data_global _publ_contact_author 'Hanton, Lyall R.' _publ_contact_author_email lhanton@Chemistry.otago.ac.nz _publ_author_address ; Department of Chemistry University of Otago PO Box 56 Dunedin New Zealand ; _publ_section_title ; ; loop_ _publ_author_name 'Hutchinson, Daniel J.' 'Hanton, Lyall R.' 'Moratti, Stephen C.' _journal_name_full 'Inorganic Chemistry' _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _ccdc_journal_depnumber ? _audit_creation_method SHELXL-97 data_Complex_1(djh783) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H28 F12 N8 O16 Pb2 S4' _chemical_formula_sum 'C31 H28 F12 N8 O16 Pb2 S4' _chemical_formula_weight 1539.23 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 '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 10.9614(5) _cell_length_b 14.1662(6) _cell_length_c 16.4345(7) _cell_angle_alpha 102.640(3) _cell_angle_beta 104.898(3) _cell_angle_gamma 100.224(3) _cell_volume 2331.31(19) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9916 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 31.35 _exptl_crystal_description 'rhomb' _exptl_crystal_colour 'yellow' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_max 0.93 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 7.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2961 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27213 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8638 _reflns_number_gt 7074 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^ > 2\s(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^)+(0.0793P)^2^+30.8234P] 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 8638 _refine_ls_number_parameters 661 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1575 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6716(14) 0.7545(11) 0.2141(10) 0.058(4) Uani 1 1 d . . . H1A H 0.7197 0.7080 0.2242 0.069 Uiso 1 1 calc R . . H1B H 0.5810 0.7350 0.1956 0.069 Uiso 1 1 calc R . . C2 C 0.7292(14) 0.8440(11) 0.2255(9) 0.053(3) Uani 1 1 d . . . H2 H 0.6793 0.8892 0.2150 0.064 Uiso 1 1 calc R . . C3 C 0.8710(12) 0.8795(9) 0.2544(8) 0.041(3) Uani 1 1 d . . . C4 C 1.0516(12) 1.0137(9) 0.2855(8) 0.045(3) Uani 1 1 d . . . H4A H 1.0691 1.0762 0.2705 0.054 Uiso 1 1 calc R . . H4B H 1.0863 0.9667 0.2513 0.054 Uiso 1 1 calc R . . C5 C 1.1187(11) 1.0306(8) 0.3817(8) 0.037(2) Uani 1 1 d . . . C6 C 1.1053(13) 1.1093(9) 0.4443(8) 0.043(3) Uani 1 1 d . . . H6 H 1.0502 1.1492 0.4274 0.052 Uiso 1 1 calc R . . C7 C 1.1745(12) 1.1271(8) 0.5312(8) 0.043(3) Uani 1 1 d . . . H7 H 1.1636 1.1772 0.5738 0.051 Uiso 1 1 calc R . . C8 C 1.2602(12) 1.0700(8) 0.5544(7) 0.040(3) Uani 1 1 d . . . H8 H 1.3120 1.0837 0.6121 0.048 Uiso 1 1 calc R . . C9 C 1.2675(11) 0.9916(8) 0.4896(7) 0.032(2) Uani 1 1 d . . . C10 C 1.3589(11) 0.9326(7) 0.5131(7) 0.031(2) Uani 1 1 d . . . H10 H 1.4119 0.9478 0.5708 0.038 Uiso 1 1 calc R . . C11 C 1.5206(12) 0.8189(9) 0.5693(7) 0.039(3) Uani 1 1 d . . . H11A H 1.5791 0.8842 0.5920 0.059 Uiso 1 1 calc R . . H11B H 1.5692 0.7695 0.5761 0.059 Uiso 1 1 calc R . . H11C H 1.4582 0.8140 0.6009 0.059 Uiso 1 1 calc R . . C12 C 1.4547(10) 0.7225(7) 0.4120(6) 0.027(2) Uani 1 1 d . . . C13 C 1.5363(11) 0.6595(9) 0.4292(6) 0.035(2) Uani 1 1 d . . . H13 H 1.5926 0.6694 0.4851 0.043 Uiso 1 1 calc R . . C14 C 1.5295(10) 0.5819(8) 0.3595(6) 0.030(2) Uani 1 1 d . . . C15 C 1.3796(10) 0.6333(7) 0.2669(6) 0.025(2) Uani 1 1 d . . . C16 C 1.2896(11) 0.6183(8) 0.1768(6) 0.033(2) Uani 1 1 d . . . H16A H 1.3138 0.5727 0.1348 0.049 Uiso 1 1 calc R . . H16B H 1.2958 0.6812 0.1632 0.049 Uiso 1 1 calc R . . H16C H 1.2017 0.5913 0.1746 0.049 Uiso 1 1 calc R . . C17 C 1.668(2) 0.5050(16) 0.4593(8) 0.101(8) Uani 1 1 d . . . H17A H 1.7604 0.5312 0.4738 0.151 Uiso 1 1 calc R . . H17B H 1.6504 0.4361 0.4589 0.151 Uiso 1 1 calc R . . H17C H 1.6363 0.5422 0.5020 0.151 Uiso 1 1 calc R . . C18 C 1.6683(10) 0.3784(8) 0.3095(7) 0.031(2) Uani 1 1 d . . . H18 H 1.7219 0.3838 0.3651 0.037 Uiso 1 1 calc R . . C19 C 1.6653(11) 0.2998(7) 0.2358(7) 0.033(2) Uani 1 1 d . . . C20 C 1.7450(15) 0.2370(10) 0.2472(9) 0.056(3) Uani 1 1 d . . . H20 H 1.8013 0.2443 0.3025 0.067 Uiso 1 1 calc R . . C21 C 1.7417(18) 0.1628(12) 0.1764(12) 0.076(5) Uani 1 1 d . . . H21 H 1.7974 0.1207 0.1829 0.091 Uiso 1 1 calc R . . C22 C 1.6549(17) 0.1517(12) 0.0960(10) 0.071(5) Uani 1 1 d . . . H22 H 1.6511 0.1017 0.0475 0.086 Uiso 1 1 calc R . . C23 C 1.5716(15) 0.2165(9) 0.0873(8) 0.049(3) Uani 1 1 d . . . C24 C 1.4646(16) 0.1978(14) -0.0011(10) 0.090(7) Uani 1 1 d D . . H24A H 1.4943 0.2388 -0.0358 0.107 Uiso 1 1 calc R . . H24B H 1.4418 0.1282 -0.0344 0.107 Uiso 1 1 calc R . . C25 C 1.2430(18) 0.1562(17) -0.0135(15) 0.103(6) Uani 1 1 d DU . . C26 C 1.129(4) 0.196(3) -0.011(3) 0.200(14) Uani 1 1 d DU . . H26 H 1.1565 0.2432 0.0437 0.240 Uiso 1 1 calc R . . C27 C 1.008(4) 0.200(5) -0.046(4) 0.35(3) Uani 1 1 d DU . . H27A H 0.9598 0.1587 -0.1013 0.421 Uiso 1 1 calc R . . H27B H 0.9715 0.2438 -0.0147 0.421 Uiso 1 1 calc R . . C28 C 1.0006(18) 0.5864(15) 0.3824(13) 0.110(7) Uani 1 1 d DU . . C29 C 1.3648(18) 1.0264(12) 0.1736(11) 0.069(4) Uani 1 1 d . . . C30 C 1.104(3) 0.3462(17) 0.2459(16) 0.179(14) Uani 1 1 d DU . . C31 C 1.8455(18) 0.491(2) 0.1011(15) 0.120(10) Uani 1 1 d . . . N1 N 1.1978(9) 0.9722(6) 0.4055(6) 0.0321(19) Uani 1 1 d . . . N2 N 1.3673(8) 0.8580(6) 0.4538(5) 0.0261(17) Uani 1 1 d . . . N3 N 1.4529(8) 0.8020(6) 0.4769(5) 0.0305(18) Uani 1 1 d . . . N4 N 1.3761(8) 0.7092(6) 0.3309(5) 0.0273(18) Uani 1 1 d . . . N5 N 1.4531(8) 0.5693(6) 0.2775(5) 0.0257(17) Uani 1 1 d . . . N6 N 1.6036(10) 0.5135(7) 0.3732(6) 0.040(2) Uani 1 1 d . . . N7 N 1.5982(8) 0.4405(6) 0.2994(5) 0.0267(17) Uani 1 1 d . . . N8 N 1.5764(9) 0.2885(6) 0.1563(6) 0.0323(19) Uani 1 1 d . . . O1 O 0.9456(9) 0.8268(7) 0.2672(8) 0.070(3) Uani 1 1 d . . . O2 O 0.9144(9) 0.9760(6) 0.2641(6) 0.050(2) Uani 1 1 d . . . O3 O 1.3517(14) 0.2253(10) 0.0222(9) 0.108(5) Uani 1 1 d DU . . O4 O 1.215(3) 0.0707(17) -0.0593(16) 0.190(9) Uani 1 1 d U . . O11 O 1.0830(9) 0.7777(7) 0.4326(7) 0.059(3) Uani 1 1 d . . . O12 O 1.2140(12) 0.6796(8) 0.5004(10) 0.091(4) Uani 1 1 d . . . O13 O 1.022(3) 0.6964(11) 0.5302(13) 0.168(10) Uani 1 1 d . . . O21 O 1.3608(16) 0.9403(8) 0.2915(7) 0.096(5) Uani 1 1 d . . . O22 O 1.3983(16) 0.8505(9) 0.1619(8) 0.096(4) Uani 1 1 d . . . O23 O 1.5571(13) 0.9927(13) 0.2676(10) 0.111(5) Uani 1 1 d . . . O31 O 1.3169(13) 0.3120(11) 0.2228(10) 0.101(4) Uani 1 1 d U . . O32 O 1.2339(17) 0.244(2) 0.329(2) 0.244(17) Uani 1 1 d . . . O33 O 1.350(2) 0.3837(17) 0.3605(12) 0.158(7) Uani 1 1 d U . . O41 O 1.6454(10) 0.5190(7) 0.1423(6) 0.053(2) Uani 1 1 d . . . O42 O 1.6116(13) 0.4107(11) 0.0017(7) 0.097(5) Uani 1 1 d . . . O43 O 1.7011(14) 0.5832(12) 0.0273(9) 0.105(5) Uani 1 1 d . . . F11 F 0.8824(11) 0.5941(12) 0.3420(10) 0.179(9) Uani 1 1 d D . . F12 F 0.9847(14) 0.5087(7) 0.4130(7) 0.142(6) Uani 1 1 d D . . F13 F 1.0648(17) 0.5786(10) 0.3223(8) 0.177(9) Uani 1 1 d D . . F21 F 1.2390(18) 1.0054(14) 0.1412(14) 0.173(8) Uani 1 1 d . . . F22 F 1.3975(18) 1.0230(9) 0.1004(7) 0.143(7) Uani 1 1 d . . . F23 F 1.4062(16) 1.1165(8) 0.2211(7) 0.118(5) Uani 1 1 d . . . F31 F 1.1326(16) 0.4219(15) 0.2150(16) 0.242(14) Uani 1 1 d D . . F32 F 1.0328(18) 0.2653(19) 0.1793(12) 0.50(4) Uani 1 1 d D . . F33 F 1.0477(16) 0.3638(12) 0.3044(14) 0.200(10) Uani 1 1 d D . . F41 F 1.8496(13) 0.4180(15) 0.1411(11) 0.166(8) Uani 1 1 d . . . F42 F 1.8901(13) 0.4659(18) 0.0333(11) 0.194(10) Uani 1 1 d . . . F43 F 1.9248(14) 0.5710(16) 0.1563(10) 0.169(7) Uani 1 1 d U . . S1 S 1.0943(3) 0.6963(2) 0.46835(19) 0.0363(6) Uani 1 1 d . . . S2 S 1.4150(4) 0.9357(3) 0.2247(2) 0.0620(10) Uani 1 1 d . . . S3 S 1.2512(5) 0.3089(4) 0.2825(2) 0.0715(12) Uani 1 1 d DU . . S4 S 1.6849(3) 0.5028(3) 0.0642(2) 0.0495(8) Uani 1 1 d . . . Pb1 Pb 1.18978(4) 0.80613(3) 0.31103(2) 0.03619(14) Uani 1 1 d . . . Pb2 Pb 1.44078(4) 0.41295(3) 0.15022(2) 0.03172(14) 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 C1 0.047(8) 0.054(8) 0.079(10) 0.029(7) 0.022(7) 0.014(7) C2 0.055(8) 0.058(8) 0.051(8) 0.018(6) 0.020(6) 0.019(7) C3 0.051(7) 0.038(6) 0.041(6) 0.015(5) 0.017(6) 0.019(6) C4 0.046(7) 0.046(7) 0.049(7) 0.021(6) 0.016(6) 0.010(6) C5 0.041(6) 0.035(6) 0.042(6) 0.016(5) 0.017(5) 0.011(5) C6 0.052(7) 0.037(6) 0.051(7) 0.021(5) 0.022(6) 0.019(6) C7 0.051(7) 0.035(6) 0.042(7) 0.000(5) 0.019(6) 0.015(5) C8 0.052(7) 0.037(6) 0.032(6) 0.005(5) 0.016(5) 0.012(5) C9 0.034(6) 0.032(5) 0.028(5) 0.007(4) 0.012(4) 0.003(4) C10 0.040(6) 0.031(5) 0.023(5) 0.005(4) 0.014(4) 0.006(5) C11 0.050(7) 0.043(6) 0.021(5) 0.003(4) 0.006(5) 0.017(5) C12 0.026(5) 0.030(5) 0.024(5) 0.006(4) 0.010(4) 0.002(4) C13 0.033(6) 0.054(7) 0.017(5) 0.007(4) 0.003(4) 0.013(5) C14 0.030(5) 0.036(5) 0.023(5) 0.007(4) 0.008(4) 0.011(4) C15 0.029(5) 0.027(5) 0.018(4) 0.005(4) 0.009(4) 0.006(4) C16 0.047(7) 0.031(5) 0.018(5) 0.004(4) 0.006(4) 0.014(5) C17 0.150(18) 0.145(17) 0.022(6) 0.009(8) 0.003(8) 0.124(15) C18 0.030(6) 0.041(6) 0.028(5) 0.016(4) 0.012(4) 0.012(5) C19 0.039(6) 0.028(5) 0.038(6) 0.014(4) 0.017(5) 0.011(5) C20 0.064(9) 0.055(8) 0.054(8) 0.012(6) 0.018(7) 0.036(7) C21 0.085(12) 0.061(9) 0.082(11) 0.007(8) 0.017(9) 0.050(9) C22 0.090(12) 0.063(9) 0.061(9) 0.001(7) 0.019(9) 0.047(9) C23 0.075(9) 0.044(7) 0.038(6) 0.008(5) 0.027(6) 0.028(7) C24 0.142(18) 0.110(14) 0.049(9) 0.027(9) 0.035(10) 0.099(14) C25 0.110(10) 0.097(10) 0.095(9) 0.032(8) 0.037(8) -0.007(8) C26 0.199(16) 0.203(16) 0.195(16) 0.049(10) 0.060(10) 0.054(10) C27 0.33(3) 0.37(3) 0.34(3) 0.06(2) 0.13(2) 0.06(2) C28 0.118(11) 0.105(10) 0.106(10) 0.041(8) 0.035(9) 0.008(8) C29 0.074(11) 0.059(9) 0.067(10) 0.025(8) 0.015(9) -0.004(8) C30 0.184(17) 0.191(16) 0.180(16) 0.076(11) 0.073(11) 0.037(10) C31 0.043(10) 0.24(3) 0.098(15) 0.114(19) 0.023(10) 0.010(14) N1 0.036(5) 0.030(4) 0.031(5) 0.007(4) 0.014(4) 0.006(4) N2 0.027(4) 0.026(4) 0.025(4) 0.005(3) 0.011(3) 0.005(3) N3 0.033(5) 0.035(5) 0.020(4) 0.001(3) 0.007(4) 0.010(4) N4 0.037(5) 0.028(4) 0.019(4) 0.009(3) 0.010(4) 0.010(4) N5 0.031(4) 0.031(4) 0.017(4) 0.007(3) 0.008(3) 0.009(4) N6 0.051(6) 0.048(5) 0.022(4) 0.005(4) 0.004(4) 0.031(5) N7 0.023(4) 0.033(4) 0.024(4) 0.006(3) 0.010(3) 0.008(4) N8 0.040(5) 0.027(4) 0.032(5) 0.006(3) 0.014(4) 0.010(4) O1 0.043(6) 0.056(6) 0.098(8) 0.013(6) 0.002(5) 0.018(5) O2 0.053(5) 0.042(5) 0.059(5) 0.017(4) 0.019(4) 0.011(4) O3 0.114(8) 0.084(7) 0.091(7) 0.014(6) -0.022(6) 0.028(6) O4 0.260(19) 0.132(13) 0.158(15) 0.009(11) 0.039(13) 0.074(13) O11 0.038(5) 0.055(5) 0.096(8) 0.049(5) 0.015(5) 0.013(4) O12 0.068(8) 0.060(7) 0.131(11) 0.042(7) -0.006(7) 0.014(6) O13 0.36(3) 0.089(10) 0.165(16) 0.079(11) 0.20(2) 0.109(15) O21 0.177(14) 0.061(7) 0.058(7) 0.022(5) 0.061(8) 0.003(8) O22 0.167(14) 0.060(7) 0.057(7) 0.003(5) 0.033(8) 0.037(8) O23 0.064(8) 0.169(15) 0.089(10) 0.028(10) 0.003(7) 0.037(9) O31 0.077(7) 0.108(8) 0.122(8) 0.020(6) 0.065(6) 0.001(6) O32 0.088(12) 0.32(3) 0.49(4) 0.37(3) 0.126(19) 0.093(16) O33 0.158(14) 0.187(15) 0.098(11) 0.010(10) 0.049(10) -0.013(12) O41 0.075(7) 0.061(5) 0.039(5) 0.029(4) 0.029(5) 0.021(5) O42 0.083(9) 0.132(11) 0.044(6) -0.007(7) 0.020(6) -0.019(8) O43 0.111(11) 0.165(14) 0.102(10) 0.106(10) 0.062(9) 0.061(10) F11 0.087(9) 0.219(17) 0.160(13) 0.128(13) -0.063(9) -0.080(10) F12 0.208(14) 0.048(5) 0.088(8) 0.029(5) -0.040(8) -0.059(7) F13 0.29(2) 0.100(10) 0.079(8) -0.009(7) 0.047(11) -0.063(12) F21 0.140(14) 0.179(16) 0.214(19) 0.128(15) 0.012(13) 0.041(12) F22 0.28(2) 0.081(7) 0.050(6) 0.025(5) 0.044(9) -0.009(9) F23 0.209(15) 0.063(6) 0.068(7) 0.009(5) 0.038(8) 0.017(8) F31 0.136(13) 0.33(3) 0.46(4) 0.35(3) 0.163(19) 0.146(16) F32 0.32(4) 0.80(9) 0.15(2) -0.03(3) 0.13(2) -0.33(5) F33 0.157(15) 0.190(16) 0.39(3) 0.169(19) 0.22(2) 0.090(13) F41 0.095(9) 0.33(2) 0.194(15) 0.202(17) 0.084(10) 0.137(13) F42 0.085(9) 0.45(3) 0.167(14) 0.195(18) 0.098(10) 0.139(14) F43 0.080(8) 0.262(15) 0.124(10) 0.112(11) -0.019(7) -0.060(9) S1 0.0345(15) 0.0312(13) 0.0418(15) 0.0111(11) 0.0074(12) 0.0098(11) S2 0.096(3) 0.074(2) 0.0458(19) 0.0308(17) 0.043(2) 0.046(2) S3 0.087(3) 0.110(3) 0.0428(19) 0.045(2) 0.0259(19) 0.049(3) S4 0.0383(17) 0.087(2) 0.0337(15) 0.0348(16) 0.0145(13) 0.0143(16) Pb1 0.0434(3) 0.0401(2) 0.0209(2) 0.00075(16) 0.00369(17) 0.0188(2) Pb2 0.0392(3) 0.0313(2) 0.0210(2) 0.00186(15) 0.00307(16) 0.01545(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.262(19) . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? C2 C3 1.460(19) . ? C2 H2 0.9300 . ? C3 O1 1.211(14) . ? C3 O2 1.325(14) . ? C4 O2 1.425(15) . ? C4 C5 1.506(17) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.347(14) . ? C5 C6 1.399(16) . ? C6 C7 1.376(17) . ? C6 H6 0.9300 . ? C7 C8 1.378(17) . ? C7 H7 0.9300 . ? C8 C9 1.390(15) . ? C8 H8 0.9300 . ? C9 N1 1.336(14) . ? C9 C10 1.447(15) . ? C10 N2 1.306(12) . ? C10 H10 0.9300 . ? C11 N3 1.455(13) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.340(13) . ? C12 N3 1.379(12) . ? C12 C13 1.392(15) . ? C13 C14 1.380(14) . ? C13 H13 0.9300 . ? C14 N5 1.346(12) . ? C14 N6 1.389(13) . ? C15 N5 1.327(13) . ? C15 N4 1.343(12) . ? C15 C16 1.499(14) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N6 1.451(15) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N7 1.277(13) . ? C18 C19 1.444(14) . ? C18 H18 0.9300 . ? C19 C20 1.363(16) . ? C19 N8 1.370(14) . ? C20 C21 1.37(2) . ? C20 H20 0.9300 . ? C21 C22 1.37(2) . ? C21 H21 0.9300 . ? C22 C23 1.409(19) . ? C22 H22 0.9300 . ? C23 N8 1.332(14) . ? C23 C24 1.55(2) . ? C24 O3 1.475(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.22(3) . ? C25 O3 1.302(15) . ? C25 C26 1.464(19) . ? C26 C27 1.32(2) . ? C26 H26 0.9300 . ? C27 H27A 0.9300 . ? C27 H27B 0.9300 . ? C28 F12 1.310(15) . ? C28 F11 1.330(16) . ? C28 F13 1.349(16) . ? C28 S1 1.79(2) . ? C29 F23 1.273(18) . ? C29 F21 1.30(2) . ? C29 F22 1.33(2) . ? C29 S2 1.774(17) . ? C30 F33 1.271(18) . ? C30 F31 1.307(18) . ? C30 F32 1.346(19) . ? C30 S3 1.79(3) . ? C31 F43 1.29(3) . ? C31 F42 1.33(3) . ? C31 F41 1.34(3) . ? C31 S4 1.76(2) . ? N1 Pb1 2.491(8) . ? N2 N3 1.366(12) . ? N2 Pb1 2.494(8) . ? N4 Pb1 2.647(8) . ? N5 Pb2 2.649(8) . ? N6 N7 1.392(11) . ? N7 Pb2 2.511(8) . ? N8 Pb2 2.502(8) . ? O1 Pb1 2.673(10) . ? O11 S1 1.414(9) . ? O11 Pb1 2.629(10) . ? O12 S1 1.365(12) . ? O13 S1 1.440(15) . ? O21 S2 1.371(12) . ? O21 Pb1 2.558(12) . ? O22 S2 1.354(11) . ? O23 S2 1.522(15) . ? O31 S3 1.362(12) . ? O31 Pb2 2.490(12) . ? O32 S3 1.329(14) . ? O33 S3 1.493(19) . ? O41 S4 1.442(8) . ? O41 Pb2 2.518(9) . ? O42 S4 1.422(13) . ? O43 S4 1.408(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 122.8(13) . . ? C1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? O1 C3 O2 121.1(12) . . ? O1 C3 C2 124.4(12) . . ? O2 C3 C2 114.5(10) . . ? O2 C4 C5 111.2(10) . . ? O2 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? O2 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C6 120.8(11) . . ? N1 C5 C4 118.6(10) . . ? C6 C5 C4 120.6(10) . . ? C7 C6 C5 119.3(11) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 119.4(10) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 118.6(11) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? N1 C9 C8 122.2(10) . . ? N1 C9 C10 118.8(9) . . ? C8 C9 C10 118.9(10) . . ? N2 C10 C9 120.3(9) . . ? N2 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 N3 117.1(9) . . ? N4 C12 C13 121.2(9) . . ? N3 C12 C13 121.7(9) . . ? C14 C13 C12 116.8(9) . . ? C14 C13 H13 121.6 . . ? C12 C13 H13 121.6 . . ? N5 C14 C13 122.4(9) . . ? N5 C14 N6 117.9(9) . . ? C13 C14 N6 119.7(9) . . ? N5 C15 N4 125.4(9) . . ? N5 C15 C16 117.6(8) . . ? N4 C15 C16 117.0(9) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 120.9(9) . . ? N7 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 N8 122.0(10) . . ? C20 C19 C18 120.0(11) . . ? N8 C19 C18 117.9(9) . . ? C19 C20 C21 119.5(13) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C22 119.1(13) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C22 C23 119.7(13) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? N8 C23 C22 120.6(12) . . ? N8 C23 C24 119.4(11) . . ? C22 C23 C24 119.7(11) . . ? O3 C24 C23 105.6(11) . . ? O3 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? O3 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.7 . . ? O4 C25 O3 133(2) . . ? O4 C25 C26 114(3) . . ? O3 C25 C26 112(3) . . ? C27 C26 C25 152(6) . . ? C27 C26 H26 104.0 . . ? C25 C26 H26 104.0 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? F12 C28 F11 107.1(15) . . ? F12 C28 F13 114.2(16) . . ? F11 C28 F13 106.5(15) . . ? F12 C28 S1 110.9(13) . . ? F11 C28 S1 112.8(14) . . ? F13 C28 S1 105.4(12) . . ? F23 C29 F21 109.3(19) . . ? F23 C29 F22 107.2(13) . . ? F21 C29 F22 99.8(17) . . ? F23 C29 S2 115.7(13) . . ? F21 C29 S2 111.1(12) . . ? F22 C29 S2 112.4(14) . . ? F33 C30 F31 114(2) . . ? F33 C30 F32 112(2) . . ? F31 C30 F32 109.6(19) . . ? F33 C30 S3 113.3(19) . . ? F31 C30 S3 106.8(17) . . ? F32 C30 S3 100.9(18) . . ? F43 C31 F42 108.6(17) . . ? F43 C31 F41 106.9(18) . . ? F42 C31 F41 107(3) . . ? F43 C31 S4 113(2) . . ? F42 C31 S4 110.1(14) . . ? F41 C31 S4 110.7(12) . . ? C9 N1 C5 119.5(9) . . ? C9 N1 Pb1 114.8(7) . . ? C5 N1 Pb1 124.2(7) . . ? C10 N2 N3 119.8(8) . . ? C10 N2 Pb1 115.5(7) . . ? N3 N2 Pb1 123.4(6) . . ? N2 N3 C12 117.3(8) . . ? N2 N3 C11 118.7(8) . . ? C12 N3 C11 123.3(9) . . ? C12 N4 C15 117.5(8) . . ? C12 N4 Pb1 118.6(6) . . ? C15 N4 Pb1 122.7(6) . . ? C15 N5 C14 116.6(8) . . ? C15 N5 Pb2 123.5(6) . . ? C14 N5 Pb2 119.6(6) . . ? C14 N6 N7 116.7(8) . . ? C14 N6 C17 123.7(9) . . ? N7 N6 C17 118.9(9) . . ? C18 N7 N6 118.2(8) . . ? C18 N7 Pb2 118.0(7) . . ? N6 N7 Pb2 123.4(6) . . ? C23 N8 C19 119.0(10) . . ? C23 N8 Pb2 124.3(8) . . ? C19 N8 Pb2 116.6(6) . . ? C3 O1 Pb1 149.6(9) . . ? C3 O2 C4 117.2(10) . . ? C25 O3 C24 114.6(14) . . ? S1 O11 Pb1 121.3(6) . . ? S2 O21 Pb1 128.7(7) . . ? S3 O31 Pb2 148.8(9) . . ? S4 O41 Pb2 122.3(6) . . ? O12 S1 O11 120.1(7) . . ? O12 S1 O13 111.5(12) . . ? O11 S1 O13 109.5(8) . . ? O12 S1 C28 106.2(8) . . ? O11 S1 C28 106.2(7) . . ? O13 S1 C28 101.5(11) . . ? O22 S2 O21 123.7(8) . . ? O22 S2 O23 113.2(10) . . ? O21 S2 O23 105.8(9) . . ? O22 S2 C29 108.8(8) . . ? O21 S2 C29 105.2(9) . . ? O23 S2 C29 96.4(9) . . ? O32 S3 O31 131.4(14) . . ? O32 S3 O33 91.6(17) . . ? O31 S3 O33 99.0(10) . . ? O32 S3 C30 109.7(10) . . ? O31 S3 C30 108.7(10) . . ? O33 S3 C30 113.8(12) . . ? O43 S4 O42 113.4(9) . . ? O43 S4 O41 117.3(8) . . ? O42 S4 O41 112.0(6) . . ? O43 S4 C31 102.3(9) . . ? O42 S4 C31 106.4(13) . . ? O41 S4 C31 103.8(8) . . ? N1 Pb1 N2 67.0(3) . . ? N1 Pb1 O21 70.7(3) . . ? N2 Pb1 O21 76.4(4) . . ? N1 Pb1 O11 71.5(3) . . ? N2 Pb1 O11 72.3(3) . . ? O21 Pb1 O11 137.9(3) . . ? N1 Pb1 N4 126.2(3) . . ? N2 Pb1 N4 61.0(2) . . ? O21 Pb1 N4 84.4(4) . . ? O11 Pb1 N4 103.7(2) . . ? N1 Pb1 O1 74.3(3) . . ? N2 Pb1 O1 132.4(3) . . ? O21 Pb1 O1 115.8(4) . . ? O11 Pb1 O1 70.0(3) . . ? N4 Pb1 O1 156.6(3) . . ? O31 Pb2 N8 84.0(4) . . ? O31 Pb2 N7 75.7(4) . . ? N8 Pb2 N7 66.4(3) . . ? O31 Pb2 O41 152.9(4) . . ? N8 Pb2 O41 81.9(3) . . ? N7 Pb2 O41 77.5(3) . . ? O31 Pb2 N5 85.9(4) . . ? N8 Pb2 N5 128.0(3) . . ? N7 Pb2 N5 61.7(2) . . ? O41 Pb2 N5 84.7(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.824 _refine_diff_density_min -2.023 _refine_diff_density_rms 0.228 #===END data_Complex_2(sdjh780) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H37 Cu2 N11 O4' _chemical_formula_sum 'C33 H37 Cu2 N11 O4' _chemical_formula_weight 778.84 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 13.2961(9) _cell_length_b 13.8546(9) _cell_length_c 16.5011(12) _cell_angle_alpha 86.432(3) _cell_angle_beta 82.154(3) _cell_angle_gamma 73.922(3) _cell_volume 2892.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9861 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.38 _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.73 _exptl_crystal_size_max 0.74 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26515 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 24.43 _reflns_number_total 9192 _reflns_number_gt 6749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^ > 2\s(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^)+(0.1464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9192 _refine_ls_number_parameters 457 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0896 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2318 _refine_ls_wR_factor_gt 0.2199 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.090 _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 C1 C 0.2496(8) 0.0696(7) 0.4612(6) 0.108(3) Uani 1 1 d . . . H1A H 0.2117 0.0436 0.4289 0.130 Uiso 1 1 calc R . . H1B H 0.2145 0.1195 0.4982 0.130 Uiso 1 1 calc R . . C2 C 0.3507(7) 0.0365(6) 0.4546(5) 0.084(2) Uani 1 1 d . . . H2 H 0.3871 0.0636 0.4874 0.101 Uiso 1 1 calc R . . C3 C 0.4122(6) -0.0430(5) 0.3968(4) 0.0648(17) Uani 1 1 d . . . C4 C 0.4089(4) -0.1368(4) 0.2826(4) 0.0590(16) Uani 1 1 d . . . H4A H 0.3589 -0.1649 0.2613 0.071 Uiso 1 1 calc R . . H4B H 0.4577 -0.1907 0.3093 0.071 Uiso 1 1 calc R . . C5 C 0.4675(4) -0.0928(4) 0.2146(4) 0.0454(12) Uani 1 1 d . . . C6 C 0.4407(4) 0.0096(4) 0.1960(4) 0.0521(13) Uani 1 1 d . . . H6 H 0.3861 0.0531 0.2282 0.062 Uiso 1 1 calc R . . C7 C 0.4936(5) 0.0461(4) 0.1316(4) 0.0545(14) Uani 1 1 d . . . H7 H 0.4760 0.1147 0.1195 0.065 Uiso 1 1 calc R . . C8 C 0.5749(4) -0.0192(4) 0.0828(4) 0.0498(13) Uani 1 1 d . . . H8 H 0.6124 0.0049 0.0381 0.060 Uiso 1 1 calc R . . C9 C 0.5978(4) -0.1190(4) 0.1025(3) 0.0414(11) Uani 1 1 d . . . C10 C 0.6805(4) -0.1950(3) 0.0553(3) 0.0382(10) Uani 1 1 d . . . H10 H 0.7224 -0.1778 0.0100 0.046 Uiso 1 1 calc R . . C11 C 0.8288(4) -0.3535(4) -0.0282(3) 0.0489(12) Uani 1 1 d . . . H11A H 0.7893 -0.3169 -0.0703 0.073 Uiso 1 1 calc R . . H11B H 0.8698 -0.4181 -0.0480 0.073 Uiso 1 1 calc R . . H11C H 0.8750 -0.3168 -0.0137 0.073 Uiso 1 1 calc R . . C12 C 0.7540(4) -0.4565(3) 0.0809(3) 0.0347(10) Uani 1 1 d . . . C13 C 0.8112(3) -0.5487(3) 0.0498(3) 0.0341(10) Uani 1 1 d . . . H13 H 0.8575 -0.5532 0.0017 0.041 Uiso 1 1 calc R . . C14 C 0.7973(3) -0.6337(3) 0.0925(3) 0.0343(10) Uani 1 1 d . . . C15 C 0.6811(3) -0.5355(3) 0.1926(3) 0.0359(10) Uani 1 1 d . . . C16 C 0.6160(5) -0.5284(4) 0.2732(4) 0.0576(15) Uani 1 1 d . . . H16A H 0.6590 -0.5628 0.3140 0.086 Uiso 1 1 calc R . . H16B H 0.5597 -0.5587 0.2710 0.086 Uiso 1 1 calc R . . H16C H 0.5871 -0.4590 0.2869 0.086 Uiso 1 1 calc R . . C17 C 0.9111(4) -0.7536(4) -0.0129(3) 0.0460(12) Uani 1 1 d . . . H17A H 0.9251 -0.6938 -0.0386 0.069 Uiso 1 1 calc R . . H17B H 0.8726 -0.7805 -0.0467 0.069 Uiso 1 1 calc R . . H17C H 0.9766 -0.8025 -0.0057 0.069 Uiso 1 1 calc R . . C18 C 0.8517(4) -0.8962(3) 0.1000(3) 0.0371(10) Uani 1 1 d . . . H18 H 0.8953 -0.9217 0.0528 0.044 Uiso 1 1 calc R . . C19 C 0.8115(4) -0.9591(4) 0.1622(3) 0.0389(10) Uani 1 1 d . . . C20 C 0.8339(4) 0.9369(3) 0.1595(4) 0.0446(12) Uani 1 1 d . . . H20 H 0.8800 0.9022 0.1168 0.054 Uiso 1 1 calc R . . C21 C 0.7867(4) 0.8857(4) 0.2213(4) 0.0529(14) Uani 1 1 d . . . H21 H 0.8008 0.8161 0.2206 0.064 Uiso 1 1 calc R . . C22 C 0.7210(6) 0.9373(4) 0.2817(4) 0.0631(16) Uani 1 1 d . . . H22 H 0.6872 0.9037 0.3225 0.076 Uiso 1 1 calc R . . C23 C 0.7026(4) -0.9596(4) 0.2845(4) 0.0499(13) Uani 1 1 d . . . C24 C 0.6385(6) -0.8986(6) 0.3548(5) 0.084(2) Uani 1 1 d . . . H24A H 0.6450 -0.9398 0.4045 0.101 Uiso 1 1 calc R . . H24B H 0.6667 -0.8424 0.3611 0.101 Uiso 1 1 calc R . . C25 C 0.5118(9) -0.7673(7) 0.3137(6) 0.104(3) Uani 1 1 d U . . C26 C 0.3968(9) -0.7230(11) 0.3228(8) 0.179(7) Uani 1 1 d . . . H26 H 0.3563 -0.7615 0.3523 0.215 Uiso 1 1 calc RD . . C27 C 0.3486(18) -0.6426(14) 0.2963(11) 0.229(9) Uani 1 1 d DU . . H27A H 0.3849 -0.6009 0.2663 0.275 Uiso 1 1 calc R . . H27B H 0.2754 -0.6225 0.3061 0.275 Uiso 1 1 calc R . . C28 C 0.3811(5) -0.3494(4) 0.1932(4) 0.0532(14) Uani 1 1 d . . . C29 C 0.2756(6) -0.3622(8) 0.1916(5) 0.092(3) Uani 1 1 d . . . H29A H 0.2605 -0.4061 0.2361 0.138 Uiso 1 1 calc R . . H29B H 0.2730 -0.3909 0.1407 0.138 Uiso 1 1 calc R . . H29C H 0.2242 -0.2981 0.1969 0.138 Uiso 1 1 calc R . . C30 C 0.6661(7) -0.3073(6) 0.3570(5) 0.077(2) Uani 1 1 d . . . C31 C 0.6957(13) -0.3201(12) 0.4398(10) 0.186(6) Uani 1 1 d U . . H31A H 0.6826 -0.3808 0.4644 0.278 Uiso 1 1 calc R . . H31B H 0.6548 -0.2638 0.4718 0.278 Uiso 1 1 calc R . . H31C H 0.7693 -0.3243 0.4376 0.278 Uiso 1 1 calc R . . C32 C 0.8733(7) -0.7688(5) 0.3539(7) 0.094(3) Uani 1 1 d . . . C33 C 0.9517(12) -0.7816(12) 0.4210(9) 0.203(8) Uani 1 1 d . . . H33A H 0.9207 -0.7338 0.4632 0.305 Uiso 1 1 calc R . . H33B H 1.0171 -0.7704 0.3959 0.305 Uiso 1 1 calc R . . H33C H 0.9645 -0.8484 0.4445 0.305 Uiso 1 1 calc R . . N1 N 0.5460(3) -0.1560(3) 0.1678(3) 0.0416(10) Uani 1 1 d . . . N2 N 0.6914(3) -0.2850(3) 0.0796(3) 0.0385(9) Uani 1 1 d . . . N3 N 0.7573(3) -0.3666(3) 0.0425(2) 0.0382(9) Uani 1 1 d . . . N4 N 0.6873(3) -0.4497(3) 0.1514(3) 0.0381(9) Uani 1 1 d . . . N5 N 0.7345(3) -0.6282(3) 0.1648(2) 0.0351(8) Uani 1 1 d . . . N6 N 0.8486(3) -0.7293(3) 0.0671(2) 0.0380(9) Uani 1 1 d . . . N7 N 0.8220(3) -0.8020(3) 0.1156(2) 0.0366(9) Uani 1 1 d . . . N8 N 0.7463(3) -0.9097(3) 0.2247(2) 0.0383(9) Uani 1 1 d . . . N9 N 0.4591(3) -0.3376(3) 0.1951(3) 0.0451(10) Uani 1 1 d . . . N10 N 0.6472(4) -0.3052(3) 0.2946(3) 0.0493(11) Uani 1 1 d . . . N11 N 0.8143(4) -0.7551(4) 0.3116(3) 0.0615(14) Uani 1 1 d . . . O1 O 0.5048(4) -0.0831(3) 0.3966(3) 0.0701(12) Uani 1 1 d . . . O2 O 0.3533(3) -0.0611(3) 0.3413(3) 0.0697(13) Uani 1 1 d . . . O3 O 0.5357(6) -0.8634(5) 0.3452(4) 0.114(2) Uani 1 1 d . . . O4 O 0.5871(5) -0.7402(6) 0.2913(4) 0.119(3) Uani 1 1 d . . . Cu1 Cu 0.60146(5) -0.30847(4) 0.17887(4) 0.0402(2) Uani 1 1 d . . . Cu2 Cu 0.72342(5) -0.76185(4) 0.21465(4) 0.0390(2) 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 C1 0.097(7) 0.106(7) 0.114(8) -0.044(6) 0.022(6) -0.022(5) C2 0.091(5) 0.072(4) 0.094(6) -0.040(4) 0.010(4) -0.031(4) C3 0.084(5) 0.055(3) 0.060(4) -0.013(3) 0.004(3) -0.029(3) C4 0.041(3) 0.048(3) 0.083(4) -0.030(3) 0.004(3) -0.004(2) C5 0.037(3) 0.039(3) 0.064(3) -0.010(2) -0.015(2) -0.010(2) C6 0.051(3) 0.042(3) 0.064(4) -0.011(3) -0.016(3) -0.006(2) C7 0.059(3) 0.031(2) 0.074(4) -0.003(2) -0.028(3) -0.004(2) C8 0.050(3) 0.037(3) 0.067(4) 0.000(2) -0.022(3) -0.013(2) C9 0.048(3) 0.037(2) 0.042(3) 0.000(2) -0.014(2) -0.011(2) C10 0.046(3) 0.033(2) 0.036(2) 0.0049(19) -0.003(2) -0.0131(19) C11 0.056(3) 0.041(3) 0.051(3) 0.006(2) -0.001(3) -0.020(2) C12 0.036(2) 0.035(2) 0.042(3) -0.0028(18) -0.008(2) -0.0215(18) C13 0.024(2) 0.039(2) 0.041(3) -0.0043(19) -0.0002(18) -0.0119(17) C14 0.022(2) 0.033(2) 0.048(3) -0.0098(19) -0.0073(19) -0.0041(16) C15 0.031(2) 0.028(2) 0.052(3) -0.0065(19) -0.005(2) -0.0123(17) C16 0.069(4) 0.048(3) 0.049(3) -0.004(2) 0.011(3) -0.014(3) C17 0.051(3) 0.044(3) 0.040(3) -0.005(2) 0.004(2) -0.010(2) C18 0.032(2) 0.035(2) 0.046(3) -0.0074(19) -0.008(2) -0.0087(18) C19 0.041(3) 0.042(2) 0.038(3) -0.002(2) -0.019(2) -0.011(2) C20 0.031(2) 0.034(2) 0.068(4) -0.012(2) -0.016(2) -0.0015(18) C21 0.056(3) 0.028(2) 0.079(4) 0.008(2) -0.013(3) -0.018(2) C22 0.086(4) 0.049(3) 0.064(4) 0.008(3) -0.012(3) -0.034(3) C23 0.057(3) 0.043(3) 0.051(3) -0.003(2) -0.003(3) -0.018(2) C24 0.074(5) 0.087(5) 0.095(6) -0.030(4) 0.034(4) -0.043(4) C25 0.124(6) 0.074(5) 0.113(6) -0.013(4) 0.004(5) -0.035(4) C26 0.111(9) 0.184(13) 0.163(12) 0.064(10) 0.066(8) 0.038(8) C27 0.229(9) 0.229(9) 0.228(9) -0.006(2) -0.028(2) -0.061(3) C28 0.050(3) 0.063(3) 0.053(3) -0.017(3) -0.005(3) -0.024(3) C29 0.059(4) 0.145(8) 0.087(6) -0.030(5) -0.004(4) -0.050(5) C30 0.109(6) 0.079(5) 0.068(5) 0.005(3) -0.042(4) -0.054(4) C31 0.188(7) 0.186(7) 0.184(7) -0.004(2) -0.026(2) -0.053(3) C32 0.078(5) 0.052(4) 0.146(9) -0.033(5) 0.010(5) -0.010(3) C33 0.191(14) 0.208(15) 0.195(15) -0.068(12) -0.135(12) 0.038(11) N1 0.043(2) 0.0322(19) 0.054(3) -0.0146(18) -0.0078(19) -0.0132(17) N2 0.049(2) 0.0228(18) 0.047(2) -0.0074(15) -0.0149(19) -0.0082(15) N3 0.040(2) 0.037(2) 0.038(2) 0.0009(16) -0.0047(17) -0.0113(16) N4 0.036(2) 0.0330(19) 0.043(2) -0.0034(16) -0.0029(18) -0.0070(15) N5 0.036(2) 0.0293(18) 0.043(2) 0.0037(15) -0.0046(17) -0.0161(15) N6 0.034(2) 0.036(2) 0.043(2) 0.0001(16) -0.0015(17) -0.0081(16) N7 0.035(2) 0.036(2) 0.042(2) 0.0004(16) -0.0158(17) -0.0110(16) N8 0.047(2) 0.0290(18) 0.040(2) -0.0017(16) -0.0077(18) -0.0100(16) N9 0.035(2) 0.041(2) 0.063(3) -0.0124(19) -0.005(2) -0.0143(17) N10 0.054(3) 0.043(2) 0.055(3) -0.0045(19) -0.010(2) -0.0168(19) N11 0.068(3) 0.055(3) 0.075(4) -0.001(2) -0.047(3) -0.020(2) O1 0.062(3) 0.066(3) 0.085(3) -0.025(2) -0.003(2) -0.019(2) O2 0.061(3) 0.059(2) 0.085(3) -0.032(2) 0.014(2) -0.0142(19) O3 0.126(6) 0.099(4) 0.124(5) -0.010(4) 0.023(4) -0.058(4) O4 0.100(4) 0.184(6) 0.107(5) -0.085(5) 0.060(4) -0.109(5) Cu1 0.0429(4) 0.0289(3) 0.0481(4) -0.0049(2) -0.0025(3) -0.0092(2) Cu2 0.0444(4) 0.0283(3) 0.0432(4) -0.0018(2) -0.0012(3) -0.0101(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.286(12) . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? C2 C3 1.487(9) . ? C2 H2 0.9300 . ? C3 O1 1.203(8) . ? C3 O2 1.359(8) . ? C4 O2 1.444(6) . ? C4 C5 1.476(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.346(6) . ? C5 C6 1.389(7) . ? C6 C7 1.343(9) . ? C6 H6 0.9300 . ? C7 C8 1.395(8) . ? C7 H7 0.9300 . ? C8 C9 1.359(7) . ? C8 H8 0.9300 . ? C9 N1 1.350(7) . ? C9 C10 1.467(7) . ? C10 N2 1.262(6) . ? C10 H10 0.9300 . ? C11 N3 1.437(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.353(6) . ? C12 N3 1.371(6) . ? C12 C13 1.382(6) . ? C13 C14 1.377(7) . ? C13 H13 0.9300 . ? C14 N5 1.353(6) . ? C14 N6 1.373(6) . ? C15 N4 1.350(6) . ? C15 N5 1.357(6) . ? C15 C16 1.477(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N6 1.465(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N7 1.286(6) . ? C18 C19 1.448(7) . ? C18 H18 0.9300 . ? C19 N8 1.341(6) . ? C19 C20 1.390(7) 1_535 ? C20 C21 1.385(8) . ? C20 C19 1.390(7) 1_575 ? C20 H20 0.9300 . ? C21 C22 1.332(9) . ? C21 H21 0.9300 . ? C22 C23 1.383(8) 1_575 ? C22 H22 0.9300 . ? C23 N8 1.331(7) . ? C23 C22 1.383(8) 1_535 ? C23 C24 1.497(9) . ? C24 O3 1.345(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.171(10) . ? C25 O3 1.367(11) . ? C25 C26 1.472(15) . ? C26 C27 1.209(17) . ? C26 H26 0.9300 . ? C27 H27A 0.9300 . ? C27 H27B 0.9300 . ? C28 N9 1.098(7) . ? C28 C29 1.466(9) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N10 1.090(8) . ? C30 C31 1.459(16) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N11 1.091(11) . ? C32 C33 1.592(15) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? N1 Cu1 2.041(4) . ? N2 N3 1.346(5) . ? N2 Cu1 1.957(4) . ? N4 Cu1 2.017(4) . ? N5 Cu2 2.015(4) . ? N6 N7 1.341(5) . ? N7 Cu2 1.955(4) . ? N8 Cu2 1.986(4) . ? N9 Cu1 2.022(4) . ? N10 Cu1 2.089(5) . ? N11 Cu2 2.153(5) . ? O4 Cu2 2.024(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 123.0(8) . . ? C1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? O1 C3 O2 123.8(6) . . ? O1 C3 C2 123.7(7) . . ? O2 C3 C2 112.4(7) . . ? O2 C4 C5 110.4(5) . . ? O2 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? O2 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N1 C5 C6 120.1(5) . . ? N1 C5 C4 117.7(4) . . ? C6 C5 C4 122.1(5) . . ? C7 C6 C5 120.2(5) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 119.9(5) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 118.1(6) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? N1 C9 C8 122.3(5) . . ? N1 C9 C10 114.5(4) . . ? C8 C9 C10 123.1(5) . . ? N2 C10 C9 116.2(4) . . ? N2 C10 H10 121.9 . . ? C9 C10 H10 121.9 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 N3 115.3(4) . . ? N4 C12 C13 121.3(4) . . ? N3 C12 C13 123.4(4) . . ? C14 C13 C12 117.7(4) . . ? C14 C13 H13 121.1 . . ? C12 C13 H13 121.1 . . ? N5 C14 N6 115.2(4) . . ? N5 C14 C13 121.7(4) . . ? N6 C14 C13 123.1(4) . . ? N4 C15 N5 123.1(4) . . ? N4 C15 C16 118.5(4) . . ? N5 C15 C16 118.3(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 114.3(4) . . ? N7 C18 H18 122.9 . . ? C19 C18 H18 122.9 . . ? N8 C19 C20 120.1(5) . 1_535 ? N8 C19 C18 115.1(4) . . ? C20 C19 C18 124.8(5) 1_535 . ? C21 C20 C19 119.2(5) . 1_575 ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 1_575 . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.6(6) . 1_575 ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 1_575 . ? N8 C23 C22 120.5(5) . 1_535 ? N8 C23 C24 116.1(5) . . ? C22 C23 C24 123.2(6) 1_535 . ? O3 C24 C23 113.1(7) . . ? O3 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? O3 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O4 C25 O3 112.4(10) . . ? O4 C25 C26 136.9(11) . . ? O3 C25 C26 110.4(9) . . ? C27 C26 C25 127.7(15) . . ? C27 C26 H26 116.2 . . ? C25 C26 H26 116.2 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? N9 C28 C29 178.3(7) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N10 C30 C31 174.6(10) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N11 C32 C33 174.7(9) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C5 N1 C9 119.4(4) . . ? C5 N1 Cu1 129.0(4) . . ? C9 N1 Cu1 111.6(3) . . ? C10 N2 N3 126.0(4) . . ? C10 N2 Cu1 117.0(3) . . ? N3 N2 Cu1 117.0(3) . . ? N2 N3 C12 114.8(4) . . ? N2 N3 C11 119.3(4) . . ? C12 N3 C11 125.7(4) . . ? C15 N4 C12 118.2(4) . . ? C15 N4 Cu1 127.4(3) . . ? C12 N4 Cu1 114.3(3) . . ? C14 N5 C15 117.8(4) . . ? C14 N5 Cu2 114.6(3) . . ? C15 N5 Cu2 127.4(3) . . ? N7 N6 C14 114.1(4) . . ? N7 N6 C17 120.2(4) . . ? C14 N6 C17 124.7(4) . . ? C18 N7 N6 125.1(4) . . ? C18 N7 Cu2 116.9(3) . . ? N6 N7 Cu2 117.9(3) . . ? C23 N8 C19 120.4(4) . . ? C23 N8 Cu2 126.5(3) . . ? C19 N8 Cu2 113.1(3) . . ? C28 N9 Cu1 170.4(5) . . ? C30 N10 Cu1 175.0(5) . . ? C32 N11 Cu2 165.6(6) . . ? C3 O2 C4 115.1(5) . . ? C24 O3 C25 112.2(7) . . ? C25 O4 Cu2 147.0(6) . . ? N2 Cu1 N4 78.48(15) . . ? N2 Cu1 N9 131.56(18) . . ? N4 Cu1 N9 96.45(16) . . ? N2 Cu1 N1 80.58(16) . . ? N4 Cu1 N1 159.03(17) . . ? N9 Cu1 N1 96.55(16) . . ? N2 Cu1 N10 121.00(17) . . ? N4 Cu1 N10 97.49(17) . . ? N9 Cu1 N10 107.44(18) . . ? N1 Cu1 N10 94.22(17) . . ? N7 Cu2 N8 80.50(16) . . ? N7 Cu2 N5 78.01(16) . . ? N8 Cu2 N5 158.44(17) . . ? N7 Cu2 O4 157.91(19) . . ? N8 Cu2 O4 90.7(2) . . ? N5 Cu2 O4 108.7(3) . . ? N7 Cu2 N11 107.7(2) . . ? N8 Cu2 N11 94.65(18) . . ? N5 Cu2 N11 93.51(18) . . ? O4 Cu2 N11 93.1(3) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 24.43 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.008 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.109 #===END data_Complex_3(djh740) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H31 Cl4 N9 O20 Pb2' _chemical_formula_sum 'C29 H31 Cl4 N9 O20 Pb2' _chemical_formula_weight 1381.83 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' 'Pb' 'Pb' -3.3944 10.1111 '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 13.3813(5) _cell_length_b 13.6338(5) _cell_length_c 14.6157(6) _cell_angle_alpha 117.6600(10) _cell_angle_beta 92.1710(10) _cell_angle_gamma 115.2450(10) _cell_volume 2041.48(14) _cell_formula_units_Z 2 _cell_measurement_temperature 91(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 28.89 _exptl_crystal_description 'rod' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.57 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 8.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3955 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 91(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26459 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.49 _reflns_number_total 6916 _reflns_number_gt 6259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^ > 2\s(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^)+(0.0101P)^2^+5.2836P] 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 6916 _refine_ls_number_parameters 581 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0432 _refine_ls_wR_factor_gt 0.0416 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6383(4) 0.9677(5) 0.7835(4) 0.0371(12) Uani 1 1 d . . . H1A H 0.6885 1.0006 0.7499 0.045 Uiso 1 1 calc R . . H1B H 0.6023 0.8808 0.7581 0.045 Uiso 1 1 calc R . . C2 C 0.6185(4) 1.0431(4) 0.8658(3) 0.0246(10) Uani 1 1 d . . . H2 H 0.5683 1.0099 0.8991 0.030 Uiso 1 1 calc R . . C3 C 0.6752(4) 1.1814(4) 0.9068(3) 0.0216(10) Uani 1 1 d . . . C4 C 0.6802(4) 1.3726(4) 1.0260(4) 0.0233(10) Uani 1 1 d . . . H4A H 0.6410 1.4043 1.0769 0.028 Uiso 1 1 calc R . . H4B H 0.6571 1.3736 0.9628 0.028 Uiso 1 1 calc R . . C5 C 0.8087(4) 1.4606(4) 1.0768(3) 0.0164(9) Uani 1 1 d . . . C6 C 0.8695(4) 1.5535(4) 1.0535(3) 0.0190(9) Uani 1 1 d . . . H6 H 0.8313 1.5606 1.0044 0.023 Uiso 1 1 calc R . . C7 C 0.9867(4) 1.6352(4) 1.1033(3) 0.0182(9) Uani 1 1 d . . . H7 H 1.0282 1.6985 1.0889 0.022 Uiso 1 1 calc R . . C8 C 1.0411(4) 1.6213(4) 1.1746(3) 0.0163(9) Uani 1 1 d . . . H8 H 1.1203 1.6743 1.2085 0.020 Uiso 1 1 calc R . . C9 C 0.9763(3) 1.5274(4) 1.1952(3) 0.0130(8) Uani 1 1 d . . . C10 C 1.0333(4) 1.5124(4) 1.2712(3) 0.0141(9) Uani 1 1 d . . . H10 H 1.1126 1.5654 1.3043 0.017 Uiso 1 1 calc R . . C11 C 1.1577(3) 1.4839(4) 1.4000(3) 0.0177(9) Uani 1 1 d . . . H11A H 1.1855 1.5737 1.4472 0.027 Uiso 1 1 calc R . . H11B H 1.1863 1.4699 1.3384 0.027 Uiso 1 1 calc R . . H11C H 1.1843 1.4540 1.4380 0.027 Uiso 1 1 calc R . . C12 C 0.9630(3) 1.3279(3) 1.3901(3) 0.0103(8) Uani 1 1 d . . . C13 C 1.0093(3) 1.3124(4) 1.4659(3) 0.0125(8) Uani 1 1 d . . . H13 H 1.0881 1.3601 1.5015 0.015 Uiso 1 1 calc R . . C14 C 0.9321(3) 1.2219(4) 1.4859(3) 0.0114(8) Uani 1 1 d . . . C15 C 0.7799(3) 1.1791(4) 1.3669(3) 0.0121(8) Uani 1 1 d . . . C16 C 0.6534(3) 1.1104(4) 1.3148(3) 0.0145(9) Uani 1 1 d . . . H16A H 0.6348 1.1626 1.2989 0.022 Uiso 1 1 calc R . . H16B H 0.6124 1.0932 1.3628 0.022 Uiso 1 1 calc R . . H16C H 0.6313 1.0312 1.2489 0.022 Uiso 1 1 calc R . . C17 C 1.0919(3) 1.2691(4) 1.6203(3) 0.0171(9) Uani 1 1 d . . . H17A H 1.0971 1.2870 1.6926 0.026 Uiso 1 1 calc R . . H17B H 1.1312 1.3481 1.6225 0.026 Uiso 1 1 calc R . . H17C H 1.1273 1.2186 1.5867 0.026 Uiso 1 1 calc R . . C18 C 0.9263(3) 1.0623(4) 1.6206(3) 0.0146(9) Uani 1 1 d . . . H18 H 1.0022 1.1129 1.6650 0.018 Uiso 1 1 calc R . . C19 C 0.8471(3) 0.9485(4) 1.6204(3) 0.0133(9) Uani 1 1 d . . . C20 C 0.8858(4) 0.9192(4) 1.6882(3) 0.0183(9) Uani 1 1 d . . . H20 H 0.9601 0.9737 1.7361 0.022 Uiso 1 1 calc R . . C21 C 0.8123(4) 0.8078(4) 1.6839(3) 0.0197(9) Uani 1 1 d . . . H21 H 0.8365 0.7862 1.7287 0.024 Uiso 1 1 calc R . . C22 C 0.7029(4) 0.7293(4) 1.6123(3) 0.0185(9) Uani 1 1 d . . . H22 H 0.6526 0.6533 1.6073 0.022 Uiso 1 1 calc R . . C23 C 0.6680(3) 0.7648(4) 1.5472(3) 0.0137(9) Uani 1 1 d . . . C24 C 0.5461(3) 0.6843(4) 1.4741(3) 0.0174(9) Uani 1 1 d . . . H24A H 0.5122 0.5990 1.4620 0.021 Uiso 1 1 calc R . . H24B H 0.5002 0.7217 1.5082 0.021 Uiso 1 1 calc R . . C25 C 0.4561(4) 0.5621(4) 1.2865(3) 0.0208(10) Uani 1 1 d . . . C26 C 0.4669(4) 0.5544(4) 1.1837(4) 0.0274(11) Uani 1 1 d . . . H26 H 0.5339 0.6151 1.1829 0.033 Uiso 1 1 calc R . . C27 C 0.3838(4) 0.4637(4) 1.0938(4) 0.0334(12) Uani 1 1 d . . . H27A H 0.3165 0.4028 1.0939 0.040 Uiso 1 1 calc R . . H27B H 0.3918 0.4600 1.0295 0.040 Uiso 1 1 calc R . . C28 C 0.6802(5) 0.9160(5) 0.0041(4) 0.0336(12) Uani 1 1 d . . . C29 C 0.7327(5) 0.8466(5) -0.0613(4) 0.0420(13) Uani 1 1 d . . . H29A H 0.7786 0.8913 -0.0927 0.063 Uiso 1 1 calc R . . H29B H 0.6734 0.7624 -0.1177 0.063 Uiso 1 1 calc R . . H29C H 0.7811 0.8398 -0.0170 0.063 Uiso 1 1 calc R . . N1 N 0.8606(3) 1.4481(3) 1.1474(3) 0.0136(7) Uani 1 1 d . . . N2 N 0.9752(3) 1.4268(3) 1.2928(2) 0.0123(7) Uani 1 1 d . . . N3 N 1.0319(3) 1.4144(3) 1.3641(2) 0.0123(7) Uani 1 1 d . . . N4 N 0.8483(3) 1.2618(3) 1.3409(2) 0.0110(7) Uani 1 1 d . . . N5 N 0.8169(3) 1.1560(3) 1.4369(2) 0.0119(7) Uani 1 1 d . . . N6 N 0.9705(3) 1.1986(3) 1.5581(2) 0.0110(7) Uani 1 1 d . . . N7 N 0.8925(3) 1.0937(3) 1.5600(2) 0.0116(7) Uani 1 1 d . . . N8 N 0.7391(3) 0.8731(3) 1.5511(3) 0.0133(7) Uani 1 1 d . . . N9 N 0.6428(4) 0.9767(4) 0.0560(4) 0.0413(11) Uani 1 1 d . . . O1 O 0.7423(3) 1.2364(3) 0.8715(2) 0.0305(8) Uani 1 1 d . . . O2 O 0.6442(2) 1.2427(3) 0.9942(2) 0.0196(6) Uani 1 1 d . . . O3 O 0.5447(2) 0.6762(3) 1.3725(2) 0.0183(6) Uani 1 1 d . . . O4 O 0.3820(3) 0.4799(3) 1.2955(2) 0.0259(7) Uani 1 1 d . . . O11 O 0.7494(2) 1.4295(3) 1.3395(2) 0.0191(6) Uani 1 1 d . . . O12 O 0.5693(3) 1.2878(3) 1.2089(3) 0.0330(8) Uani 1 1 d . . . O13 O 0.6440(3) 1.5085(3) 1.2932(3) 0.0339(8) Uani 1 1 d . . . O14 O 0.5805(3) 1.4096(4) 1.3906(3) 0.0412(9) Uani 1 1 d . . . O21 O 0.8988(3) 1.2284(3) 1.0422(2) 0.0283(7) Uani 1 1 d . . . O22 O 0.9518(4) 1.1589(3) 1.1428(3) 0.0517(11) Uani 1 1 d . . . O23 O 1.0942(3) 1.3048(4) 1.1114(3) 0.0553(11) Uani 1 1 d . . . O24 O 0.9747(3) 1.0921(3) 0.9675(3) 0.0393(9) Uani 1 1 d . . . O31 O 0.6975(2) 1.1275(3) 1.6279(2) 0.0216(7) Uani 1 1 d . . . O32 O 0.5462(2) 1.1517(3) 1.6952(2) 0.0196(6) Uani 1 1 d . . . O33 O 0.5621(2) 1.1386(3) 1.5308(2) 0.0237(7) Uani 1 1 d . . . O34 O 0.6989(2) 1.3218(3) 1.6951(3) 0.0273(7) Uani 1 1 d . . . O41 O 0.8170(2) 0.8985(3) 1.3354(2) 0.0210(7) Uani 1 1 d . . . O42 O 0.6543(2) 0.8294(3) 1.2062(2) 0.0283(7) Uani 1 1 d . . . O43 O 0.7661(5) 0.7343(6) 1.1607(4) 0.124(3) Uani 1 1 d U . . O44 O 0.8385(4) 0.9437(6) 1.1990(4) 0.0971(19) Uani 1 1 d U . . Cl1 Cl 0.63385(8) 1.40993(9) 1.30897(8) 0.0166(2) Uani 1 1 d . . . Cl2 Cl 0.98206(9) 1.19483(10) 1.06553(8) 0.0223(2) Uani 1 1 d . . . Cl3 Cl 0.62579(8) 1.18618(9) 1.63814(8) 0.0158(2) Uani 1 1 d . . . Cl4 Cl 0.76730(10) 0.84602(14) 1.22128(9) 0.0383(3) Uani 1 1 d . . . Pb1 Pb 0.773980(12) 1.257289(14) 1.172446(12) 0.01352(5) Uani 1 1 d . . . Pb2 Pb 0.682649(12) 0.955744(13) 1.441753(11) 0.01142(5) 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 C1 0.035(3) 0.033(3) 0.041(3) 0.018(3) 0.016(2) 0.016(3) C2 0.022(2) 0.027(3) 0.020(2) 0.014(2) 0.0034(19) 0.008(2) C3 0.016(2) 0.025(2) 0.018(2) 0.012(2) -0.0018(19) 0.005(2) C4 0.022(2) 0.029(3) 0.028(2) 0.020(2) 0.007(2) 0.016(2) C5 0.019(2) 0.016(2) 0.019(2) 0.0098(19) 0.0077(18) 0.0113(19) C6 0.024(2) 0.024(2) 0.019(2) 0.015(2) 0.0078(19) 0.016(2) C7 0.024(2) 0.016(2) 0.022(2) 0.0141(19) 0.0116(19) 0.010(2) C8 0.015(2) 0.017(2) 0.016(2) 0.0096(19) 0.0066(17) 0.0070(19) C9 0.013(2) 0.014(2) 0.013(2) 0.0074(18) 0.0070(17) 0.0083(18) C10 0.015(2) 0.014(2) 0.015(2) 0.0079(18) 0.0056(17) 0.0080(18) C11 0.011(2) 0.019(2) 0.023(2) 0.014(2) 0.0036(18) 0.0038(19) C12 0.013(2) 0.0090(19) 0.0102(19) 0.0048(17) 0.0046(16) 0.0068(17) C13 0.009(2) 0.012(2) 0.013(2) 0.0063(17) 0.0021(16) 0.0033(17) C14 0.014(2) 0.0097(19) 0.0090(19) 0.0026(17) 0.0032(16) 0.0078(18) C15 0.013(2) 0.014(2) 0.015(2) 0.0088(18) 0.0081(17) 0.0089(18) C16 0.010(2) 0.018(2) 0.020(2) 0.0149(19) 0.0036(17) 0.0055(18) C17 0.009(2) 0.019(2) 0.024(2) 0.015(2) 0.0019(17) 0.0037(18) C18 0.012(2) 0.017(2) 0.013(2) 0.0073(18) 0.0020(16) 0.0066(18) C19 0.015(2) 0.013(2) 0.015(2) 0.0074(18) 0.0078(17) 0.0094(18) C20 0.015(2) 0.024(2) 0.020(2) 0.015(2) 0.0056(18) 0.009(2) C21 0.022(2) 0.023(2) 0.025(2) 0.019(2) 0.0077(19) 0.012(2) C22 0.021(2) 0.018(2) 0.024(2) 0.016(2) 0.0112(19) 0.011(2) C23 0.016(2) 0.011(2) 0.015(2) 0.0076(18) 0.0073(17) 0.0068(18) C24 0.018(2) 0.015(2) 0.021(2) 0.0131(19) 0.0044(18) 0.0052(19) C25 0.020(2) 0.017(2) 0.027(2) 0.010(2) 0.004(2) 0.012(2) C26 0.032(3) 0.022(2) 0.024(2) 0.011(2) 0.005(2) 0.010(2) C27 0.040(3) 0.025(3) 0.032(3) 0.016(2) 0.000(2) 0.013(2) C28 0.053(3) 0.025(3) 0.024(3) 0.014(2) 0.014(3) 0.020(3) C29 0.060(4) 0.029(3) 0.030(3) 0.009(2) 0.011(3) 0.024(3) N1 0.0136(18) 0.0141(18) 0.0170(17) 0.0099(15) 0.0060(14) 0.0081(15) N2 0.0163(18) 0.0113(17) 0.0111(16) 0.0061(15) 0.0063(14) 0.0078(15) N3 0.0080(17) 0.0151(17) 0.0149(17) 0.0105(15) 0.0018(14) 0.0041(15) N4 0.0105(17) 0.0121(17) 0.0113(16) 0.0066(14) 0.0029(13) 0.0059(15) N5 0.0128(18) 0.0118(17) 0.0156(17) 0.0105(15) 0.0055(14) 0.0060(15) N6 0.0078(17) 0.0096(16) 0.0153(17) 0.0091(15) 0.0022(13) 0.0014(14) N7 0.0121(17) 0.0138(17) 0.0136(17) 0.0085(15) 0.0050(14) 0.0086(15) N8 0.0152(18) 0.0143(18) 0.0151(17) 0.0092(15) 0.0067(14) 0.0092(16) N9 0.054(3) 0.035(3) 0.035(3) 0.021(2) 0.019(2) 0.018(2) O1 0.0255(18) 0.0347(19) 0.0240(17) 0.0181(16) 0.0073(14) 0.0066(16) O2 0.0173(16) 0.0214(16) 0.0180(15) 0.0111(13) 0.0047(12) 0.0074(13) O3 0.0202(16) 0.0171(15) 0.0158(15) 0.0084(13) 0.0033(12) 0.0084(13) O4 0.0219(17) 0.0228(17) 0.0331(18) 0.0179(15) 0.0049(14) 0.0082(15) O11 0.0153(15) 0.0206(16) 0.0198(15) 0.0090(13) 0.0021(12) 0.0099(13) O12 0.0207(17) 0.0269(18) 0.0297(18) 0.0045(15) -0.0024(14) 0.0077(15) O13 0.0276(19) 0.0338(19) 0.059(2) 0.0335(18) 0.0137(17) 0.0198(16) O14 0.038(2) 0.063(3) 0.038(2) 0.033(2) 0.0275(17) 0.030(2) O21 0.0339(19) 0.0380(19) 0.0214(16) 0.0150(15) 0.0095(14) 0.0253(16) O22 0.106(3) 0.044(2) 0.030(2) 0.0279(18) 0.026(2) 0.046(2) O23 0.0186(19) 0.056(3) 0.043(2) 0.003(2) 0.0088(17) 0.0073(19) O24 0.058(2) 0.042(2) 0.0249(18) 0.0107(17) 0.0177(17) 0.038(2) O31 0.0196(16) 0.0249(16) 0.0209(16) 0.0081(14) 0.0050(13) 0.0161(14) O32 0.0145(15) 0.0271(17) 0.0226(16) 0.0173(14) 0.0095(13) 0.0098(14) O33 0.0244(17) 0.0322(18) 0.0230(16) 0.0189(15) 0.0090(13) 0.0159(15) O34 0.0168(16) 0.0128(15) 0.044(2) 0.0125(15) 0.0092(14) 0.0035(13) O41 0.0243(17) 0.0321(17) 0.0163(15) 0.0135(14) 0.0086(13) 0.0208(15) O42 0.0165(16) 0.0365(19) 0.0331(18) 0.0226(16) 0.0006(14) 0.0101(15) O43 0.135(5) 0.150(5) 0.042(3) -0.028(3) -0.023(3) 0.128(4) O44 0.033(2) 0.181(5) 0.089(3) 0.112(4) 0.019(2) 0.018(3) Cl1 0.0137(5) 0.0166(5) 0.0196(5) 0.0102(4) 0.0064(4) 0.0070(4) Cl2 0.0273(6) 0.0262(6) 0.0188(5) 0.0116(5) 0.0093(5) 0.0179(5) Cl3 0.0117(5) 0.0147(5) 0.0206(5) 0.0092(4) 0.0060(4) 0.0063(4) Cl4 0.0265(6) 0.0725(10) 0.0179(6) 0.0206(6) 0.0091(5) 0.0301(7) Pb1 0.01243(9) 0.01221(8) 0.01495(8) 0.00864(7) 0.00325(6) 0.00392(7) Pb2 0.00903(8) 0.01186(8) 0.01438(8) 0.00852(7) 0.00278(6) 0.00436(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.296(6) . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? C2 C3 1.478(6) . ? C2 H2 0.9300 . ? C3 O1 1.207(5) . ? C3 O2 1.359(5) . ? C4 O2 1.442(5) . ? C4 C5 1.504(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.336(5) . ? C5 C6 1.387(6) . ? C6 C7 1.379(6) . ? C6 H6 0.9300 . ? C7 C8 1.378(6) . ? C7 H7 0.9300 . ? C8 C9 1.383(6) . ? C8 H8 0.9300 . ? C9 N1 1.357(5) . ? C9 C10 1.461(6) . ? C10 N2 1.286(5) . ? C10 H10 0.9300 . ? C11 N3 1.456(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.349(5) . ? C12 N3 1.379(5) . ? C12 C13 1.390(5) . ? C13 C14 1.396(5) . ? C13 H13 0.9300 . ? C14 N5 1.354(5) . ? C14 N6 1.374(5) . ? C15 N5 1.335(5) . ? C15 N4 1.342(5) . ? C15 C16 1.487(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N6 1.461(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N7 1.288(5) . ? C18 C19 1.457(6) . ? C18 H18 0.9300 . ? C19 N8 1.352(5) . ? C19 C20 1.385(6) . ? C20 C21 1.381(6) . ? C20 H20 0.9300 . ? C21 C22 1.376(6) . ? C21 H21 0.9300 . ? C22 C23 1.394(6) . ? C22 H22 0.9300 . ? C23 N8 1.344(5) . ? C23 C24 1.503(6) . ? C24 O3 1.436(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.207(5) . ? C25 O3 1.380(5) . ? C25 C26 1.474(6) . ? C26 C27 1.304(6) . ? C26 H26 0.9300 . ? C27 H27A 0.9300 . ? C27 H27B 0.9300 . ? C28 N9 1.144(6) . ? C28 C29 1.443(7) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? N1 Pb1 2.567(3) . ? N2 N3 1.378(4) . ? N2 Pb1 2.499(3) . ? N4 Pb1 2.584(3) . ? N5 Pb2 2.587(3) . ? N6 N7 1.378(4) . ? N7 Pb2 2.553(3) . ? N8 Pb2 2.588(3) . ? O11 Cl1 1.465(3) . ? O11 Pb1 2.642(3) . ? O12 Cl1 1.440(3) . ? O13 Cl1 1.419(3) . ? O14 Cl1 1.415(3) . ? O21 Cl2 1.455(3) . ? O21 Pb1 2.584(3) . ? O22 Cl2 1.435(3) . ? O23 Cl2 1.422(4) . ? O24 Cl2 1.425(3) . ? O31 Cl3 1.462(3) . ? O31 Pb2 2.563(3) . ? O32 Cl3 1.434(3) . ? O33 Cl3 1.446(3) . ? O34 Cl3 1.426(3) . ? O41 Cl4 1.462(3) . ? O41 Pb2 2.557(3) . ? O42 Cl4 1.422(3) . ? O43 Cl4 1.352(5) . ? O44 Cl4 1.459(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 120.5(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? O1 C3 O2 122.8(4) . . ? O1 C3 C2 126.4(4) . . ? O2 C3 C2 110.8(4) . . ? O2 C4 C5 112.7(3) . . ? O2 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? O2 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N1 C5 C6 121.7(4) . . ? N1 C5 C4 117.4(4) . . ? C6 C5 C4 120.9(4) . . ? C7 C6 C5 119.9(4) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 C6 118.7(4) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C7 C8 C9 119.1(4) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? N1 C9 C8 122.2(4) . . ? N1 C9 C10 118.4(3) . . ? C8 C9 C10 119.4(4) . . ? N2 C10 C9 120.9(4) . . ? N2 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 N3 116.8(3) . . ? N4 C12 C13 121.6(3) . . ? N3 C12 C13 121.5(3) . . ? C12 C13 C14 116.9(4) . . ? C12 C13 H13 121.5 . . ? C14 C13 H13 121.5 . . ? N5 C14 N6 117.7(3) . . ? N5 C14 C13 121.4(3) . . ? N6 C14 C13 120.9(3) . . ? N5 C15 N4 125.0(3) . . ? N5 C15 C16 118.2(3) . . ? N4 C15 C16 116.8(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 120.8(4) . . ? N7 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? N8 C19 C20 122.4(4) . . ? N8 C19 C18 118.4(3) . . ? C20 C19 C18 119.2(4) . . ? C21 C20 C19 119.0(4) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C22 C21 C20 119.1(4) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 119.4(4) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? N8 C23 C22 121.8(4) . . ? N8 C23 C24 118.3(3) . . ? C22 C23 C24 119.8(4) . . ? O3 C24 C23 110.3(3) . . ? O3 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? O3 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? O4 C25 O3 123.9(4) . . ? O4 C25 C26 125.5(4) . . ? O3 C25 C26 110.6(4) . . ? C27 C26 C25 120.9(5) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? N9 C28 C29 176.3(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C5 N1 C9 118.5(3) . . ? C5 N1 Pb1 125.9(3) . . ? C9 N1 Pb1 114.2(2) . . ? C10 N2 N3 119.4(3) . . ? C10 N2 Pb1 117.6(3) . . ? N3 N2 Pb1 121.4(2) . . ? N2 N3 C12 116.2(3) . . ? N2 N3 C11 119.2(3) . . ? C12 N3 C11 124.5(3) . . ? C15 N4 C12 117.5(3) . . ? C15 N4 Pb1 121.5(2) . . ? C12 N4 Pb1 119.4(2) . . ? C15 N5 C14 117.5(3) . . ? C15 N5 Pb2 120.5(2) . . ? C14 N5 Pb2 120.2(2) . . ? C14 N6 N7 117.1(3) . . ? C14 N6 C17 122.5(3) . . ? N7 N6 C17 119.9(3) . . ? C18 N7 N6 119.6(3) . . ? C18 N7 Pb2 119.0(3) . . ? N6 N7 Pb2 121.4(2) . . ? C23 N8 C19 118.3(3) . . ? C23 N8 Pb2 125.0(3) . . ? C19 N8 Pb2 116.6(2) . . ? C3 O2 C4 113.1(3) . . ? C25 O3 C24 113.4(3) . . ? Cl1 O11 Pb1 108.53(14) . . ? Cl2 O21 Pb1 115.55(16) . . ? Cl3 O31 Pb2 120.56(15) . . ? Cl4 O41 Pb2 109.30(15) . . ? O14 Cl1 O13 111.2(2) . . ? O14 Cl1 O12 110.4(2) . . ? O13 Cl1 O12 109.8(2) . . ? O14 Cl1 O11 109.57(19) . . ? O13 Cl1 O11 108.91(18) . . ? O12 Cl1 O11 106.79(18) . . ? O23 Cl2 O24 111.2(2) . . ? O23 Cl2 O22 110.1(3) . . ? O24 Cl2 O22 111.9(2) . . ? O23 Cl2 O21 108.4(2) . . ? O24 Cl2 O21 108.77(19) . . ? O22 Cl2 O21 106.3(2) . . ? O34 Cl3 O32 110.37(18) . . ? O34 Cl3 O33 110.26(18) . . ? O32 Cl3 O33 109.40(18) . . ? O34 Cl3 O31 108.86(18) . . ? O32 Cl3 O31 109.57(17) . . ? O33 Cl3 O31 108.34(17) . . ? O43 Cl4 O42 112.0(3) . . ? O43 Cl4 O44 113.2(4) . . ? O42 Cl4 O44 107.6(2) . . ? O43 Cl4 O41 109.0(3) . . ? O42 Cl4 O41 108.54(18) . . ? O44 Cl4 O41 106.3(2) . . ? N2 Pb1 N1 66.22(10) . . ? N2 Pb1 N4 61.37(10) . . ? N1 Pb1 N4 124.73(10) . . ? N2 Pb1 O21 76.64(10) . . ? N1 Pb1 O21 69.80(10) . . ? N4 Pb1 O21 112.04(9) . . ? N2 Pb1 O11 75.08(9) . . ? N1 Pb1 O11 78.30(9) . . ? N4 Pb1 O11 72.74(9) . . ? O21 Pb1 O11 143.77(10) . . ? N7 Pb2 O41 68.25(9) . . ? N7 Pb2 O31 70.89(9) . . ? O41 Pb2 O31 138.71(9) . . ? N7 Pb2 N5 61.93(10) . . ? O41 Pb2 N5 74.50(10) . . ? O31 Pb2 N5 81.51(10) . . ? N7 Pb2 N8 64.98(10) . . ? O41 Pb2 N8 85.06(9) . . ? O31 Pb2 N8 83.12(9) . . ? N5 Pb2 N8 126.88(10) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 1.350 _refine_diff_density_min -1.368 _refine_diff_density_rms 0.104 #===END data_Complex_4(djh816) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H72 F18 N20 O28 S6 Zn4, 2(C F3 O3 S), 2(O)' _chemical_formula_sum 'C35 H36 F12 N10 O18 S4 Zn2' _chemical_formula_weight 1371.72 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 '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 11.7789(6) _cell_length_b 14.4891(7) _cell_length_c 17.0456(9) _cell_angle_alpha 92.881(3) _cell_angle_beta 108.955(3) _cell_angle_gamma 98.791(3) _cell_volume 2703.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6587 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.24 _exptl_crystal_description 'rod' _exptl_crystal_colour 'yellow' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.67 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 1.159 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19039 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9934 _reflns_number_gt 7905 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^ > 2\s(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^)+(0.0709P)^2^+30.7576P] 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 9934 _refine_ls_number_parameters 741 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1287 _refine_ls_R_factor_gt 0.1055 _refine_ls_wR_factor_ref 0.2511 _refine_ls_wR_factor_gt 0.2361 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3855(15) 0.1457(13) 0.2908(9) 0.085(5) Uani 1 1 d . . . H1A H 0.3308 0.0917 0.2627 0.102 Uiso 1 1 calc R . . H1B H 0.3589 0.1933 0.3150 0.102 Uiso 1 1 calc R . . C2 C 0.5001(13) 0.1549(11) 0.2961(8) 0.070(4) Uani 1 1 d . . . H2 H 0.5548 0.2089 0.3242 0.084 Uiso 1 1 calc R . . C3 C 0.5427(10) 0.0796(9) 0.2577(7) 0.049(3) Uani 1 1 d . . . C4 C 0.7128(9) 0.0257(6) 0.2391(7) 0.037(2) Uani 1 1 d . . . H4A H 0.6728 -0.0359 0.2450 0.045 Uiso 1 1 calc R . . H4B H 0.7992 0.0317 0.2700 0.045 Uiso 1 1 calc R . . C5 C 0.6954(8) 0.0335(6) 0.1492(7) 0.034(2) Uani 1 1 d . . . C6 C 0.6536(9) 0.1102(6) 0.1099(7) 0.037(2) Uani 1 1 d . . . H6 H 0.6389 0.1594 0.1403 0.045 Uiso 1 1 calc R . . C7 C 0.6344(9) 0.1123(6) 0.0266(7) 0.041(2) Uani 1 1 d . . . H7 H 0.6070 0.1633 0.0001 0.050 Uiso 1 1 calc R . . C8 C 0.6556(8) 0.0392(6) -0.0183(6) 0.033(2) Uani 1 1 d . . . H8 H 0.6427 0.0397 -0.0750 0.040 Uiso 1 1 calc R . . C9 C 0.6967(8) -0.0352(6) 0.0235(6) 0.0279(19) Uani 1 1 d . . . C10 C 0.7154(8) -0.1168(6) -0.0224(6) 0.0299(19) Uani 1 1 d . . . H10 H 0.7001 -0.1195 -0.0796 0.036 Uiso 1 1 calc R . . C11 C 0.7564(8) -0.2709(6) -0.1053(5) 0.0284(19) Uani 1 1 d . . . H11A H 0.6723 -0.2730 -0.1379 0.043 Uiso 1 1 calc R . . H11B H 0.7819 -0.3274 -0.1196 0.043 Uiso 1 1 calc R . . H11C H 0.8057 -0.2177 -0.1168 0.043 Uiso 1 1 calc R . . C12 C 0.8140(7) -0.3272(5) 0.0360(5) 0.0196(16) Uani 1 1 d . . . C13 C 0.8301(7) -0.4156(5) 0.0061(5) 0.0211(16) Uani 1 1 d . . . H13 H 0.8171 -0.4317 -0.0500 0.025 Uiso 1 1 calc R . . C14 C 0.8663(7) -0.4763(5) 0.0655(5) 0.0189(16) Uani 1 1 d . . . C15 C 0.8799(7) -0.3665(6) 0.1713(5) 0.0228(17) Uani 1 1 d . . . C16 C 0.9138(8) -0.3361(6) 0.2620(5) 0.0270(18) Uani 1 1 d . . . H16A H 0.9641 -0.2749 0.2750 0.041 Uiso 1 1 calc R . . H16B H 0.9580 -0.3800 0.2938 0.041 Uiso 1 1 calc R . . H16C H 0.8412 -0.3339 0.2755 0.041 Uiso 1 1 calc R . . C17 C 0.8470(8) -0.6083(6) -0.0423(5) 0.0293(19) Uani 1 1 d . . . H17A H 0.9127 -0.6350 -0.0504 0.044 Uiso 1 1 calc R . . H17B H 0.8268 -0.5616 -0.0800 0.044 Uiso 1 1 calc R . . H17C H 0.7769 -0.6569 -0.0530 0.044 Uiso 1 1 calc R . . C18 C 0.9243(7) -0.7060(6) 0.0948(5) 0.0234(17) Uani 1 1 d . . . H18 H 0.9088 -0.7362 0.0419 0.028 Uiso 1 1 calc R . . C19 C 0.9603(7) -0.7535(5) 0.1692(5) 0.0220(17) Uani 1 1 d . . . C20 C 0.9892(8) -0.8433(6) 0.1654(5) 0.0259(18) Uani 1 1 d . . . H20 H 0.9801 -0.8757 0.1146 0.031 Uiso 1 1 calc R . . C21 C 1.0319(8) -0.8832(6) 0.2399(5) 0.0296(19) Uani 1 1 d . . . H21 H 1.0509 -0.9432 0.2394 0.035 Uiso 1 1 calc R . . C22 C 1.0457(8) -0.8330(6) 0.3136(6) 0.032(2) Uani 1 1 d . . . H22 H 1.0760 -0.8582 0.3637 0.039 Uiso 1 1 calc R . . C23 C 1.0142(8) -0.7442(6) 0.3137(5) 0.0263(18) Uani 1 1 d . . . C24 C 1.0250(8) -0.6914(6) 0.3937(5) 0.0272(18) Uani 1 1 d . . . H24A H 1.1003 -0.6971 0.4369 0.033 Uiso 1 1 calc R . . H24B H 1.0242 -0.6254 0.3870 0.033 Uiso 1 1 calc R . . C25 C 0.9125(10) -0.6936(8) 0.4832(7) 0.045(3) Uani 1 1 d . . . C26 C 0.8055(12) -0.7438(12) 0.5008(9) 0.074(4) Uani 1 1 d . . . H26 H 0.7588 -0.7975 0.4665 0.088 Uiso 1 1 calc R . . C27 C 0.7760(14) -0.7141(11) 0.5628(10) 0.082(5) Uani 1 1 d . . . H27A H 0.8223 -0.6604 0.5974 0.098 Uiso 1 1 calc R . . H27B H 0.7086 -0.7464 0.5730 0.098 Uiso 1 1 calc R . . C28 C 1.1845(9) -0.1542(7) 0.1874(7) 0.041(2) Uani 1 1 d . . . C29 C 1.3140(8) -0.5414(8) 0.3429(6) 0.039(2) Uani 1 1 d . . . C30 C 0.5518(10) -0.5457(8) 0.1360(10) 0.063(4) Uani 1 1 d . . . C32 C 0.5606(10) -0.2715(8) 0.1787(7) 0.045(3) Uani 1 1 d . . . C33 C 0.4675(10) -0.3246(9) 0.2061(9) 0.062(3) Uani 1 1 d . . . H33A H 0.4285 -0.3802 0.1681 0.092 Uiso 1 1 calc R . . H33B H 0.4079 -0.2866 0.2072 0.092 Uiso 1 1 calc R . . H33C H 0.5048 -0.3419 0.2610 0.092 Uiso 1 1 calc R . . C34 C 0.8125(8) -0.5212(6) 0.3659(6) 0.032(2) Uani 1 1 d . . . C35 C 0.7540(10) -0.4996(9) 0.4267(7) 0.051(3) Uani 1 1 d . . . H35A H 0.6795 -0.5437 0.4154 0.077 Uiso 1 1 calc R . . H35B H 0.7363 -0.4371 0.4226 0.077 Uiso 1 1 calc R . . H35C H 0.8078 -0.5038 0.4819 0.077 Uiso 1 1 calc R . . N1 N 0.7180(6) -0.0388(5) 0.1061(5) 0.0288(16) Uani 1 1 d . . . N2 N 0.7535(6) -0.1842(4) 0.0187(4) 0.0220(14) Uani 1 1 d . . . N3 N 0.7705(6) -0.2628(5) -0.0172(4) 0.0243(15) Uani 1 1 d . . . N4 N 0.8403(6) -0.3032(4) 0.1186(4) 0.0212(14) Uani 1 1 d . . . N5 N 0.8904(6) -0.4529(4) 0.1472(4) 0.0204(14) Uani 1 1 d . . . N6 N 0.8837(6) -0.5656(4) 0.0424(4) 0.0202(14) Uani 1 1 d . . . N7 N 0.9151(6) -0.6196(4) 0.1063(4) 0.0195(14) Uani 1 1 d . . . N8 N 0.9706(6) -0.7062(4) 0.2424(4) 0.0214(14) Uani 1 1 d . . . N9 N 0.6348(8) -0.2333(6) 0.1606(6) 0.043(2) Uani 1 1 d . . . N10 N 0.8584(7) -0.5371(5) 0.3200(4) 0.0245(15) Uani 1 1 d . . . O1 O 0.4795(7) 0.0096(7) 0.2168(5) 0.060(2) Uani 1 1 d . . . O2 O 0.6642(6) 0.0970(5) 0.2746(5) 0.0454(18) Uani 1 1 d . . . O3 O 0.9218(6) -0.7325(5) 0.4151(4) 0.0373(15) Uani 1 1 d . . . O4 O 1.0170(7) -0.3740(5) 0.4723(5) 0.0492(19) Uani 1 1 d . . . O11 O 0.9808(5) -0.0944(4) 0.1550(4) 0.0271(13) Uani 1 1 d . . . O12 O 1.1373(6) -0.0069(4) 0.1114(4) 0.0341(15) Uani 1 1 d . . . O13 O 1.0306(6) -0.1614(4) 0.0398(4) 0.0331(14) Uani 1 1 d . . . O21 O 1.0991(5) -0.5047(4) 0.2951(3) 0.0235(12) Uani 1 1 d . . . O22 O 1.2594(7) -0.3917(5) 0.2767(5) 0.051(2) Uani 1 1 d . . . O23 O 1.1864(6) -0.5401(5) 0.1891(4) 0.0407(16) Uani 1 1 d . . . O31 O 0.7211(5) -0.6431(4) 0.1693(4) 0.0285(13) Uani 1 1 d . . . O32 O 0.6201(8) -0.6193(6) 0.0235(5) 0.061(2) Uani 1 1 d . . . O33 O 0.5131(6) -0.7217(4) 0.0987(5) 0.048(2) Uani 1 1 d . . . O41 O 0.699(2) -0.2991(14) 0.399(2) 0.34(2) Uani 1 1 d . . . O42 O 0.8151(18) -0.1664(12) 0.4893(8) 0.179(8) Uani 1 1 d . . . O43 O 0.7012(16) -0.1735(16) 0.3523(8) 0.202(11) Uani 1 1 d . . . F11 F 1.2344(6) -0.1031(5) 0.2600(4) 0.0647(19) Uani 1 1 d . . . F12 F 1.1313(6) -0.2377(4) 0.1992(5) 0.0599(19) Uani 1 1 d . . . F13 F 1.2715(5) -0.1683(4) 0.1563(4) 0.0511(16) Uani 1 1 d . . . F21 F 1.3369(6) -0.5017(6) 0.4200(4) 0.069(2) Uani 1 1 d . . . F22 F 1.2742(6) -0.6320(5) 0.3391(5) 0.072(2) Uani 1 1 d . . . F23 F 1.4203(5) -0.5320(5) 0.3291(4) 0.0597(18) Uani 1 1 d . . . F31 F 0.6255(6) -0.4645(4) 0.1404(7) 0.106(4) Uani 1 1 d . . . F32 F 0.5422(8) -0.5575(6) 0.2123(5) 0.083(3) Uani 1 1 d . . . F33 F 0.4414(6) -0.5389(5) 0.0836(6) 0.086(3) Uani 1 1 d . . . S1 S 1.07155(18) -0.09786(14) 0.11425(13) 0.0236(4) Uani 1 1 d . . . S2 S 1.20422(19) -0.48799(15) 0.26667(13) 0.0258(5) Uani 1 1 d . . . S3 S 0.6070(2) -0.64321(17) 0.10266(17) 0.0384(6) Uani 1 1 d . . . S4 S 0.7151(4) -0.2018(3) 0.4229(2) 0.0711(10) Uani 1 1 d D . . Zn1 Zn 0.79905(9) -0.16449(6) 0.14739(6) 0.0257(3) Uani 1 1 d . . . Zn2 Zn 0.91800(8) -0.56921(6) 0.22368(6) 0.0198(2) Uani 1 1 d . . . O5 O 0.8666(8) -0.1267(5) 0.2708(5) 0.0488(19) Uani 1 1 d D . . H5A H 0.924(7) -0.106(10) 0.313(4) 0.073 Uiso 1 1 d D . . H5B H 0.817(7) -0.132(9) 0.294(6) 0.073 Uiso 1 1 d D . . C31 C 0.5903(19) -0.188(2) 0.4564(15) 0.39(3) Uani 1 1 d DU . . F43 F 0.585(2) -0.249(3) 0.5116(15) 0.62(5) Uani 1 1 d D . . F42 F 0.4886(12) -0.212(3) 0.3933(12) 0.48(3) Uani 1 1 d D . . F41 F 0.608(2) -0.100(2) 0.489(2) 0.43(2) Uani 1 1 d D . . O6 O 1.091(2) -0.0555(10) 0.3924(15) 0.246(12) 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 C1 0.093(12) 0.116(13) 0.075(10) 0.017(9) 0.049(9) 0.061(10) C2 0.066(9) 0.090(10) 0.049(7) -0.013(7) 0.004(6) 0.043(8) C3 0.037(6) 0.063(8) 0.049(7) -0.004(6) 0.015(5) 0.016(5) C4 0.038(5) 0.023(5) 0.056(6) 0.004(4) 0.023(5) 0.006(4) C5 0.022(4) 0.026(5) 0.056(6) 0.007(4) 0.015(4) 0.000(4) C6 0.034(5) 0.022(5) 0.057(7) 0.007(4) 0.014(5) 0.009(4) C7 0.031(5) 0.023(5) 0.069(8) 0.019(5) 0.013(5) 0.008(4) C8 0.029(5) 0.026(5) 0.047(6) 0.018(4) 0.014(4) 0.006(4) C9 0.028(5) 0.024(4) 0.035(5) 0.010(4) 0.014(4) 0.005(4) C10 0.028(5) 0.029(5) 0.033(5) 0.013(4) 0.011(4) 0.001(4) C11 0.027(4) 0.033(5) 0.028(5) 0.014(4) 0.012(4) 0.006(4) C12 0.013(4) 0.019(4) 0.026(4) 0.008(3) 0.008(3) -0.002(3) C13 0.020(4) 0.023(4) 0.022(4) 0.006(3) 0.009(3) 0.004(3) C14 0.013(4) 0.020(4) 0.023(4) -0.001(3) 0.008(3) -0.002(3) C15 0.022(4) 0.023(4) 0.029(4) 0.008(3) 0.016(4) 0.001(3) C16 0.041(5) 0.016(4) 0.024(4) 0.004(3) 0.013(4) 0.001(4) C17 0.036(5) 0.031(5) 0.022(4) 0.003(4) 0.012(4) 0.003(4) C18 0.025(4) 0.026(4) 0.018(4) -0.008(3) 0.008(3) 0.002(3) C19 0.023(4) 0.016(4) 0.026(4) -0.006(3) 0.012(3) -0.002(3) C20 0.028(4) 0.023(4) 0.030(5) -0.006(3) 0.016(4) 0.002(3) C21 0.035(5) 0.020(4) 0.032(5) 0.002(4) 0.008(4) 0.010(4) C22 0.035(5) 0.030(5) 0.034(5) 0.008(4) 0.012(4) 0.010(4) C23 0.024(4) 0.026(4) 0.027(5) 0.003(3) 0.007(4) 0.002(3) C24 0.028(4) 0.023(4) 0.032(5) 0.004(4) 0.012(4) 0.005(4) C25 0.040(6) 0.057(7) 0.041(6) 0.012(5) 0.018(5) 0.013(5) C26 0.051(8) 0.108(12) 0.064(9) -0.009(8) 0.034(7) -0.005(7) C27 0.073(10) 0.090(11) 0.099(12) 0.015(9) 0.058(9) 0.001(8) C28 0.039(6) 0.039(6) 0.045(6) 0.014(5) 0.014(5) 0.007(4) C29 0.026(5) 0.062(7) 0.031(5) 0.014(5) 0.012(4) 0.011(5) C30 0.036(6) 0.034(6) 0.116(12) 0.001(6) 0.025(7) 0.003(5) C32 0.037(6) 0.051(6) 0.051(7) 0.013(5) 0.016(5) 0.016(5) C33 0.038(6) 0.065(8) 0.087(10) 0.035(7) 0.026(6) 0.010(6) C34 0.029(5) 0.027(5) 0.037(5) 0.010(4) 0.007(4) 0.005(4) C35 0.049(6) 0.067(8) 0.045(6) -0.010(5) 0.032(5) -0.001(6) N1 0.023(4) 0.016(3) 0.046(5) 0.002(3) 0.012(3) -0.002(3) N2 0.019(3) 0.018(3) 0.028(4) 0.006(3) 0.008(3) -0.002(3) N3 0.026(4) 0.023(4) 0.026(4) 0.008(3) 0.011(3) 0.006(3) N4 0.021(3) 0.014(3) 0.026(4) 0.003(3) 0.007(3) -0.002(3) N5 0.025(3) 0.018(3) 0.021(3) 0.005(3) 0.011(3) 0.002(3) N6 0.023(3) 0.020(3) 0.020(3) 0.001(3) 0.010(3) 0.002(3) N7 0.019(3) 0.021(3) 0.018(3) 0.003(3) 0.006(3) 0.002(3) N8 0.015(3) 0.019(3) 0.029(4) -0.001(3) 0.009(3) -0.002(3) N9 0.048(5) 0.034(4) 0.070(6) 0.019(4) 0.047(5) 0.015(4) N10 0.037(4) 0.022(4) 0.022(4) 0.002(3) 0.021(3) 0.006(3) O1 0.035(4) 0.087(6) 0.051(5) -0.009(4) 0.012(4) -0.002(4) O2 0.041(4) 0.037(4) 0.053(5) -0.007(3) 0.007(3) 0.013(3) O3 0.032(4) 0.050(4) 0.030(3) 0.001(3) 0.015(3) -0.001(3) O4 0.057(5) 0.055(5) 0.040(4) -0.007(4) 0.026(4) 0.003(4) O11 0.024(3) 0.021(3) 0.037(3) -0.003(2) 0.015(3) -0.003(2) O12 0.033(3) 0.020(3) 0.054(4) 0.004(3) 0.022(3) -0.001(3) O13 0.034(3) 0.029(3) 0.038(4) -0.004(3) 0.017(3) 0.003(3) O21 0.023(3) 0.022(3) 0.025(3) 0.000(2) 0.009(2) 0.002(2) O22 0.048(4) 0.033(4) 0.086(6) 0.010(4) 0.044(4) 0.000(3) O23 0.041(4) 0.053(4) 0.032(4) 0.001(3) 0.018(3) 0.008(3) O31 0.021(3) 0.026(3) 0.039(4) 0.006(3) 0.010(3) 0.005(2) O32 0.057(5) 0.077(6) 0.059(5) 0.015(4) 0.036(4) 0.000(4) O33 0.023(3) 0.024(3) 0.097(6) 0.002(3) 0.019(4) 0.002(3) O41 0.17(2) 0.102(14) 0.61(6) 0.06(2) -0.08(3) 0.037(14) O42 0.229(19) 0.162(15) 0.074(9) -0.019(9) -0.058(10) 0.070(14) O43 0.166(15) 0.31(3) 0.055(8) 0.026(11) 0.008(9) -0.114(16) F11 0.057(4) 0.083(5) 0.040(4) 0.006(3) -0.001(3) 0.007(4) F12 0.049(4) 0.050(4) 0.093(5) 0.046(4) 0.031(4) 0.017(3) F13 0.037(3) 0.049(4) 0.080(5) 0.027(3) 0.027(3) 0.023(3) F21 0.045(4) 0.144(7) 0.023(3) 0.015(4) 0.010(3) 0.034(4) F22 0.057(4) 0.056(4) 0.120(7) 0.050(4) 0.038(4) 0.028(4) F23 0.034(3) 0.097(5) 0.060(4) 0.023(4) 0.024(3) 0.026(3) F31 0.036(4) 0.024(3) 0.255(12) 0.017(5) 0.045(6) 0.002(3) F32 0.083(6) 0.094(6) 0.082(6) -0.024(5) 0.051(5) 0.000(5) F33 0.027(3) 0.050(4) 0.172(9) 0.041(5) 0.015(4) 0.010(3) S1 0.0234(10) 0.0180(10) 0.0301(11) 0.0015(8) 0.0116(9) 0.0004(8) S2 0.0262(11) 0.0263(11) 0.0273(11) 0.0050(8) 0.0136(9) 0.0011(8) S3 0.0281(12) 0.0305(12) 0.0546(16) 0.0082(11) 0.0116(11) 0.0029(10) S4 0.079(2) 0.082(3) 0.064(2) 0.0337(19) 0.0342(19) 0.020(2) Zn1 0.0283(5) 0.0185(5) 0.0351(6) 0.0065(4) 0.0165(4) 0.0041(4) Zn2 0.0238(5) 0.0161(4) 0.0211(5) 0.0027(3) 0.0096(4) 0.0032(4) O5 0.079(6) 0.042(4) 0.047(4) 0.010(4) 0.043(4) 0.021(4) C31 0.39(3) 0.39(3) 0.39(3) 0.041(3) 0.131(9) 0.069(5) F43 0.48(5) 1.07(11) 0.21(3) 0.02(4) 0.20(3) -0.37(6) F42 0.083(11) 1.14(10) 0.20(2) 0.04(4) 0.068(13) 0.07(3) F41 0.24(3) 0.41(5) 0.66(7) 0.00(5) 0.12(4) 0.20(3) O6 0.35(3) 0.055(9) 0.26(2) 0.026(12) 0.01(2) 0.031(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.308(19) . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? C2 C3 1.476(16) . ? C2 H2 0.9300 . ? C3 O1 1.196(13) . ? C3 O2 1.345(13) . ? C4 O2 1.450(11) . ? C4 C5 1.492(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.358(12) . ? C5 C6 1.398(13) . ? C6 C7 1.367(15) . ? C6 H6 0.9300 . ? C7 C8 1.376(14) . ? C7 H7 0.9300 . ? C8 C9 1.384(12) . ? C8 H8 0.9300 . ? C9 N1 1.352(11) . ? C9 C10 1.469(13) . ? C10 N2 1.283(11) . ? C10 H10 0.9300 . ? C11 N3 1.454(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.353(10) . ? C12 N3 1.374(10) . ? C12 C13 1.417(11) . ? C13 C14 1.380(11) . ? C13 H13 0.9300 . ? C14 N5 1.342(10) . ? C14 N6 1.398(10) . ? C15 N5 1.333(10) . ? C15 N4 1.345(10) . ? C15 C16 1.489(11) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N6 1.441(10) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N7 1.285(10) . ? C18 C19 1.445(12) . ? C18 H18 0.9300 . ? C19 N8 1.354(10) . ? C19 C20 1.397(11) . ? C20 C21 1.395(12) . ? C20 H20 0.9300 . ? C21 C22 1.370(12) . ? C21 H21 0.9300 . ? C22 C23 1.392(12) . ? C22 H22 0.9300 . ? C23 N8 1.339(11) . ? C23 C24 1.488(12) . ? C24 O3 1.433(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.222(13) 2_746 ? C25 O3 1.309(12) . ? C25 C26 1.481(16) . ? C26 C27 1.289(18) . ? C26 H26 0.9300 . ? C27 H27A 0.9300 . ? C27 H27B 0.9300 . ? C28 F11 1.314(12) . ? C28 F12 1.332(11) . ? C28 F13 1.335(12) . ? C28 S1 1.830(10) . ? C29 F22 1.316(12) . ? C29 F21 1.333(12) . ? C29 F23 1.336(11) . ? C29 S2 1.809(10) . ? C30 F31 1.334(13) . ? C30 F33 1.339(14) . ? C30 F32 1.358(16) . ? C30 S3 1.783(12) . ? C32 N9 1.100(12) . ? C32 C33 1.457(15) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 N10 1.119(11) . ? C34 C35 1.464(13) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? N1 Zn1 2.224(7) . ? N2 N3 1.337(9) . ? N2 Zn1 2.075(7) . ? N4 Zn1 2.206(7) . ? N5 Zn2 2.182(6) . ? N6 N7 1.359(9) . ? N7 Zn2 2.083(6) . ? N8 Zn2 2.176(7) . ? N9 Zn1 2.122(8) . ? N10 Zn2 2.044(6) . ? O4 C25 1.222(13) 2_746 ? O11 S1 1.457(6) . ? O11 Zn1 2.185(5) . ? O12 S1 1.434(6) . ? O13 S1 1.429(6) . ? O21 S2 1.462(6) . ? O21 Zn2 2.120(6) . ? O22 S2 1.422(7) . ? O23 S2 1.425(7) . ? O31 S3 1.451(6) . ? O31 Zn2 2.265(6) . ? O32 S3 1.459(8) . ? O33 S3 1.443(7) . ? O41 S4 1.41(2) . ? O42 S4 1.350(14) . ? O43 S4 1.259(14) . ? S4 C31 1.774(18) . ? Zn1 O5 2.005(8) . ? O5 H5A 0.82(2) . ? O5 H5B 0.80(2) . ? C31 F42 1.308(18) . ? C31 F41 1.321(18) . ? C31 F43 1.323(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 120.1(14) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? O1 C3 O2 122.0(10) . . ? O1 C3 C2 125.6(11) . . ? O2 C3 C2 112.4(10) . . ? O2 C4 C5 112.3(8) . . ? O2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? O2 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C6 121.1(9) . . ? N1 C5 C4 117.2(8) . . ? C6 C5 C4 121.7(9) . . ? C7 C6 C5 119.5(9) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C8 120.1(9) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 118.1(9) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? N1 C9 C8 123.2(8) . . ? N1 C9 C10 116.7(7) . . ? C8 C9 C10 120.1(8) . . ? N2 C10 C9 118.1(8) . . ? N2 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 N3 117.2(7) . . ? N4 C12 C13 121.1(7) . . ? N3 C12 C13 121.6(7) . . ? C14 C13 C12 115.8(7) . . ? C14 C13 H13 122.1 . . ? C12 C13 H13 122.1 . . ? N5 C14 C13 122.9(7) . . ? N5 C14 N6 116.8(7) . . ? C13 C14 N6 120.3(7) . . ? N5 C15 N4 124.1(7) . . ? N5 C15 C16 119.3(7) . . ? N4 C15 C16 116.6(7) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 115.8(7) . . ? N7 C18 H18 122.1 . . ? C19 C18 H18 122.1 . . ? N8 C19 C20 121.7(8) . . ? N8 C19 C18 117.6(7) . . ? C20 C19 C18 120.6(7) . . ? C21 C20 C19 118.3(8) . . ? C21 C20 H20 120.9 . . ? C19 C20 H20 120.9 . . ? C22 C21 C20 119.2(8) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.1(8) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? N8 C23 C22 121.1(8) . . ? N8 C23 C24 119.0(8) . . ? C22 C23 C24 119.9(8) . . ? O3 C24 C23 106.2(7) . . ? O3 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? O3 C24 H24B 110.5 . . ? C23 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? O4 C25 O3 125.2(9) 2_746 . ? O4 C25 C26 123.9(11) 2_746 . ? O3 C25 C26 110.9(10) . . ? C27 C26 C25 121.0(14) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? F11 C28 F12 108.4(9) . . ? F11 C28 F13 109.4(9) . . ? F12 C28 F13 107.6(8) . . ? F11 C28 S1 111.4(7) . . ? F12 C28 S1 109.7(7) . . ? F13 C28 S1 110.2(7) . . ? F22 C29 F21 109.1(9) . . ? F22 C29 F23 107.0(9) . . ? F21 C29 F23 107.1(8) . . ? F22 C29 S2 110.6(7) . . ? F21 C29 S2 111.4(7) . . ? F23 C29 S2 111.4(7) . . ? F31 C30 F33 107.0(10) . . ? F31 C30 F32 109.2(12) . . ? F33 C30 F32 107.9(10) . . ? F31 C30 S3 112.0(9) . . ? F33 C30 S3 111.6(10) . . ? F32 C30 S3 109.0(9) . . ? N9 C32 C33 176.7(12) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N10 C34 C35 179.3(11) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C9 N1 C5 117.9(8) . . ? C9 N1 Zn1 110.3(5) . . ? C5 N1 Zn1 131.6(6) . . ? C10 N2 N3 123.0(7) . . ? C10 N2 Zn1 117.2(6) . . ? N3 N2 Zn1 119.8(5) . . ? N2 N3 C12 115.6(7) . . ? N2 N3 C11 120.0(6) . . ? C12 N3 C11 124.1(7) . . ? C15 N4 C12 117.9(7) . . ? C15 N4 Zn1 128.3(6) . . ? C12 N4 Zn1 113.6(5) . . ? C15 N5 C14 117.9(7) . . ? C15 N5 Zn2 126.9(5) . . ? C14 N5 Zn2 114.6(5) . . ? N7 N6 C14 114.4(6) . . ? N7 N6 C17 119.4(6) . . ? C14 N6 C17 124.8(7) . . ? C18 N7 N6 122.4(7) . . ? C18 N7 Zn2 117.7(5) . . ? N6 N7 Zn2 119.0(5) . . ? C23 N8 C19 119.5(7) . . ? C23 N8 Zn2 129.1(6) . . ? C19 N8 Zn2 111.2(5) . . ? C32 N9 Zn1 169.5(10) . . ? C34 N10 Zn2 171.9(7) . . ? C3 O2 C4 115.5(8) . . ? C25 O3 C24 115.6(8) . . ? S1 O11 Zn1 140.9(4) . . ? S2 O21 Zn2 127.3(3) . . ? S3 O31 Zn2 143.2(4) . . ? O13 S1 O12 116.9(4) . . ? O13 S1 O11 114.3(4) . . ? O12 S1 O11 113.2(4) . . ? O13 S1 C28 103.2(4) . . ? O12 S1 C28 104.4(4) . . ? O11 S1 C28 102.6(4) . . ? O22 S2 O23 116.5(4) . . ? O22 S2 O21 113.7(4) . . ? O23 S2 O21 113.9(4) . . ? O22 S2 C29 104.5(5) . . ? O23 S2 C29 104.3(5) . . ? O21 S2 C29 101.5(4) . . ? O33 S3 O31 113.3(4) . . ? O33 S3 O32 116.7(5) . . ? O31 S3 O32 114.6(4) . . ? O33 S3 C30 102.9(5) . . ? O31 S3 C30 103.5(5) . . ? O32 S3 C30 103.4(6) . . ? O43 S4 O42 121.1(12) . . ? O43 S4 O41 98.2(19) . . ? O42 S4 O41 115.5(12) . . ? O43 S4 C31 111.4(14) . . ? O42 S4 C31 104.7(12) . . ? O41 S4 C31 105.1(17) . . ? O5 Zn1 N2 169.7(3) . . ? O5 Zn1 N9 89.5(4) . . ? N2 Zn1 N9 100.3(3) . . ? O5 Zn1 O11 81.8(3) . . ? N2 Zn1 O11 88.6(2) . . ? N9 Zn1 O11 170.9(3) . . ? O5 Zn1 N4 110.1(3) . . ? N2 Zn1 N4 73.8(3) . . ? N9 Zn1 N4 88.9(3) . . ? O11 Zn1 N4 91.5(2) . . ? O5 Zn1 N1 99.4(3) . . ? N2 Zn1 N1 77.1(3) . . ? N9 Zn1 N1 92.0(3) . . ? O11 Zn1 N1 92.1(2) . . ? N4 Zn1 N1 150.5(3) . . ? N10 Zn2 N7 160.3(3) . . ? N10 Zn2 O21 91.1(3) . . ? N7 Zn2 O21 108.6(2) . . ? N10 Zn2 N8 105.5(3) . . ? N7 Zn2 N8 76.4(3) . . ? O21 Zn2 N8 89.3(2) . . ? N10 Zn2 N5 105.0(3) . . ? N7 Zn2 N5 73.9(2) . . ? O21 Zn2 N5 92.7(2) . . ? N8 Zn2 N5 149.3(2) . . ? N10 Zn2 O31 80.1(3) . . ? N7 Zn2 O31 80.3(2) . . ? O21 Zn2 O31 169.9(2) . . ? N8 Zn2 O31 88.3(2) . . ? N5 Zn2 O31 94.3(2) . . ? Zn1 O5 H5A 151(8) . . ? Zn1 O5 H5B 115(8) . . ? H5A O5 H5B 95(3) . . ? F42 C31 F41 112.7(18) . . ? F42 C31 F43 106.4(17) . . ? F41 C31 F43 112.0(19) . . ? F42 C31 S4 109.3(14) . . ? F41 C31 S4 107.8(15) . . ? F43 C31 S4 108.5(15) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.526 _refine_diff_density_min -0.946 _refine_diff_density_rms 0.151 #===END data_Complex_5(djh865) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H30 B3 F12 N8 O5 Zn2, B F4, C2 H3 N, O' _chemical_formula_sum 'C29 H33 B4 F16 N9 O6 Zn2' _chemical_formula_weight 1081.62 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' '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' 'F' 'F' 0.0171 0.0103 '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) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.4633(11) _cell_length_b 15.6954(16) _cell_length_c 13.1984(12) _cell_angle_alpha 90.000(5) _cell_angle_beta 106.125(4) _cell_angle_gamma 90.000(5) _cell_volume 2082.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9980 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 22.51 _exptl_crystal_description rhomb _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 1.277 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33121 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0464 _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 -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 22.64 _reflns_number_total 5511 _reflns_number_gt 5283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^ > 2\s(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^)+(0.0359P)^2^+3.1033P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(11) _refine_ls_number_reflns 5511 _refine_ls_number_parameters 607 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8123(7) 0.8212(4) 0.0030(5) 0.0417(17) Uani 1 1 d . . . H1A H 0.7713 0.8255 -0.0689 0.050 Uiso 1 1 calc R . . H1B H 0.8413 0.8700 0.0427 0.050 Uiso 1 1 calc R . . C2 C 0.8292(6) 0.7460(4) 0.0488(5) 0.0308(15) Uani 1 1 d . . . H2 H 0.8705 0.7435 0.1209 0.037 Uiso 1 1 calc R . . C3 C 0.7864(5) 0.6656(4) -0.0078(4) 0.0279(14) Uani 1 1 d . . . C4 C 0.6796(6) 0.6024(3) -0.1710(4) 0.0250(13) Uani 1 1 d . . . H4A H 0.5992 0.5798 -0.1581 0.030 Uiso 1 1 calc R . . H4B H 0.7477 0.5586 -0.1541 0.030 Uiso 1 1 calc R . . C5 C 0.6532(5) 0.6295(4) -0.2844(4) 0.0214(13) Uani 1 1 d . . . C6 C 0.6192(5) 0.7126(4) -0.3157(4) 0.0225(13) Uani 1 1 d . . . H6 H 0.6135 0.7531 -0.2657 0.027 Uiso 1 1 calc R . . C7 C 0.5937(5) 0.7363(4) -0.4206(4) 0.0260(14) Uani 1 1 d . . . H7 H 0.5708 0.7920 -0.4419 0.031 Uiso 1 1 calc R . . C8 C 0.6032(5) 0.6747(4) -0.4919(4) 0.0226(13) Uani 1 1 d . . . H8 H 0.5859 0.6880 -0.5631 0.027 Uiso 1 1 calc R . . C9 C 0.6389(5) 0.5922(4) -0.4569(4) 0.0201(12) Uani 1 1 d . . . C10 C 0.6534(5) 0.5259(3) -0.5300(4) 0.0178(12) Uani 1 1 d . . . H10 H 0.6372 0.5366 -0.6017 0.021 Uiso 1 1 calc R . . C11 C 0.6986(6) 0.3959(4) -0.6624(4) 0.0250(13) Uani 1 1 d . . . H11A H 0.6072 0.4026 -0.7021 0.038 Uiso 1 1 calc R . . H11B H 0.7355 0.3470 -0.6876 0.038 Uiso 1 1 calc R . . H11C H 0.7478 0.4458 -0.6706 0.038 Uiso 1 1 calc R . . C12 C 0.7355(5) 0.3078(3) -0.4991(4) 0.0187(12) Uani 1 1 d . . . C13 C 0.7387(5) 0.2333(4) -0.5529(4) 0.0207(12) Uani 1 1 d . . . H13 H 0.7186 0.2324 -0.6261 0.025 Uiso 1 1 calc R . . C14 C 0.7727(5) 0.1599(3) -0.4946(4) 0.0182(12) Uani 1 1 d . . . C15 C 0.7921(5) 0.2354(4) -0.3423(4) 0.0214(13) Uani 1 1 d . . . C16 C 0.8183(6) 0.2355(4) -0.2242(4) 0.0250(13) Uani 1 1 d . . . H16A H 0.7412 0.2146 -0.2061 0.038 Uiso 1 1 calc R . . H16B H 0.8372 0.2926 -0.1980 0.038 Uiso 1 1 calc R . . H16C H 0.8930 0.1995 -0.1931 0.038 Uiso 1 1 calc R . . C17 C 0.7420(7) 0.0670(4) -0.6539(4) 0.0418(18) Uani 1 1 d . . . H17A H 0.7155 0.1197 -0.6908 0.063 Uiso 1 1 calc R . . H17B H 0.6697 0.0271 -0.6730 0.063 Uiso 1 1 calc R . . H17C H 0.8175 0.0442 -0.6725 0.063 Uiso 1 1 calc R . . C18 C 0.8353(5) -0.0595(4) -0.5031(4) 0.0230(12) Uani 1 1 d . . . H18 H 0.8049 -0.0741 -0.5740 0.028 Uiso 1 1 calc R . . C19 C 0.8955(5) -0.1230(4) -0.4220(4) 0.0212(12) Uani 1 1 d . . . C20 C 0.9031(6) -0.2071(4) -0.4487(5) 0.0264(14) Uani 1 1 d . . . H20 H 0.8710 -0.2249 -0.5184 0.032 Uiso 1 1 calc R . . C21 C 0.9598(5) -0.2646(4) -0.3694(5) 0.0285(14) Uani 1 1 d . . . H21 H 0.9645 -0.3221 -0.3848 0.034 Uiso 1 1 calc R . . C22 C 1.0090(6) -0.2360(4) -0.2680(4) 0.0270(14) Uani 1 1 d . . . H22 H 1.0500 -0.2734 -0.2142 0.032 Uiso 1 1 calc R . . C23 C 0.9966(5) -0.1498(4) -0.2466(4) 0.0236(13) Uani 1 1 d . . . C24 C 1.0567(5) -0.1169(4) -0.1367(4) 0.0283(14) Uani 1 1 d . . . H24A H 0.9995 -0.0745 -0.1185 0.034 Uiso 1 1 calc R . . H24B H 1.0702 -0.1630 -0.0859 0.034 Uiso 1 1 calc R . . C25 C 1.2819(5) -0.0783(4) -0.0461(4) 0.0243(13) Uani 1 1 d . . . C26 C 1.4026(6) -0.0387(4) -0.0624(5) 0.0312(15) Uani 1 1 d . . . H26 H 1.3967 -0.0107 -0.1256 0.037 Uiso 1 1 calc R . . C27 C 1.5176(6) -0.0418(4) 0.0091(5) 0.0423(17) Uani 1 1 d . . . H27A H 1.5253 -0.0696 0.0727 0.051 Uiso 1 1 calc R . . H27B H 1.5918 -0.0161 -0.0037 0.051 Uiso 1 1 calc R . . C28 C 0.5827(6) 0.2162(4) 0.0771(5) 0.0283(14) Uani 1 1 d . . . C29 C 0.5377(6) 0.2072(4) -0.0368(4) 0.0381(16) Uani 1 1 d . . . H29A H 0.4677 0.2474 -0.0652 0.057 Uiso 1 1 calc R . . H29B H 0.5050 0.1504 -0.0546 0.057 Uiso 1 1 calc R . . H29C H 0.6106 0.2179 -0.0660 0.057 Uiso 1 1 calc R . . B1 B 0.4862(6) 0.3574(4) -0.2916(5) 0.0237(15) Uani 1 1 d . . . B2 B 1.1396(6) 0.1264(4) -0.3126(5) 0.0241(15) Uani 1 1 d . . . B3 B 0.6470(7) -0.0130(5) -0.2547(5) 0.0290(17) Uani 1 1 d . . . B4 B 0.8928(7) 0.0871(4) 0.0677(5) 0.0263(16) Uani 1 1 d . . . N1 N 0.6644(4) 0.5694(3) -0.3545(3) 0.0191(10) Uani 1 1 d . . . N2 N 0.6891(4) 0.4523(3) -0.4912(3) 0.0192(10) Uani 1 1 d . . . N3 N 0.7066(4) 0.3843(3) -0.5510(3) 0.0201(10) Uani 1 1 d . . . N4 N 0.7588(4) 0.3103(3) -0.3935(3) 0.0187(10) Uani 1 1 d . . . N5 N 0.8040(4) 0.1610(3) -0.3859(3) 0.0183(10) Uani 1 1 d . . . N6 N 0.7776(5) 0.0826(3) -0.5392(3) 0.0230(11) Uani 1 1 d . . . N7 N 0.8268(4) 0.0166(3) -0.4718(3) 0.0227(11) Uani 1 1 d . . . N8 N 0.9390(4) -0.0947(3) -0.3215(3) 0.0193(10) Uani 1 1 d . . . N9 N 0.6173(5) 0.2262(4) 0.1671(4) 0.0391(13) Uani 1 1 d . . . O1 O 0.8044(4) 0.5959(3) 0.0338(3) 0.0302(9) Uani 1 1 d . . . O2 O 0.7233(4) 0.6768(2) -0.1080(3) 0.0305(10) Uani 1 1 d . . . O3 O 1.1844(3) -0.0791(2) -0.1382(3) 0.0258(9) Uani 1 1 d . . . O4 O 1.2709(4) -0.1097(3) 0.0340(3) 0.0281(9) Uani 1 1 d . . . O5 O 0.9044(4) 0.4528(3) -0.2414(3) 0.0387(11) Uani 1 1 d D . . O6 O 1.1170(4) 0.3772(3) -0.2684(3) 0.0418(11) Uani 1 1 d . . . F11 F 0.6089(3) 0.4037(2) -0.2416(3) 0.0407(9) Uani 1 1 d . . . F12 F 0.5030(3) 0.2705(2) -0.2798(3) 0.0381(9) Uani 1 1 d . . . F13 F 0.3845(3) 0.3838(2) -0.2480(3) 0.0393(9) Uani 1 1 d . . . F14 F 0.4517(3) 0.3801(2) -0.3981(2) 0.0313(8) Uani 1 1 d . . . F21 F 1.0641(3) 0.0883(2) -0.2465(3) 0.0399(9) Uani 1 1 d . . . F22 F 1.1100(4) 0.2152(2) -0.3227(3) 0.0488(10) Uani 1 1 d . . . F23 F 1.0951(3) 0.0921(2) -0.4128(2) 0.0383(9) Uani 1 1 d . . . F24 F 1.2725(3) 0.1156(2) -0.2691(3) 0.0388(9) Uani 1 1 d . . . F31 F 0.7813(3) 0.0235(3) -0.2137(3) 0.0471(10) Uani 1 1 d . . . F32 F 0.6226(3) -0.0185(3) -0.3637(2) 0.0451(10) Uani 1 1 d . . . F33 F 0.6397(4) -0.0928(2) -0.2126(3) 0.0511(10) Uani 1 1 d . . . F34 F 0.5537(3) 0.0391(2) -0.2290(2) 0.0362(8) Uani 1 1 d . . . F41 F 0.9013(4) 0.0279(3) -0.0071(3) 0.0602(11) Uani 1 1 d . . . F42 F 1.0185(4) 0.0963(2) 0.1398(3) 0.0518(10) Uani 1 1 d . . . F43 F 0.8108(4) 0.0573(3) 0.1249(3) 0.0687(13) Uani 1 1 d . . . F44 F 0.8527(4) 0.1647(3) 0.0229(3) 0.0608(11) Uani 1 1 d . . . Zn1 Zn 0.72205(6) 0.43429(3) -0.33199(4) 0.01913(16) Uani 1 1 d . . . Zn2 Zn 0.88595(6) 0.04181(4) -0.31239(4) 0.01985(16) Uani 1 1 d . . . H5A H 0.945(12) 0.497(6) -0.264(11) 0.19(7) Uiso 1 1 d D . . H5B H 0.970(5) 0.418(4) -0.246(5) 0.05(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(5) 0.030(4) 0.031(4) -0.008(3) 0.004(3) -0.003(3) C2 0.033(4) 0.027(4) 0.026(3) -0.006(3) -0.002(3) -0.001(3) C3 0.025(3) 0.033(4) 0.027(3) -0.002(3) 0.010(3) 0.006(3) C4 0.038(3) 0.017(3) 0.018(3) -0.007(2) 0.004(3) 0.001(3) C5 0.017(3) 0.028(3) 0.017(3) 0.002(3) 0.001(2) 0.001(2) C6 0.023(3) 0.022(3) 0.024(3) 0.003(3) 0.009(2) 0.004(2) C7 0.020(3) 0.025(3) 0.035(4) 0.004(3) 0.010(3) 0.006(3) C8 0.016(3) 0.028(3) 0.022(3) 0.006(3) 0.002(2) -0.002(3) C9 0.015(3) 0.026(3) 0.017(3) 0.005(2) 0.001(2) 0.005(2) C10 0.020(3) 0.021(3) 0.012(3) 0.001(2) 0.004(2) -0.002(2) C11 0.033(3) 0.025(3) 0.019(3) 0.003(3) 0.011(2) 0.002(3) C12 0.017(3) 0.023(3) 0.017(3) 0.003(2) 0.008(2) -0.004(2) C13 0.024(3) 0.024(3) 0.015(3) 0.001(3) 0.007(2) -0.001(3) C14 0.018(3) 0.022(3) 0.014(3) -0.007(2) 0.004(2) -0.006(2) C15 0.012(3) 0.027(3) 0.026(3) 0.005(3) 0.008(2) 0.004(2) C16 0.037(3) 0.023(3) 0.014(3) 0.001(2) 0.006(2) 0.013(3) C17 0.072(5) 0.033(4) 0.014(3) -0.003(3) 0.003(3) 0.008(3) C18 0.023(3) 0.033(4) 0.012(3) -0.006(3) 0.003(2) 0.003(3) C19 0.018(3) 0.024(3) 0.022(3) 0.001(3) 0.008(2) -0.001(2) C20 0.032(3) 0.022(3) 0.023(3) -0.001(3) 0.003(3) 0.002(3) C21 0.024(3) 0.022(3) 0.039(4) -0.001(3) 0.010(3) 0.000(3) C22 0.030(3) 0.021(4) 0.028(3) 0.008(3) 0.005(3) 0.007(3) C23 0.017(3) 0.030(4) 0.024(3) 0.004(3) 0.005(2) -0.005(2) C24 0.032(3) 0.034(4) 0.019(3) 0.004(3) 0.007(2) -0.001(3) C25 0.033(3) 0.019(3) 0.019(3) 0.001(3) 0.004(3) 0.007(3) C26 0.034(4) 0.033(4) 0.029(3) -0.002(3) 0.012(3) 0.001(3) C27 0.029(4) 0.058(5) 0.040(4) -0.003(3) 0.011(3) -0.005(3) C28 0.029(3) 0.022(3) 0.036(4) 0.002(3) 0.012(3) 0.003(3) C29 0.043(4) 0.042(4) 0.028(4) 0.003(3) 0.008(3) 0.000(3) B1 0.024(4) 0.027(4) 0.019(3) -0.003(3) 0.004(3) -0.003(3) B2 0.021(4) 0.027(4) 0.028(4) 0.006(3) 0.014(3) 0.000(3) B3 0.025(4) 0.033(4) 0.030(4) -0.007(3) 0.010(3) -0.003(3) B4 0.025(4) 0.023(4) 0.024(4) -0.003(3) -0.004(3) 0.005(3) N1 0.021(2) 0.017(3) 0.018(2) -0.003(2) 0.0034(19) -0.0025(19) N2 0.020(2) 0.024(3) 0.015(2) -0.004(2) 0.0067(18) -0.001(2) N3 0.027(3) 0.023(3) 0.011(2) 0.000(2) 0.0068(19) 0.003(2) N4 0.014(2) 0.028(3) 0.013(2) 0.004(2) 0.0032(18) 0.005(2) N5 0.021(2) 0.017(3) 0.016(2) -0.0015(19) 0.0050(18) 0.0031(19) N6 0.031(3) 0.024(3) 0.012(2) 0.002(2) 0.002(2) 0.008(2) N7 0.021(2) 0.026(3) 0.023(3) 0.003(2) 0.010(2) 0.005(2) N8 0.019(2) 0.021(3) 0.017(2) 0.003(2) 0.0033(19) 0.0015(19) N9 0.048(3) 0.042(3) 0.027(3) 0.006(3) 0.009(3) 0.007(3) O1 0.041(2) 0.024(2) 0.025(2) 0.0009(19) 0.0070(18) 0.0018(19) O2 0.043(2) 0.026(2) 0.016(2) -0.0004(17) -0.0033(18) 0.0037(19) O3 0.030(2) 0.028(2) 0.0179(19) 0.0046(17) 0.0037(16) -0.0006(18) O4 0.034(2) 0.033(2) 0.016(2) 0.0037(19) 0.0057(17) 0.0022(19) O5 0.024(2) 0.040(3) 0.045(3) -0.015(2) -0.002(2) 0.002(2) O6 0.037(2) 0.042(3) 0.051(3) 0.012(2) 0.020(2) 0.006(2) F11 0.037(2) 0.045(2) 0.040(2) 0.0025(17) 0.0110(16) -0.0008(17) F12 0.049(2) 0.025(2) 0.0337(19) 0.0018(16) -0.0009(16) -0.0120(16) F13 0.0264(18) 0.057(2) 0.0368(19) 0.0026(18) 0.0124(15) 0.0008(17) F14 0.0299(18) 0.040(2) 0.0195(17) 0.0061(15) -0.0001(13) 0.0031(16) F21 0.037(2) 0.047(2) 0.0357(19) 0.0025(17) 0.0092(16) 0.0003(17) F22 0.067(3) 0.031(2) 0.055(2) 0.0126(18) 0.028(2) 0.0022(19) F23 0.0330(19) 0.058(2) 0.0252(18) -0.0049(17) 0.0108(15) -0.0044(17) F24 0.0262(19) 0.056(2) 0.0348(19) -0.0043(18) 0.0103(15) -0.0022(17) F31 0.042(2) 0.063(3) 0.040(2) -0.0047(19) 0.0174(17) -0.005(2) F32 0.0254(19) 0.084(3) 0.0267(19) -0.0110(19) 0.0090(15) -0.0058(18) F33 0.053(2) 0.027(2) 0.069(3) 0.0055(19) 0.010(2) -0.0036(17) F34 0.0266(17) 0.041(2) 0.0437(19) -0.0040(19) 0.0141(15) 0.0050(18) F41 0.088(3) 0.054(3) 0.038(2) -0.013(2) 0.016(2) 0.009(2) F42 0.049(2) 0.040(2) 0.054(2) -0.0006(19) -0.0066(19) 0.0066(19) F43 0.077(3) 0.083(4) 0.063(3) 0.011(3) 0.047(2) 0.003(3) F44 0.077(3) 0.049(3) 0.049(2) 0.006(2) 0.007(2) 0.017(2) Zn1 0.0219(3) 0.0209(3) 0.0141(3) 0.0003(3) 0.0041(2) 0.0009(3) Zn2 0.0218(3) 0.0232(3) 0.0143(3) 0.0009(3) 0.0046(2) 0.0031(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.315(9) . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? C2 C3 1.472(8) . ? C2 H2 0.9300 . ? C3 O1 1.214(7) . ? C3 O2 1.315(7) . ? C4 O2 1.433(6) . ? C4 C5 1.506(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.349(7) . ? C5 C6 1.385(8) . ? C6 C7 1.386(8) . ? C6 H6 0.9300 . ? C7 C8 1.373(8) . ? C7 H7 0.9300 . ? C8 C9 1.390(8) . ? C8 H8 0.9300 . ? C9 N1 1.351(7) . ? C9 C10 1.455(7) . ? C10 N2 1.277(7) . ? C10 H10 0.9300 . ? C11 N3 1.460(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.347(7) . ? C12 N3 1.373(7) . ? C12 C13 1.374(8) . ? C13 C14 1.376(8) . ? C13 H13 0.9300 . ? C14 N6 1.355(7) . ? C14 N5 1.380(6) . ? C15 N5 1.322(7) . ? C15 N4 1.353(7) . ? C15 C16 1.506(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N6 1.476(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N7 1.275(7) . ? C18 C19 1.471(8) . ? C18 H18 0.9300 . ? C19 N8 1.352(7) . ? C19 C20 1.374(8) . ? C20 C21 1.385(8) . ? C20 H20 0.9300 . ? C21 C22 1.369(8) . ? C21 H21 0.9300 . ? C22 C23 1.396(8) . ? C22 H22 0.9300 . ? C23 N8 1.326(7) . ? C23 C24 1.502(7) . ? C24 O3 1.467(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.200(6) . ? C25 O3 1.353(6) . ? C25 C26 1.476(8) . ? C26 C27 1.308(8) . ? C26 H26 0.9300 . ? C27 H27A 0.9300 . ? C27 H27B 0.9300 . ? C28 N9 1.152(7) . ? C28 C29 1.452(9) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? B1 F12 1.378(8) . ? B1 F14 1.396(7) . ? B1 F13 1.406(7) . ? B1 F11 1.463(7) . ? B2 F24 1.360(7) . ? B2 F23 1.383(7) . ? B2 F22 1.426(8) . ? B2 F21 1.458(7) . ? B3 F33 1.381(8) . ? B3 F34 1.385(8) . ? B3 F32 1.392(7) . ? B3 F31 1.474(8) . ? B4 F44 1.368(8) . ? B4 F43 1.374(8) . ? B4 F41 1.376(8) . ? B4 F42 1.400(7) . ? N1 Zn1 2.202(4) . ? N2 N3 1.370(6) . ? N2 Zn1 2.052(4) . ? N4 Zn1 2.183(4) . ? N5 Zn2 2.172(4) . ? N6 N7 1.369(6) . ? N7 Zn2 2.059(5) . ? N8 Zn2 2.225(4) . ? O5 Zn1 1.971(4) . ? O5 H5A 0.91(2) . ? O5 H5B 0.89(2) . ? F11 Zn1 1.960(3) . ? F21 Zn2 1.966(4) . ? F31 Zn2 1.942(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 123.6(6) . . ? C1 C2 H2 118.2 . . ? C3 C2 H2 118.2 . . ? O1 C3 O2 123.1(5) . . ? O1 C3 C2 123.7(5) . . ? O2 C3 C2 113.1(5) . . ? O2 C4 C5 106.7(4) . . ? O2 C4 H4A 110.4 . . ? C5 C4 H4A 110.4 . . ? O2 C4 H4B 110.4 . . ? C5 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? N1 C5 C6 121.2(5) . . ? N1 C5 C4 117.2(5) . . ? C6 C5 C4 121.6(5) . . ? C5 C6 C7 120.9(5) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 117.8(5) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C7 C8 C9 119.5(5) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? N1 C9 C8 122.6(5) . . ? N1 C9 C10 116.4(5) . . ? C8 C9 C10 120.9(5) . . ? N2 C10 C9 117.1(4) . . ? N2 C10 H10 121.5 . . ? C9 C10 H10 121.5 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 N3 116.2(5) . . ? N4 C12 C13 122.4(5) . . ? N3 C12 C13 121.4(5) . . ? C12 C13 C14 117.7(5) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? N6 C14 C13 122.8(4) . . ? N6 C14 N5 115.9(5) . . ? C13 C14 N5 121.3(5) . . ? N5 C15 N4 126.3(5) . . ? N5 C15 C16 116.1(5) . . ? N4 C15 C16 117.6(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 117.0(5) . . ? N7 C18 H18 121.5 . . ? C19 C18 H18 121.5 . . ? N8 C19 C20 122.7(5) . . ? N8 C19 C18 116.8(5) . . ? C20 C19 C18 120.5(5) . . ? C19 C20 C21 118.3(5) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 119.4(6) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 119.1(5) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? N8 C23 C22 121.9(5) . . ? N8 C23 C24 118.6(5) . . ? C22 C23 C24 119.4(5) . . ? O3 C24 C23 105.4(4) . . ? O3 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? O3 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? O4 C25 O3 123.7(5) . . ? O4 C25 C26 126.6(5) . . ? O3 C25 C26 109.6(5) . . ? C27 C26 C25 122.2(6) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? N9 C28 C29 177.7(7) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? F12 B1 F14 110.8(5) . . ? F12 B1 F13 109.4(5) . . ? F14 B1 F13 108.9(5) . . ? F12 B1 F11 111.8(5) . . ? F14 B1 F11 106.1(5) . . ? F13 B1 F11 109.8(5) . . ? F24 B2 F23 112.9(5) . . ? F24 B2 F22 109.3(5) . . ? F23 B2 F22 106.5(5) . . ? F24 B2 F21 110.9(5) . . ? F23 B2 F21 108.6(5) . . ? F22 B2 F21 108.4(5) . . ? F33 B3 F34 108.4(5) . . ? F33 B3 F32 110.2(5) . . ? F34 B3 F32 110.5(5) . . ? F33 B3 F31 111.0(5) . . ? F34 B3 F31 110.2(5) . . ? F32 B3 F31 106.6(5) . . ? F44 B4 F43 112.1(5) . . ? F44 B4 F41 111.3(5) . . ? F43 B4 F41 109.9(6) . . ? F44 B4 F42 108.6(5) . . ? F43 B4 F42 105.9(5) . . ? F41 B4 F42 108.8(5) . . ? C5 N1 C9 118.1(4) . . ? C5 N1 Zn1 130.8(3) . . ? C9 N1 Zn1 111.1(3) . . ? C10 N2 N3 123.0(4) . . ? C10 N2 Zn1 118.8(3) . . ? N3 N2 Zn1 118.2(3) . . ? N2 N3 C12 116.1(4) . . ? N2 N3 C11 120.2(4) . . ? C12 N3 C11 123.7(4) . . ? C12 N4 C15 116.0(5) . . ? C12 N4 Zn1 114.3(3) . . ? C15 N4 Zn1 129.5(3) . . ? C15 N5 C14 116.1(4) . . ? C15 N5 Zn2 129.7(3) . . ? C14 N5 Zn2 113.8(3) . . ? C14 N6 N7 116.6(4) . . ? C14 N6 C17 124.3(4) . . ? N7 N6 C17 118.9(4) . . ? C18 N7 N6 123.0(4) . . ? C18 N7 Zn2 118.9(4) . . ? N6 N7 Zn2 118.1(3) . . ? C23 N8 C19 118.5(5) . . ? C23 N8 Zn2 131.0(4) . . ? C19 N8 Zn2 110.4(3) . . ? C3 O2 C4 117.7(4) . . ? C25 O3 C24 117.0(4) . . ? Zn1 O5 H5A 112(9) . . ? Zn1 O5 H5B 120(4) . . ? H5A O5 H5B 90(9) . . ? B1 F11 Zn1 116.7(3) . . ? B2 F21 Zn2 119.4(3) . . ? B3 F31 Zn2 118.0(3) . . ? F11 Zn1 O5 108.28(18) . . ? F11 Zn1 N2 134.35(15) . . ? O5 Zn1 N2 117.35(19) . . ? F11 Zn1 N4 101.94(15) . . ? O5 Zn1 N4 96.67(17) . . ? N2 Zn1 N4 74.83(16) . . ? F11 Zn1 N1 97.40(15) . . ? O5 Zn1 N1 97.05(18) . . ? N2 Zn1 N1 76.57(16) . . ? N4 Zn1 N1 151.38(15) . . ? F31 Zn2 F21 113.60(15) . . ? F31 Zn2 N7 126.23(16) . . ? F21 Zn2 N7 120.17(16) . . ? F31 Zn2 N5 101.57(16) . . ? F21 Zn2 N5 94.95(16) . . ? N7 Zn2 N5 74.91(17) . . ? F31 Zn2 N8 95.14(16) . . ? F21 Zn2 N8 99.28(15) . . ? N7 Zn2 N8 76.63(16) . . ? N5 Zn2 N8 151.54(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.64 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.613 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.072 #===END data_Complex_6(dh210) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H35 Cl Cu2 N11 O8, 3(Cl O4)' _chemical_formula_sum 'C33 H35 Cl4 Cu2 N11 O20' _chemical_formula_weight 1174.60 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 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.742(4) _cell_length_b 14.056(4) _cell_length_c 15.538(4) _cell_angle_alpha 111.517(10) _cell_angle_beta 103.767(11) _cell_angle_gamma 104.831(11) _cell_volume 2326.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5340 _cell_measurement_theta_min 2.499 _cell_measurement_theta_max 25.542 _exptl_crystal_description 'plate' _exptl_crystal_colour 'dark green' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.59 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32463 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8188 _reflns_number_gt 6580 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^ > 2\s(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^)+(0.0771P)^2^+4.5682P] 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 8188 _refine_ls_number_parameters 758 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.115 _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 C5 C 0.1219(4) 0.1718(4) 0.2328(3) 0.0292(10) Uani 1 1 d . . . C6 C 0.0345(4) 0.1330(4) 0.1400(4) 0.0363(11) Uani 1 1 d . . . H6 H 0.0391 0.1743 0.1051 0.044 Uiso 1 1 calc R . . C7 C -0.0576(4) 0.0348(4) 0.1006(3) 0.0367(11) Uani 1 1 d . . . H7 H -0.1153 0.0089 0.0388 0.044 Uiso 1 1 calc R . . C8 C -0.0642(4) -0.0261(4) 0.1537(3) 0.0301(10) Uani 1 1 d . . . H8 H -0.1257 -0.0935 0.1281 0.036 Uiso 1 1 calc R . . C9 C 0.0231(4) 0.0163(4) 0.2456(3) 0.0268(9) Uani 1 1 d . . . C10 C 0.0226(4) -0.0408(4) 0.3074(3) 0.0270(9) Uani 1 1 d . . . H10 H -0.0330 -0.1104 0.2861 0.032 Uiso 1 1 calc R . . C11 C 0.0465(4) -0.1332(4) 0.4414(4) 0.0365(11) Uani 1 1 d . . . H11A H -0.0335 -0.1401 0.4214 0.055 Uiso 1 1 calc R . . H11B H 0.0664 -0.1445 0.4995 0.055 Uiso 1 1 calc R . . H11C H 0.0569 -0.1876 0.3884 0.055 Uiso 1 1 calc R . . C12 C 0.2226(4) 0.0450(4) 0.5466(3) 0.0254(9) Uani 1 1 d . . . C13 C 0.3853(4) 0.2094(3) 0.6272(3) 0.0257(9) Uani 1 1 d . . . C14 C 0.4550(4) 0.3141(4) 0.6313(3) 0.0320(10) Uani 1 1 d . . . H14A H 0.4384 0.3737 0.6727 0.048 Uiso 1 1 calc R . . H14B H 0.4352 0.3079 0.5653 0.048 Uiso 1 1 calc R . . H14C H 0.5367 0.3285 0.6584 0.048 Uiso 1 1 calc R . . C15 C 0.3564(4) 0.0963(4) 0.7047(3) 0.0272(10) Uani 1 1 d . . . C16 C 0.2550(4) 0.0209(4) 0.6247(3) 0.0299(10) Uani 1 1 d . . . H16 H 0.2104 -0.0435 0.6236 0.036 Uiso 1 1 calc R . . C17 C 0.3350(5) -0.0010(5) 0.8096(4) 0.0477(14) Uani 1 1 d . . . H17A H 0.3745 -0.0507 0.8094 0.072 Uiso 1 1 calc R . . H17B H 0.2572 -0.0417 0.7604 0.072 Uiso 1 1 calc R . . H17C H 0.3314 0.0343 0.8740 0.072 Uiso 1 1 calc R . . C18 C 0.5587(4) 0.1628(4) 0.9362(3) 0.0338(11) Uani 1 1 d . . . H18 H 0.5294 0.1097 0.9557 0.041 Uiso 1 1 calc R . . C19 C 0.6701(4) 0.2547(4) 0.9954(3) 0.0295(10) Uani 1 1 d . . . C20 C 0.7419(4) 0.2674(4) 1.0848(3) 0.0378(11) Uani 1 1 d . . . H20 H 0.7196 0.2170 1.1089 0.045 Uiso 1 1 calc R . . C21 C 0.8474(4) 0.3569(4) 1.1374(3) 0.0397(12) Uani 1 1 d . . . H21 H 0.8972 0.3671 1.1973 0.048 Uiso 1 1 calc R . . C22 C 0.8784(4) 0.4310(4) 1.1004(3) 0.0346(11) Uani 1 1 d . . . H22 H 0.9493 0.4913 1.1351 0.041 Uiso 1 1 calc R . . C23 C 0.8027(4) 0.4149(4) 1.0106(3) 0.0284(10) Uani 1 1 d . . . C24 C 0.8329(4) 0.4921(4) 0.9662(3) 0.0323(10) Uani 1 1 d . . . H24A H 0.8350 0.4519 0.9013 0.039 Uiso 1 1 calc R . . H24B H 0.7743 0.5239 0.9582 0.039 Uiso 1 1 calc R . . C25 C 0.9681(4) 0.6756(4) 1.0284(3) 0.0334(11) Uani 1 1 d . . . C26 C 1.0813(4) 0.7571(4) 1.1052(3) 0.0347(11) Uani 1 1 d . . . H26 H 1.1161 0.7416 1.1555 0.042 Uiso 1 1 calc R . . C27 C 1.1356(5) 0.8502(4) 1.1065(4) 0.0412(12) Uani 1 1 d . . . H27A H 1.1026 0.8676 1.0570 0.049 Uiso 1 1 calc R . . H27B H 1.2074 0.8991 1.1570 0.049 Uiso 1 1 calc R . . C28 C 0.4596(4) 0.1779(4) 0.3885(4) 0.0385(12) Uani 1 1 d . . . C29 C 0.5751(6) 0.1871(6) 0.3846(5) 0.0638(16) Uani 1 1 d U . . H29A H 0.5811 0.1996 0.3289 0.096 Uiso 1 1 calc R . . H29B H 0.5860 0.1198 0.3773 0.096 Uiso 1 1 calc R . . H29C H 0.6340 0.2478 0.4450 0.096 Uiso 1 1 calc R . . C32 C 0.5522(4) 0.5121(4) 0.8868(3) 0.0389(12) Uani 1 1 d . . . C33 C 0.5393(6) 0.6174(5) 0.9193(5) 0.0588(16) Uani 1 1 d . . . H33A H 0.5950 0.6671 0.9078 0.088 Uiso 1 1 calc R . . H33B H 0.5525 0.6479 0.9890 0.088 Uiso 1 1 calc R . . H33C H 0.4617 0.6071 0.8826 0.088 Uiso 1 1 calc R . . N1 N 0.1158(3) 0.1142(3) 0.2852(3) 0.0263(8) Uani 1 1 d . . . N2 N 0.1054(3) 0.0131(3) 0.3936(3) 0.0267(8) Uani 1 1 d . . . N3 N 0.1217(3) -0.0234(3) 0.4639(3) 0.0278(8) Uani 1 1 d . . . N4 N 0.2872(3) 0.1386(3) 0.5470(2) 0.0255(8) Uani 1 1 d . . . N5 N 0.4227(3) 0.1908(3) 0.7057(2) 0.0260(8) Uani 1 1 d . . . N6 N 0.3982(3) 0.0820(3) 0.7866(3) 0.0299(8) Uani 1 1 d . . . N7 N 0.5037(3) 0.1610(3) 0.8542(3) 0.0282(8) Uani 1 1 d . . . N8 N 0.7003(3) 0.3286(3) 0.9591(3) 0.0276(8) Uani 1 1 d . . . N9 N 0.3719(3) 0.1738(3) 0.3941(3) 0.0293(8) Uani 1 1 d . . . N11 N 0.5637(3) 0.4303(3) 0.8608(3) 0.0383(10) Uani 1 1 d . . . O3 O 0.9448(3) 0.5778(3) 1.0314(2) 0.0303(7) Uani 1 1 d . . . O4 O 0.9027(3) 0.6888(3) 0.9682(3) 0.0569(11) Uani 1 1 d . . . O11 O 0.7540(3) 0.1348(3) 0.6499(3) 0.0465(9) Uani 1 1 d . . . O12 O 0.5876(3) 0.0644(3) 0.6828(3) 0.0402(8) Uani 1 1 d . . . O13 O 0.5756(3) 0.1432(3) 0.5725(2) 0.0448(9) Uani 1 1 d . . . O14 O 0.6824(3) 0.2565(3) 0.7448(2) 0.0304(7) Uani 1 1 d . . . O31 O -0.6037(14) 0.0309(10) 0.0403(8) 0.260(8) Uani 1 1 d . A . O32 O -0.6754(7) 0.1455(5) 0.0345(7) 0.070(3) Uani 0.626(13) 1 d P A 1 O33 O -0.6812(12) 0.0793(10) 0.1513(10) 0.119(5) Uani 0.626(13) 1 d P A 1 O34 O -0.4992(6) 0.1805(12) 0.1391(11) 0.106(5) Uani 0.626(13) 1 d P A 1 O34A O -0.5406(12) 0.2290(9) 0.1970(8) 0.054(4) Uani 0.374(13) 1 d P A 2 O33A O -0.5989(12) 0.0576(9) 0.1804(7) 0.052(4) Uani 0.374(13) 1 d P A 2 O32A O -0.6956(9) 0.1469(10) 0.1075(14) 0.073(6) Uani 0.374(13) 1 d P A 2 Cl1 Cl 0.64896(9) 0.14668(9) 0.65985(8) 0.0302(3) Uani 1 1 d . . . Cl3 Cl -0.61195(12) 0.11459(11) 0.10846(10) 0.0456(3) Uani 1 1 d . . . Cu1 Cu 0.22281(4) 0.15349(4) 0.42245(4) 0.02512(16) Uani 1 1 d . . . Cu2 Cu 0.57025(4) 0.28319(4) 0.82812(4) 0.02668(16) Uani 1 1 d . . . N10 N 0.2106(5) 0.3016(4) 0.4958(3) 0.0631(16) Uani 1 1 d . . . C30 C 0.1991(9) 0.3771(7) 0.5427(5) 0.117(4) Uani 1 1 d . . . C31 C 0.1840(13) 0.4774(12) 0.6052(11) 0.175(5) Uani 1 1 d U . . H31A H 0.1714 0.4715 0.6618 0.263 Uiso 1 1 calc R . . H31B H 0.1179 0.4846 0.5669 0.263 Uiso 1 1 calc R . . H31C H 0.2530 0.5413 0.6274 0.263 Uiso 1 1 calc R . . O2 O 0.1848(3) 0.3609(3) 0.2783(4) 0.0653(12) Uani 1 1 d . . . C4 C 0.2263(4) 0.2778(4) 0.2750(4) 0.0444(13) Uani 1 1 d . B . O1 O 0.3310(6) 0.4593(6) 0.2594(5) 0.071(2) Uani 0.638(9) 1 d P B 3 C3 C 0.2495(9) 0.4553(7) 0.2799(7) 0.045(2) Uani 0.638(9) 1 d P B 3 C2 C 0.2017(12) 0.5428(11) 0.3058(10) 0.059(4) Uani 0.638(9) 1 d P B 3 H2 H 0.2256 0.5982 0.2874 0.071 Uiso 0.638(9) 1 calc PR B 3 C1 C 0.1302(11) 0.5491(11) 0.3515(9) 0.072(3) Uani 0.638(9) 1 d P B 3 H1A H 0.1040 0.4954 0.3713 0.086 Uiso 0.638(9) 1 calc PR B 3 H1B H 0.1045 0.6073 0.3649 0.086 Uiso 0.638(9) 1 calc PR B 3 O1A O 0.2521(9) 0.4882(9) 0.4160(8) 0.054(4) Uani 0.362(9) 1 d P B 4 C3A C 0.2041(11) 0.4533(10) 0.3225(10) 0.027(3) Uani 0.362(9) 1 d P B 4 C1A C 0.1438(15) 0.6052(14) 0.3339(15) 0.048(4) Uani 0.362(9) 1 d P B 4 H1A1 H 0.1812 0.6389 0.4027 0.058 Uiso 0.362(9) 1 calc PR B 4 H1A2 H 0.1053 0.6394 0.3040 0.058 Uiso 0.362(9) 1 calc PR B 4 C2A C 0.1454(19) 0.508(2) 0.2781(19) 0.055(6) Uani 0.362(9) 1 d P B 4 H2A H 0.1078 0.4743 0.2093 0.066 Uiso 0.362(9) 1 calc PR B 4 Cl2 Cl -0.10311(11) 0.27501(10) 0.37028(10) 0.0418(3) Uani 1 1 d . . . O22 O -0.2040(7) 0.2614(5) 0.2929(4) 0.129(3) Uani 1 1 d . C . O21 O -0.0146(5) 0.3598(6) 0.3728(7) 0.098(3) Uani 0.743(8) 1 d P C 5 O23 O -0.1275(8) 0.3035(8) 0.4548(6) 0.094(2) Uani 0.743(8) 1 d PU C 5 O24 O -0.0705(4) 0.1806(4) 0.3537(4) 0.0429(15) Uani 0.743(8) 1 d P C 5 O24A O -0.107(2) 0.234(2) 0.2715(18) 0.101(7) Uani 0.257(8) 1 d PU C 6 O21A O -0.0003(9) 0.3804(8) 0.4545(8) 0.017(3) Uani 0.257(8) 1 d PU C 6 O23A O -0.1866(10) 0.2466(10) 0.4185(8) 0.022(3) Uani 0.257(8) 1 d PU C 6 Cl4 Cl 0.23886(11) 0.32948(10) 0.81191(9) 0.0436(3) Uani 1 1 d . . . O41 O 0.1185(4) 0.3101(4) 0.7989(4) 0.0773(15) Uani 1 1 d . D . O42 O 0.2699(5) 0.2428(4) 0.8299(4) 0.0618(18) Uani 0.865(9) 1 d P D 7 O43 O 0.2568(4) 0.3258(5) 0.7250(3) 0.0604(19) Uani 0.865(9) 1 d P D 7 O44 O 0.3133(5) 0.4330(5) 0.8959(4) 0.0561(16) Uani 0.865(9) 1 d P D 7 O43A O 0.219(2) 0.236(2) 0.7529(19) 0.036(8) Uani 0.135(9) 1 d PU D 8 O44A O 0.275(2) 0.413(3) 0.762(2) 0.044(8) Uani 0.135(9) 1 d PU D 8 O42A O 0.276(3) 0.397(3) 0.902(3) 0.041(9) Uani 0.135(9) 1 d PU D 8 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 C5 0.025(2) 0.026(2) 0.034(2) 0.011(2) 0.0074(19) 0.0112(19) C6 0.036(3) 0.039(3) 0.035(3) 0.019(2) 0.009(2) 0.016(2) C7 0.030(3) 0.044(3) 0.029(2) 0.014(2) 0.004(2) 0.013(2) C8 0.025(2) 0.028(2) 0.030(2) 0.009(2) 0.0047(19) 0.0088(19) C9 0.024(2) 0.026(2) 0.025(2) 0.0055(19) 0.0064(18) 0.0141(19) C10 0.024(2) 0.024(2) 0.029(2) 0.0064(19) 0.0102(19) 0.0102(19) C11 0.027(2) 0.043(3) 0.037(3) 0.022(2) 0.007(2) 0.009(2) C12 0.023(2) 0.031(2) 0.027(2) 0.0105(19) 0.0125(18) 0.0162(19) C13 0.027(2) 0.029(2) 0.023(2) 0.0079(19) 0.0079(18) 0.019(2) C14 0.036(3) 0.025(2) 0.024(2) 0.0070(19) -0.0025(19) 0.013(2) C15 0.028(2) 0.036(3) 0.026(2) 0.013(2) 0.0152(19) 0.022(2) C16 0.026(2) 0.038(3) 0.031(2) 0.017(2) 0.0129(19) 0.017(2) C17 0.040(3) 0.070(4) 0.043(3) 0.039(3) 0.018(2) 0.014(3) C18 0.041(3) 0.045(3) 0.030(2) 0.022(2) 0.018(2) 0.027(2) C19 0.031(2) 0.040(3) 0.022(2) 0.014(2) 0.0108(19) 0.021(2) C20 0.048(3) 0.046(3) 0.028(2) 0.023(2) 0.012(2) 0.022(3) C21 0.043(3) 0.051(3) 0.026(2) 0.019(2) 0.007(2) 0.021(3) C22 0.041(3) 0.042(3) 0.025(2) 0.016(2) 0.013(2) 0.022(2) C23 0.029(2) 0.039(3) 0.024(2) 0.013(2) 0.0143(19) 0.022(2) C24 0.028(2) 0.043(3) 0.028(2) 0.016(2) 0.0089(19) 0.018(2) C25 0.036(3) 0.046(3) 0.033(2) 0.023(2) 0.019(2) 0.025(2) C26 0.037(3) 0.042(3) 0.029(2) 0.016(2) 0.009(2) 0.025(2) C27 0.040(3) 0.046(3) 0.043(3) 0.022(3) 0.011(2) 0.024(3) C28 0.036(3) 0.043(3) 0.042(3) 0.030(2) 0.009(2) 0.011(2) C29 0.0623(19) 0.0660(19) 0.0643(19) 0.0317(12) 0.0231(11) 0.0233(11) C32 0.038(3) 0.039(3) 0.029(2) 0.009(2) 0.000(2) 0.019(2) C33 0.075(4) 0.038(3) 0.059(4) 0.014(3) 0.017(3) 0.034(3) N1 0.0247(19) 0.0241(19) 0.0261(18) 0.0068(16) 0.0069(15) 0.0127(16) N2 0.0269(19) 0.031(2) 0.0241(18) 0.0098(16) 0.0092(16) 0.0192(17) N3 0.0224(19) 0.031(2) 0.0291(19) 0.0122(17) 0.0075(16) 0.0132(16) N4 0.0243(18) 0.030(2) 0.0230(18) 0.0087(16) 0.0079(15) 0.0181(16) N5 0.0295(19) 0.032(2) 0.0213(17) 0.0105(16) 0.0094(15) 0.0209(17) N6 0.030(2) 0.041(2) 0.0271(19) 0.0192(18) 0.0113(17) 0.0182(18) N7 0.0257(19) 0.039(2) 0.0238(18) 0.0129(17) 0.0093(16) 0.0196(18) N8 0.033(2) 0.040(2) 0.0230(18) 0.0175(17) 0.0153(16) 0.0259(19) N9 0.026(2) 0.028(2) 0.033(2) 0.0167(17) 0.0072(17) 0.0100(17) N11 0.040(2) 0.036(2) 0.027(2) 0.0047(18) -0.0011(17) 0.024(2) O3 0.0327(17) 0.0327(18) 0.0277(16) 0.0129(14) 0.0088(13) 0.0190(14) O4 0.036(2) 0.073(3) 0.072(3) 0.056(2) 0.0062(19) 0.0138(19) O11 0.043(2) 0.058(2) 0.042(2) 0.0143(18) 0.0236(17) 0.0289(18) O12 0.052(2) 0.0356(19) 0.049(2) 0.0249(17) 0.0280(17) 0.0248(17) O13 0.060(2) 0.049(2) 0.0251(17) 0.0149(16) 0.0085(16) 0.0297(19) O14 0.0318(17) 0.0338(18) 0.0257(15) 0.0097(14) 0.0126(13) 0.0169(14) O31 0.60(2) 0.283(12) 0.247(10) 0.221(10) 0.341(14) 0.383(16) O32 0.061(5) 0.039(4) 0.071(6) 0.028(4) -0.027(4) 0.005(3) O33 0.136(10) 0.145(10) 0.166(11) 0.115(9) 0.120(9) 0.061(8) O34 0.030(4) 0.178(12) 0.164(11) 0.144(11) 0.028(5) 0.030(5) O34A 0.050(8) 0.046(7) 0.044(6) 0.027(5) -0.007(5) -0.001(5) O33A 0.062(8) 0.054(7) 0.034(5) 0.028(5) 0.019(5) 0.000(6) O32A 0.034(6) 0.055(8) 0.113(14) 0.017(8) 0.026(7) 0.023(6) Cl1 0.0359(6) 0.0339(6) 0.0266(5) 0.0132(5) 0.0134(5) 0.0211(5) Cl3 0.0483(8) 0.0497(8) 0.0489(7) 0.0239(6) 0.0299(6) 0.0207(6) Cu1 0.0233(3) 0.0250(3) 0.0227(3) 0.0072(2) 0.0038(2) 0.0125(2) Cu2 0.0296(3) 0.0335(3) 0.0212(3) 0.0124(2) 0.0078(2) 0.0199(3) N10 0.092(4) 0.048(3) 0.029(2) 0.000(2) -0.011(2) 0.054(3) C30 0.208(10) 0.099(6) 0.028(3) 0.002(4) -0.011(4) 0.127(7) C31 0.176(5) 0.175(5) 0.175(5) 0.079(3) 0.063(2) 0.069(2) O2 0.045(2) 0.042(3) 0.097(3) 0.036(3) 0.005(2) 0.012(2) C4 0.037(3) 0.028(3) 0.063(3) 0.022(3) 0.008(3) 0.013(2) O1 0.050(4) 0.072(5) 0.067(5) 0.033(4) 0.014(4) -0.009(4) C3 0.043(5) 0.038(5) 0.043(5) 0.019(4) 0.008(5) 0.002(4) C2 0.054(8) 0.041(8) 0.068(8) 0.037(6) 0.002(7) -0.002(6) C1 0.077(8) 0.043(7) 0.059(8) 0.002(6) 0.019(6) 0.006(6) O1A 0.054(7) 0.053(7) 0.042(6) 0.015(5) 0.006(5) 0.020(5) C3A 0.026(7) 0.020(7) 0.026(7) 0.007(6) 0.006(6) 0.003(5) C1A 0.050(10) 0.033(10) 0.081(12) 0.034(9) 0.041(9) 0.018(8) C2A 0.034(12) 0.057(15) 0.068(15) 0.044(13) 0.008(11) -0.007(10) Cl2 0.0498(7) 0.0305(7) 0.0534(8) 0.0189(6) 0.0331(6) 0.0153(6) O22 0.202(7) 0.100(5) 0.079(4) 0.057(4) 0.004(4) 0.068(5) O21 0.054(4) 0.067(5) 0.166(9) 0.080(5) 0.001(4) 0.006(3) O23 0.094(3) 0.095(3) 0.093(3) 0.0426(14) 0.0352(13) 0.0371(13) O24 0.075(4) 0.026(2) 0.061(3) 0.026(2) 0.053(3) 0.035(2) O24A 0.101(7) 0.101(7) 0.101(7) 0.046(4) 0.038(3) 0.038(3) O21A 0.017(3) 0.017(3) 0.017(3) 0.0074(16) 0.0071(14) 0.0059(15) O23A 0.021(3) 0.022(3) 0.022(3) 0.0099(16) 0.0089(15) 0.0066(15) Cl4 0.0479(7) 0.0367(7) 0.0329(6) 0.0023(5) 0.0235(6) 0.0084(6) O41 0.054(3) 0.056(3) 0.086(3) -0.008(2) 0.050(2) 0.004(2) O42 0.105(4) 0.052(3) 0.076(4) 0.043(3) 0.065(3) 0.053(3) O43 0.062(3) 0.116(5) 0.037(2) 0.043(3) 0.034(2) 0.059(3) O44 0.051(3) 0.044(3) 0.045(3) -0.003(3) 0.005(3) 0.022(3) O43A 0.036(8) 0.036(8) 0.036(8) 0.016(4) 0.013(3) 0.014(3) O44A 0.044(8) 0.044(8) 0.044(8) 0.020(4) 0.016(3) 0.017(3) O42A 0.041(9) 0.041(9) 0.041(9) 0.019(4) 0.015(4) 0.016(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C5 N1 1.343(6) . ? C5 C6 1.402(6) . ? C5 C4 1.508(7) . ? C6 C7 1.365(7) . ? C6 H6 0.9300 . ? C7 C8 1.391(7) . ? C7 H7 0.9300 . ? C8 C9 1.383(6) . ? C8 H8 0.9300 . ? C9 N1 1.367(6) . ? C9 C10 1.460(6) . ? C10 N2 1.287(6) . ? C10 H10 0.9300 . ? C11 N3 1.453(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.359(6) . ? C12 C16 1.375(6) . ? C12 N3 1.379(6) . ? C13 N5 1.343(5) . ? C13 N4 1.349(5) . ? C13 C14 1.481(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N6 1.366(5) . ? C15 N5 1.372(6) . ? C15 C16 1.381(6) . ? C16 H16 0.9300 . ? C17 N6 1.448(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N7 1.287(6) . ? C18 C19 1.449(7) . ? C18 H18 0.9300 . ? C19 N8 1.369(6) . ? C19 C20 1.389(6) . ? C20 C21 1.383(7) . ? C20 H20 0.9300 . ? C21 C22 1.382(7) . ? C21 H21 0.9300 . ? C22 C23 1.395(6) . ? C22 H22 0.9300 . ? C23 N8 1.340(6) . ? C23 C24 1.504(6) . ? C24 O3 1.432(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.200(5) . ? C25 O3 1.351(6) . ? C25 C26 1.466(7) . ? C26 C27 1.305(7) . ? C26 H26 0.9300 . ? C27 H27A 0.9300 . ? C27 H27B 0.9300 . ? C28 N9 1.131(6) . ? C28 C29 1.461(8) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C32 N11 1.131(6) . ? C32 C33 1.446(7) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? N1 Cu1 2.020(3) . ? N2 N3 1.362(5) . ? N2 Cu1 1.963(4) . ? N4 Cu1 2.023(3) . ? N5 Cu2 2.019(4) . ? N6 N7 1.361(5) . ? N7 Cu2 1.940(4) . ? N8 Cu2 2.048(4) . ? N9 Cu1 2.024(4) . ? N11 Cu2 1.970(4) . ? O11 Cl1 1.428(3) . ? O12 Cl1 1.431(3) . ? O13 Cl1 1.429(3) . ? O14 Cl1 1.485(3) . ? O14 Cu2 2.159(3) . ? O31 Cl3 1.312(7) . ? O32 Cl3 1.505(6) . ? O33 Cl3 1.329(8) . ? O34 Cl3 1.348(7) . ? O34A Cl3 1.530(11) . ? O33A Cl3 1.599(10) . ? O32A Cl3 1.260(10) . ? Cu1 N10 2.041(4) . ? N10 C30 1.115(7) . ? C30 C31 1.480(15) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? O2 C3A 1.149(12) . ? O2 C3 1.360(10) . ? O2 C4 1.388(6) . ? O1 C3 1.151(13) . ? C3 C2 1.477(17) . ? C2 C1 1.283(19) . ? C2 H2 0.9300 . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? O1A C3A 1.274(16) . ? C3A C2A 1.43(3) . ? C1A C2A 1.34(3) . ? C1A H1A1 0.9300 . ? C1A H1A2 0.9300 . ? C2A H2A 0.9300 . ? Cl2 O23 1.361(8) . ? Cl2 O21 1.397(6) . ? Cl2 O24A 1.41(2) . ? Cl2 O24 1.444(4) . ? Cl2 O22 1.451(6) . ? Cl2 O23A 1.494(11) . ? Cl2 O21A 1.546(10) . ? O22 O24A 1.46(2) . ? Cl4 O43A 1.21(2) . ? Cl4 O42A 1.25(4) . ? Cl4 O43 1.406(4) . ? Cl4 O44 1.425(5) . ? Cl4 O41 1.437(4) . ? Cl4 O42 1.470(4) . ? Cl4 O44A 1.66(3) . ? 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 C5 C6 120.7(4) . . ? N1 C5 C4 118.6(4) . . ? C6 C5 C4 120.7(4) . . ? C7 C6 C5 120.4(4) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C8 119.3(4) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 118.2(4) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? N1 C9 C8 122.7(4) . . ? N1 C9 C10 115.2(4) . . ? C8 C9 C10 122.1(4) . . ? N2 C10 C9 114.5(4) . . ? N2 C10 H10 122.8 . . ? C9 C10 H10 122.8 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C16 121.9(4) . . ? N4 C12 N3 115.9(4) . . ? C16 C12 N3 122.1(4) . . ? N5 C13 N4 123.0(4) . . ? N5 C13 C14 117.6(4) . . ? N4 C13 C14 119.3(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N6 C15 N5 115.7(4) . . ? N6 C15 C16 123.0(4) . . ? N5 C15 C16 121.3(4) . . ? C12 C16 C15 117.3(4) . . ? C12 C16 H16 121.4 . . ? C15 C16 H16 121.4 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 114.1(4) . . ? N7 C18 H18 122.9 . . ? C19 C18 H18 122.9 . . ? N8 C19 C20 121.9(4) . . ? N8 C19 C18 116.6(4) . . ? C20 C19 C18 121.6(4) . . ? C21 C20 C19 118.5(5) . . ? C21 C20 H20 120.8 . . ? C19 C20 H20 120.8 . . ? C22 C21 C20 119.7(4) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 119.5(5) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? N8 C23 C22 121.3(4) . . ? N8 C23 C24 117.0(4) . . ? C22 C23 C24 121.7(4) . . ? O3 C24 C23 108.6(3) . . ? O3 C24 H24A 110.0 . . ? C23 C24 H24A 110.0 . . ? O3 C24 H24B 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? O4 C25 O3 122.2(5) . . ? O4 C25 C26 127.1(5) . . ? O3 C25 C26 110.7(4) . . ? C27 C26 C25 123.3(4) . . ? C27 C26 H26 118.3 . . ? C25 C26 H26 118.3 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? N9 C28 C29 177.9(6) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N11 C32 C33 178.9(6) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C5 N1 C9 118.6(4) . . ? C5 N1 Cu1 129.3(3) . . ? C9 N1 Cu1 112.0(3) . . ? C10 N2 N3 124.8(4) . . ? C10 N2 Cu1 117.5(3) . . ? N3 N2 Cu1 117.6(3) . . ? N2 N3 C12 113.7(4) . . ? N2 N3 C11 119.8(4) . . ? C12 N3 C11 125.8(4) . . ? C13 N4 C12 118.2(4) . . ? C13 N4 Cu1 127.4(3) . . ? C12 N4 Cu1 114.4(3) . . ? C13 N5 C15 118.2(4) . . ? C13 N5 Cu2 128.4(3) . . ? C15 N5 Cu2 113.4(3) . . ? N7 N6 C15 114.4(4) . . ? N7 N6 C17 119.9(4) . . ? C15 N6 C17 125.5(4) . . ? C18 N7 N6 124.4(4) . . ? C18 N7 Cu2 118.2(3) . . ? N6 N7 Cu2 117.3(3) . . ? C23 N8 C19 119.1(4) . . ? C23 N8 Cu2 130.9(3) . . ? C19 N8 Cu2 110.0(3) . . ? C28 N9 Cu1 168.8(4) . . ? C32 N11 Cu2 171.2(5) . . ? C25 O3 C24 117.5(3) . . ? Cl1 O14 Cu2 120.06(18) . . ? O11 Cl1 O13 111.4(2) . . ? O11 Cl1 O12 111.0(2) . . ? O13 Cl1 O12 110.8(2) . . ? O11 Cl1 O14 107.5(2) . . ? O13 Cl1 O14 108.32(19) . . ? O12 Cl1 O14 107.66(19) . . ? O32A Cl3 O31 130.0(10) . . ? O32A Cl3 O33 64.4(9) . . ? O31 Cl3 O33 110.5(8) . . ? O32A Cl3 O34 125.2(8) . . ? O31 Cl3 O34 93.9(10) . . ? O33 Cl3 O34 135.8(9) . . ? O32A Cl3 O32 51.2(8) . . ? O31 Cl3 O32 93.9(6) . . ? O33 Cl3 O32 110.5(7) . . ? O34 Cl3 O32 103.5(5) . . ? O32A Cl3 O34A 83.8(9) . . ? O31 Cl3 O34A 143.4(10) . . ? O33 Cl3 O34A 95.7(8) . . ? O34 Cl3 O34A 50.1(6) . . ? O32 Cl3 O34A 100.4(5) . . ? O32A Cl3 O33A 110.4(10) . . ? O31 Cl3 O33A 89.1(6) . . ? O33 Cl3 O33A 47.2(6) . . ? O34 Cl3 O33A 99.5(6) . . ? O32 Cl3 O33A 156.4(6) . . ? O34A Cl3 O33A 90.7(5) . . ? N2 Cu1 N1 80.64(15) . . ? N2 Cu1 N4 78.43(15) . . ? N1 Cu1 N4 159.05(15) . . ? N2 Cu1 N9 126.50(14) . . ? N1 Cu1 N9 96.83(14) . . ? N4 Cu1 N9 94.71(14) . . ? N2 Cu1 N10 121.8(2) . . ? N1 Cu1 N10 97.15(15) . . ? N4 Cu1 N10 94.77(16) . . ? N9 Cu1 N10 111.6(2) . . ? N7 Cu2 N11 135.84(17) . . ? N7 Cu2 N5 79.17(15) . . ? N11 Cu2 N5 99.42(14) . . ? N7 Cu2 N8 80.88(15) . . ? N11 Cu2 N8 96.72(15) . . ? N5 Cu2 N8 159.87(15) . . ? N7 Cu2 O14 114.00(13) . . ? N11 Cu2 O14 110.15(15) . . ? N5 Cu2 O14 93.33(13) . . ? N8 Cu2 O14 92.33(13) . . ? C30 N10 Cu1 171.6(7) . . ? N10 C30 C31 179.8(10) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C3A O2 C3 45.0(7) . . ? C3A O2 C4 143.9(7) . . ? C3 O2 C4 122.2(6) . . ? O2 C4 C5 107.6(4) . . ? O1 C3 O2 119.4(9) . . ? O1 C3 C2 126.9(10) . . ? O2 C3 C2 113.7(10) . . ? C1 C2 C3 125.7(13) . . ? C1 C2 H2 117.1 . . ? C3 C2 H2 117.1 . . ? C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? O2 C3A O1A 112.1(12) . . ? O2 C3A C2A 120.4(15) . . ? O1A C3A C2A 124.5(16) . . ? C2A C1A H1A1 120.0 . . ? C2A C1A H1A2 120.0 . . ? H1A1 C1A H1A2 120.0 . . ? C1A C2A C3A 121(2) . . ? C1A C2A H2A 119.5 . . ? C3A C2A H2A 119.5 . . ? O23 Cl2 O21 113.9(6) . . ? O23 Cl2 O24A 166.2(11) . . ? O21 Cl2 O24A 76.4(11) . . ? O23 Cl2 O24 108.4(4) . . ? O21 Cl2 O24 109.4(4) . . ? O24A Cl2 O24 74.7(11) . . ? O23 Cl2 O22 106.4(5) . . ? O21 Cl2 O22 101.8(4) . . ? O24A Cl2 O22 61.3(10) . . ? O24 Cl2 O22 117.0(3) . . ? O23 Cl2 O23A 33.3(5) . . ? O21 Cl2 O23A 145.5(6) . . ? O24A Cl2 O23A 134.2(11) . . ? O24 Cl2 O23A 96.3(5) . . ? O22 Cl2 O23A 85.7(5) . . ? O23 Cl2 O21A 71.4(5) . . ? O21 Cl2 O21A 45.6(5) . . ? O24A Cl2 O21A 120.8(11) . . ? O24 Cl2 O21A 109.5(4) . . ? O22 Cl2 O21A 130.9(5) . . ? O23A Cl2 O21A 104.7(6) . . ? Cl2 O22 O24A 58.0(10) . . ? Cl2 O24A O22 60.7(11) . . ? O43A Cl4 O42A 145(2) . . ? O43A Cl4 O43 68.5(12) . . ? O42A Cl4 O43 138.1(16) . . ? O43A Cl4 O44 152.3(12) . . ? O42A Cl4 O44 27.3(14) . . ? O43 Cl4 O44 110.9(4) . . ? O43A Cl4 O41 94.8(11) . . ? O42A Cl4 O41 93.7(17) . . ? O43 Cl4 O41 109.9(3) . . ? O44 Cl4 O41 110.5(3) . . ? O43A Cl4 O42 50.7(12) . . ? O42A Cl4 O42 95.0(17) . . ? O43 Cl4 O42 107.9(3) . . ? O44 Cl4 O42 107.6(3) . . ? O41 Cl4 O42 110.0(3) . . ? O43A Cl4 O44A 108.6(16) . . ? O42A Cl4 O44A 101.4(18) . . ? O43 Cl4 O44A 40.1(10) . . ? O44 Cl4 O44A 76.3(11) . . ? O41 Cl4 O44A 105.3(10) . . ? O42 Cl4 O44A 139.8(11) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.698 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.098 #===END data_Complex_7(djh869) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H37 Ag2 F3 N11 O7 S, C F3 O3 S' _chemical_formula_sum 'C35 H37 Ag2 F6 N11 O10 S2' _chemical_formula_weight 1165.64 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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 11.9718(4) _cell_length_b 12.9367(5) _cell_length_c 15.4355(6) _cell_angle_alpha 84.843(2) _cell_angle_beta 68.834(2) _cell_angle_gamma 79.247(2) _cell_volume 2189.50(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9971 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 29.53 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33806 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 30.37 _reflns_number_total 12714 _reflns_number_gt 10252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^ > 2\s(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^)+(0.0476P)^2^+0.7955P] 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 12714 _refine_ls_number_parameters 601 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 C1 C -0.3267(3) -0.5216(3) 0.6229(2) 0.0381(7) Uani 1 1 d . . . H1A H -0.3141 -0.4704 0.6553 0.046 Uiso 1 1 calc R . . H1B H -0.3266 -0.5904 0.6462 0.046 Uiso 1 1 calc R . . C2 C -0.3449(3) -0.4964(2) 0.5431(2) 0.0330(6) Uani 1 1 d . . . H2 H -0.3575 -0.5479 0.5109 0.040 Uiso 1 1 calc R . . C3 C -0.3453(2) -0.3871(2) 0.5050(2) 0.0300(6) Uani 1 1 d . . . C4 C -0.3268(2) -0.2794(2) 0.3692(2) 0.0268(6) Uani 1 1 d . . . H4A H -0.2571 -0.2524 0.3704 0.032 Uiso 1 1 calc R . . H4B H -0.3997 -0.2301 0.3999 0.032 Uiso 1 1 calc R . . C5 C -0.3154(2) -0.29474(19) 0.2712(2) 0.0230(5) Uani 1 1 d . . . C6 C -0.3963(2) -0.3474(2) 0.2532(2) 0.0261(6) Uani 1 1 d . . . H6 H -0.4607 -0.3695 0.3017 0.031 Uiso 1 1 calc R . . C7 C -0.3789(2) -0.3660(2) 0.1625(2) 0.0267(6) Uani 1 1 d . . . H7 H -0.4315 -0.4012 0.1490 0.032 Uiso 1 1 calc R . . C8 C -0.2826(2) -0.33201(19) 0.0915(2) 0.0245(5) Uani 1 1 d . . . H8 H -0.2680 -0.3453 0.0298 0.029 Uiso 1 1 calc R . . C9 C -0.2078(2) -0.27719(18) 0.11484(19) 0.0219(5) Uani 1 1 d . . . C10 C -0.1049(2) -0.24166(19) 0.03945(19) 0.0221(5) Uani 1 1 d . . . H10 H -0.0859 -0.2613 -0.0214 0.027 Uiso 1 1 calc R . . C11 C 0.0907(3) -0.1856(2) -0.10528(19) 0.0290(6) Uani 1 1 d . . . H11A H 0.1299 -0.2578 -0.1087 0.044 Uiso 1 1 calc R . . H11B H 0.1458 -0.1431 -0.1473 0.044 Uiso 1 1 calc R . . H11C H 0.0199 -0.1798 -0.1221 0.044 Uiso 1 1 calc R . . C12 C 0.1222(2) -0.08980(18) 0.01528(18) 0.0191(5) Uani 1 1 d . . . C13 C 0.2275(2) -0.06064(19) -0.04911(18) 0.0201(5) Uani 1 1 d . . . H13 H 0.2574 -0.0827 -0.1102 0.024 Uiso 1 1 calc R . . C14 C 0.2865(2) 0.00335(18) -0.01809(17) 0.0177(5) Uani 1 1 d . . . C15 C 0.1449(2) -0.00184(19) 0.12818(18) 0.0213(5) Uani 1 1 d . . . C16 C 0.1020(3) 0.0269(2) 0.22862(19) 0.0291(6) Uani 1 1 d . . . H16A H 0.1578 -0.0107 0.2567 0.044 Uiso 1 1 calc R . . H16B H 0.0229 0.0085 0.2606 0.044 Uiso 1 1 calc R . . H16C H 0.0978 0.1012 0.2327 0.044 Uiso 1 1 calc R . . C17 C 0.4393(2) 0.0144(2) -0.17711(18) 0.0250(5) Uani 1 1 d . . . H17A H 0.4088 0.0717 -0.2109 0.037 Uiso 1 1 calc R . . H17B H 0.4146 -0.0490 -0.1863 0.037 Uiso 1 1 calc R . . H17C H 0.5263 0.0053 -0.1991 0.037 Uiso 1 1 calc R . . C18 C 0.5298(2) 0.14685(19) -0.09832(18) 0.0200(5) Uani 1 1 d . . . H18 H 0.5661 0.1287 -0.1605 0.024 Uiso 1 1 calc R . . C19 C 0.5763(2) 0.22306(19) -0.06027(18) 0.0207(5) Uani 1 1 d . . . C20 C 0.6824(2) 0.2594(2) -0.1164(2) 0.0267(6) Uani 1 1 d . . . H20 H 0.7240 0.2351 -0.1764 0.032 Uiso 1 1 calc R . . C21 C 0.7246(3) 0.3327(2) -0.0810(2) 0.0313(6) Uani 1 1 d . . . H21 H 0.7952 0.3583 -0.1169 0.038 Uiso 1 1 calc R . . C22 C 0.6604(3) 0.3671(2) 0.0084(2) 0.0306(6) Uani 1 1 d . . . H22 H 0.6873 0.4160 0.0335 0.037 Uiso 1 1 calc R . . C23 C 0.5544(2) 0.3274(2) 0.0605(2) 0.0237(5) Uani 1 1 d . . . C24 C 0.4763(2) 0.3649(2) 0.1559(2) 0.0272(6) Uani 1 1 d . . . H24A H 0.4139 0.4224 0.1509 0.033 Uiso 1 1 calc R . . H24B H 0.4362 0.3082 0.1915 0.033 Uiso 1 1 calc R . . C25 C 0.6104(2) 0.3220(2) 0.23856(19) 0.0236(5) Uani 1 1 d . . . C26 C 0.6708(3) 0.3653(2) 0.2923(2) 0.0292(6) Uani 1 1 d . . . H26 H 0.6558 0.4374 0.3017 0.035 Uiso 1 1 calc R . . C27 C 0.7455(3) 0.3031(2) 0.3270(2) 0.0320(6) Uani 1 1 d . . . H27A H 0.7609 0.2310 0.3179 0.038 Uiso 1 1 calc R . . H27B H 0.7829 0.3313 0.3606 0.038 Uiso 1 1 calc R . . C28 C 0.0020(3) 0.4761(2) 0.1705(3) 0.0429(9) Uani 1 1 d . . . C29 C 0.1657(2) -0.1449(2) 0.47648(19) 0.0283(6) Uani 1 1 d . . . C30 C -0.3361(3) 0.0298(2) 0.35296(19) 0.0259(5) Uani 1 1 d . . . C31 C -0.4506(3) 0.0913(2) 0.4076(2) 0.0308(6) Uani 1 1 d . . . H31A H -0.4659 0.1554 0.3743 0.046 Uiso 1 1 calc R . . H31B H -0.4466 0.1076 0.4658 0.046 Uiso 1 1 calc R . . H31C H -0.5149 0.0517 0.4190 0.046 Uiso 1 1 calc R . . C32 C 0.0083(3) -0.3156(2) 0.3546(2) 0.0344(7) Uani 1 1 d . . . C33 C 0.0103(3) -0.4087(3) 0.4165(3) 0.0466(8) Uani 1 1 d . . . H33A H -0.0708 -0.4234 0.4466 0.070 Uiso 1 1 calc R . . H33B H 0.0421 -0.3954 0.4625 0.070 Uiso 1 1 calc R . . H33C H 0.0607 -0.4680 0.3808 0.070 Uiso 1 1 calc R . . C34 C 0.2536(2) 0.1608(2) 0.3429(2) 0.0265(6) Uani 1 1 d . . . C35 C 0.1831(3) 0.1611(3) 0.4419(2) 0.0427(8) Uani 1 1 d . . . H35A H 0.1125 0.2148 0.4541 0.064 Uiso 1 1 calc R . . H35B H 0.2318 0.1749 0.4757 0.064 Uiso 1 1 calc R . . H35C H 0.1583 0.0938 0.4612 0.064 Uiso 1 1 calc R . . N1 N -0.22368(18) -0.25843(16) 0.20327(16) 0.0218(4) Uani 1 1 d . . . N2 N -0.04109(19) -0.18295(16) 0.05853(15) 0.0206(4) Uani 1 1 d . . . N3 N 0.05502(19) -0.14970(16) -0.01114(15) 0.0217(4) Uani 1 1 d . . . N4 N 0.08025(19) -0.06170(16) 0.10491(15) 0.0217(4) Uani 1 1 d . . . N5 N 0.24459(19) 0.03386(16) 0.07109(15) 0.0203(4) Uani 1 1 d . . . N6 N 0.39091(18) 0.03752(16) -0.07852(14) 0.0184(4) Uani 1 1 d . . . N7 N 0.43867(18) 0.10586(15) -0.04455(15) 0.0182(4) Uani 1 1 d . . . N8 N 0.51260(19) 0.25623(16) 0.02700(16) 0.0214(4) Uani 1 1 d . . . N9 N -0.2470(2) -0.01866(19) 0.30961(18) 0.0329(5) Uani 1 1 d . . . N10 N 0.0022(2) -0.2437(2) 0.30858(19) 0.0385(6) Uani 1 1 d . . . N11 N 0.3062(2) 0.16025(19) 0.26580(18) 0.0310(5) Uani 1 1 d . . . O1 O -0.3525(2) -0.31068(18) 0.54768(17) 0.0430(5) Uani 1 1 d . . . O2 O -0.33312(18) -0.38271(15) 0.41521(14) 0.0307(4) Uani 1 1 d . . . O3 O 0.54406(17) 0.40017(14) 0.20509(14) 0.0257(4) Uani 1 1 d . . . O4 O 0.61879(17) 0.23064(14) 0.22387(14) 0.0281(4) Uani 1 1 d . . . O11 O 0.1548(2) 0.30751(19) 0.14253(18) 0.0534(7) Uani 1 1 d . . . O12 O 0.1858(2) 0.44490(19) 0.2223(2) 0.0616(8) Uani 1 1 d . . . O13 O 0.0260(2) 0.3453(3) 0.3001(2) 0.0720(9) Uani 1 1 d . . . O21 O 0.3209(2) -0.19906(19) 0.31620(15) 0.0415(5) Uani 1 1 d . . . O22 O 0.3616(2) -0.06602(18) 0.39672(17) 0.0435(6) Uani 1 1 d . . . O23 O 0.37973(17) -0.24785(16) 0.45150(15) 0.0326(5) Uani 1 1 d . . . F11 F -0.07564(17) 0.43233(15) 0.15010(15) 0.0470(5) Uani 1 1 d . . . F12 F 0.0618(3) 0.5241(2) 0.0939(3) 0.1060(14) Uani 1 1 d . . . F13 F -0.0613(3) 0.5479(3) 0.2316(3) 0.1401(18) Uani 1 1 d . . . F21 F 0.14998(16) -0.10458(15) 0.55673(12) 0.0402(4) Uani 1 1 d . . . F22 F 0.12127(16) -0.23552(15) 0.49494(14) 0.0422(5) Uani 1 1 d . . . F23 F 0.09756(15) -0.07895(15) 0.43652(13) 0.0394(4) Uani 1 1 d . . . S1 S 0.10363(6) 0.38221(5) 0.21473(5) 0.02790(15) Uani 1 1 d . . . S2 S 0.32528(6) -0.16694(6) 0.40138(5) 0.02619(14) Uani 1 1 d . . . Ag1 Ag -0.089976(18) -0.134029(16) 0.215963(14) 0.02656(6) Uani 1 1 d . . . Ag2 Ag 0.338811(17) 0.166230(15) 0.111447(14) 0.02234(6) 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 C1 0.0324(15) 0.0437(18) 0.0339(17) -0.0003(14) -0.0044(13) -0.0105(13) C2 0.0346(15) 0.0343(15) 0.0269(15) -0.0014(12) -0.0041(12) -0.0112(12) C3 0.0227(13) 0.0339(15) 0.0316(16) -0.0059(12) -0.0051(12) -0.0068(11) C4 0.0227(12) 0.0229(12) 0.0327(15) -0.0022(11) -0.0055(11) -0.0069(10) C5 0.0190(11) 0.0173(11) 0.0315(14) -0.0006(10) -0.0086(11) -0.0009(9) C6 0.0191(11) 0.0210(12) 0.0380(16) 0.0026(11) -0.0096(11) -0.0049(9) C7 0.0235(12) 0.0187(11) 0.0436(17) 0.0005(11) -0.0180(12) -0.0056(10) C8 0.0262(12) 0.0185(11) 0.0329(15) -0.0005(10) -0.0153(12) -0.0040(10) C9 0.0190(11) 0.0157(11) 0.0324(14) -0.0007(10) -0.0112(11) -0.0022(9) C10 0.0239(12) 0.0214(11) 0.0233(13) -0.0021(10) -0.0104(10) -0.0045(10) C11 0.0294(14) 0.0364(15) 0.0237(14) -0.0070(12) -0.0069(11) -0.0131(12) C12 0.0209(11) 0.0163(10) 0.0221(12) -0.0003(9) -0.0099(10) -0.0035(9) C13 0.0225(11) 0.0200(11) 0.0194(12) -0.0028(9) -0.0077(10) -0.0058(9) C14 0.0207(11) 0.0145(10) 0.0185(12) 0.0014(9) -0.0082(9) -0.0022(9) C15 0.0251(12) 0.0183(11) 0.0213(13) 0.0002(10) -0.0085(10) -0.0053(9) C16 0.0332(14) 0.0360(15) 0.0199(13) -0.0032(11) -0.0057(11) -0.0162(12) C17 0.0258(12) 0.0299(13) 0.0192(12) -0.0055(10) -0.0048(10) -0.0088(11) C18 0.0228(11) 0.0193(11) 0.0198(12) -0.0002(9) -0.0102(10) -0.0029(9) C19 0.0210(11) 0.0199(11) 0.0229(13) 0.0004(10) -0.0099(10) -0.0037(9) C20 0.0303(13) 0.0285(13) 0.0239(14) 0.0028(11) -0.0096(11) -0.0126(11) C21 0.0313(14) 0.0352(15) 0.0307(15) 0.0016(12) -0.0095(12) -0.0178(12) C22 0.0338(15) 0.0301(14) 0.0332(16) -0.0033(12) -0.0124(13) -0.0158(12) C23 0.0250(12) 0.0216(12) 0.0274(14) -0.0011(10) -0.0118(11) -0.0050(10) C24 0.0245(13) 0.0294(13) 0.0307(15) -0.0097(11) -0.0107(11) -0.0054(11) C25 0.0238(12) 0.0234(12) 0.0216(13) -0.0011(10) -0.0037(10) -0.0078(10) C26 0.0331(14) 0.0271(13) 0.0318(15) -0.0030(12) -0.0141(12) -0.0095(11) C27 0.0338(15) 0.0369(15) 0.0273(15) 0.0025(12) -0.0108(12) -0.0123(12) C28 0.0370(16) 0.0221(14) 0.080(3) -0.0085(16) -0.0341(18) -0.0008(12) C29 0.0270(13) 0.0344(15) 0.0221(14) 0.0004(11) -0.0064(11) -0.0064(11) C30 0.0363(15) 0.0243(12) 0.0219(13) -0.0011(11) -0.0130(12) -0.0107(11) C31 0.0312(14) 0.0314(14) 0.0273(15) 0.0010(12) -0.0063(12) -0.0077(12) C32 0.0319(15) 0.0380(16) 0.0350(17) -0.0056(14) -0.0146(13) -0.0017(13) C33 0.051(2) 0.0361(17) 0.054(2) 0.0024(16) -0.0245(18) 0.0001(15) C34 0.0208(12) 0.0268(13) 0.0341(16) -0.0086(12) -0.0099(11) -0.0052(10) C35 0.0373(16) 0.0457(19) 0.0344(18) -0.0114(15) 0.0075(14) -0.0172(14) N1 0.0178(10) 0.0176(9) 0.0299(12) -0.0005(9) -0.0085(9) -0.0024(8) N2 0.0204(10) 0.0176(9) 0.0243(11) 0.0008(8) -0.0079(9) -0.0047(8) N3 0.0237(10) 0.0222(10) 0.0216(11) -0.0022(9) -0.0075(9) -0.0095(8) N4 0.0238(10) 0.0209(10) 0.0214(11) -0.0003(8) -0.0078(9) -0.0067(8) N5 0.0247(10) 0.0178(9) 0.0200(11) -0.0014(8) -0.0084(9) -0.0057(8) N6 0.0202(10) 0.0190(9) 0.0182(10) -0.0009(8) -0.0076(8) -0.0063(8) N7 0.0210(10) 0.0142(9) 0.0231(11) 0.0007(8) -0.0117(8) -0.0042(7) N8 0.0201(10) 0.0198(10) 0.0261(12) -0.0011(9) -0.0093(9) -0.0046(8) N9 0.0353(13) 0.0330(13) 0.0335(14) -0.0088(11) -0.0147(11) -0.0041(11) N10 0.0400(14) 0.0449(15) 0.0359(15) 0.0046(12) -0.0196(12) -0.0095(12) N11 0.0342(13) 0.0330(13) 0.0270(13) -0.0040(10) -0.0144(11) 0.0003(10) O1 0.0567(15) 0.0364(12) 0.0397(13) -0.0081(10) -0.0187(12) -0.0100(11) O2 0.0349(11) 0.0273(10) 0.0274(11) -0.0011(8) -0.0071(9) -0.0069(8) O3 0.0301(10) 0.0213(9) 0.0301(10) -0.0049(8) -0.0145(8) -0.0051(7) O4 0.0319(10) 0.0209(9) 0.0304(11) -0.0038(8) -0.0077(9) -0.0069(8) O11 0.0590(15) 0.0518(14) 0.0501(16) -0.0265(12) -0.0335(13) 0.0299(12) O12 0.0506(15) 0.0432(14) 0.116(3) -0.0045(15) -0.0585(17) -0.0079(12) O13 0.0352(13) 0.123(3) 0.0492(17) 0.0269(18) -0.0105(12) -0.0149(15) O21 0.0363(11) 0.0621(15) 0.0237(11) -0.0085(10) -0.0086(9) -0.0025(11) O22 0.0411(12) 0.0417(13) 0.0473(15) 0.0091(11) -0.0115(11) -0.0194(10) O23 0.0252(9) 0.0382(11) 0.0313(11) 0.0018(9) -0.0075(8) -0.0041(8) F11 0.0366(10) 0.0462(11) 0.0719(15) 0.0063(10) -0.0341(10) -0.0135(8) F12 0.0739(17) 0.0893(19) 0.186(4) 0.097(2) -0.088(2) -0.0524(16) F13 0.153(3) 0.100(2) 0.211(4) -0.117(3) -0.149(3) 0.101(2) F21 0.0386(10) 0.0540(11) 0.0221(9) -0.0104(8) -0.0064(8) 0.0023(8) F22 0.0291(9) 0.0458(11) 0.0510(12) 0.0087(9) -0.0099(8) -0.0181(8) F23 0.0302(9) 0.0478(10) 0.0373(10) 0.0022(8) -0.0135(8) 0.0020(8) S1 0.0213(3) 0.0249(3) 0.0385(4) -0.0066(3) -0.0126(3) 0.0006(2) S2 0.0221(3) 0.0339(3) 0.0212(3) -0.0001(3) -0.0048(3) -0.0075(3) Ag1 0.02662(11) 0.03104(11) 0.02258(11) -0.00142(8) -0.00642(8) -0.01037(8) Ag2 0.02380(10) 0.02405(10) 0.02044(10) -0.00269(7) -0.00810(8) -0.00537(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.328(4) . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? C2 C3 1.483(4) . ? C2 H2 0.9300 . ? C3 O1 1.209(3) . ? C3 O2 1.337(4) . ? C4 O2 1.457(3) . ? C4 C5 1.498(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.341(3) . ? C5 C6 1.397(4) . ? C6 C7 1.376(4) . ? C6 H6 0.9300 . ? C7 C8 1.383(4) . ? C7 H7 0.9300 . ? C8 C9 1.396(4) . ? C8 H8 0.9300 . ? C9 N1 1.347(3) . ? C9 C10 1.471(4) . ? C10 N2 1.291(3) . ? C10 H10 0.9300 . ? C11 N3 1.452(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.349(3) . ? C12 C13 1.388(3) . ? C12 N3 1.392(3) . ? C13 C14 1.395(3) . ? C13 H13 0.9300 . ? C14 N5 1.352(3) . ? C14 N6 1.385(3) . ? C15 N5 1.337(3) . ? C15 N4 1.342(3) . ? C15 C16 1.504(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N6 1.456(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N7 1.282(3) . ? C18 C19 1.474(3) . ? C18 H18 0.9300 . ? C19 N8 1.349(3) . ? C19 C20 1.392(4) . ? C20 C21 1.388(4) . ? C20 H20 0.9300 . ? C21 C22 1.381(4) . ? C21 H21 0.9300 . ? C22 C23 1.397(4) . ? C22 H22 0.9300 . ? C23 N8 1.346(3) . ? C23 C24 1.497(4) . ? C24 O3 1.446(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.202(3) . ? C25 O3 1.351(3) . ? C25 C26 1.481(4) . ? C26 C27 1.316(4) . ? C26 H26 0.9300 . ? C27 H27A 0.9300 . ? C27 H27B 0.9300 . ? C28 F13 1.306(4) . ? C28 F12 1.312(5) . ? C28 F11 1.313(3) . ? C28 S1 1.822(3) . ? C29 F21 1.324(3) . ? C29 F23 1.335(3) . ? C29 F22 1.342(3) . ? C29 S2 1.825(3) . ? C30 N9 1.135(4) . ? C30 C31 1.450(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N10 1.126(4) . ? C32 C33 1.469(4) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 N11 1.127(4) . ? C34 C35 1.455(4) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? N1 Ag1 2.537(2) . ? N2 N3 1.369(3) . ? N2 Ag1 2.400(2) . ? N4 Ag1 2.422(2) . ? N5 Ag2 2.452(2) . ? N6 N7 1.368(3) . ? N7 Ag2 2.397(2) . ? N8 Ag2 2.461(2) . ? N9 Ag1 2.287(3) . ? N10 Ag1 2.338(3) . ? N11 Ag2 2.267(2) . ? O11 S1 1.425(2) . ? O11 Ag2 2.513(2) . ? O12 S1 1.427(2) . ? O13 S1 1.412(3) . ? O21 S2 1.435(2) . ? O22 S2 1.439(2) . ? O23 S2 1.443(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 120.6(3) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? O1 C3 O2 123.2(3) . . ? O1 C3 C2 125.3(3) . . ? O2 C3 C2 111.4(2) . . ? O2 C4 C5 106.1(2) . . ? O2 C4 H4A 110.5 . . ? C5 C4 H4A 110.5 . . ? O2 C4 H4B 110.5 . . ? C5 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? N1 C5 C6 122.5(3) . . ? N1 C5 C4 117.2(2) . . ? C6 C5 C4 120.3(2) . . ? C7 C6 C5 118.9(3) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C6 C7 C8 119.5(2) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 118.3(3) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? N1 C9 C8 122.9(2) . . ? N1 C9 C10 118.8(2) . . ? C8 C9 C10 118.3(3) . . ? N2 C10 C9 119.4(2) . . ? N2 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C13 122.2(2) . . ? N4 C12 N3 117.3(2) . . ? C13 C12 N3 120.5(2) . . ? C12 C13 C14 117.0(2) . . ? C12 C13 H13 121.5 . . ? C14 C13 H13 121.5 . . ? N5 C14 N6 117.9(2) . . ? N5 C14 C13 121.6(2) . . ? N6 C14 C13 120.5(2) . . ? N5 C15 N4 126.4(2) . . ? N5 C15 C16 116.7(2) . . ? N4 C15 C16 116.9(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 119.0(2) . . ? N7 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? N8 C19 C20 122.9(2) . . ? N8 C19 C18 118.4(2) . . ? C20 C19 C18 118.7(2) . . ? C21 C20 C19 118.6(3) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C22 C21 C20 119.1(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 119.1(3) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? N8 C23 C22 122.4(3) . . ? N8 C23 C24 115.2(2) . . ? C22 C23 C24 122.3(2) . . ? O3 C24 C23 112.9(2) . . ? O3 C24 H24A 109.0 . . ? C23 C24 H24A 109.0 . . ? O3 C24 H24B 109.0 . . ? C23 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? O4 C25 O3 122.9(2) . . ? O4 C25 C26 126.4(3) . . ? O3 C25 C26 110.7(2) . . ? C27 C26 C25 120.8(3) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? F13 C28 F12 107.7(3) . . ? F13 C28 F11 107.1(3) . . ? F12 C28 F11 105.8(3) . . ? F13 C28 S1 110.7(3) . . ? F12 C28 S1 111.8(2) . . ? F11 C28 S1 113.3(2) . . ? F21 C29 F23 107.5(2) . . ? F21 C29 F22 107.8(2) . . ? F23 C29 F22 107.1(2) . . ? F21 C29 S2 111.86(19) . . ? F23 C29 S2 111.57(19) . . ? F22 C29 S2 110.8(2) . . ? N9 C30 C31 179.4(3) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N10 C32 C33 177.4(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N11 C34 C35 178.5(3) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C5 N1 C9 117.9(2) . . ? C5 N1 Ag1 128.28(18) . . ? C9 N1 Ag1 113.23(16) . . ? C10 N2 N3 119.8(2) . . ? C10 N2 Ag1 119.96(18) . . ? N3 N2 Ag1 120.27(15) . . ? N2 N3 C12 116.4(2) . . ? N2 N3 C11 120.5(2) . . ? C12 N3 C11 122.8(2) . . ? C15 N4 C12 116.2(2) . . ? C15 N4 Ag1 123.86(17) . . ? C12 N4 Ag1 119.62(16) . . ? C15 N5 C14 116.5(2) . . ? C15 N5 Ag2 124.71(17) . . ? C14 N5 Ag2 118.30(16) . . ? N7 N6 C14 117.0(2) . . ? N7 N6 C17 120.4(2) . . ? C14 N6 C17 122.1(2) . . ? C18 N7 N6 120.4(2) . . ? C18 N7 Ag2 118.89(17) . . ? N6 N7 Ag2 120.29(15) . . ? C23 N8 C19 118.0(2) . . ? C23 N8 Ag2 127.28(18) . . ? C19 N8 Ag2 114.57(16) . . ? C30 N9 Ag1 169.3(2) . . ? C32 N10 Ag1 151.6(3) . . ? C34 N11 Ag2 158.1(2) . . ? C3 O2 C4 116.3(2) . . ? C25 O3 C24 114.6(2) . . ? S1 O11 Ag2 129.49(14) . . ? O13 S1 O11 115.4(2) . . ? O13 S1 O12 115.1(2) . . ? O11 S1 O12 114.92(18) . . ? O13 S1 C28 104.11(17) . . ? O11 S1 C28 101.65(15) . . ? O12 S1 C28 102.95(14) . . ? O21 S2 O22 115.02(15) . . ? O21 S2 O23 115.31(14) . . ? O22 S2 O23 114.54(14) . . ? O21 S2 C29 102.99(13) . . ? O22 S2 C29 103.64(14) . . ? O23 S2 C29 102.92(12) . . ? N9 Ag1 N10 108.63(9) . . ? N9 Ag1 N2 131.36(8) . . ? N10 Ag1 N2 118.21(9) . . ? N9 Ag1 N4 117.46(8) . . ? N10 Ag1 N4 101.91(8) . . ? N2 Ag1 N4 65.93(7) . . ? N9 Ag1 N1 94.91(8) . . ? N10 Ag1 N1 97.33(8) . . ? N2 Ag1 N1 67.83(7) . . ? N4 Ag1 N1 133.70(7) . . ? N11 Ag2 N7 154.00(8) . . ? N11 Ag2 N5 111.25(8) . . ? N7 Ag2 N5 65.93(7) . . ? N11 Ag2 N8 109.81(8) . . ? N7 Ag2 N8 68.72(7) . . ? N5 Ag2 N8 134.64(7) . . ? N11 Ag2 O11 88.13(8) . . ? N7 Ag2 O11 117.64(7) . . ? N5 Ag2 O11 94.67(8) . . ? N8 Ag2 O11 105.15(8) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 30.37 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.748 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.125 #===END data_Complex_8(sdjh963) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 Ag3.50 F9 N8 O14 S3' _chemical_formula_sum 'C30 H28 Ag3.50 F9 N8 O14 S3' _chemical_formula_weight 1369.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 '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 11.7250(9) _cell_length_b 13.5150(11) _cell_length_c 16.5799(13) _cell_angle_alpha 104.351(4) _cell_angle_beta 94.273(4) _cell_angle_gamma 96.468(4) _cell_volume 2514.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7457 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 24.00 _exptl_crystal_description 'rod' _exptl_crystal_colour 'yellow' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1339 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24608 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 24.07 _reflns_number_total 7908 _reflns_number_gt 6327 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _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^ > 2\s(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^)+(0.0901P)^2^+11.9869P] 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 7908 _refine_ls_number_parameters 613 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8608(11) 0.7158(9) 0.0678(6) 0.067(3) Uani 1 1 d . . . H1A H 0.9288 0.7613 0.0856 0.081 Uiso 1 1 calc R . . H1B H 0.8285 0.6806 0.1040 0.081 Uiso 1 1 calc R . . C2 C 0.8104(8) 0.7012(7) -0.0086(5) 0.041(2) Uani 1 1 d . . . H2 H 0.7424 0.6557 -0.0262 0.049 Uiso 1 1 calc R . . C3 C 0.8612(8) 0.7569(7) -0.0670(5) 0.035(2) Uani 1 1 d . . . C4 C 0.8430(7) 0.7838(6) -0.2009(5) 0.0322(18) Uani 1 1 d . . . H4A H 0.9205 0.7680 -0.2096 0.039 Uiso 1 1 calc R . . H4B H 0.8461 0.8580 -0.1810 0.039 Uiso 1 1 calc R . . C5 C 0.7647(7) 0.7441(6) -0.2809(5) 0.0294(18) Uani 1 1 d . . . C6 C 0.6865(7) 0.6541(6) -0.2984(5) 0.0329(19) Uani 1 1 d . . . H6 H 0.6791 0.6166 -0.2586 0.039 Uiso 1 1 calc R . . C7 C 0.6190(7) 0.6202(6) -0.3758(6) 0.037(2) Uani 1 1 d . . . H7 H 0.5648 0.5613 -0.3878 0.044 Uiso 1 1 calc R . . C8 C 0.6354(7) 0.6765(6) -0.4335(5) 0.0329(18) Uani 1 1 d . . . H8 H 0.5942 0.6544 -0.4863 0.039 Uiso 1 1 calc R . . C9 C 0.7143(6) 0.7676(6) -0.4126(5) 0.0262(16) Uani 1 1 d . . . C10 C 0.7274(6) 0.8254(6) -0.4743(5) 0.0263(16) Uani 1 1 d . . . H10 H 0.6860 0.8028 -0.5271 0.032 Uiso 1 1 calc R . . C11 C 0.7586(8) 0.9394(7) -0.5928(5) 0.040(2) Uani 1 1 d . . . H11A H 0.7475 0.8656 -0.6124 0.060 Uiso 1 1 calc R . . H11B H 0.8037 0.9683 -0.6296 0.060 Uiso 1 1 calc R . . H11C H 0.6849 0.9641 -0.5921 0.060 Uiso 1 1 calc R . . C12 C 0.8897(6) 1.0640(6) -0.4768(4) 0.0256(17) Uani 1 1 d . . . C13 C 0.9105(6) 1.1303(6) -0.5267(5) 0.0259(16) Uani 1 1 d . . . H13 H 0.8779 1.1138 -0.5820 0.031 Uiso 1 1 calc R . . C14 C 0.9822(7) 1.2232(6) -0.4914(4) 0.0253(16) Uani 1 1 d . . . C15 C 1.0056(7) 1.1768(6) -0.3665(5) 0.0302(18) Uani 1 1 d . . . C16 C 1.0545(8) 1.2037(6) -0.2783(5) 0.0348(19) Uani 1 1 d . . . H16A H 0.9946 1.2203 -0.2428 0.052 Uiso 1 1 calc R . . H16B H 1.1133 1.2622 -0.2680 0.052 Uiso 1 1 calc R . . H16C H 1.0875 1.1463 -0.2666 0.052 Uiso 1 1 calc R . . C17 C 0.9547(7) 1.2753(6) -0.6233(5) 0.0285(17) Uani 1 1 d . . . H17A H 1.0015 1.2357 -0.6604 0.043 Uiso 1 1 calc R . . H17B H 0.9508 1.3403 -0.6363 0.043 Uiso 1 1 calc R . . H17C H 0.8783 1.2383 -0.6298 0.043 Uiso 1 1 calc R . . C18 C 1.1198(6) 1.4432(6) -0.5385(5) 0.0289(18) Uani 1 1 d . . . H18 H 1.0938 1.4344 -0.5946 0.035 Uiso 1 1 calc R . . C19 C 1.2029(7) 1.5344(6) -0.4928(5) 0.0292(17) Uani 1 1 d . . . C20 C 1.2523(7) 1.6038(7) -0.5332(5) 0.037(2) Uani 1 1 d . . . H20 H 1.2347 1.5936 -0.5905 0.044 Uiso 1 1 calc R . . C21 C 1.3282(7) 1.6886(7) -0.4876(6) 0.039(2) Uani 1 1 d . . . H21 H 1.3630 1.7353 -0.5141 0.047 Uiso 1 1 calc R . . C22 C 1.3516(7) 1.7030(7) -0.4024(6) 0.036(2) Uani 1 1 d . . . H22 H 1.4012 1.7601 -0.3705 0.043 Uiso 1 1 calc R . . C23 C 1.2996(7) 1.6306(6) -0.3650(5) 0.0313(18) Uani 1 1 d . . . C24 C 1.3077(8) 0.6435(7) -0.2719(5) 0.040(2) Uani 1 1 d . . . H24A H 1.2404 0.6716 -0.2499 0.048 Uiso 1 1 calc R . . H24B H 1.3096 0.5770 -0.2600 0.048 Uiso 1 1 calc R . . C25 C 1.4221(8) 0.7373(8) -0.1491(6) 0.044(2) Uani 1 1 d . . . C26 C 1.5330(9) 0.7981(10) -0.1138(6) 0.062(3) Uani 1 1 d . . . H26 H 1.5830 0.8185 -0.1495 0.075 Uiso 1 1 calc R . . C27 C 1.5643(11) 0.8247(13) -0.0329(8) 0.100(5) Uani 1 1 d . . . H27A H 1.5150 0.8047 0.0033 0.120 Uiso 1 1 calc R . . H27B H 1.6356 0.8635 -0.0118 0.120 Uiso 1 1 calc R . . C28 C 0.9001(9) 0.4442(7) -0.1907(7) 0.050(3) Uani 1 1 d . . . C29 C 1.3040(7) 0.9905(7) -0.1924(5) 0.0349(19) Uani 1 1 d . . . C30 C 1.3534(13) 0.9528(11) 0.1385(7) 0.116(6) Uani 1 1 d D . . N1 N 0.7767(5) 0.8002(5) -0.3367(4) 0.0254(14) Uani 1 1 d . . . N2 N 0.8002(5) 0.9116(5) -0.4533(4) 0.0266(14) Uani 1 1 d . . . N3 N 0.8193(6) 0.9707(5) -0.5077(4) 0.0293(15) Uani 1 1 d . . . N4 N 0.9363(6) 1.0864(5) -0.3964(4) 0.0275(14) Uani 1 1 d . . . N5 N 1.0300(6) 1.2460(5) -0.4113(4) 0.0282(14) Uani 1 1 d . . . N6 N 1.0053(5) 1.2931(5) -0.5372(4) 0.0254(14) Uani 1 1 d . . . N7 N 1.0849(5) 1.3780(5) -0.5003(4) 0.0280(15) Uani 1 1 d . . . N8 N 1.2267(6) 1.5483(5) -0.4087(4) 0.0302(15) Uani 1 1 d . . . O1 O 0.9521(5) 0.8136(4) -0.0510(3) 0.0304(12) Uani 1 1 d . . . O2 O 0.7959(5) 0.7335(5) -0.1402(3) 0.0349(13) Uani 1 1 d . . . O3 O 1.4097(5) 0.7114(5) -0.2326(4) 0.0400(14) Uani 1 1 d . . . O4 O 1.3471(5) 0.7095(6) -0.1098(4) 0.0540(18) Uani 1 1 d . . . O11 O 1.1140(5) 0.4644(4) -0.2092(3) 0.0368(13) Uani 1 1 d . . . O12 O 1.0416(6) 0.5947(5) -0.1063(4) 0.0583(18) Uani 1 1 d . . . O13 O 0.9969(6) 0.5834(6) -0.2526(5) 0.061(2) Uani 1 1 d . . . O23 O 1.1527(5) 0.8382(4) -0.1880(3) 0.0343(13) Uani 1 1 d . . . O21 O 1.0950(4) 0.9621(4) -0.2599(3) 0.0323(12) Uani 1 1 d . . . O22 O 1.1287(5) 1.0099(5) -0.1077(3) 0.0417(15) Uani 1 1 d . . . O31 O 1.1737(10) 0.9732(6) 0.0825(5) 0.105(4) Uani 1 1 d . . . O32 O 1.1920(6) 0.7951(5) 0.0699(4) 0.0437(15) Uani 1 1 d . . . O33 O 1.1576(12) 0.9037(7) 0.1982(6) 0.148(6) Uani 1 1 d . . . F11 F 0.9129(5) 0.3868(5) -0.1382(4) 0.0683(18) Uani 1 1 d . . . F12 F 0.8725(6) 0.3780(5) -0.2675(4) 0.0746(18) Uani 1 1 d . . . F13 F 0.8093(5) 0.4947(5) -0.1742(4) 0.0655(17) Uani 1 1 d . . . F23 F 1.3716(4) 0.9740(4) -0.1297(3) 0.0510(13) Uani 1 1 d . . . F22 F 1.3201(4) 1.0891(4) -0.1901(4) 0.0510(13) Uani 1 1 d . . . F21 F 1.3376(4) 0.9387(4) -0.2634(3) 0.0497(13) Uani 1 1 d . . . F32 F 1.3674(8) 1.0295(6) 0.2085(8) 0.133(4) Uani 1 1 d D . . F33 F 1.4177(5) 0.8880(7) 0.1531(4) 0.086(2) Uani 1 1 d D . . F31 F 1.3846(9) 0.9486(9) 0.0617(6) 0.136(4) Uani 1 1 d D . . S1 S 1.0260(2) 0.53024(16) -0.19111(14) 0.0407(5) Uani 1 1 d . . . S2 S 1.15367(16) 0.94623(14) -0.18526(11) 0.0255(4) Uani 1 1 d . . . S3 S 1.19892(17) 0.89930(16) 0.12277(12) 0.0321(5) Uani 1 1 d . . . Ag1 Ag 0.89523(5) 0.96476(4) -0.31270(3) 0.02762(18) Uani 1 1 d . . . Ag2 Ag 1.15622(6) 1.40511(5) -0.35493(4) 0.03406(19) Uani 1 1 d . . . Ag3 Ag 1.15233(6) 0.76336(5) -0.07488(4) 0.03371(19) Uani 1 1 d . . . Ag4 Ag 1.0000 1.0000 0.0000 0.0475(3) Uani 1 2 d S . . O5 O 1.334(4) 1.348(3) -0.300(3) 0.43(2) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.109(10) 0.059(7) 0.032(6) 0.019(5) 0.015(6) -0.014(6) C2 0.047(5) 0.052(6) 0.029(5) 0.023(4) 0.009(4) 0.003(4) C3 0.049(6) 0.041(5) 0.027(4) 0.016(4) 0.018(4) 0.027(5) C4 0.043(5) 0.029(4) 0.030(4) 0.015(4) 0.009(4) 0.009(4) C5 0.038(5) 0.031(4) 0.027(4) 0.012(3) 0.015(3) 0.019(4) C6 0.030(4) 0.040(5) 0.036(5) 0.018(4) 0.012(4) 0.009(4) C7 0.030(4) 0.031(4) 0.051(5) 0.015(4) 0.005(4) -0.001(4) C8 0.027(4) 0.040(5) 0.032(4) 0.006(4) 0.004(3) 0.012(4) C9 0.023(4) 0.029(4) 0.029(4) 0.007(3) 0.003(3) 0.013(3) C10 0.025(4) 0.028(4) 0.021(4) 0.000(3) -0.001(3) 0.003(3) C11 0.049(5) 0.050(5) 0.017(4) 0.006(4) -0.005(4) 0.002(4) C12 0.032(4) 0.036(4) 0.016(4) 0.012(3) 0.008(3) 0.018(4) C13 0.029(4) 0.032(4) 0.021(4) 0.009(3) 0.001(3) 0.017(3) C14 0.034(4) 0.027(4) 0.020(4) 0.009(3) 0.011(3) 0.018(3) C15 0.048(5) 0.023(4) 0.023(4) 0.006(3) 0.009(4) 0.015(4) C16 0.057(5) 0.023(4) 0.024(4) 0.006(3) 0.003(4) 0.007(4) C17 0.038(4) 0.031(4) 0.024(4) 0.015(3) 0.004(3) 0.015(4) C18 0.026(4) 0.043(5) 0.027(4) 0.018(4) 0.015(3) 0.019(4) C19 0.033(4) 0.029(4) 0.031(4) 0.011(3) 0.010(3) 0.018(3) C20 0.038(5) 0.044(5) 0.034(5) 0.016(4) 0.012(4) 0.013(4) C21 0.034(5) 0.046(5) 0.043(5) 0.018(4) 0.013(4) 0.009(4) C22 0.027(4) 0.037(5) 0.049(5) 0.012(4) 0.016(4) 0.017(4) C23 0.029(4) 0.038(5) 0.031(4) 0.010(4) 0.009(3) 0.017(4) C24 0.052(6) 0.034(5) 0.034(5) 0.001(4) 0.009(4) 0.014(4) C25 0.033(5) 0.068(6) 0.034(5) 0.012(5) 0.001(4) 0.029(5) C26 0.048(6) 0.100(9) 0.036(6) 0.006(6) 0.004(5) 0.027(6) C27 0.063(8) 0.157(15) 0.056(8) -0.026(8) -0.006(6) 0.041(9) C28 0.058(6) 0.028(5) 0.070(7) 0.018(5) 0.020(5) 0.015(4) C29 0.031(4) 0.037(5) 0.037(5) 0.012(4) 0.001(4) 0.005(4) C30 0.082(11) 0.17(2) 0.127(16) 0.082(15) 0.030(11) 0.021(12) N1 0.025(3) 0.032(4) 0.022(3) 0.009(3) 0.005(3) 0.011(3) N2 0.031(3) 0.041(4) 0.015(3) 0.013(3) 0.006(3) 0.019(3) N3 0.036(4) 0.033(4) 0.023(3) 0.014(3) 0.003(3) 0.006(3) N4 0.038(4) 0.027(4) 0.018(3) 0.003(3) 0.007(3) 0.010(3) N5 0.039(4) 0.029(3) 0.020(3) 0.007(3) 0.010(3) 0.012(3) N6 0.027(3) 0.033(4) 0.018(3) 0.007(3) 0.001(3) 0.011(3) N7 0.033(4) 0.029(4) 0.027(3) 0.007(3) 0.014(3) 0.016(3) N8 0.033(4) 0.026(4) 0.032(4) 0.003(3) 0.009(3) 0.012(3) O1 0.034(3) 0.027(3) 0.032(3) 0.009(2) 0.006(2) 0.010(3) O2 0.033(3) 0.052(4) 0.027(3) 0.022(3) 0.000(2) 0.010(3) O3 0.040(3) 0.049(4) 0.032(3) 0.007(3) 0.011(3) 0.011(3) O4 0.038(4) 0.097(6) 0.039(4) 0.026(4) 0.015(3) 0.032(4) O11 0.047(3) 0.034(3) 0.030(3) 0.005(2) 0.010(3) 0.010(3) O12 0.070(5) 0.052(4) 0.045(4) -0.005(3) 0.019(4) 0.009(4) O13 0.075(5) 0.061(4) 0.069(5) 0.047(4) 0.029(4) 0.025(4) O23 0.049(3) 0.033(3) 0.023(3) 0.010(2) -0.001(2) 0.008(3) O21 0.032(3) 0.038(3) 0.030(3) 0.016(3) -0.005(2) 0.005(2) O22 0.054(4) 0.048(4) 0.025(3) 0.004(3) 0.021(3) 0.016(3) O31 0.202(11) 0.058(5) 0.051(5) 0.005(4) -0.052(6) 0.059(6) O32 0.062(4) 0.042(4) 0.032(3) 0.011(3) 0.010(3) 0.017(3) O33 0.249(14) 0.067(6) 0.097(7) -0.033(5) 0.133(9) -0.067(8) F11 0.070(4) 0.062(4) 0.096(5) 0.056(4) 0.022(4) 0.016(3) F12 0.068(4) 0.062(4) 0.083(5) 0.002(4) -0.009(4) 0.013(3) F13 0.056(4) 0.069(4) 0.085(5) 0.033(4) 0.027(3) 0.025(3) F23 0.036(3) 0.066(4) 0.050(3) 0.020(3) -0.015(2) 0.005(3) F22 0.043(3) 0.044(3) 0.067(4) 0.019(3) 0.006(3) -0.001(2) F21 0.046(3) 0.067(4) 0.043(3) 0.017(3) 0.023(2) 0.023(3) F32 0.094(6) 0.049(4) 0.212(11) -0.018(6) -0.074(7) -0.002(4) F33 0.050(4) 0.141(7) 0.062(4) 0.008(4) 0.009(3) 0.036(4) F31 0.122(8) 0.170(10) 0.125(8) 0.044(7) 0.053(7) 0.021(7) S1 0.0624(15) 0.0295(11) 0.0358(12) 0.0115(9) 0.0198(11) 0.0127(10) S2 0.0281(10) 0.0292(10) 0.0204(9) 0.0069(8) 0.0036(8) 0.0069(8) S3 0.0334(11) 0.0402(12) 0.0242(10) 0.0077(9) 0.0039(8) 0.0120(9) Ag1 0.0328(3) 0.0312(3) 0.0207(3) 0.0095(2) 0.0010(2) 0.0072(3) Ag2 0.0517(4) 0.0295(3) 0.0223(3) 0.0080(3) 0.0038(3) 0.0081(3) Ag3 0.0452(4) 0.0344(4) 0.0259(3) 0.0094(3) 0.0100(3) 0.0160(3) Ag4 0.0807(8) 0.0305(5) 0.0428(6) 0.0155(4) 0.0351(5) 0.0240(5) O5 0.43(2) 0.42(2) 0.43(2) 0.110(11) 0.049(10) 0.068(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.317(14) . ? C1 H1A 0.9300 . ? C1 H1B 0.9300 . ? C2 C3 1.484(11) . ? C2 H2 0.9300 . ? C3 O1 1.211(10) . ? C3 O2 1.333(10) . ? C4 O2 1.456(9) . ? C4 C5 1.499(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N1 1.339(9) . ? C5 C6 1.392(12) . ? C6 C7 1.400(12) . ? C6 H6 0.9300 . ? C7 C8 1.373(11) . ? C7 H7 0.9300 . ? C8 C9 1.406(11) . ? C8 H8 0.9300 . ? C9 N1 1.352(10) . ? C9 C10 1.440(10) . ? C10 N2 1.319(10) . ? C10 H10 0.9300 . ? C11 N3 1.472(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N4 1.349(10) . ? C12 C13 1.376(10) . ? C12 N3 1.385(10) . ? C13 C14 1.396(11) . ? C13 H13 0.9300 . ? C14 N5 1.348(10) . ? C14 N6 1.368(9) . ? C15 N4 1.347(10) . ? C15 N5 1.351(9) . ? C15 C16 1.471(11) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N6 1.455(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N7 1.257(9) . ? C18 C19 1.483(12) . ? C18 H18 0.9300 . ? C19 N8 1.363(10) . ? C19 C20 1.381(11) . ? C20 C21 1.385(13) . ? C20 H20 0.9300 . ? C21 C22 1.378(12) . ? C21 H21 0.9300 . ? C22 C23 1.391(11) . ? C22 H22 0.9300 . ? C23 N8 1.337(11) . ? C23 C24 1.504(11) 1_565 ? C24 O3 1.428(11) . ? C24 C23 1.504(11) 1_545 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O4 1.213(11) . ? C25 O3 1.334(10) . ? C25 C26 1.455(15) . ? C26 C27 1.312(16) . ? C26 H26 0.9300 . ? C27 H27A 0.9300 . ? C27 H27B 0.9300 . ? C28 F11 1.312(11) . ? C28 F13 1.337(10) . ? C28 F12 1.355(12) . ? C28 S1 1.775(10) . ? C29 F22 1.316(10) . ? C29 F21 1.325(10) . ? C29 F23 1.338(10) . ? C29 S2 1.818(8) . ? C30 F33 1.273(9) . ? C30 F32 1.337(9) . ? C30 F31 1.341(9) . ? C30 S3 1.847(15) . ? N1 Ag1 2.412(6) . ? N2 N3 1.359(8) . ? N2 Ag1 2.407(6) . ? N4 Ag1 2.432(6) . ? N5 Ag2 2.402(7) . ? N6 N7 1.375(9) . ? N7 Ag2 2.415(6) . ? N8 Ag2 2.414(6) . ? O1 Ag4 2.435(5) . ? O1 Ag3 2.548(5) . ? O4 Ag3 2.538(6) . ? O11 S1 1.438(6) . ? O11 Ag2 2.456(5) 1_545 ? O12 S1 1.445(7) . ? O12 Ag3 2.408(7) . ? O13 S1 1.427(7) . ? O23 S2 1.448(6) . ? O23 Ag3 2.341(5) . ? O21 S2 1.446(5) . ? O21 Ag1 2.445(5) . ? O22 S2 1.430(6) . ? O22 Ag4 2.441(5) . ? O31 S3 1.378(7) . ? O31 Ag4 2.479(9) . ? O32 S3 1.453(6) . ? O32 Ag3 2.333(6) . ? O33 S3 1.365(8) . ? O33 Ag1 2.428(8) 2_775 ? Ag1 O33 2.428(8) 2_775 ? Ag2 O11 2.456(5) 1_565 ? Ag2 O5 2.49(4) . ? Ag4 O1 2.435(5) 2_775 ? Ag4 O22 2.441(5) 2_775 ? Ag4 O31 2.479(9) 2_775 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 120.5(9) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? O1 C3 O2 124.4(7) . . ? O1 C3 C2 124.3(8) . . ? O2 C3 C2 111.2(8) . . ? O2 C4 C5 107.2(6) . . ? O2 C4 H4A 110.3 . . ? C5 C4 H4A 110.3 . . ? O2 C4 H4B 110.3 . . ? C5 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? N1 C5 C6 121.4(7) . . ? N1 C5 C4 115.2(7) . . ? C6 C5 C4 123.4(7) . . ? C5 C6 C7 120.0(7) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 117.9(8) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? C7 C8 C9 120.0(8) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? N1 C9 C8 121.0(7) . . ? N1 C9 C10 120.7(7) . . ? C8 C9 C10 118.3(7) . . ? N2 C10 C9 117.5(7) . . ? N2 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C13 122.1(7) . . ? N4 C12 N3 117.1(6) . . ? C13 C12 N3 120.8(7) . . ? C12 C13 C14 117.7(7) . . ? C12 C13 H13 121.1 . . ? C14 C13 H13 121.1 . . ? N5 C14 N6 118.6(7) . . ? N5 C14 C13 120.7(6) . . ? N6 C14 C13 120.7(7) . . ? N4 C15 N5 124.3(7) . . ? N4 C15 C16 117.9(7) . . ? N5 C15 C16 117.8(7) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 118.9(7) . . ? N7 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? N8 C19 C20 121.2(8) . . ? N8 C19 C18 117.1(6) . . ? C20 C19 C18 121.6(7) . . ? C19 C20 C21 119.5(8) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 119.3(8) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 118.8(9) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? N8 C23 C22 122.2(8) . . ? N8 C23 C24 113.6(7) . 1_565 ? C22 C23 C24 123.8(8) . 1_565 ? O3 C24 C23 109.7(7) . 1_545 ? O3 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 1_545 . ? O3 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 1_545 . ? H24A C24 H24B 108.2 . . ? O4 C25 O3 121.3(9) . . ? O4 C25 C26 126.0(9) . . ? O3 C25 C26 112.7(8) . . ? C27 C26 C25 121.5(12) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C26 C27 H27A 120.0 . . ? C26 C27 H27B 120.0 . . ? H27A C27 H27B 120.0 . . ? F11 C28 F13 109.5(8) . . ? F11 C28 F12 106.1(8) . . ? F13 C28 F12 106.5(9) . . ? F11 C28 S1 113.4(8) . . ? F13 C28 S1 111.3(6) . . ? F12 C28 S1 109.7(7) . . ? F22 C29 F21 107.9(7) . . ? F22 C29 F23 109.2(7) . . ? F21 C29 F23 107.4(7) . . ? F22 C29 S2 111.6(6) . . ? F21 C29 S2 110.4(6) . . ? F23 C29 S2 110.2(6) . . ? F33 C30 F32 105.5(10) . . ? F33 C30 F31 95.0(10) . . ? F32 C30 F31 131.7(15) . . ? F33 C30 S3 111.9(10) . . ? F32 C30 S3 106.2(8) . . ? F31 C30 S3 105.6(10) . . ? C5 N1 C9 119.6(7) . . ? C5 N1 Ag1 125.7(5) . . ? C9 N1 Ag1 114.6(5) . . ? C10 N2 N3 121.8(6) . . ? C10 N2 Ag1 117.7(5) . . ? N3 N2 Ag1 120.6(5) . . ? N2 N3 C12 116.9(6) . . ? N2 N3 C11 120.4(6) . . ? C12 N3 C11 122.4(6) . . ? C15 N4 C12 117.2(6) . . ? C15 N4 Ag1 122.9(5) . . ? C12 N4 Ag1 120.0(5) . . ? C14 N5 C15 118.0(7) . . ? C14 N5 Ag2 119.2(5) . . ? C15 N5 Ag2 122.8(5) . . ? C14 N6 N7 116.9(6) . . ? C14 N6 C17 121.9(7) . . ? N7 N6 C17 121.1(6) . . ? C18 N7 N6 122.6(7) . . ? C18 N7 Ag2 118.9(6) . . ? N6 N7 Ag2 118.5(4) . . ? C23 N8 C19 119.0(7) . . ? C23 N8 Ag2 124.6(5) . . ? C19 N8 Ag2 115.6(5) . . ? C3 O1 Ag4 132.6(5) . . ? C3 O1 Ag3 127.1(5) . . ? Ag4 O1 Ag3 100.1(2) . . ? C3 O2 C4 113.7(6) . . ? C25 O3 C24 116.0(7) . . ? C25 O4 Ag3 134.8(6) . . ? S1 O11 Ag2 118.7(3) . 1_545 ? S1 O12 Ag3 119.9(4) . . ? S2 O23 Ag3 127.4(3) . . ? S2 O21 Ag1 136.4(3) . . ? S2 O22 Ag4 138.4(4) . . ? S3 O31 Ag4 134.3(7) . . ? S3 O32 Ag3 120.0(3) . . ? S3 O33 Ag1 137.1(6) . 2_775 ? O13 S1 O11 116.1(4) . . ? O13 S1 O12 113.8(5) . . ? O11 S1 O12 113.2(4) . . ? O13 S1 C28 105.4(5) . . ? O11 S1 C28 104.1(4) . . ? O12 S1 C28 102.3(5) . . ? O22 S2 O21 115.7(4) . . ? O22 S2 O23 115.2(3) . . ? O21 S2 O23 112.8(3) . . ? O22 S2 C29 104.3(4) . . ? O21 S2 C29 102.9(3) . . ? O23 S2 C29 103.8(4) . . ? O33 S3 O31 117.7(8) . . ? O33 S3 O32 113.5(5) . . ? O31 S3 O32 115.9(4) . . ? O33 S3 C30 110.1(7) . . ? O31 S3 C30 90.4(6) . . ? O32 S3 C30 105.8(5) . . ? N2 Ag1 N1 69.3(2) . . ? N2 Ag1 O33 125.8(4) . 2_775 ? N1 Ag1 O33 113.4(2) . 2_775 ? N2 Ag1 N4 65.4(2) . . ? N1 Ag1 N4 134.7(2) . . ? O33 Ag1 N4 92.8(3) 2_775 . ? N2 Ag1 O21 130.53(19) . . ? N1 Ag1 O21 113.00(19) . . ? O33 Ag1 O21 99.5(4) 2_775 . ? N4 Ag1 O21 97.11(19) . . ? N5 Ag2 N8 134.9(2) . . ? N5 Ag2 N7 66.4(2) . . ? N8 Ag2 N7 68.5(2) . . ? N5 Ag2 O11 105.05(19) . 1_565 ? N8 Ag2 O11 111.2(2) . 1_565 ? N7 Ag2 O11 145.48(19) . 1_565 ? N5 Ag2 O5 103.1(10) . . ? N8 Ag2 O5 104.3(10) . . ? N7 Ag2 O5 126.8(10) . . ? O11 Ag2 O5 87.5(10) 1_565 . ? O32 Ag3 O23 144.7(2) . . ? O32 Ag3 O12 100.1(2) . . ? O23 Ag3 O12 114.0(2) . . ? O32 Ag3 O4 95.9(2) . . ? O23 Ag3 O4 87.9(2) . . ? O12 Ag3 O4 98.6(2) . . ? O32 Ag3 O1 88.21(19) . . ? O23 Ag3 O1 89.11(18) . . ? O12 Ag3 O1 80.2(2) . . ? O4 Ag3 O1 175.91(19) . . ? O1 Ag4 O1 180.000(1) 2_775 . ? O1 Ag4 O22 92.93(19) 2_775 2_775 ? O1 Ag4 O22 87.07(19) . 2_775 ? O1 Ag4 O22 87.07(19) 2_775 . ? O1 Ag4 O22 92.93(19) . . ? O22 Ag4 O22 180.0(3) 2_775 . ? O1 Ag4 O31 88.7(2) 2_775 2_775 ? O1 Ag4 O41 91.3(2) . 2_775 ? O22 Ag4 O31 85.0(3) 2_775 2_775 ? O22 Ag4 O31 95.0(3) . 2_775 ? O1 Ag4 O31 91.3(2) 2_775 . ? O1 Ag4 O31 88.7(2) . . ? O22 Ag4 O31 95.0(3) 2_775 . ? O22 Ag4 O31 85.0(3) . . ? O31 Ag4 O31 180.0(4) 2_775 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 24.07 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.210 _refine_diff_density_min -1.168 _refine_diff_density_rms 0.157 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.529 1.029 595 144 ' ' _platon_squeeze_details ; ;