# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global #TrackingRef '- Communication_CIF.cif' _journal_coden_Cambridge 182 # SUBMISSION DETAILS _publ_contact_author_name 'Laurence K. Thompson' _publ_contact_author_address ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; _publ_contact_author_email lk.thompson@mun.ca _publ_contact_author_phone 1-709-737-8750 _publ_contact_author_fax 1-709-737-3702 _publ_requested_journal 'Chem Comm' _publ_section_title ; Unexpected Ni(II) and Cu(II) polynuclear assemblies a balance between ligand and metal ion coordination preferences ; _publ_section_abstract ; Please see full paper. ; loop_ _publ_author_name _publ_author_address 'Kontantin V. Shuvaev' ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Santokh S. Tandon' ; Department of Chemistry, Kent State University at Salem, Salem, Ohio, 44440, USA ; 'Louise N. Dawe' ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; 'Laurence K. Thompson' ; Department of chemistry Memorial University of Newfoundland St. Johns, NL, A1B 3X7, Canada ; data_2 _database_code_depnum_ccdc_archive 'CCDC 775196' #TrackingRef '- Communication_CIF.cif' # start Validation Reply Form _vrf_PLAT306_2 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O10 RESPONSE: Solvent (water) lattice molecule for which protons could not be located in the difference map; protons were omitted from the model but included in the formula ; _vrf_PLAT430_2 ; PROBLEM: Short Inter D...A Contact O1 .. O11 .. 2.45 Ang. RESPONSE: Solvent (water) lattice molecule hydrogen bonded to ligand oxygen atom. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C18 H14 O2 N10)3 Ni4 (Cl O4)2 (H2 O)7.5' _chemical_formula_sum 'C54 H57 Cl2 N30 Ni4 O21.50' _chemical_formula_weight 1776.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.051(9) _cell_length_b 9.569(2) _cell_length_c 19.109(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.296(3) _cell_angle_gamma 90.00 _cell_volume 6787(3) _cell_formula_units_Z 4 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 12074 _cell_measurement_theta_min 2.3808 _cell_measurement_theta_max 30.8212 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3636 _exptl_absorpt_coefficient_mu 1.272 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.9042 _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 14603 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6979 _reflns_number_gt 5288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'Patterson search(DIRDIF,Beurskens,1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+33.0701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6979 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1149 _refine_ls_R_factor_gt 0.0907 _refine_ls_wR_factor_ref 0.2352 _refine_ls_wR_factor_gt 0.2153 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 0.35460(2) 0.48141(9) 0.06440(4) 0.0348(2) Uani 1 1 d . . . Ni2 Ni 0.452224(19) 0.47354(9) 0.18784(4) 0.0313(2) Uani 1 1 d . . . Cl1 Cl 0.30242(6) -0.0058(2) 0.14500(13) 0.0676(6) Uani 1 1 d . . . O1 O 0.40060(14) 0.2653(7) -0.0583(3) 0.0698(17) Uani 1 1 d . . . O2 O 0.38660(13) 0.3872(7) 0.2919(3) 0.0604(15) Uani 1 1 d . . . O3 O 0.41074(14) 0.8486(5) 0.0885(3) 0.0636(15) Uani 1 1 d . . . O4 O 0.3294(2) -0.0926(10) 0.1840(9) 0.225(8) Uani 1 1 d . . . O5 O 0.31512(19) 0.1321(7) 0.1447(4) 0.100(2) Uani 1 1 d . . . O6 O 0.2791(3) -0.0038(12) 0.1877(6) 0.153(4) Uani 1 1 d . . . O7 O 0.2775(2) -0.0467(10) 0.0742(4) 0.124(3) Uani 1 1 d . . . O8 O 0.4755(4) 0.0217(9) 0.3892(7) 0.109(4) Uani 0.75 1 d P . . O9 O 0.3852(3) 0.9035(15) -0.1863(7) 0.084(4) Uani 0.50 1 d P . . O10 O 0.46039(13) 0.6997(6) -0.1280(3) 0.0528(12) Uani 1 1 d . . . O11 O 0.4248(4) 1.0399(14) -0.0739(12) 0.111(6) Uani 0.50 1 d P . . O12 O 0.4456(3) 1.0151(13) 0.0141(7) 0.061(3) Uani 0.50 1 d P . . O13 O 0.4618(5) 0.9015(17) 0.0586(11) 0.114(6) Uani 0.50 1 d P . . N1 N 0.32602(13) 0.3279(5) -0.0146(3) 0.0350(11) Uani 1 1 d . . . N2 N 0.39139(13) 0.4154(6) 0.0263(3) 0.0372(12) Uani 1 1 d . . . N3 N 0.42786(13) 0.4531(6) 0.0669(3) 0.0350(12) Uani 1 1 d . . . N4 N 0.42592(14) 0.5714(6) -0.0431(3) 0.0396(12) Uani 1 1 d . . . H5 H 0.4037 0.5458 -0.0730 0.047 Uiso 1 1 calc R . . H6 H 0.4379 0.6242 -0.0617 0.047 Uiso 1 1 calc R . . N5 N 0.48999(12) 0.5470(5) 0.1537(3) 0.0312(11) Uani 1 1 d . . . N6 N 0.31984(15) 0.5155(6) 0.1143(3) 0.0419(13) Uani 1 1 d . . . N7 N 0.37910(13) 0.3654(6) 0.1656(3) 0.0390(12) Uani 1 1 d . . . N8 N 0.41644(13) 0.3306(6) 0.1952(3) 0.0362(12) Uani 1 1 d . . . N9 N 0.40007(17) 0.0996(7) 0.1550(4) 0.0624(18) Uani 1 1 d . . . H12 H 0.3769 0.1155 0.1392 0.075 Uiso 1 1 calc R . . H13 H 0.4076 0.0154 0.1507 0.075 Uiso 1 1 calc R . . N10 N 0.48231(13) 0.2946(5) 0.2316(3) 0.0336(11) Uani 1 1 d . . . N11 N 0.33458(13) 0.6381(6) -0.0220(3) 0.0368(12) Uani 1 1 d . . . N12 N 0.38582(12) 0.6539(6) 0.1174(3) 0.0368(12) Uani 1 1 d . . . N13 N 0.41820(13) 0.6345(6) 0.1843(3) 0.0370(12) Uani 1 1 d . . . N14 N 0.39415(15) 0.7435(7) 0.2614(3) 0.0608(19) Uani 1 1 d . . . H19 H 0.3738 0.7657 0.2219 0.073 Uiso 1 1 calc R . . H20 H 0.3977 0.7666 0.3087 0.073 Uiso 1 1 calc R . . N15 N 0.47645(12) 0.5715(5) 0.2958(3) 0.0316(11) Uani 1 1 d . . . C1 C 0.29148(17) 0.2902(7) -0.0368(4) 0.0415(15) Uani 1 1 d . . . H1 H 0.2797 0.3193 -0.0061 0.050 Uiso 1 1 calc R . . C2 C 0.27250(17) 0.2121(7) -0.1015(4) 0.0443(16) Uani 1 1 d . . . H2 H 0.2480 0.1894 -0.1156 0.053 Uiso 1 1 calc R . . C3 C 0.28934(19) 0.1671(8) -0.1455(4) 0.0488(17) Uani 1 1 d . . . H3 H 0.2766 0.1128 -0.1907 0.059 Uiso 1 1 calc R . . C4 C 0.32546(19) 0.2020(7) -0.1233(4) 0.0466(16) Uani 1 1 d . . . H4 H 0.3379 0.1719 -0.1527 0.056 Uiso 1 1 calc R . . C5 C 0.34254(17) 0.2815(7) -0.0574(3) 0.0375(14) Uani 1 1 d . . . C6 C 0.38177(17) 0.3225(8) -0.0281(4) 0.0426(15) Uani 1 1 d . . . C7 C 0.44139(16) 0.5303(7) 0.0301(3) 0.0330(13) Uani 1 1 d . . . C8 C 0.47887(15) 0.5792(7) 0.0792(3) 0.0333(13) Uani 1 1 d . . . C9 C 0.50175(16) 0.6445(7) 0.0530(3) 0.0389(15) Uani 1 1 d . . . H7 H 0.4941 0.6649 -0.0003 0.047 Uiso 1 1 calc R . . C10 C 0.28885(17) 0.5843(7) 0.0854(4) 0.0410(15) Uani 1 1 d . . . H8 H 0.2790 0.6127 0.0327 0.049 Uiso 1 1 calc R . . C11 C 0.27023(19) 0.6163(8) 0.1292(4) 0.0490(17) Uani 1 1 d . . . H9 H 0.2477 0.6632 0.1065 0.059 Uiso 1 1 calc R . . C12 C 0.28487(18) 0.5790(8) 0.2057(4) 0.0500(17) Uani 1 1 d . . . H10 H 0.2729 0.6015 0.2373 0.060 Uiso 1 1 calc R . . C13 C 0.3169(2) 0.5090(8) 0.2359(4) 0.0484(17) Uani 1 1 d . . . H11 H 0.3275 0.4829 0.2889 0.058 Uiso 1 1 calc R . . C14 C 0.33379(17) 0.4763(7) 0.1897(4) 0.0407(15) Uani 1 1 d . . . C15 C 0.36948(17) 0.4031(8) 0.2200(3) 0.0409(15) Uani 1 1 d . . . C16 C 0.42379(17) 0.2033(8) 0.1856(4) 0.0422(15) Uani 1 1 d . . . C17 C 0.46361(18) 0.1756(7) 0.2153(4) 0.0382(14) Uani 1 1 d . . . C18 C 0.4813(2) 0.0469(8) 0.2333(4) 0.0524(18) Uani 1 1 d . . . H14 H 0.4681 -0.0382 0.2230 0.063 Uiso 1 1 calc R . . C19 C 0.30716(17) 0.6295(8) -0.0937(3) 0.0443(16) Uani 1 1 d . . . H15 H 0.2911 0.5523 -0.1050 0.053 Uiso 1 1 calc R . . C20 C 0.30129(19) 0.7262(7) -0.1508(4) 0.0465(17) Uani 1 1 d . . . H16 H 0.2820 0.7153 -0.2006 0.056 Uiso 1 1 calc R . . C21 C 0.3235(2) 0.8368(9) -0.1345(5) 0.066(2) Uani 1 1 d . . . H17 H 0.3202 0.9054 -0.1729 0.079 Uiso 1 1 calc R . . C22 C 0.3513(2) 0.8498(8) -0.0613(5) 0.063(2) Uani 1 1 d . . . H18 H 0.3670 0.9279 -0.0491 0.076 Uiso 1 1 calc R . . C23 C 0.35608(18) 0.7504(7) -0.0067(4) 0.0450(16) Uani 1 1 d . . . C24 C 0.38685(18) 0.7549(7) 0.0723(4) 0.0462(17) Uani 1 1 d . . . C25 C 0.41956(16) 0.6749(7) 0.2496(4) 0.0409(15) Uani 1 1 d . . . C26 C 0.45423(15) 0.6424(7) 0.3167(3) 0.0357(14) Uani 1 1 d . . . C27 C 0.46400(17) 0.6789(8) 0.3929(4) 0.0434(16) Uani 1 1 d . . . H21 H 0.4476 0.7264 0.4078 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0274(4) 0.0468(5) 0.0265(4) -0.0011(3) 0.0080(3) -0.0040(3) Ni2 0.0239(4) 0.0424(5) 0.0244(4) -0.0006(3) 0.0074(3) -0.0010(3) Cl1 0.0480(11) 0.0604(12) 0.0624(12) 0.0105(10) -0.0069(10) -0.0092(10) O1 0.049(3) 0.098(4) 0.076(4) -0.044(3) 0.040(3) -0.029(3) O2 0.047(3) 0.097(4) 0.031(2) 0.010(3) 0.011(2) 0.013(3) O3 0.054(3) 0.043(3) 0.063(3) 0.005(3) -0.004(3) -0.014(3) O4 0.054(5) 0.097(6) 0.389(18) 0.064(9) -0.035(7) 0.020(5) O5 0.090(5) 0.074(4) 0.116(6) 0.013(4) 0.025(4) -0.032(4) O6 0.162(10) 0.186(10) 0.115(7) -0.001(7) 0.061(7) -0.074(8) O7 0.107(6) 0.157(8) 0.071(5) -0.010(5) 0.002(4) -0.040(6) O8 0.160(11) 0.059(5) 0.117(8) 0.010(5) 0.067(8) 0.023(6) O9 0.082(9) 0.096(10) 0.075(8) 0.021(8) 0.035(7) 0.019(8) O10 0.047(3) 0.071(3) 0.037(2) 0.004(2) 0.014(2) 0.001(3) O11 0.110(12) 0.064(8) 0.207(19) -0.006(10) 0.113(14) -0.004(8) O12 0.043(6) 0.080(8) 0.066(7) 0.037(6) 0.028(5) 0.004(5) O13 0.127(13) 0.093(11) 0.165(16) -0.027(12) 0.103(13) -0.015(10) N1 0.031(3) 0.043(3) 0.028(2) -0.004(2) 0.010(2) -0.007(2) N2 0.024(2) 0.053(3) 0.030(3) -0.005(2) 0.007(2) -0.008(2) N3 0.027(3) 0.053(3) 0.021(2) -0.004(2) 0.007(2) -0.004(2) N4 0.032(3) 0.058(3) 0.026(2) 0.000(2) 0.010(2) 0.000(3) N5 0.022(2) 0.040(3) 0.028(2) 0.001(2) 0.007(2) 0.000(2) N6 0.039(3) 0.051(3) 0.034(3) -0.006(2) 0.013(2) -0.007(3) N7 0.029(3) 0.050(3) 0.034(3) -0.001(2) 0.010(2) -0.006(2) N8 0.028(3) 0.045(3) 0.032(3) 0.001(2) 0.009(2) 0.000(2) N9 0.045(4) 0.056(4) 0.084(5) -0.008(4) 0.026(3) -0.009(3) N10 0.031(2) 0.038(3) 0.031(3) 0.000(2) 0.013(2) -0.002(2) N11 0.027(2) 0.048(3) 0.030(3) -0.001(2) 0.006(2) 0.002(2) N12 0.022(2) 0.050(3) 0.028(3) -0.001(2) 0.001(2) 0.004(2) N13 0.025(2) 0.052(3) 0.026(2) -0.002(2) 0.003(2) -0.006(2) N14 0.033(3) 0.092(5) 0.043(3) -0.023(3) 0.003(3) 0.018(3) N15 0.023(2) 0.044(3) 0.025(2) -0.002(2) 0.0078(19) -0.004(2) C1 0.034(3) 0.046(4) 0.041(3) -0.006(3) 0.012(3) -0.011(3) C2 0.032(3) 0.047(4) 0.046(4) -0.007(3) 0.010(3) -0.015(3) C3 0.046(4) 0.053(4) 0.037(4) -0.005(3) 0.008(3) -0.015(3) C4 0.051(4) 0.048(4) 0.043(4) -0.006(3) 0.022(3) -0.015(3) C5 0.038(3) 0.043(3) 0.030(3) -0.002(3) 0.014(3) -0.008(3) C6 0.036(3) 0.057(4) 0.037(3) -0.002(3) 0.017(3) -0.006(3) C7 0.027(3) 0.047(4) 0.023(3) -0.005(3) 0.008(2) 0.001(3) C8 0.031(3) 0.041(3) 0.028(3) -0.001(3) 0.012(2) 0.001(3) C9 0.030(3) 0.057(4) 0.023(3) 0.005(3) 0.005(2) -0.004(3) C10 0.033(3) 0.049(4) 0.039(3) 0.007(3) 0.013(3) -0.004(3) C11 0.041(4) 0.061(5) 0.048(4) -0.002(4) 0.022(3) 0.000(3) C12 0.039(4) 0.067(5) 0.052(4) -0.009(4) 0.027(3) -0.007(4) C13 0.046(4) 0.069(5) 0.035(3) -0.003(3) 0.021(3) -0.006(4) C14 0.031(3) 0.055(4) 0.036(3) -0.002(3) 0.014(3) -0.010(3) C15 0.034(3) 0.057(4) 0.032(3) 0.002(3) 0.014(3) -0.007(3) C16 0.032(3) 0.054(4) 0.035(3) 0.002(3) 0.008(3) -0.007(3) C17 0.043(3) 0.040(3) 0.035(3) -0.001(3) 0.020(3) -0.003(3) C18 0.052(4) 0.046(4) 0.055(4) -0.001(3) 0.019(4) -0.007(3) C19 0.037(3) 0.059(4) 0.030(3) -0.005(3) 0.008(3) -0.004(3) C20 0.046(4) 0.051(4) 0.030(3) -0.002(3) 0.005(3) 0.008(3) C21 0.070(5) 0.058(5) 0.049(4) 0.017(4) 0.004(4) 0.004(4) C22 0.054(5) 0.050(4) 0.058(5) 0.013(4) -0.003(4) -0.001(4) C23 0.040(4) 0.042(4) 0.044(4) 0.000(3) 0.009(3) 0.008(3) C24 0.034(3) 0.037(4) 0.048(4) 0.000(3) -0.001(3) 0.001(3) C25 0.029(3) 0.053(4) 0.035(3) -0.006(3) 0.008(3) 0.000(3) C26 0.026(3) 0.049(4) 0.030(3) -0.003(3) 0.009(2) 0.000(3) C27 0.032(3) 0.058(4) 0.041(4) -0.006(3) 0.017(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.037(5) . ? Ni1 N6 2.053(6) . ? Ni1 N12 2.069(5) . ? Ni1 N1 2.073(5) . ? Ni1 N7 2.080(5) . ? Ni1 N11 2.119(5) . ? Ni2 N5 2.046(5) . ? Ni2 N8 2.056(5) . ? Ni2 N13 2.061(5) . ? Ni2 N10 2.067(5) . ? Ni2 N15 2.091(5) . ? Ni2 N3 2.099(5) . ? Cl1 O4 1.330(8) . ? Cl1 O7 1.360(7) . ? Cl1 O5 1.420(7) . ? Cl1 O6 1.502(11) . ? O1 C6 1.270(8) . ? O2 C15 1.257(7) . ? O3 C24 1.265(8) . ? O11 O12 1.54(2) . ? O12 O13 1.36(2) . ? N1 C5 1.341(8) . ? N1 C1 1.344(8) . ? N2 C6 1.294(8) . ? N2 N3 1.407(6) . ? N3 C7 1.297(8) . ? N4 C7 1.325(7) . ? N4 H5 0.8800 . ? N4 H6 0.8800 . ? N5 N15 1.322(6) 2_655 ? N5 C8 1.333(7) . ? N6 C10 1.325(8) . ? N6 C14 1.357(8) . ? N7 C15 1.310(8) . ? N7 N8 1.428(7) . ? N8 C16 1.286(9) . ? N9 C16 1.337(9) . ? N9 H12 0.8800 . ? N9 H13 0.8800 . ? N10 N10 1.316(9) 2_655 ? N10 C17 1.334(8) . ? N11 C23 1.341(9) . ? N11 C19 1.354(7) . ? N12 C24 1.308(9) . ? N12 N13 1.408(6) . ? N13 C25 1.286(8) . ? N14 C25 1.330(8) . ? N14 H19 0.8800 . ? N14 H20 0.8800 . ? N15 N5 1.322(6) 2_655 ? N15 C26 1.328(7) . ? C1 C2 1.368(9) . ? C1 H1 0.9500 . ? C2 C3 1.367(10) . ? C2 H2 0.9500 . ? C3 C4 1.397(10) . ? C3 H3 0.9500 . ? C4 C5 1.379(9) . ? C4 H4 0.9500 . ? C5 C6 1.514(9) . ? C7 C8 1.494(8) . ? C8 C9 1.387(8) . ? C9 C27 1.382(8) 2_655 ? C9 H7 0.9500 . ? C10 C11 1.388(9) . ? C10 H8 0.9500 . ? C11 C12 1.369(10) . ? C11 H9 0.9500 . ? C12 C13 1.365(10) . ? C12 H10 0.9500 . ? C13 C14 1.371(9) . ? C13 H11 0.9500 . ? C14 C15 1.499(9) . ? C16 C17 1.507(9) . ? C17 C18 1.396(9) . ? C18 C18 1.387(15) 2_655 ? C18 H14 0.9500 . ? C19 C20 1.371(9) . ? C19 H15 0.9500 . ? C20 C21 1.345(11) . ? C20 H16 0.9500 . ? C21 C22 1.381(10) . ? C21 H17 0.9500 . ? C22 C23 1.362(10) . ? C22 H18 0.9500 . ? C23 C24 1.498(9) . ? C25 C26 1.485(8) . ? C26 C27 1.379(8) . ? C27 C9 1.382(8) 2_655 ? C27 H21 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 N2 Ni1 N6 169.7(2) . . ? N2 Ni1 N12 91.3(2) . . ? N6 Ni1 N12 93.1(2) . . ? N2 Ni1 N1 78.2(2) . . ? N6 Ni1 N1 99.3(2) . . ? N12 Ni1 N1 163.9(2) . . ? N2 Ni1 N7 91.7(2) . . ? N6 Ni1 N7 79.0(2) . . ? N12 Ni1 N7 91.1(2) . . ? N1 Ni1 N7 101.4(2) . . ? N2 Ni1 N11 92.3(2) . . ? N6 Ni1 N11 97.7(2) . . ? N12 Ni1 N11 76.7(2) . . ? N1 Ni1 N11 91.4(2) . . ? N7 Ni1 N11 167.2(2) . . ? N5 Ni2 N8 155.7(2) . . ? N5 Ni2 N13 109.1(2) . . ? N8 Ni2 N13 90.3(2) . . ? N5 Ni2 N10 90.58(19) . . ? N8 Ni2 N10 75.05(19) . . ? N13 Ni2 N10 155.8(2) . . ? N5 Ni2 N15 93.13(18) . . ? N8 Ni2 N15 106.46(19) . . ? N13 Ni2 N15 74.18(19) . . ? N10 Ni2 N15 91.28(19) . . ? N5 Ni2 N3 75.56(19) . . ? N8 Ni2 N3 89.7(2) . . ? N13 Ni2 N3 92.1(2) . . ? N10 Ni2 N3 106.8(2) . . ? N15 Ni2 N3 158.5(2) . . ? O4 Cl1 O7 118.0(8) . . ? O4 Cl1 O5 111.3(5) . . ? O7 Cl1 O5 112.7(5) . . ? O4 Cl1 O6 106.0(9) . . ? O7 Cl1 O6 99.3(6) . . ? O5 Cl1 O6 108.1(6) . . ? O13 O12 O11 134.1(14) . . ? C5 N1 C1 117.3(5) . . ? C5 N1 Ni1 113.7(4) . . ? C1 N1 Ni1 127.8(4) . . ? C6 N2 N3 120.4(5) . . ? C6 N2 Ni1 118.8(4) . . ? N3 N2 Ni1 120.0(4) . . ? C7 N3 N2 116.7(5) . . ? C7 N3 Ni2 115.5(4) . . ? N2 N3 Ni2 121.6(4) . . ? C7 N4 H5 120.0 . . ? C7 N4 H6 120.0 . . ? H5 N4 H6 120.0 . . ? N15 N5 C8 120.8(5) 2_655 . ? N15 N5 Ni2 121.6(4) 2_655 . ? C8 N5 Ni2 117.4(4) . . ? C10 N6 C14 118.3(6) . . ? C10 N6 Ni1 128.3(5) . . ? C14 N6 Ni1 112.8(4) . . ? C15 N7 N8 112.8(5) . . ? C15 N7 Ni1 113.6(4) . . ? N8 N7 Ni1 120.2(4) . . ? C16 N8 N7 116.2(5) . . ? C16 N8 Ni2 113.7(4) . . ? N7 N8 Ni2 119.7(4) . . ? C16 N9 H12 120.0 . . ? C16 N9 H13 120.0 . . ? H12 N9 H13 120.0 . . ? N10 N10 C17 121.2(4) 2_655 . ? N10 N10 Ni2 123.27(15) 2_655 . ? C17 N10 Ni2 115.3(4) . . ? C23 N11 C19 117.1(6) . . ? C23 N11 Ni1 113.4(4) . . ? C19 N11 Ni1 128.6(5) . . ? C24 N12 N13 114.3(5) . . ? C24 N12 Ni1 117.1(4) . . ? N13 N12 Ni1 119.1(4) . . ? C25 N13 N12 118.3(5) . . ? C25 N13 Ni2 116.4(4) . . ? N12 N13 Ni2 119.5(4) . . ? C25 N14 H19 120.0 . . ? C25 N14 H20 120.0 . . ? H19 N14 H20 120.0 . . ? N5 N15 C26 120.5(5) 2_655 . ? N5 N15 Ni2 123.2(4) 2_655 . ? C26 N15 Ni2 115.3(4) . . ? N1 C1 C2 123.3(6) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 119.1(6) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.2(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.0(7) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? N1 C5 C4 123.2(6) . . ? N1 C5 C6 115.1(5) . . ? C4 C5 C6 121.7(6) . . ? O1 C6 N2 128.7(6) . . ? O1 C6 C5 118.6(6) . . ? N2 C6 C5 112.7(6) . . ? N3 C7 N4 128.2(6) . . ? N3 C7 C8 113.8(5) . . ? N4 C7 C8 118.0(5) . . ? N5 C8 C9 120.9(5) . . ? N5 C8 C7 112.9(5) . . ? C9 C8 C7 126.1(5) . . ? C27 C9 C8 117.8(5) 2_655 . ? C27 C9 H7 121.1 2_655 . ? C8 C9 H7 121.1 . . ? N6 C10 C11 122.4(6) . . ? N6 C10 H8 118.8 . . ? C11 C10 H8 118.8 . . ? C12 C11 C10 118.9(7) . . ? C12 C11 H9 120.6 . . ? C10 C11 H9 120.6 . . ? C13 C12 C11 118.9(6) . . ? C13 C12 H10 120.6 . . ? C11 C12 H10 120.6 . . ? C12 C13 C14 120.1(7) . . ? C12 C13 H11 120.0 . . ? C14 C13 H11 120.0 . . ? N6 C14 C13 121.3(6) . . ? N6 C14 C15 116.0(6) . . ? C13 C14 C15 122.5(6) . . ? O2 C15 N7 128.0(6) . . ? O2 C15 C14 118.5(6) . . ? N7 C15 C14 113.5(5) . . ? N8 C16 N9 126.4(6) . . ? N8 C16 C17 113.3(6) . . ? N9 C16 C17 120.3(6) . . ? N10 C17 C18 120.6(6) . . ? N10 C17 C16 111.2(6) . . ? C18 C17 C16 127.9(6) . . ? C18 C18 C17 118.0(4) 2_655 . ? C18 C18 H14 121.0 2_655 . ? C17 C18 H14 121.0 . . ? N11 C19 C20 123.5(7) . . ? N11 C19 H15 118.3 . . ? C20 C19 H15 118.3 . . ? C21 C20 C19 118.4(6) . . ? C21 C20 H16 120.8 . . ? C19 C20 H16 120.8 . . ? C20 C21 C22 119.3(7) . . ? C20 C21 H17 120.3 . . ? C22 C21 H17 120.3 . . ? C23 C22 C21 120.0(8) . . ? C23 C22 H18 120.0 . . ? C21 C22 H18 120.0 . . ? N11 C23 C22 121.7(6) . . ? N11 C23 C24 115.8(6) . . ? C22 C23 C24 122.4(7) . . ? O3 C24 N12 127.0(6) . . ? O3 C24 C23 119.9(6) . . ? N12 C24 C23 113.1(6) . . ? N13 C25 N14 126.9(6) . . ? N13 C25 C26 113.8(5) . . ? N14 C25 C26 119.3(6) . . ? N15 C26 C27 121.3(5) . . ? N15 C26 C25 112.1(5) . . ? C27 C26 C25 126.7(6) . . ? C26 C27 C9 118.2(6) . 2_655 ? C26 C27 H21 120.9 . . ? C9 C27 H21 120.9 2_655 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.948 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.112 data_5 _database_code_depnum_ccdc_archive 'CCDC 775197' #TrackingRef '- Communication_CIF.cif' # start Validation Reply Form _vrf_CHEMW03_5 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: Platon's Squeeze procedure was applied to this structure. The given molecular weight includes the lattice solvent molecules that were omitted from the model via Squeeze. ; _vrf_PLAT220_5 ; PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) ... 9.52 Ratio RESPONSE: This is part of a perchlorate anion and was refined anisotropically. ; _vrf_PLAT241_5 ; PROBLEM: Check High Ueq as Compared to Neighbors for O24 RESPONSE: This is part of a perchlorate anion and was refined anisotropically. ; _vrf_PLAT242_5 ; PROBLEM: Check Low Ueq as Compared to Neighbors for Cl3 RESPONSE: This is part of a perchlorate anion and was refined anisotropically. ; _vrf_PLAT043_5 ; PROBLEM: Check Reported Molecular Weight ................ 4061.42 RESPONSE: Platon's Squeeze procedure was applied to this structure. The given molecular weight includes the lattice solvent molecules that were omitted from the model via Squeeze. ; _vrf_PLAT044_5 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: Platon's Squeeze procedure was applied to this structure. The given density includes the lattice solvent molecules that were omitted from the model via Squeeze. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[3(C28 H18 O2 N12), Cu11, 2(OH)], 4(C2 H3 O2), 4(Cl O4), Na, (O H), 55 (H2 O)' _chemical_formula_sum 'C92 H179 Cl4 Cu11 N36 Na O88' _chemical_formula_weight 4061.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.024(7) _cell_length_b 20.901(6) _cell_length_c 24.333(7) _cell_angle_alpha 67.954(10) _cell_angle_beta 78.882(12) _cell_angle_gamma 86.105(14) _cell_volume 8337(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 26278 _cell_measurement_theta_min 1.7118 _cell_measurement_theta_max 29.7530 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Brown' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4170 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9635 _exptl_absorpt_correction_T_min 0.8206 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 58641 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.1011 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 26.50 _reflns_number_total 32789 _reflns_number_gt 23554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1286P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 32789 _refine_ls_number_parameters 1712 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2273 _refine_ls_wR_factor_gt 0.2073 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 -0.028 -0.042 0.500 2835 853 '42(H2 O)' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 853 electrons per unit cell in one void (total volume 2835 ^A^3); that is 426.5 electrons per formula unit. Disordered solvent lattice water molecules (approx. 42 molecules) were present,however, a good point atom model could not be achieved. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 Cu1 Cu 0.73460(3) 0.76056(3) 0.89360(3) 0.03141(15) Uani 1 1 d . . . Cu2 Cu 0.67582(3) 0.54953(3) 1.03281(3) 0.02949(14) Uani 1 1 d . . . Cu3 Cu 0.64251(3) 0.37702(3) 1.08878(3) 0.02938(14) Uani 1 1 d . . . Cu4 Cu 0.59971(3) 0.18871(3) 1.07803(3) 0.03047(14) Uani 1 1 d . . . Cu5 Cu 0.77334(3) 0.15593(3) 1.06178(3) 0.03243(15) Uani 1 1 d . . . Cu6 Cu 0.77467(3) 0.19762(3) 0.87698(3) 0.03461(15) Uani 1 1 d . . . Cu7 Cu 0.79480(4) 0.29953(4) 0.72960(3) 0.03945(17) Uani 1 1 d . . . Cu8 Cu 0.80995(4) 0.49466(4) 0.56374(3) 0.03694(16) Uani 1 1 d . . . Cu9 Cu 0.63317(3) 0.50024(3) 0.59630(3) 0.03334(15) Uani 1 1 d . . . Cu10 Cu 0.65671(4) 0.68240(4) 0.63408(3) 0.04153(17) Uani 1 1 d . . . Cu11 Cu 0.90552(3) 0.71091(3) 0.90799(3) 0.03389(15) Uani 1 1 d . . . Cl1 Cl 0.61653(7) 0.54618(7) 0.89177(6) 0.0385(3) Uani 1 1 d . . . Cl2 Cl 0.86644(17) 0.40781(16) 0.80927(14) 0.1036(8) Uani 1 1 d . . . Cl3 Cl 1.07630(10) 0.60545(13) 0.87495(12) 0.0877(7) Uani 1 1 d . . . Cl4 Cl 0.52957(10) 0.19281(9) 0.81697(8) 0.0567(4) Uani 1 1 d . . . Na1 Na 0.65155(12) 0.46631(11) 1.17850(9) 0.0374(5) Uani 1 1 d . . . O1 O 0.7677(2) 0.6635(2) 1.06754(16) 0.0390(8) Uani 1 1 d . . . O2 O 0.6899(2) 0.2215(2) 1.20565(17) 0.0387(8) Uani 1 1 d . . . O3 O 0.6645(2) 0.0515(2) 0.98868(18) 0.0433(9) Uani 1 1 d . . . O4 O 0.7208(3) 0.3033(2) 0.6068(2) 0.0534(11) Uani 1 1 d . . . O5 O 0.7161(2) 0.6918(2) 0.48501(18) 0.0489(10) Uani 1 1 d . . . O6 O 0.9021(3) 0.8770(2) 0.75201(19) 0.0515(10) Uani 1 1 d . . . O7 O 0.61304(19) 0.62220(19) 1.04699(16) 0.0351(8) Uani 1 1 d . . . O8 O 0.5914(2) 0.5751(2) 1.14698(18) 0.0442(9) Uani 1 1 d . . . O9 O 0.56019(19) 0.33091(19) 1.15442(16) 0.0332(8) Uani 1 1 d . . . O10 O 0.5073(2) 0.2778(2) 1.10715(17) 0.0404(9) Uani 1 1 d . . . O11 O 0.8397(2) 0.1202(2) 0.91059(19) 0.0461(10) Uani 1 1 d . . . O12 O 0.8749(2) 0.1520(2) 0.97974(19) 0.0431(9) Uani 1 1 d . . . O13 O 0.5690(2) 0.6807(2) 0.59989(19) 0.0469(10) Uani 1 1 d . . . O14 O 0.4702(3) 0.7164(2) 0.5560(2) 0.0529(11) Uani 1 1 d . . . O15 O 0.6022(3) 0.5694(3) 0.9411(2) 0.0604(12) Uani 1 1 d . . . O16 O 0.6276(3) 0.6050(2) 0.8358(2) 0.0584(12) Uani 1 1 d . . . O17 O 0.6818(2) 0.5033(3) 0.8952(2) 0.0582(12) Uani 1 1 d . . . O18 O 0.5522(2) 0.5081(2) 0.8937(2) 0.0514(11) Uani 1 1 d . . . O19 O 0.8547(5) 0.3411(4) 0.8593(4) 0.124(3) Uani 1 1 d . . . O20 O 0.9202(3) 0.4523(3) 0.8118(3) 0.0796(17) Uani 1 1 d . . . O21 O 0.7902(7) 0.4444(8) 0.8120(9) 0.267(9) Uani 1 1 d . . . O22 O 0.9036(8) 0.4101(3) 0.7518(3) 0.200(7) Uani 1 1 d . . . O23 O 1.0829(13) 0.5611(5) 0.9239(5) 0.300(12) Uani 1 1 d . . . O24 O 1.0453(4) 0.6650(4) 0.8759(5) 0.132(4) Uani 1 1 d . . . O25 O 1.1314(3) 0.6127(5) 0.8237(4) 0.131(3) Uani 1 1 d . . . O26 O 1.0170(4) 0.5679(4) 0.8611(5) 0.131(3) Uani 1 1 d . . . O27 O 0.4578(4) 0.1781(4) 0.8163(5) 0.132(3) Uani 1 1 d . . . O28 O 0.5843(3) 0.1506(3) 0.7910(3) 0.0731(15) Uani 1 1 d . . . O29 O 0.5442(3) 0.2633(2) 0.7846(3) 0.0754(17) Uani 1 1 d . . . O30 O 0.5371(5) 0.1737(4) 0.8775(3) 0.114(3) Uani 1 1 d . . . O31 O 0.7617(2) 0.5230(2) 1.1179(2) 0.0525(10) Uani 1 1 d . . . O32 O 0.61533(18) 0.46959(18) 1.08519(15) 0.0316(7) Uani 1 1 d . . . O33 O 0.5631(2) 0.3890(2) 1.00615(18) 0.0438(9) Uani 1 1 d . . . O34 O 0.7140(2) 0.3611(2) 1.17830(19) 0.0424(9) Uani 1 1 d . . . O35 O 0.7045(2) 0.1114(2) 0.8671(2) 0.0506(10) Uani 1 1 d . . . O36 O 0.8324(2) 0.2294(2) 0.79574(18) 0.0446(9) Uani 1 1 d . . . O37 O 0.7268(3) 0.2116(2) 0.7163(2) 0.0611(12) Uani 1 1 d . . . O38 O 0.8851(3) 0.3060(3) 0.6695(2) 0.0613(12) Uani 1 1 d . . . O39 O 0.9266(2) 0.4347(3) 0.5783(2) 0.0589(12) Uani 1 1 d . . . O40 O 0.5168(2) 0.5478(2) 0.62526(17) 0.0405(9) Uani 1 1 d . . . O41 O 0.5943(2) 0.5776(2) 0.73208(19) 0.0483(10) Uani 1 1 d . . . O42 O 0.7645(5) 0.7690(3) 0.5425(4) 0.117(3) Uani 1 1 d . . . O43 O 0.6149(3) 0.7588(2) 0.6564(2) 0.0587(12) Uani 1 1 d . . . O44 O 0.6134(2) 0.7405(2) 0.93871(18) 0.0412(9) Uani 1 1 d . . . O45 O 0.5527(2) 0.3872(2) 1.24264(18) 0.0451(9) Uani 1 1 d . . . O46 O 0.6839(3) 0.4700(3) 1.2705(2) 0.0740(15) Uani 1 1 d . . . N1 N 0.7208(3) 0.8600(2) 0.8343(2) 0.0386(10) Uani 1 1 d . . . N2 N 0.7501(2) 0.8137(2) 0.94116(19) 0.0318(9) Uani 1 1 d . . . N3 N 0.7656(2) 0.6855(2) 0.96710(19) 0.0305(9) Uani 1 1 d . . . N4 N 0.7604(2) 0.6133(2) 0.97982(19) 0.0305(9) Uani 1 1 d . . . N5 N 0.8767(2) 0.6215(2) 0.91398(19) 0.0328(9) Uani 1 1 d . . . H8 H 0.9099 0.5954 0.8951 0.039 Uiso 1 1 d . . . N6 N 0.7456(2) 0.4854(2) 1.00461(18) 0.0272(8) Uani 1 1 d . . . N7 N 0.7308(2) 0.4188(2) 1.0251(2) 0.0330(9) Uani 1 1 d . . . N8 N 0.7914(2) 0.2525(2) 1.0228(2) 0.0338(9) Uani 1 1 d . . . H11 H 0.8410 0.2660 1.0126 0.038 Uiso 1 1 d . . . N9 N 0.6990(2) 0.2943(2) 1.08429(19) 0.0289(8) Uani 1 1 d . . . N10 N 0.6699(2) 0.2264(2) 1.11305(18) 0.0300(9) Uani 1 1 d . . . N11 N 0.5841(3) 0.1220(2) 1.1599(2) 0.0352(9) Uani 1 1 d . . . N12 N 0.5245(2) 0.1220(2) 1.0729(2) 0.0369(10) Uani 1 1 d . . . N13 N 0.8211(3) 0.1359(3) 1.1370(2) 0.0432(11) Uani 1 1 d . . . N14 N 0.7469(2) 0.0604(2) 1.1060(2) 0.0342(9) Uani 1 1 d . . . N15 N 0.7057(2) 0.1419(2) 1.01028(19) 0.0337(9) Uani 1 1 d . . . N16 N 0.7022(2) 0.1905(2) 0.95209(19) 0.0330(9) Uani 1 1 d . . . N17 N 0.6150(2) 0.2549(2) 0.99649(18) 0.0309(9) Uani 1 1 d . . . H26 H 0.5992 0.3025 0.9864 0.037 Uiso 1 1 d . . . N18 N 0.7108(2) 0.2817(2) 0.84815(18) 0.0323(9) Uani 1 1 d . . . N19 N 0.7173(2) 0.3198(2) 0.7904(2) 0.0337(9) Uani 1 1 d . . . N20 N 0.6476(2) 0.4625(2) 0.67906(19) 0.0375(10) Uani 1 1 d . . . H29 H 0.6282 0.4910 0.7010 0.040 Uiso 1 1 d . . . N21 N 0.7370(2) 0.3739(2) 0.67777(19) 0.0338(9) Uani 1 1 d . . . N22 N 0.7518(3) 0.4048(2) 0.61488(19) 0.0352(10) Uani 1 1 d . . . N23 N 0.7968(3) 0.4619(3) 0.5014(2) 0.0438(12) Uani 1 1 d . . . N24 N 0.8562(3) 0.5762(3) 0.4869(2) 0.0480(12) Uani 1 1 d . . . N25 N 0.5797(2) 0.4188(3) 0.5915(2) 0.0396(11) Uani 1 1 d . . . N26 N 0.6309(2) 0.5343(2) 0.51073(19) 0.0357(10) Uani 1 1 d . . . N27 N 0.6950(2) 0.5873(2) 0.56728(19) 0.0325(9) Uani 1 1 d . . . N28 N 0.7172(2) 0.6168(2) 0.60437(19) 0.0319(9) Uani 1 1 d . . . N29 N 0.8133(3) 0.5336(3) 0.6233(2) 0.0425(11) Uani 1 1 d . . . H44 H 0.8521 0.5265 0.6459 0.050 Uiso 1 1 d . . . N30 N 0.7376(3) 0.6625(2) 0.6839(2) 0.0361(10) Uani 1 1 d . . . N31 N 0.7408(3) 0.6947(2) 0.7218(2) 0.0370(10) Uani 1 1 d . . . N32 N 0.7409(3) 0.7131(2) 0.83735(19) 0.0355(9) Uani 1 1 d . . . H47 H 0.6914 0.6999 0.8373 0.041 Uiso 1 1 d . . . N33 N 0.8640(3) 0.7425(3) 0.7859(2) 0.0401(10) Uani 1 1 d . . . N34 N 0.8825(2) 0.7686(2) 0.8274(2) 0.0356(10) Uani 1 1 d . . . N35 N 0.9362(2) 0.8005(2) 0.9010(2) 0.0367(10) Uani 1 1 d . . . N36 N 0.9413(3) 0.6872(3) 0.9885(2) 0.0402(11) Uani 1 1 d . . . C1 C 0.7034(4) 0.8789(3) 0.7797(3) 0.0505(15) Uani 1 1 d . . . H1 H 0.6978 0.8440 0.7646 0.061 Uiso 1 1 calc R . . C2 C 0.6931(4) 0.9467(4) 0.7442(3) 0.0565(16) Uani 1 1 d . . . H2 H 0.6784 0.9585 0.7061 0.068 Uiso 1 1 calc R . . C3 C 0.7047(4) 0.9972(4) 0.7658(3) 0.0598(18) Uani 1 1 d . . . H3 H 0.6998 1.0445 0.7417 0.072 Uiso 1 1 calc R . . C4 C 0.7230(4) 0.9796(3) 0.8206(3) 0.0536(16) Uani 1 1 d . . . H4 H 0.7302 1.0141 0.8358 0.064 Uiso 1 1 calc R . . C5 C 0.7310(3) 0.9105(3) 0.8546(3) 0.0399(12) Uani 1 1 d . . . C6 C 0.7471(3) 0.8833(3) 0.9171(3) 0.0371(12) Uani 1 1 d . . . C7 C 0.7597(3) 0.9213(3) 0.9509(3) 0.0456(14) Uani 1 1 d . . . H5 H 0.7593 0.9703 0.9343 0.055 Uiso 1 1 calc R . . C8 C 0.7724(4) 0.8869(3) 1.0079(3) 0.0533(16) Uani 1 1 d . . . H6 H 0.7800 0.9123 1.0316 0.064 Uiso 1 1 calc R . . C9 C 0.7747(3) 0.8140(3) 1.0326(3) 0.0441(13) Uani 1 1 d . . . H7 H 0.7840 0.7898 1.0723 0.053 Uiso 1 1 calc R . . C10 C 0.7628(3) 0.7794(3) 0.9967(2) 0.0323(11) Uani 1 1 d . . . C11 C 0.7647(3) 0.7027(3) 1.0141(2) 0.0329(11) Uani 1 1 d . . . C12 C 0.8159(3) 0.5881(3) 0.9501(2) 0.0343(11) Uani 1 1 d . . . C13 C 0.8060(3) 0.5131(3) 0.9636(2) 0.0321(10) Uani 1 1 d . . . C14 C 0.8551(3) 0.4721(3) 0.9391(3) 0.0364(12) Uani 1 1 d . . . H9 H 0.8975 0.4917 0.9084 0.044 Uiso 1 1 calc R . . C15 C 0.8401(3) 0.4020(3) 0.9609(3) 0.0448(14) Uani 1 1 d . . . H10 H 0.8721 0.3720 0.9459 0.054 Uiso 1 1 calc R . . C16 C 0.7770(3) 0.3770(3) 1.0053(2) 0.0307(10) Uani 1 1 d . . . C17 C 0.7553(3) 0.3023(3) 1.0378(2) 0.0311(10) Uani 1 1 d . . . C18 C 0.6638(3) 0.1992(3) 1.1728(2) 0.0324(11) Uani 1 1 d . . . C19 C 0.6180(3) 0.1337(3) 1.1998(2) 0.0338(11) Uani 1 1 d . . . C20 C 0.6078(4) 0.0887(3) 1.2593(3) 0.0482(14) Uani 1 1 d . . . H12 H 0.6329 0.0952 1.2878 0.058 Uiso 1 1 calc R . . C21 C 0.5577(4) 0.0322(3) 1.2754(3) 0.0535(16) Uani 1 1 d . . . H13 H 0.5476 0.0009 1.3161 0.064 Uiso 1 1 calc R . . C22 C 0.5233(4) 0.0218(3) 1.2335(3) 0.0500(15) Uani 1 1 d . . . H14 H 0.4907 -0.0167 1.2447 0.060 Uiso 1 1 calc R . . C23 C 0.5373(3) 0.0679(3) 1.1756(2) 0.0354(11) Uani 1 1 d . . . C24 C 0.5078(3) 0.0676(3) 1.1224(2) 0.0393(12) Uani 1 1 d . . . C25 C 0.4651(4) 0.0123(3) 1.1248(3) 0.0502(15) Uani 1 1 d . . . H15 H 0.4531 -0.0269 1.1609 0.060 Uiso 1 1 calc R . . C26 C 0.4416(4) 0.0171(4) 1.0732(3) 0.0559(16) Uani 1 1 d . . . H16 H 0.4128 -0.0195 1.0736 0.067 Uiso 1 1 calc R . . C27 C 0.4590(3) 0.0743(4) 1.0205(3) 0.0494(15) Uani 1 1 d . . . H17 H 0.4428 0.0779 0.9846 0.059 Uiso 1 1 calc R . . C28 C 0.5014(3) 0.1262(3) 1.0227(3) 0.0388(12) Uani 1 1 d . . . H18 H 0.5143 0.1660 0.9872 0.047 Uiso 1 1 calc R . . C29 C 0.8562(3) 0.1794(3) 1.1499(3) 0.0459(14) Uani 1 1 d . . . H19 H 0.8657 0.2246 1.1205 0.055 Uiso 1 1 calc R . . C30 C 0.8811(4) 0.1634(4) 1.2051(3) 0.0544(17) Uani 1 1 d . . . H20 H 0.9062 0.1969 1.2129 0.065 Uiso 1 1 calc R . . C31 C 0.8680(5) 0.0986(5) 1.2467(3) 0.072(2) Uani 1 1 d . . . H21 H 0.8859 0.0851 1.2837 0.086 Uiso 1 1 calc R . . C32 C 0.8276(4) 0.0511(4) 1.2347(3) 0.0618(18) Uani 1 1 d . . . H22 H 0.8154 0.0063 1.2641 0.074 Uiso 1 1 calc R . . C33 C 0.8066(3) 0.0718(3) 1.1793(3) 0.0438(13) Uani 1 1 d . . . C34 C 0.7620(3) 0.0275(3) 1.1615(3) 0.0458(14) Uani 1 1 d . . . C35 C 0.7349(4) -0.0390(3) 1.1967(3) 0.0549(16) Uani 1 1 d . . . H23 H 0.7458 -0.0623 1.2361 0.066 Uiso 1 1 calc R . . C36 C 0.6915(4) -0.0696(4) 1.1722(3) 0.0576(17) Uani 1 1 d . . . H24 H 0.6719 -0.1148 1.1953 0.069 Uiso 1 1 calc R . . C37 C 0.6760(3) -0.0360(3) 1.1147(3) 0.0465(14) Uani 1 1 d . . . H25 H 0.6466 -0.0576 1.0980 0.056 Uiso 1 1 calc R . . C38 C 0.7047(3) 0.0304(3) 1.0821(2) 0.0359(11) Uani 1 1 d . . . C39 C 0.6884(3) 0.0756(3) 1.0215(2) 0.0339(11) Uani 1 1 d . . . C40 C 0.6591(3) 0.2458(2) 0.9509(2) 0.0297(10) Uani 1 1 d . . . C41 C 0.6642(3) 0.2991(3) 0.8891(2) 0.0308(10) Uani 1 1 d . . . C42 C 0.6242(3) 0.3608(3) 0.8727(2) 0.0321(10) Uani 1 1 d . . . H27 H 0.5934 0.3750 0.9024 0.039 Uiso 1 1 calc R . . C43 C 0.6304(3) 0.4004(3) 0.8127(2) 0.0340(11) Uani 1 1 d . . . H28 H 0.6038 0.4427 0.7996 0.041 Uiso 1 1 calc R . . C44 C 0.6768(3) 0.3769(3) 0.7712(2) 0.0314(10) Uani 1 1 d . . . C45 C 0.6877(3) 0.4088(3) 0.7047(2) 0.0314(10) Uani 1 1 d . . . C46 C 0.7453(3) 0.3647(3) 0.5855(3) 0.0419(13) Uani 1 1 d . . . C47 C 0.7667(3) 0.3991(3) 0.5186(2) 0.0368(12) Uani 1 1 d . . . C48 C 0.7546(4) 0.3727(4) 0.4762(3) 0.0535(16) Uani 1 1 d . . . H30 H 0.7322 0.3286 0.4881 0.064 Uiso 1 1 calc R . . C49 C 0.7769(4) 0.4136(4) 0.4159(3) 0.0633(19) Uani 1 1 d . . . H31 H 0.7707 0.3966 0.3859 0.076 Uiso 1 1 calc R . . C50 C 0.8073(4) 0.4776(4) 0.3987(3) 0.0609(19) Uani 1 1 d . . . H32 H 0.8206 0.5055 0.3572 0.073 Uiso 1 1 calc R . . C51 C 0.8187(3) 0.5019(3) 0.4433(3) 0.0435(13) Uani 1 1 d . . . C52 C 0.8510(4) 0.5671(4) 0.4353(3) 0.0515(15) Uani 1 1 d . . . C53 C 0.8749(5) 0.6180(4) 0.3797(3) 0.067(2) Uani 1 1 d . . . H33 H 0.8709 0.6119 0.3436 0.080 Uiso 1 1 calc R . . C54 C 0.9050(5) 0.6787(4) 0.3778(4) 0.083(3) Uani 1 1 d . . . H34 H 0.9225 0.7140 0.3400 0.100 Uiso 1 1 calc R . . C55 C 0.9096(4) 0.6879(4) 0.4295(4) 0.069(2) Uani 1 1 d . . . H35 H 0.9295 0.7294 0.4284 0.082 Uiso 1 1 calc R . . C56 C 0.8838(4) 0.6336(3) 0.4848(3) 0.0536(16) Uani 1 1 d . . . H36 H 0.8865 0.6390 0.5215 0.064 Uiso 1 1 calc R . . C57 C 0.5565(3) 0.3601(3) 0.6367(2) 0.0409(12) Uani 1 1 d . . . H37 H 0.5612 0.3548 0.6764 0.049 Uiso 1 1 calc R . . C58 C 0.5254(4) 0.3061(3) 0.6281(3) 0.0503(15) Uani 1 1 d . . . H38 H 0.5081 0.2653 0.6614 0.060 Uiso 1 1 calc R . . C59 C 0.5202(4) 0.3127(4) 0.5705(3) 0.0536(16) Uani 1 1 d . . . H39 H 0.5013 0.2758 0.5634 0.064 Uiso 1 1 calc R . . C60 C 0.5429(3) 0.3734(3) 0.5236(3) 0.0462(14) Uani 1 1 d . . . H40 H 0.5379 0.3798 0.4837 0.055 Uiso 1 1 calc R . . C61 C 0.5735(3) 0.4262(3) 0.5353(2) 0.0388(12) Uani 1 1 d . . . C62 C 0.6028(3) 0.4946(3) 0.4883(2) 0.0350(11) Uani 1 1 d . . . C63 C 0.6017(3) 0.5169(3) 0.4264(2) 0.0409(12) Uani 1 1 d . . . H41 H 0.5802 0.4894 0.4100 0.049 Uiso 1 1 calc R . . C64 C 0.6328(4) 0.5802(4) 0.3908(3) 0.0528(16) Uani 1 1 d . . . H42 H 0.6338 0.5967 0.3486 0.063 Uiso 1 1 calc R . . C65 C 0.6637(3) 0.6216(3) 0.4153(2) 0.0441(13) Uani 1 1 d . . . H43 H 0.6854 0.6656 0.3906 0.053 Uiso 1 1 calc R . . C66 C 0.6606(3) 0.5954(3) 0.4761(3) 0.0402(12) Uani 1 1 d . . . C67 C 0.6926(3) 0.6310(3) 0.5101(2) 0.0399(13) Uani 1 1 d . . . C68 C 0.7731(3) 0.5848(3) 0.6327(2) 0.0342(11) Uani 1 1 d . . . C69 C 0.7855(3) 0.6128(3) 0.6788(2) 0.0395(12) Uani 1 1 d . . . C70 C 0.8424(4) 0.5917(4) 0.7115(3) 0.0573(17) Uani 1 1 d . . . H45 H 0.8766 0.5566 0.7071 0.069 Uiso 1 1 calc R . . C71 C 0.8482(4) 0.6230(4) 0.7508(3) 0.0626(19) Uani 1 1 d . . . H46 H 0.8865 0.6101 0.7748 0.075 Uiso 1 1 calc R . . C72 C 0.7958(3) 0.6750(3) 0.7546(2) 0.0400(12) Uani 1 1 d . . . C73 C 0.7982(3) 0.7110(3) 0.7959(2) 0.0360(11) Uani 1 1 d . . . C74 C 0.9030(3) 0.8361(3) 0.8039(3) 0.0414(12) Uani 1 1 d . . . C75 C 0.9330(3) 0.8551(3) 0.8489(3) 0.0401(12) Uani 1 1 d . . . C76 C 0.9574(3) 0.9208(3) 0.8393(3) 0.0468(14) Uani 1 1 d . . . H48 H 0.9547 0.9588 0.8029 0.056 Uiso 1 1 calc R . . C77 C 0.9863(4) 0.9277(3) 0.8866(3) 0.0500(15) Uani 1 1 d . . . H49 H 1.0021 0.9720 0.8825 0.060 Uiso 1 1 calc R . . C78 C 0.9922(3) 0.8721(3) 0.9385(3) 0.0435(13) Uani 1 1 d . . . H50 H 1.0155 0.8766 0.9687 0.052 Uiso 1 1 calc R . . C79 C 0.9627(3) 0.8081(3) 0.9455(3) 0.0422(13) Uani 1 1 d . . . C80 C 0.9629(3) 0.7430(3) 0.9972(3) 0.0399(12) Uani 1 1 d . . . C81 C 0.9812(3) 0.7364(3) 1.0512(3) 0.0495(15) Uani 1 1 d . . . H51 H 0.9964 0.7758 1.0568 0.059 Uiso 1 1 calc R . . C82 C 0.9775(4) 0.6708(4) 1.0985(3) 0.0555(17) Uani 1 1 d . . . H52 H 0.9899 0.6658 1.1362 0.067 Uiso 1 1 calc R . . C83 C 0.9556(3) 0.6144(3) 1.0888(3) 0.0493(15) Uani 1 1 d . . . H53 H 0.9516 0.5700 1.1200 0.059 Uiso 1 1 calc R . . C84 C 0.9396(3) 0.6236(3) 1.0328(3) 0.0453(13) Uani 1 1 d . . . H54 H 0.9272 0.5846 1.0253 0.054 Uiso 1 1 calc R . . C85 C 0.5896(3) 0.6238(3) 1.0984(3) 0.0368(12) Uani 1 1 d . . . C86 C 0.5626(4) 0.6937(3) 1.0996(3) 0.0453(14) Uani 1 1 d . . . H55 H 0.5442 0.7205 1.0622 0.054 Uiso 1 1 calc R . . H56 H 0.6046 0.7184 1.1032 0.054 Uiso 1 1 calc R . . H57 H 0.5216 0.6872 1.1341 0.054 Uiso 1 1 calc R . . C87 C 0.5131(3) 0.2881(3) 1.1531(2) 0.0336(11) Uani 1 1 d . . . C88 C 0.4647(3) 0.2473(3) 1.2125(3) 0.0462(13) Uani 1 1 d . . . H58 H 0.4579 0.2737 1.2389 0.055 Uiso 1 1 calc R . . H59 H 0.4894 0.2034 1.2315 0.055 Uiso 1 1 calc R . . H60 H 0.4153 0.2383 1.2057 0.055 Uiso 1 1 calc R . . C89 C 0.8730(3) 0.1101(3) 0.9557(3) 0.0408(13) Uani 1 1 d . . . C90 C 0.9078(4) 0.0407(3) 0.9793(3) 0.0566(17) Uani 1 1 d . . . H61 H 0.9510 0.0438 0.9973 0.068 Uiso 1 1 calc R . . H62 H 0.9251 0.0243 0.9462 0.068 Uiso 1 1 calc R . . H63 H 0.8703 0.0083 1.0100 0.068 Uiso 1 1 calc R . . C91 C 0.5363(4) 0.7265(3) 0.5603(3) 0.0484(15) Uani 1 1 d . . . C92 C 0.5769(5) 0.7923(4) 0.5176(4) 0.069(2) Uani 1 1 d . . . H64 H 0.6314 0.7837 0.5107 0.083 Uiso 1 1 calc R . . H65 H 0.5669 0.8279 0.5353 0.083 Uiso 1 1 calc R . . H66 H 0.5588 0.8081 0.4792 0.083 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0326(3) 0.0326(3) 0.0348(3) -0.0178(3) -0.0091(2) 0.0022(2) Cu2 0.0256(3) 0.0311(3) 0.0336(3) -0.0157(3) -0.0029(2) 0.0027(2) Cu3 0.0256(3) 0.0311(3) 0.0325(3) -0.0147(3) -0.0017(2) 0.0010(2) Cu4 0.0313(3) 0.0304(3) 0.0291(3) -0.0100(3) -0.0064(2) 0.0011(2) Cu5 0.0331(3) 0.0309(3) 0.0349(3) -0.0132(3) -0.0096(2) 0.0060(2) Cu6 0.0343(3) 0.0355(4) 0.0349(3) -0.0147(3) -0.0082(2) 0.0097(3) Cu7 0.0397(3) 0.0424(4) 0.0341(3) -0.0155(3) -0.0025(3) 0.0107(3) Cu8 0.0359(3) 0.0472(4) 0.0333(3) -0.0214(3) -0.0064(3) 0.0023(3) Cu9 0.0349(3) 0.0412(4) 0.0269(3) -0.0146(3) -0.0090(2) 0.0022(3) Cu10 0.0419(4) 0.0490(4) 0.0435(4) -0.0263(3) -0.0150(3) 0.0096(3) Cu11 0.0292(3) 0.0373(4) 0.0381(3) -0.0164(3) -0.0068(2) -0.0025(3) Cl1 0.0326(6) 0.0466(8) 0.0377(6) -0.0157(6) -0.0103(5) 0.0029(5) Cl2 0.1075(19) 0.106(2) 0.110(2) -0.0375(17) -0.0476(16) -0.0188(16) Cl3 0.0346(8) 0.0911(15) 0.1132(18) -0.0186(14) -0.0010(9) 0.0128(9) Cl4 0.0599(9) 0.0482(9) 0.0558(9) -0.0164(7) -0.0057(7) 0.0098(7) Na1 0.0394(11) 0.0394(12) 0.0363(11) -0.0186(9) -0.0037(8) -0.0005(9) O1 0.044(2) 0.041(2) 0.0336(19) -0.0115(17) -0.0118(16) -0.0038(16) O2 0.0380(19) 0.045(2) 0.038(2) -0.0180(18) -0.0116(15) 0.0031(16) O3 0.053(2) 0.035(2) 0.044(2) -0.0153(18) -0.0135(18) -0.0018(17) O4 0.068(3) 0.052(3) 0.048(2) -0.027(2) -0.014(2) 0.006(2) O5 0.055(2) 0.047(3) 0.037(2) -0.0078(19) -0.0057(18) -0.005(2) O6 0.066(3) 0.041(2) 0.044(2) -0.013(2) -0.008(2) -0.005(2) O7 0.0306(17) 0.043(2) 0.0346(19) -0.0200(17) -0.0050(14) 0.0081(15) O8 0.055(2) 0.039(2) 0.037(2) -0.0155(18) -0.0031(17) 0.0050(18) O9 0.0301(17) 0.038(2) 0.0359(19) -0.0196(16) -0.0041(14) -0.0001(15) O10 0.0313(18) 0.051(2) 0.041(2) -0.0173(19) -0.0086(15) -0.0056(16) O11 0.046(2) 0.047(2) 0.049(2) -0.022(2) -0.0144(18) 0.0170(18) O12 0.0358(19) 0.044(2) 0.060(3) -0.030(2) -0.0141(17) 0.0096(17) O13 0.044(2) 0.049(2) 0.053(2) -0.022(2) -0.0209(19) 0.0151(18) O14 0.058(3) 0.060(3) 0.048(2) -0.022(2) -0.025(2) 0.015(2) O15 0.062(3) 0.074(3) 0.056(3) -0.035(3) -0.021(2) 0.019(2) O16 0.062(3) 0.056(3) 0.042(2) 0.005(2) -0.015(2) -0.017(2) O17 0.038(2) 0.081(3) 0.061(3) -0.032(3) -0.0169(19) 0.019(2) O18 0.036(2) 0.040(2) 0.078(3) -0.018(2) -0.016(2) 0.0006(17) O19 0.152(8) 0.119(6) 0.099(6) -0.029(5) -0.024(5) -0.045(6) O20 0.073(3) 0.062(3) 0.106(5) -0.022(3) -0.034(3) -0.015(3) O21 0.116(9) 0.275(16) 0.51(3) -0.223(19) -0.142(13) 0.065(10) O22 0.52(2) 0.043(3) 0.037(3) -0.015(3) -0.062(7) 0.055(7) O23 0.74(4) 0.072(6) 0.129(9) -0.026(6) -0.194(16) 0.015(11) O24 0.068(4) 0.102(5) 0.236(10) -0.109(6) 0.060(5) -0.034(4) O25 0.046(3) 0.249(10) 0.151(7) -0.140(8) -0.008(4) 0.018(5) O26 0.067(4) 0.134(6) 0.213(10) -0.108(7) 0.029(5) -0.023(4) O27 0.080(5) 0.092(5) 0.218(10) -0.050(6) -0.029(6) 0.002(4) O28 0.071(3) 0.065(3) 0.085(4) -0.040(3) 0.005(3) 0.009(3) O29 0.100(4) 0.034(3) 0.074(4) -0.018(2) 0.018(3) 0.003(2) O30 0.150(7) 0.129(6) 0.045(3) -0.022(3) -0.025(4) 0.080(5) O31 0.045(2) 0.057(3) 0.050(2) -0.015(2) -0.0050(19) -0.002(2) O32 0.0252(15) 0.040(2) 0.0309(17) -0.0147(16) -0.0059(13) 0.0029(14) O33 0.043(2) 0.040(2) 0.045(2) -0.0160(18) -0.0020(17) 0.0055(17) O34 0.0323(18) 0.047(2) 0.052(2) -0.0241(19) -0.0069(16) 0.0022(16) O35 0.051(2) 0.052(3) 0.054(3) -0.024(2) -0.013(2) 0.0000(19) O36 0.044(2) 0.041(2) 0.041(2) -0.0119(18) -0.0021(17) 0.0096(17) O37 0.063(3) 0.055(3) 0.071(3) -0.031(3) -0.010(2) 0.003(2) O38 0.049(2) 0.067(3) 0.055(3) -0.019(2) 0.010(2) 0.010(2) O39 0.042(2) 0.078(3) 0.058(3) -0.030(3) -0.006(2) 0.012(2) O40 0.047(2) 0.047(2) 0.0350(19) -0.0220(18) -0.0136(16) 0.0076(17) O41 0.041(2) 0.060(3) 0.050(2) -0.027(2) -0.0106(18) 0.0052(19) O42 0.193(9) 0.066(4) 0.120(6) -0.037(4) -0.085(6) 0.002(5) O43 0.078(3) 0.056(3) 0.048(3) -0.027(2) -0.016(2) 0.020(2) O44 0.0316(18) 0.046(2) 0.047(2) -0.0181(19) -0.0096(16) -0.0004(16) O45 0.039(2) 0.054(2) 0.041(2) -0.0192(19) 0.0011(16) -0.0051(18) O46 0.089(4) 0.083(4) 0.060(3) -0.025(3) -0.038(3) -0.003(3) N1 0.039(2) 0.041(3) 0.042(2) -0.020(2) -0.0107(19) 0.0021(19) N2 0.0279(19) 0.035(2) 0.037(2) -0.020(2) -0.0051(16) 0.0048(17) N3 0.0286(19) 0.030(2) 0.035(2) -0.0142(18) -0.0054(16) -0.0008(16) N4 0.0298(19) 0.032(2) 0.039(2) -0.0238(19) -0.0067(17) 0.0043(17) N5 0.0238(19) 0.036(2) 0.036(2) -0.0136(19) 0.0020(16) -0.0027(17) N6 0.0302(19) 0.027(2) 0.028(2) -0.0139(17) -0.0057(15) -0.0002(16) N7 0.0278(19) 0.036(2) 0.039(2) -0.018(2) -0.0098(17) 0.0085(17) N8 0.029(2) 0.038(2) 0.040(2) -0.020(2) -0.0076(17) 0.0054(17) N9 0.0291(19) 0.018(2) 0.036(2) -0.0068(17) -0.0027(16) -0.0021(15) N10 0.036(2) 0.027(2) 0.029(2) -0.0111(17) -0.0090(16) 0.0025(17) N11 0.041(2) 0.025(2) 0.035(2) -0.0083(19) -0.0048(18) 0.0000(18) N12 0.030(2) 0.037(3) 0.049(3) -0.022(2) -0.0081(18) 0.0073(18) N13 0.039(2) 0.053(3) 0.044(3) -0.025(2) -0.013(2) 0.007(2) N14 0.040(2) 0.026(2) 0.038(2) -0.0127(19) -0.0137(18) 0.0079(18) N15 0.035(2) 0.035(2) 0.032(2) -0.0130(19) -0.0092(17) 0.0048(18) N16 0.040(2) 0.030(2) 0.028(2) -0.0093(18) -0.0090(17) 0.0035(18) N17 0.038(2) 0.027(2) 0.0238(19) -0.0059(17) -0.0044(16) 0.0039(17) N18 0.038(2) 0.033(2) 0.0211(19) -0.0062(17) -0.0029(16) 0.0064(18) N19 0.034(2) 0.034(2) 0.040(2) -0.019(2) -0.0136(18) 0.0096(18) N20 0.035(2) 0.049(3) 0.031(2) -0.020(2) -0.0059(17) 0.0113(19) N21 0.040(2) 0.034(2) 0.027(2) -0.0111(18) -0.0031(17) -0.0002(18) N22 0.043(2) 0.041(3) 0.028(2) -0.022(2) -0.0086(18) 0.0083(19) N23 0.039(2) 0.064(3) 0.032(2) -0.023(2) -0.0069(19) 0.010(2) N24 0.033(2) 0.058(3) 0.045(3) -0.015(2) 0.005(2) -0.001(2) N25 0.032(2) 0.054(3) 0.046(3) -0.030(2) -0.0181(19) 0.007(2) N26 0.030(2) 0.049(3) 0.031(2) -0.018(2) -0.0055(17) -0.0010(19) N27 0.033(2) 0.036(2) 0.031(2) -0.0152(19) -0.0080(17) -0.0018(17) N28 0.038(2) 0.035(2) 0.032(2) -0.0204(19) -0.0108(17) 0.0007(18) N29 0.038(2) 0.052(3) 0.048(3) -0.031(2) -0.011(2) 0.010(2) N30 0.044(2) 0.035(2) 0.033(2) -0.018(2) -0.0040(18) -0.0062(19) N31 0.042(2) 0.036(3) 0.037(2) -0.017(2) -0.0098(19) 0.0006(19) N32 0.042(2) 0.036(2) 0.030(2) -0.0125(19) -0.0127(18) 0.0012(19) N33 0.040(2) 0.045(3) 0.038(2) -0.017(2) -0.0057(19) -0.007(2) N34 0.040(2) 0.035(3) 0.042(2) -0.023(2) -0.0118(19) -0.0047(19) N35 0.029(2) 0.039(3) 0.041(2) -0.013(2) -0.0065(18) -0.0077(18) N36 0.036(2) 0.057(3) 0.034(2) -0.023(2) -0.0107(18) 0.001(2) C1 0.058(4) 0.048(4) 0.049(3) -0.021(3) -0.018(3) 0.014(3) C2 0.065(4) 0.059(4) 0.044(3) -0.013(3) -0.020(3) 0.009(3) C3 0.069(4) 0.042(4) 0.058(4) -0.004(3) -0.018(3) -0.002(3) C4 0.058(4) 0.035(3) 0.065(4) -0.012(3) -0.019(3) 0.005(3) C5 0.035(3) 0.044(3) 0.045(3) -0.022(3) -0.008(2) 0.005(2) C6 0.031(2) 0.035(3) 0.048(3) -0.021(3) -0.002(2) 0.004(2) C7 0.045(3) 0.042(3) 0.060(4) -0.032(3) -0.005(3) 0.001(3) C8 0.055(4) 0.053(4) 0.063(4) -0.038(3) -0.004(3) -0.003(3) C9 0.041(3) 0.053(4) 0.049(3) -0.029(3) -0.012(2) 0.000(3) C10 0.027(2) 0.037(3) 0.034(3) -0.016(2) -0.0035(19) 0.002(2) C11 0.028(2) 0.034(3) 0.044(3) -0.024(2) -0.007(2) 0.005(2) C12 0.027(2) 0.048(3) 0.035(3) -0.020(2) -0.0106(19) 0.000(2) C13 0.029(2) 0.030(3) 0.037(3) -0.014(2) -0.005(2) 0.0032(19) C14 0.027(2) 0.036(3) 0.046(3) -0.021(2) 0.005(2) 0.001(2) C15 0.042(3) 0.034(3) 0.053(3) -0.019(3) 0.006(2) 0.005(2) C16 0.032(2) 0.025(3) 0.037(3) -0.014(2) -0.007(2) 0.0004(19) C17 0.027(2) 0.035(3) 0.035(3) -0.018(2) -0.0050(19) 0.0040(19) C18 0.035(2) 0.038(3) 0.024(2) -0.010(2) -0.0108(19) 0.010(2) C19 0.039(3) 0.032(3) 0.030(3) -0.013(2) -0.005(2) 0.005(2) C20 0.066(4) 0.039(3) 0.040(3) -0.014(3) -0.014(3) 0.008(3) C21 0.073(4) 0.044(4) 0.032(3) -0.001(3) -0.002(3) -0.020(3) C22 0.061(4) 0.043(4) 0.045(3) -0.018(3) -0.003(3) -0.009(3) C23 0.035(3) 0.029(3) 0.035(3) -0.005(2) -0.002(2) -0.003(2) C24 0.038(3) 0.044(3) 0.033(3) -0.011(2) -0.007(2) 0.003(2) C25 0.048(3) 0.050(4) 0.052(4) -0.021(3) 0.001(3) -0.012(3) C26 0.047(3) 0.061(4) 0.062(4) -0.023(4) -0.011(3) -0.010(3) C27 0.037(3) 0.062(4) 0.061(4) -0.036(3) -0.009(3) 0.000(3) C28 0.038(3) 0.040(3) 0.042(3) -0.018(3) -0.011(2) 0.002(2) C29 0.042(3) 0.050(4) 0.056(4) -0.031(3) -0.015(3) 0.014(3) C30 0.060(4) 0.068(5) 0.055(4) -0.042(4) -0.023(3) 0.014(3) C31 0.072(5) 0.096(6) 0.052(4) -0.023(4) -0.034(4) 0.008(4) C32 0.071(5) 0.065(5) 0.051(4) -0.017(3) -0.030(3) 0.014(4) C33 0.050(3) 0.042(3) 0.042(3) -0.018(3) -0.012(2) 0.009(3) C34 0.046(3) 0.047(4) 0.038(3) -0.011(3) -0.008(2) 0.011(3) C35 0.076(4) 0.048(4) 0.039(3) -0.013(3) -0.014(3) 0.006(3) C36 0.076(5) 0.047(4) 0.042(3) -0.006(3) -0.013(3) -0.001(3) C37 0.046(3) 0.033(3) 0.056(4) -0.011(3) -0.009(3) -0.001(2) C38 0.037(3) 0.030(3) 0.042(3) -0.017(2) -0.002(2) 0.003(2) C39 0.035(2) 0.033(3) 0.034(3) -0.015(2) -0.003(2) 0.001(2) C40 0.029(2) 0.025(2) 0.031(2) -0.006(2) -0.0045(18) 0.0019(18) C41 0.034(2) 0.032(3) 0.028(2) -0.012(2) -0.0075(19) -0.001(2) C42 0.034(2) 0.035(3) 0.031(2) -0.015(2) -0.0094(19) 0.004(2) C43 0.040(3) 0.030(3) 0.033(3) -0.012(2) -0.012(2) 0.010(2) C44 0.031(2) 0.040(3) 0.029(2) -0.017(2) -0.0090(19) 0.006(2) C45 0.034(2) 0.033(3) 0.029(2) -0.012(2) -0.0084(19) 0.005(2) C46 0.037(3) 0.050(4) 0.042(3) -0.023(3) -0.007(2) 0.010(2) C47 0.042(3) 0.044(3) 0.034(3) -0.023(2) -0.013(2) 0.006(2) C48 0.056(4) 0.064(4) 0.052(4) -0.033(3) -0.013(3) 0.002(3) C49 0.071(4) 0.090(6) 0.044(4) -0.042(4) -0.014(3) 0.009(4) C50 0.060(4) 0.088(6) 0.031(3) -0.019(3) -0.006(3) 0.004(4) C51 0.037(3) 0.061(4) 0.036(3) -0.024(3) -0.005(2) 0.002(3) C52 0.047(3) 0.066(4) 0.037(3) -0.017(3) -0.005(2) 0.006(3) C53 0.076(5) 0.082(6) 0.033(3) -0.013(3) 0.003(3) -0.019(4) C54 0.088(6) 0.063(5) 0.066(5) 0.003(4) 0.010(4) -0.008(4) C55 0.059(4) 0.067(5) 0.070(5) -0.021(4) 0.004(4) -0.009(4) C56 0.049(3) 0.047(4) 0.062(4) -0.021(3) -0.004(3) 0.003(3) C57 0.041(3) 0.045(3) 0.032(3) -0.009(3) -0.008(2) -0.001(2) C58 0.057(4) 0.039(3) 0.052(4) -0.016(3) -0.003(3) -0.007(3) C59 0.058(4) 0.050(4) 0.060(4) -0.031(3) -0.004(3) -0.008(3) C60 0.043(3) 0.061(4) 0.046(3) -0.030(3) -0.014(2) 0.004(3) C61 0.033(2) 0.052(3) 0.039(3) -0.026(3) -0.006(2) 0.003(2) C62 0.037(2) 0.034(3) 0.038(3) -0.017(2) -0.009(2) 0.001(2) C63 0.046(3) 0.046(3) 0.036(3) -0.016(3) -0.015(2) -0.007(3) C64 0.055(3) 0.078(5) 0.038(3) -0.029(3) -0.023(3) 0.002(3) C65 0.045(3) 0.058(4) 0.027(3) -0.014(3) -0.008(2) 0.009(3) C66 0.036(3) 0.049(3) 0.038(3) -0.018(3) -0.012(2) 0.007(2) C67 0.041(3) 0.054(4) 0.024(2) -0.014(2) -0.005(2) 0.004(3) C68 0.037(3) 0.040(3) 0.032(3) -0.019(2) -0.006(2) -0.005(2) C69 0.047(3) 0.047(3) 0.032(3) -0.022(2) -0.012(2) 0.010(2) C70 0.064(4) 0.062(4) 0.068(4) -0.042(4) -0.032(3) 0.020(3) C71 0.067(4) 0.077(5) 0.071(5) -0.050(4) -0.041(4) 0.027(4) C72 0.049(3) 0.041(3) 0.036(3) -0.016(2) -0.015(2) -0.006(2) C73 0.042(3) 0.038(3) 0.032(3) -0.017(2) -0.010(2) -0.002(2) C74 0.045(3) 0.035(3) 0.038(3) -0.010(2) 0.000(2) -0.008(2) C75 0.037(3) 0.038(3) 0.044(3) -0.015(3) -0.005(2) -0.001(2) C76 0.041(3) 0.048(4) 0.057(4) -0.026(3) -0.007(3) -0.006(3) C77 0.054(3) 0.037(3) 0.074(4) -0.034(3) -0.022(3) 0.008(3) C78 0.037(3) 0.047(3) 0.062(4) -0.037(3) -0.009(3) -0.001(2) C79 0.029(2) 0.055(4) 0.054(3) -0.029(3) -0.018(2) 0.007(2) C80 0.026(2) 0.054(4) 0.049(3) -0.029(3) -0.010(2) 0.001(2) C81 0.036(3) 0.056(4) 0.061(4) -0.025(3) -0.014(3) 0.006(3) C82 0.045(3) 0.082(5) 0.056(4) -0.041(4) -0.020(3) 0.011(3) C83 0.036(3) 0.057(4) 0.044(3) -0.005(3) -0.015(2) 0.012(3) C84 0.039(3) 0.052(4) 0.044(3) -0.014(3) -0.013(2) 0.001(3) C85 0.028(2) 0.046(3) 0.044(3) -0.025(3) -0.008(2) 0.005(2) C86 0.054(3) 0.045(3) 0.037(3) -0.020(3) -0.006(2) 0.014(3) C87 0.023(2) 0.041(3) 0.034(3) -0.011(2) -0.0047(18) 0.003(2) C88 0.047(3) 0.042(3) 0.049(3) -0.018(3) -0.005(3) -0.001(3) C89 0.025(2) 0.049(3) 0.052(3) -0.020(3) -0.013(2) 0.004(2) C90 0.073(4) 0.043(4) 0.067(4) -0.026(3) -0.041(4) 0.023(3) C91 0.057(4) 0.048(4) 0.046(3) -0.020(3) -0.023(3) 0.018(3) C92 0.077(5) 0.057(5) 0.077(5) -0.026(4) -0.023(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.945(4) . ? Cu1 N32 1.953(4) . ? Cu1 N3 2.033(4) . ? Cu1 N1 2.069(5) . ? Cu1 O44 2.237(4) . ? Cu2 O7 1.928(3) . ? Cu2 O32 1.928(4) . ? Cu2 N6 1.994(4) . ? Cu2 N4 1.998(4) . ? Cu2 Na1 3.265(2) . ? Cu3 O32 1.937(4) . ? Cu3 O9 1.951(4) . ? Cu3 N9 1.975(4) . ? Cu3 N7 1.980(4) . ? Cu3 Na1 3.393(2) . ? Cu4 N17 1.925(4) . ? Cu4 N11 1.935(4) . ? Cu4 N10 2.000(4) . ? Cu4 N12 2.061(5) . ? Cu5 N8 1.900(5) . ? Cu5 N14 1.920(4) . ? Cu5 N15 2.014(4) . ? Cu5 N13 2.061(5) . ? Cu6 O36 1.936(4) . ? Cu6 O11 1.944(4) . ? Cu6 N16 1.992(4) . ? Cu6 N18 2.004(4) . ? Cu6 O35 2.379(4) . ? Cu7 O36 1.927(4) . ? Cu7 O38 1.941(4) . ? Cu7 N21 1.977(4) . ? Cu7 N19 1.979(4) . ? Cu7 O37 2.427(5) . ? Cu8 N29 1.921(5) . ? Cu8 N23 1.940(5) . ? Cu8 N22 2.047(5) . ? Cu8 N24 2.072(5) . ? Cu8 O39 2.390(4) . ? Cu9 N20 1.931(4) . ? Cu9 N26 1.939(4) . ? Cu9 N27 2.014(4) . ? Cu9 N25 2.062(5) . ? Cu9 O40 2.358(4) . ? Cu10 O13 1.932(4) . ? Cu10 O43 1.935(4) . ? Cu10 N28 1.957(4) . ? Cu10 N30 1.996(5) . ? Cu11 N5 1.918(4) . ? Cu11 N35 1.925(5) . ? Cu11 N34 1.986(5) . ? Cu11 N36 2.053(4) . ? Cl1 O17 1.426(4) . ? Cl1 O15 1.430(5) . ? Cl1 O18 1.433(4) . ? Cl1 O16 1.441(4) . ? Cl2 O20 1.411(6) . ? Cl2 O22 1.415(8) . ? Cl2 O19 1.462(8) . ? Cl2 O21 1.528(12) . ? Cl3 O23 1.226(10) . ? Cl3 O24 1.336(7) . ? Cl3 O25 1.401(7) . ? Cl3 O26 1.524(8) . ? Cl4 O27 1.354(8) . ? Cl4 O29 1.401(5) . ? Cl4 O30 1.406(6) . ? Cl4 O28 1.486(5) . ? Na1 O31 2.324(5) . ? Na1 O8 2.368(4) . ? Na1 O45 2.394(4) . ? Na1 O34 2.403(4) . ? Na1 O46 2.450(5) . ? Na1 O32 2.457(4) . ? O1 C11 1.258(6) . ? O2 C18 1.238(6) . ? O3 C39 1.240(6) . ? O4 C46 1.265(8) . ? O5 C67 1.247(7) . ? O6 C74 1.234(7) . ? O7 C85 1.254(6) . ? O8 C85 1.241(7) . ? O9 C87 1.288(6) . ? O10 C87 1.240(6) . ? O11 C89 1.294(7) . ? O12 C89 1.227(7) . ? O13 C91 1.281(7) . ? O14 C91 1.255(8) . ? N1 C1 1.331(8) . ? N1 C5 1.356(7) . ? N2 C10 1.329(7) . ? N2 C6 1.350(7) . ? N3 C11 1.319(6) . ? N3 N4 1.427(6) . ? N4 C12 1.319(6) . ? N5 C12 1.317(7) . ? N5 H8 0.9517 . ? N6 N7 1.319(6) . ? N6 C13 1.322(6) . ? N7 C16 1.322(6) . ? N8 C17 1.319(6) . ? N8 H11 0.9149 . ? N9 C17 1.332(6) . ? N9 N10 1.412(6) . ? N10 C18 1.333(6) . ? N11 C19 1.340(7) . ? N11 C23 1.349(7) . ? N12 C24 1.310(7) . ? N12 C28 1.337(7) . ? N13 C29 1.303(8) . ? N13 C33 1.353(8) . ? N14 C34 1.338(7) . ? N14 C38 1.347(7) . ? N15 C39 1.354(7) . ? N15 N16 1.409(6) . ? N16 C40 1.343(6) . ? N17 C40 1.302(6) . ? N17 H26 0.9688 . ? N18 N19 1.315(6) . ? N18 C41 1.319(6) . ? N19 C44 1.329(6) . ? N20 C45 1.307(7) . ? N20 H29 0.9482 . ? N21 C45 1.342(6) . ? N21 N22 1.398(6) . ? N22 C46 1.311(7) . ? N23 C47 1.338(8) . ? N23 C51 1.342(8) . ? N24 C56 1.311(9) . ? N24 C52 1.358(8) . ? N25 C57 1.330(7) . ? N25 C61 1.345(7) . ? N26 C66 1.320(8) . ? N26 C62 1.322(7) . ? N27 C67 1.356(7) . ? N27 N28 1.394(6) . ? N28 C68 1.329(7) . ? N29 C68 1.317(7) . ? N29 H44 0.9423 . ? N30 C69 1.332(7) . ? N30 N31 1.342(6) . ? N31 C72 1.338(7) . ? N32 C73 1.308(7) . ? N32 H47 0.9526 . ? N33 C73 1.331(7) . ? N33 N34 1.413(6) . ? N34 C74 1.357(7) . ? N35 C79 1.329(7) . ? N35 C75 1.359(7) . ? N36 C80 1.354(7) . ? N36 C84 1.360(8) . ? C1 C2 1.377(9) . ? C1 H1 0.9500 . ? C2 C3 1.388(10) . ? C2 H2 0.9500 . ? C3 C4 1.345(10) . ? C3 H3 0.9500 . ? C4 C5 1.384(8) . ? C4 H4 0.9500 . ? C5 C6 1.491(8) . ? C6 C7 1.393(8) . ? C7 C8 1.359(10) . ? C7 H5 0.9500 . ? C8 C9 1.414(9) . ? C8 H6 0.9500 . ? C9 C10 1.378(7) . ? C9 H7 0.9500 . ? C10 C11 1.497(7) . ? C12 C13 1.490(8) . ? C13 C14 1.397(7) . ? C14 C15 1.383(8) . ? C14 H9 0.9500 . ? C15 C16 1.384(8) . ? C15 H10 0.9500 . ? C16 C17 1.501(7) . ? C18 C19 1.503(8) . ? C19 C20 1.383(8) . ? C20 C21 1.424(9) . ? C20 H12 0.9500 . ? C21 C22 1.378(9) . ? C21 H13 0.9500 . ? C22 C23 1.362(8) . ? C22 H14 0.9500 . ? C23 C24 1.493(8) . ? C24 C25 1.407(9) . ? C25 C26 1.367(9) . ? C25 H15 0.9500 . ? C26 C27 1.384(10) . ? C26 H16 0.9500 . ? C27 C28 1.390(8) . ? C27 H17 0.9500 . ? C28 H18 0.9500 . ? C29 C30 1.411(9) . ? C29 H19 0.9500 . ? C30 C31 1.356(11) . ? C30 H20 0.9500 . ? C31 C32 1.412(11) . ? C31 H21 0.9500 . ? C32 C33 1.375(9) . ? C32 H22 0.9500 . ? C33 C34 1.492(9) . ? C34 C35 1.393(9) . ? C35 C36 1.385(10) . ? C35 H23 0.9500 . ? C36 C37 1.382(9) . ? C36 H24 0.9500 . ? C37 C38 1.392(8) . ? C37 H25 0.9500 . ? C38 C39 1.497(8) . ? C40 C41 1.487(7) . ? C41 C42 1.393(7) . ? C42 C43 1.369(7) . ? C42 H27 0.9500 . ? C43 C44 1.397(7) . ? C43 H28 0.9500 . ? C44 C45 1.477(7) . ? C46 C47 1.494(8) . ? C47 C48 1.395(8) . ? C48 C49 1.386(10) . ? C48 H30 0.9500 . ? C49 C50 1.362(11) . ? C49 H31 0.9500 . ? C50 C51 1.409(9) . ? C50 H32 0.9500 . ? C51 C52 1.450(10) . ? C52 C53 1.382(9) . ? C53 C54 1.394(12) . ? C53 H33 0.9500 . ? C54 C55 1.360(13) . ? C54 H34 0.9500 . ? C55 C56 1.414(10) . ? C55 H35 0.9500 . ? C56 H36 0.9500 . ? C57 C58 1.394(9) . ? C57 H37 0.9500 . ? C58 C59 1.376(9) . ? C58 H38 0.9500 . ? C59 C60 1.373(10) . ? C59 H39 0.9500 . ? C60 C61 1.406(8) . ? C60 H40 0.9500 . ? C61 C62 1.508(8) . ? C62 C63 1.402(7) . ? C63 C64 1.367(9) . ? C63 H41 0.9500 . ? C64 C65 1.412(9) . ? C64 H42 0.9500 . ? C65 C66 1.362(8) . ? C65 H43 0.9500 . ? C66 C67 1.507(8) . ? C68 C69 1.504(7) . ? C69 C70 1.368(8) . ? C70 C71 1.366(9) . ? C70 H45 0.9500 . ? C71 C72 1.408(9) . ? C71 H46 0.9500 . ? C72 C73 1.472(7) . ? C74 C75 1.494(8) . ? C75 C76 1.390(8) . ? C76 C77 1.409(9) . ? C76 H48 0.9500 . ? C77 C78 1.375(9) . ? C77 H49 0.9500 . ? C78 C79 1.411(8) . ? C78 H50 0.9500 . ? C79 C80 1.467(9) . ? C80 C81 1.370(8) . ? C81 C82 1.417(10) . ? C81 H51 0.9500 . ? C82 C83 1.383(10) . ? C82 H52 0.9500 . ? C83 C84 1.386(8) . ? C83 H53 0.9500 . ? C84 H54 0.9500 . ? C85 C86 1.516(8) . ? C86 H55 0.9800 . ? C86 H56 0.9800 . ? C86 H57 0.9800 . ? C87 C88 1.504(8) . ? C88 H58 0.9800 . ? C88 H59 0.9800 . ? C88 H60 0.9800 . ? C89 C90 1.488(8) . ? C90 H61 0.9800 . ? C90 H62 0.9800 . ? C90 H63 0.9800 . ? C91 C92 1.509(10) . ? C92 H64 0.9800 . ? C92 H65 0.9800 . ? C92 H66 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N32 167.88(18) . . ? N2 Cu1 N3 78.61(17) . . ? N32 Cu1 N3 102.29(17) . . ? N2 Cu1 N1 79.11(18) . . ? N32 Cu1 N1 98.27(18) . . ? N3 Cu1 N1 156.97(17) . . ? N2 Cu1 O44 91.71(16) . . ? N32 Cu1 O44 100.37(17) . . ? N3 Cu1 O44 89.33(15) . . ? N1 Cu1 O44 97.11(16) . . ? O7 Cu2 O32 100.68(15) . . ? O7 Cu2 N6 170.71(16) . . ? O32 Cu2 N6 87.16(15) . . ? O7 Cu2 N4 94.01(16) . . ? O32 Cu2 N4 164.53(15) . . ? N6 Cu2 N4 78.67(16) . . ? O7 Cu2 Na1 88.56(12) . . ? O32 Cu2 Na1 48.50(11) . . ? N6 Cu2 Na1 100.43(12) . . ? N4 Cu2 Na1 127.93(13) . . ? O32 Cu3 O9 95.69(14) . . ? O32 Cu3 N9 163.81(15) . . ? O9 Cu3 N9 98.42(16) . . ? O32 Cu3 N7 87.17(16) . . ? O9 Cu3 N7 176.03(16) . . ? N9 Cu3 N7 78.38(17) . . ? O32 Cu3 Na1 45.40(11) . . ? O9 Cu3 Na1 81.29(11) . . ? N9 Cu3 Na1 129.45(13) . . ? N7 Cu3 Na1 98.87(13) . . ? N17 Cu4 N11 179.8(2) . . ? N17 Cu4 N10 100.50(18) . . ? N11 Cu4 N10 79.66(18) . . ? N17 Cu4 N12 100.49(19) . . ? N11 Cu4 N12 79.36(19) . . ? N10 Cu4 N12 158.91(18) . . ? N8 Cu5 N14 174.50(18) . . ? N8 Cu5 N15 100.15(18) . . ? N14 Cu5 N15 79.92(18) . . ? N8 Cu5 N13 100.3(2) . . ? N14 Cu5 N13 78.9(2) . . ? N15 Cu5 N13 157.9(2) . . ? O36 Cu6 O11 96.26(17) . . ? O36 Cu6 N16 164.15(17) . . ? O11 Cu6 N16 99.09(18) . . ? O36 Cu6 N18 86.35(16) . . ? O11 Cu6 N18 173.95(18) . . ? N16 Cu6 N18 78.00(17) . . ? O36 Cu6 O35 96.37(17) . . ? O11 Cu6 O35 82.92(17) . . ? N16 Cu6 O35 89.44(17) . . ? N18 Cu6 O35 102.25(17) . . ? O36 Cu7 O38 96.17(19) . . ? O36 Cu7 N21 165.92(17) . . ? O38 Cu7 N21 97.47(19) . . ? O36 Cu7 N19 87.40(17) . . ? O38 Cu7 N19 161.6(2) . . ? N21 Cu7 N19 78.55(17) . . ? O36 Cu7 O37 89.70(18) . . ? O38 Cu7 O37 99.1(2) . . ? N21 Cu7 O37 91.55(18) . . ? N19 Cu7 O37 98.91(18) . . ? N29 Cu8 N23 173.6(2) . . ? N29 Cu8 N22 101.38(19) . . ? N23 Cu8 N22 79.44(19) . . ? N29 Cu8 N24 99.4(2) . . ? N23 Cu8 N24 79.2(2) . . ? N22 Cu8 N24 158.2(2) . . ? N29 Cu8 O39 93.11(18) . . ? N23 Cu8 O39 93.26(18) . . ? N22 Cu8 O39 89.90(18) . . ? N24 Cu8 O39 95.44(18) . . ? N20 Cu9 N26 173.09(18) . . ? N20 Cu9 N27 99.08(19) . . ? N26 Cu9 N27 79.47(18) . . ? N20 Cu9 N25 100.9(2) . . ? N26 Cu9 N25 79.67(19) . . ? N27 Cu9 N25 158.24(18) . . ? N20 Cu9 O40 90.22(15) . . ? N26 Cu9 O40 96.65(16) . . ? N27 Cu9 O40 96.68(16) . . ? N25 Cu9 O40 91.81(16) . . ? O13 Cu10 O43 90.62(19) . . ? O13 Cu10 N28 96.73(17) . . ? O43 Cu10 N28 168.5(2) . . ? O13 Cu10 N30 166.26(19) . . ? O43 Cu10 N30 94.53(19) . . ? N28 Cu10 N30 80.33(17) . . ? N5 Cu11 N35 178.89(19) . . ? N5 Cu11 N34 100.38(18) . . ? N35 Cu11 N34 79.40(18) . . ? N5 Cu11 N36 101.2(2) . . ? N35 Cu11 N36 79.0(2) . . ? N34 Cu11 N36 158.37(19) . . ? O17 Cl1 O15 110.2(3) . . ? O17 Cl1 O18 109.6(3) . . ? O15 Cl1 O18 109.3(3) . . ? O17 Cl1 O16 110.0(3) . . ? O15 Cl1 O16 109.4(3) . . ? O18 Cl1 O16 108.3(3) . . ? O20 Cl2 O22 92.5(6) . . ? O20 Cl2 O19 116.3(4) . . ? O22 Cl2 O19 119.1(5) . . ? O20 Cl2 O21 106.5(6) . . ? O22 Cl2 O21 116.6(9) . . ? O19 Cl2 O21 105.2(9) . . ? O23 Cl3 O24 116.3(8) . . ? O23 Cl3 O25 120.4(10) . . ? O24 Cl3 O25 113.9(6) . . ? O23 Cl3 O26 97.0(9) . . ? O24 Cl3 O26 106.6(5) . . ? O25 Cl3 O26 97.6(5) . . ? O27 Cl4 O29 109.7(5) . . ? O27 Cl4 O30 107.7(6) . . ? O29 Cl4 O30 111.5(5) . . ? O27 Cl4 O28 110.6(5) . . ? O29 Cl4 O28 110.4(3) . . ? O30 Cl4 O28 106.9(4) . . ? O31 Na1 O8 86.82(17) . . ? O31 Na1 O45 168.39(18) . . ? O8 Na1 O45 104.63(17) . . ? O31 Na1 O34 86.67(16) . . ? O8 Na1 O34 162.16(17) . . ? O45 Na1 O34 81.82(15) . . ? O31 Na1 O46 93.5(2) . . ? O8 Na1 O46 97.48(18) . . ? O45 Na1 O46 86.91(18) . . ? O34 Na1 O46 99.49(19) . . ? O31 Na1 O32 86.39(15) . . ? O8 Na1 O32 78.97(14) . . ? O45 Na1 O32 93.87(15) . . ? O34 Na1 O32 84.06(14) . . ? O46 Na1 O32 176.45(19) . . ? O31 Na1 Cu2 54.49(12) . . ? O8 Na1 Cu2 64.83(11) . . ? O45 Na1 Cu2 128.62(13) . . ? O34 Na1 Cu2 98.02(12) . . ? O46 Na1 Cu2 142.30(16) . . ? O32 Na1 Cu2 36.00(9) . . ? O31 Na1 Cu3 92.22(13) . . ? O8 Na1 Cu3 112.88(12) . . ? O45 Na1 Cu3 81.69(12) . . ? O34 Na1 Cu3 50.86(10) . . ? O46 Na1 Cu3 149.36(16) . . ? O32 Na1 Cu3 34.15(9) . . ? Cu2 Na1 Cu3 61.22(4) . . ? C85 O7 Cu2 123.4(4) . . ? C85 O8 Na1 136.3(3) . . ? C87 O9 Cu3 125.0(3) . . ? C89 O11 Cu6 125.9(4) . . ? C91 O13 Cu10 133.3(4) . . ? Cu2 O32 Cu3 122.73(17) . . ? Cu2 O32 Na1 95.50(15) . . ? Cu3 O32 Na1 100.45(15) . . ? Cu7 O36 Cu6 121.9(2) . . ? C1 N1 C5 117.9(5) . . ? C1 N1 Cu1 127.2(4) . . ? C5 N1 Cu1 114.9(4) . . ? C10 N2 C6 122.6(5) . . ? C10 N2 Cu1 118.0(4) . . ? C6 N2 Cu1 119.5(4) . . ? C11 N3 N4 115.6(4) . . ? C11 N3 Cu1 116.0(3) . . ? N4 N3 Cu1 124.1(3) . . ? C12 N4 N3 115.2(4) . . ? C12 N4 Cu2 117.6(4) . . ? N3 N4 Cu2 127.1(3) . . ? C12 N5 Cu11 123.5(4) . . ? C12 N5 H8 114.8 . . ? Cu11 N5 H8 121.1 . . ? N7 N6 C13 121.9(4) . . ? N7 N6 Cu2 121.1(3) . . ? C13 N6 Cu2 117.0(3) . . ? N6 N7 C16 120.5(4) . . ? N6 N7 Cu3 121.7(3) . . ? C16 N7 Cu3 117.7(4) . . ? C17 N8 Cu5 127.5(4) . . ? C17 N8 H11 104.0 . . ? Cu5 N8 H11 115.9 . . ? C17 N9 N10 114.1(4) . . ? C17 N9 Cu3 118.2(3) . . ? N10 N9 Cu3 124.0(3) . . ? C18 N10 N9 116.0(4) . . ? C18 N10 Cu4 116.4(4) . . ? N9 N10 Cu4 122.0(3) . . ? C19 N11 C23 122.5(5) . . ? C19 N11 Cu4 118.0(4) . . ? C23 N11 Cu4 119.4(4) . . ? C24 N12 C28 120.1(5) . . ? C24 N12 Cu4 113.9(4) . . ? C28 N12 Cu4 125.4(4) . . ? C29 N13 C33 118.1(5) . . ? C29 N13 Cu5 127.3(4) . . ? C33 N13 Cu5 114.2(4) . . ? C34 N14 C38 121.1(5) . . ? C34 N14 Cu5 121.0(4) . . ? C38 N14 Cu5 117.4(4) . . ? C39 N15 N16 117.0(4) . . ? C39 N15 Cu5 116.1(3) . . ? N16 N15 Cu5 121.8(3) . . ? C40 N16 N15 114.8(4) . . ? C40 N16 Cu6 117.2(3) . . ? N15 N16 Cu6 125.7(3) . . ? C40 N17 Cu4 124.9(3) . . ? C40 N17 H26 111.3 . . ? Cu4 N17 H26 122.6 . . ? N19 N18 C41 121.1(4) . . ? N19 N18 Cu6 121.1(3) . . ? C41 N18 Cu6 117.7(3) . . ? N18 N19 C44 121.4(4) . . ? N18 N19 Cu7 121.1(3) . . ? C44 N19 Cu7 117.2(4) . . ? C45 N20 Cu9 128.0(3) . . ? C45 N20 H29 118.1 . . ? Cu9 N20 H29 113.3 . . ? C45 N21 N22 113.9(4) . . ? C45 N21 Cu7 117.1(3) . . ? N22 N21 Cu7 127.5(3) . . ? C46 N22 N21 116.2(5) . . ? C46 N22 Cu8 114.4(4) . . ? N21 N22 Cu8 126.9(3) . . ? C47 N23 C51 122.4(5) . . ? C47 N23 Cu8 118.0(4) . . ? C51 N23 Cu8 119.6(4) . . ? C56 N24 C52 120.6(6) . . ? C56 N24 Cu8 126.6(5) . . ? C52 N24 Cu8 112.7(5) . . ? C57 N25 C61 118.8(5) . . ? C57 N25 Cu9 126.9(4) . . ? C61 N25 Cu9 114.1(4) . . ? C66 N26 C62 121.8(5) . . ? C66 N26 Cu9 118.8(4) . . ? C62 N26 Cu9 119.4(4) . . ? C67 N27 N28 115.5(4) . . ? C67 N27 Cu9 115.5(4) . . ? N28 N27 Cu9 125.2(3) . . ? C68 N28 N27 115.5(4) . . ? C68 N28 Cu10 117.6(3) . . ? N27 N28 Cu10 124.6(3) . . ? C68 N29 Cu8 128.5(4) . . ? C68 N29 H44 104.9 . . ? Cu8 N29 H44 125.4 . . ? C69 N30 N31 122.7(5) . . ? C69 N30 Cu10 115.1(3) . . ? N31 N30 Cu10 122.1(3) . . ? C72 N31 N30 116.7(5) . . ? C73 N32 Cu1 128.1(4) . . ? C73 N32 H47 121.3 . . ? Cu1 N32 H47 109.1 . . ? C73 N33 N34 121.4(4) . . ? C74 N34 N33 115.2(5) . . ? C74 N34 Cu11 118.0(4) . . ? N33 N34 Cu11 124.8(3) . . ? C79 N35 C75 120.7(5) . . ? C79 N35 Cu11 120.4(4) . . ? C75 N35 Cu11 118.8(4) . . ? C80 N36 C84 120.2(5) . . ? C80 N36 Cu11 113.7(4) . . ? C84 N36 Cu11 125.9(4) . . ? N1 C1 C2 122.9(6) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 117.8(6) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 120.4(6) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 118.8(6) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.1(6) . . ? N1 C5 C6 113.2(5) . . ? C4 C5 C6 124.6(5) . . ? N2 C6 C7 119.3(5) . . ? N2 C6 C5 113.2(5) . . ? C7 C6 C5 127.4(5) . . ? C8 C7 C6 118.7(6) . . ? C8 C7 H5 120.6 . . ? C6 C7 H5 120.6 . . ? C7 C8 C9 121.2(6) . . ? C7 C8 H6 119.4 . . ? C9 C8 H6 119.4 . . ? C10 C9 C8 117.3(6) . . ? C10 C9 H7 121.4 . . ? C8 C9 H7 121.4 . . ? N2 C10 C9 120.8(5) . . ? N2 C10 C11 113.9(4) . . ? C9 C10 C11 125.3(5) . . ? O1 C11 N3 128.2(5) . . ? O1 C11 C10 120.5(4) . . ? N3 C11 C10 111.2(5) . . ? N5 C12 N4 126.5(5) . . ? N5 C12 C13 120.7(5) . . ? N4 C12 C13 112.7(5) . . ? N6 C13 C14 120.2(5) . . ? N6 C13 C12 113.6(4) . . ? C14 C13 C12 126.1(5) . . ? C15 C14 C13 118.0(5) . . ? C15 C14 H9 121.0 . . ? C13 C14 H9 121.0 . . ? C14 C15 C16 118.0(5) . . ? C14 C15 H10 121.0 . . ? C16 C15 H10 121.0 . . ? N7 C16 C15 121.4(5) . . ? N7 C16 C17 113.1(4) . . ? C15 C16 C17 125.5(4) . . ? N8 C17 N9 126.2(5) . . ? N8 C17 C16 122.8(4) . . ? N9 C17 C16 110.9(4) . . ? O2 C18 N10 128.3(5) . . ? O2 C18 C19 120.3(4) . . ? N10 C18 C19 111.4(4) . . ? N11 C19 C20 120.8(5) . . ? N11 C19 C18 113.0(4) . . ? C20 C19 C18 126.2(5) . . ? C19 C20 C21 116.1(6) . . ? C19 C20 H12 121.9 . . ? C21 C20 H12 121.9 . . ? C22 C21 C20 121.7(6) . . ? C22 C21 H13 119.1 . . ? C20 C21 H13 119.1 . . ? C23 C22 C21 118.3(6) . . ? C23 C22 H14 120.8 . . ? C21 C22 H14 120.8 . . ? N11 C23 C22 120.4(5) . . ? N11 C23 C24 111.1(5) . . ? C22 C23 C24 128.4(5) . . ? N12 C24 C25 121.7(5) . . ? N12 C24 C23 115.7(5) . . ? C25 C24 C23 122.6(5) . . ? C26 C25 C24 117.7(6) . . ? C26 C25 H15 121.1 . . ? C24 C25 H15 121.1 . . ? C25 C26 C27 121.2(6) . . ? C25 C26 H16 119.4 . . ? C27 C26 H16 119.4 . . ? C26 C27 C28 116.9(6) . . ? C26 C27 H17 121.6 . . ? C28 C27 H17 121.6 . . ? N12 C28 C27 122.4(6) . . ? N12 C28 H18 118.8 . . ? C27 C28 H18 118.8 . . ? N13 C29 C30 124.0(6) . . ? N13 C29 H19 118.0 . . ? C30 C29 H19 118.0 . . ? C31 C30 C29 117.6(7) . . ? C31 C30 H20 121.2 . . ? C29 C30 H20 121.2 . . ? C30 C31 C32 119.6(6) . . ? C30 C31 H21 120.2 . . ? C32 C31 H21 120.2 . . ? C33 C32 C31 118.0(7) . . ? C33 C32 H22 121.0 . . ? C31 C32 H22 121.0 . . ? N13 C33 C32 122.6(6) . . ? N13 C33 C34 113.9(5) . . ? C32 C33 C34 123.4(6) . . ? N14 C34 C35 121.4(6) . . ? N14 C34 C33 111.6(5) . . ? C35 C34 C33 127.0(6) . . ? C36 C35 C34 117.4(6) . . ? C36 C35 H23 121.3 . . ? C34 C35 H23 121.3 . . ? C37 C36 C35 121.5(6) . . ? C37 C36 H24 119.3 . . ? C35 C36 H24 119.3 . . ? C36 C37 C38 118.1(6) . . ? C36 C37 H25 121.0 . . ? C38 C37 H25 121.0 . . ? N14 C38 C37 120.6(5) . . ? N14 C38 C39 114.7(5) . . ? C37 C38 C39 124.6(5) . . ? O3 C39 N15 128.9(5) . . ? O3 C39 C38 121.7(5) . . ? N15 C39 C38 109.4(4) . . ? N17 C40 N16 126.8(4) . . ? N17 C40 C41 120.5(4) . . ? N16 C40 C41 112.6(4) . . ? N18 C41 C42 120.7(5) . . ? N18 C41 C40 112.8(4) . . ? C42 C41 C40 126.4(4) . . ? C43 C42 C41 118.2(5) . . ? C43 C42 H27 120.9 . . ? C41 C42 H27 120.9 . . ? C42 C43 C44 118.2(5) . . ? C42 C43 H28 120.9 . . ? C44 C43 H28 120.9 . . ? N19 C44 C43 120.0(5) . . ? N19 C44 C45 112.9(4) . . ? C43 C44 C45 127.2(5) . . ? N20 C45 N21 127.5(5) . . ? N20 C45 C44 120.0(4) . . ? N21 C45 C44 112.4(4) . . ? O4 C46 N22 128.0(5) . . ? O4 C46 C47 118.1(5) . . ? N22 C46 C47 113.8(5) . . ? N23 C47 C48 121.0(5) . . ? N23 C47 C46 112.9(5) . . ? C48 C47 C46 126.0(6) . . ? C49 C48 C47 117.1(6) . . ? C49 C48 H30 121.5 . . ? C47 C48 H30 121.5 . . ? C50 C49 C48 121.6(6) . . ? C50 C49 H31 119.2 . . ? C48 C49 H31 119.2 . . ? C49 C50 C51 119.2(6) . . ? C49 C50 H32 120.4 . . ? C51 C50 H32 120.4 . . ? N23 C51 C50 118.7(6) . . ? N23 C51 C52 112.8(5) . . ? C50 C51 C52 128.6(6) . . ? N24 C52 C53 120.8(7) . . ? N24 C52 C51 115.7(6) . . ? C53 C52 C51 123.5(6) . . ? C52 C53 C54 118.3(7) . . ? C52 C53 H33 120.9 . . ? C54 C53 H33 120.9 . . ? C55 C54 C53 120.9(7) . . ? C55 C54 H34 119.6 . . ? C53 C54 H34 119.6 . . ? C54 C55 C56 117.7(8) . . ? C54 C55 H35 121.1 . . ? C56 C55 H35 121.1 . . ? N24 C56 C55 121.7(7) . . ? N24 C56 H36 119.1 . . ? C55 C56 H36 119.1 . . ? N25 C57 C58 122.5(5) . . ? N25 C57 H37 118.8 . . ? C58 C57 H37 118.8 . . ? C59 C58 C57 119.1(6) . . ? C59 C58 H38 120.5 . . ? C57 C58 H38 120.5 . . ? C60 C59 C58 119.0(6) . . ? C60 C59 H39 120.5 . . ? C58 C59 H39 120.5 . . ? C59 C60 C61 119.2(6) . . ? C59 C60 H40 120.4 . . ? C61 C60 H40 120.4 . . ? N25 C61 C60 121.4(6) . . ? N25 C61 C62 113.4(5) . . ? C60 C61 C62 125.2(5) . . ? N26 C62 C63 120.9(5) . . ? N26 C62 C61 113.3(5) . . ? C63 C62 C61 125.8(5) . . ? C64 C63 C62 116.9(5) . . ? C64 C63 H41 121.5 . . ? C62 C63 H41 121.5 . . ? C63 C64 C65 121.5(5) . . ? C63 C64 H42 119.2 . . ? C65 C64 H42 119.2 . . ? C66 C65 C64 116.7(6) . . ? C66 C65 H43 121.7 . . ? C64 C65 H43 121.7 . . ? N26 C66 C65 122.1(5) . . ? N26 C66 C67 113.5(5) . . ? C65 C66 C67 124.3(6) . . ? O5 C67 N27 127.6(5) . . ? O5 C67 C66 121.4(5) . . ? N27 C67 C66 110.9(5) . . ? N29 C68 N28 125.4(5) . . ? N29 C68 C69 122.4(5) . . ? N28 C68 C69 112.1(4) . . ? N30 C69 C70 122.0(5) . . ? N30 C69 C68 114.1(5) . . ? C70 C69 C68 123.8(5) . . ? C71 C70 C69 117.5(6) . . ? C71 C70 H45 121.3 . . ? C69 C70 H45 121.3 . . ? C70 C71 C72 118.1(6) . . ? C70 C71 H46 120.9 . . ? C72 C71 H46 120.9 . . ? N31 C72 C71 123.0(5) . . ? N31 C72 C73 115.7(5) . . ? C71 C72 C73 121.3(5) . . ? N32 C73 N33 123.4(5) . . ? N32 C73 C72 123.3(5) . . ? N33 C73 C72 113.2(5) . . ? O6 C74 N34 126.7(5) . . ? O6 C74 C75 122.6(5) . . ? N34 C74 C75 110.6(5) . . ? N35 C75 C76 122.3(5) . . ? N35 C75 C74 112.8(5) . . ? C76 C75 C74 124.9(5) . . ? C75 C76 C77 116.3(6) . . ? C75 C76 H48 121.9 . . ? C77 C76 H48 121.9 . . ? C78 C77 C76 121.6(6) . . ? C78 C77 H49 119.2 . . ? C76 C77 H49 119.2 . . ? C77 C78 C79 118.0(5) . . ? C77 C78 H50 121.0 . . ? C79 C78 H50 121.0 . . ? N35 C79 C78 120.8(6) . . ? N35 C79 C80 112.4(5) . . ? C78 C79 C80 126.6(5) . . ? N36 C80 C81 120.6(6) . . ? N36 C80 C79 114.3(5) . . ? C81 C80 C79 125.1(6) . . ? C80 C81 C82 120.0(6) . . ? C80 C81 H51 120.0 . . ? C82 C81 H51 120.0 . . ? C83 C82 C81 118.6(6) . . ? C83 C82 H52 120.7 . . ? C81 C82 H52 120.7 . . ? C82 C83 C84 119.0(6) . . ? C82 C83 H53 120.5 . . ? C84 C83 H53 120.5 . . ? N36 C84 C83 121.5(6) . . ? N36 C84 H54 119.3 . . ? C83 C84 H54 119.3 . . ? O8 C85 O7 125.7(5) . . ? O8 C85 C86 118.8(5) . . ? O7 C85 C86 115.3(5) . . ? C85 C86 H55 109.5 . . ? C85 C86 H56 109.5 . . ? H55 C86 H56 109.5 . . ? C85 C86 H57 109.5 . . ? H55 C86 H57 109.5 . . ? H56 C86 H57 109.5 . . ? O10 C87 O9 124.1(5) . . ? O10 C87 C88 119.7(5) . . ? O9 C87 C88 116.2(5) . . ? C87 C88 H58 109.5 . . ? C87 C88 H59 109.5 . . ? H58 C88 H59 109.5 . . ? C87 C88 H60 109.5 . . ? H58 C88 H60 109.5 . . ? H59 C88 H60 109.5 . . ? O12 C89 O11 124.5(5) . . ? O12 C89 C90 120.8(5) . . ? O11 C89 C90 114.6(5) . . ? C89 C90 H61 109.5 . . ? C89 C90 H62 109.5 . . ? H61 C90 H62 109.5 . . ? C89 C90 H63 109.5 . . ? H61 C90 H63 109.5 . . ? H62 C90 H63 109.5 . . ? O14 C91 O13 120.0(6) . . ? O14 C91 C92 119.1(6) . . ? O13 C91 C92 120.8(6) . . ? C91 C92 H64 109.5 . . ? C91 C92 H65 109.5 . . ? H64 C92 H65 109.5 . . ? C91 C92 H66 109.5 . . ? H64 C92 H66 109.5 . . ? H65 C92 H66 109.5 . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 2.046 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.129 data_6 _database_code_depnum_ccdc_archive 'CCDC 775198' #TrackingRef '- Communication_CIF.cif' # start Validation Reply Form _vrf_CHEMW03_6 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: The structure was treated by Platon's SQUEEZE procedure. 595.5 electrons were recovered per formula unit. This accounts for 13 nitrate anions and 17 water molecules. These were included in the formula for the calculation of intenstive properties, but do not "appear" in the model. Also, please see platon_squeeze_details. ; _vrf_PLAT432_6 ; PROBLEM: Short Inter X...Y Contact O35 .. C27 .. 2.57 Ang. RESPONSE: The first atom listed is part of a disordered nitrate group. It appears to lie in the central cavity of the grid, and does seem to make short contacts to the grid moiety. Also, please see platon_squeeze_details. ; _vrf_PLAT043_6 ; PROBLEM: Check Reported Molecular Weight ................ 5726.76 RESPONSE: The structure was treated by Platon's SQUEEZE procedure. 595.5 electrons were recovered per formula unit. This accounts for 13 nitrate anions and 17 water molecules. These were included in the formula for the calculation of intenstive properties, but do not "appear" in the model. Also, please see platon_squeeze_details. ; _vrf_PLAT044_6 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: The structure was treated by Platon's SQUEEZE procedure. 595.5 electrons were recovered per formula unit. This accounts for 13 nitrate anions and 17 water molecules. These were included in the formula for the calculation of intenstive properties, but do not "appear" in the model. Also, please see platon_squeeze_details. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C144 H112 N80 Ni16 O34, 16 (N O3), 32 (H2 O)' _chemical_formula_sum 'C144 H176 N96 Ni16 O96' _chemical_formula_weight 5726.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 19.483(6) _cell_length_b 24.701(8) _cell_length_c 26.510(9) _cell_angle_alpha 111.723(6) _cell_angle_beta 94.468(6) _cell_angle_gamma 97.249(7) _cell_volume 11649(6) _cell_formula_units_Z 2 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used 38098 _cell_measurement_theta_min 2.3127 _cell_measurement_theta_max 31.2311 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5856 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.8466 _exptl_absorpt_correction_T_min 0.7486 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 128(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 90389 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 39271 _reflns_number_gt 20567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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. Distance, angle and rigid bond restraints were applied to the disordered nitrate anion (PART A: N82, O35-37; PART B: N83, O38-40). Another nitrate (N84, O41-43) was treated with distance and similarity restraints. All terminal pyridine rings (16 in total) were treated with angle and similarity restraints. Also, please refer to platon_squeeze_details, which follow. ; _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 39271 _refine_ls_number_parameters 2585 _refine_ls_number_restraints 742 _refine_ls_R_factor_all 0.1609 _refine_ls_R_factor_gt 0.1299 _refine_ls_wR_factor_ref 0.3785 _refine_ls_wR_factor_gt 0.3304 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 -0.011 0.003 0.000 4084 1191 '26(NO3), 34(H2O)' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 1191 electrons per unit cell in one void (total volume 4084 ^A^3); that is 595.5 electrons per formula unit. Due to poor diffraction, and many, many peaks associated with disordered lattice solvent and anions, charge could not be conclusively balanced based on this X-ray analysis. The model formula corresponds to (L-2H)8(Ni(II))16(H2O)15(NO3)3) Therefore, for charge balance, an additional 13 nitrate anions per formula unit are required. This would account for 416 electrons. The additional electron density is attributed to partial occupancy, disordered, lattice solvent molecules; that is, approximately 17 water molecules per formula unit, accounting for another 170 electrons. The application of Squeeze gave a significant improvement in the data statistics, however, this report is only intended to support to the gross connectivity in the core of the structure. Further conclusions based on the X-ray analysis would constitute over-interpretation of a weak data set. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. ; 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 O35 O 0.4085(6) 0.1643(5) 0.2971(5) 0.097(3) Uani 0.50 1 d PDU A 1 O36 O 0.5126(5) 0.1902(5) 0.3373(6) 0.103(3) Uani 0.50 1 d PDU A 1 O37 O 0.4885(17) 0.1353(10) 0.2426(9) 0.102(6) Uani 0.50 1 d PDU A 1 N82 N 0.4739(10) 0.1634(14) 0.2902(8) 0.153(13) Uani 0.50 1 d PDU A 1 O38 O 0.5020(4) 0.0803(4) 0.2204(4) 0.0626(19) Uani 0.50 1 d PDU B 2 O39 O 0.5085(4) 0.1628(4) 0.2089(4) 0.074(2) Uani 0.50 1 d PDU B 2 O40 O 0.4701(6) 0.1579(4) 0.2865(6) 0.065(3) Uani 0.50 1 d PDU B 2 N83 N 0.4982(16) 0.1371(8) 0.2429(8) 0.071(4) Uani 0.50 1 d PDU B 2 Ni1 Ni 0.16196(7) 0.32967(7) 0.09007(7) 0.1214(5) Uani 1 1 d . . . Ni2 Ni 0.32503(5) 0.39116(5) 0.20499(5) 0.0927(3) Uani 1 1 d . . . Ni3 Ni 0.63283(6) 0.47033(5) 0.33188(6) 0.1075(4) Uani 1 1 d . . . Ni4 Ni 0.83817(7) 0.50751(7) 0.37056(8) 0.1397(6) Uani 1 1 d . . . Ni5 Ni 0.17186(6) 0.16715(6) 0.07953(5) 0.1002(4) Uani 1 1 d . . . Ni6 Ni 0.33732(4) 0.22998(4) 0.19004(4) 0.0733(3) Uani 1 1 d . . . Ni7 Ni 0.64567(5) 0.30682(4) 0.31057(4) 0.0776(3) Uani 1 1 d . . . Ni8 Ni 0.84925(5) 0.34023(6) 0.34546(6) 0.1045(4) Uani 1 1 d . . . Ni9 Ni 0.14793(5) -0.07510(5) 0.11871(5) 0.0957(3) Uani 1 1 d . . . Ni10 Ni 0.31638(4) -0.01011(4) 0.22461(4) 0.0709(3) Uani 1 1 d . . . Ni11 Ni 0.62870(4) 0.06300(4) 0.33779(4) 0.0712(3) Uani 1 1 d . . . Ni12 Ni 0.83200(5) 0.08833(5) 0.36754(5) 0.0957(3) Uani 1 1 d . . . Ni13 Ni 0.11016(6) -0.19970(6) 0.17842(6) 0.1159(4) Uani 1 1 d . . . Ni14 Ni 0.28510(5) -0.13408(5) 0.28289(5) 0.0886(3) Uani 1 1 d . . . Ni15 Ni 0.60460(6) -0.06456(5) 0.39204(5) 0.0920(3) Uani 1 1 d . . . Ni16 Ni 0.81132(6) -0.04767(6) 0.41561(6) 0.1061(4) Uani 1 1 d . . . O1 O 0.2197(3) 0.3567(3) 0.1659(3) 0.1015(17) Uani 1 1 d . . . O2 O 0.7339(3) 0.4908(3) 0.3788(4) 0.112(2) Uani 1 1 d . . . O3 O 0.2297(2) 0.2041(2) 0.1563(2) 0.0804(13) Uani 1 1 d . . . O4 O 0.7469(2) 0.3313(3) 0.3573(3) 0.0907(15) Uani 1 1 d . . . O5 O 0.2086(2) -0.0261(2) 0.1923(2) 0.0803(13) Uani 1 1 d . . . O6 O 0.7310(2) 0.0963(2) 0.3820(2) 0.0825(13) Uani 1 1 d . . . O7 O 0.1786(3) -0.1483(3) 0.2474(3) 0.0976(16) Uani 1 1 d . . . O8 O 0.7102(3) -0.0327(3) 0.4295(3) 0.0942(15) Uani 1 1 d . . . O9 O 0.1940(3) 0.2468(3) 0.0653(3) 0.111(2) Uani 1 1 d . . . O10 O 0.1523(3) -0.1551(3) 0.1333(3) 0.0985(17) Uani 1 1 d . . . O11 O 0.3525(3) 0.3087(2) 0.1746(2) 0.0778(12) Uani 1 1 d . . . O12 O 0.3178(2) -0.0924(2) 0.2314(2) 0.0773(12) Uani 1 1 d . . . O13 O 0.6450(3) 0.3852(2) 0.2933(3) 0.0875(14) Uani 1 1 d . . . O14 O 0.6194(2) -0.0246(2) 0.3374(2) 0.0754(12) Uani 1 1 d . . . O15 O 0.8402(3) 0.4181(3) 0.3287(4) 0.1095(19) Uani 1 1 d . . . O16 O 0.8165(3) -0.0011(3) 0.3633(3) 0.0939(15) Uani 1 1 d . . . O17 O 0.0901(4) 0.3049(4) 0.0205(4) 0.159(3) Uani 1 1 d . . . O18 O 0.1393(4) 0.4150(4) 0.1091(4) 0.153(3) Uani 1 1 d . . . O19 O 0.3023(3) 0.4749(3) 0.2270(3) 0.116(2) Uani 1 1 d . . . O20 O 0.6256(4) 0.5585(3) 0.3601(3) 0.132(2) Uani 1 1 d . . . O21 O 0.8343(5) 0.5964(4) 0.4041(6) 0.197(5) Uani 1 1 d . . . O22 O 0.9446(4) 0.5281(4) 0.3752(5) 0.182(4) Uani 1 1 d . . . O23 O 0.1024(3) 0.1322(3) 0.0090(3) 0.114(2) Uani 1 1 d . . . O24 O 0.9538(3) 0.3584(3) 0.3449(3) 0.131(2) Uani 1 1 d . . . O25 O 0.0770(3) -0.1208(4) 0.0484(3) 0.132(2) Uani 1 1 d . . . O26 O 0.9352(3) 0.0854(3) 0.3614(3) 0.1108(19) Uani 1 1 d . . . O27 O 0.0340(4) -0.2454(4) 0.1140(4) 0.160(3) Uani 1 1 d . . . O28 O 0.0696(4) -0.2524(4) 0.2174(4) 0.154(3) Uani 1 1 d . . . O29 O 0.2568(3) -0.1833(3) 0.3284(3) 0.1093(18) Uani 1 1 d . . . O30 O 0.5853(3) -0.1097(3) 0.4461(3) 0.1058(17) Uani 1 1 d . . . O31 O 0.8086(4) -0.1038(4) 0.4591(4) 0.145(3) Uani 1 1 d . . . O32 O 0.9161(3) -0.0574(3) 0.4069(4) 0.133(2) Uani 1 1 d . . . O33 O 0.6697(4) -0.1584(3) 0.4335(3) 0.119(2) Uani 1 1 d . . . O34 O 0.6375(5) -0.1276(3) 0.5125(3) 0.133(2) Uani 1 1 d . . . O41 O 0.3490(8) 0.2662(6) 0.5192(8) 0.278(9) Uani 1 1 d DU . . O42 O 0.3686(10) 0.2387(5) 0.4401(4) 0.247(9) Uani 1 1 d DU . . O43 O 0.4416(8) 0.2559(8) 0.4994(8) 0.290(9) Uani 1 1 d DU . . N1 N 0.0862(4) 0.3139(4) 0.1314(4) 0.127(3) Uani 1 1 d DU . . N2 N 0.2052(4) 0.3602(3) 0.2523(4) 0.102(2) Uani 1 1 d . . . N3 N 0.2754(4) 0.3800(3) 0.2625(4) 0.0917(19) Uani 1 1 d . . . N4 N 0.2755(4) 0.3900(4) 0.3530(4) 0.114(2) Uani 1 1 d . . . H4A H 0.2302 0.3783 0.3495 0.137 Uiso 1 1 calc R . . H4B H 0.3013 0.3999 0.3849 0.137 Uiso 1 1 calc R . . N5 N 0.4054(3) 0.4197(3) 0.2754(3) 0.0899(18) Uani 1 1 d . . . N6 N 0.5196(4) 0.4473(3) 0.3213(4) 0.103(2) Uani 1 1 d . . . N7 N 0.5309(5) 0.4471(4) 0.4552(4) 0.129(3) Uani 1 1 d . . . H7A H 0.5622 0.4534 0.4834 0.155 Uiso 1 1 calc R . . H7B H 0.4863 0.4380 0.4569 0.155 Uiso 1 1 calc R . . N8 N 0.6131(4) 0.4641(3) 0.4001(3) 0.098(2) Uani 1 1 d . . . N9 N 0.6659(4) 0.4752(3) 0.4430(3) 0.103(2) Uani 1 1 d . . . N10 N 0.8460(5) 0.5073(4) 0.4487(4) 0.138(3) Uani 1 1 d DU . . N11 N 0.0947(4) 0.1713(4) 0.1260(4) 0.114(2) Uani 1 1 d D . . N12 N 0.2155(3) 0.2226(3) 0.2450(3) 0.0799(16) Uani 1 1 d . . . N13 N 0.2861(3) 0.2401(3) 0.2541(2) 0.0717(14) Uani 1 1 d . . . N14 N 0.2890(4) 0.2522(3) 0.3442(3) 0.099(2) Uani 1 1 d . . . H14A H 0.2436 0.2408 0.3404 0.118 Uiso 1 1 calc R . . H14B H 0.3144 0.2623 0.3762 0.118 Uiso 1 1 calc R . . N15 N 0.4196(3) 0.2652(3) 0.2593(3) 0.0743(15) Uani 1 1 d . . . N16 N 0.5349(3) 0.2923(2) 0.3032(2) 0.0695(14) Uani 1 1 d . . . N17 N 0.5503(4) 0.3154(3) 0.4463(3) 0.0926(19) Uani 1 1 d . . . H17A H 0.5840 0.3256 0.4738 0.111 Uiso 1 1 calc R . . H17B H 0.5066 0.3077 0.4512 0.111 Uiso 1 1 calc R . . N18 N 0.6272(3) 0.3219(3) 0.3838(3) 0.0857(18) Uani 1 1 d . . . N19 N 0.6814(3) 0.3352(3) 0.4278(3) 0.0876(18) Uani 1 1 d . . . N20 N 0.8611(4) 0.3587(3) 0.4267(4) 0.114(2) Uani 1 1 d DU . . N21 N 0.0772(3) -0.0335(4) 0.1611(3) 0.103(2) Uani 1 1 d DU . . N22 N 0.2044(3) 0.0478(3) 0.2751(3) 0.0864(17) Uani 1 1 d . . . N23 N 0.2718(3) 0.0433(3) 0.2832(2) 0.0724(15) Uani 1 1 d . . . N24 N 0.2854(4) 0.1265(3) 0.3629(3) 0.0965(19) Uani 1 1 d . . . H24A H 0.2413 0.1306 0.3585 0.116 Uiso 1 1 calc R . . H24B H 0.3138 0.1519 0.3917 0.116 Uiso 1 1 calc R . . N25 N 0.4013(3) 0.0329(3) 0.2902(3) 0.0780(16) Uani 1 1 d . . . N26 N 0.5171(3) 0.0595(2) 0.3315(2) 0.0668(13) Uani 1 1 d . . . N27 N 0.5455(3) 0.1858(3) 0.4600(3) 0.0857(17) Uani 1 1 d . . . H27A H 0.5804 0.2081 0.4852 0.103 Uiso 1 1 calc R . . H27B H 0.5030 0.1941 0.4629 0.103 Uiso 1 1 calc R . . N28 N 0.6149(3) 0.1220(3) 0.4074(2) 0.0716(14) Uani 1 1 d . . . N29 N 0.6713(3) 0.1557(3) 0.4453(2) 0.0808(16) Uani 1 1 d . . . N30 N 0.8507(4) 0.1462(3) 0.4452(3) 0.099(2) Uani 1 1 d DU . . N31 N 0.0484(4) -0.1404(4) 0.2153(4) 0.117(2) Uani 1 1 d DU . . N32 N 0.1851(4) -0.0598(3) 0.3234(3) 0.099(2) Uani 1 1 d . . . N33 N 0.2508(3) -0.0659(3) 0.3333(3) 0.0825(16) Uani 1 1 d . . . N34 N 0.2686(4) 0.0203(3) 0.4105(3) 0.100(2) Uani 1 1 d . . . H34A H 0.2250 0.0257 0.4064 0.120 Uiso 1 1 calc R . . H34B H 0.2983 0.0458 0.4384 0.120 Uiso 1 1 calc R . . N35 N 0.3767(3) -0.0859(3) 0.3449(3) 0.0840(17) Uani 1 1 d . . . N36 N 0.4941(3) -0.0613(3) 0.3836(3) 0.0816(16) Uani 1 1 d . . . N37 N 0.5358(3) 0.0783(3) 0.5002(3) 0.0853(17) Uani 1 1 d . . . H37A H 0.5735 0.1000 0.5224 0.102 Uiso 1 1 calc R . . H37B H 0.4951 0.0902 0.5047 0.102 Uiso 1 1 calc R . . N38 N 0.5980(3) 0.0086(3) 0.4517(3) 0.0850(17) Uani 1 1 d . . . N39 N 0.6590(4) 0.0418(3) 0.4862(3) 0.101(2) Uani 1 1 d . . . N40 N 0.8335(4) 0.0245(3) 0.4871(3) 0.103(2) Uani 1 1 d DU . . N41 N 0.2380(4) 0.3418(4) 0.0470(4) 0.121(3) Uani 1 1 d DU . . N42 N 0.2769(5) 0.1984(5) 0.0206(4) 0.114(3) Uani 1 1 d . . . N43 N 0.2490(4) 0.1577(4) 0.0400(3) 0.105(2) Uani 1 1 d . . . N44 N 0.3255(6) 0.0998(5) -0.0083(4) 0.152(4) Uani 1 1 d . . . H44A H 0.3460 0.1279 -0.0176 0.183 Uiso 1 1 calc R . . H44B H 0.3393 0.0652 -0.0191 0.183 Uiso 1 1 calc R . . N45 N 0.1911(4) 0.0790(3) 0.0716(3) 0.0950(19) Uani 1 1 d . . . N46 N 0.1827(4) -0.0096(3) 0.0869(3) 0.0890(18) Uani 1 1 d . . . N47 N 0.3080(5) -0.1000(4) 0.0256(5) 0.151(4) Uani 1 1 d . . . H47A H 0.3216 -0.1334 0.0233 0.181 Uiso 1 1 calc R . . H47B H 0.3282 -0.0789 0.0087 0.181 Uiso 1 1 calc R . . N48 N 0.2242(4) -0.1064(3) 0.0804(3) 0.0939(19) Uani 1 1 d . . . N49 N 0.2404(4) -0.1586(4) 0.0760(3) 0.105(2) Uani 1 1 d . . . N50 N 0.1740(5) -0.2530(4) 0.1442(4) 0.132(3) Uani 1 1 d DU . . N51 N 0.3840(3) 0.4027(3) 0.1504(3) 0.097(2) Uani 1 1 d DU . . N52 N 0.4208(3) 0.2557(3) 0.1130(3) 0.0816(16) Uani 1 1 d . . . N53 N 0.3980(3) 0.2144(3) 0.1315(3) 0.0851(17) Uani 1 1 d . . . N54 N 0.4705(4) 0.1546(4) 0.0809(4) 0.121(3) Uani 1 1 d . . . H54A H 0.4874 0.1824 0.0699 0.145 Uiso 1 1 calc R . . H54B H 0.4857 0.1205 0.0699 0.145 Uiso 1 1 calc R . . N55 N 0.3499(3) 0.1395(2) 0.1731(2) 0.0698(14) Uani 1 1 d . . . N56 N 0.3429(3) 0.0507(3) 0.1850(2) 0.0679(13) Uani 1 1 d . . . N57 N 0.4540(4) -0.0470(3) 0.1099(4) 0.120(3) Uani 1 1 d . . . H57A H 0.4626 -0.0826 0.1051 0.144 Uiso 1 1 calc R . . H57B H 0.4763 -0.0266 0.0933 0.144 Uiso 1 1 calc R . . N58 N 0.3724(3) -0.0520(3) 0.1682(2) 0.0714(14) Uani 1 1 d . . . N59 N 0.3884(3) -0.1050(2) 0.1645(3) 0.0779(15) Uani 1 1 d . . . N60 N 0.3307(4) -0.1972(3) 0.2330(3) 0.097(2) Uani 1 1 d DU . . N61 N 0.6394(4) 0.4686(4) 0.2567(3) 0.104(2) Uani 1 1 d DU . . N62 N 0.6469(3) 0.3176(4) 0.2053(3) 0.0897(19) Uani 1 1 d . . . N63 N 0.6531(3) 0.2779(3) 0.2310(3) 0.0781(16) Uani 1 1 d . . . N64 N 0.6375(4) 0.2014(3) 0.1466(3) 0.0943(19) Uani 1 1 d . . . H64A H 0.6382 0.2252 0.1288 0.113 Uiso 1 1 calc R . . H64B H 0.6320 0.1629 0.1284 0.113 Uiso 1 1 calc R . . N65 N 0.6502(3) 0.2127(2) 0.2867(2) 0.0656(13) Uani 1 1 d . . . N66 N 0.6432(3) 0.1238(3) 0.2969(2) 0.0683(13) Uani 1 1 d . . . N67 N 0.6247(3) -0.0020(3) 0.1692(3) 0.0897(18) Uani 1 1 d . . . H67A H 0.6179 -0.0408 0.1577 0.108 Uiso 1 1 calc R . . H67B H 0.6264 0.0151 0.1454 0.108 Uiso 1 1 calc R . . N68 N 0.6307(3) 0.0107(3) 0.2598(2) 0.0709(15) Uani 1 1 d . . . N69 N 0.6193(3) -0.0486(3) 0.2457(3) 0.0857(18) Uani 1 1 d . . . N70 N 0.5992(3) -0.1360(3) 0.3241(3) 0.0897(18) Uani 1 1 d DU . . N71 N 0.8210(5) 0.5012(7) 0.2926(7) 0.175(5) Uani 1 1 d DU . . N72 N 0.8229(3) 0.3505(5) 0.2398(4) 0.118(3) Uani 1 1 d . . . N73 N 0.8305(4) 0.3101(5) 0.2663(4) 0.107(2) Uani 1 1 d . . . N74 N 0.8109(4) 0.2328(5) 0.1800(4) 0.122(3) Uani 1 1 d . . . H74A H 0.8060 0.2550 0.1609 0.147 Uiso 1 1 calc R . . H74B H 0.8073 0.1943 0.1631 0.147 Uiso 1 1 calc R . . N75 N 0.8436(3) 0.2443(4) 0.3205(4) 0.100(2) Uani 1 1 d . . . N76 N 0.8370(3) 0.1529(4) 0.3280(3) 0.0928(19) Uani 1 1 d . . . N77 N 0.7996(4) 0.0299(4) 0.2007(4) 0.121(3) Uani 1 1 d . . . H77A H 0.7904 -0.0087 0.1901 0.145 Uiso 1 1 calc R . . H77B H 0.8015 0.0460 0.1761 0.145 Uiso 1 1 calc R . . N78 N 0.8079(3) 0.0418(4) 0.2895(4) 0.103(2) Uani 1 1 d . . . N79 N 0.7935(3) -0.0196(4) 0.2721(4) 0.102(2) Uani 1 1 d . . . N80 N 0.7828(4) -0.1140(4) 0.3424(4) 0.110(2) Uani 1 1 d DU . . N81 N 0.6310(4) -0.1331(4) 0.4635(4) 0.102(2) Uani 1 1 d . . . N84 N 0.3843(6) 0.2527(5) 0.4818(6) 0.134(3) Uani 1 1 d U . . C1 C 0.0166(5) 0.2987(5) 0.1113(6) 0.180(6) Uani 1 1 d DU . . H1 H 0.0003 0.2890 0.0738 0.216 Uiso 1 1 calc R . . C2 C -0.0302(7) 0.2982(7) 0.1507(8) 0.203(7) Uani 1 1 d DU . . H2 H -0.0790 0.2890 0.1388 0.244 Uiso 1 1 calc R . . C3 C -0.0081(6) 0.3101(7) 0.2024(6) 0.199(7) Uani 1 1 d DU . . H3 H -0.0407 0.3074 0.2265 0.238 Uiso 1 1 calc R . . C4 C 0.0623(6) 0.3263(6) 0.2216(6) 0.157(5) Uani 1 1 d DU . . H4 H 0.0793 0.3351 0.2588 0.188 Uiso 1 1 calc R . . C5 C 0.1067(5) 0.3292(4) 0.1844(5) 0.114(3) Uani 1 1 d DU . . C6 C 0.1815(4) 0.3490(3) 0.2017(5) 0.092(2) Uani 1 1 d . . . C7 C 0.3054(5) 0.3927(4) 0.3096(5) 0.095(2) Uani 1 1 d . . . C8 C 0.4748(4) 0.4353(4) 0.2755(4) 0.095(2) Uani 1 1 d . . . H8 H 0.4918 0.4379 0.2436 0.114 Uiso 1 1 calc R . . C9 C 0.3806(4) 0.4147(4) 0.3166(4) 0.089(2) Uani 1 1 d . . . C10 C 0.4252(5) 0.4245(4) 0.3626(4) 0.097(2) Uani 1 1 d . . . H10 H 0.4074 0.4204 0.3936 0.116 Uiso 1 1 calc R . . C11 C 0.4992(5) 0.4409(4) 0.3642(4) 0.100(3) Uani 1 1 d . . . C12 C 0.5511(6) 0.4514(4) 0.4103(4) 0.105(3) Uani 1 1 d . . . C13 C 0.7252(5) 0.4878(4) 0.4245(6) 0.113(3) Uani 1 1 d . . . C14 C 0.7849(5) 0.4995(4) 0.4671(6) 0.124(4) Uani 1 1 d DU . . C15 C 0.7875(6) 0.5052(5) 0.5168(6) 0.156(5) Uani 1 1 d DU . . H15 H 0.7437 0.4994 0.5291 0.187 Uiso 1 1 calc R . . C16 C 0.8432(7) 0.5181(5) 0.5539(5) 0.150(5) Uani 1 1 d DU . . H16 H 0.8393 0.5210 0.5903 0.180 Uiso 1 1 calc R . . C17 C 0.9086(7) 0.5273(6) 0.5362(6) 0.161(5) Uani 1 1 d DU . . H17 H 0.9510 0.5380 0.5605 0.193 Uiso 1 1 calc R . . C18 C 0.9085(6) 0.5203(6) 0.4843(7) 0.166(6) Uani 1 1 d DU . . H18 H 0.9517 0.5241 0.4707 0.199 Uiso 1 1 calc R . . C19 C 0.0281(4) 0.1521(5) 0.1083(6) 0.149(5) Uani 1 1 d D . . H19 H 0.0124 0.1416 0.0705 0.179 Uiso 1 1 calc R . . C20 C -0.0194(6) 0.1465(6) 0.1416(6) 0.187(6) Uani 1 1 d DU . . H20 H -0.0674 0.1332 0.1272 0.224 Uiso 1 1 calc R . . C21 C 0.0021(5) 0.1602(7) 0.1963(6) 0.176(6) Uani 1 1 d DU . . H21 H -0.0299 0.1546 0.2199 0.211 Uiso 1 1 calc R . . C22 C 0.0737(5) 0.1829(6) 0.2160(5) 0.142(4) Uani 1 1 d DU . . H22 H 0.0903 0.1954 0.2538 0.170 Uiso 1 1 calc R . . C23 C 0.1192(4) 0.1867(4) 0.1792(4) 0.108(3) Uani 1 1 d DU . . C24 C 0.1936(4) 0.2048(3) 0.1949(4) 0.079(2) Uani 1 1 d . . . C25 C 0.3189(4) 0.2540(3) 0.3021(3) 0.0767(18) Uani 1 1 d . . . C26 C 0.4874(3) 0.2777(3) 0.2604(3) 0.0703(17) Uani 1 1 d . . . H26 H 0.5035 0.2760 0.2270 0.084 Uiso 1 1 calc R . . C27 C 0.3954(4) 0.2695(3) 0.3052(3) 0.0744(18) Uani 1 1 d . . . C28 C 0.4414(4) 0.2868(4) 0.3545(3) 0.083(2) Uani 1 1 d . . . H28 H 0.4250 0.2913 0.3884 0.100 Uiso 1 1 calc R . . C29 C 0.5116(4) 0.2967(3) 0.3503(4) 0.084(2) Uani 1 1 d . . . C30 C 0.5651(4) 0.3119(3) 0.3988(4) 0.087(2) Uani 1 1 d . . . C31 C 0.7405(4) 0.3390(3) 0.4081(4) 0.0759(19) Uani 1 1 d . . . C32 C 0.8034(5) 0.3536(3) 0.4462(4) 0.102(3) Uani 1 1 d DU . . C33 C 0.8006(5) 0.3590(4) 0.5003(4) 0.102(3) Uani 1 1 d DU . . H33 H 0.7572 0.3551 0.5136 0.123 Uiso 1 1 calc R . . C34 C 0.8640(6) 0.3704(5) 0.5344(5) 0.126(4) Uani 1 1 d DU . . H34 H 0.8643 0.3743 0.5714 0.151 Uiso 1 1 calc R . . C35 C 0.9261(6) 0.3758(5) 0.5130(5) 0.131(4) Uani 1 1 d DU . . H35 H 0.9700 0.3843 0.5349 0.158 Uiso 1 1 calc R . . C36 C 0.9213(4) 0.3684(4) 0.4584(5) 0.117(3) Uani 1 1 d DU . . H36 H 0.9633 0.3703 0.4427 0.141 Uiso 1 1 calc R . . C37 C 0.0076(4) -0.0379(5) 0.1408(5) 0.124(4) Uani 1 1 d DU . . H37 H -0.0114 -0.0668 0.1056 0.149 Uiso 1 1 calc R . . C38 C -0.0331(5) -0.0008(8) 0.1712(7) 0.172(6) Uani 1 1 d DU . . H38 H -0.0798 -0.0030 0.1564 0.207 Uiso 1 1 calc R . . C39 C -0.0063(6) 0.0412(7) 0.2250(7) 0.176(6) Uani 1 1 d DU . . H39 H -0.0346 0.0661 0.2475 0.211 Uiso 1 1 calc R . . C40 C 0.0634(6) 0.0438(7) 0.2427(5) 0.150(5) Uani 1 1 d DU . . H40 H 0.0841 0.0722 0.2777 0.180 Uiso 1 1 calc R . . C41 C 0.1036(4) 0.0054(5) 0.2101(4) 0.109(3) Uani 1 1 d DU . . C42 C 0.1763(4) 0.0092(4) 0.2257(4) 0.0801(19) Uani 1 1 d . . . C43 C 0.3087(4) 0.0825(3) 0.3264(3) 0.0786(19) Uani 1 1 d . . . C44 C 0.4670(3) 0.0282(3) 0.2926(3) 0.0653(15) Uani 1 1 d . . . H44 H 0.4799 -0.0018 0.2621 0.078 Uiso 1 1 calc R . . C45 C 0.3825(4) 0.0762(3) 0.3314(3) 0.0766(18) Uani 1 1 d . . . C46 C 0.4295(4) 0.1105(3) 0.3752(3) 0.0757(18) Uani 1 1 d . . . H46 H 0.4149 0.1393 0.4057 0.091 Uiso 1 1 calc R . . C47 C 0.4989(4) 0.1040(3) 0.3758(3) 0.0680(16) Uani 1 1 d . . . C48 C 0.5567(4) 0.1405(3) 0.4182(3) 0.0734(18) Uani 1 1 d . . . C49 C 0.7276(4) 0.1377(4) 0.4288(3) 0.079(2) Uani 1 1 d . . . C50 C 0.7928(4) 0.1661(4) 0.4621(4) 0.098(2) Uani 1 1 d DU . . C51 C 0.7976(4) 0.2141(4) 0.5130(4) 0.109(3) Uani 1 1 d DU . . H51 H 0.7565 0.2288 0.5251 0.131 Uiso 1 1 calc R . . C52 C 0.8603(5) 0.2394(5) 0.5450(4) 0.118(3) Uani 1 1 d DU . . H52 H 0.8637 0.2713 0.5794 0.142 Uiso 1 1 calc R . . C53 C 0.9181(6) 0.2175(5) 0.5257(5) 0.133(4) Uani 1 1 d DU . . H53 H 0.9627 0.2347 0.5467 0.159 Uiso 1 1 calc R . . C54 C 0.9126(4) 0.1719(5) 0.4774(4) 0.112(3) Uani 1 1 d DU . . H54 H 0.9536 0.1571 0.4654 0.134 Uiso 1 1 calc R . . C55 C -0.0195(6) -0.1410(6) 0.1984(5) 0.146(5) Uani 1 1 d DU . . H55 H -0.0396 -0.1687 0.1631 0.176 Uiso 1 1 calc R . . C56 C -0.0579(6) -0.1067(8) 0.2272(6) 0.175(6) Uani 1 1 d DU . . H56 H -0.1053 -0.1101 0.2133 0.210 Uiso 1 1 calc R . . C57 C -0.0289(6) -0.0614(7) 0.2822(6) 0.171(5) Uani 1 1 d DU . . H57 H -0.0557 -0.0347 0.3045 0.205 Uiso 1 1 calc R . . C58 C 0.0408(6) -0.0614(8) 0.2986(6) 0.178(6) Uani 1 1 d DU . . H58 H 0.0631 -0.0339 0.3335 0.213 Uiso 1 1 calc R . . C59 C 0.0782(5) -0.1011(5) 0.2646(5) 0.116(3) Uani 1 1 d DU . . C60 C 0.1526(5) -0.1074(6) 0.2766(5) 0.115(3) Uani 1 1 d . . . C61 C 0.2900(4) -0.0277(4) 0.3738(4) 0.086(2) Uani 1 1 d . . . C62 C 0.4405(4) -0.0964(3) 0.3466(3) 0.083(2) Uani 1 1 d . . . H62 H 0.4496 -0.1317 0.3196 0.100 Uiso 1 1 calc R . . C63 C 0.3609(5) -0.0359(4) 0.3813(4) 0.089(2) Uani 1 1 d . . . C64 C 0.4132(4) 0.0023(4) 0.4218(4) 0.085(2) Uani 1 1 d . . . H64 H 0.4027 0.0367 0.4493 0.102 Uiso 1 1 calc R . . C65 C 0.4801(4) -0.0093(4) 0.4223(3) 0.084(2) Uani 1 1 d . . . C66 C 0.5401(5) 0.0279(3) 0.4600(3) 0.082(2) Uani 1 1 d . . . C67 C 0.7128(4) 0.0164(4) 0.4696(4) 0.087(2) Uani 1 1 d . . . C68 C 0.7798(4) 0.0476(4) 0.5046(4) 0.093(2) Uani 1 1 d DU . . C69 C 0.7844(5) 0.0940(4) 0.5510(4) 0.104(3) Uani 1 1 d DU . . H69 H 0.7437 0.1101 0.5623 0.125 Uiso 1 1 calc R . . C70 C 0.8486(5) 0.1193(5) 0.5832(4) 0.113(3) Uani 1 1 d DU . . H70 H 0.8527 0.1518 0.6173 0.136 Uiso 1 1 calc R . . C71 C 0.9056(6) 0.0958(6) 0.5644(5) 0.129(4) Uani 1 1 d DU . . H71 H 0.9507 0.1128 0.5846 0.155 Uiso 1 1 calc R . . C72 C 0.8976(5) 0.0481(6) 0.5164(5) 0.126(3) Uani 1 1 d DU . . H72 H 0.9372 0.0313 0.5034 0.151 Uiso 1 1 calc R . . C73 C 0.2543(7) 0.3887(7) 0.0368(6) 0.164(5) Uani 1 1 d DU . . H73 H 0.2358 0.4237 0.0544 0.196 Uiso 1 1 calc R . . C74 C 0.3036(9) 0.3846(7) -0.0042(8) 0.190(6) Uani 1 1 d DU . . H74 H 0.3154 0.4180 -0.0133 0.228 Uiso 1 1 calc R . . C75 C 0.3319(8) 0.3375(8) -0.0285(7) 0.179(6) Uani 1 1 d DU . . H75 H 0.3636 0.3370 -0.0541 0.215 Uiso 1 1 calc R . . C76 C 0.3129(8) 0.2868(6) -0.0148(6) 0.160(5) Uani 1 1 d DU . . H76 H 0.3318 0.2516 -0.0304 0.192 Uiso 1 1 calc R . . C77 C 0.2642(6) 0.2925(5) 0.0233(5) 0.120(3) Uani 1 1 d DU . . C78 C 0.2457(6) 0.2413(6) 0.0355(4) 0.108(3) Uani 1 1 d . . . C79 C 0.2730(6) 0.1097(6) 0.0224(4) 0.113(3) Uani 1 1 d . . . C80 C 0.1629(4) 0.0397(5) 0.0904(4) 0.098(3) Uani 1 1 d . . . H80 H 0.1233 0.0488 0.1087 0.118 Uiso 1 1 calc R . . C81 C 0.2431(5) 0.0639(6) 0.0427(5) 0.116(3) Uani 1 1 d . . . C82 C 0.2655(5) 0.0105(5) 0.0349(4) 0.115(3) Uani 1 1 d . . . H82 H 0.3002 -0.0023 0.0120 0.138 Uiso 1 1 calc R . . C83 C 0.2366(5) -0.0228(4) 0.0606(4) 0.093(2) Uani 1 1 d . . . C84 C 0.2570(5) -0.0814(5) 0.0547(4) 0.107(3) Uani 1 1 d . . . C85 C 0.1992(5) -0.1817(5) 0.1079(5) 0.114(3) Uani 1 1 d . . . C86 C 0.2084(4) -0.2364(4) 0.1089(4) 0.100(3) Uani 1 1 d DU . . C87 C 0.2474(7) -0.2728(6) 0.0754(6) 0.160(5) Uani 1 1 d DU . . H87 H 0.2720 -0.2586 0.0519 0.192 Uiso 1 1 calc R . . C88 C 0.2539(9) -0.3303(6) 0.0730(7) 0.175(6) Uani 1 1 d DU . . H88 H 0.2788 -0.3557 0.0475 0.210 Uiso 1 1 calc R . . C89 C 0.2214(10) -0.3459(7) 0.1103(8) 0.178(6) Uani 1 1 d DU . . H89 H 0.2247 -0.3827 0.1132 0.214 Uiso 1 1 calc R . . C90 C 0.1823(7) -0.3060(6) 0.1448(7) 0.165(6) Uani 1 1 d DU . . H90 H 0.1600 -0.3179 0.1706 0.198 Uiso 1 1 calc R . . C91 C 0.4005(5) 0.4461(4) 0.1379(4) 0.118(3) Uani 1 1 d DU . . H91 H 0.3803 0.4800 0.1564 0.141 Uiso 1 1 calc R . . C92 C 0.4428(6) 0.4513(5) 0.1020(5) 0.145(4) Uani 1 1 d DU . . H92 H 0.4512 0.4866 0.0951 0.174 Uiso 1 1 calc R . . C93 C 0.4755(7) 0.4004(5) 0.0737(6) 0.153(5) Uani 1 1 d DU . . H93 H 0.5080 0.4015 0.0491 0.183 Uiso 1 1 calc R . . C94 C 0.4571(6) 0.3522(5) 0.0844(5) 0.128(3) Uani 1 1 d DU . . H94 H 0.4741 0.3167 0.0656 0.154 Uiso 1 1 calc R . . C95 C 0.4129(5) 0.3548(4) 0.1233(4) 0.103(3) Uani 1 1 d DU . . C96 C 0.3942(4) 0.3023(3) 0.1388(3) 0.0797(19) Uani 1 1 d . . . C97 C 0.4213(4) 0.1640(4) 0.1146(4) 0.089(2) Uani 1 1 d . . . C98 C 0.3266(3) 0.1045(3) 0.1958(3) 0.0697(17) Uani 1 1 d . . . H98 H 0.2956 0.1176 0.2220 0.084 Uiso 1 1 calc R . . C99 C 0.3943(4) 0.1218(4) 0.1364(3) 0.081(2) Uani 1 1 d . . . C100 C 0.4117(4) 0.0676(4) 0.1228(3) 0.088(2) Uani 1 1 d . . . H100 H 0.4413 0.0543 0.0954 0.105 Uiso 1 1 calc R . . C101 C 0.3867(4) 0.0312(4) 0.1487(4) 0.094(2) Uani 1 1 d . . . C102 C 0.4066(4) -0.0236(4) 0.1429(3) 0.083(2) Uani 1 1 d . . . C103 C 0.3561(4) -0.1232(3) 0.1978(3) 0.079(2) Uani 1 1 d . . . C104 C 0.3627(4) -0.1800(3) 0.1981(3) 0.089(2) Uani 1 1 d DU . . C105 C 0.4031(5) -0.2157(4) 0.1610(4) 0.117(3) Uani 1 1 d DU . . H105 H 0.4263 -0.2027 0.1362 0.141 Uiso 1 1 calc R . . C106 C 0.4068(6) -0.2720(5) 0.1631(5) 0.129(4) Uani 1 1 d DU . . H106 H 0.4319 -0.2986 0.1388 0.155 Uiso 1 1 calc R . . C107 C 0.3743(5) -0.2870(5) 0.1998(5) 0.123(3) Uani 1 1 d DU . . H107 H 0.3772 -0.3241 0.2023 0.148 Uiso 1 1 calc R . . C108 C 0.3360(5) -0.2481(4) 0.2345(5) 0.116(3) Uani 1 1 d DU . . H108 H 0.3131 -0.2597 0.2602 0.139 Uiso 1 1 calc R . . C109 C 0.6340(6) 0.5147(5) 0.2403(7) 0.148(5) Uani 1 1 d DU . . H109 H 0.6351 0.5534 0.2668 0.177 Uiso 1 1 calc R . . C110 C 0.6268(8) 0.5044(7) 0.1838(8) 0.168(5) Uani 1 1 d DU . . H110 H 0.6231 0.5362 0.1725 0.201 Uiso 1 1 calc R . . C111 C 0.6253(7) 0.4478(7) 0.1448(6) 0.162(5) Uani 1 1 d DU . . H111 H 0.6202 0.4402 0.1068 0.195 Uiso 1 1 calc R . . C112 C 0.6315(5) 0.4033(5) 0.1633(5) 0.135(4) Uani 1 1 d DU . . H112 H 0.6310 0.3641 0.1381 0.161 Uiso 1 1 calc R . . C113 C 0.6387(5) 0.4166(5) 0.2212(6) 0.116(3) Uani 1 1 d DU . . C114 C 0.6443(4) 0.3690(4) 0.2416(5) 0.094(3) Uani 1 1 d . . . C115 C 0.6446(4) 0.2228(4) 0.1992(4) 0.081(2) Uani 1 1 d . . . C116 C 0.6491(3) 0.1799(4) 0.3158(3) 0.081(2) Uani 1 1 d . . . H116 H 0.6531 0.1998 0.3545 0.097 Uiso 1 1 calc R . . C117 C 0.6470(3) 0.1856(4) 0.2321(3) 0.0747(19) Uani 1 1 d . . . C118 C 0.6450(3) 0.1262(3) 0.2089(3) 0.0741(18) Uani 1 1 d . . . H118 H 0.6459 0.1067 0.1706 0.089 Uiso 1 1 calc R . . C119 C 0.6418(4) 0.0960(4) 0.2426(4) 0.087(2) Uani 1 1 d . . . C120 C 0.6322(4) 0.0302(4) 0.2217(4) 0.083(2) Uani 1 1 d . . . C121 C 0.6129(4) -0.0603(4) 0.2894(4) 0.0771(19) Uani 1 1 d . . . C122 C 0.5978(4) -0.1251(4) 0.2790(4) 0.088(2) Uani 1 1 d DU . . C123 C 0.5829(5) -0.1669(5) 0.2263(4) 0.113(3) Uani 1 1 d DU . . H123 H 0.5810 -0.1569 0.1949 0.136 Uiso 1 1 calc R . . C124 C 0.5702(6) -0.2272(5) 0.2227(6) 0.139(4) Uani 1 1 d DU . . H124 H 0.5633 -0.2592 0.1881 0.167 Uiso 1 1 calc R . . C125 C 0.5685(5) -0.2370(5) 0.2681(5) 0.128(4) Uani 1 1 d DU . . H125 H 0.5564 -0.2763 0.2660 0.153 Uiso 1 1 calc R . . C126 C 0.5831(4) -0.1934(4) 0.3162(4) 0.105(3) Uani 1 1 d DU . . H126 H 0.5823 -0.2030 0.3477 0.126 Uiso 1 1 calc R . . C127 C 0.8128(8) 0.5416(10) 0.2770(11) 0.235(9) Uani 1 1 d DU . . H127 H 0.8131 0.5798 0.3040 0.282 Uiso 1 1 calc R . . C128 C 0.8046(10) 0.5356(10) 0.2294(11) 0.241(11) Uani 1 1 d DU . . H128 H 0.7977 0.5696 0.2222 0.289 Uiso 1 1 calc R . . C129 C 0.8042(8) 0.4844(10) 0.1847(9) 0.223(9) Uani 1 1 d DU . . H129 H 0.7996 0.4811 0.1476 0.267 Uiso 1 1 calc R . . C130 C 0.8117(7) 0.4376(8) 0.2021(8) 0.207(7) Uani 1 1 d DU . . H130 H 0.8117 0.3987 0.1763 0.249 Uiso 1 1 calc R . . C131 C 0.8190(6) 0.4499(8) 0.2576(9) 0.156(5) Uani 1 1 d DU . . C132 C 0.8286(6) 0.4049(6) 0.2764(6) 0.124(4) Uani 1 1 d . . . C133 C 0.8241(4) 0.2587(5) 0.2367(5) 0.102(3) Uani 1 1 d . . . C134 C 0.8477(4) 0.2097(5) 0.3492(4) 0.100(3) Uani 1 1 d . . . H134 H 0.8594 0.2286 0.3878 0.120 Uiso 1 1 calc R . . C135 C 0.8311(4) 0.2156(5) 0.2656(4) 0.090(2) Uani 1 1 d . . . C136 C 0.8224(4) 0.1569(5) 0.2414(4) 0.098(3) Uani 1 1 d . . . H136 H 0.8164 0.1374 0.2026 0.118 Uiso 1 1 calc R . . C137 C 0.8224(4) 0.1262(4) 0.2741(4) 0.092(2) Uani 1 1 d . . . C138 C 0.8102(4) 0.0633(5) 0.2525(4) 0.097(3) Uani 1 1 d . . . C139 C 0.7978(4) -0.0351(5) 0.3133(6) 0.108(3) Uani 1 1 d . . . C140 C 0.7814(4) -0.0999(4) 0.3002(4) 0.097(2) Uani 1 1 d DU . . C141 C 0.7660(6) -0.1397(6) 0.2476(5) 0.139(4) Uani 1 1 d DU . . H141 H 0.7634 -0.1272 0.2177 0.167 Uiso 1 1 calc R . . C142 C 0.7541(7) -0.1995(7) 0.2389(6) 0.160(5) Uani 1 1 d DU . . H142 H 0.7452 -0.2285 0.2025 0.192 Uiso 1 1 calc R . . C143 C 0.7551(6) -0.2156(6) 0.2799(8) 0.163(5) Uani 1 1 d DU . . H143 H 0.7461 -0.2561 0.2745 0.196 Uiso 1 1 calc R . . C144 C 0.7700(5) -0.1711(7) 0.3328(6) 0.143(4) Uani 1 1 d DU . . H144 H 0.7708 -0.1826 0.3632 0.172 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O35 0.080(7) 0.109(8) 0.097(7) 0.042(6) 0.008(5) -0.004(6) O36 0.063(6) 0.094(7) 0.158(10) 0.065(7) -0.004(6) -0.004(5) O37 0.055(13) 0.142(16) 0.146(11) 0.096(11) 0.022(11) 0.018(10) N82 0.088(12) 0.29(4) 0.114(11) 0.110(16) 0.010(9) 0.031(17) O38 0.037(4) 0.073(5) 0.089(6) 0.044(4) 0.005(4) 0.011(4) O39 0.041(4) 0.089(6) 0.096(6) 0.051(5) -0.012(4) -0.012(4) O40 0.042(7) 0.041(4) 0.110(9) 0.034(5) 0.007(6) -0.010(4) N83 0.034(9) 0.084(9) 0.086(9) 0.033(7) -0.019(6) -0.005(8) Ni1 0.0830(8) 0.1397(11) 0.1534(12) 0.0785(9) -0.0085(7) 0.0063(7) Ni2 0.0621(6) 0.0871(7) 0.1316(9) 0.0489(6) 0.0024(5) 0.0070(5) Ni3 0.0723(7) 0.0958(8) 0.1507(11) 0.0524(7) -0.0100(6) 0.0011(6) Ni4 0.0755(8) 0.1213(10) 0.2251(18) 0.0841(11) -0.0102(9) -0.0092(7) Ni5 0.0681(6) 0.1214(9) 0.1128(9) 0.0559(7) -0.0017(5) -0.0035(6) Ni6 0.0503(5) 0.0869(6) 0.0895(6) 0.0443(5) 0.0055(4) 0.0059(4) Ni7 0.0528(5) 0.0852(6) 0.0946(7) 0.0403(5) 0.0001(4) -0.0011(4) Ni8 0.0572(6) 0.1190(9) 0.1389(10) 0.0594(7) -0.0023(6) -0.0010(6) Ni9 0.0639(6) 0.1203(8) 0.1023(8) 0.0514(6) -0.0037(5) -0.0048(6) Ni10 0.0508(5) 0.0791(6) 0.0862(6) 0.0385(4) 0.0064(4) 0.0037(4) Ni11 0.0540(5) 0.0822(6) 0.0795(6) 0.0358(4) 0.0006(4) 0.0097(4) Ni12 0.0602(6) 0.1175(8) 0.1129(8) 0.0530(6) -0.0025(5) 0.0091(6) Ni13 0.0840(8) 0.1178(9) 0.1398(11) 0.0605(8) -0.0130(7) -0.0215(7) Ni14 0.0714(6) 0.0926(7) 0.1062(8) 0.0509(6) -0.0001(5) -0.0033(5) Ni15 0.0778(7) 0.0990(7) 0.1087(8) 0.0523(6) 0.0032(5) 0.0156(6) Ni16 0.0720(7) 0.1251(9) 0.1352(10) 0.0657(7) 0.0051(6) 0.0229(6) O1 0.062(3) 0.095(4) 0.147(5) 0.051(3) 0.003(3) 0.004(3) O2 0.071(4) 0.111(5) 0.140(6) 0.045(4) -0.028(4) -0.001(3) O3 0.044(2) 0.091(3) 0.108(4) 0.044(3) 0.001(2) 0.002(2) O4 0.047(3) 0.122(4) 0.111(4) 0.058(3) 0.000(3) 0.011(3) O5 0.045(2) 0.099(3) 0.099(4) 0.046(3) -0.001(2) -0.001(2) O6 0.046(2) 0.101(4) 0.099(4) 0.042(3) -0.003(2) 0.005(2) O7 0.069(3) 0.115(4) 0.120(5) 0.060(4) 0.012(3) 0.012(3) O8 0.065(3) 0.118(4) 0.114(4) 0.063(4) -0.001(3) 0.018(3) O9 0.088(4) 0.124(5) 0.129(5) 0.074(4) -0.021(4) -0.015(3) O10 0.074(4) 0.098(4) 0.121(4) 0.054(3) -0.015(3) -0.017(3) O11 0.070(3) 0.077(3) 0.092(3) 0.042(2) 0.004(3) 0.004(2) O12 0.059(3) 0.089(3) 0.092(3) 0.044(3) 0.013(2) 0.008(2) O13 0.069(3) 0.089(3) 0.102(4) 0.041(3) -0.001(3) -0.002(3) O14 0.072(3) 0.079(3) 0.078(3) 0.031(3) 0.005(2) 0.022(2) O15 0.067(3) 0.116(5) 0.160(6) 0.073(4) 0.009(4) 0.010(3) O16 0.059(3) 0.111(4) 0.118(5) 0.050(4) 0.011(3) 0.023(3) O17 0.119(6) 0.174(8) 0.191(8) 0.096(6) -0.034(5) -0.004(5) O18 0.129(6) 0.130(6) 0.216(9) 0.086(6) 0.000(6) 0.036(5) O19 0.099(4) 0.084(3) 0.173(6) 0.056(4) 0.020(4) 0.020(3) O20 0.124(5) 0.075(3) 0.189(7) 0.050(4) -0.012(5) 0.012(3) O21 0.133(7) 0.105(5) 0.324(14) 0.060(7) 0.005(8) -0.002(5) O22 0.076(5) 0.163(7) 0.296(13) 0.096(8) 0.006(6) -0.027(5) O23 0.081(4) 0.133(5) 0.125(5) 0.067(4) -0.028(3) -0.026(3) O24 0.049(3) 0.150(6) 0.187(7) 0.065(5) 0.005(3) -0.007(3) O25 0.085(4) 0.169(6) 0.116(5) 0.041(4) -0.024(3) -0.002(4) O26 0.057(3) 0.131(5) 0.136(5) 0.047(4) -0.007(3) 0.008(3) O27 0.097(5) 0.171(7) 0.178(8) 0.057(6) -0.041(5) -0.031(5) O28 0.138(6) 0.155(6) 0.170(7) 0.097(5) -0.016(5) -0.052(5) O29 0.117(5) 0.110(4) 0.114(4) 0.062(3) 0.013(3) 0.012(4) O30 0.090(4) 0.118(4) 0.138(5) 0.074(4) 0.026(3) 0.034(3) O31 0.116(5) 0.159(6) 0.202(8) 0.119(6) -0.005(5) 0.031(5) O32 0.065(4) 0.157(6) 0.199(7) 0.089(5) 0.025(4) 0.033(4) O33 0.098(4) 0.157(6) 0.135(5) 0.084(5) 0.022(4) 0.045(4) O34 0.180(7) 0.137(5) 0.101(5) 0.064(4) 0.018(5) 0.042(5) O41 0.290(17) 0.165(10) 0.46(2) 0.153(13) 0.216(18) 0.108(11) O42 0.45(2) 0.143(8) 0.101(6) 0.017(6) -0.067(10) 0.044(10) O43 0.163(12) 0.34(2) 0.41(2) 0.152(18) 0.101(14) 0.115(13) N1 0.066(5) 0.140(7) 0.165(8) 0.057(6) -0.001(5) -0.006(4) N2 0.068(4) 0.091(5) 0.129(6) 0.033(4) -0.002(4) -0.006(3) N3 0.081(5) 0.071(4) 0.128(6) 0.045(4) 0.008(4) 0.010(3) N4 0.073(4) 0.143(7) 0.122(6) 0.047(5) 0.019(4) 0.008(4) N5 0.058(4) 0.096(4) 0.110(5) 0.039(4) -0.006(3) 0.001(3) N6 0.067(4) 0.093(5) 0.138(7) 0.039(4) -0.002(4) 0.006(4) N7 0.111(6) 0.153(7) 0.089(6) 0.012(5) -0.006(4) 0.021(5) N8 0.056(4) 0.091(4) 0.124(6) 0.019(4) -0.003(4) 0.007(3) N9 0.069(5) 0.097(5) 0.126(6) 0.032(4) -0.019(4) 0.003(4) N10 0.095(6) 0.114(6) 0.174(9) 0.034(5) -0.031(6) 0.000(5) N11 0.062(4) 0.141(6) 0.133(7) 0.051(5) 0.006(4) 0.006(4) N12 0.051(3) 0.102(4) 0.092(4) 0.043(3) 0.006(3) 0.012(3) N13 0.049(3) 0.101(4) 0.082(4) 0.047(3) 0.021(3) 0.023(3) N14 0.070(4) 0.120(5) 0.089(5) 0.027(4) 0.014(3) -0.003(4) N15 0.050(3) 0.096(4) 0.088(4) 0.046(3) 0.010(3) 0.012(3) N16 0.055(3) 0.069(3) 0.082(4) 0.029(3) 0.001(3) 0.005(3) N17 0.082(4) 0.132(5) 0.071(4) 0.050(4) 0.007(3) 0.016(4) N18 0.060(4) 0.073(4) 0.104(5) 0.025(3) -0.021(3) -0.009(3) N19 0.064(4) 0.098(4) 0.084(4) 0.023(3) -0.006(3) 0.006(3) N20 0.087(5) 0.091(5) 0.156(7) 0.046(4) 0.023(5) -0.007(4) N21 0.055(4) 0.144(6) 0.118(6) 0.062(5) 0.013(4) 0.007(4) N22 0.062(4) 0.111(5) 0.097(5) 0.046(4) 0.017(3) 0.027(3) N23 0.039(3) 0.087(4) 0.092(4) 0.033(3) 0.009(3) 0.017(3) N24 0.074(4) 0.116(5) 0.103(5) 0.039(4) 0.018(3) 0.037(4) N25 0.056(3) 0.086(4) 0.100(4) 0.047(3) 0.014(3) 0.005(3) N26 0.056(3) 0.068(3) 0.072(3) 0.030(3) -0.011(2) -0.001(3) N27 0.069(4) 0.096(4) 0.096(5) 0.039(4) 0.011(3) 0.022(3) N28 0.066(3) 0.093(4) 0.051(3) 0.024(3) 0.002(2) 0.011(3) N29 0.076(4) 0.082(4) 0.082(4) 0.034(3) -0.012(3) 0.007(3) N30 0.083(5) 0.101(5) 0.113(5) 0.049(4) -0.013(4) 0.001(4) N31 0.078(5) 0.156(7) 0.135(7) 0.079(6) 0.019(5) 0.008(5) N32 0.079(5) 0.106(5) 0.125(6) 0.064(4) 0.008(4) 0.011(4) N33 0.045(3) 0.097(4) 0.105(5) 0.044(4) -0.001(3) 0.001(3) N34 0.088(5) 0.122(6) 0.094(5) 0.047(4) 0.011(4) 0.019(4) N35 0.067(4) 0.103(5) 0.095(4) 0.056(4) 0.007(3) 0.007(3) N36 0.060(3) 0.089(4) 0.099(4) 0.046(4) -0.001(3) 0.003(3) N37 0.074(4) 0.088(4) 0.108(5) 0.054(4) 0.008(3) 0.012(3) N38 0.063(4) 0.089(4) 0.114(5) 0.055(4) 0.001(3) 0.006(3) N39 0.085(5) 0.123(5) 0.096(5) 0.057(4) -0.011(4) -0.006(4) N40 0.071(4) 0.117(5) 0.135(6) 0.064(4) 0.000(4) 0.022(4) N41 0.112(6) 0.119(6) 0.137(7) 0.071(5) -0.013(5) -0.014(5) N42 0.088(5) 0.153(8) 0.111(6) 0.074(6) 0.008(4) -0.014(5) N43 0.092(5) 0.134(6) 0.101(5) 0.065(5) 0.003(4) 0.008(5) N44 0.153(9) 0.154(8) 0.176(9) 0.082(7) 0.082(8) 0.023(7) N45 0.076(4) 0.106(5) 0.092(5) 0.032(4) 0.000(4) 0.000(4) N46 0.078(4) 0.100(5) 0.104(5) 0.055(4) 0.007(4) 0.020(4) N47 0.121(7) 0.141(8) 0.218(11) 0.095(7) 0.056(8) 0.022(6) N48 0.074(4) 0.091(5) 0.115(5) 0.040(4) 0.003(4) 0.010(4) N49 0.087(5) 0.115(6) 0.119(6) 0.055(4) 0.008(4) 0.008(4) N50 0.146(8) 0.094(5) 0.145(7) 0.065(5) -0.052(6) -0.031(5) N51 0.073(4) 0.093(5) 0.148(6) 0.073(4) 0.015(4) 0.019(4) N52 0.073(4) 0.083(4) 0.099(4) 0.048(3) 0.017(3) 0.007(3) N53 0.061(3) 0.119(5) 0.089(4) 0.056(4) 0.020(3) 0.006(4) N54 0.109(6) 0.156(7) 0.147(7) 0.095(6) 0.068(5) 0.050(5) N55 0.049(3) 0.077(3) 0.082(4) 0.030(3) 0.009(3) 0.010(3) N56 0.046(3) 0.081(4) 0.082(4) 0.038(3) 0.010(2) 0.007(3) N57 0.096(5) 0.105(5) 0.193(8) 0.077(5) 0.072(5) 0.045(4) N58 0.054(3) 0.081(4) 0.080(4) 0.030(3) 0.015(3) 0.013(3) N59 0.071(4) 0.059(3) 0.100(4) 0.028(3) 0.007(3) 0.008(3) N60 0.085(4) 0.090(4) 0.132(6) 0.061(4) 0.013(4) 0.011(4) N61 0.071(4) 0.096(5) 0.147(7) 0.062(5) -0.012(4) -0.014(4) N62 0.055(3) 0.124(6) 0.106(5) 0.072(5) 0.002(3) -0.009(3) N63 0.052(3) 0.108(5) 0.091(4) 0.061(4) 0.011(3) 0.001(3) N64 0.099(5) 0.106(5) 0.077(5) 0.040(4) 0.007(3) 0.000(4) N65 0.056(3) 0.075(3) 0.070(4) 0.035(3) 0.006(2) 0.008(3) N66 0.059(3) 0.069(3) 0.072(4) 0.026(3) -0.002(2) 0.004(3) N67 0.094(5) 0.085(4) 0.086(5) 0.028(3) 0.013(3) 0.011(3) N68 0.057(3) 0.080(4) 0.061(3) 0.010(3) -0.002(2) 0.020(3) N69 0.057(3) 0.086(4) 0.096(5) 0.018(3) 0.003(3) 0.004(3) N70 0.094(5) 0.078(4) 0.098(5) 0.041(3) 0.005(3) 0.002(3) N71 0.102(7) 0.173(10) 0.307(17) 0.172(12) -0.011(9) 0.001(8) N72 0.050(4) 0.177(9) 0.141(7) 0.089(7) 0.005(4) -0.012(5) N73 0.074(5) 0.146(7) 0.137(7) 0.090(6) 0.024(4) 0.027(5) N74 0.069(4) 0.175(8) 0.161(8) 0.106(7) 0.019(5) 0.024(5) N75 0.054(4) 0.122(5) 0.139(7) 0.068(5) 0.013(4) 0.014(4) N76 0.068(4) 0.117(6) 0.108(6) 0.060(4) 0.005(4) 0.021(4) N77 0.071(5) 0.155(7) 0.143(8) 0.064(6) 0.009(4) 0.024(5) N78 0.046(3) 0.108(6) 0.141(7) 0.040(5) -0.011(3) 0.001(3) N79 0.055(4) 0.137(7) 0.121(6) 0.060(5) 0.005(4) 0.016(4) N80 0.078(5) 0.112(6) 0.132(7) 0.042(5) 0.004(4) 0.006(4) N81 0.077(5) 0.115(5) 0.126(7) 0.056(5) 0.008(4) 0.031(4) N84 0.113(7) 0.117(7) 0.169(10) 0.050(7) -0.005(7) 0.039(6) C1 0.059(6) 0.207(13) 0.215(14) 0.020(10) 0.002(7) 0.008(7) C2 0.085(9) 0.294(19) 0.193(15) 0.065(14) 0.018(9) -0.010(10) C3 0.086(8) 0.293(18) 0.148(11) 0.034(12) -0.006(8) -0.037(10) C4 0.069(6) 0.204(13) 0.169(11) 0.050(9) 0.008(7) -0.004(7) C5 0.080(6) 0.113(7) 0.125(8) 0.032(6) -0.009(6) -0.010(5) C6 0.069(5) 0.075(5) 0.131(8) 0.043(5) 0.004(5) 0.005(4) C7 0.077(6) 0.101(6) 0.116(7) 0.045(5) 0.027(5) 0.032(5) C8 0.062(5) 0.088(5) 0.131(7) 0.040(5) 0.001(5) 0.012(4) C9 0.078(5) 0.085(5) 0.101(6) 0.028(4) 0.010(5) 0.033(4) C10 0.087(6) 0.108(6) 0.096(6) 0.035(5) 0.024(5) 0.021(5) C11 0.087(6) 0.099(6) 0.113(7) 0.035(5) 0.024(5) 0.027(5) C12 0.118(9) 0.094(6) 0.098(7) 0.031(5) 0.009(6) 0.027(6) C13 0.077(7) 0.076(5) 0.160(10) 0.032(6) -0.036(7) 0.000(4) C14 0.079(7) 0.119(7) 0.163(10) 0.044(7) -0.018(7) 0.024(6) C15 0.110(9) 0.144(10) 0.174(12) 0.040(9) -0.051(9) -0.012(7) C16 0.131(10) 0.135(9) 0.150(10) 0.036(7) -0.048(8) -0.001(8) C17 0.115(10) 0.195(12) 0.162(12) 0.074(10) -0.054(9) 0.014(9) C18 0.096(8) 0.156(10) 0.220(14) 0.072(10) -0.072(9) -0.013(7) C19 0.031(4) 0.202(12) 0.211(13) 0.085(10) 0.012(5) -0.012(5) C20 0.075(7) 0.297(19) 0.158(12) 0.072(12) -0.003(7) -0.013(9) C21 0.056(6) 0.309(17) 0.143(10) 0.079(10) 0.007(6) -0.006(8) C22 0.068(6) 0.210(12) 0.130(8) 0.049(8) 0.007(5) 0.013(7) C23 0.064(5) 0.130(7) 0.113(7) 0.028(5) 0.016(5) 0.009(5) C24 0.061(4) 0.070(4) 0.106(6) 0.034(4) 0.014(4) 0.009(3) C25 0.063(4) 0.083(4) 0.079(5) 0.026(4) 0.004(4) 0.012(4) C26 0.053(4) 0.069(4) 0.090(5) 0.037(3) -0.001(3) 0.000(3) C27 0.058(4) 0.085(4) 0.079(5) 0.032(3) -0.006(3) 0.014(3) C28 0.063(4) 0.113(6) 0.083(5) 0.048(4) 0.016(3) 0.013(4) C29 0.070(5) 0.083(5) 0.098(6) 0.038(4) 0.005(4) -0.001(4) C30 0.062(5) 0.084(5) 0.111(7) 0.044(4) -0.021(4) -0.003(4) C31 0.053(4) 0.063(4) 0.105(6) 0.031(4) -0.004(4) 0.001(3) C32 0.068(5) 0.086(5) 0.130(8) 0.027(5) -0.022(5) 0.001(4) C33 0.091(6) 0.107(6) 0.099(6) 0.032(5) -0.006(5) 0.016(5) C34 0.104(8) 0.137(8) 0.132(8) 0.068(6) -0.028(6) -0.024(6) C35 0.106(8) 0.122(8) 0.146(10) 0.049(7) -0.045(7) -0.009(6) C36 0.058(5) 0.115(7) 0.142(8) 0.032(6) -0.043(5) -0.029(5) C37 0.047(4) 0.189(10) 0.162(9) 0.108(8) -0.015(5) 0.000(6) C38 0.055(6) 0.299(18) 0.198(13) 0.129(13) 0.018(7) 0.050(9) C39 0.065(6) 0.255(16) 0.200(13) 0.066(11) 0.021(7) 0.063(8) C40 0.090(7) 0.250(14) 0.104(7) 0.067(8) -0.001(6) 0.022(8) C41 0.041(4) 0.202(10) 0.114(7) 0.090(7) 0.016(4) 0.033(5) C42 0.068(4) 0.090(5) 0.090(5) 0.043(4) 0.010(4) 0.014(4) C43 0.068(4) 0.082(5) 0.091(5) 0.039(4) 0.005(4) 0.018(4) C44 0.049(4) 0.074(4) 0.076(4) 0.033(3) 0.014(3) 0.009(3) C45 0.081(5) 0.067(4) 0.091(5) 0.038(4) 0.014(4) 0.020(4) C46 0.064(4) 0.073(4) 0.092(5) 0.035(4) 0.005(4) 0.011(3) C47 0.075(4) 0.068(4) 0.068(4) 0.032(3) 0.005(3) 0.019(3) C48 0.063(4) 0.070(4) 0.091(5) 0.037(4) 0.005(3) 0.013(3) C49 0.056(4) 0.099(5) 0.086(5) 0.050(4) -0.011(4) -0.001(4) C50 0.069(5) 0.131(7) 0.095(6) 0.049(5) -0.003(4) 0.010(5) C51 0.066(5) 0.141(8) 0.137(8) 0.076(7) -0.003(5) 0.022(5) C52 0.089(7) 0.139(8) 0.118(7) 0.048(6) -0.024(5) 0.016(6) C53 0.097(7) 0.148(9) 0.147(9) 0.071(8) -0.052(7) -0.007(7) C54 0.065(5) 0.145(8) 0.121(7) 0.057(6) -0.032(5) 0.011(5) C55 0.086(7) 0.227(13) 0.122(9) 0.089(9) -0.021(6) -0.038(8) C56 0.080(7) 0.292(18) 0.130(10) 0.062(11) 0.020(7) 0.004(9) C57 0.091(8) 0.270(16) 0.158(11) 0.082(11) 0.018(7) 0.052(9) C58 0.070(7) 0.292(17) 0.159(11) 0.074(11) 0.010(7) 0.026(9) C59 0.075(6) 0.149(8) 0.122(8) 0.060(7) 0.004(5) -0.009(6) C60 0.068(6) 0.161(10) 0.140(9) 0.099(8) -0.011(6) -0.013(6) C61 0.071(5) 0.095(5) 0.112(6) 0.059(5) 0.014(5) 0.020(5) C62 0.084(5) 0.084(5) 0.091(5) 0.045(4) 0.006(4) 0.012(4) C63 0.104(6) 0.098(6) 0.092(6) 0.057(5) 0.025(5) 0.040(5) C64 0.081(5) 0.092(5) 0.098(6) 0.055(4) 0.008(4) 0.013(4) C65 0.087(5) 0.088(5) 0.085(5) 0.053(4) -0.008(4) -0.001(4) C66 0.093(6) 0.078(5) 0.083(5) 0.043(4) 0.010(4) 0.011(4) C67 0.076(5) 0.114(7) 0.098(6) 0.067(5) 0.009(4) 0.033(5) C68 0.061(4) 0.135(7) 0.114(7) 0.079(6) 0.013(4) 0.025(5) C69 0.095(6) 0.125(7) 0.088(6) 0.041(5) 0.011(5) 0.004(5) C70 0.081(6) 0.126(7) 0.139(8) 0.061(6) 0.001(6) 0.015(6) C71 0.094(7) 0.151(9) 0.139(9) 0.076(7) -0.033(6) -0.022(7) C72 0.068(5) 0.180(11) 0.131(8) 0.069(8) -0.009(5) 0.009(6) C73 0.157(12) 0.176(12) 0.174(12) 0.094(10) 0.035(9) -0.004(9) C74 0.186(14) 0.129(10) 0.273(18) 0.105(11) 0.049(13) -0.006(10) C75 0.161(12) 0.170(13) 0.244(16) 0.125(12) 0.045(11) 0.007(10) C76 0.170(12) 0.172(12) 0.158(11) 0.093(9) 0.002(9) 0.015(9) C77 0.110(8) 0.128(8) 0.143(9) 0.080(7) 0.024(6) 0.004(6) C78 0.092(7) 0.150(9) 0.094(6) 0.075(6) -0.001(5) -0.013(6) C79 0.100(7) 0.161(10) 0.082(6) 0.048(6) 0.019(5) 0.026(7) C80 0.057(4) 0.128(7) 0.098(6) 0.043(5) 0.003(4) -0.019(5) C81 0.090(6) 0.168(10) 0.137(8) 0.109(8) 0.021(6) 0.030(6) C82 0.090(6) 0.161(9) 0.115(7) 0.074(7) 0.033(5) 0.023(6) C83 0.078(5) 0.107(6) 0.099(6) 0.051(5) 0.008(4) -0.003(5) C84 0.088(6) 0.113(7) 0.118(7) 0.038(6) 0.030(5) 0.020(5) C85 0.076(6) 0.129(8) 0.132(8) 0.056(6) -0.021(6) 0.006(6) C86 0.077(5) 0.106(7) 0.111(7) 0.035(5) 0.002(5) 0.017(5) C87 0.167(12) 0.155(11) 0.178(12) 0.092(9) 0.004(10) 0.016(10) C88 0.222(16) 0.109(9) 0.191(14) 0.044(9) 0.036(12) 0.052(9) C89 0.202(16) 0.160(13) 0.184(15) 0.079(11) 0.007(12) 0.042(12) C90 0.138(11) 0.136(10) 0.205(14) 0.084(10) -0.065(10) -0.045(9) C91 0.117(7) 0.094(6) 0.167(9) 0.079(6) 0.025(7) 0.011(5) C92 0.142(9) 0.107(7) 0.231(13) 0.112(8) 0.055(9) 0.023(7) C93 0.158(10) 0.125(8) 0.209(12) 0.094(8) 0.083(9) 0.016(8) C94 0.144(9) 0.098(6) 0.168(10) 0.075(6) 0.043(8) 0.023(6) C95 0.099(6) 0.092(6) 0.123(7) 0.058(5) -0.007(5) -0.011(5) C96 0.083(5) 0.069(4) 0.096(5) 0.041(4) 0.014(4) 0.013(4) C97 0.085(5) 0.093(5) 0.110(6) 0.059(5) 0.026(5) 0.016(4) C98 0.047(3) 0.086(5) 0.081(4) 0.042(4) 0.000(3) 0.004(3) C99 0.056(4) 0.111(6) 0.089(5) 0.052(4) 0.007(3) 0.028(4) C100 0.072(5) 0.096(5) 0.096(5) 0.043(4) 0.016(4) -0.003(4) C101 0.050(4) 0.143(8) 0.110(6) 0.075(5) 0.011(4) 0.012(4) C102 0.068(4) 0.094(5) 0.108(6) 0.059(4) 0.020(4) 0.016(4) C103 0.057(4) 0.085(5) 0.105(6) 0.053(4) 0.000(4) -0.001(4) C104 0.097(6) 0.083(5) 0.094(5) 0.040(4) 0.004(4) 0.022(4) C105 0.124(8) 0.098(6) 0.138(8) 0.056(6) 0.018(6) 0.016(6) C106 0.139(9) 0.110(7) 0.161(10) 0.069(7) 0.062(8) 0.031(6) C107 0.099(7) 0.109(7) 0.185(10) 0.078(7) 0.017(7) 0.036(6) C108 0.100(7) 0.091(6) 0.171(9) 0.071(6) 0.007(6) 0.014(5) C109 0.120(9) 0.116(8) 0.217(14) 0.086(9) -0.021(9) 0.012(7) C110 0.188(13) 0.146(11) 0.218(15) 0.128(11) 0.037(11) 0.018(10) C111 0.213(14) 0.142(10) 0.153(11) 0.092(9) 0.024(10) -0.003(10) C112 0.172(11) 0.125(8) 0.135(9) 0.079(7) 0.033(8) 0.029(7) C113 0.089(6) 0.107(7) 0.186(11) 0.090(7) 0.025(6) 0.024(5) C114 0.044(4) 0.081(5) 0.135(8) 0.028(5) 0.000(4) -0.014(4) C115 0.054(4) 0.089(5) 0.097(6) 0.040(4) 0.010(3) -0.012(4) C116 0.042(3) 0.113(6) 0.086(5) 0.049(5) -0.012(3) -0.013(4) C117 0.043(3) 0.102(5) 0.076(5) 0.037(4) -0.006(3) 0.001(3) C118 0.058(4) 0.079(5) 0.079(5) 0.024(4) 0.009(3) 0.008(3) C119 0.052(4) 0.112(6) 0.101(6) 0.051(5) 0.003(4) 0.003(4) C120 0.049(4) 0.116(6) 0.087(6) 0.044(5) 0.006(3) 0.009(4) C121 0.056(4) 0.101(5) 0.084(5) 0.042(5) 0.007(3) 0.029(4) C122 0.084(5) 0.088(5) 0.098(6) 0.038(5) 0.018(4) 0.023(4) C123 0.115(7) 0.115(7) 0.110(7) 0.040(6) 0.020(5) 0.023(6) C124 0.139(9) 0.095(7) 0.153(11) 0.018(7) 0.004(8) 0.015(6) C125 0.158(10) 0.097(7) 0.127(9) 0.048(7) 0.003(7) 0.012(6) C126 0.090(6) 0.098(6) 0.117(7) 0.045(5) -0.031(5) -0.005(5) C127 0.122(12) 0.30(2) 0.37(3) 0.22(2) 0.031(16) 0.046(13) C128 0.177(15) 0.29(2) 0.36(3) 0.24(2) 0.03(2) 0.070(16) C129 0.186(15) 0.31(2) 0.25(2) 0.196(18) 0.026(15) 0.020(17) C130 0.171(13) 0.271(18) 0.258(18) 0.208(16) -0.007(13) 0.004(12) C131 0.088(7) 0.168(12) 0.254(18) 0.140(13) -0.010(9) 0.010(9) C132 0.092(7) 0.132(9) 0.123(9) 0.028(8) -0.004(6) -0.001(6) C133 0.053(4) 0.120(8) 0.120(8) 0.045(6) -0.011(4) -0.014(5) C134 0.069(5) 0.113(7) 0.125(7) 0.069(6) -0.015(4) -0.011(5) C135 0.049(4) 0.119(7) 0.098(6) 0.046(5) -0.005(4) -0.006(4) C136 0.059(5) 0.137(8) 0.091(6) 0.040(6) 0.006(4) 0.000(5) C137 0.062(5) 0.099(6) 0.106(7) 0.038(5) -0.014(4) 0.006(4) C138 0.068(5) 0.171(10) 0.071(5) 0.058(6) 0.013(4) 0.045(5) C139 0.057(5) 0.111(7) 0.142(10) 0.033(7) 0.003(5) 0.026(5) C140 0.068(5) 0.118(7) 0.102(7) 0.039(6) 0.003(4) 0.018(5) C141 0.119(9) 0.146(10) 0.146(10) 0.051(8) 0.029(7) 0.011(8) C142 0.149(11) 0.133(11) 0.154(12) 0.005(9) 0.031(9) 0.015(9) C143 0.165(12) 0.113(9) 0.220(17) 0.070(11) 0.021(12) 0.042(8) C144 0.111(8) 0.145(10) 0.173(12) 0.061(9) 0.034(8) 0.011(8) _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 O35 N82 1.303(18) . ? O36 N82 1.298(17) . ? O37 N82 1.270(17) . ? O38 N83 1.321(17) . ? O39 N83 1.297(17) . ? O40 N83 1.275(16) . ? Ni1 N1 1.989(9) . ? Ni1 N41 1.998(10) . ? Ni1 O1 2.052(7) . ? Ni1 O17 2.069(8) . ? Ni1 O18 2.091(8) . ? Ni1 O9 2.099(7) . ? Ni2 N3 1.951(8) . ? Ni2 N51 1.995(7) . ? Ni2 O19 2.049(6) . ? Ni2 O11 2.052(5) . ? Ni2 O1 2.142(5) . ? Ni2 N5 2.174(7) . ? Ni3 N8 1.933(9) . ? Ni3 N61 1.991(8) . ? Ni3 O13 2.023(6) . ? Ni3 O20 2.052(6) . ? Ni3 O2 2.141(6) . ? Ni3 N6 2.176(7) . ? Ni4 N71 2.012(15) . ? Ni4 O22 2.055(8) . ? Ni4 O21 2.056(9) . ? Ni4 O2 2.066(7) . ? Ni4 N10 2.067(11) . ? Ni4 O15 2.080(7) . ? Ni5 N43 1.888(9) . ? Ni5 N11 2.005(8) . ? Ni5 O23 2.046(6) . ? Ni5 O3 2.062(5) . ? Ni5 O9 2.135(6) . ? Ni5 N45 2.192(8) . ? Ni6 N53 1.978(6) . ? Ni6 N13 1.988(5) . ? Ni6 O11 2.121(5) . ? Ni6 O3 2.134(4) . ? Ni6 N55 2.161(6) . ? Ni6 N15 2.170(6) . ? Ni7 N18 1.909(7) . ? Ni7 N63 1.985(6) . ? Ni7 N16 2.125(5) . ? Ni7 O4 2.133(5) . ? Ni7 O13 2.149(5) . ? Ni7 N65 2.187(6) . ? Ni8 N73 1.935(10) . ? Ni8 N20 2.015(9) . ? Ni8 O24 2.033(6) . ? Ni8 O4 2.040(5) . ? Ni8 O15 2.152(6) . ? Ni8 N75 2.198(8) . ? Ni9 N48 1.945(8) . ? Ni9 N21 1.990(7) . ? Ni9 O5 2.048(5) . ? Ni9 O25 2.074(6) . ? Ni9 N46 2.148(7) . ? Ni9 O10 2.160(6) . ? Ni10 N23 1.972(6) . ? Ni10 N58 1.973(5) . ? Ni10 O12 2.108(5) . ? Ni10 O5 2.136(4) . ? Ni10 N25 2.152(6) . ? Ni10 N56 2.165(6) . ? Ni11 N28 1.946(5) . ? Ni11 N68 1.998(5) . ? Ni11 O6 2.128(5) . ? Ni11 O14 2.146(5) . ? Ni11 N26 2.155(5) . ? Ni11 N66 2.156(6) . ? Ni12 N78 1.943(9) . ? Ni12 N30 1.997(8) . ? Ni12 O26 2.037(6) . ? Ni12 O6 2.054(5) . ? Ni12 O16 2.152(6) . ? Ni12 N76 2.205(7) . ? Ni13 N50 1.951(11) . ? Ni13 N31 2.029(9) . ? Ni13 O27 2.036(7) . ? Ni13 O7 2.051(6) . ? Ni13 O10 2.054(6) . ? Ni13 O28 2.062(7) . ? Ni14 N33 1.954(7) . ? Ni14 N60 1.994(8) . ? Ni14 O29 2.063(6) . ? Ni14 O12 2.084(5) . ? Ni14 O7 2.141(6) . ? Ni14 N35 2.204(6) . ? Ni15 N38 1.938(7) . ? Ni15 N70 1.986(7) . ? Ni15 O14 2.050(5) . ? Ni15 O8 2.128(5) . ? Ni15 O30 2.146(6) . ? Ni15 N36 2.161(6) . ? Ni16 N80 2.002(9) . ? Ni16 N40 2.033(8) . ? Ni16 O8 2.087(6) . ? Ni16 O16 2.103(6) . ? Ni16 O31 2.105(7) . ? Ni16 O32 2.106(6) . ? O1 C6 1.303(11) . ? O2 C13 1.262(14) . ? O3 C24 1.280(9) . ? O4 C31 1.307(9) . ? O5 C42 1.262(9) . ? O6 C49 1.297(10) . ? O7 C60 1.219(14) . ? O8 C67 1.274(11) . ? O9 C78 1.317(13) . ? O10 C85 1.280(13) . ? O11 C96 1.276(9) . ? O12 C103 1.295(9) . ? O13 C114 1.277(11) . ? O14 C121 1.237(9) . ? O15 C132 1.294(13) . ? O16 C139 1.272(12) . ? O30 N81 1.266(9) . ? O33 N81 1.199(10) . ? O34 N81 1.249(10) . ? O41 N84 1.220(16) . ? O42 N84 1.036(13) . ? O43 N84 1.158(16) . ? N1 C5 1.326(13) . ? N1 C1 1.368(13) . ? N2 C6 1.300(12) . ? N2 N3 1.363(10) . ? N3 C7 1.245(11) . ? N4 C7 1.350(12) . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? N5 C9 1.268(11) . ? N5 C8 1.359(10) . ? N6 C11 1.292(12) . ? N6 C8 1.351(11) . ? N7 C12 1.318(13) . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? N8 C12 1.283(13) . ? N8 N9 1.395(10) . ? N9 C13 1.335(15) . ? N10 C14 1.339(15) . ? N10 C18 1.405(13) . ? N11 C19 1.309(11) . ? N11 C23 1.347(12) . ? N12 C24 1.256(10) . ? N12 N13 1.363(8) . ? N13 C25 1.280(9) . ? N14 C25 1.311(10) . ? N14 H14A 0.8800 . ? N14 H14B 0.8800 . ? N15 C27 1.311(9) . ? N15 C26 1.313(8) . ? N16 C26 1.313(8) . ? N16 C29 1.332(10) . ? N17 C30 1.287(10) . ? N17 H17A 0.8800 . ? N17 H17B 0.8800 . ? N18 C30 1.325(11) . ? N18 N19 1.422(8) . ? N19 C31 1.308(10) . ? N20 C32 1.286(12) . ? N20 C36 1.329(11) . ? N21 C41 1.311(12) . ? N21 C37 1.396(10) . ? N22 C42 1.325(10) . ? N22 N23 1.340(8) . ? N23 C43 1.282(9) . ? N24 C43 1.320(10) . ? N24 H24A 0.8800 . ? N24 H24B 0.8800 . ? N25 C44 1.299(8) . ? N25 C45 1.329(10) . ? N26 C44 1.295(8) . ? N26 C47 1.386(9) . ? N27 C48 1.307(9) . ? N27 H27A 0.8800 . ? N27 H27B 0.8800 . ? N28 C48 1.290(9) . ? N28 N29 1.375(8) . ? N29 C49 1.283(10) . ? N30 C50 1.330(11) . ? N30 C54 1.352(10) . ? N31 C59 1.337(13) . ? N31 C55 1.359(13) . ? N32 N33 1.326(9) . ? N32 C60 1.390(14) . ? N33 C61 1.253(10) . ? N34 C61 1.365(11) . ? N34 H34A 0.8800 . ? N34 H34B 0.8800 . ? N35 C62 1.304(10) . ? N35 C63 1.345(10) . ? N36 C62 1.336(10) . ? N36 C65 1.391(11) . ? N37 C66 1.324(10) . ? N37 H37A 0.8800 . ? N37 H37B 0.8800 . ? N38 C66 1.283(10) . ? N38 N39 1.397(9) . ? N39 C67 1.311(11) . ? N40 C68 1.291(10) . ? N40 C72 1.354(12) . ? N41 C73 1.291(15) . ? N41 C77 1.334(14) . ? N42 C78 1.240(13) . ? N42 N43 1.364(11) . ? N43 C79 1.267(13) . ? N44 C79 1.346(13) . ? N44 H44A 0.8800 . ? N44 H44B 0.8800 . ? N45 C80 1.325(11) . ? N45 C81 1.327(12) . ? N46 C80 1.296(11) . ? N46 C83 1.313(11) . ? N47 C84 1.328(13) . ? N47 H47A 0.8800 . ? N47 H47B 0.8800 . ? N48 C84 1.240(12) . ? N48 N49 1.330(10) . ? N49 C85 1.426(14) . ? N50 C86 1.344(13) . ? N50 C90 1.347(15) . ? N51 C91 1.248(11) . ? N51 C95 1.355(12) . ? N52 C96 1.298(9) . ? N52 N53 1.331(9) . ? N53 C97 1.310(10) . ? N54 C97 1.343(11) . ? N54 H54A 0.8800 . ? N54 H54B 0.8800 . ? N55 C98 1.282(9) . ? N55 C99 1.342(9) . ? N56 C101 1.331(10) . ? N56 C98 1.337(9) . ? N57 C102 1.357(11) . ? N57 H57A 0.8800 . ? N57 H57B 0.8800 . ? N58 C102 1.299(9) . ? N58 N59 1.354(8) . ? N59 C103 1.298(9) . ? N60 C108 1.288(11) . ? N60 C104 1.319(11) . ? N61 C113 1.278(13) . ? N61 C109 1.375(13) . ? N62 C114 1.289(11) . ? N62 N63 1.398(9) . ? N63 C115 1.289(10) . ? N64 C115 1.284(10) . ? N64 H64A 0.8800 . ? N64 H64B 0.8800 . ? N65 C116 1.308(9) . ? N65 C117 1.343(9) . ? N66 C116 1.275(10) . ? N66 C119 1.344(10) . ? N67 C120 1.307(10) . ? N67 H67A 0.8800 . ? N67 H67B 0.8800 . ? N68 C120 1.271(10) . ? N68 N69 1.355(9) . ? N69 C121 1.305(10) . ? N70 C122 1.319(10) . ? N70 C126 1.345(11) . ? N71 C127 1.24(2) . ? N71 C131 1.26(2) . ? N72 C132 1.318(14) . ? N72 N73 1.434(11) . ? N73 C133 1.204(12) . ? N74 C133 1.387(13) . ? N74 H74A 0.8800 . ? N74 H74B 0.8800 . ? N75 C134 1.341(11) . ? N75 C135 1.349(11) . ? N76 C134 1.287(11) . ? N76 C137 1.323(11) . ? N77 C138 1.297(12) . ? N77 H77A 0.8800 . ? N77 H77B 0.8800 . ? N78 C138 1.278(11) . ? N78 N79 1.395(11) . ? N79 C139 1.287(13) . ? N80 C140 1.289(12) . ? N80 C144 1.324(15) . ? C1 C2 1.44(2) . ? C1 H1 0.9500 . ? C2 C3 1.31(2) . ? C2 H2 0.9500 . ? C3 C4 1.379(16) . ? C3 H3 0.9500 . ? C4 C5 1.377(16) . ? C4 H4 0.9500 . ? C5 C6 1.458(13) . ? C7 C9 1.469(13) . ? C8 H8 0.9500 . ? C9 C10 1.365(12) . ? C10 C11 1.439(13) . ? C10 H10 0.9500 . ? C11 C12 1.445(14) . ? C13 C14 1.478(14) . ? C14 C15 1.269(17) . ? C15 C16 1.328(15) . ? C15 H15 0.9500 . ? C16 C17 1.41(2) . ? C16 H16 0.9500 . ? C17 C18 1.32(2) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.358(17) . ? C19 H19 0.9500 . ? C20 C21 1.378(18) . ? C20 H20 0.9500 . ? C21 C22 1.416(14) . ? C21 H21 0.9500 . ? C22 C23 1.388(14) . ? C22 H22 0.9500 . ? C23 C24 1.443(11) . ? C25 C27 1.479(10) . ? C26 H26 0.9500 . ? C27 C28 1.415(10) . ? C28 C29 1.379(11) . ? C28 H28 0.9500 . ? C29 C30 1.488(11) . ? C31 C32 1.442(11) . ? C32 C33 1.395(13) . ? C33 C34 1.403(13) . ? C33 H33 0.9500 . ? C34 C35 1.388(16) . ? C34 H34 0.9500 . ? C35 C36 1.384(15) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.361(18) . ? C37 H37 0.9500 . ? C38 C39 1.428(19) . ? C38 H38 0.9500 . ? C39 C40 1.387(15) . ? C39 H39 0.9500 . ? C40 C41 1.396(15) . ? C40 H40 0.9500 . ? C41 C42 1.427(10) . ? C43 C45 1.466(10) . ? C44 H44 0.9500 . ? C45 C46 1.348(10) . ? C46 C47 1.381(10) . ? C46 H46 0.9500 . ? C47 C48 1.464(10) . ? C49 C50 1.423(11) . ? C50 C51 1.416(14) . ? C51 C52 1.363(12) . ? C51 H51 0.9500 . ? C52 C53 1.364(15) . ? C52 H52 0.9500 . ? C53 C54 1.342(15) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.278(18) . ? C55 H55 0.9500 . ? C56 C57 1.483(19) . ? C56 H56 0.9500 . ? C57 C58 1.393(15) . ? C57 H57 0.9500 . ? C58 C59 1.390(17) . ? C58 H58 0.9500 . ? C59 C60 1.499(14) . ? C61 C63 1.430(11) . ? C62 H62 0.9500 . ? C63 C64 1.386(12) . ? C64 C65 1.370(11) . ? C64 H64 0.9500 . ? C65 C66 1.441(11) . ? C67 C68 1.479(12) . ? C68 C69 1.324(13) . ? C69 C70 1.387(13) . ? C69 H69 0.9500 . ? C70 C71 1.361(15) . ? C70 H70 0.9500 . ? C71 C72 1.358(16) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.49(2) . ? C73 H73 0.9500 . ? C74 C75 1.32(2) . ? C74 H74 0.9500 . ? C75 C76 1.442(18) . ? C75 H75 0.9500 . ? C76 C77 1.421(18) . ? C76 H76 0.9500 . ? C77 C78 1.428(15) . ? C79 C81 1.497(15) . ? C80 H80 0.9500 . ? C81 C82 1.391(15) . ? C82 C83 1.348(12) . ? C82 H82 0.9500 . ? C83 C84 1.503(14) . ? C85 C86 1.394(14) . ? C86 C87 1.364(17) . ? C87 C88 1.420(18) . ? C87 H87 0.9500 . ? C88 C89 1.36(2) . ? C88 H88 0.9500 . ? C89 C90 1.42(2) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C92 1.339(15) . ? C91 H91 0.9500 . ? C92 C93 1.459(16) . ? C92 H92 0.9500 . ? C93 C94 1.335(14) . ? C93 H93 0.9500 . ? C94 C95 1.383(15) . ? C94 H94 0.9500 . ? C95 C96 1.510(11) . ? C97 C99 1.433(11) . ? C98 H98 0.9500 . ? C99 C100 1.347(11) . ? C100 C101 1.384(11) . ? C100 H100 0.9500 . ? C101 C102 1.412(12) . ? C103 C104 1.428(11) . ? C104 C105 1.422(13) . ? C105 C106 1.425(14) . ? C105 H105 0.9500 . ? C106 C107 1.335(14) . ? C106 H106 0.9500 . ? C107 C108 1.400(15) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C110 1.415(19) . ? C109 H109 0.9500 . ? C110 C111 1.39(2) . ? C110 H110 0.9500 . ? C111 C112 1.373(15) . ? C111 H111 0.9500 . ? C112 C113 1.435(16) . ? C112 H112 0.9500 . ? C113 C114 1.478(13) . ? C115 C117 1.484(11) . ? C116 H116 0.9500 . ? C117 C118 1.359(10) . ? C118 C119 1.361(11) . ? C118 H118 0.9500 . ? C119 C120 1.491(12) . ? C121 C122 1.503(11) . ? C122 C123 1.377(13) . ? C123 C124 1.445(15) . ? C123 H123 0.9500 . ? C124 C125 1.316(15) . ? C124 H124 0.9500 . ? C125 C126 1.309(14) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C127 C128 1.21(3) . ? C127 H127 0.9500 . ? C128 C129 1.375(17) . ? C128 H128 0.9500 . ? C129 C130 1.415(16) . ? C129 H129 0.9500 . ? C130 C131 1.38(2) . ? C130 H130 0.9500 . ? C131 C132 1.403(18) . ? C133 C135 1.536(14) . ? C134 H134 0.9500 . ? C135 C136 1.333(13) . ? C136 C137 1.346(13) . ? C136 H136 0.9500 . ? C137 C138 1.423(14) . ? C139 C140 1.492(14) . ? C140 C141 1.359(15) . ? C141 C142 1.393(18) . ? C141 H141 0.9500 . ? C142 C143 1.288(19) . ? C142 H142 0.9500 . ? C143 C144 1.40(2) . ? C143 H143 0.9500 . ? C144 H144 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 O37 N82 O36 132(2) . . ? O37 N82 O35 119(2) . . ? O36 N82 O35 109.1(16) . . ? O40 N83 O39 125.1(17) . . ? O40 N83 O38 121.2(15) . . ? O39 N83 O38 111.3(13) . . ? N1 Ni1 N41 177.6(4) . . ? N1 Ni1 O1 81.4(3) . . ? N41 Ni1 O1 99.3(3) . . ? N1 Ni1 O17 90.1(4) . . ? N41 Ni1 O17 89.4(4) . . ? O1 Ni1 O17 170.7(4) . . ? N1 Ni1 O18 89.0(4) . . ? N41 Ni1 O18 93.3(4) . . ? O1 Ni1 O18 90.1(3) . . ? O17 Ni1 O18 86.3(4) . . ? N1 Ni1 O9 98.1(3) . . ? N41 Ni1 O9 79.5(4) . . ? O1 Ni1 O9 91.4(2) . . ? O17 Ni1 O9 93.3(3) . . ? O18 Ni1 O9 172.8(3) . . ? N3 Ni2 N51 174.6(3) . . ? N3 Ni2 O19 90.4(3) . . ? N51 Ni2 O19 91.5(3) . . ? N3 Ni2 O11 96.8(2) . . ? N51 Ni2 O11 81.5(3) . . ? O19 Ni2 O11 172.8(3) . . ? N3 Ni2 O1 76.1(3) . . ? N51 Ni2 O1 108.9(3) . . ? O19 Ni2 O1 89.1(2) . . ? O11 Ni2 O1 91.6(2) . . ? N3 Ni2 N5 76.0(3) . . ? N51 Ni2 N5 98.9(3) . . ? O19 Ni2 N5 91.4(3) . . ? O11 Ni2 N5 91.4(2) . . ? O1 Ni2 N5 152.1(3) . . ? N8 Ni3 N61 171.3(3) . . ? N8 Ni3 O13 96.3(3) . . ? N61 Ni3 O13 80.4(3) . . ? N8 Ni3 O20 92.8(3) . . ? N61 Ni3 O20 90.7(3) . . ? O13 Ni3 O20 170.8(3) . . ? N8 Ni3 O2 76.5(3) . . ? N61 Ni3 O2 111.4(3) . . ? O13 Ni3 O2 90.9(2) . . ? O20 Ni3 O2 90.3(3) . . ? N8 Ni3 N6 75.9(3) . . ? N61 Ni3 N6 96.2(3) . . ? O13 Ni3 N6 92.8(2) . . ? O20 Ni3 N6 90.4(3) . . ? O2 Ni3 N6 152.4(4) . . ? N71 Ni4 O22 93.2(5) . . ? N71 Ni4 O21 94.5(6) . . ? O22 Ni4 O21 88.8(4) . . ? N71 Ni4 O2 95.4(4) . . ? O22 Ni4 O2 171.2(4) . . ? O21 Ni4 O2 88.7(3) . . ? N71 Ni4 N10 173.7(4) . . ? O22 Ni4 N10 92.2(4) . . ? O21 Ni4 N10 88.7(5) . . ? O2 Ni4 N10 79.3(4) . . ? N71 Ni4 O15 79.6(5) . . ? O22 Ni4 O15 91.6(3) . . ? O21 Ni4 O15 174.1(4) . . ? O2 Ni4 O15 91.8(3) . . ? N10 Ni4 O15 97.2(3) . . ? N43 Ni5 N11 173.1(4) . . ? N43 Ni5 O23 92.1(3) . . ? N11 Ni5 O23 91.8(3) . . ? N43 Ni5 O3 96.0(3) . . ? N11 Ni5 O3 80.2(3) . . ? O23 Ni5 O3 171.9(3) . . ? N43 Ni5 O9 75.1(4) . . ? N11 Ni5 O9 110.7(3) . . ? O23 Ni5 O9 89.1(2) . . ? O3 Ni5 O9 92.7(2) . . ? N43 Ni5 N45 77.3(3) . . ? N11 Ni5 N45 96.8(3) . . ? O23 Ni5 N45 91.3(3) . . ? O3 Ni5 N45 90.7(2) . . ? O9 Ni5 N45 152.5(3) . . ? N53 Ni6 N13 171.3(3) . . ? N53 Ni6 O11 74.9(3) . . ? N13 Ni6 O11 111.2(2) . . ? N53 Ni6 O3 111.1(2) . . ? N13 Ni6 O3 75.1(2) . . ? O11 Ni6 O3 95.82(19) . . ? N53 Ni6 N55 77.6(3) . . ? N13 Ni6 N55 96.3(2) . . ? O11 Ni6 N55 152.5(2) . . ? O3 Ni6 N55 91.9(2) . . ? N53 Ni6 N15 97.5(2) . . ? N13 Ni6 N15 76.5(2) . . ? O11 Ni6 N15 92.4(2) . . ? O3 Ni6 N15 151.4(2) . . ? N55 Ni6 N15 93.3(2) . . ? N18 Ni7 N63 169.8(2) . . ? N18 Ni7 N16 76.4(2) . . ? N63 Ni7 N16 97.0(2) . . ? N18 Ni7 O4 76.0(2) . . ? N63 Ni7 O4 110.5(2) . . ? N16 Ni7 O4 152.4(2) . . ? N18 Ni7 O13 110.1(3) . . ? N63 Ni7 O13 77.4(3) . . ? N16 Ni7 O13 90.6(2) . . ? O4 Ni7 O13 97.7(2) . . ? N18 Ni7 N65 97.0(2) . . ? N63 Ni7 N65 75.4(2) . . ? N16 Ni7 N65 92.7(2) . . ? O4 Ni7 N65 91.8(2) . . ? O13 Ni7 N65 152.7(2) . . ? N73 Ni8 N20 170.8(3) . . ? N73 Ni8 O24 92.3(3) . . ? N20 Ni8 O24 92.6(3) . . ? N73 Ni8 O4 95.3(3) . . ? N20 Ni8 O4 80.4(3) . . ? O24 Ni8 O4 171.6(3) . . ? N73 Ni8 O15 76.6(4) . . ? N20 Ni8 O15 111.4(3) . . ? O24 Ni8 O15 87.6(3) . . ? O4 Ni8 O15 90.7(2) . . ? N73 Ni8 N75 76.2(4) . . ? N20 Ni8 N75 95.5(3) . . ? O24 Ni8 N75 96.0(3) . . ? O4 Ni8 N75 89.3(2) . . ? O15 Ni8 N75 152.7(3) . . ? N48 Ni9 N21 173.0(3) . . ? N48 Ni9 O5 95.6(3) . . ? N21 Ni9 O5 79.7(3) . . ? N48 Ni9 O25 90.9(3) . . ? N21 Ni9 O25 93.7(3) . . ? O5 Ni9 O25 173.5(3) . . ? N48 Ni9 N46 77.7(3) . . ? N21 Ni9 N46 97.1(3) . . ? O5 Ni9 N46 90.6(2) . . ? O25 Ni9 N46 90.5(3) . . ? N48 Ni9 O10 76.6(3) . . ? N21 Ni9 O10 108.5(3) . . ? O5 Ni9 O10 90.7(2) . . ? O25 Ni9 O10 91.1(3) . . ? N46 Ni9 O10 154.2(3) . . ? N23 Ni10 N58 170.6(2) . . ? N23 Ni10 O12 112.1(2) . . ? N58 Ni10 O12 75.0(2) . . ? N23 Ni10 O5 74.6(2) . . ? N58 Ni10 O5 111.4(2) . . ? O12 Ni10 O5 96.80(19) . . ? N23 Ni10 N25 76.9(2) . . ? N58 Ni10 N25 97.1(2) . . ? O12 Ni10 N25 92.2(2) . . ? O5 Ni10 N25 151.4(2) . . ? N23 Ni10 N56 96.8(2) . . ? N58 Ni10 N56 76.2(2) . . ? O12 Ni10 N56 151.1(2) . . ? O5 Ni10 N56 92.10(19) . . ? N25 Ni10 N56 93.0(2) . . ? N28 Ni11 N68 168.6(2) . . ? N28 Ni11 O6 75.6(2) . . ? N68 Ni11 O6 111.8(2) . . ? N28 Ni11 O14 113.3(2) . . ? N68 Ni11 O14 75.1(2) . . ? O6 Ni11 O14 97.95(19) . . ? N28 Ni11 N26 76.1(2) . . ? N68 Ni11 N26 96.4(2) . . ? O6 Ni11 N26 151.7(2) . . ? O14 Ni11 N26 91.82(19) . . ? N28 Ni11 N66 95.4(2) . . ? N68 Ni11 N66 76.2(3) . . ? O6 Ni11 N66 90.7(2) . . ? O14 Ni11 N66 151.2(2) . . ? N26 Ni11 N66 93.4(2) . . ? N78 Ni12 N30 171.0(3) . . ? N78 Ni12 O26 90.6(3) . . ? N30 Ni12 O26 93.4(3) . . ? N78 Ni12 O6 95.1(2) . . ? N30 Ni12 O6 80.9(3) . . ? O26 Ni12 O6 174.3(3) . . ? N78 Ni12 O16 76.9(3) . . ? N30 Ni12 O16 111.1(3) . . ? O26 Ni12 O16 90.0(2) . . ? O6 Ni12 O16 91.4(2) . . ? N78 Ni12 N76 74.4(3) . . ? N30 Ni12 N76 97.6(3) . . ? O26 Ni12 N76 88.9(3) . . ? O6 Ni12 N76 92.5(2) . . ? O16 Ni12 N76 151.3(3) . . ? N50 Ni13 N31 176.7(3) . . ? N50 Ni13 O27 90.4(4) . . ? N31 Ni13 O27 92.1(4) . . ? N50 Ni13 O7 96.0(3) . . ? N31 Ni13 O7 81.6(3) . . ? O27 Ni13 O7 173.6(4) . . ? N50 Ni13 O10 81.6(4) . . ? N31 Ni13 O10 96.3(3) . . ? O27 Ni13 O10 89.0(3) . . ? O7 Ni13 O10 92.5(2) . . ? N50 Ni13 O28 93.2(4) . . ? N31 Ni13 O28 89.0(4) . . ? O27 Ni13 O28 88.0(4) . . ? O7 Ni13 O28 91.0(3) . . ? O10 Ni13 O28 174.0(4) . . ? N33 Ni14 N60 173.2(3) . . ? N33 Ni14 O29 91.2(3) . . ? N60 Ni14 O29 92.8(3) . . ? N33 Ni14 O12 95.0(2) . . ? N60 Ni14 O12 81.0(3) . . ? O29 Ni14 O12 173.8(2) . . ? N33 Ni14 O7 77.9(3) . . ? N60 Ni14 O7 107.5(3) . . ? O29 Ni14 O7 90.3(2) . . ? O12 Ni14 O7 91.2(2) . . ? N33 Ni14 N35 76.3(3) . . ? N60 Ni14 N35 98.2(3) . . ? O29 Ni14 N35 89.8(2) . . ? O12 Ni14 N35 91.5(2) . . ? O7 Ni14 N35 154.3(3) . . ? N38 Ni15 N70 170.6(3) . . ? N38 Ni15 O14 93.7(2) . . ? N70 Ni15 O14 80.7(2) . . ? N38 Ni15 O8 77.3(3) . . ? N70 Ni15 O8 110.1(3) . . ? O14 Ni15 O8 91.2(2) . . ? N38 Ni15 O30 88.3(3) . . ? N70 Ni15 O30 97.0(3) . . ? O14 Ni15 O30 177.1(2) . . ? O8 Ni15 O30 91.4(2) . . ? N38 Ni15 N36 77.3(3) . . ? N70 Ni15 N36 95.2(3) . . ? O14 Ni15 N36 90.9(2) . . ? O8 Ni15 N36 154.6(3) . . ? O30 Ni15 N36 87.5(2) . . ? N80 Ni16 N40 174.0(3) . . ? N80 Ni16 O8 95.5(3) . . ? N40 Ni16 O8 80.5(3) . . ? N80 Ni16 O16 79.2(4) . . ? N40 Ni16 O16 96.4(3) . . ? O8 Ni16 O16 92.4(2) . . ? N80 Ni16 O31 94.1(4) . . ? N40 Ni16 O31 90.5(3) . . ? O8 Ni16 O31 91.5(3) . . ? O16 Ni16 O31 172.5(3) . . ? N80 Ni16 O32 88.6(3) . . ? N40 Ni16 O32 95.4(3) . . ? O8 Ni16 O32 175.9(3) . . ? O16 Ni16 O32 88.0(3) . . ? O31 Ni16 O32 88.5(3) . . ? C6 O1 Ni1 111.3(5) . . ? C6 O1 Ni2 108.6(6) . . ? Ni1 O1 Ni2 140.0(4) . . ? C13 O2 Ni4 112.5(6) . . ? C13 O2 Ni3 107.2(6) . . ? Ni4 O2 Ni3 140.1(5) . . ? C24 O3 Ni5 113.4(5) . . ? C24 O3 Ni6 108.4(5) . . ? Ni5 O3 Ni6 137.4(3) . . ? C31 O4 Ni8 111.4(4) . . ? C31 O4 Ni7 109.2(4) . . ? Ni8 O4 Ni7 139.3(3) . . ? C42 O5 Ni9 112.6(4) . . ? C42 O5 Ni10 110.0(5) . . ? Ni9 O5 Ni10 136.7(3) . . ? C49 O6 Ni12 112.4(4) . . ? C49 O6 Ni11 109.2(4) . . ? Ni12 O6 Ni11 137.8(3) . . ? C60 O7 Ni13 110.5(6) . . ? C60 O7 Ni14 106.7(6) . . ? Ni13 O7 Ni14 142.2(4) . . ? C67 O8 Ni16 109.5(5) . . ? C67 O8 Ni15 108.6(5) . . ? Ni16 O8 Ni15 140.9(4) . . ? C78 O9 Ni1 114.7(7) . . ? C78 O9 Ni5 107.3(7) . . ? Ni1 O9 Ni5 137.8(4) . . ? C85 O10 Ni13 109.7(6) . . ? C85 O10 Ni9 109.6(6) . . ? Ni13 O10 Ni9 140.5(4) . . ? C96 O11 Ni2 114.0(4) . . ? C96 O11 Ni6 108.0(4) . . ? Ni2 O11 Ni6 137.8(3) . . ? C103 O12 Ni14 110.6(4) . . ? C103 O12 Ni10 110.9(4) . . ? Ni14 O12 Ni10 138.0(3) . . ? C114 O13 Ni3 114.1(5) . . ? C114 O13 Ni7 106.2(5) . . ? Ni3 O13 Ni7 139.1(3) . . ? C121 O14 Ni15 113.0(5) . . ? C121 O14 Ni11 108.7(5) . . ? Ni15 O14 Ni11 137.6(3) . . ? C132 O15 Ni4 109.7(7) . . ? C132 O15 Ni8 110.6(8) . . ? Ni4 O15 Ni8 139.6(4) . . ? C139 O16 Ni16 112.1(7) . . ? C139 O16 Ni12 107.5(7) . . ? Ni16 O16 Ni12 139.9(3) . . ? N81 O30 Ni15 123.0(6) . . ? C5 N1 C1 120.2(10) . . ? C5 N1 Ni1 113.9(7) . . ? C1 N1 Ni1 124.9(10) . . ? C6 N2 N3 110.8(8) . . ? C7 N3 N2 118.0(8) . . ? C7 N3 Ni2 122.0(7) . . ? N2 N3 Ni2 119.9(6) . . ? C7 N4 H4A 120.0 . . ? C7 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C9 N5 C8 122.5(8) . . ? C9 N5 Ni2 111.3(6) . . ? C8 N5 Ni2 126.0(7) . . ? C11 N6 C8 122.0(8) . . ? C11 N6 Ni3 110.6(6) . . ? C8 N6 Ni3 127.1(7) . . ? C12 N7 H7A 120.0 . . ? C12 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? C12 N8 N9 114.7(9) . . ? C12 N8 Ni3 123.4(7) . . ? N9 N8 Ni3 121.8(6) . . ? C13 N9 N8 105.3(8) . . ? C14 N10 C18 119.3(12) . . ? C14 N10 Ni4 115.0(8) . . ? C18 N10 Ni4 125.4(10) . . ? C19 N11 C23 120.5(9) . . ? C19 N11 Ni5 126.3(8) . . ? C23 N11 Ni5 112.1(6) . . ? C24 N12 N13 110.3(6) . . ? C25 N13 N12 119.3(6) . . ? C25 N13 Ni6 121.1(5) . . ? N12 N13 Ni6 118.8(5) . . ? C25 N14 H14A 120.0 . . ? C25 N14 H14B 120.0 . . ? H14A N14 H14B 120.0 . . ? C27 N15 C26 118.4(6) . . ? C27 N15 Ni6 111.7(4) . . ? C26 N15 Ni6 129.6(5) . . ? C26 N16 C29 116.6(6) . . ? C26 N16 Ni7 130.9(5) . . ? C29 N16 Ni7 112.5(5) . . ? C30 N17 H17A 120.0 . . ? C30 N17 H17B 120.0 . . ? H17A N17 H17B 120.0 . . ? C30 N18 N19 111.1(7) . . ? C30 N18 Ni7 125.7(5) . . ? N19 N18 Ni7 122.3(5) . . ? C31 N19 N18 106.8(7) . . ? C32 N20 C36 119.4(10) . . ? C32 N20 Ni8 114.1(7) . . ? C36 N20 Ni8 125.9(7) . . ? C41 N21 C37 120.4(8) . . ? C41 N21 Ni9 113.5(5) . . ? C37 N21 Ni9 125.7(8) . . ? C42 N22 N23 109.0(6) . . ? C43 N23 N22 116.8(6) . . ? C43 N23 Ni10 120.8(5) . . ? N22 N23 Ni10 121.2(5) . . ? C43 N24 H24A 120.0 . . ? C43 N24 H24B 120.0 . . ? H24A N24 H24B 120.0 . . ? C44 N25 C45 117.1(7) . . ? C44 N25 Ni10 130.8(5) . . ? C45 N25 Ni10 111.5(5) . . ? C44 N26 C47 116.3(6) . . ? C44 N26 Ni11 132.1(5) . . ? C47 N26 Ni11 111.2(4) . . ? C48 N27 H27A 120.0 . . ? C48 N27 H27B 120.0 . . ? H27A N27 H27B 120.0 . . ? C48 N28 N29 113.8(6) . . ? C48 N28 Ni11 124.7(5) . . ? N29 N28 Ni11 120.4(5) . . ? C49 N29 N28 109.6(6) . . ? C50 N30 C54 119.2(8) . . ? C50 N30 Ni12 110.9(6) . . ? C54 N30 Ni12 129.1(7) . . ? C59 N31 C55 118.9(10) . . ? C59 N31 Ni13 113.0(7) . . ? C55 N31 Ni13 127.6(9) . . ? N33 N32 C60 109.0(8) . . ? C61 N33 N32 119.8(7) . . ? C61 N33 Ni14 121.3(5) . . ? N32 N33 Ni14 118.9(6) . . ? C61 N34 H34A 120.0 . . ? C61 N34 H34B 120.0 . . ? H34A N34 H34B 120.0 . . ? C62 N35 C63 120.2(7) . . ? C62 N35 Ni14 129.6(6) . . ? C63 N35 Ni14 109.8(5) . . ? C62 N36 C65 116.8(7) . . ? C62 N36 Ni15 132.4(6) . . ? C65 N36 Ni15 110.5(5) . . ? C66 N37 H37A 120.0 . . ? C66 N37 H37B 120.0 . . ? H37A N37 H37B 120.0 . . ? C66 N38 N39 119.1(7) . . ? C66 N38 Ni15 122.5(6) . . ? N39 N38 Ni15 118.4(5) . . ? C67 N39 N38 110.0(8) . . ? C68 N40 C72 119.9(9) . . ? C68 N40 Ni16 114.3(6) . . ? C72 N40 Ni16 125.8(7) . . ? C73 N41 C77 122.7(11) . . ? C73 N41 Ni1 124.9(10) . . ? C77 N41 Ni1 111.8(7) . . ? C78 N42 N43 109.0(9) . . ? C79 N43 N42 113.4(10) . . ? C79 N43 Ni5 123.0(7) . . ? N42 N43 Ni5 122.8(8) . . ? C79 N44 H44A 120.0 . . ? C79 N44 H44B 120.0 . . ? H44A N44 H44B 120.0 . . ? C80 N45 C81 115.5(9) . . ? C80 N45 Ni5 133.6(7) . . ? C81 N45 Ni5 110.9(7) . . ? C80 N46 C83 116.1(8) . . ? C80 N46 Ni9 133.1(6) . . ? C83 N46 Ni9 110.8(6) . . ? C84 N47 H47A 120.0 . . ? C84 N47 H47B 120.0 . . ? H47A N47 H47B 120.0 . . ? C84 N48 N49 115.6(8) . . ? C84 N48 Ni9 122.0(7) . . ? N49 N48 Ni9 122.2(6) . . ? N48 N49 C85 109.3(8) . . ? C86 N50 C90 115.8(12) . . ? C86 N50 Ni13 112.6(6) . . ? C90 N50 Ni13 130.9(11) . . ? C91 N51 C95 114.7(9) . . ? C91 N51 Ni2 131.9(8) . . ? C95 N51 Ni2 113.4(6) . . ? C96 N52 N53 107.5(6) . . ? C97 N53 N52 119.6(6) . . ? C97 N53 Ni6 118.5(5) . . ? N52 N53 Ni6 121.6(6) . . ? C97 N54 H54A 120.0 . . ? C97 N54 H54B 120.0 . . ? H54A N54 H54B 120.0 . . ? C98 N55 C99 118.5(7) . . ? C98 N55 Ni6 129.9(5) . . ? C99 N55 Ni6 111.3(5) . . ? C101 N56 C98 119.2(7) . . ? C101 N56 Ni10 111.4(5) . . ? C98 N56 Ni10 129.0(5) . . ? C102 N57 H57A 120.0 . . ? C102 N57 H57B 120.0 . . ? H57A N57 H57B 120.0 . . ? C102 N58 N59 118.6(6) . . ? C102 N58 Ni10 119.4(5) . . ? N59 N58 Ni10 120.2(5) . . ? C103 N59 N58 110.1(6) . . ? C108 N60 C104 119.8(8) . . ? C108 N60 Ni14 127.9(7) . . ? C104 N60 Ni14 112.1(5) . . ? C113 N61 C109 120.2(10) . . ? C113 N61 Ni3 113.1(7) . . ? C109 N61 Ni3 125.9(9) . . ? C114 N62 N63 109.4(8) . . ? C115 N63 N62 116.2(7) . . ? C115 N63 Ni7 124.1(5) . . ? N62 N63 Ni7 117.1(6) . . ? C115 N64 H64A 120.0 . . ? C115 N64 H64B 120.0 . . ? H64A N64 H64B 120.0 . . ? C116 N65 C117 117.9(7) . . ? C116 N65 Ni7 130.7(5) . . ? C117 N65 Ni7 111.1(5) . . ? C116 N66 C119 117.1(7) . . ? C116 N66 Ni11 130.3(5) . . ? C119 N66 Ni11 112.5(5) . . ? C120 N67 H67A 120.0 . . ? C120 N67 H67B 120.0 . . ? H67A N67 H67B 120.0 . . ? C120 N68 N69 118.2(6) . . ? C120 N68 Ni11 122.5(6) . . ? N69 N68 Ni11 118.6(5) . . ? C121 N69 N68 109.6(6) . . ? C122 N70 C126 115.2(7) . . ? C122 N70 Ni15 113.9(5) . . ? C126 N70 Ni15 129.4(6) . . ? C127 N71 C131 119.3(19) . . ? C127 N71 Ni4 126.9(18) . . ? C131 N71 Ni4 113.8(11) . . ? C132 N72 N73 110.4(10) . . ? C133 N73 N72 116.2(10) . . ? C133 N73 Ni8 124.6(8) . . ? N72 N73 Ni8 119.3(8) . . ? C133 N74 H74A 120.0 . . ? C133 N74 H74B 120.0 . . ? H74A N74 H74B 120.0 . . ? C134 N75 C135 115.5(9) . . ? C134 N75 Ni8 132.5(8) . . ? C135 N75 Ni8 111.9(6) . . ? C134 N76 C137 118.1(8) . . ? C134 N76 Ni12 130.4(7) . . ? C137 N76 Ni12 111.3(6) . . ? C138 N77 H77A 120.0 . . ? C138 N77 H77B 120.0 . . ? H77A N77 H77B 120.0 . . ? C138 N78 N79 117.2(9) . . ? C138 N78 Ni12 124.3(8) . . ? N79 N78 Ni12 118.2(7) . . ? C139 N79 N78 110.5(9) . . ? C140 N80 C144 116.7(10) . . ? C140 N80 Ni16 116.6(7) . . ? C144 N80 Ni16 126.6(9) . . ? O33 N81 O34 120.3(7) . . ? O33 N81 O30 119.7(9) . . ? O34 N81 O30 119.9(8) . . ? O42 N84 O43 122.0(19) . . ? O42 N84 O41 128.7(17) . . ? O43 N84 O41 109.3(17) . . ? N1 C1 C2 115.7(13) . . ? N1 C1 H1 122.2 . . ? C2 C1 H1 122.2 . . ? C3 C2 C1 122.8(13) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 120.2(14) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 116.9(13) . . ? C5 C4 H4 121.6 . . ? C3 C4 H4 121.6 . . ? N1 C5 C4 124.0(10) . . ? N1 C5 C6 115.2(10) . . ? C4 C5 C6 120.8(11) . . ? N2 C6 O1 124.4(8) . . ? N2 C6 C5 117.8(10) . . ? O1 C6 C5 117.7(10) . . ? N3 C7 N4 126.8(9) . . ? N3 C7 C9 113.7(9) . . ? N4 C7 C9 119.4(9) . . ? N6 C8 N5 119.5(9) . . ? N6 C8 H8 120.3 . . ? N5 C8 H8 120.3 . . ? N5 C9 C10 119.0(9) . . ? N5 C9 C7 117.0(8) . . ? C10 C9 C7 123.7(10) . . ? C9 C10 C11 120.2(9) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? N6 C11 C10 116.7(9) . . ? N6 C11 C12 118.4(9) . . ? C10 C11 C12 124.9(10) . . ? N8 C12 N7 129.1(10) . . ? N8 C12 C11 111.6(10) . . ? N7 C12 C11 119.3(10) . . ? O2 C13 N9 129.2(8) . . ? O2 C13 C14 121.4(11) . . ? N9 C13 C14 109.4(13) . . ? C15 C14 N10 116.8(10) . . ? C15 C14 C13 131.5(13) . . ? N10 C14 C13 111.6(13) . . ? C14 C15 C16 128.7(15) . . ? C14 C15 H15 115.6 . . ? C16 C15 H15 115.6 . . ? C15 C16 C17 116.1(14) . . ? C15 C16 H16 122.0 . . ? C17 C16 H16 122.0 . . ? C18 C17 C16 117.2(10) . . ? C18 C17 H17 121.4 . . ? C16 C17 H17 121.4 . . ? C17 C18 N10 121.7(14) . . ? C17 C18 H18 119.1 . . ? N10 C18 H18 119.1 . . ? N11 C19 C20 122.8(12) . . ? N11 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C19 C20 C21 119.8(11) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 117.5(11) . . ? C20 C21 H21 121.2 . . ? C22 C21 H21 121.2 . . ? C23 C22 C21 119.0(11) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? N11 C23 C22 120.1(8) . . ? N11 C23 C24 117.1(9) . . ? C22 C23 C24 122.8(10) . . ? N12 C24 O3 127.1(7) . . ? N12 C24 C23 116.6(8) . . ? O3 C24 C23 116.1(8) . . ? N13 C25 N14 124.2(7) . . ? N13 C25 C27 113.3(7) . . ? N14 C25 C27 122.3(7) . . ? N16 C26 N15 126.1(7) . . ? N16 C26 H26 116.9 . . ? N15 C26 H26 116.9 . . ? N15 C27 C28 120.6(7) . . ? N15 C27 C25 116.7(6) . . ? C28 C27 C25 122.7(7) . . ? C29 C28 C27 115.8(7) . . ? C29 C28 H28 122.1 . . ? C27 C28 H28 122.1 . . ? N16 C29 C28 122.4(7) . . ? N16 C29 C30 117.0(7) . . ? C28 C29 C30 120.6(8) . . ? N17 C30 N18 128.4(7) . . ? N17 C30 C29 123.8(8) . . ? N18 C30 C29 107.8(8) . . ? O4 C31 N19 125.5(6) . . ? O4 C31 C32 118.0(7) . . ? N19 C31 C32 116.5(9) . . ? N20 C32 C33 122.9(8) . . ? N20 C32 C31 115.9(10) . . ? C33 C32 C31 121.1(9) . . ? C32 C33 C34 118.1(9) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? C35 C34 C33 118.8(10) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C36 C35 C34 117.2(9) . . ? C36 C35 H35 121.4 . . ? C34 C35 H35 121.4 . . ? N20 C36 C35 123.6(10) . . ? N20 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? C38 C37 N21 120.2(11) . . ? C38 C37 H37 119.9 . . ? N21 C37 H37 119.9 . . ? C37 C38 C39 120.7(9) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 116.3(11) . . ? C40 C39 H39 121.8 . . ? C38 C39 H39 121.8 . . ? C39 C40 C41 121.2(11) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? N21 C41 C40 121.2(7) . . ? N21 C41 C42 116.2(8) . . ? C40 C41 C42 122.5(10) . . ? O5 C42 N22 124.8(7) . . ? O5 C42 C41 117.5(8) . . ? N22 C42 C41 117.6(8) . . ? N23 C43 N24 125.0(7) . . ? N23 C43 C45 113.7(6) . . ? N24 C43 C45 121.2(7) . . ? N26 C44 N25 127.9(6) . . ? N26 C44 H44 116.0 . . ? N25 C44 H44 116.0 . . ? N25 C45 C46 120.4(7) . . ? N25 C45 C43 116.1(7) . . ? C46 C45 C43 123.4(7) . . ? C45 C46 C47 120.2(7) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C46 C47 N26 117.8(6) . . ? C46 C47 C48 126.6(6) . . ? N26 C47 C48 115.6(6) . . ? N28 C48 N27 128.4(7) . . ? N28 C48 C47 111.4(6) . . ? N27 C48 C47 120.2(6) . . ? N29 C49 O6 125.0(6) . . ? N29 C49 C50 119.4(8) . . ? O6 C49 C50 115.6(8) . . ? N30 C50 C51 119.2(7) . . ? N30 C50 C49 118.9(9) . . ? C51 C50 C49 121.8(9) . . ? C52 C51 C50 120.8(9) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C53 117.6(10) . . ? C51 C52 H52 121.2 . . ? C53 C52 H52 121.2 . . ? C54 C53 C52 120.7(9) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 N30 122.5(10) . . ? C53 C54 H54 118.8 . . ? N30 C54 H54 118.8 . . ? C56 C55 N31 124.1(12) . . ? C56 C55 H55 117.9 . . ? N31 C55 H55 117.9 . . ? C55 C56 C57 120.5(11) . . ? C55 C56 H56 119.8 . . ? C57 C56 H56 119.8 . . ? C58 C57 C56 114.5(12) . . ? C58 C57 H57 122.8 . . ? C56 C57 H57 122.8 . . ? C59 C58 C57 120.8(13) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? N31 C59 C58 121.1(9) . . ? N31 C59 C60 111.6(11) . . ? C58 C59 C60 127.2(11) . . ? O7 C60 N32 127.4(9) . . ? O7 C60 C59 122.8(11) . . ? N32 C60 C59 109.8(12) . . ? N33 C61 N34 123.7(7) . . ? N33 C61 C63 117.1(8) . . ? N34 C61 C63 119.3(8) . . ? N35 C62 N36 125.0(8) . . ? N35 C62 H62 117.5 . . ? N36 C62 H62 117.5 . . ? N35 C63 C64 118.5(8) . . ? N35 C63 C61 115.3(8) . . ? C64 C63 C61 126.2(8) . . ? C65 C64 C63 120.1(8) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 N36 119.3(7) . . ? C64 C65 C66 126.1(8) . . ? N36 C65 C66 114.6(7) . . ? N38 C66 N37 122.5(8) . . ? N38 C66 C65 115.1(8) . . ? N37 C66 C65 122.4(8) . . ? O8 C67 N39 125.5(8) . . ? O8 C67 C68 120.3(8) . . ? N39 C67 C68 114.0(9) . . ? N40 C68 C69 122.5(8) . . ? N40 C68 C67 114.4(9) . . ? C69 C68 C67 123.1(8) . . ? C68 C69 C70 119.9(10) . . ? C68 C69 H69 120.0 . . ? C70 C69 H69 120.0 . . ? C71 C70 C69 117.7(10) . . ? C71 C70 H70 121.1 . . ? C69 C70 H70 121.1 . . ? C72 C71 C70 119.6(9) . . ? C72 C71 H71 120.2 . . ? C70 C71 H71 120.2 . . ? N40 C72 C71 120.3(10) . . ? N40 C72 H72 119.9 . . ? C71 C72 H72 119.9 . . ? N41 C73 C74 116.1(13) . . ? N41 C73 H73 121.9 . . ? C74 C73 H73 121.9 . . ? C75 C74 C73 124.1(13) . . ? C75 C74 H74 117.9 . . ? C73 C74 H74 117.9 . . ? C74 C75 C76 117.4(15) . . ? C74 C75 H75 121.3 . . ? C76 C75 H75 121.3 . . ? C77 C76 C75 116.2(13) . . ? C77 C76 H76 121.9 . . ? C75 C76 H76 121.9 . . ? N41 C77 C76 123.4(10) . . ? N41 C77 C78 121.7(11) . . ? C76 C77 C78 114.9(13) . . ? N42 C78 O9 125.6(10) . . ? N42 C78 C77 122.7(11) . . ? O9 C78 C77 111.6(12) . . ? N43 C79 N44 125.3(12) . . ? N43 C79 C81 114.8(9) . . ? N44 C79 C81 119.7(11) . . ? N46 C80 N45 128.1(9) . . ? N46 C80 H80 116.0 . . ? N45 C80 H80 116.0 . . ? N45 C81 C82 119.9(9) . . ? N45 C81 C79 113.4(10) . . ? C82 C81 C79 126.7(10) . . ? C83 C82 C81 118.4(9) . . ? C83 C82 H82 120.8 . . ? C81 C82 H82 120.8 . . ? N46 C83 C82 121.6(9) . . ? N46 C83 C84 115.6(8) . . ? C82 C83 C84 122.3(10) . . ? N48 C84 N47 126.8(10) . . ? N48 C84 C83 113.6(8) . . ? N47 C84 C83 119.5(10) . . ? O10 C85 C86 119.5(11) . . ? O10 C85 N49 122.0(10) . . ? C86 C85 N49 118.4(11) . . ? N50 C86 C87 120.6(11) . . ? N50 C86 C85 115.7(10) . . ? C87 C86 C85 123.6(12) . . ? C86 C87 C88 124.8(14) . . ? C86 C87 H87 117.6 . . ? C88 C87 H87 117.6 . . ? C89 C88 C87 114.4(14) . . ? C89 C88 H88 122.8 . . ? C87 C88 H88 122.8 . . ? C88 C89 C90 118.6(14) . . ? C88 C89 H89 120.7 . . ? C90 C89 H89 120.7 . . ? N50 C90 C89 125.7(15) . . ? N50 C90 H90 117.2 . . ? C89 C90 H90 117.2 . . ? N51 C91 C92 128.5(10) . . ? N51 C91 H91 115.7 . . ? C92 C91 H91 115.7 . . ? C91 C92 C93 117.0(9) . . ? C91 C92 H92 121.5 . . ? C93 C92 H92 121.5 . . ? C94 C93 C92 116.3(11) . . ? C94 C93 H93 121.8 . . ? C92 C93 H93 121.8 . . ? C93 C94 C95 118.9(11) . . ? C93 C94 H94 120.5 . . ? C95 C94 H94 120.5 . . ? N51 C95 C94 124.5(8) . . ? N51 C95 C96 115.0(9) . . ? C94 C95 C96 120.5(9) . . ? O11 C96 N52 127.9(7) . . ? O11 C96 C95 115.9(7) . . ? N52 C96 C95 116.1(8) . . ? N53 C97 N54 120.9(7) . . ? N53 C97 C99 116.3(7) . . ? N54 C97 C99 122.7(8) . . ? N55 C98 N56 124.5(7) . . ? N55 C98 H98 117.8 . . ? N56 C98 H98 117.8 . . ? N55 C99 C100 120.0(7) . . ? N55 C99 C97 115.8(7) . . ? C100 C99 C97 124.1(8) . . ? C99 C100 C101 120.1(8) . . ? C99 C100 H100 120.0 . . ? C101 C100 H100 120.0 . . ? N56 C101 C100 117.7(8) . . ? N56 C101 C102 116.2(7) . . ? C100 C101 C102 126.0(8) . . ? N58 C102 N57 122.2(7) . . ? N58 C102 C101 115.1(7) . . ? N57 C102 C101 122.5(7) . . ? O12 C103 N59 123.4(7) . . ? O12 C103 C104 117.3(7) . . ? N59 C103 C104 119.3(8) . . ? N60 C104 C105 122.7(8) . . ? N60 C104 C103 118.4(8) . . ? C105 C104 C103 118.9(8) . . ? C104 C105 C106 115.9(9) . . ? C104 C105 H105 122.0 . . ? C106 C105 H105 122.0 . . ? C107 C106 C105 119.0(10) . . ? C107 C106 H106 120.5 . . ? C105 C106 H106 120.5 . . ? C106 C107 C108 120.0(9) . . ? C106 C107 H107 120.0 . . ? C108 C107 H107 120.0 . . ? N60 C108 C107 122.5(10) . . ? N60 C108 H108 118.7 . . ? C107 C108 H108 118.7 . . ? N61 C109 C110 119.7(12) . . ? N61 C109 H109 120.2 . . ? C110 C109 H109 120.2 . . ? C111 C110 C109 120.5(11) . . ? C111 C110 H110 119.8 . . ? C109 C110 H110 119.8 . . ? C112 C111 C110 117.6(12) . . ? C112 C111 H111 121.2 . . ? C110 C111 H111 121.2 . . ? C111 C112 C113 119.4(11) . . ? C111 C112 H112 120.3 . . ? C113 C112 H112 120.3 . . ? N61 C113 C112 122.7(9) . . ? N61 C113 C114 117.3(11) . . ? C112 C113 C114 120.0(11) . . ? O13 C114 N62 129.5(9) . . ? O13 C114 C113 114.2(9) . . ? N62 C114 C113 116.3(11) . . ? N64 C115 N63 126.6(8) . . ? N64 C115 C117 123.1(8) . . ? N63 C115 C117 110.2(7) . . ? N66 C116 N65 125.8(7) . . ? N66 C116 H116 117.1 . . ? N65 C116 H116 117.1 . . ? N65 C117 C118 120.1(7) . . ? N65 C117 C115 117.6(7) . . ? C118 C117 C115 122.3(7) . . ? C117 C118 C119 117.2(7) . . ? C117 C118 H118 121.4 . . ? C119 C118 H118 121.4 . . ? N66 C119 C118 121.6(8) . . ? N66 C119 C120 115.6(7) . . ? C118 C119 C120 122.7(8) . . ? N68 C120 N67 125.8(8) . . ? N68 C120 C119 112.8(8) . . ? N67 C120 C119 121.4(8) . . ? O14 C121 N69 127.4(8) . . ? O14 C121 C122 117.7(7) . . ? N69 C121 C122 114.8(7) . . ? N70 C122 C123 125.6(8) . . ? N70 C122 C121 113.7(7) . . ? C123 C122 C121 120.6(8) . . ? C122 C123 C124 114.4(10) . . ? C122 C123 H123 122.8 . . ? C124 C123 H123 122.8 . . ? C125 C124 C123 118.9(10) . . ? C125 C124 H124 120.6 . . ? C123 C124 H124 120.6 . . ? C126 C125 C124 121.1(10) . . ? C126 C125 H125 119.4 . . ? C124 C125 H125 119.4 . . ? C125 C126 N70 124.6(9) . . ? C125 C126 H126 117.7 . . ? N70 C126 H126 117.7 . . ? C128 C127 N71 124(2) . . ? C128 C127 H127 118.0 . . ? N71 C127 H127 118.0 . . ? C127 C128 C129 127(2) . . ? C127 C128 H128 116.7 . . ? C129 C128 H128 116.7 . . ? C128 C129 C130 109.7(17) . . ? C128 C129 H129 125.1 . . ? C130 C129 H129 125.1 . . ? C131 C130 C129 118.2(17) . . ? C131 C130 H130 120.9 . . ? C129 C130 H130 120.9 . . ? N71 C131 C130 122.1(13) . . ? N71 C131 C132 118.1(17) . . ? C130 C131 C132 119.7(18) . . ? O15 C132 N72 123.1(13) . . ? O15 C132 C131 118.8(13) . . ? N72 C132 C131 118.0(15) . . ? N73 C133 N74 128.9(11) . . ? N73 C133 C135 115.8(10) . . ? N74 C133 C135 115.3(10) . . ? N76 C134 N75 124.7(9) . . ? N76 C134 H134 117.7 . . ? N75 C134 H134 117.7 . . ? C136 C135 N75 122.3(9) . . ? C136 C135 C133 126.2(9) . . ? N75 C135 C133 111.5(9) . . ? C135 C136 C137 117.4(9) . . ? C135 C136 H136 121.3 . . ? C137 C136 H136 121.3 . . ? N76 C137 C136 121.8(9) . . ? N76 C137 C138 116.3(9) . . ? C136 C137 C138 121.9(9) . . ? N78 C138 N77 122.0(12) . . ? N78 C138 C137 113.2(9) . . ? N77 C138 C137 124.7(10) . . ? O16 C139 N79 126.7(10) . . ? O16 C139 C140 117.5(11) . . ? N79 C139 C140 115.8(10) . . ? N80 C140 C141 124.0(11) . . ? N80 C140 C139 114.5(10) . . ? C141 C140 C139 121.5(11) . . ? C140 C141 C142 117.8(12) . . ? C140 C141 H141 121.1 . . ? C142 C141 H141 121.1 . . ? C143 C142 C141 120.2(13) . . ? C143 C142 H142 119.9 . . ? C141 C142 H142 119.9 . . ? C142 C143 C144 117.8(13) . . ? C142 C143 H143 121.1 . . ? C144 C143 H143 121.1 . . ? N80 C144 C143 123.4(13) . . ? N80 C144 H144 118.3 . . ? C143 C144 H144 118.3 . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 2.999 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.142