# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'Ke Wen' _publ_contact_author_name 'Prof. Ke Wen' _publ_contact_author_email kwen@brain.ecnu.edu.cn # Attachment '- 3.cif' data_z_1 _database_code_depnum_ccdc_archive 'CCDC 825937' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H24 N8 O16' _chemical_formula_weight 920.71 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' _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 10.7260(2) _cell_length_b 11.7585(2) _cell_length_c 16.2804(2) _cell_angle_alpha 98.8300(10) _cell_angle_beta 104.4450(10) _cell_angle_gamma 92.6660(10) _cell_volume 1957.10(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7925 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 28.47 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9391 _exptl_absorpt_correction_T_max 0.9570 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18915 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6671 _reflns_number_gt 5401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0565P)^2^+0.7372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6671 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N5 N 0.58403(14) 0.10194(14) 0.16425(10) 0.0335(4) Uani 1 1 d . . . N6 N 0.67684(12) 0.18695(12) 0.03935(8) 0.0234(3) Uani 1 1 d . . . N7 N 1.09911(14) 0.31772(14) 0.23135(9) 0.0347(4) Uani 1 1 d . . . N8 N 0.92908(12) 0.30070(11) 0.07013(8) 0.0221(3) Uani 1 1 d . . . O9 O 0.36037(13) 0.31481(14) -0.14480(8) 0.0484(4) Uani 1 1 d . . . O10 O 0.40098(11) 0.29376(11) -0.00873(8) 0.0359(3) Uani 1 1 d . . . H10B H 0.4616 0.3071 0.0365 0.054 Uiso 1 1 calc R . . O11 O 1.12967(12) 0.21027(13) -0.15510(8) 0.0429(4) Uani 1 1 d . . . H11B H 1.2039 0.2453 -0.1376 0.064 Uiso 1 1 calc R . . O12 O 1.15792(11) 0.22268(11) -0.01400(7) 0.0316(3) Uani 1 1 d . . . O13 O 0.72952(12) 0.00478(10) -0.00672(8) 0.0319(3) Uani 1 1 d . . . O14 O 0.64027(11) 0.37028(10) 0.09556(7) 0.0270(3) Uani 1 1 d . . . O15 O 0.87356(11) 0.48458(10) 0.10831(8) 0.0291(3) Uani 1 1 d . . . O16 O 0.97552(11) 0.11170(10) 0.03912(7) 0.0269(3) Uani 1 1 d . . . C23 C 0.66123(15) 0.40507(14) 0.02213(11) 0.0240(4) Uani 1 1 d . . . C24 C 0.77983(16) 0.46334(14) 0.02939(11) 0.0256(4) Uani 1 1 d . . . C25 C 0.80528(17) 0.50603(15) -0.03952(12) 0.0325(4) Uani 1 1 d . . . H25A H 0.8868 0.5460 -0.0338 0.039 Uiso 1 1 calc R . . C26 C 0.71202(18) 0.49061(17) -0.11681(13) 0.0397(5) Uani 1 1 d . . . H26A H 0.7290 0.5204 -0.1643 0.048 Uiso 1 1 calc R . . C27 C 0.59390(17) 0.43171(17) -0.12495(12) 0.0351(4) Uani 1 1 d . . . H27A H 0.5305 0.4205 -0.1786 0.042 Uiso 1 1 calc R . . C28 C 0.56609(16) 0.38854(14) -0.05601(11) 0.0268(4) Uani 1 1 d . . . C29 C 0.90195(15) 0.10812(13) -0.04452(10) 0.0234(4) Uani 1 1 d . . . C30 C 0.95224(15) 0.14743(14) -0.10753(10) 0.0239(4) Uani 1 1 d . . . C31 C 0.87399(16) 0.13391(15) -0.19112(11) 0.0282(4) Uani 1 1 d . . . H31A H 0.9059 0.1629 -0.2340 0.034 Uiso 1 1 calc R . . C32 C 0.75084(16) 0.07922(16) -0.21283(11) 0.0312(4) Uani 1 1 d . . . H32A H 0.6992 0.0699 -0.2705 0.037 Uiso 1 1 calc R . . C33 C 0.70246(16) 0.03795(15) -0.15079(12) 0.0304(4) Uani 1 1 d . . . H33A H 0.6181 -0.0007 -0.1657 0.036 Uiso 1 1 calc R . . C34 C 0.77738(16) 0.05329(14) -0.06739(11) 0.0251(4) Uani 1 1 d . . . C35 C 0.63058(17) 0.03275(16) 0.10859(12) 0.0316(4) Uani 1 1 d . . . H35A H 0.6309 -0.0475 0.1108 0.038 Uiso 1 1 calc R . . C36 C 0.67859(15) 0.07707(14) 0.04736(11) 0.0249(4) Uani 1 1 d . . . C37 C 0.63440(15) 0.25440(14) 0.09694(10) 0.0235(4) Uani 1 1 d . . . C38 C 0.58721(16) 0.21409(16) 0.15942(11) 0.0306(4) Uani 1 1 d . . . H38A H 0.5569 0.2663 0.1991 0.037 Uiso 1 1 calc R . . C39 C 1.08133(16) 0.22144(16) 0.17401(11) 0.0301(4) Uani 1 1 d . . . H39A H 1.1281 0.1572 0.1877 0.036 Uiso 1 1 calc R . . C40 C 0.99477(15) 0.21433(14) 0.09418(10) 0.0226(3) Uani 1 1 d . . . C41 C 0.94464(15) 0.39436(14) 0.12905(10) 0.0236(4) Uani 1 1 d . . . C42 C 1.03003(16) 0.40515(16) 0.20965(11) 0.0310(4) Uani 1 1 d . . . H42A H 1.0395 0.4749 0.2496 0.037 Uiso 1 1 calc R . . C43 C 0.43626(16) 0.32790(15) -0.06688(11) 0.0270(4) Uani 1 1 d . . . C44 C 1.08789(16) 0.19680(14) -0.09295(11) 0.0258(4) Uani 1 1 d . . . O1 O 0.64885(13) 0.23239(13) 0.63301(9) 0.0484(4) Uani 1 1 d . . . O2 O 0.60125(13) 0.20535(13) 0.49048(9) 0.0385(3) Uani 1 1 d . . . O3 O -0.11088(13) 0.31468(13) 0.65332(8) 0.0398(3) Uani 1 1 d . . . O4 O -0.15132(11) 0.27193(11) 0.51079(7) 0.0314(3) Uani 1 1 d . . . O5 O 0.14107(11) 0.00075(10) 0.40454(8) 0.0331(3) Uani 1 1 d . . . O6 O 0.01797(11) 0.37154(10) 0.43809(7) 0.0284(3) Uani 1 1 d . . . O7 O 0.25551(11) 0.49235(10) 0.46802(8) 0.0336(3) Uani 1 1 d . . . O8 O 0.36244(11) 0.12170(10) 0.40078(7) 0.0288(3) Uani 1 1 d . . . N1 N -0.11981(15) 0.12781(16) 0.27497(10) 0.0416(4) Uani 1 1 d . . . N2 N 0.07592(12) 0.18465(12) 0.42561(9) 0.0247(3) Uani 1 1 d . . . N3 N 0.40185(14) 0.36947(14) 0.30343(10) 0.0348(4) Uani 1 1 d . . . N4 N 0.31826(12) 0.30897(12) 0.44006(9) 0.0245(3) Uani 1 1 d . . . C1 C 0.23745(16) 0.03787(14) 0.48093(12) 0.0284(4) Uani 1 1 d . . . C2 C 0.34958(16) 0.10033(14) 0.47995(11) 0.0263(4) Uani 1 1 d . . . C3 C 0.44632(16) 0.13436(15) 0.55630(12) 0.0289(4) Uani 1 1 d . . . C4 C 0.42542(17) 0.10667(17) 0.63222(12) 0.0364(4) Uani 1 1 d . . . H4B H 0.4891 0.1321 0.6850 0.044 Uiso 1 1 calc R . . C5 C 0.31432(18) 0.04313(18) 0.63238(13) 0.0409(5) Uani 1 1 d . . . H5A H 0.3027 0.0233 0.6845 0.049 Uiso 1 1 calc R . . C6 C 0.22001(18) 0.00845(16) 0.55624(13) 0.0357(4) Uani 1 1 d . . . H6A H 0.1433 -0.0356 0.5558 0.043 Uiso 1 1 calc R . . C7 C 0.09628(15) 0.39386(14) 0.52163(11) 0.0246(4) Uani 1 1 d . . . C8 C 0.05445(16) 0.36661(14) 0.59151(11) 0.0255(4) Uani 1 1 d . . . C9 C 0.13626(17) 0.39788(15) 0.67406(11) 0.0309(4) Uani 1 1 d . . . H9A H 0.1102 0.3767 0.7217 0.037 Uiso 1 1 calc R . . C10 C 0.25464(17) 0.45921(17) 0.68768(12) 0.0367(4) Uani 1 1 d . . . H10A H 0.3093 0.4805 0.7443 0.044 Uiso 1 1 calc R . . C11 C 0.29324(17) 0.48957(16) 0.61820(13) 0.0354(4) Uani 1 1 d . . . H11A H 0.3735 0.5336 0.6273 0.043 Uiso 1 1 calc R . . C12 C 0.21559(16) 0.45600(15) 0.53623(12) 0.0284(4) Uani 1 1 d . . . C13 C -0.10217(17) 0.23296(18) 0.32142(11) 0.0349(4) Uani 1 1 d . . . H13A H -0.1583 0.2898 0.3038 0.042 Uiso 1 1 calc R . . C14 C -0.00210(15) 0.26018(15) 0.39562(11) 0.0265(4) Uani 1 1 d . . . C15 C 0.05920(16) 0.08157(15) 0.37760(11) 0.0276(4) Uani 1 1 d . . . C16 C -0.03828(17) 0.05089(18) 0.30199(12) 0.0375(5) Uani 1 1 d . . . H16A H -0.0470 -0.0247 0.2695 0.045 Uiso 1 1 calc R . . C17 C 0.35453(16) 0.44609(16) 0.35377(12) 0.0329(4) Uani 1 1 d . . . H17A H 0.3512 0.5236 0.3440 0.039 Uiso 1 1 calc R . . C18 C 0.30990(15) 0.41359(15) 0.42060(11) 0.0264(4) Uani 1 1 d . . . C19 C 0.36113(15) 0.23364(14) 0.38751(10) 0.0246(4) Uani 1 1 d . . . C20 C 0.40289(16) 0.26170(16) 0.31890(11) 0.0318(4) Uani 1 1 d . . . H20A H 0.4325 0.2038 0.2826 0.038 Uiso 1 1 calc R . . C21 C -0.07790(16) 0.31267(14) 0.58162(11) 0.0265(4) Uani 1 1 d . . . C22 C 0.57365(16) 0.19565(15) 0.56173(11) 0.0290(4) Uani 1 1 d . . . H2A H 0.676(3) 0.231(3) 0.499(2) 0.112(12) Uiso 1 1 d . . . H3A H -0.191(3) 0.278(2) 0.6418(17) 0.086(9) 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 N5 0.0303(8) 0.0413(10) 0.0302(8) 0.0118(7) 0.0086(7) -0.0053(7) N6 0.0198(7) 0.0258(8) 0.0252(7) 0.0057(6) 0.0067(6) -0.0011(5) N7 0.0282(8) 0.0468(10) 0.0263(8) 0.0008(7) 0.0050(6) 0.0040(7) N8 0.0194(7) 0.0236(7) 0.0227(7) 0.0020(6) 0.0059(5) -0.0011(5) O9 0.0340(8) 0.0728(11) 0.0340(8) 0.0124(7) 0.0017(6) -0.0106(7) O10 0.0208(6) 0.0497(8) 0.0376(7) 0.0157(6) 0.0044(5) -0.0003(5) O11 0.0302(7) 0.0620(10) 0.0335(7) 0.0026(7) 0.0093(6) -0.0138(6) O12 0.0239(6) 0.0404(7) 0.0266(6) 0.0003(6) 0.0031(5) -0.0005(5) O13 0.0357(7) 0.0230(6) 0.0420(7) 0.0089(6) 0.0176(6) 0.0026(5) O14 0.0307(6) 0.0261(6) 0.0263(6) 0.0025(5) 0.0127(5) 0.0012(5) O15 0.0258(6) 0.0240(6) 0.0346(7) -0.0026(5) 0.0073(5) 0.0013(5) O16 0.0321(6) 0.0228(6) 0.0233(6) 0.0035(5) 0.0026(5) 0.0058(5) C23 0.0258(9) 0.0193(8) 0.0312(9) 0.0053(7) 0.0139(7) 0.0062(6) C24 0.0243(9) 0.0203(9) 0.0328(9) 0.0017(7) 0.0093(7) 0.0065(6) C25 0.0254(9) 0.0291(10) 0.0482(11) 0.0126(9) 0.0157(8) 0.0028(7) C26 0.0350(10) 0.0473(12) 0.0463(12) 0.0252(10) 0.0174(9) 0.0066(9) C27 0.0291(9) 0.0426(11) 0.0363(10) 0.0152(9) 0.0077(8) 0.0079(8) C28 0.0250(9) 0.0243(9) 0.0336(10) 0.0067(8) 0.0102(7) 0.0068(7) C29 0.0255(9) 0.0179(8) 0.0252(9) 0.0010(7) 0.0048(7) 0.0063(6) C30 0.0231(8) 0.0194(8) 0.0277(9) 0.0003(7) 0.0061(7) 0.0036(6) C31 0.0277(9) 0.0309(10) 0.0262(9) 0.0039(7) 0.0077(7) 0.0056(7) C32 0.0240(9) 0.0384(11) 0.0270(9) 0.0001(8) 0.0015(7) 0.0049(7) C33 0.0215(8) 0.0283(10) 0.0380(10) -0.0015(8) 0.0058(7) 0.0016(7) C34 0.0264(9) 0.0193(9) 0.0310(9) 0.0023(7) 0.0108(7) 0.0044(6) C35 0.0292(9) 0.0302(10) 0.0355(10) 0.0122(8) 0.0056(8) -0.0036(7) C36 0.0201(8) 0.0256(9) 0.0280(9) 0.0055(7) 0.0045(7) -0.0005(6) C37 0.0178(8) 0.0283(9) 0.0228(8) 0.0033(7) 0.0036(6) -0.0017(6) C38 0.0257(9) 0.0395(11) 0.0270(9) 0.0045(8) 0.0097(7) -0.0033(7) C39 0.0277(9) 0.0377(11) 0.0250(9) 0.0057(8) 0.0063(7) 0.0064(7) C40 0.0212(8) 0.0254(9) 0.0222(8) 0.0030(7) 0.0083(6) 0.0003(6) C41 0.0182(8) 0.0254(9) 0.0278(9) 0.0006(7) 0.0100(7) -0.0020(6) C42 0.0262(9) 0.0363(10) 0.0269(9) -0.0066(8) 0.0085(7) -0.0021(7) C43 0.0233(9) 0.0290(9) 0.0306(9) 0.0074(8) 0.0086(7) 0.0058(7) C44 0.0252(9) 0.0246(9) 0.0269(9) 0.0024(7) 0.0065(7) 0.0037(7) O1 0.0333(7) 0.0687(10) 0.0396(8) 0.0127(7) 0.0031(6) -0.0099(7) O2 0.0224(7) 0.0561(9) 0.0398(8) 0.0131(7) 0.0112(6) -0.0007(6) O3 0.0357(8) 0.0548(9) 0.0293(7) 0.0071(6) 0.0112(6) -0.0077(6) O4 0.0240(6) 0.0380(7) 0.0298(7) -0.0016(6) 0.0079(5) -0.0022(5) O5 0.0287(7) 0.0274(7) 0.0405(7) -0.0052(6) 0.0113(6) -0.0022(5) O6 0.0281(6) 0.0300(7) 0.0262(6) 0.0058(5) 0.0045(5) 0.0034(5) O7 0.0327(7) 0.0273(7) 0.0470(8) 0.0100(6) 0.0194(6) 0.0047(5) O8 0.0307(6) 0.0270(7) 0.0301(7) 0.0009(5) 0.0134(5) 0.0008(5) N1 0.0263(8) 0.0618(12) 0.0303(9) -0.0074(8) 0.0060(7) -0.0024(8) N2 0.0196(7) 0.0287(8) 0.0248(7) -0.0005(6) 0.0080(6) -0.0022(6) N3 0.0294(8) 0.0431(10) 0.0336(9) 0.0101(7) 0.0104(7) -0.0043(7) N4 0.0187(7) 0.0281(8) 0.0265(7) 0.0041(6) 0.0063(6) -0.0009(5) C1 0.0255(9) 0.0237(9) 0.0375(10) 0.0018(8) 0.0125(8) 0.0057(7) C2 0.0270(9) 0.0228(9) 0.0331(9) 0.0050(7) 0.0141(7) 0.0072(7) C3 0.0245(9) 0.0277(9) 0.0383(10) 0.0098(8) 0.0117(8) 0.0083(7) C4 0.0279(10) 0.0461(12) 0.0377(11) 0.0156(9) 0.0075(8) 0.0063(8) C5 0.0354(11) 0.0526(13) 0.0437(12) 0.0219(10) 0.0182(9) 0.0063(9) C6 0.0311(10) 0.0325(10) 0.0486(12) 0.0094(9) 0.0184(9) 0.0019(8) C7 0.0235(8) 0.0221(9) 0.0263(9) 0.0006(7) 0.0045(7) 0.0059(6) C8 0.0237(8) 0.0231(9) 0.0287(9) 0.0015(7) 0.0061(7) 0.0044(6) C9 0.0287(9) 0.0351(10) 0.0283(9) 0.0025(8) 0.0071(7) 0.0076(7) C10 0.0280(10) 0.0420(11) 0.0324(10) -0.0047(9) 0.0003(8) 0.0036(8) C11 0.0222(9) 0.0327(10) 0.0470(12) -0.0025(9) 0.0067(8) 0.0003(7) C12 0.0256(9) 0.0241(9) 0.0380(10) 0.0044(8) 0.0128(8) 0.0054(7) C13 0.0251(9) 0.0503(12) 0.0278(9) 0.0029(9) 0.0065(7) 0.0026(8) C14 0.0221(8) 0.0340(10) 0.0251(9) 0.0033(8) 0.0111(7) -0.0010(7) C15 0.0219(8) 0.0301(10) 0.0312(9) -0.0022(8) 0.0133(7) -0.0036(7) C16 0.0270(10) 0.0474(12) 0.0327(10) -0.0131(9) 0.0119(8) -0.0074(8) C17 0.0259(9) 0.0352(10) 0.0378(10) 0.0120(9) 0.0064(8) -0.0029(7) C18 0.0174(8) 0.0295(10) 0.0309(9) 0.0052(8) 0.0041(7) -0.0008(7) C19 0.0174(8) 0.0289(9) 0.0254(9) 0.0018(7) 0.0041(7) -0.0017(6) C20 0.0266(9) 0.0399(11) 0.0285(9) 0.0014(8) 0.0101(7) -0.0040(7) C21 0.0268(9) 0.0253(9) 0.0274(9) 0.0052(7) 0.0066(7) 0.0038(7) C22 0.0238(9) 0.0319(10) 0.0332(10) 0.0107(8) 0.0074(8) 0.0057(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N5 C35 1.330(2) . ? N5 C38 1.332(2) . ? N6 C37 1.317(2) . ? N6 C36 1.319(2) . ? N7 C39 1.325(2) . ? N7 C42 1.335(2) . ? N8 C40 1.316(2) . ? N8 C41 1.319(2) . ? O9 C43 1.307(2) . ? O10 C43 1.217(2) . ? O10 H10B 0.8400 . ? O11 C44 1.232(2) . ? O11 H11B 0.8400 . ? O12 C44 1.298(2) . ? O13 C36 1.360(2) . ? O13 C34 1.401(2) . ? O14 C37 1.365(2) . ? O14 C23 1.3866(19) . ? O15 C41 1.370(2) . ? O15 C24 1.399(2) . ? O16 C40 1.362(2) . ? O16 C29 1.3863(19) . ? C23 C24 1.386(2) . ? C23 C28 1.398(2) . ? C24 C25 1.378(2) . ? C25 C26 1.379(3) . ? C25 H25A 0.9500 . ? C26 C27 1.382(3) . ? C26 H26A 0.9500 . ? C27 C28 1.391(2) . ? C27 H27A 0.9500 . ? C28 C43 1.492(2) . ? C29 C34 1.392(2) . ? C29 C30 1.398(2) . ? C30 C31 1.390(2) . ? C30 C44 1.489(2) . ? C31 C32 1.379(2) . ? C31 H31A 0.9500 . ? C32 C33 1.383(3) . ? C32 H32A 0.9500 . ? C33 C34 1.374(2) . ? C33 H33A 0.9500 . ? C35 C36 1.386(2) . ? C35 H35A 0.9500 . ? C37 C38 1.378(2) . ? C38 H38A 0.9500 . ? C39 C40 1.384(2) . ? C39 H39A 0.9500 . ? C41 C42 1.384(2) . ? C42 H42A 0.9500 . ? O1 C22 1.237(2) . ? O2 C22 1.286(2) . ? O2 H2A 0.81(3) . ? O3 C21 1.299(2) . ? O3 H3A 0.90(3) . ? O4 C21 1.234(2) . ? O5 C15 1.371(2) . ? O5 C1 1.398(2) . ? O6 C14 1.364(2) . ? O6 C7 1.3871(19) . ? O7 C18 1.360(2) . ? O7 C12 1.402(2) . ? O8 C19 1.366(2) . ? O8 C2 1.389(2) . ? N1 C13 1.325(3) . ? N1 C16 1.334(3) . ? N2 C14 1.314(2) . ? N2 C15 1.316(2) . ? N3 C17 1.328(2) . ? N3 C20 1.329(2) . ? N4 C19 1.315(2) . ? N4 C18 1.318(2) . ? C1 C6 1.377(3) . ? C1 C2 1.385(2) . ? C2 C3 1.395(2) . ? C3 C4 1.393(3) . ? C3 C22 1.490(2) . ? C4 C5 1.377(3) . ? C4 H4B 0.9500 . ? C5 C6 1.381(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.391(2) . ? C7 C8 1.397(2) . ? C8 C9 1.393(2) . ? C8 C21 1.488(2) . ? C9 C10 1.381(3) . ? C9 H9A 0.9500 . ? C10 C11 1.386(3) . ? C10 H10A 0.9500 . ? C11 C12 1.372(3) . ? C11 H11A 0.9500 . ? C13 C14 1.384(2) . ? C13 H13A 0.9500 . ? C15 C16 1.388(2) . ? C16 H16A 0.9500 . ? C17 C18 1.389(2) . ? C17 H17A 0.9500 . ? C19 C20 1.381(2) . ? C20 H20A 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 C35 N5 C38 117.66(15) . . ? C37 N6 C36 115.91(14) . . ? C39 N7 C42 117.84(15) . . ? C40 N8 C41 115.79(14) . . ? C43 O10 H10B 109.5 . . ? C44 O11 H11B 109.5 . . ? C36 O13 C34 117.05(12) . . ? C37 O14 C23 116.83(13) . . ? C41 O15 C24 116.10(13) . . ? C40 O16 C29 117.96(12) . . ? C24 C23 O14 117.41(15) . . ? C24 C23 C28 119.92(15) . . ? O14 C23 C28 122.60(14) . . ? C25 C24 C23 120.78(16) . . ? C25 C24 O15 118.86(15) . . ? C23 C24 O15 120.29(15) . . ? C24 C25 C26 119.82(16) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C25 C26 C27 119.86(17) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C26 C27 C28 121.19(17) . . ? C26 C27 H27A 119.4 . . ? C28 C27 H27A 119.4 . . ? C27 C28 C23 118.44(16) . . ? C27 C28 C43 119.51(15) . . ? C23 C28 C43 122.05(15) . . ? O16 C29 C34 117.72(14) . . ? O16 C29 C30 122.49(14) . . ? C34 C29 C30 119.52(15) . . ? C31 C30 C29 118.63(15) . . ? C31 C30 C44 116.77(15) . . ? C29 C30 C44 124.48(15) . . ? C32 C31 C30 121.15(16) . . ? C32 C31 H31A 119.4 . . ? C30 C31 H31A 119.4 . . ? C31 C32 C33 120.06(16) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 119.49(16) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C33 C34 C29 121.10(16) . . ? C33 C34 O13 118.50(15) . . ? C29 C34 O13 120.23(15) . . ? N5 C35 C36 120.38(16) . . ? N5 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? N6 C36 O13 118.51(14) . . ? N6 C36 C35 122.54(16) . . ? O13 C36 C35 118.95(15) . . ? N6 C37 O14 118.12(14) . . ? N6 C37 C38 123.26(16) . . ? O14 C37 C38 118.60(15) . . ? N5 C38 C37 120.10(17) . . ? N5 C38 H38A 119.9 . . ? C37 C38 H38A 119.9 . . ? N7 C39 C40 120.09(16) . . ? N7 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? N8 C40 O16 119.01(14) . . ? N8 C40 C39 123.21(16) . . ? O16 C40 C39 117.76(14) . . ? N8 C41 O15 117.89(14) . . ? N8 C41 C42 122.81(16) . . ? O15 C41 C42 119.29(15) . . ? N7 C42 C41 120.15(16) . . ? N7 C42 H42A 119.9 . . ? C41 C42 H42A 119.9 . . ? O10 C43 O9 121.54(16) . . ? O10 C43 C28 123.87(15) . . ? O9 C43 C28 114.58(14) . . ? O11 C44 O12 122.76(15) . . ? O11 C44 C30 119.60(15) . . ? O12 C44 C30 117.64(14) . . ? C22 O2 H2A 111(2) . . ? C21 O3 H3A 108.8(18) . . ? C15 O5 C1 115.74(13) . . ? C14 O6 C7 118.12(12) . . ? C18 O7 C12 116.65(13) . . ? C19 O8 C2 117.32(13) . . ? C13 N1 C16 117.88(16) . . ? C14 N2 C15 115.86(15) . . ? C17 N3 C20 117.57(15) . . ? C19 N4 C18 115.79(15) . . ? C6 C1 C2 120.95(17) . . ? C6 C1 O5 118.76(15) . . ? C2 C1 O5 120.28(15) . . ? C1 C2 O8 117.42(15) . . ? C1 C2 C3 119.67(16) . . ? O8 C2 C3 122.85(15) . . ? C4 C3 C2 118.57(16) . . ? C4 C3 C22 117.30(16) . . ? C2 C3 C22 124.10(15) . . ? C5 C4 C3 121.32(18) . . ? C5 C4 H4B 119.3 . . ? C3 C4 H4B 119.3 . . ? C4 C5 C6 119.59(17) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C1 C6 C5 119.86(17) . . ? C1 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? O6 C7 C12 117.79(15) . . ? O6 C7 C8 122.44(14) . . ? C12 C7 C8 119.46(15) . . ? C9 C8 C7 118.93(15) . . ? C9 C8 C21 118.64(15) . . ? C7 C8 C21 122.28(15) . . ? C10 C9 C8 120.99(17) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C9 C10 C11 119.60(17) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C12 C11 C10 120.04(17) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 120.89(16) . . ? C11 C12 O7 118.34(15) . . ? C7 C12 O7 120.64(15) . . ? N1 C13 C14 120.17(18) . . ? N1 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? N2 C14 O6 118.75(15) . . ? N2 C14 C13 123.11(17) . . ? O6 C14 C13 118.12(16) . . ? N2 C15 O5 118.16(15) . . ? N2 C15 C16 122.98(17) . . ? O5 C15 C16 118.85(16) . . ? N1 C16 C15 119.87(18) . . ? N1 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? N3 C17 C18 120.43(17) . . ? N3 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? N4 C18 O7 118.47(15) . . ? N4 C18 C17 122.50(17) . . ? O7 C18 C17 119.03(15) . . ? N4 C19 O8 118.26(14) . . ? N4 C19 C20 123.27(16) . . ? O8 C19 C20 118.46(16) . . ? N3 C20 C19 120.20(17) . . ? N3 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? O4 C21 O3 122.82(15) . . ? O4 C21 C8 122.58(15) . . ? O3 C21 C8 114.58(15) . . ? O1 C22 O2 122.88(16) . . ? O1 C22 C3 119.70(16) . . ? O2 C22 C3 117.40(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C37 O14 C23 C24 -110.23(16) . . . . ? C37 O14 C23 C28 72.99(19) . . . . ? O14 C23 C24 C25 -176.51(14) . . . . ? C28 C23 C24 C25 0.4(2) . . . . ? O14 C23 C24 O15 0.4(2) . . . . ? C28 C23 C24 O15 177.27(14) . . . . ? C41 O15 C24 C25 -102.64(17) . . . . ? C41 O15 C24 C23 80.39(19) . . . . ? C23 C24 C25 C26 -0.1(3) . . . . ? O15 C24 C25 C26 -177.07(16) . . . . ? C24 C25 C26 C27 -0.5(3) . . . . ? C25 C26 C27 C28 0.9(3) . . . . ? C26 C27 C28 C23 -0.6(3) . . . . ? C26 C27 C28 C43 178.55(17) . . . . ? C24 C23 C28 C27 0.0(2) . . . . ? O14 C23 C28 C27 176.71(15) . . . . ? C24 C23 C28 C43 -179.13(15) . . . . ? O14 C23 C28 C43 -2.4(2) . . . . ? C40 O16 C29 C34 -106.36(17) . . . . ? C40 O16 C29 C30 79.73(19) . . . . ? O16 C29 C30 C31 175.99(14) . . . . ? C34 C29 C30 C31 2.2(2) . . . . ? O16 C29 C30 C44 0.0(2) . . . . ? C34 C29 C30 C44 -173.78(15) . . . . ? C29 C30 C31 C32 -2.3(3) . . . . ? C44 C30 C31 C32 173.93(16) . . . . ? C30 C31 C32 C33 0.8(3) . . . . ? C31 C32 C33 C34 0.9(3) . . . . ? C32 C33 C34 C29 -1.0(3) . . . . ? C32 C33 C34 O13 -176.24(15) . . . . ? O16 C29 C34 C33 -174.65(14) . . . . ? C30 C29 C34 C33 -0.5(2) . . . . ? O16 C29 C34 O13 0.5(2) . . . . ? C30 C29 C34 O13 174.62(14) . . . . ? C36 O13 C34 C33 -101.19(18) . . . . ? C36 O13 C34 C29 83.52(19) . . . . ? C38 N5 C35 C36 -0.9(2) . . . . ? C37 N6 C36 O13 -175.66(13) . . . . ? C37 N6 C36 C35 4.4(2) . . . . ? C34 O13 C36 N6 0.3(2) . . . . ? C34 O13 C36 C35 -179.76(14) . . . . ? N5 C35 C36 N6 -2.2(3) . . . . ? N5 C35 C36 O13 177.78(15) . . . . ? C36 N6 C37 O14 174.92(13) . . . . ? C36 N6 C37 C38 -3.6(2) . . . . ? C23 O14 C37 N6 14.9(2) . . . . ? C23 O14 C37 C38 -166.48(14) . . . . ? C35 N5 C38 C37 1.7(2) . . . . ? N6 C37 C38 N5 0.7(2) . . . . ? O14 C37 C38 N5 -177.86(14) . . . . ? C42 N7 C39 C40 0.9(2) . . . . ? C41 N8 C40 O16 174.73(13) . . . . ? C41 N8 C40 C39 -3.8(2) . . . . ? C29 O16 C40 N8 9.4(2) . . . . ? C29 O16 C40 C39 -171.95(14) . . . . ? N7 C39 C40 N8 1.6(3) . . . . ? N7 C39 C40 O16 -176.96(15) . . . . ? C40 N8 C41 O15 -176.98(13) . . . . ? C40 N8 C41 C42 3.7(2) . . . . ? C24 O15 C41 N8 7.1(2) . . . . ? C24 O15 C41 C42 -173.61(14) . . . . ? C39 N7 C42 C41 -1.0(2) . . . . ? N8 C41 C42 N7 -1.4(3) . . . . ? O15 C41 C42 N7 179.29(15) . . . . ? C27 C28 C43 O10 -175.32(17) . . . . ? C23 C28 C43 O10 3.8(3) . . . . ? C27 C28 C43 O9 3.8(2) . . . . ? C23 C28 C43 O9 -177.03(16) . . . . ? C31 C30 C44 O11 -8.7(2) . . . . ? C29 C30 C44 O11 167.34(17) . . . . ? C31 C30 C44 O12 172.12(15) . . . . ? C29 C30 C44 O12 -11.9(2) . . . . ? C15 O5 C1 C6 100.34(18) . . . . ? C15 O5 C1 C2 -81.38(19) . . . . ? C6 C1 C2 O8 176.94(15) . . . . ? O5 C1 C2 O8 -1.3(2) . . . . ? C6 C1 C2 C3 -0.2(3) . . . . ? O5 C1 C2 C3 -178.42(15) . . . . ? C19 O8 C2 C1 112.57(16) . . . . ? C19 O8 C2 C3 -70.4(2) . . . . ? C1 C2 C3 C4 -1.6(3) . . . . ? O8 C2 C3 C4 -178.59(15) . . . . ? C1 C2 C3 C22 176.27(15) . . . . ? O8 C2 C3 C22 -0.7(3) . . . . ? C2 C3 C4 C5 2.6(3) . . . . ? C22 C3 C4 C5 -175.48(17) . . . . ? C3 C4 C5 C6 -1.7(3) . . . . ? C2 C1 C6 C5 1.1(3) . . . . ? O5 C1 C6 C5 179.38(16) . . . . ? C4 C5 C6 C1 -0.2(3) . . . . ? C14 O6 C7 C12 111.20(17) . . . . ? C14 O6 C7 C8 -75.3(2) . . . . ? O6 C7 C8 C9 -176.31(15) . . . . ? C12 C7 C8 C9 -2.9(2) . . . . ? O6 C7 C8 C21 -0.7(2) . . . . ? C12 C7 C8 C21 172.70(15) . . . . ? C7 C8 C9 C10 2.8(3) . . . . ? C21 C8 C9 C10 -173.02(16) . . . . ? C8 C9 C10 C11 -0.4(3) . . . . ? C9 C10 C11 C12 -1.8(3) . . . . ? C10 C11 C12 C7 1.6(3) . . . . ? C10 C11 C12 O7 177.44(16) . . . . ? O6 C7 C12 C11 174.47(15) . . . . ? C8 C7 C12 C11 0.8(3) . . . . ? O6 C7 C12 O7 -1.3(2) . . . . ? C8 C7 C12 O7 -174.96(14) . . . . ? C18 O7 C12 C11 101.18(19) . . . . ? C18 O7 C12 C7 -82.95(19) . . . . ? C16 N1 C13 C14 -0.3(3) . . . . ? C15 N2 C14 O6 -173.90(14) . . . . ? C15 N2 C14 C13 4.4(2) . . . . ? C7 O6 C14 N2 -16.5(2) . . . . ? C7 O6 C14 C13 165.13(15) . . . . ? N1 C13 C14 N2 -2.8(3) . . . . ? N1 C13 C14 O6 175.49(15) . . . . ? C14 N2 C15 O5 177.79(14) . . . . ? C14 N2 C15 C16 -3.2(2) . . . . ? C1 O5 C15 N2 -1.3(2) . . . . ? C1 O5 C15 C16 179.61(15) . . . . ? C13 N1 C16 C15 1.4(3) . . . . ? N2 C15 C16 N1 0.3(3) . . . . ? O5 C15 C16 N1 179.37(16) . . . . ? C20 N3 C17 C18 0.9(2) . . . . ? C19 N4 C18 O7 174.24(14) . . . . ? C19 N4 C18 C17 -5.8(2) . . . . ? C12 O7 C18 N4 1.8(2) . . . . ? C12 O7 C18 C17 -178.18(15) . . . . ? N3 C17 C18 N4 3.6(3) . . . . ? N3 C17 C18 O7 -176.42(15) . . . . ? C18 N4 C19 O8 -175.08(13) . . . . ? C18 N4 C19 C20 3.9(2) . . . . ? C2 O8 C19 N4 -15.7(2) . . . . ? C2 O8 C19 C20 165.31(14) . . . . ? C17 N3 C20 C19 -2.8(2) . . . . ? N4 C19 C20 N3 0.4(3) . . . . ? O8 C19 C20 N3 179.35(14) . . . . ? C9 C8 C21 O4 -172.43(16) . . . . ? C7 C8 C21 O4 11.9(3) . . . . ? C9 C8 C21 O3 9.3(2) . . . . ? C7 C8 C21 O3 -166.40(16) . . . . ? C4 C3 C22 O1 -9.0(3) . . . . ? C2 C3 C22 O1 173.09(17) . . . . ? C4 C3 C22 O2 169.42(16) . . . . ? C2 C3 C22 O2 -8.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.517 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.043 # Attachment '- 3+P.cif' data_z_3 _database_code_depnum_ccdc_archive 'CCDC 825938' #TrackingRef '- 3+P.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H22 N6 O8' _chemical_formula_weight 618.56 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8522(6) _cell_length_b 12.9196(5) _cell_length_c 14.5605(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.9900(10) _cell_angle_gamma 90.00 _cell_volume 2965.77(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9995 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.667 _exptl_crystal_size_mid 0.345 _exptl_crystal_size_min 0.308 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747702 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33650 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5217 _reflns_number_gt 4169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0479P)^2^+1.3451P] 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 5217 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N01 N 0.01670(11) 0.75025(16) 0.56334(12) 0.0547(5) Uani 1 1 d . . . C01 C 0.03691(14) 0.6618(2) 0.52633(16) 0.0612(6) Uani 1 1 d . . . H01A H 0.0252 0.5993 0.5569 0.073 Uiso 1 1 calc R . . C02 C 0.07405(14) 0.6561(2) 0.44593(16) 0.0610(6) Uani 1 1 d . . . H02A H 0.0870 0.5905 0.4215 0.073 Uiso 1 1 calc R . . C03 C 0.09247(13) 0.7440(2) 0.40076(15) 0.0576(6) Uani 1 1 d . . . H03A H 0.1182 0.7409 0.3447 0.069 Uiso 1 1 calc R . . C04 C 0.07291(14) 0.8380(2) 0.43826(17) 0.0633(6) Uani 1 1 d . . . H04A H 0.0851 0.9014 0.4093 0.076 Uiso 1 1 calc R . . C05 C 0.03407(14) 0.8365(2) 0.52143(16) 0.0566(6) Uani 1 1 d . . . H05A H 0.0200 0.9005 0.5481 0.068 Uiso 1 1 calc R . . O1 O 0.36443(8) 0.41155(10) 0.32739(9) 0.0444(3) Uani 1 1 d . . . O2 O 0.11973(8) 0.33591(10) 0.13904(8) 0.0393(3) Uani 1 1 d . . . O3 O 0.19212(8) 0.29756(11) -0.01981(8) 0.0430(3) Uani 1 1 d . . . O4 O 0.42840(8) 0.41726(9) 0.16109(8) 0.0358(3) Uani 1 1 d . . . O5 O 0.55939(14) 0.15428(14) 0.08005(12) 0.0886(7) Uani 1 1 d . . . H5A H 0.5812 0.1583 0.0300 0.133 Uiso 1 1 calc R . . O6 O 0.51312(9) 0.31027(11) 0.03979(10) 0.0523(4) Uani 1 1 d . . . O7 O 0.06530(9) 0.25134(12) 0.29076(9) 0.0534(4) Uani 1 1 d . . . H7B H 0.0773 0.2942 0.2507 0.080 Uiso 1 1 calc R . . O8 O 0.06988(9) 0.08142(12) 0.30799(10) 0.0529(4) Uani 1 1 d . . . N1 N 0.17585(11) 0.56054(13) 0.27454(12) 0.0501(4) Uani 1 1 d . . . N2 N 0.24071(9) 0.36715(11) 0.23804(9) 0.0331(3) Uani 1 1 d . . . N3 N 0.31180(11) 0.52991(13) -0.03809(11) 0.0482(4) Uani 1 1 d . . . N4 N 0.31402(9) 0.35116(11) 0.06802(9) 0.0310(3) Uani 1 1 d . . . C1 C 0.16539(11) 0.39769(14) 0.20175(11) 0.0341(4) Uani 1 1 d . . . C2 C 0.13070(13) 0.49265(15) 0.22087(13) 0.0442(5) Uani 1 1 d . . . H2A H 0.0747 0.5094 0.1957 0.053 Uiso 1 1 calc R . . C3 C 0.25417(13) 0.53315(15) 0.30839(13) 0.0449(5) Uani 1 1 d . . . H3A H 0.2888 0.5803 0.3455 0.054 Uiso 1 1 calc R . . C4 C 0.28478(11) 0.43666(14) 0.28954(11) 0.0358(4) Uani 1 1 d . . . C5 C 0.25456(11) 0.36935(14) -0.00084(11) 0.0329(4) Uani 1 1 d . . . C6 C 0.25283(12) 0.45701(15) -0.05484(13) 0.0420(4) Uani 1 1 d . . . H6A H 0.2093 0.4655 -0.1043 0.050 Uiso 1 1 calc R . . C7 C 0.37072(12) 0.51517(15) 0.03284(13) 0.0429(4) Uani 1 1 d . . . H7A H 0.4132 0.5661 0.0474 0.051 Uiso 1 1 calc R . . C8 C 0.37022(11) 0.42578(13) 0.08540(11) 0.0313(4) Uani 1 1 d . . . C9 C 0.43340(10) 0.32385(13) 0.20969(11) 0.0327(4) Uani 1 1 d . . . C10 C 0.40077(11) 0.32213(14) 0.29396(12) 0.0367(4) Uani 1 1 d . . . C11 C 0.40893(12) 0.23624(17) 0.34990(13) 0.0455(5) Uani 1 1 d . . . H11A H 0.3857 0.2360 0.4075 0.055 Uiso 1 1 calc R . . C12 C 0.45120(12) 0.15033(16) 0.32161(14) 0.0478(5) Uani 1 1 d . . . H12A H 0.4565 0.0902 0.3594 0.057 Uiso 1 1 calc R . . C13 C 0.48564(12) 0.15179(15) 0.23883(13) 0.0426(4) Uani 1 1 d . . . H13A H 0.5156 0.0929 0.2205 0.051 Uiso 1 1 calc R . . C14 C 0.47744(11) 0.23842(14) 0.18115(12) 0.0354(4) Uani 1 1 d . . . C15 C 0.18560(11) 0.21835(14) 0.04369(12) 0.0363(4) Uani 1 1 d . . . C16 C 0.14816(10) 0.23619(14) 0.12435(12) 0.0338(4) Uani 1 1 d . . . C17 C 0.13278(11) 0.15305(14) 0.18205(12) 0.0369(4) Uani 1 1 d . . . C18 C 0.15905(12) 0.05485(15) 0.15739(14) 0.0449(5) Uani 1 1 d . . . H18A H 0.1499 -0.0024 0.1961 0.054 Uiso 1 1 calc R . . C19 C 0.19772(13) 0.03866(16) 0.07861(15) 0.0504(5) Uani 1 1 d . . . H19A H 0.2158 -0.0289 0.0638 0.060 Uiso 1 1 calc R . . C20 C 0.21029(13) 0.12045(16) 0.02103(14) 0.0465(5) Uani 1 1 d . . . H20A H 0.2360 0.1093 -0.0342 0.056 Uiso 1 1 calc R . . C21 C 0.51805(12) 0.23962(15) 0.09323(13) 0.0397(4) Uani 1 1 d . . . C22 C 0.08660(11) 0.15888(16) 0.26645(13) 0.0421(4) Uani 1 1 d . . . N02 N 0.36548(13) -0.15889(15) 0.07319(13) 0.0593(5) Uani 1 1 d . . . C06 C 0.38841(14) -0.10103(19) 0.14588(16) 0.0590(6) Uani 1 1 d . . . H06A H 0.4320 -0.0514 0.1413 0.071 Uiso 1 1 calc R . . C07 C 0.35360(16) -0.1080(2) 0.22693(16) 0.0664(7) Uani 1 1 d . . . H07A H 0.3730 -0.0645 0.2774 0.080 Uiso 1 1 calc R . . C08 C 0.29168(19) -0.1768(3) 0.2351(2) 0.0786(8) Uani 1 1 d . . . H08A H 0.2666 -0.1830 0.2914 0.094 Uiso 1 1 calc R . . C09 C 0.26498(19) -0.2384(2) 0.1603(3) 0.0910(10) Uani 1 1 d . . . H09A H 0.2205 -0.2872 0.1635 0.109 Uiso 1 1 calc R . . C010 C 0.3047(2) -0.22735(19) 0.0800(2) 0.0753(8) Uani 1 1 d . . . H01B H 0.2875 -0.2704 0.0286 0.090 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 N01 0.0430(10) 0.0751(13) 0.0456(10) 0.0006(9) 0.0027(8) 0.0061(9) C01 0.0503(13) 0.0751(16) 0.0589(14) 0.0016(12) 0.0095(11) 0.0123(11) C02 0.0514(13) 0.0777(17) 0.0554(13) -0.0069(12) 0.0124(11) 0.0113(12) C03 0.0420(12) 0.0828(17) 0.0494(12) -0.0062(12) 0.0117(9) 0.0072(11) C04 0.0493(13) 0.0755(16) 0.0644(15) 0.0055(12) 0.0021(11) -0.0037(12) C05 0.0464(12) 0.0663(15) 0.0562(13) -0.0158(11) 0.0014(10) 0.0032(11) O1 0.0397(7) 0.0537(8) 0.0383(7) -0.0111(6) -0.0035(6) -0.0011(6) O2 0.0351(7) 0.0423(7) 0.0389(7) -0.0022(6) -0.0041(5) 0.0062(5) O3 0.0391(7) 0.0563(8) 0.0320(6) 0.0054(6) -0.0039(5) -0.0112(6) O4 0.0395(7) 0.0315(6) 0.0341(6) 0.0023(5) -0.0069(5) -0.0026(5) O5 0.1363(17) 0.0798(12) 0.0551(10) 0.0178(9) 0.0362(11) 0.0637(12) O6 0.0635(9) 0.0484(8) 0.0478(8) 0.0089(7) 0.0198(7) 0.0048(7) O7 0.0583(9) 0.0615(9) 0.0423(8) 0.0061(7) 0.0146(7) 0.0058(7) O8 0.0472(8) 0.0633(9) 0.0486(8) 0.0111(7) 0.0078(6) -0.0119(7) N1 0.0564(11) 0.0444(9) 0.0511(10) -0.0073(8) 0.0126(8) 0.0072(8) N2 0.0336(8) 0.0391(8) 0.0270(7) -0.0024(6) 0.0045(6) 0.0024(6) N3 0.0560(10) 0.0426(9) 0.0434(9) 0.0112(7) -0.0079(8) -0.0018(8) N4 0.0309(7) 0.0361(8) 0.0263(7) -0.0003(6) 0.0037(6) 0.0013(6) C1 0.0348(9) 0.0402(10) 0.0282(8) 0.0012(7) 0.0072(7) 0.0014(8) C2 0.0422(11) 0.0469(11) 0.0445(11) 0.0002(9) 0.0091(8) 0.0087(9) C3 0.0518(12) 0.0447(11) 0.0391(10) -0.0092(8) 0.0094(9) -0.0026(9) C4 0.0376(10) 0.0448(10) 0.0258(8) -0.0023(7) 0.0073(7) -0.0022(8) C5 0.0311(9) 0.0419(10) 0.0261(8) -0.0024(7) 0.0050(7) 0.0008(7) C6 0.0420(10) 0.0478(11) 0.0344(10) 0.0043(8) -0.0045(8) 0.0043(9) C7 0.0472(11) 0.0371(10) 0.0424(10) 0.0056(8) -0.0050(8) -0.0047(8) C8 0.0315(9) 0.0336(9) 0.0285(8) -0.0010(7) 0.0016(7) 0.0022(7) C9 0.0302(9) 0.0345(9) 0.0315(9) 0.0045(7) -0.0057(7) -0.0048(7) C10 0.0297(9) 0.0446(10) 0.0344(9) -0.0012(8) -0.0035(7) -0.0020(8) C11 0.0358(10) 0.0638(13) 0.0360(10) 0.0094(9) -0.0001(8) -0.0064(9) C12 0.0445(11) 0.0506(12) 0.0466(11) 0.0192(9) -0.0028(9) -0.0021(9) C13 0.0405(10) 0.0385(10) 0.0469(11) 0.0071(8) -0.0042(8) 0.0014(8) C14 0.0327(9) 0.0375(10) 0.0344(9) 0.0035(7) -0.0049(7) -0.0006(7) C15 0.0302(9) 0.0463(11) 0.0314(9) -0.0003(8) -0.0010(7) -0.0070(8) C16 0.0258(8) 0.0396(10) 0.0346(9) -0.0023(7) -0.0036(7) 0.0004(7) C17 0.0278(9) 0.0477(11) 0.0340(9) 0.0007(8) -0.0023(7) -0.0035(8) C18 0.0427(11) 0.0414(11) 0.0493(11) 0.0032(9) -0.0019(9) -0.0042(9) C19 0.0509(12) 0.0445(11) 0.0554(13) -0.0083(10) 0.0041(10) 0.0034(9) C20 0.0419(11) 0.0562(12) 0.0417(10) -0.0114(9) 0.0062(8) -0.0008(9) C21 0.0392(10) 0.0411(10) 0.0375(10) 0.0003(8) -0.0028(8) 0.0043(8) C22 0.0319(10) 0.0539(12) 0.0389(10) 0.0015(9) -0.0033(8) -0.0014(9) N02 0.0663(12) 0.0586(12) 0.0533(11) -0.0041(9) 0.0077(9) 0.0250(10) C06 0.0455(12) 0.0664(15) 0.0647(15) -0.0042(12) 0.0034(11) 0.0080(11) C07 0.0642(16) 0.0832(18) 0.0505(13) -0.0096(12) -0.0003(12) 0.0202(14) C08 0.0689(17) 0.099(2) 0.0705(17) 0.0312(16) 0.0186(14) 0.0269(17) C09 0.0690(18) 0.0665(18) 0.134(3) 0.0411(19) -0.0048(19) -0.0079(14) C010 0.102(2) 0.0420(13) 0.0756(18) -0.0066(12) -0.0220(16) 0.0163(14) _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 N01 C05 1.313(3) . ? N01 C01 1.317(3) . ? C01 C02 1.366(3) . ? C01 H01A 0.9500 . ? C02 C03 1.360(3) . ? C02 H02A 0.9500 . ? C03 C04 1.380(3) . ? C03 H03A 0.9500 . ? C04 C05 1.415(3) . ? C04 H04A 0.9500 . ? C05 H05A 0.9500 . ? O1 C4 1.363(2) . ? O1 C10 1.401(2) . ? O2 C1 1.363(2) . ? O2 C16 1.389(2) . ? O3 C5 1.364(2) . ? O3 C15 1.390(2) . ? O4 C8 1.366(2) . ? O4 C9 1.397(2) . ? O5 C21 1.307(2) . ? O5 H5A 0.8400 . ? O6 C21 1.197(2) . ? O7 C22 1.300(2) . ? O7 H7B 0.8400 . ? O8 C22 1.213(2) . ? N1 C2 1.332(3) . ? N1 C3 1.335(3) . ? N2 C1 1.315(2) . ? N2 C4 1.322(2) . ? N3 C6 1.331(2) . ? N3 C7 1.332(2) . ? N4 C8 1.319(2) . ? N4 C5 1.324(2) . ? C1 C2 1.385(3) . ? C2 H2A 0.9500 . ? C3 C4 1.376(3) . ? C3 H3A 0.9500 . ? C5 C6 1.377(2) . ? C6 H6A 0.9500 . ? C7 C8 1.386(2) . ? C7 H7A 0.9500 . ? C9 C10 1.381(2) . ? C9 C14 1.392(3) . ? C10 C11 1.375(3) . ? C11 C12 1.381(3) . ? C11 H11A 0.9500 . ? C12 C13 1.374(3) . ? C12 H12A 0.9500 . ? C13 C14 1.397(2) . ? C13 H13A 0.9500 . ? C14 C21 1.492(3) . ? C15 C20 1.374(3) . ? C15 C16 1.389(2) . ? C16 C17 1.401(2) . ? C17 C18 1.394(3) . ? C17 C22 1.497(3) . ? C18 C19 1.372(3) . ? C18 H18A 0.9500 . ? C19 C20 1.376(3) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? N02 C06 1.316(3) . ? N02 C010 1.319(4) . ? C06 C07 1.357(3) . ? C06 H06A 0.9500 . ? C07 C08 1.338(4) . ? C07 H07A 0.9500 . ? C08 C09 1.380(4) . ? C08 H08A 0.9500 . ? C09 C010 1.391(4) . ? C09 H09A 0.9500 . ? C010 H01B 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 C05 N01 C01 118.32(19) . . ? N01 C01 C02 122.8(2) . . ? N01 C01 H01A 118.6 . . ? C02 C01 H01A 118.6 . . ? C03 C02 C01 120.2(2) . . ? C03 C02 H02A 119.9 . . ? C01 C02 H02A 119.9 . . ? C02 C03 C04 118.4(2) . . ? C02 C03 H03A 120.8 . . ? C04 C03 H03A 120.8 . . ? C03 C04 C05 117.5(2) . . ? C03 C04 H04A 121.2 . . ? C05 C04 H04A 121.2 . . ? N01 C05 C04 122.7(2) . . ? N01 C05 H05A 118.6 . . ? C04 C05 H05A 118.6 . . ? C4 O1 C10 116.93(13) . . ? C1 O2 C16 119.24(13) . . ? C5 O3 C15 117.95(13) . . ? C8 O4 C9 118.43(13) . . ? C21 O5 H5A 109.5 . . ? C22 O7 H7B 109.5 . . ? C2 N1 C3 117.65(17) . . ? C1 N2 C4 115.34(15) . . ? C6 N3 C7 117.58(16) . . ? C8 N4 C5 115.40(15) . . ? N2 C1 O2 119.34(15) . . ? N2 C1 C2 123.24(17) . . ? O2 C1 C2 117.36(16) . . ? N1 C2 C1 120.07(18) . . ? N1 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? N1 C3 C4 120.03(18) . . ? N1 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? N2 C4 O1 118.69(16) . . ? N2 C4 C3 123.52(17) . . ? O1 C4 C3 117.78(17) . . ? N4 C5 O3 118.50(15) . . ? N4 C5 C6 123.27(16) . . ? O3 C5 C6 118.22(15) . . ? N3 C6 C5 120.35(17) . . ? N3 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? N3 C7 C8 120.23(17) . . ? N3 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? N4 C8 O4 118.79(14) . . ? N4 C8 C7 123.07(16) . . ? O4 C8 C7 118.07(15) . . ? C10 C9 C14 119.90(16) . . ? C10 C9 O4 117.22(15) . . ? C14 C9 O4 122.50(15) . . ? C11 C10 C9 121.26(17) . . ? C11 C10 O1 118.46(16) . . ? C9 C10 O1 120.09(16) . . ? C10 C11 C12 119.36(17) . . ? C10 C11 H11A 120.3 . . ? C12 C11 H11A 120.3 . . ? C13 C12 C11 120.00(18) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 121.18(18) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C9 C14 C13 118.27(16) . . ? C9 C14 C21 121.50(16) . . ? C13 C14 C21 120.19(17) . . ? C20 C15 C16 120.87(17) . . ? C20 C15 O3 118.36(16) . . ? C16 C15 O3 120.54(16) . . ? O2 C16 C15 117.27(16) . . ? O2 C16 C17 122.65(15) . . ? C15 C16 C17 119.75(16) . . ? C18 C17 C16 117.91(17) . . ? C18 C17 C22 116.24(17) . . ? C16 C17 C22 125.78(17) . . ? C19 C18 C17 121.72(19) . . ? C19 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? C18 C19 C20 119.87(19) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C15 C20 C19 119.83(18) . . ? C15 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? O6 C21 O5 123.21(18) . . ? O6 C21 C14 124.14(17) . . ? O5 C21 C14 112.65(16) . . ? O8 C22 O7 123.07(18) . . ? O8 C22 C17 121.27(18) . . ? O7 C22 C17 115.65(17) . . ? C06 N02 C010 117.6(2) . . ? N02 C06 C07 124.0(2) . . ? N02 C06 H06A 118.0 . . ? C07 C06 H06A 118.0 . . ? C08 C07 C06 119.4(3) . . ? C08 C07 H07A 120.3 . . ? C06 C07 H07A 120.3 . . ? C07 C08 C09 118.7(3) . . ? C07 C08 H08A 120.7 . . ? C09 C08 H08A 120.7 . . ? C08 C09 C010 118.4(3) . . ? C08 C09 H09A 120.8 . . ? C010 C09 H09A 120.8 . . ? N02 C010 C09 122.0(3) . . ? N02 C010 H01B 119.0 . . ? C09 C010 H01B 119.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C05 N01 C01 C02 -0.8(3) . . . . ? N01 C01 C02 C03 0.6(4) . . . . ? C01 C02 C03 C04 0.1(3) . . . . ? C02 C03 C04 C05 -0.5(3) . . . . ? C01 N01 C05 C04 0.4(3) . . . . ? C03 C04 C05 N01 0.2(3) . . . . ? C4 N2 C1 O2 172.25(14) . . . . ? C4 N2 C1 C2 -4.8(2) . . . . ? C16 O2 C1 N2 8.9(2) . . . . ? C16 O2 C1 C2 -173.87(15) . . . . ? C3 N1 C2 C1 -0.2(3) . . . . ? N2 C1 C2 N1 3.7(3) . . . . ? O2 C1 C2 N1 -173.41(16) . . . . ? C2 N1 C3 C4 -1.7(3) . . . . ? C1 N2 C4 O1 -178.20(14) . . . . ? C1 N2 C4 C3 2.8(2) . . . . ? C10 O1 C4 N2 12.8(2) . . . . ? C10 O1 C4 C3 -168.16(16) . . . . ? N1 C3 C4 N2 0.5(3) . . . . ? N1 C3 C4 O1 -178.58(16) . . . . ? C8 N4 C5 O3 -177.01(14) . . . . ? C8 N4 C5 C6 3.4(2) . . . . ? C15 O3 C5 N4 11.1(2) . . . . ? C15 O3 C5 C6 -169.31(16) . . . . ? C7 N3 C6 C5 -1.0(3) . . . . ? N4 C5 C6 N3 -1.4(3) . . . . ? O3 C5 C6 N3 179.06(16) . . . . ? C6 N3 C7 C8 1.0(3) . . . . ? C5 N4 C8 O4 173.53(14) . . . . ? C5 N4 C8 C7 -3.3(2) . . . . ? C9 O4 C8 N4 8.6(2) . . . . ? C9 O4 C8 C7 -174.38(16) . . . . ? N3 C7 C8 N4 1.2(3) . . . . ? N3 C7 C8 O4 -175.69(17) . . . . ? C8 O4 C9 C10 -106.08(17) . . . . ? C8 O4 C9 C14 81.1(2) . . . . ? C14 C9 C10 C11 -1.7(3) . . . . ? O4 C9 C10 C11 -174.75(15) . . . . ? C14 C9 C10 O1 173.17(15) . . . . ? O4 C9 C10 O1 0.1(2) . . . . ? C4 O1 C10 C11 -107.96(18) . . . . ? C4 O1 C10 C9 77.0(2) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? O1 C10 C11 C12 -174.40(16) . . . . ? C10 C11 C12 C13 0.9(3) . . . . ? C11 C12 C13 C14 -1.2(3) . . . . ? C10 C9 C14 C13 1.3(2) . . . . ? O4 C9 C14 C13 174.03(15) . . . . ? C10 C9 C14 C21 -176.32(15) . . . . ? O4 C9 C14 C21 -3.6(3) . . . . ? C12 C13 C14 C9 0.1(3) . . . . ? C12 C13 C14 C21 177.79(17) . . . . ? C5 O3 C15 C20 -107.46(19) . . . . ? C5 O3 C15 C16 78.1(2) . . . . ? C1 O2 C16 C15 -104.63(18) . . . . ? C1 O2 C16 C17 82.0(2) . . . . ? C20 C15 C16 O2 -175.66(16) . . . . ? O3 C15 C16 O2 -1.3(2) . . . . ? C20 C15 C16 C17 -2.1(3) . . . . ? O3 C15 C16 C17 172.26(15) . . . . ? O2 C16 C17 C18 175.63(16) . . . . ? C15 C16 C17 C18 2.4(2) . . . . ? O2 C16 C17 C22 -1.3(3) . . . . ? C15 C16 C17 C22 -174.52(16) . . . . ? C16 C17 C18 C19 -0.9(3) . . . . ? C22 C17 C18 C19 176.28(17) . . . . ? C17 C18 C19 C20 -0.9(3) . . . . ? C16 C15 C20 C19 0.2(3) . . . . ? O3 C15 C20 C19 -174.27(17) . . . . ? C18 C19 C20 C15 1.3(3) . . . . ? C9 C14 C21 O6 -3.3(3) . . . . ? C13 C14 C21 O6 179.12(19) . . . . ? C9 C14 C21 O5 177.30(18) . . . . ? C13 C14 C21 O5 -0.3(3) . . . . ? C18 C17 C22 O8 -3.3(3) . . . . ? C16 C17 C22 O8 173.67(17) . . . . ? C18 C17 C22 O7 177.46(16) . . . . ? C16 C17 C22 O7 -5.6(3) . . . . ? C010 N02 C06 C07 0.3(3) . . . . ? N02 C06 C07 C08 -0.5(4) . . . . ? C06 C07 C08 C09 -0.2(4) . . . . ? C07 C08 C09 C010 1.0(4) . . . . ? C06 N02 C010 C09 0.6(3) . . . . ? C08 C09 C010 N02 -1.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.457 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.038 # Attachment '- 3+G.cif' data_z_2 _database_code_depnum_ccdc_archive 'CCDC 825939' #TrackingRef '- 3+G.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H11 N5 O4' _chemical_formula_weight 289.26 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 17.3714(7) _cell_length_b 24.5657(6) _cell_length_c 12.4327(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5305.5(3) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9950 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 28.18 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9449 _exptl_absorpt_correction_T_max 0.9866 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14917 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2342 _reflns_number_gt 2287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0432P)^2^+1.7847P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.1(7) _refine_ls_number_reflns 2342 _refine_ls_number_parameters 190 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _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 O1 O 0.26396(7) 0.52497(4) 0.34271(9) 0.0547(3) Uani 1 1 d . . . O2 O 0.21143(6) 0.55433(4) 0.19233(9) 0.0468(3) Uani 1 1 d . . . O3 O 0.14730(5) 0.47305(4) 0.46565(8) 0.0396(2) Uani 1 1 d . . . O4 O 0.03833(6) 0.39276(4) 0.45380(9) 0.0474(3) Uani 1 1 d . . . N1 N 0.05772(6) 0.54210(4) 0.45423(9) 0.0325(2) Uani 1 1 d . . . N2 N 0.07800(7) 0.56099(5) 0.67255(10) 0.0414(3) Uani 1 1 d . . . C1 C 0.21527(7) 0.52216(5) 0.27023(11) 0.0340(3) Uani 1 1 d . . . C2 C 0.15675(7) 0.47606(5) 0.27085(11) 0.0322(3) Uani 1 1 d . . . C3 C 0.13464(9) 0.45284(6) 0.17385(12) 0.0408(3) Uani 1 1 d . . . H3C H 0.1562 0.4657 0.1103 0.049 Uiso 1 1 calc R . . C4 C 0.08139(10) 0.41098(6) 0.16925(14) 0.0479(4) Uani 1 1 d . . . H4C H 0.0688 0.3953 0.1035 0.058 Uiso 1 1 calc R . . C5 C 0.04706(8) 0.39250(6) 0.26246(14) 0.0457(3) Uani 1 1 d . . . H5C H 0.0102 0.3651 0.2597 0.055 Uiso 1 1 calc R . . C6 C 0.06782(7) 0.41491(5) 0.35880(12) 0.0374(3) Uani 1 1 d . . . C7 C 0.12337(7) 0.45590(5) 0.36446(11) 0.0322(3) Uani 1 1 d . . . C8 C 0.10719(7) 0.51393(5) 0.51282(11) 0.0316(3) Uani 1 1 d . . . C9 C 0.11848(8) 0.52278(6) 0.62179(12) 0.0382(3) Uani 1 1 d . . . H9A H 0.1543 0.5020 0.6594 0.046 Uiso 1 1 calc R . . C10 C 0.02714(8) 0.58921(6) 0.61541(13) 0.0404(3) Uani 1 1 d . . . H10A H -0.0019 0.6162 0.6485 0.049 Uiso 1 1 calc R . . C11 C -0.01702(7) 0.42130(5) 0.50721(12) 0.0348(3) Uani 1 1 d . . . N3 N 0.10376(7) 0.62411(5) 0.07041(11) 0.0459(3) Uani 1 1 d . . . H3A H 0.0735 0.6517 0.0743 0.055 Uiso 1 1 calc R . . H3B H 0.1288 0.6137 0.1264 0.055 Uiso 1 1 calc R . . N4 N 0.07350(8) 0.61371(6) -0.10691(11) 0.0510(3) Uani 1 1 d . . . H4A H 0.0432 0.6413 -0.1031 0.061 Uiso 1 1 calc R . . H4B H 0.0788 0.5965 -0.1667 0.061 Uiso 1 1 calc R . . N5 N 0.16065(8) 0.55626(5) -0.02576(11) 0.0465(3) Uani 1 1 d . . . H5A H 0.1677 0.5393 -0.0854 0.056 Uiso 1 1 calc R . . H5B H 0.1852 0.5464 0.0310 0.056 Uiso 1 1 calc R . . C12 C 0.11176(7) 0.59779(5) -0.02134(11) 0.0363(3) 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 O1 0.0574(6) 0.0517(6) 0.0550(7) 0.0157(5) -0.0225(6) -0.0162(5) O2 0.0504(6) 0.0453(5) 0.0448(5) 0.0150(5) -0.0090(5) -0.0100(5) O3 0.0460(5) 0.0425(5) 0.0304(5) -0.0004(4) -0.0018(4) 0.0151(4) O4 0.0412(5) 0.0449(5) 0.0562(7) 0.0205(5) 0.0172(5) 0.0138(4) N1 0.0317(5) 0.0310(5) 0.0349(6) -0.0034(4) -0.0017(4) -0.0007(4) N2 0.0406(6) 0.0460(6) 0.0377(6) -0.0089(5) -0.0004(5) -0.0034(5) C1 0.0349(6) 0.0309(6) 0.0361(7) 0.0024(5) -0.0001(6) 0.0016(5) C2 0.0331(6) 0.0280(6) 0.0355(7) 0.0010(5) 0.0004(6) 0.0045(5) C3 0.0485(8) 0.0400(7) 0.0338(7) 0.0011(6) 0.0026(6) -0.0029(6) C4 0.0559(9) 0.0452(8) 0.0427(8) -0.0066(7) -0.0065(7) -0.0068(7) C5 0.0394(7) 0.0378(7) 0.0601(10) 0.0031(7) -0.0055(7) -0.0056(6) C6 0.0308(6) 0.0342(6) 0.0470(8) 0.0090(6) 0.0075(6) 0.0080(5) C7 0.0334(6) 0.0308(6) 0.0324(6) 0.0006(5) 0.0017(5) 0.0102(5) C8 0.0306(6) 0.0297(6) 0.0346(7) 0.0006(5) 0.0020(5) 0.0002(4) C9 0.0412(7) 0.0400(7) 0.0333(7) -0.0007(6) -0.0027(6) 0.0009(5) C10 0.0354(6) 0.0414(7) 0.0444(8) -0.0144(6) 0.0003(6) -0.0003(6) C11 0.0273(6) 0.0306(6) 0.0466(7) 0.0093(5) 0.0038(5) -0.0005(5) N3 0.0525(7) 0.0517(7) 0.0335(6) -0.0053(5) -0.0047(5) 0.0128(6) N4 0.0622(8) 0.0565(7) 0.0342(6) -0.0057(6) -0.0072(6) 0.0202(6) N5 0.0570(7) 0.0441(7) 0.0385(6) -0.0014(6) 0.0008(5) 0.0126(6) C12 0.0379(7) 0.0357(7) 0.0352(6) 0.0016(5) 0.0039(6) 0.0002(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 O1 C1 1.2379(16) . ? O2 C1 1.2518(17) . ? O3 C8 1.3556(16) . ? O3 C7 1.3904(17) . ? O4 C11 1.3627(17) . ? O4 C6 1.3977(18) . ? N1 C11 1.3198(16) 2_565 ? N1 C8 1.3221(17) . ? N2 C10 1.3289(19) . ? N2 C9 1.3320(18) . ? C1 C2 1.5218(18) . ? C2 C3 1.388(2) . ? C2 C7 1.3914(19) . ? C3 C4 1.384(2) . ? C3 H3C 0.9300 . ? C4 C5 1.380(2) . ? C4 H4C 0.9300 . ? C5 C6 1.367(2) . ? C5 H5C 0.9300 . ? C6 C7 1.3964(19) . ? C8 C9 1.3861(19) . ? C9 H9A 0.9300 . ? C10 C11 1.381(2) 2_565 ? C10 H10A 0.9300 . ? C11 N1 1.3198(16) 2_565 ? C11 C10 1.381(2) 2_565 ? N3 C12 1.3185(19) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C12 1.3139(18) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 C12 1.3286(18) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? 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 C8 O3 C7 117.53(9) . . ? C11 O4 C6 118.04(10) . . ? C11 N1 C8 115.45(12) 2_565 . ? C10 N2 C9 117.73(12) . . ? O1 C1 O2 124.36(13) . . ? O1 C1 C2 119.62(12) . . ? O2 C1 C2 115.99(12) . . ? C3 C2 C7 117.72(11) . . ? C3 C2 C1 119.09(12) . . ? C7 C2 C1 123.20(12) . . ? C4 C3 C2 121.73(14) . . ? C4 C3 H3C 119.1 . . ? C2 C3 H3C 119.1 . . ? C5 C4 C3 119.89(15) . . ? C5 C4 H4C 120.1 . . ? C3 C4 H4C 120.1 . . ? C6 C5 C4 119.30(12) . . ? C6 C5 H5C 120.3 . . ? C4 C5 H5C 120.3 . . ? C5 C6 C7 121.13(13) . . ? C5 C6 O4 119.15(12) . . ? C7 C6 O4 119.44(13) . . ? O3 C7 C2 121.63(12) . . ? O3 C7 C6 118.08(12) . . ? C2 C7 C6 120.16(13) . . ? N1 C8 O3 118.91(12) . . ? N1 C8 C9 123.26(12) . . ? O3 C8 C9 117.79(12) . . ? N2 C9 C8 119.93(13) . . ? N2 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? N2 C10 C11 120.52(13) . 2_565 ? N2 C10 H10A 119.7 . . ? C11 C10 H10A 119.7 2_565 . ? N1 C11 O4 119.03(12) 2_565 . ? N1 C11 C10 123.05(13) 2_565 2_565 ? O4 C11 C10 117.91(12) . 2_565 ? C12 N3 H3A 120.0 . . ? C12 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C12 N4 H4A 120.0 . . ? C12 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C12 N5 H5A 120.0 . . ? C12 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? N4 C12 N3 120.08(12) . . ? N4 C12 N5 121.23(13) . . ? N3 C12 N5 118.66(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -142.67(14) . . . . ? O2 C1 C2 C3 35.39(18) . . . . ? O1 C1 C2 C7 37.78(19) . . . . ? O2 C1 C2 C7 -144.16(13) . . . . ? C7 C2 C3 C4 -0.1(2) . . . . ? C1 C2 C3 C4 -179.68(13) . . . . ? C2 C3 C4 C5 2.0(2) . . . . ? C3 C4 C5 C6 -1.8(2) . . . . ? C4 C5 C6 C7 -0.3(2) . . . . ? C4 C5 C6 O4 -174.14(13) . . . . ? C11 O4 C6 C5 -106.52(15) . . . . ? C11 O4 C6 C7 79.58(15) . . . . ? C8 O3 C7 C2 95.31(14) . . . . ? C8 O3 C7 C6 -88.78(13) . . . . ? C3 C2 C7 O3 173.81(11) . . . . ? C1 C2 C7 O3 -6.63(17) . . . . ? C3 C2 C7 C6 -2.02(17) . . . . ? C1 C2 C7 C6 177.54(11) . . . . ? C5 C6 C7 O3 -173.68(11) . . . . ? O4 C6 C7 O3 0.10(16) . . . . ? C5 C6 C7 C2 2.29(18) . . . . ? O4 C6 C7 C2 176.07(11) . . . . ? C11 N1 C8 O3 175.53(11) 2_565 . . . ? C11 N1 C8 C9 -2.15(18) 2_565 . . . ? C7 O3 C8 N1 -12.53(17) . . . . ? C7 O3 C8 C9 165.29(12) . . . . ? C10 N2 C9 C8 0.53(19) . . . . ? N1 C8 C9 N2 0.5(2) . . . . ? O3 C8 C9 N2 -177.22(12) . . . . ? C9 N2 C10 C11 0.2(2) . . . 2_565 ? C6 O4 C11 N1 21.37(19) . . . 2_565 ? C6 O4 C11 C10 -157.87(13) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.131 _refine_diff_density_min -0.124 _refine_diff_density_rms 0.028 # Attachment '- 7.cif' data_z_4 _database_code_depnum_ccdc_archive 'CCDC 825940' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H33 Ag B F4 N7 O10' _chemical_formula_weight 894.35 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' B B 0.0013 0.0007 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.4288(8) _cell_length_b 14.0202(6) _cell_length_c 14.9352(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.3390(10) _cell_angle_gamma 90.00 _cell_volume 3783.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9836 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7274 _exptl_absorpt_correction_T_max 0.8127 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42908 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0124 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6662 _reflns_number_gt 6208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0480P)^2^+5.7831P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6662 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Ag1 Ag 0.011826(10) 0.262473(16) 0.467128(13) 0.03102(9) Uani 1 1 d . . . O1 O 0.40206(14) 0.79714(18) 0.4997(2) 0.0742(9) Uani 1 1 d . . . O2 O 0.28539(12) 0.78662(16) 0.42867(16) 0.0422(5) Uani 1 1 d . . . O3 O 0.32046(12) 0.27267(15) 0.69849(16) 0.0415(5) Uani 1 1 d . . . O4 O 0.44070(15) 0.27317(18) 0.7042(3) 0.0786(10) Uani 1 1 d . . . O5 O 0.22950(9) 0.60581(13) 0.41209(11) 0.0274(4) Uani 1 1 d . . . O6 O 0.26393(10) 0.63062(13) 0.72551(12) 0.0312(4) Uani 1 1 d . . . O7 O 0.24926(9) 0.44041(13) 0.69067(11) 0.0260(4) Uani 1 1 d . . . O8 O 0.26231(10) 0.42052(13) 0.38471(12) 0.0289(4) Uani 1 1 d . . . N1 N 0.10615(12) 0.68628(16) 0.55232(15) 0.0292(5) Uani 1 1 d . . . N2 N 0.25077(11) 0.62461(14) 0.56893(14) 0.0242(4) Uani 1 1 d . . . N3 N 0.12064(12) 0.34547(16) 0.50210(14) 0.0278(5) Uani 1 1 d . . . N4 N 0.26084(11) 0.42533(14) 0.53937(14) 0.0237(4) Uani 1 1 d . . . C1 C 0.20583(14) 0.63328(17) 0.48858(16) 0.0243(5) Uani 1 1 d . . . C2 C 0.13338(14) 0.66487(19) 0.47819(18) 0.0292(5) Uani 1 1 d . . . H2A H 0.1034 0.6712 0.4190 0.035 Uiso 1 1 calc R . . C3 C 0.14948(14) 0.67484(18) 0.63483(17) 0.0280(5) Uani 1 1 d . . . H3A H 0.1311 0.6883 0.6886 0.034 Uiso 1 1 calc R . . C4 C 0.22133(14) 0.64317(17) 0.64086(16) 0.0246(5) Uani 1 1 d . . . C5 C 0.22654(14) 0.40392(17) 0.45552(16) 0.0244(5) Uani 1 1 d . . . C6 C 0.15656(14) 0.36443(18) 0.43458(17) 0.0270(5) Uani 1 1 d . . . H6A H 0.1342 0.3509 0.3730 0.032 Uiso 1 1 calc R . . C7 C 0.15252(14) 0.36914(18) 0.58750(17) 0.0267(5) Uani 1 1 d . . . H7A H 0.1277 0.3576 0.6365 0.032 Uiso 1 1 calc R . . C8 C 0.22236(13) 0.41077(17) 0.60382(16) 0.0228(5) Uani 1 1 d . . . C9 C 0.36040(15) 0.64964(19) 0.43341(18) 0.0302(6) Uani 1 1 d . . . C10 C 0.30375(14) 0.58229(18) 0.41763(16) 0.0249(5) Uani 1 1 d . . . C11 C 0.31908(14) 0.48793(18) 0.40023(16) 0.0262(5) Uani 1 1 d . . . C12 C 0.38931(15) 0.4602(2) 0.39268(18) 0.0317(6) Uani 1 1 d . . . H12A H 0.3990 0.3960 0.3784 0.038 Uiso 1 1 calc R . . C13 C 0.44562(16) 0.5272(2) 0.4062(2) 0.0367(6) Uani 1 1 d . . . H13A H 0.4942 0.5092 0.4005 0.044 Uiso 1 1 calc R . . C14 C 0.43154(16) 0.6198(2) 0.4279(2) 0.0369(6) Uani 1 1 d . . . H14A H 0.4711 0.6644 0.4394 0.044 Uiso 1 1 calc R . . C15 C 0.38398(14) 0.41976(18) 0.72617(16) 0.0268(5) Uani 1 1 d . . . C16 C 0.45254(15) 0.4633(2) 0.75615(19) 0.0331(6) Uani 1 1 d . . . H16A H 0.4961 0.4254 0.7657 0.040 Uiso 1 1 calc R . . C17 C 0.45856(15) 0.5602(2) 0.77231(19) 0.0360(6) Uani 1 1 d . . . H17A H 0.5059 0.5884 0.7919 0.043 Uiso 1 1 calc R . . C18 C 0.39578(16) 0.6163(2) 0.76003(18) 0.0336(6) Uani 1 1 d . . . H18A H 0.3996 0.6830 0.7712 0.040 Uiso 1 1 calc R . . C19 C 0.32723(14) 0.57426(18) 0.73123(16) 0.0268(5) Uani 1 1 d . . . C20 C 0.32092(14) 0.47681(18) 0.71360(16) 0.0246(5) Uani 1 1 d . . . C21 C 0.35071(17) 0.7518(2) 0.4570(2) 0.0369(7) Uani 1 1 d . . . C22 C 0.38473(15) 0.3142(2) 0.70878(19) 0.0343(6) Uani 1 1 d . . . B1 B 0.01626(18) 0.2669(3) 0.7336(2) 0.0371(7) Uani 1 1 d . . . F4 F 0.01379(11) 0.23657(14) 0.64512(11) 0.0452(4) Uani 1 1 d . . . F3 F 0.08463(12) 0.3003(2) 0.77032(14) 0.0698(7) Uani 1 1 d . . . F2 F 0.00590(14) 0.18590(19) 0.78689(14) 0.0732(7) Uani 1 1 d . . . F1 F -0.04057(15) 0.3257(2) 0.73880(17) 0.0989(10) Uani 1 1 d . . . O01 O 0.27146(12) 0.96911(17) 0.44476(18) 0.0524(6) Uani 1 1 d . . . O02 O 0.32016(12) 0.40865(14) 0.17503(16) 0.0436(5) Uani 1 1 d . . . N01 N 0.30167(15) 1.12379(19) 0.43161(18) 0.0437(6) Uani 1 1 d . . . N02 N 0.24678(15) 0.53986(17) 0.17652(17) 0.0412(6) Uani 1 1 d . . . C01 C 0.3196(2) 1.0344(2) 0.4567(2) 0.0438(7) Uani 1 1 d . . . C02 C 0.39812(19) 1.0244(3) 0.4976(3) 0.0530(8) Uani 1 1 d . . . H02A H 0.4233 0.9812 0.4610 0.064 Uiso 1 1 calc R . . H02B H 0.4049 0.9998 0.5608 0.064 Uiso 1 1 calc R . . C03 C 0.4282(2) 1.1292(3) 0.4962(3) 0.0696(11) Uani 1 1 d . . . H03A H 0.4501 1.1508 0.5588 0.083 Uiso 1 1 calc R . . H03B H 0.4664 1.1332 0.4581 0.083 Uiso 1 1 calc R . . C04 C 0.3628(2) 1.1883(3) 0.4567(2) 0.0532(8) Uani 1 1 d . . . H04A H 0.3524 1.2351 0.5021 0.064 Uiso 1 1 calc R . . H04B H 0.3719 1.2233 0.4023 0.064 Uiso 1 1 calc R . . C05 C 0.22938(18) 1.1525(2) 0.3880(2) 0.0494(8) Uani 1 1 d . . . H05A H 0.1969 1.0966 0.3780 0.074 Uiso 1 1 calc R . . H05B H 0.2314 1.1822 0.3292 0.074 Uiso 1 1 calc R . . H05C H 0.2100 1.1985 0.4268 0.074 Uiso 1 1 calc R . . C06 C 0.25775(19) 0.4470(2) 0.17286(19) 0.0393(7) Uani 1 1 d . . . C07 C 0.18502(18) 0.3945(2) 0.1644(2) 0.0455(7) Uani 1 1 d . . . H07A H 0.1888 0.3423 0.2098 0.055 Uiso 1 1 calc R . . H07B H 0.1690 0.3676 0.1024 0.055 Uiso 1 1 calc R . . C08 C 0.1319(2) 0.4719(3) 0.1834(3) 0.0603(10) Uani 1 1 d . . . H08A H 0.0834 0.4661 0.1412 0.072 Uiso 1 1 calc R . . H08B H 0.1242 0.4678 0.2470 0.072 Uiso 1 1 calc R . . C09 C 0.1699(2) 0.5652(3) 0.1674(3) 0.0534(9) Uani 1 1 d . . . H09A H 0.1499 0.5907 0.1057 0.064 Uiso 1 1 calc R . . H09B H 0.1633 0.6136 0.2135 0.064 Uiso 1 1 calc R . . C010 C 0.3042(2) 0.6098(2) 0.1786(3) 0.0544(9) Uani 1 1 d . . . H01A H 0.3521 0.5776 0.1846 0.082 Uiso 1 1 calc R . . H01B H 0.3052 0.6526 0.2306 0.082 Uiso 1 1 calc R . . H01C H 0.2944 0.6468 0.1218 0.082 Uiso 1 1 calc R . . N03 N 0.04030(15) 0.10629(19) 0.45256(18) 0.0443(6) Uani 1 1 d . . . C012 C 0.05939(18) 0.0425(2) 0.4181(2) 0.0450(7) Uani 1 1 d . . . C011 C 0.0843(2) -0.0399(3) 0.3736(4) 0.0813(15) Uani 1 1 d . . . H01D H 0.0748 -0.0294 0.3074 0.122 Uiso 1 1 calc R . . H01E H 0.0574 -0.0967 0.3871 0.122 Uiso 1 1 calc R . . H01F H 0.1374 -0.0492 0.3960 0.122 Uiso 1 1 calc R . . H3B H 0.326(2) 0.217(3) 0.695(3) 0.062(12) Uiso 1 1 d . . . H2B H 0.290(3) 0.845(4) 0.440(3) 0.080(15) 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 Ag1 0.02072(12) 0.04334(14) 0.02917(13) -0.00164(8) 0.00529(8) -0.00100(8) O1 0.0376(14) 0.0370(13) 0.140(3) -0.0179(15) -0.0028(15) -0.0049(11) O2 0.0419(12) 0.0278(11) 0.0532(13) 0.0030(10) 0.0004(10) 0.0017(9) O3 0.0371(12) 0.0245(11) 0.0633(15) -0.0014(10) 0.0110(10) -0.0023(9) O4 0.0398(14) 0.0416(14) 0.155(3) -0.0265(17) 0.0200(17) 0.0054(11) O5 0.0252(9) 0.0342(10) 0.0228(8) 0.0001(7) 0.0052(7) 0.0031(7) O6 0.0354(10) 0.0340(10) 0.0222(9) -0.0026(7) 0.0011(7) 0.0079(8) O7 0.0233(9) 0.0334(9) 0.0212(8) -0.0020(7) 0.0040(7) -0.0039(7) O8 0.0337(10) 0.0310(10) 0.0243(9) -0.0046(7) 0.0117(7) -0.0071(8) N1 0.0243(11) 0.0337(12) 0.0300(11) -0.0017(9) 0.0063(9) 0.0015(9) N2 0.0240(10) 0.0239(10) 0.0244(10) 0.0000(8) 0.0040(8) 0.0012(8) N3 0.0244(11) 0.0307(11) 0.0280(11) -0.0014(9) 0.0040(9) -0.0023(9) N4 0.0245(10) 0.0226(10) 0.0245(10) -0.0003(8) 0.0058(8) -0.0011(8) C1 0.0251(12) 0.0245(12) 0.0238(12) 0.0010(9) 0.0062(10) 0.0001(10) C2 0.0251(13) 0.0356(14) 0.0264(12) 0.0007(11) 0.0040(10) 0.0032(11) C3 0.0300(13) 0.0291(13) 0.0260(12) -0.0016(10) 0.0085(10) 0.0012(10) C4 0.0296(13) 0.0216(12) 0.0220(12) -0.0014(9) 0.0034(10) -0.0005(10) C5 0.0289(13) 0.0218(12) 0.0234(12) -0.0003(9) 0.0079(10) 0.0010(10) C6 0.0270(13) 0.0286(13) 0.0249(12) -0.0024(10) 0.0041(10) -0.0020(10) C7 0.0242(12) 0.0306(13) 0.0258(12) 0.0007(10) 0.0066(10) -0.0012(10) C8 0.0247(12) 0.0217(12) 0.0216(11) 0.0010(9) 0.0035(9) 0.0012(9) C9 0.0339(14) 0.0284(13) 0.0306(13) 0.0042(11) 0.0122(11) -0.0011(11) C10 0.0240(12) 0.0302(13) 0.0219(12) 0.0033(10) 0.0078(10) 0.0033(10) C11 0.0302(13) 0.0285(13) 0.0212(12) 0.0013(10) 0.0080(10) -0.0035(10) C12 0.0346(15) 0.0299(14) 0.0330(14) 0.0012(11) 0.0126(11) 0.0049(11) C13 0.0296(14) 0.0416(16) 0.0423(16) 0.0035(13) 0.0153(12) 0.0033(12) C14 0.0292(14) 0.0383(16) 0.0461(16) 0.0023(13) 0.0144(12) -0.0056(12) C15 0.0292(13) 0.0291(13) 0.0224(12) 0.0005(10) 0.0054(10) 0.0001(10) C16 0.0256(13) 0.0396(15) 0.0335(14) 0.0011(12) 0.0040(11) 0.0017(11) C17 0.0281(14) 0.0404(16) 0.0373(15) -0.0041(12) 0.0012(11) -0.0086(12) C18 0.0402(16) 0.0276(13) 0.0308(14) -0.0031(11) 0.0017(11) -0.0058(12) C19 0.0298(13) 0.0295(13) 0.0202(11) 0.0002(10) 0.0028(10) 0.0034(11) C20 0.0247(12) 0.0313(13) 0.0177(11) 0.0002(9) 0.0039(9) -0.0036(10) C21 0.0379(17) 0.0303(15) 0.0455(17) 0.0047(12) 0.0157(14) -0.0019(12) C22 0.0315(15) 0.0318(15) 0.0389(15) -0.0012(12) 0.0049(12) 0.0028(12) B1 0.0252(16) 0.059(2) 0.0259(15) -0.0017(14) 0.0017(12) 0.0024(14) F4 0.0491(11) 0.0614(12) 0.0251(8) -0.0003(7) 0.0076(8) -0.0031(9) F3 0.0505(12) 0.1090(19) 0.0483(12) -0.0118(12) 0.0054(9) -0.0321(13) F2 0.0896(17) 0.0929(18) 0.0388(11) 0.0067(11) 0.0170(11) -0.0260(14) F1 0.0849(18) 0.139(3) 0.0651(15) -0.0226(16) -0.0046(13) 0.0658(18) O01 0.0388(12) 0.0421(13) 0.0740(16) 0.0010(11) 0.0058(11) -0.0010(10) O02 0.0469(13) 0.0282(10) 0.0579(13) 0.0019(9) 0.0155(10) 0.0040(9) N01 0.0447(15) 0.0410(14) 0.0447(14) -0.0001(11) 0.0074(12) 0.0025(12) N02 0.0545(16) 0.0312(13) 0.0388(13) 0.0037(10) 0.0115(12) 0.0066(11) C01 0.071(2) 0.0241(14) 0.0393(16) -0.0003(12) 0.0193(15) 0.0063(14) C02 0.0406(18) 0.065(2) 0.054(2) 0.0022(17) 0.0103(15) -0.0030(16) C03 0.053(2) 0.066(3) 0.083(3) 0.004(2) -0.004(2) 0.0024(19) C04 0.055(2) 0.056(2) 0.0485(19) -0.0046(16) 0.0104(16) -0.0104(17) C05 0.0458(18) 0.0447(18) 0.059(2) -0.0032(15) 0.0136(16) 0.0076(15) C06 0.062(2) 0.0303(15) 0.0253(13) 0.0008(11) 0.0065(13) 0.0029(14) C07 0.0445(18) 0.0460(18) 0.0416(17) 0.0022(14) -0.0027(14) -0.0007(14) C08 0.045(2) 0.064(2) 0.069(2) 0.0122(19) 0.0052(17) 0.0084(17) C09 0.059(2) 0.0476(19) 0.052(2) 0.0095(15) 0.0091(16) 0.0173(16) C010 0.075(2) 0.0373(17) 0.053(2) 0.0042(15) 0.0196(18) -0.0077(17) N03 0.0506(16) 0.0367(14) 0.0455(15) -0.0006(12) 0.0096(12) -0.0018(12) C012 0.0367(16) 0.0405(18) 0.0564(19) -0.0039(15) 0.0053(14) -0.0082(14) C011 0.054(2) 0.058(2) 0.135(4) -0.043(3) 0.026(3) -0.0082(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.254(2) 3_566 ? Ag1 N03 2.272(3) . ? Ag1 N3 2.288(2) . ? O1 C21 1.211(4) . ? O2 C21 1.291(4) . ? O2 H2B 0.83(5) . ? O3 C22 1.302(4) . ? O3 H3B 0.80(4) . ? O4 C22 1.195(4) . ? O5 C1 1.356(3) . ? O5 C10 1.394(3) . ? O6 C4 1.362(3) . ? O6 C19 1.398(3) . ? O7 C8 1.359(3) . ? O7 C20 1.394(3) . ? O8 C5 1.372(3) . ? O8 C11 1.395(3) . ? N1 C2 1.336(3) . ? N1 C3 1.340(3) . ? N1 Ag1 2.254(2) 3_566 ? N2 C4 1.321(3) . ? N2 C1 1.323(3) . ? N3 C7 1.337(3) . ? N3 C6 1.337(3) . ? N4 C8 1.319(3) . ? N4 C5 1.321(3) . ? C1 C2 1.386(4) . ? C2 H2A 0.9500 . ? C3 C4 1.383(4) . ? C3 H3A 0.9500 . ? C5 C6 1.382(4) . ? C6 H6A 0.9500 . ? C7 C8 1.390(3) . ? C7 H7A 0.9500 . ? C9 C10 1.393(4) . ? C9 C14 1.394(4) . ? C9 C21 1.495(4) . ? C10 C11 1.388(4) . ? C11 C12 1.377(4) . ? C12 C13 1.385(4) . ? C12 H12A 0.9500 . ? C13 C14 1.375(4) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C20 1.393(4) . ? C15 C16 1.395(4) . ? C15 C22 1.503(4) . ? C16 C17 1.381(4) . ? C16 H16A 0.9500 . ? C17 C18 1.381(4) . ? C17 H17A 0.9500 . ? C18 C19 1.384(4) . ? C18 H18A 0.9500 . ? C19 C20 1.392(4) . ? B1 F1 1.347(4) . ? B1 F3 1.355(4) . ? B1 F4 1.380(4) . ? B1 F2 1.422(4) . ? O01 C01 1.263(4) . ? O02 C06 1.264(4) . ? N01 C01 1.330(4) . ? N01 C05 1.421(4) . ? N01 C04 1.436(4) . ? N02 C06 1.320(4) . ? N02 C010 1.439(4) . ? N02 C09 1.440(4) . ? C01 C02 1.463(5) . ? C02 C03 1.572(5) . ? C02 H02A 0.9900 . ? C02 H02B 0.9900 . ? C03 C04 1.485(5) . ? C03 H03A 0.9900 . ? C03 H03B 0.9900 . ? C04 H04A 0.9900 . ? C04 H04B 0.9900 . ? C05 H05A 0.9800 . ? C05 H05B 0.9800 . ? C05 H05C 0.9800 . ? C06 C07 1.513(5) . ? C07 C08 1.525(5) . ? C07 H07A 0.9900 . ? C07 H07B 0.9900 . ? C08 C09 1.525(5) . ? C08 H08A 0.9900 . ? C08 H08B 0.9900 . ? C09 H09A 0.9900 . ? C09 H09B 0.9900 . ? C010 H01A 0.9800 . ? C010 H01B 0.9800 . ? C010 H01C 0.9800 . ? N03 C012 1.122(4) . ? C012 C011 1.452(5) . ? C011 H01D 0.9800 . ? C011 H01E 0.9800 . ? C011 H01F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N03 122.01(9) 3_566 . ? N1 Ag1 N3 130.33(8) 3_566 . ? N03 Ag1 N3 107.66(9) . . ? C21 O2 H2B 105(3) . . ? C22 O3 H3B 109(3) . . ? C1 O5 C10 119.45(19) . . ? C4 O6 C19 116.85(19) . . ? C8 O7 C20 119.76(18) . . ? C5 O8 C11 116.44(18) . . ? C2 N1 C3 118.8(2) . . ? C2 N1 Ag1 118.33(17) . 3_566 ? C3 N1 Ag1 122.83(17) . 3_566 ? C4 N2 C1 115.8(2) . . ? C7 N3 C6 118.7(2) . . ? C7 N3 Ag1 123.02(17) . . ? C6 N3 Ag1 118.06(16) . . ? C8 N4 C5 115.5(2) . . ? N2 C1 O5 119.4(2) . . ? N2 C1 C2 123.3(2) . . ? O5 C1 C2 117.3(2) . . ? N1 C2 C1 119.3(2) . . ? N1 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? N1 C3 C4 119.2(2) . . ? N1 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? N2 C4 O6 118.4(2) . . ? N2 C4 C3 123.5(2) . . ? O6 C4 C3 118.2(2) . . ? N4 C5 O8 118.6(2) . . ? N4 C5 C6 123.8(2) . . ? O8 C5 C6 117.5(2) . . ? N3 C6 C5 119.2(2) . . ? N3 C6 H6A 120.4 . . ? C5 C6 H6A 120.4 . . ? N3 C7 C8 119.3(2) . . ? N3 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? N4 C8 O7 120.1(2) . . ? N4 C8 C7 123.3(2) . . ? O7 C8 C7 116.5(2) . . ? C10 C9 C14 118.0(2) . . ? C10 C9 C21 124.7(2) . . ? C14 C9 C21 117.3(3) . . ? C11 C10 C9 120.3(2) . . ? C11 C10 O5 116.6(2) . . ? C9 C10 O5 123.0(2) . . ? C12 C11 C10 120.9(2) . . ? C12 C11 O8 118.8(2) . . ? C10 C11 O8 120.2(2) . . ? C11 C12 C13 119.1(3) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 120.3(3) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C13 C14 C9 121.4(3) . . ? C13 C14 H14A 119.3 . . ? C9 C14 H14A 119.3 . . ? C20 C15 C16 118.1(2) . . ? C20 C15 C22 125.3(2) . . ? C16 C15 C22 116.6(2) . . ? C17 C16 C15 121.5(3) . . ? C17 C16 H16A 119.2 . . ? C15 C16 H16A 119.2 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 119.3(3) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C18 C19 C20 120.9(2) . . ? C18 C19 O6 118.6(2) . . ? C20 C19 O6 120.4(2) . . ? C19 C20 C15 120.1(2) . . ? C19 C20 O7 116.5(2) . . ? C15 C20 O7 123.2(2) . . ? O1 C21 O2 123.8(3) . . ? O1 C21 C9 120.6(3) . . ? O2 C21 C9 115.6(3) . . ? O4 C22 O3 123.6(3) . . ? O4 C22 C15 121.4(3) . . ? O3 C22 C15 115.0(2) . . ? F1 B1 F3 116.0(3) . . ? F1 B1 F4 111.4(3) . . ? F3 B1 F4 110.3(3) . . ? F1 B1 F2 105.4(3) . . ? F3 B1 F2 105.4(3) . . ? F4 B1 F2 107.9(3) . . ? C01 N01 C05 123.6(3) . . ? C01 N01 C04 112.4(3) . . ? C05 N01 C04 123.9(3) . . ? C06 N02 C010 123.7(3) . . ? C06 N02 C09 113.3(3) . . ? C010 N02 C09 122.6(3) . . ? O01 C01 N01 121.0(3) . . ? O01 C01 C02 126.8(3) . . ? N01 C01 C02 112.2(3) . . ? C01 C02 C03 103.2(3) . . ? C01 C02 H02A 111.1 . . ? C03 C02 H02A 111.1 . . ? C01 C02 H02B 111.1 . . ? C03 C02 H02B 111.1 . . ? H02A C02 H02B 109.1 . . ? C04 C03 C02 105.4(3) . . ? C04 C03 H03A 110.7 . . ? C02 C03 H03A 110.7 . . ? C04 C03 H03B 110.7 . . ? C02 C03 H03B 110.7 . . ? H03A C03 H03B 108.8 . . ? N01 C04 C03 106.6(3) . . ? N01 C04 H04A 110.4 . . ? C03 C04 H04A 110.4 . . ? N01 C04 H04B 110.4 . . ? C03 C04 H04B 110.4 . . ? H04A C04 H04B 108.6 . . ? N01 C05 H05A 109.5 . . ? N01 C05 H05B 109.5 . . ? H05A C05 H05B 109.5 . . ? N01 C05 H05C 109.5 . . ? H05A C05 H05C 109.5 . . ? H05B C05 H05C 109.5 . . ? O02 C06 N02 124.4(3) . . ? O02 C06 C07 125.6(3) . . ? N02 C06 C07 110.1(3) . . ? C06 C07 C08 103.2(3) . . ? C06 C07 H07A 111.1 . . ? C08 C07 H07A 111.1 . . ? C06 C07 H07B 111.1 . . ? C08 C07 H07B 111.1 . . ? H07A C07 H07B 109.1 . . ? C09 C08 C07 104.5(3) . . ? C09 C08 H08A 110.8 . . ? C07 C08 H08A 110.8 . . ? C09 C08 H08B 110.8 . . ? C07 C08 H08B 110.8 . . ? H08A C08 H08B 108.9 . . ? N02 C09 C08 104.3(3) . . ? N02 C09 H09A 110.9 . . ? C08 C09 H09A 110.9 . . ? N02 C09 H09B 110.9 . . ? C08 C09 H09B 110.9 . . ? H09A C09 H09B 108.9 . . ? N02 C010 H01A 109.5 . . ? N02 C010 H01B 109.5 . . ? H01A C010 H01B 109.5 . . ? N02 C010 H01C 109.5 . . ? H01A C010 H01C 109.5 . . ? H01B C010 H01C 109.5 . . ? C012 N03 Ag1 155.7(3) . . ? N03 C012 C011 179.8(4) . . ? C012 C011 H01D 109.5 . . ? C012 C011 H01E 109.5 . . ? H01D C011 H01E 109.5 . . ? C012 C011 H01F 109.5 . . ? H01D C011 H01F 109.5 . . ? H01E C011 H01F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N3 C7 83.1(2) 3_566 . . . ? N03 Ag1 N3 C7 -97.1(2) . . . . ? N1 Ag1 N3 C6 -102.3(2) 3_566 . . . ? N03 Ag1 N3 C6 77.6(2) . . . . ? C4 N2 C1 O5 -173.1(2) . . . . ? C4 N2 C1 C2 3.5(4) . . . . ? C10 O5 C1 N2 -9.4(3) . . . . ? C10 O5 C1 C2 173.8(2) . . . . ? C3 N1 C2 C1 -1.2(4) . . . . ? Ag1 N1 C2 C1 179.96(19) 3_566 . . . ? N2 C1 C2 N1 -1.3(4) . . . . ? O5 C1 C2 N1 175.3(2) . . . . ? C2 N1 C3 C4 1.3(4) . . . . ? Ag1 N1 C3 C4 -179.94(18) 3_566 . . . ? C1 N2 C4 O6 176.6(2) . . . . ? C1 N2 C4 C3 -3.4(4) . . . . ? C19 O6 C4 N2 -17.7(3) . . . . ? C19 O6 C4 C3 162.4(2) . . . . ? N1 C3 C4 N2 1.1(4) . . . . ? N1 C3 C4 O6 -179.0(2) . . . . ? C8 N4 C5 O8 177.7(2) . . . . ? C8 N4 C5 C6 -3.1(4) . . . . ? C11 O8 C5 N4 -22.1(3) . . . . ? C11 O8 C5 C6 158.6(2) . . . . ? C7 N3 C6 C5 2.8(4) . . . . ? Ag1 N3 C6 C5 -172.12(18) . . . . ? N4 C5 C6 N3 -0.6(4) . . . . ? O8 C5 C6 N3 178.6(2) . . . . ? C6 N3 C7 C8 -1.3(4) . . . . ? Ag1 N3 C7 C8 173.32(17) . . . . ? C5 N4 C8 O7 -172.6(2) . . . . ? C5 N4 C8 C7 4.7(4) . . . . ? C20 O7 C8 N4 -6.9(3) . . . . ? C20 O7 C8 C7 175.6(2) . . . . ? N3 C7 C8 N4 -2.6(4) . . . . ? N3 C7 C8 O7 174.7(2) . . . . ? C14 C9 C10 C11 2.2(4) . . . . ? C21 C9 C10 C11 -177.0(3) . . . . ? C14 C9 C10 O5 -173.3(2) . . . . ? C21 C9 C10 O5 7.5(4) . . . . ? C1 O5 C10 C11 114.2(2) . . . . ? C1 O5 C10 C9 -70.2(3) . . . . ? C9 C10 C11 C12 -4.0(4) . . . . ? O5 C10 C11 C12 171.8(2) . . . . ? C9 C10 C11 O8 179.8(2) . . . . ? O5 C10 C11 O8 -4.4(3) . . . . ? C5 O8 C11 C12 120.9(2) . . . . ? C5 O8 C11 C10 -62.8(3) . . . . ? C10 C11 C12 C13 2.5(4) . . . . ? O8 C11 C12 C13 178.7(2) . . . . ? C11 C12 C13 C14 0.7(4) . . . . ? C12 C13 C14 C9 -2.5(4) . . . . ? C10 C9 C14 C13 1.0(4) . . . . ? C21 C9 C14 C13 -179.7(3) . . . . ? C20 C15 C16 C17 -0.6(4) . . . . ? C22 C15 C16 C17 178.6(3) . . . . ? C15 C16 C17 C18 0.9(4) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C17 C18 C19 C20 -0.7(4) . . . . ? C17 C18 C19 O6 175.4(2) . . . . ? C4 O6 C19 C18 115.9(3) . . . . ? C4 O6 C19 C20 -68.0(3) . . . . ? C18 C19 C20 C15 1.0(4) . . . . ? O6 C19 C20 C15 -175.1(2) . . . . ? C18 C19 C20 O7 176.0(2) . . . . ? O6 C19 C20 O7 -0.1(3) . . . . ? C16 C15 C20 C19 -0.3(4) . . . . ? C22 C15 C20 C19 -179.4(2) . . . . ? C16 C15 C20 O7 -174.9(2) . . . . ? C22 C15 C20 O7 6.0(4) . . . . ? C8 O7 C20 C19 109.6(2) . . . . ? C8 O7 C20 C15 -75.6(3) . . . . ? C10 C9 C21 O1 154.1(3) . . . . ? C14 C9 C21 O1 -25.1(4) . . . . ? C10 C9 C21 O2 -26.3(4) . . . . ? C14 C9 C21 O2 154.5(3) . . . . ? C20 C15 C22 O4 165.6(3) . . . . ? C16 C15 C22 O4 -13.5(4) . . . . ? C20 C15 C22 O3 -13.8(4) . . . . ? C16 C15 C22 O3 167.1(2) . . . . ? C05 N01 C01 O01 -1.9(5) . . . . ? C04 N01 C01 O01 175.9(3) . . . . ? C05 N01 C01 C02 178.3(3) . . . . ? C04 N01 C01 C02 -3.9(4) . . . . ? O01 C01 C02 C03 -178.4(3) . . . . ? N01 C01 C02 C03 1.4(4) . . . . ? C01 C02 C03 C04 1.4(4) . . . . ? C01 N01 C04 C03 4.7(4) . . . . ? C05 N01 C04 C03 -177.5(3) . . . . ? C02 C03 C04 N01 -3.5(4) . . . . ? C010 N02 C06 O02 3.5(5) . . . . ? C09 N02 C06 O02 176.6(3) . . . . ? C010 N02 C06 C07 -175.7(3) . . . . ? C09 N02 C06 C07 -2.6(4) . . . . ? O02 C06 C07 C08 169.6(3) . . . . ? N02 C06 C07 C08 -11.2(3) . . . . ? C06 C07 C08 C09 19.4(4) . . . . ? C06 N02 C09 C08 15.3(4) . . . . ? C010 N02 C09 C08 -171.5(3) . . . . ? C07 C08 C09 N02 -21.1(4) . . . . ? N1 Ag1 N03 C012 105.5(6) 3_566 . . . ? N3 Ag1 N03 C012 -74.3(6) . . . . ? Ag1 N03 C012 C011 48(100) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.084 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.069 # Attachment '- 8.cif' data_z_5 _database_code_depnum_ccdc_archive 'CCDC 825941' #TrackingRef '- 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H72 Cl4 Cu2 N12 O26' _chemical_formula_weight 1694.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.3423(3) _cell_length_b 13.8845(4) _cell_length_c 15.2876(4) _cell_angle_alpha 70.1160(10) _cell_angle_beta 85.990(4) _cell_angle_gamma 71.108(2) _cell_volume 1762.53(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7390 _exptl_absorpt_correction_T_max 0.8694 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20573 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6171 _reflns_number_gt 5524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0564P)^2^+2.7904P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6171 _refine_ls_number_parameters 493 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.63216(4) 0.62330(3) 1.01243(2) 0.02110(11) Uani 1 1 d . . . Cl1 Cl 0.72707(10) 0.44115(6) 1.04841(5) 0.0380(2) Uani 1 1 d . . . Cl2 Cl 0.48539(9) 0.80269(6) 0.96251(5) 0.03136(18) Uani 1 1 d . . . O1 O 0.8508(2) 0.38126(15) 0.79288(13) 0.0230(4) Uani 1 1 d . . . O2 O 0.9986(2) 0.53438(16) 0.74568(13) 0.0246(4) Uani 1 1 d . . . O3 O 0.4865(2) 0.70455(15) 0.67090(12) 0.0217(4) Uani 1 1 d . . . O4 O 0.3895(2) 0.56045(16) 0.62603(13) 0.0240(4) Uani 1 1 d . . . O5 O 0.9332(3) 0.1731(2) 0.63581(19) 0.0485(6) Uani 1 1 d . . . H5A H 0.8855 0.1284 0.6495 0.073 Uiso 1 1 calc R . . O6 O 0.8119(3) 0.2163(2) 0.75355(17) 0.0439(6) Uani 1 1 d . . . O7 O 0.5958(3) 0.87900(19) 0.60009(15) 0.0388(5) Uani 1 1 d . . . O8 O 0.6927(3) 0.89631(18) 0.46071(15) 0.0388(5) Uani 1 1 d . . . H8A H 0.7169 0.9454 0.4699 0.058 Uiso 1 1 calc R . . O9 O 0.8155(2) 0.65058(18) 1.07396(15) 0.0355(5) Uani 1 1 d . . . O10 O 0.7894(3) 0.04817(17) 0.46157(14) 0.0339(5) Uani 1 1 d . . . N1 N 0.6960(3) 0.63801(18) 0.87980(15) 0.0224(5) Uani 1 1 d . . . N2 N 0.7473(2) 0.62800(18) 0.70196(15) 0.0211(5) Uani 1 1 d . . . N3 N 0.6242(2) 0.46452(18) 0.70374(15) 0.0211(5) Uani 1 1 d . . . N4 N 0.4761(2) 0.40345(18) 0.86648(15) 0.0211(5) Uani 1 1 d . . . N5 N 0.8038(3) 0.7975(3) 1.1112(2) 0.0445(7) Uani 1 1 d . . . N6 N 0.8862(3) 0.1685(2) 0.3533(2) 0.0473(7) Uani 1 1 d . . . C1 C 0.9626(3) 0.3211(2) 0.6634(2) 0.0258(6) Uani 1 1 d . . . C2 C 1.0623(3) 0.3309(2) 0.5906(2) 0.0296(6) Uani 1 1 d . . . H2A H 1.0814 0.2833 0.5557 0.035 Uiso 1 1 calc R . . C3 C 1.1330(3) 0.4083(3) 0.5689(2) 0.0297(6) Uani 1 1 d . . . H3A H 1.2004 0.4139 0.5193 0.036 Uiso 1 1 calc R . . C4 C 1.1063(3) 0.4781(2) 0.6190(2) 0.0265(6) Uani 1 1 d . . . H4A H 1.1551 0.5317 0.6037 0.032 Uiso 1 1 calc R . . C5 C 1.0089(3) 0.4698(2) 0.69132(19) 0.0234(6) Uani 1 1 d . . . C6 C 0.9356(3) 0.3928(2) 0.71356(19) 0.0236(6) Uani 1 1 d . . . C7 C 0.4306(3) 0.6402(2) 0.46655(19) 0.0241(6) Uani 1 1 d . . . H7A H 0.3904 0.5924 0.4522 0.029 Uiso 1 1 calc R . . C8 C 0.4465(3) 0.6331(2) 0.55792(18) 0.0216(5) Uani 1 1 d . . . C9 C 0.5011(3) 0.7046(2) 0.57957(18) 0.0199(5) Uani 1 1 d . . . C10 C 0.5498(3) 0.7804(2) 0.50944(19) 0.0211(5) Uani 1 1 d . . . C11 C 0.5349(3) 0.7859(2) 0.41749(19) 0.0235(6) Uani 1 1 d . . . H11A H 0.5671 0.8374 0.3687 0.028 Uiso 1 1 calc R . . C12 C 0.4739(3) 0.7176(2) 0.39644(19) 0.0263(6) Uani 1 1 d . . . H12A H 0.4617 0.7240 0.3333 0.032 Uiso 1 1 calc R . . C13 C 0.8568(3) 0.5869(2) 0.76758(19) 0.0213(5) Uani 1 1 d . . . C14 C 0.8365(3) 0.5920(2) 0.85654(19) 0.0231(6) Uani 1 1 d . . . H14A H 0.9199 0.5636 0.9002 0.028 Uiso 1 1 calc R . . C15 C 0.5820(3) 0.6771(2) 0.81653(18) 0.0225(6) Uani 1 1 d . . . H15A H 0.4816 0.7090 0.8320 0.027 Uiso 1 1 calc R . . C16 C 0.6107(3) 0.6709(2) 0.72816(18) 0.0199(5) Uani 1 1 d . . . C17 C 0.4742(3) 0.4953(2) 0.70659(18) 0.0204(5) Uani 1 1 d . . . C18 C 0.6981(3) 0.4064(2) 0.78490(19) 0.0204(5) Uani 1 1 d . . . C19 C 0.6268(3) 0.3736(2) 0.86754(19) 0.0212(5) Uani 1 1 d . . . H19A H 0.6849 0.3305 0.9241 0.025 Uiso 1 1 calc R . . C20 C 0.3969(3) 0.4656(2) 0.78568(18) 0.0217(5) Uani 1 1 d . . . H20A H 0.2893 0.4884 0.7833 0.026 Uiso 1 1 calc R . . C21 C 0.8943(3) 0.2320(2) 0.6896(2) 0.0296(6) Uani 1 1 d . . . C22 C 0.6133(3) 0.8570(2) 0.52977(19) 0.0242(6) Uani 1 1 d . . . C23 C 0.8549(5) 0.8908(4) 1.0808(3) 0.0608(11) Uani 1 1 d . . . H23A H 0.9023 0.8977 1.1333 0.073 Uiso 1 1 calc R . . H23B H 0.7700 0.9579 1.0523 0.073 Uiso 1 1 calc R . . C24 C 0.9711(6) 0.8673(4) 1.0088(4) 0.0660(12) Uani 1 1 d . . . H24A H 0.9588 0.9330 0.9536 0.079 Uiso 1 1 calc R . . H24B H 1.0755 0.8414 1.0358 0.079 Uiso 1 1 calc R . . C25 C 0.9387(5) 0.7806(3) 0.9827(3) 0.0487(9) Uani 1 1 d . . . H25A H 1.0339 0.7244 0.9787 0.058 Uiso 1 1 calc R . . H25B H 0.8811 0.8118 0.9222 0.058 Uiso 1 1 calc R . . C26 C 0.8456(4) 0.7338(3) 1.0605(2) 0.0349(7) Uani 1 1 d . . . C27 C 0.6976(5) 0.7839(4) 1.1840(3) 0.0550(10) Uani 1 1 d . . . H27A H 0.6771 0.7160 1.1948 0.083 Uiso 1 1 calc R . . H27B H 0.6030 0.8445 1.1653 0.083 Uiso 1 1 calc R . . H27C H 0.7407 0.7820 1.2415 0.083 Uiso 1 1 calc R . . C28 C 0.8190(3) 0.0960(2) 0.3803(2) 0.0345(7) Uani 1 1 d . . . C29 C 0.7733(5) 0.0761(3) 0.2942(2) 0.0590(12) Uani 1 1 d . . . H29A H 0.8075 -0.0020 0.3028 0.071 Uiso 1 1 calc R . . H29B H 0.6622 0.1056 0.2818 0.071 Uiso 1 1 calc R . . C30 C 0.8533(5) 0.1355(4) 0.2167(3) 0.0637(12) Uani 1 1 d . . . H30A H 0.9431 0.0842 0.2002 0.076 Uiso 1 1 calc R . . H30B H 0.7847 0.1779 0.1607 0.076 Uiso 1 1 calc R . . C31 C 0.8990(5) 0.2074(4) 0.2527(3) 0.0634(12) Uani 1 1 d . . . H31A H 1.0045 0.2047 0.2370 0.076 Uiso 1 1 calc R . . H31B H 0.8318 0.2829 0.2253 0.076 Uiso 1 1 calc R . . C32 C 0.9434(5) 0.2029(3) 0.4144(3) 0.0565(10) Uani 1 1 d . . . H32A H 0.9214 0.1658 0.4783 0.085 Uiso 1 1 calc R . . H32B H 0.8960 0.2811 0.3991 0.085 Uiso 1 1 calc R . . H32C H 1.0532 0.1862 0.4088 0.085 Uiso 1 1 calc R . . O3W O 0.8187(3) 0.02570(19) 0.65153(17) 0.0439(6) Uani 1 1 d . . . H3WA H 0.8056 0.0288 0.5960 0.066 Uiso 1 1 d R . . H3WB H 0.7486 -0.0003 0.6755 0.066 Uiso 1 1 d R . . O2W O 0.6821(6) 0.0849(3) 0.8891(3) 0.0936(12) Uani 1 1 d D . . H2WA H 0.718(8) 0.134(4) 0.851(4) 0.140 Uiso 1 1 d D . . H2WB H 0.700(9) 0.034(4) 0.865(4) 0.140 Uiso 1 1 d D . . O1W O 0.6175(6) 0.9678(5) 0.7836(4) 0.142(2) Uani 1 1 d . . . H1WA H 0.5961 0.9400 0.7467 0.213 Uiso 1 1 d R . . H1WB H 0.7030 0.9376 0.8132 0.213 Uiso 1 1 d 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 0.02419(19) 0.02391(19) 0.01540(18) -0.00729(13) 0.00301(13) -0.00766(14) Cl1 0.0556(5) 0.0252(4) 0.0255(4) -0.0083(3) 0.0069(3) -0.0041(3) Cl2 0.0414(4) 0.0246(4) 0.0253(4) -0.0093(3) 0.0026(3) -0.0061(3) O1 0.0182(9) 0.0310(10) 0.0211(10) -0.0107(8) 0.0030(7) -0.0078(8) O2 0.0169(9) 0.0344(11) 0.0278(10) -0.0168(9) 0.0020(8) -0.0087(8) O3 0.0192(9) 0.0314(10) 0.0149(9) -0.0095(8) 0.0008(7) -0.0069(8) O4 0.0219(9) 0.0344(11) 0.0168(9) -0.0042(8) -0.0004(7) -0.0145(8) O5 0.0536(15) 0.0527(15) 0.0627(17) -0.0411(13) 0.0245(13) -0.0291(12) O6 0.0548(15) 0.0468(14) 0.0472(14) -0.0268(12) 0.0210(12) -0.0307(12) O7 0.0554(14) 0.0468(13) 0.0292(12) -0.0207(10) 0.0086(10) -0.0290(12) O8 0.0549(14) 0.0407(13) 0.0369(12) -0.0195(10) 0.0178(11) -0.0325(11) O9 0.0333(11) 0.0397(13) 0.0370(12) -0.0102(10) -0.0029(9) -0.0180(10) O10 0.0454(13) 0.0351(12) 0.0282(12) -0.0123(9) 0.0075(9) -0.0215(10) N1 0.0268(12) 0.0238(12) 0.0173(11) -0.0075(9) 0.0019(9) -0.0087(10) N2 0.0209(11) 0.0264(12) 0.0195(11) -0.0098(9) 0.0023(9) -0.0102(9) N3 0.0213(11) 0.0262(12) 0.0196(11) -0.0100(9) 0.0030(9) -0.0105(9) N4 0.0218(11) 0.0241(12) 0.0211(12) -0.0101(9) 0.0035(9) -0.0099(9) N5 0.0456(17) 0.0509(18) 0.0428(17) -0.0206(14) 0.0090(13) -0.0195(14) N6 0.0409(16) 0.0370(16) 0.0547(19) -0.0059(14) 0.0057(14) -0.0113(13) C1 0.0202(13) 0.0303(15) 0.0275(15) -0.0136(12) 0.0004(11) -0.0046(11) C2 0.0260(14) 0.0354(16) 0.0293(16) -0.0172(13) 0.0024(12) -0.0060(12) C3 0.0202(14) 0.0395(17) 0.0267(15) -0.0130(13) 0.0059(11) -0.0051(12) C4 0.0181(13) 0.0330(15) 0.0289(15) -0.0101(12) 0.0017(11) -0.0094(12) C5 0.0161(12) 0.0298(15) 0.0239(14) -0.0115(12) -0.0019(11) -0.0035(11) C6 0.0163(12) 0.0307(15) 0.0228(14) -0.0100(12) 0.0019(10) -0.0053(11) C7 0.0225(13) 0.0308(15) 0.0221(14) -0.0110(12) -0.0009(11) -0.0098(12) C8 0.0186(13) 0.0262(14) 0.0192(13) -0.0069(11) 0.0026(10) -0.0073(11) C9 0.0157(12) 0.0259(14) 0.0172(13) -0.0088(11) 0.0001(10) -0.0035(10) C10 0.0169(12) 0.0233(13) 0.0213(14) -0.0079(11) 0.0003(10) -0.0038(10) C11 0.0221(13) 0.0264(14) 0.0186(14) -0.0052(11) 0.0018(11) -0.0060(11) C12 0.0268(14) 0.0362(16) 0.0170(13) -0.0098(12) 0.0016(11) -0.0107(12) C13 0.0190(13) 0.0242(13) 0.0242(14) -0.0095(11) 0.0021(11) -0.0101(11) C14 0.0225(13) 0.0279(14) 0.0203(14) -0.0076(11) 0.0002(11) -0.0104(11) C15 0.0231(13) 0.0244(14) 0.0201(13) -0.0088(11) 0.0017(11) -0.0067(11) C16 0.0217(13) 0.0204(13) 0.0194(13) -0.0071(10) 0.0005(10) -0.0085(11) C17 0.0199(13) 0.0260(14) 0.0199(13) -0.0100(11) -0.0002(10) -0.0107(11) C18 0.0191(13) 0.0217(13) 0.0244(14) -0.0117(11) 0.0014(11) -0.0075(10) C19 0.0208(13) 0.0235(13) 0.0214(14) -0.0099(11) -0.0003(10) -0.0072(11) C20 0.0207(13) 0.0268(14) 0.0210(14) -0.0091(11) 0.0005(10) -0.0108(11) C21 0.0248(14) 0.0309(16) 0.0343(17) -0.0148(13) -0.0003(13) -0.0062(12) C22 0.0221(13) 0.0214(13) 0.0255(15) -0.0069(11) 0.0000(11) -0.0032(11) C23 0.076(3) 0.053(2) 0.068(3) -0.030(2) 0.015(2) -0.033(2) C24 0.070(3) 0.062(3) 0.081(3) -0.028(2) 0.028(2) -0.040(2) C25 0.053(2) 0.049(2) 0.047(2) -0.0179(17) 0.0209(17) -0.0206(18) C26 0.0295(16) 0.0389(18) 0.0354(17) -0.0101(14) -0.0043(13) -0.0112(14) C27 0.047(2) 0.073(3) 0.045(2) -0.024(2) 0.0159(18) -0.017(2) C28 0.0229(15) 0.0251(15) 0.0444(19) -0.0050(14) 0.0034(13) -0.0007(12) C29 0.055(2) 0.053(2) 0.0270(18) 0.0041(16) 0.0110(16) 0.0169(18) C30 0.060(3) 0.077(3) 0.040(2) -0.008(2) 0.0023(19) -0.015(2) C31 0.055(2) 0.064(3) 0.041(2) 0.014(2) 0.0069(19) -0.015(2) C32 0.051(2) 0.049(2) 0.061(3) -0.012(2) 0.0001(19) -0.0117(19) O3W 0.0470(14) 0.0450(14) 0.0472(14) -0.0246(12) -0.0012(11) -0.0144(11) O2W 0.122(3) 0.081(3) 0.089(3) -0.036(2) 0.028(2) -0.045(3) O1W 0.148(5) 0.143(4) 0.118(4) -0.001(3) 0.045(3) -0.078(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 2.025(2) 2_667 ? Cu1 N1 2.034(2) . ? Cu1 O9 2.203(2) . ? Cu1 Cl1 2.2704(8) . ? Cu1 Cl2 2.3040(8) . ? O1 C18 1.358(3) . ? O1 C6 1.392(3) . ? O2 C13 1.370(3) . ? O2 C5 1.394(3) . ? O3 C16 1.358(3) . ? O3 C9 1.393(3) . ? O4 C17 1.370(3) . ? O4 C8 1.393(3) . ? O5 C21 1.305(4) . ? O5 H5A 0.8400 . ? O6 C21 1.206(4) . ? O7 C22 1.201(3) . ? O8 C22 1.313(3) . ? O8 H8A 0.8400 . ? O9 C26 1.223(4) . ? O10 C28 1.254(4) . ? N1 C15 1.333(4) . ? N1 C14 1.343(4) . ? N2 C16 1.319(3) . ? N2 C13 1.325(4) . ? N3 C18 1.321(4) . ? N3 C17 1.328(3) . ? N4 C19 1.332(3) . ? N4 C20 1.344(4) . ? N4 Cu1 2.025(2) 2_667 ? N5 C26 1.317(4) . ? N5 C27 1.443(5) . ? N5 C23 1.443(5) . ? N6 C28 1.292(4) . ? N6 C32 1.387(5) . ? N6 C31 1.457(5) . ? C1 C2 1.399(4) . ? C1 C6 1.405(4) . ? C1 C21 1.495(4) . ? C2 C3 1.374(4) . ? C2 H2A 0.9500 . ? C3 C4 1.383(4) . ? C3 H3A 0.9500 . ? C4 C5 1.379(4) . ? C4 H4A 0.9500 . ? C5 C6 1.387(4) . ? C7 C12 1.380(4) . ? C7 C8 1.382(4) . ? C7 H7A 0.9500 . ? C8 C9 1.389(4) . ? C9 C10 1.392(4) . ? C10 C11 1.396(4) . ? C10 C22 1.496(4) . ? C11 C12 1.382(4) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.382(4) . ? C14 H14A 0.9500 . ? C15 C16 1.385(4) . ? C15 H15A 0.9500 . ? C17 C20 1.373(4) . ? C18 C19 1.391(4) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C23 C24 1.531(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.510(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.513(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.546(6) . ? C29 C30 1.501(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.471(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O3W H3WA 0.8504 . ? O3W H3WB 0.8500 . ? O2W H2WA 0.873(10) . ? O2W H2WB 0.871(10) . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cu1 N1 164.31(9) 2_667 . ? N4 Cu1 O9 92.41(9) 2_667 . ? N1 Cu1 O9 103.18(9) . . ? N4 Cu1 Cl1 87.55(7) 2_667 . ? N1 Cu1 Cl1 88.18(7) . . ? O9 Cu1 Cl1 99.55(6) . . ? N4 Cu1 Cl2 90.74(7) 2_667 . ? N1 Cu1 Cl2 89.75(7) . . ? O9 Cu1 Cl2 94.44(6) . . ? Cl1 Cu1 Cl2 165.96(3) . . ? C18 O1 C6 120.0(2) . . ? C13 O2 C5 117.5(2) . . ? C16 O3 C9 120.8(2) . . ? C17 O4 C8 119.5(2) . . ? C21 O5 H5A 109.5 . . ? C22 O8 H8A 109.5 . . ? C26 O9 Cu1 130.2(2) . . ? C15 N1 C14 119.0(2) . . ? C15 N1 Cu1 114.88(18) . . ? C14 N1 Cu1 124.60(19) . . ? C16 N2 C13 115.2(2) . . ? C18 N3 C17 115.2(2) . . ? C19 N4 C20 119.1(2) . . ? C19 N4 Cu1 120.16(18) . 2_667 ? C20 N4 Cu1 119.99(18) . 2_667 ? C26 N5 C27 122.6(3) . . ? C26 N5 C23 115.3(3) . . ? C27 N5 C23 121.6(3) . . ? C28 N6 C32 123.2(3) . . ? C28 N6 C31 112.7(3) . . ? C32 N6 C31 124.0(3) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 C21 120.1(3) . . ? C6 C1 C21 121.4(3) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 O2 117.4(2) . . ? C6 C5 O2 121.7(2) . . ? C5 C6 O1 117.7(2) . . ? C5 C6 C1 119.9(2) . . ? O1 C6 C1 121.9(2) . . ? C12 C7 C8 119.1(3) . . ? C12 C7 H7A 120.4 . . ? C8 C7 H7A 120.4 . . ? C7 C8 C9 120.9(2) . . ? C7 C8 O4 117.4(2) . . ? C9 C8 O4 121.2(2) . . ? C8 C9 C10 120.1(2) . . ? C8 C9 O3 116.6(2) . . ? C10 C9 O3 122.9(2) . . ? C9 C10 C11 118.4(2) . . ? C9 C10 C22 122.0(2) . . ? C11 C10 C22 119.6(2) . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C7 C12 C11 120.4(3) . . ? C7 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? N2 C13 O2 117.4(2) . . ? N2 C13 C14 124.3(2) . . ? O2 C13 C14 118.3(2) . . ? N1 C14 C13 118.4(2) . . ? N1 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? N1 C15 C16 119.6(2) . . ? N1 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? N2 C16 O3 121.0(2) . . ? N2 C16 C15 123.4(2) . . ? O3 C16 C15 115.4(2) . . ? N3 C17 O4 118.7(2) . . ? N3 C17 C20 124.2(2) . . ? O4 C17 C20 117.1(2) . . ? N3 C18 O1 120.7(2) . . ? N3 C18 C19 123.4(2) . . ? O1 C18 C19 115.8(2) . . ? N4 C19 C18 119.2(2) . . ? N4 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? N4 C20 C17 118.8(2) . . ? N4 C20 H20A 120.6 . . ? C17 C20 H20A 120.6 . . ? O6 C21 O5 123.6(3) . . ? O6 C21 C1 123.7(3) . . ? O5 C21 C1 112.7(3) . . ? O7 C22 O8 124.2(3) . . ? O7 C22 C10 124.9(3) . . ? O8 C22 C10 110.9(2) . . ? N5 C23 C24 103.3(3) . . ? N5 C23 H23A 111.1 . . ? C24 C23 H23A 111.1 . . ? N5 C23 H23B 111.1 . . ? C24 C23 H23B 111.1 . . ? H23A C23 H23B 109.1 . . ? C25 C24 C23 105.0(3) . . ? C25 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? C25 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? C24 C25 C26 104.6(3) . . ? C24 C25 H25A 110.8 . . ? C26 C25 H25A 110.8 . . ? C24 C25 H25B 110.8 . . ? C26 C25 H25B 110.8 . . ? H25A C25 H25B 108.9 . . ? O9 C26 N5 126.2(3) . . ? O9 C26 C25 125.5(3) . . ? N5 C26 C25 108.3(3) . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O10 C28 N6 128.1(3) . . ? O10 C28 C29 122.7(3) . . ? N6 C28 C29 109.1(3) . . ? C30 C29 C28 103.5(4) . . ? C30 C29 H29A 111.1 . . ? C28 C29 H29A 111.1 . . ? C30 C29 H29B 111.1 . . ? C28 C29 H29B 111.1 . . ? H29A C29 H29B 109.0 . . ? C31 C30 C29 105.5(4) . . ? C31 C30 H30A 110.6 . . ? C29 C30 H30A 110.6 . . ? C31 C30 H30B 110.6 . . ? C29 C30 H30B 110.6 . . ? H30A C30 H30B 108.8 . . ? N6 C31 C30 106.4(3) . . ? N6 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? N6 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? N6 C32 H32A 109.5 . . ? N6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? H3WA O3W H3WB 97.7 . . ? H2WA O2W H2WB 105.5(16) . . ? H1WA O1W H1WB 118.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 O9 C26 -109.6(3) 2_667 . . . ? N1 Cu1 O9 C26 72.1(3) . . . . ? Cl1 Cu1 O9 C26 162.5(3) . . . . ? Cl2 Cu1 O9 C26 -18.6(3) . . . . ? N4 Cu1 N1 C15 37.7(4) 2_667 . . . ? O9 Cu1 N1 C15 -148.60(19) . . . . ? Cl1 Cu1 N1 C15 112.02(19) . . . . ? Cl2 Cu1 N1 C15 -54.10(19) . . . . ? N4 Cu1 N1 C14 -127.9(3) 2_667 . . . ? O9 Cu1 N1 C14 45.7(2) . . . . ? Cl1 Cu1 N1 C14 -53.7(2) . . . . ? Cl2 Cu1 N1 C14 140.2(2) . . . . ? C6 C1 C2 C3 0.3(4) . . . . ? C21 C1 C2 C3 -176.2(3) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C3 C4 C5 O2 173.4(2) . . . . ? C13 O2 C5 C4 135.5(3) . . . . ? C13 O2 C5 C6 -50.4(3) . . . . ? C4 C5 C6 O1 173.7(2) . . . . ? O2 C5 C6 O1 -0.3(4) . . . . ? C4 C5 C6 C1 1.2(4) . . . . ? O2 C5 C6 C1 -172.7(2) . . . . ? C18 O1 C6 C5 114.4(3) . . . . ? C18 O1 C6 C1 -73.2(3) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? C21 C1 C6 C5 175.6(3) . . . . ? C2 C1 C6 O1 -173.1(2) . . . . ? C21 C1 C6 O1 3.4(4) . . . . ? C12 C7 C8 C9 1.9(4) . . . . ? C12 C7 C8 O4 174.5(2) . . . . ? C17 O4 C8 C7 135.8(3) . . . . ? C17 O4 C8 C9 -51.6(3) . . . . ? C7 C8 C9 C10 -4.2(4) . . . . ? O4 C8 C9 C10 -176.5(2) . . . . ? C7 C8 C9 O3 168.3(2) . . . . ? O4 C8 C9 O3 -4.1(4) . . . . ? C16 O3 C9 C8 113.7(3) . . . . ? C16 O3 C9 C10 -74.1(3) . . . . ? C8 C9 C10 C11 3.3(4) . . . . ? O3 C9 C10 C11 -168.6(2) . . . . ? C8 C9 C10 C22 -178.3(2) . . . . ? O3 C9 C10 C22 9.7(4) . . . . ? C9 C10 C11 C12 -0.3(4) . . . . ? C22 C10 C11 C12 -178.7(2) . . . . ? C8 C7 C12 C11 1.1(4) . . . . ? C10 C11 C12 C7 -1.9(4) . . . . ? C16 N2 C13 O2 175.3(2) . . . . ? C16 N2 C13 C14 -3.5(4) . . . . ? C5 O2 C13 N2 -39.2(3) . . . . ? C5 O2 C13 C14 139.6(3) . . . . ? C15 N1 C14 C13 -0.1(4) . . . . ? Cu1 N1 C14 C13 165.01(19) . . . . ? N2 C13 C14 N1 2.5(4) . . . . ? O2 C13 C14 N1 -176.3(2) . . . . ? C14 N1 C15 C16 -0.9(4) . . . . ? Cu1 N1 C15 C16 -167.47(19) . . . . ? C13 N2 C16 O3 -172.4(2) . . . . ? C13 N2 C16 C15 2.3(4) . . . . ? C9 O3 C16 N2 -6.4(4) . . . . ? C9 O3 C16 C15 178.4(2) . . . . ? N1 C15 C16 N2 -0.2(4) . . . . ? N1 C15 C16 O3 174.8(2) . . . . ? C18 N3 C17 O4 176.7(2) . . . . ? C18 N3 C17 C20 -3.6(4) . . . . ? C8 O4 C17 N3 -30.6(3) . . . . ? C8 O4 C17 C20 149.7(2) . . . . ? C17 N3 C18 O1 -172.0(2) . . . . ? C17 N3 C18 C19 3.5(4) . . . . ? C6 O1 C18 N3 -15.8(4) . . . . ? C6 O1 C18 C19 168.4(2) . . . . ? C20 N4 C19 C18 -0.8(4) . . . . ? Cu1 N4 C19 C18 -170.80(18) 2_667 . . . ? N3 C18 C19 N4 -1.4(4) . . . . ? O1 C18 C19 N4 174.3(2) . . . . ? C19 N4 C20 C17 0.7(4) . . . . ? Cu1 N4 C20 C17 170.68(19) 2_667 . . . ? N3 C17 C20 N4 1.7(4) . . . . ? O4 C17 C20 N4 -178.7(2) . . . . ? C2 C1 C21 O6 177.3(3) . . . . ? C6 C1 C21 O6 0.8(5) . . . . ? C2 C1 C21 O5 -2.9(4) . . . . ? C6 C1 C21 O5 -179.3(3) . . . . ? C9 C10 C22 O7 -18.7(4) . . . . ? C11 C10 C22 O7 159.7(3) . . . . ? C9 C10 C22 O8 160.6(3) . . . . ? C11 C10 C22 O8 -21.1(4) . . . . ? C26 N5 C23 C24 -11.5(5) . . . . ? C27 N5 C23 C24 176.6(4) . . . . ? N5 C23 C24 C25 17.7(5) . . . . ? C23 C24 C25 C26 -17.9(5) . . . . ? Cu1 O9 C26 N5 95.9(4) . . . . ? Cu1 O9 C26 C25 -84.6(4) . . . . ? C27 N5 C26 O9 -8.5(6) . . . . ? C23 N5 C26 O9 179.7(4) . . . . ? C27 N5 C26 C25 171.9(3) . . . . ? C23 N5 C26 C25 0.1(4) . . . . ? C24 C25 C26 O9 -168.0(4) . . . . ? C24 C25 C26 N5 11.6(4) . . . . ? C32 N6 C28 O10 2.6(5) . . . . ? C31 N6 C28 O10 -179.1(3) . . . . ? C32 N6 C28 C29 -178.8(3) . . . . ? C31 N6 C28 C29 -0.5(4) . . . . ? O10 C28 C29 C30 -171.0(3) . . . . ? N6 C28 C29 C30 10.3(4) . . . . ? C28 C29 C30 C31 -15.6(4) . . . . ? C28 N6 C31 C30 -9.8(5) . . . . ? C32 N6 C31 C30 168.5(4) . . . . ? C29 C30 C31 N6 15.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.012 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.074 # Attachment '- 9.cif' data_z_6 _database_code_depnum_ccdc_archive 'CCDC 825942' #TrackingRef '- 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H54 Cl4 Cu2 N16 O32' _chemical_formula_weight 2212.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.2076(6) _cell_length_b 15.5977(5) _cell_length_c 31.7601(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10010.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.70 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4496 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8071 _exptl_absorpt_correction_T_max 0.8753 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 112590 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8833 _reflns_number_gt 6676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1390P)^2^+31.0713P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8833 _refine_ls_number_parameters 672 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2534 _refine_ls_wR_factor_gt 0.2244 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.48998(3) 0.49047(4) 0.069249(19) 0.0341(2) Uani 1 1 d . . . Cl2 Cl 0.48395(6) 0.34906(8) 0.08759(4) 0.0419(3) Uani 1 1 d . . . Cl1 Cl 0.49775(7) 0.61786(10) 0.03580(6) 0.0565(4) Uani 1 1 d . . . N1 N 0.2619(2) 0.4944(3) 0.02587(14) 0.0400(10) Uani 1 1 d . . . N2 N 0.3907(2) 0.4907(2) 0.05531(13) 0.0343(9) Uani 1 1 d . . . N3 N 0.4083(2) 0.5141(3) -0.07184(13) 0.0366(9) Uani 1 1 d . . . N4 N 0.2714(2) 0.5175(3) -0.06304(14) 0.0390(10) Uani 1 1 d . . . N7 N 0.4704(3) 0.5397(3) 0.13756(16) 0.0573(13) Uani 1 1 d . . . O1 O 0.28086(18) 0.3597(2) -0.00259(13) 0.0475(10) Uani 1 1 d . . . O2 O 0.26776(18) 0.3776(2) -0.08657(13) 0.0498(10) Uani 1 1 d . . . O3 O 0.25345(19) 0.6342(2) 0.04929(13) 0.0489(9) Uani 1 1 d . . . O4 O 0.28378(16) 0.6530(2) -0.03358(13) 0.0429(9) Uani 1 1 d . . . O5 O 0.1078(4) 0.3217(7) 0.0672(3) 0.157(4) Uani 1 1 d . . . O6 O 0.2167(4) 0.3321(4) 0.0718(2) 0.0996(19) Uani 1 1 d . . . O7 O 0.2357(2) 0.6811(3) -0.11266(14) 0.0633(11) Uani 1 1 d . . . O8 O 0.1315(2) 0.7290(3) -0.11657(15) 0.0683(12) Uani 1 1 d . . . O10 O 0.4447(3) 0.7234(3) 0.20173(14) 0.0771(15) Uani 1 1 d . . . O13 O 0.5232(9) 0.4930(15) 0.3639(7) 0.325(15) Uani 1 1 d . B . O14 O 0.4422(7) 0.4778(7) 0.4096(4) 0.181(4) Uani 1 1 d . B . C1 C 0.2896(2) 0.5599(3) 0.04505(17) 0.0394(11) Uani 1 1 d . . . C2 C 0.3530(2) 0.5601(3) 0.06068(16) 0.0386(11) Uani 1 1 d . . . H2A H 0.3697 0.6089 0.0751 0.046 Uiso 1 1 calc R . . C3 C 0.3653(2) 0.4234(3) 0.03510(17) 0.0378(11) Uani 1 1 d . . . H3A H 0.3911 0.3733 0.0307 0.045 Uiso 1 1 calc R . . C4 C 0.3007(2) 0.4277(3) 0.02068(16) 0.0376(11) Uani 1 1 d . . . C5 C 0.3098(2) 0.5821(3) -0.05264(16) 0.0349(10) Uani 1 1 d . . . C6 C 0.3776(2) 0.5827(3) -0.05652(16) 0.0372(11) Uani 1 1 d . . . H6A H 0.4023 0.6318 -0.0483 0.045 Uiso 1 1 calc R . . C7 C 0.3715(2) 0.4463(3) -0.08250(17) 0.0397(11) Uani 1 1 d . . . H7A H 0.3918 0.3961 -0.0935 0.048 Uiso 1 1 calc R . . C8 C 0.3038(2) 0.4497(3) -0.07737(16) 0.0373(11) Uani 1 1 d . . . C9 C 0.1624(3) 0.3346(4) 0.0053(3) 0.0641(19) Uani 1 1 d . . . C10 C 0.1035(3) 0.3167(5) -0.0162(4) 0.084(3) Uani 1 1 d . . . H10A H 0.0650 0.3023 -0.0005 0.101 Uiso 1 1 calc R . . C11 C 0.0999(3) 0.3195(5) -0.0591(4) 0.082(3) Uani 1 1 d . . . H11A H 0.0597 0.3055 -0.0729 0.099 Uiso 1 1 calc R . . C12 C 0.1537(3) 0.3421(4) -0.0818(3) 0.0630(18) Uani 1 1 d . . . H12A H 0.1509 0.3450 -0.1116 0.076 Uiso 1 1 calc R . . C13 C 0.2124(3) 0.3610(3) -0.0618(2) 0.0479(14) Uani 1 1 d . . . C14 C 0.2179(3) 0.3551(3) -0.0191(2) 0.0468(14) Uani 1 1 d . . . C15 C 0.1415(3) 0.6670(4) 0.0350(2) 0.0538(15) Uani 1 1 d . . . H15A H 0.1321 0.6618 0.0642 0.065 Uiso 1 1 calc R . . C16 C 0.0926(3) 0.6922(4) 0.0076(2) 0.0578(16) Uani 1 1 d . . . H16A H 0.0496 0.7050 0.0179 0.069 Uiso 1 1 calc R . . C17 C 0.1054(3) 0.6989(4) -0.0347(2) 0.0549(15) Uani 1 1 d . . . H17A H 0.0708 0.7152 -0.0532 0.066 Uiso 1 1 calc R . . C18 C 0.1682(3) 0.6824(3) -0.05102(19) 0.0435(12) Uani 1 1 d . . . C19 C 0.2174(2) 0.6572(3) -0.02234(18) 0.0389(12) Uani 1 1 d . . . C20 C 0.2032(3) 0.6496(3) 0.02043(19) 0.0428(12) Uani 1 1 d . . . C21 C 0.1659(5) 0.3285(5) 0.0508(3) 0.083(2) Uani 1 1 d . . . C22 C 0.1837(3) 0.6963(3) -0.0962(2) 0.0512(14) Uani 1 1 d . . . C28 C 0.4482(7) 0.4798(5) 0.1648(3) 0.115(4) Uani 1 1 d . B . H28A H 0.4480 0.4211 0.1568 0.139 Uiso 1 1 calc R . . C29 C 0.4687(3) 0.6198(4) 0.15015(18) 0.0491(13) Uani 1 1 d . . . H29A H 0.4834 0.6638 0.1317 0.059 Uiso 1 1 calc R . . C30 C 0.4457(3) 0.6411(4) 0.18994(18) 0.0516(14) Uani 1 1 d . . . N8 N 0.4232(4) 0.5839(4) 0.21601(19) 0.093(3) Uani 1 1 d . B . C32 C 0.4261(7) 0.5029(5) 0.2037(3) 0.134(5) Uani 1 1 d D . . C33 C 0.3770(2) 0.46428(17) 0.26827(13) 0.130(6) Uani 1 1 d GD . . C34 C 0.4243(2) 0.46600(17) 0.29735(12) 0.117(4) Uani 1 1 d G A . C35 C 0.4085(2) 0.4767(2) 0.33765(12) 0.108(3) Uani 1 1 d G A . C36 C 0.3455(3) 0.4856(2) 0.34884(15) 0.109(4) Uani 1 1 d G A . H36A H 0.3343 0.4933 0.3776 0.131 Uiso 1 1 calc R . . C37 C 0.2983(2) 0.4839(2) 0.31976(17) 0.129(5) Uani 1 1 d G A . H37A H 0.2533 0.4903 0.3278 0.155 Uiso 1 1 calc R . . C38 C 0.3140(2) 0.4732(2) 0.27946(16) 0.138(5) Uani 1 1 d GD A . C39 C 0.41795(19) 0.74468(17) 0.24096(11) 0.073(2) Uani 1 1 d G A . C40 C 0.4569(2) 0.75587(18) 0.27628(10) 0.109(4) Uani 1 1 d G A . C41 C 0.4285(3) 0.7816(2) 0.31379(11) 0.153(7) Uani 1 1 d G A . H41A H 0.4553 0.7893 0.3381 0.184 Uiso 1 1 calc R . . C42 C 0.3612(3) 0.7962(2) 0.31597(14) 0.192(11) Uani 1 1 d G A . H42A H 0.3417 0.8139 0.3418 0.231 Uiso 1 1 calc R . . C43 C 0.3222(2) 0.7850(2) 0.28064(16) 0.201(11) Uani 1 1 d G A . H43A H 0.2759 0.7950 0.2821 0.241 Uiso 1 1 calc R . . C44 C 0.3506(2) 0.7593(2) 0.24314(14) 0.117(4) Uani 1 1 d G A . O11 O 0.4859(2) 0.4489(2) 0.28005(13) 0.109(5) Uani 0.50 1 d PG A 1 O12 O 0.5295(2) 0.7371(2) 0.27007(12) 0.114(3) Uani 0.50 1 d PG A 1 C45 C 0.55535(18) 0.6557(2) 0.26680(13) 0.285(13) Uani 0.50 1 d PG A 1 C46 C 0.6170(2) 0.6367(3) 0.25320(18) 0.187(8) Uani 0.50 1 d PG A 1 H46A H 0.6467 0.6816 0.2459 0.224 Uiso 0.50 1 calc PR A 1 N9 N 0.6364(2) 0.5541(4) 0.2500(2) 0.119(6) Uani 0.50 1 d PG A 1 C48 C 0.5942(2) 0.4904(3) 0.26044(18) 0.103(6) Uani 0.50 1 d PG A 1 H48A H 0.6078 0.4323 0.2582 0.123 Uiso 0.50 1 calc PR A 1 C49 C 0.53254(19) 0.5094(2) 0.27406(13) 0.071(4) Uani 0.50 1 d PG A 1 N10 N 0.51315(17) 0.5920(2) 0.27724(10) 0.053(2) Uani 0.50 1 d PG A 1 C70 C 0.3072(2) 0.7520(3) 0.20068(17) 0.163(6) Uani 0.50 1 d PG A 1 O18 O 0.3060(2) 0.6955(3) 0.18610(16) 0.288(13) Uani 0.50 1 d PG A 1 C71 C 0.2598(3) 0.6528(4) 0.1495(2) 0.321(15) Uani 0.50 1 d PGU A 1 O16 O 0.2497(2) 0.7836(3) 0.2145(2) 0.256(16) Uani 0.50 1 d PG A 1 O9 O 0.3823(2) 0.4441(2) 0.22417(13) 0.098(6) Uani 0.50 1 d PGD B 1 C51 C 0.4628(12) 0.4842(10) 0.3693(6) 0.165(7) Uani 1 1 d . . . C60 C 0.1431(5) 0.7501(6) -0.1605(3) 0.100(3) Uani 1 1 d . . . H60A H 0.1025 0.7734 -0.1729 0.150 Uiso 1 1 calc R . . H60B H 0.1563 0.6982 -0.1758 0.150 Uiso 1 1 calc R . . H60C H 0.1785 0.7929 -0.1624 0.150 Uiso 1 1 calc R . . C61 C 0.1026(9) 0.3229(14) 0.1113(5) 0.216(9) Uani 1 1 d . . . H61A H 0.0561 0.3167 0.1195 0.324 Uiso 1 1 calc R . . H61B H 0.1198 0.3774 0.1221 0.324 Uiso 1 1 calc R . . H61C H 0.1284 0.2755 0.1232 0.324 Uiso 1 1 calc R . . C62 C 0.4928(14) 0.4840(13) 0.4457(9) 0.294(18) Uani 1 1 d . . . H62A H 0.4698 0.4782 0.4728 0.441 Uiso 1 1 calc R B . H62B H 0.5151 0.5397 0.4445 0.441 Uiso 1 1 calc R . . H62C H 0.5255 0.4381 0.4429 0.441 Uiso 1 1 calc R . . C72 C 0.5295(2) 0.7371(2) 0.27007(12) 0.114(3) Uani 0.50 1 d P A 2 O20 O 0.55535(18) 0.6557(2) 0.26680(13) 0.285(13) Uani 0.50 1 d P A 2 C73 C 0.6170(2) 0.6367(3) 0.25320(18) 0.187(8) Uani 0.50 1 d P A 2 O9' O 0.4318(9) 0.4413(7) 0.2365(4) 0.111(6) Uani 0.50 1 d PD B 2 N12 N 0.2527(15) 0.530(2) 0.1530(9) 0.24(2) Uani 0.50 1 d P A 2 C53 C 0.3060(2) 0.6955(3) 0.18610(16) 0.288(13) Uani 0.50 1 d P A 2 C54 C 0.2598(3) 0.6528(4) 0.1495(2) 0.321(15) Uani 0.50 1 d P A 2 N11 N 0.3027(9) 0.6037(13) 0.2159(7) 0.118(6) Uani 0.50 1 d P A 2 C56 C 0.251(4) 0.470(4) 0.1462(12) 0.34(5) Uani 0.50 1 d P A 2 C57 C 0.2944(13) 0.4954(18) 0.2086(6) 0.30(4) Uani 0.50 1 d PD A 2 O19 O 0.5513(19) 0.7543(16) 0.3110(7) 0.244(15) Uani 0.50 1 d P A 2 O15 O 0.3072(2) 0.7520(3) 0.20068(17) 0.163(6) Uani 0.50 1 d P A 2 O17 O 0.321(3) 0.441(3) 0.2386(7) 0.37(3) Uani 0.50 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0281(4) 0.0347(4) 0.0395(4) 0.0001(2) 0.0014(2) 0.0013(2) Cl2 0.0414(7) 0.0371(6) 0.0473(7) 0.0045(5) 0.0031(5) 0.0036(5) Cl1 0.0411(7) 0.0489(8) 0.0796(11) 0.0235(7) -0.0008(7) -0.0047(6) N1 0.033(2) 0.035(2) 0.052(3) -0.0028(19) -0.0028(19) 0.0028(17) N2 0.032(2) 0.032(2) 0.039(2) -0.0006(17) 0.0020(17) 0.0017(16) N3 0.032(2) 0.037(2) 0.040(2) -0.0071(18) -0.0005(17) 0.0017(17) N4 0.030(2) 0.034(2) 0.053(3) -0.0060(18) -0.0062(18) 0.0005(17) N7 0.075(4) 0.055(3) 0.041(3) -0.008(2) 0.010(2) 0.002(3) O1 0.0367(19) 0.0312(18) 0.075(3) -0.0107(17) -0.0100(18) 0.0024(15) O2 0.042(2) 0.0365(19) 0.071(3) -0.0184(18) -0.0092(19) -0.0028(16) O3 0.046(2) 0.0400(19) 0.061(2) -0.0147(18) -0.0131(18) 0.0141(16) O4 0.0270(17) 0.0309(17) 0.071(3) -0.0130(16) 0.0016(16) 0.0012(13) O5 0.113(6) 0.233(11) 0.126(7) -0.026(6) 0.053(5) -0.060(6) O6 0.113(5) 0.102(5) 0.084(4) 0.018(3) 0.011(4) -0.009(4) O7 0.068(3) 0.056(2) 0.066(3) -0.004(2) 0.006(2) 0.010(2) O8 0.072(3) 0.073(3) 0.059(3) -0.003(2) -0.016(2) 0.016(2) O10 0.131(5) 0.049(2) 0.051(3) -0.013(2) 0.032(3) -0.011(3) O13 0.182(15) 0.49(4) 0.31(2) 0.23(2) 0.040(15) 0.008(16) O14 0.232(14) 0.140(8) 0.172(10) -0.023(7) -0.011(10) -0.010(8) C1 0.032(3) 0.039(3) 0.046(3) -0.004(2) 0.001(2) 0.005(2) C2 0.036(3) 0.036(3) 0.044(3) -0.009(2) -0.001(2) 0.003(2) C3 0.032(2) 0.033(2) 0.049(3) -0.001(2) 0.002(2) 0.0049(19) C4 0.037(3) 0.032(2) 0.044(3) -0.003(2) 0.000(2) -0.001(2) C5 0.031(2) 0.030(2) 0.043(3) -0.006(2) -0.003(2) 0.0044(19) C6 0.033(3) 0.034(2) 0.044(3) -0.004(2) 0.001(2) -0.001(2) C7 0.036(3) 0.038(3) 0.045(3) -0.014(2) -0.003(2) 0.004(2) C8 0.035(3) 0.030(2) 0.047(3) -0.008(2) -0.007(2) 0.002(2) C9 0.046(3) 0.041(3) 0.105(6) -0.017(3) 0.008(3) -0.008(3) C10 0.037(3) 0.064(4) 0.150(9) -0.030(5) 0.009(4) -0.014(3) C11 0.036(4) 0.064(4) 0.147(8) -0.028(5) -0.018(4) -0.011(3) C12 0.044(3) 0.046(3) 0.099(5) -0.016(3) -0.024(3) -0.002(3) C13 0.030(3) 0.028(2) 0.085(5) -0.013(3) -0.005(3) -0.001(2) C14 0.032(3) 0.025(2) 0.083(4) -0.014(3) -0.005(3) -0.0016(19) C15 0.044(3) 0.052(3) 0.065(4) -0.002(3) 0.009(3) 0.006(3) C16 0.032(3) 0.066(4) 0.076(4) -0.004(3) 0.005(3) 0.009(3) C17 0.036(3) 0.053(3) 0.076(4) -0.007(3) -0.010(3) 0.011(2) C18 0.038(3) 0.033(2) 0.060(3) -0.006(2) -0.006(2) 0.004(2) C19 0.026(2) 0.027(2) 0.064(4) -0.012(2) -0.003(2) 0.0025(18) C20 0.034(3) 0.032(2) 0.063(4) -0.010(2) -0.005(2) 0.006(2) C21 0.093(6) 0.062(4) 0.094(7) -0.010(4) 0.031(5) -0.022(4) C22 0.056(4) 0.036(3) 0.061(4) -0.006(3) -0.007(3) 0.005(3) C28 0.237(13) 0.047(4) 0.063(5) -0.010(4) 0.064(7) -0.010(6) C29 0.053(3) 0.051(3) 0.043(3) -0.004(3) 0.003(3) -0.001(3) C30 0.066(4) 0.047(3) 0.042(3) -0.007(3) 0.006(3) 0.001(3) N8 0.178(8) 0.049(3) 0.053(4) -0.009(3) 0.044(4) -0.012(4) C32 0.275(17) 0.064(5) 0.062(5) -0.009(4) 0.075(8) -0.014(7) C33 0.287(19) 0.061(5) 0.041(5) -0.008(4) 0.056(7) -0.046(8) C34 0.147(10) 0.052(5) 0.151(10) 0.006(6) 0.080(9) -0.001(5) C35 0.135(10) 0.077(6) 0.111(8) 0.017(6) -0.004(8) -0.015(6) C36 0.174(12) 0.073(5) 0.081(7) -0.009(5) 0.051(7) -0.037(7) C37 0.123(10) 0.089(7) 0.175(13) -0.013(8) 0.068(9) -0.021(6) C38 0.225(17) 0.077(7) 0.113(10) -0.001(6) -0.004(10) -0.053(9) C39 0.110(6) 0.049(4) 0.060(4) -0.007(3) 0.034(4) -0.004(4) C40 0.206(12) 0.062(5) 0.058(5) -0.007(4) 0.002(6) -0.038(6) C41 0.33(2) 0.071(6) 0.057(6) -0.013(5) 0.032(9) -0.055(10) C42 0.34(3) 0.081(8) 0.157(14) -0.002(8) 0.157(17) -0.008(11) C43 0.27(2) 0.087(8) 0.24(2) 0.027(10) 0.200(18) 0.041(10) C44 0.174(11) 0.054(4) 0.124(8) 0.003(5) 0.084(8) 0.013(6) O11 0.122(9) 0.032(5) 0.172(13) 0.003(6) 0.100(10) 0.004(5) O12 0.144(8) 0.058(4) 0.139(8) 0.016(4) -0.048(6) -0.040(5) C45 0.094(8) 0.49(3) 0.270(19) -0.25(2) 0.016(10) -0.058(13) C46 0.133(13) 0.26(2) 0.165(14) 0.044(15) -0.007(11) -0.070(13) N9 0.082(11) 0.141(16) 0.135(15) 0.029(14) 0.030(10) 0.015(11) C48 0.108(15) 0.072(11) 0.128(17) 0.005(10) 0.033(13) 0.018(10) C49 0.090(11) 0.058(8) 0.065(9) 0.010(7) 0.027(8) 0.004(7) N10 0.068(7) 0.050(6) 0.040(5) 0.007(4) 0.003(5) -0.023(5) C70 0.116(8) 0.095(7) 0.276(18) -0.007(8) -0.072(10) 0.005(6) O18 0.32(2) 0.35(3) 0.199(15) -0.073(19) -0.140(16) 0.19(2) C71 0.321(15) 0.322(15) 0.321(15) 0.000(2) 0.000(2) 0.000(2) O16 0.095(13) 0.24(3) 0.44(4) -0.13(3) -0.03(2) 0.069(15) O9 0.198(17) 0.057(7) 0.038(6) -0.018(5) 0.030(8) -0.061(9) C51 0.22(2) 0.145(12) 0.131(13) 0.056(10) 0.046(14) -0.003(12) C60 0.111(7) 0.104(7) 0.084(6) -0.001(5) -0.020(5) 0.026(6) C61 0.194(17) 0.30(2) 0.154(14) 0.105(15) 0.067(12) 0.001(16) C62 0.43(4) 0.144(17) 0.31(3) -0.014(17) -0.23(3) 0.021(18) C72 0.144(8) 0.058(4) 0.139(8) 0.016(4) -0.048(6) -0.040(5) O20 0.094(8) 0.49(3) 0.270(19) -0.25(2) 0.016(10) -0.058(13) C73 0.133(13) 0.26(2) 0.165(14) 0.044(15) -0.007(11) -0.070(13) O9' 0.23(2) 0.052(6) 0.052(7) 0.001(5) 0.038(10) 0.004(9) N12 0.18(2) 0.35(4) 0.18(3) -0.22(3) 0.08(2) -0.12(3) C53 0.32(2) 0.35(3) 0.199(15) -0.073(19) -0.140(16) 0.19(2) C54 0.321(15) 0.322(15) 0.321(15) 0.000(2) 0.000(2) 0.000(2) N11 0.094(12) 0.127(14) 0.134(15) -0.010(12) 0.013(11) -0.004(11) C56 0.59(11) 0.33(7) 0.10(2) -0.03(3) 0.00(4) -0.28(8) C57 0.15(3) 0.44(7) 0.31(5) -0.32(5) 0.14(3) -0.18(4) O19 0.45(5) 0.18(2) 0.110(15) -0.022(14) 0.01(2) -0.06(2) O15 0.116(8) 0.095(7) 0.276(18) -0.007(8) -0.072(10) 0.005(6) O17 0.37(3) 0.37(3) 0.37(3) 0.000(2) 0.000(2) 0.000(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 Cu1 N2 2.054(4) . ? Cu1 N3 2.058(4) 5_665 ? Cu1 Cl1 2.2587(15) . ? Cu1 Cl2 2.2846(13) . ? Cu1 N7 2.335(5) . ? N1 C4 1.313(6) . ? N1 C1 1.315(7) . ? N2 C3 1.333(6) . ? N2 C2 1.336(6) . ? N3 C6 1.330(6) . ? N3 C7 1.336(6) . ? N3 Cu1 2.058(4) 5_665 ? N4 C5 1.315(6) . ? N4 C8 1.324(6) . ? N7 C29 1.312(8) . ? N7 C28 1.351(9) . ? O1 C4 1.352(6) . ? O1 C14 1.378(6) . ? O2 C8 1.372(6) . ? O2 C13 1.391(7) . ? O3 C1 1.377(6) . ? O3 C20 1.389(6) . ? O4 C5 1.366(6) . ? O4 C19 1.390(6) . ? O5 C21 1.290(11) . ? O5 C61 1.405(16) . ? O6 C21 1.227(11) . ? O7 C22 1.198(7) . ? O8 C22 1.338(7) . ? O8 C60 1.452(11) . ? O10 C30 1.338(7) . ? O10 C39 1.398(5) . ? O13 C51 1.24(2) . ? O14 C51 1.348(18) . ? O14 C62 1.54(2) . ? C1 C2 1.373(7) . ? C2 H2A 0.9500 . ? C3 C4 1.385(7) . ? C3 H3A 0.9500 . ? C5 C6 1.376(7) . ? C6 H6A 0.9500 . ? C7 C8 1.378(7) . ? C7 H7A 0.9500 . ? C9 C10 1.400(11) . ? C9 C14 1.401(9) . ? C9 C21 1.449(12) . ? C10 C11 1.366(13) . ? C10 H10A 0.9500 . ? C11 C12 1.351(11) . ? C11 H11A 0.9500 . ? C12 C13 1.377(8) . ? C12 H12A 0.9500 . ? C13 C14 1.364(9) . ? C15 C20 1.358(8) . ? C15 C16 1.375(9) . ? C15 H15A 0.9500 . ? C16 C17 1.370(9) . ? C16 H16A 0.9500 . ? C17 C18 1.395(8) . ? C17 H17A 0.9500 . ? C18 C19 1.404(7) . ? C18 C22 1.484(9) . ? C19 C20 1.393(8) . ? C28 C32 1.361(10) . ? C28 H28A 0.9500 . ? C29 C30 1.387(8) . ? C29 H29A 0.9500 . ? C30 N8 1.298(8) . ? N8 C32 1.324(10) . ? C32 O9' 1.424(12) . ? C32 O9 1.432(9) . ? C33 C34 1.3289 . ? C33 C38 1.3290 . ? C33 O9 1.4395 . ? C33 O9' 1.540(13) . ? C34 C35 1.3293 . ? C34 O11 1.3874 . ? C35 C36 1.3292 . ? C35 C51 1.49(2) . ? C36 C37 1.3287 . ? C36 H36A 0.9500 . ? C37 C38 1.3292 . ? C37 H37A 0.9500 . ? C38 O17 1.40(2) . ? C39 C40 1.3817 . ? C39 C44 1.3820 . ? C40 C41 1.3818 . ? C40 O12 1.5085(10) . ? C41 C42 1.3819 . ? C41 H41A 0.9500 . ? C42 C43 1.3821 . ? C42 H42A 0.9500 . ? C43 C44 1.3818 . ? C43 H43A 0.9500 . ? C44 C70 1.6123(11) . ? O11 C49 1.3467 . ? O12 C45 1.3775 . ? C45 C46 1.3504 . ? C45 N10 1.3505 . ? C46 N9 1.3506 . ? C46 H46A 0.9500 . ? N9 C48 1.3505 . ? C48 C49 1.3509 . ? C48 H48A 0.9500 . ? C49 N10 1.3507 . ? C70 O18 0.9952 . ? C70 O16 1.3366 . ? O18 C71 1.6317(11) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? N12 C56 0.97(6) . ? N11 C57 1.71(3) . ? C57 O17 1.38(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N3 169.68(17) . 5_665 ? N2 Cu1 Cl1 88.01(12) . . ? N3 Cu1 Cl1 88.83(12) 5_665 . ? N2 Cu1 Cl2 90.24(11) . . ? N3 Cu1 Cl2 90.56(12) 5_665 . ? Cl1 Cu1 Cl2 166.65(7) . . ? N2 Cu1 N7 91.97(19) . . ? N3 Cu1 N7 98.24(18) 5_665 . ? Cl1 Cu1 N7 99.17(14) . . ? Cl2 Cu1 N7 94.11(14) . . ? C4 N1 C1 114.8(4) . . ? C3 N2 C2 118.7(4) . . ? C3 N2 Cu1 118.6(3) . . ? C2 N2 Cu1 122.1(3) . . ? C6 N3 C7 118.0(4) . . ? C6 N3 Cu1 118.6(3) . 5_665 ? C7 N3 Cu1 122.6(3) . 5_665 ? C5 N4 C8 114.0(4) . . ? C29 N7 C28 117.1(6) . . ? C29 N7 Cu1 126.9(4) . . ? C28 N7 Cu1 115.1(4) . . ? C4 O1 C14 121.6(4) . . ? C8 O2 C13 117.4(4) . . ? C1 O3 C20 118.0(4) . . ? C5 O4 C19 121.5(4) . . ? C21 O5 C61 118.1(12) . . ? C22 O8 C60 115.0(6) . . ? C30 O10 C39 118.8(4) . . ? C51 O14 C62 120(2) . . ? N1 C1 C2 124.5(5) . . ? N1 C1 O3 118.3(4) . . ? C2 C1 O3 117.2(4) . . ? N2 C2 C1 119.0(5) . . ? N2 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? N2 C3 C4 118.9(4) . . ? N2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? N1 C4 O1 120.8(4) . . ? N1 C4 C3 124.0(5) . . ? O1 C4 C3 115.0(4) . . ? N4 C5 O4 120.4(4) . . ? N4 C5 C6 124.8(4) . . ? O4 C5 C6 114.7(4) . . ? N3 C6 C5 119.5(4) . . ? N3 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? N3 C7 C8 119.4(4) . . ? N3 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? N4 C8 O2 117.7(4) . . ? N4 C8 C7 124.3(5) . . ? O2 C8 C7 118.0(4) . . ? C10 C9 C14 117.2(8) . . ? C10 C9 C21 120.9(8) . . ? C14 C9 C21 121.9(7) . . ? C11 C10 C9 121.6(7) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C12 C11 C10 120.0(7) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C13 120.2(8) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 120.9(6) . . ? C14 C13 O2 120.5(5) . . ? C12 C13 O2 118.2(6) . . ? C13 C14 O1 116.8(5) . . ? C13 C14 C9 120.1(6) . . ? O1 C14 C9 122.6(6) . . ? C20 C15 C16 120.0(6) . . ? C20 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 120.5(6) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 121.5(6) . . ? C16 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? C17 C18 C19 117.0(6) . . ? C17 C18 C22 121.6(5) . . ? C19 C18 C22 121.3(5) . . ? O4 C19 C20 116.4(5) . . ? O4 C19 C18 122.0(5) . . ? C20 C19 C18 120.7(5) . . ? C15 C20 O3 118.8(5) . . ? C15 C20 C19 120.3(5) . . ? O3 C20 C19 120.5(5) . . ? O6 C21 O5 123.0(10) . . ? O6 C21 C9 125.6(8) . . ? O5 C21 C9 111.4(10) . . ? O7 C22 O8 123.8(6) . . ? O7 C22 C18 125.3(5) . . ? O8 C22 C18 111.0(5) . . ? N7 C28 C32 120.4(7) . . ? N7 C28 H28A 119.8 . . ? C32 C28 H28A 119.8 . . ? N7 C29 C30 121.0(6) . . ? N7 C29 H29A 119.5 . . ? C30 C29 H29A 119.5 . . ? N8 C30 O10 118.4(5) . . ? N8 C30 C29 122.2(6) . . ? O10 C30 C29 119.3(5) . . ? C30 N8 C32 116.8(6) . . ? N8 C32 C28 122.4(7) . . ? N8 C32 O9' 115.5(8) . . ? C28 C32 O9' 117.3(9) . . ? N8 C32 O9 116.7(7) . . ? C28 C32 O9 116.4(8) . . ? O9' C32 O9 44.2(7) . . ? C34 C33 C38 120.0 . . ? C34 C33 O9 128.8 . . ? C38 C33 O9 110.8 . . ? C34 C33 O9' 86.8(6) . . ? C38 C33 O9' 152.6(6) . . ? O9 C33 O9' 42.1(6) . . ? C33 C34 C35 120.0 . . ? C33 C34 O11 111.5 . . ? C35 C34 O11 128.3 . . ? C36 C35 C34 120.0 . . ? C36 C35 C51 121.0(8) . . ? C34 C35 C51 118.9(8) . . ? C37 C36 C35 120.0 . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? C33 C38 C37 120.0 . . ? C33 C38 O17 68(2) . . ? C37 C38 O17 164(2) . . ? C40 C39 C44 120.0 . . ? C40 C39 O10 122.2(3) . . ? C44 C39 O10 117.7(3) . . ? C39 C40 C41 120.0 . . ? C39 C40 O12 115.0 . . ? C41 C40 O12 125.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 C70 121.0 . . ? C39 C44 C70 118.8 . . ? C49 O11 C34 123.3 . . ? C45 O12 C40 123.9 . . ? C46 C45 N10 120.0 . . ? C46 C45 O12 125.1 . . ? N10 C45 O12 114.9 . . ? C45 C46 N9 120.0 . . ? C45 C46 H46A 120.0 . . ? N9 C46 H46A 120.0 . . ? C48 N9 C46 120.0 . . ? N9 C48 C49 120.0 . . ? N9 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? O11 C49 N10 117.0 . . ? O11 C49 C48 122.5 . . ? N10 C49 C48 120.0 . . ? C45 N10 C49 120.0 . . ? O18 C70 O16 117.2 . . ? O18 C70 C44 117.7 . . ? O16 C70 C44 100.0 . . ? C70 O18 C71 135.0 . . ? C32 O9 C33 110.4(4) . . ? O13 C51 O14 116(2) . . ? O13 C51 C35 129.7(17) . . ? O14 C51 C35 114.0(17) . . ? O8 C60 H60A 109.5 . . ? O8 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O8 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O5 C61 H61A 109.5 . . ? O5 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O5 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O14 C62 H62A 109.5 . . ? O14 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O14 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C32 O9' C33 105.4(9) . . ? O17 C57 N11 118(2) . . ? C57 O17 C38 113(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 N2 C3 53.2(11) 5_665 . . . ? Cl1 Cu1 N2 C3 125.5(4) . . . . ? Cl2 Cu1 N2 C3 -41.3(4) . . . . ? N7 Cu1 N2 C3 -135.4(4) . . . . ? N3 Cu1 N2 C2 -117.6(9) 5_665 . . . ? Cl1 Cu1 N2 C2 -45.3(4) . . . . ? Cl2 Cu1 N2 C2 147.9(4) . . . . ? N7 Cu1 N2 C2 53.8(4) . . . . ? N2 Cu1 N7 C29 -91.3(5) . . . . ? N3 Cu1 N7 C29 87.2(6) 5_665 . . . ? Cl1 Cu1 N7 C29 -3.0(6) . . . . ? Cl2 Cu1 N7 C29 178.4(5) . . . . ? N2 Cu1 N7 C28 77.3(7) . . . . ? N3 Cu1 N7 C28 -104.3(7) 5_665 . . . ? Cl1 Cu1 N7 C28 165.6(7) . . . . ? Cl2 Cu1 N7 C28 -13.1(7) . . . . ? C4 N1 C1 C2 -2.9(8) . . . . ? C4 N1 C1 O3 175.9(5) . . . . ? C20 O3 C1 N1 -25.0(7) . . . . ? C20 O3 C1 C2 153.9(5) . . . . ? C3 N2 C2 C1 -0.3(7) . . . . ? Cu1 N2 C2 C1 170.5(4) . . . . ? N1 C1 C2 N2 2.1(8) . . . . ? O3 C1 C2 N2 -176.7(5) . . . . ? C2 N2 C3 C4 -0.5(7) . . . . ? Cu1 N2 C3 C4 -171.6(4) . . . . ? C1 N1 C4 O1 -172.7(5) . . . . ? C1 N1 C4 C3 2.1(8) . . . . ? C14 O1 C4 N1 -4.7(8) . . . . ? C14 O1 C4 C3 -179.9(5) . . . . ? N2 C3 C4 N1 -0.5(8) . . . . ? N2 C3 C4 O1 174.5(5) . . . . ? C8 N4 C5 O4 -173.6(5) . . . . ? C8 N4 C5 C6 1.2(8) . . . . ? C19 O4 C5 N4 3.9(8) . . . . ? C19 O4 C5 C6 -171.4(5) . . . . ? C7 N3 C6 C5 -0.7(7) . . . . ? Cu1 N3 C6 C5 -171.1(4) 5_665 . . . ? N4 C5 C6 N3 0.1(8) . . . . ? O4 C5 C6 N3 175.1(5) . . . . ? C6 N3 C7 C8 0.0(7) . . . . ? Cu1 N3 C7 C8 170.1(4) 5_665 . . . ? C5 N4 C8 O2 176.2(5) . . . . ? C5 N4 C8 C7 -1.9(8) . . . . ? C13 O2 C8 N4 -33.3(7) . . . . ? C13 O2 C8 C7 144.9(5) . . . . ? N3 C7 C8 N4 1.4(8) . . . . ? N3 C7 C8 O2 -176.7(5) . . . . ? C14 C9 C10 C11 -0.3(10) . . . . ? C21 C9 C10 C11 -177.9(7) . . . . ? C9 C10 C11 C12 -1.8(12) . . . . ? C10 C11 C12 C13 1.1(11) . . . . ? C11 C12 C13 C14 1.7(9) . . . . ? C11 C12 C13 O2 175.2(6) . . . . ? C8 O2 C13 C14 -55.4(6) . . . . ? C8 O2 C13 C12 131.0(5) . . . . ? C12 C13 C14 O1 168.5(5) . . . . ? O2 C13 C14 O1 -4.9(7) . . . . ? C12 C13 C14 C9 -3.8(8) . . . . ? O2 C13 C14 C9 -177.1(5) . . . . ? C4 O1 C14 C13 111.5(6) . . . . ? C4 O1 C14 C9 -76.5(7) . . . . ? C10 C9 C14 C13 3.0(8) . . . . ? C21 C9 C14 C13 -179.4(6) . . . . ? C10 C9 C14 O1 -168.8(5) . . . . ? C21 C9 C14 O1 8.8(9) . . . . ? C20 C15 C16 C17 0.8(10) . . . . ? C15 C16 C17 C18 -1.4(10) . . . . ? C16 C17 C18 C19 1.0(8) . . . . ? C16 C17 C18 C22 -175.0(6) . . . . ? C5 O4 C19 C20 106.0(5) . . . . ? C5 O4 C19 C18 -84.8(6) . . . . ? C17 C18 C19 O4 -169.0(5) . . . . ? C22 C18 C19 O4 7.1(7) . . . . ? C17 C18 C19 C20 -0.2(7) . . . . ? C22 C18 C19 C20 175.9(5) . . . . ? C16 C15 C20 O3 172.5(5) . . . . ? C16 C15 C20 C19 0.0(9) . . . . ? C1 O3 C20 C15 126.8(5) . . . . ? C1 O3 C20 C19 -60.8(6) . . . . ? O4 C19 C20 C15 169.0(5) . . . . ? C18 C19 C20 C15 -0.3(7) . . . . ? O4 C19 C20 O3 -3.3(6) . . . . ? C18 C19 C20 O3 -172.7(4) . . . . ? C61 O5 C21 O6 3.4(18) . . . . ? C61 O5 C21 C9 -174.4(12) . . . . ? C10 C9 C21 O6 170.1(8) . . . . ? C14 C9 C21 O6 -7.4(12) . . . . ? C10 C9 C21 O5 -12.1(11) . . . . ? C14 C9 C21 O5 170.4(7) . . . . ? C60 O8 C22 O7 -3.4(9) . . . . ? C60 O8 C22 C18 176.2(6) . . . . ? C17 C18 C22 O7 -177.6(6) . . . . ? C19 C18 C22 O7 6.5(8) . . . . ? C17 C18 C22 O8 2.8(7) . . . . ? C19 C18 C22 O8 -173.1(5) . . . . ? C29 N7 C28 C32 -0.9(17) . . . . ? Cu1 N7 C28 C32 -170.6(11) . . . . ? C28 N7 C29 C30 0.7(11) . . . . ? Cu1 N7 C29 C30 169.0(5) . . . . ? C39 O10 C30 N8 -1.9(10) . . . . ? C39 O10 C30 C29 176.4(5) . . . . ? N7 C29 C30 N8 -2.0(11) . . . . ? N7 C29 C30 O10 179.9(6) . . . . ? O10 C30 N8 C32 -178.7(10) . . . . ? C29 C30 N8 C32 3.1(14) . . . . ? C30 N8 C32 C28 -3(2) . . . . ? C30 N8 C32 O9' 151.7(11) . . . . ? C30 N8 C32 O9 -158.8(9) . . . . ? N7 C28 C32 N8 2(2) . . . . ? N7 C28 C32 O9' -152.3(13) . . . . ? N7 C28 C32 O9 157.8(10) . . . . ? C38 C33 C34 C35 0.0 . . . . ? O9 C33 C34 C35 -172.3 . . . . ? O9' C33 C34 C35 -174.1(5) . . . . ? C38 C33 C34 O11 175.3 . . . . ? O9 C33 C34 O11 3.0 . . . . ? O9' C33 C34 O11 1.2(5) . . . . ? C33 C34 C35 C36 0.0 . . . . ? O11 C34 C35 C36 -174.4 . . . . ? C33 C34 C35 C51 -176.0(7) . . . . ? O11 C34 C35 C51 9.7(7) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C51 C35 C36 C37 175.9(7) . . . . ? C35 C36 C37 C38 0.0 . . . . ? C34 C33 C38 C37 0.0 . . . . ? O9 C33 C38 C37 173.6 . . . . ? O9' C33 C38 C37 167.0(10) . . . . ? C34 C33 C38 O17 -164.8(18) . . . . ? O9 C33 C38 O17 8.7(18) . . . . ? O9' C33 C38 O17 2(2) . . . . ? C36 C37 C38 C33 0.0 . . . . ? C36 C37 C38 O17 116(6) . . . . ? C30 O10 C39 C40 96.5(6) . . . . ? C30 O10 C39 C44 -87.2(6) . . . . ? C44 C39 C40 C41 0.0 . . . . ? O10 C39 C40 C41 176.3(3) . . . . ? C44 C39 C40 O12 179.4 . . . . ? O10 C39 C40 O12 -4.3(3) . . . . ? C39 C40 C41 C42 0.0 . . . . ? O12 C40 C41 C42 -179.3 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C39 0.0 . . . . ? C42 C43 C44 C70 -175.7 . . . . ? C40 C39 C44 C43 0.0 . . . . ? O10 C39 C44 C43 -176.5(3) . . . . ? C40 C39 C44 C70 175.8 . . . . ? O10 C39 C44 C70 -0.6(3) . . . . ? C33 C34 O11 C49 106.3 . . . . ? C35 C34 O11 C49 -79.0 . . . . ? C39 C40 O12 C45 -74.8 . . . . ? C41 C40 O12 C45 104.6 . . . . ? C40 O12 C45 C46 166.3 . . . . ? C40 O12 C45 N10 -11.7 . . . . ? N10 C45 C46 N9 0.0 . . . . ? O12 C45 C46 N9 -177.9 . . . . ? C45 C46 N9 C48 0.0 . . . . ? C46 N9 C48 C49 0.0 . . . . ? C34 O11 C49 N10 -13.6 . . . . ? C34 O11 C49 C48 174.4 . . . . ? N9 C48 C49 O11 171.8 . . . . ? N9 C48 C49 N10 0.0 . . . . ? C46 C45 N10 C49 0.0 . . . . ? O12 C45 N10 C49 178.1 . . . . ? O11 C49 N10 C45 -172.3 . . . . ? C48 C49 N10 C45 0.0 . . . . ? C43 C44 C70 O18 -122.5 . . . . ? C39 C44 C70 O18 61.7 . . . . ? C43 C44 C70 O16 5.5 . . . . ? C39 C44 C70 O16 -170.3 . . . . ? O16 C70 O18 C71 46.1 . . . . ? C44 C70 O18 C71 165.4 . . . . ? N8 C32 O9 C33 -38.3(13) . . . . ? C28 C32 O9 C33 164.7(10) . . . . ? O9' C32 O9 C33 61.8(7) . . . . ? C34 C33 O9 C32 -60.5(6) . . . . ? C38 C33 O9 C32 126.6(6) . . . . ? O9' C33 O9 C32 -57.9(8) . . . . ? C62 O14 C51 O13 2(3) . . . . ? C62 O14 C51 C35 179.8(12) . . . . ? C36 C35 C51 O13 -165.6(19) . . . . ? C34 C35 C51 O13 10(2) . . . . ? C36 C35 C51 O14 16.5(15) . . . . ? C34 C35 C51 O14 -167.6(9) . . . . ? N8 C32 O9' C33 49.7(16) . . . . ? C28 C32 O9' C33 -154.0(12) . . . . ? O9 C32 O9' C33 -53.2(7) . . . . ? C34 C33 O9' C32 -126.2(10) . . . . ? C38 C33 O9' C32 65.1(15) . . . . ? O9 C33 O9' C32 55.9(9) . . . . ? N11 C57 O17 C38 37(6) . . . . ? C33 C38 O17 C57 -118(5) . . . . ? C37 C38 O17 C57 119(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.271 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.129 data_z _database_code_depnum_ccdc_archive 'CCDC 825943' #TrackingRef '- cif.10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H40 N8 O21 Zn' _chemical_formula_weight 1142.28 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.9673(7) _cell_length_b 20.9503(8) _cell_length_c 13.7307(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.4960(10) _cell_angle_gamma 90.00 _cell_volume 4872.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9301 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.66 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7461 _exptl_absorpt_correction_T_max 0.9650 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54979 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8552 _reflns_number_gt 6955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0619P)^2^+11.4327P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8552 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1391 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Zn1 Zn 0.64237(2) 0.764594(17) 0.40126(3) 0.02070(12) Uani 1 1 d . . . O9 O 0.56466(13) 0.80773(10) -0.08891(16) 0.0219(5) Uani 1 1 d . . . O10 O 0.56425(15) 0.86868(12) -0.2228(2) 0.0349(6) Uani 1 1 d . . . O11 O 0.09991(17) 0.88111(14) -0.1113(2) 0.0450(7) Uani 1 1 d . . . O12 O 0.07563(17) 0.83938(15) -0.2675(2) 0.0473(7) Uani 1 1 d . . . O13 O 0.52470(12) 0.89891(10) 0.04156(16) 0.0216(5) Uani 1 1 d . . . O14 O 0.40011(14) 0.97709(11) 0.04188(19) 0.0286(5) Uani 1 1 d . . . O15 O 0.34634(14) 0.76160(12) 0.10761(19) 0.0315(6) Uani 1 1 d . . . O16 O 0.21098(13) 0.83140(12) 0.04841(18) 0.0291(5) Uani 1 1 d . . . N5 N 0.54364(15) 0.80270(13) 0.2638(2) 0.0237(6) Uani 1 1 d . . . N6 N 0.43668(15) 0.82710(13) 0.0691(2) 0.0216(6) Uani 1 1 d . . . N7 N 0.2652(2) 0.97941(18) 0.1842(3) 0.0454(9) Uani 1 1 d . . . N8 N 0.30059(16) 0.90682(13) 0.0389(2) 0.0239(6) Uani 1 1 d . . . O1 O 1.15326(18) 0.57882(14) 0.8396(2) 0.0456(7) Uani 1 1 d . . . O2 O 1.21876(15) 0.61902(13) 0.9953(2) 0.0409(7) Uani 1 1 d . . . O3 O 0.70715(19) 0.59086(14) 0.9954(2) 0.0516(8) Uani 1 1 d . . . O4 O 0.71996(13) 0.66609(10) 0.88767(17) 0.0233(5) Uani 1 1 d . . . O5 O 1.05038(14) 0.66653(12) 0.71982(17) 0.0286(5) Uani 1 1 d . . . O6 O 0.93129(14) 0.74876(12) 0.71715(19) 0.0317(6) Uani 1 1 d . . . O7 O 0.84589(13) 0.52393(11) 0.67466(18) 0.0269(5) Uani 1 1 d . . . O8 O 0.74097(12) 0.60173(10) 0.72171(16) 0.0208(5) Uani 1 1 d . . . N1 N 0.95116(18) 0.56667(15) 0.5055(2) 0.0317(7) Uani 1 1 d . . . N2 N 0.95269(15) 0.59182(13) 0.7039(2) 0.0222(6) Uani 1 1 d . . . N3 N 0.73675(16) 0.72323(13) 0.5387(2) 0.0262(6) Uani 1 1 d . . . N4 N 0.83602(15) 0.67694(12) 0.7263(2) 0.0206(6) Uani 1 1 d . . . C1 C 1.09390(19) 0.66201(15) 0.9064(3) 0.0238(7) Uani 1 1 d . . . C2 C 1.04055(19) 0.68334(16) 0.8134(2) 0.0229(7) Uani 1 1 d . . . C3 C 0.98061(19) 0.72497(16) 0.8123(3) 0.0250(7) Uani 1 1 d . . . C4 C 0.9724(2) 0.74565(17) 0.9037(3) 0.0297(8) Uani 1 1 d . . . H4A H 0.9314 0.7746 0.9026 0.036 Uiso 1 1 calc R . . C5 C 1.0243(2) 0.72390(17) 0.9968(3) 0.0316(8) Uani 1 1 d . . . H5A H 1.0184 0.7372 1.0599 0.038 Uiso 1 1 calc R . . C6 C 1.0848(2) 0.68294(17) 0.9979(3) 0.0285(8) Uani 1 1 d . . . H6A H 1.1208 0.6688 1.0622 0.034 Uiso 1 1 calc R . . C7 C 0.79248(18) 0.57031(15) 0.9004(2) 0.0213(7) Uani 1 1 d . . . C8 C 0.84319(19) 0.53060(16) 0.9746(3) 0.0249(7) Uani 1 1 d . . . H8A H 0.8397 0.5294 1.0421 0.030 Uiso 1 1 calc R . . C9 C 0.89844(19) 0.49293(17) 0.9521(3) 0.0284(8) Uani 1 1 d . . . H9A H 0.9338 0.4674 1.0046 0.034 Uiso 1 1 calc R . . C10 C 0.90239(19) 0.49233(16) 0.8533(3) 0.0271(7) Uani 1 1 d . . . H10A H 0.9400 0.4663 0.8372 0.033 Uiso 1 1 calc R . . C11 C 0.85109(18) 0.53001(15) 0.7785(3) 0.0222(7) Uani 1 1 d . . . C12 C 0.79719(17) 0.56954(14) 0.8016(2) 0.0183(6) Uani 1 1 d . . . C13 C 1.00136(19) 0.62056(16) 0.6638(3) 0.0236(7) Uani 1 1 d . . . C14 C 1.0028(2) 0.60775(17) 0.5654(3) 0.0268(7) Uani 1 1 d . . . H14A H 1.0404 0.6282 0.5410 0.032 Uiso 1 1 calc R . . C15 C 0.8990(2) 0.53904(17) 0.5421(3) 0.0303(8) Uani 1 1 d . . . H15A H 0.8605 0.5105 0.5000 0.036 Uiso 1 1 calc R . . C16 C 0.90149(18) 0.55228(15) 0.6419(3) 0.0224(7) Uani 1 1 d . . . C17 C 0.85758(19) 0.72327(16) 0.6762(3) 0.0240(7) Uani 1 1 d . . . C18 C 0.8088(2) 0.74756(17) 0.5824(3) 0.0284(8) Uani 1 1 d . . . H18A H 0.8267 0.7813 0.5496 0.034 Uiso 1 1 calc R . . C19 C 0.71439(19) 0.67480(16) 0.5857(2) 0.0243(7) Uani 1 1 d . . . H19A H 0.6638 0.6559 0.5558 0.029 Uiso 1 1 calc R . . C20 C 0.76593(18) 0.65257(15) 0.6786(2) 0.0194(6) Uani 1 1 d . . . C21 C 1.1578(2) 0.61592(17) 0.9085(3) 0.0308(8) Uani 1 1 d . . . C22 C 0.73470(19) 0.61227(16) 0.9293(3) 0.0242(7) Uani 1 1 d . . . C23 C 0.4698(2) 0.89125(16) -0.1442(3) 0.0272(8) Uani 1 1 d . . . C24 C 0.46411(19) 0.91289(15) -0.0516(2) 0.0214(7) Uani 1 1 d . . . C25 C 0.4013(2) 0.95052(15) -0.0510(3) 0.0243(7) Uani 1 1 d . . . C26 C 0.3411(2) 0.96379(19) -0.1416(3) 0.0375(9) Uani 1 1 d . . . H26A H 0.2973 0.9889 -0.1405 0.045 Uiso 1 1 calc R . . C27 C 0.3446(3) 0.9406(2) -0.2336(3) 0.0552(13) Uani 1 1 d . . . H27A H 0.3026 0.9487 -0.2961 0.066 Uiso 1 1 calc R . . C28 C 0.4093(3) 0.9054(2) -0.2351(3) 0.0477(11) Uani 1 1 d . . . H28A H 0.4123 0.8908 -0.2992 0.057 Uiso 1 1 calc R . . C29 C 0.1867(2) 0.80207(17) -0.1322(3) 0.0296(8) Uani 1 1 d . . . C30 C 0.2104(2) 0.76542(18) -0.2016(3) 0.0359(9) Uani 1 1 d . . . H30A H 0.1791 0.7661 -0.2727 0.043 Uiso 1 1 calc R . . C31 C 0.2767(2) 0.72879(19) -0.1709(3) 0.0392(9) Uani 1 1 d . . . H31A H 0.2912 0.7044 -0.2201 0.047 Uiso 1 1 calc R . . C32 C 0.3228(2) 0.72738(18) -0.0677(3) 0.0356(9) Uani 1 1 d . . . H32A H 0.3691 0.7019 -0.0451 0.043 Uiso 1 1 calc R . . C33 C 0.3005(2) 0.76358(16) 0.0023(3) 0.0274(8) Uani 1 1 d . . . C34 C 0.2328(2) 0.79964(16) -0.0275(3) 0.0258(7) Uani 1 1 d . . . C35 C 0.50631(18) 0.85538(15) 0.1032(2) 0.0194(6) Uani 1 1 d . . . C36 C 0.56176(18) 0.84260(15) 0.1995(2) 0.0219(7) Uani 1 1 d . . . H36A H 0.6123 0.8622 0.2193 0.026 Uiso 1 1 calc R . . C37 C 0.47106(19) 0.77699(16) 0.2338(3) 0.0245(7) Uani 1 1 d . . . H37A H 0.4555 0.7504 0.2796 0.029 Uiso 1 1 calc R . . C38 C 0.41901(18) 0.78950(15) 0.1357(3) 0.0223(7) Uani 1 1 d . . . C39 C 0.3388(2) 0.96003(17) 0.0748(3) 0.0270(7) Uani 1 1 d . . . C40 C 0.3209(2) 0.9978(2) 0.1458(3) 0.0400(9) Uani 1 1 d . . . H40A H 0.3482 1.0369 0.1675 0.048 Uiso 1 1 calc R . . C41 C 0.2291(2) 0.92388(19) 0.1534(3) 0.0352(9) Uani 1 1 d . . . H41A H 0.1910 0.9087 0.1820 0.042 Uiso 1 1 calc R . . C42 C 0.24747(19) 0.88856(17) 0.0798(2) 0.0253(7) Uani 1 1 d . . . C43 C 0.53920(19) 0.85335(16) -0.1513(2) 0.0231(7) Uani 1 1 d . . . C44 C 0.1157(2) 0.84184(18) -0.1771(3) 0.0330(8) Uani 1 1 d . . . O01 O 0.61240(16) 0.81790(13) 0.5092(2) 0.0407(7) Uani 1 1 d . . . H01 H 0.6331 0.8540 0.5105 0.061 Uiso 1 1 calc R . . O02 O 0.67463(14) 0.71233(12) 0.2923(2) 0.0308(6) Uani 1 1 d . . . H02 H 0.6413 0.6830 0.2842 0.046 Uiso 1 1 calc R . . O03 O 0.97056(17) 0.55497(15) 0.3156(2) 0.0465(7) Uani 1 1 d . . . H03A H 0.9622 0.5520 0.3721 0.056 Uiso 1 1 calc R . . C03 C 0.9049(3) 0.5821(3) 0.2417(4) 0.0636(14) Uani 1 1 d . . . H03D H 0.8615 0.5511 0.2219 0.095 Uiso 1 1 calc R . . H03C H 0.9185 0.5939 0.1806 0.095 Uiso 1 1 calc R . . H03B H 0.8885 0.6203 0.2705 0.095 Uiso 1 1 calc R . . O04 O 0.3318(3) 0.5409(2) 1.0077(4) 0.0956(14) Uani 1 1 d . . . H04D H 0.3218 0.5035 1.0218 0.115 Uiso 1 1 calc R . . O05 O 0.5033(6) 0.4705(4) 0.8589(6) 0.194(3) Uani 1 1 d . . . H05A H 0.4818 0.4458 0.8092 0.291 Uiso 1 1 calc R . . C01 C 0.5410(2) 0.82469(16) 0.5238(4) 0.0694(16) Uani 1 1 d . . . H01A H 0.5020 0.8412 0.4604 0.104 Uiso 1 1 calc R . . H01B H 0.5464 0.8546 0.5806 0.104 Uiso 1 1 calc R . . H01C H 0.5235 0.7831 0.5408 0.104 Uiso 1 1 calc R . . C02 C 0.75033(18) 0.6853(2) 0.3069(3) 0.0514(11) Uani 1 1 d R . . H02A H 0.7909 0.7184 0.3312 0.077 Uiso 1 1 calc R . . H02B H 0.7516 0.6679 0.2412 0.077 Uiso 1 1 calc R . . H02C H 0.7606 0.6511 0.3583 0.077 Uiso 1 1 calc R . . C04 C 0.35624(19) 0.5397(3) 0.9330(3) 0.184(6) Uani 1 1 d R . . H04A H 0.3596 0.5834 0.9093 0.277 Uiso 1 1 calc R . . H04B H 0.3197 0.5149 0.8767 0.277 Uiso 1 1 calc R . . H04C H 0.4087 0.5200 0.9541 0.277 Uiso 1 1 calc R . . C05 C 0.50703(19) 0.5340(2) 0.8199(3) 0.329(15) Uani 1 1 d R . . H05B H 0.5385 0.5611 0.8770 0.493 Uiso 1 1 d R . . H05C H 0.4536 0.5515 0.7910 0.493 Uiso 1 1 d R . . H05D H 0.5317 0.5328 0.7661 0.493 Uiso 1 1 d 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 Zn1 0.0209(2) 0.0203(2) 0.0189(2) 0.00176(15) 0.00392(15) -0.00261(14) O9 0.0235(11) 0.0196(11) 0.0184(11) -0.0005(9) 0.0013(9) 0.0048(9) O10 0.0399(15) 0.0318(14) 0.0377(15) 0.0103(12) 0.0194(12) 0.0095(11) O11 0.0433(16) 0.0528(18) 0.0360(16) 0.0012(13) 0.0095(13) 0.0078(14) O12 0.0421(16) 0.0574(19) 0.0319(16) 0.0022(13) -0.0017(13) 0.0040(14) O13 0.0225(11) 0.0225(12) 0.0183(11) 0.0034(9) 0.0048(9) -0.0039(9) O14 0.0350(13) 0.0228(12) 0.0333(13) -0.0077(10) 0.0186(11) -0.0066(10) O15 0.0225(12) 0.0377(14) 0.0278(13) 0.0096(11) -0.0001(10) -0.0101(10) O16 0.0253(12) 0.0340(14) 0.0270(13) 0.0018(10) 0.0075(10) -0.0081(10) N5 0.0215(14) 0.0256(15) 0.0219(14) 0.0034(12) 0.0045(11) 0.0007(11) N6 0.0198(13) 0.0224(14) 0.0200(14) 0.0032(11) 0.0032(11) -0.0008(11) N7 0.050(2) 0.053(2) 0.044(2) -0.0146(17) 0.0284(17) -0.0067(17) N8 0.0253(14) 0.0236(15) 0.0228(14) 0.0018(12) 0.0081(12) -0.0011(12) O1 0.0653(19) 0.0385(16) 0.0426(17) 0.0041(13) 0.0309(15) 0.0141(14) O2 0.0329(14) 0.0375(15) 0.0468(17) 0.0115(13) 0.0062(13) 0.0008(12) O3 0.072(2) 0.0447(17) 0.0598(19) 0.0262(15) 0.0509(17) 0.0290(15) O4 0.0257(12) 0.0185(12) 0.0248(12) -0.0004(9) 0.0072(10) 0.0035(9) O5 0.0328(13) 0.0343(14) 0.0196(12) -0.0026(10) 0.0099(10) -0.0137(11) O6 0.0231(12) 0.0347(14) 0.0275(13) 0.0105(11) -0.0046(10) -0.0094(10) O7 0.0250(12) 0.0313(13) 0.0265(12) -0.0091(10) 0.0113(10) -0.0084(10) O8 0.0192(11) 0.0212(11) 0.0197(11) 0.0039(9) 0.0033(9) -0.0018(9) N1 0.0376(17) 0.0364(17) 0.0223(15) -0.0034(13) 0.0117(13) -0.0030(14) N2 0.0227(14) 0.0229(14) 0.0214(14) -0.0028(11) 0.0081(11) -0.0009(11) N3 0.0249(15) 0.0259(15) 0.0230(15) 0.0060(12) 0.0015(12) -0.0019(12) N4 0.0205(13) 0.0197(14) 0.0194(14) 0.0004(11) 0.0036(11) -0.0012(11) C1 0.0259(17) 0.0208(17) 0.0236(17) 0.0006(13) 0.0067(14) -0.0062(13) C2 0.0268(17) 0.0228(17) 0.0192(16) 0.0003(13) 0.0078(13) -0.0100(14) C3 0.0229(16) 0.0251(18) 0.0213(17) 0.0038(14) -0.0003(13) -0.0069(13) C4 0.0284(18) 0.0253(18) 0.032(2) -0.0018(15) 0.0060(15) -0.0014(14) C5 0.038(2) 0.032(2) 0.0240(18) -0.0057(15) 0.0087(16) -0.0014(16) C6 0.0309(18) 0.0284(19) 0.0206(17) 0.0007(14) 0.0009(14) -0.0017(15) C7 0.0226(16) 0.0181(16) 0.0228(17) -0.0003(13) 0.0071(13) -0.0014(13) C8 0.0242(17) 0.0270(18) 0.0224(17) 0.0052(14) 0.0064(14) 0.0020(14) C9 0.0210(16) 0.0256(18) 0.035(2) 0.0090(15) 0.0043(15) 0.0036(14) C10 0.0225(16) 0.0199(17) 0.040(2) 0.0006(15) 0.0122(15) 0.0023(13) C11 0.0227(16) 0.0202(16) 0.0252(17) -0.0053(13) 0.0100(14) -0.0063(13) C12 0.0179(15) 0.0135(15) 0.0208(16) 0.0021(12) 0.0029(12) -0.0018(12) C13 0.0225(16) 0.0254(17) 0.0215(17) 0.0003(14) 0.0055(13) -0.0012(13) C14 0.0299(18) 0.0311(19) 0.0208(17) 0.0005(14) 0.0105(14) -0.0026(15) C15 0.0305(18) 0.032(2) 0.0260(18) -0.0082(15) 0.0064(15) -0.0076(15) C16 0.0202(16) 0.0229(17) 0.0235(17) -0.0030(13) 0.0063(13) 0.0013(13) C17 0.0219(16) 0.0228(17) 0.0240(17) 0.0001(14) 0.0031(13) -0.0025(13) C18 0.0290(18) 0.0272(18) 0.0265(18) 0.0068(15) 0.0059(15) -0.0057(14) C19 0.0201(16) 0.0269(18) 0.0218(17) 0.0040(14) 0.0014(13) -0.0025(13) C20 0.0214(16) 0.0182(16) 0.0186(15) 0.0009(13) 0.0066(13) -0.0002(12) C21 0.036(2) 0.0282(19) 0.032(2) 0.0078(16) 0.0173(17) -0.0018(15) C22 0.0263(17) 0.0243(18) 0.0209(17) 0.0024(14) 0.0065(14) 0.0025(14) C23 0.0330(19) 0.0245(18) 0.0235(18) 0.0046(14) 0.0086(15) 0.0111(14) C24 0.0254(16) 0.0163(15) 0.0202(16) 0.0036(13) 0.0044(13) -0.0008(13) C25 0.0316(18) 0.0176(16) 0.0270(18) 0.0038(13) 0.0144(15) 0.0023(13) C26 0.044(2) 0.037(2) 0.034(2) 0.0141(17) 0.0168(18) 0.0246(18) C27 0.058(3) 0.079(3) 0.023(2) 0.014(2) 0.0065(19) 0.046(3) C28 0.054(3) 0.066(3) 0.0205(19) 0.0035(19) 0.0085(18) 0.034(2) C29 0.0241(17) 0.0289(19) 0.0305(19) 0.0078(15) 0.0018(15) -0.0100(14) C30 0.043(2) 0.038(2) 0.0248(19) -0.0047(16) 0.0086(17) -0.0169(18) C31 0.043(2) 0.037(2) 0.038(2) -0.0087(18) 0.0150(18) -0.0069(18) C32 0.033(2) 0.029(2) 0.042(2) -0.0023(17) 0.0095(17) -0.0068(16) C33 0.0246(17) 0.0272(18) 0.0250(18) 0.0049(14) 0.0011(14) -0.0101(14) C34 0.0264(17) 0.0248(18) 0.0238(17) 0.0006(14) 0.0052(14) -0.0089(14) C35 0.0221(15) 0.0169(15) 0.0188(16) -0.0001(12) 0.0063(13) 0.0001(12) C36 0.0185(15) 0.0232(17) 0.0225(17) 0.0000(13) 0.0049(13) -0.0010(13) C37 0.0229(16) 0.0245(18) 0.0252(17) 0.0053(14) 0.0069(14) 0.0003(13) C38 0.0200(16) 0.0202(16) 0.0252(17) 0.0026(13) 0.0052(13) -0.0021(13) C39 0.0283(17) 0.0267(18) 0.0278(18) 0.0008(15) 0.0118(15) 0.0005(14) C40 0.046(2) 0.036(2) 0.045(2) -0.0152(18) 0.025(2) -0.0119(18) C41 0.034(2) 0.043(2) 0.031(2) -0.0017(17) 0.0148(16) -0.0039(17) C42 0.0227(16) 0.0310(19) 0.0183(16) 0.0054(14) 0.0017(13) 0.0000(14) C43 0.0249(16) 0.0215(17) 0.0188(16) -0.0044(13) 0.0017(13) 0.0009(13) C44 0.034(2) 0.034(2) 0.031(2) 0.0017(16) 0.0103(17) -0.0085(16) O01 0.0456(16) 0.0378(15) 0.0485(17) -0.0146(13) 0.0290(14) -0.0150(13) O02 0.0277(13) 0.0293(13) 0.0387(14) -0.0059(11) 0.0152(11) -0.0052(10) O03 0.0465(17) 0.0593(19) 0.0359(16) -0.0055(14) 0.0165(13) 0.0005(14) C03 0.065(3) 0.074(4) 0.039(3) 0.004(2) 0.000(2) -0.005(3) O04 0.095(3) 0.102(4) 0.089(3) 0.012(3) 0.030(3) 0.045(3) O05 0.239(9) 0.189(8) 0.141(6) -0.014(6) 0.047(6) 0.004(7) C01 0.060(3) 0.074(4) 0.093(4) -0.024(3) 0.051(3) -0.013(3) C02 0.038(2) 0.056(3) 0.069(3) -0.001(2) 0.029(2) 0.005(2) C04 0.363(18) 0.114(7) 0.090(6) 0.027(5) 0.094(9) 0.117(10) C05 0.301(19) 0.126(9) 0.35(2) 0.136(12) -0.162(17) -0.127(11) _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 Zn1 O4 2.064(2) 4_575 ? Zn1 O9 2.095(2) 4_576 ? Zn1 N3 2.247(3) . ? Zn1 N5 2.261(3) . ? Zn1 O01 2.063(3) . ? Zn1 O02 2.083(3) . ? O9 C43 1.263(4) . ? O9 Zn1 2.095(2) 4_575 ? O10 C43 1.251(4) . ? O11 C44 1.321(5) . ? O12 C44 1.210(5) . ? O13 C35 1.358(4) . ? O13 C24 1.406(4) . ? O14 C39 1.370(4) . ? O14 C25 1.398(4) . ? O15 C38 1.364(4) . ? O15 C33 1.405(4) . ? O16 C42 1.364(4) . ? O16 C34 1.398(4) . ? N5 C36 1.333(4) . ? N5 C37 1.342(4) . ? N6 C35 1.321(4) . ? N6 C38 1.323(4) . ? N7 C41 1.330(5) . ? N7 C40 1.335(5) . ? N8 C42 1.316(4) . ? N8 C39 1.316(4) . ? O1 C21 1.206(5) . ? O2 C21 1.324(5) . ? O3 C22 1.252(4) . ? O4 C22 1.252(4) . ? O4 Zn1 2.064(2) 4_576 ? O5 C13 1.358(4) . ? O5 C2 1.399(4) . ? O6 C17 1.363(4) . ? O6 C3 1.403(4) . ? O7 C16 1.362(4) . ? O7 C11 1.403(4) . ? O8 C20 1.365(4) . ? O8 C12 1.392(4) . ? N1 C14 1.330(5) . ? N1 C15 1.335(5) . ? N2 C16 1.317(4) . ? N2 C13 1.324(4) . ? N3 C18 1.334(4) . ? N3 C19 1.334(4) . ? N4 C20 1.313(4) . ? N4 C17 1.320(4) . ? C1 C2 1.390(5) . ? C1 C6 1.392(5) . ? C1 C21 1.493(5) . ? C2 C3 1.382(5) . ? C3 C4 1.381(5) . ? C4 C5 1.385(5) . ? C4 H4A 0.9500 . ? C5 C6 1.380(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.388(4) . ? C7 C8 1.393(5) . ? C7 C22 1.511(4) . ? C8 C9 1.381(5) . ? C8 H8A 0.9500 . ? C9 C10 1.382(5) . ? C9 H9A 0.9500 . ? C10 C11 1.377(5) . ? C10 H10A 0.9500 . ? C11 C12 1.389(4) . ? C13 C14 1.385(5) . ? C14 H14A 0.9500 . ? C15 C16 1.383(5) . ? C15 H15A 0.9500 . ? C17 C18 1.390(5) . ? C18 H18A 0.9500 . ? C19 C20 1.384(4) . ? C19 H19A 0.9500 . ? C23 C24 1.386(5) . ? C23 C28 1.387(5) . ? C23 C43 1.508(5) . ? C24 C25 1.378(5) . ? C25 C26 1.378(5) . ? C26 C27 1.375(6) . ? C26 H26A 0.9500 . ? C27 C28 1.381(6) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.396(5) . ? C29 C34 1.401(5) . ? C29 C44 1.475(5) . ? C30 C31 1.360(6) . ? C30 H30A 0.9500 . ? C31 C32 1.383(6) . ? C31 H31A 0.9500 . ? C32 C33 1.384(5) . ? C32 H32A 0.9500 . ? C33 C34 1.373(5) . ? C35 C36 1.390(4) . ? C36 H36A 0.9500 . ? C37 C38 1.384(5) . ? C37 H37A 0.9500 . ? C39 C40 1.374(5) . ? C40 H40A 0.9500 . ? C41 C42 1.379(5) . ? C41 H41A 0.9500 . ? O01 C01 1.370(4) . ? O01 H01 0.8400 . ? O02 C02 1.424(4) . ? O02 H02 0.8400 . ? O03 C03 1.396(6) . ? O03 H03A 0.8400 . ? C03 H03D 0.9800 . ? C03 H03C 0.9800 . ? C03 H03B 0.9800 . ? O04 C04 1.244(5) . ? O04 H04D 0.8400 . ? O05 C05 1.445(10) . ? O05 H05A 0.8400 . ? C01 H01A 0.9800 . ? C01 H01B 0.9800 . ? C01 H01C 0.9800 . ? C02 H02A 0.9800 . ? C02 H02B 0.9800 . ? C02 H02C 0.9800 . ? C04 H04A 0.9800 . ? C04 H04B 0.9800 . ? C04 H04C 0.9800 . ? C05 H05B 0.9797 . ? C05 H05C 0.9799 . ? C05 H05D 0.9802 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O9 177.94(9) 4_575 4_576 ? O4 Zn1 N3 90.23(9) 4_575 . ? O9 Zn1 N3 89.97(9) 4_576 . ? O4 Zn1 N5 92.38(9) 4_575 . ? O9 Zn1 N5 87.42(9) 4_576 . ? N3 Zn1 N5 177.39(10) . . ? C43 O9 Zn1 127.0(2) . 4_575 ? C35 O13 C24 115.6(2) . . ? C39 O14 C25 117.1(3) . . ? C38 O15 C33 117.1(3) . . ? C42 O16 C34 115.4(2) . . ? C36 N5 C37 118.4(3) . . ? C36 N5 Zn1 118.5(2) . . ? C37 N5 Zn1 121.7(2) . . ? C35 N6 C38 116.1(3) . . ? C41 N7 C40 118.5(3) . . ? C42 N8 C39 116.7(3) . . ? C22 O4 Zn1 129.7(2) . 4_576 ? C13 O5 C2 116.2(2) . . ? C17 O6 C3 118.0(3) . . ? C16 O7 C11 119.3(2) . . ? C20 O8 C12 117.5(2) . . ? C14 N1 C15 118.7(3) . . ? C16 N2 C13 115.6(3) . . ? C18 N3 C19 118.5(3) . . ? C18 N3 Zn1 125.3(2) . . ? C19 N3 Zn1 115.8(2) . . ? C20 N4 C17 115.2(3) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 C21 121.0(3) . . ? C6 C1 C21 120.5(3) . . ? C3 C2 C1 120.6(3) . . ? C3 C2 O5 119.1(3) . . ? C1 C2 O5 120.2(3) . . ? C4 C3 C2 120.5(3) . . ? C4 C3 O6 120.6(3) . . ? C2 C3 O6 118.8(3) . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C1 121.0(3) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? C12 C7 C8 118.0(3) . . ? C12 C7 C22 122.3(3) . . ? C8 C7 C22 119.7(3) . . ? C9 C8 C7 121.4(3) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C8 C9 C10 120.1(3) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 121.1(3) . . ? C10 C11 O7 120.4(3) . . ? C12 C11 O7 118.1(3) . . ? C7 C12 C11 120.3(3) . . ? C7 C12 O8 120.0(3) . . ? C11 C12 O8 119.1(3) . . ? N2 C13 O5 118.7(3) . . ? N2 C13 C14 123.2(3) . . ? O5 C13 C14 118.0(3) . . ? N1 C14 C13 119.5(3) . . ? N1 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? N1 C15 C16 119.4(3) . . ? N1 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? N2 C16 O7 119.4(3) . . ? N2 C16 C15 123.5(3) . . ? O7 C16 C15 117.1(3) . . ? N4 C17 O6 119.2(3) . . ? N4 C17 C18 123.2(3) . . ? O6 C17 C18 117.6(3) . . ? N3 C18 C17 119.6(3) . . ? N3 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? N3 C19 C20 119.0(3) . . ? N3 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? N4 C20 O8 119.1(3) . . ? N4 C20 C19 124.3(3) . . ? O8 C20 C19 116.5(3) . . ? O1 C21 O2 123.8(4) . . ? O1 C21 C1 123.5(3) . . ? O2 C21 C1 112.7(3) . . ? O3 C22 O4 125.4(3) . . ? O3 C22 C7 117.0(3) . . ? O4 C22 C7 117.6(3) . . ? C24 C23 C28 118.7(3) . . ? C24 C23 C43 123.2(3) . . ? C28 C23 C43 118.2(3) . . ? C25 C24 C23 120.3(3) . . ? C25 C24 O13 120.0(3) . . ? C23 C24 O13 119.6(3) . . ? C26 C25 C24 120.5(3) . . ? C26 C25 O14 119.8(3) . . ? C24 C25 O14 119.7(3) . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 119.9(4) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C27 C28 C23 120.8(4) . . ? C27 C28 H28A 119.6 . . ? C23 C28 H28A 119.6 . . ? C30 C29 C34 118.0(3) . . ? C30 C29 C44 116.3(3) . . ? C34 C29 C44 125.6(3) . . ? C31 C30 C29 122.3(4) . . ? C31 C30 H30A 118.9 . . ? C29 C30 H30A 118.9 . . ? C30 C31 C32 119.5(4) . . ? C30 C31 H31A 120.3 . . ? C32 C31 H31A 120.3 . . ? C31 C32 C33 119.2(4) . . ? C31 C32 H32A 120.4 . . ? C33 C32 H32A 120.4 . . ? C34 C33 C32 121.8(3) . . ? C34 C33 O15 118.6(3) . . ? C32 C33 O15 119.5(3) . . ? C33 C34 O16 118.8(3) . . ? C33 C34 C29 119.2(3) . . ? O16 C34 C29 122.0(3) . . ? N6 C35 O13 118.6(3) . . ? N6 C35 C36 123.0(3) . . ? O13 C35 C36 118.4(3) . . ? N5 C36 C35 119.7(3) . . ? N5 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? N5 C37 C38 119.6(3) . . ? N5 C37 H37A 120.2 . . ? C38 C37 H37A 120.2 . . ? N6 C38 O15 119.2(3) . . ? N6 C38 C37 123.0(3) . . ? O15 C38 C37 117.8(3) . . ? N8 C39 O14 118.3(3) . . ? N8 C39 C40 122.5(3) . . ? O14 C39 C40 119.2(3) . . ? N7 C40 C39 119.9(4) . . ? N7 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? N7 C41 C42 119.4(3) . . ? N7 C41 H41A 120.3 . . ? C42 C41 H41A 120.3 . . ? N8 C42 O16 117.5(3) . . ? N8 C42 C41 122.9(3) . . ? O16 C42 C41 119.7(3) . . ? O10 C43 O9 125.6(3) . . ? O10 C43 C23 115.9(3) . . ? O9 C43 C23 118.4(3) . . ? O12 C44 O11 122.5(4) . . ? O12 C44 C29 122.7(4) . . ? O11 C44 C29 114.8(3) . . ? C01 O01 H01 109.5 . . ? C02 O02 H02 109.5 . . ? C03 O03 H03A 109.5 . . ? O03 C03 H03D 109.5 . . ? O03 C03 H03C 109.5 . . ? H03D C03 H03C 109.5 . . ? O03 C03 H03B 109.5 . . ? H03D C03 H03B 109.5 . . ? H03C C03 H03B 109.5 . . ? C04 O04 H04D 109.5 . . ? C05 O05 H05A 109.5 . . ? O01 C01 H01A 109.5 . . ? O01 C01 H01B 109.5 . . ? H01A C01 H01B 109.5 . . ? O01 C01 H01C 109.5 . . ? H01A C01 H01C 109.5 . . ? H01B C01 H01C 109.5 . . ? O02 C02 H02A 109.5 . . ? O02 C02 H02B 109.5 . . ? H02A C02 H02B 109.5 . . ? O02 C02 H02C 109.5 . . ? H02A C02 H02C 109.5 . . ? H02B C02 H02C 109.5 . . ? O04 C04 H04A 109.5 . . ? O04 C04 H04B 109.5 . . ? H04A C04 H04B 109.5 . . ? O04 C04 H04C 109.5 . . ? H04A C04 H04C 109.5 . . ? H04B C04 H04C 109.5 . . ? O05 C05 H05B 108.9 . . ? O05 C05 H05C 109.5 . . ? H05B C05 H05C 109.5 . . ? O05 C05 H05D 110.0 . . ? H05B C05 H05D 109.4 . . ? H05C C05 H05D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Zn1 N5 C36 16.3(2) 4_575 . . . ? O9 Zn1 N5 C36 -161.6(2) 4_576 . . . ? N3 Zn1 N5 C36 -163(2) . . . . ? O4 Zn1 N5 C37 -177.3(3) 4_575 . . . ? O9 Zn1 N5 C37 4.7(3) 4_576 . . . ? N3 Zn1 N5 C37 3(2) . . . . ? O4 Zn1 N3 C18 3.9(3) 4_575 . . . ? O9 Zn1 N3 C18 -178.1(3) 4_576 . . . ? N5 Zn1 N3 C18 -176(2) . . . . ? O4 Zn1 N3 C19 176.0(2) 4_575 . . . ? O9 Zn1 N3 C19 -6.1(2) 4_576 . . . ? N5 Zn1 N3 C19 -4(2) . . . . ? C6 C1 C2 C3 0.8(5) . . . . ? C21 C1 C2 C3 178.6(3) . . . . ? C6 C1 C2 O5 176.1(3) . . . . ? C21 C1 C2 O5 -6.0(5) . . . . ? C13 O5 C2 C3 -80.5(4) . . . . ? C13 O5 C2 C1 104.1(3) . . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? O5 C2 C3 C4 -175.9(3) . . . . ? C1 C2 C3 O6 175.7(3) . . . . ? O5 C2 C3 O6 0.3(4) . . . . ? C17 O6 C3 C4 -80.5(4) . . . . ? C17 O6 C3 C2 103.3(4) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? O6 C3 C4 C5 -176.8(3) . . . . ? C3 C4 C5 C6 1.4(5) . . . . ? C4 C5 C6 C1 -1.1(5) . . . . ? C2 C1 C6 C5 0.0(5) . . . . ? C21 C1 C6 C5 -177.8(3) . . . . ? C12 C7 C8 C9 2.0(5) . . . . ? C22 C7 C8 C9 -178.1(3) . . . . ? C7 C8 C9 C10 -2.4(5) . . . . ? C8 C9 C10 C11 0.5(5) . . . . ? C9 C10 C11 C12 1.6(5) . . . . ? C9 C10 C11 O7 -171.0(3) . . . . ? C16 O7 C11 C10 -79.8(4) . . . . ? C16 O7 C11 C12 107.3(3) . . . . ? C8 C7 C12 C11 0.1(5) . . . . ? C22 C7 C12 C11 -179.8(3) . . . . ? C8 C7 C12 O8 171.4(3) . . . . ? C22 C7 C12 O8 -8.5(4) . . . . ? C10 C11 C12 C7 -2.0(5) . . . . ? O7 C11 C12 C7 170.9(3) . . . . ? C10 C11 C12 O8 -173.3(3) . . . . ? O7 C11 C12 O8 -0.5(4) . . . . ? C20 O8 C12 C7 114.6(3) . . . . ? C20 O8 C12 C11 -74.0(4) . . . . ? C16 N2 C13 O5 173.6(3) . . . . ? C16 N2 C13 C14 -3.9(5) . . . . ? C2 O5 C13 N2 -5.0(4) . . . . ? C2 O5 C13 C14 172.6(3) . . . . ? C15 N1 C14 C13 0.2(5) . . . . ? N2 C13 C14 N1 2.9(5) . . . . ? O5 C13 C14 N1 -174.7(3) . . . . ? C14 N1 C15 C16 -1.9(5) . . . . ? C13 N2 C16 O7 -175.7(3) . . . . ? C13 N2 C16 C15 2.1(5) . . . . ? C11 O7 C16 N2 -9.1(4) . . . . ? C11 O7 C16 C15 172.9(3) . . . . ? N1 C15 C16 N2 0.8(5) . . . . ? N1 C15 C16 O7 178.6(3) . . . . ? C20 N4 C17 O6 -176.2(3) . . . . ? C20 N4 C17 C18 3.3(5) . . . . ? C3 O6 C17 N4 -1.1(5) . . . . ? C3 O6 C17 C18 179.4(3) . . . . ? C19 N3 C18 C17 -1.7(5) . . . . ? Zn1 N3 C18 C17 170.2(2) . . . . ? N4 C17 C18 N3 -0.7(5) . . . . ? O6 C17 C18 N3 178.8(3) . . . . ? C18 N3 C19 C20 1.3(5) . . . . ? Zn1 N3 C19 C20 -171.3(2) . . . . ? C17 N4 C20 O8 175.9(3) . . . . ? C17 N4 C20 C19 -3.8(5) . . . . ? C12 O8 C20 N4 -13.8(4) . . . . ? C12 O8 C20 C19 165.9(3) . . . . ? N3 C19 C20 N4 1.6(5) . . . . ? N3 C19 C20 O8 -178.1(3) . . . . ? C2 C1 C21 O1 -25.8(5) . . . . ? C6 C1 C21 O1 152.0(4) . . . . ? C2 C1 C21 O2 156.0(3) . . . . ? C6 C1 C21 O2 -26.2(4) . . . . ? Zn1 O4 C22 O3 -4.8(5) 4_576 . . . ? Zn1 O4 C22 C7 177.3(2) 4_576 . . . ? C12 C7 C22 O3 146.7(3) . . . . ? C8 C7 C22 O3 -33.2(5) . . . . ? C12 C7 C22 O4 -35.2(5) . . . . ? C8 C7 C22 O4 144.9(3) . . . . ? C28 C23 C24 C25 -3.3(5) . . . . ? C43 C23 C24 C25 176.1(3) . . . . ? C28 C23 C24 O13 179.8(3) . . . . ? C43 C23 C24 O13 -0.7(5) . . . . ? C35 O13 C24 C25 74.7(4) . . . . ? C35 O13 C24 C23 -108.4(3) . . . . ? C23 C24 C25 C26 4.1(5) . . . . ? O13 C24 C25 C26 -179.1(3) . . . . ? C23 C24 C25 O14 -173.9(3) . . . . ? O13 C24 C25 O14 3.0(4) . . . . ? C39 O14 C25 C26 62.9(4) . . . . ? C39 O14 C25 C24 -119.1(3) . . . . ? C24 C25 C26 C27 -1.6(6) . . . . ? O14 C25 C26 C27 176.3(4) . . . . ? C25 C26 C27 C28 -1.6(7) . . . . ? C26 C27 C28 C23 2.3(8) . . . . ? C24 C23 C28 C27 0.2(7) . . . . ? C43 C23 C28 C27 -179.3(4) . . . . ? C34 C29 C30 C31 -1.0(5) . . . . ? C44 C29 C30 C31 177.1(3) . . . . ? C29 C30 C31 C32 0.0(6) . . . . ? C30 C31 C32 C33 -0.3(6) . . . . ? C31 C32 C33 C34 1.7(5) . . . . ? C31 C32 C33 O15 178.9(3) . . . . ? C38 O15 C33 C34 -112.6(3) . . . . ? C38 O15 C33 C32 70.1(4) . . . . ? C32 C33 C34 O16 175.4(3) . . . . ? O15 C33 C34 O16 -1.8(4) . . . . ? C32 C33 C34 C29 -2.8(5) . . . . ? O15 C33 C34 C29 180.0(3) . . . . ? C42 O16 C34 C33 82.6(4) . . . . ? C42 O16 C34 C29 -99.2(4) . . . . ? C30 C29 C34 C33 2.4(5) . . . . ? C44 C29 C34 C33 -175.6(3) . . . . ? C30 C29 C34 O16 -175.8(3) . . . . ? C44 C29 C34 O16 6.3(5) . . . . ? C38 N6 C35 O13 -174.2(3) . . . . ? C38 N6 C35 C36 5.9(5) . . . . ? C24 O13 C35 N6 4.3(4) . . . . ? C24 O13 C35 C36 -175.8(3) . . . . ? C37 N5 C36 C35 -1.3(5) . . . . ? Zn1 N5 C36 C35 165.5(2) . . . . ? N6 C35 C36 N5 -3.7(5) . . . . ? O13 C35 C36 N5 176.4(3) . . . . ? C36 N5 C37 C38 3.6(5) . . . . ? Zn1 N5 C37 C38 -162.7(2) . . . . ? C35 N6 C38 O15 176.4(3) . . . . ? C35 N6 C38 C37 -3.4(5) . . . . ? C33 O15 C38 N6 13.1(5) . . . . ? C33 O15 C38 C37 -167.1(3) . . . . ? N5 C37 C38 N6 -1.3(5) . . . . ? N5 C37 C38 O15 178.9(3) . . . . ? C42 N8 C39 O14 173.3(3) . . . . ? C42 N8 C39 C40 -4.7(5) . . . . ? C25 O14 C39 N8 21.3(4) . . . . ? C25 O14 C39 C40 -160.5(3) . . . . ? C41 N7 C40 C39 1.1(6) . . . . ? N8 C39 C40 N7 2.9(6) . . . . ? O14 C39 C40 N7 -175.1(4) . . . . ? C40 N7 C41 C42 -3.0(6) . . . . ? C39 N8 C42 O16 -175.8(3) . . . . ? C39 N8 C42 C41 2.8(5) . . . . ? C34 O16 C42 N8 -2.2(4) . . . . ? C34 O16 C42 C41 179.2(3) . . . . ? N7 C41 C42 N8 1.1(6) . . . . ? N7 C41 C42 O16 179.6(3) . . . . ? Zn1 O9 C43 O10 -10.5(5) 4_575 . . . ? Zn1 O9 C43 C23 166.0(2) 4_575 . . . ? C24 C23 C43 O10 -137.3(3) . . . . ? C28 C23 C43 O10 42.1(5) . . . . ? C24 C23 C43 O9 45.8(5) . . . . ? C28 C23 C43 O9 -134.8(4) . . . . ? C30 C29 C44 O12 6.1(5) . . . . ? C34 C29 C44 O12 -175.9(4) . . . . ? C30 C29 C44 O11 -172.9(3) . . . . ? C34 C29 C44 O11 5.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.199 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.080