# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'L Thompson' _publ_contact_author_email LTHOMP@MUN.CA _publ_section_title ; Ligand directed self-assembly vs. the metal ion coordination algorithm - when does the ligand or the metal take control? ; loop_ _publ_author_name 'L Thompson' 'Tareque S M Abedin' 'Julie L Collins' 'Louise Dawe' 'Corey A. McClary' ; K.Shuvaev ; #=== data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 706532' # start Validation Reply Form _vrf_PLAT306_Compound3 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O7 RESPONSE: This is a lattice water molecule. Its protons could not be located in the difference map and hence were omitted from the model. They have, however, been included in the formula, for purposes of calculated molecular weight, etc. ; _vrf_PLAT761_Compound3 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Hydrogen atoms were introduced in calculated positions with thermal parameters set 20% greater than their bonding partners. They were refined on a riding model. X-H bond distances are therefore not reported. ; _vrf_PLAT762_Compound3 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: Hydrogen atoms were introduced in calculated positions with thermal parameters set 20% greater than their bonding partners. They were refined on a riding model. X-Y-H or H-Y-H angles are therefore not reported. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 Cu6 N32 O24 S4' _chemical_formula_weight 1970.65 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _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 9.8087(17) _cell_length_b 12.416(3) _cell_length_c 15.647(3) _cell_angle_alpha 110.687(5) _cell_angle_beta 90.754(4) _cell_angle_gamma 91.055(4) _cell_volume 1782.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 7340 _cell_measurement_theta_min 2.6855 _cell_measurement_theta_max 30.6378 _exptl_crystal_description Chip _exptl_crystal_colour Green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 994 _exptl_absorpt_coefficient_mu 1.975 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.7059 _exptl_absorpt_correction_T_max 0.9010 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(2) _diffrn_radiation_wavelength 0.71070 _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 17058 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7317 _reflns_number_gt 6507 _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 'ORIENT (Altomare et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Beurskens, 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^)+(0.0711P)^2^+3.1917P] 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 7317 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Cu1 Cu 0.21215(5) 0.20977(4) -0.03569(3) 0.01974(13) Uani 1 1 d . . . Cu2 Cu 0.24506(4) 0.47029(4) 0.20047(3) 0.01839(13) Uani 1 1 d . . . Cu3 Cu 0.11717(4) 0.78286(4) 0.35085(3) 0.01941(13) Uani 1 1 d . . . S1 S -0.04116(11) 0.21384(11) -0.05020(7) 0.0332(3) Uani 1 1 d . . . S2 S 0.53526(11) 0.31812(10) 0.36446(8) 0.0337(2) Uani 1 1 d . . . O1 O -0.0421(3) 0.2171(2) 0.16510(19) 0.0255(6) Uani 1 1 d . . . O2 O -0.0537(3) 0.8255(2) 0.41598(18) 0.0211(5) Uani 1 1 d . . . O3 O -0.2370(3) 0.7620(2) 0.46916(17) 0.0221(5) Uani 1 1 d . . . O4 O 0.3903(3) 0.7584(2) 0.15967(18) 0.0252(6) Uani 1 1 d . . . O5 O 0.2512(3) 0.1928(2) -0.16065(17) 0.0225(6) Uani 1 1 d . . . O6 O 0.2846(3) 0.2956(2) -0.25118(17) 0.0259(6) Uani 1 1 d . . . O7 O 0.3631(3) 0.9739(2) 0.26999(19) 0.0273(6) Uani 1 1 d . . . O8 O 0.0925(3) 0.8937(3) 0.7104(2) 0.0380(7) Uani 1 1 d . . . O9 O 0.0621(3) 0.6972(3) 0.5561(2) 0.0399(8) Uani 1 1 d . . . O10 O 0.2595(3) 0.5609(3) 0.4498(2) 0.0389(7) Uani 1 1 d . . . O11 O 0.1852(3) 0.3275(3) 0.3769(2) 0.0321(7) Uani 1 1 d . . . O12 O 0.1294(3) 0.0368(3) 0.3737(2) 0.0336(7) Uani 1 1 d . . . N1 N 0.2817(3) 0.0530(3) -0.0468(2) 0.0201(6) Uani 1 1 d . . . N2 N 0.3854(4) -0.1494(3) -0.0376(2) 0.0265(7) Uani 1 1 d . . . N3 N 0.2566(3) 0.1357(3) 0.1976(2) 0.0233(7) Uani 1 1 d . . . H4 H 0.2293 0.1952 0.2438 0.028 Uiso 1 1 calc R . . H5 H 0.2877 0.0749 0.2073 0.028 Uiso 1 1 calc R . . N4 N 0.2064(3) 0.2230(3) 0.0911(2) 0.0198(6) Uani 1 1 d . . . N5 N 0.1551(3) 0.3192(3) 0.1596(2) 0.0188(6) Uani 1 1 d . . . N6 N 0.0607(3) 0.5095(2) 0.2686(2) 0.0185(6) Uani 1 1 d . . . N7 N 0.0211(3) 0.6129(3) 0.3235(2) 0.0193(6) Uani 1 1 d . . . N8 N 0.2289(3) 0.8623(3) 0.4661(2) 0.0191(6) Uani 1 1 d . . . N9 N 0.4153(3) 0.9664(3) 0.6071(2) 0.0238(7) Uani 1 1 d . . . N10 N 0.5111(3) 0.6865(3) 0.3628(2) 0.0260(7) Uani 1 1 d . . . H11 H 0.5304 0.6319 0.3109 0.031 Uiso 1 1 calc R . . H12 H 0.5703 0.7062 0.4088 0.031 Uiso 1 1 calc R . . N11 N 0.2960(3) 0.7193(3) 0.3101(2) 0.0186(6) Uani 1 1 d . . . N12 N 0.3111(3) 0.6297(2) 0.22545(19) 0.0183(6) Uani 1 1 d . . . N13 N 0.2900(3) 0.4657(3) 0.0655(2) 0.0186(6) Uani 1 1 d . . . N14 N 0.2746(3) 0.3779(2) -0.0136(2) 0.0189(6) Uani 1 1 d . . . N15 N -0.0624(3) 0.2079(3) -0.2307(2) 0.0249(7) Uani 1 1 d . . . N16 N 0.4225(3) 0.4148(3) 0.2433(2) 0.0259(7) Uani 1 1 d . . . C1 C 0.3175(4) -0.0324(3) -0.1228(3) 0.0232(8) Uani 1 1 d . . . H1 H 0.3070 -0.0247 -0.1808 0.028 Uiso 1 1 calc R . . C2 C 0.3702(4) -0.1327(3) -0.1162(3) 0.0263(8) Uani 1 1 d . . . H2 H 0.3964 -0.1918 -0.1706 0.032 Uiso 1 1 calc R . . C3 C 0.3465(4) -0.0635(3) 0.0376(3) 0.0228(8) Uani 1 1 d . . . H3 H 0.3542 -0.0728 0.0952 0.027 Uiso 1 1 calc R . . C4 C 0.2955(4) 0.0379(3) 0.0338(2) 0.0198(7) Uani 1 1 d . . . C5 C 0.2507(4) 0.1376(3) 0.1135(2) 0.0187(7) Uani 1 1 d . . . C6 C 0.0304(4) 0.3049(3) 0.1873(2) 0.0189(7) Uani 1 1 d . . . C7 C -0.0204(4) 0.4169(3) 0.2536(2) 0.0189(7) Uani 1 1 d . . . C8 C -0.1460(4) 0.4228(3) 0.2964(3) 0.0232(8) Uani 1 1 d . . . H6 H -0.2016 0.3558 0.2862 0.028 Uiso 1 1 calc R . . C9 C -0.1860(4) 0.5291(3) 0.3538(3) 0.0228(8) Uani 1 1 d . . . H7 H -0.2696 0.5381 0.3852 0.027 Uiso 1 1 calc R . . C10 C -0.0990(4) 0.6228(3) 0.3639(2) 0.0202(7) Uani 1 1 d . . . C11 C -0.1336(4) 0.7471(3) 0.4213(2) 0.0193(7) Uani 1 1 d . . . C12 C 0.1917(4) 0.9458(3) 0.5414(2) 0.0225(8) Uani 1 1 d . . . H8 H 0.1000 0.9702 0.5472 0.027 Uiso 1 1 calc R . . C13 C 0.2857(4) 0.9981(3) 0.6120(3) 0.0259(8) Uani 1 1 d . . . H9 H 0.2566 1.0579 0.6652 0.031 Uiso 1 1 calc R . . C14 C 0.4520(4) 0.8813(3) 0.5306(2) 0.0219(7) Uani 1 1 d . . . H10 H 0.5433 0.8559 0.5253 0.026 Uiso 1 1 calc R . . C15 C 0.3600(4) 0.8299(3) 0.4597(2) 0.0183(7) Uani 1 1 d . . . C16 C 0.3930(4) 0.7390(3) 0.3717(2) 0.0176(7) Uani 1 1 d . . . C17 C 0.3475(4) 0.6628(3) 0.1574(2) 0.0199(7) Uani 1 1 d . . . C18 C 0.3325(4) 0.5685(3) 0.0650(2) 0.0196(7) Uani 1 1 d . . . C19 C 0.3590(4) 0.5897(3) -0.0150(3) 0.0240(8) Uani 1 1 d . . . H13 H 0.3881 0.6638 -0.0135 0.029 Uiso 1 1 calc R . . C20 C 0.3414(4) 0.4991(3) -0.0960(3) 0.0236(8) Uani 1 1 d . . . H14 H 0.3574 0.5084 -0.1528 0.028 Uiso 1 1 calc R . . C21 C 0.2988(4) 0.3924(3) -0.0923(2) 0.0199(7) Uani 1 1 d . . . C22 C 0.2768(4) 0.2853(3) -0.1765(2) 0.0204(7) Uani 1 1 d . . . C23 C -0.0521(4) 0.2104(4) -0.1561(3) 0.0259(8) Uani 1 1 d . . . C24 C 0.4683(4) 0.3758(3) 0.2952(3) 0.0248(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0271(3) 0.0169(2) 0.0142(2) 0.00413(17) 0.00064(17) 0.00219(18) Cu2 0.0213(2) 0.0157(2) 0.0166(2) 0.00384(17) 0.00154(17) 0.00154(18) Cu3 0.0186(2) 0.0209(2) 0.0157(2) 0.00262(18) -0.00059(17) 0.00334(18) S1 0.0238(5) 0.0565(7) 0.0228(5) 0.0185(5) -0.0008(4) 0.0010(5) S2 0.0319(6) 0.0421(6) 0.0331(6) 0.0209(5) -0.0046(4) 0.0005(5) O1 0.0275(14) 0.0201(13) 0.0257(14) 0.0042(11) 0.0027(11) -0.0022(11) O2 0.0188(13) 0.0191(12) 0.0241(13) 0.0056(10) 0.0013(10) 0.0044(10) O3 0.0188(13) 0.0251(13) 0.0202(13) 0.0051(11) 0.0040(10) 0.0040(11) O4 0.0365(16) 0.0161(12) 0.0199(13) 0.0025(10) 0.0045(11) -0.0030(11) O5 0.0296(14) 0.0174(12) 0.0170(12) 0.0018(10) -0.0007(10) -0.0013(11) O6 0.0325(15) 0.0287(14) 0.0154(13) 0.0068(11) -0.0004(11) -0.0044(12) O7 0.0337(15) 0.0222(13) 0.0238(14) 0.0055(11) -0.0034(11) 0.0044(12) O8 0.0395(18) 0.0447(18) 0.0333(17) 0.0185(15) -0.0017(14) -0.0052(15) O9 0.0454(19) 0.0407(18) 0.0344(17) 0.0141(15) 0.0037(15) 0.0009(15) O10 0.0390(18) 0.0379(17) 0.0397(18) 0.0136(15) -0.0003(14) 0.0038(14) O11 0.0327(16) 0.0371(16) 0.0262(15) 0.0106(13) 0.0001(12) 0.0020(13) O12 0.0404(17) 0.0329(16) 0.0248(15) 0.0071(12) 0.0001(13) -0.0010(14) N1 0.0224(15) 0.0180(14) 0.0174(15) 0.0033(12) -0.0001(12) 0.0007(12) N2 0.0319(18) 0.0218(16) 0.0237(16) 0.0049(13) 0.0056(14) 0.0060(14) N3 0.0341(18) 0.0187(15) 0.0159(15) 0.0041(12) 0.0037(13) 0.0067(14) N4 0.0248(16) 0.0145(14) 0.0178(15) 0.0024(12) 0.0035(12) 0.0034(12) N5 0.0224(15) 0.0161(14) 0.0143(14) 0.0007(11) 0.0016(12) 0.0027(12) N6 0.0217(15) 0.0148(14) 0.0176(14) 0.0038(12) 0.0010(12) 0.0031(12) N7 0.0208(15) 0.0181(14) 0.0176(14) 0.0043(12) -0.0010(12) 0.0038(12) N8 0.0213(15) 0.0195(14) 0.0159(14) 0.0055(12) 0.0009(12) 0.0017(12) N9 0.0276(17) 0.0214(15) 0.0174(15) 0.0009(12) -0.0042(13) -0.0006(13) N10 0.0227(16) 0.0312(18) 0.0168(15) -0.0008(13) 0.0009(12) 0.0058(14) N11 0.0221(15) 0.0173(14) 0.0130(14) 0.0009(11) -0.0009(11) 0.0022(12) N12 0.0227(15) 0.0153(14) 0.0129(14) 0.0001(11) -0.0017(11) 0.0001(12) N13 0.0230(15) 0.0171(14) 0.0134(14) 0.0025(11) -0.0002(11) 0.0017(12) N14 0.0258(16) 0.0142(14) 0.0149(14) 0.0030(11) 0.0005(12) 0.0009(12) N15 0.0202(16) 0.0328(18) 0.0216(16) 0.0096(14) -0.0022(12) 0.0037(14) N16 0.0292(18) 0.0210(16) 0.0273(17) 0.0084(14) 0.0002(14) 0.0033(14) C1 0.029(2) 0.0179(17) 0.0181(17) 0.0011(14) 0.0000(15) 0.0009(15) C2 0.030(2) 0.0222(19) 0.0215(18) 0.0009(15) 0.0013(15) 0.0008(16) C3 0.0250(19) 0.0227(18) 0.0206(18) 0.0076(15) 0.0030(15) 0.0011(15) C4 0.0215(18) 0.0186(17) 0.0165(17) 0.0031(14) 0.0019(13) -0.0025(14) C5 0.0185(17) 0.0183(16) 0.0174(17) 0.0038(14) 0.0001(13) 0.0021(14) C6 0.0206(18) 0.0174(17) 0.0185(17) 0.0058(14) 0.0004(14) 0.0038(14) C7 0.0202(17) 0.0211(17) 0.0160(16) 0.0074(14) -0.0008(13) 0.0007(14) C8 0.0257(19) 0.0206(18) 0.0247(19) 0.0097(15) 0.0008(15) 0.0002(15) C9 0.0209(18) 0.0253(18) 0.0228(18) 0.0090(15) 0.0010(14) 0.0050(15) C10 0.0210(18) 0.0217(18) 0.0200(17) 0.0097(14) -0.0012(14) 0.0037(14) C11 0.0220(18) 0.0225(18) 0.0115(15) 0.0037(13) -0.0034(13) 0.0066(15) C12 0.0257(19) 0.0208(18) 0.0184(17) 0.0036(14) 0.0023(14) 0.0036(15) C13 0.035(2) 0.0181(17) 0.0198(18) 0.0010(14) 0.0027(16) 0.0022(16) C14 0.0203(18) 0.0221(18) 0.0193(17) 0.0025(14) -0.0028(14) 0.0003(15) C15 0.0194(17) 0.0175(16) 0.0178(17) 0.0058(14) 0.0001(13) 0.0014(14) C16 0.0179(17) 0.0184(16) 0.0146(16) 0.0036(13) 0.0009(13) 0.0008(14) C17 0.0222(18) 0.0195(17) 0.0170(17) 0.0050(14) 0.0009(14) 0.0033(14) C18 0.0219(18) 0.0200(17) 0.0158(17) 0.0044(14) 0.0013(13) 0.0064(14) C19 0.029(2) 0.0203(18) 0.0232(19) 0.0086(15) 0.0003(15) 0.0013(15) C20 0.029(2) 0.0239(18) 0.0187(17) 0.0091(15) 0.0005(15) 0.0006(16) C21 0.0237(18) 0.0176(17) 0.0171(17) 0.0044(14) 0.0006(14) 0.0001(14) C22 0.0217(18) 0.0196(17) 0.0160(17) 0.0017(14) 0.0004(13) 0.0003(14) C23 0.0204(19) 0.031(2) 0.026(2) 0.0110(16) -0.0066(15) -0.0037(16) C24 0.0222(19) 0.0242(19) 0.0248(19) 0.0046(15) 0.0020(15) 0.0017(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.933(3) . ? Cu1 O5 1.935(3) . ? Cu1 N1 2.024(3) . ? Cu1 N14 2.071(3) . ? Cu1 S1 2.4951(12) . ? Cu2 N5 1.945(3) . ? Cu2 N12 1.972(3) . ? Cu2 N16 2.072(3) . ? Cu2 N6 2.088(3) . ? Cu2 N13 2.144(3) . ? Cu3 O2 1.955(3) . ? Cu3 N11 1.957(3) . ? Cu3 N15 1.991(3) 2_565 ? Cu3 N8 2.020(3) . ? Cu3 N7 2.191(3) . ? S1 C23 1.645(4) . ? S2 C24 1.632(4) . ? O1 C6 1.229(4) . ? O2 C11 1.264(5) . ? O3 C11 1.246(4) . ? O4 C17 1.241(4) . ? O5 C22 1.278(5) . ? O6 C22 1.223(4) . ? N1 C1 1.339(4) . ? N1 C4 1.344(5) . ? N2 C2 1.324(5) . ? N2 C3 1.345(5) . ? N3 C5 1.326(5) . ? N4 C5 1.308(5) . ? N4 N5 1.401(4) . ? N5 C6 1.333(5) . ? N6 C7 1.335(5) . ? N6 N7 1.336(4) . ? N7 C10 1.331(5) . ? N8 C12 1.326(5) . ? N8 C15 1.349(5) . ? N9 C13 1.333(5) . ? N9 C14 1.346(5) . ? N10 C16 1.325(5) . ? N11 C16 1.302(5) . ? N11 N12 1.409(4) . ? N12 C17 1.320(5) . ? N13 N14 1.333(4) . ? N13 C18 1.338(5) . ? N14 C21 1.329(5) . ? N15 C23 1.160(5) . ? N15 Cu3 1.991(3) 2_565 ? N16 C24 1.171(5) . ? C1 C2 1.393(5) . ? C3 C4 1.384(5) . ? C4 C5 1.492(5) . ? C6 C7 1.509(5) . ? C7 C8 1.401(5) . ? C8 C9 1.375(5) . ? C9 C10 1.391(5) . ? C10 C11 1.534(5) . ? C12 C13 1.391(5) . ? C14 C15 1.380(5) . ? C15 C16 1.483(5) . ? C17 C18 1.508(5) . ? C18 C19 1.395(5) . ? C19 C20 1.371(5) . ? C20 C21 1.403(5) . ? C21 C22 1.516(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 O5 170.12(12) . . ? N4 Cu1 N1 80.46(12) . . ? O5 Cu1 N1 94.55(11) . . ? N4 Cu1 N14 97.24(12) . . ? O5 Cu1 N14 81.55(11) . . ? N1 Cu1 N14 142.93(13) . . ? N4 Cu1 S1 93.01(10) . . ? O5 Cu1 S1 96.81(8) . . ? N1 Cu1 S1 113.32(9) . . ? N14 Cu1 S1 103.74(9) . . ? N5 Cu2 N12 168.86(13) . . ? N5 Cu2 N16 94.44(13) . . ? N12 Cu2 N16 95.87(13) . . ? N5 Cu2 N6 79.23(12) . . ? N12 Cu2 N6 97.58(12) . . ? N16 Cu2 N6 128.12(13) . . ? N5 Cu2 N13 94.80(12) . . ? N12 Cu2 N13 78.66(12) . . ? N16 Cu2 N13 103.79(12) . . ? N6 Cu2 N13 127.95(12) . . ? O2 Cu3 N11 164.17(12) . . ? O2 Cu3 N15 99.92(12) . 2_565 ? N11 Cu3 N15 94.51(13) . 2_565 ? O2 Cu3 N8 91.81(12) . . ? N11 Cu3 N8 80.21(12) . . ? N15 Cu3 N8 143.62(13) 2_565 . ? O2 Cu3 N7 79.05(11) . . ? N11 Cu3 N7 93.38(12) . . ? N15 Cu3 N7 94.74(13) 2_565 . ? N8 Cu3 N7 121.38(12) . . ? C23 S1 Cu1 98.54(14) . . ? C11 O2 Cu3 119.2(2) . . ? C22 O5 Cu1 116.8(2) . . ? C1 N1 C4 118.5(3) . . ? C1 N1 Cu1 127.9(3) . . ? C4 N1 Cu1 113.6(2) . . ? C2 N2 C3 116.4(3) . . ? C5 N4 N5 118.7(3) . . ? C5 N4 Cu1 118.5(2) . . ? N5 N4 Cu1 122.8(2) . . ? C6 N5 N4 115.3(3) . . ? C6 N5 Cu2 120.9(2) . . ? N4 N5 Cu2 123.2(2) . . ? C7 N6 N7 120.1(3) . . ? C7 N6 Cu2 112.7(2) . . ? N7 N6 Cu2 127.2(2) . . ? C10 N7 N6 119.6(3) . . ? C10 N7 Cu3 110.7(2) . . ? N6 N7 Cu3 129.4(2) . . ? C12 N8 C15 118.3(3) . . ? C12 N8 Cu3 128.1(3) . . ? C15 N8 Cu3 113.3(2) . . ? C13 N9 C14 117.1(3) . . ? C16 N11 N12 118.7(3) . . ? C16 N11 Cu3 117.5(2) . . ? N12 N11 Cu3 121.3(2) . . ? C17 N12 N11 115.3(3) . . ? C17 N12 Cu2 120.1(2) . . ? N11 N12 Cu2 123.3(2) . . ? N14 N13 C18 119.2(3) . . ? N14 N13 Cu2 128.6(2) . . ? C18 N13 Cu2 112.1(2) . . ? C21 N14 N13 120.6(3) . . ? C21 N14 Cu1 110.9(2) . . ? N13 N14 Cu1 128.5(2) . . ? C23 N15 Cu3 168.4(3) . 2_565 ? C24 N16 Cu2 144.3(3) . . ? N1 C1 C2 119.5(4) . . ? N2 C2 C1 123.2(4) . . ? N2 C3 C4 122.0(3) . . ? N1 C4 C3 120.4(3) . . ? N1 C4 C5 113.9(3) . . ? C3 C4 C5 125.7(3) . . ? N4 C5 N3 125.3(3) . . ? N4 C5 C4 113.4(3) . . ? N3 C5 C4 121.3(3) . . ? O1 C6 N5 128.9(3) . . ? O1 C6 C7 120.3(3) . . ? N5 C6 C7 110.8(3) . . ? N6 C7 C8 122.1(3) . . ? N6 C7 C6 116.2(3) . . ? C8 C7 C6 121.6(3) . . ? C9 C8 C7 117.7(4) . . ? C8 C9 C10 117.3(3) . . ? N7 C10 C9 123.0(3) . . ? N7 C10 C11 113.8(3) . . ? C9 C10 C11 123.2(3) . . ? O3 C11 O2 125.8(3) . . ? O3 C11 C10 117.4(3) . . ? O2 C11 C10 116.7(3) . . ? N8 C12 C13 120.7(4) . . ? N9 C13 C12 121.8(3) . . ? N9 C14 C15 121.6(3) . . ? N8 C15 C14 120.5(3) . . ? N8 C15 C16 114.4(3) . . ? C14 C15 C16 125.1(3) . . ? N11 C16 N10 126.9(3) . . ? N11 C16 C15 113.2(3) . . ? N10 C16 C15 119.9(3) . . ? O4 C17 N12 129.2(3) . . ? O4 C17 C18 117.4(3) . . ? N12 C17 C18 113.3(3) . . ? N13 C18 C19 123.0(3) . . ? N13 C18 C17 115.7(3) . . ? C19 C18 C17 121.2(3) . . ? C20 C19 C18 117.2(3) . . ? C19 C20 C21 117.9(3) . . ? N14 C21 C20 122.1(3) . . ? N14 C21 C22 114.7(3) . . ? C20 C21 C22 123.2(3) . . ? O6 C22 O5 127.1(3) . . ? O6 C22 C21 117.8(3) . . ? O5 C22 C21 115.1(3) . . ? N15 C23 S1 178.7(4) . . ? N16 C24 S2 177.9(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.398 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.130 #=== data_Compound4 _database_code_depnum_ccdc_archive 'CCDC 706533' # start Validation Reply Form _vrf_PLAT306_Compound4 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O6 RESPONSE: This is a lattice solvent molecule. The corresponding H-atoms could not be located in the difference map and were omitted from the model. They were included in the formula for purposes of calculated intensive properties. ; _vrf_PLAT430_Compound4 ; PROBLEM: Short Inter D...A Contact O5 .. O8 .. 2.37 Ang. RESPONSE: O5 and O8 are both partial occupancy (0.25 each) lattice solvent molecules. The sum of their total occupancy is 0.5 and therefore the short contact does not imply a bonding interaction or shared space at any time. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C11 H7 O3 N7)2 Cu3 (H2 O)] (B F4)2 (H2 O)4' _chemical_formula_sum 'C22 H24 B2 Cu3 F8 N14 O11' _chemical_formula_weight 1024.76 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 23.874(3) _cell_length_b 9.4261(9) _cell_length_c 17.801(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.728(2) _cell_angle_gamma 90.00 _cell_volume 3695.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 7374 _cell_measurement_theta_min 2.4851 _cell_measurement_theta_max 30.6232 _exptl_crystal_description Prism _exptl_crystal_colour 'Dark Green' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.3127 _exptl_absorpt_correction_T_max 0.6688 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(2) _diffrn_radiation_wavelength 0.71070 _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 18683 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4224 _reflns_number_gt 4120 _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^)+(0.1322P)^2^+21.8533P] 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 4224 _refine_ls_number_parameters 281 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1959 _refine_ls_wR_factor_gt 0.1949 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.004 _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 Cu1 Cu 1.132832(19) 0.47061(5) 0.17725(3) 0.01885(19) Uani 1 1 d . . . Cu2 Cu 1.0000 0.51814(7) 0.2500 0.0172(2) Uani 1 2 d S . . F1 F 1.0948(3) 0.8619(5) 0.1662(4) 0.140(3) Uani 1 1 d D . . F2 F 1.1737(3) 0.9924(7) 0.1656(5) 0.133(3) Uani 1 1 d D . . F3 F 1.1321(9) 1.0267(19) 0.2554(9) 0.356(14) Uani 1 1 d D . . F4 F 1.0860(5) 1.0924(11) 0.1356(10) 0.252(7) Uani 1 1 d D . . O1 O 1.13586(12) 0.4138(3) 0.07409(16) 0.0239(6) Uani 1 1 d . . . O2 O 1.08464(13) 0.2938(3) -0.04013(17) 0.0280(6) Uani 1 1 d . . . O3 O 0.83892(11) 0.4015(3) 0.07614(16) 0.0229(5) Uani 1 1 d . . . O4 O 1.0000 0.7415(6) 0.2500 0.068(2) Uani 1 2 d S . . O5 O 1.0364(10) 0.1575(16) 0.2719(13) 0.067(5) Uani 0.25 1 d P . . O6 O 0.73400(17) 0.4583(4) 0.4628(2) 0.0426(8) Uani 1 1 d . . . O7 O 0.6389(8) 0.5304(18) 0.4964(11) 0.111(5) Uiso 0.50 1 d P . . O8 O 0.5406(12) 0.460(3) 0.3566(17) 0.086(7) Uiso 0.25 1 d P . . N1 N 1.04451(13) 0.4099(3) 0.11918(18) 0.0172(6) Uani 1 1 d . . . N2 N 0.99816(14) 0.4319(3) 0.14197(18) 0.0170(6) Uani 1 1 d . . . N3 N 0.91318(13) 0.5004(4) 0.19110(19) 0.0186(6) Uani 1 1 d . . . N4 N 0.87035(14) 0.5440(3) 0.22277(19) 0.0184(6) Uani 1 1 d . . . N5 N 0.83210(14) 0.7172(4) 0.12111(19) 0.0228(6) Uani 1 1 d . . . H3 H 0.8570 0.6931 0.0975 0.027 Uiso 1 1 calc R . . H4 H 0.8060 0.7867 0.1009 0.027 Uiso 1 1 calc R . . N6 N 0.70854(14) 0.8172(3) 0.23562(19) 0.0216(6) Uani 1 1 d . . . N7 N 0.80444(14) 0.6287(3) 0.30013(19) 0.0203(6) Uani 1 1 d . . . C1 C 1.09000(16) 0.3472(4) 0.0251(2) 0.0210(7) Uani 1 1 d . . . C2 C 1.03555(16) 0.3448(4) 0.0492(2) 0.0194(7) Uani 1 1 d . . . C3 C 0.97959(17) 0.2883(4) -0.0005(2) 0.0223(7) Uani 1 1 d . . . H1 H 0.9746 0.2368 -0.0485 0.027 Uiso 1 1 calc R . . C4 C 0.93144(16) 0.3107(4) 0.0233(2) 0.0221(7) Uani 1 1 d . . . H2 H 0.8921 0.2748 -0.0078 0.027 Uiso 1 1 calc R . . C5 C 0.94283(15) 0.3874(4) 0.0942(2) 0.0182(7) Uani 1 1 d . . . C6 C 0.89195(15) 0.4300(4) 0.1205(2) 0.0181(7) Uani 1 1 d . . . C7 C 0.83387(15) 0.6491(4) 0.1866(2) 0.0196(7) Uani 1 1 d . . . C8 C 0.79208(16) 0.6903(4) 0.2273(2) 0.0197(7) Uani 1 1 d . . . C9 C 0.74406(16) 0.7833(4) 0.1947(2) 0.0212(7) Uani 1 1 d . . . H5 H 0.7358 0.8241 0.1427 0.025 Uiso 1 1 calc R . . C10 C 0.72250(17) 0.7600(4) 0.3087(2) 0.0241(7) Uani 1 1 d . . . H6 H 0.6995 0.7856 0.3398 0.029 Uiso 1 1 calc R . . C11 C 0.77017(17) 0.6629(4) 0.3413(2) 0.0237(7) Uani 1 1 d . . . H7 H 0.7781 0.6212 0.3930 0.028 Uiso 1 1 calc R . . B1 B 1.1180(5) 0.9900(9) 0.1712(9) 0.133(8) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0135(3) 0.0280(3) 0.0190(3) -0.00134(15) 0.0106(2) -0.00153(15) Cu2 0.0118(3) 0.0258(4) 0.0174(3) 0.000 0.0091(3) 0.000 F1 0.132(5) 0.056(3) 0.130(5) 0.001(3) -0.062(4) -0.006(3) F2 0.085(4) 0.086(4) 0.177(8) -0.005(4) -0.005(4) 0.006(3) F3 0.50(3) 0.39(2) 0.235(15) -0.198(16) 0.202(18) -0.35(2) F4 0.201(10) 0.140(8) 0.404(19) 0.176(11) 0.103(11) 0.100(8) O1 0.0157(12) 0.0370(15) 0.0230(13) -0.0021(11) 0.0120(10) 0.0003(11) O2 0.0265(14) 0.0391(16) 0.0259(14) -0.0078(12) 0.0182(11) -0.0032(12) O3 0.0155(11) 0.0312(14) 0.0246(13) -0.0022(11) 0.0105(10) -0.0022(10) O4 0.054(3) 0.023(2) 0.096(5) 0.000 -0.005(3) 0.000 O5 0.101(14) 0.021(6) 0.095(15) -0.008(8) 0.057(13) -0.006(8) O6 0.0394(19) 0.044(2) 0.0395(19) -0.0057(15) 0.0099(15) -0.0101(15) N1 0.0135(13) 0.0216(14) 0.0206(13) 0.0001(11) 0.0112(11) 0.0012(11) N2 0.0149(13) 0.0218(14) 0.0188(14) -0.0003(11) 0.0115(11) 0.0000(11) N3 0.0119(13) 0.0290(14) 0.0191(14) -0.0011(12) 0.0108(11) 0.0015(11) N4 0.0144(13) 0.0271(15) 0.0190(14) -0.0007(11) 0.0122(12) 0.0023(11) N5 0.0219(15) 0.0284(16) 0.0237(15) 0.0038(12) 0.0151(12) 0.0074(12) N6 0.0196(14) 0.0243(15) 0.0261(15) -0.0014(12) 0.0145(12) 0.0026(12) N7 0.0187(14) 0.0224(14) 0.0248(15) 0.0001(12) 0.0138(12) 0.0019(11) C1 0.0187(16) 0.0270(17) 0.0220(16) 0.0025(14) 0.0131(13) 0.0047(14) C2 0.0191(16) 0.0225(16) 0.0207(16) 0.0016(13) 0.0124(13) 0.0027(13) C3 0.0215(17) 0.0262(17) 0.0235(17) -0.0042(14) 0.0134(14) 0.0005(14) C4 0.0163(16) 0.0266(18) 0.0254(17) -0.0017(15) 0.0102(13) -0.0020(13) C5 0.0162(15) 0.0217(16) 0.0208(16) 0.0016(13) 0.0117(13) 0.0019(12) C6 0.0146(15) 0.0229(16) 0.0207(16) 0.0008(13) 0.0111(13) 0.0005(13) C7 0.0149(15) 0.0261(17) 0.0205(16) -0.0016(13) 0.0099(13) -0.0010(13) C8 0.0164(15) 0.0235(16) 0.0232(16) -0.0024(13) 0.0122(13) -0.0007(13) C9 0.0166(15) 0.0278(17) 0.0227(16) 0.0000(14) 0.0114(13) 0.0020(14) C10 0.0237(17) 0.0264(18) 0.0300(19) 0.0008(15) 0.0189(15) 0.0051(15) C11 0.0241(18) 0.0288(18) 0.0251(17) 0.0033(15) 0.0172(15) 0.0048(15) B1 0.070(7) 0.036(4) 0.224(19) -0.014(7) -0.018(9) -0.008(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 N4 1.938(3) 2_755 ? Cu1 O1 1.941(3) . ? Cu1 N1 2.039(3) . ? Cu1 N7 2.040(3) 2_755 ? Cu1 N6 2.233(3) 3_545 ? Cu2 N3 1.935(3) 2_755 ? Cu2 N3 1.935(3) . ? Cu2 N2 2.073(3) . ? Cu2 N2 2.073(3) 2_755 ? Cu2 O4 2.106(5) . ? F1 B1 1.318(10) . ? F2 B1 1.370(13) . ? F3 B1 1.446(15) . ? F4 B1 1.242(11) . ? O1 C1 1.271(5) . ? O2 C1 1.226(5) . ? O3 C6 1.236(4) . ? O5 O5 1.61(4) 2_755 ? N1 C2 1.330(5) . ? N1 N2 1.334(4) . ? N2 C5 1.333(5) . ? N3 C6 1.335(5) . ? N3 N4 1.406(4) . ? N4 C7 1.312(5) . ? N4 Cu1 1.938(3) 2_755 ? N5 C7 1.317(5) . ? N5 H3 0.8800 . ? N5 H4 0.8800 . ? N6 C10 1.326(5) . ? N6 C9 1.352(4) . ? N6 Cu1 2.233(3) 3_455 ? N7 C11 1.332(4) . ? N7 C8 1.344(5) . ? N7 Cu1 2.040(3) 2_755 ? C1 C2 1.518(5) . ? C2 C3 1.392(5) . ? C3 C4 1.386(5) . ? C3 H1 0.9500 . ? C4 C5 1.387(5) . ? C4 H2 0.9500 . ? C5 C6 1.516(4) . ? C7 C8 1.493(5) . ? C8 C9 1.381(5) . ? C9 H5 0.9500 . ? C10 C11 1.400(5) . ? C10 H6 0.9500 . ? C11 H7 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 N4 Cu1 O1 175.09(13) 2_755 . ? N4 Cu1 N1 99.56(12) 2_755 . ? O1 Cu1 N1 81.49(11) . . ? N4 Cu1 N7 81.03(13) 2_755 2_755 ? O1 Cu1 N7 95.48(12) . 2_755 ? N1 Cu1 N7 147.33(12) . 2_755 ? N4 Cu1 N6 96.66(13) 2_755 3_545 ? O1 Cu1 N6 86.69(12) . 3_545 ? N1 Cu1 N6 123.14(12) . 3_545 ? N7 Cu1 N6 88.90(12) 2_755 3_545 ? N3 Cu2 N3 170.1(2) 2_755 . ? N3 Cu2 N2 95.92(13) 2_755 . ? N3 Cu2 N2 80.16(12) . . ? N3 Cu2 N2 80.16(12) 2_755 2_755 ? N3 Cu2 N2 95.92(13) . 2_755 ? N2 Cu2 N2 133.82(18) . 2_755 ? N3 Cu2 O4 94.96(10) 2_755 . ? N3 Cu2 O4 94.96(10) . . ? N2 Cu2 O4 113.09(9) . . ? N2 Cu2 O4 113.09(9) 2_755 . ? C1 O1 Cu1 116.6(2) . . ? C2 N1 N2 120.3(3) . . ? C2 N1 Cu1 111.4(2) . . ? N2 N1 Cu1 128.2(2) . . ? C5 N2 N1 119.4(3) . . ? C5 N2 Cu2 112.1(2) . . ? N1 N2 Cu2 128.4(2) . . ? C6 N3 N4 116.9(3) . . ? C6 N3 Cu2 119.4(2) . . ? N4 N3 Cu2 123.4(2) . . ? C7 N4 N3 118.2(3) . . ? C7 N4 Cu1 117.8(2) . 2_755 ? N3 N4 Cu1 123.8(2) . 2_755 ? C7 N5 H3 120.0 . . ? C7 N5 H4 120.0 . . ? H3 N5 H4 120.0 . . ? C10 N6 C9 117.4(3) . . ? C10 N6 Cu1 124.8(2) . 3_455 ? C9 N6 Cu1 117.7(2) . 3_455 ? C11 N7 C8 118.3(3) . . ? C11 N7 Cu1 128.9(3) . 2_755 ? C8 N7 Cu1 112.1(2) . 2_755 ? O2 C1 O1 126.8(3) . . ? O2 C1 C2 118.3(3) . . ? O1 C1 C2 114.7(3) . . ? N1 C2 C3 122.6(3) . . ? N1 C2 C1 114.3(3) . . ? C3 C2 C1 122.9(3) . . ? C4 C3 C2 117.0(3) . . ? C4 C3 H1 121.5 . . ? C2 C3 H1 121.5 . . ? C3 C4 C5 117.6(3) . . ? C3 C4 H2 121.2 . . ? C5 C4 H2 121.2 . . ? N2 C5 C4 122.8(3) . . ? N2 C5 C6 115.8(3) . . ? C4 C5 C6 121.4(3) . . ? O3 C6 N3 129.3(3) . . ? O3 C6 C5 119.3(3) . . ? N3 C6 C5 111.4(3) . . ? N4 C7 N5 126.2(3) . . ? N4 C7 C8 113.5(3) . . ? N5 C7 C8 120.3(3) . . ? N7 C8 C9 121.1(3) . . ? N7 C8 C7 114.6(3) . . ? C9 C8 C7 124.2(3) . . ? N6 C9 C8 121.0(3) . . ? N6 C9 H5 119.5 . . ? C8 C9 H5 119.5 . . ? N6 C10 C11 122.0(3) . . ? N6 C10 H6 119.0 . . ? C11 C10 H6 119.0 . . ? N7 C11 C10 120.2(3) . . ? N7 C11 H7 119.9 . . ? C10 C11 H7 119.9 . . ? F4 B1 F1 121.2(10) . . ? F4 B1 F2 111.9(11) . . ? F1 B1 F2 113.9(9) . . ? F4 B1 F3 101.2(14) . . ? F1 B1 F3 102.2(11) . . ? F2 B1 F3 103.1(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.137 _refine_diff_density_min -1.149 _refine_diff_density_rms 0.176 # Attachment 'Updated_cif1.cif' data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 706534' # start Validation Reply Form _vrf_PLAT431_Compound2 ; PROBLEM: Short Inter HL..A Contact F13 .. F15 .. 1.74 Ang. RESPONSE: These are members of a partial occupancy -CF3 group in a disordered triflate anion. These do not in fact form an intermolecular contact. ; _vrf_PLAT432_Compound2 ; PROBLEM: Short Inter X...Y Contact F13 .. C105 .. 2.12 Ang. RESPONSE: These are members of a partial occupancy -CF3 group in a disordered triflate anion. These do not in fact form an intermolecular contact. ; _vrf_PLAT780_Compound2 ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: This comment relates to The members of a partial occupancy -CF3 group in a disordered triflate anion. These do not in fact form connected set contacts. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C20 H15 N7 O2)2 (C20 H14 N7 O2)3 Cu9 (C F3 O3 S)5 (H2 O)13' _chemical_formula_sum 'C105 H98 Cu9 F15 N35 O38 S5' _chemical_formula_weight 3475.33 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 17.753(2) _cell_length_b 20.746(2) _cell_length_c 21.101(3) _cell_angle_alpha 70.888(8) _cell_angle_beta 86.375(12) _cell_angle_gamma 75.960(9) _cell_volume 7123.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 29620 _cell_measurement_theta_min 2.0508 _cell_measurement_theta_max 30.9626 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3506 _exptl_absorpt_coefficient_mu 1.495 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5652 _exptl_absorpt_correction_T_max 0.8697 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 138(2) _diffrn_radiation_wavelength 0.71070 _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 67786 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 26.50 _reflns_number_total 29326 _reflns_number_gt 21895 _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)' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 227.9 electrons per unit cell in three voids (total volume 1404.8 ^A^3); that is 113.95 electrons per formula unit. Disordered solvent water molecules appeared to be present prior to the application of Squeeze, and the disperse electron density was assigned as 11 water molecules per formula unit. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the framework structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 1 -0.077 0.448 0.784 42.6 15.7 2 0.077 0.552 0.216 42.6 10.6 3 0.500 0.000 0.700 1319.6 201.6 _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^)+(0.1326P)^2^+17.7440P] 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 29326 _refine_ls_number_parameters 1732 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2591 _refine_ls_wR_factor_gt 0.2395 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _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 Cu1 Cu 0.77607(4) 0.35251(4) 0.07048(3) 0.03429(17) Uani 1 1 d . . . Cu2 Cu 0.88070(4) 0.21350(4) 0.24547(4) 0.0448(2) Uani 1 1 d . . . Cu3 Cu 0.92345(5) 0.13456(4) 0.43411(4) 0.04273(19) Uani 1 1 d . . . Cu4 Cu 0.79063(5) 0.47909(4) 0.46239(4) 0.0485(2) Uani 1 1 d . . . Cu5 Cu 0.81195(5) 0.59745(4) 0.27021(4) 0.0445(2) Uani 1 1 d . . . Cu6 Cu 0.77936(4) 0.69157(4) 0.07927(4) 0.03756(18) Uani 1 1 d . . . Cu7 Cu 0.69015(5) 0.31536(4) 0.42455(4) 0.0441(2) Uani 1 1 d . . . Cu8 Cu 0.68658(4) 0.43077(4) 0.25859(4) 0.03861(18) Uani 1 1 d . . . Cu9 Cu 0.60895(4) 0.53893(4) 0.09830(4) 0.03593(17) Uani 1 1 d . . . S1 S 0.3259(3) 0.78235(19) 0.40270(19) 0.0618(9) Uani 0.65 1 d P A 1 O14 O 0.4040(7) 0.7649(7) 0.4158(6) 0.102(4) Uani 0.65 1 d P A 1 O15 O 0.2849(12) 0.7283(6) 0.4434(6) 0.103(5) Uani 0.65 1 d P A 1 S2 S 0.2827(5) 0.7743(4) 0.4003(4) 0.0625(17) Uani 0.35 1 d P A 2 O16 O 0.3458(12) 0.7280(10) 0.4473(8) 0.066(5) Uani 0.35 1 d P A 2 O17 O 0.2173(12) 0.7432(9) 0.4073(11) 0.078(5) Uani 0.35 1 d P A 2 S3 S 0.40345(15) 0.51515(14) 0.33602(14) 0.0763(6) Uani 1 1 d . . . S4 S 0.66114(9) 0.53748(8) -0.07571(7) 0.0388(3) Uani 1 1 d . . . S5 S 0.4596(3) 0.0786(3) 0.2897(3) 0.1572(17) Uiso 1 1 d . . . S6 S 0.8711(4) 0.0298(3) 0.0872(3) 0.0926(16) Uiso 0.60 1 d PD B 3 O29 O 0.8341(11) -0.0278(9) 0.0970(10) 0.130(7) Uiso 0.60 1 d PD B 3 C105 C 0.9503(9) 0.0109(10) 0.0422(9) 0.113(7) Uiso 0.60 1 d PD B 3 F13 F 0.9297(9) 0.0180(8) -0.0221(7) 0.146(5) Uiso 0.60 1 d PD . 3 F14 F 0.9980(9) 0.0542(8) 0.0356(8) 0.160(6) Uiso 0.60 1 d PD B 3 F15 F 0.9971(9) -0.0569(8) 0.0640(8) 0.154(5) Uiso 0.60 1 d PD . 3 S7 S 0.8572(5) 0.0288(5) 0.1114(5) 0.094(3) Uiso 0.40 1 d PD B 4 O30 O 0.8677(12) -0.0319(9) 0.0883(9) 0.077(5) Uiso 0.40 1 d PD B 4 C106 C 0.7648(11) 0.0459(13) 0.1400(11) 0.108(10) Uiso 0.40 1 d PD B 4 F16 F 0.7517(12) -0.0093(11) 0.1926(10) 0.146(7) Uiso 0.40 1 d PD B 4 F17 F 0.7122(11) 0.0572(11) 0.0905(10) 0.134(7) Uiso 0.40 1 d PD B 4 F18 F 0.7519(17) 0.1013(14) 0.1654(15) 0.218(13) Uiso 0.40 1 d PD B 4 F1 F 0.3497(5) 0.7121(4) 0.3164(3) 0.108(2) Uani 1 1 d . A . F2 F 0.3530(4) 0.8197(4) 0.2798(4) 0.125(3) Uani 1 1 d . A . F3 F 0.2465(4) 0.7968(6) 0.2928(4) 0.153(4) Uani 1 1 d . A . F4 F 0.3308(6) 0.5053(9) 0.2382(6) 0.255(8) Uani 1 1 d . . . F5 F 0.2832(4) 0.5966(6) 0.2621(4) 0.148(4) Uani 1 1 d . . . F6 F 0.2629(5) 0.5022(7) 0.3235(6) 0.179(5) Uani 1 1 d . . . F7 F 0.7573(3) 0.5457(4) -0.1753(3) 0.0949(19) Uani 1 1 d . . . F8 F 0.6934(4) 0.6445(3) -0.1705(3) 0.0844(16) Uani 1 1 d . . . F9 F 0.7874(3) 0.5846(3) -0.1006(3) 0.0868(17) Uani 1 1 d . . . F10 F 0.5810(11) 0.0025(11) 0.2450(9) 0.267(7) Uiso 1 1 d . . . F11 F 0.5171(9) 0.0954(9) 0.1711(9) 0.242(6) Uiso 1 1 d . . . F12 F 0.5924(10) 0.1036(9) 0.2422(8) 0.243(6) Uiso 1 1 d . . . O1 O 0.8585(2) 0.2587(2) 0.1465(2) 0.0402(9) Uani 1 1 d . . . O2 O 0.9381(2) 0.1563(2) 0.3333(2) 0.0393(9) Uani 1 1 d . . . O3 O 0.8307(3) 0.5543(2) 0.3740(2) 0.0508(11) Uani 1 1 d . . . O4 O 0.8295(3) 0.6625(2) 0.1694(2) 0.0422(10) Uani 1 1 d . . . O5 O 0.8068(3) 0.1210(2) 0.4301(2) 0.0460(10) Uani 1 1 d . . . O6 O 0.8724(3) 0.3901(2) 0.4593(2) 0.0496(11) Uani 1 1 d . . . O7 O 0.7724(2) 0.2298(2) 0.2703(2) 0.0381(9) Uani 1 1 d . . . O8 O 0.8906(3) 0.4938(2) 0.2586(2) 0.0480(11) Uani 1 1 d . . . O9 O 0.6536(3) 0.7170(2) 0.1059(2) 0.0450(10) Uani 1 1 d . . . O10 O 0.8264(2) 0.4295(2) 0.0744(2) 0.0371(9) Uani 1 1 d . . . O11 O 0.8466(6) 0.1012(5) 0.2393(5) 0.126(3) Uani 1 1 d . . . O12 O 0.7670(4) 0.3936(3) 0.5775(3) 0.0751(16) Uiso 1 1 d . . . O13 O 0.2805(5) 0.8492(4) 0.3991(4) 0.104(2) Uani 1 1 d . . . O18 O 0.4501(4) 0.5497(4) 0.2824(4) 0.088(2) Uani 1 1 d . . . O19 O 0.3743(4) 0.5470(4) 0.3842(4) 0.100(2) Uani 1 1 d . . . O20 O 0.4328(6) 0.4397(4) 0.3643(4) 0.117(3) Uani 1 1 d . . . O21 O 0.5989(3) 0.5430(3) -0.1190(2) 0.0503(11) Uani 1 1 d . . . O22 O 0.6409(3) 0.5808(2) -0.0328(2) 0.0474(11) Uani 1 1 d . . . O23 O 0.7054(3) 0.4668(3) -0.0446(2) 0.0613(14) Uani 1 1 d . . . O24 O 0.4293(9) 0.1549(9) 0.2695(8) 0.196(6) Uiso 1 1 d . . . O25 O 0.4893(11) 0.0406(10) 0.3642(10) 0.240(7) Uiso 1 1 d . . . O26 O 0.3967(8) 0.0421(7) 0.2807(7) 0.168(4) Uiso 1 1 d . . . O27 O 0.9059(6) 0.0181(5) 0.1639(5) 0.129(3) Uiso 1 1 d . . . O28 O 0.8444(8) 0.0993(8) 0.0606(7) 0.175(5) Uiso 1 1 d . . . N1 N 0.8501(3) 0.3110(2) 0.0119(2) 0.0338(10) Uani 1 1 d . . . N2 N 0.9811(3) 0.1888(3) 0.1420(2) 0.0390(11) Uani 1 1 d . . . N3 N 0.9760(3) 0.1726(3) 0.2105(2) 0.0351(10) Uani 1 1 d . . . N4 N 1.0572(3) 0.0783(3) 0.3697(2) 0.0375(11) Uani 1 1 d . . . N5 N 1.0248(3) 0.0788(2) 0.4310(2) 0.0375(11) Uani 1 1 d . . . N6 N 1.1459(3) 0.0307(3) 0.4863(3) 0.0541(15) Uani 1 1 d . . . H1 H 1.1700 0.0271 0.4494 0.065 Uiso 1 1 calc R . . H2 H 1.1723 0.0170 0.5242 0.065 Uiso 1 1 calc R . . N7 N 0.9510(4) 0.0968(3) 0.5331(3) 0.0472(13) Uani 1 1 d . . . N8 N 0.8591(4) 0.5169(3) 0.5050(3) 0.0508(14) Uani 1 1 d . . . N9 N 0.9042(4) 0.6374(3) 0.3510(3) 0.0467(13) Uani 1 1 d . . . N10 N 0.8795(3) 0.6513(3) 0.2856(3) 0.0425(12) Uani 1 1 d . . . N11 N 0.8701(3) 0.7662(3) 0.1213(2) 0.0372(11) Uani 1 1 d . . . N12 N 0.8292(3) 0.7661(3) 0.0679(2) 0.0372(11) Uani 1 1 d . . . N13 N 0.8384(4) 0.8805(3) 0.0060(3) 0.0512(14) Uani 1 1 d . . . H3 H 0.8667 0.8834 0.0373 0.061 Uiso 1 1 calc R . . H4 H 0.8260 0.9161 -0.0312 0.061 Uiso 1 1 calc R . . N14 N 0.7445(3) 0.7523(3) -0.0171(3) 0.0440(12) Uani 1 1 d . . . N15 N 0.6290(3) 0.2483(3) 0.4213(3) 0.0466(13) Uani 1 1 d . . . N16 N 0.7771(3) 0.2371(3) 0.4254(3) 0.0396(11) Uani 1 1 d . . . N17 N 0.8552(3) 0.2288(3) 0.4355(2) 0.0380(11) Uani 1 1 d . . . N18 N 0.7647(4) 0.3684(3) 0.4264(3) 0.0484(13) Uani 1 1 d . . . N19 N 0.7313(3) 0.4351(3) 0.4270(3) 0.0501(14) Uani 1 1 d . . . N20 N 0.6165(4) 0.4048(3) 0.4216(3) 0.0536(15) Uani 1 1 d . . . H5 H 0.5658 0.4137 0.4166 0.064 Uiso 1 1 calc R . . N21 N 0.6783(4) 0.5453(3) 0.4572(3) 0.0527(14) Uani 1 1 d . . . N22 N 0.6125(3) 0.3739(3) 0.2583(3) 0.0422(12) Uani 1 1 d . . . N23 N 0.7643(3) 0.3463(3) 0.2600(2) 0.0379(11) Uani 1 1 d . . . N24 N 0.8442(3) 0.3324(3) 0.2588(2) 0.0357(10) Uani 1 1 d . . . N25 N 0.7691(3) 0.4761(3) 0.2588(3) 0.0429(12) Uani 1 1 d . . . N26 N 0.7432(3) 0.5447(3) 0.2596(3) 0.0449(12) Uani 1 1 d . . . N27 N 0.6218(3) 0.5213(3) 0.2601(3) 0.0447(12) Uani 1 1 d . . . H6 H 0.5707 0.5325 0.2595 0.054 Uiso 1 1 calc R . . N28 N 0.6964(4) 0.6654(3) 0.2736(3) 0.0513(14) Uani 1 1 d . . . N29 N 0.5191(3) 0.6151(3) 0.1049(3) 0.0458(13) Uani 1 1 d . . . N30 N 0.6685(3) 0.6069(2) 0.0954(2) 0.0344(10) Uani 1 1 d . . . N31 N 0.7466(3) 0.6031(3) 0.0863(2) 0.0364(10) Uani 1 1 d . . . N32 N 0.7051(3) 0.4697(3) 0.1087(2) 0.0344(10) Uani 1 1 d . . . N33 N 0.6949(3) 0.4058(2) 0.1067(2) 0.0313(9) Uani 1 1 d . . . N34 N 0.5658(3) 0.4625(3) 0.0939(3) 0.0381(11) Uani 1 1 d . . . H7 H 0.5159 0.4648 0.0909 0.046 Uiso 1 1 calc R . . N35 N 0.6860(3) 0.3042(3) 0.0700(3) 0.0412(11) Uani 1 1 d . . . C1 C 0.8403(4) 0.3342(4) -0.0544(3) 0.0434(14) Uani 1 1 d . . . H8 H 0.7981 0.3727 -0.0740 0.052 Uiso 1 1 calc R . . C2 C 0.8898(4) 0.3040(4) -0.0963(3) 0.0483(15) Uani 1 1 d . . . H9 H 0.8817 0.3214 -0.1435 0.058 Uiso 1 1 calc R . . C3 C 0.9514(4) 0.2476(4) -0.0669(4) 0.0524(17) Uani 1 1 d . . . H10 H 0.9858 0.2256 -0.0940 0.063 Uiso 1 1 calc R . . C4 C 0.9622(4) 0.2241(4) 0.0015(3) 0.0432(14) Uani 1 1 d . . . H11 H 1.0043 0.1859 0.0220 0.052 Uiso 1 1 calc R . . C5 C 0.9114(3) 0.2563(3) 0.0403(3) 0.0365(12) Uani 1 1 d . . . C6 C 0.9173(3) 0.2335(3) 0.1153(3) 0.0379(13) Uani 1 1 d . . . C7 C 1.0266(3) 0.1243(3) 0.2515(3) 0.0371(12) Uani 1 1 d . . . C8 C 1.0922(3) 0.0750(3) 0.2329(3) 0.0376(13) Uani 1 1 d . . . C9 C 1.0787(4) 0.0453(3) 0.1853(3) 0.0442(14) Uani 1 1 d . . . H12 H 1.0296 0.0597 0.1630 0.053 Uiso 1 1 calc R . . C10 C 1.1378(4) -0.0056(4) 0.1708(3) 0.0513(17) Uani 1 1 d . . . H13 H 1.1285 -0.0259 0.1386 0.062 Uiso 1 1 calc R . . C11 C 1.2098(4) -0.0269(4) 0.2024(4) 0.0545(18) Uani 1 1 d . . . H14 H 1.2493 -0.0618 0.1920 0.065 Uiso 1 1 calc R . . C12 C 1.2241(4) 0.0022(4) 0.2490(4) 0.0517(17) Uani 1 1 d . . . H15 H 1.2736 -0.0117 0.2704 0.062 Uiso 1 1 calc R . . C13 C 1.1647(4) 0.0526(4) 0.2645(3) 0.0442(14) Uani 1 1 d . . . H16 H 1.1741 0.0720 0.2974 0.053 Uiso 1 1 calc R . . C14 C 1.0078(3) 0.1184(3) 0.3227(3) 0.0377(12) Uani 1 1 d . . . C15 C 1.0701(4) 0.0567(3) 0.4848(3) 0.0457(15) Uani 1 1 d . . . C16 C 1.0268(5) 0.0640(3) 0.5461(3) 0.0483(16) Uani 1 1 d . . . C17 C 1.0590(6) 0.0397(4) 0.6094(4) 0.062(2) Uani 1 1 d . . . H17 H 1.1125 0.0171 0.6172 0.075 Uiso 1 1 calc R . . C18 C 1.0107(6) 0.0492(4) 0.6621(4) 0.068(2) Uani 1 1 d . . . H18 H 1.0314 0.0340 0.7064 0.081 Uiso 1 1 calc R . . C19 C 0.9340(6) 0.0803(4) 0.6500(4) 0.066(2) Uani 1 1 d . . . H19 H 0.9002 0.0856 0.6856 0.079 Uiso 1 1 calc R . . C20 C 0.9061(5) 0.1040(4) 0.5842(3) 0.0565(19) Uani 1 1 d . . . H20 H 0.8527 0.1264 0.5755 0.068 Uiso 1 1 calc R . . C21 C 0.8748(5) 0.4938(4) 0.5708(4) 0.060(2) Uani 1 1 d . . . H21 H 0.8481 0.4613 0.5998 0.073 Uiso 1 1 calc R . . C22 C 0.9297(5) 0.5163(4) 0.5985(4) 0.061(2) Uani 1 1 d . . . H22 H 0.9419 0.4979 0.6451 0.073 Uiso 1 1 calc R . . C23 C 0.9648(5) 0.5651(4) 0.5566(4) 0.060(2) Uani 1 1 d . . . H23 H 1.0011 0.5820 0.5743 0.072 Uiso 1 1 calc R . . C24 C 0.9484(5) 0.5906(4) 0.4882(4) 0.0533(17) Uani 1 1 d . . . H24 H 0.9732 0.6246 0.4590 0.064 Uiso 1 1 calc R . . C25 C 0.8953(4) 0.5656(3) 0.4636(3) 0.0445(15) Uani 1 1 d . . . C26 C 0.8758(4) 0.5874(3) 0.3917(3) 0.0458(15) Uani 1 1 d . . . C27 C 0.9027(4) 0.6990(3) 0.2370(3) 0.0387(13) Uani 1 1 d . . . C28 C 0.9606(4) 0.7378(3) 0.2434(3) 0.0410(14) Uani 1 1 d . . . C29 C 1.0309(4) 0.6986(4) 0.2762(3) 0.0496(16) Uani 1 1 d . . . H25 H 1.0395 0.6491 0.2954 0.060 Uiso 1 1 calc R . . C30 C 1.0879(5) 0.7320(4) 0.2807(4) 0.060(2) Uani 1 1 d . . . H26 H 1.1360 0.7053 0.3026 0.072 Uiso 1 1 calc R . . C31 C 1.0750(5) 0.8044(5) 0.2531(4) 0.067(2) Uani 1 1 d . . . H27 H 1.1143 0.8273 0.2562 0.080 Uiso 1 1 calc R . . C32 C 1.0045(5) 0.8438(4) 0.2210(4) 0.0603(19) Uani 1 1 d . . . H28 H 0.9953 0.8934 0.2027 0.072 Uiso 1 1 calc R . . C33 C 0.9487(4) 0.8105(4) 0.2158(3) 0.0464(15) Uani 1 1 d . . . H29 H 0.9011 0.8373 0.1930 0.056 Uiso 1 1 calc R . . C34 C 0.8662(3) 0.7096(3) 0.1716(3) 0.0349(12) Uani 1 1 d . . . C35 C 0.8142(4) 0.8215(3) 0.0151(3) 0.0373(12) Uani 1 1 d . . . C36 C 0.7663(4) 0.8137(4) -0.0359(3) 0.0480(15) Uani 1 1 d . . . C37 C 0.7456(5) 0.8645(4) -0.0980(3) 0.0571(19) Uani 1 1 d . . . H30 H 0.7616 0.9074 -0.1105 0.068 Uiso 1 1 calc R . . C38 C 0.7010(5) 0.8505(4) -0.1413(4) 0.066(2) Uani 1 1 d . . . H31 H 0.6859 0.8841 -0.1841 0.080 Uiso 1 1 calc R . . C39 C 0.6784(5) 0.7876(4) -0.1220(4) 0.066(2) Uani 1 1 d . . . H32 H 0.6481 0.7776 -0.1516 0.079 Uiso 1 1 calc R . . C40 C 0.7004(4) 0.7391(4) -0.0589(4) 0.0514(16) Uani 1 1 d . . . H33 H 0.6843 0.6962 -0.0451 0.062 Uiso 1 1 calc R . . C41 C 0.5511(4) 0.2572(4) 0.4215(4) 0.0547(17) Uani 1 1 d . . . H34 H 0.5187 0.3016 0.4197 0.066 Uiso 1 1 calc R . . C42 C 0.5183(5) 0.2038(5) 0.4245(4) 0.067(2) Uani 1 1 d . . . H35 H 0.4633 0.2114 0.4255 0.081 Uiso 1 1 calc R . . C43 C 0.5617(5) 0.1395(5) 0.4259(4) 0.066(2) Uani 1 1 d . . . H36 H 0.5379 0.1028 0.4271 0.079 Uiso 1 1 calc R . . C44 C 0.6428(4) 0.1292(4) 0.4255(4) 0.0552(17) Uani 1 1 d . . . H37 H 0.6755 0.0852 0.4265 0.066 Uiso 1 1 calc R . . C45 C 0.6736(4) 0.1844(4) 0.4236(3) 0.0440(14) Uani 1 1 d . . . C46 C 0.7590(4) 0.1781(3) 0.4253(3) 0.0407(13) Uani 1 1 d . . . C47 C 0.8819(4) 0.2777(3) 0.4470(3) 0.0430(14) Uani 1 1 d . . . C48 C 0.9656(4) 0.2577(3) 0.4688(3) 0.0442(14) Uani 1 1 d . . . C49 C 0.9815(5) 0.2559(4) 0.5337(4) 0.060(2) Uani 1 1 d . . . H38 H 0.9407 0.2717 0.5603 0.072 Uiso 1 1 calc R . . C50 C 1.0566(6) 0.2312(4) 0.5585(5) 0.067(2) Uani 1 1 d . . . H39 H 1.0674 0.2273 0.6033 0.081 Uiso 1 1 calc R . . C51 C 1.1157(5) 0.2123(4) 0.5182(5) 0.072(3) Uani 1 1 d . . . H40 H 1.1675 0.1957 0.5354 0.086 Uiso 1 1 calc R . . C52 C 1.1013(4) 0.2171(4) 0.4542(5) 0.064(2) Uani 1 1 d . . . H41 H 1.1432 0.2058 0.4263 0.076 Uiso 1 1 calc R . . C53 C 1.0252(4) 0.2384(3) 0.4290(4) 0.0524(17) Uani 1 1 d . . . H42 H 1.0148 0.2396 0.3850 0.063 Uiso 1 1 calc R . . C54 C 0.8382(4) 0.3493(3) 0.4436(3) 0.0467(15) Uani 1 1 d . . . C55 C 0.6551(4) 0.4487(3) 0.4283(3) 0.0486(16) Uani 1 1 d . . . C56 C 0.6232(4) 0.5172(3) 0.4407(3) 0.0506(18) Uani 1 1 d . . . C57 C 0.5466(5) 0.5502(4) 0.4364(4) 0.060(2) Uani 1 1 d . . . H43 H 0.5091 0.5293 0.4258 0.072 Uiso 1 1 calc R . . C58 C 0.5232(6) 0.6149(4) 0.4477(4) 0.068(2) Uani 1 1 d . . . H44 H 0.4701 0.6392 0.4444 0.081 Uiso 1 1 calc R . . C59 C 0.5790(6) 0.6416(4) 0.4636(4) 0.075(3) Uani 1 1 d . . . H45 H 0.5653 0.6854 0.4717 0.090 Uiso 1 1 calc R . . C60 C 0.6553(6) 0.6057(4) 0.4678(4) 0.068(2) Uani 1 1 d . . . H46 H 0.6933 0.6256 0.4791 0.082 Uiso 1 1 calc R . . C61 C 0.5358(4) 0.3933(4) 0.2539(3) 0.0475(16) Uani 1 1 d . . . H47 H 0.5102 0.4397 0.2523 0.057 Uiso 1 1 calc R . . C62 C 0.4907(4) 0.3457(4) 0.2515(3) 0.0517(17) Uani 1 1 d . . . H48 H 0.4356 0.3601 0.2483 0.062 Uiso 1 1 calc R . . C63 C 0.5286(4) 0.2781(4) 0.2541(4) 0.0502(16) Uani 1 1 d . . . H49 H 0.4997 0.2454 0.2534 0.060 Uiso 1 1 calc R . . C64 C 0.6081(4) 0.2588(4) 0.2578(3) 0.0442(14) Uani 1 1 d . . . H50 H 0.6351 0.2129 0.2589 0.053 Uiso 1 1 calc R . . C65 C 0.6489(3) 0.3085(3) 0.2600(3) 0.0358(12) Uani 1 1 d . . . C66 C 0.7347(3) 0.2914(3) 0.2635(3) 0.0357(12) Uani 1 1 d . . . C67 C 0.8788(4) 0.3807(3) 0.2578(3) 0.0405(13) Uani 1 1 d . . . C68 C 0.9652(4) 0.3594(3) 0.2531(3) 0.0412(13) Uani 1 1 d . . . C69 C 0.9970(4) 0.3241(4) 0.2076(4) 0.0509(16) Uani 1 1 d . . . H51 H 0.9636 0.3155 0.1794 0.061 Uiso 1 1 calc R . . C70 C 1.0781(4) 0.3014(4) 0.2036(5) 0.063(2) Uani 1 1 d . . . H52 H 1.0994 0.2770 0.1731 0.076 Uiso 1 1 calc R . . C71 C 1.1268(5) 0.3145(5) 0.2440(5) 0.071(2) Uani 1 1 d . . . H53 H 1.1815 0.2995 0.2413 0.086 Uiso 1 1 calc R . . C72 C 1.0950(5) 0.3499(5) 0.2887(5) 0.069(2) Uani 1 1 d . . . H54 H 1.1286 0.3584 0.3168 0.082 Uiso 1 1 calc R . . C73 C 1.0152(4) 0.3730(4) 0.2932(4) 0.0517(17) Uani 1 1 d . . . H55 H 0.9946 0.3980 0.3234 0.062 Uiso 1 1 calc R . . C74 C 0.8457(4) 0.4543(3) 0.2586(3) 0.0375(12) Uani 1 1 d . . . C75 C 0.6667(4) 0.5630(3) 0.2622(3) 0.0445(15) Uani 1 1 d . . . C76 C 0.6398(4) 0.6344(4) 0.2695(4) 0.0500(16) Uani 1 1 d . . . C77 C 0.5615(5) 0.6669(4) 0.2714(5) 0.069(2) Uani 1 1 d . . . H56 H 0.5218 0.6444 0.2684 0.083 Uiso 1 1 calc R . . C78 C 0.5435(6) 0.7340(5) 0.2781(6) 0.081(3) Uani 1 1 d . . . H57 H 0.4908 0.7577 0.2799 0.097 Uiso 1 1 calc R . . C79 C 0.6012(6) 0.7650(5) 0.2819(5) 0.080(3) Uani 1 1 d . . . H58 H 0.5888 0.8106 0.2859 0.096 Uiso 1 1 calc R . . C80 C 0.6786(5) 0.7303(4) 0.2799(4) 0.062(2) Uani 1 1 d . . . H59 H 0.7188 0.7522 0.2829 0.075 Uiso 1 1 calc R . . C81 C 0.4436(4) 0.6149(4) 0.1097(4) 0.0532(17) Uani 1 1 d . . . H60 H 0.4274 0.5749 0.1086 0.064 Uiso 1 1 calc R . . C82 C 0.3891(4) 0.6723(5) 0.1162(5) 0.073(3) Uani 1 1 d . . . H61 H 0.3359 0.6707 0.1212 0.088 Uiso 1 1 calc R . . C83 C 0.4109(5) 0.7317(4) 0.1156(6) 0.078(3) Uani 1 1 d . . . H62 H 0.3732 0.7720 0.1181 0.093 Uiso 1 1 calc R . . C84 C 0.4891(4) 0.7314(4) 0.1113(4) 0.0576(19) Uani 1 1 d . . . H63 H 0.5059 0.7714 0.1116 0.069 Uiso 1 1 calc R . . C85 C 0.5425(4) 0.6724(3) 0.1065(4) 0.0453(15) Uani 1 1 d . . . C86 C 0.6275(3) 0.6682(3) 0.1029(3) 0.0395(13) Uani 1 1 d . . . C87 C 0.7945(3) 0.5465(3) 0.0808(3) 0.0315(11) Uani 1 1 d . . . C88 C 0.8759(3) 0.5521(3) 0.0646(3) 0.0365(12) Uani 1 1 d . . . C89 C 0.8921(4) 0.6076(3) 0.0115(3) 0.0415(13) Uani 1 1 d . . . H64 H 0.8509 0.6426 -0.0150 0.050 Uiso 1 1 calc R . . C90 C 0.9684(4) 0.6118(4) -0.0027(3) 0.0497(16) Uani 1 1 d . . . H65 H 0.9790 0.6499 -0.0389 0.060 Uiso 1 1 calc R . . C91 C 1.0289(4) 0.5615(4) 0.0349(4) 0.0506(16) Uani 1 1 d . . . H66 H 1.0810 0.5648 0.0248 0.061 Uiso 1 1 calc R . . C92 C 1.0130(4) 0.5058(4) 0.0877(3) 0.0472(15) Uani 1 1 d . . . H67 H 1.0544 0.4711 0.1143 0.057 Uiso 1 1 calc R . . C93 C 0.9373(3) 0.5006(3) 0.1018(3) 0.0405(13) Uani 1 1 d . . . H68 H 0.9270 0.4616 0.1371 0.049 Uiso 1 1 calc R . . C94 C 0.7757(3) 0.4772(3) 0.0886(3) 0.0355(12) Uani 1 1 d . . . C95 C 0.6217(3) 0.4069(3) 0.0959(3) 0.0354(12) Uani 1 1 d . . . C96 C 0.6160(3) 0.3431(3) 0.0816(3) 0.0379(13) Uani 1 1 d . . . C97 C 0.5486(4) 0.3229(4) 0.0806(4) 0.0463(15) Uani 1 1 d . . . H69 H 0.5002 0.3511 0.0878 0.056 Uiso 1 1 calc R . . C98 C 0.5524(5) 0.2584(4) 0.0685(5) 0.061(2) Uani 1 1 d . . . H70 H 0.5065 0.2431 0.0669 0.073 Uiso 1 1 calc R . . C99 C 0.6241(4) 0.2189(5) 0.0590(5) 0.068(2) Uani 1 1 d . . . H71 H 0.6292 0.1749 0.0524 0.082 Uiso 1 1 calc R . . C100 C 0.6879(4) 0.2450(4) 0.0595(4) 0.0556(18) Uani 1 1 d . . . H72 H 0.7370 0.2182 0.0517 0.067 Uiso 1 1 calc R . . C101 C 0.3161(7) 0.7744(6) 0.3191(5) 0.082(3) Uani 1 1 d . . . C102 C 0.3262(11) 0.5279(11) 0.2910(7) 0.145(6) Uani 1 1 d . . . C103 C 0.7275(5) 0.5807(4) -0.1335(4) 0.0557(18) Uani 1 1 d . . . C104 C 0.538(2) 0.068(2) 0.2380(19) 0.257(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0338(3) 0.0307(4) 0.0356(4) -0.0085(3) -0.0046(3) -0.0043(3) Cu2 0.0399(4) 0.0488(5) 0.0331(4) -0.0089(3) -0.0043(3) 0.0080(3) Cu3 0.0498(4) 0.0332(4) 0.0355(4) -0.0069(3) -0.0016(3) 0.0031(3) Cu4 0.0684(5) 0.0302(4) 0.0414(4) -0.0097(3) 0.0052(4) -0.0051(4) Cu5 0.0611(5) 0.0361(4) 0.0339(4) -0.0077(3) 0.0008(3) -0.0121(4) Cu6 0.0460(4) 0.0313(4) 0.0335(4) -0.0040(3) -0.0039(3) -0.0132(3) Cu7 0.0503(4) 0.0348(4) 0.0377(4) -0.0059(3) -0.0040(3) 0.0009(3) Cu8 0.0399(4) 0.0340(4) 0.0339(4) -0.0042(3) -0.0015(3) -0.0029(3) Cu9 0.0336(3) 0.0297(4) 0.0404(4) -0.0069(3) -0.0007(3) -0.0058(3) S1 0.074(2) 0.0454(18) 0.0550(19) -0.0146(14) -0.0066(19) 0.0057(18) O14 0.099(8) 0.105(9) 0.101(8) -0.058(7) -0.044(7) 0.023(7) O15 0.188(16) 0.053(7) 0.073(8) -0.014(6) 0.045(10) -0.056(9) S2 0.078(5) 0.043(3) 0.056(4) -0.014(3) -0.017(4) 0.010(3) O16 0.065(10) 0.054(10) 0.042(8) 0.010(7) -0.007(8) 0.019(9) O17 0.083(12) 0.045(9) 0.097(14) -0.003(9) -0.012(11) -0.024(9) S3 0.0780(15) 0.0670(14) 0.0813(15) -0.0271(12) 0.0162(12) -0.0118(12) S4 0.0371(7) 0.0411(8) 0.0345(7) -0.0076(6) -0.0037(6) -0.0077(6) F1 0.165(7) 0.095(5) 0.072(4) -0.035(3) 0.013(4) -0.034(5) F2 0.102(5) 0.118(6) 0.118(5) 0.007(4) 0.039(4) -0.029(4) F3 0.079(4) 0.223(10) 0.137(7) -0.034(7) -0.034(4) -0.021(5) F4 0.147(8) 0.54(2) 0.271(13) -0.342(17) 0.093(8) -0.172(12) F5 0.075(4) 0.244(11) 0.084(5) -0.029(6) -0.012(4) 0.009(6) F6 0.123(6) 0.297(14) 0.223(10) -0.178(10) 0.096(7) -0.134(8) F7 0.100(4) 0.137(5) 0.089(4) -0.072(4) 0.055(3) -0.068(4) F8 0.109(4) 0.079(4) 0.064(3) -0.002(3) 0.009(3) -0.053(3) F9 0.055(3) 0.135(5) 0.099(4) -0.058(4) 0.000(3) -0.047(3) O1 0.040(2) 0.038(2) 0.032(2) -0.0079(18) -0.0044(17) 0.0057(18) O2 0.037(2) 0.037(2) 0.034(2) -0.0067(17) -0.0051(17) 0.0042(17) O3 0.078(3) 0.040(3) 0.033(2) -0.0097(19) 0.003(2) -0.015(2) O4 0.059(3) 0.033(2) 0.033(2) -0.0026(17) -0.0056(19) -0.0174(19) O5 0.054(3) 0.028(2) 0.053(3) -0.0083(19) -0.005(2) -0.0092(19) O6 0.062(3) 0.035(2) 0.052(3) -0.015(2) 0.000(2) -0.010(2) O7 0.041(2) 0.028(2) 0.042(2) -0.0080(17) -0.0014(18) -0.0053(17) O8 0.059(3) 0.039(2) 0.047(3) -0.012(2) -0.005(2) -0.014(2) O9 0.043(2) 0.034(2) 0.058(3) -0.016(2) 0.002(2) -0.0084(19) O10 0.039(2) 0.032(2) 0.041(2) -0.0108(17) -0.0005(17) -0.0095(17) O11 0.151(8) 0.081(6) 0.136(8) -0.032(5) -0.033(6) -0.001(5) O13 0.107(6) 0.049(4) 0.135(7) -0.022(4) 0.006(5) 0.004(4) O18 0.067(4) 0.066(4) 0.109(5) -0.011(4) 0.026(4) -0.006(3) O19 0.082(5) 0.114(6) 0.098(5) -0.046(5) 0.026(4) -0.002(4) O20 0.157(8) 0.071(5) 0.097(6) -0.016(4) 0.039(5) -0.003(5) O21 0.036(2) 0.062(3) 0.052(3) -0.014(2) -0.004(2) -0.014(2) O22 0.053(3) 0.045(3) 0.043(2) -0.014(2) 0.000(2) -0.009(2) O23 0.070(3) 0.048(3) 0.047(3) -0.007(2) -0.003(2) 0.011(2) N1 0.033(2) 0.029(2) 0.034(2) -0.0047(19) -0.0004(19) -0.0050(19) N2 0.043(3) 0.037(3) 0.034(2) -0.010(2) 0.003(2) -0.006(2) N3 0.041(3) 0.030(2) 0.031(2) -0.0103(19) 0.001(2) -0.002(2) N4 0.039(3) 0.031(2) 0.039(3) -0.012(2) -0.005(2) 0.001(2) N5 0.048(3) 0.026(2) 0.032(2) -0.0025(19) -0.009(2) -0.003(2) N6 0.054(3) 0.042(3) 0.057(3) -0.011(3) -0.026(3) 0.006(3) N7 0.070(4) 0.036(3) 0.033(3) -0.010(2) -0.003(3) -0.007(3) N8 0.085(4) 0.027(3) 0.036(3) -0.007(2) 0.002(3) -0.010(3) N9 0.069(4) 0.037(3) 0.030(3) -0.007(2) -0.011(2) -0.008(3) N10 0.061(3) 0.030(3) 0.034(3) -0.008(2) -0.003(2) -0.008(2) N11 0.044(3) 0.035(3) 0.030(2) -0.005(2) -0.007(2) -0.011(2) N12 0.047(3) 0.034(3) 0.030(2) -0.006(2) -0.003(2) -0.012(2) N13 0.076(4) 0.033(3) 0.042(3) 0.005(2) -0.014(3) -0.027(3) N14 0.051(3) 0.038(3) 0.042(3) -0.006(2) -0.006(2) -0.016(2) N15 0.051(3) 0.046(3) 0.032(3) -0.007(2) -0.008(2) 0.003(2) N16 0.049(3) 0.028(2) 0.036(3) -0.005(2) 0.002(2) -0.006(2) N17 0.045(3) 0.032(3) 0.033(2) -0.007(2) -0.001(2) -0.004(2) N18 0.060(3) 0.029(3) 0.046(3) -0.011(2) 0.006(3) 0.005(2) N19 0.056(3) 0.037(3) 0.049(3) -0.014(2) -0.004(3) 0.008(2) N20 0.051(3) 0.046(3) 0.047(3) -0.001(3) -0.009(3) 0.004(3) N21 0.076(4) 0.037(3) 0.040(3) -0.009(2) 0.010(3) -0.011(3) N22 0.044(3) 0.034(3) 0.035(3) 0.001(2) -0.010(2) 0.002(2) N23 0.045(3) 0.029(2) 0.033(2) -0.006(2) -0.003(2) -0.001(2) N24 0.034(2) 0.038(3) 0.030(2) -0.006(2) -0.0029(19) -0.004(2) N25 0.060(3) 0.026(2) 0.035(3) -0.004(2) -0.006(2) -0.002(2) N26 0.057(3) 0.032(3) 0.039(3) -0.008(2) -0.003(2) -0.002(2) N27 0.049(3) 0.036(3) 0.043(3) -0.009(2) 0.004(2) -0.005(2) N28 0.069(4) 0.032(3) 0.047(3) -0.010(2) 0.008(3) -0.007(3) N29 0.038(3) 0.032(3) 0.060(3) -0.008(2) 0.007(2) -0.005(2) N30 0.033(2) 0.030(2) 0.035(2) -0.006(2) -0.0008(19) -0.0032(19) N31 0.036(2) 0.033(3) 0.037(3) -0.006(2) -0.002(2) -0.007(2) N32 0.040(3) 0.031(2) 0.030(2) -0.0049(19) -0.0032(19) -0.009(2) N33 0.030(2) 0.025(2) 0.036(2) -0.0079(19) -0.0016(19) -0.0045(18) N34 0.035(2) 0.038(3) 0.041(3) -0.008(2) 0.001(2) -0.012(2) N35 0.039(3) 0.034(3) 0.049(3) -0.009(2) -0.005(2) -0.010(2) C1 0.045(3) 0.043(3) 0.036(3) -0.005(3) -0.012(3) -0.008(3) C2 0.047(3) 0.053(4) 0.038(3) -0.009(3) -0.002(3) -0.007(3) C3 0.050(4) 0.064(5) 0.050(4) -0.028(4) 0.006(3) -0.015(3) C4 0.041(3) 0.044(4) 0.043(3) -0.013(3) -0.002(3) -0.007(3) C5 0.042(3) 0.032(3) 0.036(3) -0.010(2) 0.000(2) -0.011(2) C6 0.033(3) 0.034(3) 0.042(3) -0.007(3) -0.008(2) -0.005(2) C7 0.040(3) 0.029(3) 0.038(3) -0.007(2) -0.008(2) -0.003(2) C8 0.038(3) 0.029(3) 0.034(3) -0.001(2) -0.003(2) 0.002(2) C9 0.056(4) 0.026(3) 0.046(3) -0.006(3) 0.004(3) -0.009(3) C10 0.069(5) 0.037(3) 0.045(4) -0.018(3) 0.011(3) -0.005(3) C11 0.055(4) 0.035(3) 0.053(4) -0.004(3) 0.017(3) 0.010(3) C12 0.048(4) 0.040(4) 0.051(4) -0.005(3) 0.011(3) 0.003(3) C13 0.040(3) 0.043(3) 0.040(3) -0.009(3) 0.002(3) 0.002(3) C14 0.040(3) 0.032(3) 0.040(3) -0.010(2) -0.007(2) -0.006(2) C15 0.059(4) 0.022(3) 0.052(4) -0.005(3) -0.014(3) -0.009(3) C16 0.075(5) 0.026(3) 0.045(4) -0.010(3) -0.006(3) -0.015(3) C17 0.093(6) 0.052(4) 0.040(4) -0.002(3) -0.017(4) -0.028(4) C18 0.117(8) 0.058(5) 0.040(4) -0.011(3) -0.010(4) -0.045(5) C19 0.115(8) 0.044(4) 0.039(4) -0.011(3) 0.009(4) -0.029(5) C20 0.094(6) 0.036(4) 0.040(4) -0.011(3) 0.013(4) -0.021(4) C21 0.084(6) 0.050(4) 0.040(4) -0.010(3) 0.001(4) -0.009(4) C22 0.095(6) 0.043(4) 0.039(4) -0.010(3) -0.022(4) -0.002(4) C23 0.092(6) 0.051(4) 0.040(4) -0.014(3) -0.010(4) -0.018(4) C24 0.079(5) 0.038(3) 0.046(4) -0.020(3) 0.000(3) -0.011(3) C25 0.064(4) 0.027(3) 0.040(3) -0.006(2) -0.005(3) -0.009(3) C26 0.069(4) 0.028(3) 0.036(3) -0.009(2) 0.000(3) -0.004(3) C27 0.047(3) 0.035(3) 0.030(3) -0.008(2) -0.004(2) -0.007(3) C28 0.052(4) 0.040(3) 0.031(3) -0.010(2) -0.011(3) -0.009(3) C29 0.062(4) 0.040(4) 0.044(4) -0.012(3) -0.015(3) -0.005(3) C30 0.058(4) 0.064(5) 0.062(5) -0.029(4) -0.022(4) -0.002(4) C31 0.068(5) 0.071(6) 0.073(5) -0.033(5) -0.014(4) -0.022(4) C32 0.070(5) 0.048(4) 0.068(5) -0.027(4) -0.006(4) -0.010(4) C33 0.060(4) 0.045(4) 0.037(3) -0.016(3) -0.008(3) -0.012(3) C34 0.042(3) 0.030(3) 0.032(3) -0.010(2) 0.000(2) -0.007(2) C35 0.044(3) 0.034(3) 0.035(3) -0.009(2) 0.002(2) -0.013(2) C36 0.064(4) 0.045(4) 0.035(3) -0.008(3) -0.009(3) -0.017(3) C37 0.079(5) 0.043(4) 0.042(4) 0.007(3) -0.011(3) -0.028(4) C38 0.083(6) 0.058(5) 0.047(4) 0.010(3) -0.020(4) -0.028(4) C39 0.085(6) 0.056(5) 0.054(4) -0.007(4) -0.026(4) -0.020(4) C40 0.061(4) 0.044(4) 0.049(4) -0.010(3) -0.013(3) -0.016(3) C41 0.047(4) 0.059(5) 0.048(4) -0.007(3) -0.004(3) -0.006(3) C42 0.044(4) 0.081(6) 0.062(5) -0.014(4) -0.006(3) 0.003(4) C43 0.058(5) 0.070(6) 0.071(5) -0.016(4) -0.006(4) -0.026(4) C44 0.055(4) 0.052(4) 0.054(4) -0.008(3) -0.006(3) -0.016(3) C45 0.048(3) 0.045(4) 0.033(3) -0.009(3) -0.004(3) -0.005(3) C46 0.049(3) 0.032(3) 0.036(3) -0.006(2) 0.002(3) -0.007(3) C47 0.057(4) 0.029(3) 0.039(3) -0.009(2) 0.004(3) -0.006(3) C48 0.053(4) 0.026(3) 0.052(4) -0.009(3) -0.007(3) -0.008(3) C49 0.090(6) 0.030(3) 0.056(4) -0.010(3) -0.019(4) -0.009(3) C50 0.089(6) 0.044(4) 0.068(5) -0.008(4) -0.023(5) -0.022(4) C51 0.059(5) 0.050(5) 0.091(7) 0.001(4) -0.032(5) -0.007(4) C52 0.049(4) 0.036(4) 0.097(6) -0.010(4) -0.001(4) -0.008(3) C53 0.057(4) 0.030(3) 0.066(4) -0.008(3) 0.009(3) -0.013(3) C54 0.063(4) 0.031(3) 0.040(3) -0.006(3) 0.004(3) -0.008(3) C55 0.065(4) 0.030(3) 0.040(3) -0.001(3) -0.003(3) -0.005(3) C56 0.061(4) 0.030(3) 0.037(3) 0.003(3) 0.010(3) 0.011(3) C57 0.071(5) 0.041(4) 0.051(4) 0.001(3) 0.009(4) -0.004(3) C58 0.079(6) 0.047(4) 0.059(5) -0.007(4) 0.010(4) 0.003(4) C59 0.104(7) 0.042(4) 0.059(5) -0.009(4) 0.024(5) 0.004(5) C60 0.088(6) 0.040(4) 0.066(5) -0.020(4) 0.011(4) 0.006(4) C61 0.042(3) 0.056(4) 0.034(3) -0.009(3) 0.002(3) 0.000(3) C62 0.040(3) 0.063(5) 0.042(4) -0.006(3) -0.004(3) -0.007(3) C63 0.038(3) 0.058(4) 0.051(4) -0.014(3) -0.008(3) -0.009(3) C64 0.049(4) 0.041(3) 0.039(3) -0.011(3) -0.002(3) -0.007(3) C65 0.036(3) 0.034(3) 0.032(3) -0.004(2) -0.002(2) -0.004(2) C66 0.041(3) 0.032(3) 0.025(3) 0.000(2) -0.004(2) -0.005(2) C67 0.049(3) 0.033(3) 0.034(3) -0.003(2) -0.004(3) -0.008(3) C68 0.043(3) 0.030(3) 0.045(3) -0.003(3) -0.006(3) -0.008(2) C69 0.045(4) 0.045(4) 0.059(4) -0.016(3) 0.001(3) -0.007(3) C70 0.048(4) 0.054(5) 0.086(6) -0.021(4) 0.010(4) -0.012(3) C71 0.048(4) 0.056(5) 0.093(7) 0.000(5) 0.001(4) -0.015(4) C72 0.047(4) 0.067(5) 0.080(6) 0.001(4) -0.031(4) -0.017(4) C73 0.054(4) 0.043(4) 0.050(4) 0.001(3) -0.012(3) -0.017(3) C74 0.044(3) 0.033(3) 0.032(3) -0.006(2) -0.002(2) -0.010(2) C75 0.054(4) 0.034(3) 0.035(3) -0.002(3) 0.006(3) -0.004(3) C76 0.055(4) 0.034(3) 0.050(4) -0.006(3) 0.010(3) -0.004(3) C77 0.063(5) 0.051(5) 0.086(6) -0.018(4) 0.021(4) -0.009(4) C78 0.073(6) 0.049(5) 0.108(8) -0.021(5) 0.021(5) -0.005(4) C79 0.088(6) 0.047(5) 0.109(8) -0.028(5) 0.032(6) -0.025(4) C80 0.078(5) 0.038(4) 0.070(5) -0.020(4) 0.017(4) -0.011(4) C81 0.039(3) 0.044(4) 0.074(5) -0.015(3) 0.001(3) -0.009(3) C82 0.037(4) 0.057(5) 0.118(8) -0.024(5) 0.027(4) -0.011(3) C83 0.046(4) 0.047(4) 0.138(9) -0.033(5) 0.019(5) -0.008(3) C84 0.047(4) 0.039(4) 0.084(5) -0.017(4) 0.009(4) -0.010(3) C85 0.044(3) 0.033(3) 0.056(4) -0.008(3) 0.005(3) -0.013(3) C86 0.038(3) 0.037(3) 0.037(3) -0.005(2) -0.002(2) -0.005(2) C87 0.032(3) 0.030(3) 0.033(3) -0.008(2) -0.005(2) -0.009(2) C88 0.038(3) 0.037(3) 0.038(3) -0.013(2) 0.003(2) -0.014(2) C89 0.041(3) 0.045(4) 0.038(3) -0.010(3) 0.003(3) -0.015(3) C90 0.054(4) 0.061(4) 0.046(4) -0.020(3) 0.017(3) -0.033(3) C91 0.041(3) 0.065(5) 0.060(4) -0.033(4) 0.007(3) -0.021(3) C92 0.033(3) 0.064(4) 0.047(4) -0.023(3) -0.005(3) -0.009(3) C93 0.036(3) 0.043(3) 0.040(3) -0.011(3) -0.001(2) -0.009(3) C94 0.039(3) 0.029(3) 0.035(3) -0.007(2) 0.000(2) -0.006(2) C95 0.033(3) 0.037(3) 0.030(3) -0.003(2) 0.002(2) -0.009(2) C96 0.040(3) 0.040(3) 0.033(3) -0.009(2) -0.012(2) -0.009(3) C97 0.038(3) 0.045(4) 0.056(4) -0.016(3) -0.002(3) -0.009(3) C98 0.057(4) 0.052(4) 0.087(6) -0.031(4) 0.000(4) -0.026(4) C99 0.049(4) 0.058(5) 0.112(7) -0.046(5) 0.006(4) -0.015(4) C100 0.046(4) 0.038(4) 0.090(6) -0.031(4) -0.001(4) -0.007(3) C101 0.100(7) 0.072(6) 0.057(5) 0.007(5) -0.006(5) -0.025(6) C102 0.167(15) 0.193(17) 0.068(7) -0.068(10) 0.039(9) -0.006(13) C103 0.059(4) 0.063(5) 0.049(4) -0.019(4) 0.010(3) -0.023(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 N33 1.877(5) . ? Cu1 N1 1.985(5) . ? Cu1 O10 2.036(4) . ? Cu1 N35 2.086(5) . ? Cu1 O1 2.318(4) . ? Cu2 N3 1.918(5) . ? Cu2 O7 1.939(4) . ? Cu2 O1 2.009(4) . ? Cu2 O2 2.023(4) . ? Cu3 N5 1.899(5) . ? Cu3 N7 2.022(5) . ? Cu3 O2 2.039(4) . ? Cu3 N17 2.043(5) . ? Cu3 O5 2.167(5) . ? Cu4 N19 1.873(6) . ? Cu4 N8 1.991(6) . ? Cu4 O6 2.070(5) . ? Cu4 N21 2.115(6) . ? Cu4 O3 2.211(5) . ? Cu5 N26 1.893(6) . ? Cu5 N10 1.931(6) . ? Cu5 O3 2.091(4) . ? Cu5 O4 2.165(4) . ? Cu5 N28 2.202(6) . ? Cu5 O8 2.341(5) . ? Cu6 N12 1.904(5) . ? Cu6 O4 1.994(4) . ? Cu6 N31 2.015(5) . ? Cu6 N14 2.052(5) . ? Cu6 O9 2.246(4) . ? Cu7 N18 1.925(6) . ? Cu7 N16 1.946(5) . ? Cu7 N20 1.977(6) . ? Cu7 N15 1.980(6) . ? Cu8 N25 1.925(6) . ? Cu8 N23 1.942(5) . ? Cu8 N27 1.959(5) . ? Cu8 N22 1.970(6) . ? Cu9 N32 1.917(5) . ? Cu9 N30 1.941(5) . ? Cu9 N34 1.951(5) . ? Cu9 N29 1.988(5) . ? S1 O14 1.368(13) . ? S1 O13 1.404(7) . ? S1 O15 1.486(12) . ? S1 C101 1.847(11) . ? S2 O17 1.44(2) . ? S2 O16 1.468(16) . ? S2 O13 1.535(10) . ? S2 C101 1.777(13) . ? S3 O19 1.395(7) . ? S3 O20 1.452(8) . ? S3 O18 1.455(7) . ? S3 C102 1.636(19) . ? S4 O21 1.437(5) . ? S4 O23 1.440(5) . ? S4 O22 1.447(5) . ? S4 C103 1.815(8) . ? S5 O24 1.466(15) . ? S5 O26 1.545(13) . ? S5 O25 1.571(19) . ? S5 C104 1.73(4) . ? S6 O28 1.337(14) . ? S6 O29 1.450(14) . ? S6 C105 1.685(15) . ? S6 O27 1.691(12) . ? C105 F14 1.347(16) . ? C105 F13 1.380(15) . ? C105 F15 1.392(15) . ? F13 F15 1.74(2) 2_755 ? F15 F13 1.74(2) 2_755 ? S7 O27 1.376(12) . ? S7 O30 1.461(15) . ? S7 O28 1.476(17) . ? S7 C106 1.706(17) . ? C106 F16 1.365(17) . ? C106 F17 1.371(17) . ? C106 F18 1.385(17) . ? F1 C101 1.305(12) . ? F2 C101 1.310(11) . ? F3 C101 1.300(12) . ? F4 C102 1.335(14) . ? F5 C102 1.395(19) . ? F6 C102 1.405(19) . ? F7 C103 1.327(9) . ? F8 C103 1.312(9) . ? F9 C103 1.340(9) . ? F10 C104 1.36(3) . ? F11 C104 1.38(3) . ? F12 C104 1.36(3) . ? O1 C6 1.294(7) . ? O2 C14 1.343(7) . ? O3 C26 1.313(9) . ? O4 C34 1.314(7) . ? O5 C46 1.255(7) . ? O6 C54 1.284(8) . ? O7 C66 1.256(7) . ? O8 C74 1.273(8) . ? O9 C86 1.232(8) . ? O10 C94 1.269(7) . ? N1 C1 1.330(8) . ? N1 C5 1.369(7) . ? N2 C6 1.300(7) . ? N2 N3 1.376(7) . ? N3 C7 1.286(7) . ? N4 C14 1.289(7) . ? N4 N5 1.385(7) . ? N5 C15 1.318(8) . ? N6 C15 1.321(9) . ? N6 H1 0.8800 . ? N6 H2 0.8800 . ? N7 C20 1.327(9) . ? N7 C16 1.351(9) . ? N8 C21 1.336(9) . ? N8 C25 1.366(9) . ? N9 C26 1.297(9) . ? N9 N10 1.390(7) . ? N10 C27 1.298(8) . ? N11 C34 1.313(7) . ? N11 N12 1.378(7) . ? N12 C35 1.298(7) . ? N13 C35 1.345(8) . ? N13 H3 0.8800 . ? N13 H4 0.8800 . ? N14 C40 1.347(8) . ? N14 C36 1.349(8) . ? N15 C41 1.351(9) . ? N15 C45 1.357(8) . ? N16 C46 1.340(8) . ? N16 N17 1.377(7) . ? N17 C47 1.312(8) . ? N18 C54 1.307(9) . ? N18 N19 1.372(7) . ? N19 C55 1.313(9) . ? N20 C55 1.312(10) . ? N20 H5 0.8800 . ? N21 C60 1.308(9) . ? N21 C56 1.367(10) . ? N22 C61 1.324(8) . ? N22 C65 1.343(8) . ? N23 C66 1.347(8) . ? N23 N24 1.377(7) . ? N24 C67 1.290(8) . ? N25 C74 1.325(8) . ? N25 N26 1.390(7) . ? N26 C75 1.320(9) . ? N27 C75 1.324(9) . ? N27 H6 0.8800 . ? N28 C76 1.340(10) . ? N28 C80 1.355(9) . ? N29 C81 1.339(8) . ? N29 C85 1.361(8) . ? N30 C86 1.356(8) . ? N30 N31 1.375(7) . ? N31 C87 1.307(7) . ? N32 C94 1.326(8) . ? N32 N33 1.394(6) . ? N33 C95 1.327(7) . ? N34 C95 1.316(8) . ? N34 H7 0.8800 . ? N35 C100 1.310(8) . ? N35 C96 1.363(8) . ? C1 C2 1.392(10) . ? C1 H8 0.9500 . ? C2 C3 1.393(10) . ? C2 H9 0.9500 . ? C3 C4 1.374(10) . ? C3 H10 0.9500 . ? C4 C5 1.379(9) . ? C4 H11 0.9500 . ? C5 C6 1.498(8) . ? C7 C8 1.479(8) . ? C7 C14 1.491(9) . ? C8 C13 1.389(8) . ? C8 C9 1.398(9) . ? C9 C10 1.393(9) . ? C9 H12 0.9500 . ? C10 C11 1.383(11) . ? C10 H13 0.9500 . ? C11 C12 1.376(11) . ? C11 H14 0.9500 . ? C12 C13 1.400(9) . ? C12 H15 0.9500 . ? C13 H16 0.9500 . ? C15 C16 1.496(10) . ? C16 C17 1.372(10) . ? C17 C18 1.397(13) . ? C17 H17 0.9500 . ? C18 C19 1.357(13) . ? C18 H18 0.9500 . ? C19 C20 1.391(11) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.406(12) . ? C21 H21 0.9500 . ? C22 C23 1.358(12) . ? C22 H22 0.9500 . ? C23 C24 1.387(10) . ? C23 H23 0.9500 . ? C24 C25 1.379(10) . ? C24 H24 0.9500 . ? C25 C26 1.473(9) . ? C27 C28 1.487(9) . ? C27 C34 1.488(8) . ? C28 C33 1.395(9) . ? C28 C29 1.395(9) . ? C29 C30 1.380(11) . ? C29 H25 0.9500 . ? C30 C31 1.389(12) . ? C30 H26 0.9500 . ? C31 C32 1.394(11) . ? C31 H27 0.9500 . ? C32 C33 1.366(10) . ? C32 H28 0.9500 . ? C33 H29 0.9500 . ? C35 C36 1.486(9) . ? C36 C37 1.390(9) . ? C37 C38 1.386(11) . ? C37 H30 0.9500 . ? C38 C39 1.385(11) . ? C38 H31 0.9500 . ? C39 C40 1.392(10) . ? C39 H32 0.9500 . ? C40 H33 0.9500 . ? C41 C42 1.354(12) . ? C41 H34 0.9500 . ? C42 C43 1.360(12) . ? C42 H35 0.9500 . ? C43 C44 1.404(11) . ? C43 H36 0.9500 . ? C44 C45 1.372(10) . ? C44 H37 0.9500 . ? C45 C46 1.490(9) . ? C47 C54 1.482(9) . ? C47 C48 1.503(9) . ? C48 C53 1.374(10) . ? C48 C49 1.401(10) . ? C49 C50 1.376(12) . ? C49 H38 0.9500 . ? C50 C51 1.373(14) . ? C50 H39 0.9500 . ? C51 C52 1.359(13) . ? C51 H40 0.9500 . ? C52 C53 1.396(11) . ? C52 H41 0.9500 . ? C53 H42 0.9500 . ? C55 C56 1.497(9) . ? C56 C57 1.360(10) . ? C57 C58 1.400(11) . ? C57 H43 0.9500 . ? C58 C59 1.353(14) . ? C58 H44 0.9500 . ? C59 C60 1.371(13) . ? C59 H45 0.9500 . ? C60 H46 0.9500 . ? C61 C62 1.428(11) . ? C61 H47 0.9500 . ? C62 C63 1.385(10) . ? C62 H48 0.9500 . ? C63 C64 1.370(9) . ? C63 H49 0.9500 . ? C64 C65 1.411(9) . ? C64 H50 0.9500 . ? C65 C66 1.478(8) . ? C67 C68 1.497(9) . ? C67 C74 1.503(9) . ? C68 C73 1.398(9) . ? C68 C69 1.403(10) . ? C69 C70 1.410(10) . ? C69 H51 0.9500 . ? C70 C71 1.381(13) . ? C70 H52 0.9500 . ? C71 C72 1.390(14) . ? C71 H53 0.9500 . ? C72 C73 1.390(11) . ? C72 H54 0.9500 . ? C73 H55 0.9500 . ? C75 C76 1.496(9) . ? C76 C77 1.394(11) . ? C77 C78 1.402(12) . ? C77 H56 0.9500 . ? C78 C79 1.354(14) . ? C78 H57 0.9500 . ? C79 C80 1.393(13) . ? C79 H58 0.9500 . ? C80 H59 0.9500 . ? C81 C82 1.380(10) . ? C81 H60 0.9500 . ? C82 C83 1.375(12) . ? C82 H61 0.9500 . ? C83 C84 1.383(10) . ? C83 H62 0.9500 . ? C84 C85 1.384(10) . ? C84 H63 0.9500 . ? C85 C86 1.490(9) . ? C87 C88 1.487(8) . ? C87 C94 1.509(8) . ? C88 C89 1.392(8) . ? C88 C93 1.394(8) . ? C89 C90 1.385(9) . ? C89 H64 0.9500 . ? C90 C91 1.377(11) . ? C90 H65 0.9500 . ? C91 C92 1.391(10) . ? C91 H66 0.9500 . ? C92 C93 1.381(9) . ? C92 H67 0.9500 . ? C93 H68 0.9500 . ? C95 C96 1.480(9) . ? C96 C97 1.363(9) . ? C97 C98 1.427(10) . ? C97 H69 0.9500 . ? C98 C99 1.379(11) . ? C98 H70 0.9500 . ? C99 C100 1.369(10) . ? C99 H71 0.9500 . ? C100 H72 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 N33 Cu1 N1 166.5(2) . . ? N33 Cu1 O10 79.61(18) . . ? N1 Cu1 O10 100.15(18) . . ? N33 Cu1 N35 78.5(2) . . ? N1 Cu1 N35 99.4(2) . . ? O10 Cu1 N35 157.03(19) . . ? N33 Cu1 O1 116.54(18) . . ? N1 Cu1 O1 76.91(17) . . ? O10 Cu1 O1 97.82(16) . . ? N35 Cu1 O1 98.20(18) . . ? N3 Cu2 O7 159.0(2) . . ? N3 Cu2 O1 79.67(18) . . ? O7 Cu2 O1 94.67(17) . . ? N3 Cu2 O2 81.25(18) . . ? O7 Cu2 O2 103.91(17) . . ? O1 Cu2 O2 160.81(17) . . ? N5 Cu3 N7 80.5(2) . . ? N5 Cu3 O2 78.64(18) . . ? N7 Cu3 O2 158.8(2) . . ? N5 Cu3 N17 148.2(2) . . ? N7 Cu3 N17 96.0(2) . . ? O2 Cu3 N17 99.69(18) . . ? N5 Cu3 O5 134.8(2) . . ? N7 Cu3 O5 103.9(2) . . ? O2 Cu3 O5 93.51(18) . . ? N17 Cu3 O5 76.87(19) . . ? N19 Cu4 N8 174.7(2) . . ? N19 Cu4 O6 78.7(2) . . ? N8 Cu4 O6 96.9(2) . . ? N19 Cu4 N21 78.1(2) . . ? N8 Cu4 N21 106.0(2) . . ? O6 Cu4 N21 156.3(2) . . ? N19 Cu4 O3 105.0(2) . . ? N8 Cu4 O3 78.4(2) . . ? O6 Cu4 O3 97.24(19) . . ? N21 Cu4 O3 93.1(2) . . ? N26 Cu5 N10 176.9(2) . . ? N26 Cu5 O3 99.2(2) . . ? N10 Cu5 O3 78.3(2) . . ? N26 Cu5 O4 104.7(2) . . ? N10 Cu5 O4 77.88(19) . . ? O3 Cu5 O4 155.93(19) . . ? N26 Cu5 N28 76.6(2) . . ? N10 Cu5 N28 101.8(2) . . ? O3 Cu5 N28 96.5(2) . . ? O4 Cu5 N28 91.6(2) . . ? N26 Cu5 O8 74.1(2) . . ? N10 Cu5 O8 107.6(2) . . ? O3 Cu5 O8 88.91(18) . . ? O4 Cu5 O8 95.12(17) . . ? N28 Cu5 O8 150.6(2) . . ? N12 Cu6 O4 79.25(19) . . ? N12 Cu6 N31 168.9(2) . . ? O4 Cu6 N31 99.68(18) . . ? N12 Cu6 N14 79.8(2) . . ? O4 Cu6 N14 158.97(19) . . ? N31 Cu6 N14 101.2(2) . . ? N12 Cu6 O9 113.62(19) . . ? O4 Cu6 O9 100.52(18) . . ? N31 Cu6 O9 77.47(18) . . ? N14 Cu6 O9 86.4(2) . . ? N18 Cu7 N16 87.9(2) . . ? N18 Cu7 N20 81.7(2) . . ? N16 Cu7 N20 169.5(3) . . ? N18 Cu7 N15 170.2(2) . . ? N16 Cu7 N15 82.4(2) . . ? N20 Cu7 N15 108.0(3) . . ? N25 Cu8 N23 88.8(2) . . ? N25 Cu8 N27 82.3(2) . . ? N23 Cu8 N27 171.0(2) . . ? N25 Cu8 N22 172.8(2) . . ? N23 Cu8 N22 83.9(2) . . ? N27 Cu8 N22 104.9(2) . . ? N32 Cu9 N30 88.2(2) . . ? N32 Cu9 N34 82.8(2) . . ? N30 Cu9 N34 169.5(2) . . ? N32 Cu9 N29 166.7(2) . . ? N30 Cu9 N29 83.4(2) . . ? N34 Cu9 N29 106.4(2) . . ? O14 S1 O13 121.0(7) . . ? O14 S1 O15 113.7(10) . . ? O13 S1 O15 109.1(8) . . ? O14 S1 C101 105.4(6) . . ? O13 S1 C101 105.3(6) . . ? O15 S1 C101 99.6(7) . . ? O17 S2 O16 111.0(14) . . ? O17 S2 O13 126.4(10) . . ? O16 S2 O13 106.1(11) . . ? O17 S2 C101 102.2(10) . . ? O16 S2 C101 106.0(9) . . ? O13 S2 C101 103.2(7) . . ? O19 S3 O20 113.1(5) . . ? O19 S3 O18 118.8(5) . . ? O20 S3 O18 114.5(4) . . ? O19 S3 C102 102.9(6) . . ? O20 S3 C102 106.8(9) . . ? O18 S3 C102 98.0(7) . . ? O21 S4 O23 114.2(3) . . ? O21 S4 O22 114.3(3) . . ? O23 S4 O22 116.1(3) . . ? O21 S4 C103 103.0(3) . . ? O23 S4 C103 104.9(4) . . ? O22 S4 C103 101.9(3) . . ? O24 S5 O26 110.8(9) . . ? O24 S5 O25 116.9(10) . . ? O26 S5 O25 105.0(9) . . ? O24 S5 C104 103.5(15) . . ? O26 S5 C104 113.1(14) . . ? O25 S5 C104 107.7(15) . . ? O28 S6 O29 131.4(11) . . ? O28 S6 C105 104.5(10) . . ? O29 S6 C105 104.0(11) . . ? O28 S6 O27 104.6(8) . . ? O29 S6 O27 104.9(9) . . ? C105 S6 O27 105.1(8) . . ? F14 C105 F13 106.1(15) . . ? F14 C105 F15 106.0(15) . . ? F13 C105 F15 102.5(14) . . ? F14 C105 S6 112.6(13) . . ? F13 C105 S6 110.9(13) . . ? F15 C105 S6 117.8(13) . . ? C105 F13 F15 97.7(12) . 2_755 ? C105 F15 F13 84.7(11) . 2_755 ? O27 S7 O30 113.7(11) . . ? O27 S7 O28 114.9(9) . . ? O30 S7 O28 118.3(12) . . ? O27 S7 C106 106.4(10) . . ? O30 S7 C106 108.2(13) . . ? O28 S7 C106 92.1(11) . . ? F16 C106 F17 106.7(18) . . ? F16 C106 F18 104.7(19) . . ? F17 C106 F18 112(2) . . ? F16 C106 S7 111.7(16) . . ? F17 C106 S7 110.2(15) . . ? F18 C106 S7 111.2(18) . . ? C6 O1 Cu2 107.9(3) . . ? C6 O1 Cu1 109.5(3) . . ? Cu2 O1 Cu1 141.4(2) . . ? C14 O2 Cu2 110.9(3) . . ? C14 O2 Cu3 108.6(3) . . ? Cu2 O2 Cu3 140.5(2) . . ? C26 O3 Cu5 108.1(4) . . ? C26 O3 Cu4 111.4(4) . . ? Cu5 O3 Cu4 140.2(3) . . ? C34 O4 Cu6 109.5(3) . . ? C34 O4 Cu5 109.8(3) . . ? Cu6 O4 Cu5 137.0(2) . . ? C46 O5 Cu3 109.1(4) . . ? C54 O6 Cu4 109.0(4) . . ? C66 O7 Cu2 119.3(4) . . ? C74 O8 Cu5 106.9(4) . . ? C86 O9 Cu6 105.7(4) . . ? C94 O10 Cu1 109.5(4) . . ? S1 O13 S2 32.4(3) . . ? S7 O27 S6 17.0(5) . . ? S6 O28 S7 21.8(5) . . ? C1 N1 C5 119.2(5) . . ? C1 N1 Cu1 121.4(4) . . ? C5 N1 Cu1 119.4(4) . . ? C6 N2 N3 107.9(5) . . ? C7 N3 N2 122.9(5) . . ? C7 N3 Cu2 118.8(4) . . ? N2 N3 Cu2 117.5(4) . . ? C14 N4 N5 108.8(5) . . ? C15 N5 N4 119.5(5) . . ? C15 N5 Cu3 118.2(5) . . ? N4 N5 Cu3 119.8(3) . . ? C15 N6 H1 120.0 . . ? C15 N6 H2 120.0 . . ? H1 N6 H2 120.0 . . ? C20 N7 C16 118.1(6) . . ? C20 N7 Cu3 128.4(5) . . ? C16 N7 Cu3 113.3(4) . . ? C21 N8 C25 119.1(7) . . ? C21 N8 Cu4 123.4(5) . . ? C25 N8 Cu4 117.4(4) . . ? C26 N9 N10 110.0(5) . . ? C27 N10 N9 119.6(5) . . ? C27 N10 Cu5 122.0(4) . . ? N9 N10 Cu5 118.4(4) . . ? C34 N11 N12 107.6(5) . . ? C35 N12 N11 119.8(5) . . ? C35 N12 Cu6 120.2(4) . . ? N11 N12 Cu6 119.0(4) . . ? C35 N13 H3 120.0 . . ? C35 N13 H4 120.0 . . ? H3 N13 H4 120.0 . . ? C40 N14 C36 119.9(6) . . ? C40 N14 Cu6 127.6(5) . . ? C36 N14 Cu6 112.4(4) . . ? C41 N15 C45 118.1(7) . . ? C41 N15 Cu7 128.4(5) . . ? C45 N15 Cu7 113.3(5) . . ? C46 N16 N17 113.1(5) . . ? C46 N16 Cu7 116.2(4) . . ? N17 N16 Cu7 130.0(4) . . ? C47 N17 N16 121.4(5) . . ? C47 N17 Cu3 123.8(4) . . ? N16 N17 Cu3 114.8(4) . . ? C54 N18 N19 112.0(6) . . ? C54 N18 Cu7 132.1(5) . . ? N19 N18 Cu7 113.4(5) . . ? C55 N19 N18 113.2(6) . . ? C55 N19 Cu4 123.5(5) . . ? N18 N19 Cu4 117.5(5) . . ? C55 N20 Cu7 109.3(5) . . ? C55 N20 H5 125.3 . . ? Cu7 N20 H5 125.3 . . ? C60 N21 C56 118.0(7) . . ? C60 N21 Cu4 130.6(7) . . ? C56 N21 Cu4 111.5(4) . . ? C61 N22 C65 119.6(6) . . ? C61 N22 Cu8 128.5(5) . . ? C65 N22 Cu8 111.8(4) . . ? C66 N23 N24 114.3(5) . . ? C66 N23 Cu8 114.1(4) . . ? N24 N23 Cu8 131.6(4) . . ? C67 N24 N23 119.5(5) . . ? C74 N25 N26 114.1(5) . . ? C74 N25 Cu8 132.2(4) . . ? N26 N25 Cu8 113.6(4) . . ? C75 N26 N25 111.8(6) . . ? C75 N26 Cu5 125.3(5) . . ? N25 N26 Cu5 122.2(4) . . ? C75 N27 Cu8 109.5(4) . . ? C75 N27 H6 125.2 . . ? Cu8 N27 H6 125.2 . . ? C76 N28 C80 120.2(7) . . ? C76 N28 Cu5 111.4(4) . . ? C80 N28 Cu5 128.4(6) . . ? C81 N29 C85 119.8(6) . . ? C81 N29 Cu9 128.6(5) . . ? C85 N29 Cu9 111.5(4) . . ? C86 N30 N31 114.0(5) . . ? C86 N30 Cu9 116.0(4) . . ? N31 N30 Cu9 130.0(4) . . ? C87 N31 N30 121.6(5) . . ? C87 N31 Cu6 123.5(4) . . ? N30 N31 Cu6 114.9(4) . . ? C94 N32 N33 110.3(5) . . ? C94 N32 Cu9 129.9(4) . . ? N33 N32 Cu9 112.4(3) . . ? C95 N33 N32 113.4(5) . . ? C95 N33 Cu1 120.1(4) . . ? N32 N33 Cu1 116.7(3) . . ? C95 N34 Cu9 110.5(4) . . ? C95 N34 H7 124.7 . . ? Cu9 N34 H7 124.7 . . ? C100 N35 C96 118.4(6) . . ? C100 N35 Cu1 129.7(5) . . ? C96 N35 Cu1 111.9(4) . . ? N1 C1 C2 122.4(6) . . ? N1 C1 H8 118.8 . . ? C2 C1 H8 118.8 . . ? C1 C2 C3 118.1(6) . . ? C1 C2 H9 120.9 . . ? C3 C2 H9 120.9 . . ? C4 C3 C2 119.7(6) . . ? C4 C3 H10 120.1 . . ? C2 C3 H10 120.1 . . ? C3 C4 C5 119.5(6) . . ? C3 C4 H11 120.3 . . ? C5 C4 H11 120.3 . . ? N1 C5 C4 121.1(5) . . ? N1 C5 C6 115.4(5) . . ? C4 C5 C6 123.5(6) . . ? O1 C6 N2 127.0(6) . . ? O1 C6 C5 117.3(5) . . ? N2 C6 C5 115.7(5) . . ? N3 C7 C8 125.6(5) . . ? N3 C7 C14 111.9(5) . . ? C8 C7 C14 122.2(5) . . ? C13 C8 C9 118.8(6) . . ? C13 C8 C7 122.8(6) . . ? C9 C8 C7 118.2(5) . . ? C10 C9 C8 119.4(6) . . ? C10 C9 H12 120.3 . . ? C8 C9 H12 120.3 . . ? C11 C10 C9 121.2(7) . . ? C11 C10 H13 119.4 . . ? C9 C10 H13 119.4 . . ? C12 C11 C10 120.0(6) . . ? C12 C11 H14 120.0 . . ? C10 C11 H14 120.0 . . ? C11 C12 C13 119.1(7) . . ? C11 C12 H15 120.4 . . ? C13 C12 H15 120.4 . . ? C8 C13 C12 121.5(7) . . ? C8 C13 H16 119.2 . . ? C12 C13 H16 119.2 . . ? N4 C14 O2 124.2(6) . . ? N4 C14 C7 119.7(5) . . ? O2 C14 C7 116.1(5) . . ? N5 C15 N6 125.2(7) . . ? N5 C15 C16 112.9(6) . . ? N6 C15 C16 121.9(6) . . ? N7 C16 C17 122.7(7) . . ? N7 C16 C15 112.8(6) . . ? C17 C16 C15 124.5(7) . . ? C16 C17 C18 117.9(8) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C19 C18 C17 119.9(7) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 118.5(8) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? N7 C20 C19 122.8(8) . . ? N7 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? N8 C21 C22 121.9(8) . . ? N8 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C23 C22 C21 118.1(7) . . ? C23 C22 H22 120.9 . . ? C21 C22 H22 120.9 . . ? C22 C23 C24 120.8(8) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 118.6(7) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? N8 C25 C24 121.4(6) . . ? N8 C25 C26 115.7(6) . . ? C24 C25 C26 122.9(6) . . ? N9 C26 O3 125.3(6) . . ? N9 C26 C25 117.9(6) . . ? O3 C26 C25 116.9(6) . . ? N10 C27 C28 125.4(5) . . ? N10 C27 C34 111.8(5) . . ? C28 C27 C34 122.7(5) . . ? C33 C28 C29 119.3(6) . . ? C33 C28 C27 122.9(6) . . ? C29 C28 C27 117.7(6) . . ? C30 C29 C28 119.9(7) . . ? C30 C29 H25 120.1 . . ? C28 C29 H25 120.1 . . ? C29 C30 C31 120.1(7) . . ? C29 C30 H26 120.0 . . ? C31 C30 H26 120.0 . . ? C30 C31 C32 120.1(7) . . ? C30 C31 H27 119.9 . . ? C32 C31 H27 119.9 . . ? C33 C32 C31 119.6(8) . . ? C33 C32 H28 120.2 . . ? C31 C32 H28 120.2 . . ? C32 C33 C28 120.9(7) . . ? C32 C33 H29 119.5 . . ? C28 C33 H29 119.5 . . ? N11 C34 O4 124.6(5) . . ? N11 C34 C27 118.4(5) . . ? O4 C34 C27 117.0(5) . . ? N12 C35 N13 125.0(6) . . ? N12 C35 C36 112.7(5) . . ? N13 C35 C36 122.2(6) . . ? N14 C36 C37 122.2(6) . . ? N14 C36 C35 114.1(5) . . ? C37 C36 C35 123.7(6) . . ? C38 C37 C36 117.9(7) . . ? C38 C37 H30 121.1 . . ? C36 C37 H30 121.1 . . ? C37 C38 C39 120.0(7) . . ? C37 C38 H31 120.0 . . ? C39 C38 H31 120.0 . . ? C38 C39 C40 119.4(7) . . ? C38 C39 H32 120.3 . . ? C40 C39 H32 120.3 . . ? N14 C40 C39 120.6(7) . . ? N14 C40 H33 119.7 . . ? C39 C40 H33 119.7 . . ? N15 C41 C42 121.1(7) . . ? N15 C41 H34 119.5 . . ? C42 C41 H34 119.5 . . ? C41 C42 C43 122.0(8) . . ? C41 C42 H35 119.0 . . ? C43 C42 H35 119.0 . . ? C42 C43 C44 117.9(8) . . ? C42 C43 H36 121.1 . . ? C44 C43 H36 121.1 . . ? C45 C44 C43 118.2(7) . . ? C45 C44 H37 120.9 . . ? C43 C44 H37 120.9 . . ? N15 C45 C44 122.8(7) . . ? N15 C45 C46 114.9(6) . . ? C44 C45 C46 122.3(6) . . ? O5 C46 N16 125.4(6) . . ? O5 C46 C45 121.5(6) . . ? N16 C46 C45 113.0(5) . . ? N17 C47 C54 127.6(6) . . ? N17 C47 C48 116.2(5) . . ? C54 C47 C48 116.2(6) . . ? C53 C48 C49 120.1(7) . . ? C53 C48 C47 122.4(6) . . ? C49 C48 C47 117.4(7) . . ? C50 C49 C48 119.7(8) . . ? C50 C49 H38 120.2 . . ? C48 C49 H38 120.2 . . ? C51 C50 C49 119.6(8) . . ? C51 C50 H39 120.2 . . ? C49 C50 H39 120.2 . . ? C52 C51 C50 121.0(8) . . ? C52 C51 H40 119.5 . . ? C50 C51 H40 119.5 . . ? C51 C52 C53 120.3(8) . . ? C51 C52 H41 119.8 . . ? C53 C52 H41 119.8 . . ? C48 C53 C52 119.1(8) . . ? C48 C53 H42 120.5 . . ? C52 C53 H42 120.5 . . ? O6 C54 N18 121.9(6) . . ? O6 C54 C47 119.8(6) . . ? N18 C54 C47 118.3(6) . . ? N20 C55 N19 121.8(6) . . ? N20 C55 C56 127.9(7) . . ? N19 C55 C56 110.3(6) . . ? C57 C56 N21 121.4(7) . . ? C57 C56 C55 124.5(8) . . ? N21 C56 C55 114.2(6) . . ? C56 C57 C58 119.8(9) . . ? C56 C57 H43 120.1 . . ? C58 C57 H43 120.1 . . ? C59 C58 C57 117.6(8) . . ? C59 C58 H44 121.2 . . ? C57 C58 H44 121.2 . . ? C58 C59 C60 120.1(9) . . ? C58 C59 H45 119.9 . . ? C60 C59 H45 119.9 . . ? N21 C60 C59 123.2(10) . . ? N21 C60 H46 118.4 . . ? C59 C60 H46 118.4 . . ? N22 C61 C62 121.2(7) . . ? N22 C61 H47 119.4 . . ? C62 C61 H47 119.4 . . ? C63 C62 C61 118.8(6) . . ? C63 C62 H48 120.6 . . ? C61 C62 H48 120.6 . . ? C64 C63 C62 119.6(7) . . ? C64 C63 H49 120.2 . . ? C62 C63 H49 120.2 . . ? C63 C64 C65 118.6(6) . . ? C63 C64 H50 120.7 . . ? C65 C64 H50 120.7 . . ? N22 C65 C64 122.2(5) . . ? N22 C65 C66 116.4(5) . . ? C64 C65 C66 121.4(5) . . ? O7 C66 N23 126.6(5) . . ? O7 C66 C65 119.8(5) . . ? N23 C66 C65 113.6(5) . . ? N24 C67 C68 113.6(5) . . ? N24 C67 C74 130.2(6) . . ? C68 C67 C74 116.2(5) . . ? C73 C68 C69 119.1(6) . . ? C73 C68 C67 121.9(6) . . ? C69 C68 C67 119.0(6) . . ? C68 C69 C70 120.3(7) . . ? C68 C69 H51 119.9 . . ? C70 C69 H51 119.9 . . ? C71 C70 C69 120.0(8) . . ? C71 C70 H52 120.0 . . ? C69 C70 H52 120.0 . . ? C70 C71 C72 119.5(8) . . ? C70 C71 H53 120.3 . . ? C72 C71 H53 120.3 . . ? C73 C72 C71 121.4(8) . . ? C73 C72 H54 119.3 . . ? C71 C72 H54 119.3 . . ? C72 C73 C68 119.7(8) . . ? C72 C73 H55 120.1 . . ? C68 C73 H55 120.1 . . ? O8 C74 N25 122.0(6) . . ? O8 C74 C67 120.3(6) . . ? N25 C74 C67 117.6(5) . . ? N26 C75 N27 122.6(6) . . ? N26 C75 C76 111.4(6) . . ? N27 C75 C76 126.0(6) . . ? N28 C76 C77 121.9(7) . . ? N28 C76 C75 115.2(6) . . ? C77 C76 C75 122.9(7) . . ? C76 C77 C78 117.6(9) . . ? C76 C77 H56 121.2 . . ? C78 C77 H56 121.2 . . ? C79 C78 C77 119.9(9) . . ? C79 C78 H57 120.0 . . ? C77 C78 H57 120.0 . . ? C78 C79 C80 120.4(8) . . ? C78 C79 H58 119.8 . . ? C80 C79 H58 119.8 . . ? N28 C80 C79 119.9(8) . . ? N28 C80 H59 120.1 . . ? C79 C80 H59 120.1 . . ? N29 C81 C82 120.6(7) . . ? N29 C81 H60 119.7 . . ? C82 C81 H60 119.7 . . ? C83 C82 C81 120.7(7) . . ? C83 C82 H61 119.7 . . ? C81 C82 H61 119.7 . . ? C82 C83 C84 118.5(7) . . ? C82 C83 H62 120.8 . . ? C84 C83 H62 120.8 . . ? C83 C84 C85 119.4(7) . . ? C83 C84 H63 120.3 . . ? C85 C84 H63 120.3 . . ? N29 C85 C84 121.0(6) . . ? N29 C85 C86 116.8(6) . . ? C84 C85 C86 122.2(6) . . ? O9 C86 N30 127.0(6) . . ? O9 C86 C85 120.9(6) . . ? N30 C86 C85 112.1(5) . . ? N31 C87 C88 115.7(5) . . ? N31 C87 C94 126.9(5) . . ? C88 C87 C94 117.4(5) . . ? C89 C88 C93 119.1(6) . . ? C89 C88 C87 121.0(5) . . ? C93 C88 C87 120.0(5) . . ? C90 C89 C88 120.0(6) . . ? C90 C89 H64 120.0 . . ? C88 C89 H64 120.0 . . ? C91 C90 C89 120.8(7) . . ? C91 C90 H65 119.6 . . ? C89 C90 H65 119.6 . . ? C90 C91 C92 119.4(6) . . ? C90 C91 H66 120.3 . . ? C92 C91 H66 120.3 . . ? C93 C92 C91 120.2(6) . . ? C93 C92 H67 119.9 . . ? C91 C92 H67 119.9 . . ? C92 C93 C88 120.4(6) . . ? C92 C93 H68 119.8 . . ? C88 C93 H68 119.8 . . ? O10 C94 N32 122.7(5) . . ? O10 C94 C87 119.5(5) . . ? N32 C94 C87 117.8(5) . . ? N34 C95 N33 120.6(6) . . ? N34 C95 C96 128.0(5) . . ? N33 C95 C96 111.2(5) . . ? N35 C96 C97 121.8(6) . . ? N35 C96 C95 113.4(5) . . ? C97 C96 C95 124.8(6) . . ? C96 C97 C98 118.5(6) . . ? C96 C97 H69 120.7 . . ? C98 C97 H69 120.7 . . ? C99 C98 C97 118.6(7) . . ? C99 C98 H70 120.7 . . ? C97 C98 H70 120.7 . . ? C100 C99 C98 118.0(7) . . ? C100 C99 H71 121.0 . . ? C98 C99 H71 121.0 . . ? N35 C100 C99 124.7(7) . . ? N35 C100 H72 117.7 . . ? C99 C100 H72 117.7 . . ? F3 C101 F1 112.2(11) . . ? F3 C101 F2 102.8(9) . . ? F1 C101 F2 108.6(10) . . ? F3 C101 S2 93.4(8) . . ? F1 C101 S2 113.4(7) . . ? F2 C101 S2 124.4(10) . . ? F3 C101 S1 116.0(9) . . ? F1 C101 S1 112.5(7) . . ? F2 C101 S1 103.6(8) . . ? S2 C101 S1 26.4(3) . . ? F4 C102 F5 99.6(14) . . ? F4 C102 F6 99.7(15) . . ? F5 C102 F6 95.1(13) . . ? F4 C102 S3 120.9(13) . . ? F5 C102 S3 118.4(14) . . ? F6 C102 S3 118.3(11) . . ? F8 C103 F7 106.9(7) . . ? F8 C103 F9 108.1(7) . . ? F7 C103 F9 106.7(7) . . ? F8 C103 S4 112.3(5) . . ? F7 C103 S4 111.5(6) . . ? F9 C103 S4 111.1(5) . . ? F10 C104 F12 104(3) . . ? F10 C104 F11 104(3) . . ? F12 C104 F11 103(3) . . ? F10 C104 S5 119(3) . . ? F12 C104 S5 114(3) . . ? F11 C104 S5 112(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 3.111 _refine_diff_density_min -2.102 _refine_diff_density_rms 0.131 #=== data_Compound12 _database_code_depnum_ccdc_archive 'CCDC 706535' # start Validation Reply Form _vrf_CHEMW03_Compound12 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: This is a Squeezed structure, molecular formula adjusted for excluded lattice solvent ; _vrf_PLAT306_Compound12 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O10 RESPONSE: Hydrogen atoms not found in difference map on solvent water molecules ; _vrf_PLAT602_Compound12 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Platon Squeeze detected a 5000 cubic angstrom void ; _vrf_PLAT043_Compound12 ; PROBLEM: Check Reported Molecular Weight ................ 2184.98 RESPONSE: This is a Squeezed structure, molecular formula adjusted for 17 lattice solvent water molecules ; _vrf_PLAT044_Compound12 ; PROBLEM: Calculated and Reported Dx Differ .............. ? RESPONSE: This is a Squeezed structure, molecular formula adjusted for 17 lattice solvent water molecules ; _vrf_PLAT761_Compound12 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Hydrogen atoms were introduced in calculated positions with thermal parameters set 20% greater than their bonding partners. They were refined on a riding model. X-H bond distances are therefore not reported. ; _vrf_PLAT762_Compound12 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: Hydrogen atoms were introduced in calculated positions with thermal parameters set 20% greater than their bonding partners. They were refined on a riding model. X-Y-H or H-Y-H angles are therefore not reported. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H84 Cl4.50 N36 Ni3 O45' _chemical_formula_weight 2184.981 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.467(2) _cell_length_b 23.324(3) _cell_length_c 27.695(3) _cell_angle_alpha 91.222(4) _cell_angle_beta 90.503(2) _cell_angle_gamma 103.174(4) _cell_volume 11612(2) _cell_formula_units_Z 4 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 45898 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 30.9 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4506 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.9087 _exptl_absorpt_correction_T_max 0.9625 _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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95759 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.50 _reflns_number_total 47379 _reflns_number_gt 30514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 3.7.0' _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.1395P)^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 47379 _refine_ls_number_parameters 2099 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2393 _refine_ls_wR_factor_gt 0.2177 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.002 _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 0.07716(3) 0.85320(2) 1.102780(18) 0.04206(13) Uani 1 1 d . . . Ni2 Ni 0.47514(3) 0.67171(2) 1.088970(17) 0.03757(12) Uani 1 1 d . . . Ni3 Ni 0.22645(3) 0.72903(2) 0.810218(17) 0.03786(13) Uani 1 1 d . . . Ni4 Ni 0.42587(3) 1.13639(2) 0.596138(18) 0.03847(13) Uani 1 1 d . . . Ni5 Ni 0.26607(3) 1.27186(2) 0.305893(18) 0.04022(13) Uani 1 1 d . . . Ni6 Ni 0.04262(3) 1.32985(2) 0.593583(17) 0.04121(13) Uani 1 1 d . . . Cl1 Cl 0.18760(9) 0.76267(7) 1.29006(5) 0.0735(4) Uani 1 1 d . . . Cl2 Cl 0.30184(13) 0.93983(9) 1.20582(7) 0.1052(6) Uani 1 1 d . . . Cl3 Cl 0.54519(9) 0.56055(6) 0.91632(4) 0.0667(4) Uani 1 1 d . . . Cl4 Cl 0.20397(7) 0.53370(5) 0.89917(4) 0.0543(3) Uani 1 1 d . . . Cl5 Cl 0.46233(8) 0.92760(6) 0.59899(4) 0.0629(3) Uani 1 1 d . . . Cl6 Cl 0.11934(7) 1.22046(6) 0.77389(4) 0.0575(3) Uani 1 1 d . . . Cl7 Cl -0.06249(8) 1.18269(8) 0.45825(5) 0.0763(4) Uani 1 1 d . . . Cl8 Cl 0.00937(10) 1.36922(8) 0.30333(5) 0.0803(5) Uani 1 1 d . . . Cl9 Cl 0.04581(13) 1.17388(11) 0.18319(6) 0.1138(8) Uani 1 1 d . . . O1 O 0.20325(16) 0.74222(13) 1.06018(10) 0.0460(7) Uani 1 1 d . . . O2 O 0.48505(19) 0.82716(17) 1.20420(12) 0.0678(10) Uani 1 1 d . . . O3 O 0.29712(16) 0.67470(13) 1.00158(9) 0.0454(7) Uani 1 1 d . . . O4 O 0.4537(2) 0.6705(2) 0.79232(13) 0.0775(12) Uani 1 1 d . . . O5 O 0.17848(17) 0.72979(14) 0.94745(10) 0.0494(7) Uani 1 1 d . . . O6 O 0.0150(5) 0.9442(3) 0.96270(15) 0.170(4) Uani 1 1 d . . . O7 O 0.1840(2) 0.90546(15) 1.10464(13) 0.0641(9) Uani 1 1 d . . . O8 O 0.52122(18) 0.72825(15) 1.03480(11) 0.0581(8) Uani 1 1 d . . . O9 O 0.2580(2) 0.81223(14) 0.84127(13) 0.0625(9) Uani 1 1 d . . . O10 O 0.3233(2) 0.81107(17) 0.99316(15) 0.0794(11) Uani 1 1 d . . . O11 O 0.29648(17) 1.18627(14) 0.49436(10) 0.0507(7) Uani 1 1 d . . . O12 O 0.5197(2) 1.2614(2) 0.31589(14) 0.0934(15) Uani 1 1 d . . . O13 O 0.17903(18) 1.23353(14) 0.43771(10) 0.0500(7) Uani 1 1 d . . . O14 O 0.0185(4) 1.4491(2) 0.46075(13) 0.126(2) Uani 1 1 d . . . O15 O 0.17642(18) 1.23051(15) 0.55306(10) 0.0518(8) Uani 1 1 d . . . O16 O 0.35630(19) 1.19844(18) 0.74983(12) 0.0686(11) Uani 1 1 d . . . O17 O 0.49059(19) 1.21580(14) 0.57372(13) 0.0588(8) Uani 1 1 d . . . O18 O 0.27559(19) 1.35161(13) 0.34227(11) 0.0549(8) Uani 1 1 d . . . O19 O 0.1516(2) 1.37082(18) 0.60978(12) 0.0717(10) Uani 1 1 d . . . O20 O 0.3078(3) 1.31482(19) 0.50546(17) 0.0869(12) Uani 1 1 d . . . O21 O 0.1789(3) 0.7068(2) 1.31397(17) 0.0920(13) Uani 1 1 d . . . O22 O 0.2556(3) 0.8007(3) 1.3066(2) 0.133(2) Uani 1 1 d . . . O23 O 0.1838(3) 0.7531(2) 1.23924(15) 0.1059(16) Uani 1 1 d . . . O24 O 0.1283(3) 0.7881(2) 1.30255(16) 0.0894(13) Uani 1 1 d . . . O25 O 0.3225(4) 0.9569(3) 1.2535(2) 0.159(3) Uani 1 1 d . . . O26 O 0.3673(7) 0.9255(5) 1.1885(5) 0.265(6) Uani 1 1 d . . . O27 O 0.2561(4) 0.8804(3) 1.2007(3) 0.160(3) Uani 1 1 d . . . O28 O 0.2572(9) 0.9715(5) 1.1871(4) 0.359(11) Uani 1 1 d . . . O29 O 0.5742(3) 0.52417(19) 0.94654(15) 0.0862(13) Uani 1 1 d . . . O30 O 0.5916(5) 0.6160(3) 0.9106(2) 0.178(4) Uani 1 1 d . . . O31 O 0.5323(4) 0.5333(3) 0.86959(16) 0.1224(19) Uani 1 1 d . . . O32 O 0.4748(3) 0.5631(3) 0.93646(19) 0.122(2) Uani 1 1 d . . . O33 O 0.26313(19) 0.53615(14) 0.93324(12) 0.0591(8) Uani 1 1 d . . . O34 O 0.2327(3) 0.5500(2) 0.85317(14) 0.0850(12) Uani 1 1 d . . . O35 O 0.1580(2) 0.57232(16) 0.91416(15) 0.0749(11) Uani 1 1 d . . . O36 O 0.1613(2) 0.47361(16) 0.89598(19) 0.0916(14) Uani 1 1 d . . . O37 O 0.4802(3) 0.97251(19) 0.63590(15) 0.0863(12) Uani 1 1 d . . . O38 O 0.4173(3) 0.9442(2) 0.56430(14) 0.0919(14) Uani 1 1 d . . . O39 O 0.4292(3) 0.8726(2) 0.61796(18) 0.1065(16) Uani 1 1 d . . . O40 O 0.5317(2) 0.9224(2) 0.57655(18) 0.0903(13) Uani 1 1 d . . . O41 O 0.1175(3) 1.1684(2) 0.80130(14) 0.0888(13) Uani 1 1 d . . . O42 O 0.1911(2) 1.2576(2) 0.77353(15) 0.0935(14) Uani 1 1 d . . . O43 O 0.0970(2) 1.20161(17) 0.72416(11) 0.0648(9) Uani 1 1 d . . . O44 O 0.0684(2) 1.25158(18) 0.79396(13) 0.0722(10) Uani 1 1 d . . . O45 O -0.0144(2) 1.16821(19) 0.49420(14) 0.0801(11) Uani 1 1 d . . . O46 O -0.0279(2) 1.19115(19) 0.41322(14) 0.0789(11) Uani 1 1 d . . . O47 O -0.1328(2) 1.1454(2) 0.45571(17) 0.0944(14) Uani 1 1 d . . . O48 O -0.0779(3) 1.2402(2) 0.47422(18) 0.1036(16) Uani 1 1 d . . . O49 O 0.0204(4) 1.3155(3) 0.3276(2) 0.135(2) Uani 1 1 d . . . O50 O 0.0559(6) 1.4240(4) 0.3073(4) 0.276(7) Uani 1 1 d . . . O51 O -0.0554(5) 1.3767(4) 0.3251(3) 0.191(4) Uani 1 1 d . . . O52 O -0.0010(3) 1.3509(2) 0.25410(15) 0.0968(14) Uani 1 1 d . . . O53 O 0.0473(3) 1.1784(2) 0.23343(17) 0.1079(16) Uani 1 1 d . . . O54 O 0.0006(8) 1.1194(4) 0.1689(3) 0.266(7) Uani 1 1 d . . . O55 O 0.0171(2) 1.2204(2) 0.16190(16) 0.0897(13) Uani 1 1 d . . . O56 O 0.1242(6) 1.1851(6) 0.1684(3) 0.259(7) Uani 1 1 d . . . N1 N -0.0218(2) 0.78816(17) 1.09974(12) 0.0471(9) Uani 1 1 d . . . N2 N -0.0660(2) 0.6846(2) 1.10652(18) 0.0684(12) Uani 1 1 d . . . N3 N 0.0733(2) 0.67662(15) 1.13233(13) 0.0502(9) Uani 1 1 d . . . H1 H 0.1182 0.6735 1.1408 0.060 Uiso 1 1 calc R . . H2 H 0.0366 0.6451 1.1304 0.060 Uiso 1 1 calc R . . N4 N 0.11154(18) 0.77982(14) 1.12392(11) 0.0362(7) Uani 1 1 d . . . N5 N 0.18345(18) 0.77483(15) 1.13548(11) 0.0405(8) Uani 1 1 d . . . H79 H 0.2011 0.7828 1.1651 0.049 Uiso 1 1 calc R . . N6 N 0.33766(17) 0.72200(15) 1.09111(11) 0.0379(7) Uani 1 1 d . . . H3 H 0.3180 0.6998 1.0661 0.046 Uiso 1 1 calc R . . N7 N 0.40606(18) 0.72506(15) 1.10827(12) 0.0408(8) Uani 1 1 d . . . N8 N 0.5416(2) 0.76145(17) 1.17330(13) 0.0495(9) Uani 1 1 d . . . H80 H 0.5791 0.7757 1.1932 0.059 Uiso 1 1 calc R . . N9 N 0.5486(2) 0.71507(15) 1.14194(12) 0.0438(8) Uani 1 1 d . . . N10 N 0.6710(2) 0.7233(2) 1.17383(15) 0.0636(12) Uani 1 1 d . . . H4 H 0.6693 0.7528 1.1937 0.076 Uiso 1 1 calc R . . H5 H 0.7113 0.7091 1.1727 0.076 Uiso 1 1 calc R . . N11 N 0.6824(2) 0.63244(17) 1.11434(15) 0.0534(10) Uani 1 1 d . . . N12 N 0.56211(19) 0.63020(15) 1.08183(12) 0.0430(8) Uani 1 1 d . . . N13 N 0.41658(19) 0.60523(15) 1.13345(11) 0.0408(7) Uani 1 1 d . . . N14 N 0.3129(2) 0.52342(17) 1.13206(14) 0.0550(9) Uani 1 1 d . . . N15 N 0.2924(2) 0.54159(16) 1.03663(13) 0.0485(9) Uani 1 1 d . . . H6 H 0.2855 0.5455 1.0055 0.058 Uiso 1 1 calc R . . H7 H 0.2616 0.5143 1.0525 0.058 Uiso 1 1 calc R . . N16 N 0.40064(18) 0.61971(14) 1.04128(11) 0.0355(7) Uani 1 1 d . . . N17 N 0.39122(18) 0.62773(15) 0.99149(11) 0.0388(7) Uani 1 1 d . . . H81 H 0.4182 0.6129 0.9707 0.047 Uiso 1 1 calc R . . N18 N 0.28798(19) 0.68974(14) 0.90346(11) 0.0383(7) Uani 1 1 d . . . H8 H 0.2489 0.6946 0.9197 0.046 Uiso 1 1 calc R . . N19 N 0.29859(18) 0.70118(15) 0.85610(11) 0.0384(7) Uani 1 1 d . . . N20 N 0.3755(2) 0.7203(2) 0.76116(14) 0.0622(11) Uani 1 1 d . . . H82 H 0.4038 0.7261 0.7355 0.075 Uiso 1 1 calc R . . N21 N 0.3112(2) 0.74139(16) 0.76023(13) 0.0466(8) Uani 1 1 d . . . N22 N 0.3555(3) 0.7962(2) 0.69123(17) 0.0769(14) Uani 1 1 d . . . H9 H 0.3991 0.7870 0.6917 0.092 Uiso 1 1 calc R . . H10 H 0.3449 0.8191 0.6687 0.092 Uiso 1 1 calc R . . N23 N 0.2179(2) 0.8177(2) 0.68048(15) 0.0628(11) Uani 1 1 d . . . N24 N 0.18158(19) 0.76775(15) 0.75325(12) 0.0426(8) Uani 1 1 d . . . N25 N 0.1776(2) 0.64348(15) 0.78680(12) 0.0423(8) Uani 1 1 d . . . N26 N 0.0770(2) 0.56248(17) 0.80426(15) 0.0563(10) Uani 1 1 d . . . N27 N 0.0266(2) 0.63262(18) 0.86848(15) 0.0576(10) Uani 1 1 d . . . H11 H 0.0080 0.6542 0.8893 0.069 Uiso 1 1 calc R . . H12 H 0.0031 0.5960 0.8621 0.069 Uiso 1 1 calc R . . N28 N 0.13200(19) 0.70870(15) 0.85224(12) 0.0413(8) Uani 1 1 d . . . N29 N 0.1045(2) 0.74486(16) 0.88512(12) 0.0447(8) Uani 1 1 d . . . H83 H 0.0683 0.7612 0.8759 0.054 Uiso 1 1 calc R . . N30 N 0.11478(19) 0.79958(15) 1.00757(11) 0.0400(7) Uani 1 1 d . . . H13 H 0.1369 0.7755 1.0229 0.048 Uiso 1 1 calc R . . N31 N 0.0878(2) 0.84109(15) 1.02927(12) 0.0439(8) Uani 1 1 d . . . N32 N 0.0157(4) 0.9433(2) 1.04276(15) 0.095(2) Uani 1 1 d . . . H84 H -0.0040 0.9742 1.0426 0.114 Uiso 1 1 calc R . . N33 N 0.0311(3) 0.92258(17) 1.08759(13) 0.0566(11) Uani 1 1 d . . . N34 N -0.0051(4) 1.0043(3) 1.12552(17) 0.120(3) Uani 1 1 d . . . H14 H -0.0136 1.0204 1.0983 0.144 Uiso 1 1 calc R . . H15 H -0.0118 1.0212 1.1533 0.144 Uiso 1 1 calc R . . N35 N 0.0171(3) 0.95994(19) 1.21136(14) 0.0660(12) Uani 1 1 d . . . N36 N 0.0607(2) 0.88360(16) 1.17174(12) 0.0457(8) Uani 1 1 d . . . N37 N 0.3528(2) 1.05515(15) 0.60857(12) 0.0414(8) Uani 1 1 d . . . N38 N 0.2652(3) 0.97912(19) 0.56748(16) 0.0707(13) Uani 1 1 d . . . N39 N 0.2894(2) 1.04101(17) 0.48540(13) 0.0537(9) Uani 1 1 d . . . H16 H 0.2967 1.0597 0.4580 0.064 Uiso 1 1 calc R . . H17 H 0.2562 1.0075 0.4869 0.064 Uiso 1 1 calc R . . N40 N 0.3804(2) 1.11304(15) 0.52835(12) 0.0414(8) Uani 1 1 d . . . N41 N 0.3935(2) 1.14368(15) 0.48453(12) 0.0440(8) Uani 1 1 d . . . H26 H 0.4308 1.1393 0.4663 0.053 Uiso 1 1 calc R . . N42 N 0.31225(19) 1.22462(14) 0.40035(11) 0.0376(7) Uani 1 1 d . . . H18 H 0.2674 1.2221 0.4119 0.045 Uiso 1 1 calc R . . N43 N 0.33424(19) 1.24685(14) 0.35729(11) 0.0385(7) Uani 1 1 d . . . N44 N 0.4324(2) 1.29285(19) 0.27537(13) 0.0574(10) Uani 1 1 d . . . H74 H 0.4668 1.3078 0.2544 0.069 Uiso 1 1 calc R . . N45 N 0.3603(2) 1.29816(17) 0.26536(12) 0.0481(9) Uani 1 1 d . . . N46 N 0.4037(3) 1.3503(2) 0.19407(16) 0.0766(14) Uani 1 1 d . . . H19 H 0.4504 1.3483 0.1979 0.092 Uiso 1 1 calc R . . H20 H 0.3903 1.3683 0.1690 0.092 Uiso 1 1 calc R . . N47 N 0.2663(3) 1.3601(2) 0.17557(15) 0.0651(12) Uani 1 1 d . . . N48 N 0.2235(2) 1.30734(16) 0.24689(12) 0.0472(8) Uani 1 1 d . . . N49 N 0.2374(2) 1.18675(16) 0.27640(11) 0.0439(8) Uani 1 1 d . . . N50 N 0.1490(2) 1.0945(2) 0.28534(16) 0.0654(11) Uani 1 1 d . . . N51 N 0.0760(2) 1.14911(17) 0.35066(14) 0.0539(9) Uani 1 1 d . . . H21 H 0.0501 1.1653 0.3713 0.065 Uiso 1 1 calc R . . H22 H 0.0613 1.1115 0.3427 0.065 Uiso 1 1 calc R . . N52 N 0.1664(2) 1.23722(15) 0.33906(11) 0.0416(8) Uani 1 1 d . . . N53 N 0.12858(19) 1.26596(15) 0.37209(11) 0.0405(7) Uani 1 1 d . . . H75 H 0.0960 1.2851 0.3613 0.049 Uiso 1 1 calc R . . N54 N 0.10010(17) 1.29191(13) 0.49834(11) 0.0339(7) Uani 1 1 d . . . H23 H 0.1151 1.2631 0.5124 0.041 Uiso 1 1 calc R . . N55 N 0.0696(2) 1.33066(14) 0.52119(11) 0.0391(7) Uani 1 1 d . . . N56 N 0.0100(3) 1.4378(2) 0.53956(14) 0.0830(17) Uani 1 1 d . . . H76 H 0.0001 1.4729 0.5415 0.100 Uiso 1 1 calc R . . N57 N 0.0097(3) 1.40745(17) 0.58269(12) 0.0576(11) Uani 1 1 d . . . N58 N -0.0244(4) 1.4863(2) 0.62493(16) 0.102(2) Uani 1 1 d . . . H24 H -0.0233 1.5076 0.5990 0.123 Uiso 1 1 calc R . . H25 H -0.0360 1.4998 0.6530 0.123 Uiso 1 1 calc R . . N59 N -0.0337(3) 1.42344(18) 0.70521(13) 0.0620(11) Uani 1 1 d . . . N60 N 0.0118(2) 1.34991(16) 0.66352(12) 0.0444(8) Uani 1 1 d . . . N61 N -0.0647(2) 1.27545(17) 0.58150(12) 0.0464(8) Uani 1 1 d . . . N62 N -0.1285(2) 1.1760(2) 0.58476(16) 0.0628(11) Uani 1 1 d . . . N63 N -0.0017(2) 1.14864(18) 0.61724(13) 0.0564(10) Uani 1 1 d . . . H27 H 0.0384 1.1383 0.6279 0.068 Uiso 1 1 calc R . . H28 H -0.0440 1.1222 0.6141 0.068 Uiso 1 1 calc R . . N64 N 0.05884(18) 1.24722(14) 0.60846(11) 0.0368(7) Uani 1 1 d . . . N65 N 0.12323(19) 1.23199(16) 0.62697(12) 0.0439(8) Uani 1 1 d . . . H77 H 0.1272 1.2263 0.6581 0.053 Uiso 1 1 calc R . . N66 N 0.29267(19) 1.19157(14) 0.59378(12) 0.0407(7) Uani 1 1 d . . . H29 H 0.2896 1.1878 0.5621 0.049 Uiso 1 1 calc R . . N67 N 0.34669(19) 1.17836(14) 0.62037(12) 0.0394(7) Uani 1 1 d . . . N68 N 0.4393(2) 1.16382(17) 0.70699(13) 0.0489(9) Uani 1 1 d . . . H78 H 0.4631 1.1619 0.7344 0.059 Uiso 1 1 calc R . . N69 N 0.46885(19) 1.14456(15) 0.66560(12) 0.0412(8) Uani 1 1 d . . . N70 N 0.5693(3) 1.1271(2) 0.71207(16) 0.0753(14) Uani 1 1 d . . . H30 H 0.5539 1.1395 0.7395 0.090 Uiso 1 1 calc R . . H31 H 0.6106 1.1143 0.7115 0.090 Uiso 1 1 calc R . . N71 N 0.6214(2) 1.08434(19) 0.63171(14) 0.0552(10) Uani 1 1 d . . . N72 N 0.5182(2) 1.10164(15) 0.58693(12) 0.0450(8) Uani 1 1 d . . . C1 C -0.0910(3) 0.7931(3) 1.08810(18) 0.0631(13) Uani 1 1 d . . . H32 H -0.1008 0.8306 1.0821 0.076 Uiso 1 1 calc R . . C2 C -0.1491(3) 0.7415(3) 1.0849(2) 0.0821(18) Uani 1 1 d . . . H33 H -0.1983 0.7435 1.0762 0.099 Uiso 1 1 calc R . . C3 C -0.1328(4) 0.6903(3) 1.0946(3) 0.092(2) Uani 1 1 d . . . H34 H -0.1719 0.6558 1.0927 0.110 Uiso 1 1 calc R . . C4 C -0.0144(2) 0.73373(19) 1.10847(15) 0.0425(9) Uani 1 1 d . . . C5 C 0.0609(2) 0.72897(19) 1.12236(14) 0.0426(9) Uani 1 1 d . . . C6 C 0.2256(2) 0.75786(17) 1.10143(13) 0.0360(8) Uani 1 1 d . . . C7 C 0.3020(2) 0.75688(18) 1.11660(14) 0.0386(8) Uani 1 1 d . . . C8 C 0.3488(2) 0.7841(2) 1.15296(15) 0.0466(10) Uani 1 1 d . . . H35 H 0.3391 0.8104 1.1774 0.056 Uiso 1 1 calc R . . C9 C 0.4144(2) 0.76448(19) 1.14621(15) 0.0450(10) Uani 1 1 d . . . C10 C 0.4838(3) 0.7855(2) 1.17560(16) 0.0529(12) Uani 1 1 d . . . C11 C 0.6125(2) 0.6999(2) 1.14525(15) 0.0453(10) Uani 1 1 d . . . C12 C 0.6202(2) 0.65116(19) 1.11110(16) 0.0459(10) Uani 1 1 d . . . C13 C 0.6874(3) 0.5884(2) 1.08411(19) 0.0573(12) Uani 1 1 d . . . H36 H 0.7314 0.5738 1.0844 0.069 Uiso 1 1 calc R . . C14 C 0.6300(3) 0.5631(2) 1.05200(19) 0.0556(12) Uani 1 1 d . . . H37 H 0.6337 0.5312 1.0311 0.067 Uiso 1 1 calc R . . C15 C 0.5686(3) 0.5857(2) 1.05162(18) 0.0533(11) Uani 1 1 d . . . H38 H 0.5292 0.5697 1.0295 0.064 Uiso 1 1 calc R . . C16 C 0.4292(3) 0.5969(2) 1.18004(15) 0.0505(11) Uani 1 1 d . . . H39 H 0.4693 0.6227 1.1966 0.061 Uiso 1 1 calc R . . C17 C 0.3846(3) 0.5510(2) 1.20452(17) 0.0617(13) Uani 1 1 d . . . H40 H 0.3943 0.5439 1.2373 0.074 Uiso 1 1 calc R . . C18 C 0.3240(3) 0.5152(2) 1.17856(18) 0.0650(14) Uani 1 1 d . . . H41 H 0.2907 0.4847 1.1947 0.078 Uiso 1 1 calc R . . C19 C 0.3608(2) 0.56811(18) 1.11256(14) 0.0405(9) Uani 1 1 d . . . C20 C 0.3493(2) 0.57666(17) 1.05952(14) 0.0368(8) Uani 1 1 d . . . C21 C 0.3425(2) 0.65725(17) 0.97526(13) 0.0373(8) Uani 1 1 d . . . C22 C 0.3452(2) 0.66985(18) 0.92285(14) 0.0403(9) Uani 1 1 d . . . C23 C 0.3948(2) 0.66713(18) 0.88627(14) 0.0402(9) Uani 1 1 d . . . H42 H 0.4399 0.6543 0.8884 0.048 Uiso 1 1 calc R . . C24 C 0.3642(2) 0.68741(19) 0.84549(14) 0.0436(9) Uani 1 1 d . . . C25 C 0.3984(3) 0.6915(2) 0.79815(16) 0.0572(12) Uani 1 1 d . . . C26 C 0.3053(3) 0.7753(2) 0.72472(16) 0.0530(11) Uani 1 1 d . . . C27 C 0.2302(3) 0.78932(19) 0.72009(16) 0.0474(10) Uani 1 1 d . . . C28 C 0.1496(3) 0.8247(3) 0.6754(2) 0.0739(16) Uani 1 1 d . . . H43 H 0.1376 0.8439 0.6475 0.089 Uiso 1 1 calc R . . C29 C 0.0944(3) 0.8057(3) 0.7084(2) 0.0735(16) Uani 1 1 d . . . H44 H 0.0460 0.8124 0.7041 0.088 Uiso 1 1 calc R . . C30 C 0.1125(2) 0.7766(2) 0.74814(17) 0.0516(11) Uani 1 1 d . . . H45 H 0.0761 0.7628 0.7718 0.062 Uiso 1 1 calc R . . C31 C 0.2011(3) 0.6106(2) 0.75215(16) 0.0558(12) Uani 1 1 d . . . H46 H 0.2439 0.6275 0.7341 0.067 Uiso 1 1 calc R . . C32 C 0.1647(4) 0.5537(2) 0.74252(19) 0.0685(15) Uani 1 1 d . . . H47 H 0.1811 0.5307 0.7180 0.082 Uiso 1 1 calc R . . C33 C 0.1041(4) 0.5313(2) 0.7694(2) 0.0692(15) Uani 1 1 d . . . H48 H 0.0791 0.4914 0.7635 0.083 Uiso 1 1 calc R . . C34 C 0.1167(3) 0.61761(19) 0.81005(16) 0.0460(10) Uani 1 1 d . . . C35 C 0.0904(2) 0.65538(19) 0.84674(15) 0.0430(9) Uani 1 1 d . . . C36 C 0.1319(2) 0.75494(19) 0.92980(14) 0.0421(9) Uani 1 1 d . . . C37 C 0.1045(2) 0.7984(2) 0.95922(14) 0.0442(9) Uani 1 1 d . . . C38 C 0.0683(3) 0.8416(2) 0.94906(16) 0.0587(13) Uani 1 1 d . . . H49 H 0.0523 0.8516 0.9183 0.070 Uiso 1 1 calc R . . C39 C 0.0599(3) 0.8678(2) 0.99381(16) 0.0554(12) Uani 1 1 d . . . C40 C 0.0283(5) 0.9202(3) 1.00001(19) 0.101(3) Uani 1 1 d . . . C41 C 0.0181(3) 0.9541(2) 1.12473(17) 0.0648(14) Uani 1 1 d . . . C42 C 0.0330(3) 0.9316(2) 1.17255(16) 0.0531(11) Uani 1 1 d . . . C43 C 0.0304(3) 0.9390(2) 1.25384(16) 0.0608(13) Uani 1 1 d . . . H50 H 0.0211 0.9591 1.2825 0.073 Uiso 1 1 calc R . . C44 C 0.0576(3) 0.8885(2) 1.25758(16) 0.0533(11) Uani 1 1 d . . . H51 H 0.0652 0.8727 1.2880 0.064 Uiso 1 1 calc R . . C45 C 0.0729(2) 0.8628(2) 1.21540(14) 0.0461(10) Uani 1 1 d . . . H52 H 0.0931 0.8288 1.2168 0.055 Uiso 1 1 calc R . . C46 C 0.3405(3) 1.0258(2) 0.65013(17) 0.0560(12) Uani 1 1 d . . . H53 H 0.3666 1.0422 0.6787 0.067 Uiso 1 1 calc R . . C47 C 0.2902(3) 0.9722(3) 0.6516(2) 0.0715(15) Uani 1 1 d . . . H54 H 0.2811 0.9511 0.6807 0.086 Uiso 1 1 calc R . . C48 C 0.2531(4) 0.9503(3) 0.6086(2) 0.0775(17) Uani 1 1 d . . . H55 H 0.2181 0.9135 0.6087 0.093 Uiso 1 1 calc R . . C49 C 0.3147(3) 1.03030(18) 0.56998(16) 0.0455(10) Uani 1 1 d . . . C50 C 0.3290(3) 1.06363(19) 0.52481(15) 0.0453(10) Uani 1 1 d . . . C51 C 0.3506(2) 1.17879(17) 0.47044(14) 0.0379(8) Uani 1 1 d . . . C52 C 0.3664(2) 1.20681(17) 0.42350(13) 0.0376(8) Uani 1 1 d . . . C53 C 0.4283(2) 1.21819(19) 0.39444(15) 0.0450(9) Uani 1 1 d . . . H56 H 0.4758 1.2105 0.4007 0.054 Uiso 1 1 calc R . . C54 C 0.4048(2) 1.24354(18) 0.35375(14) 0.0417(9) Uani 1 1 d . . . C55 C 0.4545(3) 1.2670(2) 0.31409(17) 0.0603(13) Uani 1 1 d . . . C56 C 0.3527(3) 1.3261(2) 0.22663(16) 0.0531(11) Uani 1 1 d . . . C57 C 0.2755(3) 1.3313(2) 0.21525(16) 0.0500(10) Uani 1 1 d . . . C58 C 0.1958(3) 1.3629(3) 0.1662(2) 0.0706(15) Uani 1 1 d . . . H57 H 0.1859 1.3826 0.1381 0.085 Uiso 1 1 calc R . . C59 C 0.1372(3) 1.3387(3) 0.1952(2) 0.0712(15) Uani 1 1 d . . . H58 H 0.0875 1.3406 0.1877 0.085 Uiso 1 1 calc R . . C60 C 0.1557(3) 1.3114(3) 0.23596(19) 0.0673(14) Uani 1 1 d . . . H59 H 0.1169 1.2946 0.2572 0.081 Uiso 1 1 calc R . . C61 C 0.2721(3) 1.1603(2) 0.24305(16) 0.0553(12) Uani 1 1 d . . . H60 H 0.3156 1.1830 0.2287 0.066 Uiso 1 1 calc R . . C62 C 0.2487(3) 1.1035(3) 0.2290(2) 0.0748(16) Uani 1 1 d . . . H61 H 0.2735 1.0865 0.2045 0.090 Uiso 1 1 calc R . . C63 C 0.1847(4) 1.0697(3) 0.2525(2) 0.0772(17) Uani 1 1 d . . . H62 H 0.1677 1.0290 0.2444 0.093 Uiso 1 1 calc R . . C64 C 0.1766(3) 1.1511(2) 0.29493(16) 0.0489(10) Uani 1 1 d . . . C65 C 0.1361(2) 1.1811(2) 0.33172(14) 0.0435(9) Uani 1 1 d . . . C66 C 0.1411(2) 1.26487(17) 0.41973(13) 0.0375(8) Uani 1 1 d . . . C67 C 0.1052(2) 1.30246(18) 0.45043(14) 0.0419(9) Uani 1 1 d . . . C68 C 0.0756(3) 1.34974(19) 0.44211(15) 0.0478(10) Uani 1 1 d . . . H63 H 0.0710 1.3677 0.4121 0.057 Uiso 1 1 calc R . . C69 C 0.0535(3) 1.3660(2) 0.48754(14) 0.0519(11) Uani 1 1 d . . . C70 C 0.0238(4) 1.4184(2) 0.49644(18) 0.0769(18) Uani 1 1 d . . . C71 C -0.0083(4) 1.4332(2) 0.62159(17) 0.0681(15) Uani 1 1 d . . . C72 C -0.0094(3) 1.4013(2) 0.66657(15) 0.0494(10) Uani 1 1 d . . . C73 C -0.0370(3) 1.3908(2) 0.74590(15) 0.0585(12) Uani 1 1 d . . . H64 H -0.0548 1.4049 0.7748 0.070 Uiso 1 1 calc R . . C74 C -0.0162(3) 1.3403(2) 0.74622(16) 0.0584(12) Uani 1 1 d . . . H65 H -0.0186 1.3183 0.7749 0.070 Uiso 1 1 calc R . . C75 C 0.0088(3) 1.3204(2) 0.70391(15) 0.0505(11) Uani 1 1 d . . . H66 H 0.0245 1.2843 0.7037 0.061 Uiso 1 1 calc R . . C76 C -0.1252(3) 1.2914(3) 0.5683(2) 0.0705(16) Uani 1 1 d . . . H67 H -0.1237 1.3316 0.5624 0.085 Uiso 1 1 calc R . . C77 C -0.1914(3) 1.2497(3) 0.5629(2) 0.0823(19) Uani 1 1 d . . . H68 H -0.2362 1.2604 0.5540 0.099 Uiso 1 1 calc R . . C78 C -0.1897(3) 1.1915(3) 0.5711(2) 0.0824(18) Uani 1 1 d . . . H69 H -0.2342 1.1619 0.5668 0.099 Uiso 1 1 calc R . . C79 C -0.0700(2) 1.2187(2) 0.58951(15) 0.0448(10) Uani 1 1 d . . . C80 C 0.0016(2) 1.20296(18) 0.60606(14) 0.0409(9) Uani 1 1 d . . . C81 C 0.1784(2) 1.22607(18) 0.59743(14) 0.0399(9) Uani 1 1 d . . . C82 C 0.2431(2) 1.21139(18) 0.62138(14) 0.0401(9) Uani 1 1 d . . . C83 C 0.2676(2) 1.21279(18) 0.66884(14) 0.0419(9) Uani 1 1 d . . . H70 H 0.2453 1.2255 0.6967 0.050 Uiso 1 1 calc R . . C84 C 0.3320(2) 1.19152(18) 0.66683(14) 0.0397(9) Uani 1 1 d . . . C85 C 0.3776(2) 1.1853(2) 0.70914(16) 0.0491(10) Uani 1 1 d . . . C86 C 0.5305(3) 1.1275(2) 0.67186(17) 0.0514(11) Uani 1 1 d . . . C87 C 0.5590(2) 1.1031(2) 0.62746(16) 0.0491(10) Uani 1 1 d . . . C88 C 0.6450(3) 1.0628(2) 0.59123(18) 0.0615(13) Uani 1 1 d . . . H71 H 0.6895 1.0490 0.5929 0.074 Uiso 1 1 calc R . . C89 C 0.6097(3) 1.0596(2) 0.54840(17) 0.0545(11) Uani 1 1 d . . . H72 H 0.6290 1.0449 0.5202 0.065 Uiso 1 1 calc R . . C90 C 0.5431(3) 1.07863(19) 0.54692(16) 0.0478(10) Uani 1 1 d . . . H73 H 0.5152 1.0753 0.5176 0.057 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 0.0521(3) 0.0530(3) 0.0286(2) 0.0082(2) 0.0053(2) 0.0267(3) Ni2 0.0387(3) 0.0508(3) 0.0275(2) 0.0001(2) -0.0017(2) 0.0195(2) Ni3 0.0390(3) 0.0499(3) 0.0277(2) 0.0065(2) 0.0017(2) 0.0160(2) Ni4 0.0405(3) 0.0465(3) 0.0322(3) 0.0047(2) 0.0031(2) 0.0174(2) Ni5 0.0456(3) 0.0525(3) 0.0277(2) 0.0083(2) 0.0054(2) 0.0212(2) Ni6 0.0498(3) 0.0531(3) 0.0253(2) 0.0037(2) 0.0003(2) 0.0209(2) Cl1 0.0793(9) 0.0903(10) 0.0556(8) 0.0063(7) -0.0028(7) 0.0290(8) Cl2 0.1274(16) 0.1116(14) 0.0870(12) -0.0138(10) -0.0150(11) 0.0514(13) Cl3 0.0929(10) 0.0810(8) 0.0413(6) 0.0174(6) 0.0193(6) 0.0492(8) Cl4 0.0614(7) 0.0540(6) 0.0502(6) -0.0007(5) -0.0169(5) 0.0196(5) Cl5 0.0790(9) 0.0682(7) 0.0487(6) 0.0130(5) 0.0127(6) 0.0302(7) Cl6 0.0491(6) 0.0951(9) 0.0312(5) 0.0073(5) -0.0004(5) 0.0215(6) Cl7 0.0535(7) 0.1211(12) 0.0465(7) 0.0135(7) 0.0002(6) 0.0026(7) Cl8 0.1033(11) 0.1054(11) 0.0537(7) 0.0012(7) -0.0065(7) 0.0685(10) Cl9 0.1420(17) 0.1654(19) 0.0684(10) -0.0204(11) -0.0330(11) 0.1099(16) O1 0.0443(16) 0.0642(18) 0.0350(15) -0.0062(13) -0.0016(13) 0.0242(14) O2 0.063(2) 0.098(3) 0.054(2) -0.0297(19) -0.0256(17) 0.046(2) O3 0.0521(17) 0.0694(18) 0.0251(13) 0.0009(12) 0.0008(12) 0.0352(15) O4 0.067(2) 0.132(3) 0.055(2) 0.041(2) 0.0306(18) 0.061(2) O5 0.0539(18) 0.073(2) 0.0305(14) 0.0021(13) -0.0020(13) 0.0336(16) O6 0.378(10) 0.169(5) 0.038(2) 0.001(3) -0.018(4) 0.219(7) O7 0.069(2) 0.063(2) 0.057(2) 0.0066(16) 0.0138(18) 0.0075(17) O8 0.0560(19) 0.077(2) 0.0429(17) 0.0096(15) -0.0016(15) 0.0175(17) O9 0.068(2) 0.0575(19) 0.063(2) -0.0050(16) -0.0106(18) 0.0167(16) O10 0.090(3) 0.080(2) 0.064(2) 0.0114(19) 0.009(2) 0.007(2) O11 0.0556(18) 0.074(2) 0.0327(15) 0.0236(13) 0.0101(13) 0.0341(16) O12 0.058(2) 0.188(5) 0.057(2) 0.062(3) 0.0252(18) 0.068(3) O13 0.0587(19) 0.0730(19) 0.0312(14) 0.0136(13) 0.0082(13) 0.0404(16) O14 0.277(7) 0.116(3) 0.0336(19) 0.016(2) 0.017(3) 0.145(4) O15 0.0562(18) 0.082(2) 0.0287(14) 0.0112(14) 0.0074(13) 0.0392(17) O16 0.062(2) 0.117(3) 0.0407(18) -0.0293(18) -0.0172(16) 0.052(2) O17 0.062(2) 0.0523(18) 0.062(2) 0.0048(15) 0.0110(17) 0.0107(15) O18 0.067(2) 0.0520(17) 0.0467(18) 0.0004(14) 0.0078(16) 0.0159(15) O19 0.068(2) 0.095(3) 0.0391(18) 0.0017(17) 0.0036(17) -0.009(2) O20 0.095(3) 0.085(3) 0.084(3) 0.006(2) 0.009(2) 0.025(2) O21 0.115(4) 0.092(3) 0.077(3) 0.012(2) -0.014(3) 0.041(3) O22 0.089(4) 0.160(5) 0.126(5) 0.002(4) -0.029(3) -0.023(3) O23 0.160(5) 0.108(3) 0.052(2) 0.004(2) 0.017(3) 0.035(3) O24 0.108(3) 0.101(3) 0.072(3) -0.002(2) 0.007(2) 0.051(3) O25 0.186(7) 0.174(6) 0.099(5) -0.019(4) -0.045(5) 0.007(5) O26 0.278(13) 0.210(9) 0.350(16) -0.049(10) 0.058(11) 0.144(10) O27 0.130(5) 0.105(4) 0.233(8) -0.100(5) -0.041(5) 0.014(4) O28 0.62(2) 0.243(10) 0.313(13) -0.163(10) -0.321(16) 0.333(15) O29 0.116(3) 0.102(3) 0.062(2) 0.016(2) 0.003(2) 0.066(3) O30 0.267(9) 0.116(4) 0.105(5) 0.042(4) 0.001(5) -0.056(5) O31 0.151(5) 0.180(5) 0.050(3) -0.007(3) 0.001(3) 0.068(4) O32 0.152(5) 0.158(5) 0.093(4) 0.012(3) 0.041(3) 0.110(4) O33 0.066(2) 0.066(2) 0.0479(18) -0.0044(15) -0.0218(16) 0.0219(17) O34 0.098(3) 0.119(3) 0.049(2) 0.004(2) -0.006(2) 0.047(3) O35 0.084(3) 0.072(2) 0.080(3) 0.0024(19) 0.003(2) 0.039(2) O36 0.077(3) 0.055(2) 0.139(4) 0.002(2) -0.046(3) 0.0095(19) O37 0.105(3) 0.096(3) 0.069(3) -0.009(2) -0.002(2) 0.045(3) O38 0.127(4) 0.117(3) 0.055(2) 0.010(2) -0.002(2) 0.077(3) O39 0.117(4) 0.102(3) 0.095(3) 0.053(3) 0.029(3) 0.007(3) O40 0.082(3) 0.099(3) 0.097(3) -0.006(2) 0.024(3) 0.036(2) O41 0.114(4) 0.120(3) 0.050(2) 0.025(2) 0.009(2) 0.062(3) O42 0.051(2) 0.158(4) 0.064(3) -0.026(3) -0.0060(19) 0.012(2) O43 0.066(2) 0.090(2) 0.0331(16) 0.0064(16) 0.0031(15) 0.0072(19) O44 0.069(2) 0.106(3) 0.048(2) 0.0088(19) 0.0104(18) 0.033(2) O45 0.082(3) 0.096(3) 0.057(2) -0.001(2) -0.021(2) 0.010(2) O46 0.070(2) 0.110(3) 0.052(2) 0.002(2) 0.0211(19) 0.011(2) O47 0.054(2) 0.127(4) 0.084(3) 0.017(3) -0.002(2) -0.016(2) O48 0.131(4) 0.095(3) 0.099(4) -0.019(3) 0.014(3) 0.056(3) O49 0.170(6) 0.174(5) 0.098(4) 0.007(4) -0.035(4) 0.117(5) O50 0.239(9) 0.171(7) 0.345(13) -0.175(8) 0.161(9) -0.093(7) O51 0.195(8) 0.247(9) 0.170(7) 0.025(6) 0.095(6) 0.126(7) O52 0.113(4) 0.137(4) 0.056(2) -0.004(2) -0.017(2) 0.062(3) O53 0.122(4) 0.147(4) 0.063(3) 0.005(3) -0.031(3) 0.048(3) O54 0.485(19) 0.135(6) 0.209(9) -0.091(6) -0.201(11) 0.154(9) O55 0.078(3) 0.122(3) 0.083(3) 0.001(2) -0.026(2) 0.054(3) O56 0.228(9) 0.540(19) 0.118(6) 0.015(8) 0.016(6) 0.312(12) N1 0.0431(19) 0.078(2) 0.0284(17) 0.0023(16) -0.0003(15) 0.0304(18) N2 0.044(2) 0.089(3) 0.072(3) 0.004(2) 0.009(2) 0.012(2) N3 0.057(2) 0.048(2) 0.049(2) 0.0145(16) 0.0138(18) 0.0163(17) N4 0.0366(17) 0.0470(18) 0.0283(15) 0.0059(13) 0.0021(13) 0.0158(15) N5 0.0402(18) 0.061(2) 0.0268(16) -0.0027(14) -0.0053(14) 0.0249(16) N6 0.0333(16) 0.0551(19) 0.0292(16) -0.0006(14) -0.0013(13) 0.0184(15) N7 0.0359(17) 0.060(2) 0.0323(17) -0.0011(15) -0.0043(14) 0.0236(16) N8 0.047(2) 0.069(2) 0.0401(19) -0.0109(17) -0.0120(16) 0.0295(18) N9 0.0450(19) 0.056(2) 0.0358(18) -0.0068(15) -0.0044(15) 0.0241(16) N10 0.052(2) 0.085(3) 0.061(3) -0.021(2) -0.022(2) 0.032(2) N11 0.043(2) 0.059(2) 0.065(3) -0.0082(19) -0.0057(18) 0.0263(18) N12 0.0393(18) 0.055(2) 0.0399(18) -0.0042(15) 0.0005(15) 0.0233(16) N13 0.0474(19) 0.0515(19) 0.0286(16) 0.0058(14) 0.0005(15) 0.0216(16) N14 0.068(3) 0.057(2) 0.044(2) 0.0056(17) 0.0011(19) 0.021(2) N15 0.051(2) 0.053(2) 0.042(2) 0.0053(16) -0.0080(17) 0.0138(17) N16 0.0358(17) 0.0488(18) 0.0263(15) 0.0016(13) -0.0016(13) 0.0185(14) N17 0.0414(18) 0.057(2) 0.0228(15) -0.0002(13) 0.0011(13) 0.0204(16) N18 0.0424(18) 0.0480(18) 0.0287(16) 0.0054(13) -0.0018(14) 0.0189(15) N19 0.0402(18) 0.0528(19) 0.0271(15) 0.0097(13) 0.0068(13) 0.0196(15) N20 0.051(2) 0.109(3) 0.040(2) 0.031(2) 0.0199(18) 0.041(2) N21 0.0429(19) 0.063(2) 0.0389(19) 0.0168(16) 0.0042(15) 0.0213(17) N22 0.057(3) 0.113(4) 0.070(3) 0.060(3) 0.028(2) 0.033(3) N23 0.052(2) 0.083(3) 0.053(2) 0.027(2) -0.0060(19) 0.011(2) N24 0.0442(19) 0.0530(19) 0.0328(17) 0.0077(14) -0.0064(15) 0.0150(16) N25 0.047(2) 0.0520(19) 0.0296(16) 0.0051(14) -0.0050(15) 0.0143(16) N26 0.060(2) 0.051(2) 0.056(2) 0.0088(18) -0.012(2) 0.0089(19) N27 0.051(2) 0.066(2) 0.058(2) 0.0150(19) 0.0045(19) 0.0172(19) N28 0.0412(18) 0.056(2) 0.0306(17) 0.0037(14) -0.0003(14) 0.0195(16) N29 0.047(2) 0.066(2) 0.0305(17) 0.0030(15) 0.0013(15) 0.0305(17) N30 0.0433(18) 0.057(2) 0.0269(15) 0.0081(14) 0.0042(14) 0.0258(16) N31 0.059(2) 0.0498(19) 0.0308(17) 0.0044(14) 0.0075(16) 0.0292(17) N32 0.184(6) 0.103(4) 0.036(2) 0.014(2) 0.014(3) 0.109(4) N33 0.090(3) 0.065(2) 0.0318(18) 0.0079(16) 0.0073(19) 0.052(2) N34 0.240(8) 0.125(5) 0.042(3) -0.001(3) 0.010(4) 0.139(5) N35 0.102(4) 0.072(3) 0.037(2) 0.0044(18) 0.009(2) 0.048(3) N36 0.055(2) 0.056(2) 0.0310(17) 0.0048(15) 0.0036(16) 0.0234(17) N37 0.0474(19) 0.0513(19) 0.0299(16) 0.0043(14) -0.0006(15) 0.0199(16) N38 0.084(3) 0.062(3) 0.055(3) 0.015(2) -0.018(2) -0.006(2) N39 0.071(3) 0.058(2) 0.0379(19) -0.0001(16) -0.0117(18) 0.027(2) N40 0.048(2) 0.0465(19) 0.0333(17) 0.0088(14) 0.0044(15) 0.0167(16) N41 0.049(2) 0.058(2) 0.0331(17) 0.0161(15) 0.0105(15) 0.0253(17) N42 0.0461(19) 0.0479(18) 0.0242(15) 0.0088(13) 0.0093(14) 0.0211(15) N43 0.0419(18) 0.0476(18) 0.0295(16) 0.0085(13) 0.0051(14) 0.0170(15) N44 0.048(2) 0.096(3) 0.0368(19) 0.0309(19) 0.0181(17) 0.031(2) N45 0.057(2) 0.068(2) 0.0286(17) 0.0162(15) 0.0127(16) 0.0324(19) N46 0.067(3) 0.115(4) 0.057(3) 0.050(3) 0.019(2) 0.034(3) N47 0.072(3) 0.089(3) 0.047(2) 0.034(2) 0.013(2) 0.042(2) N48 0.051(2) 0.066(2) 0.0311(17) 0.0103(16) 0.0044(16) 0.0258(18) N49 0.048(2) 0.062(2) 0.0247(16) -0.0059(15) 0.0017(14) 0.0199(17) N50 0.058(3) 0.074(3) 0.061(3) -0.018(2) -0.002(2) 0.011(2) N51 0.050(2) 0.058(2) 0.052(2) -0.0062(18) 0.0025(18) 0.0081(18) N52 0.051(2) 0.051(2) 0.0285(16) 0.0016(14) 0.0064(15) 0.0237(17) N53 0.0441(19) 0.0539(19) 0.0299(16) 0.0046(14) 0.0046(14) 0.0239(16) N54 0.0397(17) 0.0394(16) 0.0256(15) 0.0046(12) 0.0023(13) 0.0147(14) N55 0.053(2) 0.0472(18) 0.0236(15) 0.0041(13) 0.0062(14) 0.0245(16) N56 0.171(5) 0.074(3) 0.0275(19) 0.0070(18) 0.006(3) 0.076(3) N57 0.097(3) 0.062(2) 0.0266(17) 0.0052(16) 0.0052(19) 0.045(2) N58 0.219(7) 0.075(3) 0.037(2) 0.005(2) 0.020(3) 0.081(4) N59 0.091(3) 0.065(2) 0.0301(19) -0.0048(17) 0.007(2) 0.018(2) N60 0.051(2) 0.057(2) 0.0256(16) -0.0033(14) -0.0009(15) 0.0133(17) N61 0.045(2) 0.066(2) 0.0323(17) -0.0032(16) -0.0009(15) 0.0212(18) N62 0.043(2) 0.079(3) 0.061(3) 0.000(2) 0.000(2) 0.004(2) N63 0.064(3) 0.068(3) 0.037(2) 0.0005(17) -0.0019(18) 0.016(2) N64 0.0352(17) 0.0509(19) 0.0288(16) 0.0077(13) 0.0031(13) 0.0185(15) N65 0.0432(19) 0.065(2) 0.0288(16) 0.0105(15) -0.0008(14) 0.0231(17) N66 0.0441(19) 0.0508(19) 0.0311(16) 0.0053(14) 0.0017(14) 0.0182(16) N67 0.0411(18) 0.0494(18) 0.0326(17) 0.0057(14) -0.0011(14) 0.0200(15) N68 0.0436(19) 0.075(2) 0.0337(18) -0.0106(17) -0.0064(15) 0.0277(18) N69 0.0399(18) 0.0497(19) 0.0380(18) -0.0020(15) 0.0000(15) 0.0187(15) N70 0.063(3) 0.122(4) 0.057(3) -0.029(3) -0.020(2) 0.059(3) N71 0.042(2) 0.084(3) 0.049(2) -0.0037(19) -0.0010(17) 0.034(2) N72 0.051(2) 0.056(2) 0.0353(18) 0.0089(15) 0.0056(16) 0.0261(17) C1 0.052(3) 0.097(4) 0.050(3) 0.008(3) 0.005(2) 0.036(3) C2 0.040(3) 0.135(6) 0.071(4) 0.011(4) -0.005(3) 0.018(3) C3 0.056(4) 0.098(5) 0.121(6) 0.007(4) -0.004(4) 0.017(3) C4 0.042(2) 0.053(2) 0.036(2) -0.0003(18) 0.0054(17) 0.0156(19) C5 0.047(2) 0.056(2) 0.0282(19) 0.0093(17) 0.0136(17) 0.018(2) C6 0.040(2) 0.043(2) 0.0286(18) 0.0039(15) 0.0022(16) 0.0156(17) C7 0.039(2) 0.050(2) 0.0308(19) -0.0012(16) 0.0017(16) 0.0176(18) C8 0.050(2) 0.066(3) 0.032(2) -0.0087(18) -0.0078(18) 0.031(2) C9 0.048(2) 0.061(3) 0.033(2) -0.0058(18) -0.0058(18) 0.027(2) C10 0.055(3) 0.075(3) 0.035(2) -0.017(2) -0.013(2) 0.032(2) C11 0.039(2) 0.060(3) 0.041(2) -0.0064(19) -0.0053(18) 0.0209(19) C12 0.041(2) 0.053(2) 0.046(2) 0.0012(19) -0.0007(19) 0.0152(19) C13 0.048(3) 0.060(3) 0.072(3) -0.003(2) 0.000(2) 0.029(2) C14 0.045(2) 0.061(3) 0.065(3) -0.018(2) -0.004(2) 0.024(2) C15 0.052(3) 0.058(3) 0.054(3) -0.012(2) 0.004(2) 0.021(2) C16 0.062(3) 0.063(3) 0.030(2) 0.0055(19) -0.001(2) 0.022(2) C17 0.076(3) 0.075(3) 0.037(2) 0.014(2) -0.003(2) 0.022(3) C18 0.090(4) 0.059(3) 0.049(3) 0.016(2) 0.010(3) 0.023(3) C19 0.044(2) 0.051(2) 0.033(2) 0.0032(17) 0.0025(17) 0.0217(19) C20 0.0329(19) 0.045(2) 0.038(2) 0.0017(17) -0.0012(16) 0.0214(17) C21 0.041(2) 0.048(2) 0.0255(18) 0.0057(15) -0.0021(16) 0.0160(18) C22 0.041(2) 0.057(2) 0.0270(18) 0.0095(16) 0.0001(16) 0.0189(19) C23 0.038(2) 0.054(2) 0.035(2) 0.0098(17) 0.0069(17) 0.0216(18) C24 0.044(2) 0.060(3) 0.030(2) 0.0099(17) 0.0059(17) 0.018(2) C25 0.051(3) 0.091(3) 0.040(2) 0.028(2) 0.012(2) 0.034(3) C26 0.043(2) 0.082(3) 0.040(2) 0.022(2) 0.0053(19) 0.024(2) C27 0.050(2) 0.054(2) 0.040(2) 0.0187(19) 0.0025(19) 0.012(2) C28 0.060(3) 0.091(4) 0.071(4) 0.050(3) -0.008(3) 0.013(3) C29 0.049(3) 0.094(4) 0.078(4) 0.049(3) -0.009(3) 0.014(3) C30 0.039(2) 0.064(3) 0.054(3) 0.021(2) -0.001(2) 0.016(2) C31 0.074(3) 0.065(3) 0.035(2) 0.003(2) 0.002(2) 0.027(3) C32 0.107(5) 0.060(3) 0.042(3) -0.006(2) -0.008(3) 0.027(3) C33 0.089(4) 0.058(3) 0.060(3) -0.001(3) -0.027(3) 0.016(3) C34 0.050(2) 0.052(2) 0.040(2) 0.0007(18) -0.0116(19) 0.023(2) C35 0.035(2) 0.061(3) 0.036(2) 0.0179(18) -0.0004(17) 0.0164(19) C36 0.041(2) 0.059(2) 0.033(2) 0.0083(17) 0.0054(17) 0.0229(19) C37 0.047(2) 0.065(3) 0.0277(19) 0.0083(18) 0.0051(17) 0.027(2) C38 0.088(4) 0.067(3) 0.035(2) 0.010(2) 0.001(2) 0.045(3) C39 0.085(4) 0.059(3) 0.033(2) 0.0040(19) 0.010(2) 0.041(3) C40 0.197(8) 0.112(5) 0.031(3) 0.013(3) 0.003(4) 0.110(6) C41 0.100(4) 0.071(3) 0.039(2) 0.010(2) 0.007(3) 0.051(3) C42 0.073(3) 0.056(3) 0.038(2) 0.0055(19) 0.004(2) 0.029(2) C43 0.089(4) 0.066(3) 0.032(2) -0.006(2) 0.007(2) 0.029(3) C44 0.065(3) 0.066(3) 0.033(2) 0.002(2) 0.002(2) 0.024(2) C45 0.050(2) 0.059(3) 0.031(2) 0.0066(18) -0.0012(18) 0.018(2) C46 0.067(3) 0.062(3) 0.040(2) 0.022(2) 0.003(2) 0.014(2) C47 0.070(3) 0.082(4) 0.054(3) 0.026(3) 0.003(3) -0.002(3) C48 0.087(4) 0.066(3) 0.065(3) 0.027(3) 0.000(3) -0.014(3) C49 0.052(2) 0.040(2) 0.045(2) 0.0090(18) -0.001(2) 0.0113(19) C50 0.062(3) 0.050(2) 0.033(2) 0.0047(17) -0.0016(19) 0.032(2) C51 0.038(2) 0.052(2) 0.0302(19) 0.0127(16) 0.0091(16) 0.0208(18) C52 0.047(2) 0.042(2) 0.0274(18) 0.0033(15) 0.0027(16) 0.0179(17) C53 0.045(2) 0.055(2) 0.038(2) 0.0065(18) 0.0035(18) 0.0177(19) C54 0.049(2) 0.054(2) 0.0293(19) 0.0095(17) 0.0089(17) 0.026(2) C55 0.058(3) 0.095(4) 0.038(2) 0.028(2) 0.009(2) 0.036(3) C56 0.059(3) 0.072(3) 0.037(2) 0.018(2) 0.015(2) 0.032(2) C57 0.056(3) 0.060(3) 0.037(2) 0.0117(19) 0.005(2) 0.019(2) C58 0.074(4) 0.101(4) 0.050(3) 0.018(3) -0.004(3) 0.045(3) C59 0.068(3) 0.101(4) 0.055(3) 0.027(3) 0.001(3) 0.038(3) C60 0.058(3) 0.105(4) 0.051(3) 0.021(3) 0.006(2) 0.043(3) C61 0.062(3) 0.071(3) 0.039(2) -0.006(2) 0.009(2) 0.029(2) C62 0.079(4) 0.082(4) 0.065(4) -0.023(3) 0.005(3) 0.024(3) C63 0.081(4) 0.068(3) 0.080(4) -0.023(3) 0.008(3) 0.012(3) C64 0.050(3) 0.062(3) 0.037(2) -0.004(2) 0.0001(19) 0.019(2) C65 0.042(2) 0.059(3) 0.032(2) 0.0010(18) -0.0055(17) 0.018(2) C66 0.041(2) 0.047(2) 0.0280(18) 0.0045(16) 0.0015(16) 0.0169(17) C67 0.054(2) 0.052(2) 0.0251(18) 0.0064(16) 0.0034(17) 0.023(2) C68 0.070(3) 0.052(2) 0.029(2) 0.0087(17) 0.0051(19) 0.029(2) C69 0.081(3) 0.056(3) 0.0260(19) 0.0085(17) 0.004(2) 0.030(2) C70 0.140(6) 0.071(3) 0.040(3) 0.009(2) 0.017(3) 0.066(4) C71 0.118(5) 0.062(3) 0.032(2) -0.006(2) 0.013(3) 0.037(3) C72 0.061(3) 0.055(3) 0.032(2) 0.0026(18) 0.007(2) 0.012(2) C73 0.080(3) 0.068(3) 0.026(2) -0.0017(19) 0.012(2) 0.011(3) C74 0.072(3) 0.076(3) 0.030(2) 0.011(2) 0.010(2) 0.022(3) C75 0.060(3) 0.065(3) 0.031(2) 0.0073(19) 0.0086(19) 0.021(2) C76 0.071(4) 0.089(4) 0.064(3) -0.013(3) -0.017(3) 0.047(3) C77 0.048(3) 0.115(5) 0.092(5) -0.015(4) -0.023(3) 0.038(3) C78 0.048(3) 0.121(5) 0.072(4) -0.008(4) -0.002(3) 0.005(3) C79 0.036(2) 0.064(3) 0.033(2) -0.0005(19) 0.0056(17) 0.008(2) C80 0.045(2) 0.049(2) 0.0299(19) 0.0024(16) 0.0048(17) 0.0121(19) C81 0.038(2) 0.055(2) 0.0318(19) 0.0066(17) 0.0036(16) 0.0217(18) C82 0.038(2) 0.055(2) 0.0306(19) 0.0038(17) -0.0007(16) 0.0183(18) C83 0.047(2) 0.055(2) 0.0278(19) -0.0020(17) -0.0052(17) 0.0217(19) C84 0.040(2) 0.051(2) 0.033(2) -0.0041(17) -0.0069(17) 0.0198(18) C85 0.042(2) 0.064(3) 0.045(2) -0.010(2) -0.0074(19) 0.022(2) C86 0.045(2) 0.066(3) 0.049(3) -0.004(2) -0.006(2) 0.025(2) C87 0.040(2) 0.067(3) 0.044(2) 0.000(2) -0.0009(19) 0.020(2) C88 0.054(3) 0.088(4) 0.054(3) -0.010(3) -0.002(2) 0.040(3) C89 0.053(3) 0.071(3) 0.046(3) -0.002(2) -0.001(2) 0.027(2) C90 0.049(2) 0.059(3) 0.040(2) 0.0102(19) 0.0048(19) 0.021(2) _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 N33 2.041(3) . ? Ni1 N4 2.051(3) . ? Ni1 N31 2.067(3) . ? Ni1 O7 2.068(4) . ? Ni1 N36 2.072(3) . ? Ni1 N1 2.091(4) . ? Ni2 N7 2.042(3) . ? Ni2 N16 2.061(3) . ? Ni2 N12 2.065(3) . ? Ni2 N9 2.072(3) . ? Ni2 O8 2.076(3) . ? Ni2 N13 2.105(4) . ? Ni3 N19 2.052(3) . ? Ni3 O9 2.061(3) . ? Ni3 N21 2.073(4) . ? Ni3 N28 2.074(4) . ? Ni3 N25 2.081(3) . ? Ni3 N24 2.090(3) . ? Ni4 N67 2.047(3) . ? Ni4 N40 2.060(3) . ? Ni4 N69 2.063(3) . ? Ni4 N72 2.064(3) . ? Ni4 O17 2.073(3) . ? Ni4 N37 2.097(4) . ? Ni5 N45 2.059(4) . ? Ni5 N52 2.066(4) . ? Ni5 O18 2.067(3) . ? Ni5 N43 2.071(3) . ? Ni5 N48 2.075(3) . ? Ni5 N49 2.081(3) . ? Ni6 O19 2.063(4) . ? Ni6 N57 2.064(4) . ? Ni6 N64 2.066(3) . ? Ni6 N55 2.069(3) . ? Ni6 N60 2.097(3) . ? Ni6 N61 2.115(4) . ? Cl1 O24 1.401(4) . ? Cl1 O23 1.419(4) . ? Cl1 O22 1.428(5) . ? Cl1 O21 1.450(5) . ? Cl2 O28 1.334(7) . ? Cl2 O25 1.394(6) . ? Cl2 O26 1.411(10) . ? Cl2 O27 1.454(6) . ? Cl3 O29 1.392(4) . ? Cl3 O30 1.393(6) . ? Cl3 O31 1.424(5) . ? Cl3 O32 1.433(5) . ? Cl4 O34 1.411(4) . ? Cl4 O33 1.428(3) . ? Cl4 O35 1.429(4) . ? Cl4 O36 1.444(4) . ? Cl5 O38 1.384(4) . ? Cl5 O39 1.404(4) . ? Cl5 O37 1.429(4) . ? Cl5 O40 1.458(4) . ? Cl6 O42 1.409(4) . ? Cl6 O44 1.423(4) . ? Cl6 O41 1.439(4) . ? Cl6 O43 1.464(3) . ? Cl7 O47 1.388(4) . ? Cl7 O46 1.404(4) . ? Cl7 O45 1.425(4) . ? Cl7 O48 1.492(4) . ? Cl8 O50 1.369(7) . ? Cl8 O51 1.389(7) . ? Cl8 O52 1.418(4) . ? Cl8 O49 1.489(6) . ? Cl9 O53 1.393(5) . ? Cl9 O54 1.400(10) . ? Cl9 O55 1.445(4) . ? Cl9 O56 1.474(10) . ? O1 C6 1.230(5) . ? O2 C10 1.236(5) . ? O3 C21 1.246(5) . ? O4 C25 1.238(5) . ? O5 C36 1.249(5) . ? O6 C40 1.235(6) . ? O11 C51 1.247(5) . ? O12 C55 1.240(6) . ? O13 C66 1.232(4) . ? O14 C70 1.250(6) . ? O15 C81 1.237(5) . ? O16 C85 1.252(5) . ? N1 C4 1.334(6) . ? N1 C1 1.347(6) . ? N2 C3 1.312(8) . ? N2 C4 1.312(6) . ? N3 C5 1.327(5) . ? N3 H1 0.8800 . ? N3 H2 0.8800 . ? N4 C5 1.332(5) . ? N4 N5 1.394(4) . ? N5 C6 1.338(5) . ? N5 H79 0.8800 . ? N6 N7 1.332(4) . ? N6 C7 1.350(5) . ? N6 H3 0.8800 . ? N7 C9 1.365(5) . ? N8 C10 1.315(5) . ? N8 N9 1.403(5) . ? N8 H80 0.8800 . ? N9 C11 1.310(5) . ? N10 C11 1.338(5) . ? N10 H4 0.8800 . ? N10 H5 0.8800 . ? N11 C12 1.322(5) . ? N11 C13 1.331(6) . ? N12 C12 1.333(5) . ? N12 C15 1.348(5) . ? N13 C19 1.307(5) . ? N13 C16 1.335(5) . ? N14 C18 1.327(6) . ? N14 C19 1.331(6) . ? N15 C20 1.322(5) . ? N15 H6 0.8800 . ? N15 H7 0.8800 . ? N16 C20 1.327(5) . ? N16 N17 1.410(4) . ? N17 C21 1.332(5) . ? N17 H81 0.8800 . ? N18 N19 1.351(4) . ? N18 C22 1.358(5) . ? N18 H8 0.8800 . ? N19 C24 1.355(5) . ? N20 C25 1.353(6) . ? N20 N21 1.385(5) . ? N20 H82 0.8800 . ? N21 C26 1.295(5) . ? N22 C26 1.336(6) . ? N22 H9 0.8800 . ? N22 H10 0.8800 . ? N23 C28 1.315(7) . ? N23 C27 1.337(5) . ? N24 C27 1.316(5) . ? N24 C30 1.345(5) . ? N25 C34 1.327(6) . ? N25 C31 1.351(6) . ? N26 C34 1.333(6) . ? N26 C33 1.364(7) . ? N27 C35 1.332(6) . ? N27 H11 0.8800 . ? N27 H12 0.8800 . ? N28 C35 1.309(5) . ? N28 N29 1.403(5) . ? N29 C36 1.328(5) . ? N29 H83 0.8800 . ? N30 N31 1.322(4) . ? N30 C37 1.349(5) . ? N30 H13 0.8800 . ? N31 C39 1.334(5) . ? N32 C40 1.334(7) . ? N32 N33 1.392(5) . ? N32 H84 0.8800 . ? N33 C41 1.307(6) . ? N34 C41 1.334(6) . ? N34 H14 0.8800 . ? N34 H15 0.8800 . ? N35 C42 1.319(6) . ? N35 C43 1.326(6) . ? N36 C42 1.333(5) . ? N36 C45 1.349(5) . ? N37 C49 1.322(5) . ? N37 C46 1.346(5) . ? N38 C49 1.328(6) . ? N38 C48 1.330(7) . ? N39 C50 1.338(6) . ? N39 H16 0.8800 . ? N39 H17 0.8800 . ? N40 C50 1.317(6) . ? N40 N41 1.416(4) . ? N41 C51 1.325(5) . ? N41 H26 0.8800 . ? N42 C52 1.332(5) . ? N42 N43 1.340(4) . ? N42 H18 0.8800 . ? N43 C54 1.327(5) . ? N44 C55 1.346(5) . ? N44 N45 1.392(5) . ? N44 H74 0.8800 . ? N45 C56 1.289(5) . ? N46 C56 1.346(6) . ? N46 H19 0.8800 . ? N46 H20 0.8800 . ? N47 C57 1.330(5) . ? N47 C58 1.341(7) . ? N48 C60 1.311(6) . ? N48 C57 1.339(6) . ? N49 C61 1.346(5) . ? N49 C64 1.349(6) . ? N50 C64 1.322(6) . ? N50 C63 1.327(7) . ? N51 C65 1.309(6) . ? N51 H21 0.8800 . ? N51 H22 0.8800 . ? N52 C65 1.312(6) . ? N52 N53 1.404(4) . ? N53 C66 1.339(5) . ? N53 H75 0.8800 . ? N54 N55 1.323(4) . ? N54 C67 1.355(5) . ? N54 H23 0.8800 . ? N55 C69 1.333(5) . ? N56 C70 1.316(6) . ? N56 N57 1.400(5) . ? N56 H76 0.8800 . ? N57 C71 1.305(6) . ? N58 C71 1.340(6) . ? N58 H24 0.8800 . ? N58 H25 0.8800 . ? N59 C72 1.305(6) . ? N59 C73 1.367(6) . ? N60 C75 1.322(5) . ? N60 C72 1.345(6) . ? N61 C76 1.308(6) . ? N61 C79 1.327(6) . ? N62 C79 1.296(6) . ? N62 C78 1.316(7) . ? N63 C80 1.299(6) . ? N63 H27 0.8800 . ? N63 H28 0.8800 . ? N64 C80 1.299(5) . ? N64 N65 1.412(4) . ? N65 C81 1.342(5) . ? N65 H77 0.8800 . ? N66 N67 1.330(4) . ? N66 C82 1.351(5) . ? N66 H29 0.8800 . ? N67 C84 1.360(5) . ? N68 C85 1.347(5) . ? N68 N69 1.383(5) . ? N68 H78 0.8800 . ? N69 C86 1.300(5) . ? N70 C86 1.321(6) . ? N70 H30 0.8800 . ? N70 H31 0.8800 . ? N71 C87 1.329(5) . ? N71 C88 1.335(6) . ? N72 C87 1.341(5) . ? N72 C90 1.350(5) . ? C1 C2 1.418(9) . ? C1 H32 0.9500 . ? C2 C3 1.328(9) . ? C2 H33 0.9500 . ? C3 H34 0.9500 . ? C4 C5 1.469(6) . ? C6 C7 1.474(5) . ? C7 C8 1.369(6) . ? C8 C9 1.401(6) . ? C8 H35 0.9500 . ? C9 C10 1.492(6) . ? C11 C12 1.495(6) . ? C13 C14 1.393(7) . ? C13 H36 0.9500 . ? C14 C15 1.353(6) . ? C14 H37 0.9500 . ? C15 H38 0.9500 . ? C16 C17 1.386(7) . ? C16 H39 0.9500 . ? C17 C18 1.414(8) . ? C17 H40 0.9500 . ? C18 H41 0.9500 . ? C19 C20 1.506(5) . ? C21 C22 1.486(5) . ? C22 C23 1.381(5) . ? C23 C24 1.397(5) . ? C23 H42 0.9500 . ? C24 C25 1.456(6) . ? C26 C27 1.500(6) . ? C28 C29 1.377(8) . ? C28 H43 0.9500 . ? C29 C30 1.383(6) . ? C29 H44 0.9500 . ? C30 H45 0.9500 . ? C31 C32 1.365(7) . ? C31 H46 0.9500 . ? C32 C33 1.356(8) . ? C32 H47 0.9500 . ? C33 H48 0.9500 . ? C34 C35 1.487(6) . ? C36 C37 1.467(6) . ? C37 C38 1.362(6) . ? C38 C39 1.396(6) . ? C38 H49 0.9500 . ? C39 C40 1.478(7) . ? C41 C42 1.481(6) . ? C43 C44 1.387(7) . ? C43 H50 0.9500 . ? C44 C45 1.363(6) . ? C44 H51 0.9500 . ? C45 H52 0.9500 . ? C46 C47 1.379(7) . ? C46 H53 0.9500 . ? C47 C48 1.395(8) . ? C47 H54 0.9500 . ? C48 H55 0.9500 . ? C49 C50 1.481(6) . ? C51 C52 1.469(5) . ? C52 C53 1.383(6) . ? C53 C54 1.395(5) . ? C53 H56 0.9500 . ? C54 C55 1.471(6) . ? C56 C57 1.491(7) . ? C58 C59 1.375(8) . ? C58 H57 0.9500 . ? C59 C60 1.387(7) . ? C59 H58 0.9500 . ? C60 H59 0.9500 . ? C61 C62 1.344(8) . ? C61 H60 0.9500 . ? C62 C63 1.432(9) . ? C62 H61 0.9500 . ? C63 H62 0.9500 . ? C64 C65 1.518(6) . ? C66 C67 1.474(5) . ? C67 C68 1.361(6) . ? C68 C69 1.397(6) . ? C68 H63 0.9500 . ? C69 C70 1.465(6) . ? C71 C72 1.462(6) . ? C73 C74 1.320(7) . ? C73 H64 0.9500 . ? C74 C75 1.374(6) . ? C74 H65 0.9500 . ? C75 H66 0.9500 . ? C76 C77 1.382(9) . ? C76 H67 0.9500 . ? C77 C78 1.388(9) . ? C77 H68 0.9500 . ? C78 H69 0.9500 . ? C79 C80 1.520(6) . ? C81 C82 1.472(5) . ? C82 C83 1.384(5) . ? C83 C84 1.390(6) . ? C83 H70 0.9500 . ? C84 C85 1.466(6) . ? C86 C87 1.494(6) . ? C88 C89 1.341(7) . ? C88 H71 0.9500 . ? C89 C90 1.401(6) . ? C89 H72 0.9500 . ? C90 H73 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 N33 Ni1 N4 172.38(15) . . ? N33 Ni1 N31 87.85(13) . . ? N4 Ni1 N31 97.13(12) . . ? N33 Ni1 O7 92.71(17) . . ? N4 Ni1 O7 93.17(14) . . ? N31 Ni1 O7 88.66(15) . . ? N33 Ni1 N36 79.02(14) . . ? N4 Ni1 N36 96.19(13) . . ? N31 Ni1 N36 166.62(13) . . ? O7 Ni1 N36 89.41(15) . . ? N33 Ni1 N1 96.80(17) . . ? N4 Ni1 N1 77.62(13) . . ? N31 Ni1 N1 88.78(14) . . ? O7 Ni1 N1 170.06(14) . . ? N36 Ni1 N1 95.25(14) . . ? N7 Ni2 N16 95.22(13) . . ? N7 Ni2 N12 165.98(13) . . ? N16 Ni2 N12 98.79(13) . . ? N7 Ni2 N9 87.56(13) . . ? N16 Ni2 N9 173.10(14) . . ? N12 Ni2 N9 78.45(13) . . ? N7 Ni2 O8 91.36(14) . . ? N16 Ni2 O8 92.01(13) . . ? N12 Ni2 O8 88.81(14) . . ? N9 Ni2 O8 94.24(14) . . ? N7 Ni2 N13 90.42(14) . . ? N16 Ni2 N13 77.40(13) . . ? N12 Ni2 N13 91.98(14) . . ? N9 Ni2 N13 96.30(14) . . ? O8 Ni2 N13 169.37(13) . . ? N19 Ni3 O9 89.35(14) . . ? N19 Ni3 N21 86.57(13) . . ? O9 Ni3 N21 95.41(15) . . ? N19 Ni3 N28 98.32(13) . . ? O9 Ni3 N28 91.78(14) . . ? N21 Ni3 N28 171.36(14) . . ? N19 Ni3 N25 92.63(13) . . ? O9 Ni3 N25 169.50(15) . . ? N21 Ni3 N25 95.00(15) . . ? N28 Ni3 N25 77.73(14) . . ? N19 Ni3 N24 163.38(14) . . ? O9 Ni3 N24 87.04(14) . . ? N21 Ni3 N24 77.64(14) . . ? N28 Ni3 N24 98.00(13) . . ? N25 Ni3 N24 93.87(13) . . ? N67 Ni4 N40 97.27(13) . . ? N67 Ni4 N69 87.55(13) . . ? N40 Ni4 N69 170.24(13) . . ? N67 Ni4 N72 166.39(14) . . ? N40 Ni4 N72 96.25(13) . . ? N69 Ni4 N72 79.33(13) . . ? N67 Ni4 O17 90.39(13) . . ? N40 Ni4 O17 93.51(14) . . ? N69 Ni4 O17 94.95(14) . . ? N72 Ni4 O17 87.22(14) . . ? N67 Ni4 N37 89.33(13) . . ? N40 Ni4 N37 78.04(13) . . ? N69 Ni4 N37 93.60(13) . . ? N72 Ni4 N37 95.00(14) . . ? O17 Ni4 N37 171.43(13) . . ? N45 Ni5 N52 172.20(14) . . ? N45 Ni5 O18 95.77(14) . . ? N52 Ni5 O18 91.24(13) . . ? N45 Ni5 N43 86.67(13) . . ? N52 Ni5 N43 96.76(13) . . ? O18 Ni5 N43 89.96(13) . . ? N45 Ni5 N48 79.00(14) . . ? N52 Ni5 N48 97.83(14) . . ? O18 Ni5 N48 88.51(14) . . ? N43 Ni5 N48 165.35(14) . . ? N45 Ni5 N49 95.21(14) . . ? N52 Ni5 N49 77.75(14) . . ? O18 Ni5 N49 168.99(14) . . ? N43 Ni5 N49 91.40(13) . . ? N48 Ni5 N49 92.88(14) . . ? O19 Ni6 N57 94.45(18) . . ? O19 Ni6 N64 93.14(15) . . ? N57 Ni6 N64 170.98(16) . . ? O19 Ni6 N55 88.96(14) . . ? N57 Ni6 N55 87.29(13) . . ? N64 Ni6 N55 97.73(12) . . ? O19 Ni6 N60 89.95(14) . . ? N57 Ni6 N60 78.74(14) . . ? N64 Ni6 N60 96.41(13) . . ? N55 Ni6 N60 165.85(13) . . ? O19 Ni6 N61 170.67(16) . . ? N57 Ni6 N61 94.63(17) . . ? N64 Ni6 N61 77.63(14) . . ? N55 Ni6 N61 93.60(14) . . ? N60 Ni6 N61 89.73(14) . . ? O24 Cl1 O23 107.1(3) . . ? O24 Cl1 O22 109.0(4) . . ? O23 Cl1 O22 113.5(4) . . ? O24 Cl1 O21 109.0(3) . . ? O23 Cl1 O21 109.7(3) . . ? O22 Cl1 O21 108.4(4) . . ? O28 Cl2 O25 112.0(5) . . ? O28 Cl2 O26 131.8(10) . . ? O25 Cl2 O26 101.3(7) . . ? O28 Cl2 O27 101.6(7) . . ? O25 Cl2 O27 113.7(5) . . ? O26 Cl2 O27 95.3(5) . . ? O29 Cl3 O30 114.3(4) . . ? O29 Cl3 O31 109.0(3) . . ? O30 Cl3 O31 107.1(4) . . ? O29 Cl3 O32 105.2(3) . . ? O30 Cl3 O32 112.9(5) . . ? O31 Cl3 O32 108.3(4) . . ? O34 Cl4 O33 110.3(2) . . ? O34 Cl4 O35 109.2(2) . . ? O33 Cl4 O35 110.4(2) . . ? O34 Cl4 O36 108.5(3) . . ? O33 Cl4 O36 107.8(2) . . ? O35 Cl4 O36 110.5(3) . . ? O38 Cl5 O39 111.5(3) . . ? O38 Cl5 O37 109.4(3) . . ? O39 Cl5 O37 111.8(3) . . ? O38 Cl5 O40 108.6(3) . . ? O39 Cl5 O40 107.7(3) . . ? O37 Cl5 O40 107.6(3) . . ? O42 Cl6 O44 109.7(3) . . ? O42 Cl6 O41 111.8(3) . . ? O44 Cl6 O41 109.2(2) . . ? O42 Cl6 O43 108.6(2) . . ? O44 Cl6 O43 109.8(2) . . ? O41 Cl6 O43 107.7(3) . . ? O47 Cl7 O46 113.1(3) . . ? O47 Cl7 O45 114.6(3) . . ? O46 Cl7 O45 111.7(3) . . ? O47 Cl7 O48 103.2(3) . . ? O46 Cl7 O48 107.3(3) . . ? O45 Cl7 O48 106.0(3) . . ? O50 Cl8 O51 103.5(5) . . ? O50 Cl8 O52 110.3(5) . . ? O51 Cl8 O52 113.3(5) . . ? O50 Cl8 O49 125.6(7) . . ? O51 Cl8 O49 100.8(5) . . ? O52 Cl8 O49 103.2(3) . . ? O53 Cl9 O54 108.9(6) . . ? O53 Cl9 O55 111.5(3) . . ? O54 Cl9 O55 109.2(4) . . ? O53 Cl9 O56 105.9(4) . . ? O54 Cl9 O56 116.4(7) . . ? O55 Cl9 O56 104.9(5) . . ? C4 N1 C1 115.6(4) . . ? C4 N1 Ni1 115.1(3) . . ? C1 N1 Ni1 129.2(4) . . ? C3 N2 C4 115.3(5) . . ? C5 N3 H1 120.0 . . ? C5 N3 H2 120.0 . . ? H1 N3 H2 120.0 . . ? C5 N4 N5 114.5(3) . . ? C5 N4 Ni1 116.9(3) . . ? N5 N4 Ni1 128.2(2) . . ? C6 N5 N4 119.8(3) . . ? C6 N5 H79 120.1 . . ? N4 N5 H79 120.1 . . ? N7 N6 C7 112.1(3) . . ? N7 N6 H3 124.0 . . ? C7 N6 H3 124.0 . . ? N6 N7 C9 105.0(3) . . ? N6 N7 Ni2 126.6(2) . . ? C9 N7 Ni2 127.7(3) . . ? C10 N8 N9 125.7(4) . . ? C10 N8 H80 117.1 . . ? N9 N8 H80 117.1 . . ? C11 N9 N8 114.5(3) . . ? C11 N9 Ni2 116.4(3) . . ? N8 N9 Ni2 128.9(2) . . ? C11 N10 H4 120.0 . . ? C11 N10 H5 120.0 . . ? H4 N10 H5 120.0 . . ? C12 N11 C13 115.6(4) . . ? C12 N12 C15 115.8(4) . . ? C12 N12 Ni2 114.9(3) . . ? C15 N12 Ni2 129.3(3) . . ? C19 N13 C16 116.7(4) . . ? C19 N13 Ni2 115.3(3) . . ? C16 N13 Ni2 128.0(3) . . ? C18 N14 C19 115.6(4) . . ? C20 N15 H6 120.0 . . ? C20 N15 H7 120.0 . . ? H6 N15 H7 120.0 . . ? C20 N16 N17 114.0(3) . . ? C20 N16 Ni2 117.4(3) . . ? N17 N16 Ni2 128.2(3) . . ? C21 N17 N16 121.5(3) . . ? C21 N17 H81 119.3 . . ? N16 N17 H81 119.3 . . ? N19 N18 C22 111.4(3) . . ? N19 N18 H8 124.3 . . ? C22 N18 H8 124.3 . . ? N18 N19 C24 105.3(3) . . ? N18 N19 Ni3 126.3(2) . . ? C24 N19 Ni3 128.2(3) . . ? C25 N20 N21 125.5(4) . . ? C25 N20 H82 117.2 . . ? N21 N20 H82 117.2 . . ? C26 N21 N20 115.5(4) . . ? C26 N21 Ni3 116.2(3) . . ? N20 N21 Ni3 128.2(3) . . ? C26 N22 H9 120.0 . . ? C26 N22 H10 120.0 . . ? H9 N22 H10 120.0 . . ? C28 N23 C27 114.9(4) . . ? C27 N24 C30 117.3(4) . . ? C27 N24 Ni3 113.8(3) . . ? C30 N24 Ni3 128.7(3) . . ? C34 N25 C31 116.3(4) . . ? C34 N25 Ni3 115.4(3) . . ? C31 N25 Ni3 128.3(3) . . ? C34 N26 C33 113.1(5) . . ? C35 N27 H11 120.0 . . ? C35 N27 H12 120.0 . . ? H11 N27 H12 120.0 . . ? C35 N28 N29 114.5(3) . . ? C35 N28 Ni3 116.4(3) . . ? N29 N28 Ni3 129.0(3) . . ? C36 N29 N28 121.5(3) . . ? C36 N29 H83 119.3 . . ? N28 N29 H83 119.3 . . ? N31 N30 C37 112.2(3) . . ? N31 N30 H13 123.9 . . ? C37 N30 H13 123.9 . . ? N30 N31 C39 105.2(3) . . ? N30 N31 Ni1 126.8(3) . . ? C39 N31 Ni1 127.4(3) . . ? C40 N32 N33 125.6(4) . . ? C40 N32 H84 117.2 . . ? N33 N32 H84 117.2 . . ? C41 N33 N32 115.0(3) . . ? C41 N33 Ni1 116.0(3) . . ? N32 N33 Ni1 128.8(3) . . ? C41 N34 H14 120.0 . . ? C41 N34 H15 120.0 . . ? H14 N34 H15 120.0 . . ? C42 N35 C43 117.1(4) . . ? C42 N36 C45 115.4(4) . . ? C42 N36 Ni1 113.8(3) . . ? C45 N36 Ni1 130.8(3) . . ? C49 N37 C46 117.0(4) . . ? C49 N37 Ni4 114.5(3) . . ? C46 N37 Ni4 128.5(3) . . ? C49 N38 C48 115.6(4) . . ? C50 N39 H16 120.0 . . ? C50 N39 H17 120.0 . . ? H16 N39 H17 120.0 . . ? C50 N40 N41 113.9(3) . . ? C50 N40 Ni4 116.4(3) . . ? N41 N40 Ni4 129.7(3) . . ? C51 N41 N40 121.1(3) . . ? C51 N41 H26 119.4 . . ? N40 N41 H26 119.4 . . ? C52 N42 N43 111.8(3) . . ? C52 N42 H18 124.1 . . ? N43 N42 H18 124.1 . . ? C54 N43 N42 105.4(3) . . ? C54 N43 Ni5 128.9(3) . . ? N42 N43 Ni5 125.4(3) . . ? C55 N44 N45 126.0(4) . . ? C55 N44 H74 117.0 . . ? N45 N44 H74 117.0 . . ? C56 N45 N44 115.0(4) . . ? C56 N45 Ni5 116.1(3) . . ? N44 N45 Ni5 128.8(3) . . ? C56 N46 H19 120.0 . . ? C56 N46 H20 120.0 . . ? H19 N46 H20 120.0 . . ? C57 N47 C58 114.7(5) . . ? C60 N48 C57 115.2(4) . . ? C60 N48 Ni5 131.4(3) . . ? C57 N48 Ni5 113.4(3) . . ? C61 N49 C64 114.0(4) . . ? C61 N49 Ni5 130.2(3) . . ? C64 N49 Ni5 115.7(3) . . ? C64 N50 C63 116.1(5) . . ? C65 N51 H21 120.0 . . ? C65 N51 H22 120.0 . . ? H21 N51 H22 120.0 . . ? C65 N52 N53 114.5(3) . . ? C65 N52 Ni5 117.9(3) . . ? N53 N52 Ni5 127.3(3) . . ? C66 N53 N52 121.3(3) . . ? C66 N53 H75 119.3 . . ? N52 N53 H75 119.3 . . ? N55 N54 C67 111.0(3) . . ? N55 N54 H23 124.5 . . ? C67 N54 H23 124.5 . . ? N54 N55 C69 106.2(3) . . ? N54 N55 Ni6 126.0(2) . . ? C69 N55 Ni6 127.5(3) . . ? C70 N56 N57 125.7(4) . . ? C70 N56 H76 117.1 . . ? N57 N56 H76 117.1 . . ? C71 N57 N56 116.5(4) . . ? C71 N57 Ni6 115.3(3) . . ? N56 N57 Ni6 127.9(3) . . ? C71 N58 H24 120.0 . . ? C71 N58 H25 120.0 . . ? H24 N58 H25 120.0 . . ? C72 N59 C73 115.9(4) . . ? C75 N60 C72 116.1(4) . . ? C75 N60 Ni6 130.9(3) . . ? C72 N60 Ni6 113.0(3) . . ? C76 N61 C79 117.5(4) . . ? C76 N61 Ni6 127.7(4) . . ? C79 N61 Ni6 114.7(3) . . ? C79 N62 C78 115.4(5) . . ? C80 N63 H27 120.0 . . ? C80 N63 H28 120.0 . . ? H27 N63 H28 120.0 . . ? C80 N64 N65 112.9(3) . . ? C80 N64 Ni6 118.1(3) . . ? N65 N64 Ni6 128.5(3) . . ? C81 N65 N64 120.5(3) . . ? C81 N65 H77 119.8 . . ? N64 N65 H77 119.8 . . ? N67 N66 C82 111.7(3) . . ? N67 N66 H29 124.1 . . ? C82 N66 H29 124.1 . . ? N66 N67 C84 105.6(3) . . ? N66 N67 Ni4 126.0(2) . . ? C84 N67 Ni4 127.9(3) . . ? C85 N68 N69 125.9(4) . . ? C85 N68 H78 117.1 . . ? N69 N68 H78 117.1 . . ? C86 N69 N68 115.3(3) . . ? C86 N69 Ni4 116.1(3) . . ? N68 N69 Ni4 128.6(2) . . ? C86 N70 H30 120.0 . . ? C86 N70 H31 120.0 . . ? H30 N70 H31 120.0 . . ? C87 N71 C88 115.6(4) . . ? C87 N72 C90 116.7(4) . . ? C87 N72 Ni4 113.4(3) . . ? C90 N72 Ni4 129.9(3) . . ? N1 C1 C2 119.1(5) . . ? N1 C1 H32 120.5 . . ? C2 C1 H32 120.5 . . ? C3 C2 C1 118.1(5) . . ? C3 C2 H33 120.9 . . ? C1 C2 H33 120.9 . . ? N2 C3 C2 123.8(6) . . ? N2 C3 H34 118.1 . . ? C2 C3 H34 118.1 . . ? N2 C4 N1 128.0(4) . . ? N2 C4 C5 116.7(4) . . ? N1 C4 C5 115.3(4) . . ? N3 C5 N4 125.7(4) . . ? N3 C5 C4 119.5(4) . . ? N4 C5 C4 114.8(3) . . ? O1 C6 N5 123.8(4) . . ? O1 C6 C7 120.5(3) . . ? N5 C6 C7 115.7(3) . . ? N6 C7 C8 107.8(3) . . ? N6 C7 C6 117.9(3) . . ? C8 C7 C6 134.3(3) . . ? C7 C8 C9 104.7(3) . . ? C7 C8 H35 127.6 . . ? C9 C8 H35 127.6 . . ? N7 C9 C8 110.3(4) . . ? N7 C9 C10 125.3(4) . . ? C8 C9 C10 124.3(4) . . ? O2 C10 N8 119.5(4) . . ? O2 C10 C9 116.7(4) . . ? N8 C10 C9 123.7(4) . . ? N9 C11 N10 128.5(4) . . ? N9 C11 C12 114.3(4) . . ? N10 C11 C12 117.2(4) . . ? N11 C12 N12 127.3(4) . . ? N11 C12 C11 116.8(4) . . ? N12 C12 C11 115.9(4) . . ? N11 C13 C14 121.9(4) . . ? N11 C13 H36 119.0 . . ? C14 C13 H36 119.0 . . ? C15 C14 C13 117.7(4) . . ? C15 C14 H37 121.1 . . ? C13 C14 H37 121.1 . . ? N12 C15 C14 121.6(4) . . ? N12 C15 H38 119.2 . . ? C14 C15 H38 119.2 . . ? N13 C16 C17 120.9(5) . . ? N13 C16 H39 119.5 . . ? C17 C16 H39 119.5 . . ? C16 C17 C18 117.2(4) . . ? C16 C17 H40 121.4 . . ? C18 C17 H40 121.4 . . ? N14 C18 C17 121.2(5) . . ? N14 C18 H41 119.4 . . ? C17 C18 H41 119.4 . . ? N13 C19 N14 128.3(4) . . ? N13 C19 C20 116.0(4) . . ? N14 C19 C20 115.7(4) . . ? N15 C20 N16 127.8(4) . . ? N15 C20 C19 118.9(4) . . ? N16 C20 C19 113.3(3) . . ? O3 C21 N17 123.5(3) . . ? O3 C21 C22 120.2(3) . . ? N17 C21 C22 116.2(3) . . ? N18 C22 C23 107.4(3) . . ? N18 C22 C21 117.5(3) . . ? C23 C22 C21 135.1(4) . . ? C22 C23 C24 105.1(3) . . ? C22 C23 H42 127.4 . . ? C24 C23 H42 127.4 . . ? N19 C24 C23 110.7(3) . . ? N19 C24 C25 125.5(4) . . ? C23 C24 C25 123.7(4) . . ? O4 C25 N20 118.5(4) . . ? O4 C25 C24 118.4(4) . . ? N20 C25 C24 123.0(4) . . ? N21 C26 N22 128.4(4) . . ? N21 C26 C27 114.0(4) . . ? N22 C26 C27 117.5(4) . . ? N24 C27 N23 127.0(4) . . ? N24 C27 C26 116.3(4) . . ? N23 C27 C26 116.4(4) . . ? N23 C28 C29 123.5(5) . . ? N23 C28 H43 118.3 . . ? C29 C28 H43 118.3 . . ? C28 C29 C30 117.3(5) . . ? C28 C29 H44 121.3 . . ? C30 C29 H44 121.3 . . ? N24 C30 C29 119.9(5) . . ? N24 C30 H45 120.0 . . ? C29 C30 H45 120.0 . . ? N25 C31 C32 121.3(5) . . ? N25 C31 H46 119.3 . . ? C32 C31 H46 119.3 . . ? C33 C32 C31 117.3(5) . . ? C33 C32 H47 121.3 . . ? C31 C32 H47 121.3 . . ? C32 C33 N26 124.1(5) . . ? C32 C33 H48 118.0 . . ? N26 C33 H48 118.0 . . ? N25 C34 N26 127.8(4) . . ? N25 C34 C35 115.2(4) . . ? N26 C34 C35 116.9(4) . . ? N28 C35 N27 127.6(4) . . ? N28 C35 C34 115.1(4) . . ? N27 C35 C34 117.3(4) . . ? O5 C36 N29 123.9(4) . . ? O5 C36 C37 119.5(4) . . ? N29 C36 C37 116.6(3) . . ? N30 C37 C38 107.0(4) . . ? N30 C37 C36 118.9(3) . . ? C38 C37 C36 134.1(4) . . ? C37 C38 C39 104.7(4) . . ? C37 C38 H49 127.7 . . ? C39 C38 H49 127.7 . . ? N31 C39 C38 110.9(4) . . ? N31 C39 C40 125.3(4) . . ? C38 C39 C40 123.8(4) . . ? O6 C40 N32 119.3(5) . . ? O6 C40 C39 116.5(5) . . ? N32 C40 C39 124.2(4) . . ? N33 C41 N34 129.1(4) . . ? N33 C41 C42 115.3(4) . . ? N34 C41 C42 115.6(4) . . ? N35 C42 N36 126.4(4) . . ? N35 C42 C41 117.9(4) . . ? N36 C42 C41 115.6(4) . . ? N35 C43 C44 121.8(4) . . ? N35 C43 H50 119.1 . . ? C44 C43 H50 119.1 . . ? C45 C44 C43 116.7(4) . . ? C45 C44 H51 121.6 . . ? C43 C44 H51 121.6 . . ? N36 C45 C44 122.6(4) . . ? N36 C45 H52 118.7 . . ? C44 C45 H52 118.7 . . ? N37 C46 C47 120.6(5) . . ? N37 C46 H53 119.7 . . ? C47 C46 H53 119.7 . . ? C46 C47 C48 117.3(5) . . ? C46 C47 H54 121.4 . . ? C48 C47 H54 121.4 . . ? N38 C48 C47 122.3(5) . . ? N38 C48 H55 118.9 . . ? C47 C48 H55 118.9 . . ? N37 C49 N38 127.2(4) . . ? N37 C49 C50 116.0(4) . . ? N38 C49 C50 116.9(4) . . ? N40 C50 N39 127.2(4) . . ? N40 C50 C49 115.0(4) . . ? N39 C50 C49 117.7(4) . . ? O11 C51 N41 122.4(3) . . ? O11 C51 C52 120.1(3) . . ? N41 C51 C52 117.4(3) . . ? N42 C52 C53 107.5(3) . . ? N42 C52 C51 118.9(3) . . ? C53 C52 C51 133.5(4) . . ? C52 C53 C54 103.9(4) . . ? C52 C53 H56 128.0 . . ? C54 C53 H56 128.0 . . ? N43 C54 C53 111.3(4) . . ? N43 C54 C55 125.3(4) . . ? C53 C54 C55 123.3(4) . . ? O12 C55 N44 118.3(4) . . ? O12 C55 C54 118.3(4) . . ? N44 C55 C54 123.4(4) . . ? N45 C56 N46 130.0(5) . . ? N45 C56 C57 115.4(4) . . ? N46 C56 C57 114.5(4) . . ? N47 C57 N48 127.5(4) . . ? N47 C57 C56 116.6(4) . . ? N48 C57 C56 115.9(4) . . ? N47 C58 C59 123.4(5) . . ? N47 C58 H57 118.3 . . ? C59 C58 H57 118.3 . . ? C58 C59 C60 115.3(5) . . ? C58 C59 H58 122.3 . . ? C60 C59 H58 122.3 . . ? N48 C60 C59 123.9(5) . . ? N48 C60 H59 118.1 . . ? C59 C60 H59 118.1 . . ? C62 C61 N49 123.6(5) . . ? C62 C61 H60 118.2 . . ? N49 C61 H60 118.2 . . ? C61 C62 C63 117.1(5) . . ? C61 C62 H61 121.4 . . ? C63 C62 H61 121.4 . . ? N50 C63 C62 120.8(5) . . ? N50 C63 H62 119.6 . . ? C62 C63 H62 119.6 . . ? N50 C64 N49 128.4(4) . . ? N50 C64 C65 117.3(4) . . ? N49 C64 C65 114.3(4) . . ? N51 C65 N52 128.8(4) . . ? N51 C65 C64 117.4(4) . . ? N52 C65 C64 113.8(4) . . ? O13 C66 N53 122.7(3) . . ? O13 C66 C67 120.8(3) . . ? N53 C66 C67 116.4(3) . . ? N54 C67 C68 107.6(3) . . ? N54 C67 C66 118.2(3) . . ? C68 C67 C66 134.1(4) . . ? C67 C68 C69 104.6(4) . . ? C67 C68 H63 127.7 . . ? C69 C68 H63 127.7 . . ? N55 C69 C68 110.5(4) . . ? N55 C69 C70 125.8(4) . . ? C68 C69 C70 123.5(4) . . ? O14 C70 N56 118.6(4) . . ? O14 C70 C69 116.6(4) . . ? N56 C70 C69 124.3(4) . . ? N57 C71 N58 126.9(5) . . ? N57 C71 C72 116.6(4) . . ? N58 C71 C72 116.5(4) . . ? N59 C72 N60 125.9(4) . . ? N59 C72 C71 117.9(4) . . ? N60 C72 C71 116.1(4) . . ? C74 C73 N59 122.1(4) . . ? C74 C73 H64 119.0 . . ? N59 C73 H64 119.0 . . ? C73 C74 C75 118.1(4) . . ? C73 C74 H65 121.0 . . ? C75 C74 H65 121.0 . . ? N60 C75 C74 121.9(4) . . ? N60 C75 H66 119.0 . . ? C74 C75 H66 119.0 . . ? N61 C76 C77 119.9(5) . . ? N61 C76 H67 120.1 . . ? C77 C76 H67 120.1 . . ? C76 C77 C78 117.4(5) . . ? C76 C77 H68 121.3 . . ? C78 C77 H68 121.3 . . ? N62 C78 C77 122.2(6) . . ? N62 C78 H69 118.9 . . ? C77 C78 H69 118.9 . . ? N62 C79 N61 127.6(4) . . ? N62 C79 C80 117.1(4) . . ? N61 C79 C80 115.3(4) . . ? N64 C80 N63 128.0(4) . . ? N64 C80 C79 114.3(3) . . ? N63 C80 C79 117.7(4) . . ? O15 C81 N65 124.4(4) . . ? O15 C81 C82 120.5(3) . . ? N65 C81 C82 115.1(3) . . ? N66 C82 C83 107.4(3) . . ? N66 C82 C81 118.4(3) . . ? C83 C82 C81 134.2(4) . . ? C82 C83 C84 104.8(4) . . ? C82 C83 H70 127.6 . . ? C84 C83 H70 127.6 . . ? N67 C84 C83 110.4(3) . . ? N67 C84 C85 125.4(4) . . ? C83 C84 C85 124.1(4) . . ? O16 C85 N68 118.0(4) . . ? O16 C85 C84 118.1(4) . . ? N68 C85 C84 123.8(4) . . ? N69 C86 N70 128.9(4) . . ? N69 C86 C87 114.7(4) . . ? N70 C86 C87 116.4(4) . . ? N71 C87 N72 126.1(4) . . ? N71 C87 C86 117.5(4) . . ? N72 C87 C86 116.5(4) . . ? N71 C88 C89 124.0(4) . . ? N71 C88 H71 118.0 . . ? C89 C88 H71 118.0 . . ? C88 C89 C90 117.3(4) . . ? C88 C89 H72 121.4 . . ? C90 C89 H72 121.4 . . ? N72 C90 C89 120.4(4) . . ? N72 C90 H73 119.8 . . ? C89 C90 H73 119.8 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.834 _refine_diff_density_min -1.073 _refine_diff_density_rms 0.092 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 0.117 0.345 -0.017 5405 700 ' ' _platon_squeeze_details ; ; data_Compound10-Unsqueezed _database_code_depnum_ccdc_archive 'CCDC 706536' # start Validation Reply Form _vrf_PLAT306_Compound10-Unsqueezed ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O35 RESPONSE: This is a lattice solvent molecule (water) for which the corresponding protons could not be located in the difference map, and hence were omitted from the model (though they were included in the reported formula). ; _vrf_PLAT430_Compound10-Unsqueezed ; PROBLEM: Short Inter D...A Contact O36 .. O38 .. 1.90 Ang. RESPONSE: These are partial occupancy lattice solvent (water) molecules. The sum of their occupancies does not exceed one. ; _vrf_PLAT601_Compound10-Unsqueezed ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 278.00 A**3 RESPONSE: This model contains a very large number of partial occupancy lattice water molecules. While an attempt was made to model the lattice water content, residual water peaks were still present. All lattice water molecules were subsequently removed and the structure was Squeezed to better treat these regions of disperse electron density. The .cif for this model is also provided. ; # 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)8 Cu12 Na1.525] (N O3)9.525 (H2 O)8.3' _chemical_formula_sum 'C144 H128.60 Cu12 N89.525 Na1.525 O52.875' _chemical_formula_weight 4756.76 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' 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 20.114(3) _cell_length_b 21.693(3) _cell_length_c 24.540(3) _cell_angle_alpha 95.631(2) _cell_angle_beta 101.818(2) _cell_angle_gamma 101.020(3) _cell_volume 10182(2) _cell_formula_units_Z 2 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 33130 _cell_measurement_theta_min 2.5401 _cell_measurement_theta_max 30.6692 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4814.14 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9271 _exptl_absorpt_correction_T_min 0.7913 _exptl_absorpt_process_details '(T. Higashi, 2000)' _exptl_special_details ; Note that only six nitrates could be unambiguously identified from the difference map, though 9.525 are required for charge balance. The model contains a very large number of partial occupancy lattice water molecules, and electron density from these regions was used to represent the 'missing' 3.525 nitrate anions in the reported formula. ; _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 100148 _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.50 _reflns_number_total 42008 _reflns_number_gt 29615 _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^)+(0.2000P)^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 42008 _refine_ls_number_parameters 2702 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1788 _refine_ls_R_factor_gt 0.1466 _refine_ls_wR_factor_ref 0.4339 _refine_ls_wR_factor_gt 0.4067 _refine_ls_goodness_of_fit_ref 1.446 _refine_ls_restrained_S_all 1.447 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.62836(7) 0.42511(6) 0.11877(5) 0.0532(3) Uani 1 1 d . . . Cu2 Cu 0.70897(7) 0.30964(6) 0.02090(5) 0.0492(3) Uani 1 1 d . . . Cu3 Cu 0.84344(6) 0.26297(6) -0.05238(5) 0.0479(3) Uani 1 1 d . . . Cu4 Cu 1.02234(7) 0.28013(7) -0.07507(5) 0.0566(3) Uani 1 1 d . . . Cu5 Cu 1.10170(6) 0.27188(6) 0.07792(5) 0.0458(3) Uani 1 1 d . . . Cu6 Cu 1.12882(6) 0.18669(5) 0.20628(4) 0.0432(3) Uani 1 1 d . . . Cu7 Cu 1.11900(6) 0.04302(5) 0.29303(5) 0.0458(3) Uani 1 1 d . . . Cu8 Cu 0.92180(6) 0.01831(5) 0.30327(5) 0.0451(3) Uani 1 1 d . . . Cu9 Cu 0.77665(6) 0.05658(5) 0.36991(5) 0.0439(3) Uani 1 1 d . . . Cu10 Cu 0.68840(7) 0.15557(6) 0.47455(5) 0.0537(3) Uani 1 1 d . . . Cu11 Cu 0.73589(7) 0.29969(7) 0.40155(6) 0.0600(4) Uani 1 1 d . . . Cu12 Cu 0.71268(7) 0.39269(7) 0.27795(6) 0.0601(4) Uani 1 1 d . . . Na1 Na 0.7957(7) 0.2804(7) 0.1742(6) 0.049(3) Uani 0.25 1 d P . . Na2 Na 0.9194(16) 0.2452(14) 0.1119(12) 0.050(7) Uiso 0.13 1 d P . . Na3 Na 0.8104(4) 0.2062(4) 0.2826(3) 0.0515(18) Uani 0.50 1 d P . . Na4 Na 0.9374(3) 0.1777(3) 0.2246(2) 0.0448(12) Uani 0.65 1 d P . . O1 O 0.7000(4) 0.3922(3) 0.0747(3) 0.0520(17) Uani 1 1 d . . . O2 O 0.9360(3) 0.3125(3) -0.0511(3) 0.0505(16) Uani 1 1 d . . . O3 O 0.7844(4) 0.3604(4) 0.2472(4) 0.078(2) Uani 1 1 d . . . O4 O 1.0217(3) 0.2983(3) 0.1007(3) 0.0508(16) Uani 1 1 d . . . O5 O 0.8057(4) 0.2673(4) 0.3688(3) 0.065(2) Uani 1 1 d . . . O6 O 1.0510(3) 0.2114(3) 0.2326(3) 0.0530(16) Uani 1 1 d . . . O7 O 0.7664(3) 0.1208(3) 0.4417(3) 0.0475(15) Uani 1 1 d . . . O8 O 1.0210(3) 0.0514(3) 0.3322(2) 0.0468(15) Uani 1 1 d . . . O9 O 0.6438(4) 0.3797(3) 0.1965(3) 0.0560(17) Uani 1 1 d . . . O10 O 0.6764(4) 0.2191(3) 0.4082(3) 0.0509(16) Uani 1 1 d . . . O11 O 0.7311(3) 0.2642(3) 0.0855(3) 0.0532(17) Uani 1 1 d . . . O12 O 0.7674(3) 0.1070(3) 0.3090(3) 0.0477(15) Uani 1 1 d . . . O13 O 0.8678(4) 0.2250(3) 0.0161(3) 0.0544(17) Uani 1 1 d . . . O14 O 0.9149(4) 0.0744(3) 0.2442(3) 0.0521(16) Uani 1 1 d . . . O15 O 1.0537(4) 0.2353(3) 0.0023(2) 0.0466(15) Uani 1 1 d . . . O16 O 1.1019(3) 0.0897(3) 0.2260(3) 0.0457(14) Uani 1 1 d . . . O17 O 1.4379(6) 0.3341(6) 0.3628(6) 0.154(6) Uani 1 1 d . . . O18 O 1.4773(8) 0.2724(8) 0.4150(8) 0.167(6) Uani 1 1 d . . . O19 O 1.5063(6) 0.2833(8) 0.3368(7) 0.184(9) Uani 1 1 d . . . O20 O 1.2599(9) 0.4877(9) 0.1328(8) 0.179(8) Uani 1 1 d . . . O21 O 1.3651(7) 0.4709(6) 0.1504(6) 0.130(4) Uani 1 1 d . . . O22 O 1.3074(7) 0.4551(6) 0.0643(6) 0.121(4) Uani 1 1 d . . . O23 O 0.7558(7) 0.1038(9) -0.3113(5) 0.171(7) Uani 1 1 d . . . O24 O 0.6547(6) 0.0899(8) -0.3044(5) 0.149(6) Uani 1 1 d . . . O25 O 0.7380(5) 0.0982(5) -0.2306(4) 0.094(3) Uani 1 1 d . . . O26 O 0.8579(7) -0.0559(7) -0.0473(6) 0.136(4) Uiso 1 1 d D . . O27 O 0.8261(10) -0.0281(9) 0.0259(7) 0.202(7) Uiso 1 1 d D . . O28 O 0.8751(8) -0.1056(7) 0.0259(6) 0.151(5) Uiso 1 1 d D . . O29 O 0.4661(9) -0.2077(8) 0.2787(7) 0.171(6) Uiso 1 1 d D . . O30 O 0.5471(8) -0.2085(8) 0.3413(7) 0.173(6) Uiso 1 1 d D . . O31 O 0.4925(8) -0.2980(7) 0.2971(6) 0.155(5) Uiso 1 1 d D . . O32 O 0.8022(9) -0.2903(8) 0.2644(7) 0.166(6) Uiso 1 1 d D . . O33 O 0.9122(9) -0.2535(8) 0.2631(7) 0.171(6) Uiso 1 1 d D . . O34 O 0.8509(11) -0.1989(10) 0.2420(9) 0.228(9) Uiso 1 1 d D . . O35 O 0.4580(5) -0.1129(5) 0.3735(4) 0.090(3) Uani 1 1 d . . . O36 O 1.0522(8) 0.0383(7) 0.4714(6) 0.088(4) Uiso 0.65 1 d P . . O37 O 0.5171(4) 0.0249(4) 0.2477(3) 0.074(2) Uani 1 1 d . . . O38 O 0.9728(7) 0.0326(6) 0.4915(5) 0.121(4) Uiso 1 1 d . . . O39 O 0.8566(6) -0.1009(5) 0.1347(5) 0.107(3) Uani 1 1 d . . . O40 O 0.4533(5) 0.0819(5) 0.1625(4) 0.103(3) Uani 1 1 d . . . O41 O 0.3774(6) 0.2153(8) -0.0759(8) 0.140(7) Uani 0.75 1 d P . . O42 O 0.5340(7) -0.1277(7) 0.1817(5) 0.097(4) Uani 0.70 1 d P . . O43 O 0.5706(6) 0.0900(5) -0.2313(4) 0.109(3) Uani 1 1 d . . . O44 O 1.3225(7) 0.0022(5) 0.1618(6) 0.074(3) Uani 0.65 1 d P . . O45 O 1.1029(8) 0.4415(6) 0.2182(5) 0.135(4) Uani 1 1 d . . . O46 O 1.4059(6) 0.3987(6) 0.2608(5) 0.127(4) Uani 1 1 d . . . O47 O 1.1269(9) 0.5327(6) 0.0916(6) 0.172(7) Uani 1 1 d . . . O48 O 0.7965(6) 0.0420(6) -0.0833(5) 0.090(3) Uani 0.80 1 d P . . O49 O 0.4755(11) 0.1406(7) 0.0708(6) 0.129(7) Uani 0.70 1 d P . . O50 O 0.9235(8) 0.5518(7) 0.2198(8) 0.107(6) Uani 0.65 1 d P . . O51 O 1.3773(7) 0.2656(9) 0.4826(8) 0.152(7) Uani 0.80 1 d P . . O52 O 0.8187(14) 0.6844(10) 0.4245(12) 0.071(8) Uani 0.30 1 d P . . O53 O 0.4973(10) 0.6073(9) 0.3855(12) 0.131(10) Uani 0.50 1 d P . . O54 O 1.0702 0.5352 0.1941 0.162 Uiso 0.50 1 d P . . O55 O 1.0256(14) 0.4776(9) 0.3594(7) 0.161(9) Uani 0.65 1 d P . . O56 O 1.4042(12) 0.5116(10) 0.3317(12) 0.168(10) Uani 0.65 1 d P . . O57 O 1.1641(13) 0.4204(12) 0.2873(8) 0.176(11) Uani 0.65 1 d P . . O58 O 1.2729(11) 0.3736(9) 0.4273(8) 0.127(6) Uani 0.65 1 d P . . O59 O 1.1835(17) 0.2788(14) 0.5075(13) 0.195(14) Uani 0.60 1 d P . . O60 O 1.4092(17) 0.4250(14) 0.4249(12) 0.133(10) Uani 0.50 1 d P . . O61 O 1.4181(18) 0.4041(16) 0.4675(14) 0.172(17) Uani 0.50 1 d P . . O62 O 0.6694(13) -0.2406(12) 0.2367(10) 0.118(7) Uiso 0.50 1 d P . . O63 O 0.5731(18) -0.0319(11) 0.1291(9) 0.174(15) Uani 0.50 1 d P . . O64 O 0.6483(10) 0.0553(10) -0.0297(10) 0.157(8) Uani 0.70 1 d P . . O65 O 0.8275(13) 0.4150(12) 0.6563(10) 0.124(8) Uiso 0.50 1 d P . . N1 N 0.5957(5) 0.4937(4) 0.1732(4) 0.054(2) Uani 1 1 d . . . N2 N 0.7742(7) 0.5853(5) 0.2027(5) 0.089(4) Uani 1 1 d . . . H1 H 0.8125 0.5824 0.1915 0.107 Uiso 1 1 calc R . . H2 H 0.7747 0.6162 0.2289 0.107 Uiso 1 1 calc R . . N3 N 0.7081(5) 0.4929(4) 0.1391(3) 0.056(2) Uani 1 1 d . . . N4 N 0.7691(5) 0.4890(4) 0.1210(4) 0.061(2) Uani 1 1 d . . . N5 N 0.8021(4) 0.3701(4) 0.0294(3) 0.0463(18) Uani 1 1 d . . . N6 N 0.8491(4) 0.3540(4) 0.0019(3) 0.0443(18) Uani 1 1 d . . . N7 N 1.0229(5) 0.4000(5) -0.0094(4) 0.061(2) Uani 1 1 d . . . N8 N 1.0615(5) 0.3663(4) -0.0381(4) 0.058(2) Uani 1 1 d . . . N9 N 1.1629(5) 0.4381(4) 0.0127(4) 0.070(3) Uani 1 1 d . . . H3 H 1.1395 0.4596 0.0311 0.084 Uiso 1 1 calc R . . H4 H 1.2085 0.4498 0.0193 0.084 Uiso 1 1 calc R . . N10 N 1.1283(5) 0.2935(4) -0.0838(3) 0.053(2) Uani 1 1 d . . . N11 N 0.6736(5) 0.4490(4) 0.3276(4) 0.057(2) Uani 1 1 d . . . N12 N 0.8257(8) 0.5659(6) 0.3478(7) 0.128(5) Uani 1 1 d . . . H5 H 0.8670 0.5704 0.3401 0.153 Uiso 1 1 calc R . . H6 H 0.8152 0.5974 0.3674 0.153 Uiso 1 1 calc R . . N13 N 0.7866(5) 0.4606(5) 0.3006(4) 0.075(3) Uani 1 1 d . . . N14 N 0.8445(6) 0.4578(6) 0.2766(5) 0.101(4) Uani 1 1 d . . . N15 N 0.8670(6) 0.3437(5) 0.1725(5) 0.085(3) Uani 1 1 d . . . N16 N 0.9167(7) 0.3274(6) 0.1464(5) 0.094(4) Uani 1 1 d . . . N17 N 1.1061(5) 0.3504(4) 0.1777(4) 0.058(2) Uani 1 1 d . . . N18 N 1.1470(5) 0.3257(4) 0.1457(4) 0.060(2) Uani 1 1 d . . . N19 N 1.2519(6) 0.3734(5) 0.2120(4) 0.075(3) Uani 1 1 d . . . H7 H 1.2304 0.3891 0.2362 0.090 Uiso 1 1 calc R . . H8 H 1.2976 0.3801 0.2201 0.090 Uiso 1 1 calc R . . N20 N 1.2021(5) 0.2757(4) 0.0748(4) 0.054(2) Uani 1 1 d . . . N21 N 0.6943(5) 0.3575(5) 0.4490(4) 0.061(2) Uani 1 1 d . . . N22 N 0.8495(9) 0.4740(8) 0.4604(7) 0.129(5) Uiso 1 1 d . . . H9 H 0.8829 0.4770 0.4420 0.155 Uiso 1 1 calc R . . H10 H 0.8457 0.5074 0.4820 0.155 Uiso 1 1 calc R . . N23 N 0.8082(5) 0.3678(5) 0.4241(5) 0.080(3) Uani 1 1 d . . . N24 N 0.8705(5) 0.3650(6) 0.4051(6) 0.094(4) Uani 1 1 d . . . N25 N 0.9061(5) 0.2387(7) 0.3189(5) 0.093(4) Uani 1 1 d . . . N26 N 0.9570(5) 0.2230(6) 0.2961(4) 0.088(3) Uani 1 1 d . . . N27 N 1.1422(4) 0.2705(4) 0.3062(3) 0.0444(17) Uani 1 1 d . . . N28 N 1.1786(4) 0.2442(4) 0.2714(3) 0.0474(18) Uani 1 1 d . . . N29 N 1.2872(4) 0.2971(4) 0.3279(4) 0.053(2) Uani 1 1 d . . . H11 H 1.2691 0.3146 0.3535 0.064 Uiso 1 1 calc R . . H12 H 1.3327 0.3046 0.3320 0.064 Uiso 1 1 calc R . . N30 N 1.2256(4) 0.1887(3) 0.1976(3) 0.0433(17) Uani 1 1 d . . . N31 N 0.6480(5) 0.2137(4) 0.5293(4) 0.063(2) Uani 1 1 d . . . N32 N 0.8260(6) 0.2989(5) 0.5834(4) 0.079(3) Uani 1 1 d . . . H13 H 0.8668 0.2967 0.5765 0.095 Uiso 1 1 calc R . . H14 H 0.8226 0.3300 0.6079 0.095 Uiso 1 1 calc R . . N33 N 0.7721(5) 0.2081(4) 0.5204(3) 0.051(2) Uani 1 1 d . . . N34 N 0.8360(5) 0.2071(4) 0.5059(3) 0.0491(19) Uani 1 1 d . . . N35 N 0.8758(4) 0.1028(4) 0.4027(3) 0.0430(17) Uani 1 1 d . . . N36 N 0.9258(4) 0.0889(3) 0.3795(3) 0.0403(16) Uani 1 1 d . . . N37 N 1.1050(4) 0.1364(4) 0.3858(3) 0.0495(19) Uani 1 1 d . . . N38 N 1.1498(4) 0.1128(4) 0.3560(3) 0.0444(18) Uani 1 1 d . . . N39 N 1.2357(5) 0.1932(4) 0.4180(3) 0.060(2) Uani 1 1 d . . . H15 H 1.2049 0.2042 0.4356 0.071 Uiso 1 1 calc R . . H16 H 1.2796 0.2133 0.4287 0.071 Uiso 1 1 calc R . . N40 N 1.2388(4) 0.0749(4) 0.3041(3) 0.0472(19) Uani 1 1 d . . . N41 N 0.5685(5) 0.4305(5) 0.0322(3) 0.061(2) Uani 1 1 d . . . N42 N 0.4820(5) 0.2713(5) 0.0327(4) 0.065(2) Uani 1 1 d . . . H17 H 0.4832 0.2430 0.0560 0.079 Uiso 1 1 calc R . . H18 H 0.4560 0.2606 -0.0018 0.079 Uiso 1 1 calc R . . N43 N 0.5585(5) 0.3478(4) 0.1000(3) 0.053(2) Uani 1 1 d . . . N44 N 0.5552(4) 0.3022(4) 0.1364(3) 0.051(2) Uani 1 1 d . . . N45 N 0.6501(4) 0.3070(4) 0.2761(3) 0.0406(16) Uani 1 1 d . . . N46 N 0.6551(4) 0.2756(4) 0.3194(3) 0.0449(19) Uani 1 1 d . . . N47 N 0.5907(5) 0.1300(4) 0.3640(3) 0.053(2) Uani 1 1 d . . . N48 N 0.6103(4) 0.1081(4) 0.4165(3) 0.050(2) Uani 1 1 d . . . N49 N 0.5322(5) 0.0145(4) 0.3750(4) 0.060(2) Uani 1 1 d . . . H19 H 0.5209 0.0291 0.3430 0.072 Uiso 1 1 calc R . . H20 H 0.5126 -0.0243 0.3787 0.072 Uiso 1 1 calc R . . N50 N 0.6488(5) 0.0670(4) 0.5098(4) 0.057(2) Uani 1 1 d . . . N51 N 0.6632(5) 0.3232(4) -0.0574(4) 0.054(2) Uani 1 1 d . . . N52 N 0.5380(5) 0.1787(5) -0.0609(4) 0.075(3) Uani 1 1 d . . . H21 H 0.5310 0.1499 -0.0386 0.090 Uiso 1 1 calc R . . H22 H 0.5105 0.1740 -0.0946 0.090 Uiso 1 1 calc R . . N53 N 0.6320(5) 0.2395(5) 0.0043(3) 0.057(2) Uani 1 1 d . . . N54 N 0.6259(5) 0.1968(4) 0.0439(3) 0.059(2) Uani 1 1 d . . . N55 N 0.7304(6) 0.2125(5) 0.1840(5) 0.080(3) Uani 1 1 d . . . N56 N 0.7377(5) 0.1803(5) 0.2298(4) 0.071(3) Uani 1 1 d . . . N57 N 0.6648(4) 0.0318(4) 0.2738(3) 0.0485(19) Uani 1 1 d . . . N58 N 0.6914(4) 0.0103(4) 0.3231(3) 0.0491(19) Uani 1 1 d . . . N59 N 0.6069(5) -0.0862(5) 0.3008(4) 0.071(3) Uani 1 1 d . . . H23 H 0.5856 -0.0768 0.2686 0.085 Uiso 1 1 calc R . . H24 H 0.5916 -0.1227 0.3117 0.085 Uiso 1 1 calc R . . N60 N 0.7635(4) -0.0209(4) 0.4110(3) 0.0512(19) Uani 1 1 d . . . N61 N 0.7928(4) 0.2740(4) -0.1291(3) 0.0507(19) Uani 1 1 d . . . N62 N 0.6626(5) 0.1372(5) -0.1233(4) 0.068(3) Uani 1 1 d . . . H25 H 0.6547 0.1117 -0.0985 0.082 Uiso 1 1 calc R . . H26 H 0.6332 0.1319 -0.1562 0.082 Uiso 1 1 calc R . . N63 N 0.7659(4) 0.1966(4) -0.0641(3) 0.0473(18) Uani 1 1 d . . . N64 N 0.7635(5) 0.1562(4) -0.0225(3) 0.053(2) Uani 1 1 d . . . N65 N 0.8901(7) 0.1677(5) 0.1096(4) 0.083(3) Uani 1 1 d . . . N66 N 0.8970(8) 0.1374(5) 0.1545(4) 0.092(4) Uani 1 1 d . . . N67 N 0.8096(4) 0.0023(4) 0.2099(3) 0.0515(19) Uani 1 1 d . . . N68 N 0.8318(4) -0.0209(4) 0.2576(3) 0.0499(19) Uani 1 1 d . . . N69 N 0.7386(6) -0.1105(5) 0.2373(4) 0.080(3) Uani 1 1 d . . . H27 H 0.7168 -0.0972 0.2074 0.096 Uiso 1 1 calc R . . H28 H 0.7204 -0.1468 0.2471 0.096 Uiso 1 1 calc R . . N70 N 0.9032(5) -0.0609(4) 0.3405(3) 0.0505(19) Uani 1 1 d . . . N71 N 0.9730(5) 0.2768(4) -0.1611(4) 0.060(2) Uani 1 1 d . . . N72 N 0.8719(4) 0.1218(4) -0.1503(3) 0.057(2) Uani 1 1 d . . . H29 H 0.8708 0.0954 -0.1254 0.069 Uiso 1 1 calc R . . H30 H 0.8401 0.1135 -0.1821 0.069 Uiso 1 1 calc R . . N73 N 0.9722(4) 0.1919(4) -0.0938(3) 0.052(2) Uani 1 1 d . . . N74 N 0.9713(5) 0.1499(4) -0.0539(3) 0.054(2) Uani 1 1 d . . . N75 N 1.0624(4) 0.1688(4) 0.0869(3) 0.0426(17) Uani 1 1 d . . . N76 N 1.0724(4) 0.1388(4) 0.1329(3) 0.0439(17) Uani 1 1 d . . . N77 N 1.0310(4) -0.0087(4) 0.1834(3) 0.0452(17) Uani 1 1 d . . . N78 N 1.0592(4) -0.0229(4) 0.2361(3) 0.0444(17) Uani 1 1 d . . . N79 N 0.9745(5) -0.1176(4) 0.2203(3) 0.056(2) Uani 1 1 d . . . H31 H 0.9535 -0.1100 0.1873 0.067 Uiso 1 1 calc R . . H32 H 0.9585 -0.1526 0.2331 0.067 Uiso 1 1 calc R . . N80 N 1.1156(5) -0.0340(4) 0.3355(3) 0.052(2) Uani 1 1 d . . . N81 N 1.4762(7) 0.2986(7) 0.3689(7) 0.099(4) Uani 1 1 d . . . N82 N 1.3116(10) 0.4693(7) 0.1132(8) 0.126(6) Uani 1 1 d . . . N83 N 0.7154(6) 0.0993(6) -0.2832(5) 0.089(4) Uani 1 1 d . . . N84 N 0.8468(7) -0.0695(6) -0.0030(5) 0.100(4) Uiso 1 1 d D . . N85 N 0.5040(7) -0.2390(6) 0.3007(6) 0.098(4) Uiso 1 1 d D . . N86 N 0.8534(10) -0.2518(10) 0.2543(9) 0.165(7) Uiso 1 1 d D . . C1 C 0.5368(7) 0.4901(6) 0.1880(5) 0.071(3) Uani 1 1 d . . . H33 H 0.5001 0.4548 0.1708 0.085 Uiso 1 1 calc R . . C2 C 0.5240(9) 0.5335(8) 0.2267(6) 0.084(4) Uani 1 1 d . . . H34 H 0.4800 0.5285 0.2363 0.101 Uiso 1 1 calc R . . C3 C 0.5767(12) 0.5843(8) 0.2508(6) 0.110(6) Uani 1 1 d . . . H35 H 0.5685 0.6165 0.2761 0.131 Uiso 1 1 calc R . . C4 C 0.6448(7) 0.5899(6) 0.2387(5) 0.074(3) Uani 1 1 d . . . H36 H 0.6836 0.6230 0.2567 0.088 Uiso 1 1 calc R . . C5 C 0.6473(7) 0.5416(6) 0.1978(5) 0.063(3) Uani 1 1 d . . . C6 C 0.7122(7) 0.5405(5) 0.1787(5) 0.061(3) Uani 1 1 d . . . C7 C 0.7583(6) 0.4368(6) 0.0893(4) 0.056(3) Uani 1 1 d . . . C8 C 0.8165(6) 0.4241(5) 0.0627(5) 0.056(3) Uani 1 1 d . . . C9 C 0.8830(6) 0.4649(5) 0.0755(5) 0.061(3) Uani 1 1 d . . . H37 H 0.8933 0.5027 0.1016 0.074 Uiso 1 1 calc R . . C10 C 0.9307(6) 0.4488(5) 0.0499(5) 0.062(3) Uani 1 1 d . . . H38 H 0.9759 0.4751 0.0567 0.075 Uiso 1 1 calc R . . C11 C 0.9118(6) 0.3918(5) 0.0127(4) 0.049(2) Uani 1 1 d . . . C12 C 0.9606(5) 0.3667(5) -0.0177(4) 0.051(2) Uani 1 1 d . . . C13 C 1.1297(5) 0.3883(5) -0.0247(5) 0.056(3) Uani 1 1 d . . . C14 C 1.1684(6) 0.3489(5) -0.0563(4) 0.056(3) Uani 1 1 d . . . C15 C 1.2350(6) 0.3693(7) -0.0573(6) 0.076(4) Uani 1 1 d . . . H39 H 1.2615 0.4094 -0.0382 0.092 Uiso 1 1 calc R . . C16 C 1.2640(9) 0.3266(10) -0.0892(7) 0.105(6) Uani 1 1 d . . . H40 H 1.3112 0.3382 -0.0915 0.125 Uiso 1 1 calc R . . C17 C 1.2244(10) 0.2697(9) -0.1162(6) 0.095(5) Uani 1 1 d . . . H41 H 1.2435 0.2402 -0.1360 0.114 Uiso 1 1 calc R . . C18 C 1.1553(9) 0.2563(7) -0.1137(5) 0.083(4) Uani 1 1 d . . . H42 H 1.1261 0.2182 -0.1347 0.100 Uiso 1 1 calc R . . C19 C 0.6094(7) 0.4357(7) 0.3388(6) 0.084(4) Uani 1 1 d . . . H43 H 0.5784 0.3963 0.3230 0.100 Uiso 1 1 calc R . . C20 C 0.5892(8) 0.4794(8) 0.3732(6) 0.088(4) Uani 1 1 d . . . H44 H 0.5435 0.4718 0.3794 0.105 Uiso 1 1 calc R . . C21 C 0.6387(9) 0.5359(8) 0.3990(6) 0.089(5) Uani 1 1 d . . . H45 H 0.6289 0.5641 0.4268 0.107 Uiso 1 1 calc R . . C22 C 0.6975(7) 0.5483(7) 0.3840(6) 0.096(5) Uani 1 1 d . . . H46 H 0.7265 0.5896 0.3945 0.115 Uiso 1 1 calc R . . C23 C 0.7186(7) 0.5014(5) 0.3526(6) 0.079(4) Uani 1 1 d . . . C24 C 0.7803(7) 0.5129(6) 0.3304(7) 0.085(4) Uani 1 1 d . . . C25 C 0.8381(6) 0.4013(5) 0.2528(5) 0.060(3) Uani 1 1 d . . . C26 C 0.8910(6) 0.3841(5) 0.2246(5) 0.062(3) Uani 1 1 d . . . C27 C 0.9564(6) 0.4048(6) 0.2477(5) 0.075(4) Uani 1 1 d . . . H47 H 0.9700 0.4321 0.2826 0.090 Uiso 1 1 calc R . . C28 C 1.0057(6) 0.3882(6) 0.2229(5) 0.073(4) Uani 1 1 d . . . H48 H 1.0536 0.4029 0.2407 0.088 Uiso 1 1 calc R . . C29 C 0.9874(6) 0.3526(5) 0.1756(4) 0.055(2) Uani 1 1 d . . . C30 C 1.0395(6) 0.3315(5) 0.1481(4) 0.050(2) Uani 1 1 d . . . C31 C 1.2153(5) 0.3396(4) 0.1635(4) 0.047(2) Uani 1 1 d . . . C32 C 1.2504(6) 0.3111(4) 0.1228(4) 0.051(2) Uani 1 1 d . . . C33 C 1.3192(6) 0.3180(5) 0.1278(5) 0.060(3) Uani 1 1 d . . . H49 H 1.3507 0.3436 0.1598 0.072 Uiso 1 1 calc R . . C34 C 1.3439(8) 0.2890(7) 0.0879(7) 0.082(4) Uani 1 1 d . . . H50 H 1.3926 0.2923 0.0925 0.099 Uiso 1 1 calc R . . C35 C 1.2995(8) 0.2552(7) 0.0414(6) 0.085(5) Uani 1 1 d . . . H51 H 1.3176 0.2377 0.0121 0.101 Uiso 1 1 calc R . . C36 C 1.2253(7) 0.2448(6) 0.0346(5) 0.078(4) Uani 1 1 d . . . H52 H 1.1942 0.2175 0.0034 0.094 Uiso 1 1 calc R . . C37 C 0.6308(6) 0.3421(7) 0.4617(5) 0.076(4) Uani 1 1 d . . . H53 H 0.6015 0.3014 0.4479 0.092 Uiso 1 1 calc R . . C38 C 0.6098(8) 0.3858(7) 0.4945(6) 0.074(3) Uani 1 1 d . . . H54 H 0.5629 0.3777 0.4982 0.089 Uiso 1 1 calc R . . C39 C 0.6505(9) 0.4364(10) 0.5201(7) 0.106(6) Uani 1 1 d . . . H55 H 0.6386 0.4613 0.5492 0.128 Uiso 1 1 calc R . . C40 C 0.7200(9) 0.4571(9) 0.5031(8) 0.138(8) Uani 1 1 d . . . H56 H 0.7477 0.4990 0.5132 0.165 Uiso 1 1 calc R . . C41 C 0.7382(6) 0.4102(6) 0.4725(5) 0.070(3) Uani 1 1 d . . . C42 C 0.8035(8) 0.4173(7) 0.4555(9) 0.120(7) Uani 1 1 d . . . C43 C 0.8627(6) 0.3116(5) 0.3793(4) 0.052(2) Uani 1 1 d . . . C44 C 0.9192(5) 0.2939(5) 0.3565(5) 0.054(2) Uani 1 1 d . . . C45 C 0.9815(7) 0.3312(6) 0.3693(8) 0.108(6) Uani 1 1 d . . . H57 H 0.9900 0.3699 0.3939 0.130 Uiso 1 1 calc R . . C46 C 1.0340(6) 0.3150(6) 0.3476(7) 0.099(6) Uani 1 1 d . . . H58 H 1.0797 0.3406 0.3596 0.119 Uiso 1 1 calc R . . C47 C 1.0217(5) 0.2649(5) 0.3106(4) 0.047(2) Uani 1 1 d . . . C48 C 1.0746(5) 0.2483(5) 0.2802(4) 0.050(2) Uani 1 1 d . . . C49 C 1.2459(5) 0.2592(5) 0.2827(4) 0.045(2) Uani 1 1 d . . . C50 C 1.2755(5) 0.2255(4) 0.2407(4) 0.047(2) Uani 1 1 d . . . C51 C 1.3457(5) 0.2301(5) 0.2429(4) 0.056(3) Uani 1 1 d . . . H59 H 1.3792 0.2574 0.2728 0.067 Uiso 1 1 calc R . . C52 C 1.3675(6) 0.1959(6) 0.2024(5) 0.063(3) Uani 1 1 d . . . H60 H 1.4155 0.1974 0.2044 0.076 Uiso 1 1 calc R . . C53 C 1.3164(6) 0.1593(5) 0.1588(5) 0.057(3) Uani 1 1 d . . . H61 H 1.3290 0.1357 0.1294 0.068 Uiso 1 1 calc R . . C54 C 1.2465(6) 0.1569(5) 0.1577(5) 0.058(3) Uani 1 1 d . . . H62 H 1.2124 0.1313 0.1272 0.070 Uiso 1 1 calc R . . C55 C 0.5838(7) 0.2111(7) 0.5341(6) 0.083(4) Uani 1 1 d . . . H63 H 0.5462 0.1807 0.5101 0.099 Uiso 1 1 calc R . . C56 C 0.5718(11) 0.2559(9) 0.5772(8) 0.106(7) Uani 1 1 d . . . H64 H 0.5252 0.2550 0.5800 0.127 Uiso 1 1 calc R . . C57 C 0.6220(10) 0.2976(8) 0.6125(7) 0.089(5) Uani 1 1 d . . . H65 H 0.6110 0.3250 0.6404 0.107 Uiso 1 1 calc R . . C58 C 0.6915(8) 0.3021(6) 0.6092(5) 0.077(4) Uani 1 1 d . . . H66 H 0.7290 0.3328 0.6329 0.092 Uiso 1 1 calc R . . C59 C 0.7012(7) 0.2547(6) 0.5654(5) 0.065(3) Uani 1 1 d . . . C60 C 0.7718(6) 0.2569(5) 0.5581(4) 0.053(3) Uani 1 1 d . . . C61 C 0.8249(6) 0.1604(5) 0.4653(4) 0.050(2) Uani 1 1 d . . . C62 C 0.8882(5) 0.1527(4) 0.4450(3) 0.0376(18) Uani 1 1 d . . . C63 C 0.9545(5) 0.1895(5) 0.4652(4) 0.048(2) Uani 1 1 d . . . H67 H 0.9633 0.2238 0.4947 0.058 Uiso 1 1 calc R . . C64 C 1.0075(5) 0.1758(4) 0.4422(4) 0.048(2) Uani 1 1 d . . . H68 H 1.0539 0.1998 0.4548 0.057 Uiso 1 1 calc R . . C65 C 0.9887(5) 0.1239(4) 0.3986(3) 0.045(2) Uani 1 1 d . . . C66 C 1.0416(5) 0.1014(4) 0.3692(4) 0.043(2) Uani 1 1 d . . . C67 C 1.2159(5) 0.1459(5) 0.3750(4) 0.049(2) Uani 1 1 d . . . C68 C 1.2667(6) 0.1232(5) 0.3473(4) 0.053(3) Uani 1 1 d . . . C69 C 1.3383(5) 0.1507(5) 0.3653(4) 0.056(3) Uani 1 1 d . . . H69 H 1.3556 0.1837 0.3963 0.067 Uiso 1 1 calc R . . C70 C 1.3829(7) 0.1273(6) 0.3354(5) 0.067(3) Uani 1 1 d . . . H70 H 1.4317 0.1436 0.3463 0.080 Uiso 1 1 calc R . . C71 C 1.3550(7) 0.0804(7) 0.2901(6) 0.076(4) Uani 1 1 d . . . H71 H 1.3843 0.0643 0.2690 0.091 Uiso 1 1 calc R . . C72 C 1.2809(6) 0.0558(5) 0.2750(5) 0.058(3) Uani 1 1 d . . . H72 H 1.2618 0.0246 0.2427 0.069 Uiso 1 1 calc R . . C73 C 0.5788(6) 0.4750(6) -0.0014(5) 0.067(3) Uani 1 1 d . . . H73 H 0.6120 0.5135 0.0131 0.081 Uiso 1 1 calc R . . C74 C 0.5420(9) 0.4656(8) -0.0567(6) 0.088(5) Uani 1 1 d . . . H74 H 0.5505 0.4978 -0.0795 0.106 Uiso 1 1 calc R . . C75 C 0.4948(7) 0.4125(7) -0.0786(5) 0.074(4) Uani 1 1 d . . . H75 H 0.4695 0.4070 -0.1166 0.088 Uiso 1 1 calc R . . C76 C 0.4830(6) 0.3654(6) -0.0457(4) 0.063(3) Uani 1 1 d . . . H76 H 0.4492 0.3272 -0.0601 0.076 Uiso 1 1 calc R . . C77 C 0.5228(5) 0.3759(5) 0.0102(4) 0.052(2) Uani 1 1 d . . . C78 C 0.5187(5) 0.3291(6) 0.0490(4) 0.052(2) Uani 1 1 d . . . C79 C 0.6016(5) 0.3257(5) 0.1841(4) 0.046(2) Uani 1 1 d . . . C80 C 0.6039(5) 0.2829(5) 0.2291(4) 0.049(2) Uani 1 1 d . . . C81 C 0.5616(5) 0.2201(5) 0.2208(4) 0.052(2) Uani 1 1 d . . . H77 H 0.5298 0.2025 0.1860 0.063 Uiso 1 1 calc R . . C82 C 0.5688(5) 0.1873(5) 0.2643(4) 0.046(2) Uani 1 1 d . . . H78 H 0.5426 0.1453 0.2615 0.056 Uiso 1 1 calc R . . C83 C 0.6156(5) 0.2166(5) 0.3134(4) 0.045(2) Uani 1 1 d . . . C84 C 0.6283(5) 0.1863(4) 0.3666(4) 0.044(2) Uani 1 1 d . . . C85 C 0.5768(6) 0.0492(6) 0.4159(5) 0.061(3) Uani 1 1 d . . . C86 C 0.5991(5) 0.0274(5) 0.4718(4) 0.052(2) Uani 1 1 d . . . C87 C 0.5689(7) -0.0306(6) 0.4858(5) 0.069(3) Uani 1 1 d . . . H79 H 0.5328 -0.0595 0.4590 0.083 Uiso 1 1 calc R . . C88 C 0.5915(7) -0.0458(6) 0.5382(5) 0.067(3) Uani 1 1 d . . . H80 H 0.5720 -0.0856 0.5476 0.080 Uiso 1 1 calc R . . C89 C 0.6412(8) -0.0042(7) 0.5762(6) 0.082(4) Uani 1 1 d . . . H81 H 0.6571 -0.0136 0.6130 0.098 Uiso 1 1 calc R . . C90 C 0.6676(6) 0.0506(6) 0.5609(5) 0.062(3) Uani 1 1 d . . . H82 H 0.7023 0.0802 0.5882 0.075 Uiso 1 1 calc R . . C91 C 0.6810(7) 0.3697(5) -0.0874(4) 0.067(3) Uani 1 1 d . . . H83 H 0.7224 0.4009 -0.0715 0.080 Uiso 1 1 calc R . . C92 C 0.6455(10) 0.3750(7) -0.1366(6) 0.091(5) Uani 1 1 d . . . H84 H 0.6606 0.4095 -0.1554 0.109 Uiso 1 1 calc R . . C93 C 0.5879(12) 0.3317(9) -0.1603(6) 0.113(8) Uani 1 1 d . . . H85 H 0.5617 0.3360 -0.1961 0.136 Uiso 1 1 calc R . . C94 C 0.5640(8) 0.2780(8) -0.1332(5) 0.091(5) Uani 1 1 d . . . H86 H 0.5241 0.2457 -0.1504 0.110 Uiso 1 1 calc R . . C95 C 0.6046(7) 0.2776(6) -0.0796(4) 0.066(3) Uani 1 1 d . . . C96 C 0.5891(5) 0.2283(6) -0.0440(5) 0.057(3) Uani 1 1 d . . . C97 C 0.6822(4) 0.2173(4) 0.0843(4) 0.042(2) Uani 1 1 d . . . C98 C 0.6868(5) 0.1833(5) 0.1348(4) 0.053(2) Uani 1 1 d . . . C99 C 0.6481(5) 0.1246(5) 0.1313(4) 0.046(2) Uani 1 1 d . . . H87 H 0.6164 0.1055 0.0968 0.056 Uiso 1 1 calc R . . C100 C 0.6531(5) 0.0929(4) 0.1746(4) 0.045(2) Uani 1 1 d . . . H88 H 0.6245 0.0519 0.1715 0.053 Uiso 1 1 calc R . . C101 C 0.6994(5) 0.1191(5) 0.2236(4) 0.053(2) Uani 1 1 d . . . C102 C 0.7118(5) 0.0836(5) 0.2713(4) 0.048(2) Uani 1 1 d . . . C103 C 0.6623(5) -0.0452(6) 0.3330(4) 0.056(3) Uani 1 1 d . . . C104 C 0.7026(5) -0.0620(5) 0.3883(4) 0.049(2) Uani 1 1 d . . . C105 C 0.6804(7) -0.1115(6) 0.4125(5) 0.074(3) Uani 1 1 d . . . H89 H 0.6359 -0.1384 0.3972 0.088 Uiso 1 1 calc R . . C106 C 0.7219(7) -0.1230(6) 0.4593(5) 0.072(3) Uani 1 1 d . . . H90 H 0.7067 -0.1591 0.4762 0.086 Uiso 1 1 calc R . . C107 C 0.7841(7) -0.0849(5) 0.4826(5) 0.065(3) Uani 1 1 d . . . H91 H 0.8137 -0.0936 0.5151 0.078 Uiso 1 1 calc R . . C108 C 0.8036(6) -0.0318(5) 0.4571(4) 0.057(3) Uani 1 1 d . . . H92 H 0.8466 -0.0029 0.4733 0.069 Uiso 1 1 calc R . . C109 C 0.8092(6) 0.3208(5) -0.1608(5) 0.062(3) Uani 1 1 d . . . H93 H 0.8506 0.3525 -0.1469 0.074 Uiso 1 1 calc R . . C110 C 0.7682(6) 0.3232(6) -0.2113(5) 0.069(3) Uani 1 1 d . . . H94 H 0.7808 0.3560 -0.2326 0.083 Uiso 1 1 calc R . . C111 C 0.7086(7) 0.2777(6) -0.2312(5) 0.071(3) Uani 1 1 d . . . H95 H 0.6803 0.2781 -0.2673 0.085 Uiso 1 1 calc R . . C112 C 0.6892(6) 0.2321(5) -0.2000(4) 0.057(3) Uani 1 1 d . . . H96 H 0.6465 0.2017 -0.2129 0.068 Uiso 1 1 calc R . . C113 C 0.7328(6) 0.2310(5) -0.1496(4) 0.049(2) Uani 1 1 d . . . C114 C 0.7181(6) 0.1833(5) -0.1112(4) 0.056(3) Uani 1 1 d . . . C115 C 0.8208(5) 0.1781(5) 0.0169(4) 0.046(2) Uani 1 1 d . . . C116 C 0.8308(6) 0.1444(5) 0.0674(4) 0.055(3) Uani 1 1 d . . . C117 C 0.7825(5) 0.0953(5) 0.0719(4) 0.051(2) Uani 1 1 d . . . H97 H 0.7419 0.0813 0.0423 0.061 Uiso 1 1 calc R . . C118 C 0.7893(5) 0.0653(5) 0.1161(4) 0.055(3) Uani 1 1 d . . . H98 H 0.7540 0.0304 0.1187 0.066 Uiso 1 1 calc R . . C119 C 0.8460(6) 0.0846(5) 0.1571(4) 0.052(2) Uani 1 1 d . . . C120 C 0.8568(5) 0.0509(5) 0.2061(4) 0.050(2) Uani 1 1 d . . . C121 C 0.8003(5) -0.0752(5) 0.2684(4) 0.054(2) Uani 1 1 d . . . C122 C 0.8395(6) -0.0968(5) 0.3191(4) 0.058(3) Uani 1 1 d . . . C123 C 0.8123(8) -0.1508(5) 0.3418(5) 0.070(3) Uani 1 1 d . . . H99 H 0.7669 -0.1759 0.3260 0.085 Uiso 1 1 calc R . . C124 C 0.8542(8) -0.1651(6) 0.3871(6) 0.081(4) Uani 1 1 d . . . H100 H 0.8383 -0.2012 0.4037 0.097 Uiso 1 1 calc R . . C125 C 0.9214(8) -0.1270(6) 0.4102(4) 0.074(4) Uani 1 1 d . . . H101 H 0.9512 -0.1368 0.4420 0.089 Uiso 1 1 calc R . . C126 C 0.9415(6) -0.0761(5) 0.3850(4) 0.053(2) Uani 1 1 d . . . H102 H 0.9863 -0.0497 0.4006 0.063 Uiso 1 1 calc R . . C127 C 0.9797(7) 0.3217(6) -0.1945(5) 0.075(3) Uani 1 1 d . . . H103 H 1.0140 0.3599 -0.1819 0.089 Uiso 1 1 calc R . . C128 C 0.9342(11) 0.3111(9) -0.2500(8) 0.112(7) Uani 1 1 d . . . H104 H 0.9386 0.3429 -0.2739 0.134 Uiso 1 1 calc R . . C129 C 0.8846(9) 0.2555(8) -0.2687(5) 0.080(4) Uani 1 1 d . . . H105 H 0.8544 0.2486 -0.3050 0.096 Uiso 1 1 calc R . . C130 C 0.8804(7) 0.2114(6) -0.2338(5) 0.067(3) Uani 1 1 d . . . H106 H 0.8470 0.1725 -0.2450 0.081 Uiso 1 1 calc R . . C131 C 0.9259(5) 0.2239(5) -0.1808(4) 0.051(2) Uani 1 1 d . . . C132 C 0.9221(5) 0.1749(5) -0.1399(4) 0.048(2) Uani 1 1 d . . . C133 C 1.0156(5) 0.1771(5) -0.0074(4) 0.049(2) Uani 1 1 d . . . C134 C 1.0211(5) 0.1380(5) 0.0394(4) 0.046(2) Uani 1 1 d . . . C135 C 0.9837(6) 0.0748(5) 0.0344(4) 0.056(3) Uani 1 1 d . . . H107 H 0.9523 0.0544 0.0002 0.068 Uiso 1 1 calc R . . C136 C 0.9946(6) 0.0434(5) 0.0814(4) 0.058(3) Uani 1 1 d . . . H108 H 0.9715 0.0005 0.0798 0.069 Uiso 1 1 calc R . . C137 C 1.0406(5) 0.0770(4) 0.1312(4) 0.046(2) Uani 1 1 d . . . C138 C 1.0584(5) 0.0511(4) 0.1834(4) 0.046(2) Uani 1 1 d . . . C139 C 1.0307(5) -0.0763(4) 0.2508(4) 0.044(2) Uani 1 1 d . . . C140 C 1.0670(6) -0.0855(5) 0.3085(4) 0.051(2) Uani 1 1 d . . . C141 C 1.0535(6) -0.1403(5) 0.3316(4) 0.056(3) Uani 1 1 d . . . H109 H 1.0180 -0.1754 0.3119 0.067 Uiso 1 1 calc R . . C142 C 1.0934(7) -0.1433(5) 0.3851(4) 0.064(3) Uani 1 1 d . . . H110 H 1.0867 -0.1812 0.4016 0.077 Uiso 1 1 calc R . . C143 C 1.1403(7) -0.0926(5) 0.4120(5) 0.063(3) Uani 1 1 d . . . H111 H 1.1663 -0.0935 0.4488 0.076 Uiso 1 1 calc R . . C144 C 1.1523(6) -0.0377(5) 0.3872(4) 0.054(2) Uani 1 1 d . . . H112 H 1.1871 -0.0021 0.4071 0.065 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 0.0717(9) 0.0559(7) 0.0415(6) 0.0128(5) 0.0191(6) 0.0274(7) Cu2 0.0521(7) 0.0506(7) 0.0478(6) 0.0129(5) 0.0104(5) 0.0161(6) Cu3 0.0483(7) 0.0517(7) 0.0467(6) 0.0121(5) 0.0144(5) 0.0115(6) Cu4 0.0474(7) 0.0765(9) 0.0460(7) 0.0121(6) 0.0163(6) 0.0057(6) Cu5 0.0481(7) 0.0505(7) 0.0422(6) 0.0105(5) 0.0165(5) 0.0106(5) Cu6 0.0416(6) 0.0447(6) 0.0423(6) 0.0091(5) 0.0100(5) 0.0049(5) Cu7 0.0507(7) 0.0469(6) 0.0412(6) 0.0144(5) 0.0113(5) 0.0089(5) Cu8 0.0481(7) 0.0459(6) 0.0410(6) 0.0083(5) 0.0119(5) 0.0060(5) Cu9 0.0444(6) 0.0451(6) 0.0420(6) 0.0084(5) 0.0110(5) 0.0072(5) Cu10 0.0675(8) 0.0552(7) 0.0494(7) 0.0178(6) 0.0263(6) 0.0209(7) Cu11 0.0484(7) 0.0631(8) 0.0680(8) -0.0049(6) 0.0169(6) 0.0145(6) Cu12 0.0499(8) 0.0624(8) 0.0651(8) -0.0125(6) 0.0166(6) 0.0126(6) Na1 0.029(7) 0.058(9) 0.050(8) -0.011(7) -0.001(6) 0.006(7) Na3 0.057(5) 0.056(5) 0.040(4) -0.001(3) 0.012(3) 0.011(4) Na4 0.047(3) 0.045(3) 0.037(3) 0.000(2) 0.001(2) 0.007(3) O1 0.056(4) 0.060(4) 0.052(4) 0.013(3) 0.021(3) 0.028(4) O2 0.044(4) 0.045(4) 0.068(4) 0.016(3) 0.024(3) 0.010(3) O3 0.058(5) 0.072(5) 0.095(6) -0.031(5) 0.026(4) 0.000(4) O4 0.038(4) 0.060(4) 0.056(4) 0.014(3) 0.013(3) 0.010(3) O5 0.043(4) 0.075(5) 0.070(5) -0.017(4) 0.016(4) 0.009(4) O6 0.030(3) 0.070(5) 0.052(4) -0.003(3) 0.005(3) 0.003(3) O7 0.040(4) 0.062(4) 0.047(4) 0.012(3) 0.018(3) 0.018(3) O8 0.049(4) 0.053(4) 0.037(3) 0.006(3) 0.008(3) 0.011(3) O9 0.060(4) 0.056(4) 0.059(4) 0.022(3) 0.023(4) 0.013(4) O10 0.049(4) 0.059(4) 0.054(4) 0.026(3) 0.021(3) 0.015(3) O11 0.044(4) 0.061(4) 0.051(4) 0.024(3) 0.000(3) 0.006(3) O12 0.041(4) 0.055(4) 0.043(3) 0.014(3) 0.005(3) 0.003(3) O13 0.053(4) 0.053(4) 0.050(4) 0.016(3) 0.007(3) -0.003(3) O14 0.056(4) 0.058(4) 0.037(3) 0.009(3) 0.008(3) 0.003(3) O15 0.061(4) 0.048(4) 0.038(3) 0.011(3) 0.022(3) 0.015(3) O16 0.051(4) 0.038(3) 0.045(3) 0.012(3) 0.006(3) 0.005(3) O17 0.078(7) 0.143(11) 0.210(14) -0.086(10) -0.015(8) 0.058(8) O18 0.113(11) 0.171(15) 0.197(17) 0.052(13) 0.011(11) -0.006(10) O19 0.079(8) 0.203(15) 0.232(17) -0.133(13) 0.061(10) -0.005(9) O20 0.124(12) 0.227(19) 0.220(18) 0.141(16) 0.049(12) 0.055(13) O21 0.106(9) 0.124(10) 0.156(11) 0.082(9) -0.002(8) 0.017(8) O22 0.101(9) 0.138(11) 0.101(8) -0.003(8) 0.014(7) -0.006(7) O23 0.099(10) 0.30(2) 0.076(8) -0.041(10) 0.008(7) -0.004(11) O24 0.074(8) 0.262(18) 0.089(8) -0.011(9) -0.022(6) 0.045(9) O25 0.075(6) 0.097(7) 0.088(7) -0.013(5) -0.022(5) 0.022(5) O35 0.090(7) 0.082(6) 0.091(6) 0.031(5) 0.007(5) 0.007(5) O37 0.066(5) 0.086(6) 0.068(5) 0.020(4) 0.017(4) 0.006(4) O39 0.127(9) 0.069(6) 0.111(8) 0.010(5) 0.014(7) 0.003(6) O40 0.083(7) 0.113(8) 0.102(7) 0.032(6) 0.002(6) 0.009(6) O41 0.045(7) 0.124(12) 0.219(18) -0.065(12) -0.015(9) 0.035(8) O42 0.064(8) 0.131(13) 0.075(8) -0.015(8) -0.004(7) 0.002(8) O43 0.112(8) 0.099(8) 0.086(7) 0.016(6) 0.001(6) -0.025(6) O44 0.078(9) 0.046(6) 0.100(9) 0.013(6) 0.025(7) 0.008(6) O45 0.162(12) 0.112(10) 0.125(10) 0.020(8) 0.015(9) 0.032(9) O46 0.071(7) 0.156(11) 0.126(9) -0.028(8) 0.009(6) -0.007(7) O47 0.247(18) 0.071(7) 0.146(11) -0.038(7) -0.039(11) 0.025(9) O48 0.087(8) 0.080(8) 0.098(8) 0.024(6) 0.029(7) -0.008(6) O49 0.21(2) 0.067(9) 0.086(10) 0.034(8) 0.019(11) -0.012(11) O50 0.072(9) 0.061(8) 0.201(18) 0.028(10) 0.058(11) 0.012(7) O51 0.056(8) 0.208(18) 0.172(15) -0.012(13) 0.058(9) -0.034(9) O52 0.081(18) 0.033(12) 0.11(2) 0.030(13) 0.053(17) 0.006(12) O53 0.066(12) 0.070(12) 0.24(3) -0.037(15) 0.005(15) 0.038(11) O55 0.27(3) 0.086(12) 0.083(11) -0.024(9) -0.002(14) -0.013(15) O56 0.155(19) 0.106(14) 0.29(3) 0.025(17) 0.14(2) 0.049(14) O57 0.18(2) 0.20(2) 0.100(13) -0.069(14) -0.063(13) 0.078(19) O58 0.152(17) 0.106(13) 0.126(14) -0.022(11) 0.066(13) 0.019(12) O59 0.26(3) 0.18(2) 0.24(3) 0.10(2) 0.17(3) 0.15(3) O60 0.14(2) 0.11(2) 0.11(2) -0.019(17) 0.03(2) -0.036(16) O61 0.16(3) 0.16(3) 0.16(3) -0.10(2) 0.10(3) -0.05(2) O63 0.29(4) 0.092(16) 0.086(14) -0.043(12) 0.09(2) -0.106(19) O64 0.098(14) 0.134(16) 0.22(2) 0.011(16) 0.019(14) 0.009(12) N1 0.072(6) 0.041(5) 0.055(5) 0.009(4) 0.015(5) 0.020(4) N2 0.114(10) 0.060(6) 0.095(8) -0.010(6) 0.048(8) 0.007(7) N3 0.070(6) 0.054(5) 0.049(5) 0.006(4) 0.021(4) 0.018(5) N4 0.086(7) 0.048(5) 0.061(5) 0.012(4) 0.038(5) 0.015(5) N5 0.052(5) 0.041(4) 0.049(4) 0.013(3) 0.011(4) 0.012(4) N6 0.043(4) 0.052(5) 0.047(4) 0.021(4) 0.018(4) 0.019(4) N7 0.060(6) 0.075(6) 0.061(5) 0.017(5) 0.028(5) 0.022(5) N8 0.048(5) 0.066(6) 0.065(5) 0.018(4) 0.019(4) 0.011(4) N9 0.056(6) 0.054(6) 0.089(7) -0.009(5) 0.013(5) 0.000(5) N10 0.066(6) 0.052(5) 0.047(4) 0.015(4) 0.024(4) 0.012(4) N11 0.062(6) 0.060(5) 0.056(5) 0.005(4) 0.019(4) 0.028(5) N12 0.134(13) 0.076(9) 0.158(14) -0.004(9) 0.053(11) -0.026(8) N13 0.068(6) 0.062(6) 0.086(7) -0.028(5) 0.043(6) -0.016(5) N14 0.071(7) 0.099(9) 0.118(10) -0.052(7) 0.045(7) -0.012(6) N15 0.077(7) 0.067(7) 0.114(9) -0.006(6) 0.047(7) 0.005(6) N16 0.106(10) 0.078(8) 0.109(9) 0.006(7) 0.065(8) 0.012(7) N17 0.057(5) 0.065(6) 0.059(5) 0.006(4) 0.021(4) 0.022(5) N18 0.044(5) 0.066(6) 0.069(6) 0.000(4) 0.020(4) 0.007(4) N19 0.073(7) 0.058(6) 0.086(7) 0.008(5) 0.019(6) -0.007(5) N20 0.054(5) 0.056(5) 0.058(5) 0.020(4) 0.023(4) 0.012(4) N21 0.057(6) 0.075(6) 0.059(5) 0.009(5) 0.017(4) 0.028(5) N23 0.055(6) 0.070(7) 0.105(8) -0.035(6) 0.036(6) -0.002(5) N24 0.053(6) 0.087(8) 0.135(10) -0.032(7) 0.032(7) 0.012(6) N25 0.047(6) 0.138(11) 0.081(7) -0.033(7) 0.025(5) 0.003(6) N26 0.052(6) 0.127(10) 0.071(7) -0.012(6) 0.016(5) -0.004(6) N27 0.039(4) 0.050(4) 0.043(4) 0.005(3) 0.011(3) 0.006(3) N28 0.030(4) 0.059(5) 0.053(5) 0.011(4) 0.015(3) 0.002(4) N29 0.033(4) 0.052(5) 0.065(5) -0.001(4) 0.004(4) 0.000(4) N30 0.052(5) 0.042(4) 0.038(4) 0.009(3) 0.017(3) 0.007(4) N31 0.072(7) 0.052(5) 0.070(6) 0.024(5) 0.017(5) 0.021(5) N32 0.097(8) 0.069(7) 0.062(6) -0.016(5) 0.009(6) 0.019(6) N33 0.068(6) 0.045(4) 0.049(4) 0.016(4) 0.023(4) 0.022(4) N34 0.068(6) 0.041(4) 0.045(4) 0.016(3) 0.015(4) 0.019(4) N35 0.040(4) 0.044(4) 0.043(4) 0.011(3) 0.008(3) 0.005(3) N36 0.039(4) 0.034(4) 0.048(4) 0.012(3) 0.012(3) 0.004(3) N37 0.054(5) 0.060(5) 0.042(4) 0.020(4) 0.018(4) 0.016(4) N38 0.045(4) 0.048(4) 0.046(4) 0.017(3) 0.015(4) 0.016(4) N39 0.044(5) 0.072(6) 0.053(5) 0.003(4) 0.008(4) -0.004(4) N40 0.054(5) 0.043(4) 0.052(5) 0.020(4) 0.016(4) 0.018(4) N41 0.074(6) 0.076(6) 0.040(4) 0.015(4) 0.009(4) 0.033(5) N42 0.055(6) 0.075(7) 0.060(5) 0.010(5) 0.014(4) -0.003(5) N43 0.057(5) 0.066(5) 0.051(5) 0.021(4) 0.027(4) 0.026(5) N44 0.051(5) 0.067(5) 0.043(4) 0.012(4) 0.020(4) 0.017(4) N45 0.041(4) 0.046(4) 0.040(4) 0.012(3) 0.014(3) 0.012(3) N46 0.055(5) 0.050(4) 0.048(4) 0.026(4) 0.031(4) 0.024(4) N47 0.064(6) 0.053(5) 0.053(5) 0.024(4) 0.024(4) 0.016(4) N48 0.055(5) 0.045(4) 0.061(5) 0.022(4) 0.025(4) 0.019(4) N49 0.071(6) 0.052(5) 0.057(5) 0.025(4) 0.005(5) 0.016(5) N50 0.069(6) 0.063(5) 0.052(5) 0.027(4) 0.029(5) 0.022(5) N51 0.058(5) 0.051(5) 0.054(5) 0.010(4) 0.008(4) 0.018(4) N52 0.073(7) 0.084(7) 0.053(5) -0.001(5) -0.002(5) 0.001(6) N53 0.056(5) 0.077(6) 0.042(4) 0.024(4) 0.011(4) 0.017(5) N54 0.057(5) 0.071(6) 0.047(5) 0.011(4) 0.011(4) 0.010(5) N55 0.074(7) 0.068(7) 0.096(8) 0.032(6) 0.015(6) 0.006(6) N56 0.059(6) 0.080(7) 0.073(6) 0.020(5) 0.019(5) 0.005(5) N57 0.049(5) 0.046(4) 0.054(5) 0.017(4) 0.014(4) 0.011(4) N58 0.056(5) 0.051(5) 0.042(4) 0.010(4) 0.020(4) 0.006(4) N59 0.069(7) 0.071(6) 0.073(6) 0.020(5) 0.023(5) 0.005(5) N60 0.051(5) 0.058(5) 0.045(4) 0.010(4) 0.012(4) 0.012(4) N61 0.050(5) 0.056(5) 0.045(4) 0.004(4) 0.005(4) 0.016(4) N62 0.061(6) 0.066(6) 0.062(6) 0.009(5) -0.011(5) 0.002(5) N63 0.057(5) 0.044(4) 0.040(4) 0.008(3) 0.008(4) 0.012(4) N64 0.057(5) 0.053(5) 0.047(4) 0.005(4) 0.011(4) 0.010(4) N65 0.128(10) 0.068(7) 0.058(6) 0.023(5) 0.020(6) 0.027(7) N66 0.140(11) 0.067(7) 0.058(6) 0.006(5) 0.007(7) 0.014(7) N67 0.045(5) 0.046(5) 0.058(5) 0.004(4) 0.003(4) 0.009(4) N68 0.051(5) 0.049(5) 0.043(4) 0.005(3) 0.011(4) -0.004(4) N69 0.080(7) 0.070(6) 0.076(7) 0.022(5) 0.018(6) -0.026(5) N70 0.068(6) 0.034(4) 0.048(4) 0.000(3) 0.022(4) 0.004(4) N71 0.073(6) 0.057(5) 0.062(5) 0.016(4) 0.033(5) 0.020(5) N72 0.048(5) 0.070(6) 0.047(5) 0.000(4) 0.005(4) 0.008(4) N73 0.052(5) 0.063(5) 0.041(4) 0.011(4) 0.011(4) 0.008(4) N74 0.071(6) 0.058(5) 0.037(4) 0.008(4) 0.015(4) 0.019(5) N75 0.047(4) 0.046(4) 0.035(4) 0.012(3) 0.009(3) 0.007(4) N76 0.046(4) 0.049(4) 0.037(4) 0.007(3) 0.009(3) 0.011(4) N77 0.050(5) 0.043(4) 0.043(4) 0.013(3) 0.008(3) 0.010(4) N78 0.054(5) 0.040(4) 0.044(4) 0.010(3) 0.019(4) 0.011(4) N79 0.071(6) 0.034(4) 0.054(5) 0.008(4) 0.006(4) -0.002(4) N80 0.073(6) 0.052(5) 0.033(4) 0.006(3) 0.011(4) 0.021(4) N81 0.076(9) 0.097(10) 0.108(10) -0.008(8) 0.007(8) 0.004(8) N82 0.113(13) 0.091(10) 0.134(14) 0.055(10) -0.043(12) -0.015(9) N83 0.063(7) 0.117(10) 0.071(7) -0.027(6) 0.010(6) 0.008(7) C1 0.086(9) 0.069(8) 0.073(8) 0.032(6) 0.030(7) 0.029(7) C2 0.101(11) 0.109(12) 0.065(8) 0.025(8) 0.045(8) 0.047(10) C3 0.18(2) 0.092(11) 0.071(9) -0.007(8) 0.050(11) 0.064(13) C4 0.082(9) 0.062(7) 0.078(8) -0.017(6) 0.022(7) 0.029(7) C5 0.090(9) 0.062(7) 0.055(6) 0.019(5) 0.029(6) 0.039(7) C6 0.089(9) 0.048(6) 0.059(6) 0.012(5) 0.038(6) 0.022(6) C7 0.064(7) 0.067(7) 0.050(6) 0.029(5) 0.024(5) 0.026(6) C8 0.061(7) 0.054(6) 0.068(7) 0.026(5) 0.030(6) 0.023(5) C9 0.064(7) 0.055(6) 0.079(7) 0.008(5) 0.042(6) 0.019(5) C10 0.064(7) 0.053(6) 0.066(7) 0.013(5) 0.022(6) -0.008(5) C11 0.063(6) 0.040(5) 0.048(5) 0.009(4) 0.020(5) 0.009(5) C12 0.040(5) 0.047(6) 0.061(6) 0.006(5) 0.007(5) 0.002(4) C13 0.045(6) 0.056(6) 0.073(7) 0.024(5) 0.017(5) 0.016(5) C14 0.060(7) 0.070(7) 0.059(6) 0.037(6) 0.026(5) 0.032(6) C15 0.055(7) 0.092(9) 0.092(9) 0.036(8) 0.034(7) 0.009(7) C16 0.093(12) 0.157(17) 0.118(13) 0.073(13) 0.065(11) 0.087(13) C17 0.136(16) 0.108(13) 0.061(8) 0.018(8) 0.020(9) 0.075(12) C18 0.105(11) 0.100(11) 0.066(8) 0.032(7) 0.039(8) 0.042(9) C19 0.055(7) 0.099(10) 0.093(9) -0.019(8) 0.025(7) 0.014(7) C20 0.090(10) 0.112(12) 0.071(8) -0.009(8) 0.024(8) 0.052(10) C21 0.117(12) 0.099(11) 0.078(9) 0.002(8) 0.056(9) 0.055(10) C22 0.080(9) 0.081(9) 0.116(11) -0.053(8) 0.045(9) 0.001(7) C23 0.084(9) 0.048(6) 0.110(10) -0.011(6) 0.062(8) -0.006(6) C24 0.074(9) 0.059(7) 0.113(11) -0.004(7) 0.032(8) -0.009(6) C25 0.068(7) 0.043(5) 0.068(7) -0.003(5) 0.036(6) -0.007(5) C26 0.059(7) 0.058(6) 0.071(7) -0.010(5) 0.028(6) 0.010(5) C27 0.041(6) 0.096(9) 0.072(7) -0.044(6) 0.026(5) -0.008(6) C28 0.043(6) 0.097(9) 0.065(7) -0.033(6) 0.028(5) -0.017(6) C29 0.049(6) 0.061(6) 0.053(6) 0.009(5) 0.018(5) 0.001(5) C30 0.058(6) 0.052(6) 0.044(5) 0.009(4) 0.021(5) 0.007(5) C31 0.059(6) 0.030(4) 0.052(5) 0.011(4) 0.015(5) 0.003(4) C32 0.064(7) 0.033(5) 0.060(6) 0.015(4) 0.021(5) 0.009(5) C33 0.050(6) 0.064(7) 0.072(7) 0.024(6) 0.019(5) 0.013(5) C34 0.068(9) 0.085(10) 0.096(10) 0.014(8) 0.029(8) 0.006(7) C35 0.107(12) 0.101(11) 0.084(9) 0.043(8) 0.059(9) 0.059(10) C36 0.106(10) 0.102(10) 0.076(8) 0.044(7) 0.073(8) 0.069(9) C37 0.050(7) 0.098(10) 0.082(8) -0.013(7) 0.034(6) 0.012(6) C38 0.079(9) 0.072(8) 0.086(9) 0.016(7) 0.029(8) 0.037(8) C39 0.096(12) 0.151(17) 0.086(10) -0.010(10) 0.024(9) 0.071(13) C40 0.085(12) 0.135(15) 0.162(17) -0.091(13) 0.003(11) 0.032(11) C41 0.056(7) 0.079(8) 0.071(7) -0.020(6) 0.012(6) 0.021(6) C42 0.063(9) 0.054(8) 0.22(2) -0.050(10) 0.041(11) -0.011(7) C43 0.053(6) 0.042(5) 0.061(6) 0.005(4) 0.010(5) 0.014(5) C44 0.048(6) 0.050(6) 0.068(6) 0.016(5) 0.022(5) 0.007(5) C45 0.072(9) 0.056(8) 0.190(17) -0.033(9) 0.068(11) -0.016(6) C46 0.053(7) 0.063(7) 0.164(14) -0.059(8) 0.057(8) -0.027(6) C47 0.039(5) 0.049(5) 0.056(6) 0.015(4) 0.014(4) 0.009(4) C48 0.042(5) 0.047(5) 0.064(6) 0.012(5) 0.016(5) 0.011(4) C49 0.037(5) 0.051(5) 0.040(5) 0.002(4) 0.001(4) 0.000(4) C50 0.049(5) 0.041(5) 0.054(5) 0.017(4) 0.018(5) 0.006(4) C51 0.042(5) 0.070(7) 0.059(6) 0.008(5) 0.016(5) 0.016(5) C52 0.049(6) 0.069(7) 0.072(7) 0.015(6) 0.020(6) 0.004(6) C53 0.063(7) 0.055(6) 0.066(7) 0.020(5) 0.030(6) 0.023(6) C54 0.055(6) 0.054(6) 0.071(7) 0.021(5) 0.022(5) 0.011(5) C55 0.065(8) 0.112(11) 0.094(10) 0.051(9) 0.039(7) 0.034(8) C56 0.130(16) 0.129(15) 0.121(14) 0.072(12) 0.090(13) 0.087(14) C57 0.133(15) 0.088(11) 0.088(10) 0.032(8) 0.070(11) 0.064(11) C58 0.107(11) 0.090(9) 0.056(6) 0.021(6) 0.026(7) 0.064(9) C59 0.100(10) 0.065(7) 0.051(6) 0.028(5) 0.037(7) 0.041(7) C60 0.075(7) 0.058(6) 0.040(5) 0.015(5) 0.021(5) 0.035(6) C61 0.064(7) 0.054(6) 0.044(5) 0.026(5) 0.015(5) 0.030(5) C62 0.043(5) 0.040(5) 0.030(4) 0.011(3) 0.005(4) 0.008(4) C63 0.055(6) 0.049(5) 0.040(5) 0.005(4) 0.007(4) 0.013(5) C64 0.037(5) 0.038(5) 0.062(6) 0.009(4) 0.009(4) -0.005(4) C65 0.065(6) 0.029(4) 0.033(4) 0.008(3) -0.002(4) 0.000(4) C66 0.042(5) 0.048(5) 0.045(5) 0.023(4) 0.017(4) 0.011(4) C67 0.048(6) 0.051(6) 0.048(5) 0.023(4) 0.010(4) 0.007(5) C68 0.063(7) 0.065(7) 0.050(5) 0.036(5) 0.026(5) 0.029(6) C69 0.049(6) 0.061(6) 0.058(6) 0.029(5) 0.011(5) 0.006(5) C70 0.061(7) 0.058(7) 0.083(8) 0.032(6) 0.019(6) 0.004(6) C71 0.082(9) 0.090(10) 0.080(9) 0.046(8) 0.039(8) 0.038(8) C72 0.063(7) 0.051(6) 0.064(6) 0.020(5) 0.017(6) 0.015(5) C73 0.048(6) 0.075(8) 0.082(8) 0.029(6) 0.012(6) 0.013(6) C74 0.130(14) 0.101(11) 0.063(8) 0.050(8) 0.033(9) 0.065(11) C75 0.067(8) 0.101(11) 0.062(7) 0.031(7) 0.007(6) 0.039(8) C76 0.056(7) 0.099(9) 0.042(5) 0.015(6) 0.011(5) 0.031(7) C77 0.049(6) 0.065(7) 0.053(6) 0.017(5) 0.021(5) 0.019(5) C78 0.039(5) 0.083(8) 0.036(5) 0.004(5) 0.017(4) 0.014(5) C79 0.051(6) 0.050(5) 0.051(5) 0.024(4) 0.027(5) 0.019(5) C80 0.043(5) 0.049(5) 0.069(6) 0.020(5) 0.029(5) 0.024(5) C81 0.050(6) 0.057(6) 0.051(5) 0.017(5) 0.014(5) 0.007(5) C82 0.039(5) 0.053(5) 0.054(5) 0.016(4) 0.025(4) 0.008(4) C83 0.051(6) 0.051(5) 0.044(5) 0.018(4) 0.017(4) 0.020(5) C84 0.047(5) 0.044(5) 0.054(5) 0.019(4) 0.022(5) 0.022(4) C85 0.064(7) 0.064(7) 0.076(8) 0.036(6) 0.037(6) 0.028(6) C86 0.044(5) 0.056(6) 0.053(6) 0.008(5) 0.006(5) 0.011(5) C87 0.072(8) 0.079(8) 0.077(8) 0.047(7) 0.032(6) 0.030(7) C88 0.076(8) 0.066(7) 0.065(7) 0.040(6) 0.014(6) 0.018(6) C89 0.102(11) 0.085(9) 0.068(8) 0.040(7) 0.020(8) 0.032(9) C90 0.069(7) 0.061(7) 0.062(7) 0.017(5) 0.019(6) 0.018(6) C91 0.102(10) 0.057(7) 0.051(6) 0.013(5) 0.017(6) 0.037(7) C92 0.143(15) 0.064(9) 0.066(8) 0.020(7) 0.010(9) 0.033(10) C93 0.22(2) 0.109(13) 0.049(7) 0.033(8) 0.041(11) 0.117(16) C94 0.102(11) 0.118(12) 0.054(7) -0.007(7) -0.010(7) 0.062(10) C95 0.084(9) 0.087(9) 0.047(6) 0.015(6) 0.019(6) 0.058(8) C96 0.042(6) 0.067(7) 0.061(6) 0.008(5) 0.004(5) 0.015(5) C97 0.029(4) 0.048(5) 0.045(5) 0.002(4) 0.006(4) 0.002(4) C98 0.036(5) 0.066(7) 0.054(6) 0.006(5) 0.013(4) 0.004(5) C99 0.044(5) 0.054(6) 0.033(4) 0.007(4) 0.008(4) -0.005(4) C100 0.038(5) 0.047(5) 0.043(5) 0.010(4) 0.007(4) -0.006(4) C101 0.049(6) 0.053(6) 0.060(6) 0.013(5) 0.021(5) 0.010(5) C102 0.045(5) 0.060(6) 0.042(5) 0.012(4) 0.008(4) 0.016(5) C103 0.045(6) 0.071(7) 0.047(5) 0.007(5) 0.010(5) -0.001(5) C104 0.051(6) 0.048(5) 0.049(5) 0.019(4) 0.017(4) 0.005(5) C105 0.082(9) 0.057(7) 0.072(8) 0.006(6) 0.018(7) -0.008(6) C106 0.087(9) 0.050(6) 0.076(8) 0.027(6) 0.011(7) 0.009(6) C107 0.083(9) 0.056(7) 0.055(6) 0.017(5) 0.024(6) 0.002(6) C108 0.063(7) 0.047(6) 0.063(6) 0.011(5) 0.020(5) 0.009(5) C109 0.066(7) 0.057(6) 0.067(7) 0.018(5) 0.020(6) 0.015(6) C110 0.063(7) 0.077(8) 0.069(7) 0.027(6) 0.014(6) 0.011(6) C111 0.097(10) 0.072(8) 0.048(6) 0.024(6) 0.009(6) 0.028(7) C112 0.069(7) 0.049(6) 0.056(6) 0.011(5) 0.005(5) 0.027(5) C113 0.068(7) 0.055(6) 0.035(4) 0.011(4) 0.016(4) 0.035(5) C114 0.060(7) 0.067(7) 0.042(5) 0.009(5) 0.006(5) 0.023(6) C115 0.042(5) 0.060(6) 0.038(5) 0.006(4) 0.009(4) 0.017(5) C116 0.058(6) 0.068(7) 0.044(5) 0.012(5) 0.008(5) 0.025(6) C117 0.036(5) 0.066(6) 0.050(5) 0.029(5) 0.000(4) 0.011(5) C118 0.049(6) 0.070(7) 0.054(6) 0.029(5) 0.013(5) 0.019(5) C119 0.063(7) 0.055(6) 0.049(5) 0.016(5) 0.024(5) 0.020(5) C120 0.053(6) 0.043(5) 0.051(5) -0.005(4) 0.012(5) 0.007(5) C121 0.052(6) 0.053(6) 0.048(5) -0.001(4) 0.020(5) -0.012(5) C122 0.079(8) 0.053(6) 0.041(5) -0.005(4) 0.025(5) 0.004(6) C123 0.103(10) 0.053(6) 0.062(7) 0.017(5) 0.037(7) 0.007(6) C124 0.113(12) 0.053(7) 0.083(9) 0.030(7) 0.029(8) 0.020(8) C125 0.125(12) 0.068(8) 0.035(5) 0.018(5) 0.024(6) 0.020(8) C126 0.079(7) 0.045(5) 0.035(5) 0.008(4) 0.010(5) 0.016(5) C127 0.085(9) 0.077(8) 0.070(8) 0.027(7) 0.030(7) 0.020(7) C128 0.153(17) 0.114(14) 0.125(14) 0.064(12) 0.095(14) 0.075(14) C129 0.121(12) 0.097(10) 0.037(6) 0.014(6) 0.019(7) 0.059(10) C130 0.076(8) 0.079(8) 0.052(6) 0.002(6) 0.015(6) 0.030(7) C131 0.050(6) 0.074(7) 0.042(5) 0.016(5) 0.024(4) 0.032(5) C132 0.044(5) 0.062(6) 0.033(4) 0.012(4) -0.003(4) 0.012(5) C133 0.043(5) 0.075(7) 0.032(4) 0.009(4) 0.009(4) 0.017(5) C134 0.045(5) 0.052(6) 0.046(5) 0.011(4) 0.011(4) 0.018(5) C135 0.066(7) 0.055(6) 0.046(5) 0.007(4) 0.009(5) 0.010(5) C136 0.068(7) 0.050(6) 0.042(5) 0.003(4) 0.002(5) -0.005(5) C137 0.059(6) 0.045(5) 0.037(5) 0.008(4) 0.017(4) 0.012(5) C138 0.046(5) 0.043(5) 0.044(5) 0.008(4) 0.006(4) 0.006(4) C139 0.069(6) 0.027(4) 0.046(5) 0.011(4) 0.029(5) 0.016(4) C140 0.069(7) 0.045(5) 0.044(5) 0.014(4) 0.021(5) 0.012(5) C141 0.076(7) 0.047(6) 0.047(5) 0.010(4) 0.019(5) 0.013(5) C142 0.112(10) 0.051(6) 0.053(6) 0.031(5) 0.045(7) 0.035(7) C143 0.096(9) 0.057(7) 0.049(6) 0.019(5) 0.020(6) 0.037(7) C144 0.060(6) 0.059(6) 0.046(5) 0.011(5) 0.016(5) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 1.900(10) . ? Cu1 N43 1.918(10) . ? Cu1 O1 2.153(6) . ? Cu1 N1 2.185(8) . ? Cu1 O9 2.226(6) . ? Cu1 N41 2.244(8) . ? Cu2 N53 1.896(10) . ? Cu2 O11 1.968(6) . ? Cu2 N51 2.030(8) . ? Cu2 N5 2.030(8) . ? Cu2 O1 2.177(7) . ? Cu3 N63 1.861(8) . ? Cu3 O2 1.957(7) . ? Cu3 O13 1.957(6) . ? Cu3 N61 2.008(8) . ? Cu3 N6 2.240(8) . ? Cu4 N8 1.936(10) . ? Cu4 N73 1.948(9) . ? Cu4 N71 2.129(9) . ? Cu4 N10 2.152(9) . ? Cu4 O2 2.158(6) . ? Cu4 O15 2.248(6) . ? Cu5 N18 1.885(9) . ? Cu5 O15 1.922(6) . ? Cu5 O4 1.972(6) . ? Cu5 N20 2.023(8) . ? Cu5 N75 2.273(7) . ? Cu6 N28 1.894(8) . ? Cu6 O6 1.955(6) . ? Cu6 N76 1.988(8) . ? Cu6 N30 1.994(8) . ? Cu6 O16 2.197(6) . ? Cu7 N78 1.925(8) . ? Cu7 N38 1.962(8) . ? Cu7 O16 2.019(6) . ? Cu7 N80 2.052(8) . ? Cu7 N40 2.328(8) . ? Cu7 O8 2.393(6) . ? Cu8 N68 1.910(8) . ? Cu8 O8 1.942(7) . ? Cu8 O14 1.982(6) . ? Cu8 N70 2.033(8) . ? Cu8 N36 2.275(7) . ? Cu9 N58 1.891(9) . ? Cu9 O12 1.936(6) . ? Cu9 N35 2.013(8) . ? Cu9 N60 2.045(8) . ? Cu9 O7 2.205(6) . ? Cu10 N33 1.908(9) . ? Cu10 N48 1.933(9) . ? Cu10 O7 2.129(6) . ? Cu10 N31 2.136(9) . ? Cu10 O10 2.240(6) . ? Cu10 N50 2.257(8) . ? Cu11 N23 1.814(10) . ? Cu11 O5 1.960(7) . ? Cu11 O10 1.963(7) . ? Cu11 N21 2.034(9) . ? Cu11 N46 2.260(8) . ? Cu12 N13 1.832(10) . ? Cu12 O3 1.967(7) . ? Cu12 N11 2.016(8) . ? Cu12 N45 2.027(8) . ? Cu12 O9 2.144(7) . ? Na1 N15 1.797(19) . ? Na1 N55 1.848(19) . ? Na1 O11 2.250(15) . ? Na1 O3 2.447(16) . ? Na1 C26 2.665(18) . ? Na1 C98 2.672(18) . ? Na1 N16 2.702(19) . ? Na1 C97 2.846(16) . ? Na1 N56 2.863(19) . ? Na1 C25 2.969(18) . ? Na1 Na3 3.234(17) . ? Na1 Na2 3.34(3) . ? Na2 N65 1.66(3) . ? Na2 N16 1.91(3) . ? Na2 O4 2.24(3) . ? Na2 O13 2.33(3) . ? Na2 C116 2.53(3) . ? Na2 C29 2.63(3) . ? Na2 N66 2.65(3) . ? Na2 C30 2.68(3) . ? Na2 C115 2.80(3) . ? Na2 N15 2.96(3) . ? Na2 Na4 3.24(3) . ? Na3 N56 1.703(13) . ? Na3 N25 1.910(13) . ? Na3 O12 2.365(10) . ? Na3 O5 2.411(10) . ? Na3 N55 2.649(13) . ? Na3 C101 2.679(14) . ? Na3 C44 2.793(14) . ? Na3 N26 2.846(13) . ? Na3 C102 2.949(13) . ? Na3 C43 2.993(13) . ? Na3 Na4 3.295(9) . ? Na4 N66 1.800(12) . ? Na4 N26 1.852(12) . ? Na4 O6 2.224(8) . ? Na4 O14 2.318(9) . ? Na4 C119 2.623(13) . ? Na4 C47 2.727(12) . ? Na4 N65 2.759(11) . ? Na4 N25 2.798(11) . ? Na4 C120 2.854(11) . ? Na4 C48 2.872(12) . ? O1 C7 1.328(13) . ? O2 C12 1.312(12) . ? O3 C25 1.233(13) . ? O4 C30 1.252(12) . ? O5 C43 1.310(12) . ? O6 C48 1.292(12) . ? O7 C61 1.301(13) . ? O8 C66 1.285(11) . ? O9 C79 1.276(12) . ? O10 C84 1.293(12) . ? O11 C97 1.267(11) . ? O12 C102 1.278(11) . ? O13 C115 1.256(12) . ? O14 C120 1.315(12) . ? O15 C133 1.317(12) . ? O16 C138 1.317(11) . ? O17 N81 1.188(16) . ? O18 N81 1.314(19) . ? O19 N81 1.149(16) . ? O20 N82 1.34(2) . ? O21 N82 1.253(17) . ? O22 N82 1.19(2) . ? O23 N83 1.164(15) . ? O24 N83 1.194(14) . ? O25 N83 1.283(14) . ? O26 N84 1.207(12) . ? O27 N84 1.273(14) . ? O28 N84 1.247(13) . ? O29 N85 1.198(13) . ? O30 N85 1.216(14) . ? O31 N85 1.248(13) . ? O32 N86 1.279(15) . ? O33 N86 1.165(15) . ? O34 N86 1.224(16) . ? O36 O38 1.751(18) . ? O52 O59 1.79(4) 2_766 ? O59 O52 1.79(4) 2_766 ? O60 O61 1.17(4) . ? N1 C1 1.298(15) . ? N1 C5 1.315(15) . ? N2 C6 1.403(17) . ? N2 H1 0.8800 . ? N2 H2 0.8800 . ? N3 C6 1.325(13) . ? N3 N4 1.401(12) . ? N4 C7 1.263(14) . ? N5 C8 1.306(13) . ? N5 N6 1.347(10) . ? N6 C11 1.326(13) . ? N7 C12 1.286(13) . ? N7 N8 1.407(12) . ? N8 C13 1.322(13) . ? N9 C13 1.317(14) . ? N9 H3 0.8800 . ? N9 H4 0.8800 . ? N10 C18 1.303(15) . ? N10 C14 1.341(14) . ? N11 C23 1.315(15) . ? N11 C19 1.358(15) . ? N12 C24 1.296(17) . ? N12 H5 0.8800 . ? N12 H6 0.8800 . ? N13 C24 1.330(16) . ? N13 N14 1.419(13) . ? N14 C25 1.274(14) . ? N15 N16 1.374(14) . ? N15 C26 1.416(15) . ? N16 C29 1.430(16) . ? N17 C30 1.350(14) . ? N17 N18 1.389(11) . ? N18 C31 1.319(13) . ? N19 C31 1.327(14) . ? N19 H7 0.8800 . ? N19 H8 0.8800 . ? N20 C36 1.348(13) . ? N20 C32 1.410(13) . ? N21 C41 1.302(15) . ? N21 C37 1.364(14) . ? N22 C42 1.37(2) . ? N22 H9 0.8800 . ? N22 H10 0.8800 . ? N23 C42 1.289(16) . ? N23 N24 1.435(13) . ? N24 C43 1.229(14) . ? N25 N26 1.345(14) . ? N25 C44 1.384(15) . ? N26 C47 1.394(14) . ? N27 C48 1.351(12) . ? N27 N28 1.382(10) . ? N28 C49 1.293(11) . ? N29 C49 1.334(12) . ? N29 H11 0.8800 . ? N29 H12 0.8800 . ? N30 C54 1.326(13) . ? N30 C50 1.363(12) . ? N31 C55 1.312(15) . ? N31 C59 1.346(16) . ? N32 C60 1.280(15) . ? N32 H13 0.8800 . ? N32 H14 0.8800 . ? N33 C60 1.335(12) . ? N33 N34 1.408(11) . ? N34 C61 1.300(13) . ? N35 N36 1.321(10) . ? N35 C62 1.371(11) . ? N36 C65 1.310(12) . ? N37 C66 1.313(12) . ? N37 N38 1.409(10) . ? N38 C67 1.348(12) . ? N39 C67 1.336(13) . ? N39 H15 0.8800 . ? N39 H16 0.8800 . ? N40 C72 1.313(13) . ? N40 C68 1.360(14) . ? N41 C77 1.339(14) . ? N41 C73 1.342(14) . ? N42 C78 1.305(14) . ? N42 H17 0.8800 . ? N42 H18 0.8800 . ? N43 C78 1.317(13) . ? N43 N44 1.399(11) . ? N44 C79 1.324(13) . ? N45 N46 1.313(9) . ? N45 C80 1.313(13) . ? N46 C83 1.348(12) . ? N47 C84 1.296(12) . ? N47 N48 1.422(11) . ? N48 C85 1.323(14) . ? N49 C85 1.266(15) . ? N49 H19 0.8800 . ? N49 H20 0.8800 . ? N50 C86 1.319(14) . ? N50 C90 1.338(13) . ? N51 C91 1.342(14) . ? N51 C95 1.360(16) . ? N52 C96 1.305(14) . ? N52 H21 0.8800 . ? N52 H22 0.8800 . ? N53 C96 1.287(13) . ? N53 N54 1.416(11) . ? N54 C97 1.313(12) . ? N55 C98 1.354(15) . ? N55 N56 1.377(13) . ? N56 C101 1.379(14) . ? N57 C102 1.339(12) . ? N57 N58 1.381(10) . ? N58 C103 1.304(13) . ? N59 C103 1.334(14) . ? N59 H23 0.8800 . ? N59 H24 0.8800 . ? N60 C108 1.319(13) . ? N60 C104 1.346(13) . ? N61 C113 1.345(13) . ? N61 C109 1.370(13) . ? N62 C114 1.308(14) . ? N62 H25 0.8800 . ? N62 H26 0.8800 . ? N63 C114 1.310(13) . ? N63 N64 1.412(10) . ? N64 C115 1.315(12) . ? N65 N66 1.336(13) . ? N65 C116 1.383(15) . ? N66 C119 1.399(16) . ? N67 C120 1.303(12) . ? N67 N68 1.346(11) . ? N68 C121 1.304(12) . ? N69 C121 1.358(14) . ? N69 H27 0.8800 . ? N69 H28 0.8800 . ? N70 C126 1.311(12) . ? N70 C122 1.336(14) . ? N71 C131 1.318(14) . ? N71 C127 1.337(14) . ? N72 C132 1.342(13) . ? N72 H29 0.8800 . ? N72 H30 0.8800 . ? N73 C132 1.319(12) . ? N73 N74 1.402(11) . ? N74 C133 1.301(12) . ? N75 C134 1.317(12) . ? N75 N76 1.356(10) . ? N76 C137 1.363(12) . ? N77 C138 1.309(12) . ? N77 N78 1.392(10) . ? N78 C139 1.309(11) . ? N79 C139 1.332(13) . ? N79 H31 0.8800 . ? N79 H32 0.8800 . ? N80 C144 1.348(12) . ? N80 C140 1.349(13) . ? C1 C2 1.370(18) . ? C1 H33 0.9500 . ? C2 C3 1.36(2) . ? C2 H34 0.9500 . ? C3 C4 1.45(2) . ? C3 H35 0.9500 . ? C4 C5 1.395(15) . ? C4 H36 0.9500 . ? C5 C6 1.479(16) . ? C7 C8 1.510(14) . ? C8 C9 1.411(16) . ? C9 C10 1.329(14) . ? C9 H37 0.9500 . ? C10 C11 1.403(15) . ? C10 H38 0.9500 . ? C11 C12 1.496(14) . ? C13 C14 1.519(14) . ? C14 C15 1.334(15) . ? C15 C16 1.44(2) . ? C15 H39 0.9500 . ? C16 C17 1.36(2) . ? C16 H40 0.9500 . ? C17 C18 1.38(2) . ? C17 H41 0.9500 . ? C18 H42 0.9500 . ? C19 C20 1.379(17) . ? C19 H43 0.9500 . ? C20 C21 1.42(2) . ? C20 H44 0.9500 . ? C21 C22 1.298(19) . ? C21 H45 0.9500 . ? C22 C23 1.399(15) . ? C22 H46 0.9500 . ? C23 C24 1.443(17) . ? C25 C26 1.467(14) . ? C26 C27 1.293(15) . ? C27 C28 1.350(14) . ? C27 H47 0.9500 . ? C28 C29 1.272(14) . ? C28 H48 0.9500 . ? C29 C30 1.475(14) . ? C31 C32 1.487(13) . ? C32 C33 1.343(14) . ? C33 C34 1.341(17) . ? C33 H49 0.9500 . ? C34 C35 1.34(2) . ? C34 H50 0.9500 . ? C35 C36 1.437(19) . ? C35 H51 0.9500 . ? C36 H52 0.9500 . ? C37 C38 1.367(17) . ? C37 H53 0.9500 . ? C38 C39 1.26(2) . ? C38 H54 0.9500 . ? C39 C40 1.54(3) . ? C39 H55 0.9500 . ? C40 C41 1.357(17) . ? C40 H56 0.9500 . ? C41 C42 1.444(18) . ? C43 C44 1.463(14) . ? C44 C45 1.313(16) . ? C45 C46 1.363(16) . ? C45 H57 0.9500 . ? C46 C47 1.296(15) . ? C46 H58 0.9500 . ? C47 C48 1.496(13) . ? C49 C50 1.490(13) . ? C50 C51 1.385(13) . ? C51 C52 1.374(15) . ? C51 H59 0.9500 . ? C52 C53 1.379(16) . ? C52 H60 0.9500 . ? C53 C54 1.392(14) . ? C53 H61 0.9500 . ? C54 H62 0.9500 . ? C55 C56 1.45(2) . ? C55 H63 0.9500 . ? C56 C57 1.31(2) . ? C56 H64 0.9500 . ? C57 C58 1.40(2) . ? C57 H65 0.9500 . ? C58 C59 1.482(15) . ? C58 H66 0.9500 . ? C59 C60 1.460(16) . ? C61 C62 1.491(13) . ? C62 C63 1.380(13) . ? C63 C64 1.369(13) . ? C63 H67 0.9500 . ? C64 C65 1.412(13) . ? C64 H68 0.9500 . ? C65 C66 1.528(13) . ? C67 C68 1.470(14) . ? C68 C69 1.407(15) . ? C69 C70 1.405(16) . ? C69 H69 0.9500 . ? C70 C71 1.375(18) . ? C70 H70 0.9500 . ? C71 C72 1.440(17) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.381(18) . ? C73 H73 0.9500 . ? C74 C75 1.33(2) . ? C74 H74 0.9500 . ? C75 C76 1.379(17) . ? C75 H75 0.9500 . ? C76 C77 1.412(15) . ? C76 H76 0.9500 . ? C77 C78 1.462(14) . ? C79 C80 1.511(12) . ? C80 C81 1.433(14) . ? C81 C82 1.339(13) . ? C81 H77 0.9500 . ? C82 C83 1.376(14) . ? C82 H78 0.9500 . ? C83 C84 1.518(12) . ? C85 C86 1.505(14) . ? C86 C87 1.397(15) . ? C87 C88 1.367(15) . ? C87 H79 0.9500 . ? C88 C89 1.337(19) . ? C88 H80 0.9500 . ? C89 C90 1.327(17) . ? C89 H81 0.9500 . ? C90 H82 0.9500 . ? C91 C92 1.297(17) . ? C91 H83 0.9500 . ? C92 C93 1.33(2) . ? C92 H84 0.9500 . ? C93 C94 1.45(2) . ? C93 H85 0.9500 . ? C94 C95 1.401(15) . ? C94 H86 0.9500 . ? C95 C96 1.473(16) . ? C97 C98 1.497(13) . ? C98 C99 1.343(14) . ? C99 C100 1.319(12) . ? C99 H87 0.9500 . ? C100 C101 1.357(14) . ? C100 H88 0.9500 . ? C101 C102 1.468(13) . ? C103 C104 1.546(14) . ? C104 C105 1.326(14) . ? C105 C106 1.350(17) . ? C105 H89 0.9500 . ? C106 C107 1.340(17) . ? C106 H90 0.9500 . ? C107 C108 1.392(14) . ? C107 H91 0.9500 . ? C108 H92 0.9500 . ? C109 C110 1.352(16) . ? C109 H93 0.9500 . ? C110 C111 1.365(18) . ? C110 H94 0.9500 . ? C111 C112 1.356(15) . ? C111 H95 0.9500 . ? C112 C113 1.368(13) . ? C112 H96 0.9500 . ? C113 C114 1.496(14) . ? C115 C116 1.497(13) . ? C116 C117 1.328(15) . ? C117 C118 1.316(12) . ? C117 H97 0.9500 . ? C118 C119 1.324(15) . ? C118 H98 0.9500 . ? C119 C120 1.466(14) . ? C121 C122 1.499(15) . ? C122 C123 1.411(15) . ? C123 C124 1.352(18) . ? C123 H99 0.9500 . ? C124 C125 1.414(19) . ? C124 H100 0.9500 . ? C125 C126 1.353(14) . ? C125 H101 0.9500 . ? C126 H102 0.9500 . ? C127 C128 1.45(2) . ? C127 H103 0.9500 . ? C128 C129 1.38(2) . ? C128 H104 0.9500 . ? C129 C130 1.348(17) . ? C129 H105 0.9500 . ? C130 C131 1.396(15) . ? C130 H106 0.9500 . ? C131 C132 1.535(13) . ? C133 C134 1.491(13) . ? C134 C135 1.412(14) . ? C135 C136 1.396(13) . ? C135 H107 0.9500 . ? C136 C137 1.410(13) . ? C136 H108 0.9500 . ? C137 C138 1.453(12) . ? C139 C140 1.507(13) . ? C140 C141 1.369(13) . ? C141 C142 1.407(15) . ? C141 H109 0.9500 . ? C142 C143 1.321(17) . ? C142 H110 0.9500 . ? C143 C144 1.393(14) . ? C143 H111 0.9500 . ? C144 H112 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 N3 Cu1 N43 170.6(3) . . ? N3 Cu1 O1 76.8(3) . . ? N43 Cu1 O1 96.1(3) . . ? N3 Cu1 N1 77.6(4) . . ? N43 Cu1 N1 109.4(3) . . ? O1 Cu1 N1 154.4(3) . . ? N3 Cu1 O9 99.1(3) . . ? N43 Cu1 O9 76.2(3) . . ? O1 Cu1 O9 102.8(2) . . ? N1 Cu1 O9 81.9(3) . . ? N3 Cu1 N41 109.1(4) . . ? N43 Cu1 N41 75.9(4) . . ? O1 Cu1 N41 84.0(3) . . ? N1 Cu1 N41 103.9(3) . . ? O9 Cu1 N41 151.8(3) . . ? N53 Cu2 O11 78.6(3) . . ? N53 Cu2 N51 80.8(4) . . ? O11 Cu2 N51 158.1(3) . . ? N53 Cu2 N5 166.4(4) . . ? O11 Cu2 N5 100.0(3) . . ? N51 Cu2 N5 98.3(3) . . ? N53 Cu2 O1 116.4(3) . . ? O11 Cu2 O1 92.1(3) . . ? N51 Cu2 O1 103.6(3) . . ? N5 Cu2 O1 77.1(3) . . ? N63 Cu3 O2 162.5(3) . . ? N63 Cu3 O13 80.4(3) . . ? O2 Cu3 O13 98.2(3) . . ? N63 Cu3 N61 79.9(3) . . ? O2 Cu3 N61 99.6(3) . . ? O13 Cu3 N61 160.0(3) . . ? N63 Cu3 N6 120.4(3) . . ? O2 Cu3 N6 76.9(3) . . ? O13 Cu3 N6 88.6(3) . . ? N61 Cu3 N6 104.3(3) . . ? N8 Cu4 N73 164.0(3) . . ? N8 Cu4 N71 112.0(4) . . ? N73 Cu4 N71 78.9(3) . . ? N8 Cu4 N10 77.9(3) . . ? N73 Cu4 N10 113.1(3) . . ? N71 Cu4 N10 98.3(3) . . ? N8 Cu4 O2 75.5(3) . . ? N73 Cu4 O2 93.6(3) . . ? N71 Cu4 O2 89.3(3) . . ? N10 Cu4 O2 153.2(3) . . ? N8 Cu4 O15 94.8(3) . . ? N73 Cu4 O15 74.6(3) . . ? N71 Cu4 O15 153.1(3) . . ? N10 Cu4 O15 88.3(3) . . ? O2 Cu4 O15 96.4(2) . . ? N18 Cu5 O15 166.7(3) . . ? N18 Cu5 O4 79.5(3) . . ? O15 Cu5 O4 96.5(3) . . ? N18 Cu5 N20 80.0(4) . . ? O15 Cu5 N20 101.7(3) . . ? O4 Cu5 N20 158.0(3) . . ? N18 Cu5 N75 115.3(3) . . ? O15 Cu5 N75 77.4(3) . . ? O4 Cu5 N75 92.7(3) . . ? N20 Cu5 N75 103.1(3) . . ? N28 Cu6 O6 80.3(3) . . ? N28 Cu6 N76 170.6(3) . . ? O6 Cu6 N76 96.0(3) . . ? N28 Cu6 N30 80.6(3) . . ? O6 Cu6 N30 160.1(3) . . ? N76 Cu6 N30 101.9(3) . . ? N28 Cu6 O16 111.3(3) . . ? O6 Cu6 O16 92.8(3) . . ? N76 Cu6 O16 77.4(3) . . ? N30 Cu6 O16 99.6(3) . . ? N78 Cu7 N38 160.8(3) . . ? N78 Cu7 O16 78.0(3) . . ? N38 Cu7 O16 102.1(3) . . ? N78 Cu7 N80 78.8(3) . . ? N38 Cu7 N80 100.8(3) . . ? O16 Cu7 N80 156.6(3) . . ? N78 Cu7 N40 124.9(3) . . ? N38 Cu7 N40 74.3(3) . . ? O16 Cu7 N40 91.0(3) . . ? N80 Cu7 N40 99.5(3) . . ? N78 Cu7 O8 88.7(3) . . ? N38 Cu7 O8 72.4(3) . . ? O16 Cu7 O8 101.8(2) . . ? N80 Cu7 O8 80.9(3) . . ? N40 Cu7 O8 146.1(3) . . ? N68 Cu8 O8 165.1(3) . . ? N68 Cu8 O14 79.6(3) . . ? O8 Cu8 O14 93.7(3) . . ? N68 Cu8 N70 81.1(3) . . ? O8 Cu8 N70 103.0(3) . . ? O14 Cu8 N70 159.0(3) . . ? N68 Cu8 N36 116.9(3) . . ? O8 Cu8 N36 77.2(3) . . ? O14 Cu8 N36 99.8(3) . . ? N70 Cu8 N36 96.3(3) . . ? N58 Cu9 O12 79.5(3) . . ? N58 Cu9 N35 166.1(3) . . ? O12 Cu9 N35 92.3(3) . . ? N58 Cu9 N60 81.4(3) . . ? O12 Cu9 N60 159.0(3) . . ? N35 Cu9 N60 104.7(3) . . ? N58 Cu9 O7 114.9(3) . . ? O12 Cu9 O7 103.0(3) . . ? N35 Cu9 O7 77.7(3) . . ? N60 Cu9 O7 92.8(3) . . ? N33 Cu10 N48 169.2(3) . . ? N33 Cu10 O7 77.7(3) . . ? N48 Cu10 O7 96.2(3) . . ? N33 Cu10 N31 78.8(4) . . ? N48 Cu10 N31 107.1(4) . . ? O7 Cu10 N31 156.5(4) . . ? N33 Cu10 O10 95.6(3) . . ? N48 Cu10 O10 75.5(3) . . ? O7 Cu10 O10 91.0(2) . . ? N31 Cu10 O10 92.0(3) . . ? N33 Cu10 N50 114.2(3) . . ? N48 Cu10 N50 75.0(3) . . ? O7 Cu10 N50 96.4(3) . . ? N31 Cu10 N50 92.5(3) . . ? O10 Cu10 N50 150.2(3) . . ? N23 Cu11 O5 80.4(4) . . ? N23 Cu11 O10 155.9(5) . . ? O5 Cu11 O10 99.7(3) . . ? N23 Cu11 N21 79.4(4) . . ? O5 Cu11 N21 159.5(4) . . ? O10 Cu11 N21 97.2(4) . . ? N23 Cu11 N46 128.3(5) . . ? O5 Cu11 N46 93.1(3) . . ? O10 Cu11 N46 75.8(3) . . ? N21 Cu11 N46 102.4(3) . . ? N13 Cu12 O3 78.8(4) . . ? N13 Cu12 N11 79.7(4) . . ? O3 Cu12 N11 157.3(4) . . ? N13 Cu12 N45 160.0(4) . . ? O3 Cu12 N45 96.6(3) . . ? N11 Cu12 N45 101.1(3) . . ? N13 Cu12 O9 121.4(4) . . ? O3 Cu12 O9 92.5(3) . . ? N11 Cu12 O9 104.9(3) . . ? N45 Cu12 O9 78.0(3) . . ? N15 Na1 N55 172.3(11) . . ? N15 Na1 O11 102.9(8) . . ? N55 Na1 O11 84.2(7) . . ? N15 Na1 O3 79.4(6) . . ? N55 Na1 O3 99.5(7) . . ? O11 Na1 O3 122.9(7) . . ? N15 Na1 C26 29.6(5) . . ? N55 Na1 C26 145.6(9) . . ? O11 Na1 C26 126.7(8) . . ? O3 Na1 C26 53.2(4) . . ? N15 Na1 C98 158.2(9) . . ? N55 Na1 C98 28.0(5) . . ? O11 Na1 C98 56.7(4) . . ? O3 Na1 C98 116.9(6) . . ? C26 Na1 C98 170.2(7) . . ? N15 Na1 N16 27.2(5) . . ? N55 Na1 N16 150.7(8) . . ? O11 Na1 N16 94.9(6) . . ? O3 Na1 N16 105.4(6) . . ? C26 Na1 N16 52.6(4) . . ? C98 Na1 N16 137.1(6) . . ? N15 Na1 C97 128.3(9) . . ? N55 Na1 C97 58.7(5) . . ? O11 Na1 C97 25.5(3) . . ? O3 Na1 C97 122.6(6) . . ? C26 Na1 C97 150.6(7) . . ? C98 Na1 C97 31.3(3) . . ? N16 Na1 C97 116.8(6) . . ? N15 Na1 N56 149.1(8) . . ? N55 Na1 N56 23.3(5) . . ? O11 Na1 N56 107.0(6) . . ? O3 Na1 N56 91.0(6) . . ? C26 Na1 N56 125.3(6) . . ? C98 Na1 N56 50.3(4) . . ? N16 Na1 N56 139.4(6) . . ? C97 Na1 N56 81.5(5) . . ? N15 Na1 C25 55.8(5) . . ? N55 Na1 C25 122.2(8) . . ? O11 Na1 C25 126.8(7) . . ? O3 Na1 C25 23.9(3) . . ? C26 Na1 C25 29.6(3) . . ? C98 Na1 C25 140.6(6) . . ? N16 Na1 C25 81.5(5) . . ? C97 Na1 C25 138.3(6) . . ? N56 Na1 C25 109.5(6) . . ? N15 Na1 Na3 117.4(7) . . ? N55 Na1 Na3 55.0(6) . . ? O11 Na1 Na3 137.9(7) . . ? O3 Na1 Na3 78.4(5) . . ? C26 Na1 Na3 95.4(5) . . ? C98 Na1 Na3 81.6(5) . . ? N16 Na1 Na3 115.1(5) . . ? C97 Na1 Na3 112.9(5) . . ? N56 Na1 Na3 31.7(3) . . ? C25 Na1 Na3 88.1(4) . . ? N15 Na1 Na2 62.1(7) . . ? N55 Na1 Na2 116.4(9) . . ? O11 Na1 Na2 83.7(7) . . ? O3 Na1 Na2 138.0(8) . . ? C26 Na1 Na2 85.1(7) . . ? C98 Na1 Na2 104.7(7) . . ? N16 Na1 Na2 34.9(6) . . ? C97 Na1 Na2 95.5(7) . . ? N56 Na1 Na2 113.1(7) . . ? C25 Na1 Na2 114.6(7) . . ? Na3 Na1 Na2 104.0(6) . . ? N65 Na2 N16 144.2(19) . . ? N65 Na2 O4 129.9(16) . . ? N16 Na2 O4 81.8(12) . . ? N65 Na2 O13 83.9(13) . . ? N16 Na2 O13 113.3(14) . . ? O4 Na2 O13 94.5(11) . . ? N65 Na2 C116 30.5(7) . . ? N16 Na2 C116 135.9(15) . . ? O4 Na2 C116 138.0(13) . . ? O13 Na2 C116 57.7(8) . . ? N65 Na2 C29 146.0(16) . . ? N16 Na2 C29 31.9(7) . . ? O4 Na2 C29 57.7(8) . . ? O13 Na2 C29 130.1(13) . . ? C116 Na2 C29 164.4(13) . . ? N65 Na2 N66 24.6(6) . . ? N16 Na2 N66 126.7(14) . . ? O4 Na2 N66 126.5(13) . . ? O13 Na2 N66 108.5(12) . . ? C116 Na2 N66 52.9(7) . . ? C29 Na2 N66 121.4(12) . . ? N65 Na2 C30 138.5(16) . . ? N16 Na2 C30 61.6(10) . . ? O4 Na2 C30 27.6(5) . . ? O13 Na2 C30 118.9(12) . . ? C116 Na2 C30 162.4(13) . . ? C29 Na2 C30 32.2(5) . . ? N66 Na2 C30 121.5(12) . . ? N65 Na2 C115 61.1(10) . . ? N16 Na2 C115 123.5(14) . . ? O4 Na2 C115 118.7(12) . . ? O13 Na2 C115 26.4(4) . . ? C116 Na2 C115 32.2(5) . . ? C29 Na2 C115 151.0(12) . . ? N66 Na2 C115 84.8(10) . . ? C30 Na2 C115 144.9(12) . . ? N65 Na2 N15 123.6(15) . . ? N16 Na2 N15 21.5(6) . . ? O4 Na2 N15 103.2(11) . . ? O13 Na2 N15 112.5(11) . . ? C116 Na2 N15 116.0(11) . . ? C29 Na2 N15 49.9(6) . . ? N66 Na2 N15 110.6(10) . . ? C30 Na2 N15 81.6(9) . . ? C115 Na2 N15 112.5(10) . . ? N65 Na2 Na4 58.3(9) . . ? N16 Na2 Na4 97.6(11) . . ? O4 Na2 Na4 111.8(11) . . ? O13 Na2 Na4 142.1(13) . . ? C116 Na2 Na4 85.0(9) . . ? C29 Na2 Na4 87.8(9) . . ? N66 Na2 Na4 33.7(4) . . ? C30 Na2 Na4 94.5(9) . . ? C115 Na2 Na4 117.1(10) . . ? N15 Na2 Na4 88.3(8) . . ? N65 Na2 Na1 92.1(13) . . ? N16 Na2 Na1 54.0(8) . . ? O4 Na2 Na1 135.6(12) . . ? O13 Na2 Na1 105.2(10) . . ? C116 Na2 Na1 85.1(9) . . ? C29 Na2 Na1 79.7(8) . . ? N66 Na2 Na1 84.6(9) . . ? C30 Na2 Na1 111.9(10) . . ? C115 Na2 Na1 91.9(9) . . ? N15 Na2 Na1 32.4(4) . . ? Na4 Na2 Na1 75.2(7) . . ? N56 Na3 N25 159.3(6) . . ? N56 Na3 O12 80.5(5) . . ? N25 Na3 O12 111.4(6) . . ? N56 Na3 O5 120.7(5) . . ? N25 Na3 O5 76.4(4) . . ? O12 Na3 O5 94.7(4) . . ? N56 Na3 N55 27.2(4) . . ? N25 Na3 N55 135.1(6) . . ? O12 Na3 N55 107.1(4) . . ? O5 Na3 N55 122.6(4) . . ? N56 Na3 C101 26.4(4) . . ? N25 Na3 C101 156.1(6) . . ? O12 Na3 C101 54.5(3) . . ? O5 Na3 C101 120.8(4) . . ? N55 Na3 C101 52.7(3) . . ? N56 Na3 C44 157.3(6) . . ? N25 Na3 C44 26.7(4) . . ? O12 Na3 C44 120.0(4) . . ? O5 Na3 C44 52.7(3) . . ? N55 Na3 C44 132.7(4) . . ? C101 Na3 C44 172.5(4) . . ? N56 Na3 N26 137.5(5) . . ? N25 Na3 N26 23.9(4) . . ? O12 Na3 N26 108.5(4) . . ? O5 Na3 N26 100.3(4) . . ? N55 Na3 N26 120.3(4) . . ? C101 Na3 N26 135.0(4) . . ? C44 Na3 N26 49.6(3) . . ? N56 Na3 C102 55.7(4) . . ? N25 Na3 C102 134.8(6) . . ? O12 Na3 C102 24.8(2) . . ? O5 Na3 C102 106.6(4) . . ? N55 Na3 C102 82.4(4) . . ? C101 Na3 C102 29.7(3) . . ? C44 Na3 C102 144.2(4) . . ? N26 Na3 C102 125.5(4) . . ? N56 Na3 C43 137.1(5) . . ? N25 Na3 C43 55.0(4) . . ? O12 Na3 C43 113.7(4) . . ? O5 Na3 C43 25.2(3) . . ? N55 Na3 C43 125.8(4) . . ? C101 Na3 C43 145.3(4) . . ? C44 Na3 C43 29.0(3) . . ? N26 Na3 C43 78.5(4) . . ? C102 Na3 C43 130.4(4) . . ? N56 Na3 Na1 62.1(5) . . ? N25 Na3 Na1 101.3(6) . . ? O12 Na3 Na1 140.3(4) . . ? O5 Na3 Na1 114.8(4) . . ? N55 Na3 Na1 34.8(3) . . ? C101 Na3 Na1 86.8(4) . . ? C44 Na3 Na1 99.3(4) . . ? N26 Na3 Na1 92.3(4) . . ? C102 Na3 Na1 116.4(4) . . ? C43 Na3 Na1 103.2(4) . . ? N56 Na3 Na4 103.8(4) . . ? N25 Na3 Na4 57.9(4) . . ? O12 Na3 Na4 102.6(3) . . ? O5 Na3 Na4 134.3(4) . . ? N55 Na3 Na4 92.2(3) . . ? C101 Na3 Na4 103.5(3) . . ? C44 Na3 Na4 82.3(3) . . ? N26 Na3 Na4 34.1(2) . . ? C102 Na3 Na4 106.6(3) . . ? C43 Na3 Na4 111.2(3) . . ? Na1 Na3 Na4 75.9(3) . . ? N66 Na4 N26 165.6(7) . . ? N66 Na4 O6 109.9(5) . . ? N26 Na4 O6 83.0(4) . . ? N66 Na4 O14 80.9(4) . . ? N26 Na4 O14 101.0(5) . . ? O6 Na4 O14 109.7(3) . . ? N66 Na4 C119 30.2(4) . . ? N26 Na4 C119 141.8(5) . . ? O6 Na4 C119 131.4(4) . . ? O14 Na4 C119 56.4(3) . . ? N66 Na4 C47 160.8(5) . . ? N26 Na4 C47 28.0(4) . . ? O6 Na4 C47 56.2(3) . . ? O14 Na4 C47 115.3(3) . . ? C119 Na4 C47 169.0(4) . . ? N66 Na4 N65 24.1(4) . . ? N26 Na4 N65 150.8(5) . . ? O6 Na4 N65 100.3(4) . . ? O14 Na4 N65 104.9(3) . . ? C119 Na4 N65 52.2(3) . . ? C47 Na4 N65 138.1(4) . . ? N66 Na4 N25 141.5(6) . . ? N26 Na4 N25 24.3(4) . . ? O6 Na4 N25 106.4(3) . . ? O14 Na4 N25 98.8(4) . . ? C119 Na4 N25 121.2(4) . . ? C47 Na4 N25 50.2(3) . . ? N65 Na4 N25 135.5(4) . . ? N66 Na4 C120 58.9(4) . . ? N26 Na4 C120 118.1(5) . . ? O6 Na4 C120 129.2(4) . . ? O14 Na4 C120 27.0(3) . . ? C119 Na4 C120 30.7(3) . . ? C47 Na4 C120 139.5(3) . . ? N65 Na4 C120 82.3(3) . . ? N25 Na4 C120 106.0(4) . . ? N66 Na4 C48 135.0(6) . . ? N26 Na4 C48 57.6(4) . . ? O6 Na4 C48 25.5(3) . . ? O14 Na4 C48 113.2(3) . . ? C119 Na4 C48 155.4(4) . . ? C47 Na4 C48 30.9(3) . . ? N65 Na4 C48 121.1(4) . . ? N25 Na4 C48 80.9(3) . . ? C120 Na4 C48 139.5(3) . . ? N66 Na4 Na2 54.9(7) . . ? N26 Na4 Na2 122.5(7) . . ? O6 Na4 Na2 85.3(6) . . ? O14 Na4 Na2 135.7(6) . . ? C119 Na4 Na2 82.0(6) . . ? C47 Na4 Na2 107.8(6) . . ? N65 Na4 Na2 30.8(6) . . ? N25 Na4 Na2 117.1(6) . . ? C120 Na4 Na2 112.6(6) . . ? C48 Na4 Na2 98.1(6) . . ? N66 Na4 Na3 106.4(5) . . ? N26 Na4 Na3 59.5(4) . . ? O6 Na4 Na3 141.0(3) . . ? O14 Na4 Na3 89.3(3) . . ? C119 Na4 Na3 87.6(3) . . ? C47 Na4 Na3 85.0(3) . . ? N65 Na4 Na3 107.4(3) . . ? N25 Na4 Na3 35.4(3) . . ? C120 Na4 Na3 82.1(3) . . ? C48 Na4 Na3 115.8(3) . . ? Na2 Na4 Na3 104.8(5) . . ? C7 O1 Cu1 105.9(6) . . ? C7 O1 Cu2 113.1(6) . . ? Cu1 O1 Cu2 140.8(4) . . ? C12 O2 Cu3 120.0(6) . . ? C12 O2 Cu4 108.1(6) . . ? Cu3 O2 Cu4 128.5(3) . . ? C25 O3 Cu12 112.6(7) . . ? C25 O3 Na1 102.5(7) . . ? Cu12 O3 Na1 140.6(5) . . ? C30 O4 Cu5 111.5(6) . . ? C30 O4 Na2 96.2(10) . . ? Cu5 O4 Na2 133.6(8) . . ? C43 O5 Cu11 108.9(6) . . ? C43 O5 Na3 103.1(6) . . ? Cu11 O5 Na3 137.9(4) . . ? C48 O6 Cu6 109.2(6) . . ? C48 O6 Na4 106.5(6) . . ? Cu6 O6 Na4 140.7(4) . . ? C61 O7 Cu10 106.0(6) . . ? C61 O7 Cu9 111.9(5) . . ? Cu10 O7 Cu9 140.1(3) . . ? C66 O8 Cu8 119.0(6) . . ? C66 O8 Cu7 105.4(6) . . ? Cu8 O8 Cu7 131.9(3) . . ? C79 O9 Cu12 113.5(6) . . ? C79 O9 Cu1 105.5(6) . . ? Cu12 O9 Cu1 140.5(4) . . ? C84 O10 Cu11 122.6(5) . . ? C84 O10 Cu10 105.8(5) . . ? Cu11 O10 Cu10 130.3(4) . . ? C97 O11 Cu2 111.1(6) . . ? C97 O11 Na1 104.5(7) . . ? Cu2 O11 Na1 140.8(6) . . ? C102 O12 Cu9 111.3(6) . . ? C102 O12 Na3 104.1(6) . . ? Cu9 O12 Na3 143.6(4) . . ? C115 O13 Cu3 110.2(6) . . ? C115 O13 Na2 98.2(9) . . ? Cu3 O13 Na2 145.3(8) . . ? C120 O14 Cu8 108.4(6) . . ? C120 O14 Na4 99.9(6) . . ? Cu8 O14 Na4 146.1(4) . . ? C133 O15 Cu5 119.5(5) . . ? C133 O15 Cu4 106.6(5) . . ? Cu5 O15 Cu4 131.4(3) . . ? C138 O16 Cu7 109.5(5) . . ? C138 O16 Cu6 112.0(5) . . ? Cu7 O16 Cu6 138.3(3) . . ? C1 N1 C5 118.1(10) . . ? C1 N1 Cu1 129.4(9) . . ? C5 N1 Cu1 112.0(7) . . ? C6 N2 H1 120.0 . . ? C6 N2 H2 120.0 . . ? H1 N2 H2 120.0 . . ? C6 N3 N4 117.0(10) . . ? C6 N3 Cu1 120.5(8) . . ? N4 N3 Cu1 121.5(6) . . ? C7 N4 N3 108.3(10) . . ? C8 N5 N6 120.5(9) . . ? C8 N5 Cu2 119.4(7) . . ? N6 N5 Cu2 120.1(6) . . ? C11 N6 N5 118.3(8) . . ? C11 N6 Cu3 112.0(6) . . ? N5 N6 Cu3 129.0(6) . . ? C12 N7 N8 108.8(9) . . ? C13 N8 N7 115.7(10) . . ? C13 N8 Cu4 120.5(7) . . ? N7 N8 Cu4 120.9(7) . . ? C13 N9 H3 120.0 . . ? C13 N9 H4 120.0 . . ? H3 N9 H4 120.0 . . ? C18 N10 C14 118.7(11) . . ? C18 N10 Cu4 128.1(10) . . ? C14 N10 Cu4 113.2(6) . . ? C23 N11 C19 120.3(10) . . ? C23 N11 Cu12 113.2(7) . . ? C19 N11 Cu12 126.4(9) . . ? C24 N12 H5 120.0 . . ? C24 N12 H6 120.0 . . ? H5 N12 H6 120.0 . . ? C24 N13 N14 122.9(10) . . ? C24 N13 Cu12 120.3(8) . . ? N14 N13 Cu12 115.9(7) . . ? C25 N14 N13 109.0(10) . . ? N16 N15 C26 117.0(11) . . ? N16 N15 Na1 116.2(9) . . ? C26 N15 Na1 111.6(9) . . ? N16 N15 Na2 30.7(9) . . ? C26 N15 Na2 135.4(10) . . ? Na1 N15 Na2 85.5(8) . . ? N15 N16 C29 115.9(11) . . ? N15 N16 Na2 127.7(13) . . ? C29 N16 Na2 103.0(12) . . ? N15 N16 Na1 36.6(6) . . ? C29 N16 Na1 136.5(9) . . ? Na2 N16 Na1 91.1(11) . . ? C30 N17 N18 107.0(8) . . ? C31 N18 N17 119.9(9) . . ? C31 N18 Cu5 122.2(7) . . ? N17 N18 Cu5 118.0(7) . . ? C31 N19 H7 120.0 . . ? C31 N19 H8 120.0 . . ? H7 N19 H8 120.0 . . ? C36 N20 C32 119.4(10) . . ? C36 N20 Cu5 126.8(9) . . ? C32 N20 Cu5 113.7(6) . . ? C41 N21 C37 121.0(10) . . ? C41 N21 Cu11 112.7(7) . . ? C37 N21 Cu11 125.9(9) . . ? C42 N22 H9 120.0 . . ? C42 N22 H10 120.0 . . ? H9 N22 H10 120.0 . . ? C42 N23 N24 121.1(11) . . ? C42 N23 Cu11 121.3(9) . . ? N24 N23 Cu11 117.6(7) . . ? C43 N24 N23 107.7(10) . . ? N26 N25 C44 120.2(10) . . ? N26 N25 Na3 120.9(9) . . ? C44 N25 Na3 115.1(8) . . ? N26 N25 Na4 34.5(6) . . ? C44 N25 Na4 146.6(8) . . ? Na3 N25 Na4 86.7(4) . . ? N25 N26 C47 117.5(11) . . ? N25 N26 Na4 121.3(9) . . ? C47 N26 Na4 113.5(8) . . ? N25 N26 Na3 35.2(6) . . ? C47 N26 Na3 147.3(9) . . ? Na4 N26 Na3 86.4(4) . . ? C48 N27 N28 104.7(7) . . ? C49 N28 N27 120.5(8) . . ? C49 N28 Cu6 120.3(7) . . ? N27 N28 Cu6 119.2(6) . . ? C49 N29 H11 120.0 . . ? C49 N29 H12 120.0 . . ? H11 N29 H12 120.0 . . ? C54 N30 C50 117.6(9) . . ? C54 N30 Cu6 128.6(7) . . ? C50 N30 Cu6 113.7(6) . . ? C55 N31 C59 120.4(12) . . ? C55 N31 Cu10 130.1(11) . . ? C59 N31 Cu10 109.3(7) . . ? C60 N32 H13 120.0 . . ? C60 N32 H14 120.0 . . ? H13 N32 H14 120.0 . . ? C60 N33 N34 116.1(9) . . ? C60 N33 Cu10 122.2(7) . . ? N34 N33 Cu10 119.7(6) . . ? C61 N34 N33 107.4(9) . . ? N36 N35 C62 121.8(8) . . ? N36 N35 Cu9 119.6(6) . . ? C62 N35 Cu9 118.3(6) . . ? C65 N36 N35 117.9(8) . . ? C65 N36 Cu8 110.8(6) . . ? N35 N36 Cu8 131.0(6) . . ? C66 N37 N38 110.5(8) . . ? C67 N38 N37 111.1(8) . . ? C67 N38 Cu7 124.7(6) . . ? N37 N38 Cu7 124.2(6) . . ? C67 N39 H15 120.0 . . ? C67 N39 H16 120.0 . . ? H15 N39 H16 120.0 . . ? C72 N40 C68 117.6(9) . . ? C72 N40 Cu7 131.0(8) . . ? C68 N40 Cu7 111.4(6) . . ? C77 N41 C73 118.2(10) . . ? C77 N41 Cu1 111.2(7) . . ? C73 N41 Cu1 129.8(9) . . ? C78 N42 H17 120.0 . . ? C78 N42 H18 120.0 . . ? H17 N42 H18 120.0 . . ? C78 N43 N44 114.9(9) . . ? C78 N43 Cu1 122.5(7) . . ? N44 N43 Cu1 121.6(7) . . ? C79 N44 N43 108.1(8) . . ? N46 N45 C80 120.3(8) . . ? N46 N45 Cu12 122.5(6) . . ? C80 N45 Cu12 117.2(6) . . ? N45 N46 C83 118.9(8) . . ? N45 N46 Cu11 128.2(6) . . ? C83 N46 Cu11 112.0(5) . . ? C84 N47 N48 108.2(9) . . ? C85 N48 N47 111.7(9) . . ? C85 N48 Cu10 125.8(8) . . ? N47 N48 Cu10 121.6(6) . . ? C85 N49 H19 120.0 . . ? C85 N49 H20 120.0 . . ? H19 N49 H20 120.0 . . ? C86 N50 C90 118.6(10) . . ? C86 N50 Cu10 111.0(6) . . ? C90 N50 Cu10 130.4(8) . . ? C91 N51 C95 118.8(10) . . ? C91 N51 Cu2 130.0(9) . . ? C95 N51 Cu2 111.1(7) . . ? C96 N52 H21 120.0 . . ? C96 N52 H22 120.0 . . ? H21 N52 H22 120.0 . . ? C96 N53 N54 120.4(10) . . ? C96 N53 Cu2 120.4(8) . . ? N54 N53 Cu2 119.0(6) . . ? C97 N54 N53 104.7(8) . . ? C98 N55 N56 119.5(10) . . ? C98 N55 Na1 112.2(9) . . ? N56 N55 Na1 124.6(10) . . ? C98 N55 Na3 150.1(8) . . ? N56 N55 Na3 34.5(6) . . ? Na1 N55 Na3 90.2(7) . . ? N55 N56 C101 118.1(10) . . ? N55 N56 Na3 118.3(9) . . ? C101 N56 Na3 120.4(8) . . ? N55 N56 Na1 32.1(6) . . ? C101 N56 Na1 146.3(8) . . ? Na3 N56 Na1 86.2(5) . . ? C102 N57 N58 105.2(8) . . ? C103 N58 N57 119.5(9) . . ? C103 N58 Cu9 120.8(7) . . ? N57 N58 Cu9 119.2(6) . . ? C103 N59 H23 120.0 . . ? C103 N59 H24 120.0 . . ? H23 N59 H24 120.0 . . ? C108 N60 C104 119.1(9) . . ? C108 N60 Cu9 128.5(8) . . ? C104 N60 Cu9 112.2(6) . . ? C113 N61 C109 117.0(9) . . ? C113 N61 Cu3 114.0(6) . . ? C109 N61 Cu3 128.9(8) . . ? C114 N62 H25 120.0 . . ? C114 N62 H26 120.0 . . ? H25 N62 H26 120.0 . . ? C114 N63 N64 120.1(9) . . ? C114 N63 Cu3 122.2(7) . . ? N64 N63 Cu3 117.4(6) . . ? C115 N64 N63 106.2(8) . . ? N66 N65 C116 116.5(11) . . ? N66 N65 Na2 124.2(14) . . ? C116 N65 Na2 111.9(13) . . ? N66 N65 Na4 33.4(6) . . ? C116 N65 Na4 141.2(8) . . ? Na2 N65 Na4 90.8(11) . . ? N65 N66 C119 120.2(11) . . ? N65 N66 Na4 122.6(9) . . ? C119 N66 Na4 109.5(8) . . ? N65 N66 Na2 31.2(9) . . ? C119 N66 Na2 144.1(11) . . ? Na4 N66 Na2 91.4(8) . . ? C120 N67 N68 108.6(8) . . ? C121 N68 N67 122.1(9) . . ? C121 N68 Cu8 118.5(7) . . ? N67 N68 Cu8 118.2(6) . . ? C121 N69 H27 120.0 . . ? C121 N69 H28 120.0 . . ? H27 N69 H28 120.0 . . ? C126 N70 C122 118.5(9) . . ? C126 N70 Cu8 128.4(7) . . ? C122 N70 Cu8 112.6(7) . . ? C131 N71 C127 118.2(11) . . ? C131 N71 Cu4 112.3(6) . . ? C127 N71 Cu4 129.2(9) . . ? C132 N72 H29 120.0 . . ? C132 N72 H30 120.0 . . ? H29 N72 H30 120.0 . . ? C132 N73 N74 115.7(9) . . ? C132 N73 Cu4 118.9(7) . . ? N74 N73 Cu4 122.7(6) . . ? C133 N74 N73 109.0(9) . . ? C134 N75 N76 119.7(8) . . ? C134 N75 Cu5 110.4(6) . . ? N76 N75 Cu5 129.7(6) . . ? N75 N76 C137 121.4(8) . . ? N75 N76 Cu6 120.0(6) . . ? C137 N76 Cu6 118.4(6) . . ? C138 N77 N78 106.1(7) . . ? C139 N78 N77 118.1(8) . . ? C139 N78 Cu7 119.4(6) . . ? N77 N78 Cu7 120.2(6) . . ? C139 N79 H31 120.0 . . ? C139 N79 H32 120.0 . . ? H31 N79 H32 120.0 . . ? C144 N80 C140 117.6(8) . . ? C144 N80 Cu7 128.4(7) . . ? C140 N80 Cu7 113.9(6) . . ? O19 N81 O17 126(2) . . ? O19 N81 O18 120.5(19) . . ? O17 N81 O18 113.7(17) . . ? O22 N82 O21 123(2) . . ? O22 N82 O20 122.3(17) . . ? O21 N82 O20 114(2) . . ? O23 N83 O24 120.0(14) . . ? O23 N83 O25 117.7(13) . . ? O24 N83 O25 121.9(13) . . ? O26 N84 O28 126.0(15) . . ? O26 N84 O27 115.6(15) . . ? O28 N84 O27 113.3(14) . . ? O29 N85 O30 112.0(16) . . ? O29 N85 O31 127.1(16) . . ? O30 N85 O31 117.6(15) . . ? O33 N86 O34 105.3(19) . . ? O33 N86 O32 130(2) . . ? O34 N86 O32 124(2) . . ? N1 C1 C2 124.6(14) . . ? N1 C1 H33 117.7 . . ? C2 C1 H33 117.7 . . ? C3 C2 C1 117.4(14) . . ? C3 C2 H34 121.3 . . ? C1 C2 H34 121.3 . . ? C2 C3 C4 121.3(12) . . ? C2 C3 H35 119.4 . . ? C4 C3 H35 119.4 . . ? C5 C4 C3 112.7(13) . . ? C5 C4 H36 123.6 . . ? C3 C4 H36 123.6 . . ? N1 C5 C4 125.8(11) . . ? N1 C5 C6 113.7(10) . . ? C4 C5 C6 120.5(12) . . ? N3 C6 N2 122.8(10) . . ? N3 C6 C5 115.1(11) . . ? N2 C6 C5 122.0(10) . . ? N4 C7 O1 127.4(10) . . ? N4 C7 C8 117.2(11) . . ? O1 C7 C8 115.4(10) . . ? N5 C8 C9 122.3(9) . . ? N5 C8 C7 114.7(10) . . ? C9 C8 C7 122.9(10) . . ? C10 C9 C8 117.9(11) . . ? C10 C9 H37 121.1 . . ? C8 C9 H37 121.1 . . ? C9 C10 C11 117.7(11) . . ? C9 C10 H38 121.1 . . ? C11 C10 H38 121.1 . . ? N6 C11 C10 123.1(9) . . ? N6 C11 C12 113.3(8) . . ? C10 C11 C12 123.6(10) . . ? N7 C12 O2 125.2(9) . . ? N7 C12 C11 117.7(9) . . ? O2 C12 C11 117.1(9) . . ? N9 C13 N8 125.4(10) . . ? N9 C13 C14 121.6(10) . . ? N8 C13 C14 113.0(10) . . ? C15 C14 N10 124.5(11) . . ? C15 C14 C13 122.3(12) . . ? N10 C14 C13 113.1(9) . . ? C14 C15 C16 115.6(15) . . ? C14 C15 H39 122.2 . . ? C16 C15 H39 122.2 . . ? C17 C16 C15 120.5(15) . . ? C17 C16 H40 119.7 . . ? C15 C16 H40 119.7 . . ? C16 C17 C18 117.4(14) . . ? C16 C17 H41 121.3 . . ? C18 C17 H41 121.3 . . ? N10 C18 C17 123.2(16) . . ? N10 C18 H42 118.4 . . ? C17 C18 H42 118.4 . . ? N11 C19 C20 120.1(14) . . ? N11 C19 H43 120.0 . . ? C20 C19 H43 120.0 . . ? C19 C20 C21 118.2(13) . . ? C19 C20 H44 120.9 . . ? C21 C20 H44 120.9 . . ? C22 C21 C20 119.1(12) . . ? C22 C21 H45 120.5 . . ? C20 C21 H45 120.5 . . ? C21 C22 C23 120.4(14) . . ? C21 C22 H46 119.8 . . ? C23 C22 H46 119.8 . . ? N11 C23 C22 120.2(11) . . ? N11 C23 C24 113.4(10) . . ? C22 C23 C24 123.6(12) . . ? N12 C24 N13 128.6(14) . . ? N12 C24 C23 119.3(13) . . ? N13 C24 C23 111.1(11) . . ? O3 C25 N14 122.0(11) . . ? O3 C25 C26 116.5(9) . . ? N14 C25 C26 121.1(10) . . ? O3 C25 Na1 53.6(6) . . ? N14 C25 Na1 164.7(11) . . ? C26 C25 Na1 63.7(6) . . ? C27 C26 N15 122.5(10) . . ? C27 C26 C25 120.4(10) . . ? N15 C26 C25 117.1(10) . . ? C27 C26 Na1 143.3(9) . . ? N15 C26 Na1 38.8(6) . . ? C25 C26 Na1 86.7(7) . . ? C26 C27 C28 121.1(10) . . ? C26 C27 H47 119.5 . . ? C28 C27 H47 119.5 . . ? C29 C28 C27 119.4(11) . . ? C29 C28 H48 120.3 . . ? C27 C28 H48 120.3 . . ? C28 C29 N16 124.2(10) . . ? C28 C29 C30 121.1(10) . . ? N16 C29 C30 114.7(9) . . ? C28 C29 Na2 150.8(11) . . ? N16 C29 Na2 45.0(8) . . ? C30 C29 Na2 75.7(9) . . ? O4 C30 N17 123.7(9) . . ? O4 C30 C29 121.1(10) . . ? N17 C30 C29 115.3(9) . . ? O4 C30 Na2 56.1(8) . . ? N17 C30 Na2 152.3(10) . . ? C29 C30 Na2 72.1(8) . . ? N18 C31 N19 126.8(10) . . ? N18 C31 C32 112.2(9) . . ? N19 C31 C32 120.9(10) . . ? C33 C32 N20 121.4(10) . . ? C33 C32 C31 126.7(11) . . ? N20 C32 C31 111.9(9) . . ? C34 C33 C32 120.5(13) . . ? C34 C33 H49 119.8 . . ? C32 C33 H49 119.8 . . ? C33 C34 C35 119.6(13) . . ? C33 C34 H50 120.2 . . ? C35 C34 H50 120.2 . . ? C34 C35 C36 122.1(12) . . ? C34 C35 H51 119.0 . . ? C36 C35 H51 119.0 . . ? N20 C36 C35 116.7(14) . . ? N20 C36 H52 121.7 . . ? C35 C36 H52 121.7 . . ? N21 C37 C38 119.4(13) . . ? N21 C37 H53 120.3 . . ? C38 C37 H53 120.3 . . ? C39 C38 C37 122.2(14) . . ? C39 C38 H54 118.9 . . ? C37 C38 H54 118.9 . . ? C38 C39 C40 118.4(13) . . ? C38 C39 H55 120.8 . . ? C40 C39 H55 120.8 . . ? C41 C40 C39 113.9(16) . . ? C41 C40 H56 123.0 . . ? C39 C40 H56 123.0 . . ? N21 C41 C40 122.5(13) . . ? N21 C41 C42 113.3(10) . . ? C40 C41 C42 123.6(14) . . ? N23 C42 N22 121.0(15) . . ? N23 C42 C41 113.0(12) . . ? N22 C42 C41 124.4(13) . . ? N24 C43 O5 125.2(10) . . ? N24 C43 C44 120.1(11) . . ? O5 C43 C44 114.6(9) . . ? N24 C43 Na3 157.0(9) . . ? O5 C43 Na3 51.7(5) . . ? C44 C43 Na3 67.9(6) . . ? C45 C44 N25 119.7(10) . . ? C45 C44 C43 120.6(11) . . ? N25 C44 C43 119.6(10) . . ? C45 C44 Na3 152.3(10) . . ? N25 C44 Na3 38.3(6) . . ? C43 C44 Na3 83.1(6) . . ? C44 C45 C46 120.7(12) . . ? C44 C45 H57 119.7 . . ? C46 C45 H57 119.7 . . ? C47 C46 C45 120.2(11) . . ? C47 C46 H58 119.9 . . ? C45 C46 H58 119.9 . . ? C46 C47 N26 121.4(10) . . ? C46 C47 C48 123.2(10) . . ? N26 C47 C48 115.4(9) . . ? C46 C47 Na4 152.5(9) . . ? N26 C47 Na4 38.5(5) . . ? C48 C47 Na4 79.9(6) . . ? O6 C48 N27 126.2(8) . . ? O6 C48 C47 116.7(9) . . ? N27 C48 C47 117.0(9) . . ? O6 C48 Na4 47.9(5) . . ? N27 C48 Na4 169.0(7) . . ? C47 C48 Na4 69.2(6) . . ? N28 C49 N29 126.4(9) . . ? N28 C49 C50 112.5(8) . . ? N29 C49 C50 120.9(9) . . ? N30 C50 C51 121.5(9) . . ? N30 C50 C49 112.8(8) . . ? C51 C50 C49 125.7(10) . . ? C52 C51 C50 121.0(11) . . ? C52 C51 H59 119.5 . . ? C50 C51 H59 119.5 . . ? C51 C52 C53 116.7(10) . . ? C51 C52 H60 121.6 . . ? C53 C52 H60 121.6 . . ? C52 C53 C54 120.4(11) . . ? C52 C53 H61 119.8 . . ? C54 C53 H61 119.8 . . ? N30 C54 C53 122.6(11) . . ? N30 C54 H62 118.7 . . ? C53 C54 H62 118.7 . . ? N31 C55 C56 118.0(16) . . ? N31 C55 H63 121.0 . . ? C56 C55 H63 121.0 . . ? C57 C56 C55 123.6(15) . . ? C57 C56 H64 118.2 . . ? C55 C56 H64 118.2 . . ? C56 C57 C58 120.5(14) . . ? C56 C57 H65 119.8 . . ? C58 C57 H65 119.8 . . ? C57 C58 C59 114.0(14) . . ? C57 C58 H66 123.0 . . ? C59 C58 H66 123.0 . . ? N31 C59 C60 118.7(10) . . ? N31 C59 C58 123.4(12) . . ? C60 C59 C58 117.7(12) . . ? N32 C60 N33 124.1(10) . . ? N32 C60 C59 125.9(10) . . ? N33 C60 C59 110.0(11) . . ? N34 C61 O7 127.8(9) . . ? N34 C61 C62 114.0(10) . . ? O7 C61 C62 118.1(8) . . ? N35 C62 C63 120.3(8) . . ? N35 C62 C61 113.3(8) . . ? C63 C62 C61 126.4(8) . . ? C64 C63 C62 119.2(9) . . ? C64 C63 H67 120.4 . . ? C62 C63 H67 120.4 . . ? C63 C64 C65 115.7(9) . . ? C63 C64 H68 122.1 . . ? C65 C64 H68 122.1 . . ? N36 C65 C64 125.1(9) . . ? N36 C65 C66 112.4(8) . . ? C64 C65 C66 122.5(9) . . ? O8 C66 N37 126.9(8) . . ? O8 C66 C65 118.6(8) . . ? N37 C66 C65 114.5(8) . . ? N39 C67 N38 123.6(9) . . ? N39 C67 C68 121.4(10) . . ? N38 C67 C68 114.8(9) . . ? N40 C68 C69 124.3(9) . . ? N40 C68 C67 114.7(10) . . ? C69 C68 C67 121.0(10) . . ? C70 C69 C68 117.1(11) . . ? C70 C69 H69 121.4 . . ? C68 C69 H69 121.4 . . ? C71 C70 C69 119.1(12) . . ? C71 C70 H70 120.4 . . ? C69 C70 H70 120.4 . . ? C70 C71 C72 119.2(11) . . ? C70 C71 H71 120.4 . . ? C72 C71 H71 120.4 . . ? N40 C72 C71 122.4(11) . . ? N40 C72 H72 118.8 . . ? C71 C72 H72 118.8 . . ? N41 C73 C74 121.0(13) . . ? N41 C73 H73 119.5 . . ? C74 C73 H73 119.5 . . ? C75 C74 C73 121.5(12) . . ? C75 C74 H74 119.3 . . ? C73 C74 H74 119.3 . . ? C74 C75 C76 119.3(12) . . ? C74 C75 H75 120.4 . . ? C76 C75 H75 120.4 . . ? C75 C76 C77 117.7(13) . . ? C75 C76 H76 121.1 . . ? C77 C76 H76 121.1 . . ? N41 C77 C76 122.1(10) . . ? N41 C77 C78 114.0(9) . . ? C76 C77 C78 123.8(11) . . ? N42 C78 N43 122.7(10) . . ? N42 C78 C77 121.7(10) . . ? N43 C78 C77 115.3(10) . . ? O9 C79 N44 128.1(8) . . ? O9 C79 C80 116.6(9) . . ? N44 C79 C80 115.3(9) . . ? N45 C80 C81 122.4(9) . . ? N45 C80 C79 114.4(9) . . ? C81 C80 C79 123.1(10) . . ? C82 C81 C80 117.0(10) . . ? C82 C81 H77 121.5 . . ? C80 C81 H77 121.5 . . ? C81 C82 C83 117.7(9) . . ? C81 C82 H78 121.2 . . ? C83 C82 H78 121.2 . . ? N46 C83 C82 123.6(8) . . ? N46 C83 C84 112.5(8) . . ? C82 C83 C84 123.8(9) . . ? O10 C84 N47 128.4(8) . . ? O10 C84 C83 116.0(8) . . ? N47 C84 C83 115.5(9) . . ? N49 C85 N48 126.6(10) . . ? N49 C85 C86 123.0(10) . . ? N48 C85 C86 110.4(11) . . ? N50 C86 C87 119.1(10) . . ? N50 C86 C85 116.9(10) . . ? C87 C86 C85 123.9(11) . . ? C88 C87 C86 119.8(13) . . ? C88 C87 H79 120.1 . . ? C86 C87 H79 120.1 . . ? C89 C88 C87 119.7(12) . . ? C89 C88 H80 120.1 . . ? C87 C88 H80 120.1 . . ? C90 C89 C88 118.0(12) . . ? C90 C89 H81 121.0 . . ? C88 C89 H81 121.0 . . ? C89 C90 N50 124.7(13) . . ? C89 C90 H82 117.7 . . ? N50 C90 H82 117.7 . . ? C92 C91 N51 124.5(14) . . ? C92 C91 H83 117.8 . . ? N51 C91 H83 117.8 . . ? C91 C92 C93 119.3(14) . . ? C91 C92 H84 120.4 . . ? C93 C92 H84 120.4 . . ? C92 C93 C94 121.8(14) . . ? C92 C93 H85 119.1 . . ? C94 C93 H85 119.1 . . ? C95 C94 C93 114.5(16) . . ? C95 C94 H86 122.7 . . ? C93 C94 H86 122.7 . . ? N51 C95 C94 121.0(12) . . ? N51 C95 C96 115.3(9) . . ? C94 C95 C96 123.7(14) . . ? N53 C96 N52 124.8(11) . . ? N53 C96 C95 112.3(11) . . ? N52 C96 C95 122.9(11) . . ? O11 C97 N54 126.3(9) . . ? O11 C97 C98 117.4(8) . . ? N54 C97 C98 116.2(8) . . ? O11 C97 Na1 49.9(5) . . ? N54 C97 Na1 170.5(8) . . ? C98 C97 Na1 67.9(6) . . ? C99 C98 N55 120.4(10) . . ? C99 C98 C97 120.5(9) . . ? N55 C98 C97 119.2(9) . . ? C99 C98 Na1 156.4(8) . . ? N55 C98 Na1 39.8(6) . . ? C97 C98 Na1 80.8(6) . . ? C100 C99 C98 121.5(9) . . ? C100 C99 H87 119.3 . . ? C98 C99 H87 119.3 . . ? C99 C100 C101 119.8(9) . . ? C99 C100 H88 120.1 . . ? C101 C100 H88 120.1 . . ? C100 C101 N56 120.5(9) . . ? C100 C101 C102 121.9(9) . . ? N56 C101 C102 117.6(10) . . ? C100 C101 Na3 151.2(7) . . ? N56 C101 Na3 33.3(5) . . ? C102 C101 Na3 85.4(7) . . ? O12 C102 N57 124.8(8) . . ? O12 C102 C101 115.5(9) . . ? N57 C102 C101 119.7(9) . . ? O12 C102 Na3 51.0(5) . . ? N57 C102 Na3 170.8(7) . . ? C101 C102 Na3 64.9(6) . . ? N58 C103 N59 127.7(10) . . ? N58 C103 C104 111.2(9) . . ? N59 C103 C104 121.0(10) . . ? C105 C104 N60 121.7(10) . . ? C105 C104 C103 124.5(10) . . ? N60 C104 C103 113.8(8) . . ? C104 C105 C106 119.0(12) . . ? C104 C105 H89 120.5 . . ? C106 C105 H89 120.5 . . ? C107 C106 C105 121.7(11) . . ? C107 C106 H90 119.1 . . ? C105 C106 H90 119.1 . . ? C106 C107 C108 117.1(11) . . ? C106 C107 H91 121.5 . . ? C108 C107 H91 121.5 . . ? N60 C108 C107 121.3(11) . . ? N60 C108 H92 119.3 . . ? C107 C108 H92 119.3 . . ? C110 C109 N61 122.1(12) . . ? C110 C109 H93 119.0 . . ? N61 C109 H93 119.0 . . ? C109 C110 C111 119.0(11) . . ? C109 C110 H94 120.5 . . ? C111 C110 H94 120.5 . . ? C112 C111 C110 120.6(11) . . ? C112 C111 H95 119.7 . . ? C110 C111 H95 119.7 . . ? C111 C112 C113 118.2(12) . . ? C111 C112 H96 120.9 . . ? C113 C112 H96 120.9 . . ? N61 C113 C112 123.0(9) . . ? N61 C113 C114 113.2(8) . . ? C112 C113 C114 123.8(11) . . ? N62 C114 N63 126.3(10) . . ? N62 C114 C113 123.1(9) . . ? N63 C114 C113 110.5(10) . . ? O13 C115 N64 125.8(9) . . ? O13 C115 C116 116.8(9) . . ? N64 C115 C116 117.4(9) . . ? O13 C115 Na2 55.5(8) . . ? N64 C115 Na2 164.1(9) . . ? C116 C115 Na2 64.0(8) . . ? C117 C116 N65 121.7(9) . . ? C117 C116 C115 120.3(10) . . ? N65 C116 C115 117.9(10) . . ? C117 C116 Na2 149.9(10) . . ? N65 C116 Na2 37.6(8) . . ? C115 C116 Na2 83.9(9) . . ? C118 C117 C116 121.7(10) . . ? C118 C117 H97 119.1 . . ? C116 C117 H97 119.1 . . ? C117 C118 C119 119.0(11) . . ? C117 C118 H98 120.5 . . ? C119 C118 H98 120.5 . . ? C118 C119 N66 120.7(9) . . ? C118 C119 C120 120.7(10) . . ? N66 C119 C120 118.6(10) . . ? C118 C119 Na4 149.3(8) . . ? N66 C119 Na4 40.3(5) . . ? C120 C119 Na4 83.4(6) . . ? N67 C120 O14 124.8(9) . . ? N67 C120 C119 119.8(10) . . ? O14 C120 C119 115.4(9) . . ? N67 C120 Na4 160.0(7) . . ? O14 C120 Na4 53.2(5) . . ? C119 C120 Na4 65.9(6) . . ? N68 C121 N69 125.0(10) . . ? N68 C121 C122 113.4(9) . . ? N69 C121 C122 121.6(9) . . ? N70 C122 C123 122.8(11) . . ? N70 C122 C121 113.9(9) . . ? C123 C122 C121 123.2(11) . . ? C124 C123 C122 116.5(13) . . ? C124 C123 H99 121.8 . . ? C122 C123 H99 121.8 . . ? C123 C124 C125 121.0(11) . . ? C123 C124 H100 119.5 . . ? C125 C124 H100 119.5 . . ? C126 C125 C124 117.1(11) . . ? C126 C125 H101 121.4 . . ? C124 C125 H101 121.4 . . ? N70 C126 C125 124.1(12) . . ? N70 C126 H102 118.0 . . ? C125 C126 H102 118.0 . . ? N71 C127 C128 119.1(14) . . ? N71 C127 H103 120.4 . . ? C128 C127 H103 120.4 . . ? C129 C128 C127 120.9(13) . . ? C129 C128 H104 119.6 . . ? C127 C128 H104 119.6 . . ? C130 C129 C128 117.9(13) . . ? C130 C129 H105 121.1 . . ? C128 C129 H105 121.1 . . ? C129 C130 C131 118.8(13) . . ? C129 C130 H106 120.6 . . ? C131 C130 H106 120.6 . . ? N71 C131 C130 125.0(10) . . ? N71 C131 C132 114.8(9) . . ? C130 C131 C132 120.2(11) . . ? N73 C132 N72 124.9(9) . . ? N73 C132 C131 112.4(9) . . ? N72 C132 C131 122.7(8) . . ? N74 C133 O15 126.4(9) . . ? N74 C133 C134 115.5(10) . . ? O15 C133 C134 118.1(8) . . ? N75 C134 C135 122.7(8) . . ? N75 C134 C133 113.6(9) . . ? C135 C134 C133 123.7(9) . . ? C136 C135 C134 117.8(9) . . ? C136 C135 H107 121.1 . . ? C134 C135 H107 121.1 . . ? C135 C136 C137 118.2(9) . . ? C135 C136 H108 120.9 . . ? C137 C136 H108 120.9 . . ? N76 C137 C136 120.1(8) . . ? N76 C137 C138 114.8(8) . . ? C136 C137 C138 125.1(9) . . ? N77 C138 O16 125.9(8) . . ? N77 C138 C137 117.2(8) . . ? O16 C138 C137 116.9(8) . . ? N78 C139 N79 125.5(9) . . ? N78 C139 C140 112.2(9) . . ? N79 C139 C140 122.3(8) . . ? N80 C140 C141 122.8(9) . . ? N80 C140 C139 112.8(8) . . ? C141 C140 C139 124.5(10) . . ? C140 C141 C142 118.5(11) . . ? C140 C141 H109 120.8 . . ? C142 C141 H109 120.8 . . ? C143 C142 C141 118.9(9) . . ? C143 C142 H110 120.6 . . ? C141 C142 H110 120.6 . . ? C142 C143 C144 120.8(10) . . ? C142 C143 H111 119.6 . . ? C144 C143 H111 119.6 . . ? N80 C144 C143 121.4(11) . . ? N80 C144 H112 119.3 . . ? C143 C144 H112 119.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.589 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.193 #=== data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 717941' # start Validation Reply Form _vrf_PLAT306_Compound1 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O2W RESPONSE: These are lattice solvent molecules for which the corresponding protons could not be located in the difference map and hence were omitted from the model ; _vrf_PLAT430_Compound1 ; PROBLEM: Short Inter D...A Contact O18W .. O19W .. 1.79 Ang. RESPONSE: These are partial occupancy lattice solvent water molecules for which the sum of the occupancies does not exceed one. ; _vrf_PLAT031_Compound1 ; PROBLEM: Refined Extinction Parameter within Range ...... 0.33 Sigma RESPONSE: The extinction was refined and it's value and corresponding s.u. are reported. ; _vrf_PLAT761_Compound1 ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: Hydrogen atoms were introduced in calculated positions with thermal parameters set 20% greater than their bonding partners. They were refined on a riding model. X-H bond distances are therefore not reported. ; _vrf_PLAT762_Compound1 ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: Hydrogen atoms were introduced in calculated positions with thermal parameters set 20% greater than their bonding partners. They were refined on a riding model. X-Y-H or H-Y-H angles are therefore not reported. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H48 N33 Na Ni3 O33.50' _chemical_formula_weight 1894.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.211(3) _cell_length_b 15.363(3) _cell_length_c 19.525(4) _cell_angle_alpha 111.999(2) _cell_angle_beta 91.168(3) _cell_angle_gamma 109.541(2) _cell_volume 3931.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 875 _cell_measurement_theta_min 14.86 _cell_measurement_theta_max 22.83 _exptl_crystal_description 'triangular block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1932 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 48465 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13820 _reflns_number_gt 10510 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+9.4922P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13820 _refine_ls_number_parameters 1097 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1530 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _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 0.16160(4) 0.38057(4) 0.08180(3) 0.01765(14) Uani 1 1 d . . . Ni2 Ni 0.30147(4) 0.28455(4) 0.16851(3) 0.01826(14) Uani 1 1 d . . . Ni3 Ni 0.59438(4) 0.10939(4) 0.34089(3) 0.01974(15) Uani 1 1 d . . . O101 O 0.3367(2) 0.0811(3) 0.39794(19) 0.0344(8) Uani 1 1 d . . . N101 N 0.6959(3) 0.2145(3) 0.4351(2) 0.0256(8) Uani 1 1 d . . . C101 C 0.7818(3) 0.2143(4) 0.4518(3) 0.0307(11) Uani 1 1 d . . . H10A H 0.8006 0.1653 0.4179 0.037 Uiso 1 1 calc R . . O102 O 0.0134(2) 0.1287(2) 0.15836(18) 0.0264(7) Uani 1 1 d . . . N102 N 0.5477(3) 0.3603(3) 0.4959(2) 0.0300(9) Uani 1 1 d . . . H10B H 0.4929 0.3582 0.4817 0.036 Uiso 1 1 calc R . . H10C H 0.5848 0.4117 0.5339 0.036 Uiso 1 1 calc R . . C102 C 0.8431(4) 0.2830(4) 0.5164(3) 0.0407(13) Uani 1 1 d . . . H10D H 0.9026 0.2814 0.5259 0.049 Uiso 1 1 calc R . . N103 N 0.5247(2) 0.2026(3) 0.4013(2) 0.0219(8) Uani 1 1 d . . . C103 C 0.8147(4) 0.3549(4) 0.5673(3) 0.0468(14) Uani 1 1 d . . . H10E H 0.8544 0.4011 0.6123 0.056 Uiso 1 1 calc R . . N104 N 0.4409(2) 0.2055(3) 0.3721(2) 0.0223(8) Uani 1 1 d . . . H10F H 0.4455 0.2505 0.3548 0.027 Uiso 1 1 calc R . . C104 C 0.7269(3) 0.3580(4) 0.5511(3) 0.0364(12) Uani 1 1 d . . . H10G H 0.7070 0.4063 0.5846 0.044 Uiso 1 1 calc R . . N105 N 0.3117(2) 0.2099(3) 0.28798(19) 0.0213(8) Uani 1 1 d . . . H10H H 0.3713 0.2447 0.2958 0.026 Uiso 1 1 calc R . . C105 C 0.6694(3) 0.2872(3) 0.4836(2) 0.0230(9) Uani 1 1 d . . . N106 N 0.2533(2) 0.2163(3) 0.24061(19) 0.0200(7) Uani 1 1 d . . . C106 C 0.5748(3) 0.2841(3) 0.4594(2) 0.0209(9) Uani 1 1 d . . . N107 N 0.1571(2) 0.2104(2) 0.12863(18) 0.0174(7) Uani 1 1 d . . . C107 C 0.3548(3) 0.1425(3) 0.3699(2) 0.0197(9) Uani 1 1 d . . . N108 N 0.1153(2) 0.2320(3) 0.07462(18) 0.0171(7) Uani 1 1 d . . . C108 C 0.2786(3) 0.1497(3) 0.3237(2) 0.0181(8) Uani 1 1 d . . . N109 N 0.0937(3) 0.0705(3) -0.0156(2) 0.0218(8) Uani 1 1 d . . . H10I H 0.1128 0.0523 0.0167 0.026 Uiso 1 1 calc R . . H10J H 0.0763 0.0292 -0.0619 0.026 Uiso 1 1 calc R . . C109 C 0.1829(3) 0.0978(3) 0.3174(2) 0.0241(9) Uani 1 1 d . . . H10K H 0.1608 0.0592 0.3449 0.029 Uiso 1 1 calc R . . N110 N 0.0918(2) 0.2982(3) -0.02804(19) 0.0201(7) Uani 1 1 d . . . C110 C 0.1214(3) 0.1053(3) 0.2689(2) 0.0213(9) Uani 1 1 d . . . H11A H 0.0563 0.0737 0.2637 0.026 Uiso 1 1 calc R . . C111 C 0.1607(3) 0.1620(3) 0.2280(2) 0.0167(8) Uani 1 1 d . . . C112 C 0.1024(3) 0.1667(3) 0.1668(2) 0.0176(8) Uani 1 1 d . . . C113 C 0.0909(3) 0.1634(3) 0.0064(2) 0.0172(8) Uani 1 1 d . . . C114 C 0.0644(3) 0.1970(3) -0.0509(2) 0.0184(8) Uani 1 1 d . . . C115 C 0.0170(3) 0.1310(3) -0.1225(2) 0.0234(9) Uani 1 1 d . . . H11B H -0.0006 0.0617 -0.1374 0.028 Uiso 1 1 calc R . . C116 C -0.0042(3) 0.1694(4) -0.1721(3) 0.0301(11) Uani 1 1 d . . . H11C H -0.0374 0.1262 -0.2201 0.036 Uiso 1 1 calc R . . C117 C 0.0249(3) 0.2726(4) -0.1489(3) 0.0339(11) Uani 1 1 d . . . H11D H 0.0126 0.3003 -0.1813 0.041 Uiso 1 1 calc R . . C118 C 0.0728(3) 0.3342(4) -0.0769(3) 0.0276(10) Uani 1 1 d . . . H11E H 0.0927 0.4038 -0.0616 0.033 Uiso 1 1 calc R . . O201 O 0.4675(3) -0.0717(3) 0.10641(18) 0.0357(8) Uani 1 1 d . . . N201 N 0.5408(2) -0.0026(3) 0.38136(19) 0.0205(8) Uani 1 1 d . . . C201 C 0.5838(3) -0.0094(4) 0.4389(3) 0.0268(10) Uani 1 1 d . . . H20A H 0.6362 0.0456 0.4700 0.032 Uiso 1 1 calc R . . O202 O 0.3265(2) 0.2163(2) -0.05491(17) 0.0310(8) Uani 1 1 d . . . N202 N 0.3340(3) -0.1292(3) 0.2389(2) 0.0316(9) Uani 1 1 d . . . H20B H 0.3088 -0.1206 0.2033 0.038 Uiso 1 1 calc R . . H20C H 0.3033 -0.1786 0.2505 0.038 Uiso 1 1 calc R . . C202 C 0.5527(4) -0.0955(4) 0.4536(3) 0.0312(11) Uani 1 1 d . . . H20D H 0.5838 -0.0981 0.4939 0.037 Uiso 1 1 calc R . . N203 N 0.4737(2) 0.0109(3) 0.26409(19) 0.0192(7) Uani 1 1 d . . . C203 C 0.4751(4) -0.1767(4) 0.4076(3) 0.0325(11) Uani 1 1 d . . . H20E H 0.4543 -0.2359 0.4154 0.039 Uiso 1 1 calc R . . N204 N 0.4307(3) 0.0319(3) 0.21028(19) 0.0214(8) Uani 1 1 d . . . H20F H 0.3995 0.0711 0.2253 0.026 Uiso 1 1 calc R . . C204 C 0.4278(4) -0.1700(3) 0.3492(3) 0.0295(10) Uani 1 1 d . . . H20G H 0.3741 -0.2235 0.3184 0.035 Uiso 1 1 calc R . . N205 N 0.3729(2) 0.1167(3) 0.13771(19) 0.0199(7) Uani 1 1 d . . . H20H H 0.3738 0.1304 0.1847 0.024 Uiso 1 1 calc R . . C205 C 0.4628(3) -0.0812(3) 0.3380(2) 0.0208(9) Uani 1 1 d . . . N206 N 0.3468(2) 0.1703(3) 0.10826(19) 0.0195(7) Uani 1 1 d . . . C206 C 0.4194(3) -0.0669(3) 0.2757(2) 0.0200(9) Uani 1 1 d . . . N207 N 0.3207(2) 0.3022(3) 0.0700(2) 0.0192(7) Uani 1 1 d . . . C207 C 0.4361(3) -0.0058(3) 0.1374(2) 0.0200(9) Uani 1 1 d . . . N208 N 0.2901(2) 0.3721(3) 0.0562(2) 0.0195(7) Uani 1 1 d . . . C208 C 0.3980(3) 0.0412(3) 0.0948(2) 0.0192(9) Uani 1 1 d . . . N209 N 0.4487(3) 0.4742(3) 0.0728(2) 0.0301(9) Uani 1 1 d . . . H20I H 0.4683 0.4288 0.0751 0.036 Uiso 1 1 calc R . . H20J H 0.4887 0.5316 0.0769 0.036 Uiso 1 1 calc R . . C209 C 0.3919(3) 0.0118(3) 0.0182(2) 0.0225(9) Uani 1 1 d . . . H20K H 0.4030 -0.0455 -0.0119 0.027 Uiso 1 1 calc R . . N210 N 0.2294(3) 0.5164(3) 0.0707(2) 0.0221(8) Uani 1 1 d . . . C210 C 0.3688(3) 0.0709(3) -0.0115(2) 0.0237(9) Uani 1 1 d . . . H21A H 0.3657 0.0559 -0.0625 0.028 Uiso 1 1 calc R . . C211 C 0.3504(3) 0.1532(3) 0.0361(2) 0.0183(8) Uani 1 1 d . . . C212 C 0.3306(3) 0.2285(3) 0.0127(2) 0.0194(9) Uani 1 1 d . . . C213 C 0.3561(3) 0.4557(3) 0.0630(2) 0.0215(9) Uani 1 1 d . . . C214 C 0.3205(3) 0.5340(3) 0.0607(2) 0.0211(9) Uani 1 1 d . . . C215 C 0.3747(3) 0.6180(3) 0.0490(3) 0.0292(10) Uani 1 1 d . . . H21B H 0.4372 0.6285 0.0424 0.035 Uiso 1 1 calc R . . C216 C 0.3351(4) 0.6862(3) 0.0473(3) 0.0359(12) Uani 1 1 d . . . H21C H 0.3698 0.7420 0.0380 0.043 Uiso 1 1 calc R . . C217 C 0.2430(4) 0.6700(3) 0.0598(3) 0.0302(11) Uani 1 1 d . . . H21D H 0.2154 0.7159 0.0606 0.036 Uiso 1 1 calc R . . C218 C 0.1929(3) 0.5850(3) 0.0710(3) 0.0279(10) Uani 1 1 d . . . H21E H 0.1309 0.5745 0.0791 0.033 Uiso 1 1 calc R . . O301 O 0.6973(2) 0.3959(2) 0.3723(2) 0.0370(8) Uani 1 1 d . . . N301 N 0.6884(2) 0.0440(3) 0.2864(2) 0.0221(8) Uani 1 1 d . . . C301 C 0.7095(3) -0.0302(3) 0.2935(3) 0.0291(10) Uani 1 1 d . . . H30A H 0.6832 -0.0546 0.3283 0.035 Uiso 1 1 calc R . . O302 O 0.3781(2) 0.5948(2) 0.26750(19) 0.0298(7) Uani 1 1 d . . . N302 N 0.7338(3) 0.2014(3) 0.1824(2) 0.0317(9) Uani 1 1 d . . . H30B H 0.7175 0.2482 0.1789 0.038 Uiso 1 1 calc R . . H30C H 0.7712 0.1797 0.1541 0.038 Uiso 1 1 calc R . . C302 C 0.7685(3) -0.0726(4) 0.2518(3) 0.0331(11) Uani 1 1 d . . . H30D H 0.7837 -0.1220 0.2600 0.040 Uiso 1 1 calc R . . N303 N 0.6446(2) 0.1890(3) 0.2769(2) 0.0222(8) Uani 1 1 d . . . C303 C 0.8036(4) -0.0401(4) 0.1983(3) 0.0421(13) Uani 1 1 d . . . H30E H 0.8403 -0.0702 0.1675 0.050 Uiso 1 1 calc R . . N304 N 0.6105(3) 0.2585(3) 0.2675(2) 0.0232(8) Uani 1 1 d . . . H30F H 0.5713 0.2385 0.2275 0.028 Uiso 1 1 calc R . . C304 C 0.7845(3) 0.0378(4) 0.1901(3) 0.0349(12) Uani 1 1 d . . . H30G H 0.8092 0.0618 0.1547 0.042 Uiso 1 1 calc R . . C305 C 0.7276(3) 0.0793(3) 0.2359(3) 0.0244(9) Uani 1 1 d . . . N306 N 0.4956(2) 0.3436(3) 0.2513(2) 0.0216(8) Uani 1 1 d . . . H30H H 0.4860 0.2804 0.2289 0.026 Uiso 1 1 calc R . . C306 C 0.7016(3) 0.1628(3) 0.2309(3) 0.0242(10) Uani 1 1 d . . . N307 N 0.4329(2) 0.3784(3) 0.2355(2) 0.0197(7) Uani 1 1 d . . . C307 C 0.6350(3) 0.3538(3) 0.3167(2) 0.0210(9) Uani 1 1 d . . . C308 C 0.5734(3) 0.4054(3) 0.3016(2) 0.0199(9) Uani 1 1 d . . . N309 N 0.2881(2) 0.4227(3) 0.2218(2) 0.0196(7) Uani 1 1 d . . . C309 C 0.5931(3) 0.5084(3) 0.3385(3) 0.0270(10) Uani 1 1 d . . . H30I H 0.6482 0.5511 0.3730 0.032 Uiso 1 1 calc R . . N310 N 0.2085(2) 0.4364(2) 0.1959(2) 0.0188(7) Uani 1 1 d . . . C310 C 0.5280(3) 0.5446(3) 0.3220(3) 0.0263(10) Uani 1 1 d . . . H31A H 0.5380 0.6130 0.3446 0.032 Uiso 1 1 calc R . . N311 N 0.1458(3) 0.4132(3) 0.2992(2) 0.0279(9) Uani 1 1 d . . . H31B H 0.1977 0.4141 0.3183 0.033 Uiso 1 1 calc R . . H31C H 0.0975 0.4053 0.3216 0.033 Uiso 1 1 calc R . . C311 C 0.4467(3) 0.4761(3) 0.2708(2) 0.0184(9) Uani 1 1 d . . . C312 C 0.3658(3) 0.5042(3) 0.2519(2) 0.0183(9) Uani 1 1 d . . . N312 N 0.0449(2) 0.4070(3) 0.1284(2) 0.0216(8) Uani 1 1 d . . . C313 C 0.1402(3) 0.4241(3) 0.2342(2) 0.0187(9) Uani 1 1 d . . . C314 C 0.0512(3) 0.4243(3) 0.2016(2) 0.0212(9) Uani 1 1 d . . . C315 C -0.0197(3) 0.4419(3) 0.2423(3) 0.0272(10) Uani 1 1 d . . . H31D H -0.0139 0.4532 0.2927 0.033 Uiso 1 1 calc R . . C316 C -0.0986(3) 0.4422(4) 0.2066(3) 0.0324(11) Uani 1 1 d . . . H31E H -0.1463 0.4549 0.2329 0.039 Uiso 1 1 calc R . . C317 C -0.1062(3) 0.4234(4) 0.1312(3) 0.0303(11) Uani 1 1 d . . . H31F H -0.1590 0.4228 0.1058 0.036 Uiso 1 1 calc R . . C318 C -0.0330(3) 0.4056(3) 0.0948(3) 0.0263(10) Uani 1 1 d . . . H31G H -0.0385 0.3919 0.0439 0.032 Uiso 1 1 calc R . . N1 N 0.1832(3) 0.9201(3) 0.0951(2) 0.0268(9) Uani 1 1 d . . . O1 O 0.1699(3) 0.8378(3) 0.0417(2) 0.0525(11) Uani 1 1 d . . . O2 O 0.2171(2) 0.9359(3) 0.1592(2) 0.0401(9) Uani 1 1 d . . . O3 O 0.1601(2) 0.9845(2) 0.0836(2) 0.0320(8) Uani 1 1 d . . . N2 N 0.5998(3) 0.3130(4) 0.1166(2) 0.0364(10) Uani 1 1 d . . . O4 O 0.5568(3) 0.3546(4) 0.0943(3) 0.0720(16) Uani 1 1 d . . . O5 O 0.5652(3) 0.2207(3) 0.1008(2) 0.0505(10) Uani 1 1 d . . . O6 O 0.6808(2) 0.3645(3) 0.1578(2) 0.0410(9) Uani 1 1 d . . . N3 N 0.3052(3) 0.3844(3) 0.4313(2) 0.0457(12) Uani 1 1 d D . . O7 O 0.2154(3) 0.3452(4) 0.4181(3) 0.0516(7) Uiso 0.80 1 d PD . . O8 O 0.3390(3) 0.4410(4) 0.3991(3) 0.0516(7) Uiso 0.80 1 d PD . . O9 O 0.3473(4) 0.3612(4) 0.4712(3) 0.0516(7) Uiso 0.80 1 d PD . . O7A O 0.3911(6) 0.4195(13) 0.4252(11) 0.0516(7) Uiso 0.20 1 d PD . . O8A O 0.2542(10) 0.4284(13) 0.4241(11) 0.0516(7) Uiso 0.20 1 d PD . . O9A O 0.2913(12) 0.3317(13) 0.4685(10) 0.0516(7) Uiso 0.20 1 d PD . . Na1 Na 0.4576(7) 0.1961(7) 0.2607(5) 0.016(4) Uiso 0.152(7) 1 d P . . O2W O 0.5515(3) 0.8247(3) 0.1568(2) 0.0426(9) Uani 1 1 d . . . O3W O 0.3650(3) 0.3588(3) -0.1139(2) 0.0449(9) Uani 1 1 d . . . O4W O 0.5489(3) 0.7152(3) 0.2386(2) 0.0425(9) Uani 1 1 d . . . O5W O -0.1232(2) 0.1734(3) 0.0984(2) 0.0413(9) Uani 1 1 d . . . O6W O 0.9566(6) 0.0887(7) 0.3934(5) 0.0838(12) Uiso 0.70 1 d P . . O6WA O 0.9963(15) 0.1075(15) 0.4223(12) 0.0838(12) Uiso 0.30 1 d P . . O7W O 0.8303(6) 0.0810(6) 0.6028(5) 0.0838(12) Uiso 0.70 1 d P . . O7WA O 0.9006(13) 0.0933(14) 0.5420(11) 0.0838(12) Uiso 0.30 1 d P . . O8W O 1.1247(6) 0.2208(6) 0.4899(5) 0.0838(12) Uiso 0.70 1 d P . . O8WA O 1.1774(15) 0.2205(15) 0.5056(11) 0.0838(12) Uiso 0.30 1 d P . . O9W O 0.0216(4) 0.0989(4) -0.3499(3) 0.0889(17) Uani 1 1 d . . . O10W O 0.9223(4) 0.2865(4) 0.6843(3) 0.0756(14) Uani 1 1 d . . . O11W O 0.6972(3) 0.7759(4) 0.3530(3) 0.0684(13) Uani 1 1 d . . . O12W O 1.0794(3) 0.3485(4) 0.6109(3) 0.0718(13) Uani 1 1 d . . . O13W O 0.8334(3) 0.7009(4) 0.2913(3) 0.0684(13) Uani 1 1 d . . . O14W O 0.8880(3) 0.4973(3) 0.4360(2) 0.0567(11) Uani 1 1 d . . . O15W O 0.7534(3) 0.5586(3) 0.1508(3) 0.0614(12) Uani 1 1 d . . . O16W O 0.7746(3) 0.3236(3) 0.7560(2) 0.0521(10) Uani 1 1 d . . . O17W O 1.0174(3) 0.4031(3) 0.4093(2) 0.0550(11) Uani 1 1 d . . . O18W O 0.8097(9) -0.0062(10) 0.4548(7) 0.101(4) Uiso 0.50 1 d P . . O19W O 0.7807(7) -0.1034(7) 0.4891(5) 0.063(2) Uiso 0.50 1 d P . . O20W O 0.9512(4) 0.2021(4) 0.3162(4) 0.0939(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0186(3) 0.0162(3) 0.0217(3) 0.0096(2) 0.0043(2) 0.0084(2) Ni2 0.0190(3) 0.0171(3) 0.0213(3) 0.0094(2) 0.0040(2) 0.0080(2) Ni3 0.0209(3) 0.0208(3) 0.0205(3) 0.0087(2) 0.0041(2) 0.0108(2) O101 0.0251(17) 0.047(2) 0.042(2) 0.0336(18) 0.0030(15) 0.0089(15) N101 0.0243(19) 0.026(2) 0.028(2) 0.0107(17) 0.0046(16) 0.0114(16) C101 0.025(2) 0.032(3) 0.036(3) 0.012(2) 0.002(2) 0.014(2) O102 0.0161(15) 0.0336(17) 0.0340(18) 0.0220(15) 0.0029(13) 0.0052(13) N102 0.027(2) 0.024(2) 0.032(2) 0.0036(17) -0.0007(17) 0.0101(17) C102 0.025(3) 0.040(3) 0.050(3) 0.009(3) -0.003(2) 0.015(2) N103 0.0195(18) 0.0243(19) 0.0232(19) 0.0090(16) 0.0016(15) 0.0105(15) C103 0.035(3) 0.039(3) 0.043(3) -0.002(3) -0.016(2) 0.009(2) N104 0.0181(18) 0.0242(19) 0.029(2) 0.0130(16) 0.0029(15) 0.0105(15) C104 0.031(3) 0.030(3) 0.037(3) 0.002(2) -0.001(2) 0.012(2) N105 0.0178(17) 0.0263(19) 0.0204(18) 0.0121(16) 0.0026(14) 0.0060(15) C105 0.020(2) 0.021(2) 0.026(2) 0.0095(19) 0.0013(18) 0.0066(18) N106 0.0228(18) 0.0235(19) 0.0172(18) 0.0104(15) 0.0026(14) 0.0105(15) C106 0.023(2) 0.021(2) 0.022(2) 0.0111(18) 0.0065(18) 0.0089(18) N107 0.0199(17) 0.0201(18) 0.0162(17) 0.0103(15) 0.0019(14) 0.0087(14) C107 0.025(2) 0.022(2) 0.015(2) 0.0071(17) 0.0072(17) 0.0117(18) N108 0.0177(17) 0.0206(18) 0.0166(18) 0.0106(15) 0.0019(14) 0.0078(14) C108 0.021(2) 0.020(2) 0.0115(19) 0.0044(17) 0.0022(16) 0.0075(17) N109 0.032(2) 0.0184(18) 0.0174(18) 0.0084(15) -0.0003(15) 0.0107(16) C109 0.026(2) 0.026(2) 0.026(2) 0.018(2) 0.0067(18) 0.0068(19) N110 0.0202(18) 0.0229(19) 0.0232(19) 0.0142(16) 0.0046(15) 0.0094(15) C110 0.016(2) 0.023(2) 0.027(2) 0.0141(19) 0.0040(17) 0.0049(17) C111 0.019(2) 0.0125(19) 0.019(2) 0.0057(16) 0.0054(16) 0.0058(16) C112 0.018(2) 0.0143(19) 0.021(2) 0.0068(17) 0.0018(17) 0.0070(17) C113 0.0097(18) 0.019(2) 0.023(2) 0.0087(18) 0.0038(16) 0.0044(16) C114 0.018(2) 0.022(2) 0.020(2) 0.0123(18) 0.0071(16) 0.0084(17) C115 0.021(2) 0.022(2) 0.024(2) 0.0085(19) 0.0025(18) 0.0048(18) C116 0.027(2) 0.036(3) 0.024(2) 0.013(2) -0.0011(19) 0.007(2) C117 0.036(3) 0.042(3) 0.035(3) 0.026(2) 0.001(2) 0.016(2) C118 0.032(2) 0.028(2) 0.029(3) 0.017(2) 0.004(2) 0.013(2) O201 0.063(2) 0.043(2) 0.0225(17) 0.0161(15) 0.0135(16) 0.0419(19) N201 0.0220(18) 0.0263(19) 0.0181(18) 0.0096(16) 0.0055(15) 0.0139(16) C201 0.025(2) 0.037(3) 0.023(2) 0.013(2) 0.0050(18) 0.017(2) O202 0.051(2) 0.0344(18) 0.0238(17) 0.0174(15) 0.0121(15) 0.0289(16) N202 0.033(2) 0.029(2) 0.028(2) 0.0156(18) -0.0073(17) 0.0008(18) C202 0.039(3) 0.046(3) 0.023(2) 0.021(2) 0.007(2) 0.024(2) N203 0.0248(19) 0.0211(18) 0.0168(18) 0.0104(15) 0.0021(14) 0.0116(15) C203 0.048(3) 0.038(3) 0.032(3) 0.026(2) 0.016(2) 0.027(2) N204 0.030(2) 0.0252(19) 0.0185(18) 0.0121(15) 0.0062(15) 0.0176(16) C204 0.039(3) 0.024(2) 0.029(3) 0.012(2) 0.004(2) 0.014(2) N205 0.0265(19) 0.0202(18) 0.0166(18) 0.0083(15) 0.0052(14) 0.0119(15) C205 0.027(2) 0.023(2) 0.016(2) 0.0080(18) 0.0068(17) 0.0141(19) N206 0.0228(18) 0.0187(18) 0.0232(19) 0.0121(15) 0.0052(15) 0.0108(15) C206 0.025(2) 0.019(2) 0.018(2) 0.0060(17) 0.0031(17) 0.0120(18) N207 0.0244(18) 0.0182(17) 0.0245(19) 0.0132(15) 0.0081(15) 0.0138(15) C207 0.024(2) 0.016(2) 0.023(2) 0.0096(18) 0.0042(17) 0.0081(18) N208 0.0238(18) 0.0167(17) 0.0258(19) 0.0134(15) 0.0071(15) 0.0113(15) C208 0.023(2) 0.017(2) 0.024(2) 0.0121(18) 0.0062(17) 0.0092(17) N209 0.021(2) 0.025(2) 0.052(3) 0.0243(19) 0.0091(18) 0.0085(16) C209 0.025(2) 0.022(2) 0.025(2) 0.0100(19) 0.0064(18) 0.0130(18) N210 0.0255(19) 0.0171(18) 0.026(2) 0.0089(15) 0.0025(15) 0.0107(15) C210 0.031(2) 0.028(2) 0.020(2) 0.0134(19) 0.0063(18) 0.017(2) C211 0.019(2) 0.021(2) 0.020(2) 0.0109(18) 0.0064(17) 0.0107(17) C212 0.021(2) 0.019(2) 0.021(2) 0.0106(18) 0.0050(17) 0.0082(17) C213 0.026(2) 0.025(2) 0.022(2) 0.0149(19) 0.0077(18) 0.0115(19) C214 0.028(2) 0.019(2) 0.018(2) 0.0071(17) 0.0002(17) 0.0101(18) C215 0.030(2) 0.025(2) 0.038(3) 0.019(2) 0.006(2) 0.010(2) C216 0.048(3) 0.019(2) 0.039(3) 0.017(2) 0.002(2) 0.006(2) C217 0.044(3) 0.021(2) 0.033(3) 0.013(2) 0.000(2) 0.018(2) C218 0.033(3) 0.024(2) 0.030(3) 0.011(2) 0.000(2) 0.015(2) O301 0.0312(18) 0.0276(18) 0.046(2) 0.0115(16) -0.0114(16) 0.0086(15) N301 0.0237(19) 0.0214(19) 0.0248(19) 0.0105(16) 0.0060(15) 0.0113(15) C301 0.034(3) 0.028(2) 0.035(3) 0.017(2) 0.009(2) 0.018(2) O302 0.0275(17) 0.0173(16) 0.041(2) 0.0089(14) -0.0053(14) 0.0082(13) N302 0.035(2) 0.039(2) 0.043(2) 0.028(2) 0.0184(19) 0.0263(19) C302 0.035(3) 0.033(3) 0.048(3) 0.024(2) 0.013(2) 0.023(2) N303 0.0234(19) 0.0207(18) 0.029(2) 0.0125(16) 0.0049(16) 0.0137(15) C303 0.043(3) 0.046(3) 0.063(4) 0.030(3) 0.031(3) 0.036(3) N304 0.0245(19) 0.0200(19) 0.026(2) 0.0079(16) -0.0004(15) 0.0114(15) C304 0.034(3) 0.042(3) 0.049(3) 0.029(3) 0.024(2) 0.025(2) C305 0.024(2) 0.023(2) 0.032(2) 0.015(2) 0.0060(19) 0.0118(19) N306 0.0182(18) 0.0152(17) 0.029(2) 0.0072(15) 0.0015(15) 0.0060(15) C306 0.019(2) 0.024(2) 0.033(3) 0.015(2) 0.0023(18) 0.0076(18) N307 0.0165(17) 0.0177(18) 0.028(2) 0.0102(15) 0.0044(15) 0.0083(14) C307 0.017(2) 0.021(2) 0.028(2) 0.0140(19) 0.0009(18) 0.0049(17) C308 0.019(2) 0.019(2) 0.025(2) 0.0121(18) 0.0074(17) 0.0085(17) N309 0.0180(18) 0.0168(17) 0.0254(19) 0.0099(15) 0.0037(15) 0.0067(14) C309 0.022(2) 0.020(2) 0.032(3) 0.008(2) -0.0046(19) 0.0013(18) N310 0.0179(17) 0.0161(17) 0.0255(19) 0.0091(15) 0.0036(15) 0.0092(14) C310 0.029(2) 0.015(2) 0.031(3) 0.0059(19) -0.001(2) 0.0091(19) N311 0.0218(19) 0.041(2) 0.027(2) 0.0165(18) 0.0060(16) 0.0153(18) C311 0.022(2) 0.014(2) 0.021(2) 0.0098(17) 0.0063(17) 0.0059(17) C312 0.021(2) 0.018(2) 0.020(2) 0.0089(17) 0.0074(17) 0.0116(17) N312 0.0223(18) 0.0186(18) 0.027(2) 0.0100(16) 0.0030(15) 0.0106(15) C313 0.019(2) 0.014(2) 0.021(2) 0.0037(17) 0.0013(17) 0.0082(17) C314 0.019(2) 0.016(2) 0.029(2) 0.0094(18) 0.0031(18) 0.0068(17) C315 0.022(2) 0.033(3) 0.024(2) 0.009(2) 0.0033(18) 0.011(2) C316 0.023(2) 0.038(3) 0.038(3) 0.011(2) 0.008(2) 0.017(2) C317 0.022(2) 0.040(3) 0.037(3) 0.019(2) 0.004(2) 0.017(2) C318 0.026(2) 0.029(2) 0.025(2) 0.010(2) 0.0010(19) 0.012(2) N1 0.0226(19) 0.027(2) 0.037(2) 0.0189(19) 0.0073(17) 0.0104(16) O1 0.098(3) 0.043(2) 0.038(2) 0.0187(19) 0.016(2) 0.049(2) O2 0.0335(19) 0.053(2) 0.037(2) 0.0264(18) -0.0047(16) 0.0109(17) O3 0.0337(18) 0.0259(17) 0.047(2) 0.0226(16) 0.0069(15) 0.0150(15) N2 0.031(2) 0.062(3) 0.043(3) 0.038(2) 0.019(2) 0.030(2) O4 0.056(3) 0.133(4) 0.104(4) 0.100(4) 0.045(3) 0.067(3) O5 0.043(2) 0.049(2) 0.051(2) 0.014(2) 0.0056(19) 0.0129(19) O6 0.0272(19) 0.042(2) 0.056(2) 0.0280(19) 0.0041(17) 0.0065(16) N3 0.067(3) 0.029(2) 0.032(2) 0.010(2) 0.024(2) 0.010(2) O2W 0.045(2) 0.046(2) 0.045(2) 0.0229(18) 0.0098(17) 0.0220(18) O3W 0.051(2) 0.046(2) 0.044(2) 0.0228(19) 0.0124(18) 0.0188(19) O4W 0.046(2) 0.044(2) 0.051(2) 0.0272(19) 0.0187(18) 0.0225(18) O5W 0.0360(19) 0.066(3) 0.041(2) 0.0308(19) 0.0186(16) 0.0304(19) O9W 0.092(4) 0.085(4) 0.077(4) 0.028(3) 0.006(3) 0.022(3) O10W 0.077(3) 0.085(4) 0.085(4) 0.047(3) 0.018(3) 0.040(3) O11W 0.072(3) 0.073(3) 0.080(3) 0.045(3) 0.024(3) 0.034(3) O12W 0.065(3) 0.078(3) 0.077(3) 0.032(3) 0.015(3) 0.030(3) O13W 0.059(3) 0.069(3) 0.076(3) 0.024(3) 0.010(2) 0.027(2) O14W 0.040(2) 0.070(3) 0.060(3) 0.028(2) 0.004(2) 0.019(2) O15W 0.046(2) 0.049(3) 0.086(3) 0.028(2) 0.017(2) 0.014(2) O16W 0.062(3) 0.036(2) 0.053(2) 0.0208(19) 0.001(2) 0.0084(19) O17W 0.048(2) 0.072(3) 0.049(2) 0.027(2) 0.0164(19) 0.024(2) O20W 0.061(3) 0.089(4) 0.106(5) 0.013(3) 0.008(3) 0.028(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 N208 2.061(3) . ? Ni1 N310 2.074(4) . ? Ni1 N110 2.075(4) . ? Ni1 N210 2.092(3) . ? Ni1 N108 2.099(3) . ? Ni1 N312 2.101(4) . ? Ni2 N207 2.054(3) . ? Ni2 N206 2.057(3) . ? Ni2 N106 2.062(3) . ? Ni2 N309 2.067(3) . ? Ni2 N107 2.078(3) . ? Ni2 N307 2.083(3) . ? Ni3 N303 2.049(4) . ? Ni3 N203 2.058(3) . ? Ni3 N201 2.087(4) . ? Ni3 N103 2.089(4) . ? Ni3 N101 2.090(4) . ? Ni3 N301 2.100(4) . ? Ni3 Na1 3.441(10) . ? O101 C107 1.218(5) . ? N101 C101 1.342(6) . ? N101 C105 1.353(6) . ? C101 C102 1.367(7) . ? O102 C112 1.262(5) . ? N102 C106 1.327(6) . ? C102 C103 1.381(8) . ? N103 C106 1.302(6) . ? N103 N104 1.407(5) . ? N103 Na1 2.863(10) . ? C103 C104 1.387(7) . ? N104 C107 1.331(5) . ? N104 Na1 2.151(10) . ? C104 C105 1.389(7) . ? N105 N106 1.322(5) . ? N105 C108 1.335(5) . ? N105 Na1 2.351(10) . ? C105 C106 1.484(6) . ? N106 C111 1.336(5) . ? N107 C112 1.314(5) . ? N107 N108 1.415(5) . ? C107 C108 1.512(6) . ? C107 Na1 2.873(10) . ? N108 C113 1.300(5) . ? C108 C109 1.383(6) . ? C108 Na1 2.988(10) . ? N109 C113 1.344(5) . ? C109 C110 1.378(6) . ? N110 C118 1.337(6) . ? N110 C114 1.353(5) . ? C110 C111 1.396(6) . ? C111 C112 1.510(6) . ? C113 C114 1.494(6) . ? C114 C115 1.383(6) . ? C115 C116 1.389(6) . ? C116 C117 1.378(7) . ? C117 C118 1.380(7) . ? O201 C207 1.225(5) . ? N201 C201 1.343(6) . ? N201 C205 1.348(6) . ? C201 C202 1.388(7) . ? O202 C212 1.259(5) . ? N202 C206 1.318(6) . ? C202 C203 1.375(7) . ? N203 C206 1.308(5) . ? N203 N204 1.415(5) . ? N203 Na1 2.961(10) . ? C203 C204 1.389(7) . ? N204 C207 1.336(5) . ? N204 Na1 2.221(10) . ? C204 C205 1.390(6) . ? N205 N206 1.317(5) . ? N205 C208 1.332(5) . ? N205 Na1 2.355(10) . ? C205 C206 1.493(6) . ? N206 C211 1.339(5) . ? N207 C212 1.315(5) . ? N207 N208 1.411(5) . ? C207 C208 1.502(6) . ? C207 Na1 3.036(11) . ? N208 C213 1.295(5) . ? C208 C209 1.382(6) . ? C208 Na1 3.106(11) . ? N209 C213 1.335(6) . ? C209 C210 1.373(6) . ? N210 C218 1.344(6) . ? N210 C214 1.353(6) . ? C210 C211 1.382(6) . ? C211 C212 1.504(6) . ? C213 C214 1.489(6) . ? C214 C215 1.383(6) . ? C215 C216 1.382(7) . ? C216 C217 1.382(7) . ? C217 C218 1.373(6) . ? O301 C307 1.231(5) . ? N301 C301 1.335(6) . ? N301 C305 1.353(6) . ? C301 C302 1.384(7) . ? O302 C312 1.255(5) . ? N302 C306 1.317(6) . ? C302 C303 1.363(7) . ? N303 C306 1.309(6) . ? N303 N304 1.399(5) . ? N303 Na1 2.899(10) . ? C303 C304 1.385(7) . ? N304 C307 1.330(6) . ? N304 Na1 2.179(10) . ? C304 C305 1.388(6) . ? C305 C306 1.497(6) . ? N306 N307 1.320(5) . ? N306 C308 1.331(5) . ? N306 Na1 2.223(10) . ? N307 C311 1.334(5) . ? C307 C308 1.503(6) . ? C307 Na1 2.805(10) . ? C308 C309 1.391(6) . ? C308 Na1 2.883(10) . ? N309 C312 1.319(5) . ? N309 N310 1.412(5) . ? C309 C310 1.371(6) . ? N310 C313 1.295(5) . ? C310 C311 1.389(6) . ? N311 C313 1.346(6) . ? C311 C312 1.513(6) . ? N312 C318 1.334(6) . ? N312 C314 1.348(6) . ? C313 C314 1.486(6) . ? C314 C315 1.391(6) . ? C315 C316 1.378(6) . ? C316 C317 1.384(7) . ? C317 C318 1.382(6) . ? N1 O3 1.243(5) . ? N1 O2 1.247(5) . ? N1 O1 1.249(5) . ? N2 O4 1.226(5) . ? N2 O5 1.244(6) . ? N2 O6 1.274(6) . ? N3 O9 1.217(4) . ? N3 O8A 1.223(5) . ? N3 O8 1.242(4) . ? N3 O9A 1.249(5) . ? N3 O7A 1.264(5) . ? N3 O7 1.270(4) . ? O7 O8A 1.172(16) . ? O7 O9A 1.616(14) . ? O8 O7A 1.132(14) . ? O8 O8A 1.367(14) . ? O9 O9A 0.811(15) . ? O9 O7A 1.510(13) . ? O6W O6WA 0.72(2) . ? O7W O7WA 1.63(2) . ? O8W O8WA 0.855(19) . ? O18W O19W 1.788(16) . ? 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 N208 Ni1 N310 92.36(14) . . ? N208 Ni1 N110 94.35(14) . . ? N310 Ni1 N110 166.84(13) . . ? N208 Ni1 N210 77.48(13) . . ? N310 Ni1 N210 96.17(14) . . ? N110 Ni1 N210 96.33(14) . . ? N208 Ni1 N108 89.81(13) . . ? N310 Ni1 N108 90.57(13) . . ? N110 Ni1 N108 78.16(13) . . ? N210 Ni1 N108 165.81(14) . . ? N208 Ni1 N312 169.19(14) . . ? N310 Ni1 N312 77.28(13) . . ? N110 Ni1 N312 96.42(14) . . ? N210 Ni1 N312 100.32(13) . . ? N108 Ni1 N312 93.33(13) . . ? N207 Ni2 N206 76.50(13) . . ? N207 Ni2 N106 159.71(14) . . ? N206 Ni2 N106 91.12(14) . . ? N207 Ni2 N309 93.58(13) . . ? N206 Ni2 N309 164.48(13) . . ? N106 Ni2 N309 101.53(14) . . ? N207 Ni2 N107 89.54(13) . . ? N206 Ni2 N107 99.15(14) . . ? N106 Ni2 N107 76.44(13) . . ? N309 Ni2 N107 92.59(13) . . ? N207 Ni2 N307 101.96(14) . . ? N206 Ni2 N307 94.36(14) . . ? N106 Ni2 N307 94.88(14) . . ? N309 Ni2 N307 75.81(13) . . ? N107 Ni2 N307 164.01(14) . . ? N303 Ni3 N203 93.89(14) . . ? N303 Ni3 N201 165.54(14) . . ? N203 Ni3 N201 77.48(13) . . ? N303 Ni3 N103 95.09(14) . . ? N203 Ni3 N103 92.19(14) . . ? N201 Ni3 N103 96.80(14) . . ? N303 Ni3 N101 93.54(15) . . ? N203 Ni3 N101 167.37(14) . . ? N201 Ni3 N101 97.13(14) . . ? N103 Ni3 N101 76.99(14) . . ? N303 Ni3 N301 77.41(13) . . ? N203 Ni3 N301 97.53(14) . . ? N201 Ni3 N301 92.08(13) . . ? N103 Ni3 N301 168.06(14) . . ? N101 Ni3 N301 94.04(14) . . ? N303 Ni3 Na1 57.23(19) . . ? N203 Ni3 Na1 58.94(19) . . ? N201 Ni3 Na1 124.46(19) . . ? N103 Ni3 Na1 56.16(19) . . ? N101 Ni3 Na1 117.75(19) . . ? N301 Ni3 Na1 124.02(19) . . ? C101 N101 C105 118.6(4) . . ? C101 N101 Ni3 126.2(3) . . ? C105 N101 Ni3 115.3(3) . . ? N101 C101 C102 123.0(5) . . ? C101 C102 C103 118.5(5) . . ? C106 N103 N104 114.3(3) . . ? C106 N103 Ni3 117.3(3) . . ? N104 N103 Ni3 124.7(3) . . ? C106 N103 Na1 125.5(3) . . ? N104 N103 Na1 46.5(3) . . ? Ni3 N103 Na1 86.5(2) . . ? C102 C103 C104 119.9(5) . . ? C107 N104 N103 123.6(4) . . ? C107 N104 Na1 108.9(4) . . ? N103 N104 Na1 105.2(4) . . ? C103 C104 C105 118.3(5) . . ? N106 N105 C108 120.2(3) . . ? N106 N105 Na1 122.3(3) . . ? C108 N105 Na1 104.9(4) . . ? N101 C105 C104 121.7(4) . . ? N101 C105 C106 115.0(4) . . ? C104 C105 C106 123.3(4) . . ? N105 N106 C111 120.1(3) . . ? N105 N106 Ni2 122.0(3) . . ? C111 N106 Ni2 116.7(3) . . ? N103 C106 N102 125.4(4) . . ? N103 C106 C105 114.3(4) . . ? N102 C106 C105 120.3(4) . . ? C112 N107 N108 118.8(3) . . ? C112 N107 Ni2 119.5(3) . . ? N108 N107 Ni2 119.1(2) . . ? O101 C107 N104 125.6(4) . . ? O101 C107 C108 121.7(4) . . ? N104 C107 C108 112.6(4) . . ? O101 C107 Na1 142.0(4) . . ? N104 C107 Na1 45.1(3) . . ? C108 C107 Na1 79.3(3) . . ? C113 N108 N107 116.9(3) . . ? C113 N108 Ni1 113.9(3) . . ? N107 N108 Ni1 119.6(2) . . ? N105 C108 C109 122.3(4) . . ? N105 C108 C107 114.0(3) . . ? C109 C108 C107 123.7(4) . . ? N105 C108 Na1 49.5(3) . . ? C109 C108 Na1 152.6(4) . . ? C107 C108 Na1 70.9(3) . . ? C110 C109 C108 117.7(4) . . ? C118 N110 C114 118.4(4) . . ? C118 N110 Ni1 127.4(3) . . ? C114 N110 Ni1 114.2(3) . . ? C109 C110 C111 117.5(4) . . ? N106 C111 C110 121.8(4) . . ? N106 C111 C112 115.4(3) . . ? C110 C111 C112 122.8(4) . . ? O102 C112 N107 130.1(4) . . ? O102 C112 C111 119.0(3) . . ? N107 C112 C111 110.9(3) . . ? N108 C113 N109 125.5(4) . . ? N108 C113 C114 114.8(4) . . ? N109 C113 C114 119.6(4) . . ? N110 C114 C115 121.7(4) . . ? N110 C114 C113 114.9(4) . . ? C115 C114 C113 123.4(4) . . ? C114 C115 C116 119.3(4) . . ? C117 C116 C115 118.9(4) . . ? C116 C117 C118 118.8(4) . . ? N110 C118 C117 122.9(4) . . ? C201 N201 C205 118.5(4) . . ? C201 N201 Ni3 125.9(3) . . ? C205 N201 Ni3 114.8(3) . . ? N201 C201 C202 122.4(4) . . ? C203 C202 C201 118.7(4) . . ? C206 N203 N204 114.5(3) . . ? C206 N203 Ni3 118.2(3) . . ? N204 N203 Ni3 125.2(3) . . ? C206 N203 Na1 136.2(3) . . ? N204 N203 Na1 45.9(3) . . ? Ni3 N203 Na1 84.5(2) . . ? C202 C203 C204 119.7(4) . . ? C207 N204 N203 123.6(3) . . ? C207 N204 Na1 114.9(4) . . ? N203 N204 Na1 106.9(3) . . ? C203 C204 C205 118.3(4) . . ? N206 N205 C208 120.1(4) . . ? N206 N205 Na1 119.4(3) . . ? C208 N205 Na1 111.8(4) . . ? N201 C205 C204 122.3(4) . . ? N201 C205 C206 114.8(4) . . ? C204 C205 C206 122.9(4) . . ? N205 N206 C211 120.2(3) . . ? N205 N206 Ni2 123.2(3) . . ? C211 N206 Ni2 116.5(3) . . ? N203 C206 N202 126.5(4) . . ? N203 C206 C205 113.5(4) . . ? N202 C206 C205 120.1(4) . . ? C212 N207 N208 118.7(3) . . ? C212 N207 Ni2 118.7(3) . . ? N208 N207 Ni2 118.8(2) . . ? O201 C207 N204 125.5(4) . . ? O201 C207 C208 121.8(4) . . ? N204 C207 C208 112.8(4) . . ? O201 C207 Na1 150.4(4) . . ? N204 C207 Na1 41.6(3) . . ? C208 C207 Na1 78.4(3) . . ? C213 N208 N207 115.9(3) . . ? C213 N208 Ni1 116.4(3) . . ? N207 N208 Ni1 119.8(2) . . ? N205 C208 C209 122.2(4) . . ? N205 C208 C207 114.0(4) . . ? C209 C208 C207 123.7(4) . . ? N205 C208 Na1 44.8(3) . . ? C209 C208 Na1 154.6(3) . . ? C207 C208 Na1 73.3(3) . . ? C210 C209 C208 117.1(4) . . ? C218 N210 C214 117.9(4) . . ? C218 N210 Ni1 127.9(3) . . ? C214 N210 Ni1 114.2(3) . . ? C209 C210 C211 118.4(4) . . ? N206 C211 C210 121.2(4) . . ? N206 C211 C212 114.4(3) . . ? C210 C211 C212 124.4(4) . . ? O202 C212 N207 128.5(4) . . ? O202 C212 C211 119.8(4) . . ? N207 C212 C211 111.7(4) . . ? N208 C213 N209 124.9(4) . . ? N208 C213 C214 114.1(4) . . ? N209 C213 C214 120.9(4) . . ? N210 C214 C215 121.9(4) . . ? N210 C214 C213 114.4(4) . . ? C215 C214 C213 123.6(4) . . ? C216 C215 C214 119.4(4) . . ? C215 C216 C217 118.7(4) . . ? C218 C217 C216 119.0(4) . . ? N210 C218 C217 123.0(4) . . ? C301 N301 C305 117.7(4) . . ? C301 N301 Ni3 127.5(3) . . ? C305 N301 Ni3 114.7(3) . . ? N301 C301 C302 123.4(4) . . ? C303 C302 C301 118.4(4) . . ? C306 N303 N304 114.8(4) . . ? C306 N303 Ni3 119.0(3) . . ? N304 N303 Ni3 125.2(3) . . ? C306 N303 Na1 135.3(3) . . ? N304 N303 Na1 46.2(3) . . ? Ni3 N303 Na1 86.3(2) . . ? C302 C303 C304 119.8(5) . . ? C307 N304 N303 124.1(4) . . ? C307 N304 Na1 103.5(4) . . ? N303 N304 Na1 106.2(4) . . ? C303 C304 C305 118.6(4) . . ? N301 C305 C304 122.1(4) . . ? N301 C305 C306 115.0(4) . . ? C304 C305 C306 122.9(4) . . ? N307 N306 C308 120.5(4) . . ? N307 N306 Na1 123.9(4) . . ? C308 N306 Na1 105.7(4) . . ? N303 C306 N302 126.0(4) . . ? N303 C306 C305 113.6(4) . . ? N302 C306 C305 120.4(4) . . ? N306 N307 C311 120.1(4) . . ? N306 N307 Ni2 122.9(3) . . ? C311 N307 Ni2 116.4(3) . . ? O301 C307 N304 125.2(4) . . ? O301 C307 C308 121.5(4) . . ? N304 C307 C308 113.1(4) . . ? O301 C307 Na1 139.6(4) . . ? N304 C307 Na1 49.1(3) . . ? C308 C307 Na1 77.6(3) . . ? N306 C308 C309 122.0(4) . . ? N306 C308 C307 114.3(4) . . ? C309 C308 C307 123.6(4) . . ? N306 C308 Na1 47.9(3) . . ? C309 C308 Na1 152.8(4) . . ? C307 C308 Na1 71.8(3) . . ? C312 N309 N310 116.3(3) . . ? C312 N309 Ni2 118.4(3) . . ? N310 N309 Ni2 118.3(2) . . ? C310 C309 C308 117.4(4) . . ? C313 N310 N309 114.2(3) . . ? C313 N310 Ni1 113.2(3) . . ? N309 N310 Ni1 120.0(2) . . ? C309 C310 C311 118.1(4) . . ? N307 C311 C310 121.8(4) . . ? N307 C311 C312 114.5(4) . . ? C310 C311 C312 123.7(4) . . ? O302 C312 N309 129.6(4) . . ? O302 C312 C311 120.3(4) . . ? N309 C312 C311 110.1(3) . . ? C318 N312 C314 117.8(4) . . ? C318 N312 Ni1 128.7(3) . . ? C314 N312 Ni1 113.5(3) . . ? N310 C313 N311 125.1(4) . . ? N310 C313 C314 114.8(4) . . ? N311 C313 C314 120.1(4) . . ? N312 C314 C315 122.2(4) . . ? N312 C314 C313 114.0(4) . . ? C315 C314 C313 123.8(4) . . ? C316 C315 C314 118.8(4) . . ? C315 C316 C317 119.5(4) . . ? C318 C317 C316 118.0(4) . . ? N312 C318 C317 123.7(4) . . ? O3 N1 O2 120.9(4) . . ? O3 N1 O1 119.2(4) . . ? O2 N1 O1 119.9(4) . . ? O4 N2 O5 121.3(5) . . ? O4 N2 O6 120.0(5) . . ? O5 N2 O6 118.7(4) . . ? O9 N3 O8A 149.7(10) . . ? O9 N3 O8 128.0(4) . . ? O8A N3 O8 67.4(8) . . ? O9 N3 O9A 38.3(7) . . ? O8A N3 O9A 124.4(8) . . ? O8 N3 O9A 166.4(8) . . ? O9 N3 O7A 74.9(7) . . ? O8A N3 O7A 118.0(8) . . ? O8 N3 O7A 53.7(7) . . ? O9A N3 O7A 112.8(7) . . ? O9 N3 O7 118.2(4) . . ? O8A N3 O7 56.1(8) . . ? O8 N3 O7 113.8(4) . . ? O9A N3 O7 79.8(8) . . ? O7A N3 O7 163.7(9) . . ? O8A O7 N3 60.0(4) . . ? O8A O7 O9A 102.2(8) . . ? N3 O7 O9A 49.5(4) . . ? O7A O8 N3 64.2(5) . . ? O7A O8 O8A 116.8(7) . . ? N3 O8 O8A 55.7(4) . . ? O9A O9 N3 72.9(6) . . ? O9A O9 O7A 126.1(8) . . ? N3 O9 O7A 53.9(4) . . ? O8 O7A N3 62.1(4) . . ? O8 O7A O9 112.8(5) . . ? N3 O7A O9 51.1(4) . . ? O7 O8A N3 64.0(5) . . ? O7 O8A O8 111.6(9) . . ? N3 O8A O8 57.0(4) . . ? O9 O9A N3 68.7(5) . . ? O9 O9A O7 119.4(6) . . ? N3 O9A O7 50.6(5) . . ? N104 Na1 N304 103.4(4) . . ? N104 Na1 N204 95.7(4) . . ? N304 Na1 N204 100.4(4) . . ? N104 Na1 N306 113.7(4) . . ? N304 Na1 N306 71.9(3) . . ? N204 Na1 N306 150.6(5) . . ? N104 Na1 N105 69.5(3) . . ? N304 Na1 N105 152.9(5) . . ? N204 Na1 N105 106.2(4) . . ? N306 Na1 N105 86.8(4) . . ? N104 Na1 N205 141.2(5) . . ? N304 Na1 N205 113.9(4) . . ? N204 Na1 N205 68.1(3) . . ? N306 Na1 N205 88.7(4) . . ? N105 Na1 N205 81.2(3) . . ? N104 Na1 C307 90.3(4) . . ? N304 Na1 C307 27.47(18) . . ? N204 Na1 C307 126.3(4) . . ? N306 Na1 C307 55.1(2) . . ? N105 Na1 C307 125.6(4) . . ? N205 Na1 C307 128.1(4) . . ? N104 Na1 N103 28.32(17) . . ? N304 Na1 N103 77.9(3) . . ? N204 Na1 N103 88.4(3) . . ? N306 Na1 N103 116.4(4) . . ? N105 Na1 N103 97.8(3) . . ? N205 Na1 N103 154.9(4) . . ? C307 Na1 N103 72.8(3) . . ? N104 Na1 C107 26.00(17) . . ? N304 Na1 C107 127.6(4) . . ? N204 Na1 C107 82.1(3) . . ? N306 Na1 C107 125.6(4) . . ? N105 Na1 C107 53.3(2) . . ? N205 Na1 C107 115.2(4) . . ? C307 Na1 C107 116.2(4) . . ? N103 Na1 C107 49.8(2) . . ? N104 Na1 C308 97.4(4) . . ? N304 Na1 C308 53.6(2) . . ? N204 Na1 C308 153.0(4) . . ? N306 Na1 C308 26.38(17) . . ? N105 Na1 C308 100.5(4) . . ? N205 Na1 C308 112.9(4) . . ? C307 Na1 C308 30.60(15) . . ? N103 Na1 C308 92.1(3) . . ? C107 Na1 C308 118.2(4) . . ? N104 Na1 N303 92.3(4) . . ? N304 Na1 N303 27.61(17) . . ? N204 Na1 N303 76.4(3) . . ? N306 Na1 N303 99.5(4) . . ? N105 Na1 N303 161.7(4) . . ? N205 Na1 N303 115.9(4) . . ? C307 Na1 N303 50.0(2) . . ? N103 Na1 N303 64.0(2) . . ? C107 Na1 N303 110.3(3) . . ? C308 Na1 N303 79.6(3) . . ? N104 Na1 N203 74.3(3) . . ? N304 Na1 N203 89.1(3) . . ? N204 Na1 N203 27.20(16) . . ? N306 Na1 N203 160.5(4) . . ? N105 Na1 N203 112.7(4) . . ? N205 Na1 N203 95.3(3) . . ? C307 Na1 N203 108.9(3) . . ? N103 Na1 N203 61.7(2) . . ? C107 Na1 N203 69.6(2) . . ? C308 Na1 N203 139.4(4) . . ? N303 Na1 N203 61.6(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.267 _refine_diff_density_min -0.980 _refine_diff_density_rms 0.095 #=== data_Compound10 _database_code_depnum_ccdc_archive 'CCDC 723423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[(C18 H14 O2 N10)8 Cu12 Na1.525] (N O3)9.525 (H2 O)8.9' _chemical_formula_sum 'C144 H129.80 Cu12 N89.525 Na1.525 O53.475' _chemical_formula_weight 4767.57 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' 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 20.114(3) _cell_length_b 21.693(3) _cell_length_c 24.540(3) _cell_angle_alpha 95.631(2) _cell_angle_beta 101.818(2) _cell_angle_gamma 101.020(3) _cell_volume 10182(2) _cell_formula_units_Z 2 _cell_measurement_temperature 138(2) _cell_measurement_reflns_used 33130 _cell_measurement_theta_min 2.5401 _cell_measurement_theta_max 30.6692 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4826.14 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9271 _exptl_absorpt_correction_T_min 0.7913 _exptl_absorpt_process_details '(T. Higashi, 2000)' _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 100095 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0876 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.50 _reflns_number_total 41995 _reflns_number_gt 25860 _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)' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 395.6 electrons per unit cell in four voids (total volume 2279 ^A^3); that is 197.8 electrons per formula unit. The electron density was assigned as 3.525 nitrate ions (109.275 electrons) and 8.9 lattice water molecules (88.525 electrons). The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the framework structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 1 0.000 0.000 0.500 35.8 24.2 2 0.132 0.388 0.611 2229.6 357.2 3 0.448 0.870 0.383 6.8 8.2 4 0.552 0.130 0.617 6.8 6.0 _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^)+(0.1437P)^2^+1.7323P] 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 41995 _refine_ls_number_parameters 2462 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.2750 _refine_ls_wR_factor_gt 0.2460 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _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 Cu1 Cu 0.62844(5) 0.42512(4) 0.11879(3) 0.0548(2) Uani 1 1 d . . . Cu2 Cu 0.70897(4) 0.30956(4) 0.02093(3) 0.0508(2) Uani 1 1 d . . . Cu3 Cu 0.84348(4) 0.26300(4) -0.05239(3) 0.0496(2) Uani 1 1 d . . . Cu4 Cu 1.02235(4) 0.28009(4) -0.07501(3) 0.0583(2) Uani 1 1 d . . . Cu5 Cu 1.10181(4) 0.27199(4) 0.07793(3) 0.04738(19) Uani 1 1 d . . . Cu6 Cu 1.12877(4) 0.18667(3) 0.20628(3) 0.04479(18) Uani 1 1 d . . . Cu7 Cu 1.11887(4) 0.04291(4) 0.29297(3) 0.04735(19) Uani 1 1 d . . . Cu8 Cu 0.92177(4) 0.01832(4) 0.30326(3) 0.04681(19) Uani 1 1 d . . . Cu9 Cu 0.77673(4) 0.05660(3) 0.36991(3) 0.04547(18) Uani 1 1 d . . . Cu10 Cu 0.68837(5) 0.15562(4) 0.47448(3) 0.0554(2) Uani 1 1 d . . . Cu11 Cu 0.73589(4) 0.29971(4) 0.40151(4) 0.0614(2) Uani 1 1 d . . . Cu12 Cu 0.71268(4) 0.39270(4) 0.27792(4) 0.0615(2) Uani 1 1 d . . . Na1 Na 0.7964(5) 0.2804(5) 0.1750(4) 0.057(2) Uani 0.25 1 d P . . Na2 Na 0.9170(10) 0.2463(10) 0.1114(8) 0.056(5) Uani 0.13 1 d P . . Na3 Na 0.8102(3) 0.2057(2) 0.2826(2) 0.0547(12) Uani 0.50 1 d P . . Na4 Na 0.93731(18) 0.17809(16) 0.22421(13) 0.0441(8) Uani 0.65 1 d P . . O1 O 0.7012(2) 0.3931(2) 0.07529(18) 0.0531(11) Uani 1 1 d . . . O2 O 0.9358(2) 0.3127(2) -0.05112(18) 0.0517(10) Uani 1 1 d . . . O3 O 0.7840(3) 0.3596(2) 0.2473(2) 0.0788(16) Uani 1 1 d . . . O4 O 1.0217(2) 0.2981(2) 0.10142(18) 0.0515(10) Uani 1 1 d . . . O5 O 0.8061(2) 0.2675(2) 0.3688(2) 0.0657(13) Uani 1 1 d . . . O6 O 1.0507(2) 0.2118(2) 0.23268(18) 0.0522(10) Uani 1 1 d . . . O7 O 0.7662(2) 0.1213(2) 0.44162(17) 0.0489(10) Uani 1 1 d . . . O8 O 1.0209(2) 0.0518(2) 0.33254(16) 0.0480(10) Uani 1 1 d . . . O9 O 0.6434(2) 0.3796(2) 0.19624(18) 0.0573(11) Uani 1 1 d . . . O10 O 0.6765(2) 0.2188(2) 0.40845(18) 0.0512(10) Uani 1 1 d . . . O11 O 0.7317(2) 0.2647(2) 0.08634(18) 0.0554(11) Uani 1 1 d . . . O12 O 0.7681(2) 0.1077(2) 0.30907(16) 0.0485(10) Uani 1 1 d . . . O13 O 0.8681(2) 0.2252(2) 0.01607(18) 0.0570(11) Uani 1 1 d . . . O14 O 0.9150(2) 0.0738(2) 0.24418(16) 0.0520(10) Uani 1 1 d . . . O15 O 1.0536(2) 0.2348(2) 0.00235(15) 0.0470(10) Uani 1 1 d . . . O16 O 1.1020(2) 0.08972(19) 0.22590(16) 0.0478(10) Uani 1 1 d . . . O17 O 1.4386(4) 0.3346(4) 0.3635(4) 0.143(3) Uani 1 1 d . . . O18 O 1.4779(5) 0.2718(5) 0.4144(5) 0.163(4) Uani 1 1 d . . . O19 O 1.5063(4) 0.2847(6) 0.3352(5) 0.207(6) Uani 1 1 d . . . O20 O 1.2620(5) 0.4880(6) 0.1320(5) 0.174(4) Uani 1 1 d . . . O21 O 1.3660(4) 0.4710(4) 0.1510(3) 0.118(2) Uani 1 1 d . . . O22 O 1.3081(4) 0.4549(4) 0.0644(3) 0.121(3) Uani 1 1 d . . . O23 O 0.7579(5) 0.1039(5) -0.3114(3) 0.162(4) Uani 1 1 d . . . O24 O 0.6542(4) 0.0898(5) -0.3046(3) 0.138(3) Uani 1 1 d . . . O25 O 0.7366(3) 0.0983(3) -0.2305(3) 0.0976(19) Uani 1 1 d . . . O26 O 0.8570(4) -0.0560(4) -0.0477(4) 0.132(3) Uiso 1 1 d D . . O27 O 0.8239(7) -0.0297(7) 0.0243(6) 0.231(5) Uiso 1 1 d D . . O28 O 0.8757(5) -0.1044(5) 0.0272(4) 0.164(3) Uiso 1 1 d D . . O29 O 0.4662(6) -0.2082(5) 0.2787(5) 0.184(4) Uiso 1 1 d D . . O30 O 0.5457(6) -0.2087(6) 0.3416(5) 0.191(4) Uiso 1 1 d D . . O31 O 0.4914(5) -0.2990(5) 0.2971(4) 0.161(3) Uiso 1 1 d D . . O32 O 0.8014(6) -0.2915(5) 0.2664(5) 0.179(4) Uiso 1 1 d D . . O33 O 0.9148(7) -0.2532(6) 0.2633(5) 0.188(4) Uiso 1 1 d D . . O34 O 0.8496(8) -0.2038(7) 0.2394(6) 0.241(6) Uiso 1 1 d D . . N1 N 0.5950(3) 0.4937(3) 0.1728(2) 0.0560(14) Uani 1 1 d . . . N2 N 0.7736(4) 0.5842(3) 0.2017(3) 0.087(2) Uani 1 1 d . . . H1 H 0.8116 0.5817 0.1898 0.105 Uiso 1 1 calc R . . H2 H 0.7745 0.6151 0.2281 0.105 Uiso 1 1 calc R . . N3 N 0.7085(3) 0.4927(3) 0.1395(2) 0.0586(14) Uani 1 1 d . . . N4 N 0.7694(3) 0.4888(3) 0.1216(2) 0.0628(15) Uani 1 1 d . . . N5 N 0.8024(3) 0.3700(2) 0.0293(2) 0.0498(12) Uani 1 1 d . . . N6 N 0.8495(3) 0.3541(2) 0.0021(2) 0.0468(12) Uani 1 1 d . . . N7 N 1.0235(3) 0.4000(3) -0.0086(2) 0.0602(14) Uani 1 1 d . . . N8 N 1.0619(3) 0.3662(3) -0.0381(2) 0.0595(14) Uani 1 1 d . . . N9 N 1.1627(3) 0.4374(3) 0.0123(3) 0.0681(16) Uani 1 1 d . . . H3 H 1.1395 0.4589 0.0309 0.082 Uiso 1 1 calc R . . H4 H 1.2083 0.4491 0.0187 0.082 Uiso 1 1 calc R . . N10 N 1.1281(3) 0.2933(3) -0.0842(2) 0.0548(13) Uani 1 1 d . . . N11 N 0.6739(3) 0.4493(3) 0.3275(2) 0.0594(14) Uani 1 1 d . . . N12 N 0.8272(5) 0.5661(4) 0.3462(4) 0.136(4) Uani 1 1 d . . . H5 H 0.8668 0.5705 0.3356 0.163 Uiso 1 1 calc R . . H6 H 0.8184 0.5979 0.3667 0.163 Uiso 1 1 calc R . . N13 N 0.7870(4) 0.4603(3) 0.3013(3) 0.082(2) Uani 1 1 d . . . N14 N 0.8464(4) 0.4580(4) 0.2777(4) 0.105(3) Uani 1 1 d . . . N15 N 0.8671(4) 0.3441(3) 0.1729(3) 0.088(2) Uani 1 1 d . . . N16 N 0.9174(4) 0.3276(4) 0.1470(3) 0.090(2) Uani 1 1 d . . . N17 N 1.1056(3) 0.3501(3) 0.1777(2) 0.0610(14) Uani 1 1 d . . . N18 N 1.1472(3) 0.3260(3) 0.1460(2) 0.0587(14) Uani 1 1 d . . . N19 N 1.2530(4) 0.3732(3) 0.2116(3) 0.0724(17) Uani 1 1 d . . . H7 H 1.2321 0.3892 0.2361 0.087 Uiso 1 1 calc R . . H8 H 1.2986 0.3795 0.2192 0.087 Uiso 1 1 calc R . . N20 N 1.2027(3) 0.2757(3) 0.0751(2) 0.0522(13) Uani 1 1 d . . . N21 N 0.6943(3) 0.3573(3) 0.4490(2) 0.0630(15) Uani 1 1 d . . . N22 N 0.8500(5) 0.4748(5) 0.4631(5) 0.165(5) Uani 1 1 d . . . H9 H 0.8859 0.4786 0.4474 0.197 Uiso 1 1 calc R . . H10 H 0.8441 0.5075 0.4843 0.197 Uiso 1 1 calc R . . N23 N 0.8087(3) 0.3677(3) 0.4239(3) 0.082(2) Uani 1 1 d . . . N24 N 0.8710(4) 0.3653(4) 0.4057(4) 0.104(3) Uani 1 1 d . . . N25 N 0.9060(3) 0.2385(4) 0.3198(3) 0.095(2) Uani 1 1 d . . . N26 N 0.9577(3) 0.2243(4) 0.2963(3) 0.091(2) Uani 1 1 d . . . N27 N 1.1416(2) 0.2704(2) 0.3059(2) 0.0474(11) Uani 1 1 d . . . N28 N 1.1785(2) 0.2436(2) 0.2709(2) 0.0467(11) Uani 1 1 d . . . N29 N 1.2872(3) 0.2972(3) 0.3281(2) 0.0550(13) Uani 1 1 d . . . H11 H 1.2686 0.3150 0.3533 0.066 Uiso 1 1 calc R . . H12 H 1.3327 0.3047 0.3328 0.066 Uiso 1 1 calc R . . N30 N 1.2256(3) 0.1888(2) 0.1972(2) 0.0463(12) Uani 1 1 d . . . N31 N 0.6488(4) 0.2138(3) 0.5300(3) 0.0650(16) Uani 1 1 d . . . N32 N 0.8271(4) 0.2993(3) 0.5833(3) 0.0767(18) Uani 1 1 d . . . H13 H 0.8678 0.2965 0.5766 0.092 Uiso 1 1 calc R . . H14 H 0.8239 0.3308 0.6074 0.092 Uiso 1 1 calc R . . N33 N 0.7720(3) 0.2080(2) 0.5203(2) 0.0528(13) Uani 1 1 d . . . N34 N 0.8364(3) 0.2073(2) 0.5062(2) 0.0501(12) Uani 1 1 d . . . N35 N 0.8752(3) 0.1031(2) 0.40259(19) 0.0437(11) Uani 1 1 d . . . N36 N 0.9257(3) 0.0892(2) 0.37900(19) 0.0423(11) Uani 1 1 d . . . N37 N 1.1048(3) 0.1368(3) 0.3858(2) 0.0493(12) Uani 1 1 d . . . N38 N 1.1494(3) 0.1127(2) 0.3560(2) 0.0466(12) Uani 1 1 d . . . N39 N 1.2353(3) 0.1936(3) 0.4176(2) 0.0591(14) Uani 1 1 d . . . H15 H 1.2043 0.2044 0.4350 0.071 Uiso 1 1 calc R . . H16 H 1.2791 0.2140 0.4283 0.071 Uiso 1 1 calc R . . N40 N 1.2393(3) 0.0752(3) 0.3038(2) 0.0521(13) Uani 1 1 d . . . N41 N 0.5687(3) 0.4306(3) 0.0323(2) 0.0586(14) Uani 1 1 d . . . N42 N 0.4808(3) 0.2700(3) 0.0319(3) 0.0666(16) Uani 1 1 d . . . H17 H 0.4808 0.2417 0.0553 0.080 Uiso 1 1 calc R . . H18 H 0.4556 0.2596 -0.0028 0.080 Uiso 1 1 calc R . . N43 N 0.5585(3) 0.3484(3) 0.1002(2) 0.0566(14) Uani 1 1 d . . . N44 N 0.5550(3) 0.3026(3) 0.1368(2) 0.0531(13) Uani 1 1 d . . . N45 N 0.6494(2) 0.3070(2) 0.27590(19) 0.0419(11) Uani 1 1 d . . . N46 N 0.6550(3) 0.2750(2) 0.3197(2) 0.0449(12) Uani 1 1 d . . . N47 N 0.5912(3) 0.1306(3) 0.3642(2) 0.0554(14) Uani 1 1 d . . . N48 N 0.6098(3) 0.1083(3) 0.4163(2) 0.0546(13) Uani 1 1 d . . . N49 N 0.5318(3) 0.0142(3) 0.3747(2) 0.0630(15) Uani 1 1 d . . . H19 H 0.5205 0.0289 0.3427 0.076 Uiso 1 1 calc R . . H20 H 0.5123 -0.0246 0.3783 0.076 Uiso 1 1 calc R . . N50 N 0.6489(3) 0.0669(3) 0.5093(2) 0.0587(15) Uani 1 1 d . . . N51 N 0.6629(3) 0.3228(3) -0.0576(2) 0.0561(13) Uani 1 1 d . . . N52 N 0.5376(3) 0.1788(3) -0.0609(3) 0.0785(18) Uani 1 1 d . . . H21 H 0.5305 0.1500 -0.0386 0.094 Uiso 1 1 calc R . . H22 H 0.5098 0.1744 -0.0944 0.094 Uiso 1 1 calc R . . N53 N 0.6335(3) 0.2394(3) 0.0043(2) 0.0572(14) Uani 1 1 d . . . N54 N 0.6259(3) 0.1972(3) 0.0437(2) 0.0572(14) Uani 1 1 d . . . N55 N 0.7311(4) 0.2127(3) 0.1837(3) 0.083(2) Uani 1 1 d . . . N56 N 0.7368(3) 0.1806(3) 0.2296(3) 0.0758(18) Uani 1 1 d . . . N57 N 0.6648(3) 0.0319(3) 0.2737(2) 0.0508(12) Uani 1 1 d . . . N58 N 0.6911(3) 0.0102(2) 0.3231(2) 0.0501(12) Uani 1 1 d . . . N59 N 0.6074(3) -0.0857(3) 0.3010(3) 0.0715(17) Uani 1 1 d . . . H23 H 0.5865 -0.0757 0.2689 0.086 Uiso 1 1 calc R . . H24 H 0.5917 -0.1224 0.3114 0.086 Uiso 1 1 calc R . . N60 N 0.7632(3) -0.0211(2) 0.4102(2) 0.0523(12) Uani 1 1 d . . . N61 N 0.7928(3) 0.2744(3) -0.1292(2) 0.0519(13) Uani 1 1 d . . . N62 N 0.6623(3) 0.1373(3) -0.1228(3) 0.0705(16) Uani 1 1 d . . . H25 H 0.6550 0.1114 -0.0982 0.085 Uiso 1 1 calc R . . H26 H 0.6324 0.1321 -0.1554 0.085 Uiso 1 1 calc R . . N63 N 0.7659(3) 0.1963(2) -0.0640(2) 0.0507(12) Uani 1 1 d . . . N64 N 0.7626(3) 0.1560(3) -0.0230(2) 0.0522(13) Uani 1 1 d . . . N65 N 0.8896(4) 0.1684(3) 0.1094(3) 0.086(2) Uani 1 1 d . . . N66 N 0.8972(5) 0.1371(3) 0.1555(3) 0.091(2) Uani 1 1 d . . . N67 N 0.8089(3) 0.0022(3) 0.2089(2) 0.0558(13) Uani 1 1 d . . . N68 N 0.8323(3) -0.0215(2) 0.2581(2) 0.0516(12) Uani 1 1 d . . . N69 N 0.7391(3) -0.1092(3) 0.2373(3) 0.0794(19) Uani 1 1 d . . . H27 H 0.7176 -0.0945 0.2080 0.095 Uiso 1 1 calc R . . H28 H 0.7201 -0.1457 0.2462 0.095 Uiso 1 1 calc R . . N70 N 0.9031(3) -0.0613(2) 0.3405(2) 0.0519(13) Uani 1 1 d . . . N71 N 0.9723(3) 0.2764(3) -0.1614(2) 0.0597(14) Uani 1 1 d . . . N72 N 0.8726(3) 0.1223(3) -0.1502(2) 0.0624(15) Uani 1 1 d . . . H29 H 0.8713 0.0960 -0.1251 0.075 Uiso 1 1 calc R . . H30 H 0.8410 0.1138 -0.1821 0.075 Uiso 1 1 calc R . . N73 N 0.9715(3) 0.1916(3) -0.0939(2) 0.0538(13) Uani 1 1 d . . . N74 N 0.9716(3) 0.1503(3) -0.0539(2) 0.0556(14) Uani 1 1 d . . . N75 N 1.0621(3) 0.1687(2) 0.08674(19) 0.0444(11) Uani 1 1 d . . . N76 N 1.0718(3) 0.1387(2) 0.13274(19) 0.0454(11) Uani 1 1 d . . . N77 N 1.0309(3) -0.0085(2) 0.1832(2) 0.0481(12) Uani 1 1 d . . . N78 N 1.0598(3) -0.0225(2) 0.2359(2) 0.0466(12) Uani 1 1 d . . . N79 N 0.9757(3) -0.1175(2) 0.2204(2) 0.0570(14) Uani 1 1 d . . . H31 H 0.9555 -0.1101 0.1871 0.068 Uiso 1 1 calc R . . H32 H 0.9592 -0.1524 0.2332 0.068 Uiso 1 1 calc R . . N80 N 1.1164(3) -0.0338(2) 0.33622(19) 0.0496(12) Uani 1 1 d . . . N81 N 1.4755(5) 0.2969(5) 0.3700(5) 0.106(3) Uani 1 1 d . . . N82 N 1.3132(6) 0.4698(5) 0.1129(5) 0.121(4) Uani 1 1 d . . . N83 N 0.7146(4) 0.0992(4) -0.2838(3) 0.089(2) Uani 1 1 d . . . N84 N 0.8459(5) -0.0706(5) -0.0041(4) 0.112(3) Uiso 1 1 d D . . N85 N 0.5055(5) -0.2386(5) 0.3002(4) 0.107(3) Uiso 1 1 d D . . N86 N 0.8568(8) -0.2545(8) 0.2554(7) 0.210(6) Uiso 1 1 d D . . C1 C 0.5361(5) 0.4907(4) 0.1881(3) 0.072(2) Uani 1 1 d . . . H33 H 0.4987 0.4558 0.1711 0.086 Uiso 1 1 calc R . . C2 C 0.5249(6) 0.5342(5) 0.2268(4) 0.089(3) Uani 1 1 d . . . H34 H 0.4810 0.5298 0.2364 0.106 Uiso 1 1 calc R . . C3 C 0.5788(6) 0.5849(5) 0.2517(4) 0.098(3) Uani 1 1 d . . . H35 H 0.5720 0.6167 0.2782 0.118 Uiso 1 1 calc R . . C4 C 0.6429(5) 0.5891(4) 0.2381(3) 0.074(2) Uani 1 1 d . . . H36 H 0.6814 0.6227 0.2554 0.089 Uiso 1 1 calc R . . C5 C 0.6479(4) 0.5425(3) 0.1984(3) 0.0623(19) Uani 1 1 d . . . C6 C 0.7134(4) 0.5402(3) 0.1792(3) 0.0597(18) Uani 1 1 d . . . C7 C 0.7580(4) 0.4359(3) 0.0894(3) 0.0560(17) Uani 1 1 d . . . C8 C 0.8167(4) 0.4245(3) 0.0636(3) 0.0559(16) Uani 1 1 d . . . C9 C 0.8829(4) 0.4650(3) 0.0756(3) 0.0644(19) Uani 1 1 d . . . H37 H 0.8934 0.5030 0.1015 0.077 Uiso 1 1 calc R . . C10 C 0.9301(4) 0.4489(3) 0.0501(3) 0.0640(18) Uani 1 1 d . . . H38 H 0.9752 0.4755 0.0569 0.077 Uiso 1 1 calc R . . C11 C 0.9128(4) 0.3921(3) 0.0129(3) 0.0518(15) Uani 1 1 d . . . C12 C 0.9611(3) 0.3674(3) -0.0173(3) 0.0525(15) Uani 1 1 d . . . C13 C 1.1295(3) 0.3881(3) -0.0249(3) 0.0541(16) Uani 1 1 d . . . C14 C 1.1677(4) 0.3487(3) -0.0562(3) 0.0567(17) Uani 1 1 d . . . C15 C 1.2359(4) 0.3693(4) -0.0577(4) 0.077(2) Uani 1 1 d . . . H39 H 1.2621 0.4095 -0.0384 0.092 Uiso 1 1 calc R . . C16 C 1.2656(5) 0.3291(6) -0.0885(4) 0.097(3) Uani 1 1 d . . . H40 H 1.3128 0.3415 -0.0905 0.117 Uiso 1 1 calc R . . C17 C 1.2257(7) 0.2708(5) -0.1162(4) 0.095(3) Uani 1 1 d . . . H41 H 1.2453 0.2418 -0.1362 0.114 Uiso 1 1 calc R . . C18 C 1.1557(5) 0.2563(4) -0.1136(3) 0.081(2) Uani 1 1 d . . . H42 H 1.1270 0.2177 -0.1342 0.097 Uiso 1 1 calc R . . C19 C 0.6094(5) 0.4351(5) 0.3399(4) 0.085(2) Uani 1 1 d . . . H43 H 0.5789 0.3952 0.3250 0.102 Uiso 1 1 calc R . . C20 C 0.5896(5) 0.4786(5) 0.3737(4) 0.090(3) Uani 1 1 d . . . H44 H 0.5440 0.4705 0.3803 0.107 Uiso 1 1 calc R . . C21 C 0.6362(5) 0.5345(5) 0.3983(4) 0.089(3) Uani 1 1 d . . . H45 H 0.6250 0.5630 0.4252 0.107 Uiso 1 1 calc R . . C22 C 0.6965(5) 0.5479(4) 0.3840(4) 0.105(4) Uani 1 1 d . . . H46 H 0.7259 0.5889 0.3960 0.126 Uiso 1 1 calc R . . C23 C 0.7170(4) 0.5016(4) 0.3510(4) 0.077(2) Uani 1 1 d . . . C24 C 0.7810(5) 0.5117(4) 0.3316(4) 0.092(3) Uani 1 1 d . . . C25 C 0.8388(4) 0.4012(3) 0.2538(3) 0.0625(18) Uani 1 1 d . . . C26 C 0.8920(4) 0.3844(3) 0.2244(3) 0.0646(19) Uani 1 1 d . . . C27 C 0.9572(4) 0.4052(4) 0.2480(3) 0.075(2) Uani 1 1 d . . . H47 H 0.9708 0.4322 0.2830 0.091 Uiso 1 1 calc R . . C28 C 1.0058(4) 0.3884(4) 0.2227(3) 0.073(2) Uani 1 1 d . . . H48 H 1.0538 0.4038 0.2397 0.087 Uiso 1 1 calc R . . C29 C 0.9868(4) 0.3514(3) 0.1753(3) 0.0609(17) Uani 1 1 d . . . C30 C 1.0394(4) 0.3317(3) 0.1486(3) 0.0526(15) Uani 1 1 d . . . C31 C 1.2153(4) 0.3393(3) 0.1630(3) 0.0508(15) Uani 1 1 d . . . C32 C 1.2488(4) 0.3105(3) 0.1219(3) 0.0511(15) Uani 1 1 d . . . C33 C 1.3189(4) 0.3175(4) 0.1277(3) 0.0647(18) Uani 1 1 d . . . H49 H 1.3499 0.3426 0.1602 0.078 Uiso 1 1 calc R . . C34 C 1.3444(5) 0.2893(4) 0.0883(4) 0.083(2) Uani 1 1 d . . . H50 H 1.3932 0.2934 0.0929 0.099 Uiso 1 1 calc R . . C35 C 1.2988(5) 0.2539(4) 0.0406(4) 0.082(3) Uani 1 1 d . . . H51 H 1.3161 0.2352 0.0113 0.099 Uiso 1 1 calc R . . C36 C 1.2267(4) 0.2457(4) 0.0356(3) 0.069(2) Uani 1 1 d . . . H52 H 1.1952 0.2189 0.0043 0.082 Uiso 1 1 calc R . . C37 C 0.6317(4) 0.3419(4) 0.4621(4) 0.080(2) Uani 1 1 d . . . H53 H 0.6028 0.3009 0.4488 0.096 Uiso 1 1 calc R . . C38 C 0.6099(5) 0.3860(4) 0.4947(4) 0.077(2) Uani 1 1 d . . . H54 H 0.5634 0.3774 0.4993 0.093 Uiso 1 1 calc R . . C39 C 0.6516(5) 0.4388(6) 0.5191(4) 0.103(3) Uani 1 1 d . . . H55 H 0.6393 0.4658 0.5464 0.123 Uiso 1 1 calc R . . C40 C 0.7168(6) 0.4553(5) 0.5037(5) 0.119(4) Uani 1 1 d . . . H56 H 0.7451 0.4968 0.5151 0.143 Uiso 1 1 calc R . . C41 C 0.7378(4) 0.4099(4) 0.4721(3) 0.074(2) Uani 1 1 d . . . C42 C 0.8031(5) 0.4176(5) 0.4546(5) 0.122(4) Uani 1 1 d . . . C43 C 0.8621(4) 0.3110(3) 0.3791(3) 0.0526(15) Uani 1 1 d . . . C44 C 0.9193(4) 0.2930(3) 0.3562(3) 0.0565(16) Uani 1 1 d . . . C45 C 0.9819(5) 0.3314(4) 0.3690(5) 0.109(4) Uani 1 1 d . . . H57 H 0.9903 0.3698 0.3940 0.131 Uiso 1 1 calc R . . C46 C 1.0328(4) 0.3162(4) 0.3471(4) 0.098(3) Uani 1 1 d . . . H58 H 1.0782 0.3427 0.3582 0.117 Uiso 1 1 calc R . . C47 C 1.0211(3) 0.2649(3) 0.3100(3) 0.0497(14) Uani 1 1 d . . . C48 C 1.0744(3) 0.2477(3) 0.2801(3) 0.0526(15) Uani 1 1 d . . . C49 C 1.2468(3) 0.2591(3) 0.2833(2) 0.0457(13) Uani 1 1 d . . . C50 C 1.2756(3) 0.2256(3) 0.2406(3) 0.0468(14) Uani 1 1 d . . . C51 C 1.3455(3) 0.2300(3) 0.2430(3) 0.0588(17) Uani 1 1 d . . . H59 H 1.3793 0.2563 0.2733 0.071 Uiso 1 1 calc R . . C52 C 1.3663(4) 0.1963(4) 0.2012(3) 0.0613(17) Uani 1 1 d . . . H60 H 1.4142 0.1989 0.2023 0.074 Uiso 1 1 calc R . . C53 C 1.3168(4) 0.1596(3) 0.1587(3) 0.0597(18) Uani 1 1 d . . . H61 H 1.3298 0.1356 0.1298 0.072 Uiso 1 1 calc R . . C54 C 1.2461(4) 0.1569(3) 0.1572(3) 0.0569(16) Uani 1 1 d . . . H62 H 1.2120 0.1314 0.1266 0.068 Uiso 1 1 calc R . . C55 C 0.5836(5) 0.2115(5) 0.5345(4) 0.086(3) Uani 1 1 d . . . H63 H 0.5468 0.1810 0.5099 0.103 Uiso 1 1 calc R . . C56 C 0.5686(6) 0.2535(6) 0.5752(5) 0.105(4) Uani 1 1 d . . . H64 H 0.5218 0.2518 0.5775 0.126 Uiso 1 1 calc R . . C57 C 0.6206(7) 0.2961(5) 0.6110(4) 0.093(3) Uani 1 1 d . . . H65 H 0.6097 0.3238 0.6388 0.112 Uiso 1 1 calc R . . C58 C 0.6903(5) 0.3006(4) 0.6083(3) 0.079(3) Uani 1 1 d . . . H66 H 0.7275 0.3310 0.6326 0.094 Uiso 1 1 calc R . . C59 C 0.7005(5) 0.2555(4) 0.5657(3) 0.065(2) Uani 1 1 d . . . C60 C 0.7722(4) 0.2575(3) 0.5577(3) 0.0552(17) Uani 1 1 d . . . C61 C 0.8250(4) 0.1603(3) 0.4650(3) 0.0508(16) Uani 1 1 d . . . C62 C 0.8883(3) 0.1521(3) 0.4445(2) 0.0415(13) Uani 1 1 d . . . C63 C 0.9542(3) 0.1891(3) 0.4647(2) 0.0497(14) Uani 1 1 d . . . H67 H 0.9627 0.2237 0.4939 0.060 Uiso 1 1 calc R . . C64 C 1.0068(3) 0.1754(3) 0.4422(3) 0.0472(14) Uani 1 1 d . . . H68 H 1.0531 0.1995 0.4551 0.057 Uiso 1 1 calc R . . C65 C 0.9896(3) 0.1233(3) 0.3984(2) 0.0460(14) Uani 1 1 d . . . C66 C 1.0420(3) 0.1021(3) 0.3695(2) 0.0442(13) Uani 1 1 d . . . C67 C 1.2159(3) 0.1458(3) 0.3745(3) 0.0498(15) Uani 1 1 d . . . C68 C 1.2666(4) 0.1235(3) 0.3468(3) 0.0530(16) Uani 1 1 d . . . C69 C 1.3388(4) 0.1505(4) 0.3640(3) 0.0620(18) Uani 1 1 d . . . H69 H 1.3568 0.1837 0.3949 0.074 Uiso 1 1 calc R . . C70 C 1.3818(4) 0.1271(4) 0.3347(3) 0.0652(19) Uani 1 1 d . . . H70 H 1.4306 0.1436 0.3453 0.078 Uiso 1 1 calc R . . C71 C 1.3547(5) 0.0805(4) 0.2905(4) 0.074(2) Uani 1 1 d . . . H71 H 1.3843 0.0648 0.2697 0.089 Uiso 1 1 calc R . . C72 C 1.2823(4) 0.0554(3) 0.2755(3) 0.0598(17) Uani 1 1 d . . . H72 H 1.2638 0.0231 0.2440 0.072 Uiso 1 1 calc R . . C73 C 0.5793(4) 0.4753(4) -0.0012(3) 0.069(2) Uani 1 1 d . . . H73 H 0.6128 0.5136 0.0137 0.083 Uiso 1 1 calc R . . C74 C 0.5434(5) 0.4674(5) -0.0556(4) 0.087(3) Uani 1 1 d . . . H74 H 0.5524 0.4998 -0.0783 0.104 Uiso 1 1 calc R . . C75 C 0.4950(5) 0.4135(5) -0.0777(3) 0.078(2) Uani 1 1 d . . . H75 H 0.4688 0.4085 -0.1153 0.093 Uiso 1 1 calc R . . C76 C 0.4840(4) 0.3657(4) -0.0450(3) 0.0655(19) Uani 1 1 d . . . H76 H 0.4508 0.3271 -0.0597 0.079 Uiso 1 1 calc R . . C77 C 0.5231(3) 0.3758(3) 0.0101(3) 0.0525(16) Uani 1 1 d . . . C78 C 0.5190(3) 0.3284(4) 0.0490(2) 0.0518(16) Uani 1 1 d . . . C79 C 0.6011(3) 0.3254(3) 0.1838(3) 0.0486(15) Uani 1 1 d . . . C80 C 0.6029(3) 0.2823(3) 0.2281(3) 0.0472(14) Uani 1 1 d . . . C81 C 0.5621(3) 0.2202(3) 0.2204(3) 0.0524(15) Uani 1 1 d . . . H77 H 0.5309 0.2020 0.1854 0.063 Uiso 1 1 calc R . . C82 C 0.5689(3) 0.1877(3) 0.2643(3) 0.0494(15) Uani 1 1 d . . . H78 H 0.5423 0.1458 0.2616 0.059 Uiso 1 1 calc R . . C83 C 0.6163(3) 0.2172(3) 0.3142(3) 0.0463(14) Uani 1 1 d . . . C84 C 0.6285(3) 0.1862(3) 0.3664(3) 0.0461(14) Uani 1 1 d . . . C85 C 0.5776(4) 0.0501(3) 0.4169(3) 0.0582(17) Uani 1 1 d . . . C86 C 0.5991(3) 0.0265(3) 0.4717(3) 0.0541(15) Uani 1 1 d . . . C87 C 0.5687(4) -0.0317(4) 0.4849(3) 0.071(2) Uani 1 1 d . . . H79 H 0.5327 -0.0606 0.4580 0.085 Uiso 1 1 calc R . . C88 C 0.5922(4) -0.0464(4) 0.5377(3) 0.067(2) Uani 1 1 d . . . H80 H 0.5734 -0.0865 0.5472 0.080 Uiso 1 1 calc R . . C89 C 0.6411(5) -0.0047(4) 0.5757(3) 0.077(2) Uani 1 1 d . . . H81 H 0.6563 -0.0141 0.6126 0.093 Uiso 1 1 calc R . . C90 C 0.6688(4) 0.0511(4) 0.5608(3) 0.0652(19) Uani 1 1 d . . . H82 H 0.7039 0.0806 0.5880 0.078 Uiso 1 1 calc R . . C91 C 0.6806(5) 0.3689(4) -0.0871(3) 0.070(2) Uani 1 1 d . . . H83 H 0.7215 0.4004 -0.0706 0.084 Uiso 1 1 calc R . . C92 C 0.6460(7) 0.3747(5) -0.1376(4) 0.093(3) Uani 1 1 d . . . H84 H 0.6622 0.4083 -0.1569 0.112 Uiso 1 1 calc R . . C93 C 0.5867(7) 0.3308(5) -0.1609(4) 0.104(4) Uani 1 1 d . . . H85 H 0.5598 0.3348 -0.1965 0.125 Uiso 1 1 calc R . . C94 C 0.5639(5) 0.2787(5) -0.1332(3) 0.088(3) Uani 1 1 d . . . H86 H 0.5234 0.2467 -0.1495 0.105 Uiso 1 1 calc R . . C95 C 0.6056(4) 0.2785(4) -0.0800(3) 0.0620(19) Uani 1 1 d . . . C96 C 0.5898(4) 0.2285(4) -0.0440(3) 0.0630(18) Uani 1 1 d . . . C97 C 0.6820(3) 0.2172(3) 0.0845(2) 0.0450(13) Uani 1 1 d . . . C98 C 0.6863(3) 0.1823(3) 0.1349(3) 0.0530(15) Uani 1 1 d . . . C99 C 0.6472(3) 0.1249(3) 0.1310(2) 0.0465(14) Uani 1 1 d . . . H87 H 0.6150 0.1060 0.0967 0.056 Uiso 1 1 calc R . . C100 C 0.6531(3) 0.0935(3) 0.1750(2) 0.0436(13) Uani 1 1 d . . . H88 H 0.6247 0.0524 0.1721 0.052 Uiso 1 1 calc R . . C101 C 0.6988(3) 0.1196(3) 0.2234(3) 0.0527(15) Uani 1 1 d . . . C102 C 0.7114(3) 0.0838(3) 0.2710(3) 0.0512(15) Uani 1 1 d . . . C103 C 0.6628(4) -0.0453(4) 0.3337(3) 0.0606(17) Uani 1 1 d . . . C104 C 0.7024(3) -0.0615(3) 0.3876(3) 0.0499(14) Uani 1 1 d . . . C105 C 0.6792(4) -0.1126(4) 0.4121(3) 0.072(2) Uani 1 1 d . . . H89 H 0.6352 -0.1401 0.3963 0.087 Uiso 1 1 calc R . . C106 C 0.7217(5) -0.1233(4) 0.4607(3) 0.072(2) Uani 1 1 d . . . H90 H 0.7067 -0.1586 0.4786 0.087 Uiso 1 1 calc R . . C107 C 0.7840(4) -0.0842(3) 0.4826(3) 0.0655(19) Uani 1 1 d . . . H91 H 0.8139 -0.0923 0.5152 0.079 Uiso 1 1 calc R . . C108 C 0.8035(4) -0.0320(3) 0.4568(3) 0.0603(17) Uani 1 1 d . . . H92 H 0.8468 -0.0033 0.4727 0.072 Uiso 1 1 calc R . . C109 C 0.8094(4) 0.3208(3) -0.1602(3) 0.0623(18) Uani 1 1 d . . . H93 H 0.8508 0.3525 -0.1459 0.075 Uiso 1 1 calc R . . C110 C 0.7682(4) 0.3234(4) -0.2117(3) 0.070(2) Uani 1 1 d . . . H94 H 0.7814 0.3558 -0.2333 0.084 Uiso 1 1 calc R . . C111 C 0.7074(5) 0.2781(4) -0.2314(3) 0.070(2) Uani 1 1 d . . . H95 H 0.6784 0.2790 -0.2670 0.084 Uiso 1 1 calc R . . C112 C 0.6887(4) 0.2323(3) -0.2001(3) 0.0605(18) Uani 1 1 d . . . H96 H 0.6460 0.2019 -0.2129 0.073 Uiso 1 1 calc R . . C113 C 0.7324(4) 0.2305(3) -0.1497(2) 0.0487(15) Uani 1 1 d . . . C114 C 0.7181(4) 0.1840(3) -0.1108(3) 0.0541(16) Uani 1 1 d . . . C115 C 0.8209(3) 0.1780(3) 0.0171(2) 0.0473(14) Uani 1 1 d . . . C116 C 0.8307(4) 0.1446(3) 0.0673(3) 0.0536(16) Uani 1 1 d . . . C117 C 0.7821(3) 0.0949(3) 0.0717(3) 0.0537(16) Uani 1 1 d . . . H97 H 0.7415 0.0804 0.0423 0.064 Uiso 1 1 calc R . . C118 C 0.7904(3) 0.0661(3) 0.1162(3) 0.0542(16) Uani 1 1 d . . . H98 H 0.7553 0.0312 0.1190 0.065 Uiso 1 1 calc R . . C119 C 0.8460(4) 0.0845(3) 0.1569(3) 0.0535(16) Uani 1 1 d . . . C120 C 0.8574(4) 0.0514(3) 0.2062(3) 0.0515(15) Uani 1 1 d . . . C121 C 0.8001(3) -0.0761(3) 0.2680(3) 0.0529(16) Uani 1 1 d . . . C122 C 0.8392(4) -0.0975(3) 0.3189(3) 0.0575(17) Uani 1 1 d . . . C123 C 0.8131(5) -0.1492(4) 0.3425(3) 0.074(2) Uani 1 1 d . . . H99 H 0.7671 -0.1734 0.3278 0.089 Uiso 1 1 calc R . . C124 C 0.8551(6) -0.1647(4) 0.3876(4) 0.083(3) Uani 1 1 d . . . H100 H 0.8391 -0.2011 0.4038 0.099 Uiso 1 1 calc R . . C125 C 0.9209(5) -0.1276(4) 0.4098(3) 0.073(2) Uani 1 1 d . . . H101 H 0.9506 -0.1377 0.4415 0.088 Uiso 1 1 calc R . . C126 C 0.9419(4) -0.0760(3) 0.3850(2) 0.0567(17) Uani 1 1 d . . . H102 H 0.9866 -0.0496 0.4006 0.068 Uiso 1 1 calc R . . C127 C 0.9765(5) 0.3194(4) -0.1962(4) 0.079(2) Uani 1 1 d . . . H103 H 1.0106 0.3578 -0.1838 0.095 Uiso 1 1 calc R . . C128 C 0.9339(7) 0.3114(6) -0.2499(5) 0.107(4) Uani 1 1 d . . . H104 H 0.9379 0.3439 -0.2731 0.128 Uiso 1 1 calc R . . C129 C 0.8864(6) 0.2558(5) -0.2683(3) 0.084(3) Uani 1 1 d . . . H105 H 0.8573 0.2486 -0.3051 0.101 Uiso 1 1 calc R . . C130 C 0.8808(4) 0.2101(4) -0.2334(3) 0.0666(19) Uani 1 1 d . . . H106 H 0.8475 0.1711 -0.2452 0.080 Uiso 1 1 calc R . . C131 C 0.9245(4) 0.2226(4) -0.1815(3) 0.0537(17) Uani 1 1 d . . . C132 C 0.9225(3) 0.1750(3) -0.1399(2) 0.0483(14) Uani 1 1 d . . . C133 C 1.0150(3) 0.1765(3) -0.0071(2) 0.0508(15) Uani 1 1 d . . . C134 C 1.0206(3) 0.1380(3) 0.0392(2) 0.0474(14) Uani 1 1 d . . . C135 C 0.9841(4) 0.0750(3) 0.0349(3) 0.0563(16) Uani 1 1 d . . . H107 H 0.9528 0.0540 0.0008 0.068 Uiso 1 1 calc R . . C136 C 0.9950(4) 0.0447(3) 0.0818(3) 0.0588(17) Uani 1 1 d . . . H108 H 0.9717 0.0020 0.0807 0.071 Uiso 1 1 calc R . . C137 C 1.0407(3) 0.0776(3) 0.1306(2) 0.0478(14) Uani 1 1 d . . . C138 C 1.0586(3) 0.0515(3) 0.1837(2) 0.0446(13) Uani 1 1 d . . . C139 C 1.0310(4) -0.0762(3) 0.2512(2) 0.0467(14) Uani 1 1 d . . . C140 C 1.0679(4) -0.0851(3) 0.3083(3) 0.0541(16) Uani 1 1 d . . . C141 C 1.0538(4) -0.1404(3) 0.3313(3) 0.0609(18) Uani 1 1 d . . . H109 H 1.0190 -0.1758 0.3110 0.073 Uiso 1 1 calc R . . C142 C 1.0921(4) -0.1433(3) 0.3853(3) 0.064(2) Uani 1 1 d . . . H110 H 1.0839 -0.1805 0.4026 0.076 Uiso 1 1 calc R . . C143 C 1.1410(4) -0.0917(4) 0.4119(3) 0.066(2) Uani 1 1 d . . . H111 H 1.1683 -0.0928 0.4482 0.079 Uiso 1 1 calc R . . C144 C 1.1518(4) -0.0374(3) 0.3869(3) 0.0566(16) Uani 1 1 d . . . H112 H 1.1858 -0.0014 0.4070 0.068 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 0.0724(6) 0.0582(5) 0.0432(4) 0.0129(3) 0.0195(4) 0.0278(4) Cu2 0.0529(5) 0.0524(5) 0.0500(4) 0.0135(3) 0.0108(4) 0.0164(4) Cu3 0.0497(5) 0.0533(5) 0.0486(4) 0.0121(3) 0.0142(3) 0.0119(4) Cu4 0.0487(5) 0.0788(6) 0.0477(4) 0.0120(4) 0.0164(4) 0.0071(4) Cu5 0.0496(4) 0.0515(4) 0.0444(4) 0.0106(3) 0.0170(3) 0.0107(4) Cu6 0.0426(4) 0.0467(4) 0.0440(4) 0.0094(3) 0.0103(3) 0.0051(3) Cu7 0.0522(5) 0.0483(4) 0.0426(4) 0.0146(3) 0.0115(3) 0.0087(4) Cu8 0.0497(4) 0.0476(4) 0.0423(4) 0.0081(3) 0.0121(3) 0.0058(3) Cu9 0.0467(4) 0.0469(4) 0.0429(4) 0.0089(3) 0.0116(3) 0.0075(3) Cu10 0.0694(6) 0.0568(5) 0.0508(4) 0.0180(4) 0.0265(4) 0.0211(4) Cu11 0.0494(5) 0.0656(5) 0.0686(5) -0.0052(4) 0.0166(4) 0.0149(4) Cu12 0.0512(5) 0.0637(5) 0.0668(5) -0.0122(4) 0.0169(4) 0.0128(4) Na1 0.029(5) 0.063(6) 0.069(6) -0.008(5) 0.005(4) 0.006(4) Na2 0.050(12) 0.062(13) 0.052(11) 0.014(9) 0.020(9) -0.012(10) Na3 0.054(3) 0.059(3) 0.048(3) 0.000(2) 0.014(2) 0.006(2) Na4 0.044(2) 0.0446(19) 0.0372(17) 0.0000(14) 0.0014(15) 0.0057(16) O1 0.055(3) 0.059(3) 0.056(3) 0.014(2) 0.023(2) 0.026(2) O2 0.050(3) 0.050(2) 0.063(3) 0.014(2) 0.024(2) 0.014(2) O3 0.056(3) 0.068(3) 0.100(4) -0.033(3) 0.027(3) -0.003(3) O4 0.042(2) 0.061(3) 0.053(2) 0.011(2) 0.012(2) 0.010(2) O5 0.045(3) 0.072(3) 0.076(3) -0.014(2) 0.015(2) 0.012(2) O6 0.035(2) 0.064(3) 0.053(2) 0.001(2) 0.0064(19) 0.007(2) O7 0.043(2) 0.061(3) 0.048(2) 0.012(2) 0.0157(19) 0.018(2) O8 0.052(3) 0.053(2) 0.039(2) 0.0057(18) 0.0085(18) 0.013(2) O9 0.065(3) 0.055(3) 0.059(3) 0.023(2) 0.021(2) 0.013(2) O10 0.049(3) 0.060(3) 0.053(2) 0.024(2) 0.017(2) 0.016(2) O11 0.048(3) 0.059(3) 0.053(2) 0.020(2) 0.001(2) 0.003(2) O12 0.042(2) 0.056(3) 0.044(2) 0.0128(19) 0.0052(18) 0.003(2) O13 0.050(3) 0.063(3) 0.053(2) 0.020(2) 0.007(2) -0.001(2) O14 0.055(3) 0.057(3) 0.039(2) 0.0082(19) 0.0076(19) 0.002(2) O15 0.059(3) 0.049(2) 0.037(2) 0.0105(18) 0.0156(19) 0.012(2) O16 0.055(3) 0.042(2) 0.043(2) 0.0127(18) 0.0067(19) 0.006(2) O17 0.072(5) 0.134(6) 0.193(8) -0.067(6) -0.012(5) 0.043(5) O18 0.116(7) 0.164(9) 0.189(10) 0.056(8) 0.009(7) -0.004(6) O19 0.074(5) 0.262(12) 0.236(11) -0.166(10) 0.051(6) 0.001(6) O20 0.111(7) 0.218(11) 0.205(11) 0.107(9) 0.029(7) 0.031(8) O21 0.093(5) 0.114(6) 0.135(6) 0.061(5) -0.012(4) 0.010(4) O22 0.100(6) 0.154(7) 0.087(5) 0.002(5) 0.011(4) -0.008(5) O23 0.105(6) 0.270(12) 0.082(5) -0.042(6) 0.021(5) 0.000(7) O24 0.069(5) 0.212(9) 0.105(5) -0.014(5) -0.023(4) 0.032(5) O25 0.078(4) 0.089(4) 0.103(5) -0.014(3) -0.014(3) 0.015(3) N1 0.075(4) 0.045(3) 0.054(3) 0.013(2) 0.016(3) 0.023(3) N2 0.103(6) 0.062(4) 0.096(5) -0.007(4) 0.043(5) 0.004(4) N3 0.076(4) 0.055(3) 0.052(3) 0.007(3) 0.023(3) 0.021(3) N4 0.081(4) 0.053(3) 0.066(4) 0.016(3) 0.035(3) 0.019(3) N5 0.054(3) 0.046(3) 0.054(3) 0.014(2) 0.016(3) 0.015(3) N6 0.045(3) 0.052(3) 0.052(3) 0.020(2) 0.018(2) 0.018(2) N7 0.055(4) 0.071(4) 0.062(3) 0.014(3) 0.025(3) 0.018(3) N8 0.053(3) 0.062(4) 0.067(4) 0.014(3) 0.019(3) 0.009(3) N9 0.056(4) 0.059(4) 0.086(4) -0.003(3) 0.018(3) 0.011(3) N10 0.065(4) 0.058(3) 0.050(3) 0.017(3) 0.023(3) 0.017(3) N11 0.063(4) 0.066(4) 0.056(3) 0.002(3) 0.018(3) 0.029(3) N12 0.137(8) 0.074(5) 0.177(9) -0.037(6) 0.068(7) -0.030(5) N13 0.077(4) 0.059(4) 0.103(5) -0.032(3) 0.050(4) -0.013(3) N14 0.076(5) 0.096(6) 0.129(7) -0.052(5) 0.052(5) -0.011(4) N15 0.084(5) 0.072(4) 0.111(6) -0.004(4) 0.047(5) 0.008(4) N16 0.092(6) 0.089(5) 0.097(5) 0.001(4) 0.051(5) 0.011(4) N17 0.064(4) 0.061(4) 0.063(3) 0.005(3) 0.023(3) 0.017(3) N18 0.045(3) 0.063(4) 0.070(4) 0.003(3) 0.023(3) 0.007(3) N19 0.068(4) 0.062(4) 0.078(4) 0.006(3) 0.012(3) -0.002(3) N20 0.051(3) 0.053(3) 0.060(3) 0.020(3) 0.023(3) 0.012(3) N21 0.057(4) 0.080(4) 0.058(3) 0.010(3) 0.015(3) 0.029(3) N22 0.092(7) 0.126(8) 0.235(12) -0.097(8) 0.026(7) 0.001(6) N23 0.056(4) 0.074(4) 0.107(5) -0.032(4) 0.031(4) 0.000(3) N24 0.061(4) 0.090(5) 0.150(7) -0.039(5) 0.037(5) 0.006(4) N25 0.048(4) 0.146(7) 0.079(5) -0.032(5) 0.017(3) 0.015(4) N26 0.051(4) 0.132(7) 0.072(4) -0.018(4) 0.008(3) -0.005(4) N27 0.036(3) 0.056(3) 0.048(3) 0.003(2) 0.012(2) 0.004(2) N28 0.036(3) 0.054(3) 0.050(3) 0.010(2) 0.013(2) 0.006(2) N29 0.037(3) 0.057(3) 0.062(3) 0.000(3) 0.008(2) -0.003(2) N30 0.055(3) 0.044(3) 0.043(3) 0.015(2) 0.018(2) 0.008(2) N31 0.073(4) 0.061(4) 0.069(4) 0.022(3) 0.022(3) 0.022(3) N32 0.090(5) 0.067(4) 0.068(4) -0.006(3) 0.011(4) 0.021(4) N33 0.068(4) 0.050(3) 0.054(3) 0.019(2) 0.028(3) 0.025(3) N34 0.064(3) 0.045(3) 0.047(3) 0.017(2) 0.016(3) 0.018(3) N35 0.044(3) 0.044(3) 0.043(3) 0.011(2) 0.012(2) 0.006(2) N36 0.043(3) 0.036(2) 0.044(3) 0.010(2) 0.008(2) 0.001(2) N37 0.051(3) 0.060(3) 0.043(3) 0.019(2) 0.017(2) 0.014(3) N38 0.051(3) 0.050(3) 0.044(3) 0.017(2) 0.014(2) 0.015(2) N39 0.045(3) 0.064(4) 0.057(3) 0.003(3) 0.005(3) -0.003(3) N40 0.057(3) 0.053(3) 0.054(3) 0.025(3) 0.017(3) 0.017(3) N41 0.068(4) 0.072(4) 0.043(3) 0.016(3) 0.012(3) 0.030(3) N42 0.056(4) 0.078(4) 0.060(3) 0.011(3) 0.014(3) -0.001(3) N43 0.055(3) 0.073(4) 0.055(3) 0.023(3) 0.025(3) 0.025(3) N44 0.059(3) 0.067(4) 0.042(3) 0.015(2) 0.022(3) 0.018(3) N45 0.042(3) 0.048(3) 0.043(3) 0.017(2) 0.017(2) 0.015(2) N46 0.050(3) 0.051(3) 0.048(3) 0.024(2) 0.025(2) 0.023(2) N47 0.067(4) 0.054(3) 0.056(3) 0.027(3) 0.027(3) 0.016(3) N48 0.061(3) 0.052(3) 0.063(3) 0.024(3) 0.026(3) 0.021(3) N49 0.067(4) 0.062(4) 0.065(4) 0.030(3) 0.013(3) 0.018(3) N50 0.074(4) 0.064(4) 0.055(3) 0.026(3) 0.033(3) 0.028(3) N51 0.061(4) 0.054(3) 0.055(3) 0.008(3) 0.009(3) 0.022(3) N52 0.070(4) 0.095(5) 0.054(3) 0.002(3) -0.001(3) -0.001(4) N53 0.054(3) 0.081(4) 0.044(3) 0.025(3) 0.013(3) 0.021(3) N54 0.046(3) 0.074(4) 0.049(3) 0.012(3) 0.009(2) 0.008(3) N55 0.069(4) 0.080(5) 0.096(5) 0.034(4) 0.015(4) 0.004(4) N56 0.057(4) 0.089(5) 0.082(4) 0.031(4) 0.019(3) 0.005(3) N57 0.051(3) 0.054(3) 0.048(3) 0.013(2) 0.013(2) 0.011(3) N58 0.057(3) 0.051(3) 0.046(3) 0.011(2) 0.020(2) 0.010(3) N59 0.062(4) 0.073(4) 0.070(4) 0.016(3) 0.009(3) -0.006(3) N60 0.056(3) 0.051(3) 0.048(3) 0.006(2) 0.013(3) 0.008(3) N61 0.054(3) 0.057(3) 0.046(3) 0.007(2) 0.011(2) 0.017(3) N62 0.061(4) 0.069(4) 0.066(4) 0.011(3) -0.010(3) 0.000(3) N63 0.061(3) 0.049(3) 0.044(3) 0.009(2) 0.009(2) 0.016(3) N64 0.054(3) 0.058(3) 0.045(3) 0.010(2) 0.010(2) 0.014(3) N65 0.139(7) 0.070(4) 0.054(4) 0.024(3) 0.020(4) 0.028(5) N66 0.137(7) 0.068(4) 0.063(4) 0.012(3) 0.018(4) 0.018(5) N67 0.049(3) 0.055(3) 0.059(3) 0.009(3) 0.005(3) 0.009(3) N68 0.055(3) 0.053(3) 0.045(3) 0.008(2) 0.015(2) 0.002(3) N69 0.072(4) 0.068(4) 0.082(4) 0.013(3) 0.016(4) -0.027(3) N70 0.064(4) 0.043(3) 0.050(3) 0.002(2) 0.021(3) 0.007(3) N71 0.068(4) 0.064(4) 0.056(3) 0.015(3) 0.029(3) 0.017(3) N72 0.056(4) 0.078(4) 0.047(3) -0.001(3) 0.006(3) 0.011(3) N73 0.049(3) 0.070(4) 0.041(3) 0.015(2) 0.010(2) 0.007(3) N74 0.068(4) 0.063(3) 0.041(3) 0.011(2) 0.016(3) 0.021(3) N75 0.049(3) 0.049(3) 0.037(2) 0.014(2) 0.012(2) 0.009(2) N76 0.050(3) 0.049(3) 0.040(3) 0.012(2) 0.013(2) 0.013(2) N77 0.056(3) 0.044(3) 0.046(3) 0.015(2) 0.014(2) 0.011(2) N78 0.059(3) 0.041(3) 0.042(3) 0.010(2) 0.016(2) 0.009(2) N79 0.073(4) 0.034(3) 0.055(3) 0.007(2) 0.005(3) -0.002(3) N80 0.065(3) 0.050(3) 0.036(2) 0.009(2) 0.012(2) 0.015(3) N81 0.084(6) 0.095(6) 0.121(7) 0.006(6) 0.005(6) 0.004(5) N82 0.101(8) 0.092(7) 0.153(10) 0.061(7) -0.009(8) -0.003(6) N83 0.071(5) 0.107(6) 0.072(5) -0.025(4) 0.006(4) 0.010(4) C1 0.087(6) 0.082(5) 0.063(4) 0.032(4) 0.029(4) 0.034(5) C2 0.108(8) 0.122(8) 0.069(5) 0.037(6) 0.048(5) 0.062(7) C3 0.139(10) 0.093(7) 0.077(6) -0.005(5) 0.048(6) 0.046(7) C4 0.087(6) 0.068(5) 0.074(5) -0.001(4) 0.023(4) 0.035(5) C5 0.090(6) 0.057(4) 0.056(4) 0.017(3) 0.035(4) 0.033(4) C6 0.080(5) 0.050(4) 0.055(4) 0.012(3) 0.024(4) 0.020(4) C7 0.069(5) 0.061(4) 0.052(4) 0.024(3) 0.027(3) 0.025(4) C8 0.060(4) 0.053(4) 0.066(4) 0.019(3) 0.027(3) 0.021(3) C9 0.070(5) 0.055(4) 0.079(5) 0.008(4) 0.038(4) 0.017(4) C10 0.068(5) 0.052(4) 0.068(4) 0.008(3) 0.024(4) -0.008(3) C11 0.060(4) 0.045(3) 0.056(4) 0.014(3) 0.022(3) 0.011(3) C12 0.041(3) 0.052(4) 0.064(4) 0.011(3) 0.013(3) 0.007(3) C13 0.041(3) 0.049(4) 0.074(4) 0.019(3) 0.013(3) 0.011(3) C14 0.060(4) 0.064(4) 0.060(4) 0.032(3) 0.024(3) 0.025(4) C15 0.059(5) 0.085(6) 0.098(6) 0.036(5) 0.038(5) 0.009(4) C16 0.085(7) 0.141(10) 0.106(7) 0.060(7) 0.055(6) 0.068(7) C17 0.146(10) 0.107(8) 0.056(5) 0.020(5) 0.031(6) 0.076(8) C18 0.103(7) 0.089(6) 0.067(5) 0.027(4) 0.033(5) 0.039(6) C19 0.065(5) 0.090(6) 0.093(6) -0.011(5) 0.019(5) 0.011(5) C20 0.083(6) 0.120(8) 0.071(5) -0.015(5) 0.021(5) 0.049(6) C21 0.107(8) 0.099(7) 0.087(6) 0.008(5) 0.053(6) 0.055(6) C22 0.096(7) 0.077(6) 0.136(8) -0.050(6) 0.064(7) -0.004(5) C23 0.079(5) 0.055(4) 0.097(6) -0.013(4) 0.053(5) -0.010(4) C24 0.088(6) 0.064(5) 0.113(7) -0.020(5) 0.042(6) -0.019(4) C25 0.066(5) 0.049(4) 0.072(4) -0.002(3) 0.034(4) -0.004(3) C26 0.066(5) 0.053(4) 0.076(5) -0.008(3) 0.032(4) 0.008(4) C27 0.040(4) 0.105(6) 0.070(5) -0.042(4) 0.026(3) 0.000(4) C28 0.043(4) 0.094(6) 0.064(4) -0.031(4) 0.023(3) -0.016(4) C29 0.059(4) 0.061(4) 0.062(4) 0.008(3) 0.023(4) 0.000(3) C30 0.060(4) 0.058(4) 0.045(3) 0.010(3) 0.022(3) 0.013(3) C31 0.065(4) 0.030(3) 0.055(4) 0.012(3) 0.014(3) 0.001(3) C32 0.057(4) 0.037(3) 0.065(4) 0.019(3) 0.023(3) 0.009(3) C33 0.058(4) 0.064(4) 0.077(5) 0.024(4) 0.017(4) 0.014(4) C34 0.067(5) 0.089(6) 0.094(6) 0.018(5) 0.029(5) 0.008(5) C35 0.098(7) 0.094(6) 0.086(6) 0.039(5) 0.056(6) 0.046(6) C36 0.082(5) 0.082(5) 0.068(4) 0.030(4) 0.045(4) 0.042(5) C37 0.067(5) 0.095(6) 0.086(6) -0.001(5) 0.043(5) 0.020(5) C38 0.076(6) 0.082(6) 0.089(6) 0.011(5) 0.029(5) 0.043(5) C39 0.085(7) 0.141(10) 0.086(6) -0.023(6) 0.017(5) 0.057(7) C40 0.097(8) 0.108(8) 0.135(9) -0.057(7) 0.017(7) 0.028(6) C41 0.054(4) 0.082(6) 0.078(5) -0.018(4) 0.009(4) 0.019(4) C42 0.070(6) 0.074(6) 0.193(12) -0.071(7) 0.034(7) -0.012(5) C43 0.050(4) 0.050(4) 0.057(4) 0.003(3) 0.012(3) 0.012(3) C44 0.053(4) 0.051(4) 0.070(4) 0.016(3) 0.021(3) 0.009(3) C45 0.072(6) 0.057(5) 0.196(11) -0.033(6) 0.075(7) -0.012(4) C46 0.059(5) 0.059(5) 0.161(9) -0.052(5) 0.054(6) -0.022(4) C47 0.042(3) 0.054(4) 0.053(4) 0.015(3) 0.014(3) 0.005(3) C48 0.046(4) 0.048(4) 0.065(4) 0.010(3) 0.015(3) 0.010(3) C49 0.035(3) 0.049(3) 0.045(3) 0.004(3) 0.002(2) -0.001(3) C50 0.049(4) 0.042(3) 0.052(3) 0.017(3) 0.015(3) 0.006(3) C51 0.043(4) 0.074(5) 0.061(4) 0.012(3) 0.016(3) 0.012(3) C52 0.048(4) 0.071(5) 0.065(4) 0.015(4) 0.016(3) 0.008(4) C53 0.067(5) 0.061(4) 0.067(4) 0.023(4) 0.030(4) 0.027(4) C54 0.063(4) 0.054(4) 0.062(4) 0.020(3) 0.024(3) 0.015(3) C55 0.074(6) 0.109(7) 0.093(6) 0.043(5) 0.036(5) 0.034(5) C56 0.106(9) 0.131(10) 0.131(9) 0.076(8) 0.075(8) 0.076(8) C57 0.141(10) 0.091(7) 0.095(7) 0.045(6) 0.076(7) 0.072(7) C58 0.104(7) 0.100(6) 0.053(4) 0.023(4) 0.024(4) 0.063(6) C59 0.098(6) 0.065(5) 0.054(4) 0.029(4) 0.033(4) 0.043(5) C60 0.084(5) 0.052(4) 0.040(3) 0.011(3) 0.019(3) 0.032(4) C61 0.066(4) 0.055(4) 0.045(3) 0.024(3) 0.019(3) 0.032(4) C62 0.048(3) 0.041(3) 0.035(3) 0.015(2) 0.005(2) 0.009(3) C63 0.055(4) 0.050(4) 0.043(3) 0.006(3) 0.007(3) 0.012(3) C64 0.040(3) 0.040(3) 0.054(3) 0.006(3) 0.008(3) -0.006(3) C65 0.060(4) 0.036(3) 0.035(3) 0.013(2) -0.002(3) 0.002(3) C66 0.046(3) 0.048(3) 0.045(3) 0.021(3) 0.017(3) 0.012(3) C67 0.050(4) 0.049(4) 0.052(3) 0.025(3) 0.009(3) 0.007(3) C68 0.060(4) 0.063(4) 0.048(3) 0.031(3) 0.021(3) 0.022(3) C69 0.058(4) 0.067(4) 0.063(4) 0.032(4) 0.016(3) 0.005(4) C70 0.063(5) 0.061(4) 0.077(5) 0.029(4) 0.021(4) 0.012(4) C71 0.082(6) 0.079(6) 0.085(6) 0.042(5) 0.042(5) 0.035(5) C72 0.069(5) 0.054(4) 0.065(4) 0.021(3) 0.024(4) 0.017(4) C73 0.056(4) 0.067(5) 0.086(5) 0.026(4) 0.013(4) 0.012(4) C74 0.107(7) 0.106(7) 0.072(5) 0.060(5) 0.028(5) 0.053(6) C75 0.076(6) 0.109(7) 0.059(5) 0.030(5) 0.010(4) 0.044(6) C76 0.058(4) 0.099(6) 0.042(3) 0.012(4) 0.011(3) 0.024(4) C77 0.050(4) 0.066(4) 0.050(4) 0.015(3) 0.019(3) 0.024(3) C78 0.038(3) 0.080(5) 0.041(3) 0.006(3) 0.018(3) 0.014(3) C79 0.053(4) 0.051(4) 0.053(4) 0.022(3) 0.025(3) 0.017(3) C80 0.040(3) 0.044(3) 0.067(4) 0.016(3) 0.024(3) 0.016(3) C81 0.055(4) 0.059(4) 0.046(3) 0.014(3) 0.016(3) 0.009(3) C82 0.046(4) 0.052(4) 0.059(4) 0.018(3) 0.026(3) 0.014(3) C83 0.049(4) 0.048(3) 0.050(3) 0.017(3) 0.018(3) 0.018(3) C84 0.048(4) 0.045(3) 0.055(4) 0.017(3) 0.021(3) 0.019(3) C85 0.062(4) 0.057(4) 0.071(5) 0.027(4) 0.032(4) 0.021(4) C86 0.046(4) 0.062(4) 0.055(4) 0.012(3) 0.009(3) 0.013(3) C87 0.074(5) 0.075(5) 0.079(5) 0.042(4) 0.029(4) 0.027(4) C88 0.074(5) 0.069(5) 0.066(4) 0.038(4) 0.016(4) 0.018(4) C89 0.091(6) 0.085(6) 0.063(5) 0.037(4) 0.016(4) 0.022(5) C90 0.074(5) 0.070(5) 0.061(4) 0.018(4) 0.024(4) 0.024(4) C91 0.105(6) 0.063(5) 0.056(4) 0.018(3) 0.019(4) 0.043(5) C92 0.152(10) 0.069(6) 0.061(5) 0.017(4) 0.011(6) 0.039(6) C93 0.180(12) 0.108(8) 0.056(5) 0.034(5) 0.031(6) 0.091(9) C94 0.097(7) 0.105(7) 0.058(4) -0.002(4) -0.010(4) 0.054(6) C95 0.069(5) 0.081(5) 0.047(4) 0.009(3) 0.015(3) 0.042(4) C96 0.050(4) 0.070(5) 0.066(4) 0.004(4) 0.005(3) 0.017(4) C97 0.037(3) 0.049(3) 0.045(3) 0.001(3) 0.008(3) 0.005(3) C98 0.044(4) 0.063(4) 0.053(4) 0.006(3) 0.016(3) 0.010(3) C99 0.044(3) 0.054(4) 0.034(3) 0.006(2) 0.008(2) -0.007(3) C100 0.040(3) 0.043(3) 0.043(3) 0.008(2) 0.011(3) -0.005(3) C101 0.042(3) 0.060(4) 0.061(4) 0.016(3) 0.019(3) 0.012(3) C102 0.045(4) 0.066(4) 0.048(3) 0.015(3) 0.014(3) 0.018(3) C103 0.050(4) 0.071(5) 0.058(4) 0.008(3) 0.018(3) 0.001(3) C104 0.052(4) 0.051(4) 0.048(3) 0.016(3) 0.015(3) 0.007(3) C105 0.080(5) 0.059(4) 0.066(5) 0.008(4) 0.012(4) -0.007(4) C106 0.088(6) 0.056(4) 0.075(5) 0.027(4) 0.020(4) 0.013(4) C107 0.080(5) 0.062(4) 0.056(4) 0.023(3) 0.018(4) 0.006(4) C108 0.067(5) 0.056(4) 0.060(4) 0.012(3) 0.020(4) 0.011(4) C109 0.066(5) 0.057(4) 0.068(4) 0.015(3) 0.019(4) 0.015(4) C110 0.078(5) 0.072(5) 0.068(5) 0.025(4) 0.023(4) 0.023(4) C111 0.088(6) 0.074(5) 0.051(4) 0.019(4) 0.008(4) 0.032(5) C112 0.074(5) 0.051(4) 0.057(4) 0.015(3) 0.002(3) 0.025(4) C113 0.066(4) 0.057(4) 0.033(3) 0.007(3) 0.013(3) 0.036(3) C114 0.058(4) 0.063(4) 0.040(3) 0.007(3) 0.003(3) 0.017(3) C115 0.043(3) 0.055(4) 0.044(3) 0.008(3) 0.009(3) 0.011(3) C116 0.059(4) 0.066(4) 0.041(3) 0.014(3) 0.008(3) 0.025(4) C117 0.038(3) 0.077(5) 0.049(3) 0.027(3) 0.002(3) 0.016(3) C118 0.049(4) 0.062(4) 0.056(4) 0.027(3) 0.013(3) 0.012(3) C119 0.063(4) 0.058(4) 0.047(3) 0.015(3) 0.023(3) 0.018(3) C120 0.054(4) 0.045(3) 0.055(4) -0.001(3) 0.018(3) 0.009(3) C121 0.057(4) 0.046(3) 0.050(3) -0.005(3) 0.025(3) -0.013(3) C122 0.075(5) 0.051(4) 0.046(3) -0.001(3) 0.025(3) 0.005(3) C123 0.105(7) 0.056(4) 0.066(5) 0.015(4) 0.038(5) 0.006(4) C124 0.132(8) 0.049(4) 0.077(5) 0.022(4) 0.040(6) 0.022(5) C125 0.115(7) 0.062(5) 0.043(4) 0.010(3) 0.016(4) 0.022(5) C126 0.081(5) 0.054(4) 0.036(3) 0.010(3) 0.010(3) 0.017(4) C127 0.088(6) 0.072(5) 0.092(6) 0.031(5) 0.040(5) 0.020(5) C128 0.155(11) 0.116(9) 0.096(7) 0.060(7) 0.071(8) 0.072(9) C129 0.122(8) 0.106(7) 0.044(4) 0.027(5) 0.022(5) 0.063(7) C130 0.070(5) 0.082(5) 0.050(4) 0.003(4) 0.011(3) 0.029(4) C131 0.056(4) 0.080(5) 0.041(3) 0.018(3) 0.023(3) 0.037(4) C132 0.044(3) 0.061(4) 0.036(3) 0.010(3) 0.001(3) 0.009(3) C133 0.048(4) 0.075(5) 0.033(3) 0.009(3) 0.010(3) 0.020(3) C134 0.051(4) 0.051(4) 0.041(3) 0.007(3) 0.009(3) 0.015(3) C135 0.068(4) 0.051(4) 0.046(3) 0.007(3) 0.008(3) 0.008(3) C136 0.072(5) 0.047(4) 0.047(3) 0.004(3) 0.005(3) -0.002(3) C137 0.055(4) 0.051(4) 0.039(3) 0.005(3) 0.013(3) 0.012(3) C138 0.047(3) 0.043(3) 0.041(3) 0.005(2) 0.006(3) 0.006(3) C139 0.074(4) 0.028(3) 0.047(3) 0.011(2) 0.027(3) 0.016(3) C140 0.072(5) 0.054(4) 0.044(3) 0.017(3) 0.023(3) 0.018(4) C141 0.093(6) 0.047(4) 0.052(4) 0.014(3) 0.029(4) 0.020(4) C142 0.099(6) 0.054(4) 0.057(4) 0.030(3) 0.039(4) 0.030(4) C143 0.097(6) 0.066(5) 0.048(4) 0.020(3) 0.028(4) 0.035(5) C144 0.065(4) 0.060(4) 0.050(4) 0.015(3) 0.018(3) 0.017(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 N3 1.902(6) . ? Cu1 N43 1.911(6) . ? Cu1 O1 2.156(4) . ? Cu1 N1 2.186(5) . ? Cu1 O9 2.220(4) . ? Cu1 N41 2.242(5) . ? Cu2 N53 1.879(6) . ? Cu2 O11 1.978(4) . ? Cu2 N51 2.033(5) . ? Cu2 N5 2.034(5) . ? Cu2 O1 2.193(4) . ? Cu3 N63 1.867(6) . ? Cu3 O2 1.954(4) . ? Cu3 O13 1.955(4) . ? Cu3 N61 2.013(5) . ? Cu3 N6 2.243(5) . ? Cu4 N8 1.936(6) . ? Cu4 N73 1.956(6) . ? Cu4 N71 2.140(6) . ? Cu4 N10 2.152(6) . ? Cu4 O2 2.163(4) . ? Cu4 O15 2.253(4) . ? Cu5 N18 1.892(6) . ? Cu5 O15 1.924(4) . ? Cu5 O4 1.979(4) . ? Cu5 N20 2.031(5) . ? Cu5 N75 2.278(5) . ? Cu6 N28 1.880(5) . ? Cu6 O6 1.964(4) . ? Cu6 N76 1.996(5) . ? Cu6 N30 1.997(5) . ? Cu6 O16 2.195(4) . ? Cu7 N78 1.916(5) . ? Cu7 N38 1.963(5) . ? Cu7 O16 2.022(4) . ? Cu7 N80 2.057(5) . ? Cu7 N40 2.342(6) . ? Cu7 O8 2.400(4) . ? Cu8 N68 1.901(6) . ? Cu8 O8 1.943(4) . ? Cu8 O14 1.974(4) . ? Cu8 N70 2.039(5) . ? Cu8 N36 2.271(5) . ? Cu9 N58 1.897(6) . ? Cu9 O12 1.944(4) . ? Cu9 N35 2.003(5) . ? Cu9 N60 2.039(5) . ? Cu9 O7 2.212(4) . ? Cu10 N33 1.905(6) . ? Cu10 N48 1.938(6) . ? Cu10 O7 2.121(4) . ? Cu10 N31 2.140(6) . ? Cu10 O10 2.228(4) . ? Cu10 N50 2.255(5) . ? Cu11 N23 1.819(7) . ? Cu11 O5 1.964(4) . ? Cu11 O10 1.969(4) . ? Cu11 N21 2.032(6) . ? Cu11 N46 2.255(5) . ? Cu12 N13 1.832(6) . ? Cu12 O3 1.966(5) . ? Cu12 N11 2.014(5) . ? Cu12 N45 2.032(5) . ? Cu12 O9 2.152(5) . ? Na1 N15 1.797(12) . ? Na1 N55 1.834(12) . ? Na1 O11 2.251(11) . ? Na1 O3 2.432(11) . ? Na1 C26 2.668(12) . ? Na1 C98 2.699(12) . ? Na1 N16 2.705(12) . ? Na1 N56 2.855(13) . ? Na1 C97 2.865(11) . ? Na1 C25 2.969(12) . ? Na1 Na3 3.223(12) . ? Na1 Na2 3.30(2) . ? Na2 N65 1.67(2) . ? Na2 N16 1.89(2) . ? Na2 O4 2.262(19) . ? Na2 O13 2.31(2) . ? Na2 C116 2.52(2) . ? Na2 C29 2.61(2) . ? Na2 N66 2.69(2) . ? Na2 C30 2.71(2) . ? Na2 C115 2.77(2) . ? Na2 N15 2.93(2) . ? Na2 Na4 3.255(19) . ? Na3 N56 1.712(9) . ? Na3 N25 1.920(9) . ? Na3 O12 2.339(6) . ? Na3 O5 2.417(6) . ? Na3 N55 2.651(9) . ? Na3 C101 2.675(9) . ? Na3 C44 2.791(9) . ? Na3 N26 2.861(8) . ? Na3 C102 2.938(9) . ? Na3 C43 2.989(8) . ? Na3 Na4 3.296(6) . ? Na4 N66 1.778(8) . ? Na4 N26 1.871(8) . ? Na4 O6 2.218(5) . ? Na4 O14 2.340(5) . ? Na4 C119 2.626(8) . ? Na4 C47 2.715(8) . ? Na4 N65 2.758(7) . ? Na4 N25 2.817(7) . ? Na4 C120 2.848(7) . ? Na4 C48 2.866(8) . ? O1 C7 1.287(9) . ? O2 C12 1.327(8) . ? O3 C25 1.255(8) . ? O4 C30 1.250(7) . ? O5 C43 1.286(8) . ? O6 C48 1.280(8) . ? O7 C61 1.299(8) . ? O8 C66 1.290(7) . ? O9 C79 1.281(8) . ? O10 C84 1.298(8) . ? O11 C97 1.281(7) . ? O12 C102 1.298(8) . ? O13 C115 1.262(7) . ? O14 C120 1.304(8) . ? O15 C133 1.323(8) . ? O16 C138 1.306(7) . ? O17 N81 1.206(10) . ? O18 N81 1.261(12) . ? O19 N81 1.189(12) . ? O20 N82 1.324(14) . ? O21 N82 1.257(11) . ? O22 N82 1.180(13) . ? O23 N83 1.203(9) . ? O24 N83 1.187(9) . ? O25 N83 1.297(9) . ? O26 N84 1.196(9) . ? O27 N84 1.273(11) . ? O28 N84 1.256(10) . ? O29 N85 1.197(10) . ? O30 N85 1.199(11) . ? O31 N85 1.279(10) . ? O32 N86 1.334(13) . ? O33 N86 1.138(13) . ? O34 N86 1.227(14) . ? N1 C1 1.308(9) . ? N1 C5 1.347(10) . ? N2 C6 1.365(10) . ? N2 H1 0.8800 . ? N2 H2 0.8800 . ? N3 C6 1.320(8) . ? N3 N4 1.398(8) . ? N4 C7 1.282(9) . ? N5 C8 1.327(9) . ? N5 N6 1.342(7) . ? N6 C11 1.337(8) . ? N7 C12 1.281(8) . ? N7 N8 1.414(7) . ? N8 C13 1.313(8) . ? N9 C13 1.306(9) . ? N9 H3 0.8800 . ? N9 H4 0.8800 . ? N10 C18 1.303(9) . ? N10 C14 1.341(9) . ? N11 C23 1.289(9) . ? N11 C19 1.378(10) . ? N12 C24 1.320(11) . ? N12 H5 0.8800 . ? N12 H6 0.8800 . ? N13 C24 1.319(10) . ? N13 N14 1.436(9) . ? N14 C25 1.279(9) . ? N15 N16 1.383(9) . ? N15 C26 1.405(10) . ? N16 C29 1.398(10) . ? N17 C30 1.340(9) . ? N17 N18 1.389(7) . ? N18 C31 1.313(8) . ? N19 C31 1.334(9) . ? N19 H7 0.8800 . ? N19 H8 0.8800 . ? N20 C36 1.335(8) . ? N20 C32 1.370(9) . ? N21 C41 1.296(10) . ? N21 C37 1.351(9) . ? N22 C42 1.377(13) . ? N22 H9 0.8800 . ? N22 H10 0.8800 . ? N23 C42 1.292(10) . ? N23 N24 1.421(9) . ? N24 C43 1.251(9) . ? N25 C44 1.357(10) . ? N25 N26 1.357(9) . ? N26 C47 1.361(9) . ? N27 C48 1.344(8) . ? N27 N28 1.400(7) . ? N28 C49 1.312(7) . ? N29 C49 1.324(8) . ? N29 H11 0.8800 . ? N29 H12 0.8800 . ? N30 C54 1.326(8) . ? N30 C50 1.368(8) . ? N31 C55 1.329(10) . ? N31 C59 1.334(10) . ? N32 C60 1.287(10) . ? N32 H13 0.8800 . ? N32 H14 0.8800 . ? N33 C60 1.342(8) . ? N33 N34 1.410(7) . ? N34 C61 1.316(8) . ? N35 N36 1.335(6) . ? N35 C62 1.351(7) . ? N36 C65 1.320(7) . ? N37 C66 1.301(8) . ? N37 N38 1.409(7) . ? N38 C67 1.354(8) . ? N39 C67 1.343(8) . ? N39 H15 0.8800 . ? N39 H16 0.8800 . ? N40 C72 1.320(8) . ? N40 C68 1.357(9) . ? N41 C77 1.342(9) . ? N41 C73 1.345(9) . ? N42 C78 1.328(9) . ? N42 H17 0.8800 . ? N42 H18 0.8800 . ? N43 C78 1.322(8) . ? N43 N44 1.405(7) . ? N44 C79 1.307(8) . ? N45 C80 1.332(8) . ? N45 N46 1.332(6) . ? N46 C83 1.323(8) . ? N47 C84 1.283(8) . ? N47 N48 1.416(7) . ? N48 C85 1.306(9) . ? N49 C85 1.306(9) . ? N49 H19 0.8800 . ? N49 H20 0.8800 . ? N50 C86 1.324(9) . ? N50 C90 1.343(8) . ? N51 C95 1.328(9) . ? N51 C91 1.329(9) . ? N52 C96 1.319(10) . ? N52 H21 0.8800 . ? N52 H22 0.8800 . ? N53 C96 1.294(9) . ? N53 N54 1.404(7) . ? N54 C97 1.315(8) . ? N55 C98 1.360(10) . ? N55 N56 1.379(8) . ? N56 C101 1.374(9) . ? N57 C102 1.337(8) . ? N57 N58 1.384(7) . ? N58 C103 1.304(8) . ? N59 C103 1.334(9) . ? N59 H23 0.8800 . ? N59 H24 0.8800 . ? N60 C108 1.330(8) . ? N60 C104 1.338(8) . ? N61 C109 1.353(8) . ? N61 C113 1.360(9) . ? N62 C114 1.319(9) . ? N62 H25 0.8800 . ? N62 H26 0.8800 . ? N63 C114 1.305(8) . ? N63 N64 1.399(7) . ? N64 C115 1.341(8) . ? N65 N66 1.373(8) . ? N65 C116 1.378(10) . ? N66 C119 1.391(10) . ? N67 C120 1.319(8) . ? N67 N68 1.386(7) . ? N68 C121 1.309(8) . ? N69 C121 1.329(9) . ? N69 H27 0.8800 . ? N69 H28 0.8800 . ? N70 C126 1.311(8) . ? N70 C122 1.342(9) . ? N71 C127 1.327(9) . ? N71 C131 1.340(9) . ? N72 C132 1.333(8) . ? N72 H29 0.8800 . ? N72 H30 0.8800 . ? N73 C132 1.306(8) . ? N73 N74 1.394(7) . ? N74 C133 1.295(8) . ? N75 C134 1.319(8) . ? N75 N76 1.355(6) . ? N76 C137 1.343(8) . ? N77 C138 1.313(7) . ? N77 N78 1.393(6) . ? N78 C139 1.324(7) . ? N79 C139 1.324(8) . ? N79 H31 0.8800 . ? N79 H32 0.8800 . ? N80 C144 1.319(8) . ? N80 C140 1.350(9) . ? C1 C2 1.353(12) . ? C1 H33 0.9500 . ? C2 C3 1.378(14) . ? C2 H34 0.9500 . ? C3 C4 1.386(13) . ? C3 H35 0.9500 . ? C4 C5 1.364(10) . ? C4 H36 0.9500 . ? C5 C6 1.497(10) . ? C7 C8 1.497(9) . ? C8 C9 1.405(10) . ? C9 C10 1.321(9) . ? C9 H37 0.9500 . ? C10 C11 1.400(9) . ? C10 H38 0.9500 . ? C11 C12 1.483(9) . ? C13 C14 1.508(9) . ? C14 C15 1.368(10) . ? C15 C16 1.393(12) . ? C15 H39 0.9500 . ? C16 C17 1.387(15) . ? C16 H40 0.9500 . ? C17 C18 1.399(14) . ? C17 H41 0.9500 . ? C18 H42 0.9500 . ? C19 C20 1.366(11) . ? C19 H43 0.9500 . ? C20 C21 1.380(13) . ? C20 H44 0.9500 . ? C21 C22 1.317(12) . ? C21 H45 0.9500 . ? C22 C23 1.406(10) . ? C22 H46 0.9500 . ? C23 C24 1.446(11) . ? C25 C26 1.488(9) . ? C26 C27 1.291(10) . ? C27 C28 1.346(9) . ? C27 H47 0.9500 . ? C28 C29 1.287(10) . ? C28 H48 0.9500 . ? C29 C30 1.463(9) . ? C31 C32 1.477(9) . ? C32 C33 1.364(9) . ? C33 C34 1.333(11) . ? C33 H49 0.9500 . ? C34 C35 1.384(13) . ? C34 H50 0.9500 . ? C35 C36 1.404(11) . ? C35 H51 0.9500 . ? C36 H52 0.9500 . ? C37 C38 1.380(10) . ? C37 H53 0.9500 . ? C38 C39 1.290(13) . ? C38 H54 0.9500 . ? C39 C40 1.427(14) . ? C39 H55 0.9500 . ? C40 C41 1.375(11) . ? C40 H56 0.9500 . ? C41 C42 1.450(12) . ? C43 C44 1.477(9) . ? C44 C45 1.326(10) . ? C45 C46 1.330(10) . ? C45 H57 0.9500 . ? C46 C47 1.318(10) . ? C46 H58 0.9500 . ? C47 C48 1.498(8) . ? C49 C50 1.490(8) . ? C50 C51 1.379(9) . ? C51 C52 1.381(10) . ? C51 H59 0.9500 . ? C52 C53 1.349(10) . ? C52 H60 0.9500 . ? C53 C54 1.404(9) . ? C53 H61 0.9500 . ? C54 H62 0.9500 . ? C55 C56 1.403(14) . ? C55 H63 0.9500 . ? C56 C57 1.347(15) . ? C56 H64 0.9500 . ? C57 C58 1.403(13) . ? C57 H65 0.9500 . ? C58 C59 1.433(10) . ? C58 H66 0.9500 . ? C59 C60 1.489(10) . ? C61 C62 1.495(8) . ? C62 C63 1.376(8) . ? C63 C64 1.359(8) . ? C63 H67 0.9500 . ? C64 C65 1.417(8) . ? C64 H68 0.9500 . ? C65 C66 1.500(8) . ? C67 C68 1.464(9) . ? C68 C69 1.416(10) . ? C69 C70 1.369(10) . ? C69 H69 0.9500 . ? C70 C71 1.350(12) . ? C70 H70 0.9500 . ? C71 C72 1.412(11) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.360(12) . ? C73 H73 0.9500 . ? C74 C75 1.354(13) . ? C74 H74 0.9500 . ? C75 C76 1.384(11) . ? C75 H75 0.9500 . ? C76 C77 1.392(9) . ? C76 H76 0.9500 . ? C77 C78 1.472(9) . ? C79 C80 1.502(8) . ? C80 C81 1.410(9) . ? C81 C82 1.344(8) . ? C81 H77 0.9500 . ? C82 C83 1.397(9) . ? C82 H78 0.9500 . ? C83 C84 1.500(8) . ? C85 C86 1.497(9) . ? C86 C87 1.391(10) . ? C87 C88 1.377(10) . ? C87 H79 0.9500 . ? C88 C89 1.331(11) . ? C88 H80 0.9500 . ? C89 C90 1.349(10) . ? C89 H81 0.9500 . ? C90 H82 0.9500 . ? C91 C92 1.321(11) . ? C91 H83 0.9500 . ? C92 C93 1.355(15) . ? C92 H84 0.9500 . ? C93 C94 1.425(14) . ? C93 H85 0.9500 . ? C94 C95 1.402(10) . ? C94 H86 0.9500 . ? C95 C96 1.492(10) . ? C97 C98 1.509(8) . ? C98 C99 1.324(9) . ? C99 C100 1.328(7) . ? C99 H87 0.9500 . ? C100 C101 1.341(9) . ? C100 H88 0.9500 . ? C101 C102 1.470(8) . ? C103 C104 1.508(9) . ? C104 C105 1.362(9) . ? C105 C106 1.385(11) . ? C105 H89 0.9500 . ? C106 C107 1.344(11) . ? C106 H90 0.9500 . ? C107 C108 1.382(9) . ? C107 H91 0.9500 . ? C108 H92 0.9500 . ? C109 C110 1.376(10) . ? C109 H93 0.9500 . ? C110 C111 1.379(11) . ? C110 H94 0.9500 . ? C111 C112 1.359(10) . ? C111 H95 0.9500 . ? C112 C113 1.372(8) . ? C112 H96 0.9500 . ? C113 C114 1.483(9) . ? C115 C116 1.488(8) . ? C116 C117 1.338(9) . ? C117 C118 1.308(8) . ? C117 H97 0.9500 . ? C118 C119 1.304(9) . ? C118 H98 0.9500 . ? C119 C120 1.465(9) . ? C121 C122 1.498(10) . ? C122 C123 1.379(9) . ? C123 C124 1.358(12) . ? C123 H99 0.9500 . ? C124 C125 1.381(12) . ? C124 H100 0.9500 . ? C125 C126 1.363(10) . ? C125 H101 0.9500 . ? C126 H102 0.9500 . ? C127 C128 1.392(14) . ? C127 H103 0.9500 . ? C128 C129 1.358(15) . ? C128 H104 0.9500 . ? C129 C130 1.376(11) . ? C129 H105 0.9500 . ? C130 C131 1.361(9) . ? C130 H106 0.9500 . ? C131 C132 1.522(8) . ? C133 C134 1.472(8) . ? C134 C135 1.404(9) . ? C135 C136 1.383(8) . ? C135 H107 0.9500 . ? C136 C137 1.385(9) . ? C136 H108 0.9500 . ? C137 C138 1.476(8) . ? C139 C140 1.493(9) . ? C140 C141 1.381(8) . ? C141 C142 1.404(10) . ? C141 H109 0.9500 . ? C142 C143 1.348(11) . ? C142 H110 0.9500 . ? C143 C144 1.383(9) . ? C143 H111 0.9500 . ? C144 H112 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 N3 Cu1 N43 170.7(2) . . ? N3 Cu1 O1 76.1(2) . . ? N43 Cu1 O1 97.2(2) . . ? N3 Cu1 N1 77.9(2) . . ? N43 Cu1 N1 108.8(2) . . ? O1 Cu1 N1 154.0(2) . . ? N3 Cu1 O9 99.0(2) . . ? N43 Cu1 O9 76.0(2) . . ? O1 Cu1 O9 102.86(16) . . ? N1 Cu1 O9 82.11(17) . . ? N3 Cu1 N41 109.4(2) . . ? N43 Cu1 N41 75.9(2) . . ? O1 Cu1 N41 84.37(18) . . ? N1 Cu1 N41 103.5(2) . . ? O9 Cu1 N41 151.6(2) . . ? N53 Cu2 O11 78.8(2) . . ? N53 Cu2 N51 80.7(2) . . ? O11 Cu2 N51 158.4(2) . . ? N53 Cu2 N5 165.6(2) . . ? O11 Cu2 N5 99.67(19) . . ? N51 Cu2 N5 98.5(2) . . ? N53 Cu2 O1 117.6(2) . . ? O11 Cu2 O1 91.53(17) . . ? N51 Cu2 O1 104.01(18) . . ? N5 Cu2 O1 76.63(19) . . ? N63 Cu3 O2 162.5(2) . . ? N63 Cu3 O13 80.4(2) . . ? O2 Cu3 O13 98.13(18) . . ? N63 Cu3 N61 80.2(2) . . ? O2 Cu3 N61 99.4(2) . . ? O13 Cu3 N61 160.3(2) . . ? N63 Cu3 N6 120.5(2) . . ? O2 Cu3 N6 76.67(18) . . ? O13 Cu3 N6 88.37(18) . . ? N61 Cu3 N6 104.34(19) . . ? N8 Cu4 N73 164.1(2) . . ? N8 Cu4 N71 112.3(2) . . ? N73 Cu4 N71 78.5(2) . . ? N8 Cu4 N10 77.8(2) . . ? N73 Cu4 N10 113.2(2) . . ? N71 Cu4 N10 98.3(2) . . ? N8 Cu4 O2 75.6(2) . . ? N73 Cu4 O2 93.4(2) . . ? N71 Cu4 O2 89.03(19) . . ? N10 Cu4 O2 153.3(2) . . ? N8 Cu4 O15 94.9(2) . . ? N73 Cu4 O15 74.60(18) . . ? N71 Cu4 O15 152.7(2) . . ? N10 Cu4 O15 88.60(17) . . ? O2 Cu4 O15 96.57(15) . . ? N18 Cu5 O15 167.0(2) . . ? N18 Cu5 O4 79.2(2) . . ? O15 Cu5 O4 96.84(18) . . ? N18 Cu5 N20 79.9(2) . . ? O15 Cu5 N20 102.0(2) . . ? O4 Cu5 N20 157.9(2) . . ? N18 Cu5 N75 115.4(2) . . ? O15 Cu5 N75 76.94(17) . . ? O4 Cu5 N75 92.32(17) . . ? N20 Cu5 N75 103.16(19) . . ? N28 Cu6 O6 80.50(19) . . ? N28 Cu6 N76 170.7(2) . . ? O6 Cu6 N76 95.79(19) . . ? N28 Cu6 N30 80.5(2) . . ? O6 Cu6 N30 160.0(2) . . ? N76 Cu6 N30 102.0(2) . . ? N28 Cu6 O16 111.28(18) . . ? O6 Cu6 O16 93.10(17) . . ? N76 Cu6 O16 77.35(17) . . ? N30 Cu6 O16 99.59(17) . . ? N78 Cu7 N38 161.0(2) . . ? N78 Cu7 O16 77.83(18) . . ? N38 Cu7 O16 102.13(18) . . ? N78 Cu7 N80 79.7(2) . . ? N38 Cu7 N80 100.25(19) . . ? O16 Cu7 N80 157.24(19) . . ? N78 Cu7 N40 124.4(2) . . ? N38 Cu7 N40 74.5(2) . . ? O16 Cu7 N40 90.60(17) . . ? N80 Cu7 N40 99.34(19) . . ? N78 Cu7 O8 89.40(18) . . ? N38 Cu7 O8 71.94(18) . . ? O16 Cu7 O8 101.92(15) . . ? N80 Cu7 O8 81.14(17) . . ? N40 Cu7 O8 145.93(18) . . ? N68 Cu8 O8 165.43(19) . . ? N68 Cu8 O14 80.0(2) . . ? O8 Cu8 O14 93.71(17) . . ? N68 Cu8 N70 80.5(2) . . ? O8 Cu8 N70 103.1(2) . . ? O14 Cu8 N70 158.7(2) . . ? N68 Cu8 N36 117.0(2) . . ? O8 Cu8 N36 76.85(17) . . ? O14 Cu8 N36 99.71(17) . . ? N70 Cu8 N36 96.78(18) . . ? N58 Cu9 O12 80.02(19) . . ? N58 Cu9 N35 166.42(19) . . ? O12 Cu9 N35 91.71(18) . . ? N58 Cu9 N60 80.8(2) . . ? O12 Cu9 N60 158.9(2) . . ? N35 Cu9 N60 105.3(2) . . ? N58 Cu9 O7 114.58(19) . . ? O12 Cu9 O7 102.52(16) . . ? N35 Cu9 O7 77.58(18) . . ? N60 Cu9 O7 93.38(18) . . ? N33 Cu10 N48 169.3(2) . . ? N33 Cu10 O7 77.58(19) . . ? N48 Cu10 O7 96.47(19) . . ? N33 Cu10 N31 78.4(2) . . ? N48 Cu10 N31 107.4(2) . . ? O7 Cu10 N31 156.0(2) . . ? N33 Cu10 O10 95.58(19) . . ? N48 Cu10 O10 75.43(19) . . ? O7 Cu10 O10 90.74(15) . . ? N31 Cu10 O10 92.41(18) . . ? N33 Cu10 N50 114.2(2) . . ? N48 Cu10 N50 75.0(2) . . ? O7 Cu10 N50 96.38(17) . . ? N31 Cu10 N50 92.7(2) . . ? O10 Cu10 N50 150.2(2) . . ? N23 Cu11 O5 79.8(2) . . ? N23 Cu11 O10 155.6(3) . . ? O5 Cu11 O10 99.8(2) . . ? N23 Cu11 N21 79.8(3) . . ? O5 Cu11 N21 159.3(2) . . ? O10 Cu11 N21 97.1(2) . . ? N23 Cu11 N46 128.7(3) . . ? O5 Cu11 N46 93.28(18) . . ? O10 Cu11 N46 75.63(17) . . ? N21 Cu11 N46 102.5(2) . . ? N13 Cu12 O3 79.2(2) . . ? N13 Cu12 N11 79.5(3) . . ? O3 Cu12 N11 157.5(2) . . ? N13 Cu12 N45 159.6(3) . . ? O3 Cu12 N45 96.3(2) . . ? N11 Cu12 N45 101.1(2) . . ? N13 Cu12 O9 122.1(3) . . ? O3 Cu12 O9 92.6(2) . . ? N11 Cu12 O9 104.9(2) . . ? N45 Cu12 O9 77.69(18) . . ? N15 Na1 N55 173.4(7) . . ? N15 Na1 O11 102.3(6) . . ? N55 Na1 O11 83.6(4) . . ? N15 Na1 O3 79.8(4) . . ? N55 Na1 O3 99.7(5) . . ? O11 Na1 O3 122.3(4) . . ? N15 Na1 C26 29.2(3) . . ? N55 Na1 C26 147.1(6) . . ? O11 Na1 C26 125.9(5) . . ? O3 Na1 C26 54.2(3) . . ? N15 Na1 C98 157.7(6) . . ? N55 Na1 C98 27.3(3) . . ? O11 Na1 C98 56.7(3) . . ? O3 Na1 C98 116.5(4) . . ? C26 Na1 C98 170.7(4) . . ? N15 Na1 N16 27.4(3) . . ? N55 Na1 N16 150.5(6) . . ? O11 Na1 N16 94.8(4) . . ? O3 Na1 N16 105.9(4) . . ? C26 Na1 N16 52.1(3) . . ? C98 Na1 N16 136.9(4) . . ? N15 Na1 N56 150.3(6) . . ? N55 Na1 N56 23.4(3) . . ? O11 Na1 N56 106.5(4) . . ? O3 Na1 N56 90.8(4) . . ? C26 Na1 N56 126.4(4) . . ? C98 Na1 N56 49.8(3) . . ? N16 Na1 N56 140.1(4) . . ? N15 Na1 C97 127.8(6) . . ? N55 Na1 C97 58.0(4) . . ? O11 Na1 C97 25.57(19) . . ? O3 Na1 C97 122.1(4) . . ? C26 Na1 C97 150.0(5) . . ? C98 Na1 C97 31.3(2) . . ? N16 Na1 C97 116.6(4) . . ? N56 Na1 C97 81.0(3) . . ? N15 Na1 C25 55.9(4) . . ? N55 Na1 C25 122.8(5) . . ? O11 Na1 C25 126.6(5) . . ? O3 Na1 C25 24.36(19) . . ? C26 Na1 C25 30.0(2) . . ? C98 Na1 C25 140.7(4) . . ? N16 Na1 C25 81.5(3) . . ? N56 Na1 C25 109.6(4) . . ? C97 Na1 C25 138.3(4) . . ? N15 Na1 Na3 118.3(5) . . ? N55 Na1 Na3 55.4(4) . . ? O11 Na1 Na3 137.7(4) . . ? O3 Na1 Na3 78.7(3) . . ? C26 Na1 Na3 96.3(4) . . ? C98 Na1 Na3 81.3(3) . . ? N16 Na1 Na3 115.4(4) . . ? N56 Na1 Na3 32.0(2) . . ? C97 Na1 Na3 112.6(4) . . ? C25 Na1 Na3 88.3(3) . . ? N15 Na1 Na2 62.2(5) . . ? N55 Na1 Na2 116.2(6) . . ? O11 Na1 Na2 82.9(5) . . ? O3 Na1 Na2 138.9(5) . . ? C26 Na1 Na2 84.9(5) . . ? C98 Na1 Na2 104.4(5) . . ? N16 Na1 Na2 34.9(4) . . ? N56 Na1 Na2 114.1(5) . . ? C97 Na1 Na2 94.8(5) . . ? C25 Na1 Na2 114.9(5) . . ? Na3 Na1 Na2 104.9(4) . . ? N65 Na2 N16 145.3(11) . . ? N65 Na2 O4 127.4(12) . . ? N16 Na2 O4 81.3(8) . . ? N65 Na2 O13 84.1(9) . . ? N16 Na2 O13 115.9(10) . . ? O4 Na2 O13 94.5(7) . . ? N65 Na2 C116 30.6(5) . . ? N16 Na2 C116 138.6(10) . . ? O4 Na2 C116 137.0(9) . . ? O13 Na2 C116 58.1(5) . . ? N65 Na2 C29 144.7(11) . . ? N16 Na2 C29 31.3(4) . . ? O4 Na2 C29 57.3(5) . . ? O13 Na2 C29 131.1(8) . . ? C116 Na2 C29 165.5(8) . . ? N65 Na2 N66 24.8(4) . . ? N16 Na2 N66 126.3(9) . . ? O4 Na2 N66 123.8(9) . . ? O13 Na2 N66 108.8(8) . . ? C116 Na2 N66 53.1(4) . . ? C29 Na2 N66 120.0(8) . . ? N65 Na2 C30 136.1(11) . . ? N16 Na2 C30 60.8(6) . . ? O4 Na2 C30 27.3(3) . . ? O13 Na2 C30 118.8(7) . . ? C116 Na2 C30 160.5(9) . . ? C29 Na2 C30 31.9(3) . . ? N66 Na2 C30 119.4(8) . . ? N65 Na2 C115 61.1(7) . . ? N16 Na2 C115 126.6(10) . . ? O4 Na2 C115 119.0(7) . . ? O13 Na2 C115 26.8(3) . . ? C116 Na2 C115 32.2(3) . . ? C29 Na2 C115 153.1(9) . . ? N66 Na2 C115 85.0(6) . . ? C30 Na2 C115 145.1(7) . . ? N65 Na2 N15 124.8(9) . . ? N16 Na2 N15 22.2(4) . . ? O4 Na2 N15 103.5(8) . . ? O13 Na2 N15 114.6(8) . . ? C116 Na2 N15 117.6(7) . . ? C29 Na2 N15 50.2(4) . . ? N66 Na2 N15 110.8(6) . . ? C30 Na2 N15 81.6(6) . . ? C115 Na2 N15 114.5(7) . . ? N65 Na2 Na4 57.9(6) . . ? N16 Na2 Na4 97.0(7) . . ? O4 Na2 Na4 109.7(7) . . ? O13 Na2 Na4 141.9(8) . . ? C116 Na2 Na4 84.7(5) . . ? C29 Na2 Na4 87.0(6) . . ? N66 Na2 Na4 33.1(3) . . ? C30 Na2 Na4 93.3(6) . . ? C115 Na2 Na4 116.9(6) . . ? N15 Na2 Na4 88.4(5) . . ? N65 Na2 Na1 92.9(8) . . ? N16 Na2 Na1 55.1(6) . . ? O4 Na2 Na1 136.2(9) . . ? O13 Na2 Na1 107.4(7) . . ? C116 Na2 Na1 86.2(6) . . ? C29 Na2 Na1 80.2(6) . . ? N66 Na2 Na1 84.7(5) . . ? C30 Na2 Na1 112.0(7) . . ? C115 Na2 Na1 93.5(6) . . ? N15 Na2 Na1 32.9(3) . . ? Na4 Na2 Na1 75.1(4) . . ? N56 Na3 N25 160.1(4) . . ? N56 Na3 O12 81.3(3) . . ? N25 Na3 O12 111.0(4) . . ? N56 Na3 O5 120.3(4) . . ? N25 Na3 O5 75.5(3) . . ? O12 Na3 O5 94.9(2) . . ? N56 Na3 N55 27.4(3) . . ? N25 Na3 N55 135.1(4) . . ? O12 Na3 N55 107.9(3) . . ? O5 Na3 N55 122.6(3) . . ? N56 Na3 C101 26.5(3) . . ? N25 Na3 C101 156.9(4) . . ? O12 Na3 C101 55.1(2) . . ? O5 Na3 C101 120.9(3) . . ? N55 Na3 C101 52.7(2) . . ? N56 Na3 C44 156.7(4) . . ? N25 Na3 C44 26.0(3) . . ? O12 Na3 C44 119.7(3) . . ? O5 Na3 C44 52.6(2) . . ? N55 Na3 C44 132.3(3) . . ? C101 Na3 C44 172.7(3) . . ? N56 Na3 N26 138.2(3) . . ? N25 Na3 N26 24.1(2) . . ? O12 Na3 N26 108.9(3) . . ? O5 Na3 N26 99.6(2) . . ? N55 Na3 N26 119.8(3) . . ? C101 Na3 N26 136.0(3) . . ? C44 Na3 N26 48.8(2) . . ? N56 Na3 C102 55.9(3) . . ? N25 Na3 C102 135.0(4) . . ? O12 Na3 C102 25.38(15) . . ? O5 Na3 C102 107.0(2) . . ? N55 Na3 C102 82.6(2) . . ? C101 Na3 C102 29.89(18) . . ? C44 Na3 C102 144.5(3) . . ? N26 Na3 C102 126.5(3) . . ? N56 Na3 C43 136.3(4) . . ? N25 Na3 C43 54.6(3) . . ? O12 Na3 C43 113.5(2) . . ? O5 Na3 C43 24.75(17) . . ? N55 Na3 C43 125.5(3) . . ? C101 Na3 C43 144.9(3) . . ? C44 Na3 C43 29.36(19) . . ? N26 Na3 C43 78.1(2) . . ? C102 Na3 C43 130.4(2) . . ? N56 Na3 Na1 62.1(3) . . ? N25 Na3 Na1 101.4(4) . . ? O12 Na3 Na1 141.0(3) . . ? O5 Na3 Na1 114.3(3) . . ? N55 Na3 Na1 34.7(2) . . ? C101 Na3 Na1 86.8(3) . . ? C44 Na3 Na1 98.9(3) . . ? N26 Na3 Na1 91.8(3) . . ? C102 Na3 Na1 116.6(3) . . ? C43 Na3 Na1 102.8(3) . . ? N56 Na3 Na4 104.3(3) . . ? N25 Na3 Na4 58.5(2) . . ? O12 Na3 Na4 103.0(2) . . ? O5 Na3 Na4 133.9(2) . . ? N55 Na3 Na4 91.7(2) . . ? C101 Na3 Na4 103.9(2) . . ? C44 Na3 Na4 81.98(19) . . ? N26 Na3 Na4 34.48(16) . . ? C102 Na3 Na4 107.11(19) . . ? C43 Na3 Na4 111.2(2) . . ? Na1 Na3 Na4 75.56(19) . . ? N66 Na4 N26 166.0(4) . . ? N66 Na4 O6 110.5(3) . . ? N26 Na4 O6 82.4(3) . . ? N66 Na4 O14 80.1(3) . . ? N26 Na4 O14 101.2(3) . . ? O6 Na4 O14 109.5(2) . . ? N66 Na4 C119 29.6(3) . . ? N26 Na4 C119 142.1(3) . . ? O6 Na4 C119 131.6(2) . . ? O14 Na4 C119 56.37(18) . . ? N66 Na4 C47 161.7(3) . . ? N26 Na4 C47 27.4(2) . . ? O6 Na4 C47 56.09(18) . . ? O14 Na4 C47 115.1(2) . . ? C119 Na4 C47 168.7(2) . . ? N66 Na4 N65 25.1(3) . . ? N26 Na4 N65 150.5(3) . . ? O6 Na4 N65 100.7(2) . . ? O14 Na4 N65 105.2(2) . . ? C119 Na4 N65 52.4(2) . . ? C47 Na4 N65 138.2(2) . . ? N66 Na4 N25 141.6(4) . . ? N26 Na4 N25 24.5(2) . . ? O6 Na4 N25 106.1(2) . . ? O14 Na4 N25 98.3(2) . . ? C119 Na4 N25 121.1(2) . . ? C47 Na4 N25 50.09(19) . . ? N65 Na4 N25 135.7(3) . . ? N66 Na4 C120 58.2(3) . . ? N26 Na4 C120 118.4(3) . . ? O6 Na4 C120 129.1(2) . . ? O14 Na4 C120 26.91(16) . . ? C119 Na4 C120 30.71(19) . . ? C47 Na4 C120 139.2(2) . . ? N65 Na4 C120 82.6(2) . . ? N25 Na4 C120 105.6(2) . . ? N66 Na4 C48 135.5(3) . . ? N26 Na4 C48 57.1(3) . . ? O6 Na4 C48 25.30(16) . . ? O14 Na4 C48 112.6(2) . . ? C119 Na4 C48 155.1(2) . . ? C47 Na4 C48 31.00(18) . . ? N65 Na4 C48 121.5(2) . . ? N25 Na4 C48 80.9(2) . . ? C120 Na4 C48 138.8(2) . . ? N66 Na4 Na2 55.9(4) . . ? N26 Na4 Na2 122.0(5) . . ? O6 Na4 Na2 86.3(4) . . ? O14 Na4 Na2 135.9(4) . . ? C119 Na4 Na2 82.0(4) . . ? C47 Na4 Na2 107.9(4) . . ? N65 Na4 Na2 30.8(4) . . ? N25 Na4 Na2 117.0(4) . . ? C120 Na4 Na2 112.7(4) . . ? C48 Na4 Na2 99.0(4) . . ? N66 Na4 Na3 106.3(3) . . ? N26 Na4 Na3 59.9(2) . . ? O6 Na4 Na3 140.9(2) . . ? O14 Na4 Na3 89.10(17) . . ? C119 Na4 Na3 87.43(19) . . ? C47 Na4 Na3 85.01(18) . . ? N65 Na4 Na3 107.3(2) . . ? N25 Na4 Na3 35.52(17) . . ? C120 Na4 Na3 81.88(17) . . ? C48 Na4 Na3 116.00(18) . . ? Na2 Na4 Na3 104.3(4) . . ? C7 O1 Cu1 107.2(4) . . ? C7 O1 Cu2 113.2(4) . . ? Cu1 O1 Cu2 139.4(2) . . ? C12 O2 Cu3 120.4(4) . . ? C12 O2 Cu4 107.8(4) . . ? Cu3 O2 Cu4 128.4(2) . . ? C25 O3 Cu12 111.8(4) . . ? C25 O3 Na1 102.6(5) . . ? Cu12 O3 Na1 141.4(3) . . ? C30 O4 Cu5 111.9(4) . . ? C30 O4 Na2 96.6(6) . . ? Cu5 O4 Na2 134.9(6) . . ? C43 O5 Cu11 109.2(4) . . ? C43 O5 Na3 103.4(4) . . ? Cu11 O5 Na3 137.5(3) . . ? C48 O6 Cu6 108.9(4) . . ? C48 O6 Na4 106.9(4) . . ? Cu6 O6 Na4 140.4(2) . . ? C61 O7 Cu10 106.8(4) . . ? C61 O7 Cu9 111.1(3) . . ? Cu10 O7 Cu9 140.2(2) . . ? C66 O8 Cu8 119.7(4) . . ? C66 O8 Cu7 105.2(4) . . ? Cu8 O8 Cu7 131.34(19) . . ? C79 O9 Cu12 113.5(4) . . ? C79 O9 Cu1 105.7(4) . . ? Cu12 O9 Cu1 140.2(2) . . ? C84 O10 Cu11 121.8(4) . . ? C84 O10 Cu10 106.3(4) . . ? Cu11 O10 Cu10 130.6(2) . . ? C97 O11 Cu2 110.0(4) . . ? C97 O11 Na1 105.1(4) . . ? Cu2 O11 Na1 141.6(4) . . ? C102 O12 Cu9 110.6(4) . . ? C102 O12 Na3 104.1(4) . . ? Cu9 O12 Na3 144.2(2) . . ? C115 O13 Cu3 110.4(4) . . ? C115 O13 Na2 97.5(6) . . ? Cu3 O13 Na2 144.9(6) . . ? C120 O14 Cu8 109.3(4) . . ? C120 O14 Na4 98.8(4) . . ? Cu8 O14 Na4 146.0(2) . . ? C133 O15 Cu5 119.6(3) . . ? C133 O15 Cu4 106.9(3) . . ? Cu5 O15 Cu4 130.9(2) . . ? C138 O16 Cu7 109.4(3) . . ? C138 O16 Cu6 112.0(3) . . ? Cu7 O16 Cu6 138.3(2) . . ? C1 N1 C5 117.2(6) . . ? C1 N1 Cu1 130.5(6) . . ? C5 N1 Cu1 111.9(4) . . ? C6 N2 H1 120.0 . . ? C6 N2 H2 120.0 . . ? H1 N2 H2 120.0 . . ? C6 N3 N4 116.3(6) . . ? C6 N3 Cu1 121.1(5) . . ? N4 N3 Cu1 121.6(4) . . ? C7 N4 N3 107.9(6) . . ? C8 N5 N6 120.7(6) . . ? C8 N5 Cu2 118.8(4) . . ? N6 N5 Cu2 120.5(4) . . ? C11 N6 N5 118.8(5) . . ? C11 N6 Cu3 112.0(4) . . ? N5 N6 Cu3 128.6(4) . . ? C12 N7 N8 108.9(6) . . ? C13 N8 N7 115.4(6) . . ? C13 N8 Cu4 120.8(5) . . ? N7 N8 Cu4 120.8(4) . . ? C13 N9 H3 120.0 . . ? C13 N9 H4 120.0 . . ? H3 N9 H4 120.0 . . ? C18 N10 C14 118.9(7) . . ? C18 N10 Cu4 128.7(6) . . ? C14 N10 Cu4 112.4(4) . . ? C23 N11 C19 119.9(6) . . ? C23 N11 Cu12 113.9(5) . . ? C19 N11 Cu12 126.1(6) . . ? C24 N12 H5 120.0 . . ? C24 N12 H6 120.0 . . ? H5 N12 H6 120.0 . . ? C24 N13 N14 122.4(7) . . ? C24 N13 Cu12 120.2(6) . . ? N14 N13 Cu12 116.7(4) . . ? C25 N14 N13 107.4(7) . . ? N16 N15 C26 115.7(7) . . ? N16 N15 Na1 116.0(6) . . ? C26 N15 Na1 112.3(6) . . ? N16 N15 Na2 31.1(5) . . ? C26 N15 Na2 135.5(7) . . ? Na1 N15 Na2 84.9(5) . . ? N15 N16 C29 116.9(7) . . ? N15 N16 Na2 126.7(8) . . ? C29 N16 Na2 104.2(8) . . ? N15 N16 Na1 36.7(4) . . ? C29 N16 Na1 136.6(6) . . ? Na2 N16 Na1 90.0(7) . . ? C30 N17 N18 107.9(5) . . ? C31 N18 N17 121.4(6) . . ? C31 N18 Cu5 121.2(4) . . ? N17 N18 Cu5 117.4(4) . . ? C31 N19 H7 120.0 . . ? C31 N19 H8 120.0 . . ? H7 N19 H8 120.0 . . ? C36 N20 C32 119.2(6) . . ? C36 N20 Cu5 127.6(6) . . ? C32 N20 Cu5 113.1(4) . . ? C41 N21 C37 120.9(7) . . ? C41 N21 Cu11 112.7(5) . . ? C37 N21 Cu11 126.0(6) . . ? C42 N22 H9 120.0 . . ? C42 N22 H10 120.0 . . ? H9 N22 H10 120.0 . . ? C42 N23 N24 121.0(7) . . ? C42 N23 Cu11 120.5(6) . . ? N24 N23 Cu11 118.5(5) . . ? C43 N24 N23 106.6(7) . . ? C44 N25 N26 118.8(7) . . ? C44 N25 Na3 115.8(5) . . ? N26 N25 Na3 120.7(5) . . ? C44 N25 Na4 145.5(6) . . ? N26 N25 Na4 34.8(4) . . ? Na3 N25 Na4 86.0(3) . . ? N25 N26 C47 119.1(7) . . ? N25 N26 Na4 120.7(5) . . ? C47 N26 Na4 113.3(5) . . ? N25 N26 Na3 35.2(4) . . ? C47 N26 Na3 148.5(6) . . ? Na4 N26 Na3 85.6(3) . . ? C48 N27 N28 104.6(5) . . ? C49 N28 N27 119.7(5) . . ? C49 N28 Cu6 121.4(4) . . ? N27 N28 Cu6 118.9(4) . . ? C49 N29 H11 120.0 . . ? C49 N29 H12 120.0 . . ? H11 N29 H12 120.0 . . ? C54 N30 C50 118.1(6) . . ? C54 N30 Cu6 128.3(5) . . ? C50 N30 Cu6 113.5(4) . . ? C55 N31 C59 119.4(7) . . ? C55 N31 Cu10 129.6(7) . . ? C59 N31 Cu10 110.9(5) . . ? C60 N32 H13 120.0 . . ? C60 N32 H14 120.0 . . ? H13 N32 H14 120.0 . . ? C60 N33 N34 115.0(6) . . ? C60 N33 Cu10 122.6(5) . . ? N34 N33 Cu10 120.4(4) . . ? C61 N34 N33 106.8(6) . . ? N36 N35 C62 121.1(5) . . ? N36 N35 Cu9 119.4(4) . . ? C62 N35 Cu9 119.2(4) . . ? C65 N36 N35 118.8(5) . . ? C65 N36 Cu8 110.1(4) . . ? N35 N36 Cu8 131.0(4) . . ? C66 N37 N38 110.2(5) . . ? C67 N38 N37 111.3(5) . . ? C67 N38 Cu7 123.9(4) . . ? N37 N38 Cu7 124.7(4) . . ? C67 N39 H15 120.0 . . ? C67 N39 H16 120.0 . . ? H15 N39 H16 120.0 . . ? C72 N40 C68 117.6(6) . . ? C72 N40 Cu7 131.5(5) . . ? C68 N40 Cu7 110.9(4) . . ? C77 N41 C73 118.4(6) . . ? C77 N41 Cu1 111.2(4) . . ? C73 N41 Cu1 129.6(6) . . ? C78 N42 H17 120.0 . . ? C78 N42 H18 120.0 . . ? H17 N42 H18 120.0 . . ? C78 N43 N44 114.0(6) . . ? C78 N43 Cu1 123.2(4) . . ? N44 N43 Cu1 121.6(4) . . ? C79 N44 N43 108.3(5) . . ? C80 N45 N46 120.4(5) . . ? C80 N45 Cu12 117.5(4) . . ? N46 N45 Cu12 122.1(4) . . ? C83 N46 N45 119.2(5) . . ? C83 N46 Cu11 112.0(4) . . ? N45 N46 Cu11 128.0(4) . . ? C84 N47 N48 109.4(6) . . ? C85 N48 N47 113.8(6) . . ? C85 N48 Cu10 124.3(5) . . ? N47 N48 Cu10 120.9(4) . . ? C85 N49 H19 120.0 . . ? C85 N49 H20 120.0 . . ? H19 N49 H20 120.0 . . ? C86 N50 C90 118.7(6) . . ? C86 N50 Cu10 112.0(4) . . ? C90 N50 Cu10 129.4(6) . . ? C95 N51 C91 118.2(6) . . ? C95 N51 Cu2 112.1(4) . . ? C91 N51 Cu2 129.6(6) . . ? C96 N52 H21 120.0 . . ? C96 N52 H22 120.0 . . ? H21 N52 H22 120.0 . . ? C96 N53 N54 119.8(6) . . ? C96 N53 Cu2 120.2(5) . . ? N54 N53 Cu2 119.9(4) . . ? C97 N54 N53 104.6(5) . . ? C98 N55 N56 117.7(7) . . ? C98 N55 Na1 114.5(6) . . ? N56 N55 Na1 124.8(6) . . ? C98 N55 Na3 148.8(5) . . ? N56 N55 Na3 34.9(4) . . ? Na1 N55 Na3 89.9(4) . . ? C101 N56 N55 118.6(7) . . ? C101 N56 Na3 119.8(5) . . ? N55 N56 Na3 117.7(6) . . ? C101 N56 Na1 146.6(5) . . ? N55 N56 Na1 31.8(4) . . ? Na3 N56 Na1 85.9(4) . . ? C102 N57 N58 105.9(5) . . ? C103 N58 N57 120.6(6) . . ? C103 N58 Cu9 120.0(5) . . ? N57 N58 Cu9 118.8(4) . . ? C103 N59 H23 120.0 . . ? C103 N59 H24 120.0 . . ? H23 N59 H24 120.0 . . ? C108 N60 C104 119.4(6) . . ? C108 N60 Cu9 128.1(5) . . ? C104 N60 Cu9 112.2(4) . . ? C109 N61 C113 118.1(6) . . ? C109 N61 Cu3 128.5(5) . . ? C113 N61 Cu3 113.3(4) . . ? C114 N62 H25 120.0 . . ? C114 N62 H26 120.0 . . ? H25 N62 H26 120.0 . . ? C114 N63 N64 120.0(6) . . ? C114 N63 Cu3 121.6(5) . . ? N64 N63 Cu3 118.3(4) . . ? C115 N64 N63 105.7(5) . . ? N66 N65 C116 116.3(7) . . ? N66 N65 Na2 124.6(9) . . ? C116 N65 Na2 111.4(9) . . ? N66 N65 Na4 33.3(4) . . ? C116 N65 Na4 141.1(5) . . ? Na2 N65 Na4 91.3(7) . . ? N65 N66 C119 119.0(7) . . ? N65 N66 Na4 121.6(6) . . ? C119 N66 Na4 111.3(5) . . ? N65 N66 Na2 30.6(6) . . ? C119 N66 Na2 142.2(7) . . ? Na4 N66 Na2 91.0(5) . . ? C120 N67 N68 107.0(5) . . ? C121 N68 N67 120.8(6) . . ? C121 N68 Cu8 119.9(5) . . ? N67 N68 Cu8 118.2(4) . . ? C121 N69 H27 120.0 . . ? C121 N69 H28 120.0 . . ? H27 N69 H28 120.0 . . ? C126 N70 C122 118.9(6) . . ? C126 N70 Cu8 127.9(5) . . ? C122 N70 Cu8 112.7(4) . . ? C127 N71 C131 115.8(7) . . ? C127 N71 Cu4 131.4(6) . . ? C131 N71 Cu4 112.5(4) . . ? C132 N72 H29 120.0 . . ? C132 N72 H30 120.0 . . ? H29 N72 H30 120.0 . . ? C132 N73 N74 116.8(6) . . ? C132 N73 Cu4 118.9(4) . . ? N74 N73 Cu4 121.9(4) . . ? C133 N74 N73 110.8(6) . . ? C134 N75 N76 119.8(5) . . ? C134 N75 Cu5 110.5(4) . . ? N76 N75 Cu5 129.6(4) . . ? C137 N76 N75 121.2(5) . . ? C137 N76 Cu6 118.8(4) . . ? N75 N76 Cu6 119.9(4) . . ? C138 N77 N78 105.3(5) . . ? C139 N78 N77 118.0(5) . . ? C139 N78 Cu7 118.6(4) . . ? N77 N78 Cu7 120.7(4) . . ? C139 N79 H31 120.0 . . ? C139 N79 H32 120.0 . . ? H31 N79 H32 120.0 . . ? C144 N80 C140 118.3(5) . . ? C144 N80 Cu7 129.0(5) . . ? C140 N80 Cu7 112.5(4) . . ? O19 N81 O17 120.1(13) . . ? O19 N81 O18 123.9(12) . . ? O17 N81 O18 116.0(12) . . ? O22 N82 O21 125.1(14) . . ? O22 N82 O20 121.4(11) . . ? O21 N82 O20 113.5(13) . . ? O24 N83 O23 122.2(9) . . ? O24 N83 O25 120.9(9) . . ? O23 N83 O25 116.5(8) . . ? O26 N84 O28 128.2(10) . . ? O26 N84 O27 114.6(11) . . ? O28 N84 O27 111.1(11) . . ? O29 N85 O30 111.8(11) . . ? O29 N85 O31 124.6(12) . . ? O30 N85 O31 117.6(11) . . ? O33 N86 O34 105.8(16) . . ? O33 N86 O32 135.8(18) . . ? O34 N86 O32 117.6(16) . . ? N1 C1 C2 124.1(9) . . ? N1 C1 H33 118.0 . . ? C2 C1 H33 118.0 . . ? C1 C2 C3 118.3(9) . . ? C1 C2 H34 120.8 . . ? C3 C2 H34 120.8 . . ? C2 C3 C4 119.7(8) . . ? C2 C3 H35 120.2 . . ? C4 C3 H35 120.2 . . ? C5 C4 C3 116.7(9) . . ? C5 C4 H36 121.6 . . ? C3 C4 H36 121.6 . . ? N1 C5 C4 124.0(7) . . ? N1 C5 C6 112.7(6) . . ? C4 C5 C6 123.3(8) . . ? N3 C6 N2 123.1(7) . . ? N3 C6 C5 115.2(7) . . ? N2 C6 C5 121.7(6) . . ? N4 C7 O1 127.1(6) . . ? N4 C7 C8 115.8(7) . . ? O1 C7 C8 117.0(6) . . ? N5 C8 C9 121.3(6) . . ? N5 C8 C7 114.1(6) . . ? C9 C8 C7 124.5(7) . . ? C10 C9 C8 118.3(7) . . ? C10 C9 H37 120.9 . . ? C8 C9 H37 120.9 . . ? C9 C10 C11 119.0(7) . . ? C9 C10 H38 120.5 . . ? C11 C10 H38 120.5 . . ? N6 C11 C10 121.8(6) . . ? N6 C11 C12 113.5(6) . . ? C10 C11 C12 124.7(6) . . ? N7 C12 O2 125.3(6) . . ? N7 C12 C11 118.0(6) . . ? O2 C12 C11 116.7(6) . . ? N9 C13 N8 125.6(6) . . ? N9 C13 C14 121.5(6) . . ? N8 C13 C14 112.8(6) . . ? N10 C14 C15 123.3(7) . . ? N10 C14 C13 114.0(6) . . ? C15 C14 C13 122.6(8) . . ? C14 C15 C16 117.6(9) . . ? C14 C15 H39 121.2 . . ? C16 C15 H39 121.2 . . ? C17 C16 C15 119.7(9) . . ? C17 C16 H40 120.2 . . ? C15 C16 H40 120.2 . . ? C16 C17 C18 117.4(8) . . ? C16 C17 H41 121.3 . . ? C18 C17 H41 121.3 . . ? N10 C18 C17 123.0(10) . . ? N10 C18 H42 118.5 . . ? C17 C18 H42 118.5 . . ? C20 C19 N11 119.6(9) . . ? C20 C19 H43 120.2 . . ? N11 C19 H43 120.2 . . ? C19 C20 C21 119.6(9) . . ? C19 C20 H44 120.2 . . ? C21 C20 H44 120.2 . . ? C22 C21 C20 119.2(8) . . ? C22 C21 H45 120.4 . . ? C20 C21 H45 120.4 . . ? C21 C22 C23 119.9(9) . . ? C21 C22 H46 120.1 . . ? C23 C22 H46 120.1 . . ? N11 C23 C22 120.9(7) . . ? N11 C23 C24 113.7(7) . . ? C22 C23 C24 124.4(8) . . ? N13 C24 N12 126.8(9) . . ? N13 C24 C23 111.6(7) . . ? N12 C24 C23 121.5(8) . . ? O3 C25 N14 123.3(7) . . ? O3 C25 C26 116.2(6) . . ? N14 C25 C26 119.9(7) . . ? O3 C25 Na1 53.1(4) . . ? N14 C25 Na1 165.1(7) . . ? C26 C25 Na1 63.7(4) . . ? C27 C26 N15 124.0(6) . . ? C27 C26 C25 119.4(7) . . ? N15 C26 C25 116.6(7) . . ? C27 C26 Na1 143.6(6) . . ? N15 C26 Na1 38.6(4) . . ? C25 C26 Na1 86.3(5) . . ? C26 C27 C28 119.9(7) . . ? C26 C27 H47 120.1 . . ? C28 C27 H47 120.1 . . ? C29 C28 C27 119.6(7) . . ? C29 C28 H48 120.2 . . ? C27 C28 H48 120.2 . . ? C28 C29 N16 123.9(7) . . ? C28 C29 C30 119.7(7) . . ? N16 C29 C30 116.3(6) . . ? C28 C29 Na2 152.1(7) . . ? N16 C29 Na2 44.5(6) . . ? C30 C29 Na2 77.8(6) . . ? O4 C30 N17 123.2(6) . . ? O4 C30 C29 120.2(6) . . ? N17 C30 C29 116.6(6) . . ? O4 C30 Na2 56.1(5) . . ? N17 C30 Na2 153.2(6) . . ? C29 C30 Na2 70.4(6) . . ? N18 C31 N19 126.8(6) . . ? N18 C31 C32 112.1(6) . . ? N19 C31 C32 121.1(7) . . ? C33 C32 N20 121.3(6) . . ? C33 C32 C31 125.1(7) . . ? N20 C32 C31 113.7(6) . . ? C34 C33 C32 120.7(8) . . ? C34 C33 H49 119.6 . . ? C32 C33 H49 119.6 . . ? C33 C34 C35 119.0(8) . . ? C33 C34 H50 120.5 . . ? C35 C34 H50 120.5 . . ? C34 C35 C36 119.8(8) . . ? C34 C35 H51 120.1 . . ? C36 C35 H51 120.1 . . ? N20 C36 C35 119.8(8) . . ? N20 C36 H52 120.1 . . ? C35 C36 H52 120.1 . . ? N21 C37 C38 119.7(9) . . ? N21 C37 H53 120.1 . . ? C38 C37 H53 120.1 . . ? C39 C38 C37 121.0(9) . . ? C39 C38 H54 119.5 . . ? C37 C38 H54 119.5 . . ? C38 C39 C40 118.1(8) . . ? C38 C39 H55 121.0 . . ? C40 C39 H55 121.0 . . ? C41 C40 C39 118.7(10) . . ? C41 C40 H56 120.7 . . ? C39 C40 H56 120.7 . . ? N21 C41 C40 120.0(8) . . ? N21 C41 C42 113.3(7) . . ? C40 C41 C42 126.2(9) . . ? N23 C42 N22 123.1(9) . . ? N23 C42 C41 113.2(8) . . ? N22 C42 C41 123.1(8) . . ? N24 C43 O5 125.7(6) . . ? N24 C43 C44 119.5(7) . . ? O5 C43 C44 114.8(6) . . ? N24 C43 Na3 157.8(6) . . ? O5 C43 Na3 51.9(3) . . ? C44 C43 Na3 67.9(4) . . ? C45 C44 N25 120.6(7) . . ? C45 C44 C43 120.2(7) . . ? N25 C44 C43 119.1(6) . . ? C45 C44 Na3 152.6(6) . . ? N25 C44 Na3 38.3(4) . . ? C43 C44 Na3 82.8(4) . . ? C44 C45 C46 120.3(8) . . ? C44 C45 H57 119.8 . . ? C46 C45 H57 119.8 . . ? C47 C46 C45 120.7(8) . . ? C47 C46 H58 119.7 . . ? C45 C46 H58 119.7 . . ? C46 C47 N26 120.4(6) . . ? C46 C47 C48 123.6(6) . . ? N26 C47 C48 116.0(6) . . ? C46 C47 Na4 151.8(6) . . ? N26 C47 Na4 39.3(4) . . ? C48 C47 Na4 80.1(4) . . ? O6 C48 N27 126.8(6) . . ? O6 C48 C47 116.1(6) . . ? N27 C48 C47 117.1(6) . . ? O6 C48 Na4 47.8(3) . . ? N27 C48 Na4 170.1(5) . . ? C47 C48 Na4 68.9(4) . . ? N28 C49 N29 126.7(6) . . ? N28 C49 C50 111.0(5) . . ? N29 C49 C50 122.2(5) . . ? N30 C50 C51 121.5(6) . . ? N30 C50 C49 113.5(5) . . ? C51 C50 C49 125.0(6) . . ? C50 C51 C52 120.0(7) . . ? C50 C51 H59 120.0 . . ? C52 C51 H59 120.0 . . ? C53 C52 C51 118.3(7) . . ? C53 C52 H60 120.9 . . ? C51 C52 H60 120.9 . . ? C52 C53 C54 120.3(7) . . ? C52 C53 H61 119.8 . . ? C54 C53 H61 119.8 . . ? N30 C54 C53 121.8(7) . . ? N30 C54 H62 119.1 . . ? C53 C54 H62 119.1 . . ? N31 C55 C56 120.8(10) . . ? N31 C55 H63 119.6 . . ? C56 C55 H63 119.6 . . ? C57 C56 C55 120.1(9) . . ? C57 C56 H64 119.9 . . ? C55 C56 H64 119.9 . . ? C56 C57 C58 121.5(9) . . ? C56 C57 H65 119.2 . . ? C58 C57 H65 119.2 . . ? C57 C58 C59 114.3(9) . . ? C57 C58 H66 122.8 . . ? C59 C58 H66 122.8 . . ? N31 C59 C58 123.8(8) . . ? N31 C59 C60 117.1(6) . . ? C58 C59 C60 118.9(8) . . ? N32 C60 N33 124.3(7) . . ? N32 C60 C59 125.9(6) . . ? N33 C60 C59 109.9(7) . . ? O7 C61 N34 127.2(6) . . ? O7 C61 C62 118.5(5) . . ? N34 C61 C62 114.3(6) . . ? N35 C62 C63 121.2(5) . . ? N35 C62 C61 113.1(5) . . ? C63 C62 C61 125.7(6) . . ? C64 C63 C62 118.9(6) . . ? C64 C63 H67 120.6 . . ? C62 C63 H67 120.6 . . ? C63 C64 C65 117.0(6) . . ? C63 C64 H68 121.5 . . ? C65 C64 H68 121.5 . . ? N36 C65 C64 122.9(6) . . ? N36 C65 C66 113.8(5) . . ? C64 C65 C66 123.3(6) . . ? O8 C66 N37 127.3(5) . . ? O8 C66 C65 117.6(5) . . ? N37 C66 C65 115.1(6) . . ? N39 C67 N38 122.7(6) . . ? N39 C67 C68 121.7(6) . . ? N38 C67 C68 115.5(6) . . ? N40 C68 C69 122.8(6) . . ? N40 C68 C67 115.1(6) . . ? C69 C68 C67 122.2(7) . . ? C70 C69 C68 117.6(7) . . ? C70 C69 H69 121.2 . . ? C68 C69 H69 121.2 . . ? C71 C70 C69 120.0(8) . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C70 C71 C72 119.8(7) . . ? C70 C71 H71 120.1 . . ? C72 C71 H71 120.1 . . ? N40 C72 C71 122.1(7) . . ? N40 C72 H72 118.9 . . ? C71 C72 H72 118.9 . . ? N41 C73 C74 121.9(8) . . ? N41 C73 H73 119.0 . . ? C74 C73 H73 119.0 . . ? C75 C74 C73 120.1(8) . . ? C75 C74 H74 119.9 . . ? C73 C74 H74 119.9 . . ? C74 C75 C76 119.6(7) . . ? C74 C75 H75 120.2 . . ? C76 C75 H75 120.2 . . ? C75 C76 C77 117.8(8) . . ? C75 C76 H76 121.1 . . ? C77 C76 H76 121.1 . . ? N41 C77 C76 122.0(6) . . ? N41 C77 C78 114.1(6) . . ? C76 C77 C78 123.9(7) . . ? N43 C78 N42 124.3(6) . . ? N43 C78 C77 114.4(6) . . ? N42 C78 C77 121.2(6) . . ? O9 C79 N44 127.9(5) . . ? O9 C79 C80 117.3(6) . . ? N44 C79 C80 114.9(6) . . ? N45 C80 C81 121.8(5) . . ? N45 C80 C79 113.7(5) . . ? C81 C80 C79 124.4(6) . . ? C82 C81 C80 117.4(6) . . ? C82 C81 H77 121.3 . . ? C80 C81 H77 121.3 . . ? C81 C82 C83 118.1(6) . . ? C81 C82 H78 121.0 . . ? C83 C82 H78 121.0 . . ? N46 C83 C82 122.9(5) . . ? N46 C83 C84 113.7(6) . . ? C82 C83 C84 123.3(6) . . ? N47 C84 O10 127.4(5) . . ? N47 C84 C83 116.7(6) . . ? O10 C84 C83 115.9(5) . . ? N49 C85 N48 125.2(6) . . ? N49 C85 C86 121.5(6) . . ? N48 C85 C86 113.3(7) . . ? N50 C86 C87 120.7(6) . . ? N50 C86 C85 114.5(6) . . ? C87 C86 C85 124.7(7) . . ? C88 C87 C86 118.4(8) . . ? C88 C87 H79 120.8 . . ? C86 C87 H79 120.8 . . ? C89 C88 C87 120.3(7) . . ? C89 C88 H80 119.8 . . ? C87 C88 H80 119.8 . . ? C88 C89 C90 118.9(7) . . ? C88 C89 H81 120.5 . . ? C90 C89 H81 120.5 . . ? N50 C90 C89 122.9(8) . . ? N50 C90 H82 118.5 . . ? C89 C90 H82 118.5 . . ? C92 C91 N51 125.4(9) . . ? C92 C91 H83 117.3 . . ? N51 C91 H83 117.3 . . ? C91 C92 C93 117.6(9) . . ? C91 C92 H84 121.2 . . ? C93 C92 H84 121.2 . . ? C92 C93 C94 121.4(9) . . ? C92 C93 H85 119.3 . . ? C94 C93 H85 119.3 . . ? C95 C94 C93 114.9(10) . . ? C95 C94 H86 122.6 . . ? C93 C94 H86 122.6 . . ? N51 C95 C94 122.5(8) . . ? N51 C95 C96 114.6(6) . . ? C94 C95 C96 122.9(8) . . ? N53 C96 N52 124.9(7) . . ? N53 C96 C95 112.2(7) . . ? N52 C96 C95 122.9(7) . . ? O11 C97 N54 126.3(6) . . ? O11 C97 C98 117.2(5) . . ? N54 C97 C98 116.5(6) . . ? O11 C97 Na1 49.3(4) . . ? N54 C97 Na1 170.3(5) . . ? C98 C97 Na1 68.3(4) . . ? C99 C98 N55 122.5(6) . . ? C99 C98 C97 120.3(6) . . ? N55 C98 C97 117.2(6) . . ? C99 C98 Na1 157.3(5) . . ? N55 C98 Na1 38.2(4) . . ? C97 C98 Na1 80.4(4) . . ? C98 C99 C100 120.0(6) . . ? C98 C99 H87 120.0 . . ? C100 C99 H87 120.0 . . ? C99 C100 C101 120.4(6) . . ? C99 C100 H88 119.8 . . ? C101 C100 H88 119.8 . . ? C100 C101 N56 120.7(6) . . ? C100 C101 C102 121.6(6) . . ? N56 C101 C102 117.6(6) . . ? C100 C101 Na3 151.6(5) . . ? N56 C101 Na3 33.7(3) . . ? C102 C101 Na3 85.0(4) . . ? O12 C102 N57 124.6(5) . . ? O12 C102 C101 115.2(6) . . ? N57 C102 C101 120.1(6) . . ? O12 C102 Na3 50.5(3) . . ? N57 C102 Na3 170.7(4) . . ? C101 C102 Na3 65.1(4) . . ? N58 C103 N59 126.0(7) . . ? N58 C103 C104 112.0(6) . . ? N59 C103 C104 122.0(6) . . ? N60 C104 C105 121.8(6) . . ? N60 C104 C103 114.4(5) . . ? C105 C104 C103 123.9(7) . . ? C104 C105 C106 118.1(8) . . ? C104 C105 H89 120.9 . . ? C106 C105 H89 120.9 . . ? C107 C106 C105 120.5(7) . . ? C107 C106 H90 119.7 . . ? C105 C106 H90 119.7 . . ? C106 C107 C108 118.6(7) . . ? C106 C107 H91 120.7 . . ? C108 C107 H91 120.7 . . ? N60 C108 C107 121.5(7) . . ? N60 C108 H92 119.3 . . ? C107 C108 H92 119.3 . . ? N61 C109 C110 121.9(7) . . ? N61 C109 H93 119.0 . . ? C110 C109 H93 119.0 . . ? C109 C110 C111 118.6(7) . . ? C109 C110 H94 120.7 . . ? C111 C110 H94 120.7 . . ? C112 C111 C110 120.3(7) . . ? C112 C111 H95 119.9 . . ? C110 C111 H95 119.9 . . ? C111 C112 C113 119.0(8) . . ? C111 C112 H96 120.5 . . ? C113 C112 H96 120.5 . . ? N61 C113 C112 122.0(6) . . ? N61 C113 C114 113.1(5) . . ? C112 C113 C114 124.7(7) . . ? N63 C114 N62 125.5(6) . . ? N63 C114 C113 111.7(6) . . ? N62 C114 C113 122.8(6) . . ? O13 C115 N64 125.2(5) . . ? O13 C115 C116 117.3(6) . . ? N64 C115 C116 117.5(6) . . ? O13 C115 Na2 55.6(5) . . ? N64 C115 Na2 162.8(6) . . ? C116 C115 Na2 64.6(5) . . ? C117 C116 N65 122.2(6) . . ? C117 C116 C115 120.4(6) . . ? N65 C116 C115 117.4(6) . . ? C117 C116 Na2 150.0(6) . . ? N65 C116 Na2 38.0(6) . . ? C115 C116 Na2 83.2(6) . . ? C118 C117 C116 120.2(6) . . ? C118 C117 H97 119.9 . . ? C116 C117 H97 119.9 . . ? C119 C118 C117 121.2(7) . . ? C119 C118 H98 119.4 . . ? C117 C118 H98 119.4 . . ? C118 C119 N66 121.0(6) . . ? C118 C119 C120 122.0(6) . . ? N66 C119 C120 117.0(6) . . ? C118 C119 Na4 148.5(5) . . ? N66 C119 Na4 39.1(3) . . ? C120 C119 Na4 83.1(4) . . ? O14 C120 N67 125.3(6) . . ? O14 C120 C119 116.7(6) . . ? N67 C120 C119 118.0(6) . . ? O14 C120 Na4 54.3(3) . . ? N67 C120 Na4 160.3(4) . . ? C119 C120 Na4 66.2(4) . . ? N68 C121 N69 124.5(7) . . ? N68 C121 C122 112.4(6) . . ? N69 C121 C122 123.1(6) . . ? N70 C122 C123 121.9(7) . . ? N70 C122 C121 114.0(6) . . ? C123 C122 C121 124.1(7) . . ? C124 C123 C122 118.0(9) . . ? C124 C123 H99 121.0 . . ? C122 C123 H99 121.0 . . ? C123 C124 C125 120.1(7) . . ? C123 C124 H100 119.9 . . ? C125 C124 H100 119.9 . . ? C126 C125 C124 118.0(7) . . ? C126 C125 H101 121.0 . . ? C124 C125 H101 121.0 . . ? N70 C126 C125 122.9(7) . . ? N70 C126 H102 118.6 . . ? C125 C126 H102 118.6 . . ? N71 C127 C128 123.7(9) . . ? N71 C127 H103 118.2 . . ? C128 C127 H103 118.2 . . ? C129 C128 C127 118.2(8) . . ? C129 C128 H104 120.9 . . ? C127 C128 H104 120.9 . . ? C128 C129 C130 119.6(8) . . ? C128 C129 H105 120.2 . . ? C130 C129 H105 120.2 . . ? C131 C130 C129 117.8(9) . . ? C131 C130 H106 121.1 . . ? C129 C130 H106 121.1 . . ? N71 C131 C130 124.9(7) . . ? N71 C131 C132 113.3(6) . . ? C130 C131 C132 121.8(7) . . ? N73 C132 N72 124.5(6) . . ? N73 C132 C131 114.3(6) . . ? N72 C132 C131 121.2(6) . . ? N74 C133 O15 125.2(6) . . ? N74 C133 C134 116.7(6) . . ? O15 C133 C134 118.2(5) . . ? N75 C134 C135 121.9(5) . . ? N75 C134 C133 113.7(6) . . ? C135 C134 C133 124.4(6) . . ? C136 C135 C134 117.8(6) . . ? C136 C135 H107 121.1 . . ? C134 C135 H107 121.1 . . ? C135 C136 C137 118.8(6) . . ? C135 C136 H108 120.6 . . ? C137 C136 H108 120.6 . . ? N76 C137 C136 120.5(5) . . ? N76 C137 C138 114.4(5) . . ? C136 C137 C138 125.1(6) . . ? O16 C138 N77 126.4(5) . . ? O16 C138 C137 117.0(5) . . ? N77 C138 C137 116.6(5) . . ? N79 C139 N78 124.8(6) . . ? N79 C139 C140 123.3(5) . . ? N78 C139 C140 112.0(6) . . ? N80 C140 C141 122.3(6) . . ? N80 C140 C139 114.1(5) . . ? C141 C140 C139 123.6(7) . . ? C140 C141 C142 118.5(7) . . ? C140 C141 H109 120.7 . . ? C142 C141 H109 120.7 . . ? C143 C142 C141 118.0(6) . . ? C143 C142 H110 121.0 . . ? C141 C142 H110 121.0 . . ? C142 C143 C144 120.7(7) . . ? C142 C143 H111 119.7 . . ? C144 C143 H111 119.7 . . ? N80 C144 C143 122.2(7) . . ? N80 C144 H112 118.9 . . ? C143 C144 H112 118.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.519 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.110