# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Steed, Jon' 'Arya, P.' 'Channa, A.' 'Cragg, Peter J.' _publ_contact_author_name 'Dr Jon Steed' _publ_contact_author_address ; Department of Chemistry King's College London Strand LONDON WC2R 2LS U.K. ; _publ_contact_author_email 'JON.STEED@KCL.AC.UK' _publ_section_title ; C-donor lariat ether 'scorpionates' ; data_allytrif #(compound8b) _database_code_CSD 180577 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H25 Ag B F4 N O4' _chemical_formula_weight 454.02 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' 'F' 'F' 0.0171 0.0103 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0985(6) _cell_length_b 9.3302(4) _cell_length_c 20.8800(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.591(3) _cell_angle_gamma 90.00 _cell_volume 1760.81(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.7145 _exptl_absorpt_correction_T_max 0.9424 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi scans & omega to complete' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14323 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3988 _reflns_number_gt 3504 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.7137P] 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 SHELXL _refine_ls_extinction_coef 0.0062(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3988 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.79128(3) 0.46237(2) 0.154387(11) 0.01562(10) Uani 1 1 d . . . F1 F 0.9965(4) 0.4442(3) 0.36116(18) 0.0746(11) Uani 1 1 d . . . F2 F 1.0809(3) 0.6732(3) 0.36860(15) 0.0489(7) Uani 1 1 d . . . F3 F 1.2152(5) 0.5008(4) 0.42502(14) 0.0877(13) Uani 1 1 d . . . F4 F 1.2045(3) 0.5041(3) 0.31763(12) 0.0407(6) Uani 1 1 d . . . O1 O 0.7953(2) 0.3112(2) 0.05428(10) 0.0176(5) Uani 1 1 d . . . O2 O 0.6788(3) 0.5932(3) 0.04469(11) 0.0209(5) Uani 1 1 d . . . O3 O 0.8939(3) 0.7389(3) 0.13527(11) 0.0219(5) Uani 1 1 d . . . O4 O 1.0532(2) 0.4931(3) 0.17937(12) 0.0218(5) Uani 1 1 d . . . N1 N 0.8997(3) 0.2246(3) 0.18540(12) 0.0164(6) Uani 1 1 d . . . C1 C 0.8987(4) 0.1319(4) 0.12754(15) 0.0210(7) Uani 1 1 d . . . H1A H 0.8905 0.0305 0.1406 0.025 Uiso 1 1 calc R . . H1B H 0.9936 0.1434 0.1092 0.025 Uiso 1 1 calc R . . C2 C 0.7722(4) 0.1672(4) 0.07608(16) 0.0209(7) Uani 1 1 d . . . H2A H 0.7709 0.0990 0.0397 0.025 Uiso 1 1 calc R . . H2B H 0.6764 0.1604 0.0941 0.025 Uiso 1 1 calc R . . C3 C 0.6837(4) 0.3549(4) 0.00440(16) 0.0220(7) Uani 1 1 d . . . H3A H 0.5843 0.3420 0.0186 0.026 Uiso 1 1 calc R . . H3B H 0.6894 0.2964 -0.0348 0.026 Uiso 1 1 calc R . . C4 C 0.7094(4) 0.5097(4) -0.00972(16) 0.0234(7) Uani 1 1 d . . . H4A H 0.8133 0.5243 -0.0180 0.028 Uiso 1 1 calc R . . H4B H 0.6439 0.5398 -0.0485 0.028 Uiso 1 1 calc R . . C5 C 0.7235(4) 0.7414(4) 0.04051(17) 0.0256(8) Uani 1 1 d . . . H5A H 0.6602 0.8021 0.0649 0.031 Uiso 1 1 calc R . . H5B H 0.7093 0.7725 -0.0051 0.031 Uiso 1 1 calc R . . C6 C 0.8832(4) 0.7616(4) 0.06711(17) 0.0249(8) Uani 1 1 d . . . H6A H 0.9465 0.6922 0.0471 0.030 Uiso 1 1 calc R . . H6B H 0.9163 0.8597 0.0578 0.030 Uiso 1 1 calc R . . C7 C 1.0425(4) 0.7453(4) 0.16750(18) 0.0260(8) Uani 1 1 d . . . H7A H 1.0382 0.7589 0.2143 0.031 Uiso 1 1 calc R . . H7B H 1.0934 0.8295 0.1514 0.031 Uiso 1 1 calc R . . C8 C 1.1312(4) 0.6125(4) 0.15735(17) 0.0219(7) Uani 1 1 d . . . H8A H 1.1430 0.6011 0.1111 0.026 Uiso 1 1 calc R . . H8B H 1.2307 0.6196 0.1819 0.026 Uiso 1 1 calc R . . C9 C 1.1342(4) 0.3608(4) 0.17978(17) 0.0228(7) Uani 1 1 d . . . H9A H 1.2361 0.3745 0.2012 0.027 Uiso 1 1 calc R . . H9B H 1.1399 0.3277 0.1351 0.027 Uiso 1 1 calc R . . C10 C 1.0532(4) 0.2520(4) 0.21613(16) 0.0194(7) Uani 1 1 d . . . H10A H 1.1092 0.1608 0.2186 0.023 Uiso 1 1 calc R . . H10B H 1.0492 0.2866 0.2607 0.023 Uiso 1 1 calc R . . C11 C 0.8063(3) 0.1648(3) 0.23327(15) 0.0159(6) Uani 1 1 d . . . H11A H 0.7048 0.1495 0.2117 0.019 Uiso 1 1 calc R . . H11B H 0.8005 0.2360 0.2680 0.019 Uiso 1 1 calc R . . C12 C 0.8641(4) 0.0246(4) 0.26305(15) 0.0188(7) Uani 1 1 d . . . H12 H 0.8388 -0.0615 0.2401 0.023 Uiso 1 1 calc R . . C13 C 0.9498(4) 0.0147(4) 0.32065(16) 0.0213(7) Uani 1 1 d . . . H13A H 0.9768 0.0988 0.3448 0.026 Uiso 1 1 calc R . . H13B H 0.9826 -0.0765 0.3368 0.026 Uiso 1 1 calc R . . B1 B 1.1224(5) 0.5299(5) 0.3687(2) 0.0296(9) 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 Ag1 0.01432(14) 0.01876(14) 0.01382(14) -0.00154(10) 0.00171(8) 0.00198(9) F1 0.081(2) 0.0502(18) 0.106(3) -0.0269(18) 0.067(2) -0.0362(16) F2 0.0369(14) 0.0286(13) 0.083(2) 0.0027(13) 0.0142(13) 0.0049(11) F3 0.169(4) 0.061(2) 0.0263(15) -0.0007(14) -0.0186(19) 0.033(2) F4 0.0292(13) 0.0541(16) 0.0404(14) -0.0078(12) 0.0112(10) -0.0028(11) O1 0.0194(12) 0.0169(11) 0.0152(11) 0.0004(9) -0.0028(9) -0.0008(9) O2 0.0278(13) 0.0190(11) 0.0157(11) -0.0004(9) 0.0012(9) 0.0010(10) O3 0.0201(12) 0.0226(12) 0.0233(12) 0.0005(10) 0.0034(9) 0.0007(10) O4 0.0150(12) 0.0213(12) 0.0297(13) 0.0059(10) 0.0051(10) 0.0001(9) N1 0.0168(14) 0.0191(14) 0.0138(13) 0.0009(11) 0.0043(10) -0.0002(10) C1 0.0301(19) 0.0196(16) 0.0137(15) -0.0001(13) 0.0047(13) 0.0044(13) C2 0.0279(19) 0.0174(16) 0.0172(16) -0.0005(13) 0.0015(13) -0.0036(14) C3 0.0262(18) 0.0237(17) 0.0150(15) -0.0006(13) -0.0022(13) -0.0004(14) C4 0.0317(19) 0.0245(18) 0.0131(15) 0.0000(13) -0.0009(13) 0.0038(14) C5 0.038(2) 0.0159(16) 0.0222(17) 0.0026(14) -0.0004(15) 0.0046(14) C6 0.034(2) 0.0194(16) 0.0224(18) -0.0012(14) 0.0095(15) -0.0018(14) C7 0.0205(18) 0.0239(18) 0.034(2) -0.0074(15) 0.0030(15) -0.0039(14) C8 0.0184(17) 0.0221(17) 0.0254(17) -0.0016(14) 0.0031(13) -0.0048(13) C9 0.0157(17) 0.0260(18) 0.0273(18) 0.0051(15) 0.0050(13) 0.0052(13) C10 0.0174(16) 0.0210(16) 0.0196(16) 0.0026(13) 0.0013(13) 0.0031(13) C11 0.0161(16) 0.0191(15) 0.0127(14) 0.0022(12) 0.0023(12) 0.0024(12) C12 0.0198(16) 0.0204(16) 0.0178(16) 0.0029(13) 0.0080(12) 0.0006(13) C13 0.0143(16) 0.0277(18) 0.0227(17) 0.0086(14) 0.0057(13) -0.0003(13) B1 0.040(2) 0.024(2) 0.026(2) -0.0008(18) 0.0079(18) 0.0017(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C13 2.363(3) 2_655 ? Ag1 O4 2.397(2) . ? Ag1 C12 2.422(3) 2_655 ? Ag1 N1 2.483(3) . ? Ag1 O1 2.525(2) . ? F1 B1 1.391(5) . ? F2 B1 1.390(5) . ? F3 B1 1.394(5) . ? F4 B1 1.391(5) . ? O1 C3 1.428(4) . ? O1 C2 1.442(4) . ? O2 C4 1.431(4) . ? O2 C5 1.447(4) . ? O3 C6 1.431(4) . ? O3 C7 1.441(4) . ? O4 C8 1.425(4) . ? O4 C9 1.437(4) . ? N1 C1 1.485(4) . ? N1 C10 1.491(4) . ? N1 C11 1.492(4) . ? C1 C2 1.518(5) . ? C3 C4 1.498(5) . ? C5 C6 1.507(5) . ? C7 C8 1.507(5) . ? C9 C10 1.509(5) . ? C11 C12 1.517(4) . ? C12 C13 1.359(5) . ? C12 Ag1 2.422(3) 2_645 ? C13 Ag1 2.363(3) 2_645 ? 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 C13 Ag1 O4 148.42(10) 2_655 . ? C13 Ag1 C12 32.98(11) 2_655 2_655 ? O4 Ag1 C12 117.59(10) . 2_655 ? C13 Ag1 N1 118.55(11) 2_655 . ? O4 Ag1 N1 72.24(8) . . ? C12 Ag1 N1 105.98(10) 2_655 . ? C13 Ag1 O1 113.57(10) 2_655 . ? O4 Ag1 O1 97.97(8) . . ? C12 Ag1 O1 142.00(9) 2_655 . ? N1 Ag1 O1 70.97(8) . . ? C3 O1 C2 112.3(2) . . ? C3 O1 Ag1 111.58(18) . . ? C2 O1 Ag1 104.05(18) . . ? C4 O2 C5 113.0(3) . . ? C6 O3 C7 114.3(3) . . ? C8 O4 C9 113.5(2) . . ? C8 O4 Ag1 122.87(19) . . ? C9 O4 Ag1 113.25(19) . . ? C1 N1 C10 111.6(3) . . ? C1 N1 C11 112.1(3) . . ? C10 N1 C11 110.7(2) . . ? C1 N1 Ag1 110.04(18) . . ? C10 N1 Ag1 106.48(18) . . ? C11 N1 Ag1 105.60(18) . . ? N1 C1 C2 112.5(3) . . ? O1 C2 C1 107.4(3) . . ? O1 C3 C4 107.7(3) . . ? O2 C4 C3 108.6(3) . . ? O2 C5 C6 111.3(3) . . ? O3 C6 C5 107.5(3) . . ? O3 C7 C8 112.9(3) . . ? O4 C8 C7 107.6(3) . . ? O4 C9 C10 107.5(3) . . ? N1 C10 C9 112.7(3) . . ? N1 C11 C12 113.6(2) . . ? C13 C12 C11 123.9(3) . . ? C13 C12 Ag1 71.11(18) . 2_645 ? C11 C12 Ag1 107.2(2) . 2_645 ? C12 C13 Ag1 75.91(19) . 2_645 ? F2 B1 F4 109.6(3) . . ? F2 B1 F1 109.4(4) . . ? F4 B1 F1 108.7(3) . . ? F2 B1 F3 109.1(3) . . ? F4 B1 F3 106.7(4) . . ? F1 B1 F3 113.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Ag1 O1 C3 40.8(2) 2_655 . . . ? O4 Ag1 O1 C3 -137.6(2) . . . . ? C12 Ag1 O1 C3 62.6(3) 2_655 . . . ? N1 Ag1 O1 C3 154.4(2) . . . . ? C13 Ag1 O1 C2 -80.5(2) 2_655 . . . ? O4 Ag1 O1 C2 101.18(19) . . . . ? C12 Ag1 O1 C2 -58.7(2) 2_655 . . . ? N1 Ag1 O1 C2 33.15(18) . . . . ? C13 Ag1 O4 C8 -84.4(3) 2_655 . . . ? C12 Ag1 O4 C8 -101.2(2) 2_655 . . . ? N1 Ag1 O4 C8 159.7(3) . . . . ? O1 Ag1 O4 C8 92.7(2) . . . . ? C13 Ag1 O4 C9 133.0(3) 2_655 . . . ? C12 Ag1 O4 C9 116.2(2) 2_655 . . . ? N1 Ag1 O4 C9 17.1(2) . . . . ? O1 Ag1 O4 C9 -49.9(2) . . . . ? C13 Ag1 N1 C1 105.2(2) 2_655 . . . ? O4 Ag1 N1 C1 -107.2(2) . . . . ? C12 Ag1 N1 C1 138.3(2) 2_655 . . . ? O1 Ag1 N1 C1 -1.88(19) . . . . ? C13 Ag1 N1 C10 -133.68(19) 2_655 . . . ? O4 Ag1 N1 C10 13.90(18) . . . . ? C12 Ag1 N1 C10 -100.6(2) 2_655 . . . ? O1 Ag1 N1 C10 119.23(19) . . . . ? C13 Ag1 N1 C11 -16.0(2) 2_655 . . . ? O4 Ag1 N1 C11 131.6(2) . . . . ? C12 Ag1 N1 C11 17.2(2) 2_655 . . . ? O1 Ag1 N1 C11 -123.05(19) . . . . ? C10 N1 C1 C2 -147.4(3) . . . . ? C11 N1 C1 C2 87.8(3) . . . . ? Ag1 N1 C1 C2 -29.4(3) . . . . ? C3 O1 C2 C1 178.7(3) . . . . ? Ag1 O1 C2 C1 -60.5(3) . . . . ? N1 C1 C2 O1 63.8(4) . . . . ? C2 O1 C3 C4 174.3(3) . . . . ? Ag1 O1 C3 C4 58.0(3) . . . . ? C5 O2 C4 C3 170.4(3) . . . . ? O1 C3 C4 O2 -68.3(3) . . . . ? C4 O2 C5 C6 -86.8(3) . . . . ? C7 O3 C6 C5 176.2(3) . . . . ? O2 C5 C6 O3 -68.7(3) . . . . ? C6 O3 C7 C8 -76.1(4) . . . . ? C9 O4 C8 C7 -172.9(3) . . . . ? Ag1 O4 C8 C7 44.6(3) . . . . ? O3 C7 C8 O4 -57.2(4) . . . . ? C8 O4 C9 C10 168.8(3) . . . . ? Ag1 O4 C9 C10 -44.9(3) . . . . ? C1 N1 C10 C9 76.4(3) . . . . ? C11 N1 C10 C9 -158.0(3) . . . . ? Ag1 N1 C10 C9 -43.7(3) . . . . ? O4 C9 C10 N1 61.0(4) . . . . ? C1 N1 C11 C12 65.7(3) . . . . ? C10 N1 C11 C12 -59.6(3) . . . . ? Ag1 N1 C11 C12 -174.5(2) . . . . ? N1 C11 C12 C13 96.2(4) . . . . ? N1 C11 C12 Ag1 174.6(2) . . . 2_645 ? C11 C12 C13 Ag1 98.4(3) . . . 2_645 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.014 _refine_diff_density_min -1.051 _refine_diff_density_rms 0.172 #===END data_allylazk #(compound9) _database_code_CSD 180578 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H25 F6 K N O4 P' _chemical_formula_weight 443.41 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8857(3) _cell_length_b 16.4547(6) _cell_length_c 11.2887(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.677(2) _cell_angle_gamma 90.00 _cell_volume 1987.03(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used n/a _cell_measurement_theta_min n/a _cell_measurement_theta_max n/a _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_decay_% 0 _diffrn_reflns_number 16968 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3890 _reflns_number_gt 3420 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Denzo-smn _computing_data_reduction Denzo-smn _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'RES2INS (Barbour, 1998)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.9337P] 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 SHELXL _refine_ls_extinction_coef 0.0109(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3890 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 K1 K 0.20711(3) 0.04389(2) 0.66876(3) 0.02059(12) Uani 1 1 d . . . P1 P 0.09963(4) 0.08553(3) 0.35514(4) 0.02207(13) Uani 1 1 d . . . F1 F 0.23949(10) 0.09775(8) 0.42579(11) 0.0469(3) Uani 1 1 d . . . F2 F 0.09340(13) 0.00082(6) 0.42356(10) 0.0459(3) Uani 1 1 d . . . F3 F 0.05011(10) 0.13027(7) 0.46240(10) 0.0383(3) Uani 1 1 d . . . F4 F 0.15011(11) 0.03941(7) 0.24969(9) 0.0410(3) Uani 1 1 d . . . F5 F 0.10433(11) 0.16964(7) 0.28765(11) 0.0417(3) Uani 1 1 d . . . F6 F -0.04153(10) 0.07263(8) 0.28596(11) 0.0449(3) Uani 1 1 d . . . O1 O 0.29609(10) -0.00438(7) 0.91316(10) 0.0232(3) Uani 1 1 d . . . O2 O 0.39792(11) -0.07729(7) 0.72854(10) 0.0258(3) Uani 1 1 d . . . O3 O 0.45463(11) 0.08026(7) 0.65305(11) 0.0287(3) Uani 1 1 d . . . O4 O 0.28131(10) 0.20301(7) 0.69906(10) 0.0265(3) Uani 1 1 d . . . N1 N 0.13024(12) 0.14168(8) 0.86978(11) 0.0202(3) Uani 1 1 d . . . C1 C 0.32557(17) -0.08881(10) 0.91322(16) 0.0260(4) Uani 1 1 d . . . H1A H 0.2553(19) -0.1197(12) 0.8712(18) 0.031(5) Uiso 1 1 d . . . H1B H 0.3465(17) -0.1093(11) 0.9958(18) 0.025(5) Uiso 1 1 d . . . C2 C 0.43600(17) -0.09819(11) 0.85214(16) 0.0285(4) Uani 1 1 d . . . H2A H 0.506(2) -0.0668(12) 0.8932(18) 0.030(5) Uiso 1 1 d . . . H2B H 0.4666(19) -0.1535(13) 0.8600(18) 0.036(5) Uiso 1 1 d . . . C3 C 0.50094(19) -0.06101(12) 0.6692(2) 0.0344(4) Uani 1 1 d . . . H3A H 0.472(2) -0.0651(14) 0.589(2) 0.047(6) Uiso 1 1 d . . . H3B H 0.567(2) -0.1017(14) 0.696(2) 0.044(6) Uiso 1 1 d . . . C4 C 0.55190(17) 0.02365(12) 0.6933(2) 0.0358(4) Uani 1 1 d . . . H4A H 0.583(2) 0.0307(14) 0.778(2) 0.048(7) Uiso 1 1 d . . . H4B H 0.622(2) 0.0315(13) 0.649(2) 0.044(6) Uiso 1 1 d . . . C5 C 0.49390(17) 0.16194(11) 0.67956(19) 0.0328(4) Uani 1 1 d . . . H5A H 0.560(2) 0.1767(13) 0.6336(19) 0.039(6) Uiso 1 1 d . . . H5B H 0.523(2) 0.1699(14) 0.771(2) 0.044(6) Uiso 1 1 d . . . C6 C 0.38458(16) 0.21790(11) 0.63982(17) 0.0299(4) Uani 1 1 d . . . H6A H 0.411(2) 0.2767(14) 0.6527(19) 0.043(6) Uiso 1 1 d . . . H6B H 0.3505(17) 0.2081(12) 0.5503(17) 0.026(5) Uiso 1 1 d . . . C7 C 0.29898(16) 0.23086(11) 0.82140(16) 0.0283(4) Uani 1 1 d . . . H7A H 0.3288(19) 0.2877(13) 0.8269(17) 0.033(5) Uiso 1 1 d . . . H7B H 0.363(2) 0.1973(14) 0.873(2) 0.042(6) Uiso 1 1 d . . . C8 C 0.17379(16) 0.22586(10) 0.86084(15) 0.0245(3) Uani 1 1 d . . . H8A H 0.1765(19) 0.2562(13) 0.9412(19) 0.035(5) Uiso 1 1 d . . . H8B H 0.1134(18) 0.2558(12) 0.8005(17) 0.027(5) Uiso 1 1 d . . . C9 C -0.00648(15) 0.13968(11) 0.86044(15) 0.0255(3) Uani 1 1 d . . . H9A H -0.0313(19) 0.1744(12) 0.9265(19) 0.034(5) Uiso 1 1 d . . . H9B H -0.0300(18) 0.0831(12) 0.8744(17) 0.026(5) Uiso 1 1 d . . . C10 C -0.07643(16) 0.16806(11) 0.74092(16) 0.0281(4) Uani 1 1 d . . . H10 H -0.052(2) 0.1430(13) 0.672(2) 0.037(5) Uiso 1 1 d . . . C11 C -0.16468(17) 0.22373(12) 0.7285(2) 0.0376(4) Uani 1 1 d . . . H11A H -0.187(2) 0.2492(16) 0.796(2) 0.055(7) Uiso 1 1 d . . . H11B H -0.211(2) 0.2378(15) 0.650(2) 0.052(7) Uiso 1 1 d . . . C12 C 0.20043(16) 0.01364(11) 0.97995(15) 0.0247(3) Uani 1 1 d . . . H12A H 0.2215(17) -0.0080(11) 1.0614(17) 0.021(4) Uiso 1 1 d . . . H12B H 0.1230(18) -0.0117(11) 0.9419(17) 0.024(5) Uiso 1 1 d . . . C15 C 0.18970(17) 0.10519(10) 0.98565(15) 0.0253(4) Uani 1 1 d . . . H15A H 0.1463(18) 0.1189(12) 1.0485(18) 0.027(5) Uiso 1 1 d . . . H15B H 0.2743(18) 0.1261(11) 1.0072(16) 0.023(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.02048(18) 0.02231(19) 0.01890(18) 0.00020(12) 0.00342(12) -0.00109(13) P1 0.0220(2) 0.0249(2) 0.0196(2) 0.00196(16) 0.00460(16) -0.00237(16) F1 0.0257(6) 0.0719(9) 0.0390(7) -0.0053(6) -0.0050(5) 0.0034(6) F2 0.0806(9) 0.0271(6) 0.0363(6) 0.0091(5) 0.0270(6) 0.0066(6) F3 0.0441(6) 0.0369(6) 0.0367(6) -0.0070(5) 0.0149(5) 0.0046(5) F4 0.0517(7) 0.0497(7) 0.0251(5) -0.0017(5) 0.0165(5) 0.0046(5) F5 0.0440(7) 0.0335(6) 0.0470(7) 0.0165(5) 0.0072(5) -0.0070(5) F6 0.0272(6) 0.0571(7) 0.0472(7) -0.0018(6) -0.0008(5) -0.0154(5) O1 0.0258(6) 0.0206(6) 0.0238(6) 0.0010(4) 0.0062(4) 0.0040(5) O2 0.0253(6) 0.0277(6) 0.0246(6) -0.0019(5) 0.0050(5) 0.0027(5) O3 0.0202(6) 0.0259(6) 0.0400(7) 0.0014(5) 0.0053(5) 0.0013(5) O4 0.0238(6) 0.0275(6) 0.0293(6) -0.0016(5) 0.0077(5) -0.0043(5) N1 0.0207(6) 0.0215(7) 0.0185(6) 0.0023(5) 0.0034(5) 0.0022(5) C1 0.0336(9) 0.0199(8) 0.0234(8) 0.0020(6) 0.0022(7) 0.0032(7) C2 0.0296(9) 0.0256(9) 0.0280(9) -0.0030(7) -0.0006(7) 0.0087(7) C3 0.0339(10) 0.0309(10) 0.0421(11) -0.0024(8) 0.0167(8) 0.0066(8) C4 0.0220(9) 0.0348(10) 0.0518(12) 0.0043(9) 0.0099(8) 0.0059(8) C5 0.0239(9) 0.0292(9) 0.0469(11) 0.0012(8) 0.0104(8) -0.0049(7) C6 0.0273(9) 0.0283(9) 0.0355(10) 0.0025(7) 0.0097(7) -0.0043(7) C7 0.0258(9) 0.0260(9) 0.0317(9) -0.0020(7) 0.0015(7) -0.0047(7) C8 0.0282(8) 0.0205(8) 0.0242(8) -0.0017(6) 0.0036(6) 0.0019(7) C9 0.0225(8) 0.0281(9) 0.0276(9) 0.0033(7) 0.0090(6) 0.0045(7) C10 0.0224(8) 0.0294(9) 0.0317(9) 0.0008(7) 0.0032(7) -0.0004(7) C11 0.0259(9) 0.0330(10) 0.0504(12) 0.0050(9) -0.0019(8) 0.0014(8) C12 0.0278(8) 0.0285(9) 0.0185(8) 0.0039(7) 0.0061(6) 0.0039(7) C15 0.0304(9) 0.0282(9) 0.0170(8) -0.0007(6) 0.0033(6) 0.0062(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O4 2.7426(12) . ? K1 F6 2.7437(12) 3_556 ? K1 O3 2.7976(12) . ? K1 O1 2.8619(12) . ? K1 O2 2.8682(12) . ? K1 F2 2.9029(13) . ? K1 F1 2.9649(13) . ? K1 F3 2.9821(12) . ? K1 N1 3.0237(13) . ? K1 F2 3.3264(15) 3_556 ? K1 C6 3.5031(18) . ? K1 P1 3.5829(5) . ? P1 F5 1.5852(11) . ? P1 F4 1.5929(11) . ? P1 F3 1.5939(11) . ? P1 F1 1.5951(11) . ? P1 F2 1.6012(11) . ? P1 F6 1.6037(11) . ? F2 K1 3.3264(15) 3_556 ? F6 K1 2.7437(12) 3_556 ? O1 C12 1.425(2) . ? O1 C1 1.4258(19) . ? O2 C2 1.422(2) . ? O2 C3 1.434(2) . ? O3 C4 1.420(2) . ? O3 C5 1.425(2) . ? O4 C6 1.432(2) . ? O4 C7 1.434(2) . ? N1 C9 1.473(2) . ? N1 C8 1.474(2) . ? N1 C15 1.475(2) . ? C1 C2 1.500(3) . ? C3 C4 1.505(3) . ? C5 C6 1.506(3) . ? C7 C8 1.512(2) . ? C9 C10 1.496(2) . ? C10 C11 1.316(3) . ? C12 C15 1.513(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 O4 K1 F6 146.34(4) . 3_556 ? O4 K1 O3 62.54(3) . . ? F6 K1 O3 146.61(4) 3_556 . ? O4 K1 O1 96.05(3) . . ? F6 K1 O1 75.12(3) 3_556 . ? O3 K1 O1 87.85(4) . . ? O4 K1 O2 116.78(3) . . ? F6 K1 O2 86.70(4) 3_556 . ? O3 K1 O2 59.98(3) . . ? O1 K1 O2 58.61(3) . . ? O4 K1 F2 114.57(3) . . ? F6 K1 F2 80.11(3) 3_556 . ? O3 K1 F2 103.73(4) . . ? O1 K1 F2 149.29(3) . . ? O2 K1 F2 102.53(3) . . ? O4 K1 F1 75.36(4) . . ? F6 K1 F1 125.17(4) 3_556 . ? O3 K1 F1 66.20(3) . . ? O1 K1 F1 153.86(3) . . ? O2 K1 F1 102.73(3) . . ? F2 K1 F1 45.06(3) . . ? O4 K1 F3 75.84(3) . . ? F6 K1 F3 100.22(3) 3_556 . ? O3 K1 F3 105.54(3) . . ? O1 K1 F3 158.12(3) . . ? O2 K1 F3 143.17(3) . . ? F2 K1 F3 44.77(3) . . ? F1 K1 F3 44.28(3) . . ? O4 K1 N1 60.95(3) . . ? F6 K1 N1 87.10(4) 3_556 . ? O3 K1 N1 109.72(4) . . ? O1 K1 N1 61.02(3) . . ? O2 K1 N1 118.84(3) . . ? F2 K1 N1 135.82(4) . . ? F1 K1 N1 129.20(4) . . ? F3 K1 N1 97.72(3) . . ? O4 K1 F2 120.00(3) . 3_556 ? F6 K1 F2 42.44(3) 3_556 3_556 ? O3 K1 F2 158.47(3) . 3_556 ? O1 K1 F2 112.22(3) . 3_556 ? O2 K1 F2 123.18(3) . 3_556 ? F2 K1 F2 55.00(4) . 3_556 ? F1 K1 F2 93.14(3) . 3_556 ? F3 K1 F2 58.17(3) . 3_556 ? N1 K1 F2 87.71(3) . 3_556 ? O4 K1 C6 22.57(4) . . ? F6 K1 C6 168.89(4) 3_556 . ? O3 K1 C6 42.69(4) . . ? O1 K1 C6 102.87(4) . . ? O2 K1 C6 101.67(4) . . ? F2 K1 C6 104.82(4) . . ? F1 K1 C6 60.48(4) . . ? F3 K1 C6 77.51(4) . . ? N1 K1 C6 82.48(4) . . ? F2 K1 C6 132.76(4) 3_556 . ? O4 K1 P1 88.59(3) . . ? F6 K1 P1 102.25(3) 3_556 . ? O3 K1 P1 92.20(3) . . ? O1 K1 P1 174.78(3) . . ? O2 K1 P1 117.07(3) . . ? F2 K1 P1 25.98(2) . . ? F1 K1 P1 26.08(2) . . ? F3 K1 P1 26.10(2) . . ? N1 K1 P1 123.69(3) . . ? F2 K1 P1 67.08(2) 3_556 . ? C6 K1 P1 80.58(3) . . ? F5 P1 F4 90.60(7) . . ? F5 P1 F3 90.43(7) . . ? F4 P1 F3 178.89(7) . . ? F5 P1 F1 91.00(7) . . ? F4 P1 F1 90.25(7) . . ? F3 P1 F1 89.30(6) . . ? F5 P1 F2 179.38(7) . . ? F4 P1 F2 89.83(6) . . ? F3 P1 F2 89.15(6) . . ? F1 P1 F2 89.45(7) . . ? F5 P1 F6 89.70(6) . . ? F4 P1 F6 90.29(7) . . ? F3 P1 F6 90.15(6) . . ? F1 P1 F6 179.11(7) . . ? F2 P1 F6 89.84(7) . . ? F5 P1 K1 127.46(5) . . ? F4 P1 K1 123.55(5) . . ? F3 P1 K1 55.40(4) . . ? F1 P1 K1 54.79(5) . . ? F2 P1 K1 52.57(5) . . ? F6 P1 K1 124.33(5) . . ? P1 F1 K1 99.14(6) . . ? P1 F2 K1 101.46(6) . . ? P1 F2 K1 99.70(6) . 3_556 ? K1 F2 K1 125.00(4) . 3_556 ? P1 F3 K1 98.49(5) . . ? P1 F6 K1 127.23(7) . 3_556 ? C12 O1 C1 112.88(13) . . ? C12 O1 K1 107.59(9) . . ? C1 O1 K1 107.87(9) . . ? C2 O2 C3 113.09(14) . . ? C2 O2 K1 117.76(9) . . ? C3 O2 K1 110.81(10) . . ? C4 O3 C5 111.99(14) . . ? C4 O3 K1 120.60(10) . . ? C5 O3 K1 116.32(10) . . ? C6 O4 C7 114.73(13) . . ? C6 O4 K1 110.11(10) . . ? C7 O4 K1 114.15(10) . . ? C9 N1 C8 110.48(12) . . ? C9 N1 C15 109.02(13) . . ? C8 N1 C15 110.46(13) . . ? C9 N1 K1 110.54(9) . . ? C8 N1 K1 108.15(9) . . ? C15 N1 K1 108.17(9) . . ? O1 C1 C2 107.43(14) . . ? O2 C2 C1 108.25(14) . . ? O2 C3 C4 112.49(15) . . ? O3 C4 C3 108.73(15) . . ? O3 C5 C6 108.93(14) . . ? O4 C6 C5 113.68(15) . . ? O4 C6 K1 47.32(7) . . ? C5 C6 K1 83.76(10) . . ? O4 C7 C8 107.38(13) . . ? N1 C8 C7 112.97(13) . . ? N1 C9 C10 113.35(14) . . ? C11 C10 C9 123.59(18) . . ? O1 C12 C15 107.42(14) . . ? N1 C15 C12 113.09(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 K1 P1 F5 -0.74(6) . . . . ? F6 K1 P1 F5 147.11(7) 3_556 . . . ? O3 K1 P1 F5 -63.19(7) . . . . ? O1 K1 P1 F5 -153.7(3) . . . . ? O2 K1 P1 F5 -120.32(6) . . . . ? F2 K1 P1 F5 179.21(9) . . . . ? F1 K1 P1 F5 -59.09(8) . . . . ? F3 K1 P1 F5 58.86(8) . . . . ? N1 K1 P1 F5 52.38(7) . . . . ? F2 K1 P1 F5 122.86(6) 3_556 . . . ? C6 K1 P1 F5 -21.95(7) . . . . ? O4 K1 P1 F4 120.85(6) . . . . ? F6 K1 P1 F4 -91.30(6) 3_556 . . . ? O3 K1 P1 F4 58.40(6) . . . . ? O1 K1 P1 F4 -32.1(3) . . . . ? O2 K1 P1 F4 1.27(6) . . . . ? F2 K1 P1 F4 -59.20(8) . . . . ? F1 K1 P1 F4 62.50(8) . . . . ? F3 K1 P1 F4 -179.55(8) . . . . ? N1 K1 P1 F4 173.97(6) . . . . ? F2 K1 P1 F4 -115.55(6) 3_556 . . . ? C6 K1 P1 F4 99.64(6) . . . . ? O4 K1 P1 F3 -59.60(6) . . . . ? F6 K1 P1 F3 88.25(6) 3_556 . . . ? O3 K1 P1 F3 -122.05(6) . . . . ? O1 K1 P1 F3 147.4(3) . . . . ? O2 K1 P1 F3 -179.18(6) . . . . ? F2 K1 P1 F3 120.35(8) . . . . ? F1 K1 P1 F3 -117.95(8) . . . . ? N1 K1 P1 F3 -6.48(6) . . . . ? F2 K1 P1 F3 64.00(6) 3_556 . . . ? C6 K1 P1 F3 -80.82(6) . . . . ? O4 K1 P1 F1 58.35(6) . . . . ? F6 K1 P1 F1 -153.80(7) 3_556 . . . ? O3 K1 P1 F1 -4.10(6) . . . . ? O1 K1 P1 F1 -94.6(3) . . . . ? O2 K1 P1 F1 -61.23(7) . . . . ? F2 K1 P1 F1 -121.70(9) . . . . ? F3 K1 P1 F1 117.95(8) . . . . ? N1 K1 P1 F1 111.46(7) . . . . ? F2 K1 P1 F1 -178.05(6) 3_556 . . . ? C6 K1 P1 F1 37.13(7) . . . . ? O4 K1 P1 F2 -179.95(7) . . . . ? F6 K1 P1 F2 -32.10(7) 3_556 . . . ? O3 K1 P1 F2 117.60(7) . . . . ? O1 K1 P1 F2 27.1(3) . . . . ? O2 K1 P1 F2 60.46(7) . . . . ? F1 K1 P1 F2 121.70(9) . . . . ? F3 K1 P1 F2 -120.35(8) . . . . ? N1 K1 P1 F2 -126.84(7) . . . . ? F2 K1 P1 F2 -56.35(7) 3_556 . . . ? C6 K1 P1 F2 158.83(7) . . . . ? O4 K1 P1 F6 -121.75(7) . . . . ? F6 K1 P1 F6 26.10(9) 3_556 . . . ? O3 K1 P1 F6 175.80(7) . . . . ? O1 K1 P1 F6 85.3(3) . . . . ? O2 K1 P1 F6 118.67(7) . . . . ? F2 K1 P1 F6 58.20(9) . . . . ? F1 K1 P1 F6 179.90(9) . . . . ? F3 K1 P1 F6 -62.15(8) . . . . ? N1 K1 P1 F6 -68.63(7) . . . . ? F2 K1 P1 F6 1.85(6) 3_556 . . . ? C6 K1 P1 F6 -142.96(7) . . . . ? F5 P1 F1 K1 137.07(6) . . . . ? F4 P1 F1 K1 -132.33(6) . . . . ? F3 P1 F1 K1 46.65(6) . . . . ? F2 P1 F1 K1 -42.50(5) . . . . ? F6 P1 F1 K1 -5(5) . . . . ? O4 K1 F1 P1 -118.42(6) . . . . ? F6 K1 F1 P1 31.86(8) 3_556 . . . ? O3 K1 F1 P1 175.52(7) . . . . ? O1 K1 F1 P1 168.13(6) . . . . ? O2 K1 F1 P1 126.85(6) . . . . ? F2 K1 F1 P1 31.76(5) . . . . ? F3 K1 F1 P1 -33.83(5) . . . . ? N1 K1 F1 P1 -87.81(7) . . . . ? F2 K1 F1 P1 1.80(6) 3_556 . . . ? C6 K1 F1 P1 -136.81(7) . . . . ? F5 P1 F2 K1 -92(7) . . . . ? F4 P1 F2 K1 134.29(6) . . . . ? F3 P1 F2 K1 -45.27(6) . . . . ? F1 P1 F2 K1 44.04(6) . . . . ? F6 P1 F2 K1 -135.42(6) . . . . ? F5 P1 F2 K1 37(7) . . . 3_556 ? F4 P1 F2 K1 -96.78(5) . . . 3_556 ? F3 P1 F2 K1 83.66(5) . . . 3_556 ? F1 P1 F2 K1 172.97(5) . . . 3_556 ? F6 P1 F2 K1 -6.49(6) . . . 3_556 ? K1 P1 F2 K1 128.93(6) . . . 3_556 ? O4 K1 F2 P1 0.05(7) . . . . ? F6 K1 F2 P1 148.19(6) 3_556 . . . ? O3 K1 F2 P1 -65.73(6) . . . . ? O1 K1 F2 P1 -175.35(5) . . . . ? O2 K1 F2 P1 -127.48(6) . . . . ? F1 K1 F2 P1 -31.89(5) . . . . ? F3 K1 F2 P1 32.62(5) . . . . ? N1 K1 F2 P1 72.85(8) . . . . ? F2 K1 F2 P1 110.60(8) 3_556 . . . ? C6 K1 F2 P1 -21.62(7) . . . . ? O4 K1 F2 K1 -110.55(4) . . . 3_556 ? F6 K1 F2 K1 37.58(4) 3_556 . . 3_556 ? O3 K1 F2 K1 -176.33(4) . . . 3_556 ? O1 K1 F2 K1 74.04(8) . . . 3_556 ? O2 K1 F2 K1 121.92(4) . . . 3_556 ? F1 K1 F2 K1 -142.49(7) . . . 3_556 ? F3 K1 F2 K1 -77.98(5) . . . 3_556 ? N1 K1 F2 K1 -37.75(7) . . . 3_556 ? F2 K1 F2 K1 0.0 3_556 . . 3_556 ? C6 K1 F2 K1 -132.22(5) . . . 3_556 ? P1 K1 F2 K1 -110.60(8) . . . 3_556 ? F5 P1 F3 K1 -137.20(5) . . . . ? F4 P1 F3 K1 20(4) . . . . ? F1 P1 F3 K1 -46.20(6) . . . . ? F2 P1 F3 K1 43.26(6) . . . . ? F6 P1 F3 K1 133.10(5) . . . . ? O4 K1 F3 P1 117.21(6) . . . . ? F6 K1 F3 P1 -97.01(5) 3_556 . . . ? O3 K1 F3 P1 61.53(6) . . . . ? O1 K1 F3 P1 -172.45(7) . . . . ? O2 K1 F3 P1 1.21(9) . . . . ? F2 K1 F3 P1 -32.46(5) . . . . ? F1 K1 F3 P1 33.79(5) . . . . ? N1 K1 F3 P1 174.56(5) . . . . ? F2 K1 F3 P1 -103.01(6) 3_556 . . . ? C6 K1 F3 P1 94.07(6) . . . . ? F5 P1 F6 K1 -169.81(8) . . . 3_556 ? F4 P1 F6 K1 99.59(8) . . . 3_556 ? F3 P1 F6 K1 -79.39(8) . . . 3_556 ? F1 P1 F6 K1 -28(5) . . . 3_556 ? F2 P1 F6 K1 9.76(8) . . . 3_556 ? K1 P1 F6 K1 -32.68(10) . . . 3_556 ? O4 K1 O1 C12 85.81(10) . . . . ? F6 K1 O1 C12 -61.11(10) 3_556 . . . ? O3 K1 O1 C12 147.90(10) . . . . ? O2 K1 O1 C12 -156.41(11) . . . . ? F2 K1 O1 C12 -98.40(11) . . . . ? F1 K1 O1 C12 154.66(10) . . . . ? F3 K1 O1 C12 19.14(15) . . . . ? N1 K1 O1 C12 33.90(9) . . . . ? F2 K1 O1 C12 -40.10(10) 3_556 . . . ? C6 K1 O1 C12 107.64(10) . . . . ? P1 K1 O1 C12 -121.4(3) . . . . ? O4 K1 O1 C1 -152.13(10) . . . . ? F6 K1 O1 C1 60.95(10) 3_556 . . . ? O3 K1 O1 C1 -90.04(10) . . . . ? O2 K1 O1 C1 -34.35(9) . . . . ? F2 K1 O1 C1 23.67(13) . . . . ? F1 K1 O1 C1 -83.27(13) . . . . ? F3 K1 O1 C1 141.21(11) . . . . ? N1 K1 O1 C1 155.96(11) . . . . ? F2 K1 O1 C1 81.96(10) 3_556 . . . ? C6 K1 O1 C1 -130.30(10) . . . . ? P1 K1 O1 C1 0.7(3) . . . . ? O4 K1 O2 C2 80.75(12) . . . . ? F6 K1 O2 C2 -74.05(11) 3_556 . . . ? O3 K1 O2 C2 108.09(12) . . . . ? O1 K1 O2 C2 0.52(11) . . . . ? F2 K1 O2 C2 -153.15(11) . . . . ? F1 K1 O2 C2 160.61(11) . . . . ? F3 K1 O2 C2 -176.72(10) . . . . ? N1 K1 O2 C2 10.81(12) . . . . ? F2 K1 O2 C2 -96.98(11) 3_556 . . . ? C6 K1 O2 C2 98.59(12) . . . . ? P1 K1 O2 C2 -176.12(11) . . . . ? O4 K1 O2 C3 -51.63(12) . . . . ? F6 K1 O2 C3 153.57(11) 3_556 . . . ? O3 K1 O2 C3 -24.30(11) . . . . ? O1 K1 O2 C3 -131.87(12) . . . . ? F2 K1 O2 C3 74.47(11) . . . . ? F1 K1 O2 C3 28.22(12) . . . . ? F3 K1 O2 C3 50.89(13) . . . . ? N1 K1 O2 C3 -121.58(11) . . . . ? F2 K1 O2 C3 130.64(11) 3_556 . . . ? C6 K1 O2 C3 -33.80(12) . . . . ? P1 K1 O2 C3 51.49(12) . . . . ? O4 K1 O3 C4 146.39(14) . . . . ? F6 K1 O3 C4 -9.97(17) 3_556 . . . ? O1 K1 O3 C4 48.43(14) . . . . ? O2 K1 O3 C4 -6.10(13) . . . . ? F2 K1 O3 C4 -102.80(14) . . . . ? F1 K1 O3 C4 -128.32(14) . . . . ? F3 K1 O3 C4 -149.12(13) . . . . ? N1 K1 O3 C4 106.53(13) . . . . ? F2 K1 O3 C4 -111.01(15) 3_556 . . . ? C6 K1 O3 C4 160.11(16) . . . . ? P1 K1 O3 C4 -126.35(13) . . . . ? O4 K1 O3 C5 5.32(11) . . . . ? F6 K1 O3 C5 -151.03(11) 3_556 . . . ? O1 K1 O3 C5 -92.63(12) . . . . ? O2 K1 O3 C5 -147.16(13) . . . . ? F2 K1 O3 C5 116.14(12) . . . . ? F1 K1 O3 C5 90.62(12) . . . . ? F3 K1 O3 C5 69.81(12) . . . . ? N1 K1 O3 C5 -34.54(13) . . . . ? F2 K1 O3 C5 107.93(14) 3_556 . . . ? C6 K1 O3 C5 19.05(11) . . . . ? P1 K1 O3 C5 92.59(12) . . . . ? F6 K1 O4 C6 -178.69(10) 3_556 . . . ? O3 K1 O4 C6 24.78(10) . . . . ? O1 K1 O4 C6 109.18(10) . . . . ? O2 K1 O4 C6 51.39(11) . . . . ? F2 K1 O4 C6 -68.47(11) . . . . ? F1 K1 O4 C6 -45.69(10) . . . . ? F3 K1 O4 C6 -91.48(10) . . . . ? N1 K1 O4 C6 161.14(11) . . . . ? F2 K1 O4 C6 -130.80(10) 3_556 . . . ? P1 K1 O4 C6 -68.44(10) . . . . ? F6 K1 O4 C7 50.59(13) 3_556 . . . ? O3 K1 O4 C7 -105.94(11) . . . . ? O1 K1 O4 C7 -21.54(10) . . . . ? O2 K1 O4 C7 -79.33(11) . . . . ? F2 K1 O4 C7 160.81(10) . . . . ? F1 K1 O4 C7 -176.41(11) . . . . ? F3 K1 O4 C7 137.79(10) . . . . ? N1 K1 O4 C7 30.41(10) . . . . ? F2 K1 O4 C7 98.48(10) 3_556 . . . ? C6 K1 O4 C7 -130.72(16) . . . . ? P1 K1 O4 C7 160.84(10) . . . . ? O4 K1 N1 C9 125.12(10) . . . . ? F6 K1 N1 C9 -43.84(10) 3_556 . . . ? O3 K1 N1 C9 165.71(9) . . . . ? O1 K1 N1 C9 -118.42(10) . . . . ? O2 K1 N1 C9 -128.46(9) . . . . ? F2 K1 N1 C9 28.76(12) . . . . ? F1 K1 N1 C9 90.82(10) . . . . ? F3 K1 N1 C9 56.09(10) . . . . ? F2 K1 N1 C9 -1.36(10) 3_556 . . . ? C6 K1 N1 C9 132.31(10) . . . . ? P1 K1 N1 C9 58.96(10) . . . . ? O4 K1 N1 C8 4.06(9) . . . . ? F6 K1 N1 C8 -164.90(10) 3_556 . . . ? O3 K1 N1 C8 44.64(10) . . . . ? O1 K1 N1 C8 120.52(10) . . . . ? O2 K1 N1 C8 110.48(9) . . . . ? F2 K1 N1 C8 -92.30(10) . . . . ? F1 K1 N1 C8 -30.24(11) . . . . ? F3 K1 N1 C8 -64.97(9) . . . . ? F2 K1 N1 C8 -122.42(9) 3_556 . . . ? C6 K1 N1 C8 11.25(9) . . . . ? P1 K1 N1 C8 -62.10(10) . . . . ? O4 K1 N1 C15 -115.58(11) . . . . ? F6 K1 N1 C15 75.45(10) 3_556 . . . ? O3 K1 N1 C15 -75.00(10) . . . . ? O1 K1 N1 C15 0.87(9) . . . . ? O2 K1 N1 C15 -9.17(11) . . . . ? F2 K1 N1 C15 148.06(9) . . . . ? F1 K1 N1 C15 -149.88(9) . . . . ? F3 K1 N1 C15 175.38(10) . . . . ? F2 K1 N1 C15 117.93(10) 3_556 . . . ? C6 K1 N1 C15 -108.39(10) . . . . ? P1 K1 N1 C15 178.25(9) . . . . ? C12 O1 C1 C2 -173.89(13) . . . . ? K1 O1 C1 C2 67.37(14) . . . . ? C3 O2 C2 C1 162.90(14) . . . . ? K1 O2 C2 C1 31.55(17) . . . . ? O1 C1 C2 O2 -66.96(17) . . . . ? C2 O2 C3 C4 -80.9(2) . . . . ? K1 O2 C3 C4 53.80(19) . . . . ? C5 O3 C4 C3 176.44(16) . . . . ? K1 O3 C4 C3 33.9(2) . . . . ? O2 C3 C4 O3 -58.9(2) . . . . ? C4 O3 C5 C6 -177.28(16) . . . . ? K1 O3 C5 C6 -32.97(18) . . . . ? C7 O4 C6 C5 74.86(19) . . . . ? K1 O4 C6 C5 -55.55(17) . . . . ? C7 O4 C6 K1 130.41(15) . . . . ? O3 C5 C6 O4 60.6(2) . . . . ? O3 C5 C6 K1 23.07(13) . . . . ? F6 K1 C6 O4 3.8(3) 3_556 . . . ? O3 K1 C6 O4 -146.74(13) . . . . ? O1 K1 C6 O4 -74.46(10) . . . . ? O2 K1 C6 O4 -134.57(10) . . . . ? F2 K1 C6 O4 118.94(10) . . . . ? F1 K1 C6 O4 127.28(11) . . . . ? F3 K1 C6 O4 83.11(10) . . . . ? N1 K1 C6 O4 -16.56(10) . . . . ? F2 K1 C6 O4 63.24(11) 3_556 . . . ? P1 K1 C6 O4 109.53(10) . . . . ? O4 K1 C6 C5 130.57(17) . . . . ? F6 K1 C6 C5 134.3(2) 3_556 . . . ? O3 K1 C6 C5 -16.17(10) . . . . ? O1 K1 C6 C5 56.11(11) . . . . ? O2 K1 C6 C5 -4.01(11) . . . . ? F2 K1 C6 C5 -110.49(11) . . . . ? F1 K1 C6 C5 -102.15(11) . . . . ? F3 K1 C6 C5 -146.32(11) . . . . ? N1 K1 C6 C5 114.00(11) . . . . ? F2 K1 C6 C5 -166.19(10) 3_556 . . . ? P1 K1 C6 C5 -119.90(11) . . . . ? C6 O4 C7 C8 168.79(14) . . . . ? K1 O4 C7 C8 -62.80(15) . . . . ? C9 N1 C8 C7 -157.59(14) . . . . ? C15 N1 C8 C7 81.70(16) . . . . ? K1 N1 C8 C7 -36.50(15) . . . . ? O4 C7 C8 N1 67.35(17) . . . . ? C8 N1 C9 C10 63.96(18) . . . . ? C15 N1 C9 C10 -174.48(14) . . . . ? K1 N1 C9 C10 -55.70(16) . . . . ? N1 C9 C10 C11 -128.95(19) . . . . ? C1 O1 C12 C15 173.11(13) . . . . ? K1 O1 C12 C15 -68.00(13) . . . . ? C9 N1 C15 C12 85.50(17) . . . . ? C8 N1 C15 C12 -152.92(14) . . . . ? K1 N1 C15 C12 -34.74(16) . . . . ? O1 C12 C15 N1 72.90(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1A F6 0.97(2) 2.76(2) 3.480(2) 131.6(15) 3_556 C3 H3B F1 0.99(2) 2.71(2) 3.259(2) 115.0(16) 3_656 C4 H4B F1 0.99(2) 2.83(2) 3.477(2) 123.7(16) 3_656 C4 H4B F4 0.99(2) 2.79(2) 3.353(2) 116.4(16) 3_656 C5 H5B F5 1.03(2) 2.78(2) 3.173(2) 103.0(14) 4_666 C6 H6B F1 1.023(19) 2.471(19) 3.290(2) 136.7(14) . C6 H6A F5 1.01(2) 2.52(2) 3.233(2) 127.5(16) 4_666 C9 H9B F4 0.99(2) 2.66(2) 3.457(2) 138.5(14) 3_556 C10 H10 F2 0.96(2) 2.60(2) 3.328(2) 132.3(16) 3_556 C11 H11A F5 0.94(3) 2.62(3) 3.236(2) 123.1(19) 4_566 C12 H12A F4 0.973(19) 2.519(18) 3.2203(19) 129.0(14) 1_556 C12 H12B F6 0.967(19) 2.750(19) 3.478(2) 132.5(14) 3_556 C15 H15A F4 0.95(2) 2.61(2) 3.274(2) 126.9(14) 1_556 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.391 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.062 #===END data_pbnoal15 #(compound10) _database_code_CSD 180579 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H25 N3 O10 Pb' _chemical_formula_weight 590.55 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2947(2) _cell_length_b 13.6796(6) _cell_length_c 15.3903(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.365(2) _cell_angle_gamma 90.00 _cell_volume 1944.78(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.017 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 8.731 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.2741 _exptl_absorpt_correction_T_max 0.6693 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11648 _diffrn_reflns_av_R_equivalents 0.0687 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4437 _reflns_number_gt 3981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+1.8293P] 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 SHELXL _refine_ls_extinction_coef 0.00191(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4437 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Pb1 Pb 0.922744(12) 0.821368(10) 0.190378(8) 0.01365(7) Uani 1 1 d . A . O1 O 0.7821(2) 0.8896(2) 0.31656(16) 0.0189(5) Uani 1 1 d . . . N1 N 1.0710(3) 0.9536(3) 0.2951(2) 0.0182(7) Uani 1 1 d . . . C1 C 1.3409(4) 0.9064(4) 0.4789(3) 0.0324(10) Uani 1 1 d . . . H1A H 1.3078 0.8429 0.4919 0.039 Uiso 1 1 calc R . . H1B H 1.4041 0.9409 0.5210 0.039 Uiso 1 1 calc R . . O2 O 0.6396(3) 0.7664(2) 0.19280(18) 0.0204(6) Uani 1 1 d . . . N2 N 0.9833(3) 0.6213(2) 0.2791(2) 0.0210(7) Uani 1 1 d . A 1 C2 C 1.2993(4) 0.9465(3) 0.4028(3) 0.0286(10) Uani 1 1 d . . . H2 H 1.3336 1.0100 0.3910 0.034 Uiso 1 1 calc R . . O3 O 0.7321(3) 0.8600(2) 0.04491(18) 0.0207(6) Uani 1 1 d . . . N3 N 1.1567(3) 0.7448(3) 0.0849(2) 0.0203(7) Uani 1 1 d . A 1 C3 C 1.2001(4) 0.8959(3) 0.3338(3) 0.0251(9) Uani 1 1 d . . . H3A H 1.1649 0.8351 0.3593 0.030 Uiso 1 1 calc R . . H3B H 1.2571 0.8767 0.2859 0.030 Uiso 1 1 calc R . . O4 O 0.9327(3) 0.9998(2) 0.12253(17) 0.0203(6) Uani 1 1 d . . . C4 C 0.9835(4) 0.9892(3) 0.3644(2) 0.0198(8) Uani 1 1 d . . . H4A H 0.9271 1.0472 0.3423 0.024 Uiso 1 1 calc R . . H4B H 1.0497 1.0098 0.4160 0.024 Uiso 1 1 calc R . . O5 O 0.9742(3) 0.7009(2) 0.32026(19) 0.0255(6) Uani 1 1 d . . . C5 C 0.8811(4) 0.9127(3) 0.3922(2) 0.0199(8) Uani 1 1 d . . . H5A H 0.9354 0.8536 0.4136 0.024 Uiso 1 1 calc R . . H5B H 0.8279 0.9382 0.4396 0.024 Uiso 1 1 calc R . . O6 O 0.9467(3) 0.6213(2) 0.19773(18) 0.0346(8) Uani 1 1 d . . . C6 C 0.6620(4) 0.8301(3) 0.3365(3) 0.0221(9) Uani 1 1 d . . . H6A H 0.6109 0.8619 0.3820 0.027 Uiso 1 1 calc R . . H6B H 0.6969 0.7653 0.3584 0.027 Uiso 1 1 calc R . . O7 O 1.0270(3) 0.5465(2) 0.31751(19) 0.0307(7) Uani 1 1 d . A 1 C7 C 0.5626(4) 0.8188(3) 0.2541(3) 0.0227(9) Uani 1 1 d . . . H7A H 0.4748 0.7822 0.2657 0.027 Uiso 1 1 calc R . . H7B H 0.5326 0.8838 0.2303 0.027 Uiso 1 1 calc R . . O8 O 1.1865(3) 0.7678(3) 0.16417(19) 0.0334(8) Uani 1 1 d . . . C8 C 0.5623(4) 0.7614(3) 0.1064(3) 0.0260(9) Uani 1 1 d . . . H8A H 0.4582 0.7510 0.1114 0.031 Uiso 1 1 calc R . . H8B H 0.5978 0.7046 0.0751 0.031 Uiso 1 1 calc R . . O9 O 1.0436(3) 0.7794(2) 0.04310(19) 0.0261(6) Uani 1 1 d . . . C9 C 0.5800(4) 0.8524(3) 0.0538(3) 0.0227(9) Uani 1 1 d . . . H9A H 0.5231 0.8474 -0.0043 0.027 Uiso 1 1 calc R . . H9B H 0.5466 0.9105 0.0843 0.027 Uiso 1 1 calc R . . O10 O 1.2341(3) 0.6869(2) 0.0496(2) 0.0357(8) Uani 1 1 d . A 1 C10 C 0.7709(4) 0.9474(3) 0.0020(3) 0.0276(9) Uani 1 1 d . . . H10A H 0.6893 0.9673 -0.0412 0.033 Uiso 1 1 calc R . . H10B H 0.8551 0.9336 -0.0302 0.033 Uiso 1 1 calc R . . C11 C 0.8079(4) 1.0300(3) 0.0643(3) 0.0264(9) Uani 1 1 d . . . H11A H 0.8304 1.0896 0.0320 0.032 Uiso 1 1 calc R . . H11B H 0.7254 1.0442 0.0979 0.032 Uiso 1 1 calc R . . C12 C 0.9879(4) 1.0762(3) 0.1808(3) 0.0245(9) Uani 1 1 d . . . H12A H 0.9110 1.0998 0.2151 0.029 Uiso 1 1 calc R . . H12B H 1.0211 1.1318 0.1470 0.029 Uiso 1 1 calc R . . C13 C 1.1131(4) 1.0357(3) 0.2413(3) 0.0229(8) Uani 1 1 d . . . H13A H 1.1897 1.0135 0.2060 0.027 Uiso 1 1 calc R . . H13B H 1.1542 1.0886 0.2804 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01530(10) 0.01178(10) 0.01402(10) -0.00013(5) 0.00225(6) 0.00165(5) O1 0.0185(12) 0.0217(15) 0.0174(13) -0.0005(12) 0.0065(10) -0.0026(11) N1 0.0170(15) 0.0191(18) 0.0190(15) -0.0023(14) 0.0049(12) -0.0013(12) C1 0.027(2) 0.040(3) 0.030(2) -0.001(2) 0.0001(17) 0.002(2) O2 0.0182(12) 0.0184(15) 0.0246(14) 0.0022(12) 0.0024(11) 0.0008(11) N2 0.0242(16) 0.0150(17) 0.0241(18) 0.0027(14) 0.0047(13) -0.0011(13) C2 0.0239(19) 0.027(2) 0.035(2) -0.008(2) 0.0021(17) -0.0038(18) O3 0.0167(12) 0.0226(15) 0.0226(14) -0.0002(12) 0.0019(10) 0.0007(11) N3 0.0157(14) 0.0238(18) 0.0227(17) -0.0023(15) 0.0086(12) -0.0002(14) C3 0.0203(18) 0.025(2) 0.029(2) -0.0069(19) 0.0011(15) 0.0038(17) O4 0.0240(13) 0.0164(14) 0.0200(14) 0.0005(11) 0.0001(10) 0.0028(11) C4 0.0212(17) 0.021(2) 0.0182(18) -0.0074(16) 0.0044(14) 0.0008(15) O5 0.0384(16) 0.0188(14) 0.0189(15) -0.0022(13) 0.0010(12) 0.0045(13) C5 0.0252(18) 0.022(2) 0.0130(17) 0.0003(16) 0.0033(14) 0.0027(16) O6 0.062(2) 0.0214(18) 0.0184(15) -0.0030(13) -0.0032(14) 0.0045(15) C6 0.0191(19) 0.024(2) 0.025(2) 0.0069(17) 0.0110(16) -0.0009(16) O7 0.0405(16) 0.0151(15) 0.0348(18) 0.0072(13) -0.0032(13) 0.0031(13) C7 0.0169(19) 0.024(2) 0.029(2) 0.0029(17) 0.0076(16) 0.0017(15) O8 0.0255(14) 0.049(2) 0.0250(16) -0.0158(15) 0.0009(12) 0.0056(14) C8 0.0248(19) 0.027(2) 0.025(2) -0.0040(19) -0.0022(16) -0.0070(17) O9 0.0243(14) 0.0295(18) 0.0249(15) 0.0043(13) 0.0038(11) 0.0062(12) C9 0.0168(18) 0.027(2) 0.024(2) -0.0008(18) -0.0001(15) 0.0022(16) O10 0.0250(16) 0.046(2) 0.0362(19) -0.0239(15) 0.0049(13) 0.0068(13) C10 0.0241(19) 0.040(3) 0.0183(19) 0.0110(19) 0.0013(15) 0.0024(18) C11 0.0221(18) 0.023(2) 0.034(2) 0.0160(19) 0.0027(16) 0.0042(17) C12 0.035(2) 0.014(2) 0.027(2) -0.0032(17) 0.0113(17) -0.0059(17) C13 0.0238(18) 0.020(2) 0.025(2) -0.0068(18) 0.0063(15) -0.0067(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O5 2.594(3) . ? Pb1 O1 2.630(2) . ? Pb1 O8 2.632(3) . ? Pb1 O4 2.661(3) . ? Pb1 N1 2.697(3) . ? Pb1 O9 2.701(3) . ? Pb1 O2 2.742(2) . ? Pb1 O6 2.747(3) . ? Pb1 O3 2.748(3) . ? O1 C5 1.437(4) . ? O1 C6 1.441(4) . ? N1 C13 1.474(5) . ? N1 C4 1.492(5) . ? N1 C3 1.503(5) . ? C1 C2 1.312(6) . ? O2 C7 1.438(5) . ? O2 C8 1.441(5) . ? N2 O7 1.229(4) . ? N2 O6 1.260(4) . ? N2 O5 1.267(4) . ? C2 C3 1.496(5) . ? O3 C10 1.431(5) . ? O3 C9 1.440(4) . ? N3 O10 1.235(4) . ? N3 O8 1.261(4) . ? N3 O9 1.261(4) . ? O4 C12 1.434(5) . ? O4 C11 1.445(4) . ? C4 C5 1.507(5) . ? C6 C7 1.492(6) . ? C8 C9 1.503(6) . ? C10 C11 1.497(6) . ? C12 C13 1.513(6) . ? 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 O5 Pb1 O1 73.78(9) . . ? O5 Pb1 O8 81.13(10) . . ? O1 Pb1 O8 139.45(8) . . ? O5 Pb1 O4 150.92(8) . . ? O1 Pb1 O4 90.35(8) . . ? O8 Pb1 O4 97.01(10) . . ? O5 Pb1 N1 85.83(10) . . ? O1 Pb1 N1 65.40(8) . . ? O8 Pb1 N1 81.70(9) . . ? O4 Pb1 N1 65.28(9) . . ? O5 Pb1 O9 116.95(9) . . ? O1 Pb1 O9 169.24(8) . . ? O8 Pb1 O9 48.01(8) . . ? O4 Pb1 O9 80.21(9) . . ? N1 Pb1 O9 114.30(9) . . ? O5 Pb1 O2 84.85(9) . . ? O1 Pb1 O2 62.01(8) . . ? O8 Pb1 O2 146.86(10) . . ? O4 Pb1 O2 109.41(8) . . ? N1 Pb1 O2 127.12(8) . . ? O9 Pb1 O2 116.26(8) . . ? O5 Pb1 O6 47.78(9) . . ? O1 Pb1 O6 111.57(9) . . ? O8 Pb1 O6 69.89(11) . . ? O4 Pb1 O6 157.52(8) . . ? N1 Pb1 O6 127.56(9) . . ? O9 Pb1 O6 77.49(9) . . ? O2 Pb1 O6 78.43(9) . . ? O5 Pb1 O3 142.86(9) . . ? O1 Pb1 O3 101.82(8) . . ? O8 Pb1 O3 117.13(8) . . ? O4 Pb1 O3 63.32(8) . . ? N1 Pb1 O3 126.75(9) . . ? O9 Pb1 O3 69.39(8) . . ? O2 Pb1 O3 62.01(8) . . ? O6 Pb1 O3 105.50(9) . . ? C5 O1 C6 113.2(3) . . ? C5 O1 Pb1 110.47(19) . . ? C6 O1 Pb1 114.6(2) . . ? C13 N1 C4 110.6(3) . . ? C13 N1 C3 111.9(3) . . ? C4 N1 C3 111.2(3) . . ? C13 N1 Pb1 109.0(2) . . ? C4 N1 Pb1 111.3(2) . . ? C3 N1 Pb1 102.6(2) . . ? C7 O2 C8 113.3(3) . . ? C7 O2 Pb1 114.9(2) . . ? C8 O2 Pb1 112.4(2) . . ? O7 N2 O6 121.2(3) . . ? O7 N2 O5 120.8(3) . . ? O6 N2 O5 118.1(3) . . ? C1 C2 C3 122.5(4) . . ? C10 O3 C9 113.9(3) . . ? C10 O3 Pb1 111.4(2) . . ? C9 O3 Pb1 117.4(2) . . ? O10 N3 O8 120.6(3) . . ? O10 N3 O9 120.6(3) . . ? O8 N3 O9 118.8(3) . . ? C2 C3 N1 116.2(4) . . ? C12 O4 C11 112.8(3) . . ? C12 O4 Pb1 116.7(2) . . ? C11 O4 Pb1 116.4(2) . . ? N1 C4 C5 112.8(3) . . ? N2 O5 Pb1 100.2(2) . . ? O1 C5 C4 106.9(3) . . ? N2 O6 Pb1 93.1(2) . . ? O1 C6 C7 107.4(3) . . ? O2 C7 C6 107.6(3) . . ? N3 O8 Pb1 96.3(2) . . ? O2 C8 C9 112.6(3) . . ? N3 O9 Pb1 93.0(2) . . ? O3 C9 C8 106.2(3) . . ? O3 C10 C11 112.7(3) . . ? O4 C11 C10 107.1(3) . . ? O4 C12 C13 108.4(3) . . ? N1 C13 C12 113.0(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.242 _refine_diff_density_min -1.983 _refine_diff_density_rms 0.207 #===END data_alpbno3 #(compound11) _database_code_CSD 180580 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H52 N6 O21 Pb2' _chemical_formula_weight 1199.12 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' '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 7.6545(5) _cell_length_b 12.0537(4) _cell_length_c 21.6309(4) _cell_angle_alpha 90.671(5) _cell_angle_beta 96.212(4) _cell_angle_gamma 96.610(4) _cell_volume 1970.28(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 8.621 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.1818 _exptl_absorpt_correction_T_max 0.4793 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20988 _diffrn_reflns_av_R_equivalents 0.105 _diffrn_reflns_av_sigmaI/netI 0.1309 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7646 _reflns_number_gt 5869 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+6.7496P] 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 SHELXL _refine_ls_extinction_coef 0.0026(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7646 _refine_ls_number_parameters 561 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1892 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.026 _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 Pb1 Pb 0.88603(5) 0.24039(3) 0.11567(2) 0.02015(18) Uani 1 1 d . . . O1 O 1.2094(11) 0.2919(7) 0.0831(4) 0.0235(18) Uani 1 1 d . . . N1 N 1.0198(13) 0.4488(7) 0.1454(4) 0.018(2) Uani 1 1 d . . . C1 C 1.2114(17) 0.4673(9) 0.1363(5) 0.023(2) Uani 1 1 d . . . H1A H 1.2815 0.4376 0.1722 0.027 Uiso 1 1 calc R . . H1B H 1.2489 0.5485 0.1349 0.027 Uiso 1 1 calc R . . Pb2 Pb 0.70653(6) 0.79220(4) 0.38179(2) 0.02899(19) Uani 1 1 d . . . O2 O 1.0643(11) 0.0754(7) 0.0644(4) 0.0245(18) Uani 1 1 d . . . N2 N 0.5541(14) 0.2650(8) 0.1801(5) 0.026(2) Uani 1 1 d . . . C2 C 1.2493(16) 0.4111(9) 0.0769(6) 0.023(3) Uani 1 1 d . . . H2A H 1.1751 0.4369 0.0408 0.027 Uiso 1 1 calc R . . H2B H 1.3752 0.4298 0.0704 0.027 Uiso 1 1 calc R . . O3 O 1.0174(11) 0.0751(6) 0.1917(4) 0.0250(18) Uani 1 1 d . . . N3 N 0.7152(15) 0.2628(9) -0.0178(5) 0.027(2) Uani 1 1 d . . . C3 C 1.2415(17) 0.2308(10) 0.0288(6) 0.030(3) Uani 1 1 d . . . H3A H 1.3573 0.2593 0.0152 0.036 Uiso 1 1 calc R . . H3B H 1.1478 0.2380 -0.0058 0.036 Uiso 1 1 calc R . . O4 O 0.9282(12) 0.2809(6) 0.2366(4) 0.0258(19) Uani 1 1 d . . . N4 N 0.5627(14) 0.5743(9) 0.3686(5) 0.026(2) Uani 1 1 d . A . C4 C 1.2401(18) 0.1118(11) 0.0474(6) 0.032(3) Uani 1 1 d . . . H4A H 1.2664 0.0651 0.0124 0.038 Uiso 1 1 calc R . . H4B H 1.3305 0.1054 0.0831 0.038 Uiso 1 1 calc R . . O5 O 0.6170(11) 0.3389(7) 0.1457(4) 0.0261(19) Uani 1 1 d . . . N5 N 1.0309(13) 0.7592(8) 0.3133(5) 0.025(2) Uani 1 1 d . . . C5 C 1.0566(19) -0.0233(10) 0.0997(7) 0.035(3) Uani 1 1 d . . . H5A H 1.1264 -0.0772 0.0816 0.043 Uiso 1 1 calc R . . H5B H 0.9323 -0.0580 0.0974 0.043 Uiso 1 1 calc R . . O6 O 0.5844(11) 0.1651(6) 0.1688(5) 0.030(2) Uani 1 1 d . . . N6 N 0.805(6) 0.779(4) 0.524(2) 0.047(12) Uani 0.455(19) 1 d P A 1 C6 C 1.1282(18) 0.0010(10) 0.1675(7) 0.033(3) Uani 1 1 d . . . H6A H 1.1245 -0.0691 0.1910 0.040 Uiso 1 1 calc R . . H6B H 1.2522 0.0364 0.1706 0.040 Uiso 1 1 calc R . . O7 O 0.4569(12) 0.2848(7) 0.2200(4) 0.029(2) Uani 1 1 d . . . C7 C 1.0783(16) 0.1133(10) 0.2547(6) 0.029(3) Uani 1 1 d . . . H7A H 1.1970 0.1564 0.2565 0.035 Uiso 1 1 calc R . . H7B H 1.0864 0.0487 0.2823 0.035 Uiso 1 1 calc R . . O8 O 0.8305(13) 0.3321(8) 0.0064(4) 0.034(2) Uani 1 1 d . . . C8 C 0.9485(16) 0.1854(10) 0.2752(6) 0.027(3) Uani 1 1 d . . . H8A H 0.8320 0.1400 0.2749 0.032 Uiso 1 1 calc R . . H8B H 0.9873 0.2118 0.3186 0.032 Uiso 1 1 calc R . . O9 O 0.6637(13) 0.1730(8) 0.0100(5) 0.036(2) Uani 1 1 d . . . C9 C 1.0469(17) 0.3771(9) 0.2556(6) 0.027(3) Uani 1 1 d . . . H9A H 1.1705 0.3626 0.2527 0.032 Uiso 1 1 calc R . . H9B H 1.0353 0.3986 0.2991 0.032 Uiso 1 1 calc R . . O10 O 0.6469(15) 0.2735(10) -0.0729(5) 0.054(3) Uani 1 1 d . . . C10 C 0.9968(17) 0.4705(9) 0.2112(6) 0.025(3) Uani 1 1 d . . . H10A H 0.8716 0.4812 0.2140 0.029 Uiso 1 1 calc R . . H10B H 1.0701 0.5411 0.2254 0.029 Uiso 1 1 calc R . . O11 O 0.3716(11) 0.7465(7) 0.4119(4) 0.0231(18) Uani 1 1 d . A . C11 C 0.9205(16) 0.5245(9) 0.1041(6) 0.023(3) Uani 1 1 d . . . H11A H 0.7932 0.4956 0.0999 0.028 Uiso 1 1 calc R . . H11B H 0.9610 0.5217 0.0622 0.028 Uiso 1 1 calc R . . O12 O 0.5246(11) 0.9674(7) 0.4195(4) 0.0256(18) Uani 1 1 d . A . C12 C 0.9413(17) 0.6453(9) 0.1267(6) 0.025(3) Uani 1 1 d . . . H12 H 1.0574 0.6818 0.1376 0.030 Uiso 1 1 calc R . . O13 O 0.6453(11) 0.9559(7) 0.2998(4) 0.0254(19) Uani 1 1 d . A . C13 C 0.807(2) 0.7018(11) 0.1318(7) 0.040(4) Uani 1 1 d . . . H13A H 0.6896 0.6672 0.1212 0.048 Uiso 1 1 calc R . . H13B H 0.8273 0.7775 0.1463 0.048 Uiso 1 1 calc R . . O14 O 0.6039(11) 0.7268(6) 0.2668(4) 0.0253(19) Uani 1 1 d . A . C14 C 0.3753(19) 0.5621(11) 0.3767(7) 0.034(3) Uani 1 1 d . . . H14A H 0.3367 0.4829 0.3848 0.041 Uiso 1 1 calc R A . H14B H 0.3076 0.5819 0.3376 0.041 Uiso 1 1 calc R . . O15 O 0.9828(12) 0.8569(7) 0.3176(5) 0.034(2) Uani 1 1 d . A . C15 C 0.332(2) 0.6334(10) 0.4289(6) 0.037(4) Uani 1 1 d . A . H15A H 0.2055 0.6174 0.4350 0.045 Uiso 1 1 calc R . . H15B H 0.4042 0.6184 0.4681 0.045 Uiso 1 1 calc R . . O16 O 0.9674(11) 0.6859(7) 0.3474(4) 0.028(2) Uani 1 1 d . A . C16 C 0.3307(19) 0.8228(11) 0.4594(6) 0.030(3) Uani 1 1 d . . . H16A H 0.4162 0.8216 0.4971 0.036 Uiso 1 1 calc R A . H16B H 0.2102 0.8004 0.4710 0.036 Uiso 1 1 calc R . . O17 O 1.1346(12) 0.7380(7) 0.2767(4) 0.032(2) Uani 1 1 d . A . C17 C 0.3423(16) 0.9389(10) 0.4327(6) 0.026(3) Uani 1 1 d . A . H17A H 0.2602 0.9396 0.3941 0.032 Uiso 1 1 calc R . . H17B H 0.3107 0.9934 0.4629 0.032 Uiso 1 1 calc R . . O18 O 0.904(3) 0.8394(16) 0.4931(10) 0.035(6) Uani 0.455(19) 1 d PU A 1 C18 C 0.5413(19) 1.0608(10) 0.3781(6) 0.031(3) Uani 1 1 d U . . H18A H 0.6625 1.1006 0.3855 0.038 Uiso 1 1 calc R A . H18B H 0.4571 1.1139 0.3869 0.038 Uiso 1 1 calc R . . O19 O 0.691(4) 0.702(2) 0.5001(11) 0.034(6) Uani 0.455(19) 1 d PU A 1 C19 C 0.5037(18) 1.0207(10) 0.3100(6) 0.027(3) Uani 1 1 d U A . H19A H 0.3877 0.9743 0.3026 0.033 Uiso 1 1 calc R . . H19B H 0.5033 1.0850 0.2819 0.033 Uiso 1 1 calc R . . O20 O 0.814(3) 0.793(2) 0.5835(15) 0.042(7) Uiso 0.455(19) 1 d P A 1 C20 C 0.6394(17) 0.9168(10) 0.2367(6) 0.027(3) Uani 1 1 d U . . H20A H 0.7608 0.9083 0.2271 0.032 Uiso 1 1 calc R A . H20B H 0.5914 0.9724 0.2083 0.032 Uiso 1 1 calc R . . O21 O 0.936(3) 0.9510(15) 0.4487(9) 0.047(6) Uani 0.545(19) 1 d PU A 2 C21 C 0.5231(17) 0.8043(9) 0.2262(6) 0.025(3) Uani 1 1 d U A . H21A H 0.4015 0.8113 0.2361 0.029 Uiso 1 1 calc R . . H21B H 0.5172 0.7786 0.1823 0.029 Uiso 1 1 calc R . . C22 C 0.5247(17) 0.6129(9) 0.2550(6) 0.026(3) Uani 1 1 d U . . H22A H 0.5523 0.5864 0.2140 0.031 Uiso 1 1 calc R A . H22B H 0.3945 0.6092 0.2538 0.031 Uiso 1 1 calc R . . C23 C 0.5942(17) 0.5393(10) 0.3049(6) 0.027(3) Uani 1 1 d U A . H23A H 0.5375 0.4619 0.2962 0.033 Uiso 1 1 calc R . . H23B H 0.7231 0.5393 0.3035 0.033 Uiso 1 1 calc R . . C24 C 0.690(4) 0.5242(19) 0.4142(11) 0.025(5) Uani 0.56(3) 1 d PU A 1 H24A H 0.6637 0.5416 0.4568 0.030 Uiso 0.56(3) 1 calc PR A 1 H24B H 0.8113 0.5598 0.4099 0.030 Uiso 0.56(3) 1 calc PR A 1 C25 C 0.686(3) 0.3986(17) 0.4065(10) 0.025(6) Uani 0.56(3) 1 d PU A 1 H25 H 0.5755 0.3531 0.4000 0.031 Uiso 0.56(3) 1 calc PR A 1 C26 C 0.838(4) 0.350(2) 0.4086(12) 0.031(6) Uani 0.56(3) 1 d PU A 1 H26A H 0.9490 0.3953 0.4150 0.037 Uiso 0.56(3) 1 calc PR A 1 H26B H 0.8332 0.2717 0.4037 0.037 Uiso 0.56(3) 1 calc PR A 1 N6A N 0.807(4) 0.774(2) 0.5487(17) 0.026(7) Uani 0.545(19) 1 d PU A 2 O18A O 0.746(4) 0.744(2) 0.5047(13) 0.041(7) Uani 0.545(19) 1 d PU A 2 O19A O 0.932(3) 0.8534(17) 0.5647(10) 0.053(6) Uani 0.545(19) 1 d PU A 2 O20A O 0.748(3) 0.7363(16) 0.5991(9) 0.043(5) Uani 0.545(19) 1 d PU A 2 C24A C 0.616(5) 0.487(3) 0.4136(15) 0.030(8) Uiso 0.44(3) 1 d P A 2 H24C H 0.5712 0.5010 0.4540 0.036 Uiso 0.44(3) 1 calc PR A 2 H24D H 0.5620 0.4126 0.3974 0.036 Uiso 0.44(3) 1 calc PR A 2 C25A C 0.811(4) 0.490(2) 0.4229(14) 0.027(8) Uani 0.44(3) 1 d PU A 2 H25A H 0.8795 0.5609 0.4301 0.033 Uiso 0.44(3) 1 calc PR A 2 C26A C 0.896(6) 0.402(3) 0.4219(18) 0.043(9) Uani 0.44(3) 1 d PU A 2 H26C H 0.8324 0.3299 0.4148 0.052 Uiso 0.44(3) 1 calc PR A 2 H26D H 1.0219 0.4104 0.4282 0.052 Uiso 0.44(3) 1 calc PR A 2 O1S O 0.409(4) 0.053(2) -0.0895(13) 0.070(7) Uani 0.50 1 d PU B 1 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 Pb1 0.0142(3) 0.0231(3) 0.0234(3) 0.00227(17) 0.00338(19) 0.00162(16) O1 0.017(4) 0.032(4) 0.023(5) -0.006(3) 0.007(4) 0.001(3) N1 0.021(5) 0.020(4) 0.016(5) 0.002(4) 0.001(4) 0.011(4) C1 0.028(7) 0.025(6) 0.013(6) -0.003(4) -0.005(5) 0.001(5) Pb2 0.0156(3) 0.0511(3) 0.0219(3) -0.0054(2) 0.0022(2) 0.0113(2) O2 0.018(4) 0.027(4) 0.025(5) -0.005(3) -0.013(4) -0.002(3) N2 0.024(6) 0.020(5) 0.037(7) 0.005(4) 0.006(5) 0.006(4) C2 0.015(6) 0.029(6) 0.026(7) 0.004(5) 0.005(5) 0.005(5) O3 0.011(4) 0.029(4) 0.033(5) 0.004(4) -0.001(4) -0.002(3) N3 0.020(6) 0.046(6) 0.017(6) 0.003(5) 0.000(5) 0.014(5) C3 0.018(7) 0.040(7) 0.034(8) 0.002(6) 0.003(6) 0.010(5) O4 0.028(5) 0.026(4) 0.023(5) 0.004(3) 0.004(4) 0.002(4) N4 0.022(6) 0.039(6) 0.021(6) 0.011(4) 0.005(5) 0.015(4) C4 0.026(7) 0.041(7) 0.029(8) -0.002(5) 0.007(6) 0.005(6) O5 0.011(4) 0.033(4) 0.033(5) 0.006(4) -0.001(4) -0.001(3) N5 0.008(5) 0.035(5) 0.029(6) -0.003(4) 0.004(5) -0.007(4) C5 0.032(8) 0.023(6) 0.048(9) -0.001(6) -0.010(7) 0.004(5) O6 0.015(4) 0.015(4) 0.060(7) 0.004(4) 0.002(4) 0.003(3) N6 0.04(2) 0.08(3) 0.02(2) -0.03(2) -0.02(2) 0.04(2) C6 0.026(7) 0.029(6) 0.048(9) 0.007(6) 0.011(7) 0.014(5) O7 0.022(5) 0.042(5) 0.026(5) 0.003(4) 0.010(4) 0.007(4) C7 0.016(6) 0.039(7) 0.032(8) 0.012(5) 0.005(6) -0.005(5) O8 0.038(6) 0.040(5) 0.025(5) 0.009(4) 0.003(5) 0.001(4) C8 0.021(6) 0.032(6) 0.028(7) 0.018(5) 0.009(6) -0.005(5) O9 0.025(5) 0.045(5) 0.035(6) 0.000(4) -0.001(5) -0.004(4) C9 0.022(6) 0.024(6) 0.035(8) 0.001(5) 0.011(6) -0.005(5) O10 0.042(7) 0.073(8) 0.041(7) 0.001(6) 0.000(6) -0.015(5) C10 0.023(6) 0.030(6) 0.021(7) -0.007(5) 0.007(5) 0.000(5) O11 0.023(5) 0.037(4) 0.007(4) 0.001(3) -0.001(4) -0.004(3) C11 0.020(6) 0.029(6) 0.023(7) 0.006(5) 0.006(5) 0.009(5) O12 0.015(4) 0.040(5) 0.021(5) -0.012(3) 0.005(4) 0.000(3) C12 0.030(7) 0.025(6) 0.020(7) 0.004(5) 0.004(6) 0.002(5) O13 0.014(4) 0.031(4) 0.033(5) -0.001(3) 0.005(4) 0.008(3) C13 0.051(10) 0.044(8) 0.032(8) 0.006(6) 0.022(7) 0.015(7) O14 0.021(4) 0.022(4) 0.033(5) -0.002(3) 0.006(4) -0.002(3) C14 0.032(8) 0.039(7) 0.033(8) -0.004(6) 0.019(7) -0.006(6) O15 0.022(5) 0.023(4) 0.054(7) -0.002(4) -0.006(5) 0.006(4) C15 0.049(9) 0.039(7) 0.030(8) 0.016(6) 0.033(7) 0.005(6) O16 0.020(5) 0.030(4) 0.033(5) 0.002(4) 0.008(4) -0.001(3) C16 0.034(8) 0.044(7) 0.013(6) 0.001(5) 0.008(6) 0.006(6) O17 0.022(5) 0.037(5) 0.038(6) -0.005(4) 0.016(4) -0.003(4) C17 0.017(6) 0.044(7) 0.023(7) 0.003(5) 0.013(5) 0.010(5) O18 0.034(7) 0.036(7) 0.034(7) 0.002(4) -0.003(5) 0.002(5) C18 0.030(5) 0.028(4) 0.037(5) -0.002(4) 0.007(4) 0.002(4) O19 0.034(7) 0.036(7) 0.032(7) 0.004(5) 0.001(5) 0.000(5) C19 0.026(5) 0.031(4) 0.025(4) -0.001(3) 0.006(4) 0.003(4) C20 0.025(4) 0.028(4) 0.028(5) 0.002(3) 0.005(4) 0.003(4) O21 0.046(7) 0.050(7) 0.044(7) 0.000(4) 0.009(5) 0.001(4) C21 0.025(4) 0.027(4) 0.022(4) 0.002(3) 0.004(4) 0.001(3) C22 0.024(4) 0.028(4) 0.024(4) -0.001(3) 0.003(4) -0.002(3) C23 0.025(4) 0.030(4) 0.028(5) -0.005(3) 0.007(4) 0.007(4) C24 0.025(7) 0.023(7) 0.025(7) 0.002(4) 0.000(5) 0.000(5) C25 0.027(7) 0.026(7) 0.024(7) 0.003(4) 0.004(5) 0.005(4) C26 0.031(7) 0.031(7) 0.031(7) 0.000(5) 0.005(5) 0.007(5) N6A 0.025(8) 0.026(7) 0.028(8) -0.002(5) 0.001(5) 0.010(4) O18A 0.044(8) 0.040(8) 0.039(8) 0.003(5) 0.002(5) 0.004(5) O19A 0.054(7) 0.052(7) 0.053(7) 0.001(5) 0.001(5) 0.006(5) O20A 0.044(7) 0.044(6) 0.042(7) -0.002(4) 0.005(5) 0.006(5) C25A 0.027(9) 0.027(8) 0.027(9) 0.001(5) 0.004(5) 0.003(5) C26A 0.042(10) 0.043(10) 0.044(10) 0.001(5) 0.002(5) 0.007(5) O1S 0.070(8) 0.068(8) 0.073(8) 0.003(5) 0.008(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O5 2.628(8) . ? Pb1 O8 2.634(9) . ? Pb1 O4 2.634(9) . ? Pb1 N1 2.646(9) . ? Pb1 O1 2.654(8) . ? Pb1 O9 2.753(10) . ? Pb1 O6 2.755(8) . ? Pb1 O3 2.805(8) . ? Pb1 O2 2.819(8) . ? O1 C3 1.437(15) . ? O1 C2 1.444(14) . ? N1 C10 1.476(14) . ? N1 C1 1.492(15) . ? N1 C11 1.497(13) . ? C1 C2 1.517(16) . ? Pb2 O14 2.610(9) . ? Pb2 O16 2.659(8) . ? Pb2 O15 2.700(10) . ? Pb2 O11 2.711(8) . ? Pb2 O13 2.715(8) . ? Pb2 O18 2.72(2) . ? Pb2 O18A 2.72(3) . ? Pb2 N4 2.728(11) . ? Pb2 O21 2.73(2) . ? Pb2 O19 2.80(2) . ? Pb2 O12 2.819(8) . ? O2 C5 1.420(15) . ? O2 C4 1.454(15) . ? N2 O7 1.238(13) . ? N2 O5 1.254(12) . ? N2 O6 1.278(12) . ? O3 C6 1.434(14) . ? O3 C7 1.444(16) . ? N3 O8 1.214(15) . ? N3 O10 1.263(15) . ? N3 O9 1.286(14) . ? C3 C4 1.493(17) . ? O4 C9 1.415(15) . ? O4 C8 1.443(13) . ? N4 C14 1.454(17) . ? N4 C24A 1.50(3) . ? N4 C23 1.490(15) . ? N4 C24 1.49(2) . ? N5 O17 1.225(12) . ? N5 O16 1.247(12) . ? N5 O15 1.279(13) . ? C5 C6 1.52(2) . ? N6 O18 1.24(6) . ? N6 O19 1.27(5) . ? N6 O20 1.29(5) . ? C7 C8 1.492(17) . ? C9 C10 1.544(16) . ? O11 C15 1.423(14) . ? O11 C16 1.453(14) . ? C11 C12 1.516(16) . ? O12 C18 1.450(15) . ? O12 C17 1.458(14) . ? C12 C13 1.310(17) . ? O13 C20 1.433(15) . ? O13 C19 1.441(14) . ? O14 C21 1.437(14) . ? O14 C22 1.444(14) . ? C14 C15 1.497(17) . ? C16 C17 1.518(17) . ? C18 C19 1.531(18) . ? C20 C21 1.535(17) . ? C22 C23 1.498(17) . ? C24 C25 1.52(3) . ? C25 C26 1.35(3) . ? N6A O18A 1.05(5) . ? N6A O19A 1.29(4) . ? N6A O20A 1.29(4) . ? C24A C25A 1.48(5) . ? C25A C26A 1.31(4) . ? 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 O5 Pb1 O8 85.9(3) . . ? O5 Pb1 O4 71.4(3) . . ? O8 Pb1 O4 144.0(3) . . ? O5 Pb1 N1 75.1(3) . . ? O8 Pb1 N1 80.4(3) . . ? O4 Pb1 N1 67.2(3) . . ? O5 Pb1 O1 139.9(2) . . ? O8 Pb1 O1 76.4(3) . . ? O4 Pb1 O1 103.2(3) . . ? N1 Pb1 O1 66.7(3) . . ? O5 Pb1 O9 84.1(3) . . ? O8 Pb1 O9 47.8(3) . . ? O4 Pb1 O9 148.8(3) . . ? N1 Pb1 O9 125.4(3) . . ? O1 Pb1 O9 108.0(3) . . ? O5 Pb1 O6 47.1(2) . . ? O8 Pb1 O6 115.0(3) . . ? O4 Pb1 O6 68.9(3) . . ? N1 Pb1 O6 115.4(3) . . ? O1 Pb1 O6 168.5(3) . . ? O9 Pb1 O6 80.4(3) . . ? O5 Pb1 O3 120.0(2) . . ? O8 Pb1 O3 151.4(3) . . ? O4 Pb1 O3 62.7(2) . . ? N1 Pb1 O3 116.0(3) . . ? O1 Pb1 O3 88.5(2) . . ? O9 Pb1 O3 118.1(3) . . ? O6 Pb1 O3 80.4(2) . . ? O5 Pb1 O2 157.9(3) . . ? O8 Pb1 O2 91.3(3) . . ? O4 Pb1 O2 120.0(2) . . ? N1 Pb1 O2 126.1(3) . . ? O1 Pb1 O2 59.6(2) . . ? O9 Pb1 O2 77.8(3) . . ? O6 Pb1 O2 116.3(2) . . ? O3 Pb1 O2 60.1(2) . . ? C3 O1 C2 112.1(9) . . ? C3 O1 Pb1 113.3(7) . . ? C2 O1 Pb1 111.1(6) . . ? C10 N1 C1 110.0(9) . . ? C10 N1 C11 110.4(8) . . ? C1 N1 C11 109.4(8) . . ? C10 N1 Pb1 108.2(6) . . ? C1 N1 Pb1 110.9(6) . . ? C11 N1 Pb1 107.9(7) . . ? N1 C1 C2 111.9(10) . . ? O14 Pb2 O16 75.1(3) . . ? O14 Pb2 O15 74.4(3) . . ? O16 Pb2 O15 47.6(2) . . ? O14 Pb2 O11 90.8(3) . . ? O16 Pb2 O11 139.6(2) . . ? O15 Pb2 O11 161.6(3) . . ? O14 Pb2 O13 63.9(2) . . ? O16 Pb2 O13 108.8(2) . . ? O15 Pb2 O13 66.2(2) . . ? O11 Pb2 O13 97.6(2) . . ? O14 Pb2 O18 162.9(5) . . ? O16 Pb2 O18 88.1(5) . . ? O15 Pb2 O18 92.4(5) . . ? O11 Pb2 O18 104.1(5) . . ? O13 Pb2 O18 121.0(5) . . ? O14 Pb2 O18A 149.2(7) . . ? O16 Pb2 O18A 97.6(6) . . ? O15 Pb2 O18A 122.8(7) . . ? O11 Pb2 O18A 75.4(7) . . ? O13 Pb2 O18A 144.2(6) . . ? O18 Pb2 O18A 34.5(8) . . ? O14 Pb2 N4 65.9(3) . . ? O16 Pb2 N4 75.9(3) . . ? O15 Pb2 N4 117.4(3) . . ? O11 Pb2 N4 63.9(3) . . ? O13 Pb2 N4 125.7(3) . . ? O18 Pb2 N4 113.1(5) . . ? O18A Pb2 N4 83.3(7) . . ? O14 Pb2 O21 140.4(4) . . ? O16 Pb2 O21 92.6(5) . . ? O15 Pb2 O21 69.9(5) . . ? O11 Pb2 O21 119.8(4) . . ? O13 Pb2 O21 86.1(4) . . ? O18 Pb2 O21 35.7(6) . . ? O18A Pb2 O21 68.6(8) . . ? N4 Pb2 O21 148.1(4) . . ? O14 Pb2 O19 136.9(6) . . ? O16 Pb2 O19 98.1(5) . . ? O15 Pb2 O19 131.7(6) . . ? O11 Pb2 O19 66.8(6) . . ? O13 Pb2 O19 150.8(5) . . ? O18 Pb2 O19 47.2(8) . . ? O18A Pb2 O19 12.9(6) . . ? N4 Pb2 O19 71.1(6) . . ? O21 Pb2 O19 81.5(7) . . ? O14 Pb2 O12 112.1(2) . . ? O16 Pb2 O12 160.0(3) . . ? O15 Pb2 O12 114.8(2) . . ? O11 Pb2 O12 60.3(2) . . ? O13 Pb2 O12 61.9(2) . . ? O18 Pb2 O12 83.0(5) . . ? O18A Pb2 O12 85.1(6) . . ? N4 Pb2 O12 124.1(3) . . ? O21 Pb2 O12 69.8(4) . . ? O19 Pb2 O12 88.9(5) . . ? C5 O2 C4 113.4(9) . . ? C5 O2 Pb1 111.9(7) . . ? C4 O2 Pb1 116.4(7) . . ? O7 N2 O5 122.7(9) . . ? O7 N2 O6 120.8(9) . . ? O5 N2 O6 116.4(10) . . ? O1 C2 C1 107.8(9) . . ? C6 O3 C7 113.0(10) . . ? C6 O3 Pb1 119.5(7) . . ? C7 O3 Pb1 113.9(6) . . ? O8 N3 O10 120.9(11) . . ? O8 N3 O9 121.9(11) . . ? O10 N3 O9 117.2(12) . . ? O1 C3 C4 106.0(10) . . ? C9 O4 C8 114.5(10) . . ? C9 O4 Pb1 114.2(7) . . ? C8 O4 Pb1 116.0(7) . . ? C14 N4 C24A 97.3(16) . . ? C14 N4 C23 112.0(11) . . ? C24A N4 C23 109.0(14) . . ? C14 N4 C24 119.9(13) . . ? C24A N4 C24 26.3(13) . . ? C23 N4 C24 108.1(11) . . ? C14 N4 Pb2 111.4(7) . . ? C24A N4 Pb2 122.1(17) . . ? C23 N4 Pb2 105.0(7) . . ? C24 N4 Pb2 98.8(11) . . ? O2 C4 C3 107.1(10) . . ? N2 O5 Pb1 98.2(6) . . ? O17 N5 O16 121.1(10) . . ? O17 N5 O15 121.3(10) . . ? O16 N5 O15 117.6(9) . . ? O2 C5 C6 111.7(10) . . ? N2 O6 Pb1 91.6(6) . . ? O18 N6 O19 123(4) . . ? O18 N6 O20 121(4) . . ? O19 N6 O20 116(4) . . ? O3 C6 C5 106.6(10) . . ? O3 C7 C8 107.6(10) . . ? N3 O8 Pb1 98.9(7) . . ? O4 C8 C7 113.3(9) . . ? N3 O9 Pb1 91.3(7) . . ? O4 C9 C10 106.4(11) . . ? N1 C10 C9 114.5(9) . . ? C15 O11 C16 111.0(9) . . ? C15 O11 Pb2 112.5(7) . . ? C16 O11 Pb2 112.8(7) . . ? N1 C11 C12 114.6(10) . . ? C18 O12 C17 111.7(9) . . ? C18 O12 Pb2 111.3(6) . . ? C17 O12 Pb2 117.5(7) . . ? C13 C12 C11 123.3(13) . . ? C20 O13 C19 113.4(9) . . ? C20 O13 Pb2 111.7(6) . . ? C19 O13 Pb2 116.8(6) . . ? C21 O14 C22 112.7(10) . . ? C21 O14 Pb2 117.7(7) . . ? C22 O14 Pb2 118.4(7) . . ? N4 C14 C15 113.3(13) . . ? N5 O15 Pb2 95.0(6) . . ? O11 C15 C14 106.8(9) . . ? N5 O16 Pb2 97.8(6) . . ? O11 C16 C17 107.6(9) . . ? O12 C17 C16 106.8(9) . . ? N6 O18 Pb2 95(2) . . ? O12 C18 C19 110.8(10) . . ? N6 O19 Pb2 91(3) . . ? O13 C19 C18 105.1(10) . . ? O13 C20 C21 110.8(10) . . ? O14 C21 C20 106.5(10) . . ? O14 C22 C23 110.0(11) . . ? N4 C23 C22 113.6(9) . . ? N4 C24 C25 114(2) . . ? C26 C25 C24 121(2) . . ? O18A N6A O19A 132(3) . . ? O18A N6A O20A 121(3) . . ? O19A N6A O20A 107(3) . . ? N6A O18A Pb2 144(3) . . ? C25A C24A N4 111(3) . . ? C26A C25A C24A 125(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Pb1 O1 C3 -131.0(7) . . . . ? O8 Pb1 O1 C3 -64.8(7) . . . . ? O4 Pb1 O1 C3 152.3(7) . . . . ? N1 Pb1 O1 C3 -150.0(8) . . . . ? O9 Pb1 O1 C3 -28.4(8) . . . . ? O6 Pb1 O1 C3 107.0(14) . . . . ? O3 Pb1 O1 C3 90.7(7) . . . . ? O2 Pb1 O1 C3 35.0(7) . . . . ? O5 Pb1 O1 C2 -3.8(9) . . . . ? O8 Pb1 O1 C2 62.5(7) . . . . ? O4 Pb1 O1 C2 -80.5(7) . . . . ? N1 Pb1 O1 C2 -22.7(7) . . . . ? O9 Pb1 O1 C2 98.8(7) . . . . ? O6 Pb1 O1 C2 -125.8(12) . . . . ? O3 Pb1 O1 C2 -142.0(7) . . . . ? O2 Pb1 O1 C2 162.2(8) . . . . ? O5 Pb1 N1 C10 61.9(7) . . . . ? O8 Pb1 N1 C10 150.1(7) . . . . ? O4 Pb1 N1 C10 -13.9(7) . . . . ? O1 Pb1 N1 C10 -130.6(7) . . . . ? O9 Pb1 N1 C10 133.2(7) . . . . ? O6 Pb1 N1 C10 36.9(8) . . . . ? O3 Pb1 N1 C10 -54.6(7) . . . . ? O2 Pb1 N1 C10 -125.3(7) . . . . ? O5 Pb1 N1 C1 -177.4(7) . . . . ? O8 Pb1 N1 C1 -89.2(7) . . . . ? O4 Pb1 N1 C1 106.8(7) . . . . ? O1 Pb1 N1 C1 -9.9(6) . . . . ? O9 Pb1 N1 C1 -106.1(7) . . . . ? O6 Pb1 N1 C1 157.6(6) . . . . ? O3 Pb1 N1 C1 66.1(7) . . . . ? O2 Pb1 N1 C1 -4.6(8) . . . . ? O5 Pb1 N1 C11 -57.7(6) . . . . ? O8 Pb1 N1 C11 30.6(6) . . . . ? O4 Pb1 N1 C11 -133.4(7) . . . . ? O1 Pb1 N1 C11 109.8(7) . . . . ? O9 Pb1 N1 C11 13.7(8) . . . . ? O6 Pb1 N1 C11 -82.6(7) . . . . ? O3 Pb1 N1 C11 -174.1(6) . . . . ? O2 Pb1 N1 C11 115.2(6) . . . . ? C10 N1 C1 C2 161.1(9) . . . . ? C11 N1 C1 C2 -77.5(11) . . . . ? Pb1 N1 C1 C2 41.5(10) . . . . ? O5 Pb1 O2 C5 -72.4(10) . . . . ? O8 Pb1 O2 C5 -154.7(8) . . . . ? O4 Pb1 O2 C5 43.9(8) . . . . ? N1 Pb1 O2 C5 126.3(8) . . . . ? O1 Pb1 O2 C5 132.0(8) . . . . ? O9 Pb1 O2 C5 -108.5(8) . . . . ? O6 Pb1 O2 C5 -35.8(8) . . . . ? O3 Pb1 O2 C5 24.4(7) . . . . ? O5 Pb1 O2 C4 155.0(8) . . . . ? O8 Pb1 O2 C4 72.7(8) . . . . ? O4 Pb1 O2 C4 -88.8(8) . . . . ? N1 Pb1 O2 C4 -6.3(9) . . . . ? O1 Pb1 O2 C4 -0.7(8) . . . . ? O9 Pb1 O2 C4 118.9(8) . . . . ? O6 Pb1 O2 C4 -168.4(8) . . . . ? O3 Pb1 O2 C4 -108.3(8) . . . . ? C3 O1 C2 C1 -179.9(10) . . . . ? Pb1 O1 C2 C1 52.2(11) . . . . ? N1 C1 C2 O1 -64.4(12) . . . . ? O5 Pb1 O3 C6 162.8(8) . . . . ? O8 Pb1 O3 C6 10.5(12) . . . . ? O4 Pb1 O3 C6 -152.6(9) . . . . ? N1 Pb1 O3 C6 -110.0(9) . . . . ? O1 Pb1 O3 C6 -46.9(9) . . . . ? O9 Pb1 O3 C6 62.8(9) . . . . ? O6 Pb1 O3 C6 136.4(9) . . . . ? O2 Pb1 O3 C6 8.4(8) . . . . ? O5 Pb1 O3 C7 -59.3(7) . . . . ? O8 Pb1 O3 C7 148.3(7) . . . . ? O4 Pb1 O3 C7 -14.7(6) . . . . ? N1 Pb1 O3 C7 27.9(7) . . . . ? O1 Pb1 O3 C7 91.0(7) . . . . ? O9 Pb1 O3 C7 -159.3(6) . . . . ? O6 Pb1 O3 C7 -85.8(7) . . . . ? O2 Pb1 O3 C7 146.3(7) . . . . ? C2 O1 C3 C4 165.9(10) . . . . ? Pb1 O1 C3 C4 -67.4(11) . . . . ? O5 Pb1 O4 C9 -99.8(7) . . . . ? O8 Pb1 O4 C9 -46.2(10) . . . . ? N1 Pb1 O4 C9 -18.7(7) . . . . ? O1 Pb1 O4 C9 38.7(8) . . . . ? O9 Pb1 O4 C9 -140.0(7) . . . . ? O6 Pb1 O4 C9 -150.0(8) . . . . ? O3 Pb1 O4 C9 120.1(8) . . . . ? O2 Pb1 O4 C9 101.1(7) . . . . ? O5 Pb1 O4 C8 123.7(8) . . . . ? O8 Pb1 O4 C8 177.4(7) . . . . ? N1 Pb1 O4 C8 -155.1(8) . . . . ? O1 Pb1 O4 C8 -97.7(7) . . . . ? O9 Pb1 O4 C8 83.5(9) . . . . ? O6 Pb1 O4 C8 73.6(7) . . . . ? O3 Pb1 O4 C8 -16.4(7) . . . . ? O2 Pb1 O4 C8 -35.4(8) . . . . ? O14 Pb2 N4 C14 -94.9(9) . . . . ? O16 Pb2 N4 C14 -174.6(9) . . . . ? O15 Pb2 N4 C14 -150.6(8) . . . . ? O11 Pb2 N4 C14 8.8(8) . . . . ? O13 Pb2 N4 C14 -71.3(9) . . . . ? O18 Pb2 N4 C14 103.7(10) . . . . ? O18A Pb2 N4 C14 85.8(10) . . . . ? O21 Pb2 N4 C14 113.8(11) . . . . ? O19 Pb2 N4 C14 81.6(10) . . . . ? O12 Pb2 N4 C14 6.4(10) . . . . ? O14 Pb2 N4 C24A 151.1(16) . . . . ? O16 Pb2 N4 C24A 71.4(16) . . . . ? O15 Pb2 N4 C24A 95.4(16) . . . . ? O11 Pb2 N4 C24A -105.2(16) . . . . ? O13 Pb2 N4 C24A 174.6(16) . . . . ? O18 Pb2 N4 C24A -10.3(17) . . . . ? O18A Pb2 N4 C24A -28.2(17) . . . . ? O21 Pb2 N4 C24A -0.3(19) . . . . ? O19 Pb2 N4 C24A -32.5(17) . . . . ? O12 Pb2 N4 C24A -107.7(16) . . . . ? O14 Pb2 N4 C23 26.5(7) . . . . ? O16 Pb2 N4 C23 -53.2(7) . . . . ? O15 Pb2 N4 C23 -29.1(8) . . . . ? O11 Pb2 N4 C23 130.2(8) . . . . ? O13 Pb2 N4 C23 50.1(8) . . . . ? O18 Pb2 N4 C23 -134.9(8) . . . . ? O18A Pb2 N4 C23 -152.8(9) . . . . ? O21 Pb2 N4 C23 -124.8(10) . . . . ? O19 Pb2 N4 C23 -157.0(9) . . . . ? O12 Pb2 N4 C23 127.8(7) . . . . ? O14 Pb2 N4 C24 138.0(11) . . . . ? O16 Pb2 N4 C24 58.3(10) . . . . ? O15 Pb2 N4 C24 82.4(10) . . . . ? O11 Pb2 N4 C24 -118.3(10) . . . . ? O13 Pb2 N4 C24 161.6(10) . . . . ? O18 Pb2 N4 C24 -23.4(12) . . . . ? O18A Pb2 N4 C24 -41.3(12) . . . . ? O21 Pb2 N4 C24 -13.3(14) . . . . ? O19 Pb2 N4 C24 -45.5(11) . . . . ? O12 Pb2 N4 C24 -120.7(10) . . . . ? C5 O2 C4 C3 -162.8(11) . . . . ? Pb1 O2 C4 C3 -30.9(13) . . . . ? O1 C3 C4 O2 62.2(13) . . . . ? O7 N2 O5 Pb1 158.2(11) . . . . ? O6 N2 O5 Pb1 -27.0(11) . . . . ? O8 Pb1 O5 N2 145.2(8) . . . . ? O4 Pb1 O5 N2 -63.1(7) . . . . ? N1 Pb1 O5 N2 -133.7(8) . . . . ? O1 Pb1 O5 N2 -151.7(7) . . . . ? O9 Pb1 O5 N2 97.2(7) . . . . ? O6 Pb1 O5 N2 14.9(7) . . . . ? O3 Pb1 O5 N2 -21.9(8) . . . . ? O2 Pb1 O5 N2 61.8(11) . . . . ? C4 O2 C5 C6 78.4(14) . . . . ? Pb1 O2 C5 C6 -55.7(12) . . . . ? O7 N2 O6 Pb1 -159.7(11) . . . . ? O5 N2 O6 Pb1 25.4(11) . . . . ? O5 Pb1 O6 N2 -14.5(7) . . . . ? O8 Pb1 O6 N2 -71.6(8) . . . . ? O4 Pb1 O6 N2 69.3(7) . . . . ? N1 Pb1 O6 N2 19.3(8) . . . . ? O1 Pb1 O6 N2 117.2(12) . . . . ? O9 Pb1 O6 N2 -105.4(7) . . . . ? O3 Pb1 O6 N2 133.7(7) . . . . ? O2 Pb1 O6 N2 -176.6(7) . . . . ? C7 O3 C6 C5 -175.1(9) . . . . ? Pb1 O3 C6 C5 -36.9(12) . . . . ? O2 C5 C6 O3 61.5(14) . . . . ? C6 O3 C7 C8 -177.7(9) . . . . ? Pb1 O3 C7 C8 41.7(10) . . . . ? O10 N3 O8 Pb1 -179.8(10) . . . . ? O9 N3 O8 Pb1 -3.4(12) . . . . ? O5 Pb1 O8 N3 -84.0(7) . . . . ? O4 Pb1 O8 N3 -133.9(7) . . . . ? N1 Pb1 O8 N3 -159.5(7) . . . . ? O1 Pb1 O8 N3 132.3(7) . . . . ? O9 Pb1 O8 N3 1.8(6) . . . . ? O6 Pb1 O8 N3 -45.9(8) . . . . ? O3 Pb1 O8 N3 72.3(10) . . . . ? O2 Pb1 O8 N3 74.0(7) . . . . ? C9 O4 C8 C7 -89.1(13) . . . . ? Pb1 O4 C8 C7 47.2(13) . . . . ? O3 C7 C8 O4 -59.2(13) . . . . ? O8 N3 O9 Pb1 3.3(11) . . . . ? O10 N3 O9 Pb1 179.8(9) . . . . ? O5 Pb1 O9 N3 88.0(6) . . . . ? O8 Pb1 O9 N3 -1.7(6) . . . . ? O4 Pb1 O9 N3 126.0(6) . . . . ? N1 Pb1 O9 N3 21.0(8) . . . . ? O1 Pb1 O9 N3 -52.8(7) . . . . ? O6 Pb1 O9 N3 135.4(7) . . . . ? O3 Pb1 O9 N3 -151.0(6) . . . . ? O2 Pb1 O9 N3 -104.9(6) . . . . ? C8 O4 C9 C10 -176.7(9) . . . . ? Pb1 O4 C9 C10 46.2(10) . . . . ? C1 N1 C10 C9 -75.9(12) . . . . ? C11 N1 C10 C9 163.3(10) . . . . ? Pb1 N1 C10 C9 45.4(11) . . . . ? O4 C9 C10 N1 -63.5(13) . . . . ? O14 Pb2 O11 C15 86.9(8) . . . . ? O16 Pb2 O11 C15 19.3(10) . . . . ? O15 Pb2 O11 C15 122.9(10) . . . . ? O13 Pb2 O11 C15 150.6(8) . . . . ? O18 Pb2 O11 C15 -84.7(9) . . . . ? O18A Pb2 O11 C15 -65.2(10) . . . . ? N4 Pb2 O11 C15 24.4(8) . . . . ? O21 Pb2 O11 C15 -119.5(9) . . . . ? O19 Pb2 O11 C15 -55.1(10) . . . . ? O12 Pb2 O11 C15 -157.9(9) . . . . ? O14 Pb2 O11 C16 -146.6(7) . . . . ? O16 Pb2 O11 C16 145.9(7) . . . . ? O15 Pb2 O11 C16 -110.6(10) . . . . ? O13 Pb2 O11 C16 -82.8(7) . . . . ? O18 Pb2 O11 C16 41.8(8) . . . . ? O18A Pb2 O11 C16 61.3(9) . . . . ? N4 Pb2 O11 C16 150.9(8) . . . . ? O21 Pb2 O11 C16 7.0(9) . . . . ? O19 Pb2 O11 C16 71.4(9) . . . . ? O12 Pb2 O11 C16 -31.4(7) . . . . ? C10 N1 C11 C12 44.6(13) . . . . ? C1 N1 C11 C12 -76.5(11) . . . . ? Pb1 N1 C11 C12 162.7(7) . . . . ? O14 Pb2 O12 C18 -55.4(8) . . . . ? O16 Pb2 O12 C18 52.1(12) . . . . ? O15 Pb2 O12 C18 26.9(9) . . . . ? O11 Pb2 O12 C18 -133.1(8) . . . . ? O13 Pb2 O12 C18 -14.6(8) . . . . ? O18 Pb2 O12 C18 116.3(9) . . . . ? O18A Pb2 O12 C18 150.9(10) . . . . ? N4 Pb2 O12 C18 -130.5(8) . . . . ? O21 Pb2 O12 C18 82.0(9) . . . . ? O19 Pb2 O12 C18 163.3(10) . . . . ? O14 Pb2 O12 C17 75.1(8) . . . . ? O16 Pb2 O12 C17 -177.3(8) . . . . ? O15 Pb2 O12 C17 157.5(8) . . . . ? O11 Pb2 O12 C17 -2.5(7) . . . . ? O13 Pb2 O12 C17 116.0(8) . . . . ? O18 Pb2 O12 C17 -113.1(9) . . . . ? O18A Pb2 O12 C17 -78.5(10) . . . . ? N4 Pb2 O12 C17 0.0(9) . . . . ? O21 Pb2 O12 C17 -147.4(9) . . . . ? O19 Pb2 O12 C17 -66.1(10) . . . . ? N1 C11 C12 C13 -128.9(13) . . . . ? O14 Pb2 O13 C20 -16.5(7) . . . . ? O16 Pb2 O13 C20 45.4(8) . . . . ? O15 Pb2 O13 C20 67.0(7) . . . . ? O11 Pb2 O13 C20 -103.7(7) . . . . ? O18 Pb2 O13 C20 144.8(9) . . . . ? O18A Pb2 O13 C20 -179.3(13) . . . . ? N4 Pb2 O13 C20 -40.5(8) . . . . ? O21 Pb2 O13 C20 136.8(8) . . . . ? O19 Pb2 O13 C20 -158.5(13) . . . . ? O12 Pb2 O13 C20 -154.0(8) . . . . ? O14 Pb2 O13 C19 116.3(8) . . . . ? O16 Pb2 O13 C19 178.2(8) . . . . ? O15 Pb2 O13 C19 -160.1(9) . . . . ? O11 Pb2 O13 C19 29.1(8) . . . . ? O18 Pb2 O13 C19 -82.4(10) . . . . ? O18A Pb2 O13 C19 -46.5(15) . . . . ? N4 Pb2 O13 C19 92.3(8) . . . . ? O21 Pb2 O13 C19 -90.4(9) . . . . ? O19 Pb2 O13 C19 -25.7(16) . . . . ? O12 Pb2 O13 C19 -21.2(8) . . . . ? O16 Pb2 O14 C21 -137.4(8) . . . . ? O15 Pb2 O14 C21 -88.0(7) . . . . ? O11 Pb2 O14 C21 80.9(7) . . . . ? O13 Pb2 O14 C21 -17.2(7) . . . . ? O18 Pb2 O14 C21 -128.0(16) . . . . ? O18A Pb2 O14 C21 142.9(13) . . . . ? N4 Pb2 O14 C21 141.6(8) . . . . ? O21 Pb2 O14 C21 -61.8(10) . . . . ? O19 Pb2 O14 C21 136.7(9) . . . . ? O12 Pb2 O14 C21 22.8(8) . . . . ? O16 Pb2 O14 C22 81.4(7) . . . . ? O15 Pb2 O14 C22 130.8(8) . . . . ? O11 Pb2 O14 C22 -60.3(7) . . . . ? O13 Pb2 O14 C22 -158.4(8) . . . . ? O18 Pb2 O14 C22 90.8(17) . . . . ? O18A Pb2 O14 C22 1.8(15) . . . . ? N4 Pb2 O14 C22 0.4(7) . . . . ? O21 Pb2 O14 C22 157.0(9) . . . . ? O19 Pb2 O14 C22 -4.5(11) . . . . ? O12 Pb2 O14 C22 -118.3(7) . . . . ? C24A N4 C14 C15 87.6(18) . . . . ? C23 N4 C14 C15 -158.4(10) . . . . ? C24 N4 C14 C15 73.4(17) . . . . ? Pb2 N4 C14 C15 -41.1(13) . . . . ? O17 N5 O15 Pb2 165.3(10) . . . . ? O16 N5 O15 Pb2 -14.2(11) . . . . ? O14 Pb2 O15 N5 -75.9(7) . . . . ? O16 Pb2 O15 N5 7.9(6) . . . . ? O11 Pb2 O15 N5 -113.5(9) . . . . ? O13 Pb2 O15 N5 -143.8(8) . . . . ? O18 Pb2 O15 N5 93.2(8) . . . . ? O18A Pb2 O15 N5 75.8(10) . . . . ? N4 Pb2 O15 N5 -24.4(8) . . . . ? O21 Pb2 O15 N5 121.5(8) . . . . ? O19 Pb2 O15 N5 64.0(11) . . . . ? O12 Pb2 O15 N5 176.5(7) . . . . ? C16 O11 C15 C14 178.9(12) . . . . ? Pb2 O11 C15 C14 -53.7(13) . . . . ? N4 C14 C15 O11 65.0(15) . . . . ? O17 N5 O16 Pb2 -165.0(10) . . . . ? O15 N5 O16 Pb2 14.5(11) . . . . ? O14 Pb2 O16 N5 74.1(7) . . . . ? O15 Pb2 O16 N5 -8.2(7) . . . . ? O11 Pb2 O16 N5 147.2(6) . . . . ? O13 Pb2 O16 N5 19.1(8) . . . . ? O18 Pb2 O16 N5 -103.1(8) . . . . ? O18A Pb2 O16 N5 -136.4(10) . . . . ? N4 Pb2 O16 N5 142.5(8) . . . . ? O21 Pb2 O16 N5 -67.7(8) . . . . ? O19 Pb2 O16 N5 -149.4(9) . . . . ? O12 Pb2 O16 N5 -39.8(12) . . . . ? C15 O11 C16 C17 -169.3(11) . . . . ? Pb2 O11 C16 C17 63.4(11) . . . . ? C18 O12 C17 C16 163.6(10) . . . . ? Pb2 O12 C17 C16 33.2(12) . . . . ? O11 C16 C17 O12 -62.3(14) . . . . ? O19 N6 O18 Pb2 19(4) . . . . ? O20 N6 O18 Pb2 -162(3) . . . . ? O14 Pb2 O18 N6 -121(2) . . . . ? O16 Pb2 O18 N6 -112.3(19) . . . . ? O15 Pb2 O18 N6 -159.7(19) . . . . ? O11 Pb2 O18 N6 29(2) . . . . ? O13 Pb2 O18 N6 136.8(18) . . . . ? O18A Pb2 O18 N6 -6(2) . . . . ? N4 Pb2 O18 N6 -39(2) . . . . ? O21 Pb2 O18 N6 151(2) . . . . ? O19 Pb2 O18 N6 -9.4(18) . . . . ? O12 Pb2 O18 N6 85.7(19) . . . . ? C17 O12 C18 C19 -86.0(12) . . . . ? Pb2 O12 C18 C19 47.5(12) . . . . ? O18 N6 O19 Pb2 -18(3) . . . . ? O20 N6 O19 Pb2 163(3) . . . . ? O14 Pb2 O19 N6 165.8(17) . . . . ? O16 Pb2 O19 N6 89.0(18) . . . . ? O15 Pb2 O19 N6 51(2) . . . . ? O11 Pb2 O19 N6 -130.1(19) . . . . ? O13 Pb2 O19 N6 -68(2) . . . . ? O18 Pb2 O19 N6 9.2(18) . . . . ? O18A Pb2 O19 N6 0(4) . . . . ? N4 Pb2 O19 N6 161.0(19) . . . . ? O21 Pb2 O19 N6 -2.5(18) . . . . ? O12 Pb2 O19 N6 -72.2(18) . . . . ? C20 O13 C19 C18 -176.1(9) . . . . ? Pb2 O13 C19 C18 51.8(11) . . . . ? O12 C18 C19 O13 -66.1(12) . . . . ? C19 O13 C20 C21 -87.7(11) . . . . ? Pb2 O13 C20 C21 46.8(11) . . . . ? C22 O14 C21 C20 -170.8(9) . . . . ? Pb2 O14 C21 C20 46.0(11) . . . . ? O13 C20 C21 O14 -61.4(12) . . . . ? C21 O14 C22 C23 -171.0(9) . . . . ? Pb2 O14 C22 C23 -28.0(11) . . . . ? C14 N4 C23 C22 66.2(14) . . . . ? C24A N4 C23 C22 172.7(18) . . . . ? C24 N4 C23 C22 -159.5(14) . . . . ? Pb2 N4 C23 C22 -54.8(11) . . . . ? O14 C22 C23 N4 57.9(14) . . . . ? C14 N4 C24 C25 76(2) . . . . ? C24A N4 C24 C25 43(3) . . . . ? C23 N4 C24 C25 -54(2) . . . . ? Pb2 N4 C24 C25 -162.7(16) . . . . ? N4 C24 C25 C26 136(2) . . . . ? O19A N6A O18A Pb2 -15(7) . . . . ? O20A N6A O18A Pb2 159(2) . . . . ? O14 Pb2 O18A N6A 168(4) . . . . ? O16 Pb2 O18A N6A 94(4) . . . . ? O15 Pb2 O18A N6A 51(4) . . . . ? O11 Pb2 O18A N6A -126(4) . . . . ? O13 Pb2 O18A N6A -44(5) . . . . ? O18 Pb2 O18A N6A 19(4) . . . . ? N4 Pb2 O18A N6A 169(4) . . . . ? O21 Pb2 O18A N6A 4(4) . . . . ? O19 Pb2 O18A N6A -173(7) . . . . ? O12 Pb2 O18A N6A -66(4) . . . . ? C14 N4 C24A C25A -172(2) . . . . ? C23 N4 C24A C25A 72(3) . . . . ? C24 N4 C24A C25A -21(3) . . . . ? Pb2 N4 C24A C25A -51(3) . . . . ? N4 C24A C25A C26A -133(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 3.356 _refine_diff_density_min -4.349 _refine_diff_density_rms 0.320 #===END data_ac45 #(Compound12) _database_code_CSD 180581 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H31 N3 O12 Pb' _chemical_formula_weight 652.62 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' '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4495(5) _cell_length_b 9.4557(3) _cell_length_c 27.680(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.563(3) _cell_angle_gamma 90.00 _cell_volume 2201.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 7.731 _exptl_absorpt_correction_type scalepack _exptl_absorpt_correction_T_min 0.6985 _exptl_absorpt_correction_T_max 0.8607 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '1.6 o phi+omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13197 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4930 _reflns_number_gt 3837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'nonius collect' _computing_cell_refinement 'denzo-smn' _computing_data_reduction 'denzo-smn' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'xseed Barbour 1999' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+0.8185P] 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 SHELXL _refine_ls_extinction_coef 0.00122(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4930 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Pb1 Pb 0.42861(2) 0.738362(18) 0.380317(7) 0.01364(9) Uani 1 1 d . . . O1 O 0.4440(4) 0.4633(4) 0.39827(15) 0.0194(9) Uani 1 1 d . . . N1 N 0.2550(5) 0.6557(4) 0.45098(18) 0.0156(10) Uani 1 1 d . . . C1 C 0.2776(6) 0.5020(5) 0.4618(2) 0.0164(12) Uani 1 1 d . . . H1A H 0.1829 0.4662 0.4764 0.020 Uiso 1 1 calc R . . H1B H 0.3705 0.4904 0.4862 0.020 Uiso 1 1 calc R . . O2 O 0.6120(4) 0.5744(3) 0.32476(14) 0.0165(9) Uani 1 1 d . . . C2 C 0.3029(7) 0.4139(5) 0.4181(2) 0.0193(13) Uani 1 1 d . . . H2A H 0.3151 0.3132 0.4274 0.023 Uiso 1 1 calc R . . H2B H 0.2101 0.4227 0.3935 0.023 Uiso 1 1 calc R . . O3 O 0.6901(4) 0.8636(3) 0.33799(15) 0.0175(9) Uani 1 1 d . . . C3 C 0.4828(7) 0.3765(5) 0.3583(2) 0.0209(13) Uani 1 1 d . . . H3A H 0.3963 0.3811 0.3315 0.025 Uiso 1 1 calc R . . H3B H 0.4959 0.2768 0.3688 0.025 Uiso 1 1 calc R . . O4 O 0.3931(4) 1.0137(3) 0.34211(15) 0.0175(9) Uani 1 1 d . . . C4 C 0.6355(7) 0.4310(5) 0.3412(2) 0.0208(13) Uani 1 1 d . . . H4A H 0.7214 0.4274 0.3682 0.025 Uiso 1 1 calc R . . H4B H 0.6670 0.3711 0.3144 0.025 Uiso 1 1 calc R . . O5 O 0.1473(4) 0.8701(3) 0.38037(15) 0.0176(9) Uani 1 1 d . . . C5 C 0.7594(6) 0.6336(5) 0.3122(2) 0.0200(13) Uani 1 1 d . . . H5A H 0.7989 0.5791 0.2853 0.024 Uiso 1 1 calc R . . H5B H 0.8405 0.6295 0.3405 0.024 Uiso 1 1 calc R . . C6 C 0.7298(7) 0.7839(5) 0.2970(2) 0.0178(12) Uani 1 1 d . . . H6A H 0.8261 0.8239 0.2845 0.021 Uiso 1 1 calc R . . H6B H 0.6414 0.7885 0.2708 0.021 Uiso 1 1 calc R . . C7 C 0.6635(6) 1.0114(5) 0.3277(2) 0.0175(13) Uani 1 1 d . . . H7A H 0.7408 1.0440 0.3054 0.021 Uiso 1 1 calc R . . H7B H 0.6828 1.0660 0.3582 0.021 Uiso 1 1 calc R . . C8 C 0.4964(6) 1.0411(5) 0.3049(2) 0.0168(12) Uani 1 1 d . . . H8A H 0.4865 1.1407 0.2940 0.020 Uiso 1 1 calc R . . H8B H 0.4696 0.9786 0.2766 0.020 Uiso 1 1 calc R . . C9 C 0.2281(6) 1.0438(5) 0.3257(2) 0.0184(13) Uani 1 1 d . . . H9A H 0.1912 0.9821 0.2980 0.022 Uiso 1 1 calc R . . H9B H 0.2162 1.1436 0.3152 0.022 Uiso 1 1 calc R . . C10 C 0.1338(7) 1.0166(5) 0.3675(2) 0.0214(13) Uani 1 1 d . . . H10A H 0.1740 1.0759 0.3955 0.026 Uiso 1 1 calc R . . H10B H 0.0208 1.0410 0.3585 0.026 Uiso 1 1 calc R . . C11 C 0.0509(6) 0.8320(6) 0.4189(2) 0.0195(13) Uani 1 1 d . . . H11A H -0.0631 0.8428 0.4074 0.023 Uiso 1 1 calc R . . H11B H 0.0756 0.8953 0.4471 0.023 Uiso 1 1 calc R . . C12 C 0.0853(6) 0.6804(5) 0.4336(2) 0.0174(13) Uani 1 1 d . . . H12A H 0.0185 0.6544 0.4597 0.021 Uiso 1 1 calc R . . H12B H 0.0554 0.6180 0.4055 0.021 Uiso 1 1 calc R . . C13 C 0.3044(6) 0.7370(5) 0.4963(2) 0.0163(12) Uani 1 1 d . . . H13A H 0.4191 0.7206 0.5055 0.020 Uiso 1 1 calc R . . H13B H 0.2897 0.8391 0.4895 0.020 Uiso 1 1 calc R . . C14 C 0.2149(6) 0.6991(6) 0.5384(2) 0.0195(13) Uani 1 1 d . . . H14 H 0.2242 0.6045 0.5500 0.023 Uiso 1 1 calc R . . C15 C 0.1244(7) 0.7852(6) 0.5610(2) 0.0271(14) Uani 1 1 d . . . H15A H 0.1118 0.8807 0.5507 0.032 Uiso 1 1 calc R . . H15B H 0.0717 0.7518 0.5876 0.032 Uiso 1 1 calc R . . O1A O 0.6608(4) 0.7066(4) 0.44662(16) 0.0247(10) Uani 1 1 d . . . N1A N 0.6691(6) 0.8350(5) 0.46173(19) 0.0231(12) Uani 1 1 d . . . O2A O 0.5701(4) 0.9217(4) 0.44254(15) 0.0224(10) Uani 1 1 d . . . O3A O 0.7718(5) 0.8691(4) 0.49445(18) 0.0338(11) Uani 1 1 d . . . O1B O 0.1990(5) 0.5899(4) 0.32155(16) 0.0242(10) Uani 1 1 d . . . N1B N 0.1894(6) 0.6576(4) 0.28258(19) 0.0185(11) Uani 1 1 d . . . O2B O 0.2944(5) 0.7464(3) 0.27496(16) 0.0233(9) Uani 1 1 d . . . O3B O 0.0738(4) 0.6372(4) 0.25151(16) 0.0263(10) Uani 1 1 d . . . O1C O -0.0062(5) 0.8387(5) 0.17544(19) 0.0303(11) Uani 1 1 d . . . H1C H 0.017(11) 0.782(9) 0.204(4) 0.09(3) Uiso 1 1 d . . . H2C H -0.037(7) 0.930(6) 0.188(2) 0.028(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01172(13) 0.01480(14) 0.01482(14) 0.00068(8) 0.00339(8) 0.00070(8) O1 0.016(2) 0.021(2) 0.021(3) -0.0013(16) 0.0078(18) -0.0011(15) N1 0.007(2) 0.020(2) 0.019(3) -0.0017(18) 0.000(2) -0.0011(17) C1 0.012(3) 0.021(3) 0.016(4) 0.007(2) 0.003(2) 0.000(2) O2 0.016(2) 0.0161(19) 0.019(2) 0.0008(15) 0.0064(18) 0.0039(14) C2 0.017(3) 0.021(3) 0.020(4) 0.005(2) 0.004(3) -0.005(2) O3 0.016(2) 0.0169(19) 0.020(3) 0.0006(15) 0.0052(18) 0.0033(14) C3 0.026(3) 0.016(3) 0.022(4) -0.005(2) 0.007(3) 0.003(2) O4 0.014(2) 0.0185(19) 0.021(3) 0.0045(15) 0.0048(18) 0.0029(14) C4 0.028(4) 0.018(3) 0.017(4) -0.002(2) 0.006(3) 0.006(2) O5 0.015(2) 0.0139(18) 0.026(3) 0.0072(15) 0.0106(18) 0.0028(14) C5 0.012(3) 0.023(3) 0.026(4) -0.003(2) 0.007(3) 0.008(2) C6 0.021(3) 0.025(3) 0.010(3) 0.001(2) 0.011(2) 0.001(2) C7 0.020(3) 0.012(3) 0.020(4) 0.002(2) 0.001(3) -0.005(2) C8 0.014(3) 0.020(3) 0.017(4) 0.000(2) 0.002(2) 0.002(2) C9 0.015(3) 0.017(3) 0.022(4) 0.004(2) -0.003(3) 0.004(2) C10 0.011(3) 0.022(3) 0.031(4) 0.001(2) 0.004(3) 0.000(2) C11 0.013(3) 0.030(3) 0.016(4) 0.001(2) 0.006(3) 0.005(2) C12 0.012(3) 0.021(3) 0.019(4) 0.004(2) -0.002(3) -0.002(2) C13 0.014(3) 0.017(3) 0.018(3) -0.002(2) 0.001(2) 0.003(2) C14 0.015(3) 0.020(3) 0.023(4) 0.005(2) 0.004(3) -0.002(2) C15 0.026(3) 0.032(3) 0.025(4) 0.004(3) 0.008(3) 0.005(3) O1A 0.018(2) 0.024(2) 0.032(3) 0.0050(18) 0.0018(19) 0.0005(16) N1A 0.022(3) 0.027(3) 0.020(3) 0.005(2) 0.004(2) -0.002(2) O2A 0.019(2) 0.024(2) 0.024(3) 0.0004(16) -0.0014(19) -0.0002(16) O3A 0.024(3) 0.047(3) 0.029(3) -0.001(2) -0.005(2) -0.0111(19) O1B 0.028(2) 0.025(2) 0.020(3) 0.0037(17) 0.000(2) -0.0049(16) N1B 0.019(3) 0.020(3) 0.018(3) -0.0011(19) 0.007(2) 0.0045(19) O2B 0.025(2) 0.022(2) 0.024(3) 0.0013(16) 0.0076(19) -0.0061(16) O3B 0.014(2) 0.041(2) 0.024(3) 0.0005(19) -0.001(2) -0.0027(17) O1C 0.032(3) 0.025(3) 0.035(3) -0.002(2) 0.005(2) 0.0001(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1A 2.571(4) . ? Pb1 O2A 2.646(4) . ? Pb1 O1 2.649(3) . ? Pb1 N1 2.673(5) . ? Pb1 O5 2.684(3) . ? Pb1 O2 2.762(3) . ? Pb1 O1B 2.787(4) . ? Pb1 O4 2.815(3) . ? Pb1 O3 2.857(4) . ? Pb1 O2B 3.026(4) . ? O1 C2 1.438(6) . ? O1 C3 1.441(7) . ? N1 C12 1.486(6) . ? N1 C1 1.492(6) . ? N1 C13 1.496(7) . ? C1 C2 1.503(8) . ? O2 C4 1.439(6) . ? O2 C5 1.439(6) . ? O3 C6 1.428(6) . ? O3 C7 1.440(6) . ? C3 C4 1.507(8) . ? O4 C8 1.437(6) . ? O4 C9 1.452(6) . ? O5 C10 1.432(6) . ? O5 C11 1.448(6) . ? C5 C6 1.496(7) . ? C7 C8 1.515(7) . ? C9 C10 1.489(8) . ? C11 C12 1.511(7) . ? C13 C14 1.493(8) . ? C14 C15 1.315(8) . ? O1A N1A 1.283(6) . ? N1A O3A 1.235(6) . ? N1A O2A 1.253(6) . ? O1B N1B 1.250(6) . ? N1B O3B 1.252(6) . ? N1B O2B 1.254(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 O1A Pb1 O2A 49.20(11) . . ? O1A Pb1 O1 74.40(12) . . ? O2A Pb1 O1 120.69(12) . . ? O1A Pb1 N1 83.01(13) . . ? O2A Pb1 N1 87.74(13) . . ? O1 Pb1 N1 66.18(12) . . ? O1A Pb1 O5 131.94(12) . . ? O2A Pb1 O5 92.27(11) . . ? O1 Pb1 O5 118.90(10) . . ? N1 Pb1 O5 65.58(12) . . ? O1A Pb1 O2 84.35(12) . . ? O2A Pb1 O2 119.19(11) . . ? O1 Pb1 O2 62.18(11) . . ? N1 Pb1 O2 128.34(11) . . ? O5 Pb1 O2 143.65(12) . . ? O1A Pb1 O1B 142.91(11) . . ? O2A Pb1 O1B 162.70(12) . . ? O1 Pb1 O1B 68.52(11) . . ? N1 Pb1 O1B 83.08(13) . . ? O5 Pb1 O1B 70.59(11) . . ? O2 Pb1 O1B 77.80(11) . . ? O1A Pb1 O4 114.99(11) . . ? O2A Pb1 O4 70.34(11) . . ? O1 Pb1 O4 168.54(12) . . ? N1 Pb1 O4 119.96(11) . . ? O5 Pb1 O4 60.57(10) . . ? O2 Pb1 O4 110.79(11) . . ? O1B Pb1 O4 101.75(11) . . ? O1A Pb1 O3 76.95(12) . . ? O2A Pb1 O3 71.14(12) . . ? O1 Pb1 O3 117.26(10) . . ? N1 Pb1 O3 157.31(13) . . ? O5 Pb1 O3 121.87(10) . . ? O2 Pb1 O3 60.43(10) . . ? O1B Pb1 O3 119.46(12) . . ? O4 Pb1 O3 61.38(10) . . ? O1A Pb1 O2B 151.62(12) . . ? O2A Pb1 O2B 135.60(10) . . ? O1 Pb1 O2B 102.26(11) . . ? N1 Pb1 O2B 122.11(12) . . ? O5 Pb1 O2B 74.91(12) . . ? O2 Pb1 O2B 69.85(11) . . ? O1B Pb1 O2B 43.57(10) . . ? O4 Pb1 O2B 66.32(10) . . ? O3 Pb1 O2B 80.03(11) . . ? C2 O1 C3 111.5(4) . . ? C2 O1 Pb1 111.3(3) . . ? C3 O1 Pb1 115.2(3) . . ? C12 N1 C1 108.6(4) . . ? C12 N1 C13 111.8(4) . . ? C1 N1 C13 108.1(4) . . ? C12 N1 Pb1 107.4(3) . . ? C1 N1 Pb1 111.3(3) . . ? C13 N1 Pb1 109.6(3) . . ? N1 C1 C2 113.8(5) . . ? C4 O2 C5 110.3(4) . . ? C4 O2 Pb1 114.9(3) . . ? C5 O2 Pb1 117.5(3) . . ? O1 C2 C1 108.4(4) . . ? C6 O3 C7 113.5(4) . . ? C6 O3 Pb1 110.9(3) . . ? C7 O3 Pb1 111.8(3) . . ? O1 C3 C4 108.1(4) . . ? C8 O4 C9 111.9(4) . . ? C8 O4 Pb1 112.7(3) . . ? C9 O4 Pb1 111.3(3) . . ? O2 C4 C3 109.0(4) . . ? C10 O5 C11 112.8(4) . . ? C10 O5 Pb1 119.9(3) . . ? C11 O5 Pb1 116.5(3) . . ? O2 C5 C6 108.2(4) . . ? O3 C6 C5 108.9(4) . . ? O3 C7 C8 112.6(4) . . ? O4 C8 C7 106.0(4) . . ? O4 C9 C10 107.1(4) . . ? O5 C10 C9 109.0(4) . . ? O5 C11 C12 109.2(4) . . ? N1 C12 C11 113.0(4) . . ? C14 C13 N1 114.2(4) . . ? C15 C14 C13 125.7(5) . . ? N1A O1A Pb1 97.8(3) . . ? O3A N1A O2A 122.2(5) . . ? O3A N1A O1A 119.9(5) . . ? O2A N1A O1A 117.9(5) . . ? N1A O2A Pb1 95.1(3) . . ? N1B O1B Pb1 103.3(3) . . ? O1B N1B O3B 119.7(5) . . ? O1B N1B O2B 120.0(5) . . ? O3B N1B O2B 120.3(5) . . ? N1B O2B Pb1 91.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1A Pb1 O1 C2 115.8(4) . . . . ? O2A Pb1 O1 C2 98.5(3) . . . . ? N1 Pb1 O1 C2 26.7(3) . . . . ? O5 Pb1 O1 C2 -13.8(4) . . . . ? O2 Pb1 O1 C2 -152.3(4) . . . . ? O1B Pb1 O1 C2 -65.2(3) . . . . ? O4 Pb1 O1 C2 -98.0(6) . . . . ? O3 Pb1 O1 C2 -178.2(3) . . . . ? O2B Pb1 O1 C2 -93.2(3) . . . . ? O1A Pb1 O1 C3 -116.0(3) . . . . ? O2A Pb1 O1 C3 -133.3(3) . . . . ? N1 Pb1 O1 C3 154.9(4) . . . . ? O5 Pb1 O1 C3 114.3(3) . . . . ? O2 Pb1 O1 C3 -24.2(3) . . . . ? O1B Pb1 O1 C3 63.0(3) . . . . ? O4 Pb1 O1 C3 30.1(7) . . . . ? O3 Pb1 O1 C3 -50.0(4) . . . . ? O2B Pb1 O1 C3 34.9(3) . . . . ? O1A Pb1 N1 C12 169.3(3) . . . . ? O2A Pb1 N1 C12 120.2(3) . . . . ? O1 Pb1 N1 C12 -114.7(3) . . . . ? O5 Pb1 N1 C12 26.7(3) . . . . ? O2 Pb1 N1 C12 -113.6(3) . . . . ? O1B Pb1 N1 C12 -45.1(3) . . . . ? O4 Pb1 N1 C12 54.5(3) . . . . ? O3 Pb1 N1 C12 141.3(3) . . . . ? O2B Pb1 N1 C12 -24.8(3) . . . . ? O1A Pb1 N1 C1 -71.9(3) . . . . ? O2A Pb1 N1 C1 -121.1(3) . . . . ? O1 Pb1 N1 C1 4.1(3) . . . . ? O5 Pb1 N1 C1 145.4(4) . . . . ? O2 Pb1 N1 C1 5.2(4) . . . . ? O1B Pb1 N1 C1 73.6(3) . . . . ? O4 Pb1 N1 C1 173.2(3) . . . . ? O3 Pb1 N1 C1 -99.9(4) . . . . ? O2B Pb1 N1 C1 93.9(3) . . . . ? O1A Pb1 N1 C13 47.7(3) . . . . ? O2A Pb1 N1 C13 -1.5(3) . . . . ? O1 Pb1 N1 C13 123.7(3) . . . . ? O5 Pb1 N1 C13 -95.0(3) . . . . ? O2 Pb1 N1 C13 124.8(3) . . . . ? O1B Pb1 N1 C13 -166.8(3) . . . . ? O4 Pb1 N1 C13 -67.2(3) . . . . ? O3 Pb1 N1 C13 19.7(5) . . . . ? O2B Pb1 N1 C13 -146.5(3) . . . . ? C12 N1 C1 C2 83.8(5) . . . . ? C13 N1 C1 C2 -154.6(4) . . . . ? Pb1 N1 C1 C2 -34.2(5) . . . . ? O1A Pb1 O2 C4 66.0(3) . . . . ? O2A Pb1 O2 C4 102.1(3) . . . . ? O1 Pb1 O2 C4 -9.3(3) . . . . ? N1 Pb1 O2 C4 -10.5(4) . . . . ? O5 Pb1 O2 C4 -111.2(3) . . . . ? O1B Pb1 O2 C4 -81.3(3) . . . . ? O4 Pb1 O2 C4 -179.4(3) . . . . ? O3 Pb1 O2 C4 144.2(4) . . . . ? O2B Pb1 O2 C4 -126.1(3) . . . . ? O1A Pb1 O2 C5 -66.3(4) . . . . ? O2A Pb1 O2 C5 -30.1(4) . . . . ? O1 Pb1 O2 C5 -141.6(4) . . . . ? N1 Pb1 O2 C5 -142.8(3) . . . . ? O5 Pb1 O2 C5 116.6(4) . . . . ? O1B Pb1 O2 C5 146.4(4) . . . . ? O4 Pb1 O2 C5 48.3(4) . . . . ? O3 Pb1 O2 C5 11.9(3) . . . . ? O2B Pb1 O2 C5 101.7(4) . . . . ? C3 O1 C2 C1 175.5(4) . . . . ? Pb1 O1 C2 C1 -54.3(5) . . . . ? N1 C1 C2 O1 60.7(6) . . . . ? O1A Pb1 O3 C6 113.6(3) . . . . ? O2A Pb1 O3 C6 164.6(3) . . . . ? O1 Pb1 O3 C6 49.1(3) . . . . ? N1 Pb1 O3 C6 142.2(4) . . . . ? O5 Pb1 O3 C6 -114.8(3) . . . . ? O2 Pb1 O3 C6 22.7(3) . . . . ? O1B Pb1 O3 C6 -30.4(3) . . . . ? O4 Pb1 O3 C6 -118.0(3) . . . . ? O2B Pb1 O3 C6 -49.7(3) . . . . ? O1A Pb1 O3 C7 -118.6(3) . . . . ? O2A Pb1 O3 C7 -67.6(3) . . . . ? O1 Pb1 O3 C7 176.9(3) . . . . ? N1 Pb1 O3 C7 -90.0(4) . . . . ? O5 Pb1 O3 C7 13.0(4) . . . . ? O2 Pb1 O3 C7 150.5(4) . . . . ? O1B Pb1 O3 C7 97.4(3) . . . . ? O4 Pb1 O3 C7 9.8(3) . . . . ? O2B Pb1 O3 C7 78.1(3) . . . . ? C2 O1 C3 C4 -177.4(4) . . . . ? Pb1 O1 C3 C4 54.5(5) . . . . ? O1A Pb1 O4 C8 82.8(3) . . . . ? O2A Pb1 O4 C8 104.0(3) . . . . ? O1 Pb1 O4 C8 -60.9(6) . . . . ? N1 Pb1 O4 C8 179.3(3) . . . . ? O5 Pb1 O4 C8 -151.5(3) . . . . ? O2 Pb1 O4 C8 -10.7(3) . . . . ? O1B Pb1 O4 C8 -92.0(3) . . . . ? O3 Pb1 O4 C8 25.3(3) . . . . ? O2B Pb1 O4 C8 -66.0(3) . . . . ? O1A Pb1 O4 C9 -150.6(3) . . . . ? O2A Pb1 O4 C9 -129.4(3) . . . . ? O1 Pb1 O4 C9 65.7(7) . . . . ? N1 Pb1 O4 C9 -54.1(4) . . . . ? O5 Pb1 O4 C9 -24.9(3) . . . . ? O2 Pb1 O4 C9 115.9(3) . . . . ? O1B Pb1 O4 C9 34.6(3) . . . . ? O3 Pb1 O4 C9 152.0(4) . . . . ? O2B Pb1 O4 C9 60.6(3) . . . . ? C5 O2 C4 C3 175.0(5) . . . . ? Pb1 O2 C4 C3 39.4(5) . . . . ? O1 C3 C4 O2 -61.5(6) . . . . ? O1A Pb1 O5 C10 89.5(4) . . . . ? O2A Pb1 O5 C10 57.1(4) . . . . ? O1 Pb1 O5 C10 -175.7(4) . . . . ? N1 Pb1 O5 C10 143.5(4) . . . . ? O2 Pb1 O5 C10 -94.3(4) . . . . ? O1B Pb1 O5 C10 -125.3(4) . . . . ? O4 Pb1 O5 C10 -8.8(4) . . . . ? O3 Pb1 O5 C10 -12.1(4) . . . . ? O2B Pb1 O5 C10 -79.8(4) . . . . ? O1A Pb1 O5 C11 -52.2(4) . . . . ? O2A Pb1 O5 C11 -84.7(3) . . . . ? O1 Pb1 O5 C11 42.6(4) . . . . ? N1 Pb1 O5 C11 1.8(3) . . . . ? O2 Pb1 O5 C11 124.0(3) . . . . ? O1B Pb1 O5 C11 92.9(3) . . . . ? O4 Pb1 O5 C11 -150.6(4) . . . . ? O3 Pb1 O5 C11 -153.8(3) . . . . ? O2B Pb1 O5 C11 138.4(3) . . . . ? C4 O2 C5 C6 -178.0(4) . . . . ? Pb1 O2 C5 C6 -43.7(5) . . . . ? C7 O3 C6 C5 178.4(4) . . . . ? Pb1 O3 C6 C5 -54.8(5) . . . . ? O2 C5 C6 O3 66.1(6) . . . . ? C6 O3 C7 C8 82.9(6) . . . . ? Pb1 O3 C7 C8 -43.5(5) . . . . ? C9 O4 C8 C7 177.6(4) . . . . ? Pb1 O4 C8 C7 -56.1(4) . . . . ? O3 C7 C8 O4 68.2(5) . . . . ? C8 O4 C9 C10 -178.1(4) . . . . ? Pb1 O4 C9 C10 54.8(4) . . . . ? C11 O5 C10 C9 -176.4(4) . . . . ? Pb1 O5 C10 C9 40.6(5) . . . . ? O4 C9 C10 O5 -62.7(5) . . . . ? C10 O5 C11 C12 -174.2(4) . . . . ? Pb1 O5 C11 C12 -29.8(5) . . . . ? C1 N1 C12 C11 -176.8(5) . . . . ? C13 N1 C12 C11 64.0(6) . . . . ? Pb1 N1 C12 C11 -56.3(5) . . . . ? O5 C11 C12 N1 59.2(6) . . . . ? C12 N1 C13 C14 61.1(6) . . . . ? C1 N1 C13 C14 -58.4(5) . . . . ? Pb1 N1 C13 C14 -179.9(3) . . . . ? N1 C13 C14 C15 -118.1(6) . . . . ? O2A Pb1 O1A N1A -1.1(3) . . . . ? O1 Pb1 O1A N1A -161.3(3) . . . . ? N1 Pb1 O1A N1A -94.2(3) . . . . ? O5 Pb1 O1A N1A -46.3(3) . . . . ? O2 Pb1 O1A N1A 136.0(3) . . . . ? O1B Pb1 O1A N1A -162.9(3) . . . . ? O4 Pb1 O1A N1A 25.7(3) . . . . ? O3 Pb1 O1A N1A 75.1(3) . . . . ? O2B Pb1 O1A N1A 111.7(3) . . . . ? Pb1 O1A N1A O3A -178.6(5) . . . . ? Pb1 O1A N1A O2A 2.0(5) . . . . ? O3A N1A O2A Pb1 178.6(5) . . . . ? O1A N1A O2A Pb1 -1.9(5) . . . . ? O1A Pb1 O2A N1A 1.1(3) . . . . ? O1 Pb1 O2A N1A 23.4(3) . . . . ? N1 Pb1 O2A N1A 83.8(3) . . . . ? O5 Pb1 O2A N1A 149.3(3) . . . . ? O2 Pb1 O2A N1A -49.7(3) . . . . ? O1B Pb1 O2A N1A 141.7(4) . . . . ? O4 Pb1 O2A N1A -153.1(3) . . . . ? O3 Pb1 O2A N1A -87.7(3) . . . . ? O2B Pb1 O2A N1A -140.1(3) . . . . ? O1A Pb1 O1B N1B -143.9(3) . . . . ? O2A Pb1 O1B N1B 89.0(5) . . . . ? O1 Pb1 O1B N1B -145.5(3) . . . . ? N1 Pb1 O1B N1B 147.4(3) . . . . ? O5 Pb1 O1B N1B 81.0(3) . . . . ? O2 Pb1 O1B N1B -80.8(3) . . . . ? O4 Pb1 O1B N1B 28.2(3) . . . . ? O3 Pb1 O1B N1B -35.4(3) . . . . ? O2B Pb1 O1B N1B -7.3(3) . . . . ? Pb1 O1B N1B O3B -165.1(4) . . . . ? Pb1 O1B N1B O2B 14.2(5) . . . . ? O1B N1B O2B Pb1 -12.7(5) . . . . ? O3B N1B O2B Pb1 166.6(4) . . . . ? O1A Pb1 O2B N1B 126.4(3) . . . . ? O2A Pb1 O2B N1B -147.9(3) . . . . ? O1 Pb1 O2B N1B 46.6(3) . . . . ? N1 Pb1 O2B N1B -22.8(3) . . . . ? O5 Pb1 O2B N1B -70.4(3) . . . . ? O2 Pb1 O2B N1B 100.5(3) . . . . ? O1B Pb1 O2B N1B 7.1(3) . . . . ? O4 Pb1 O2B N1B -134.5(3) . . . . ? O3 Pb1 O2B N1B 162.5(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1C H1C O3B 0.96(10) 1.93(10) 2.871(7) 168(8) . O1C H2C O1B 0.98(6) 2.04(6) 2.886(6) 144(5) 2 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.256 _refine_diff_density_min -2.602 _refine_diff_density_rms 0.264 #===END data_ac42 #(compound13) _database_code_CSD 180582 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H29 Ag B F4 N O5' _chemical_formula_weight 498.07 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3966(7) _cell_length_b 5.8041(2) _cell_length_c 24.5126(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.767(2) _cell_angle_gamma 90.00 _cell_volume 1905.08(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 1.122 _exptl_absorpt_correction_type scalepack _exptl_absorpt_correction_T_min 0.8960 _exptl_absorpt_correction_T_max 0.9779 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi+omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12844 _diffrn_reflns_av_R_equivalents 0.0806 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4315 _reflns_number_gt 3460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'nonius collect' _computing_cell_refinement denzo-smn _computing_data_reduction denzo-smn _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics xseed _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.6454P] 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 SHELXL _refine_ls_extinction_coef 0.0017(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4315 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0610 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Ag1 Ag 0.246765(14) 0.37045(3) 0.124343(7) 0.01406(8) Uani 1 1 d . . . F1 F 0.24097(12) -0.2118(3) -0.18061(6) 0.0269(4) Uani 1 1 d . . . O1 O 0.41895(13) 0.4265(3) 0.18950(7) 0.0166(4) Uani 1 1 d . . . N1 N 0.23605(14) 0.1201(3) 0.19976(8) 0.0122(4) Uani 1 1 d . . . C1 C 0.33036(18) 0.1074(4) 0.23360(10) 0.0151(5) Uani 1 1 d . . . H1A H 0.3755 -0.0058 0.2169 0.018 Uiso 1 1 calc R . . H1B H 0.3145 0.0497 0.2703 0.018 Uiso 1 1 calc R . . B1 B 0.2377(2) -0.0594(5) -0.13650(12) 0.0194(7) Uani 1 1 d . . . F2 F 0.14862(12) 0.0654(2) -0.14057(6) 0.0269(4) Uani 1 1 d . . . O2 O 0.45535(13) 0.4436(3) 0.07559(7) 0.0171(4) Uani 1 1 d . . . C2 C 0.38510(19) 0.3350(4) 0.23982(10) 0.0167(5) Uani 1 1 d . . . H2A H 0.3401 0.4485 0.2565 0.020 Uiso 1 1 calc R . . H2B H 0.4434 0.3134 0.2651 0.020 Uiso 1 1 calc R . . F3 F 0.24116(12) -0.1804(3) -0.08746(6) 0.0276(4) Uani 1 1 d . . . O3 O 0.27586(12) 0.2524(3) 0.02409(7) 0.0149(4) Uani 1 1 d . . . C3 C 0.49976(19) 0.3025(4) 0.16695(10) 0.0170(5) Uani 1 1 d . . . H3A H 0.4780 0.1454 0.1563 0.020 Uiso 1 1 calc R . . H3B H 0.5557 0.2894 0.1941 0.020 Uiso 1 1 calc R . . F4 F 0.31905(12) 0.0890(3) -0.13824(6) 0.0321(4) Uani 1 1 d . . . O4 O 0.08422(12) 0.3687(3) 0.05751(7) 0.0167(4) Uani 1 1 d . . . C4 C 0.53253(18) 0.4342(4) 0.11757(10) 0.0177(6) Uani 1 1 d . . . H4A H 0.5511 0.5930 0.1286 0.021 Uiso 1 1 calc R . . H4B H 0.5925 0.3596 0.1029 0.021 Uiso 1 1 calc R . . O5 O 0.06558(12) 0.4356(3) 0.17158(7) 0.0165(4) Uani 1 1 d . . . C5 C 0.4529(2) 0.2442(4) 0.04147(11) 0.0193(6) Uani 1 1 d . . . H5A H 0.4406 0.1048 0.0636 0.023 Uiso 1 1 calc R . . H5B H 0.5177 0.2256 0.0236 0.023 Uiso 1 1 calc R . . C6 C 0.37092(19) 0.2745(5) -0.00056(10) 0.0183(6) Uani 1 1 d . . . H6A H 0.3763 0.4285 -0.0176 0.022 Uiso 1 1 calc R . . H6B H 0.3772 0.1568 -0.0295 0.022 Uiso 1 1 calc R . . C7 C 0.19728(18) 0.3155(5) -0.01401(10) 0.0174(6) Uani 1 1 d . . . H7A H 0.2073 0.2388 -0.0495 0.021 Uiso 1 1 calc R . . H7B H 0.1976 0.4842 -0.0199 0.021 Uiso 1 1 calc R . . C8 C 0.0998(2) 0.2425(4) 0.00863(10) 0.0174(6) Uani 1 1 d . . . H8A H 0.0448 0.2734 -0.0183 0.021 Uiso 1 1 calc R . . H8B H 0.1010 0.0752 0.0165 0.021 Uiso 1 1 calc R . . C9 C -0.00307(19) 0.2966(5) 0.08451(10) 0.0176(6) Uani 1 1 d . . . H9A H 0.0044 0.1348 0.0967 0.021 Uiso 1 1 calc R . . H9B H -0.0620 0.3065 0.0592 0.021 Uiso 1 1 calc R . . C10 C -0.01707(19) 0.4509(4) 0.13274(10) 0.0178(6) Uani 1 1 d . . . H10A H -0.0241 0.6122 0.1200 0.021 Uiso 1 1 calc R . . H10B H -0.0794 0.4076 0.1509 0.021 Uiso 1 1 calc R . . C11 C 0.0561(2) 0.2477(4) 0.20872(11) 0.0162(6) Uani 1 1 d . . . H11A H 0.0332 0.1083 0.1887 0.019 Uiso 1 1 calc R . . H11B H 0.0063 0.2856 0.2363 0.019 Uiso 1 1 calc R . . C12 C 0.15623(18) 0.2030(4) 0.23634(10) 0.0152(5) Uani 1 1 d . . . H12A H 0.1794 0.3472 0.2542 0.018 Uiso 1 1 calc R . . H12B H 0.1474 0.0869 0.2654 0.018 Uiso 1 1 calc R . . C13 C 0.21107(19) -0.1182(4) 0.18069(10) 0.0149(5) Uani 1 1 d . . . H13A H 0.1408 -0.1224 0.1670 0.018 Uiso 1 1 calc R . . H13B H 0.2177 -0.2260 0.2119 0.018 Uiso 1 1 calc R . . C14 C 0.2778(2) -0.1959(4) 0.13623(10) 0.0161(6) Uani 1 1 d . . . H14 H 0.3464 -0.2224 0.1451 0.019 Uiso 1 1 calc R . . C15 C 0.2456(2) -0.2294(4) 0.08499(11) 0.0218(7) Uani 1 1 d . . . H15A H 0.1773 -0.2040 0.0751 0.026 Uiso 1 1 calc R . . H15B H 0.2908 -0.2787 0.0583 0.026 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01616(12) 0.01397(11) 0.01205(11) 0.00156(8) 0.00028(7) -0.00078(8) F1 0.0298(10) 0.0258(8) 0.0256(9) -0.0110(7) 0.0076(7) -0.0033(7) O1 0.0173(9) 0.0168(9) 0.0158(9) 0.0018(7) 0.0030(7) -0.0009(7) N1 0.0115(11) 0.0108(10) 0.0144(10) -0.0032(8) 0.0009(8) 0.0005(8) C1 0.0171(13) 0.0160(12) 0.0121(12) 0.0017(10) -0.0015(10) 0.0003(11) B1 0.0213(17) 0.0216(15) 0.0156(16) -0.0032(12) 0.0068(12) 0.0007(13) F2 0.0298(9) 0.0269(8) 0.0242(9) 0.0017(7) 0.0042(7) 0.0070(7) O2 0.0163(9) 0.0194(9) 0.0154(9) -0.0019(7) -0.0014(7) 0.0004(7) C2 0.0179(14) 0.0225(14) 0.0099(12) 0.0016(11) 0.0013(10) -0.0049(11) F3 0.0284(10) 0.0319(9) 0.0229(9) 0.0089(7) 0.0060(7) 0.0027(7) O3 0.0116(10) 0.0211(10) 0.0122(9) 0.0002(7) 0.0017(7) 0.0010(7) C3 0.0124(13) 0.0213(13) 0.0175(14) -0.0012(11) 0.0009(11) -0.0002(11) F4 0.0343(10) 0.0371(10) 0.0254(9) -0.0051(7) 0.0085(7) -0.0182(8) O4 0.0123(9) 0.0224(10) 0.0156(9) -0.0016(7) 0.0031(7) -0.0032(7) C4 0.0110(13) 0.0235(14) 0.0186(14) 0.0005(11) -0.0001(10) -0.0046(11) O5 0.0150(9) 0.0163(9) 0.0180(9) 0.0018(7) 0.0001(7) 0.0001(7) C5 0.0174(15) 0.0225(15) 0.0180(15) -0.0035(11) 0.0020(12) 0.0003(11) C6 0.0145(14) 0.0256(14) 0.0151(15) -0.0022(11) 0.0051(11) -0.0017(11) C7 0.0151(14) 0.0250(14) 0.0119(13) 0.0020(11) -0.0019(10) 0.0017(11) C8 0.0186(15) 0.0196(14) 0.0138(14) -0.0021(10) -0.0039(11) 0.0010(11) C9 0.0117(14) 0.0219(13) 0.0193(14) 0.0000(11) 0.0003(11) -0.0004(11) C10 0.0137(13) 0.0210(14) 0.0188(14) 0.0028(11) 0.0021(11) 0.0033(11) C11 0.0152(14) 0.0152(14) 0.0185(15) 0.0020(10) 0.0062(11) -0.0004(10) C12 0.0173(14) 0.0157(12) 0.0128(13) -0.0002(10) 0.0045(11) 0.0008(11) C13 0.0152(13) 0.0111(11) 0.0182(13) 0.0008(10) -0.0005(10) -0.0005(10) C14 0.0178(14) 0.0094(11) 0.0213(15) -0.0011(10) 0.0036(11) -0.0031(10) C15 0.0318(18) 0.0083(13) 0.0257(17) -0.0008(11) 0.0087(13) 0.0029(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.3590(19) . ? Ag1 C15 2.515(2) 1_565 ? Ag1 C14 2.566(2) 1_565 ? Ag1 O3 2.5921(17) . ? Ag1 O4 2.6843(16) . ? Ag1 O5 2.7475(17) . ? Ag1 O1 2.7840(17) . ? Ag1 O2 3.1020(17) . ? F1 B1 1.399(3) . ? O1 C3 1.426(3) . ? O1 C2 1.430(3) . ? N1 C1 1.492(3) . ? N1 C13 1.495(3) . ? N1 C12 1.496(3) . ? C1 C2 1.516(3) . ? B1 F4 1.390(3) . ? B1 F3 1.392(3) . ? B1 F2 1.397(3) . ? O2 C5 1.428(3) . ? O2 C4 1.437(3) . ? O3 C6 1.432(3) . ? O3 C7 1.433(3) . ? C3 C4 1.508(3) . ? O4 C9 1.424(3) . ? O4 C8 1.425(3) . ? O5 C11 1.428(3) . ? O5 C10 1.441(3) . ? C5 C6 1.493(4) . ? C7 C8 1.495(4) . ? C9 C10 1.499(3) . ? C11 C12 1.506(4) . ? C13 C14 1.500(3) . ? C14 C15 1.330(4) . ? C14 Ag1 2.566(2) 1_545 ? C15 Ag1 2.515(2) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 C15 150.41(8) . 1_565 ? N1 Ag1 C14 121.91(7) . 1_565 ? C15 Ag1 C14 30.32(8) 1_565 1_565 ? N1 Ag1 O3 126.49(6) . . ? C15 Ag1 O3 83.09(7) 1_565 . ? C14 Ag1 O3 109.77(7) 1_565 . ? N1 Ag1 O4 114.08(6) . . ? C15 Ag1 O4 76.94(7) 1_565 . ? C14 Ag1 O4 101.46(7) 1_565 . ? O3 Ag1 O4 64.11(5) . . ? N1 Ag1 O5 71.25(6) . . ? C15 Ag1 O5 92.26(7) 1_565 . ? C14 Ag1 O5 87.68(7) 1_565 . ? O3 Ag1 O5 126.62(5) . . ? O4 Ag1 O5 63.07(5) . . ? N1 Ag1 O1 72.05(6) . . ? C15 Ag1 O1 96.17(7) 1_565 . ? C14 Ag1 O1 72.04(7) 1_565 . ? O3 Ag1 O1 115.38(5) . . ? O4 Ag1 O1 173.11(5) . . ? O5 Ag1 O1 117.98(5) . . ? N1 Ag1 O2 117.61(6) . . ? C15 Ag1 O2 73.80(7) 1_565 . ? C14 Ag1 O2 76.39(7) 1_565 . ? O3 Ag1 O2 60.48(5) . . ? O4 Ag1 O2 119.27(5) . . ? O5 Ag1 O2 164.07(5) . . ? O1 Ag1 O2 57.64(5) . . ? C3 O1 C2 114.31(18) . . ? C3 O1 Ag1 110.13(13) . . ? C2 O1 Ag1 99.92(13) . . ? C1 N1 C13 107.80(17) . . ? C1 N1 C12 106.94(18) . . ? C13 N1 C12 109.12(18) . . ? C1 N1 Ag1 113.29(14) . . ? C13 N1 Ag1 110.08(14) . . ? C12 N1 Ag1 109.49(13) . . ? N1 C1 C2 114.30(19) . . ? F4 B1 F3 109.5(2) . . ? F4 B1 F2 110.2(2) . . ? F3 B1 F2 109.2(2) . . ? F4 B1 F1 109.0(2) . . ? F3 B1 F1 110.3(2) . . ? F2 B1 F1 108.6(2) . . ? C5 O2 C4 113.08(18) . . ? C5 O2 Ag1 96.32(14) . . ? C4 O2 Ag1 110.84(13) . . ? O1 C2 C1 113.73(19) . . ? C6 O3 C7 110.30(18) . . ? C6 O3 Ag1 122.56(14) . . ? C7 O3 Ag1 114.93(14) . . ? O1 C3 C4 107.4(2) . . ? C9 O4 C8 112.57(18) . . ? C9 O4 Ag1 112.32(13) . . ? C8 O4 Ag1 112.19(14) . . ? O2 C4 C3 111.89(19) . . ? C11 O5 C10 112.76(18) . . ? C11 O5 Ag1 105.09(13) . . ? C10 O5 Ag1 113.64(13) . . ? O2 C5 C6 108.2(2) . . ? O3 C6 C5 110.1(2) . . ? O3 C7 C8 108.5(2) . . ? O4 C8 C7 108.6(2) . . ? O4 C9 C10 108.4(2) . . ? O5 C10 C9 111.83(19) . . ? O5 C11 C12 108.8(2) . . ? N1 C12 C11 115.4(2) . . ? N1 C13 C14 111.87(19) . . ? C15 C14 C13 123.1(2) . . ? C15 C14 Ag1 72.70(14) . 1_545 ? C13 C14 Ag1 106.20(15) . 1_545 ? C14 C15 Ag1 76.98(15) . 1_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 O1 C3 100.59(14) . . . . ? C15 Ag1 O1 C3 -107.23(15) 1_565 . . . ? C14 Ag1 O1 C3 -125.84(15) 1_565 . . . ? O3 Ag1 O1 C3 -21.97(15) . . . . ? O4 Ag1 O1 C3 -106.1(4) . . . . ? O5 Ag1 O1 C3 156.90(13) . . . . ? O2 Ag1 O1 C3 -40.85(13) . . . . ? N1 Ag1 O1 C2 -20.02(13) . . . . ? C15 Ag1 O1 C2 132.16(14) 1_565 . . . ? C14 Ag1 O1 C2 113.55(14) 1_565 . . . ? O3 Ag1 O1 C2 -142.58(13) . . . . ? O4 Ag1 O1 C2 133.3(4) . . . . ? O5 Ag1 O1 C2 36.29(14) . . . . ? O2 Ag1 O1 C2 -161.46(14) . . . . ? C15 Ag1 N1 C1 -78.6(2) 1_565 . . . ? C14 Ag1 N1 C1 -62.90(17) 1_565 . . . ? O3 Ag1 N1 C1 100.10(15) . . . . ? O4 Ag1 N1 C1 174.77(13) . . . . ? O5 Ag1 N1 C1 -137.73(15) . . . . ? O1 Ag1 N1 C1 -8.61(14) . . . . ? O2 Ag1 N1 C1 27.84(16) . . . . ? C15 Ag1 N1 C13 160.60(17) 1_565 . . . ? C14 Ag1 N1 C13 176.32(14) 1_565 . . . ? O3 Ag1 N1 C13 -20.68(17) . . . . ? O4 Ag1 N1 C13 53.99(15) . . . . ? O5 Ag1 N1 C13 101.50(15) . . . . ? O1 Ag1 N1 C13 -129.39(15) . . . . ? O2 Ag1 N1 C13 -92.94(15) . . . . ? C15 Ag1 N1 C12 40.6(2) 1_565 . . . ? C14 Ag1 N1 C12 56.36(17) 1_565 . . . ? O3 Ag1 N1 C12 -140.64(13) . . . . ? O4 Ag1 N1 C12 -65.97(15) . . . . ? O5 Ag1 N1 C12 -18.46(13) . . . . ? O1 Ag1 N1 C12 110.65(14) . . . . ? O2 Ag1 N1 C12 147.10(13) . . . . ? C13 N1 C1 C2 159.9(2) . . . . ? C12 N1 C1 C2 -82.9(2) . . . . ? Ag1 N1 C1 C2 37.8(2) . . . . ? N1 Ag1 O2 C5 84.00(14) . . . . ? C15 Ag1 O2 C5 -125.55(15) 1_565 . . . ? C14 Ag1 O2 C5 -156.84(14) 1_565 . . . ? O3 Ag1 O2 C5 -34.37(13) . . . . ? O4 Ag1 O2 C5 -61.17(14) . . . . ? O5 Ag1 O2 C5 -155.31(17) . . . . ? O1 Ag1 O2 C5 126.00(14) . . . . ? N1 Ag1 O2 C4 -33.66(15) . . . . ? C15 Ag1 O2 C4 116.79(15) 1_565 . . . ? C14 Ag1 O2 C4 85.50(15) 1_565 . . . ? O3 Ag1 O2 C4 -152.03(15) . . . . ? O4 Ag1 O2 C4 -178.83(13) . . . . ? O5 Ag1 O2 C4 87.0(2) . . . . ? O1 Ag1 O2 C4 8.34(13) . . . . ? C3 O1 C2 C1 -70.8(3) . . . . ? Ag1 O1 C2 C1 46.7(2) . . . . ? N1 C1 C2 O1 -63.1(3) . . . . ? N1 Ag1 O3 C6 -102.11(17) . . . . ? C15 Ag1 O3 C6 77.25(18) 1_565 . . . ? C14 Ag1 O3 C6 62.60(18) 1_565 . . . ? O4 Ag1 O3 C6 156.05(18) . . . . ? O5 Ag1 O3 C6 164.93(15) . . . . ? O1 Ag1 O3 C6 -16.32(18) . . . . ? O2 Ag1 O3 C6 1.99(15) . . . . ? N1 Ag1 O3 C7 119.23(15) . . . . ? C15 Ag1 O3 C7 -61.40(16) 1_565 . . . ? C14 Ag1 O3 C7 -76.05(16) 1_565 . . . ? O4 Ag1 O3 C7 17.40(14) . . . . ? O5 Ag1 O3 C7 26.27(16) . . . . ? O1 Ag1 O3 C7 -154.97(14) . . . . ? O2 Ag1 O3 C7 -136.67(16) . . . . ? C2 O1 C3 C4 -174.50(19) . . . . ? Ag1 O1 C3 C4 73.98(19) . . . . ? N1 Ag1 O4 C9 24.15(16) . . . . ? C15 Ag1 O4 C9 -126.78(16) 1_565 . . . ? C14 Ag1 O4 C9 -108.81(15) 1_565 . . . ? O3 Ag1 O4 C9 144.62(16) . . . . ? O5 Ag1 O4 C9 -27.39(14) . . . . ? O1 Ag1 O4 C9 -128.0(4) . . . . ? O2 Ag1 O4 C9 170.49(14) . . . . ? N1 Ag1 O4 C8 -103.85(15) . . . . ? C15 Ag1 O4 C8 105.22(15) 1_565 . . . ? C14 Ag1 O4 C8 123.20(15) 1_565 . . . ? O3 Ag1 O4 C8 16.63(13) . . . . ? O5 Ag1 O4 C8 -155.39(15) . . . . ? O1 Ag1 O4 C8 104.0(4) . . . . ? O2 Ag1 O4 C8 42.49(15) . . . . ? C5 O2 C4 C3 -84.0(3) . . . . ? Ag1 O2 C4 C3 22.9(2) . . . . ? O1 C3 C4 O2 -63.8(3) . . . . ? N1 Ag1 O5 C11 -11.95(14) . . . . ? C15 Ag1 O5 C11 -166.86(15) 1_565 . . . ? C14 Ag1 O5 C11 -136.87(15) 1_565 . . . ? O3 Ag1 O5 C11 110.07(14) . . . . ? O4 Ag1 O5 C11 119.02(15) . . . . ? O1 Ag1 O5 C11 -68.65(14) . . . . ? O2 Ag1 O5 C11 -138.37(17) . . . . ? N1 Ag1 O5 C10 -135.69(15) . . . . ? C15 Ag1 O5 C10 69.40(15) 1_565 . . . ? C14 Ag1 O5 C10 99.38(15) 1_565 . . . ? O3 Ag1 O5 C10 -13.67(16) . . . . ? O4 Ag1 O5 C10 -4.72(13) . . . . ? O1 Ag1 O5 C10 167.61(13) . . . . ? O2 Ag1 O5 C10 97.9(2) . . . . ? C4 O2 C5 C6 -179.49(19) . . . . ? Ag1 O2 C5 C6 64.64(19) . . . . ? C7 O3 C6 C5 171.29(19) . . . . ? Ag1 O3 C6 C5 31.0(3) . . . . ? O2 C5 C6 O3 -71.9(3) . . . . ? C6 O3 C7 C8 167.9(2) . . . . ? Ag1 O3 C7 C8 -48.5(2) . . . . ? C9 O4 C8 C7 -175.1(2) . . . . ? Ag1 O4 C8 C7 -47.2(2) . . . . ? O3 C7 C8 O4 64.0(2) . . . . ? C8 O4 C9 C10 -175.71(19) . . . . ? Ag1 O4 C9 C10 56.5(2) . . . . ? C11 O5 C10 C9 -84.5(2) . . . . ? Ag1 O5 C10 C9 34.9(2) . . . . ? O4 C9 C10 O5 -61.7(3) . . . . ? C10 O5 C11 C12 163.89(19) . . . . ? Ag1 O5 C11 C12 39.6(2) . . . . ? C1 N1 C12 C11 174.90(19) . . . . ? C13 N1 C12 C11 -68.8(2) . . . . ? Ag1 N1 C12 C11 51.8(2) . . . . ? O5 C11 C12 N1 -65.5(3) . . . . ? C1 N1 C13 C14 -74.4(2) . . . . ? C12 N1 C13 C14 169.9(2) . . . . ? Ag1 N1 C13 C14 49.7(2) . . . . ? N1 C13 C14 C15 -111.9(3) . . . . ? N1 C13 C14 Ag1 168.47(14) . . . 1_545 ? C13 C14 C15 Ag1 -98.4(2) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.571 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.156 #===END data_ac60p21 #(compound14) _database_code_CSD 180583 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H31 Ag F6 N O5 P' _chemical_formula_weight 570.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.589(2) _cell_length_b 8.5424(17) _cell_length_c 23.835(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.300(3) _cell_angle_gamma 90.00 _cell_volume 2156.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.088 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.8118 _exptl_absorpt_correction_T_max 0.8990 _exptl_absorpt_process_details 'Otwinowski & Minor, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method '2o phi & omega frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9526 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7220 _reflns_number_gt 6574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.8274P] 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 0.43(5) _refine_ls_number_reflns 7220 _refine_ls_number_parameters 732 _refine_ls_number_restraints 424 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.01098(5) 0.56896(7) 0.39156(2) 0.03163(17) Uani 1 1 d . . . P1 P 0.5098(2) 0.0323(3) 0.37818(12) 0.0318(6) Uani 1 1 d . . . F1 F 0.3603(5) 0.0290(8) 0.3776(3) 0.0560(19) Uani 1 1 d . . . O1 O 0.0315(12) 0.307(2) 0.3388(7) 0.025(3) Uani 0.480(10) 1 d PU A 1 N1 N -0.1773(14) 0.521(2) 0.3181(6) 0.020(4) Uani 0.480(10) 1 d PU A 1 C1 C -0.1406(16) 0.408(2) 0.2796(7) 0.028(4) Uani 0.480(10) 1 d PU A 1 H1A H -0.0806 0.4559 0.2530 0.033 Uiso 0.480(10) 1 calc PR A 1 H1B H -0.2159 0.3746 0.2579 0.033 Uiso 0.480(10) 1 calc PR A 1 Ag2 Ag 0.48880(5) 0.82267(6) 0.10898(2) 0.02911(16) Uani 1 1 d . . . P2 P 0.0062(2) 0.3593(3) 0.11966(12) 0.0339(7) Uani 1 1 d . . . F2 F 0.5085(6) 0.1799(8) 0.4191(3) 0.0513(17) Uani 1 1 d . . . O2 O 0.2247(13) 0.5361(18) 0.3426(6) 0.020(3) Uani 0.480(10) 1 d PU A 1 N2 N 0.2960(8) 0.8648(12) 0.1660(4) 0.057(3) Uani 1 1 d DU . . C2 C -0.076(2) 0.256(3) 0.3064(10) 0.027(5) Uani 0.480(10) 1 d PU A 1 H2A H -0.1367 0.2005 0.3308 0.033 Uiso 0.480(10) 1 calc PR A 1 H2B H -0.0488 0.1835 0.2764 0.033 Uiso 0.480(10) 1 calc PR A 1 F3 F 0.5135(7) -0.0837(10) 0.4297(3) 0.064(2) Uani 1 1 d . . . O3 O 0.1884(19) 0.633(2) 0.4507(9) 0.049(5) Uani 0.480(10) 1 d PU A 1 C3 C 0.1443(16) 0.299(3) 0.3057(9) 0.030(5) Uani 0.480(10) 1 d PU A 1 H3A H 0.1641 0.1881 0.2973 0.036 Uiso 0.480(10) 1 calc PR A 1 H3B H 0.1307 0.3543 0.2697 0.036 Uiso 0.480(10) 1 calc PR A 1 F4 F 0.5134(6) -0.1135(8) 0.3361(3) 0.0550(18) Uani 1 1 d . . . O4 O -0.0367(13) 0.5862(18) 0.5032(5) 0.051(4) Uani 0.480(10) 1 d PU A 1 C4 C 0.2451(13) 0.3671(16) 0.3347(6) 0.018(3) Uani 0.480(10) 1 d PU A 1 H4A H 0.3241 0.3504 0.3135 0.021 Uiso 0.480(10) 1 calc PR A 1 H4B H 0.2547 0.3160 0.3718 0.021 Uiso 0.480(10) 1 calc PR A 1 F5 F 0.5072(6) 0.1506(8) 0.3265(3) 0.0492(16) Uani 1 1 d . . . O5 O -0.2449(19) 0.482(2) 0.4355(8) 0.067(5) Uani 0.480(10) 1 d PU A 1 C5A C 0.3053(17) 0.451(2) 0.3591(8) 0.045(5) Uani 0.520(10) 1 d PU A 2 H5A1 H 0.3817 0.4423 0.3355 0.054 Uiso 0.520(10) 1 calc PR A 2 H5A2 H 0.2907 0.3491 0.3777 0.054 Uiso 0.520(10) 1 calc PR A 2 F6 F 0.6606(5) 0.0347(9) 0.3781(3) 0.060(2) Uani 1 1 d . . . O6 O 0.4849(9) 1.1077(10) 0.1581(4) 0.064(3) Uani 1 1 d DU . . C6 C 0.3172(17) 0.587(3) 0.4330(9) 0.036(5) Uani 0.480(10) 1 d PU A 1 H6A H 0.3337 0.4755 0.4410 0.043 Uiso 0.480(10) 1 calc PR A 1 H6B H 0.3818 0.6517 0.4524 0.043 Uiso 0.480(10) 1 calc PR A 1 F7 F -0.1455(5) 0.3625(8) 0.1203(3) 0.0536(19) Uani 1 1 d . . . O7 O 0.7039(7) 0.8998(10) 0.1714(3) 0.061(2) Uani 1 1 d DU . . C7 C 0.183(2) 0.619(3) 0.5109(9) 0.047(5) Uani 0.480(10) 1 d PU A 1 H7A H 0.2551 0.6757 0.5284 0.056 Uiso 0.480(10) 1 calc PR A 1 H7B H 0.1870 0.5082 0.5225 0.056 Uiso 0.480(10) 1 calc PR A 1 F8 F 0.0085(6) 0.5072(8) 0.1612(3) 0.060(2) Uani 1 1 d . . . O8 O 0.7140(6) 0.8207(14) 0.0579(3) 0.065(2) Uani 1 1 d DU . . C8 C 0.061(2) 0.691(3) 0.5282(9) 0.040(5) Uani 0.480(10) 1 d PU A 1 H8A H 0.0534 0.7987 0.5134 0.048 Uiso 0.480(10) 1 calc PR A 1 H8B H 0.0544 0.6938 0.5696 0.048 Uiso 0.480(10) 1 calc PR A 1 F9 F 0.0042(6) 0.2462(8) 0.1722(3) 0.0535(17) Uani 1 1 d . . . O9 O 0.5067(7) 0.6890(10) 0.0111(3) 0.053(2) Uani 1 1 d DU . . C9 C -0.164(2) 0.639(2) 0.5139(8) 0.033(4) Uani 0.480(10) 1 d PU A 1 H9A H -0.1765 0.6481 0.5549 0.040 Uiso 0.480(10) 1 calc PR A 1 H9B H -0.1756 0.7444 0.4973 0.040 Uiso 0.480(10) 1 calc PR A 1 F10 F 0.0039(6) 0.2115(8) 0.0787(3) 0.0504(18) Uani 1 1 d . . . O10 O 0.2839(6) 0.8334(12) 0.0428(4) 0.072(2) Uani 1 1 d DU . . C10 C -0.255(2) 0.538(3) 0.4918(11) 0.062(6) Uani 0.480(10) 1 d PU A 1 H10A H -0.3376 0.5922 0.4948 0.074 Uiso 0.480(10) 1 calc PR A 1 H10B H -0.2587 0.4458 0.5167 0.074 Uiso 0.480(10) 1 calc PR A 1 F11 F 0.0046(6) 0.4762(9) 0.0673(3) 0.057(2) Uani 1 1 d . . . C11 C -0.3273(15) 0.546(3) 0.3975(8) 0.026(4) Uani 0.480(10) 1 d PU A 1 H11A H -0.3168 0.6609 0.3966 0.031 Uiso 0.480(10) 1 calc PR A 1 H11B H -0.4152 0.5222 0.4087 0.031 Uiso 0.480(10) 1 calc PR A 1 F12 F 0.1576(5) 0.3570(8) 0.1185(3) 0.0540(19) Uani 1 1 d . . . C12 C -0.3032(18) 0.482(3) 0.3435(9) 0.049(6) Uani 0.480(10) 1 d PU A 1 H12A H -0.3702 0.5190 0.3175 0.059 Uiso 0.480(10) 1 calc PR A 1 H12B H -0.3104 0.3668 0.3459 0.059 Uiso 0.480(10) 1 calc PR A 1 C13 C -0.1965(13) 0.6585(17) 0.2876(5) 0.077(4) Uani 1 1 d U . . H13A H -0.2622 0.7222 0.3062 0.093 Uiso 1 1 calc R A 1 H13B H -0.2274 0.6318 0.2495 0.093 Uiso 1 1 calc R A 1 C14 C -0.062(2) 0.765(3) 0.2823(10) 0.053(6) Uani 0.50 1 d PU A 1 H14A H 0.0112 0.6964 0.2748 0.064 Uiso 0.50 1 calc PR A 1 H14B H -0.0692 0.8426 0.2515 0.064 Uiso 0.50 1 calc PR A 1 C15 C -0.045(3) 0.850(4) 0.3395(16) 0.081(10) Uani 0.50 1 d PU A 1 H15 H -0.1087 0.8972 0.3617 0.098 Uiso 0.50 1 calc PR A 1 C16 C 0.0605(17) 0.844(2) 0.3493(9) 0.034(4) Uani 0.50 1 d PU A 1 H16A H 0.1162 0.7942 0.3239 0.041 Uiso 0.50 1 calc PR A 1 H16B H 0.0927 0.8898 0.3828 0.041 Uiso 0.50 1 calc PR A 1 C17 C 0.2606(16) 1.0178(19) 0.1731(8) 0.111(6) Uani 1 1 d DU . . H17A H 0.1897 1.0249 0.1999 0.134 Uiso 1 1 calc R . . H17B H 0.2329 1.0634 0.1369 0.134 Uiso 1 1 calc R . . C18 C 0.3807(12) 1.1099(19) 0.1968(6) 0.084(5) Uani 1 1 d DU . . H18A H 0.3567 1.2199 0.2045 0.101 Uiso 1 1 calc R . . H18B H 0.4078 1.0619 0.2327 0.101 Uiso 1 1 calc R . . C19 C 0.5991(13) 1.1573(18) 0.1842(6) 0.080(4) Uani 1 1 d DU . . H19A H 0.6557 1.2018 0.1554 0.096 Uiso 1 1 calc R . . H19B H 0.5798 1.2410 0.2116 0.096 Uiso 1 1 calc R . . C20 C 0.6608(11) 1.0363(14) 0.2116(5) 0.061(3) Uani 1 1 d DU . . H20A H 0.6040 0.9926 0.2405 0.074 Uiso 1 1 calc R . . H20B H 0.7361 1.0791 0.2311 0.074 Uiso 1 1 calc R . . C21 C 0.8038(11) 0.9490(15) 0.1407(5) 0.071(4) Uani 1 1 d DU . . H21A H 0.8802 0.9600 0.1645 0.085 Uiso 1 1 calc R . . H21B H 0.7855 1.0506 0.1224 0.085 Uiso 1 1 calc R . . C22 C 0.8219(10) 0.815(2) 0.0953(6) 0.073(4) Uani 1 1 d DU . . H22A H 0.9008 0.8320 0.0742 0.088 Uiso 1 1 calc R . . H22B H 0.8268 0.7114 0.1139 0.088 Uiso 1 1 calc R . . C23 C 0.7277(11) 0.7014(16) 0.0170(5) 0.065(3) Uani 1 1 d DU . . H23A H 0.7326 0.5978 0.0355 0.078 Uiso 1 1 calc R . . H23B H 0.8064 0.7179 -0.0044 0.078 Uiso 1 1 calc R . . C24 C 0.6178(10) 0.7069(17) -0.0210(5) 0.062(3) Uani 1 1 d DU . . H24A H 0.6158 0.8082 -0.0412 0.075 Uiso 1 1 calc R . . H24B H 0.6236 0.6218 -0.0491 0.075 Uiso 1 1 calc R . . C25 C 0.3986(11) 0.694(2) -0.0239(5) 0.077(4) Uani 1 1 d DU . . H25A H 0.4001 0.6052 -0.0504 0.092 Uiso 1 1 calc R . . H25B H 0.3993 0.7924 -0.0461 0.092 Uiso 1 1 calc R . . C26 C 0.2843(11) 0.6878(16) 0.0093(5) 0.063(3) Uani 1 1 d DU . . H26A H 0.2851 0.5949 0.0341 0.076 Uiso 1 1 calc R . . H26B H 0.2088 0.6826 -0.0152 0.076 Uiso 1 1 calc R . . C27 C 0.1725(11) 0.855(2) 0.0744(7) 0.088(5) Uani 1 1 d DU . . H27A H 0.1511 0.9677 0.0745 0.106 Uiso 1 1 calc R . . H27B H 0.1024 0.7989 0.0554 0.106 Uiso 1 1 calc R . . C28 C 0.1801(13) 0.805(3) 0.1277(7) 0.099(5) Uani 1 1 d DU . . H28A H 0.1833 0.6888 0.1270 0.119 Uiso 1 1 calc R . . H28B H 0.1008 0.8344 0.1468 0.119 Uiso 1 1 calc R . . C29 C 0.2960(11) 0.7511(15) 0.2111(5) 0.069(3) Uani 1 1 d DU . . H29A H 0.3184 0.8091 0.2457 0.082 Uiso 1 1 calc R . . H29B H 0.2073 0.7167 0.2156 0.082 Uiso 1 1 calc R . . C30 C 0.3713(13) 0.6117(16) 0.2115(6) 0.086(4) Uani 1 1 d DU . . H30A H 0.3834 0.5817 0.2513 0.103 Uiso 1 1 calc R . . H30B H 0.3196 0.5282 0.1940 0.103 Uiso 1 1 calc R . . C31 C 0.4909(13) 0.606(2) 0.1861(7) 0.081(5) Uani 1 1 d DU . . H31 H 0.5468 0.6684 0.2078 0.097 Uiso 1 1 calc R . . C32 C 0.5513(14) 0.5504(19) 0.1469(6) 0.084(4) Uani 1 1 d DU . . H32A H 0.5109 0.4837 0.1205 0.100 Uiso 1 1 calc R . . H32B H 0.6384 0.5746 0.1430 0.100 Uiso 1 1 calc R . . O1A O -0.0214(18) 0.290(2) 0.3403(8) 0.047(5) Uani 0.520(10) 1 d PU A 2 N1A N -0.2044(18) 0.533(2) 0.3389(8) 0.045(5) Uani 0.520(10) 1 d PU A 2 C1A C -0.237(2) 0.363(2) 0.3301(9) 0.058(6) Uani 0.520(10) 1 d PU A 2 H1A1 H -0.2604 0.3140 0.3663 0.069 Uiso 0.520(10) 1 calc PR A 2 H1A2 H -0.3095 0.3530 0.3040 0.069 Uiso 0.520(10) 1 calc PR A 2 O2A O 0.1997(17) 0.493(2) 0.3257(7) 0.045(5) Uani 0.520(10) 1 d PU A 2 C2A C -0.124(3) 0.282(3) 0.3063(13) 0.058(8) Uani 0.520(10) 1 d PU A 2 H2A1 H -0.1449 0.1707 0.2994 0.070 Uiso 0.520(10) 1 calc PR A 2 H2A2 H -0.1029 0.3303 0.2697 0.070 Uiso 0.520(10) 1 calc PR A 2 O3A O 0.2148(17) 0.574(3) 0.4410(9) 0.060(5) Uani 0.520(10) 1 d PU A 2 C3A C 0.100(2) 0.238(3) 0.3141(10) 0.055(6) Uani 0.520(10) 1 d PU A 2 H3A1 H 0.0828 0.1569 0.2854 0.066 Uiso 0.520(10) 1 calc PR A 2 H3A2 H 0.1566 0.1936 0.3430 0.066 Uiso 0.520(10) 1 calc PR A 2 O4A O 0.0034(13) 0.707(2) 0.4907(7) 0.053(4) Uani 0.520(10) 1 d PU A 2 C4A C 0.1623(19) 0.384(2) 0.2863(7) 0.040(4) Uani 0.520(10) 1 d PU A 2 H4A1 H 0.2367 0.3500 0.2645 0.048 Uiso 0.520(10) 1 calc PR A 2 H4A2 H 0.1015 0.4332 0.2600 0.048 Uiso 0.520(10) 1 calc PR A 2 O5A O -0.2158(12) 0.576(2) 0.4521(8) 0.059(4) Uani 0.520(10) 1 d PU A 2 C6A C 0.3230(17) 0.581(3) 0.4034(10) 0.040(5) Uani 0.520(10) 1 d PU A 2 H6A1 H 0.4024 0.5649 0.4247 0.048 Uiso 0.520(10) 1 calc PR A 2 H6A2 H 0.3269 0.6852 0.3850 0.048 Uiso 0.520(10) 1 calc PR A 2 C7A C 0.218(2) 0.693(3) 0.4837(11) 0.061(6) Uani 0.520(10) 1 d PU A 2 H7A1 H 0.2972 0.6844 0.5055 0.073 Uiso 0.520(10) 1 calc PR A 2 H7A2 H 0.2148 0.7974 0.4660 0.073 Uiso 0.520(10) 1 calc PR A 2 C8A C 0.120(2) 0.676(4) 0.5177(11) 0.057(7) Uani 0.520(10) 1 d PU A 2 H8A1 H 0.1298 0.7477 0.5499 0.068 Uiso 0.520(10) 1 calc PR A 2 H8A2 H 0.1191 0.5673 0.5324 0.068 Uiso 0.520(10) 1 calc PR A 2 C9A C -0.099(2) 0.694(3) 0.5245(9) 0.051(6) Uani 0.520(10) 1 d PU A 2 H9A1 H -0.1012 0.7821 0.5513 0.062 Uiso 0.520(10) 1 calc PR A 2 H9A2 H -0.0948 0.5948 0.5460 0.062 Uiso 0.520(10) 1 calc PR A 2 C10A C -0.219(2) 0.696(3) 0.4863(12) 0.068(7) Uani 0.520(10) 1 d PU A 2 H10C H -0.2957 0.6900 0.5098 0.081 Uiso 0.520(10) 1 calc PR A 2 H10D H -0.2221 0.7945 0.4646 0.081 Uiso 0.520(10) 1 calc PR A 2 C11A C -0.324(3) 0.538(5) 0.4261(14) 0.088(10) Uani 0.520(10) 1 d PU A 2 H11C H -0.3966 0.5821 0.4468 0.106 Uiso 0.520(10) 1 calc PR A 2 H11D H -0.3332 0.4229 0.4247 0.106 Uiso 0.520(10) 1 calc PR A 2 C12A C -0.320(2) 0.604(3) 0.3676(10) 0.057(6) Uani 0.520(10) 1 d PU A 2 H12C H -0.3135 0.7194 0.3687 0.069 Uiso 0.520(10) 1 calc PR A 2 H12D H -0.3982 0.5755 0.3468 0.069 Uiso 0.520(10) 1 calc PR A 2 C14A C -0.129(2) 0.785(2) 0.2895(10) 0.048(5) Uani 0.50 1 d PU A 2 H14C H -0.1833 0.8669 0.3060 0.057 Uiso 0.50 1 calc PR A 2 H14D H -0.1145 0.8162 0.2500 0.057 Uiso 0.50 1 calc PR A 2 C15A C 0.0050(19) 0.800(3) 0.3204(10) 0.041(5) Uani 0.50 1 d PU A 2 H15A H 0.0837 0.7674 0.3055 0.049 Uiso 0.50 1 calc PR A 2 C16A C -0.014(4) 0.874(4) 0.3765(14) 0.096(10) Uani 0.50 1 d PU A 2 H16C H -0.0960 0.9029 0.3881 0.116 Uiso 0.50 1 calc PR A 2 H16D H 0.0567 0.8912 0.4005 0.116 Uiso 0.50 1 calc PR A 2 C5 C 0.3169(14) 0.618(2) 0.3713(9) 0.025(4) Uani 0.480(10) 1 d PU A 1 H5A H 0.3041 0.7316 0.3649 0.031 Uiso 0.480(10) 1 calc PR A 1 H5B H 0.4005 0.5897 0.3560 0.031 Uiso 0.480(10) 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0299(3) 0.0356(4) 0.0294(3) -0.0012(3) -0.0018(2) 0.0013(3) P1 0.0357(12) 0.0249(17) 0.0347(13) -0.0002(11) 0.0001(9) 0.0031(9) F1 0.032(3) 0.044(4) 0.092(5) -0.007(3) 0.001(3) -0.004(2) O1 0.019(6) 0.032(7) 0.023(6) 0.000(6) -0.005(5) -0.001(6) N1 0.018(5) 0.026(5) 0.016(5) -0.005(4) 0.006(4) 0.002(4) C1 0.026(7) 0.030(8) 0.027(7) -0.011(6) -0.008(6) 0.001(6) Ag2 0.0286(3) 0.0306(4) 0.0282(3) -0.0023(3) 0.0033(2) -0.0008(3) P2 0.0332(12) 0.0280(19) 0.0404(14) -0.0022(12) 0.0056(10) -0.0022(9) F2 0.063(4) 0.040(4) 0.051(4) -0.008(3) 0.003(3) 0.003(3) O2 0.016(5) 0.020(7) 0.025(6) 0.003(5) 0.005(4) -0.005(5) N2 0.055(5) 0.046(6) 0.072(6) 0.001(4) 0.032(4) 0.002(4) C2 0.032(8) 0.022(8) 0.028(8) -0.006(6) -0.001(7) -0.004(7) F3 0.080(5) 0.061(5) 0.051(5) 0.018(4) 0.003(3) 0.013(4) O3 0.046(8) 0.054(9) 0.047(8) -0.017(7) -0.006(6) -0.009(7) C3 0.027(7) 0.034(9) 0.030(8) -0.016(7) 0.011(6) -0.003(7) F4 0.077(4) 0.031(4) 0.057(4) -0.013(3) -0.002(3) 0.011(3) O4 0.065(7) 0.045(7) 0.043(6) -0.001(6) 0.018(6) 0.002(7) C4 0.017(4) 0.015(5) 0.022(5) 0.001(4) 0.003(4) 0.009(4) F5 0.061(4) 0.040(4) 0.046(4) 0.006(3) -0.002(3) 0.002(3) O5 0.066(8) 0.074(9) 0.062(8) 0.004(7) 0.018(7) 0.018(7) C5A 0.043(8) 0.042(8) 0.050(8) -0.009(7) 0.004(7) 0.016(7) F6 0.038(3) 0.052(5) 0.088(6) -0.005(4) 0.004(3) 0.004(3) O6 0.106(6) 0.043(5) 0.044(4) 0.000(4) -0.004(4) -0.015(4) C6 0.027(7) 0.045(9) 0.035(8) -0.009(8) 0.003(7) -0.008(7) F7 0.029(3) 0.045(5) 0.087(5) 0.002(3) 0.007(3) -0.005(2) O7 0.048(4) 0.078(5) 0.056(5) 0.019(4) -0.010(3) -0.027(3) C7 0.061(9) 0.042(9) 0.037(8) 0.006(7) -0.005(8) -0.005(8) F8 0.075(4) 0.032(4) 0.073(5) -0.017(3) 0.013(3) -0.012(3) O8 0.041(3) 0.081(5) 0.074(5) -0.006(5) 0.014(3) 0.008(4) C8 0.057(10) 0.041(9) 0.022(8) -0.003(7) -0.006(8) 0.012(8) F9 0.084(4) 0.035(4) 0.042(4) 0.006(3) 0.007(3) -0.003(3) O9 0.060(4) 0.062(5) 0.038(4) -0.007(4) -0.001(3) -0.007(3) C9 0.044(8) 0.037(8) 0.018(7) 0.006(6) 0.019(7) 0.001(7) F10 0.063(4) 0.048(4) 0.041(4) -0.021(3) -0.006(3) -0.003(3) O10 0.041(3) 0.061(5) 0.114(6) -0.003(5) 0.003(4) -0.004(4) C10 0.059(9) 0.065(10) 0.061(10) -0.007(8) 0.002(8) 0.011(8) F11 0.066(4) 0.045(4) 0.059(5) 0.019(4) 0.005(3) -0.003(3) C11 0.013(6) 0.038(9) 0.026(7) 0.009(7) 0.009(6) -0.001(6) F12 0.032(3) 0.046(5) 0.083(5) 0.003(3) 0.002(3) 0.002(3) C12 0.030(8) 0.058(10) 0.060(9) 0.005(8) 0.014(7) 0.001(7) C13 0.079(7) 0.096(8) 0.057(6) 0.021(6) -0.015(6) 0.002(6) C14 0.057(9) 0.054(9) 0.047(9) 0.013(7) 0.013(8) 0.011(8) C15 0.094(12) 0.072(13) 0.078(12) -0.001(9) -0.010(9) -0.001(9) C16 0.040(7) 0.019(7) 0.045(8) 0.003(6) -0.004(7) 0.002(6) C17 0.118(9) 0.105(10) 0.112(9) 0.006(8) 0.029(8) 0.028(8) C18 0.082(7) 0.088(9) 0.083(8) -0.044(7) -0.014(6) 0.033(6) C19 0.090(8) 0.074(8) 0.075(8) -0.012(6) 0.017(6) -0.014(6) C20 0.068(6) 0.052(6) 0.064(6) -0.026(5) -0.004(5) -0.006(5) C21 0.066(6) 0.078(7) 0.067(7) 0.028(6) -0.033(5) -0.037(5) C22 0.030(5) 0.076(8) 0.114(8) -0.008(7) -0.004(5) 0.015(6) C23 0.060(6) 0.075(7) 0.059(6) -0.004(5) 0.027(5) 0.012(5) C24 0.067(6) 0.065(7) 0.055(6) -0.007(5) 0.019(5) 0.010(5) C25 0.074(7) 0.095(8) 0.062(7) -0.009(6) -0.014(6) -0.028(6) C26 0.070(6) 0.063(7) 0.057(6) -0.012(5) -0.013(5) -0.022(5) C27 0.056(6) 0.092(9) 0.118(9) -0.008(7) -0.005(6) -0.006(6) C28 0.059(7) 0.128(10) 0.111(9) -0.002(9) 0.000(7) -0.008(7) C29 0.065(6) 0.081(7) 0.059(6) 0.016(5) 0.010(5) -0.001(5) C30 0.106(8) 0.075(7) 0.077(7) 0.028(6) 0.021(6) -0.001(6) C31 0.090(7) 0.068(8) 0.085(8) 0.035(6) 0.012(6) 0.015(6) C32 0.101(8) 0.058(7) 0.091(8) 0.028(7) 0.004(7) 0.010(7) O1A 0.062(9) 0.040(8) 0.040(7) -0.020(6) -0.001(8) -0.004(7) N1A 0.051(8) 0.040(8) 0.045(8) 0.004(7) -0.016(7) 0.001(7) C1A 0.075(9) 0.043(9) 0.055(9) -0.004(7) -0.008(7) -0.024(7) O2A 0.047(8) 0.045(8) 0.042(8) 0.004(6) -0.007(6) 0.003(6) C2A 0.067(12) 0.047(11) 0.062(11) 0.003(8) -0.002(9) -0.009(9) O3A 0.045(8) 0.072(10) 0.063(9) 0.009(8) -0.009(6) -0.011(8) C3A 0.062(10) 0.054(10) 0.048(9) -0.010(8) 0.008(8) -0.001(8) O4A 0.039(6) 0.063(8) 0.056(8) -0.014(7) -0.006(6) -0.006(6) C4A 0.060(8) 0.031(7) 0.030(7) -0.004(6) 0.021(6) -0.005(7) O5A 0.042(6) 0.054(8) 0.082(8) -0.029(7) 0.008(6) 0.004(6) C6A 0.028(7) 0.054(9) 0.038(8) 0.011(8) -0.006(7) -0.016(7) C7A 0.059(9) 0.065(10) 0.058(10) -0.001(9) -0.007(8) -0.013(8) C8A 0.050(10) 0.074(11) 0.047(10) 0.013(8) -0.012(8) 0.004(9) C9A 0.062(9) 0.055(9) 0.037(9) -0.003(7) 0.009(7) 0.013(8) C10A 0.056(9) 0.072(11) 0.075(11) -0.011(9) 0.001(8) 0.019(8) C11A 0.076(12) 0.102(14) 0.086(13) -0.001(10) -0.008(9) 0.004(9) C12A 0.048(9) 0.068(10) 0.055(9) -0.002(8) -0.007(8) 0.003(8) C14A 0.048(8) 0.039(9) 0.056(9) 0.020(7) -0.010(8) -0.004(7) C15A 0.036(7) 0.036(9) 0.049(9) 0.036(7) 0.013(7) 0.003(7) C16A 0.114(13) 0.084(13) 0.092(13) -0.002(9) -0.013(10) 0.009(9) C5 0.004(6) 0.030(8) 0.042(8) -0.003(6) 0.010(6) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1A 2.416(18) . ? Ag1 N1 2.510(16) . ? Ag1 O3 2.59(2) . ? Ag1 O1 2.607(19) . ? Ag1 O5A 2.611(14) . ? Ag1 C15A 2.608(19) . ? Ag1 C16A 2.63(3) . ? Ag1 O4A 2.643(16) . ? Ag1 O3A 2.660(19) . ? Ag1 C16 2.671(16) . ? Ag1 O1A 2.683(19) . ? Ag1 O4 2.681(13) . ? P1 F3 1.578(8) . ? P1 F1 1.583(6) . ? P1 F2 1.594(7) . ? P1 F5 1.594(7) . ? P1 F6 1.597(6) . ? P1 F4 1.600(7) . ? O1 C2 1.44(3) . ? O1 C3 1.44(2) . ? N1 C1 1.39(2) . ? N1 C13 1.40(2) . ? N1 C12 1.50(2) . ? C1 C2 1.60(3) . ? Ag2 N2 2.485(8) . ? Ag2 C32 2.580(14) . ? Ag2 O9 2.606(7) . ? Ag2 C31 2.612(14) . ? Ag2 O10 2.677(8) . ? Ag2 O8 2.683(6) . ? Ag2 O6 2.701(9) . ? Ag2 O7 2.793(7) . ? P2 F9 1.582(7) . ? P2 F10 1.596(7) . ? P2 F11 1.598(7) . ? P2 F12 1.604(6) . ? P2 F8 1.605(7) . ? P2 F7 1.606(5) . ? O2 C5 1.38(2) . ? O2 C4 1.47(2) . ? N2 C17 1.370(16) . ? N2 C29 1.450(13) . ? N2 C28 1.609(16) . ? O3 C7 1.44(3) . ? O3 C6 1.48(2) . ? C3 C4 1.40(2) . ? O4 C9 1.45(2) . ? O4 C8 1.49(3) . ? O5 C11 1.37(3) . ? O5 C10 1.43(3) . ? C5A O2A 1.41(3) . ? C5A C6A 1.55(3) . ? O6 C19 1.422(15) . ? O6 C18 1.443(14) . ? C6 C5 1.49(3) . ? O7 C21 1.357(12) . ? O7 C20 1.578(13) . ? C7 C8 1.49(3) . ? O8 C23 1.418(14) . ? O8 C22 1.447(13) . ? O9 C25 1.413(13) . ? O9 C24 1.415(12) . ? C9 C10 1.39(3) . ? O10 C27 1.414(13) . ? O10 C26 1.478(14) . ? C11 C12 1.42(3) . ? C13 C14A 1.30(2) . ? C13 N1A 1.63(2) . ? C13 C14 1.70(3) . ? C14 C15 1.55(4) . ? C15 C16 1.14(4) . ? C17 C18 1.596(19) . ? C19 C20 1.384(17) . ? C21 C22 1.586(18) . ? C23 C24 1.472(16) . ? C25 C26 1.451(15) . ? C27 C28 1.34(2) . ? C29 C30 1.433(15) . ? C30 C31 1.407(14) . ? C31 C32 1.229(17) . ? O1A C2A 1.35(3) . ? O1A C3A 1.49(3) . ? N1A C1A 1.51(3) . ? N1A C12A 1.53(3) . ? C1A C2A 1.50(3) . ? O2A C4A 1.38(2) . ? O3A C7A 1.44(3) . ? O3A C6A 1.46(3) . ? C3A C4A 1.56(3) . ? O4A C9A 1.36(3) . ? O4A C8A 1.41(3) . ? O5A C10A 1.31(3) . ? O5A C11A 1.34(3) . ? C7A C8A 1.33(3) . ? C9A C10A 1.56(3) . ? C11A C12A 1.50(4) . ? C14A C15A 1.60(3) . ? C15A C16A 1.49(4) . ? 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 N1A Ag1 N1 13.4(5) . . ? N1A Ag1 O3 174.7(7) . . ? N1 Ag1 O3 168.7(5) . . ? N1A Ag1 O1 77.8(6) . . ? N1 Ag1 O1 69.3(5) . . ? O3 Ag1 O1 107.5(5) . . ? N1A Ag1 O5A 65.5(6) . . ? N1 Ag1 O5A 78.9(5) . . ? O3 Ag1 O5A 111.8(6) . . ? O1 Ag1 O5A 115.7(5) . . ? N1A Ag1 C15A 79.4(7) . . ? N1 Ag1 C15A 73.6(7) . . ? O3 Ag1 C15A 98.0(7) . . ? O1 Ag1 C15A 108.9(7) . . ? O5A Ag1 C15A 113.4(7) . . ? N1A Ag1 C16A 92.6(10) . . ? N1 Ag1 C16A 93.4(9) . . ? O3 Ag1 C16A 82.8(10) . . ? O1 Ag1 C16A 141.8(8) . . ? O5A Ag1 C16A 92.5(9) . . ? C15A Ag1 C16A 33.1(9) . . ? N1A Ag1 O4A 124.4(6) . . ? N1 Ag1 O4A 137.1(4) . . ? O3 Ag1 O4A 51.5(5) . . ? O1 Ag1 O4A 143.5(5) . . ? O5A Ag1 O4A 62.6(5) . . ? C15A Ag1 O4A 103.9(7) . . ? C16A Ag1 O4A 71.5(8) . . ? N1A Ag1 O3A 171.7(7) . . ? N1 Ag1 O3A 159.5(6) . . ? O3 Ag1 O3A 13.5(6) . . ? O1 Ag1 O3A 94.0(6) . . ? O5A Ag1 O3A 120.2(6) . . ? C15A Ag1 O3A 102.4(7) . . ? C16A Ag1 O3A 93.1(10) . . ? O4A Ag1 O3A 63.2(6) . . ? N1A Ag1 C16 99.0(6) . . ? N1 Ag1 C16 94.6(6) . . ? O3 Ag1 C16 77.8(6) . . ? O1 Ag1 C16 121.6(5) . . ? O5A Ag1 C16 115.1(6) . . ? C15A Ag1 C16 21.3(7) . . ? C16A Ag1 C16 22.9(8) . . ? O4A Ag1 C16 86.0(6) . . ? O3A Ag1 C16 84.1(6) . . ? N1A Ag1 O1A 67.6(6) . . ? N1 Ag1 O1A 60.7(6) . . ? O3 Ag1 O1A 117.8(6) . . ? O1 Ag1 O1A 12.5(4) . . ? O5A Ag1 O1A 103.9(6) . . ? C15A Ag1 O1A 112.3(8) . . ? C16A Ag1 O1A 144.9(9) . . ? O4A Ag1 O1A 143.6(6) . . ? O3A Ag1 O1A 104.5(7) . . ? C16 Ag1 O1A 128.5(6) . . ? N1A Ag1 O4 115.6(6) . . ? N1 Ag1 O4 128.8(4) . . ? O3 Ag1 O4 62.3(5) . . ? O1 Ag1 O4 123.0(5) . . ? O5A Ag1 O4 50.3(5) . . ? C15A Ag1 O4 127.7(7) . . ? C16A Ag1 O4 94.6(8) . . ? O4A Ag1 O4 25.0(4) . . ? O3A Ag1 O4 69.8(5) . . ? C16 Ag1 O4 110.9(6) . . ? O1A Ag1 O4 119.8(5) . . ? F3 P1 F1 90.9(4) . . ? F3 P1 F2 91.2(4) . . ? F1 P1 F2 90.4(4) . . ? F3 P1 F5 179.4(5) . . ? F1 P1 F5 89.5(4) . . ? F2 P1 F5 88.4(4) . . ? F3 P1 F6 89.3(4) . . ? F1 P1 F6 179.4(5) . . ? F2 P1 F6 90.1(4) . . ? F5 P1 F6 90.3(4) . . ? F3 P1 F4 89.9(4) . . ? F1 P1 F4 90.4(4) . . ? F2 P1 F4 178.6(4) . . ? F5 P1 F4 90.5(4) . . ? F6 P1 F4 89.0(4) . . ? C2 O1 C3 110.3(16) . . ? C2 O1 Ag1 112.4(12) . . ? C3 O1 Ag1 116.9(13) . . ? C1 N1 C13 106.4(14) . . ? C1 N1 C12 111.3(16) . . ? C13 N1 C12 105.5(15) . . ? C1 N1 Ag1 112.1(11) . . ? C13 N1 Ag1 109.0(10) . . ? C12 N1 Ag1 112.1(12) . . ? N1 C1 C2 115.0(16) . . ? N2 Ag2 C32 98.6(4) . . ? N2 Ag2 O9 128.1(3) . . ? C32 Ag2 O9 84.2(4) . . ? N2 Ag2 C31 73.9(4) . . ? C32 Ag2 C31 27.4(4) . . ? O9 Ag2 C31 108.6(4) . . ? N2 Ag2 O10 69.6(3) . . ? C32 Ag2 O10 116.3(5) . . ? O9 Ag2 O10 63.3(3) . . ? C31 Ag2 O10 116.3(4) . . ? N2 Ag2 O8 169.7(3) . . ? C32 Ag2 O8 85.8(4) . . ? O9 Ag2 O8 61.4(3) . . ? C31 Ag2 O8 108.1(4) . . ? O10 Ag2 O8 116.9(2) . . ? N2 Ag2 O6 67.6(3) . . ? C32 Ag2 O6 131.7(4) . . ? O9 Ag2 O6 141.6(3) . . ? C31 Ag2 O6 109.6(5) . . ? O10 Ag2 O6 102.1(3) . . ? O8 Ag2 O6 102.6(3) . . ? N2 Ag2 O7 110.2(3) . . ? C32 Ag2 O7 79.6(4) . . ? O9 Ag2 O7 121.2(2) . . ? C31 Ag2 O7 77.8(4) . . ? O10 Ag2 O7 164.1(3) . . ? O8 Ag2 O7 61.3(2) . . ? O6 Ag2 O7 64.6(3) . . ? F9 P2 F10 90.1(4) . . ? F9 P2 F11 178.3(4) . . ? F10 P2 F11 90.9(4) . . ? F9 P2 F12 91.3(4) . . ? F10 P2 F12 89.5(4) . . ? F11 P2 F12 90.0(4) . . ? F9 P2 F8 89.6(4) . . ? F10 P2 F8 179.7(5) . . ? F11 P2 F8 89.4(5) . . ? F12 P2 F8 90.4(4) . . ? F9 P2 F7 89.2(4) . . ? F10 P2 F7 90.5(4) . . ? F11 P2 F7 89.5(4) . . ? F12 P2 F7 179.5(5) . . ? F8 P2 F7 89.6(4) . . ? C5 O2 C4 117.2(14) . . ? C5 O2 Ag1 112.1(11) . . ? C4 O2 Ag1 106.6(8) . . ? C17 N2 C29 123.1(12) . . ? C17 N2 C28 99.6(14) . . ? C29 N2 C28 101.7(11) . . ? C17 N2 Ag2 115.6(8) . . ? C29 N2 Ag2 108.2(7) . . ? C28 N2 Ag2 105.6(8) . . ? O1 C2 C1 107.7(17) . . ? C7 O3 C6 107.6(19) . . ? C7 O3 Ag1 119.4(15) . . ? C6 O3 Ag1 122.6(13) . . ? C4 C3 O1 110.1(15) . . ? C9 O4 C8 113.0(15) . . ? C9 O4 Ag1 106.9(11) . . ? C8 O4 Ag1 110.8(11) . . ? C3 C4 O2 111.1(15) . . ? C11 O5 C10 115.8(18) . . ? C11 O5 Ag1 102.2(12) . . ? C10 O5 Ag1 109.5(16) . . ? O2A C5A C6A 107.2(16) . . ? C19 O6 C18 111.5(10) . . ? C19 O6 Ag2 116.3(8) . . ? C18 O6 Ag2 107.6(7) . . ? O3 C6 C5 103.8(17) . . ? C21 O7 C20 109.2(9) . . ? C21 O7 Ag2 114.9(7) . . ? C20 O7 Ag2 105.1(6) . . ? O3 C7 C8 106.3(19) . . ? C23 O8 C22 108.4(10) . . ? C23 O8 Ag2 114.3(7) . . ? C22 O8 Ag2 114.9(7) . . ? C7 C8 O4 104.3(17) . . ? C25 O9 C24 110.5(9) . . ? C25 O9 Ag2 116.8(7) . . ? C24 O9 Ag2 120.1(7) . . ? C10 C9 O4 112.7(17) . . ? C27 O10 C26 113.7(10) . . ? C27 O10 Ag2 111.5(8) . . ? C26 O10 Ag2 106.5(7) . . ? C9 C10 O5 120(2) . . ? O5 C11 C12 109.3(18) . . ? C11 C12 N1 116.3(19) . . ? C14A C13 N1 127.1(15) . . ? C14A C13 N1A 123.5(15) . . ? N1 C13 N1A 20.5(8) . . ? C14A C13 C14 24.6(12) . . ? N1 C13 C14 111.8(13) . . ? N1A C13 C14 117.1(13) . . ? C15 C14 C13 106.2(18) . . ? C16 C15 C14 106(4) . . ? C16 C15 Ag1 75(2) . . ? C14 C15 Ag1 90.1(19) . . ? C15 C16 Ag1 81(2) . . ? N2 C17 C18 107.2(13) . . ? O6 C18 C17 112.2(11) . . ? C20 C19 O6 112.5(12) . . ? C19 C20 O7 113.7(11) . . ? O7 C21 C22 104.0(9) . . ? O8 C22 C21 107.3(10) . . ? O8 C23 C24 108.5(9) . . ? O9 C24 C23 108.7(10) . . ? O9 C25 C26 110.6(11) . . ? C25 C26 O10 105.5(10) . . ? C28 C27 O10 114.5(13) . . ? C27 C28 N2 118.5(15) . . ? C30 C29 N2 124.0(10) . . ? C31 C30 C29 122.1(12) . . ? C32 C31 C30 144(2) . . ? C32 C31 Ag2 74.9(9) . . ? C30 C31 Ag2 105.7(9) . . ? C31 C32 Ag2 77.8(10) . . ? C2A O1A C3A 115(2) . . ? C2A O1A Ag1 110.3(16) . . ? C3A O1A Ag1 114.7(14) . . ? C1A N1A C12A 105.0(18) . . ? C1A N1A C13 122.9(16) . . ? C12A N1A C13 96.9(16) . . ? C1A N1A Ag1 112.7(13) . . ? C12A N1A Ag1 113.4(14) . . ? C13 N1A Ag1 105.1(11) . . ? C2A C1A N1A 108.3(19) . . ? C4A O2A C5A 116.0(17) . . ? C4A O2A Ag1 108.1(12) . . ? C5A O2A Ag1 111.9(12) . . ? O1A C2A C1A 113(2) . . ? C7A O3A C6A 112.9(19) . . ? C7A O3A Ag1 109.9(15) . . ? C6A O3A Ag1 115.8(14) . . ? O1A C3A C4A 108.2(19) . . ? C9A O4A C8A 114.4(19) . . ? C9A O4A Ag1 116.9(14) . . ? C8A O4A Ag1 111.7(16) . . ? O2A C4A C3A 111.7(17) . . ? C10A O5A C11A 117(2) . . ? C10A O5A Ag1 112.9(15) . . ? C11A O5A Ag1 116.7(18) . . ? O3A C6A C5A 107.2(17) . . ? C8A C7A O3A 110(2) . . ? C7A C8A O4A 113(2) . . ? O4A C9A C10A 107.7(18) . . ? O5A C10A C9A 109(2) . . ? O5A C11A C12A 108(3) . . ? C11A C12A N1A 107(2) . . ? C13 C14A C15A 124.8(18) . . ? C16A C15A C14A 109(2) . . ? C16A C15A Ag1 74.2(15) . . ? C14A C15A Ag1 100.3(11) . . ? C15A C16A Ag1 72.8(15) . . ? O2 C5 C6 113.3(16) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.915 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.135 #===END data_ac49m #(compound15) _database_code_CSD 180584 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common N-allyl-aza-18-crown-6 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H64 Cu4 I6 N2 O12' _chemical_formula_weight 1660.39 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.829(3) _cell_length_b 19.689(4) _cell_length_c 8.5073(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.09(3) _cell_angle_gamma 90.00 _cell_volume 2464.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 5.511 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.1692 _exptl_absorpt_correction_T_max 0.8978 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15252 _diffrn_reflns_av_R_equivalents 0.1220 _diffrn_reflns_av_sigmaI/netI 0.1076 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5618 _reflns_number_gt 4476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+13.5862P] 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 SHELXL _refine_ls_extinction_coef 0.0015(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5618 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 I1 I 0.25611(3) 0.73746(2) 0.64350(5) 0.01711(15) Uani 1 1 d . . . I2 I 0.50200(3) 0.80848(3) 0.97306(6) 0.02052(16) Uani 1 1 d . . . I3 I 0.41541(4) 0.60264(2) 0.99038(6) 0.02055(16) Uani 1 1 d . . . Cu1 Cu 0.35841(8) 0.72494(5) 0.90696(12) 0.0267(3) Uani 1 1 d . . . Cu2 Cu 0.43245(10) 0.79327(7) 0.68520(13) 0.0427(3) Uani 1 1 d . . . O1 O 0.9181(4) 0.4399(3) 0.7255(7) 0.0210(11) Uani 1 1 d . . . O2 O 1.0589(4) 0.5338(3) 0.7816(7) 0.0255(12) Uani 1 1 d . . . O3 O 0.9993(4) 0.6606(3) 0.9135(7) 0.0247(12) Uani 1 1 d . . . O4 O 0.8244(4) 0.7196(3) 0.7948(6) 0.0261(13) Uani 1 1 d . . . O5 O 0.6919(4) 0.6130(3) 0.7443(7) 0.0237(12) Uani 1 1 d . . . O6 O 0.8740(4) 0.5834(3) 0.6537(7) 0.0286(13) Uani 1 1 d . . . N1 N 0.7358(5) 0.4879(3) 0.5898(7) 0.0189(13) Uani 1 1 d . . . C1 C 0.7610(6) 0.4173(4) 0.6547(10) 0.0222(17) Uani 1 1 d . . . H1A H 0.7538 0.4162 0.7688 0.027 Uiso 1 1 calc R . . H1B H 0.7181 0.3838 0.6003 0.027 Uiso 1 1 calc R . . C2 C 0.8562(6) 0.3962(4) 0.6346(10) 0.0209(16) Uani 1 1 d . . . H2A H 0.8666 0.3487 0.6703 0.025 Uiso 1 1 calc R . . H2B H 0.8654 0.3990 0.5215 0.025 Uiso 1 1 calc R . . C3 C 1.0094(6) 0.4207(4) 0.7165(11) 0.0277(18) Uani 1 1 d . . . H3A H 1.0243 0.4269 0.6071 0.033 Uiso 1 1 calc R . . H3B H 1.0185 0.3723 0.7458 0.033 Uiso 1 1 calc R . . C4 C 1.0703(6) 0.4652(5) 0.8301(10) 0.0267(18) Uani 1 1 d . . . H4A H 1.0542 0.4598 0.9389 0.032 Uiso 1 1 calc R . . H4B H 1.1346 0.4515 0.8302 0.032 Uiso 1 1 calc R . . C5 C 1.1144(6) 0.5790(5) 0.8851(9) 0.0277(19) Uani 1 1 d . . . H5A H 1.1788 0.5743 0.8669 0.033 Uiso 1 1 calc R . . H5B H 1.1097 0.5670 0.9968 0.033 Uiso 1 1 calc R . . C6 C 1.0846(6) 0.6496(5) 0.8552(10) 0.0280(19) Uani 1 1 d . . . H6A H 1.1306 0.6811 0.9085 0.034 Uiso 1 1 calc R . . H6B H 1.0783 0.6590 0.7401 0.034 Uiso 1 1 calc R . . C7 C 0.9777(7) 0.7300(4) 0.9112(11) 0.0296(19) Uani 1 1 d . . . H7A H 0.9883 0.7499 0.8083 0.036 Uiso 1 1 calc R . . H7B H 1.0173 0.7538 0.9960 0.036 Uiso 1 1 calc R . . C8 C 0.8802(7) 0.7389(4) 0.9359(10) 0.032(2) Uani 1 1 d . . . H8A H 0.8661 0.7104 1.0255 0.038 Uiso 1 1 calc R . . H8B H 0.8686 0.7870 0.9613 0.038 Uiso 1 1 calc R . . C9 C 0.7292(6) 0.7275(4) 0.8049(11) 0.0275(18) Uani 1 1 d . . . H9A H 0.6978 0.7397 0.6991 0.033 Uiso 1 1 calc R . . H9B H 0.7203 0.7652 0.8783 0.033 Uiso 1 1 calc R . . C10 C 0.6870(7) 0.6641(4) 0.8619(11) 0.030(2) Uani 1 1 d . . . H10A H 0.7203 0.6493 0.9642 0.036 Uiso 1 1 calc R . . H10B H 0.6229 0.6727 0.8773 0.036 Uiso 1 1 calc R . . C11 C 0.6527(6) 0.5493(4) 0.7837(10) 0.0264(18) Uani 1 1 d . . . H11A H 0.5924 0.5567 0.8193 0.032 Uiso 1 1 calc R . . H11B H 0.6925 0.5264 0.8697 0.032 Uiso 1 1 calc R . . C12 C 0.6439(5) 0.5070(4) 0.6360(10) 0.0211(16) Uani 1 1 d . . . H12A H 0.6093 0.5327 0.5484 0.025 Uiso 1 1 calc R . . H12B H 0.6094 0.4652 0.6533 0.025 Uiso 1 1 calc R . . C13 C 0.7365(6) 0.4913(4) 0.4125(9) 0.0257(18) Uani 1 1 d . . . H13A H 0.7967 0.4766 0.3863 0.031 Uiso 1 1 calc R . . H13B H 0.6903 0.4596 0.3604 0.031 Uiso 1 1 calc R . . C14 C 0.7171(6) 0.5613(4) 0.3493(10) 0.0259(18) Uani 1 1 d . . . H14 H 0.7555 0.5970 0.3922 0.031 Uiso 1 1 calc R . . C15 C 0.6502(6) 0.5767(5) 0.2379(10) 0.0278(18) Uani 1 1 d . . . H15A H 0.6105 0.5421 0.1925 0.033 Uiso 1 1 calc R . . H15B H 0.6417 0.6224 0.2032 0.033 Uiso 1 1 calc R . . H16 H 0.9217 0.5744 0.7163 0.033 Uiso 1 1 d R . . H17 H 0.8600 0.6221 0.6939 0.033 Uiso 1 1 d R . . H1 H 0.795(7) 0.516(5) 0.632(12) 0.033 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0190(3) 0.0238(3) 0.0080(2) 0.00004(17) -0.00091(17) -0.00325(19) I2 0.0221(3) 0.0241(3) 0.0140(3) -0.00105(18) -0.00323(19) -0.0050(2) I3 0.0275(3) 0.0164(3) 0.0175(3) 0.00000(18) 0.0017(2) 0.00127(19) Cu1 0.0375(6) 0.0259(5) 0.0140(5) 0.0037(4) -0.0070(4) 0.0014(4) Cu2 0.0612(9) 0.0419(7) 0.0189(6) 0.0096(5) -0.0194(5) -0.0206(6) O1 0.017(3) 0.025(3) 0.020(3) -0.002(2) -0.001(2) -0.001(2) O2 0.024(3) 0.030(3) 0.020(3) 0.001(2) -0.006(2) -0.006(2) O3 0.031(3) 0.026(3) 0.018(3) 0.000(2) 0.005(2) -0.006(2) O4 0.038(4) 0.026(3) 0.013(3) -0.001(2) 0.000(2) -0.004(3) O5 0.038(3) 0.016(3) 0.020(3) -0.001(2) 0.011(3) -0.001(2) O6 0.034(3) 0.027(3) 0.022(3) -0.004(2) -0.007(3) -0.002(3) N1 0.022(4) 0.021(3) 0.013(3) -0.001(3) 0.002(3) 0.000(3) C1 0.030(4) 0.015(4) 0.022(4) 0.004(3) 0.005(3) -0.001(3) C2 0.030(4) 0.012(3) 0.020(4) -0.003(3) -0.002(3) -0.001(3) C3 0.024(4) 0.027(4) 0.034(5) -0.005(4) 0.010(4) 0.001(4) C4 0.017(4) 0.035(5) 0.027(4) 0.003(4) -0.001(3) 0.006(3) C5 0.025(4) 0.049(5) 0.008(4) -0.007(3) 0.002(3) -0.009(4) C6 0.027(4) 0.040(5) 0.018(4) -0.008(4) 0.008(3) -0.019(4) C7 0.039(5) 0.024(4) 0.025(4) -0.003(4) -0.003(4) -0.010(4) C8 0.057(6) 0.020(4) 0.018(4) -0.006(3) -0.002(4) -0.003(4) C9 0.036(5) 0.020(4) 0.026(4) 0.002(3) 0.004(4) 0.005(4) C10 0.045(5) 0.021(4) 0.027(5) -0.004(3) 0.011(4) 0.001(4) C11 0.033(5) 0.023(4) 0.025(4) 0.002(3) 0.011(4) 0.001(4) C12 0.020(4) 0.021(4) 0.022(4) 0.003(3) 0.001(3) 0.003(3) C13 0.039(5) 0.027(4) 0.012(4) -0.005(3) 0.005(3) 0.006(4) C14 0.031(5) 0.024(4) 0.024(4) 0.003(3) 0.008(4) 0.000(4) C15 0.033(5) 0.032(4) 0.017(4) -0.002(3) -0.003(3) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu1 2.5584(14) . ? I1 Cu1 2.7664(14) 4_575 ? I1 Cu2 2.8182(15) . ? I2 Cu2 2.5548(14) . ? I2 Cu1 2.6943(13) . ? I2 Cu2 2.9654(16) 4_576 ? I3 Cu1 2.6207(12) . ? I3 Cu2 2.6282(13) 4_576 ? Cu1 Cu2 2.5090(16) 4_576 ? Cu1 Cu2 2.6619(17) . ? Cu1 I1 2.7664(13) 4_576 ? Cu2 Cu1 2.5090(16) 4_575 ? Cu2 I3 2.6282(13) 4_575 ? Cu2 I2 2.9654(16) 4_575 ? O1 C2 1.415(9) . ? O1 C3 1.418(10) . ? O2 C4 1.416(10) . ? O2 C5 1.438(10) . ? O3 C7 1.402(11) . ? O3 C6 1.430(10) . ? O4 C8 1.423(11) . ? O4 C9 1.433(11) . ? O5 C10 1.427(10) . ? O5 C11 1.440(10) . ? N1 C13 1.511(10) . ? N1 C12 1.512(10) . ? N1 C1 1.525(10) . ? C1 C2 1.501(11) . ? C3 C4 1.517(13) . ? C5 C6 1.472(14) . ? C7 C8 1.497(14) . ? C9 C10 1.502(12) . ? C11 C12 1.500(11) . ? C13 C14 1.493(12) . ? C14 C15 1.321(13) . ? 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 Cu1 I1 Cu1 110.12(5) . 4_575 ? Cu1 I1 Cu2 59.12(4) . . ? Cu1 I1 Cu2 53.39(4) 4_575 . ? Cu2 I2 Cu1 60.88(4) . . ? Cu2 I2 Cu2 112.00(4) . 4_576 ? Cu1 I2 Cu2 52.36(4) . 4_576 ? Cu1 I3 Cu2 57.11(4) . 4_576 ? Cu2 Cu1 I1 169.51(6) 4_576 . ? Cu2 Cu1 I3 61.59(4) 4_576 . ? I1 Cu1 I3 117.53(4) . . ? Cu2 Cu1 Cu2 124.76(7) 4_576 . ? I1 Cu1 Cu2 65.31(4) . . ? I3 Cu1 Cu2 120.58(5) . . ? Cu2 Cu1 I2 69.38(5) 4_576 . ? I1 Cu1 I2 119.46(4) . . ? I3 Cu1 I2 106.51(4) . . ? Cu2 Cu1 I2 56.97(4) . . ? Cu2 Cu1 I1 64.36(4) 4_576 4_576 ? I1 Cu1 I1 107.00(4) . 4_576 ? I3 Cu1 I1 103.67(4) . 4_576 ? Cu2 Cu1 I1 133.75(5) . 4_576 ? I2 Cu1 I1 100.08(4) . 4_576 ? Cu1 Cu2 I2 177.33(6) 4_575 . ? Cu1 Cu2 I3 61.30(4) 4_575 4_575 ? I2 Cu2 I3 120.60(5) . 4_575 ? Cu1 Cu2 Cu1 115.19(6) 4_575 . ? I2 Cu2 Cu1 62.15(4) . . ? I3 Cu2 Cu1 145.59(7) 4_575 . ? Cu1 Cu2 I1 62.25(5) 4_575 . ? I2 Cu2 I1 115.14(5) . . ? I3 Cu2 I1 102.08(5) 4_575 . ? Cu1 Cu2 I1 55.57(4) . . ? Cu1 Cu2 I2 58.25(4) 4_575 4_575 ? I2 Cu2 I2 122.21(6) . 4_575 ? I3 Cu2 I2 99.01(4) 4_575 4_575 ? Cu1 Cu2 I2 107.14(5) . 4_575 ? I1 Cu2 I2 92.69(4) . 4_575 ? C2 O1 C3 111.6(6) . . ? C4 O2 C5 111.9(7) . . ? C7 O3 C6 110.6(6) . . ? C8 O4 C9 113.3(7) . . ? C10 O5 C11 113.2(6) . . ? C13 N1 C12 111.4(6) . . ? C13 N1 C1 111.8(6) . . ? C12 N1 C1 108.7(6) . . ? C2 C1 N1 113.7(6) . . ? O1 C2 C1 109.0(6) . . ? O1 C3 C4 108.1(7) . . ? O2 C4 C3 108.9(7) . . ? O2 C5 C6 110.0(7) . . ? O3 C6 C5 110.0(6) . . ? O3 C7 C8 109.6(7) . . ? O4 C8 C7 108.8(7) . . ? O4 C9 C10 112.5(7) . . ? O5 C10 C9 107.4(7) . . ? O5 C11 C12 106.6(6) . . ? C11 C12 N1 111.6(7) . . ? C14 C13 N1 112.1(6) . . ? C15 C14 C13 124.4(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 I1 Cu1 Cu2 -179(77) 4_575 . . 4_576 ? Cu2 I1 Cu1 Cu2 164.5(3) . . . 4_576 ? Cu1 I1 Cu1 I3 -96.65(4) 4_575 . . . ? Cu2 I1 Cu1 I3 -113.07(6) . . . . ? Cu1 I1 Cu1 Cu2 16.42(4) 4_575 . . . ? Cu1 I1 Cu1 I2 34.85(5) 4_575 . . . ? Cu2 I1 Cu1 I2 18.43(5) . . . . ? Cu1 I1 Cu1 I1 147.37(5) 4_575 . . 4_576 ? Cu2 I1 Cu1 I1 130.94(6) . . . 4_576 ? Cu2 I3 Cu1 I1 -168.16(7) 4_576 . . . ? Cu2 I3 Cu1 Cu2 115.67(8) 4_576 . . . ? Cu2 I3 Cu1 I2 54.70(5) 4_576 . . . ? Cu2 I3 Cu1 I1 -50.37(5) 4_576 . . 4_576 ? Cu2 I2 Cu1 Cu2 166.20(6) . . . 4_576 ? Cu2 I2 Cu1 I1 -20.04(5) . . . . ? Cu2 I2 Cu1 I1 173.76(7) 4_576 . . . ? Cu2 I2 Cu1 I3 116.12(6) . . . . ? Cu2 I2 Cu1 I3 -50.08(4) 4_576 . . . ? Cu2 I2 Cu1 Cu2 -166.20(6) 4_576 . . . ? Cu2 I2 Cu1 I1 -136.24(6) . . . 4_576 ? Cu2 I2 Cu1 I1 57.56(4) 4_576 . . 4_576 ? Cu1 I2 Cu2 Cu1 5.7(16) . . . 4_575 ? Cu2 I2 Cu2 Cu1 17.5(17) 4_576 . . 4_575 ? Cu1 I2 Cu2 I3 140.50(8) . . . 4_575 ? Cu2 I2 Cu2 I3 152.26(4) 4_576 . . 4_575 ? Cu2 I2 Cu2 Cu1 11.75(5) 4_576 . . . ? Cu1 I2 Cu2 I1 17.41(4) . . . . ? Cu2 I2 Cu2 I1 29.16(7) 4_576 . . . ? Cu1 I2 Cu2 I2 -93.51(6) . . . 4_575 ? Cu2 I2 Cu2 I2 -81.76(8) 4_576 . . 4_575 ? Cu2 Cu1 Cu2 Cu1 164.53(7) 4_576 . . 4_575 ? I1 Cu1 Cu2 Cu1 -18.87(5) . . . 4_575 ? I3 Cu1 Cu2 Cu1 89.74(9) . . . 4_575 ? I2 Cu1 Cu2 Cu1 -179.71(8) . . . 4_575 ? I1 Cu1 Cu2 Cu1 -109.18(6) 4_576 . . 4_575 ? Cu2 Cu1 Cu2 I2 -15.77(6) 4_576 . . . ? I1 Cu1 Cu2 I2 160.83(5) . . . . ? I3 Cu1 Cu2 I2 -90.55(5) . . . . ? I1 Cu1 Cu2 I2 70.52(7) 4_576 . . . ? Cu2 Cu1 Cu2 I3 -120.10(11) 4_576 . . 4_575 ? I1 Cu1 Cu2 I3 56.50(9) . . . 4_575 ? I3 Cu1 Cu2 I3 165.12(7) . . . 4_575 ? I2 Cu1 Cu2 I3 -104.33(10) . . . 4_575 ? I1 Cu1 Cu2 I3 -33.81(13) 4_576 . . 4_575 ? Cu2 Cu1 Cu2 I1 -176.60(7) 4_576 . . . ? I3 Cu1 Cu2 I1 108.62(6) . . . . ? I2 Cu1 Cu2 I1 -160.83(5) . . . . ? I1 Cu1 Cu2 I1 -90.31(7) 4_576 . . . ? Cu2 Cu1 Cu2 I2 102.13(6) 4_576 . . 4_575 ? I1 Cu1 Cu2 I2 -81.27(4) . . . 4_575 ? I3 Cu1 Cu2 I2 27.35(7) . . . 4_575 ? I2 Cu1 Cu2 I2 117.90(6) . . . 4_575 ? I1 Cu1 Cu2 I2 -171.58(5) 4_576 . . 4_575 ? Cu1 I1 Cu2 Cu1 160.69(5) . . . 4_575 ? Cu1 I1 Cu2 I2 -18.70(5) . . . . ? Cu1 I1 Cu2 I2 -179.39(8) 4_575 . . . ? Cu1 I1 Cu2 I3 -151.19(6) . . . 4_575 ? Cu1 I1 Cu2 I3 48.12(4) 4_575 . . 4_575 ? Cu1 I1 Cu2 Cu1 -160.69(5) 4_575 . . . ? Cu1 I1 Cu2 I2 109.00(5) . . . 4_575 ? Cu1 I1 Cu2 I2 -51.69(4) 4_575 . . 4_575 ? C13 N1 C1 C2 64.0(9) . . . . ? C12 N1 C1 C2 -172.5(7) . . . . ? C3 O1 C2 C1 177.6(6) . . . . ? N1 C1 C2 O1 64.4(8) . . . . ? C2 O1 C3 C4 -174.1(7) . . . . ? C5 O2 C4 C3 179.6(6) . . . . ? O1 C3 C4 O2 -62.2(8) . . . . ? C4 O2 C5 C6 -166.1(6) . . . . ? C7 O3 C6 C5 169.7(7) . . . . ? O2 C5 C6 O3 71.8(8) . . . . ? C6 O3 C7 C8 166.9(7) . . . . ? C9 O4 C8 C7 -178.9(6) . . . . ? O3 C7 C8 O4 -73.8(9) . . . . ? C8 O4 C9 C10 -91.4(9) . . . . ? C11 O5 C10 C9 -179.5(7) . . . . ? O4 C9 C10 O5 -65.3(10) . . . . ? C10 O5 C11 C12 167.5(7) . . . . ? O5 C11 C12 N1 66.8(8) . . . . ? C13 N1 C12 C11 -140.3(7) . . . . ? C1 N1 C12 C11 96.1(7) . . . . ? C12 N1 C13 C14 61.4(9) . . . . ? C1 N1 C13 C14 -176.7(7) . . . . ? N1 C13 C14 C15 -123.1(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O6 1.06(11) 1.77(11) 2.786(9) 160(9) . O6 H16 O2 0.85 2.19 2.986(9) 155.3 . O6 H17 O4 0.87 2.19 3.064(8) 179.8 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.557 _refine_diff_density_min -2.620 _refine_diff_density_rms 0.358 #===END data_ac65o #(compound16) _database_code_CSD 180585 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H38 N4 O10 Pb' _chemical_formula_weight 701.73 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.894(3) _cell_length_b 12.865(3) _cell_length_c 30.066(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5374.2(19) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2784 _exptl_absorpt_coefficient_mu 6.335 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.1438 _exptl_absorpt_correction_T_max 0.7424 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21245 _diffrn_reflns_av_R_equivalents 0.1616 _diffrn_reflns_av_sigmaI/netI 0.1271 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5248 _reflns_number_gt 3436 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0045P)^2^+26.1687P] 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 5248 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1388 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.002 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 Pb1 Pb 0.01845(3) 0.94545(3) 0.365017(12) 0.04616(15) Uani 1 1 d . . . O1 O -0.1141(6) 0.8137(7) 0.3341(3) 0.076(2) Uani 1 1 d . . . N1 N -0.1130(7) 0.8566(8) 0.4266(3) 0.065(3) Uani 1 1 d . . . C1 C -0.2015(9) 0.8534(11) 0.4004(4) 0.076(4) Uani 1 1 d . . . H1A H -0.2164 0.9227 0.3897 0.091 Uiso 1 1 calc R . . H1B H -0.2543 0.8305 0.4191 0.091 Uiso 1 1 calc R . . O2 O 0.0565(6) 0.8367(6) 0.2896(2) 0.061(2) Uani 1 1 d . . . N2 N 0.1934(6) 0.9956(7) 0.3218(3) 0.050(2) Uani 1 1 d . . . C2 C -0.1914(10) 0.7800(12) 0.3611(5) 0.093(5) Uani 1 1 d . . . H2A H -0.1792 0.7100 0.3716 0.112 Uiso 1 1 calc R . . H2B H -0.2505 0.7795 0.3439 0.112 Uiso 1 1 calc R . . O3 O 0.0788(6) 1.1443(6) 0.3692(3) 0.064(2) Uani 1 1 d . . . N3 N 0.1488(7) 0.8002(9) 0.4220(4) 0.062(3) Uani 1 1 d . . . C3 C -0.0867(10) 0.7423(10) 0.2995(5) 0.079(4) Uani 1 1 d . . . H3A H -0.1438 0.7169 0.2845 0.095 Uiso 1 1 calc R . . H3B H -0.0535 0.6833 0.3125 0.095 Uiso 1 1 calc R . . O4 O -0.0342(6) 1.0700(5) 0.4368(2) 0.061(2) Uani 1 1 d . . . N4 N -0.1260(7) 1.0856(7) 0.3066(3) 0.046(2) Uani 1 1 d . . . C4 C -0.0238(10) 0.7943(11) 0.2676(5) 0.082(4) Uani 1 1 d . . . H4A H -0.0024 0.7448 0.2453 0.098 Uiso 1 1 calc R . . H4B H -0.0590 0.8492 0.2526 0.098 Uiso 1 1 calc R . . O5 O 0.1229(6) 0.7782(6) 0.3832(3) 0.068(2) Uani 1 1 d . . . C5 C 0.1183(10) 0.8916(11) 0.2608(4) 0.071(4) Uani 1 1 d . . . H5A H 0.0857 0.9532 0.2499 0.085 Uiso 1 1 calc R . . H5B H 0.1342 0.8483 0.2355 0.085 Uiso 1 1 calc R . . O6 O 0.1305(7) 0.8913(8) 0.4352(3) 0.079(3) Uani 1 1 d . . . C6 C 0.2067(9) 0.9221(9) 0.2838(4) 0.066(3) Uani 1 1 d . . . H6A H 0.2498 0.9539 0.2624 0.079 Uiso 1 1 calc R . . H6B H 0.2379 0.8598 0.2949 0.079 Uiso 1 1 calc R . . O7 O 0.1884(8) 0.7376(9) 0.4456(4) 0.121(4) Uani 1 1 d . . . C7 C 0.1763(9) 1.1031(9) 0.3061(4) 0.063(3) Uani 1 1 d . . . H7A H 0.2323 1.1266 0.2896 0.076 Uiso 1 1 calc R . . H7B H 0.1219 1.1032 0.2859 0.076 Uiso 1 1 calc R . . O8 O -0.0540(8) 1.0463(7) 0.2898(3) 0.089(3) Uani 1 1 d . . . C8 C 0.1570(9) 1.1770(9) 0.3426(4) 0.066(3) Uani 1 1 d . . . H8A H 0.2140 1.1834 0.3610 0.079 Uiso 1 1 calc R . . H8B H 0.1429 1.2449 0.3302 0.079 Uiso 1 1 calc R . . O9 O -0.1447(7) 1.0670(7) 0.3454(3) 0.090(3) Uani 1 1 d . . . C9 C 0.0676(11) 1.1999(9) 0.4099(4) 0.077(4) Uani 1 1 d . . . H9A H 0.0747 1.2739 0.4047 0.093 Uiso 1 1 calc R . . H9B H 0.1166 1.1784 0.4310 0.093 Uiso 1 1 calc R . . O10 O -0.1726(9) 1.1455(10) 0.2840(3) 0.120(4) Uani 1 1 d . . . C10 C -0.0284(11) 1.1778(9) 0.4279(5) 0.077(4) Uani 1 1 d . . . H10A H -0.0388 1.2171 0.4550 0.093 Uiso 1 1 calc R . . H10B H -0.0774 1.1977 0.4065 0.093 Uiso 1 1 calc R . . C11 C -0.1263(10) 1.0392(11) 0.4542(4) 0.076(4) Uani 1 1 d . . . H11A H -0.1760 1.0519 0.4322 0.091 Uiso 1 1 calc R . . H11B H -0.1412 1.0797 0.4805 0.091 Uiso 1 1 calc R . . C12 C -0.1239(9) 0.9275(9) 0.4656(4) 0.067(4) Uani 1 1 d . . . H12A H -0.1829 0.9098 0.4811 0.080 Uiso 1 1 calc R . . H12B H -0.0709 0.9153 0.4859 0.080 Uiso 1 1 calc R . . C13 C -0.0792(11) 0.7533(10) 0.4414(4) 0.076(4) Uani 1 1 d . . . H13A H -0.0214 0.7630 0.4590 0.092 Uiso 1 1 calc R . . H13B H -0.0614 0.7134 0.4153 0.092 Uiso 1 1 calc R . . C14 C -0.1500(12) 0.6892(12) 0.4686(6) 0.107(6) Uani 1 1 d . . . H14A H -0.1657 0.7266 0.4956 0.129 Uiso 1 1 calc R . . H14B H -0.2089 0.6806 0.4517 0.129 Uiso 1 1 calc R . . C15 C -0.1133(15) 0.5889(14) 0.4801(6) 0.124(7) Uani 1 1 d . . . H15 H -0.0667 0.5610 0.4614 0.148 Uiso 1 1 calc R . . C16 C -0.1381(14) 0.5341(16) 0.5134(7) 0.144(8) Uani 1 1 d . . . H16A H -0.1844 0.5586 0.5331 0.173 Uiso 1 1 calc R . . H16B H -0.1098 0.4695 0.5181 0.173 Uiso 1 1 calc R . . C17 C 0.2749(8) 0.9897(8) 0.3527(3) 0.050(3) Uani 1 1 d . B . H17A H 0.2812 0.9182 0.3625 0.060 Uiso 1 1 calc R . . H17B H 0.2595 1.0312 0.3787 0.060 Uiso 1 1 calc R . . C18 C 0.3718(9) 1.0251(11) 0.3352(4) 0.074(4) Uani 1 1 d . . . H18A H 0.3659 1.0973 0.3263 0.089 Uiso 1 1 calc R A 1 H18B H 0.3860 0.9853 0.3086 0.089 Uiso 1 1 calc R A 1 C19 C 0.462(4) 1.016(4) 0.368(2) 0.062(18) Uani 0.50 1 d P B 1 H19 H 0.4597 1.0592 0.3926 0.074 Uiso 0.50 1 calc PR B 1 C20 C 0.525(6) 0.967(6) 0.3659(18) 0.12(4) Uani 0.50 1 d P B 1 H20A H 0.5322 0.9215 0.3422 0.149 Uiso 0.50 1 calc PR B 1 H20B H 0.5715 0.9709 0.3880 0.149 Uiso 0.50 1 calc PR B 1 C20A C 0.526(4) 0.953(5) 0.363(2) 0.11(3) Uani 0.50 1 d P B 2 H20C H 0.5438 0.9226 0.3366 0.135 Uiso 0.50 1 calc PR B 2 H20D H 0.5656 0.9464 0.3882 0.135 Uiso 0.50 1 calc PR B 2 C19A C 0.436(4) 1.009(6) 0.367(2) 0.09(2) Uani 0.50 1 d P B 2 H19A H 0.4223 1.0371 0.3945 0.108 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0474(2) 0.0476(2) 0.0434(2) -0.0027(2) -0.0054(2) 0.0023(2) O1 0.073(6) 0.091(6) 0.063(5) -0.013(5) -0.002(5) -0.025(5) N1 0.063(7) 0.071(7) 0.061(6) -0.012(6) 0.010(5) -0.016(6) C1 0.057(9) 0.108(10) 0.063(8) -0.013(8) 0.005(7) -0.023(8) O2 0.058(5) 0.073(5) 0.051(4) -0.007(4) -0.011(4) -0.009(4) N2 0.053(6) 0.049(5) 0.049(5) 0.008(5) -0.003(4) 0.001(5) C2 0.068(10) 0.128(12) 0.084(10) 0.002(10) -0.005(8) -0.043(9) O3 0.060(5) 0.058(5) 0.073(5) -0.006(5) 0.016(5) 0.003(4) N3 0.064(7) 0.069(7) 0.052(7) 0.010(6) -0.002(5) 0.007(6) C3 0.070(10) 0.076(9) 0.091(10) -0.024(9) -0.007(8) -0.014(7) O4 0.076(6) 0.055(5) 0.054(4) -0.003(4) 0.001(4) 0.005(4) N4 0.052(6) 0.050(6) 0.035(5) 0.002(4) -0.010(5) 0.020(5) C4 0.062(9) 0.095(10) 0.088(9) -0.042(8) 0.005(8) -0.023(8) O5 0.082(7) 0.064(5) 0.059(5) -0.003(5) 0.000(5) 0.007(4) C5 0.077(10) 0.083(9) 0.052(8) -0.015(7) -0.009(7) 0.009(8) O6 0.084(7) 0.099(7) 0.054(5) -0.014(5) -0.014(5) 0.001(6) C6 0.057(8) 0.081(9) 0.060(7) -0.014(7) 0.006(6) 0.016(7) O7 0.115(9) 0.144(10) 0.103(8) 0.057(8) -0.018(7) 0.038(8) C7 0.052(8) 0.071(8) 0.066(8) 0.020(7) -0.005(6) -0.003(6) O8 0.093(8) 0.097(7) 0.076(6) 0.012(6) 0.001(5) 0.026(6) C8 0.073(9) 0.043(7) 0.080(9) 0.012(7) -0.004(7) 0.001(6) O9 0.099(8) 0.098(7) 0.072(6) 0.008(6) 0.004(5) 0.020(6) C9 0.111(12) 0.054(7) 0.067(9) -0.010(7) -0.007(8) -0.004(8) O10 0.130(10) 0.150(10) 0.081(7) 0.018(7) -0.010(6) 0.071(8) C10 0.093(12) 0.064(8) 0.076(9) -0.017(7) -0.007(8) 0.010(8) C11 0.059(9) 0.103(11) 0.066(8) -0.009(8) 0.009(7) 0.011(8) C12 0.055(8) 0.082(10) 0.064(8) -0.003(7) 0.014(6) -0.010(7) C13 0.098(11) 0.063(8) 0.068(9) 0.016(7) 0.016(8) -0.021(8) C14 0.113(14) 0.104(13) 0.104(12) 0.034(10) 0.012(10) -0.029(11) C15 0.150(18) 0.109(14) 0.112(14) 0.054(12) 0.041(13) -0.002(12) C16 0.092(14) 0.160(19) 0.18(2) 0.042(17) -0.002(14) 0.019(13) C17 0.050(7) 0.053(6) 0.048(7) 0.002(5) 0.007(5) 0.003(5) C18 0.054(9) 0.093(10) 0.075(9) 0.005(8) -0.001(7) 0.003(7) C19 0.03(4) 0.06(2) 0.09(3) -0.04(2) -0.03(2) -0.02(2) C20 0.15(8) 0.15(7) 0.07(3) 0.05(4) 0.01(4) -0.02(5) C20A 0.04(3) 0.10(3) 0.20(6) -0.04(3) -0.04(3) 0.02(3) C19A 0.02(3) 0.14(5) 0.11(4) 0.05(3) -0.02(2) -0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O5 2.652(8) . ? Pb1 O1 2.670(8) . ? Pb1 O3 2.695(8) . ? Pb1 O6 2.712(8) . ? Pb1 O2 2.717(7) . ? O1 C2 1.415(15) . ? O1 C3 1.437(14) . ? N1 C1 1.460(15) . ? N1 C13 1.478(15) . ? N1 C12 1.493(14) . ? C1 C2 1.519(17) . ? O2 C4 1.406(14) . ? O2 C5 1.408(14) . ? N2 C17 1.469(13) . ? N2 C7 1.480(13) . ? N2 C6 1.493(13) . ? O3 C8 1.413(14) . ? O3 C9 1.428(13) . ? N3 O7 1.208(12) . ? N3 O5 1.254(12) . ? N3 O6 1.262(12) . ? C3 C4 1.461(18) . ? O4 C10 1.415(14) . ? O4 C11 1.438(15) . ? N4 O10 1.215(11) . ? N4 O9 1.218(11) . ? N4 O8 1.230(12) . ? C5 C6 1.464(17) . ? C7 C8 1.476(16) . ? C9 C10 1.468(18) . ? C11 C12 1.478(16) . ? C13 C14 1.522(17) . ? C14 C15 1.43(2) . ? C15 C16 1.27(2) . ? C17 C18 1.516(16) . ? C18 C19A 1.32(6) . ? C18 C19 1.60(6) . ? C19 C20 1.07(10) . ? C20A C19A 1.44(9) . ? 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 O5 Pb1 O1 86.2(3) . . ? O5 Pb1 O3 126.2(3) . . ? O1 Pb1 O3 146.4(3) . . ? O5 Pb1 O6 47.0(3) . . ? O1 Pb1 O6 120.3(3) . . ? O3 Pb1 O6 91.7(3) . . ? O5 Pb1 O2 69.4(2) . . ? O1 Pb1 O2 61.1(3) . . ? O3 Pb1 O2 117.8(2) . . ? O6 Pb1 O2 113.9(3) . . ? C2 O1 C3 114.8(10) . . ? C2 O1 Pb1 121.2(7) . . ? C3 O1 Pb1 118.3(7) . . ? C1 N1 C13 113.9(10) . . ? C1 N1 C12 110.8(10) . . ? C13 N1 C12 110.2(9) . . ? N1 C1 C2 111.0(11) . . ? C4 O2 C5 112.9(9) . . ? C4 O2 Pb1 115.9(7) . . ? C5 O2 Pb1 111.9(6) . . ? C17 N2 C7 111.9(9) . . ? C17 N2 C6 110.8(9) . . ? C7 N2 C6 111.6(9) . . ? O1 C2 C1 109.1(11) . . ? C8 O3 C9 114.8(10) . . ? C8 O3 Pb1 119.7(6) . . ? C9 O3 Pb1 118.8(7) . . ? O7 N3 O5 121.9(12) . . ? O7 N3 O6 121.8(12) . . ? O5 N3 O6 116.4(10) . . ? O1 C3 C4 109.9(10) . . ? C10 O4 C11 112.9(10) . . ? O10 N4 O9 123.2(11) . . ? O10 N4 O8 117.6(10) . . ? O9 N4 O8 119.1(9) . . ? O2 C4 C3 110.1(11) . . ? N3 O5 Pb1 99.5(7) . . ? O2 C5 C6 110.8(10) . . ? N3 O6 Pb1 96.3(7) . . ? C5 C6 N2 115.2(10) . . ? C8 C7 N2 113.2(9) . . ? O3 C8 C7 111.6(10) . . ? O3 C9 C10 108.5(11) . . ? O4 C10 C9 108.1(11) . . ? O4 C11 C12 109.4(10) . . ? C11 C12 N1 114.5(10) . . ? N1 C13 C14 116.4(12) . . ? C15 C14 C13 112.9(15) . . ? C16 C15 C14 126(2) . . ? N2 C17 C18 116.7(9) . . ? C19A C18 C17 108(3) . . ? C19A C18 C19 10(5) . . ? C17 C18 C19 117(3) . . ? C20 C19 C18 130(5) . . ? C18 C19A C20A 128(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Pb1 O1 C2 95.5(10) . . . . ? O3 Pb1 O1 C2 -98.4(10) . . . . ? O6 Pb1 O1 C2 61.7(11) . . . . ? O2 Pb1 O1 C2 164.0(11) . . . . ? O5 Pb1 O1 C3 -56.6(8) . . . . ? O3 Pb1 O1 C3 109.4(9) . . . . ? O6 Pb1 O1 C3 -90.4(9) . . . . ? O2 Pb1 O1 C3 11.9(8) . . . . ? C13 N1 C1 C2 -54.3(14) . . . . ? C12 N1 C1 C2 -179.1(10) . . . . ? O5 Pb1 O2 C4 116.1(9) . . . . ? O1 Pb1 O2 C4 18.7(8) . . . . ? O3 Pb1 O2 C4 -122.9(8) . . . . ? O6 Pb1 O2 C4 131.4(9) . . . . ? O5 Pb1 O2 C5 -112.5(8) . . . . ? O1 Pb1 O2 C5 150.2(8) . . . . ? O3 Pb1 O2 C5 8.5(8) . . . . ? O6 Pb1 O2 C5 -97.1(7) . . . . ? C3 O1 C2 C1 170.6(11) . . . . ? Pb1 O1 C2 C1 17.6(15) . . . . ? N1 C1 C2 O1 -58.9(15) . . . . ? O5 Pb1 O3 C8 59.5(9) . . . . ? O1 Pb1 O3 C8 -103.2(8) . . . . ? O6 Pb1 O3 C8 93.9(8) . . . . ? O2 Pb1 O3 C8 -24.3(8) . . . . ? O5 Pb1 O3 C9 -90.4(9) . . . . ? O1 Pb1 O3 C9 107.0(9) . . . . ? O6 Pb1 O3 C9 -55.9(9) . . . . ? O2 Pb1 O3 C9 -174.2(8) . . . . ? C2 O1 C3 C4 166.4(12) . . . . ? Pb1 O1 C3 C4 -39.8(14) . . . . ? C5 O2 C4 C3 -177.6(11) . . . . ? Pb1 O2 C4 C3 -46.6(13) . . . . ? O1 C3 C4 O2 56.0(15) . . . . ? O7 N3 O5 Pb1 170.0(11) . . . . ? O6 N3 O5 Pb1 -9.4(11) . . . . ? O1 Pb1 O5 N3 -133.5(7) . . . . ? O3 Pb1 O5 N3 56.0(7) . . . . ? O6 Pb1 O5 N3 5.3(6) . . . . ? O2 Pb1 O5 N3 166.1(7) . . . . ? C4 O2 C5 C6 -172.4(10) . . . . ? Pb1 O2 C5 C6 54.7(11) . . . . ? O7 N3 O6 Pb1 -170.3(11) . . . . ? O5 N3 O6 Pb1 9.1(10) . . . . ? O5 Pb1 O6 N3 -5.3(6) . . . . ? O1 Pb1 O6 N3 44.2(8) . . . . ? O3 Pb1 O6 N3 -146.6(7) . . . . ? O2 Pb1 O6 N3 -25.0(7) . . . . ? O2 C5 C6 N2 -63.4(14) . . . . ? C17 N2 C6 C5 157.7(10) . . . . ? C7 N2 C6 C5 -76.8(13) . . . . ? C17 N2 C7 C8 -58.5(13) . . . . ? C6 N2 C7 C8 176.6(10) . . . . ? C9 O3 C8 C7 168.2(10) . . . . ? Pb1 O3 C8 C7 17.1(12) . . . . ? N2 C7 C8 O3 -55.8(13) . . . . ? C8 O3 C9 C10 165.2(10) . . . . ? Pb1 O3 C9 C10 -43.5(13) . . . . ? C11 O4 C10 C9 -179.4(10) . . . . ? O3 C9 C10 O4 62.1(13) . . . . ? C10 O4 C11 C12 -175.9(10) . . . . ? O4 C11 C12 N1 -66.3(14) . . . . ? C1 N1 C12 C11 -71.9(13) . . . . ? C13 N1 C12 C11 161.2(11) . . . . ? C1 N1 C13 C14 -56.7(15) . . . . ? C12 N1 C13 C14 68.5(14) . . . . ? N1 C13 C14 C15 177.7(14) . . . . ? C13 C14 C15 C16 154(2) . . . . ? C7 N2 C17 C18 -59.8(13) . . . . ? C6 N2 C17 C18 65.6(13) . . . . ? N2 C17 C18 C19A -177(4) . . . . ? N2 C17 C18 C19 -178(2) . . . . ? C19A C18 C19 C20 106(30) . . . . ? C17 C18 C19 C20 113(8) . . . . ? C17 C18 C19A C20A 127(6) . . . . ? C19 C18 C19A C20A -60(27) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.804 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.168 #===END