 O4 137.07(10) 2_766 . ? O6 Na3 O4 94.33(11) 2_766 . ? O1 Na3 O4 91.58(10) . . ? O3 Na3 Na1 83.41(9) . . ? O5 Na3 Na1 176.40(9) 2_766 . ? O6 Na3 Na1 104.68(9) 2_766 . ? O1 Na3 Na1 45.24(8) . . ? O4 Na3 Na1 46.50(7) . . ? O3 Na3 Ni1 38.09(7) . . ? O5 Na3 Ni1 116.66(9) 2_766 . ? O6 Na3 Ni1 148.86(8) 2_766 . ? O1 Na3 Ni1 39.33(7) . . ? O4 Na3 Ni1 93.04(8) . . ? Na1 Na3 Ni1 60.76(4) . . ? O3 Na3 Ni2 133.34(9) . 2_766 ? O5 Na3 Ni2 37.56(8) 2_766 2_766 ? O6 Na3 Ni2 38.86(7) 2_766 2_766 ? O1 Na3 Ni2 127.73(9) . 2_766 ? O4 Na3 Ni2 123.05(8) . 2_766 ? Na1 Na3 Ni2 143.08(7) . 2_766 ? Ni1 Na3 Ni2 143.85(6) . 2_766 ? O3 Na3 Na2 44.13(8) . . ? O5 Na3 Na2 125.70(10) 2_766 . ? O6 Na3 Na2 139.07(9) 2_766 . ? O1 Na3 Na2 81.94(9) . . ? O4 Na3 Na2 45.26(8) . . ? Na1 Na3 Na2 55.73(5) . . ? Ni1 Na3 Na2 58.40(4) . . ? Ni2 Na3 Na2 150.32(5) 2_766 . ? O3 Na3 Na5 126.94(10) . . ? O5 Na3 Na5 127.67(9) 2_766 . ? O6 Na3 Na5 58.38(8) 2_766 . ? O1 Na3 Na5 90.90(8) . . ? O4 Na3 Na5 38.75(8) . . ? Na1 Na3 Na5 54.95(5) . . ? Ni1 Na3 Na5 115.66(5) . . ? Ni2 Na3 Na5 94.64(5) 2_766 . ? Na2 Na3 Na5 83.30(5) . . ? O3 Na3 Na4 89.50(8) . 2_766 ? O5 Na3 Na4 37.25(7) 2_766 2_766 ? O6 Na3 Na4 82.31(8) 2_766 2_766 ? O1 Na3 Na4 162.04(9) . 2_766 ? O4 Na3 Na4 100.52(7) . 2_766 ? Na1 Na3 Na4 146.08(6) . 2_766 ? Ni1 Na3 Na4 125.84(6) . 2_766 ? Ni2 Na3 Na4 55.02(4) 2_766 2_766 ? Na2 Na3 Na4 97.12(5) . 2_766 ? Na5 Na3 Na4 106.85(5) . 2_766 ? O3 Na3 Na2 116.95(8) . 2_766 ? O5 Na3 Na2 73.91(8) 2_766 2_766 ? O6 Na3 Na2 58.24(7) 2_766 2_766 ? O1 Na3 Na2 151.94(9) . 2_766 ? O4 Na3 Na2 65.93(7) . 2_766 ? Na1 Na3 Na2 109.59(5) . 2_766 ? Ni1 Na3 Na2 150.11(6) . 2_766 ? Ni2 Na3 Na2 61.61(4) 2_766 2_766 ? Na2 Na3 Na2 92.31(5) . 2_766 ? Na5 Na3 Na2 61.09(4) . 2_766 ? Na4 Na3 Na2 45.77(4) 2_766 2_766 ? O10 Na4 O7 168.05(13) . . ? O10 Na4 O4 93.81(12) . . ? O7 Na4 O4 97.34(11) . . ? O10 Na4 O5 106.31(11) . . ? O7 Na4 O5 74.75(10) . . ? O4 Na4 O5 105.82(11) . . ? O10 Na4 O8 75.38(10) . . ? O7 Na4 O8 99.86(11) . . ? O4 Na4 O8 92.03(11) . . ? O5 Na4 O8 161.79(13) . . ? O10 Na4 C14 87.47(12) . . ? O7 Na4 C14 89.44(12) . . ? O4 Na4 C14 125.96(12) . . ? O5 Na4 C14 26.03(10) . . ? O8 Na4 C14 139.54(13) . . ? O10 Na4 Na2 140.14(11) . . ? O7 Na4 Na2 49.63(8) . . ? O4 Na4 Na2 48.73(8) . . ? O5 Na4 Na2 98.19(9) . . ? O8 Na4 Na2 90.84(8) . . ? C14 Na4 Na2 123.40(10) . . ? O10 Na4 Na1 87.66(9) . . ? O7 Na4 Na1 96.80(8) . . ? O4 Na4 Na1 46.98(7) . . ? O5 Na4 Na1 151.11(10) . . ? O8 Na4 Na1 45.59(8) . . ? C14 Na4 Na1 171.05(11) . . ? Na2 Na4 Na1 57.97(5) . . ? O10 Na4 Na5 46.54(9) . . ? O7 Na4 Na5 144.73(10) . . ? O4 Na4 Na5 47.39(8) . . ? O5 Na4 Na5 111.17(10) . . ? O8 Na4 Na5 83.45(9) . . ? C14 Na4 Na5 110.81(10) . . ? Na2 Na4 Na5 95.49(6) . . ? Na1 Na4 Na5 60.61(5) . . ? O10 Na4 Ni2 140.42(9) . . ? O7 Na4 Ni2 37.71(6) . . ? O4 Na4 Ni2 109.57(8) . . ? O5 Na4 Ni2 37.61(8) . . ? O8 Na4 Ni2 132.60(10) . . ? C14 Na4 Ni2 52.97(9) . . ? Na2 Na4 Ni2 75.17(5) . . ? Na1 Na4 Ni2 131.65(6) . . ? Na5 Na4 Ni2 141.85(6) . . ? O10 Na4 Ni3 37.73(7) . . ? O7 Na4 Ni3 136.95(8) . . ? O4 Na4 Ni3 92.26(8) . . ? O5 Na4 Ni3 141.75(9) . . ? O8 Na4 Ni3 37.70(7) . . ? C14 Na4 Ni3 117.90(10) . . ? Na2 Na4 Ni3 118.59(5) . . ? Na1 Na4 Ni3 60.96(4) . . ? Na5 Na4 Ni3 58.36(4) . . ? Ni2 Na4 Ni3 157.57(6) . . ? O10 Na4 Na3 108.94(9) . 2_766 ? O7 Na4 Na3 79.07(8) . 2_766 ? O4 Na4 Na3 70.19(7) . 2_766 ? O5 Na4 Na3 35.64(8) . 2_766 ? O8 Na4 Na3 161.74(10) . 2_766 ? C14 Na4 Na3 58.64(9) . 2_766 ? Na2 Na4 Na3 74.47(5) . 2_766 ? Na1 Na4 Na3 116.20(6) . 2_766 ? Na5 Na4 Na3 87.16(5) . 2_766 ? Ni2 Na4 Na3 54.70(4) . 2_766 ? Ni3 Na4 Na3 142.89(6) . 2_766 ? O10 Na4 H4O 94.2(11) . . ? O7 Na4 H4O 97.7(11) . . ? O4 Na4 H4O 21(1) . . ? O5 Na4 H4O 85.8(5) . . ? O8 Na4 H4O 112.3(5) . . ? C14 Na4 H4O 105(1) . . ? Na2 Na4 H4O 56.3(10) . . ? Na1 Na4 H4O 68(1) . . ? Na5 Na4 H4O 50.1(11) . . ? Ni2 Na4 H4O 97.1(9) . . ? Ni3 Na4 H4O 105.2(9) . . ? Na3 Na4 H4O 50.5(6) 2_766 . ? O9 Na5 O10 79.20(11) . . ? O9 Na5 O4 93.20(11) . . ? O10 Na5 O4 92.11(12) . . ? O9 Na5 O11 145.27(13) . . ? O10 Na5 O11 133.79(11) . . ? O4 Na5 O11 95.53(11) . . ? O9 Na5 N5 98.09(13) . . ? O10 Na5 N5 107.97(14) . . ? O4 Na5 N5 158.45(15) . . ? O11 Na5 N5 65.05(13) . . ? O9 Na5 Ni3 39.65(8) . . ? O10 Na5 Ni3 39.56(7) . . ? O4 Na5 Ni3 94.26(8) . . ? O11 Na5 Ni3 168.48(10) . . ? N5 Na5 Ni3 106.14(11) . . ? O9 Na5 Na1 47.42(8) . . ? O10 Na5 Na1 85.45(9) . . ? O4 Na5 Na1 45.83(7) . . ? O11 Na5 Na1 130.17(10) . . ? N5 Na5 Na1 141.03(11) . . ? Ni3 Na5 Na1 61.35(4) . . ? O9 Na5 Na4 87.08(10) . . ? O10 Na5 Na4 45.58(8) . . ? O4 Na5 Na4 46.65(8) . . ? O11 Na5 Na4 122.57(9) . . ? N5 Na5 Na4 151.80(12) . . ? Ni3 Na5 Na4 61.48(4) . . ? Na1 Na5 Na4 58.55(5) . . ? O9 Na5 Na3 89.57(9) . . ? O10 Na5 Na3 130.01(10) . . ? O4 Na5 Na3 39.61(8) . . ? O11 Na5 Na3 76.44(9) . . ? N5 Na5 Na3 121.85(12) . . ? Ni3 Na5 Na3 115.06(5) . . ? Na1 Na5 Na3 53.74(4) . . ? Na4 Na5 Na3 85.71(6) . . ? O9 Na5 Na2 154.36(10) . 2_766 ? O10 Na5 Na2 118.30(8) . 2_766 ? O4 Na5 Na2 68.93(7) . 2_766 ? O11 Na5 Na2 30.28(8) . 2_766 ? N5 Na5 Na2 93.98(11) . 2_766 ? Ni3 Na5 Na2 153.71(6) . 2_766 ? Na1 Na5 Na2 111.93(6) . 2_766 ? Na4 Na5 Na2 92.89(5) . 2_766 ? Na3 Na5 Na2 64.89(4) . 2_766 ? O9 Na5 H4O 113.5(5) . . ? O10 Na5 H4O 92.4(11) . . ? O4 Na5 H4O 20.5(4) . . ? O11 Na5 H4O 80.5(8) . . ? N5 Na5 H4O 145.3(7) . . ? Ni3 Na5 H4O 107.4(9) . . ? Na1 Na5 H4O 66.2(4) . . ? Na4 Na5 H4O 49.2(10) . . ? Na3 Na5 H4O 48.1(9) . . ? Na2 Na5 H4O 51.3(7) 2_766 . ? O13 Na6 O12 162.52(12) . . ? O13 Na6 O16 96.85(11) . . ? O12 Na6 O16 100.04(11) . . ? O13 Na6 O21 108.15(11) . . ? O12 Na6 O21 75.67(11) . . ? O16 Na6 O21 92.49(11) . . ? O13 Na6 O14 77.68(11) . . ? O12 Na6 O14 95.93(12) . . ? O16 Na6 O14 96.34(10) . . ? O21 Na6 O14 168.79(12) . . ? O13 Na6 Na7 89.98(9) . . ? O12 Na6 Na7 97.54(9) . . ? O16 Na6 Na7 49.62(8) . . ? O21 Na6 Na7 140.40(9) . . ? O14 Na6 Na7 47.03(7) . . ? O13 Na6 Na9 144.23(9) . . ? O12 Na6 Na9 51.38(8) . . ? O16 Na6 Na9 49.22(8) . . ? O21 Na6 Na9 87.15(8) . . ? O14 Na6 Na9 93.39(8) . . ? Na7 Na6 Na9 60.57(5) . . ? O13 Na6 Na10 107.08(10) . . ? O12 Na6 Na10 87.70(10) . . ? O16 Na6 Na10 48.14(8) . . ? O21 Na6 Na10 44.39(7) . . ? O14 Na6 Na10 144.18(8) . . ? Na7 Na6 Na10 97.16(6) . . ? Na9 Na6 Na10 61.54(5) . . ? O13 Na6 Ni5 39.31(8) . . ? O12 Na6 Ni5 133.98(10) . . ? O16 Na6 Ni5 94.25(8) . . ? O21 Na6 Ni5 147.36(9) . . ? O14 Na6 Ni5 38.76(7) . . ? Na7 Na6 Ni5 60.52(4) . . ? Na9 Na6 Ni5 120.80(6) . . ? Na10 Na6 Ni5 131.83(6) . . ? O13 Na6 Na8 47.37(8) . . ? O12 Na6 Na8 149.63(9) . . ? O16 Na6 Na8 49.60(8) . . ? O21 Na6 Na8 103.02(9) . . ? O14 Na6 Na8 87.99(8) . . ? Na7 Na6 Na8 63.70(5) . . ? Na9 Na6 Na8 98.40(5) . . ? Na10 Na6 Na8 72.38(5) . . ? Ni5 Na6 Na8 59.52(4) . . ? O13 Na6 Ni4 145.22(10) . . ? O12 Na6 Ni4 37.40(8) . . ? O16 Na6 Ni4 94.73(8) . . ? O21 Na6 Ni4 38.50(7) . . ? O14 Na6 Ni4 133.30(9) . . ? Na7 Na6 Ni4 121.91(5) . . ? Na9 Na6 Ni4 61.66(4) . . ? Na10 Na6 Ni4 59.27(4) . . ? Ni5 Na6 Ni4 168.88(6) . . ? Na8 Na6 Ni4 131.59(6) . . ? O14 Na7 O15 78.30(10) . . ? O14 Na7 O22 132.44(13) . . ? O15 Na7 O22 91.98(11) . . ? O14 Na7 O16 99.14(11) . . ? O15 Na7 O16 90.01(11) . . ? O22 Na7 O16 127.61(12) . . ? O14 Na7 O19 97.13(11) . . ? O15 Na7 O19 173.20(13) . . ? O22 Na7 O19 87.42(10) . . ? O16 Na7 O19 95.72(11) . . ? O14 Na7 C67 77.77(12) . . ? O15 Na7 C67 145.73(14) . . ? O22 Na7 C67 86.39(12) . . ? O16 Na7 C67 117.77(13) . . ? O19 Na7 C67 27.48(11) . . ? O14 Na7 Na6 50.97(8) . . ? O15 Na7 Na6 85.79(9) . . ? O22 Na7 Na6 175.41(11) . . ? O16 Na7 Na6 48.49(7) . . ? O19 Na7 Na6 95.27(9) . . ? C67 Na7 Na6 97.71(10) . . ? O14 Na7 Na9 96.24(9) . . ? O15 Na7 Na9 137.79(10) . . ? O22 Na7 Na9 119.55(9) . . ? O16 Na7 Na9 49.08(8) . . ? O19 Na7 Na9 47.18(8) . . ? C67 Na7 Na9 69.24(11) . . ? Na6 Na7 Na9 60.54(5) . . ? O14 Na7 Ni5 39.17(7) . . ? O15 Na7 Ni5 39.17(7) . . ? O22 Na7 Ni5 118.41(9) . . ? O16 Na7 Ni5 94.45(7) . . ? O19 Na7 Ni5 136.24(9) . . ? C67 Na7 Ni5 113.98(10) . . ? Na6 Na7 Ni5 61.78(4) . . ? Na9 Na7 Ni5 122.04(5) . . ? O14 Na7 Na8 88.10(8) . . ? O15 Na7 Na8 42.09(8) . . ? O22 Na7 Na8 115.19(10) . . ? O16 Na7 Na8 47.94(8) . . ? O19 Na7 Na8 143.57(10) . . ? C67 Na7 Na8 158.31(11) . . ? Na6 Na7 Na8 60.64(5) . . ? Na9 Na7 Na8 96.47(6) . . ? Ni5 Na7 Na8 58.91(4) . . ? O14 Na7 Na8 157.04(10) . 2 ? O15 Na7 Na8 115.35(9) . 2 ? O22 Na7 Na8 67.99(8) . 2 ? O16 Na7 Na8 64.12(7) . 2 ? O19 Na7 Na8 70.66(8) . 2 ? C67 Na7 Na8 95.72(10) . 2 ? Na6 Na7 Na8 109.38(6) . 2 ? Na9 Na7 Na8 61.07(4) . 2 ? Ni5 Na7 Na8 149.52(6) . 2 ? Na8 Na7 Na8 90.93(5) . 2 ? O14 Na7 Na10 145.38(9) . 2 ? O15 Na7 Na10 72.95(8) . 2 ? O22 Na7 Na10 33.10(8) . 2 ? O16 Na7 Na10 99.74(8) . 2 ? O19 Na7 Na10 109.51(8) . 2 ? C67 Na7 Na10 117.45(10) . 2 ? Na6 Na7 Na10 142.34(7) . 2 ? Na9 Na7 Na10 118.00(5) . 2 ? Ni5 Na7 Na10 110.46(5) . 2 ? Na8 Na7 Na10 83.39(5) . 2 ? Na8 Na7 Na10 56.95(4) 2 2 ? O15 Na8 O17 94.42(12) . 2 ? O15 Na8 O13 77.83(11) . . ? O17 Na8 O13 130.93(11) 2 . ? O15 Na8 O18 170.16(12) . 2 ? O17 Na8 O18 75.86(11) 2 2 ? O13 Na8 O18 109.57(11) . 2 ? O15 Na8 O16 88.45(11) . . ? O17 Na8 O16 139.12(11) 2 . ? O13 Na8 O16 89.55(10) . . ? O18 Na8 O16 97.90(11) 2 . ? O15 Na8 Ni5 38.39(7) . . ? O17 Na8 Ni5 115.51(10) 2 . ? O13 Na8 Ni5 39.59(7) . . ? O18 Na8 Ni5 147.98(8) 2 . ? O16 Na8 Ni5 91.34(8) . . ? O15 Na8 Na6 82.66(9) . . ? O17 Na8 Na6 174.67(10) 2 . ? O13 Na8 Na6 44.12(7) . . ? O18 Na8 Na6 107.15(9) 2 . ? O16 Na8 Na6 45.53(7) . . ? Ni5 Na8 Na6 59.61(4) . . ? O15 Na8 Ni6 131.50(10) . 2 ? O17 Na8 Ni6 37.15(8) 2 2 ? O13 Na8 Ni6 130.02(9) . 2 ? O18 Na8 Ni6 38.73(7) 2 2 ? O16 Na8 Ni6 124.24(9) . 2 ? Ni5 Na8 Ni6 144.42(6) . 2 ? Na6 Na8 Ni6 145.79(7) . 2 ? O15 Na8 Na7 43.41(8) . . ? O17 Na8 Na7 124.54(9) 2 . ? O13 Na8 Na7 81.74(8) . . ? O18 Na8 Na7 142.23(9) 2 . ? O16 Na8 Na7 45.05(8) . . ? Ni5 Na8 Na7 57.87(4) . . ? Na6 Na8 Na7 55.66(5) . . ? Ni6 Na8 Na7 148.22(5) 2 . ? O15 Na8 Na9 86.92(8) . 2 ? O17 Na8 Na9 39.12(7) 2 2 ? O13 Na8 Na9 161.46(10) . 2 ? O18 Na8 Na9 84.53(8) 2 2 ? O16 Na8 Na9 100.63(7) . 2 ? Ni5 Na8 Na9 123.87(6) . 2 ? Na6 Na8 Na9 144.57(6) . 2 ? Ni6 Na8 Na9 55.26(4) 2 2 ? Na7 Na8 Na9 94.47(5) . 2 ? O15 Na8 Na10 124.80(10) . . ? O17 Na8 Na10 131.73(10) 2 . ? O13 Na8 Na10 88.08(8) . . ? O18 Na8 Na10 63.08(8) 2 . ? O16 Na8 Na10 37.76(7) . . ? Ni5 Na8 Na10 112.76(5) . . ? Na6 Na8 Na10 53.20(5) . . ? Ni6 Na8 Na10 98.11(5) 2 . ? Na7 Na8 Na10 82.08(5) . . ? Na9 Na8 Na10 109.47(5) 2 . ? O15 Na8 Na7 114.51(8) . 2 ? O17 Na8 Na7 77.94(8) 2 2 ? O13 Na8 Na7 149.31(9) . 2 ? O18 Na8 Na7 62.50(7) 2 2 ? O16 Na8 Na7 64.02(7) . 2 ? Ni5 Na8 Na7 146.64(5) . 2 ? Na6 Na8 Na7 107.32(5) . 2 ? Ni6 Na8 Na7 64.12(4) 2 2 ? Na7 Na8 Na7 89.07(5) . 2 ? Na9 Na8 Na7 47.90(4) 2 2 ? Na10 Na8 Na7 61.58(4) . 2 ? O20 Na9 O19 166.77(13) . . ? O20 Na9 O16 94.67(11) . . ? O19 Na9 O16 96.97(12) . . ? O20 Na9 O17 107.74(11) . . ? O19 Na9 O17 74.71(10) . . ? O16 Na9 O17 107.19(11) . . ? O20 Na9 O12 75.31(10) . . ? O19 Na9 O12 97.74(11) . . ? O16 Na9 O12 93.16(10) . . ? O17 Na9 O12 158.88(13) . . ? O20 Na9 C74 88.34(13) . . ? O19 Na9 C74 89.62(12) . . ? O16 Na9 C74 127.18(12) . . ? O17 Na9 C74 25.92(11) . . ? O12 Na9 C74 137.87(13) . . ? O20 Na9 Na6 87.96(8) . . ? O19 Na9 Na6 95.26(9) . . ? O16 Na9 Na6 47.60(7) . . ? O17 Na9 Na6 152.41(10) . . ? O12 Na9 Na6 46.06(8) . . ? C74 Na9 Na6 173.24(12) . . ? O20 Na9 Na7 141.05(10) . . ? O19 Na9 Na7 48.97(8) . . ? O16 Na9 Na7 48.56(8) . . ? O17 Na9 Na7 97.06(9) . . ? O12 Na9 Na7 92.19(9) . . ? C74 Na9 Na7 122.23(11) . . ? Na6 Na9 Na7 58.89(5) . . ? O20 Na9 Na10 47.39(8) . . ? O19 Na9 Na10 144.20(10) . . ? O16 Na9 Na10 47.36(8) . . ? O17 Na9 Na10 114.14(9) . . ? O12 Na9 Na10 83.69(9) . . ? C74 Na9 Na10 113.23(11) . . ? Na6 Na9 Na10 60.26(5) . . ? Na7 Na9 Na10 95.28(6) . . ? O20 Na9 Ni6 140.52(9) . . ? O19 Na9 Ni6 37.99(7) . . ? O16 Na9 Ni6 111.70(8) . . ? O17 Na9 Ni6 37.69(7) . . ? O12 Na9 Ni6 129.04(10) . . ? C74 Na9 Ni6 52.42(10) . . ? Na6 Na9 Ni6 131.52(7) . . ? Na7 Na9 Ni6 75.33(5) . . ? Na10 Na9 Ni6 145.50(6) . . ? O20 Na9 Ni4 37.72(7) . . ? O19 Na9 Ni4 134.85(9) . . ? O16 Na9 Ni4 93.18(8) . . ? O17 Na9 Ni4 142.40(10) . . ? O12 Na9 Ni4 37.66(7) . . ? C74 Na9 Ni4 118.01(11) . . ? Na6 Na9 Ni4 61.15(4) . . ? Na7 Na9 Ni4 119.74(5) . . ? Na10 Na9 Ni4 58.72(4) . . ? Ni6 Na9 Ni4 153.98(6) . . ? O20 Na9 Na8 112.58(9) . 2 ? O19 Na9 Na8 77.52(8) . 2 ? O16 Na9 Na8 69.91(7) . 2 ? O17 Na9 Na8 37.35(8) . 2 ? O12 Na9 Na8 161.42(9) . 2 ? C74 Na9 Na8 60.57(10) . 2 ? Na6 Na9 Na8 115.93(6) . 2 ? Na7 Na9 Na8 71.03(5) . 2 ? Na10 Na9 Na8 89.83(5) . 2 ? Ni6 Na9 Na8 55.67(4) . 2 ? Ni4 Na9 Na8 146.33(6) . 2 ? O20 Na9 H16O 92.5(10) . . ? O19 Na9 H16O 100.6(10) . . ? O16 Na9 H16O 20.0(4) . . ? O17 Na9 H16O 89.1(6) . . ? O12 Na9 H16O 111.9(6) . . ? C74 Na9 H16O 107.3(5) . . ? Na6 Na9 H16O 67.2(5) . . ? Na7 Na9 H16O 57.7(9) . . ? Na10 Na9 H16O 47.6(10) . . ? Ni6 Na9 H16O 102.5(9) . . ? Ni4 Na9 H16O 103.5(9) . . ? Na8 Na9 H16O 52.7(7) 2 . ? O21 Na10 O20 78.66(10) . . ? O21 Na10 O16 94.51(11) . . ? O20 Na10 O16 92.28(11) . . ? O21 Na10 O22 142.58(12) . 2 ? O20 Na10 O22 137.95(11) . 2 ? O16 Na10 O22 91.72(11) . 2 ? O21 Na10 N17 99.72(13) . 2 ? O20 Na10 N17 106.84(14) . 2 ? O16 Na10 N17 158.02(14) . 2 ? O22 Na10 N17 66.86(13) 2 2 ? O21 Na10 Ni4 39.33(8) . . ? O20 Na10 Ni4 39.35(6) . . ? O16 Na10 Ni4 95.24(8) . . ? O22 Na10 Ni4 172.59(10) 2 . ? N17 Na10 Ni4 106.39(11) 2 . ? O21 Na10 Na6 48.03(8) . . ? O20 Na10 Na6 84.86(9) . . ? O16 Na10 Na6 46.51(7) . . ? O22 Na10 Na6 125.84(10) 2 . ? N17 Na10 Na6 143.82(10) 2 . ? Ni4 Na10 Na6 61.37(4) . . ? O21 Na10 Na9 86.93(9) . . ? O20 Na10 Na9 45.06(8) . . ? O16 Na10 Na9 47.29(8) . . ? O22 Na10 Na9 122.87(9) 2 . ? N17 Na10 Na9 149.57(11) 2 . ? Ni4 Na10 Na9 61.27(4) . . ? Na6 Na10 Na9 58.20(5) . . ? O21 Na10 Na8 90.67(9) . . ? O20 Na10 Na8 130.04(10) . . ? O16 Na10 Na8 39.54(7) . . ? O22 Na10 Na8 71.41(9) 2 . ? N17 Na10 Na8 123.10(11) 2 . ? Ni4 Na10 Na8 115.75(5) . . ? Na6 Na10 Na8 54.43(5) . . ? Na9 Na10 Na8 86.16(5) . . ? O21 Na10 Na7 152.13(10) . 2 ? O20 Na10 Na7 118.03(8) . 2 ? O16 Na10 Na7 64.37(7) . 2 ? O22 Na10 Na7 32.41(7) 2 2 ? N17 Na10 Na7 96.36(11) 2 2 ? Ni4 Na10 Na7 151.70(6) . 2 ? Na6 Na10 Na7 108.27(6) . 2 ? Na9 Na10 Na7 90.64(5) . 2 ? Na8 Na10 Na7 61.47(4) . 2 ? O21 Na10 H16O 115.4(4) . . ? O20 Na10 H16O 94.0(11) . . ? O16 Na10 H16O 21.0(3) . . ? O22 Na10 H16O 76.5(8) 2 . ? N17 Na10 H16O 142.2(6) 2 . ? Ni4 Na10 H16O 109.6(9) . . ? Na6 Na10 H16O 67.5(4) . . ? Na9 Na10 H16O 51.5(10) . . ? Na8 Na10 H16O 47.3(10) . . ? Na7 Na10 H16O 45.8(7) 2 . ? C55 O1 Ni1 111.2(3) . . ? C55 O1 Na1 143.6(3) . . ? Ni1 O1 Na1 97.29(12) . . ? C55 O1 Na3 115.0(3) . . ? Ni1 O1 Na3 91.67(10) . . ? Na1 O1 Na3 85.16(10) . . ? C49 O2 Ni1 113.4(2) . . ? C49 O2 Na2 139.3(3) . . ? Ni1 O2 Na2 96.53(11) . . ? C49 O2 Na1 121.1(2) . . ? Ni1 O2 Na1 94.13(12) . . ? Na2 O2 Na1 81.25(10) . . ? C43 O3 Ni1 112.5(2) . . ? C43 O3 Na3 128.9(3) . . ? Ni1 O3 Na3 98.32(12) . . ? C43 O3 Na2 121.9(3) . . ? Ni1 O3 Na2 94.89(12) . . ? Na3 O3 Na2 93.38(12) . . ? Na1 O4 Na2 81.03(10) . . ? Na1 O4 Na4 85.01(10) . . ? Na2 O4 Na4 82.49(11) . . ? Na1 O4 Na5 86.60(10) . . ? Na2 O4 Na5 163.73(13) . . ? Na4 O4 Na5 85.96(11) . . ? Na1 O4 Na3 83.99(9) . . ? Na2 O4 Na3 87.61(10) . . ? Na4 O4 Na3 166.21(13) . . ? Na5 O4 Na3 101.63(12) . . ? Na1 O4 H4O 171(3) . . ? Na2 O4 H4O 103(3) . . ? Na4 O4 H4O 88(3) . . ? Na5 O4 H4O 88(3) . . ? Na3 O4 H4O 104(3) . . ? C14 O5 Ni2 111.4(3) . . ? C14 O5 Na3 132.8(2) . 2_766 ? Ni2 O5 Na3 98.36(12) . 2_766 ? C14 O5 Na4 105.2(2) . . ? Ni2 O5 Na4 96.03(11) . . ? Na3 O5 Na4 107.11(13) 2_766 . ? C1 O6 Ni2 114.3(2) . . ? C1 O6 Na3 112.6(3) . 2_766 ? Ni2 O6 Na3 94.28(11) . 2_766 ? C7 O7 Ni2 113.4(3) . . ? C7 O7 Na4 137.1(3) . . ? Ni2 O7 Na4 96.45(12) . . ? C7 O7 Na2 103.8(3) . . ? Ni2 O7 Na2 123.89(13) . . ? Na4 O7 Na2 81.79(11) . . ? C38 O8 Ni3 114.8(3) . . ? C38 O8 Na1 142.9(3) . . ? Ni3 O8 Na1 99.36(14) . . ? C38 O8 Na4 106.0(3) . . ? Ni3 O8 Na4 94.34(11) . . ? Na1 O8 Na4 84.20(10) . . ? C31 O9 Ni3 113.7(3) . . ? C31 O9 Na5 138.3(3) . . ? Ni3 O9 Na5 96.71(11) . . ? C31 O9 Na1 114.2(3) . . ? Ni3 O9 Na1 95.08(13) . . ? Na5 O9 Na1 89.46(11) . . ? C19 O10 Ni3 111.0(2) . . ? C19 O10 Na4 135.3(3) . . ? Ni3 O10 Na4 97.95(12) . . ? C19 O10 Na5 122.4(3) . . ? Ni3 O10 Na5 92.79(12) . . ? Na4 O10 Na5 87.88(11) . . ? C25 O11 Na2 115.0(3) . 2_766 ? C25 O11 Na5 122.2(3) . . ? Na2 O11 Na5 117.64(15) 2_766 . ? C115 O12 Ni4 114.6(3) . . ? C115 O12 Na6 144.6(3) . . ? Ni4 O12 Na6 99.13(14) . . ? C115 O12 Na9 104.8(2) . . ? Ni4 O12 Na9 93.68(12) . . ? Na6 O12 Na9 82.56(11) . . ? C110 O13 Ni5 110.7(3) . . ? C110 O13 Na6 140.6(3) . . ? Ni5 O13 Na6 96.17(11) . . ? C110 O13 Na8 117.5(3) . . ? Ni5 O13 Na8 92.22(10) . . ? Na6 O13 Na8 88.51(10) . . ? C103 O14 Ni5 113.0(2) . . ? C103 O14 Na7 140.3(2) . . ? Ni5 O14 Na7 95.23(12) . . ? C103 O14 Na6 121.9(3) . . ? Ni5 O14 Na6 92.49(11) . . ? Na7 O14 Na6 82.00(10) . . ? C91 O15 Ni5 110.9(2) . . ? C91 O15 Na8 128.7(3) . . ? Ni5 O15 Na8 97.61(12) . . ? C91 O15 Na7 123.4(2) . . ? Ni5 O15 Na7 94.38(12) . . ? Na8 O15 Na7 94.50(12) . . ? Na6 O16 Na7 81.90(10) . . ? Na6 O16 Na9 83.18(10) . . ? Na7 O16 Na9 82.36(11) . . ? Na6 O16 Na10 85.35(10) . . ? Na7 O16 Na10 163.23(14) . . ? Na9 O16 Na10 85.35(11) . . ? Na6 O16 Na8 84.87(9) . . ? Na7 O16 Na8 87.02(11) . . ? Na9 O16 Na8 165.00(14) . . ? Na10 O16 Na8 102.70(11) . . ? Na6 O16 H16O 166(3) . . ? Na7 O16 H16O 110(3) . . ? Na9 O16 H16O 92(3) . . ? Na10 O16 H16O 82(3) . . ? Na8 O16 H16O 102(3) . . ? C74 O17 Ni6 110.0(3) . . ? C74 O17 Na8 136.7(3) . 2 ? Ni6 O17 Na8 98.60(13) . 2 ? C74 O17 Na9 105.5(2) . . ? Ni6 O17 Na9 95.01(11) . . ? Na8 O17 Na9 103.54(12) 2 . ? C61 O18 Ni6 113.7(2) . . ? C61 O18 Na8 115.0(3) . 2 ? Ni6 O18 Na8 94.31(12) . 2 ? C67 O19 Ni6 113.7(3) . . ? C67 O19 Na9 137.5(3) . . ? Ni6 O19 Na9 97.15(13) . . ? C67 O19 Na7 99.9(3) . . ? Ni6 O19 Na7 125.08(14) . . ? Na9 O19 Na7 83.84(11) . . ? C85 O20 Ni4 109.9(2) . . ? C85 O20 Na9 136.6(2) . . ? Ni4 O20 Na9 98.49(13) . . ? C85 O20 Na10 122.0(3) . . ? Ni4 O20 Na10 92.42(10) . . ? Na9 O20 Na10 87.55(11) . . ? C79 O21 Ni4 114.9(3) . . ? C79 O21 Na10 136.3(3) . . ? Ni4 O21 Na10 96.55(11) . . ? C79 O21 Na6 117.2(3) . . ? Ni4 O21 Na6 94.88(12) . . ? Na10 O21 Na6 87.58(10) . . ? C97 O22 Na7 115.0(2) . . ? C97 O22 Na10 121.5(3) . 2 ? Na7 O22 Na10 114.50(13) . 2 ? C3 N1 C2 117.1(4) . . ? C3 N1 Ni2 128.7(3) . . ? C2 N1 Ni2 113.1(3) . . ? C8 N2 C9 118.6(4) . . ? C8 N2 Ni2 111.2(3) . . ? C9 N2 Ni2 129.1(3) . . ? C18 N3 C13 120.8(4) . . ? C18 N3 Ni2 128.2(4) . . ? C13 N3 Ni2 110.3(3) . . ? C20 N4 C21 118.8(5) . . ? C20 N4 Ni3 110.6(3) . . ? C21 N4 Ni3 130.4(4) . . ? C26 N5 C27 116.4(5) . . ? C26 N5 Na5 119.5(3) . . ? C27 N5 Na5 122.0(4) . . ? C32 N6 C33 117.8(4) . . ? C32 N6 Ni3 113.3(3) . . ? C33 N6 Ni3 128.8(4) . . ? C42 N7 C37 114.5(6) . . ? C42 N7 Ni3 133.0(5) . . ? C37 N7 Ni3 112.5(4) . . ? C44 N8 C45 119.0(4) . . ? C44 N8 Ni1 110.8(3) . . ? C45 N8 Ni1 130.1(3) . . ? C50 N9 C51 117.9(4) . . ? C50 N9 Ni1 113.1(3) . . ? C51 N9 Ni1 128.7(3) . . ? C56 N10 C57 117.2(4) . . ? C56 N10 Ni1 112.8(3) . . ? C57 N10 Ni1 129.8(4) . . ? C62 N11 C63 118.2(4) . . ? C62 N11 Ni6 113.6(3) . . ? C63 N11 Ni6 127.9(3) . . ? C68 N12 C69 116.1(4) . . ? C68 N12 Ni6 112.9(3) . . ? C69 N12 Ni6 131.0(3) . . ? C73 N13 C78 117.8(4) . . ? C73 N13 Ni6 111.4(3) . . ? C78 N13 Ni6 130.3(4) . . ? C80 N14 C81 118.0(4) . . ? C80 N14 Ni4 113.1(3) . . ? C81 N14 Ni4 128.7(4) . . ? C87 N15 C86 119.2(4) . . ? C87 N15 Ni4 129.6(3) . . ? C86 N15 Ni4 110.7(3) . . ? C93 N16 C92 119.2(4) . . ? C93 N16 Ni5 130.0(3) . . ? C92 N16 Ni5 110.8(3) . . ? C99 N17 C98 116.5(5) . . ? C99 N17 Na10 124.3(4) . 2 ? C98 N17 Na10 118.7(3) . 2 ? C104 N18 C105 118.2(4) . . ? C104 N18 Ni5 111.3(2) . . ? C105 N18 Ni5 130.4(3) . . ? C109 N19 C114 119.9(4) . . ? C109 N19 Ni5 111.4(3) . . ? C114 N19 Ni5 128.6(3) . . ? C116 N20 C117 116.8(5) . . ? C116 N20 Ni4 112.4(4) . . ? C117 N20 Ni4 129.9(4) . . ? O6 C1 C2 112.5(4) . . ? O6 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? O6 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N1 C2 C6 124.4(4) . . ? N1 C2 C1 116.0(4) . . ? C6 C2 C1 119.6(4) . . ? N1 C3 C4 123.8(5) . . ? N1 C3 H3 118.1 . . ? C4 C3 H3 118.1 . . ? C3 C4 C5 118.6(5) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 118.6(5) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C2 117.4(5) . . ? C5 C6 H6 121.3 . . ? C2 C6 H6 121.3 . . ? O7 C7 C8 115.9(4) . . ? O7 C7 Na2 50.2(2) . . ? C8 C7 Na2 132.0(3) . . ? O7 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? Na2 C7 H7A 119.7 . . ? O7 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? Na2 C7 H7B 58.2 . . ? H7A C7 H7B 107.4 . . ? N2 C8 C12 121.2(5) . . ? N2 C8 C7 116.0(4) . . ? C12 C8 C7 122.8(4) . . ? C10 C9 N2 122.4(5) . . ? C10 C9 H9 118.8 . . ? N2 C9 H9 118.8 . . ? C9 C10 C11 118.4(5) . . ? C9 C10 H10 120.8 . . ? C11 C10 H10 120.8 . . ? C12 C11 C10 119.4(6) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C8 119.9(5) . . ? C11 C12 H12 120.0 . . ? C8 C12 H12 120.0 . . ? N3 C13 C15 120.0(5) . . ? N3 C13 C14 115.8(4) . . ? C15 C13 C14 124.2(5) . . ? O5 C14 C13 112.3(4) . . ? O5 C14 Na4 48.76(17) . . ? C13 C14 Na4 88.7(2) . . ? O5 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? Na4 C14 H14A 156.8 . . ? O5 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? Na4 C14 H14B 78.5 . . ? H14A C14 H14B 107.9 . . ? C13 C15 C17 121.5(5) . . ? C13 C15 H15 119.3 . . ? C17 C15 H15 119.3 . . ? C17 C16 C18 120.0(5) . . ? C17 C16 H16 120.0 . . ? C18 C16 H16 120.0 . . ? C16 C17 C15 117.7(5) . . ? C16 C17 H17 121.2 . . ? C15 C17 H17 121.2 . . ? N3 C18 C16 120.1(5) . . ? N3 C18 H18 120.0 . . ? C16 C18 H18 120.0 . . ? O10 C19 C20 112.3(4) . . ? O10 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? O10 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N4 C20 C24 120.6(5) . . ? N4 C20 C19 116.1(4) . . ? C24 C20 C19 123.2(4) . . ? N4 C21 C22 122.2(5) . . ? N4 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C23 C22 C21 119.6(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 119.1(6) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C20 119.7(5) . . ? C23 C24 H24 120.1 . . ? C20 C24 H24 120.1 . . ? O11 C25 C26 115.0(4) . . ? O11 C25 H25A 108.5 . . ? C26 C25 H25A 108.5 . . ? O11 C25 H25B 108.5 . . ? C26 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? N5 C26 C30 121.3(5) . . ? N5 C26 C25 116.1(5) . . ? C30 C26 C25 122.5(5) . . ? N5 C27 C28 124.9(6) . . ? N5 C27 H27 117.5 . . ? C28 C27 H27 117.5 . . ? C29 C28 C27 118.1(6) . . ? C29 C28 H28 121.0 . . ? C27 C28 H28 121.0 . . ? C28 C29 C30 118.2(6) . . ? C28 C29 H29 120.9 . . ? C30 C29 H29 120.9 . . ? C29 C30 C26 121.0(6) . . ? C29 C30 H30 119.5 . . ? C26 C30 H30 119.5 . . ? O9 C31 C32 113.5(4) . . ? O9 C31 H31A 108.9 . . ? C32 C31 H31A 108.9 . . ? O9 C31 H31B 108.9 . . ? C32 C31 H31B 108.9 . . ? H31A C31 H31B 107.7 . . ? N6 C32 C36 122.5(5) . . ? N6 C32 C31 116.4(4) . . ? C36 C32 C31 121.2(5) . . ? N6 C33 C34 124.6(6) . . ? N6 C33 H33 117.7 . . ? C34 C33 H33 117.7 . . ? C35 C34 C33 116.5(5) . . ? C35 C34 H34 121.8 . . ? C33 C34 H34 121.8 . . ? C34 C35 C36 121.3(5) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C35 C36 C32 117.3(5) . . ? C35 C36 H36 121.4 . . ? C32 C36 H36 121.4 . . ? N7 C37 C39 122.9(6) . . ? N7 C37 C38 115.5(5) . . ? C39 C37 C38 121.6(7) . . ? O8 C38 C37 114.4(5) . . ? O8 C38 H38A 108.7 . . ? C37 C38 H38A 108.7 . . ? O8 C38 H38B 108.7 . . ? C37 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C37 C39 C41 119.8(7) . . ? C37 C39 H39 120.1 . . ? C41 C39 H39 120.1 . . ? C42 C40 C41 118.0(8) . . ? C42 C40 H40 121.0 . . ? C41 C40 H40 121.0 . . ? C39 C41 C40 117.3(7) . . ? C39 C41 H41 121.4 . . ? C40 C41 H41 121.4 . . ? C40 C42 N7 127.5(7) . . ? C40 C42 H42 116.3 . . ? N7 C42 H42 116.3 . . ? O3 C43 C44 112.0(4) . . ? O3 C43 H43A 109.2 . . ? C44 C43 H43A 109.2 . . ? O3 C43 H43B 109.2 . . ? C44 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? N8 C44 C48 121.3(4) . . ? N8 C44 C43 116.2(4) . . ? C48 C44 C43 122.5(4) . . ? N8 C45 C46 122.4(5) . . ? N8 C45 H45 118.8 . . ? C46 C45 H45 118.8 . . ? C47 C46 C45 119.0(6) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C46 C47 C48 118.4(6) . . ? C46 C47 H47 120.8 . . ? C48 C47 H47 120.8 . . ? C47 C48 C44 119.7(5) . . ? C47 C48 H48 120.2 . . ? C44 C48 H48 120.2 . . ? O2 C49 C50 113.9(4) . . ? O2 C49 H49A 108.8 . . ? C50 C49 H49A 108.8 . . ? O2 C49 H49B 108.8 . . ? C50 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? N9 C50 C54 122.2(4) . . ? N9 C50 C49 115.1(4) . . ? C54 C50 C49 122.7(5) . . ? N9 C51 C52 123.7(5) . . ? N9 C51 H51 118.2 . . ? C52 C51 H51 118.2 . . ? C51 C52 C53 117.1(4) . . ? C51 C52 H52 121.4 . . ? C53 C52 H52 121.4 . . ? C54 C53 C52 119.4(4) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C50 C54 C53 119.7(5) . . ? C50 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? O1 C55 C56 112.8(4) . . ? O1 C55 H55A 109.0 . . ? C56 C55 H55A 109.0 . . ? O1 C55 H55B 109.0 . . ? C56 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? N10 C56 C60 121.8(5) . . ? N10 C56 C55 115.8(4) . . ? C60 C56 C55 122.3(5) . . ? N10 C57 C58 124.7(5) . . ? N10 C57 H57 117.7 . . ? C58 C57 H57 117.7 . . ? C59 C58 C57 116.5(6) . . ? C59 C58 H58 121.7 . . ? C57 C58 H58 121.7 . . ? C60 C59 C58 120.3(6) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C59 C60 C56 119.4(6) . . ? C59 C60 H60 120.3 . . ? C56 C60 H60 120.3 . . ? O18 C61 C62 112.9(4) . . ? O18 C61 H61A 109.0 . . ? C62 C61 H61A 109.0 . . ? O18 C61 H61B 109.0 . . ? C62 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? N11 C62 C66 121.4(4) . . ? N11 C62 C61 115.8(4) . . ? C66 C62 C61 122.7(4) . . ? N11 C63 C64 123.6(5) . . ? N11 C63 H63 118.2 . . ? C64 C63 H63 118.2 . . ? C65 C64 C63 118.0(5) . . ? C65 C64 H64 121.0 . . ? C63 C64 H64 121.0 . . ? C64 C65 C66 120.4(5) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C62 C66 C65 118.3(5) . . ? C62 C66 H66 120.8 . . ? C65 C66 H66 120.8 . . ? O19 C67 C68 115.2(4) . . ? O19 C67 Na7 52.6(2) . . ? C68 C67 Na7 128.2(3) . . ? O19 C67 H67A 108.5 . . ? C68 C67 H67A 108.5 . . ? Na7 C67 H67A 55.8 . . ? O19 C67 H67B 108.5 . . ? C68 C67 H67B 108.5 . . ? Na7 C67 H67B 123.2 . . ? H67A C67 H67B 107.5 . . ? N12 C68 C72 121.6(4) . . ? N12 C68 C67 115.3(4) . . ? C72 C68 C67 123.1(4) . . ? C70 C69 N12 124.1(5) . . ? C70 C69 H69 117.9 . . ? N12 C69 H69 117.9 . . ? C69 C70 C71 120.1(5) . . ? C69 C70 H70 119.9 . . ? C71 C70 H70 119.9 . . ? C72 C71 C70 117.8(5) . . ? C72 C71 H71 121.1 . . ? C70 C71 H71 121.1 . . ? C71 C72 C68 120.2(5) . . ? C71 C72 H72 119.9 . . ? C68 C72 H72 119.9 . . ? N13 C73 C75 121.1(5) . . ? N13 C73 C74 114.9(4) . . ? C75 C73 C74 124.0(5) . . ? O17 C74 C73 110.9(4) . . ? O17 C74 Na9 48.61(18) . . ? C73 C74 Na9 84.3(2) . . ? O17 C74 H74A 109.5 . . ? C73 C74 H74A 109.5 . . ? Na9 C74 H74A 82.0 . . ? O17 C74 H74B 109.5 . . ? C73 C74 H74B 109.5 . . ? Na9 C74 H74B 158.0 . . ? H74A C74 H74B 108.0 . . ? C76 C75 C73 120.5(6) . . ? C76 C75 H75 119.8 . . ? C73 C75 H75 119.8 . . ? C75 C76 C77 118.5(6) . . ? C75 C76 H76 120.7 . . ? C77 C76 H76 120.7 . . ? C76 C77 C78 118.6(5) . . ? C76 C77 H77 120.7 . . ? C78 C77 H77 120.7 . . ? N13 C78 C77 123.4(5) . . ? N13 C78 H78 118.3 . . ? C77 C78 H78 118.3 . . ? O21 C79 C80 112.1(4) . . ? O21 C79 H79A 109.2 . . ? C80 C79 H79A 109.2 . . ? O21 C79 H79B 109.2 . . ? C80 C79 H79B 109.2 . . ? H79A C79 H79B 107.9 . . ? N14 C80 C84 123.1(5) . . ? N14 C80 C79 116.4(4) . . ? C84 C80 C79 120.5(5) . . ? N14 C81 C82 123.3(5) . . ? N14 C81 H81 118.4 . . ? C82 C81 H81 118.4 . . ? C81 C82 C83 118.3(5) . . ? C81 C82 H82 120.9 . . ? C83 C82 H82 120.9 . . ? C84 C83 C82 119.4(5) . . ? C84 C83 H83 120.3 . . ? C82 C83 H83 120.3 . . ? C83 C84 C80 118.0(5) . . ? C83 C84 H84 121.0 . . ? C80 C84 H84 121.0 . . ? O20 C85 C86 113.6(4) . . ? O20 C85 H85A 108.9 . . ? C86 C85 H85A 108.9 . . ? O20 C85 H85B 108.9 . . ? C86 C85 H85B 108.9 . . ? H85A C85 H85B 107.7 . . ? N15 C86 C90 121.8(4) . . ? N15 C86 C85 115.9(4) . . ? C90 C86 C85 122.2(4) . . ? N15 C87 C88 122.4(5) . . ? N15 C87 H87 118.8 . . ? C88 C87 H87 118.8 . . ? C89 C88 C87 118.2(5) . . ? C89 C88 H88 120.9 . . ? C87 C88 H88 120.9 . . ? C88 C89 C90 119.3(5) . . ? C88 C89 H89 120.3 . . ? C90 C89 H89 120.3 . . ? C86 C90 C89 119.1(4) . . ? C86 C90 H90 120.4 . . ? C89 C90 H90 120.4 . . ? O15 C91 C92 112.0(4) . . ? O15 C91 H91A 109.2 . . ? C92 C91 H91A 109.2 . . ? O15 C91 H91B 109.2 . . ? C92 C91 H91B 109.2 . . ? H91A C91 H91B 107.9 . . ? N16 C92 C96 121.2(5) . . ? N16 C92 C91 115.0(4) . . ? C96 C92 C91 123.8(4) . . ? N16 C93 C94 122.9(5) . . ? N16 C93 H93 118.6 . . ? C94 C93 H93 118.6 . . ? C93 C94 C95 117.4(5) . . ? C93 C94 H94 121.3 . . ? C95 C94 H94 121.3 . . ? C96 C95 C94 118.6(5) . . ? C96 C95 H95 120.7 . . ? C94 C95 H95 120.7 . . ? C95 C96 C92 120.6(5) . . ? C95 C96 H96 119.7 . . ? C92 C96 H96 119.7 . . ? O22 C97 C98 115.3(4) . . ? O22 C97 H97A 108.4 . . ? C98 C97 H97A 108.4 . . ? O22 C97 H97B 108.4 . . ? C98 C97 H97B 108.4 . . ? H97A C97 H97B 107.5 . . ? N17 C98 C102 123.1(5) . . ? N17 C98 C97 116.7(5) . . ? C102 C98 C97 120.3(5) . . ? N17 C99 C100 124.4(6) . . ? N17 C99 H99 117.8 . . ? C100 C99 H99 117.8 . . ? C101 C100 C99 117.8(6) . . ? C101 C100 H100 121.1 . . ? C99 C100 H100 121.1 . . ? C100 C101 C102 119.0(6) . . ? C100 C101 H101 120.5 . . ? C102 C101 H101 120.5 . . ? C98 C102 C101 119.2(6) . . ? C98 C102 H102 120.4 . . ? C101 C102 H102 120.4 . . ? O14 C103 C104 111.7(4) . . ? O14 C103 H10A 109.3 . . ? C104 C103 H10A 109.3 . . ? O14 C103 H10B 109.3 . . ? C104 C103 H10B 109.3 . . ? H10A C103 H10B 107.9 . . ? N18 C104 C108 122.7(4) . . ? N18 C104 C103 117.3(4) . . ? C108 C104 C103 120.0(4) . . ? N18 C105 C106 123.7(4) . . ? N18 C105 H105 118.1 . . ? C106 C105 H105 118.1 . . ? C107 C106 C105 117.8(4) . . ? C107 C106 H106 121.1 . . ? C105 C106 H106 121.1 . . ? C106 C107 C108 121.3(4) . . ? C106 C107 H107 119.3 . . ? C108 C107 H107 119.3 . . ? C107 C108 C104 116.2(5) . . ? C107 C108 H108 121.9 . . ? C104 C108 H108 121.9 . . ? N19 C109 C111 121.3(5) . . ? N19 C109 C110 116.6(4) . . ? C111 C109 C110 122.1(5) . . ? O13 C110 C109 111.6(4) . . ? O13 C110 H11A 109.3 . . ? C109 C110 H11A 109.3 . . ? O13 C110 H11B 109.3 . . ? C109 C110 H11B 109.3 . . ? H11A C110 H11B 108.0 . . ? C112 C111 C109 119.5(5) . . ? C112 C111 H111 120.2 . . ? C109 C111 H111 120.2 . . ? C111 C112 C113 119.3(6) . . ? C111 C112 H112 120.3 . . ? C113 C112 H112 120.3 . . ? C112 C113 C114 118.5(6) . . ? C112 C113 H113 120.8 . . ? C114 C113 H113 120.8 . . ? N19 C114 C113 121.5(5) . . ? N19 C114 H114 119.3 . . ? C113 C114 H114 119.3 . . ? O12 C115 C116 114.9(4) . . ? O12 C115 H11C 108.5 . . ? C116 C115 H11C 108.5 . . ? O12 C115 H11D 108.5 . . ? C116 C115 H11D 108.5 . . ? H11C C115 H11D 107.5 . . ? N20 C116 C120 124.6(5) . . ? N20 C116 C115 116.3(5) . . ? C120 C116 C115 119.0(5) . . ? N20 C117 C118 122.1(6) . . ? N20 C117 H117 119.0 . . ? C118 C117 H117 119.0 . . ? C117 C118 C119 118.7(6) . . ? C117 C118 H118 120.6 . . ? C119 C118 H118 120.6 . . ? C120 C119 C118 120.1(6) . . ? C120 C119 H119 119.9 . . ? C118 C119 H119 119.9 . . ? C119 C120 C116 117.6(6) . . ? C119 C120 H120 121.2 . . ? C116 C120 H120 121.2 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.422 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.098 # Attachment '- compound3_revised.cif' data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 776754' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C42 H49 N6 Ni3 O6, C H2 Cl2, Cl' _chemical_formula_sum 'C43 H51 Cl3 N6 Ni3 O6' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour green _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1030.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1480 0.1590 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.2974(4) _cell_length_b 18.2533(5) _cell_length_c 21.4614(5) _cell_angle_alpha 74.300(1) _cell_angle_beta 82.417(1) _cell_angle_gamma 65.885(1) _cell_volume 5264.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 48435 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2132 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 913 464 ' ' 2 0.500 0.500 0.000 149 75 ' ' _platon_squeeze_details ; ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51917 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 27.49 _reflns_number_total 24052 _reflns_number_gt 15144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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. The hydrogen atoms bound to O atoms were found in the Fo-Fc map and refined isotropically. Several molecules of dichloromethane were found in the crystals. Two of these (one per molecule) were not disordered and were refined unconstrained. The remaining were badly disordered over multiple positions and this disorder was considerably affecting the model quality. A PLATON-SQUEEZE procedure was run using the complete molecular model. The calculation estimated a residual electron density of 541 e/unit cell, indicating at least three missing dichloromethane molecules per asymmetric unit. The modified reflection data were then used for the refinement of the molecular structure, resulting in improved refinement parameters. ; _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^)+(0.0840P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24052 _refine_ls_number_parameters 1107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1492 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 0.27656(3) 0.71926(3) 0.284076(18) 0.02771(11) Uani 1 1 d . . . Ni2 Ni 0.14686(3) 0.80604(3) 0.182707(18) 0.02576(10) Uani 1 1 d . . . Ni3 Ni 0.04128(3) 0.80519(3) 0.300779(18) 0.02612(10) Uani 1 1 d . . . Ni4 Ni 0.15255(3) 0.30612(2) 0.184895(18) 0.02403(10) Uani 1 1 d . . . Ni5 Ni 0.03874(3) 0.30868(3) 0.299213(17) 0.02497(10) Uani 1 1 d . . . Ni6 Ni -0.08299(3) 0.37317(3) 0.192453(18) 0.02536(10) Uani 1 1 d . . . O1 O 0.15202(15) 0.70858(13) 0.26637(10) 0.0279(5) Uani 1 1 d . . . O2 O 0.16004(15) 0.83654(13) 0.26956(9) 0.0264(5) Uani 1 1 d . . . O3 O 0.28848(15) 0.75456(14) 0.18573(9) 0.0288(5) Uani 1 1 d . . . O4 O 0.25583(18) 0.68914(16) 0.38235(10) 0.0350(6) Uani 1 1 d . . . O5 O 0.00668(15) 0.84632(14) 0.20443(10) 0.0291(5) Uani 1 1 d . . . O6 O 0.08544(17) 0.75972(14) 0.39353(10) 0.0328(5) Uani 1 1 d . . . O7 O 0.03134(15) 0.40087(13) 0.21136(9) 0.0257(5) Uani 1 1 d . . . O8 O 0.03954(15) 0.26528(13) 0.21608(9) 0.0245(5) Uani 1 1 d . . . O9 O 0.17980(15) 0.26389(14) 0.28169(9) 0.0283(5) Uani 1 1 d . . . O10 O 0.11561(15) 0.34713(14) 0.08967(10) 0.0285(5) Uani 1 1 d . . . O11 O -0.10368(15) 0.35970(14) 0.29065(9) 0.0284(5) Uani 1 1 d . . . O12 O -0.05575(17) 0.38683(14) 0.09567(10) 0.0291(5) Uani 1 1 d . . . N1 N 0.1443(2) 0.75277(17) 0.10733(12) 0.0320(6) Uani 1 1 d . . . N2 N 0.39191(19) 0.75131(18) 0.29591(12) 0.0314(6) Uani 1 1 d . . . N3 N 0.3611(2) 0.59237(18) 0.29133(13) 0.0367(7) Uani 1 1 d . . . N4 N -0.0427(2) 0.92117(17) 0.32196(12) 0.0321(6) Uani 1 1 d . . . N5 N 0.1369(2) 0.91799(17) 0.11797(12) 0.0310(6) Uani 1 1 d . . . N6 N -0.0691(2) 0.75792(18) 0.32536(13) 0.0323(6) Uani 1 1 d . . . N7 N 0.0498(2) 0.37406(17) 0.36226(12) 0.0294(6) Uani 1 1 d . . . N8 N 0.26298(19) 0.19749(17) 0.16521(12) 0.0287(6) Uani 1 1 d . . . N9 N 0.2355(2) 0.37800(18) 0.16513(13) 0.0318(6) Uani 1 1 d . . . N10 N -0.1675(2) 0.30841(19) 0.18606(12) 0.0347(7) Uani 1 1 d . . . N11 N 0.0348(2) 0.20843(18) 0.37423(12) 0.0334(7) Uani 1 1 d . . . N12 N -0.1984(2) 0.49308(18) 0.17581(13) 0.0345(7) Uani 1 1 d . . . C1 C 0.3424(2) 0.7015(2) 0.14574(15) 0.0360(8) Uani 1 1 d . . . H7 H 0.3358 0.6490 0.1618 0.043 Uiso 1 1 calc R . . H8 H 0.4095 0.6914 0.1473 0.043 Uiso 1 1 calc R . . C2 C 0.3103(3) 0.7378(3) 0.07602(16) 0.0406(9) Uani 1 1 d . . . H5 H 0.3029 0.7952 0.0638 0.049 Uiso 1 1 calc R . . H6 H 0.3605 0.7086 0.0484 0.049 Uiso 1 1 calc R . . C3 C 0.2179(3) 0.7338(2) 0.06339(15) 0.0332(8) Uani 1 1 d . . . C4 C 0.0647(2) 0.7444(2) 0.09833(15) 0.0314(7) Uani 1 1 d . . . H4 H 0.0149 0.7572 0.1286 0.038 Uiso 1 1 calc R . . C5 C 0.0508(3) 0.7181(2) 0.04707(16) 0.0386(8) Uani 1 1 d . . . H3 H -0.0057 0.7122 0.0433 0.046 Uiso 1 1 calc R . . C6 C 0.1256(3) 0.7009(2) 0.00118(16) 0.0431(10) Uani 1 1 d . . . H2 H 0.1193 0.6847 -0.0349 0.052 Uiso 1 1 calc R . . C7 C 0.2082(3) 0.7083(2) 0.01013(16) 0.0419(9) Uani 1 1 d . . . H1 H 0.2587 0.6961 -0.0198 0.050 Uiso 1 1 calc R . . C8 C 0.2983(3) 0.7142(2) 0.42245(16) 0.0401(9) Uani 1 1 d . . . H15 H 0.2833 0.6934 0.4674 0.048 Uiso 1 1 calc R . . H16 H 0.2718 0.7741 0.4134 0.048 Uiso 1 1 calc R . . C9 C 0.4057(3) 0.6830(3) 0.41226(16) 0.0439(9) Uani 1 1 d . . . H13 H 0.4298 0.6256 0.4101 0.053 Uiso 1 1 calc R . . H14 H 0.4338 0.6850 0.4494 0.053 Uiso 1 1 calc R . . C10 C 0.4383(2) 0.7316(2) 0.35146(16) 0.0380(8) Uani 1 1 d . . . C11 C 0.4218(2) 0.7949(2) 0.24266(16) 0.0328(8) Uani 1 1 d . . . H12 H 0.3908 0.8090 0.2041 0.039 Uiso 1 1 calc R . . C12 C 0.4946(3) 0.8195(2) 0.24196(17) 0.0383(8) Uani 1 1 d . . . H11 H 0.5125 0.8496 0.2039 0.046 Uiso 1 1 calc R . . C13 C 0.5411(3) 0.7991(3) 0.29843(19) 0.0502(10) Uani 1 1 d . . . H10 H 0.5912 0.8153 0.2992 0.060 Uiso 1 1 calc R . . C14 C 0.5132(3) 0.7546(3) 0.35366(18) 0.0476(10) Uani 1 1 d . . . H9 H 0.5444 0.7400 0.3922 0.057 Uiso 1 1 calc R . . C15 C 0.3241(3) 0.5345(2) 0.31374(17) 0.0409(9) Uani 1 1 d . . . C16 C 0.2159(3) 0.5625(2) 0.32192(18) 0.0434(9) Uani 1 1 d . . . H19 H 0.1998 0.5149 0.3276 0.052 Uiso 1 1 calc R . . H20 H 0.1964 0.5820 0.3613 0.052 Uiso 1 1 calc R . . C17 C 0.1582(3) 0.6294(2) 0.26720(17) 0.0343(8) Uani 1 1 d . . . H17 H 0.1870 0.6161 0.2265 0.041 Uiso 1 1 calc R . . H18 H 0.0940 0.6302 0.2704 0.041 Uiso 1 1 calc R . . C18 C 0.3831(3) 0.4520(3) 0.3298(2) 0.0597(12) Uani 1 1 d . . . H24 H 0.3564 0.4129 0.3467 0.072 Uiso 1 1 calc R . . C19 C 0.4794(4) 0.4268(3) 0.3212(3) 0.0739(14) Uani 1 1 d . . . H23 H 0.5188 0.3709 0.3328 0.089 Uiso 1 1 calc R . . C20 C 0.5185(3) 0.4856(3) 0.2948(2) 0.0583(12) Uani 1 1 d . . . H22 H 0.5840 0.4704 0.2866 0.070 Uiso 1 1 calc R . . C21 C 0.4565(3) 0.5668(2) 0.28129(17) 0.0417(9) Uani 1 1 d . . . H21 H 0.4818 0.6067 0.2641 0.050 Uiso 1 1 calc R . . C22 C 0.1582(3) 0.9122(2) 0.27546(16) 0.0328(8) Uani 1 1 d . . . H31 H 0.1267 0.9556 0.2384 0.039 Uiso 1 1 calc R . . H32 H 0.2233 0.9083 0.2755 0.039 Uiso 1 1 calc R . . C23 C 0.1058(3) 0.9348(2) 0.33720(16) 0.0368(8) Uani 1 1 d . . . H29 H 0.1269 0.8861 0.3727 0.044 Uiso 1 1 calc R . . H30 H 0.1238 0.9759 0.3465 0.044 Uiso 1 1 calc R . . C24 C -0.0013(3) 0.9681(2) 0.33464(15) 0.0333(8) Uani 1 1 d . . . C25 C -0.1386(3) 0.9517(2) 0.31877(17) 0.0397(9) Uani 1 1 d . . . H28 H -0.1662 0.9188 0.3099 0.048 Uiso 1 1 calc R . . C26 C -0.1988(3) 1.0287(2) 0.32777(19) 0.0496(10) Uani 1 1 d . . . H27 H -0.2650 1.0477 0.3254 0.060 Uiso 1 1 calc R . . C27 C -0.1547(3) 1.0768(2) 0.34069(19) 0.0508(11) Uani 1 1 d . . . H26 H -0.1917 1.1295 0.3467 0.061 Uiso 1 1 calc R . . C28 C -0.0582(3) 1.0463(2) 0.34437(16) 0.0388(9) Uani 1 1 d . . . H25 H -0.0295 1.0781 0.3535 0.047 Uiso 1 1 calc R . . C29 C -0.0549(3) 0.9264(2) 0.17667(16) 0.0376(8) Uani 1 1 d . . . H39 H -0.0500 0.9640 0.1992 0.045 Uiso 1 1 calc R . . H40 H -0.1203 0.9297 0.1822 0.045 Uiso 1 1 calc R . . C30 C -0.0332(3) 0.9538(2) 0.10494(16) 0.0385(8) Uani 1 1 d . . . H37 H -0.0237 0.9098 0.0843 0.046 Uiso 1 1 calc R . . H38 H -0.0882 1.0017 0.0856 0.046 Uiso 1 1 calc R . . C31 C 0.0533(3) 0.9749(2) 0.09148(14) 0.0327(8) Uani 1 1 d . . . C32 C 0.2150(3) 0.9363(2) 0.10757(15) 0.0352(8) Uani 1 1 d . . . H36 H 0.2721 0.8971 0.1265 0.042 Uiso 1 1 calc R . . C33 C 0.2135(3) 1.0123(3) 0.06926(17) 0.0431(9) Uani 1 1 d . . . H35 H 0.2688 1.0233 0.0621 0.052 Uiso 1 1 calc R . . C34 C 0.1278(3) 1.0706(2) 0.04232(18) 0.0471(10) Uani 1 1 d . . . H34 H 0.1242 1.1216 0.0165 0.057 Uiso 1 1 calc R . . C35 C 0.0477(3) 1.0516(2) 0.05443(16) 0.0417(9) Uani 1 1 d . . . H33 H -0.0107 1.0908 0.0375 0.050 Uiso 1 1 calc R . . C36 C 0.0428(2) 0.7119(2) 0.43985(14) 0.0339(8) Uani 1 1 d . . . H47 H 0.0651 0.7032 0.4826 0.041 Uiso 1 1 calc R . . H48 H 0.0621 0.6583 0.4304 0.041 Uiso 1 1 calc R . . C37 C -0.0651(3) 0.7542(2) 0.43952(16) 0.0402(9) Uani 1 1 d . . . H45 H -0.0911 0.7320 0.4805 0.048 Uiso 1 1 calc R . . H46 H -0.0835 0.8128 0.4355 0.048 Uiso 1 1 calc R . . C38 C -0.1078(2) 0.7431(2) 0.38541(16) 0.0322(8) Uani 1 1 d . . . C39 C -0.1038(3) 0.7440(2) 0.27720(17) 0.0391(9) Uani 1 1 d . . . H44 H -0.0779 0.7547 0.2357 0.047 Uiso 1 1 calc R . . C40 C -0.1756(3) 0.7147(3) 0.28596(19) 0.0474(10) Uani 1 1 d . . . H43 H -0.1965 0.7046 0.2516 0.057 Uiso 1 1 calc R . . C41 C -0.2159(3) 0.7006(3) 0.3481(2) 0.0497(10) Uani 1 1 d . . . H42 H -0.2649 0.6812 0.3559 0.060 Uiso 1 1 calc R . . C42 C -0.1823(3) 0.7158(2) 0.39718(18) 0.0397(9) Uani 1 1 d . . . H41 H -0.2094 0.7079 0.4386 0.048 Uiso 1 1 calc R . . C43 C 0.2446(2) 0.2767(3) 0.31344(16) 0.0390(9) Uani 1 1 d . . . H55 H 0.2484 0.3293 0.2915 0.047 Uiso 1 1 calc R . . H56 H 0.3077 0.2336 0.3112 0.047 Uiso 1 1 calc R . . C44 C 0.2150(3) 0.2766(2) 0.38475(16) 0.0369(8) Uani 1 1 d . . . H53 H 0.1987 0.2291 0.4045 0.044 Uiso 1 1 calc R . . H54 H 0.2688 0.2712 0.4076 0.044 Uiso 1 1 calc R . . C45 C 0.1309(2) 0.3541(2) 0.39177(14) 0.0291(7) Uani 1 1 d . . . C46 C -0.0244(3) 0.4451(2) 0.36660(16) 0.0347(8) Uani 1 1 d . . . H52 H -0.0811 0.4587 0.3464 0.042 Uiso 1 1 calc R . . C47 C -0.0200(3) 0.4986(2) 0.39973(17) 0.0425(9) Uani 1 1 d . . . H51 H -0.0723 0.5475 0.4017 0.051 Uiso 1 1 calc R . . C48 C 0.0644(3) 0.4776(2) 0.43003(16) 0.0413(9) Uani 1 1 d . . . H50 H 0.0692 0.5124 0.4529 0.050 Uiso 1 1 calc R . . C49 C 0.1404(3) 0.4060(2) 0.42633(15) 0.0332(8) Uani 1 1 d . . . H49 H 0.1975 0.3915 0.4462 0.040 Uiso 1 1 calc R . . C50 C 0.1600(2) 0.3014(2) 0.04297(15) 0.0346(8) Uani 1 1 d . . . H63 H 0.1442 0.3375 0.0000 0.042 Uiso 1 1 calc R . . H64 H 0.1361 0.2584 0.0479 0.042 Uiso 1 1 calc R . . C51 C 0.2684(2) 0.2624(2) 0.05008(15) 0.0352(8) Uani 1 1 d . . . H61 H 0.2983 0.2459 0.0106 0.042 Uiso 1 1 calc R . . H62 H 0.2898 0.3035 0.0555 0.042 Uiso 1 1 calc R . . C52 C 0.3012(2) 0.1886(2) 0.10620(15) 0.0295(7) Uani 1 1 d . . . C53 C 0.2923(3) 0.1302(2) 0.21526(17) 0.0370(8) Uani 1 1 d . . . H60 H 0.2662 0.1352 0.2563 0.044 Uiso 1 1 calc R . . C54 C 0.3594(3) 0.0544(2) 0.20819(19) 0.0467(10) Uani 1 1 d . . . H59 H 0.3789 0.0096 0.2439 0.056 Uiso 1 1 calc R . . C55 C 0.3971(3) 0.0461(2) 0.14712(19) 0.0481(10) Uani 1 1 d . . . H58 H 0.4411 -0.0048 0.1409 0.058 Uiso 1 1 calc R . . C56 C 0.3689(3) 0.1136(2) 0.09592(17) 0.0370(8) Uani 1 1 d . . . H57 H 0.3947 0.1094 0.0547 0.044 Uiso 1 1 calc R . . C57 C 0.1951(3) 0.4615(2) 0.14841(15) 0.0340(8) Uani 1 1 d . . . C58 C 0.0886(3) 0.5027(2) 0.14312(16) 0.0376(8) Uani 1 1 d . . . H67 H 0.0698 0.4888 0.1079 0.045 Uiso 1 1 calc R . . H68 H 0.0703 0.5621 0.1321 0.045 Uiso 1 1 calc R . . C59 C 0.0336(3) 0.4792(2) 0.20431(16) 0.0326(8) Uani 1 1 d . . . H65 H 0.0636 0.4787 0.2416 0.039 Uiso 1 1 calc R . . H66 H -0.0315 0.5205 0.2027 0.039 Uiso 1 1 calc R . . C60 C 0.2513(3) 0.5075(3) 0.13788(19) 0.0496(11) Uani 1 1 d . . . H72 H 0.2231 0.5649 0.1253 0.060 Uiso 1 1 calc R . . C61 C 0.3478(3) 0.4685(3) 0.1459(2) 0.0631(13) Uani 1 1 d . . . H71 H 0.3854 0.4991 0.1401 0.076 Uiso 1 1 calc R . . C62 C 0.3890(3) 0.3837(3) 0.1627(2) 0.0556(12) Uani 1 1 d . . . H70 H 0.4548 0.3560 0.1676 0.067 Uiso 1 1 calc R . . C63 C 0.3310(3) 0.3406(2) 0.17208(17) 0.0390(9) Uani 1 1 d . . . H69 H 0.3589 0.2831 0.1837 0.047 Uiso 1 1 calc R . . C64 C 0.0381(2) 0.1882(2) 0.21757(16) 0.0316(8) Uani 1 1 d . . . H79 H 0.0119 0.1678 0.2591 0.038 Uiso 1 1 calc R . . H80 H 0.1032 0.1490 0.2134 0.038 Uiso 1 1 calc R . . C65 C -0.0210(3) 0.1936(2) 0.16392(16) 0.0365(8) Uani 1 1 d . . . H77 H -0.0042 0.2258 0.1239 0.044 Uiso 1 1 calc R . . H78 H -0.0037 0.1383 0.1584 0.044 Uiso 1 1 calc R . . C66 C -0.1282(2) 0.2317(2) 0.17487(15) 0.0334(8) Uani 1 1 d . . . C67 C -0.2616(3) 0.3413(3) 0.19702(17) 0.0407(9) Uani 1 1 d . . . H76 H -0.2883 0.3940 0.2046 0.049 Uiso 1 1 calc R . . C68 C -0.3220(3) 0.3020(3) 0.1978(2) 0.0542(11) Uani 1 1 d . . . H75 H -0.3876 0.3278 0.2053 0.065 Uiso 1 1 calc R . . C69 C -0.2826(3) 0.2233(3) 0.1871(2) 0.0605(12) Uani 1 1 d . . . H74 H -0.3209 0.1945 0.1876 0.073 Uiso 1 1 calc R . . C70 C -0.1834(3) 0.1880(3) 0.17554(17) 0.0475(10) Uani 1 1 d . . . H73 H -0.1550 0.1351 0.1683 0.057 Uiso 1 1 calc R . . C71 C -0.1600(3) 0.3191(2) 0.32934(15) 0.0393(9) Uani 1 1 d . . . H87 H -0.1515 0.2713 0.3138 0.047 Uiso 1 1 calc R . . H88 H -0.2270 0.3561 0.3253 0.047 Uiso 1 1 calc R . . C72 C -0.1337(3) 0.2912(2) 0.40009(16) 0.0405(9) Uani 1 1 d . . . H85 H -0.1266 0.3359 0.4123 0.049 Uiso 1 1 calc R . . H86 H -0.1860 0.2805 0.4261 0.049 Uiso 1 1 calc R . . C73 C -0.0433(3) 0.2152(2) 0.41560(15) 0.0372(9) Uani 1 1 d . . . C74 C 0.1127(3) 0.1393(2) 0.38666(16) 0.0389(9) Uani 1 1 d . . . H84 H 0.1641 0.1339 0.3573 0.047 Uiso 1 1 calc R . . C75 C 0.1223(3) 0.0748(3) 0.44041(18) 0.0503(10) Uani 1 1 d . . . H83 H 0.1788 0.0278 0.4475 0.060 Uiso 1 1 calc R . . C76 C 0.0446(4) 0.0827(3) 0.48356(18) 0.0566(12) Uani 1 1 d . . . H82 H 0.0486 0.0412 0.5208 0.068 Uiso 1 1 calc R . . C77 C -0.0383(3) 0.1527(3) 0.47041(17) 0.0488(10) Uani 1 1 d . . . H81 H -0.0912 0.1580 0.4984 0.059 Uiso 1 1 calc R . . C78 C -0.0993(3) 0.4638(2) 0.05159(16) 0.0397(9) Uani 1 1 d . . . H95 H -0.0830 0.4570 0.0077 0.048 Uiso 1 1 calc R . . H96 H -0.0747 0.5026 0.0577 0.048 Uiso 1 1 calc R . . C79 C -0.2073(3) 0.4984(2) 0.06091(16) 0.0420(9) Uani 1 1 d . . . H93 H -0.2295 0.4544 0.0661 0.050 Uiso 1 1 calc R . . H94 H -0.2356 0.5401 0.0222 0.050 Uiso 1 1 calc R . . C80 C -0.2421(3) 0.5366(2) 0.11881(16) 0.0366(8) Uani 1 1 d . . . C81 C -0.2316(3) 0.5268(2) 0.22737(18) 0.0398(9) Uani 1 1 d . . . H92 H -0.2023 0.4976 0.2669 0.048 Uiso 1 1 calc R . . C82 C -0.3073(3) 0.6028(3) 0.2242(2) 0.0487(10) Uani 1 1 d . . . H91 H -0.3285 0.6238 0.2608 0.058 Uiso 1 1 calc R . . C83 C -0.3505(3) 0.6464(3) 0.1655(2) 0.0509(10) Uani 1 1 d . . . H90 H -0.4011 0.6977 0.1618 0.061 Uiso 1 1 calc R . . C84 C -0.3178(3) 0.6132(2) 0.11283(19) 0.0480(10) Uani 1 1 d . . . H89 H -0.3462 0.6419 0.0730 0.058 Uiso 1 1 calc R . . C85 C 0.3413(3) 0.4985(3) 0.5045(2) 0.0600(12) Uani 1 1 d . . . H97 H 0.3402 0.5360 0.4625 0.072 Uiso 1 1 calc R . . H98 H 0.3803 0.4427 0.5003 0.072 Uiso 1 1 calc R . . C86 C 0.5921(3) 0.1329(3) 0.0717(2) 0.0618(12) Uani 1 1 d . . . H99 H 0.5766 0.1325 0.0294 0.074 Uiso 1 1 calc R . . H100 H 0.5711 0.0944 0.1040 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.49438(10) 0.85102(9) 0.07230(5) 0.0734(4) Uani 1 1 d . . . Cl2 Cl 0.38892(8) 0.29461(7) 0.48797(5) 0.0526(3) Uani 1 1 d . . . Cl3 Cl 0.53082(10) 0.23282(10) 0.08487(8) 0.0919(5) Uani 1 1 d . . . Cl4 Cl 0.71685(8) 0.10086(8) 0.07587(6) 0.0639(3) Uani 1 1 d . . . Cl5 Cl 0.39243(10) 0.52247(9) 0.56103(7) 0.0784(4) Uani 1 1 d . . . Cl6 Cl 0.22450(9) 0.50635(9) 0.52848(7) 0.0772(4) Uani 1 1 d . . . H1O H 0.004(5) 0.370(4) 0.082(3) 0.14(3) Uiso 1 1 d . . . H2O H 0.186(4) 0.716(3) 0.388(2) 0.102(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0309(2) 0.0320(2) 0.0227(2) -0.00657(18) 0.00299(17) -0.01586(19) Ni2 0.0307(2) 0.0324(2) 0.0198(2) -0.00770(18) 0.00261(16) -0.01804(19) Ni3 0.0312(2) 0.0307(2) 0.0215(2) -0.00893(18) 0.00443(17) -0.01704(19) Ni4 0.0271(2) 0.0258(2) 0.0204(2) -0.00668(17) 0.00162(16) -0.01153(18) Ni5 0.0301(2) 0.0294(2) 0.01802(19) -0.00731(17) 0.00071(16) -0.01362(19) Ni6 0.0270(2) 0.0307(2) 0.0202(2) -0.00770(17) 0.00055(16) -0.01229(19) O1 0.0344(13) 0.0304(13) 0.0248(11) -0.0105(10) 0.0055(9) -0.0179(11) O2 0.0305(12) 0.0315(13) 0.0237(11) -0.0094(10) 0.0040(9) -0.0181(10) O3 0.0337(13) 0.0359(13) 0.0216(11) -0.0092(10) 0.0042(9) -0.0184(11) O4 0.0388(15) 0.0442(15) 0.0216(11) -0.0037(11) 0.0013(10) -0.0192(12) O5 0.0301(12) 0.0349(14) 0.0246(11) -0.0068(10) 0.0026(9) -0.0161(11) O6 0.0405(14) 0.0406(14) 0.0201(11) -0.0051(10) 0.0037(10) -0.0213(12) O7 0.0298(12) 0.0263(12) 0.0239(11) -0.0081(9) 0.0022(9) -0.0134(10) O8 0.0329(12) 0.0251(12) 0.0180(10) -0.0065(9) -0.0006(9) -0.0128(10) O9 0.0324(12) 0.0330(13) 0.0212(11) -0.0083(10) -0.0017(9) -0.0130(10) O10 0.0297(12) 0.0343(13) 0.0218(11) -0.0107(10) 0.0060(9) -0.0121(10) O11 0.0311(12) 0.0387(14) 0.0210(11) -0.0091(10) 0.0037(9) -0.0192(11) O12 0.0285(13) 0.0320(13) 0.0224(11) -0.0048(10) -0.0017(10) -0.0081(11) N1 0.0417(17) 0.0364(17) 0.0247(14) -0.0108(12) -0.0007(12) -0.0199(14) N2 0.0306(15) 0.0373(17) 0.0265(14) -0.0073(13) -0.0010(12) -0.0137(13) N3 0.0401(18) 0.0364(17) 0.0303(15) -0.0060(13) 0.0081(13) -0.0157(14) N4 0.0394(17) 0.0329(16) 0.0260(14) -0.0097(12) 0.0035(12) -0.0157(14) N5 0.0387(17) 0.0345(16) 0.0240(14) -0.0052(12) 0.0003(12) -0.0199(14) N6 0.0339(16) 0.0380(17) 0.0323(15) -0.0130(13) 0.0067(12) -0.0208(14) N7 0.0377(16) 0.0334(16) 0.0215(13) -0.0081(12) 0.0000(12) -0.0175(14) N8 0.0305(15) 0.0291(15) 0.0262(14) -0.0103(12) 0.0049(11) -0.0107(12) N9 0.0334(16) 0.0379(17) 0.0329(15) -0.0143(13) 0.0052(12) -0.0208(14) N10 0.0368(17) 0.0500(19) 0.0249(14) -0.0124(14) -0.0001(12) -0.0225(15) N11 0.0458(18) 0.0387(18) 0.0187(13) -0.0053(12) -0.0022(12) -0.0198(15) N12 0.0332(16) 0.0348(17) 0.0360(16) -0.0123(14) 0.0030(13) -0.0123(14) C1 0.0276(18) 0.055(2) 0.0316(18) -0.0202(17) 0.0089(14) -0.0187(17) C2 0.047(2) 0.058(3) 0.0281(18) -0.0202(18) 0.0129(16) -0.029(2) C3 0.046(2) 0.034(2) 0.0202(16) -0.0024(14) 0.0019(15) -0.0195(17) C4 0.040(2) 0.0324(19) 0.0262(16) -0.0066(15) -0.0023(14) -0.0178(16) C5 0.047(2) 0.038(2) 0.0341(19) -0.0044(16) -0.0135(16) -0.0192(18) C6 0.066(3) 0.042(2) 0.0268(18) -0.0148(17) -0.0101(18) -0.019(2) C7 0.059(3) 0.043(2) 0.0243(17) -0.0115(16) 0.0046(17) -0.020(2) C8 0.038(2) 0.055(2) 0.0230(17) -0.0051(17) -0.0023(15) -0.0161(19) C9 0.043(2) 0.055(3) 0.0284(18) -0.0009(17) -0.0036(16) -0.019(2) C10 0.0311(19) 0.047(2) 0.0301(18) -0.0075(17) -0.0056(15) -0.0095(17) C11 0.0321(19) 0.036(2) 0.0322(18) -0.0095(16) 0.0001(14) -0.0142(16) C12 0.036(2) 0.040(2) 0.042(2) -0.0066(17) 0.0016(16) -0.0205(18) C13 0.041(2) 0.071(3) 0.050(2) -0.019(2) -0.0058(19) -0.029(2) C14 0.037(2) 0.074(3) 0.037(2) -0.008(2) -0.0096(17) -0.028(2) C15 0.052(2) 0.036(2) 0.0317(19) -0.0067(16) 0.0019(17) -0.0155(19) C16 0.059(3) 0.031(2) 0.041(2) -0.0067(17) 0.0113(18) -0.0240(19) C17 0.038(2) 0.034(2) 0.042(2) -0.0166(17) 0.0082(16) -0.0229(17) C18 0.066(3) 0.032(2) 0.071(3) -0.006(2) -0.007(2) -0.013(2) C19 0.062(3) 0.047(3) 0.098(4) -0.020(3) -0.002(3) -0.005(3) C20 0.050(3) 0.053(3) 0.068(3) -0.024(2) -0.001(2) -0.011(2) C21 0.037(2) 0.043(2) 0.036(2) -0.0108(17) 0.0046(16) -0.0075(18) C22 0.039(2) 0.034(2) 0.0338(18) -0.0131(16) 0.0031(15) -0.0204(17) C23 0.053(2) 0.033(2) 0.0349(19) -0.0143(16) 0.0008(16) -0.0245(18) C24 0.052(2) 0.033(2) 0.0213(16) -0.0081(15) 0.0071(15) -0.0252(18) C25 0.040(2) 0.039(2) 0.039(2) -0.0113(17) 0.0081(16) -0.0161(18) C26 0.045(2) 0.043(2) 0.051(2) -0.011(2) 0.0072(19) -0.010(2) C27 0.064(3) 0.031(2) 0.051(2) -0.0136(19) 0.021(2) -0.015(2) C28 0.056(3) 0.039(2) 0.0276(18) -0.0109(16) 0.0111(17) -0.0256(19) C29 0.033(2) 0.041(2) 0.0355(19) -0.0035(17) 0.0032(15) -0.0162(17) C30 0.042(2) 0.043(2) 0.0294(18) -0.0067(16) -0.0061(15) -0.0149(18) C31 0.043(2) 0.036(2) 0.0192(15) -0.0073(15) 0.0001(14) -0.0156(17) C32 0.045(2) 0.039(2) 0.0274(17) -0.0045(16) 0.0016(15) -0.0250(18) C33 0.054(3) 0.054(3) 0.0347(19) -0.0097(18) 0.0055(18) -0.036(2) C34 0.067(3) 0.037(2) 0.036(2) -0.0023(17) 0.0028(19) -0.025(2) C35 0.051(2) 0.040(2) 0.0263(18) -0.0067(16) -0.0010(16) -0.0114(19) C36 0.048(2) 0.041(2) 0.0175(15) -0.0051(15) 0.0008(14) -0.0231(18) C37 0.054(2) 0.047(2) 0.0253(17) -0.0141(17) 0.0162(16) -0.0266(19) C38 0.0289(18) 0.0318(19) 0.0323(18) -0.0062(15) 0.0084(14) -0.0118(15) C39 0.040(2) 0.046(2) 0.040(2) -0.0156(18) 0.0050(16) -0.0240(19) C40 0.050(2) 0.058(3) 0.047(2) -0.003(2) -0.0094(18) -0.036(2) C41 0.033(2) 0.050(3) 0.062(3) 0.007(2) -0.0025(19) -0.025(2) C42 0.032(2) 0.042(2) 0.040(2) -0.0022(17) 0.0043(16) -0.0161(17) C43 0.0277(19) 0.054(2) 0.0374(19) -0.0192(18) -0.0052(15) -0.0119(18) C44 0.038(2) 0.042(2) 0.0318(18) -0.0109(16) -0.0089(15) -0.0130(17) C45 0.0369(19) 0.038(2) 0.0169(15) -0.0035(14) -0.0018(13) -0.0204(16) C46 0.039(2) 0.037(2) 0.0310(18) -0.0112(16) -0.0032(15) -0.0152(17) C47 0.056(3) 0.040(2) 0.038(2) -0.0213(18) 0.0085(18) -0.0205(19) C48 0.063(3) 0.046(2) 0.0325(19) -0.0145(17) 0.0064(18) -0.037(2) C49 0.043(2) 0.045(2) 0.0243(16) -0.0105(16) -0.0003(15) -0.0283(18) C50 0.039(2) 0.041(2) 0.0241(17) -0.0125(15) 0.0041(14) -0.0139(17) C51 0.036(2) 0.042(2) 0.0280(17) -0.0126(16) 0.0105(15) -0.0158(17) C52 0.0287(18) 0.035(2) 0.0302(17) -0.0121(15) 0.0025(14) -0.0165(16) C53 0.039(2) 0.031(2) 0.0334(19) -0.0048(16) -0.0008(15) -0.0077(17) C54 0.052(2) 0.030(2) 0.046(2) -0.0057(18) -0.0039(18) -0.0061(18) C55 0.047(2) 0.038(2) 0.055(3) -0.024(2) -0.0021(19) -0.0043(19) C56 0.037(2) 0.039(2) 0.0361(19) -0.0153(17) 0.0038(16) -0.0133(17) C57 0.048(2) 0.033(2) 0.0259(17) -0.0121(15) 0.0055(15) -0.0190(17) C58 0.053(2) 0.0301(19) 0.0301(18) -0.0013(15) -0.0004(16) -0.0199(18) C59 0.037(2) 0.0281(19) 0.0332(18) -0.0081(15) 0.0001(15) -0.0134(16) C60 0.061(3) 0.052(3) 0.050(2) -0.023(2) 0.023(2) -0.037(2) C61 0.058(3) 0.064(3) 0.096(4) -0.041(3) 0.023(3) -0.046(3) C62 0.036(2) 0.075(3) 0.070(3) -0.033(3) 0.012(2) -0.030(2) C63 0.035(2) 0.047(2) 0.041(2) -0.0169(18) 0.0047(16) -0.0190(18) C64 0.038(2) 0.0250(18) 0.0352(18) -0.0086(15) 0.0012(15) -0.0149(16) C65 0.050(2) 0.036(2) 0.0319(18) -0.0174(16) 0.0016(16) -0.0201(18) C66 0.043(2) 0.049(2) 0.0216(16) -0.0125(16) -0.0013(14) -0.0289(18) C67 0.031(2) 0.055(3) 0.044(2) -0.0179(19) 0.0019(16) -0.0223(19) C68 0.041(2) 0.078(3) 0.053(2) -0.020(2) 0.0009(19) -0.032(2) C69 0.062(3) 0.086(4) 0.060(3) -0.019(3) -0.006(2) -0.053(3) C70 0.059(3) 0.057(3) 0.040(2) -0.0109(19) -0.0023(19) -0.036(2) C71 0.036(2) 0.057(3) 0.0291(18) -0.0140(18) 0.0049(15) -0.0219(19) C72 0.045(2) 0.055(2) 0.0260(17) -0.0132(17) 0.0101(16) -0.025(2) C73 0.056(2) 0.049(2) 0.0208(16) -0.0141(16) 0.0048(16) -0.033(2) C74 0.054(2) 0.045(2) 0.0265(18) -0.0065(17) -0.0002(16) -0.029(2) C75 0.077(3) 0.040(2) 0.041(2) -0.0068(19) -0.018(2) -0.028(2) C76 0.109(4) 0.048(3) 0.0263(19) -0.0006(18) -0.006(2) -0.048(3) C77 0.078(3) 0.052(3) 0.0259(19) -0.0111(18) 0.0070(19) -0.037(2) C78 0.036(2) 0.046(2) 0.0246(17) -0.0006(16) -0.0002(15) -0.0080(18) C79 0.042(2) 0.045(2) 0.0283(18) -0.0013(17) -0.0067(16) -0.0093(18) C80 0.036(2) 0.035(2) 0.0336(19) -0.0022(16) -0.0017(15) -0.0122(17) C81 0.039(2) 0.046(2) 0.039(2) -0.0178(18) 0.0038(16) -0.0175(18) C82 0.038(2) 0.049(3) 0.064(3) -0.034(2) 0.015(2) -0.015(2) C83 0.042(2) 0.037(2) 0.062(3) -0.009(2) 0.005(2) -0.0079(19) C84 0.045(2) 0.039(2) 0.045(2) -0.0003(18) 0.0001(18) -0.0068(19) C85 0.049(3) 0.073(3) 0.063(3) -0.030(3) 0.008(2) -0.023(2) C86 0.051(3) 0.067(3) 0.077(3) -0.023(3) -0.011(2) -0.026(2) Cl1 0.1030(10) 0.0860(9) 0.0447(6) -0.0119(6) 0.0075(6) -0.0552(8) Cl2 0.0563(6) 0.0594(7) 0.0467(5) -0.0068(5) -0.0134(5) -0.0272(5) Cl3 0.0649(9) 0.1022(12) 0.1140(12) -0.0597(10) 0.0095(8) -0.0203(8) Cl4 0.0482(6) 0.0723(8) 0.0698(7) -0.0181(6) -0.0056(5) -0.0203(6) Cl5 0.0684(8) 0.0826(10) 0.0852(9) -0.0256(8) -0.0222(7) -0.0211(7) Cl6 0.0563(7) 0.0834(9) 0.1018(10) -0.0388(8) 0.0046(7) -0.0286(7) _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 O3 2.040(2) . ? Ni1 O4 2.047(2) . ? Ni1 O1 2.085(2) . ? Ni1 N3 2.115(3) . ? Ni1 O2 2.127(2) . ? Ni1 N2 2.136(3) . ? Ni1 Ni2 2.8079(6) . ? Ni1 Ni3 3.3005(6) . ? Ni2 O3 1.980(2) . ? Ni2 O5 1.997(2) . ? Ni2 N5 2.096(3) . ? Ni2 N1 2.113(2) . ? Ni2 O2 2.1394(19) . ? Ni2 O1 2.142(2) . ? Ni2 Ni3 2.8194(5) . ? Ni3 O6 2.027(2) . ? Ni3 O5 2.060(2) . ? Ni3 O2 2.097(2) . ? Ni3 O1 2.111(2) . ? Ni3 N4 2.117(3) . ? Ni3 N6 2.141(3) . ? Ni4 O9 2.045(2) . ? Ni4 O10 2.046(2) . ? Ni4 O7 2.094(2) . ? Ni4 N9 2.104(3) . ? Ni4 O8 2.114(2) . ? Ni4 N8 2.119(3) . ? Ni4 Ni5 2.8144(5) . ? Ni4 Ni6 3.2950(6) . ? Ni5 O9 1.994(2) . ? Ni5 O11 2.001(2) . ? Ni5 N7 2.094(2) . ? Ni5 N11 2.101(3) . ? Ni5 O8 2.1359(18) . ? Ni5 O7 2.141(2) . ? Ni5 Ni6 2.8246(6) . ? Ni6 O12 2.031(2) . ? Ni6 O11 2.0517(19) . ? Ni6 O8 2.084(2) . ? Ni6 N10 2.114(3) . ? Ni6 O7 2.121(2) . ? Ni6 N12 2.150(3) . ? O1 C17 1.404(4) . ? O2 C22 1.409(4) . ? O3 C1 1.401(4) . ? O4 C8 1.406(4) . ? O4 H2O 0.98(6) . ? O5 C29 1.390(4) . ? O6 C36 1.414(4) . ? O7 C59 1.411(4) . ? O8 C64 1.407(4) . ? O9 C43 1.398(4) . ? O10 C50 1.404(3) . ? O11 C71 1.408(4) . ? O12 C78 1.412(4) . ? O12 H1O 0.87(7) . ? N1 C4 1.332(4) . ? N1 C3 1.362(4) . ? N2 C11 1.348(4) . ? N2 C10 1.355(4) . ? N3 C15 1.344(5) . ? N3 C21 1.345(5) . ? N4 C25 1.344(5) . ? N4 C24 1.350(4) . ? N5 C32 1.343(4) . ? N5 C31 1.351(4) . ? N6 C39 1.347(4) . ? N6 C38 1.351(4) . ? N7 C45 1.337(4) . ? N7 C46 1.347(4) . ? N8 C52 1.346(4) . ? N8 C53 1.351(4) . ? N9 C63 1.346(4) . ? N9 C57 1.351(4) . ? N10 C67 1.331(4) . ? N10 C66 1.354(4) . ? N11 C74 1.325(5) . ? N11 C73 1.374(4) . ? N12 C81 1.351(4) . ? N12 C80 1.353(4) . ? C1 C2 1.520(5) . ? C1 H7 0.9700 . ? C1 H8 0.9700 . ? C2 C3 1.508(5) . ? C2 H5 0.9700 . ? C2 H6 0.9700 . ? C3 C7 1.391(4) . ? C4 C5 1.385(4) . ? C4 H4 0.9300 . ? C5 C6 1.398(5) . ? C5 H3 0.9300 . ? C6 C7 1.366(5) . ? C6 H2 0.9300 . ? C7 H1 0.9300 . ? C8 C9 1.510(5) . ? C8 H15 0.9700 . ? C8 H16 0.9700 . ? C9 C10 1.516(5) . ? C9 H13 0.9700 . ? C9 H14 0.9700 . ? C10 C14 1.384(5) . ? C11 C12 1.357(5) . ? C11 H12 0.9300 . ? C12 C13 1.372(5) . ? C12 H11 0.9300 . ? C13 C14 1.369(5) . ? C13 H10 0.9300 . ? C14 H9 0.9300 . ? C15 C18 1.375(5) . ? C15 C16 1.522(5) . ? C16 C17 1.505(5) . ? C16 H19 0.9700 . ? C16 H20 0.9700 . ? C17 H17 0.9700 . ? C17 H18 0.9700 . ? C18 C19 1.355(7) . ? C18 H24 0.9300 . ? C19 C20 1.392(7) . ? C19 H23 0.9300 . ? C20 C21 1.368(6) . ? C20 H22 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.521(4) . ? C22 H31 0.9700 . ? C22 H32 0.9700 . ? C23 C24 1.499(5) . ? C23 H29 0.9700 . ? C23 H30 0.9700 . ? C24 C28 1.393(5) . ? C25 C26 1.380(5) . ? C25 H28 0.9300 . ? C26 C27 1.403(6) . ? C26 H27 0.9300 . ? C27 C28 1.353(6) . ? C27 H26 0.9300 . ? C28 H25 0.9300 . ? C29 C30 1.521(5) . ? C29 H39 0.9700 . ? C29 H40 0.9700 . ? C30 C31 1.495(5) . ? C30 H37 0.9700 . ? C30 H38 0.9700 . ? C31 C35 1.385(5) . ? C32 C33 1.401(5) . ? C32 H36 0.9300 . ? C33 C34 1.384(6) . ? C33 H35 0.9300 . ? C34 C35 1.378(5) . ? C34 H34 0.9300 . ? C35 H33 0.9300 . ? C36 C37 1.509(5) . ? C36 H47 0.9700 . ? C36 H48 0.9700 . ? C37 C38 1.500(5) . ? C37 H45 0.9700 . ? C37 H46 0.9700 . ? C38 C42 1.390(5) . ? C39 C40 1.377(5) . ? C39 H44 0.9300 . ? C40 C41 1.397(5) . ? C40 H43 0.9300 . ? C41 C42 1.367(5) . ? C41 H42 0.9300 . ? C42 H41 0.9300 . ? C43 C44 1.537(4) . ? C43 H55 0.9700 . ? C43 H56 0.9700 . ? C44 C45 1.503(5) . ? C44 H53 0.9700 . ? C44 H54 0.9700 . ? C45 C49 1.410(4) . ? C46 C47 1.381(5) . ? C46 H52 0.9300 . ? C47 C48 1.386(5) . ? C47 H51 0.9300 . ? C48 C49 1.363(5) . ? C48 H50 0.9300 . ? C49 H49 0.9300 . ? C50 C51 1.525(5) . ? C50 H63 0.9700 . ? C50 H64 0.9700 . ? C51 C52 1.499(5) . ? C51 H61 0.9700 . ? C51 H62 0.9700 . ? C52 C56 1.394(5) . ? C53 C54 1.380(5) . ? C53 H60 0.9300 . ? C54 C55 1.382(5) . ? C54 H59 0.9300 . ? C55 C56 1.367(5) . ? C55 H58 0.9300 . ? C56 H57 0.9300 . ? C57 C60 1.390(5) . ? C57 C58 1.495(5) . ? C58 C59 1.521(4) . ? C58 H67 0.9700 . ? C58 H68 0.9700 . ? C59 H65 0.9700 . ? C59 H66 0.9700 . ? C60 C61 1.362(6) . ? C60 H72 0.9300 . ? C61 C62 1.373(6) . ? C61 H71 0.9300 . ? C62 C63 1.372(5) . ? C62 H70 0.9300 . ? C63 H69 0.9300 . ? C64 C65 1.515(5) . ? C64 H79 0.9700 . ? C64 H80 0.9700 . ? C65 C66 1.511(5) . ? C65 H77 0.9700 . ? C65 H78 0.9700 . ? C66 C70 1.375(5) . ? C67 C68 1.378(5) . ? C67 H76 0.9300 . ? C68 C69 1.384(6) . ? C68 H75 0.9300 . ? C69 C70 1.403(6) . ? C69 H74 0.9300 . ? C70 H73 0.9300 . ? C71 C72 1.517(5) . ? C71 H87 0.9700 . ? C71 H88 0.9700 . ? C72 C73 1.500(5) . ? C72 H85 0.9700 . ? C72 H86 0.9700 . ? C73 C77 1.385(5) . ? C74 C75 1.381(5) . ? C74 H84 0.9300 . ? C75 C76 1.390(6) . ? C75 H83 0.9300 . ? C76 C77 1.377(6) . ? C76 H82 0.9300 . ? C77 H81 0.9300 . ? C78 C79 1.515(5) . ? C78 H95 0.9700 . ? C78 H96 0.9700 . ? C79 C80 1.518(5) . ? C79 H93 0.9700 . ? C79 H94 0.9700 . ? C80 C84 1.390(5) . ? C81 C82 1.389(5) . ? C81 H92 0.9300 . ? C82 C83 1.380(6) . ? C82 H91 0.9300 . ? C83 C84 1.367(5) . ? C83 H90 0.9300 . ? C84 H89 0.9300 . ? C85 Cl6 1.751(4) . ? C85 Cl5 1.759(4) . ? C85 H97 0.9700 . ? C85 H98 0.9700 . ? C86 Cl3 1.759(5) . ? C86 Cl4 1.760(4) . ? C86 H99 0.9700 . ? C86 H100 0.9700 . ? 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 O3 Ni1 O4 176.39(10) . . ? O3 Ni1 O1 84.88(8) . . ? O4 Ni1 O1 92.77(9) . . ? O3 Ni1 N3 95.64(10) . . ? O4 Ni1 N3 87.22(10) . . ? O1 Ni1 N3 93.17(10) . . ? O3 Ni1 O2 81.86(8) . . ? O4 Ni1 O2 94.76(9) . . ? O1 Ni1 O2 69.73(8) . . ? N3 Ni1 O2 162.85(10) . . ? O3 Ni1 N2 91.38(9) . . ? O4 Ni1 N2 90.54(10) . . ? O1 Ni1 N2 170.65(10) . . ? N3 Ni1 N2 95.72(11) . . ? O2 Ni1 N2 101.29(9) . . ? O3 Ni1 Ni2 44.83(6) . . ? O4 Ni1 Ni2 131.70(7) . . ? O1 Ni1 Ni2 49.26(6) . . ? N3 Ni1 Ni2 118.57(8) . . ? O2 Ni1 Ni2 49.03(5) . . ? N2 Ni1 Ni2 123.01(8) . . ? O3 Ni1 Ni3 99.02(6) . . ? O4 Ni1 Ni3 77.47(7) . . ? O1 Ni1 Ni3 38.42(5) . . ? N3 Ni1 Ni3 126.65(8) . . ? O2 Ni1 Ni3 38.29(5) . . ? N2 Ni1 Ni3 134.53(7) . . ? Ni2 Ni1 Ni3 54.251(12) . . ? O3 Ni2 O5 165.14(9) . . ? O3 Ni2 N5 96.69(10) . . ? O5 Ni2 N5 93.96(10) . . ? O3 Ni2 N1 92.59(10) . . ? O5 Ni2 N1 97.28(10) . . ? N5 Ni2 N1 92.52(10) . . ? O3 Ni2 O2 82.95(8) . . ? O5 Ni2 O2 85.37(8) . . ? N5 Ni2 O2 97.72(9) . . ? N1 Ni2 O2 169.23(10) . . ? O3 Ni2 O1 84.85(9) . . ? O5 Ni2 O1 82.32(9) . . ? N5 Ni2 O1 165.85(9) . . ? N1 Ni2 O1 101.48(9) . . ? O2 Ni2 O1 68.44(8) . . ? O3 Ni2 Ni1 46.58(6) . . ? O5 Ni2 Ni1 118.56(6) . . ? N5 Ni2 Ni1 125.48(8) . . ? N1 Ni2 Ni1 121.88(8) . . ? O2 Ni2 Ni1 48.65(6) . . ? O1 Ni2 Ni1 47.50(6) . . ? O3 Ni2 Ni3 118.31(6) . . ? O5 Ni2 Ni3 46.90(6) . . ? N5 Ni2 Ni3 120.52(7) . . ? N1 Ni2 Ni3 128.50(8) . . ? O2 Ni2 Ni3 47.64(5) . . ? O1 Ni2 Ni3 48.02(5) . . ? Ni1 Ni2 Ni3 71.820(15) . . ? O6 Ni3 O5 175.71(9) . . ? O6 Ni3 O2 92.20(8) . . ? O5 Ni3 O2 84.93(8) . . ? O6 Ni3 O1 94.39(9) . . ? O5 Ni3 O1 81.63(8) . . ? O2 Ni3 O1 69.80(8) . . ? O6 Ni3 N4 89.45(10) . . ? O5 Ni3 N4 93.89(10) . . ? O2 Ni3 N4 93.18(9) . . ? O1 Ni3 N4 162.65(10) . . ? O6 Ni3 N6 90.26(10) . . ? O5 Ni3 N6 92.12(10) . . ? O2 Ni3 N6 171.17(9) . . ? O1 Ni3 N6 101.56(9) . . ? N4 Ni3 N6 95.33(10) . . ? O6 Ni3 Ni2 130.78(7) . . ? O5 Ni3 Ni2 45.08(6) . . ? O2 Ni3 Ni2 48.92(5) . . ? O1 Ni3 Ni2 48.96(6) . . ? N4 Ni3 Ni2 117.19(7) . . ? N6 Ni3 Ni2 124.13(7) . . ? O6 Ni3 Ni1 76.91(6) . . ? O5 Ni3 Ni1 98.89(6) . . ? O2 Ni3 Ni1 38.94(6) . . ? O1 Ni3 Ni1 37.85(6) . . ? N4 Ni3 Ni1 127.89(8) . . ? N6 Ni3 Ni1 134.01(8) . . ? Ni2 Ni3 Ni1 53.929(13) . . ? O9 Ni4 O10 175.61(8) . . ? O9 Ni4 O7 85.59(8) . . ? O10 Ni4 O7 92.26(8) . . ? O9 Ni4 N9 95.19(10) . . ? O10 Ni4 N9 88.73(10) . . ? O7 Ni4 N9 92.86(9) . . ? O9 Ni4 O8 81.14(8) . . ? O10 Ni4 O8 94.53(8) . . ? O7 Ni4 O8 69.58(8) . . ? N9 Ni4 O8 162.22(9) . . ? O9 Ni4 N8 91.34(9) . . ? O10 Ni4 N8 90.19(9) . . ? O7 Ni4 N8 170.57(9) . . ? N9 Ni4 N8 96.30(10) . . ? O8 Ni4 N8 101.16(9) . . ? O9 Ni4 Ni5 45.09(6) . . ? O10 Ni4 Ni5 131.03(6) . . ? O7 Ni4 Ni5 49.06(6) . . ? N9 Ni4 Ni5 117.38(7) . . ? O8 Ni4 Ni5 48.86(5) . . ? N8 Ni4 Ni5 123.65(7) . . ? O9 Ni4 Ni6 99.31(6) . . ? O10 Ni4 Ni6 76.69(6) . . ? O7 Ni4 Ni6 38.88(6) . . ? N9 Ni4 Ni6 127.13(8) . . ? O8 Ni4 Ni6 37.97(6) . . ? N8 Ni4 Ni6 133.51(7) . . ? Ni5 Ni4 Ni6 54.389(12) . . ? O9 Ni5 O11 164.41(8) . . ? O9 Ni5 N7 92.31(9) . . ? O11 Ni5 N7 98.43(10) . . ? O9 Ni5 N11 97.43(10) . . ? O11 Ni5 N11 93.09(10) . . ? N7 Ni5 N11 93.87(10) . . ? O9 Ni5 O8 81.78(8) . . ? O11 Ni5 O8 84.96(8) . . ? N7 Ni5 O8 164.55(9) . . ? N11 Ni5 O8 101.02(9) . . ? O9 Ni5 O7 85.63(8) . . ? O11 Ni5 O7 81.88(8) . . ? N7 Ni5 O7 97.13(9) . . ? N11 Ni5 O7 168.47(9) . . ? O8 Ni5 O7 68.31(8) . . ? O9 Ni5 Ni4 46.58(6) . . ? O11 Ni5 Ni4 117.90(6) . . ? N7 Ni5 Ni4 118.25(7) . . ? N11 Ni5 Ni4 128.57(8) . . ? O8 Ni5 Ni4 48.20(5) . . ? O7 Ni5 Ni4 47.64(5) . . ? O9 Ni5 Ni6 117.86(6) . . ? O11 Ni5 Ni6 46.56(6) . . ? N7 Ni5 Ni6 126.64(8) . . ? N11 Ni5 Ni6 121.45(8) . . ? O8 Ni5 Ni6 47.20(6) . . ? O7 Ni5 Ni6 48.20(6) . . ? Ni4 Ni5 Ni6 71.510(14) . . ? O12 Ni6 O11 176.96(9) . . ? O12 Ni6 O8 93.41(8) . . ? O11 Ni6 O8 85.05(8) . . ? O12 Ni6 N10 88.38(9) . . ? O11 Ni6 N10 94.31(9) . . ? O8 Ni6 N10 93.11(10) . . ? O12 Ni6 O7 95.83(8) . . ? O11 Ni6 O7 81.18(8) . . ? O8 Ni6 O7 69.63(8) . . ? N10 Ni6 O7 162.39(10) . . ? O12 Ni6 N12 90.60(10) . . ? O11 Ni6 N12 90.55(10) . . ? O8 Ni6 N12 170.62(9) . . ? N10 Ni6 N12 95.48(11) . . ? O7 Ni6 N12 101.54(9) . . ? O12 Ni6 Ni5 132.22(7) . . ? O11 Ni6 Ni5 45.08(6) . . ? O8 Ni6 Ni5 48.77(5) . . ? N10 Ni6 Ni5 117.11(8) . . ? O7 Ni6 Ni5 48.79(6) . . ? N12 Ni6 Ni5 123.14(7) . . ? O12 Ni6 Ni4 78.17(7) . . ? O11 Ni6 Ni4 99.05(6) . . ? O8 Ni6 Ni4 38.62(6) . . ? N10 Ni6 Ni4 127.30(8) . . ? O7 Ni6 Ni4 38.29(5) . . ? N12 Ni6 Ni4 134.76(8) . . ? Ni5 Ni6 Ni4 54.100(12) . . ? C17 O1 Ni1 117.4(2) . . ? C17 O1 Ni3 129.92(19) . . ? Ni1 O1 Ni3 103.72(8) . . ? C17 O1 Ni2 126.91(18) . . ? Ni1 O1 Ni2 83.24(7) . . ? Ni3 O1 Ni2 83.02(8) . . ? C22 O2 Ni3 119.91(18) . . ? C22 O2 Ni1 128.5(2) . . ? Ni3 O2 Ni1 102.77(9) . . ? C22 O2 Ni2 127.10(19) . . ? Ni3 O2 Ni2 83.43(7) . . ? Ni1 O2 Ni2 82.32(7) . . ? C1 O3 Ni2 121.02(19) . . ? C1 O3 Ni1 124.9(2) . . ? Ni2 O3 Ni1 88.59(8) . . ? C8 O4 Ni1 119.8(2) . . ? C8 O4 H2O 108(3) . . ? Ni1 O4 H2O 103(3) . . ? C29 O5 Ni2 121.02(19) . . ? C29 O5 Ni3 123.56(19) . . ? Ni2 O5 Ni3 88.02(9) . . ? C36 O6 Ni3 120.76(19) . . ? C36 O6 H2O 112(2) . . ? Ni3 O6 H2O 104(2) . . ? C59 O7 Ni4 119.46(18) . . ? C59 O7 Ni6 128.3(2) . . ? Ni4 O7 Ni6 102.82(8) . . ? C59 O7 Ni5 127.54(18) . . ? Ni4 O7 Ni5 83.29(8) . . ? Ni6 O7 Ni5 83.02(7) . . ? C64 O8 Ni6 120.35(19) . . ? C64 O8 Ni4 128.14(19) . . ? Ni6 O8 Ni4 103.41(9) . . ? C64 O8 Ni5 125.24(18) . . ? Ni6 O8 Ni5 84.03(7) . . ? Ni4 O8 Ni5 82.93(7) . . ? C43 O9 Ni5 123.42(18) . . ? C43 O9 Ni4 125.8(2) . . ? Ni5 O9 Ni4 88.33(9) . . ? C50 O10 Ni4 123.6(2) . . ? C71 O11 Ni5 119.7(2) . . ? C71 O11 Ni6 124.48(18) . . ? Ni5 O11 Ni6 88.37(8) . . ? C78 O12 Ni6 121.20(19) . . ? C78 O12 H1O 103(4) . . ? Ni6 O12 H1O 119(4) . . ? C4 N1 C3 118.1(3) . . ? C4 N1 Ni2 119.2(2) . . ? C3 N1 Ni2 122.4(2) . . ? C11 N2 C10 117.0(3) . . ? C11 N2 Ni1 116.6(2) . . ? C10 N2 Ni1 126.4(2) . . ? C15 N3 C21 118.0(3) . . ? C15 N3 Ni1 121.7(2) . . ? C21 N3 Ni1 119.8(2) . . ? C25 N4 C24 118.8(3) . . ? C25 N4 Ni3 120.0(2) . . ? C24 N4 Ni3 121.0(2) . . ? C32 N5 C31 119.3(3) . . ? C32 N5 Ni2 118.0(2) . . ? C31 N5 Ni2 122.4(2) . . ? C39 N6 C38 117.9(3) . . ? C39 N6 Ni3 117.5(2) . . ? C38 N6 Ni3 124.6(2) . . ? C45 N7 C46 118.6(3) . . ? C45 N7 Ni5 122.9(2) . . ? C46 N7 Ni5 118.0(2) . . ? C52 N8 C53 117.5(3) . . ? C52 N8 Ni4 125.1(2) . . ? C53 N8 Ni4 117.2(2) . . ? C63 N9 C57 118.5(3) . . ? C63 N9 Ni4 119.6(2) . . ? C57 N9 Ni4 121.8(2) . . ? C67 N10 C66 118.3(3) . . ? C67 N10 Ni6 119.6(2) . . ? C66 N10 Ni6 122.1(2) . . ? C74 N11 C73 118.3(3) . . ? C74 N11 Ni5 119.6(2) . . ? C73 N11 Ni5 121.7(3) . . ? C81 N12 C80 117.4(3) . . ? C81 N12 Ni6 116.8(3) . . ? C80 N12 Ni6 125.8(2) . . ? O3 C1 C2 111.7(3) . . ? O3 C1 H7 109.3 . . ? C2 C1 H7 109.3 . . ? O3 C1 H8 109.3 . . ? C2 C1 H8 109.3 . . ? H7 C1 H8 107.9 . . ? C3 C2 C1 114.8(3) . . ? C3 C2 H5 108.6 . . ? C1 C2 H5 108.6 . . ? C3 C2 H6 108.6 . . ? C1 C2 H6 108.6 . . ? H5 C2 H6 107.5 . . ? N1 C3 C7 120.3(3) . . ? N1 C3 C2 118.0(3) . . ? C7 C3 C2 121.7(3) . . ? N1 C4 C5 124.7(3) . . ? N1 C4 H4 117.6 . . ? C5 C4 H4 117.6 . . ? C4 C5 C6 116.9(3) . . ? C4 C5 H3 121.6 . . ? C6 C5 H3 121.6 . . ? C7 C6 C5 119.1(3) . . ? C7 C6 H2 120.5 . . ? C5 C6 H2 120.5 . . ? C6 C7 C3 120.9(3) . . ? C6 C7 H1 119.5 . . ? C3 C7 H1 119.5 . . ? O4 C8 C9 111.7(3) . . ? O4 C8 H15 109.3 . . ? C9 C8 H15 109.3 . . ? O4 C8 H16 109.3 . . ? C9 C8 H16 109.3 . . ? H15 C8 H16 108.0 . . ? C8 C9 C10 113.9(3) . . ? C8 C9 H13 108.8 . . ? C10 C9 H13 108.8 . . ? C8 C9 H14 108.8 . . ? C10 C9 H14 108.8 . . ? H13 C9 H14 107.7 . . ? N2 C10 C14 121.8(3) . . ? N2 C10 C9 118.2(3) . . ? C14 C10 C9 120.1(3) . . ? N2 C11 C12 123.9(3) . . ? N2 C11 H12 118.1 . . ? C12 C11 H12 118.1 . . ? C11 C12 C13 118.7(3) . . ? C11 C12 H11 120.6 . . ? C13 C12 H11 120.6 . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H10 120.3 . . ? C12 C13 H10 120.3 . . ? C13 C14 C10 119.3(3) . . ? C13 C14 H9 120.3 . . ? C10 C14 H9 120.3 . . ? N3 C15 C18 120.7(4) . . ? N3 C15 C16 118.5(3) . . ? C18 C15 C16 120.9(4) . . ? C17 C16 C15 115.9(3) . . ? C17 C16 H19 108.3 . . ? C15 C16 H19 108.3 . . ? C17 C16 H20 108.3 . . ? C15 C16 H20 108.3 . . ? H19 C16 H20 107.4 . . ? O1 C17 C16 113.8(3) . . ? O1 C17 H17 108.8 . . ? C16 C17 H17 108.8 . . ? O1 C17 H18 108.8 . . ? C16 C17 H18 108.8 . . ? H17 C17 H18 107.7 . . ? C19 C18 C15 121.0(4) . . ? C19 C18 H24 119.5 . . ? C15 C18 H24 119.5 . . ? C18 C19 C20 119.1(5) . . ? C18 C19 H23 120.4 . . ? C20 C19 H23 120.4 . . ? C21 C20 C19 117.2(4) . . ? C21 C20 H22 121.4 . . ? C19 C20 H22 121.4 . . ? N3 C21 C20 123.9(4) . . ? N3 C21 H21 118.0 . . ? C20 C21 H21 118.0 . . ? O2 C22 C23 111.8(3) . . ? O2 C22 H31 109.3 . . ? C23 C22 H31 109.3 . . ? O2 C22 H32 109.3 . . ? C23 C22 H32 109.3 . . ? H31 C22 H32 107.9 . . ? C24 C23 C22 114.5(3) . . ? C24 C23 H29 108.6 . . ? C22 C23 H29 108.6 . . ? C24 C23 H30 108.6 . . ? C22 C23 H30 108.6 . . ? H29 C23 H30 107.6 . . ? N4 C24 C28 119.7(3) . . ? N4 C24 C23 119.0(3) . . ? C28 C24 C23 121.3(3) . . ? N4 C25 C26 124.2(4) . . ? N4 C25 H28 117.9 . . ? C26 C25 H28 117.9 . . ? C25 C26 C27 116.3(4) . . ? C25 C26 H27 121.8 . . ? C27 C26 H27 121.8 . . ? C28 C27 C26 119.8(4) . . ? C28 C27 H26 120.1 . . ? C26 C27 H26 120.1 . . ? C27 C28 C24 121.1(4) . . ? C27 C28 H25 119.4 . . ? C24 C28 H25 119.4 . . ? O5 C29 C30 112.7(3) . . ? O5 C29 H39 109.1 . . ? C30 C29 H39 109.1 . . ? O5 C29 H40 109.1 . . ? C30 C29 H40 109.1 . . ? H39 C29 H40 107.8 . . ? C31 C30 C29 113.8(3) . . ? C31 C30 H37 108.8 . . ? C29 C30 H37 108.8 . . ? C31 C30 H38 108.8 . . ? C29 C30 H38 108.8 . . ? H37 C30 H38 107.7 . . ? N5 C31 C35 120.4(3) . . ? N5 C31 C30 118.3(3) . . ? C35 C31 C30 121.2(3) . . ? N5 C32 C33 122.4(4) . . ? N5 C32 H36 118.8 . . ? C33 C32 H36 118.8 . . ? C34 C33 C32 118.2(4) . . ? C34 C33 H35 120.9 . . ? C32 C33 H35 120.9 . . ? C35 C34 C33 118.8(4) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C31 120.8(4) . . ? C34 C35 H33 119.6 . . ? C31 C35 H33 119.6 . . ? O6 C36 C37 111.3(3) . . ? O6 C36 H47 109.4 . . ? C37 C36 H47 109.4 . . ? O6 C36 H48 109.4 . . ? C37 C36 H48 109.4 . . ? H47 C36 H48 108.0 . . ? C38 C37 C36 112.7(3) . . ? C38 C37 H45 109.1 . . ? C36 C37 H45 109.1 . . ? C38 C37 H46 109.1 . . ? C36 C37 H46 109.1 . . ? H45 C37 H46 107.8 . . ? N6 C38 C42 121.3(3) . . ? N6 C38 C37 117.6(3) . . ? C42 C38 C37 121.0(3) . . ? N6 C39 C40 123.7(3) . . ? N6 C39 H44 118.2 . . ? C40 C39 H44 118.2 . . ? C39 C40 C41 118.0(4) . . ? C39 C40 H43 121.0 . . ? C41 C40 H43 121.0 . . ? C42 C41 C40 118.9(3) . . ? C42 C41 H42 120.6 . . ? C40 C41 H42 120.6 . . ? C41 C42 C38 120.2(3) . . ? C41 C42 H41 119.9 . . ? C38 C42 H41 119.9 . . ? O9 C43 C44 112.0(3) . . ? O9 C43 H55 109.2 . . ? C44 C43 H55 109.2 . . ? O9 C43 H56 109.2 . . ? C44 C43 H56 109.2 . . ? H55 C43 H56 107.9 . . ? C45 C44 C43 112.0(3) . . ? C45 C44 H53 109.2 . . ? C43 C44 H53 109.2 . . ? C45 C44 H54 109.2 . . ? C43 C44 H54 109.2 . . ? H53 C44 H54 107.9 . . ? N7 C45 C49 121.6(3) . . ? N7 C45 C44 118.6(3) . . ? C49 C45 C44 119.7(3) . . ? N7 C46 C47 122.8(3) . . ? N7 C46 H52 118.6 . . ? C47 C46 H52 118.6 . . ? C46 C47 C48 118.2(4) . . ? C46 C47 H51 120.9 . . ? C48 C47 H51 120.9 . . ? C49 C48 C47 120.0(3) . . ? C49 C48 H50 120.0 . . ? C47 C48 H50 120.0 . . ? C48 C49 C45 118.8(3) . . ? C48 C49 H49 120.6 . . ? C45 C49 H49 120.6 . . ? O10 C50 C51 110.7(3) . . ? O10 C50 H63 109.5 . . ? C51 C50 H63 109.5 . . ? O10 C50 H64 109.5 . . ? C51 C50 H64 109.5 . . ? H63 C50 H64 108.1 . . ? C52 C51 C50 113.2(3) . . ? C52 C51 H61 108.9 . . ? C50 C51 H61 108.9 . . ? C52 C51 H62 108.9 . . ? C50 C51 H62 108.9 . . ? H61 C51 H62 107.7 . . ? N8 C52 C56 122.2(3) . . ? N8 C52 C51 118.1(3) . . ? C56 C52 C51 119.6(3) . . ? N8 C53 C54 122.9(3) . . ? N8 C53 H60 118.5 . . ? C54 C53 H60 118.5 . . ? C53 C54 C55 118.8(4) . . ? C53 C54 H59 120.6 . . ? C55 C54 H59 120.6 . . ? C56 C55 C54 119.2(3) . . ? C56 C55 H58 120.4 . . ? C54 C55 H58 120.4 . . ? C55 C56 C52 119.3(3) . . ? C55 C56 H57 120.3 . . ? C52 C56 H57 120.3 . . ? N9 C57 C60 120.6(4) . . ? N9 C57 C58 118.2(3) . . ? C60 C57 C58 121.1(3) . . ? C57 C58 C59 114.3(3) . . ? C57 C58 H67 108.7 . . ? C59 C58 H67 108.7 . . ? C57 C58 H68 108.7 . . ? C59 C58 H68 108.7 . . ? H67 C58 H68 107.6 . . ? O7 C59 C58 111.6(2) . . ? O7 C59 H65 109.3 . . ? C58 C59 H65 109.3 . . ? O7 C59 H66 109.3 . . ? C58 C59 H66 109.3 . . ? H65 C59 H66 108.0 . . ? C61 C60 C57 120.0(4) . . ? C61 C60 H72 120.0 . . ? C57 C60 H72 120.0 . . ? C60 C61 C62 119.5(4) . . ? C60 C61 H71 120.3 . . ? C62 C61 H71 120.3 . . ? C63 C62 C61 118.7(4) . . ? C63 C62 H70 120.7 . . ? C61 C62 H70 120.7 . . ? N9 C63 C62 122.7(4) . . ? N9 C63 H69 118.6 . . ? C62 C63 H69 118.6 . . ? O8 C64 C65 112.1(3) . . ? O8 C64 H79 109.2 . . ? C65 C64 H79 109.2 . . ? O8 C64 H80 109.2 . . ? C65 C64 H80 109.2 . . ? H79 C64 H80 107.9 . . ? C66 C65 C64 115.0(3) . . ? C66 C65 H77 108.5 . . ? C64 C65 H77 108.5 . . ? C66 C65 H78 108.5 . . ? C64 C65 H78 108.5 . . ? H77 C65 H78 107.5 . . ? N10 C66 C70 121.3(3) . . ? N10 C66 C65 118.3(3) . . ? C70 C66 C65 120.4(3) . . ? N10 C67 C68 124.0(4) . . ? N10 C67 H76 118.0 . . ? C68 C67 H76 118.0 . . ? C67 C68 C69 118.2(4) . . ? C67 C68 H75 120.9 . . ? C69 C68 H75 120.9 . . ? C68 C69 C70 118.3(4) . . ? C68 C69 H74 120.9 . . ? C70 C69 H74 120.9 . . ? C66 C70 C69 119.9(4) . . ? C66 C70 H73 120.1 . . ? C69 C70 H73 120.1 . . ? O11 C71 C72 112.0(3) . . ? O11 C71 H87 109.2 . . ? C72 C71 H87 109.2 . . ? O11 C71 H88 109.2 . . ? C72 C71 H88 109.2 . . ? H87 C71 H88 107.9 . . ? C73 C72 C71 114.1(3) . . ? C73 C72 H85 108.7 . . ? C71 C72 H85 108.7 . . ? C73 C72 H86 108.7 . . ? C71 C72 H86 108.7 . . ? H85 C72 H86 107.6 . . ? N11 C73 C77 120.4(4) . . ? N11 C73 C72 118.8(3) . . ? C77 C73 C72 120.8(3) . . ? N11 C74 C75 124.2(4) . . ? N11 C74 H84 117.9 . . ? C75 C74 H84 117.9 . . ? C74 C75 C76 117.7(4) . . ? C74 C75 H83 121.2 . . ? C76 C75 H83 121.2 . . ? C77 C76 C75 119.2(4) . . ? C77 C76 H82 120.4 . . ? C75 C76 H82 120.4 . . ? C76 C77 C73 120.2(4) . . ? C76 C77 H81 119.9 . . ? C73 C77 H81 119.9 . . ? O12 C78 C79 111.4(3) . . ? O12 C78 H95 109.3 . . ? C79 C78 H95 109.3 . . ? O12 C78 H96 109.3 . . ? C79 C78 H96 109.3 . . ? H95 C78 H96 108.0 . . ? C78 C79 C80 113.8(3) . . ? C78 C79 H93 108.8 . . ? C80 C79 H93 108.8 . . ? C78 C79 H94 108.8 . . ? C80 C79 H94 108.8 . . ? H93 C79 H94 107.7 . . ? N12 C80 C84 121.8(3) . . ? N12 C80 C79 117.9(3) . . ? C84 C80 C79 120.2(3) . . ? N12 C81 C82 123.2(4) . . ? N12 C81 H92 118.4 . . ? C82 C81 H92 118.4 . . ? C83 C82 C81 118.6(3) . . ? C83 C82 H91 120.7 . . ? C81 C82 H91 120.7 . . ? C84 C83 C82 119.0(4) . . ? C84 C83 H90 120.5 . . ? C82 C83 H90 120.5 . . ? C83 C84 C80 120.1(4) . . ? C83 C84 H89 120.0 . . ? C80 C84 H89 120.0 . . ? Cl6 C85 Cl5 111.1(2) . . ? Cl6 C85 H97 109.4 . . ? Cl5 C85 H97 109.4 . . ? Cl6 C85 H98 109.4 . . ? Cl5 C85 H98 109.4 . . ? H97 C85 H98 108.0 . . ? Cl3 C86 Cl4 111.3(2) . . ? Cl3 C86 H99 109.4 . . ? Cl4 C86 H99 109.4 . . ? Cl3 C86 H100 109.4 . . ? Cl4 C86 H100 109.4 . . ? H99 C86 H100 108.0 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.047 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.142