# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1Mg _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H21 Mg N3 O10 S2' _chemical_formula_weight 563.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1013(11) _cell_length_b 10.8625(14) _cell_length_c 12.5697(16) _cell_angle_alpha 76.698(2) _cell_angle_beta 86.585(2) _cell_angle_gamma 79.993(2) _cell_volume 1190.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.314 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8901 _exptl_absorpt_correction_T_max 0.9118 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6070 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4114 _reflns_number_gt 3224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4114 _refine_ls_number_parameters 358 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1405 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 1.37888(10) -0.76520(9) 1.18872(7) 0.0278(3) Uani 1 1 d . . . C1 C 1.1435(4) -0.6863(3) 0.9960(2) 0.0420(8) Uani 1 1 d . . . H1A H 1.2284 -0.6958 0.9517 0.050 Uiso 1 1 calc R . . C2 C 1.0072(4) -0.6537(4) 0.9471(3) 0.0454(9) Uani 1 1 d . . . H2A H 1.0000 -0.6417 0.8717 0.054 Uiso 1 1 calc R . . C3 C 0.8803(4) -0.6392(4) 1.0127(3) 0.0461(9) Uani 1 1 d . . . H3A H 0.7860 -0.6168 0.9824 0.055 Uiso 1 1 calc R . . C4 C 0.8970(3) -0.6588(3) 1.1245(3) 0.0379(8) Uani 1 1 d . . . H4A H 0.8135 -0.6498 1.1702 0.046 Uiso 1 1 calc R . . C5 C 1.0373(3) -0.6916(3) 1.1678(2) 0.0280(6) Uani 1 1 d . . . C6 C 1.0665(3) -0.7127(3) 1.2866(2) 0.0259(6) Uani 1 1 d . . . C7 C 0.9574(3) -0.6918(3) 1.3656(2) 0.0293(7) Uani 1 1 d . . . H7A H 0.8580 -0.6652 1.3461 0.035 Uiso 1 1 calc R . . C8 C 0.9973(3) -0.7109(3) 1.4740(2) 0.0266(6) Uani 1 1 d . . . C9 C 1.1472(3) -0.7520(3) 1.4995(2) 0.0287(7) Uani 1 1 d . . . H9A H 1.1776 -0.7663 1.5713 0.034 Uiso 1 1 calc R . . C10 C 1.2507(3) -0.7716(3) 1.4169(2) 0.0252(6) Uani 1 1 d . . . C11 C 1.4137(3) -0.8147(3) 1.4348(2) 0.0257(6) Uani 1 1 d . . . C12 C 1.4766(3) -0.8421(3) 1.5368(2) 0.0310(7) Uani 1 1 d . . . H12A H 1.4178 -0.8317 1.5982 0.037 Uiso 1 1 calc R . . C13 C 1.6291(3) -0.8853(3) 1.5456(3) 0.0366(7) Uani 1 1 d . . . H13A H 1.6732 -0.9049 1.6136 0.044 Uiso 1 1 calc R . . C14 C 1.7145(3) -0.8990(3) 1.4546(3) 0.0362(7) Uani 1 1 d . . . H14A H 1.8166 -0.9287 1.4594 0.043 Uiso 1 1 calc R . . C15 C 1.6446(3) -0.8675(3) 1.3557(3) 0.0332(7) Uani 1 1 d . . . H15A H 1.7025 -0.8765 1.2936 0.040 Uiso 1 1 calc R . . C16 C 0.8818(3) -0.6750(3) 1.5562(2) 0.0270(6) Uani 1 1 d . . . C17 C 0.8700(3) -0.7410(3) 1.6671(2) 0.0261(6) Uani 1 1 d . . . C18 C 0.7614(3) -0.6918(3) 1.7353(2) 0.0268(6) Uani 1 1 d . . . H18A H 0.7557 -0.7343 1.8083 0.032 Uiso 1 1 calc R . . C19 C 0.6609(3) -0.5806(3) 1.6970(2) 0.0264(6) Uani 1 1 d . . . C20 C 0.6670(3) -0.5186(3) 1.5882(2) 0.0325(7) Uani 1 1 d . . . H20A H 0.5976 -0.4462 1.5608 0.039 Uiso 1 1 calc R . . C21 C 0.7777(3) -0.5656(3) 1.5201(2) 0.0318(7) Uani 1 1 d . . . H21A H 0.7823 -0.5219 1.4474 0.038 Uiso 1 1 calc R . . N1 N 1.1613(3) -0.7052(2) 1.1035(2) 0.0327(6) Uani 1 1 d . . . N2 N 1.2106(3) -0.7524(2) 1.31311(18) 0.0264(5) Uani 1 1 d . . . N3 N 1.4977(3) -0.8246(2) 1.34332(19) 0.0287(6) Uani 1 1 d . . . O1W O 1.5499(3) -0.7710(2) 1.07927(19) 0.0451(6) Uani 1 1 d D . . H1WB H 1.551(4) -0.704(2) 1.025(2) 0.068 Uiso 1 1 d D . . H1WA H 1.622(3) -0.826(3) 1.066(3) 0.068 Uiso 1 1 d D . . O1 O 1.1203(3) -0.8713(2) 1.75218(19) 0.0508(6) Uani 1 1 d . . . O2 O 0.8935(2) -0.9453(2) 1.82399(17) 0.0424(6) Uani 1 1 d . . . O2W O 1.3612(3) -0.9498(2) 1.1828(2) 0.0504(6) Uani 1 1 d D . . H2WB H 1.430(3) -1.013(3) 1.180(3) 0.076 Uiso 1 1 d D . . H2WA H 1.280(2) -0.974(4) 1.173(4) 0.076 Uiso 1 1 d D . . O3 O 0.9825(3) -0.9697(2) 1.64355(18) 0.0462(6) Uani 1 1 d . . . O3W O 1.5781(4) -1.1564(4) 1.1900(4) 0.1051(14) Uani 1 1 d D . . H3WB H 1.569(8) -1.235(3) 1.191(5) 0.158 Uiso 1 1 d D . . H3WA H 1.573(6) -1.119(4) 1.1186(18) 0.158 Uiso 1 1 d D . . O4 O 0.5010(3) -0.6242(2) 1.87402(17) 0.0405(6) Uani 1 1 d . . . O4W O 1.7722(4) -0.9585(4) 1.0434(2) 0.0812(10) Uani 1 1 d D . . H4WB H 1.824(5) -0.955(5) 0.983(2) 0.122 Uiso 1 1 d D . . H4WA H 1.835(5) -0.997(5) 1.094(3) 0.122 Uiso 1 1 d D . . O5 O 0.3999(2) -0.4518(2) 1.72376(18) 0.0419(6) Uani 1 1 d . . . O6 O 0.6036(2) -0.42832(19) 1.82879(17) 0.0352(5) Uani 1 1 d . . . S1 S 0.97701(8) -0.89518(7) 1.72519(6) 0.0313(2) Uani 1 1 d . . . S2 S 0.52866(8) -0.51529(7) 1.78713(6) 0.0276(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0231(6) 0.0339(5) 0.0256(5) -0.0082(4) 0.0040(4) -0.0020(4) C1 0.0367(19) 0.065(2) 0.0251(16) -0.0151(15) 0.0051(14) -0.0063(16) C2 0.042(2) 0.070(2) 0.0290(17) -0.0149(16) -0.0001(15) -0.0171(18) C3 0.034(2) 0.065(2) 0.0396(19) -0.0086(17) -0.0089(15) -0.0097(17) C4 0.0238(17) 0.055(2) 0.0330(17) -0.0094(15) 0.0030(13) -0.0038(14) C5 0.0261(16) 0.0335(16) 0.0247(15) -0.0081(12) 0.0006(12) -0.0039(12) C6 0.0227(15) 0.0301(15) 0.0254(15) -0.0070(12) 0.0028(12) -0.0056(12) C7 0.0219(15) 0.0335(16) 0.0324(16) -0.0086(13) 0.0028(12) -0.0040(12) C8 0.0243(16) 0.0279(15) 0.0263(15) -0.0056(12) 0.0065(12) -0.0038(12) C9 0.0280(16) 0.0330(15) 0.0234(15) -0.0057(12) 0.0034(12) -0.0030(12) C10 0.0247(16) 0.0262(14) 0.0235(14) -0.0046(11) -0.0005(12) -0.0025(12) C11 0.0216(15) 0.0250(14) 0.0280(15) -0.0029(12) 0.0037(12) -0.0029(11) C12 0.0279(17) 0.0369(16) 0.0261(15) -0.0032(12) 0.0006(12) -0.0048(13) C13 0.0321(18) 0.0362(17) 0.0386(18) -0.0012(14) -0.0100(14) -0.0048(14) C14 0.0227(16) 0.0340(17) 0.048(2) -0.0011(14) -0.0029(14) -0.0050(13) C15 0.0229(16) 0.0344(16) 0.0404(18) -0.0080(14) 0.0079(13) -0.0034(13) C16 0.0234(15) 0.0296(15) 0.0283(15) -0.0084(12) 0.0062(12) -0.0051(12) C17 0.0235(15) 0.0320(15) 0.0225(14) -0.0070(12) -0.0011(11) -0.0021(12) C18 0.0248(16) 0.0319(15) 0.0226(14) -0.0069(12) 0.0015(12) -0.0017(12) C19 0.0235(15) 0.0295(15) 0.0262(15) -0.0077(12) 0.0030(12) -0.0032(12) C20 0.0348(18) 0.0286(15) 0.0298(16) -0.0045(12) 0.0030(13) 0.0027(13) C21 0.0360(18) 0.0321(16) 0.0232(15) -0.0019(12) 0.0065(13) -0.0030(13) N1 0.0260(14) 0.0461(15) 0.0261(13) -0.0108(11) 0.0051(10) -0.0043(11) N2 0.0216(13) 0.0308(13) 0.0257(13) -0.0067(10) 0.0012(10) -0.0016(10) N3 0.0235(13) 0.0301(13) 0.0298(13) -0.0037(10) 0.0026(10) -0.0021(10) O1W 0.0425(15) 0.0443(14) 0.0395(13) -0.0036(11) 0.0184(11) 0.0033(11) O1 0.0307(13) 0.0658(16) 0.0476(14) 0.0018(12) -0.0093(11) -0.0017(11) O2 0.0422(14) 0.0412(13) 0.0344(13) 0.0015(10) 0.0072(10) 0.0029(10) O2W 0.0446(15) 0.0403(14) 0.0702(18) -0.0200(13) 0.0033(14) -0.0089(11) O3 0.0563(16) 0.0376(13) 0.0408(13) -0.0145(10) -0.0003(11) 0.0099(11) O3W 0.065(2) 0.086(2) 0.188(4) -0.082(3) 0.025(3) -0.017(2) O4 0.0492(14) 0.0358(12) 0.0335(12) -0.0049(10) 0.0170(10) -0.0088(10) O4W 0.077(2) 0.102(2) 0.0460(17) -0.0162(17) -0.0057(15) 0.0356(19) O5 0.0260(12) 0.0539(14) 0.0416(13) -0.0116(11) -0.0002(10) 0.0061(10) O6 0.0384(13) 0.0326(11) 0.0361(12) -0.0139(9) 0.0027(10) -0.0028(9) S1 0.0260(4) 0.0349(4) 0.0275(4) -0.0035(3) 0.0004(3) 0.0046(3) S2 0.0252(4) 0.0294(4) 0.0263(4) -0.0072(3) 0.0054(3) 0.0001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mg1 O1W 2.018(2) . ? Mg1 O2W 2.058(2) . ? Mg1 O6 2.096(2) 2_748 ? Mg1 N2 2.133(2) . ? Mg1 N3 2.189(3) . ? Mg1 N1 2.231(3) . ? C1 N1 1.335(4) . ? C1 C2 1.372(5) . ? C1 H1A 0.9300 . ? C2 C3 1.387(5) . ? C2 H2A 0.9300 . ? C3 C4 1.386(5) . ? C3 H3A 0.9300 . ? C4 C5 1.373(4) . ? C4 H4A 0.9300 . ? C5 N1 1.355(4) . ? C5 C6 1.491(4) . ? C6 N2 1.344(4) . ? C6 C7 1.391(4) . ? C7 C8 1.390(4) . ? C7 H7A 0.9300 . ? C8 C9 1.392(4) . ? C8 C16 1.496(4) . ? C9 C10 1.388(4) . ? C9 H9A 0.9300 . ? C10 N2 1.336(4) . ? C10 C11 1.490(4) . ? C11 N3 1.357(3) . ? C11 C12 1.382(4) . ? C12 C13 1.388(4) . ? C12 H12A 0.9300 . ? C13 C14 1.367(4) . ? C13 H13A 0.9300 . ? C14 C15 1.375(5) . ? C14 H14A 0.9300 . ? C15 N3 1.343(4) . ? C15 H15A 0.9300 . ? C16 C21 1.389(4) . ? C16 C17 1.420(4) . ? C17 C18 1.387(4) . ? C17 S1 1.801(3) . ? C18 C19 1.388(4) . ? C18 H18A 0.9300 . ? C19 C20 1.381(4) . ? C19 S2 1.773(3) . ? C20 C21 1.388(4) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? O1W H1WB 0.877(18) . ? O1W H1WA 0.843(18) . ? O1 S1 1.447(3) . ? O2 S1 1.462(2) . ? O2W H2WB 0.848(18) . ? O2W H2WA 0.851(18) . ? O3 S1 1.440(2) . ? O3W H3WB 0.87(2) . ? O3W H3WA 0.895(19) . ? O4 S2 1.460(2) . ? O4W H4WB 0.860(19) . ? O4W H4WA 0.865(19) . ? O5 S2 1.436(2) . ? O6 S2 1.458(2) . ? O6 Mg1 2.096(2) 2_748 ? 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 O1W Mg1 O2W 88.91(11) . . ? O1W Mg1 O6 86.08(10) . 2_748 ? O2W Mg1 O6 172.12(11) . 2_748 ? O1W Mg1 N2 174.74(11) . . ? O2W Mg1 N2 94.58(10) . . ? O6 Mg1 N2 90.86(9) 2_748 . ? O1W Mg1 N3 101.33(10) . . ? O2W Mg1 N3 93.70(11) . . ? O6 Mg1 N3 93.24(9) 2_748 . ? N2 Mg1 N3 74.55(9) . . ? O1W Mg1 N1 110.55(10) . . ? O2W Mg1 N1 86.69(11) . . ? O6 Mg1 N1 89.39(9) 2_748 . ? N2 Mg1 N1 73.64(9) . . ? N3 Mg1 N1 148.11(10) . . ? N1 C1 C2 123.7(3) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C1 C2 C3 118.3(3) . . ? C1 C2 H2A 120.8 . . ? C3 C2 H2A 120.8 . . ? C4 C3 C2 118.6(3) . . ? C4 C3 H3A 120.7 . . ? C2 C3 H3A 120.7 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? N1 C5 C4 121.6(3) . . ? N1 C5 C6 114.7(3) . . ? C4 C5 C6 123.7(3) . . ? N2 C6 C7 121.1(3) . . ? N2 C6 C5 114.5(2) . . ? C7 C6 C5 124.4(3) . . ? C8 C7 C6 119.8(3) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C7 C8 C9 118.1(3) . . ? C7 C8 C16 119.3(3) . . ? C9 C8 C16 122.4(3) . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? N2 C10 C9 121.8(3) . . ? N2 C10 C11 114.3(2) . . ? C9 C10 C11 123.9(3) . . ? N3 C11 C12 121.8(3) . . ? N3 C11 C10 115.2(2) . . ? C12 C11 C10 122.9(2) . . ? C11 C12 C13 118.7(3) . . ? C11 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C13 C14 C15 117.9(3) . . ? C13 C14 H14A 121.1 . . ? C15 C14 H14A 121.1 . . ? N3 C15 C14 124.0(3) . . ? N3 C15 H15A 118.0 . . ? C14 C15 H15A 118.0 . . ? C21 C16 C17 117.3(2) . . ? C21 C16 C8 116.3(2) . . ? C17 C16 C8 126.3(2) . . ? C18 C17 C16 119.6(2) . . ? C18 C17 S1 115.8(2) . . ? C16 C17 S1 124.3(2) . . ? C17 C18 C19 121.5(3) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C20 C19 C18 119.5(3) . . ? C20 C19 S2 119.8(2) . . ? C18 C19 S2 120.7(2) . . ? C19 C20 C21 119.3(3) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C20 C21 C16 122.7(3) . . ? C20 C21 H21A 118.7 . . ? C16 C21 H21A 118.7 . . ? C1 N1 C5 118.0(3) . . ? C1 N1 Mg1 125.5(2) . . ? C5 N1 Mg1 116.49(19) . . ? C10 N2 C6 119.8(2) . . ? C10 N2 Mg1 119.40(19) . . ? C6 N2 Mg1 120.45(19) . . ? C15 N3 C11 117.5(3) . . ? C15 N3 Mg1 126.4(2) . . ? C11 N3 Mg1 116.12(18) . . ? Mg1 O1W H1WB 117(2) . . ? Mg1 O1W H1WA 137(2) . . ? H1WB O1W H1WA 106(2) . . ? Mg1 O2W H2WB 129(3) . . ? Mg1 O2W H2WA 124(3) . . ? H2WB O2W H2WA 106(3) . . ? H3WB O3W H3WA 102(3) . . ? H4WB O4W H4WA 104(3) . . ? S2 O6 Mg1 143.48(14) . 2_748 ? O3 S1 O1 114.91(15) . . ? O3 S1 O2 112.99(15) . . ? O1 S1 O2 110.94(14) . . ? O3 S1 C17 105.81(13) . . ? O1 S1 C17 106.41(14) . . ? O2 S1 C17 104.90(12) . . ? O5 S2 O6 113.50(13) . . ? O5 S2 O4 114.07(14) . . ? O6 S2 O4 111.14(13) . . ? O5 S2 C19 106.83(13) . . ? O6 S2 C19 104.97(13) . . ? O4 S2 C19 105.48(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.1(6) . . . . ? C1 C2 C3 C4 -0.3(5) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C3 C4 C5 N1 0.1(5) . . . . ? C3 C4 C5 C6 179.1(3) . . . . ? N1 C5 C6 N2 -5.2(4) . . . . ? C4 C5 C6 N2 175.8(3) . . . . ? N1 C5 C6 C7 173.6(3) . . . . ? C4 C5 C6 C7 -5.4(5) . . . . ? N2 C6 C7 C8 0.7(4) . . . . ? C5 C6 C7 C8 -178.1(3) . . . . ? C6 C7 C8 C9 -0.7(4) . . . . ? C6 C7 C8 C16 173.6(3) . . . . ? C7 C8 C9 C10 0.5(4) . . . . ? C16 C8 C9 C10 -173.6(3) . . . . ? C8 C9 C10 N2 -0.3(4) . . . . ? C8 C9 C10 C11 179.6(3) . . . . ? N2 C10 C11 N3 1.8(4) . . . . ? C9 C10 C11 N3 -178.1(3) . . . . ? N2 C10 C11 C12 -178.6(3) . . . . ? C9 C10 C11 C12 1.5(4) . . . . ? N3 C11 C12 C13 -2.3(4) . . . . ? C10 C11 C12 C13 178.1(3) . . . . ? C11 C12 C13 C14 0.6(4) . . . . ? C12 C13 C14 C15 0.7(5) . . . . ? C13 C14 C15 N3 -0.2(5) . . . . ? C7 C8 C16 C21 -36.7(4) . . . . ? C9 C8 C16 C21 137.3(3) . . . . ? C7 C8 C16 C17 144.1(3) . . . . ? C9 C8 C16 C17 -41.8(4) . . . . ? C21 C16 C17 C18 -2.8(4) . . . . ? C8 C16 C17 C18 176.4(3) . . . . ? C21 C16 C17 S1 171.4(2) . . . . ? C8 C16 C17 S1 -9.5(4) . . . . ? C16 C17 C18 C19 1.5(4) . . . . ? S1 C17 C18 C19 -173.1(2) . . . . ? C17 C18 C19 C20 1.3(5) . . . . ? C17 C18 C19 S2 -177.0(2) . . . . ? C18 C19 C20 C21 -2.8(5) . . . . ? S2 C19 C20 C21 175.5(2) . . . . ? C19 C20 C21 C16 1.6(5) . . . . ? C17 C16 C21 C20 1.2(5) . . . . ? C8 C16 C21 C20 -178.0(3) . . . . ? C2 C1 N1 C5 0.2(5) . . . . ? C2 C1 N1 Mg1 177.6(3) . . . . ? C4 C5 N1 C1 -0.3(5) . . . . ? C6 C5 N1 C1 -179.3(3) . . . . ? C4 C5 N1 Mg1 -178.0(2) . . . . ? C6 C5 N1 Mg1 3.0(3) . . . . ? O1W Mg1 N1 C1 5.5(3) . . . . ? O2W Mg1 N1 C1 -82.1(3) . . . . ? O6 Mg1 N1 C1 91.1(3) 2_748 . . . ? N2 Mg1 N1 C1 -177.9(3) . . . . ? N3 Mg1 N1 C1 -173.8(2) . . . . ? O1W Mg1 N1 C5 -177.0(2) . . . . ? O2W Mg1 N1 C5 95.4(2) . . . . ? O6 Mg1 N1 C5 -91.4(2) 2_748 . . . ? N2 Mg1 N1 C5 -0.3(2) . . . . ? N3 Mg1 N1 C5 3.7(3) . . . . ? C9 C10 N2 C6 0.2(4) . . . . ? C11 C10 N2 C6 -179.7(2) . . . . ? C9 C10 N2 Mg1 173.5(2) . . . . ? C11 C10 N2 Mg1 -6.4(3) . . . . ? C7 C6 N2 C10 -0.4(4) . . . . ? C5 C6 N2 C10 178.4(2) . . . . ? C7 C6 N2 Mg1 -173.6(2) . . . . ? C5 C6 N2 Mg1 5.2(3) . . . . ? O1W Mg1 N2 C10 -32.6(12) . . . . ? O2W Mg1 N2 C10 98.8(2) . . . . ? O6 Mg1 N2 C10 -86.9(2) 2_748 . . . ? N3 Mg1 N2 C10 6.2(2) . . . . ? N1 Mg1 N2 C10 -176.0(2) . . . . ? O1W Mg1 N2 C6 140.6(11) . . . . ? O2W Mg1 N2 C6 -88.0(2) . . . . ? O6 Mg1 N2 C6 86.3(2) 2_748 . . . ? N3 Mg1 N2 C6 179.4(2) . . . . ? N1 Mg1 N2 C6 -2.8(2) . . . . ? C14 C15 N3 C11 -1.4(4) . . . . ? C14 C15 N3 Mg1 177.4(2) . . . . ? C12 C11 N3 C15 2.7(4) . . . . ? C10 C11 N3 C15 -177.7(2) . . . . ? C12 C11 N3 Mg1 -176.2(2) . . . . ? C10 C11 N3 Mg1 3.4(3) . . . . ? O1W Mg1 N3 C15 -7.1(3) . . . . ? O2W Mg1 N3 C15 82.5(2) . . . . ? O6 Mg1 N3 C15 -93.8(2) 2_748 . . . ? N2 Mg1 N3 C15 176.2(3) . . . . ? N1 Mg1 N3 C15 172.2(2) . . . . ? O1W Mg1 N3 C11 171.7(2) . . . . ? O2W Mg1 N3 C11 -98.7(2) . . . . ? O6 Mg1 N3 C11 85.1(2) 2_748 . . . ? N2 Mg1 N3 C11 -4.93(19) . . . . ? N1 Mg1 N3 C11 -9.0(3) . . . . ? C18 C17 S1 O3 134.1(2) . . . . ? C16 C17 S1 O3 -40.2(3) . . . . ? C18 C17 S1 O1 -103.2(2) . . . . ? C16 C17 S1 O1 82.4(3) . . . . ? C18 C17 S1 O2 14.4(3) . . . . ? C16 C17 S1 O2 -159.9(3) . . . . ? Mg1 O6 S2 O5 -15.6(3) 2_748 . . . ? Mg1 O6 S2 O4 -145.7(2) 2_748 . . . ? Mg1 O6 S2 C19 100.7(2) 2_748 . . . ? C20 C19 S2 O5 32.0(3) . . . . ? C18 C19 S2 O5 -149.7(2) . . . . ? C20 C19 S2 O6 -88.8(3) . . . . ? C18 C19 S2 O6 89.5(3) . . . . ? C20 C19 S2 O4 153.7(3) . . . . ? C18 C19 S2 O4 -28.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.909 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 958305' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2Ca _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H20 Ca N3 O9.50 S2' _chemical_formula_weight 570.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.538(17) _cell_length_b 16.748(16) _cell_length_c 16.019(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.804(12) _cell_angle_gamma 90.00 _cell_volume 4830(8) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1807 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.91 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_T_max 0.8784 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12245 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4734 _reflns_number_gt 2463 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4734 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.2067 _refine_ls_wR_factor_gt 0.1653 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Ca1 Ca 0.34244(5) 0.17847(6) 0.34674(6) 0.0375(3) Uani 1 1 d . . . S1 S 0.66057(6) 0.31793(8) 0.70481(8) 0.0410(4) Uani 1 1 d . . . S2 S 0.53818(7) 0.14123(9) 0.42474(7) 0.0440(4) Uani 1 1 d . . . N2 N 0.65746(19) 0.1786(2) 0.9959(2) 0.0348(9) Uani 1 1 d . . . O2W O 0.33280(19) 0.0980(2) 0.2175(2) 0.0550(10) Uani 1 1 d . . . H2WA H 0.3585 0.0801 0.1848 0.083 Uiso 1 1 d R . . H2WB H 0.2881 0.0826 0.1980 0.083 Uiso 1 1 d R . . C16 C 0.6019(2) 0.1637(3) 0.7198(3) 0.0375(12) Uani 1 1 d . . . C6 C 0.6721(2) 0.1115(3) 0.9563(3) 0.0347(11) Uani 1 1 d . . . C7 C 0.6556(2) 0.1056(3) 0.8667(3) 0.0384(11) Uani 1 1 d . . . H7A H 0.6688 0.0599 0.8411 0.046 Uiso 1 1 calc R . . N1 N 0.7079(2) 0.0524(3) 1.0985(2) 0.0425(10) Uani 1 1 d . . . C18 C 0.5969(2) 0.2170(3) 0.5772(3) 0.0390(12) Uani 1 1 d . . . H18A H 0.6062 0.2587 0.5429 0.047 Uiso 1 1 calc R . . C8 C 0.6197(2) 0.1674(3) 0.8160(3) 0.0344(11) Uani 1 1 d . . . C5 C 0.7082(2) 0.0454(3) 1.0144(3) 0.0356(11) Uani 1 1 d . . . N3 N 0.6370(2) 0.3144(3) 1.0784(3) 0.0498(12) Uani 1 1 d . . . C11 C 0.6137(3) 0.3152(3) 0.9928(3) 0.0409(12) Uani 1 1 d . . . C10 C 0.6227(2) 0.2402(3) 0.9461(3) 0.0343(11) Uani 1 1 d . . . C3 C 0.7688(3) -0.0811(4) 1.0402(3) 0.0604(16) Uani 1 1 d . . . H3A H 0.7893 -0.1258 1.0203 0.073 Uiso 1 1 calc R . . C9 C 0.6005(2) 0.2340(3) 0.8579(3) 0.0384(12) Uani 1 1 d . . . H9A H 0.5725 0.2746 0.8261 0.046 Uiso 1 1 calc R . . C21 C 0.5689(3) 0.0942(3) 0.6788(3) 0.0441(13) Uani 1 1 d . . . H21A H 0.5597 0.0519 0.7124 0.053 Uiso 1 1 calc R . . C2 C 0.7675(3) -0.0749(4) 1.1251(3) 0.0627(17) Uani 1 1 d . . . H2A H 0.7860 -0.1156 1.1638 0.075 Uiso 1 1 calc R . . C20 C 0.5494(3) 0.0863(3) 0.5900(3) 0.0472(14) Uani 1 1 d . . . H20A H 0.5267 0.0398 0.5648 0.057 Uiso 1 1 calc R . . C4 C 0.7394(3) -0.0207(3) 0.9848(3) 0.0491(14) Uani 1 1 d . . . H4A H 0.7404 -0.0241 0.9272 0.059 Uiso 1 1 calc R . . O1W O 0.3910(3) 0.2605(3) 0.2502(3) 0.0817(14) Uani 1 1 d . . . H1WA H 0.3593 0.2488 0.2039 0.123 Uiso 1 1 d R . . H1WB H 0.4259 0.2865 0.2365 0.123 Uiso 1 1 d R . . C15 C 0.6335(4) 0.3833(4) 1.1183(4) 0.0655(17) Uani 1 1 d . . . H15A H 0.6492 0.3834 1.1780 0.079 Uiso 1 1 calc R . . C1 C 0.7388(3) -0.0078(4) 1.1509(3) 0.0566(15) Uani 1 1 d . . . H1A H 0.7403 -0.0027 1.2091 0.068 Uiso 1 1 calc R . . C14 C 0.6091(3) 0.4534(4) 1.0798(4) 0.0667(17) Uani 1 1 d . . . H14A H 0.6087 0.4995 1.1120 0.080 Uiso 1 1 calc R . . C12 C 0.5885(4) 0.3843(4) 0.9482(4) 0.0696(18) Uani 1 1 d . . . H12A H 0.5736 0.3837 0.8885 0.084 Uiso 1 1 calc R . . O4 O 0.45925(18) 0.1269(3) 0.4035(2) 0.0737(14) Uani 1 1 d . . . O6 O 0.57593(19) 0.0726(3) 0.4001(2) 0.0646(12) Uani 1 1 d . . . C19 C 0.5641(2) 0.1482(3) 0.5389(3) 0.0370(11) Uani 1 1 d . . . O5 O 0.5601(3) 0.2150(3) 0.3939(2) 0.0931(17) Uani 1 1 d . . . C17 C 0.6163(2) 0.2250(3) 0.6660(3) 0.0346(11) Uani 1 1 d . . . O1 O 0.71836(17) 0.2973(2) 0.78107(19) 0.0500(10) Uani 1 1 d . . . O3 O 0.6909(2) 0.3485(2) 0.6360(2) 0.0588(11) Uani 1 1 d . . . O2 O 0.6036(2) 0.3689(2) 0.7245(2) 0.0596(11) Uani 1 1 d . . . C13 C 0.5854(4) 0.4545(4) 0.9930(4) 0.0690(17) Uani 1 1 d . . . H13A H 0.5674 0.5012 0.9642 0.083 Uiso 1 1 calc R . . O4W O 0.5000 0.4831(4) 0.7500 0.102(2) Uani 1 2 d S . . H4WA H 0.5362 0.4605 0.7353 0.152 Uiso 0.50 1 d PR . . H4WB H 0.4610 0.4563 0.7280 0.152 Uiso 0.50 1 d PR . . O3W O 0.4897(9) 0.3651(8) 0.1914(9) 0.326(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 Ca1 0.0359(5) 0.0481(7) 0.0272(5) 0.0009(4) 0.0048(4) 0.0053(4) S1 0.0437(7) 0.0435(8) 0.0334(7) 0.0025(6) 0.0044(5) -0.0095(6) S2 0.0420(7) 0.0626(10) 0.0260(6) 0.0013(6) 0.0052(5) 0.0010(6) N2 0.040(2) 0.038(2) 0.028(2) 0.0016(18) 0.0111(16) -0.0027(18) O2W 0.054(2) 0.071(3) 0.044(2) -0.011(2) 0.0181(16) 0.003(2) C16 0.036(2) 0.049(3) 0.027(2) -0.001(2) 0.0053(19) -0.003(2) C6 0.036(2) 0.043(3) 0.025(2) 0.005(2) 0.0061(18) -0.004(2) C7 0.047(3) 0.040(3) 0.029(2) -0.003(2) 0.011(2) -0.007(2) N1 0.049(2) 0.052(3) 0.026(2) -0.0018(19) 0.0078(17) 0.000(2) C18 0.035(2) 0.049(3) 0.032(3) 0.011(2) 0.0064(19) -0.002(2) C8 0.035(2) 0.041(3) 0.028(2) 0.000(2) 0.0096(18) -0.008(2) C5 0.041(2) 0.036(3) 0.028(2) -0.001(2) 0.0053(19) -0.005(2) N3 0.067(3) 0.051(3) 0.032(2) -0.007(2) 0.011(2) 0.001(2) C11 0.047(3) 0.040(3) 0.035(3) -0.005(2) 0.011(2) 0.000(2) C10 0.034(2) 0.039(3) 0.031(2) 0.004(2) 0.0093(18) -0.005(2) C3 0.079(4) 0.055(4) 0.045(3) -0.005(3) 0.011(3) 0.027(3) C9 0.041(2) 0.043(3) 0.031(3) 0.002(2) 0.0099(19) 0.000(2) C21 0.050(3) 0.048(3) 0.033(3) 0.001(2) 0.006(2) -0.011(2) C2 0.084(4) 0.060(4) 0.040(3) 0.006(3) 0.008(3) 0.026(3) C20 0.063(3) 0.054(4) 0.022(2) -0.010(2) 0.004(2) -0.009(3) C4 0.060(3) 0.054(4) 0.031(3) -0.002(3) 0.007(2) 0.011(3) O1W 0.111(4) 0.084(4) 0.065(3) -0.012(3) 0.051(3) -0.029(3) C15 0.103(5) 0.052(4) 0.041(3) -0.008(3) 0.018(3) -0.007(4) C1 0.074(4) 0.064(4) 0.031(3) 0.006(3) 0.010(3) 0.021(3) C14 0.093(5) 0.049(4) 0.062(4) -0.011(3) 0.026(3) -0.001(4) C12 0.099(5) 0.056(4) 0.049(3) 0.005(3) 0.007(3) 0.019(4) O4 0.039(2) 0.139(4) 0.038(2) -0.006(2) -0.0004(15) 0.015(2) O6 0.060(2) 0.087(3) 0.046(2) -0.006(2) 0.0109(17) 0.021(2) C19 0.036(2) 0.050(3) 0.025(2) 0.001(2) 0.0078(19) -0.001(2) O5 0.157(5) 0.082(4) 0.039(2) 0.000(2) 0.021(3) -0.044(3) C17 0.033(2) 0.042(3) 0.028(2) 0.002(2) 0.0051(18) 0.000(2) O1 0.0418(18) 0.068(3) 0.0350(18) 0.0075(18) -0.0011(14) -0.0183(18) O3 0.068(2) 0.071(3) 0.037(2) 0.0122(19) 0.0121(17) -0.029(2) O2 0.067(2) 0.046(3) 0.065(3) -0.002(2) 0.0152(19) 0.012(2) C13 0.099(5) 0.046(4) 0.059(4) 0.003(3) 0.013(3) 0.011(4) O4W 0.090(5) 0.082(6) 0.142(7) 0.000 0.045(5) 0.000 O3W 0.278(16) 0.257(13) 0.45(3) 0.024(12) 0.11(2) 0.004(12) _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 Ca1 O4 2.307(4) . ? Ca1 O1 2.326(4) 8_455 ? Ca1 O1W 2.399(4) . ? Ca1 O2W 2.441(4) . ? Ca1 N2 2.521(4) 2_656 ? Ca1 N3 2.558(5) 2_656 ? Ca1 N1 2.548(5) 2_656 ? Ca1 H1WA 2.6574 . ? S1 O2 1.450(4) . ? S1 O3 1.445(4) . ? S1 O1 1.461(3) . ? S1 C17 1.799(5) . ? S2 O5 1.425(5) . ? S2 O4 1.441(4) . ? S2 O6 1.449(4) . ? S2 C19 1.781(5) . ? N2 C6 1.348(6) . ? N2 C10 1.368(6) . ? N2 Ca1 2.521(4) 2_656 ? O2W H2WA 0.8441 . ? O2W H2WB 0.8525 . ? C16 C21 1.403(7) . ? C16 C17 1.407(7) . ? C16 C8 1.497(6) . ? C6 C7 1.397(6) . ? C6 C5 1.498(6) . ? C7 C8 1.385(7) . ? C7 H7A 0.9300 . ? N1 C5 1.354(5) . ? N1 C1 1.349(6) . ? N1 Ca1 2.548(5) 2_656 ? C18 C19 1.375(7) . ? C18 C17 1.388(6) . ? C18 H18A 0.9300 . ? C8 C9 1.390(7) . ? C5 C4 1.383(7) . ? N3 C11 1.335(6) . ? N3 C15 1.330(7) . ? N3 Ca1 2.558(5) 2_656 ? C11 C12 1.382(8) . ? C11 C10 1.491(7) . ? C10 C9 1.379(6) . ? C3 C4 1.370(7) . ? C3 C2 1.370(7) . ? C3 H3A 0.9300 . ? C9 H9A 0.9300 . ? C21 C20 1.389(6) . ? C21 H21A 0.9300 . ? C2 C1 1.350(8) . ? C2 H2A 0.9300 . ? C20 C19 1.387(7) . ? C20 H20A 0.9300 . ? C4 H4A 0.9300 . ? O1W H1WA 0.8517 . ? O1W H1WB 0.8505 . ? C15 C14 1.352(8) . ? C15 H15A 0.9300 . ? C1 H1A 0.9300 . ? C14 C13 1.355(8) . ? C14 H14A 0.9300 . ? C12 C13 1.385(8) . ? C12 H12A 0.9300 . ? O1 Ca1 2.326(4) 8_556 ? C13 H13A 0.9300 . ? O4W H4WA 0.8520 . ? O4W H4WB 0.8523 . ? O3W O3W 1.82(3) 2_655 ? 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 Ca1 O1 167.89(16) . 8_455 ? O4 Ca1 O1W 90.43(17) . . ? O1 Ca1 O1W 95.23(16) 8_455 . ? O4 Ca1 O2W 89.96(14) . . ? O1 Ca1 O2W 81.29(12) 8_455 . ? O1W Ca1 O2W 74.51(15) . . ? O4 Ca1 N2 80.17(12) . 2_656 ? O1 Ca1 N2 102.53(12) 8_455 2_656 ? O1W Ca1 N2 137.16(15) . 2_656 ? O2W Ca1 N2 146.21(14) . 2_656 ? O4 Ca1 N3 97.32(16) . 2_656 ? O1 Ca1 N3 94.45(14) 8_455 2_656 ? O1W Ca1 N3 75.85(15) . 2_656 ? O2W Ca1 N3 149.49(14) . 2_656 ? N2 Ca1 N3 64.27(14) 2_656 2_656 ? O4 Ca1 N1 86.59(16) . 2_656 ? O1 Ca1 N1 84.04(14) 8_455 2_656 ? O1W Ca1 N1 157.16(14) . 2_656 ? O2W Ca1 N1 82.85(14) . 2_656 ? N2 Ca1 N1 64.48(13) 2_656 2_656 ? N3 Ca1 N1 126.99(14) 2_656 2_656 ? O4 Ca1 H1WA 102.3 . . ? O1 Ca1 H1WA 80.8 8_455 . ? O1W Ca1 H1WA 18.5 . . ? O2W Ca1 H1WA 61.0 . . ? N2 Ca1 H1WA 152.7 2_656 . ? N3 Ca1 H1WA 88.5 2_656 . ? N1 Ca1 H1WA 142.4 2_656 . ? O2 S1 O3 113.2(3) . . ? O2 S1 O1 112.6(2) . . ? O3 S1 O1 112.3(2) . . ? O2 S1 C17 106.8(2) . . ? O3 S1 C17 105.7(2) . . ? O1 S1 C17 105.5(2) . . ? O5 S2 O4 114.9(3) . . ? O5 S2 O6 113.4(3) . . ? O4 S2 O6 109.4(3) . . ? O5 S2 C19 105.6(2) . . ? O4 S2 C19 105.3(2) . . ? O6 S2 C19 107.6(2) . . ? C6 N2 C10 118.3(4) . . ? C6 N2 Ca1 121.1(3) . 2_656 ? C10 N2 Ca1 118.1(3) . 2_656 ? Ca1 O2W H2WA 141.8 . . ? Ca1 O2W H2WB 110.2 . . ? H2WA O2W H2WB 108.0 . . ? C21 C16 C17 116.3(4) . . ? C21 C16 C8 118.7(4) . . ? C17 C16 C8 125.0(4) . . ? N2 C6 C7 121.5(4) . . ? N2 C6 C5 115.8(4) . . ? C7 C6 C5 122.7(4) . . ? C8 C7 C6 120.4(5) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C5 N1 C1 117.0(4) . . ? C5 N1 Ca1 120.2(3) . 2_656 ? C1 N1 Ca1 122.7(3) . 2_656 ? C19 C18 C17 121.1(5) . . ? C19 C18 H18A 119.4 . . ? C17 C18 H18A 119.4 . . ? C7 C8 C9 117.3(4) . . ? C7 C8 C16 122.0(4) . . ? C9 C8 C16 120.7(4) . . ? N1 C5 C4 120.7(5) . . ? N1 C5 C6 116.5(4) . . ? C4 C5 C6 122.7(4) . . ? C11 N3 C15 116.4(5) . . ? C11 N3 Ca1 117.8(4) . 2_656 ? C15 N3 Ca1 124.5(4) . 2_656 ? N3 C11 C12 121.7(5) . . ? N3 C11 C10 117.3(5) . . ? C12 C11 C10 120.7(5) . . ? C9 C10 N2 121.6(5) . . ? C9 C10 C11 122.4(4) . . ? N2 C10 C11 115.9(4) . . ? C4 C3 C2 119.2(5) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C10 C9 C8 120.5(5) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C20 C21 C16 122.5(5) . . ? C20 C21 H21A 118.8 . . ? C16 C21 H21A 118.8 . . ? C1 C2 C3 118.0(5) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C21 C20 C19 119.5(5) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C3 C4 C5 120.2(5) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? Ca1 O1W H1WA 98.2 . . ? Ca1 O1W H1WB 152.3 . . ? H1WA O1W H1WB 107.5 . . ? N3 C15 C14 125.7(6) . . ? N3 C15 H15A 117.2 . . ? C14 C15 H15A 117.2 . . ? C2 C1 N1 124.8(5) . . ? C2 C1 H1A 117.6 . . ? N1 C1 H1A 117.6 . . ? C13 C14 C15 118.1(6) . . ? C13 C14 H14A 120.9 . . ? C15 C14 H14A 120.9 . . ? C11 C12 C13 119.6(6) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? S2 O4 Ca1 146.6(3) . . ? C18 C19 C20 119.4(4) . . ? C18 C19 S2 119.6(4) . . ? C20 C19 S2 120.9(4) . . ? C18 C17 C16 121.1(4) . . ? C18 C17 S1 115.1(4) . . ? C16 C17 S1 123.8(3) . . ? S1 O1 Ca1 141.8(2) . 8_556 ? C14 C13 C12 118.5(6) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? H4WA O4W H4WB 107.3 . . ? 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 C10 N2 C6 C7 2.9(6) . . . . ? Ca1 N2 C6 C7 164.9(3) 2_656 . . . ? C10 N2 C6 C5 -178.2(4) . . . . ? Ca1 N2 C6 C5 -16.3(5) 2_656 . . . ? N2 C6 C7 C8 -3.7(7) . . . . ? C5 C6 C7 C8 177.6(4) . . . . ? C6 C7 C8 C9 -0.7(6) . . . . ? C6 C7 C8 C16 179.2(4) . . . . ? C21 C16 C8 C7 47.3(6) . . . . ? C17 C16 C8 C7 -132.3(5) . . . . ? C21 C16 C8 C9 -132.8(5) . . . . ? C17 C16 C8 C9 47.7(6) . . . . ? C1 N1 C5 C4 -0.5(7) . . . . ? Ca1 N1 C5 C4 176.1(3) 2_656 . . . ? C1 N1 C5 C6 178.5(4) . . . . ? Ca1 N1 C5 C6 -4.9(5) 2_656 . . . ? N2 C6 C5 N1 13.6(6) . . . . ? C7 C6 C5 N1 -167.5(4) . . . . ? N2 C6 C5 C4 -167.4(4) . . . . ? C7 C6 C5 C4 11.4(7) . . . . ? C15 N3 C11 C12 1.0(8) . . . . ? Ca1 N3 C11 C12 168.2(4) 2_656 . . . ? C15 N3 C11 C10 175.3(5) . . . . ? Ca1 N3 C11 C10 -17.5(6) 2_656 . . . ? C6 N2 C10 C9 2.1(6) . . . . ? Ca1 N2 C10 C9 -160.3(3) 2_656 . . . ? C6 N2 C10 C11 -175.0(4) . . . . ? Ca1 N2 C10 C11 22.5(5) 2_656 . . . ? N3 C11 C10 C9 179.8(4) . . . . ? C12 C11 C10 C9 -5.8(7) . . . . ? N3 C11 C10 N2 -3.1(6) . . . . ? C12 C11 C10 N2 171.4(5) . . . . ? N2 C10 C9 C8 -6.6(7) . . . . ? C11 C10 C9 C8 170.4(4) . . . . ? C7 C8 C9 C10 5.7(7) . . . . ? C16 C8 C9 C10 -174.3(4) . . . . ? C17 C16 C21 C20 -1.6(7) . . . . ? C8 C16 C21 C20 178.8(4) . . . . ? C4 C3 C2 C1 -1.7(9) . . . . ? C16 C21 C20 C19 1.3(8) . . . . ? C2 C3 C4 C5 -0.7(9) . . . . ? N1 C5 C4 C3 1.8(8) . . . . ? C6 C5 C4 C3 -177.2(5) . . . . ? C11 N3 C15 C14 -0.5(10) . . . . ? Ca1 N3 C15 C14 -166.8(5) 2_656 . . . ? C3 C2 C1 N1 3.1(10) . . . . ? C5 N1 C1 C2 -2.0(8) . . . . ? Ca1 N1 C1 C2 -178.6(5) 2_656 . . . ? N3 C15 C14 C13 0.7(11) . . . . ? N3 C11 C12 C13 -1.5(9) . . . . ? C10 C11 C12 C13 -175.7(5) . . . . ? O5 S2 O4 Ca1 -8.4(5) . . . . ? O6 S2 O4 Ca1 -137.2(4) . . . . ? C19 S2 O4 Ca1 107.4(4) . . . . ? O1 Ca1 O4 S2 150.1(5) 8_455 . . . ? O1W Ca1 O4 S2 32.1(4) . . . . ? O2W Ca1 O4 S2 106.6(4) . . . . ? N2 Ca1 O4 S2 -105.9(4) 2_656 . . . ? N3 Ca1 O4 S2 -43.7(4) 2_656 . . . ? N1 Ca1 O4 S2 -170.5(4) 2_656 . . . ? C17 C18 C19 C20 0.8(7) . . . . ? C17 C18 C19 S2 178.6(3) . . . . ? C21 C20 C19 C18 -0.9(7) . . . . ? C21 C20 C19 S2 -178.6(4) . . . . ? O5 S2 C19 C18 1.1(5) . . . . ? O4 S2 C19 C18 -120.9(4) . . . . ? O6 S2 C19 C18 122.5(4) . . . . ? O5 S2 C19 C20 178.8(4) . . . . ? O4 S2 C19 C20 56.9(5) . . . . ? O6 S2 C19 C20 -59.7(5) . . . . ? C19 C18 C17 C16 -1.1(7) . . . . ? C19 C18 C17 S1 178.6(4) . . . . ? C21 C16 C17 C18 1.4(7) . . . . ? C8 C16 C17 C18 -179.0(4) . . . . ? C21 C16 C17 S1 -178.2(3) . . . . ? C8 C16 C17 S1 1.4(7) . . . . ? O2 S1 C17 C18 98.9(4) . . . . ? O3 S1 C17 C18 -21.9(4) . . . . ? O1 S1 C17 C18 -141.1(3) . . . . ? O2 S1 C17 C16 -81.5(4) . . . . ? O3 S1 C17 C16 157.7(4) . . . . ? O1 S1 C17 C16 38.5(4) . . . . ? O2 S1 O1 Ca1 -109.4(4) . . . 8_556 ? O3 S1 O1 Ca1 19.8(5) . . . 8_556 ? C17 S1 O1 Ca1 134.5(4) . . . 8_556 ? C15 C14 C13 C12 -1.2(10) . . . . ? C11 C12 C13 C14 1.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.586 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 958306' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3Pb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H19 N3 O9 Pb S2' _chemical_formula_weight 728.70 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9535(11) _cell_length_b 11.4510(14) _cell_length_c 12.3912(15) _cell_angle_alpha 69.024(2) _cell_angle_beta 81.056(2) _cell_angle_gamma 79.498(2) _cell_volume 1160.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 7.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1532 _exptl_absorpt_correction_T_max 0.2117 _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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6425 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4455 _reflns_number_gt 3468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4455 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 S2 S 0.9636(2) 1.1041(2) 1.73321(18) 0.0395(5) Uani 1 1 d . . . S1 S 0.5103(2) 1.46591(19) 1.78798(17) 0.0345(5) Uani 1 1 d . . . N2 N 1.2251(7) 1.2510(5) 1.2886(5) 0.0274(14) Uani 1 1 d . . . C19 C 0.6531(8) 1.4156(7) 1.6914(6) 0.0277(17) Uani 1 1 d . . . C18 C 0.7472(8) 1.3013(7) 1.7362(6) 0.0292(17) Uani 1 1 d . . . H18A H 0.7319 1.2535 1.8144 0.035 Uiso 1 1 calc R . . C16 C 0.8863(8) 1.3309(7) 1.5464(6) 0.0296(17) Uani 1 1 d . . . C6 C 1.2636(8) 1.2311(7) 1.3956(7) 0.0313(18) Uani 1 1 d . . . O6 O 0.8724(7) 1.0511(5) 1.8438(5) 0.0507(16) Uani 1 1 d . . . C7 C 1.1556(9) 1.2533(7) 1.4815(6) 0.0310(17) Uani 1 1 d . . . H7A H 1.1851 1.2388 1.5544 0.037 Uiso 1 1 calc R . . C21 C 0.7870(9) 1.4428(7) 1.5044(6) 0.0357(19) Uani 1 1 d . . . H21A H 0.7996 1.4912 1.4261 0.043 Uiso 1 1 calc R . . N1 N 1.5209(7) 1.1661(6) 1.3274(6) 0.0358(16) Uani 1 1 d . . . C10 C 1.0773(9) 1.2916(7) 1.2666(6) 0.0314(18) Uani 1 1 d . . . C12 C 0.8933(10) 1.3471(8) 1.1162(7) 0.044(2) Uani 1 1 d . . . H12A H 0.8131 1.3630 1.1687 0.053 Uiso 1 1 calc R . . O5 O 1.1118(7) 1.1253(6) 1.7496(5) 0.0597(18) Uani 1 1 d . . . C20 C 0.6701(9) 1.4842(7) 1.5758(6) 0.0320(18) Uani 1 1 d . . . H20A H 0.6042 1.5580 1.5450 0.038 Uiso 1 1 calc R . . N3 N 1.1591(8) 1.2890(7) 1.0734(6) 0.0451(18) Uani 1 1 d . . . C4 C 1.4800(9) 1.1618(7) 1.5212(7) 0.0384(19) Uani 1 1 d . . . H4A H 1.4134 1.1746 1.5827 0.046 Uiso 1 1 calc R . . C1 C 1.6688(9) 1.1225(7) 1.3421(8) 0.042(2) Uani 1 1 d . . . H1A H 1.7336 1.1083 1.2804 0.051 Uiso 1 1 calc R . . C17 C 0.8617(8) 1.2587(7) 1.6664(6) 0.0315(18) Uani 1 1 d . . . O4 O 0.9700(7) 1.0367(5) 1.6546(5) 0.0536(16) Uani 1 1 d . . . C9 C 0.9672(9) 1.3148(7) 1.3495(6) 0.0315(18) Uani 1 1 d . . . H9A H 0.8668 1.3428 1.3317 0.038 Uiso 1 1 calc R . . C11 C 1.0420(9) 1.3107(7) 1.1479(7) 0.0338(18) Uani 1 1 d . . . C5 C 1.4249(8) 1.1867(7) 1.4165(7) 0.0326(18) Uani 1 1 d . . . O1 O 0.5873(7) 1.5317(6) 1.8402(5) 0.0540(16) Uani 1 1 d . . . O2 O 0.4656(7) 1.3529(6) 1.8745(5) 0.0592(18) Uani 1 1 d . . . O1W O 1.3901(9) 1.0408(7) 1.1568(7) 0.082(2) Uani 1 1 d . . . H1WA H 1.3202 1.0520 1.1134 0.123 Uiso 1 1 d R . . H1WB H 1.3519 1.0126 1.2269 0.123 Uiso 1 1 d R . . O3 O 0.3942(7) 1.5482(6) 1.7184(5) 0.0639(19) Uani 1 1 d . . . C8 C 1.0041(9) 1.2968(7) 1.4608(6) 0.0317(18) Uani 1 1 d . . . C2 C 1.7275(10) 1.0981(7) 1.4456(8) 0.045(2) Uani 1 1 d . . . H2A H 1.8305 1.0685 1.4533 0.054 Uiso 1 1 calc R . . C3 C 1.6324(10) 1.1181(8) 1.5371(8) 0.045(2) Uani 1 1 d . . . H3A H 1.6691 1.1027 1.6078 0.054 Uiso 1 1 calc R . . C13 C 0.8672(11) 1.3591(9) 1.0055(8) 0.053(2) Uani 1 1 d . . . H13A H 0.7686 1.3822 0.9830 0.064 Uiso 1 1 calc R . . C15 C 1.1283(13) 1.3004(11) 0.9661(8) 0.073(3) Uani 1 1 d . . . H15A H 1.2086 1.2822 0.9147 0.088 Uiso 1 1 calc R . . C14 C 0.9861(12) 1.3371(11) 0.9299(9) 0.068(3) Uani 1 1 d . . . H14A H 0.9707 1.3468 0.8544 0.081 Uiso 1 1 calc R . . O3W O 0.7279(10) 2.0656(10) 1.0698(7) 0.128(4) Uani 1 1 d . . . H3WA H 0.7779 2.0539 1.0096 0.192 Uiso 1 1 d R . . H3WB H 0.6370 2.0548 1.0718 0.192 Uiso 1 1 d R . . O2W O 1.5839(15) 0.8343(14) 1.2126(14) 0.214(7) Uani 1 1 d . . . H2WA H 1.6323 0.7629 1.2135 0.321 Uiso 1 1 d R . . H2WB H 1.6462 0.8765 1.2223 0.321 Uiso 1 1 d R . . Pb1 Pb 1.42982(4) 1.25231(3) 1.12675(3) 0.03749(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S2 0.0304(12) 0.0467(12) 0.0338(11) -0.0125(10) -0.0048(9) 0.0124(9) S1 0.0268(11) 0.0426(12) 0.0326(11) -0.0171(9) 0.0055(8) 0.0009(9) N2 0.022(3) 0.035(3) 0.021(3) -0.010(3) 0.004(3) -0.001(3) C19 0.015(4) 0.040(4) 0.028(4) -0.018(4) 0.002(3) 0.004(3) C18 0.017(4) 0.040(4) 0.027(4) -0.011(3) 0.000(3) 0.001(3) C16 0.022(4) 0.043(5) 0.026(4) -0.014(4) 0.000(3) -0.005(3) C6 0.023(4) 0.036(4) 0.036(5) -0.018(4) 0.003(3) 0.002(3) O6 0.047(4) 0.052(4) 0.037(3) -0.006(3) 0.004(3) 0.010(3) C7 0.031(5) 0.036(4) 0.027(4) -0.014(3) -0.001(3) -0.004(3) C21 0.034(5) 0.045(5) 0.022(4) -0.008(4) 0.001(3) 0.002(4) N1 0.022(4) 0.039(4) 0.042(4) -0.016(3) -0.002(3) 0.008(3) C10 0.029(4) 0.036(4) 0.031(4) -0.015(4) -0.003(3) -0.002(3) C12 0.032(5) 0.061(6) 0.034(5) -0.014(4) -0.009(4) 0.004(4) O5 0.030(4) 0.086(5) 0.049(4) -0.010(4) -0.016(3) 0.010(3) C20 0.029(4) 0.032(4) 0.029(4) -0.009(3) 0.000(3) 0.003(3) N3 0.034(4) 0.070(5) 0.035(4) -0.025(4) 0.003(3) -0.010(4) C4 0.032(5) 0.043(5) 0.043(5) -0.018(4) -0.006(4) -0.001(4) C1 0.034(5) 0.036(5) 0.052(6) -0.015(4) 0.003(4) 0.003(4) C17 0.021(4) 0.040(4) 0.031(4) -0.014(4) -0.005(3) 0.007(3) O4 0.064(4) 0.045(4) 0.049(4) -0.021(3) -0.003(3) 0.009(3) C9 0.027(4) 0.036(4) 0.033(4) -0.017(4) 0.003(3) -0.002(3) C11 0.030(5) 0.041(5) 0.035(5) -0.020(4) 0.000(4) -0.004(3) C5 0.024(4) 0.031(4) 0.044(5) -0.020(4) -0.001(4) 0.005(3) O1 0.053(4) 0.056(4) 0.065(4) -0.038(3) -0.006(3) 0.000(3) O2 0.052(4) 0.055(4) 0.059(4) -0.019(3) 0.030(3) -0.007(3) O1W 0.084(6) 0.072(5) 0.103(6) -0.041(5) -0.004(5) -0.020(4) O3 0.042(4) 0.090(5) 0.050(4) -0.028(4) -0.012(3) 0.033(3) C8 0.030(4) 0.035(4) 0.031(4) -0.011(3) 0.002(3) -0.008(3) C2 0.030(5) 0.035(5) 0.063(6) -0.011(4) -0.004(4) -0.001(4) C3 0.035(5) 0.054(6) 0.047(5) -0.013(4) -0.012(4) -0.007(4) C13 0.039(6) 0.076(7) 0.041(5) -0.018(5) -0.007(4) -0.001(5) C15 0.062(8) 0.135(11) 0.038(6) -0.047(7) 0.009(5) -0.025(7) C14 0.056(7) 0.112(9) 0.045(6) -0.030(6) -0.014(5) -0.024(6) O3W 0.080(7) 0.205(11) 0.062(5) -0.029(6) -0.005(5) 0.037(7) O2W 0.130(11) 0.258(16) 0.32(2) -0.207(16) 0.083(11) -0.060(11) Pb1 0.02995(19) 0.0481(2) 0.03569(19) -0.01973(15) 0.00615(13) -0.00499(13) _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 S2 O4 1.433(6) . ? S2 O5 1.448(6) . ? S2 O6 1.466(6) . ? S2 C17 1.802(7) . ? S1 O2 1.430(6) . ? S1 O3 1.432(6) . ? S1 O1 1.462(6) . ? S1 C19 1.774(7) . ? N2 C6 1.351(9) . ? N2 C10 1.356(9) . ? N2 Pb1 2.495(5) . ? C19 C20 1.365(10) . ? C19 C18 1.398(10) . ? C18 C17 1.371(10) . ? C18 H18A 0.9300 . ? C16 C21 1.398(10) . ? C16 C17 1.424(10) . ? C16 C8 1.479(10) . ? C6 C7 1.386(10) . ? C6 C5 1.471(10) . ? C7 C8 1.387(10) . ? C7 H7A 0.9300 . ? C21 C20 1.390(10) . ? C21 H21A 0.9300 . ? N1 C1 1.343(10) . ? N1 C5 1.353(9) . ? N1 Pb1 2.530(6) . ? C10 C9 1.372(10) . ? C10 C11 1.483(10) . ? C12 C13 1.382(11) . ? C12 C11 1.394(11) . ? C12 H12A 0.9300 . ? C20 H20A 0.9300 . ? N3 C11 1.335(10) . ? N3 C15 1.355(11) . ? N3 Pb1 2.533(7) . ? C4 C3 1.383(11) . ? C4 C5 1.375(11) . ? C4 H4A 0.9300 . ? C1 C2 1.379(12) . ? C1 H1A 0.9300 . ? C9 C8 1.403(10) . ? C9 H9A 0.9300 . ? O1 Pb1 2.622(6) 2_788 ? O1W Pb1 2.400(7) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? C2 C3 1.370(12) . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C13 C14 1.355(13) . ? C13 H13A 0.9300 . ? C15 C14 1.359(14) . ? C15 H15A 0.9300 . ? C14 H14A 0.9300 . ? O3W H3WA 0.8486 . ? O3W H3WB 0.8409 . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8483 . ? Pb1 O1 2.622(6) 2_788 ? 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 S2 O5 113.7(4) . . ? O4 S2 O6 113.4(4) . . ? O5 S2 O6 112.2(4) . . ? O4 S2 C17 106.3(3) . . ? O5 S2 C17 105.7(4) . . ? O6 S2 C17 104.6(3) . . ? O2 S1 O3 116.4(4) . . ? O2 S1 O1 109.8(4) . . ? O3 S1 O1 112.5(4) . . ? O2 S1 C19 105.8(4) . . ? O3 S1 C19 106.3(4) . . ? O1 S1 C19 105.2(4) . . ? C6 N2 C10 118.8(6) . . ? C6 N2 Pb1 119.5(4) . . ? C10 N2 Pb1 120.6(5) . . ? C20 C19 C18 120.1(7) . . ? C20 C19 S1 121.6(6) . . ? C18 C19 S1 118.2(6) . . ? C17 C18 C19 121.0(7) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C21 C16 C17 117.1(7) . . ? C21 C16 C8 116.7(7) . . ? C17 C16 C8 126.2(7) . . ? N2 C6 C7 121.1(7) . . ? N2 C6 C5 117.4(6) . . ? C7 C6 C5 121.4(7) . . ? C8 C7 C6 121.2(7) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C20 C21 C16 122.3(7) . . ? C20 C21 H21A 118.9 . . ? C16 C21 H21A 118.9 . . ? C1 N1 C5 119.6(7) . . ? C1 N1 Pb1 120.8(5) . . ? C5 N1 Pb1 118.4(5) . . ? N2 C10 C9 121.7(7) . . ? N2 C10 C11 116.3(6) . . ? C9 C10 C11 122.1(7) . . ? C13 C12 C11 118.9(8) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C19 C20 C21 119.4(7) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C11 N3 C15 117.7(8) . . ? C11 N3 Pb1 119.9(5) . . ? C15 N3 Pb1 122.0(6) . . ? C3 C4 C5 121.5(8) . . ? C3 C4 H4A 119.3 . . ? C5 C4 H4A 119.3 . . ? N1 C1 C2 122.1(8) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C18 C17 C16 120.1(7) . . ? C18 C17 S2 116.0(6) . . ? C16 C17 S2 123.6(5) . . ? C10 C9 C8 120.8(7) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? N3 C11 C12 121.5(7) . . ? N3 C11 C10 116.8(7) . . ? C12 C11 C10 121.7(7) . . ? N1 C5 C4 119.4(7) . . ? N1 C5 C6 116.9(7) . . ? C4 C5 C6 123.7(7) . . ? S1 O1 Pb1 142.1(4) . 2_788 ? Pb1 O1W H1WA 102.9 . . ? Pb1 O1W H1WB 105.2 . . ? H1WA O1W H1WB 107.7 . . ? C7 C8 C9 116.3(7) . . ? C7 C8 C16 123.5(7) . . ? C9 C8 C16 120.1(7) . . ? C3 C2 C1 119.2(8) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 118.0(8) . . ? C2 C3 H3A 121.0 . . ? C4 C3 H3A 121.0 . . ? C14 C13 C12 119.6(9) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C14 C15 N3 123.4(10) . . ? C14 C15 H15A 118.3 . . ? N3 C15 H15A 118.3 . . ? C15 C14 C13 118.9(9) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? H3WA O3W H3WB 108.7 . . ? H2WA O2W H2WB 107.9 . . ? O1W Pb1 N2 87.3(2) . . ? O1W Pb1 N1 86.7(2) . . ? N2 Pb1 N1 65.1(2) . . ? O1W Pb1 N3 78.9(3) . . ? N2 Pb1 N3 64.5(2) . . ? N1 Pb1 N3 128.0(2) . . ? O1W Pb1 O1 160.5(2) . 2_788 ? N2 Pb1 O1 73.59(19) . 2_788 ? N1 Pb1 O1 82.2(2) . 2_788 ? N3 Pb1 O1 95.4(2) . 2_788 ? 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 O2 S1 C19 C20 147.5(7) . . . . ? O3 S1 C19 C20 23.2(8) . . . . ? O1 S1 C19 C20 -96.3(7) . . . . ? O2 S1 C19 C18 -31.1(7) . . . . ? O3 S1 C19 C18 -155.4(6) . . . . ? O1 S1 C19 C18 85.1(7) . . . . ? C20 C19 C18 C17 2.7(11) . . . . ? S1 C19 C18 C17 -178.6(6) . . . . ? C10 N2 C6 C7 -1.1(11) . . . . ? Pb1 N2 C6 C7 167.5(5) . . . . ? C10 N2 C6 C5 179.8(7) . . . . ? Pb1 N2 C6 C5 -11.6(9) . . . . ? N2 C6 C7 C8 0.0(11) . . . . ? C5 C6 C7 C8 179.1(7) . . . . ? C17 C16 C21 C20 0.9(12) . . . . ? C8 C16 C21 C20 179.1(7) . . . . ? C6 N2 C10 C9 1.2(11) . . . . ? Pb1 N2 C10 C9 -167.3(5) . . . . ? C6 N2 C10 C11 -179.5(7) . . . . ? Pb1 N2 C10 C11 12.0(9) . . . . ? C18 C19 C20 C21 -3.5(11) . . . . ? S1 C19 C20 C21 177.9(6) . . . . ? C16 C21 C20 C19 1.7(12) . . . . ? C5 N1 C1 C2 -0.3(12) . . . . ? Pb1 N1 C1 C2 167.0(6) . . . . ? C19 C18 C17 C16 -0.1(12) . . . . ? C19 C18 C17 S2 -175.2(6) . . . . ? C21 C16 C17 C18 -1.7(11) . . . . ? C8 C16 C17 C18 -179.6(7) . . . . ? C21 C16 C17 S2 173.0(6) . . . . ? C8 C16 C17 S2 -4.9(11) . . . . ? O4 S2 C17 C18 131.9(6) . . . . ? O5 S2 C17 C18 -107.0(6) . . . . ? O6 S2 C17 C18 11.7(7) . . . . ? O4 S2 C17 C16 -43.0(8) . . . . ? O5 S2 C17 C16 78.1(7) . . . . ? O6 S2 C17 C16 -163.2(7) . . . . ? N2 C10 C9 C8 -0.2(12) . . . . ? C11 C10 C9 C8 -179.5(7) . . . . ? C15 N3 C11 C12 -1.6(13) . . . . ? Pb1 N3 C11 C12 171.7(6) . . . . ? C15 N3 C11 C10 177.1(8) . . . . ? Pb1 N3 C11 C10 -9.6(9) . . . . ? C13 C12 C11 N3 0.9(13) . . . . ? C13 C12 C11 C10 -177.8(8) . . . . ? N2 C10 C11 N3 -1.4(10) . . . . ? C9 C10 C11 N3 177.9(7) . . . . ? N2 C10 C11 C12 177.3(7) . . . . ? C9 C10 C11 C12 -3.4(12) . . . . ? C1 N1 C5 C4 -0.5(11) . . . . ? Pb1 N1 C5 C4 -168.1(5) . . . . ? C1 N1 C5 C6 -178.3(7) . . . . ? Pb1 N1 C5 C6 14.0(9) . . . . ? C3 C4 C5 N1 1.2(12) . . . . ? C3 C4 C5 C6 178.8(8) . . . . ? N2 C6 C5 N1 -1.8(10) . . . . ? C7 C6 C5 N1 179.1(7) . . . . ? N2 C6 C5 C4 -179.6(7) . . . . ? C7 C6 C5 C4 1.3(12) . . . . ? O2 S1 O1 Pb1 -121.4(6) . . . 2_788 ? O3 S1 O1 Pb1 9.9(7) . . . 2_788 ? C19 S1 O1 Pb1 125.2(6) . . . 2_788 ? C6 C7 C8 C9 0.9(11) . . . . ? C6 C7 C8 C16 -175.4(7) . . . . ? C10 C9 C8 C7 -0.8(11) . . . . ? C10 C9 C8 C16 175.6(7) . . . . ? C21 C16 C8 C7 135.7(8) . . . . ? C17 C16 C8 C7 -46.4(12) . . . . ? C21 C16 C8 C9 -40.5(10) . . . . ? C17 C16 C8 C9 137.4(8) . . . . ? N1 C1 C2 C3 0.4(12) . . . . ? C1 C2 C3 C4 0.2(12) . . . . ? C5 C4 C3 C2 -1.0(12) . . . . ? C11 C12 C13 C14 -0.9(14) . . . . ? C11 N3 C15 C14 2.5(16) . . . . ? Pb1 N3 C15 C14 -170.7(9) . . . . ? N3 C15 C14 C13 -2.5(18) . . . . ? C12 C13 C14 C15 1.6(16) . . . . ? C6 N2 Pb1 O1W 100.7(5) . . . . ? C10 N2 Pb1 O1W -90.9(6) . . . . ? C6 N2 Pb1 N1 13.1(5) . . . . ? C10 N2 Pb1 N1 -178.5(6) . . . . ? C6 N2 Pb1 N3 179.7(6) . . . . ? C10 N2 Pb1 N3 -11.9(5) . . . . ? C6 N2 Pb1 O1 -75.8(5) . . . 2_788 ? C10 N2 Pb1 O1 92.6(5) . . . 2_788 ? C1 N1 Pb1 O1W 90.0(6) . . . . ? C5 N1 Pb1 O1W -102.5(6) . . . . ? C1 N1 Pb1 N2 178.5(6) . . . . ? C5 N1 Pb1 N2 -14.0(5) . . . . ? C1 N1 Pb1 N3 163.1(5) . . . . ? C5 N1 Pb1 N3 -29.3(7) . . . . ? C1 N1 Pb1 O1 -106.0(6) . . . 2_788 ? C5 N1 Pb1 O1 61.5(6) . . . 2_788 ? C11 N3 Pb1 O1W 103.2(6) . . . . ? C15 N3 Pb1 O1W -83.7(8) . . . . ? C11 N3 Pb1 N2 11.0(6) . . . . ? C15 N3 Pb1 N2 -176.0(8) . . . . ? C11 N3 Pb1 N1 26.4(7) . . . . ? C15 N3 Pb1 N1 -160.5(7) . . . . ? C11 N3 Pb1 O1 -57.9(6) . . . 2_788 ? C15 N3 Pb1 O1 115.1(8) . . . 2_788 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.088 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.165 _database_code_depnum_ccdc_archive 'CCDC 958307' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4Pb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H14 N3 O6.50 Pb S2' _chemical_formula_weight 683.66 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.792(6) _cell_length_b 19.232(7) _cell_length_c 14.198(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.160(5) _cell_angle_gamma 90.00 _cell_volume 4311(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2465 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 22.22 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 8.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2109 _exptl_absorpt_correction_T_max 0.2952 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9026 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3080 _reflns_number_gt 2476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+366.7826P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3080 _refine_ls_number_parameters 303 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2229 _refine_ls_wR_factor_gt 0.2150 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.088 _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 Pb1 Pb -0.14025(5) 0.83200(4) 0.81494(5) 0.0355(3) Uani 1 1 d . . . S1 S -0.1741(4) 0.7124(3) 1.3263(4) 0.0497(15) Uani 1 1 d . . . S2 S -0.0539(3) 0.8829(3) 1.6038(3) 0.0380(13) Uani 1 1 d . . . C1 C -0.0918(18) 0.6585(14) 0.844(2) 0.062(7) Uani 1 1 d . . . H1A H -0.1037 0.6594 0.7795 0.074 Uiso 1 1 calc R . . C2 C -0.054(2) 0.5986(16) 0.884(2) 0.078(9) Uani 1 1 d . . . H2A H -0.0394 0.5609 0.8467 0.094 Uiso 1 1 calc R . . C3 C -0.039(2) 0.5973(14) 0.977(2) 0.071(8) Uani 1 1 d . . . H3A H -0.0224 0.5556 1.0049 0.086 Uiso 1 1 calc R . . C4 C -0.048(2) 0.6535(16) 1.033(2) 0.077(9) Uani 1 1 d U . . H4 H -0.0257 0.6549 1.0939 0.092 Uiso 1 1 calc R . . C5 C -0.0954(13) 0.7149(10) 0.9888(16) 0.038(5) Uani 1 1 d . . . C6 C -0.1203(12) 0.7777(10) 1.0402(13) 0.033(5) Uani 1 1 d . . . C7 C -0.1011(13) 0.7830(11) 1.1369(14) 0.037(5) Uani 1 1 d . . . H7A H -0.0695 0.7487 1.1677 0.044 Uiso 1 1 calc R . . C8 C -0.1313(12) 0.8426(10) 1.1873(13) 0.029(4) Uani 1 1 d . . . C9 C -0.1729(13) 0.8943(11) 1.1350(13) 0.035(5) Uani 1 1 d . . . H9A H -0.1923 0.9341 1.1648 0.042 Uiso 1 1 calc R . . C10 C -0.1855(13) 0.8859(10) 1.0360(13) 0.031(4) Uani 1 1 d . . . C11 C -0.2290(14) 0.9383(10) 0.9764(14) 0.039(5) Uani 1 1 d . . . C12 C -0.2589(15) 1.0037(12) 1.0126(16) 0.049(6) Uani 1 1 d . . . H12A H -0.2501 1.0150 1.0758 0.059 Uiso 1 1 calc R . . C13 C -0.3002(17) 1.0485(14) 0.9536(19) 0.061(7) Uani 1 1 d . . . H13A H -0.3183 1.0913 0.9757 0.073 Uiso 1 1 calc R . . C14 C -0.3156(17) 1.0295(14) 0.857(2) 0.063(7) Uani 1 1 d . . . H14A H -0.3480 1.0573 0.8165 0.076 Uiso 1 1 calc R . . C15 C -0.2793(17) 0.9667(13) 0.8265(18) 0.056(7) Uani 1 1 d . . . H15A H -0.2838 0.9547 0.7632 0.068 Uiso 1 1 calc R . . C16 C -0.1165(13) 0.8495(11) 1.2886(14) 0.035(5) Uani 1 1 d . . . C17 C -0.1301(12) 0.7968(10) 1.3567(14) 0.033(5) Uani 1 1 d . . . C18 C -0.1126(13) 0.8073(10) 1.4511(14) 0.033(5) Uani 1 1 d . . . H18A H -0.1223 0.7722 1.4946 0.040 Uiso 1 1 calc R . . C19 C -0.0799(13) 0.8719(12) 1.4808(14) 0.037(5) Uani 1 1 d . . . C20 C -0.0699(13) 0.9255(11) 1.4191(14) 0.036(5) Uani 1 1 d . . . H20A H -0.0514 0.9689 1.4400 0.044 Uiso 1 1 calc R . . C21 C -0.0879(13) 0.9139(11) 1.3249(14) 0.036(5) Uani 1 1 d . . . H21A H -0.0808 0.9505 1.2830 0.043 Uiso 1 1 calc R . . N1 N -0.1109(12) 0.7135(10) 0.8956(13) 0.044(5) Uani 1 1 d . . . N2 N -0.1626(12) 0.8279(9) 0.9917(11) 0.037(4) Uani 1 1 d . . . N3 N -0.2391(12) 0.9245(9) 0.8853(12) 0.043(5) Uani 1 1 d . . . O1 O -0.0936(11) 0.6694(7) 1.2997(12) 0.050(4) Uani 1 1 d U . . O1W O 0.0000 0.5546(16) 1.2500 0.114(13) Uani 1 2 d S . . O2 O -0.2328(13) 0.7273(11) 1.2476(13) 0.081(7) Uani 1 1 d . . . O3 O -0.2157(14) 0.6884(11) 1.4117(14) 0.080(6) Uani 1 1 d . . . O4 O -0.1209(10) 0.9227(9) 1.6475(10) 0.050(4) Uani 1 1 d . . . O5 O -0.0425(10) 0.8157(8) 1.6443(11) 0.047(4) Uani 1 1 d . . . O6 O 0.0270(9) 0.9182(8) 1.6034(10) 0.046(4) 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 Pb1 0.0336(5) 0.0469(5) 0.0260(5) -0.0025(3) -0.0012(3) -0.0067(4) S1 0.058(4) 0.045(3) 0.046(3) 0.002(3) -0.015(3) -0.022(3) S2 0.039(3) 0.051(3) 0.024(3) -0.004(2) -0.005(2) 0.008(2) C1 0.056(17) 0.072(19) 0.057(17) -0.034(14) -0.001(13) -0.009(14) C2 0.08(2) 0.07(2) 0.09(2) -0.037(17) 0.009(17) 0.021(17) C3 0.09(2) 0.043(15) 0.08(2) -0.013(14) -0.006(17) 0.013(14) C4 0.073(12) 0.080(12) 0.078(12) 0.003(9) 0.001(9) 0.020(9) C5 0.038(12) 0.025(10) 0.050(14) -0.001(9) 0.011(10) 0.003(9) C6 0.033(11) 0.037(11) 0.028(11) -0.002(9) 0.002(9) -0.002(9) C7 0.037(12) 0.036(12) 0.037(12) 0.003(9) -0.003(9) 0.006(9) C8 0.033(11) 0.028(10) 0.026(10) -0.004(8) -0.006(8) 0.003(8) C9 0.033(11) 0.042(12) 0.030(11) -0.011(9) 0.006(9) -0.012(9) C10 0.035(11) 0.029(10) 0.030(11) 0.001(9) -0.007(9) -0.003(9) C11 0.052(13) 0.036(12) 0.029(12) -0.008(9) -0.012(10) -0.015(10) C12 0.054(14) 0.050(14) 0.043(13) 0.009(11) -0.019(11) 0.006(12) C13 0.059(17) 0.063(17) 0.060(17) -0.012(13) -0.003(13) 0.005(13) C14 0.063(18) 0.051(15) 0.075(19) 0.014(14) -0.014(14) 0.004(13) C15 0.074(18) 0.048(14) 0.046(14) 0.008(12) -0.026(13) -0.007(13) C16 0.031(11) 0.044(12) 0.029(11) -0.006(9) 0.007(9) 0.001(9) C17 0.031(11) 0.028(11) 0.040(12) -0.001(9) -0.003(9) -0.010(9) C18 0.038(12) 0.030(10) 0.031(11) 0.003(9) -0.011(9) 0.004(9) C19 0.033(11) 0.052(14) 0.027(11) -0.002(10) -0.001(9) 0.008(10) C20 0.033(11) 0.046(12) 0.030(11) -0.009(10) -0.004(9) -0.004(10) C21 0.039(12) 0.035(11) 0.033(12) 0.002(9) -0.003(9) -0.006(9) N1 0.047(11) 0.047(11) 0.038(11) -0.009(9) -0.010(8) 0.000(9) N2 0.043(11) 0.044(11) 0.023(9) -0.002(8) -0.004(8) -0.002(8) N3 0.055(12) 0.040(10) 0.033(10) 0.000(8) -0.013(9) -0.015(9) O1 0.057(8) 0.023(6) 0.072(8) -0.007(6) 0.006(7) -0.004(6) O1W 0.15(3) 0.052(18) 0.14(3) 0.000 -0.02(3) 0.000 O2 0.081(14) 0.092(15) 0.069(13) 0.015(11) -0.035(11) -0.052(12) O3 0.089(15) 0.080(13) 0.073(14) 0.000(11) 0.032(11) -0.023(12) O4 0.049(9) 0.062(10) 0.039(9) -0.012(7) -0.003(7) 0.016(8) O5 0.054(10) 0.043(9) 0.042(9) 0.000(7) -0.011(7) 0.015(7) O6 0.044(9) 0.055(9) 0.039(9) 0.000(7) -0.014(7) -0.004(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 Pb1 O2 2.457(16) 7_467 ? Pb1 N2 2.542(17) . ? Pb1 N3 2.58(2) . ? Pb1 N1 2.589(19) . ? Pb1 O6 2.684(15) 2_557 ? S1 O2 1.465(18) . ? S1 O3 1.46(2) . ? S1 O1 1.569(18) . ? S1 C17 1.816(19) . ? S2 O5 1.425(16) . ? S2 O6 1.446(16) . ? S2 O4 1.454(16) . ? S2 C19 1.80(2) . ? C1 N1 1.33(3) . ? C1 C2 1.41(4) . ? C1 H1A 0.9300 . ? C2 C3 1.34(4) . ? C2 H2A 0.9300 . ? C3 C4 1.34(4) . ? C3 H3A 0.9300 . ? C4 C5 1.53(4) . ? C4 H4 0.9300 . ? C5 N1 1.34(3) . ? C5 C6 1.47(3) . ? C6 N2 1.35(3) . ? C6 C7 1.40(3) . ? C7 C8 1.44(3) . ? C7 H7A 0.9300 . ? C8 C9 1.40(3) . ? C8 C16 1.46(3) . ? C9 C10 1.43(3) . ? C9 H9A 0.9300 . ? C10 N2 1.33(3) . ? C10 C11 1.48(3) . ? C11 N3 1.33(3) . ? C11 C12 1.44(3) . ? C12 C13 1.36(3) . ? C12 H12A 0.9300 . ? C13 C14 1.43(4) . ? C13 H13A 0.9300 . ? C14 C15 1.41(4) . ? C14 H14A 0.9300 . ? C15 N3 1.32(3) . ? C15 H15A 0.9300 . ? C16 C17 1.42(3) . ? C16 C21 1.41(3) . ? C17 C18 1.38(3) . ? C18 C19 1.41(3) . ? C18 H18A 0.9300 . ? C19 C20 1.36(3) . ? C20 C21 1.38(3) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? O2 Pb1 2.457(16) 7_467 ? O6 Pb1 2.684(15) 2_557 ? 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 O2 Pb1 N2 102.4(6) 7_467 . ? O2 Pb1 N3 87.9(7) 7_467 . ? N2 Pb1 N3 62.7(5) . . ? O2 Pb1 N1 83.6(6) 7_467 . ? N2 Pb1 N1 64.1(5) . . ? N3 Pb1 N1 122.7(6) . . ? O2 Pb1 O6 167.0(7) 7_467 2_557 ? N2 Pb1 O6 72.4(5) . 2_557 ? N3 Pb1 O6 79.1(5) . 2_557 ? N1 Pb1 O6 103.9(5) . 2_557 ? O2 S1 O3 114.0(13) . . ? O2 S1 O1 115.0(12) . . ? O3 S1 O1 114.4(12) . . ? O2 S1 C17 103.9(10) . . ? O3 S1 C17 105.1(11) . . ? O1 S1 C17 102.7(9) . . ? O5 S2 O6 108.8(10) . . ? O5 S2 O4 113.1(10) . . ? O6 S2 O4 113.9(10) . . ? O5 S2 C19 108.1(10) . . ? O6 S2 C19 103.7(9) . . ? O4 S2 C19 108.8(9) . . ? N1 C1 C2 122(3) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C3 C2 C1 118(2) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 123(3) . . ? C2 C3 H3A 118.4 . . ? C4 C3 H3A 118.4 . . ? C3 C4 C5 116(3) . . ? C3 C4 H4 122.0 . . ? C5 C4 H4 122.0 . . ? N1 C5 C4 118(2) . . ? N1 C5 C6 117.4(18) . . ? C4 C5 C6 125(2) . . ? N2 C6 C7 122.8(18) . . ? N2 C6 C5 117.9(17) . . ? C7 C6 C5 119.3(18) . . ? C6 C7 C8 118.4(18) . . ? C6 C7 H7A 120.8 . . ? C8 C7 H7A 120.8 . . ? C9 C8 C16 121.5(17) . . ? C9 C8 C7 117.4(17) . . ? C16 C8 C7 121.0(17) . . ? C8 C9 C10 119.9(18) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? N2 C10 C9 121.7(18) . . ? N2 C10 C11 115.3(17) . . ? C9 C10 C11 122.9(18) . . ? N3 C11 C12 119.3(19) . . ? N3 C11 C10 117.8(19) . . ? C12 C11 C10 122.8(17) . . ? C13 C12 C11 119(2) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C12 C13 C14 120(2) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 117(2) . . ? C15 C14 H14A 121.7 . . ? C13 C14 H14A 121.7 . . ? N3 C15 C14 122(2) . . ? N3 C15 H15A 119.1 . . ? C14 C15 H15A 119.1 . . ? C8 C16 C17 125.7(19) . . ? C8 C16 C21 119.0(18) . . ? C17 C16 C21 115.3(18) . . ? C18 C17 C16 121.9(18) . . ? C18 C17 S1 115.5(15) . . ? C16 C17 S1 122.6(15) . . ? C17 C18 C19 119.1(19) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C20 C19 C18 121.4(18) . . ? C20 C19 S2 120.5(17) . . ? C18 C19 S2 118.0(16) . . ? C19 C20 C21 118(2) . . ? C19 C20 H20A 120.8 . . ? C21 C20 H20A 120.8 . . ? C20 C21 C16 123.7(19) . . ? C20 C21 H21A 118.2 . . ? C16 C21 H21A 118.2 . . ? C5 N1 C1 122(2) . . ? C5 N1 Pb1 116.5(13) . . ? C1 N1 Pb1 119.9(18) . . ? C10 N2 C6 119.4(16) . . ? C10 N2 Pb1 119.0(13) . . ? C6 N2 Pb1 116.5(13) . . ? C11 N3 C15 123(2) . . ? C11 N3 Pb1 117.0(15) . . ? C15 N3 Pb1 117.9(16) . . ? S1 O2 Pb1 133.1(11) . 7_467 ? S2 O6 Pb1 106.9(8) . 2_557 ? 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 C1 C2 C3 2(5) . . . . ? C1 C2 C3 C4 -10(5) . . . . ? C2 C3 C4 C5 14(5) . . . . ? C3 C4 C5 N1 -12(4) . . . . ? C3 C4 C5 C6 172(3) . . . . ? N1 C5 C6 N2 5(3) . . . . ? C4 C5 C6 N2 -180(2) . . . . ? N1 C5 C6 C7 -176.6(19) . . . . ? C4 C5 C6 C7 -1(3) . . . . ? N2 C6 C7 C8 3(3) . . . . ? C5 C6 C7 C8 -175.6(19) . . . . ? C6 C7 C8 C9 -5(3) . . . . ? C6 C7 C8 C16 177.4(19) . . . . ? C16 C8 C9 C10 179.4(18) . . . . ? C7 C8 C9 C10 1(3) . . . . ? C8 C9 C10 N2 4(3) . . . . ? C8 C9 C10 C11 179.8(19) . . . . ? N2 C10 C11 N3 -2(3) . . . . ? C9 C10 C11 N3 -178.4(19) . . . . ? N2 C10 C11 C12 179(2) . . . . ? C9 C10 C11 C12 3(3) . . . . ? N3 C11 C12 C13 3(3) . . . . ? C10 C11 C12 C13 -178(2) . . . . ? C11 C12 C13 C14 2(4) . . . . ? C12 C13 C14 C15 -6(4) . . . . ? C13 C14 C15 N3 5(4) . . . . ? C9 C8 C16 C17 135(2) . . . . ? C7 C8 C16 C17 -47(3) . . . . ? C9 C8 C16 C21 -44(3) . . . . ? C7 C8 C16 C21 134(2) . . . . ? C8 C16 C17 C18 179(2) . . . . ? C21 C16 C17 C18 -3(3) . . . . ? C8 C16 C17 S1 -3(3) . . . . ? C21 C16 C17 S1 175.3(15) . . . . ? O2 S1 C17 C18 145.4(17) . . . . ? O3 S1 C17 C18 25(2) . . . . ? O1 S1 C17 C18 -94.6(17) . . . . ? O2 S1 C17 C16 -33(2) . . . . ? O3 S1 C17 C16 -153.0(18) . . . . ? O1 S1 C17 C16 87.1(18) . . . . ? C16 C17 C18 C19 0(3) . . . . ? S1 C17 C18 C19 -178.7(15) . . . . ? C17 C18 C19 C20 4(3) . . . . ? C17 C18 C19 S2 -177.6(16) . . . . ? O5 S2 C19 C20 -160.5(17) . . . . ? O6 S2 C19 C20 -45.2(19) . . . . ? O4 S2 C19 C20 76.4(19) . . . . ? O5 S2 C19 C18 21.1(19) . . . . ? O6 S2 C19 C18 136.4(16) . . . . ? O4 S2 C19 C18 -102.1(17) . . . . ? C18 C19 C20 C21 -4(3) . . . . ? S2 C19 C20 C21 177.8(16) . . . . ? C19 C20 C21 C16 0(3) . . . . ? C8 C16 C21 C20 -178.3(19) . . . . ? C17 C16 C21 C20 3(3) . . . . ? C4 C5 N1 C1 5(3) . . . . ? C6 C5 N1 C1 -179(2) . . . . ? C4 C5 N1 Pb1 -158.3(18) . . . . ? C6 C5 N1 Pb1 17(2) . . . . ? C2 C1 N1 C5 0(4) . . . . ? C2 C1 N1 Pb1 163(2) . . . . ? O2 Pb1 N1 C5 -128.0(16) 7_467 . . . ? N2 Pb1 N1 C5 -20.9(14) . . . . ? N3 Pb1 N1 C5 -44.6(17) . . . . ? O6 Pb1 N1 C5 41.2(16) 2_557 . . . ? O2 Pb1 N1 C1 68.1(18) 7_467 . . . ? N2 Pb1 N1 C1 175(2) . . . . ? N3 Pb1 N1 C1 151.5(17) . . . . ? O6 Pb1 N1 C1 -122.7(18) 2_557 . . . ? C9 C10 N2 C6 -5(3) . . . . ? C11 C10 N2 C6 178.3(19) . . . . ? C9 C10 N2 Pb1 -159.3(14) . . . . ? C11 C10 N2 Pb1 24(2) . . . . ? C7 C6 N2 C10 2(3) . . . . ? C5 C6 N2 C10 -179.4(18) . . . . ? C7 C6 N2 Pb1 156.5(16) . . . . ? C5 C6 N2 Pb1 -25(2) . . . . ? O2 Pb1 N2 C10 -105.5(15) 7_467 . . . ? N3 Pb1 N2 C10 -24.4(14) . . . . ? N1 Pb1 N2 C10 178.0(17) . . . . ? O6 Pb1 N2 C10 62.2(14) 2_557 . . . ? O2 Pb1 N2 C6 99.7(15) 7_467 . . . ? N3 Pb1 N2 C6 -179.1(16) . . . . ? N1 Pb1 N2 C6 23.2(13) . . . . ? O6 Pb1 N2 C6 -92.6(14) 2_557 . . . ? C12 C11 N3 C15 -3(3) . . . . ? C10 C11 N3 C15 178(2) . . . . ? C12 C11 N3 Pb1 158.4(16) . . . . ? C10 C11 N3 Pb1 -20(2) . . . . ? C14 C15 N3 C11 -1(4) . . . . ? C14 C15 N3 Pb1 -162(2) . . . . ? O2 Pb1 N3 C11 127.6(15) 7_467 . . . ? N2 Pb1 N3 C11 22.5(14) . . . . ? N1 Pb1 N3 C11 46.5(16) . . . . ? O6 Pb1 N3 C11 -53.1(14) 2_557 . . . ? O2 Pb1 N3 C15 -69.8(17) 7_467 . . . ? N2 Pb1 N3 C15 -174.8(18) . . . . ? N1 Pb1 N3 C15 -150.8(16) . . . . ? O6 Pb1 N3 C15 109.5(17) 2_557 . . . ? O3 S1 O2 Pb1 -41(2) . . . 7_467 ? O1 S1 O2 Pb1 93.4(18) . . . 7_467 ? C17 S1 O2 Pb1 -155.2(16) . . . 7_467 ? O5 S2 O6 Pb1 -1.7(10) . . . 2_557 ? O4 S2 O6 Pb1 125.4(8) . . . 2_557 ? C19 S2 O6 Pb1 -116.5(9) . . . 2_557 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.839 _refine_diff_density_min -2.030 _refine_diff_density_rms 0.278 _database_code_depnum_ccdc_archive 'CCDC 958308' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5Pb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H57 N9 O27 Pb3 S6' _chemical_formula_weight 2186.11 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8500(12) _cell_length_b 14.6293(12) _cell_length_c 17.9504(16) _cell_angle_alpha 97.4430(10) _cell_angle_beta 101.7930(10) _cell_angle_gamma 90.4240(10) _cell_volume 3528.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3389 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 22.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 7.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2806 _exptl_absorpt_correction_T_max 0.3489 _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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16274 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 23.78 _reflns_number_total 10652 _reflns_number_gt 7467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10652 _refine_ls_number_parameters 1000 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.989 _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 0.32397(3) 0.19604(2) 0.36178(2) 0.04070(13) Uani 1 1 d . . . Pb2 Pb 0.70139(3) 0.87636(3) 0.11358(2) 0.04478(13) Uani 1 1 d . . . Pb3 Pb 0.99354(3) 0.35793(3) 0.20642(3) 0.05091(15) Uani 1 1 d . . . C1 C 0.7944(8) 0.9598(7) 0.3004(7) 0.059(3) Uani 1 1 d . . . H1A H 0.7941 1.0137 0.2780 0.070 Uiso 1 1 calc R . . C2 C 0.8351(8) 0.9629(8) 0.3797(8) 0.062(3) Uani 1 1 d . . . H2A H 0.8632 1.0172 0.4092 0.074 Uiso 1 1 calc R . . C3 C 0.8315(8) 0.8834(8) 0.4112(7) 0.060(3) Uani 1 1 d . . . H3A H 0.8562 0.8833 0.4634 0.072 Uiso 1 1 calc R . . C4 C 0.7918(8) 0.8035(7) 0.3664(6) 0.051(3) Uani 1 1 d . . . H4A H 0.7902 0.7493 0.3882 0.061 Uiso 1 1 calc R . . C5 C 0.7540(7) 0.8035(7) 0.2888(6) 0.039(3) Uani 1 1 d . . . C6 C 0.7106(6) 0.7200(6) 0.2382(6) 0.035(2) Uani 1 1 d . . . C7 C 0.6987(7) 0.6387(6) 0.2656(6) 0.040(3) Uani 1 1 d . . . H7A H 0.7157 0.6365 0.3182 0.048 Uiso 1 1 calc R . . C8 C 0.6623(7) 0.5598(7) 0.2172(6) 0.039(2) Uani 1 1 d . . . C9 C 0.6368(6) 0.5669(7) 0.1398(7) 0.046(3) Uani 1 1 d . . . H9A H 0.6108 0.5152 0.1055 0.056 Uiso 1 1 calc R . . C10 C 0.6488(6) 0.6489(6) 0.1122(6) 0.034(2) Uani 1 1 d . . . C11 C 0.6217(7) 0.6595(7) 0.0301(6) 0.036(2) Uani 1 1 d . . . C12 C 0.5982(7) 0.5847(7) -0.0261(6) 0.044(3) Uani 1 1 d . . . H12A H 0.5965 0.5252 -0.0133 0.053 Uiso 1 1 calc R . . C13 C 0.5773(7) 0.6004(8) -0.1019(7) 0.053(3) Uani 1 1 d . . . H13A H 0.5625 0.5509 -0.1410 0.064 Uiso 1 1 calc R . . C14 C 0.5784(9) 0.6884(9) -0.1197(7) 0.066(4) Uani 1 1 d . . . H14A H 0.5635 0.6993 -0.1706 0.079 Uiso 1 1 calc R . . C15 C 0.6015(9) 0.7592(9) -0.0624(7) 0.070(4) Uani 1 1 d . . . H15A H 0.6016 0.8191 -0.0746 0.084 Uiso 1 1 calc R . . C16 C 0.6432(7) 0.4737(6) 0.2501(6) 0.037(2) Uani 1 1 d . . . C17 C 0.6760(7) 0.3854(7) 0.2280(6) 0.040(3) Uani 1 1 d . . . C18 C 0.6545(6) 0.3128(7) 0.2661(6) 0.044(3) Uani 1 1 d . . . H18A H 0.6779 0.2546 0.2534 0.053 Uiso 1 1 calc R . . C19 C 0.5997(7) 0.3260(7) 0.3216(6) 0.044(3) Uani 1 1 d . . . C20 C 0.5648(8) 0.4102(7) 0.3429(6) 0.052(3) Uani 1 1 d . . . H20A H 0.5271 0.4184 0.3804 0.062 Uiso 1 1 calc R . . C21 C 0.5876(8) 0.4838(7) 0.3063(7) 0.061(3) Uani 1 1 d . . . H21A H 0.5644 0.5417 0.3202 0.074 Uiso 1 1 calc R . . C22 C 0.9089(9) 0.3762(8) 0.3692(7) 0.065(4) Uani 1 1 d . . . H22A H 0.9112 0.3127 0.3567 0.078 Uiso 1 1 calc R A . C23 C 0.8713(10) 0.4100(9) 0.4326(9) 0.081(4) Uani 1 1 d . . . H23A H 0.8449 0.3705 0.4604 0.097 Uiso 1 1 calc R . . C24 C 0.8743(10) 0.5043(9) 0.4533(7) 0.081(4) Uani 1 1 d . . . H24A H 0.8526 0.5291 0.4971 0.097 Uiso 1 1 calc R A . C25 C 0.9091(9) 0.5618(8) 0.4093(7) 0.069(4) Uani 1 1 d . . . H25A H 0.9110 0.6255 0.4222 0.083 Uiso 1 1 calc R . . C26 C 0.9416(7) 0.5207(7) 0.3440(6) 0.044(3) Uani 1 1 d . . . C27 C 0.9805(6) 0.5773(7) 0.2933(6) 0.041(3) Uani 1 1 d . A . C28 C 0.9854(7) 0.6744(7) 0.3047(6) 0.043(3) Uani 1 1 d . . . H28A H 0.9607 0.7058 0.3448 0.051 Uiso 1 1 calc R A . C29 C 1.0254(6) 0.7234(6) 0.2584(6) 0.034(2) Uani 1 1 d . . . C30 C 1.0564(6) 0.6734(6) 0.1958(5) 0.035(2) Uani 1 1 d . . . H30A H 1.0823 0.7044 0.1618 0.041 Uiso 1 1 calc R A . C31 C 1.0484(7) 0.5784(6) 0.1846(5) 0.032(2) Uani 1 1 d . A . C32 C 1.0828(7) 0.5237(6) 0.1197(5) 0.034(2) Uani 1 1 d . . . C33 C 1.1345(7) 0.5626(7) 0.0727(6) 0.049(3) Uani 1 1 d . . . H33A H 1.1514 0.6253 0.0820 0.059 Uiso 1 1 calc R . . C34 C 1.1606(8) 0.5077(8) 0.0122(7) 0.056(3) Uani 1 1 d . . . H34A H 1.1954 0.5331 -0.0198 0.067 Uiso 1 1 calc R A . C35 C 1.1349(8) 0.4148(8) -0.0007(7) 0.055(3) Uani 1 1 d . . . H35A H 1.1518 0.3766 -0.0413 0.066 Uiso 1 1 calc R . . C36 C 1.0850(8) 0.3814(8) 0.0468(8) 0.068(4) Uani 1 1 d . . . H36A H 1.0679 0.3187 0.0381 0.082 Uiso 1 1 calc R A . C37 C 1.0311(6) 0.8278(6) 0.2729(6) 0.033(2) Uani 1 1 d . . . C38 C 1.0056(6) 0.8890(6) 0.2202(5) 0.031(2) Uani 1 1 d . . . C39 C 1.0180(7) 0.9844(6) 0.2455(6) 0.039(2) Uani 1 1 d . . . H39A H 1.0000 1.0256 0.2102 0.046 Uiso 1 1 calc R A . C40 C 1.0563(6) 1.0181(6) 0.3211(5) 0.033(2) Uani 1 1 d . . . C41 C 1.0829(7) 0.9568(6) 0.3741(6) 0.038(2) Uani 1 1 d . . . H41A H 1.1089 0.9782 0.4254 0.046 Uiso 1 1 calc R A . C42 C 1.0699(7) 0.8627(6) 0.3487(5) 0.036(2) Uani 1 1 d . . . H42A H 1.0879 0.8215 0.3841 0.043 Uiso 1 1 calc R . . C43 C 1.4185(7) 1.1800(8) 0.5516(7) 0.058(3) Uani 1 1 d . . . H43A H 1.4297 1.2429 0.5520 0.070 Uiso 1 1 calc R . . C44 C 1.4339(7) 1.1455(9) 0.6203(7) 0.054(3) Uani 1 1 d . . . H44A H 1.4536 1.1843 0.6664 0.064 Uiso 1 1 calc R . . C45 C 1.4202(7) 1.0551(9) 0.6197(7) 0.055(3) Uani 1 1 d . . . H45A H 1.4322 1.0302 0.6657 0.066 Uiso 1 1 calc R . . C46 C 1.3883(8) 0.9982(7) 0.5516(7) 0.050(3) Uani 1 1 d . . . H46A H 1.3757 0.9356 0.5513 0.061 Uiso 1 1 calc R . . C47 C 1.3752(6) 1.0362(6) 0.4832(5) 0.032(2) Uani 1 1 d . . . C48 C 1.3431(6) 0.9775(6) 0.4068(5) 0.028(2) Uani 1 1 d . . . C49 C 1.3415(6) 0.8825(6) 0.4002(6) 0.034(2) Uani 1 1 d . . . H49A H 1.3612 0.8531 0.4435 0.040 Uiso 1 1 calc R . . C50 C 1.3097(6) 0.8308(6) 0.3276(6) 0.037(3) Uani 1 1 d . . . C51 C 1.2806(7) 0.8792(6) 0.2661(6) 0.039(2) Uani 1 1 d . . . H51A H 1.2569 0.8472 0.2174 0.047 Uiso 1 1 calc R . . C52 C 1.2864(6) 0.9748(6) 0.2760(6) 0.035(2) Uani 1 1 d . . . C53 C 1.2525(7) 1.0262(7) 0.2097(6) 0.039(2) Uani 1 1 d . . . C54 C 1.2110(8) 0.9842(7) 0.1374(6) 0.054(3) Uani 1 1 d . . . H54A H 1.2067 0.9201 0.1272 0.065 Uiso 1 1 calc R . . C55 C 1.1754(9) 1.0367(8) 0.0794(7) 0.070(4) Uani 1 1 d . . . H55A H 1.1465 1.0091 0.0302 0.084 Uiso 1 1 calc R . . C56 C 1.1843(10) 1.1299(8) 0.0971(7) 0.077(4) Uani 1 1 d . . . H56A H 1.1612 1.1672 0.0596 0.093 Uiso 1 1 calc R . . C57 C 1.2273(8) 1.1691(8) 0.1703(7) 0.059(3) Uani 1 1 d . . . H57A H 1.2342 1.2330 0.1807 0.070 Uiso 1 1 calc R . . C58 C 1.2997(6) 0.7276(6) 0.3209(6) 0.032(2) Uani 1 1 d . . . C59 C 1.3239(7) 0.6648(6) 0.2618(6) 0.037(2) Uani 1 1 d . . . C60 C 1.3075(6) 0.5714(6) 0.2618(5) 0.034(2) Uani 1 1 d . . . H60A H 1.3218 0.5296 0.2222 0.041 Uiso 1 1 calc R . . C61 C 1.2704(7) 0.5392(6) 0.3193(6) 0.041(3) Uani 1 1 d . A . C62 C 1.2456(8) 0.5986(6) 0.3772(6) 0.049(3) Uani 1 1 d . . . H62A H 1.2180 0.5770 0.4150 0.059 Uiso 1 1 calc R . . C63 C 1.2631(8) 0.6930(6) 0.3777(6) 0.045(3) Uani 1 1 d . . . H63A H 1.2494 0.7340 0.4181 0.054 Uiso 1 1 calc R . . N1 N 0.7565(6) 0.8819(5) 0.2568(5) 0.045(2) Uani 1 1 d . . . N2 N 0.6842(5) 0.7257(5) 0.1625(4) 0.036(2) Uani 1 1 d . . . N3 N 0.6247(6) 0.7456(6) 0.0132(5) 0.047(2) Uani 1 1 d . . . N4 N 1.0118(5) 0.5304(5) 0.2323(5) 0.040(2) Uani 1 1 d . A . N04 N 0.9415(6) 0.4299(6) 0.3260(5) 0.050(2) Uani 1 1 d . . . N6 N 1.0576(6) 0.4333(6) 0.1071(6) 0.056(3) Uani 1 1 d . . . N7 N 1.3873(6) 1.1259(5) 0.4823(5) 0.042(2) Uani 1 1 d . . . N8 N 1.3184(5) 1.0238(5) 0.3458(4) 0.0297(18) Uani 1 1 d . . . N9 N 1.2592(6) 1.1199(6) 0.2261(5) 0.047(2) Uani 1 1 d . . . O1 O 0.6737(6) 0.3566(5) 0.0831(4) 0.064(2) Uani 1 1 d . . . O2 O 0.7895(6) 0.2719(5) 0.1692(5) 0.069(2) Uani 1 1 d . . . O3 O 0.8216(5) 0.4322(5) 0.1656(4) 0.054(2) Uani 1 1 d . . . O4 O 0.5518(7) 0.2630(6) 0.4385(5) 0.087(3) Uani 1 1 d . . . O5 O 0.6603(6) 0.1734(6) 0.3671(6) 0.107(4) Uani 1 1 d . . . O6 O 0.4868(5) 0.1791(5) 0.3141(5) 0.064(2) Uani 1 1 d . . . O7 O 0.8702(5) 0.7894(4) 0.1220(4) 0.0484(19) Uani 1 1 d . . . O8 O 0.9061(6) 0.9411(5) 0.0947(4) 0.060(2) Uani 1 1 d . . . O9 O 1.0227(5) 0.8195(5) 0.0822(4) 0.0532(19) Uani 1 1 d . . . O10 O 1.1654(5) 1.1546(5) 0.3982(5) 0.062(2) Uani 1 1 d . . . O11 O 1.0475(8) 1.1863(5) 0.2882(5) 0.092(3) Uani 1 1 d . . . O12 O 0.9967(6) 1.1542(5) 0.4031(6) 0.086(3) Uani 1 1 d . . . O13 O 1.2947(5) 0.7332(5) 0.1319(4) 0.0528(19) Uani 1 1 d . . . O14 O 1.4534(5) 0.7644(5) 0.2181(4) 0.059(2) Uani 1 1 d . . . O15 O 1.4121(6) 0.6121(5) 0.1492(4) 0.067(2) Uani 1 1 d . . . O16 O 1.3408(11) 0.3769(11) 0.3164(12) 0.058(5) Uani 0.50 1 d PU A 1 O17 O 1.1768(9) 0.3911(8) 0.2414(8) 0.043(3) Uani 0.50 1 d PU A 1 O18 O 1.2017(14) 0.4068(11) 0.3790(10) 0.063(4) Uani 0.50 1 d PU A 1 O18' O 1.3036(17) 0.4049(12) 0.4000(12) 0.100(6) Uani 0.50 1 d PU A 2 O17' O 1.1547(13) 0.4019(12) 0.3248(13) 0.078(5) Uani 0.50 1 d PU A 2 O16' O 1.3004(16) 0.3688(13) 0.2696(12) 0.081(5) Uani 0.50 1 d PU A 2 S1 S 0.7447(2) 0.36017(19) 0.15546(18) 0.0499(7) Uani 1 1 d . . . S2 S 0.5742(2) 0.2278(2) 0.3649(2) 0.0584(8) Uani 1 1 d . . . S3 S 0.94804(19) 0.85738(18) 0.12125(15) 0.0414(6) Uani 1 1 d . . . S4 S 1.06443(19) 1.13886(17) 0.35291(17) 0.0436(7) Uani 1 1 d . . . S5 S 1.3762(2) 0.69553(18) 0.18390(16) 0.0439(7) Uani 1 1 d . . . S6 S 1.2486(2) 0.41860(17) 0.31712(19) 0.0506(8) Uani 1 1 d . . . O1W O 0.5363(6) 0.8855(5) 0.1467(5) 0.083(3) Uani 1 1 d . . . H1WA H 0.4975 0.8636 0.1050 0.124 Uiso 1 1 d R . . H1WB H 0.5370 0.8465 0.1783 0.124 Uiso 1 1 d R . . O2W O 0.5982(8) 0.9974(8) -0.0071(9) 0.160(5) Uani 1 1 d . . . O3W O 0.3224(11) -0.1800(7) 0.0073(6) 0.144(5) Uani 1 1 d . . . O4W O 0.5026(10) 1.0706(7) 0.1755(7) 0.136(4) Uani 1 1 d . . . O5W O 0.8412(6) 0.1963(6) 0.4777(5) 0.078(3) Uani 1 1 d . . . O6W O 0.7267(19) 1.0858(9) 0.1495(9) 0.291(13) Uani 1 1 d . . . O7W O 0.4906(14) 0.4163(10) 0.5287(10) 0.219(7) Uani 1 1 d . . . O8W O 1.0794(9) 0.7808(9) -0.0616(7) 0.156(6) Uani 1 1 d . . . O9W O 1.267(2) 0.3383(15) 0.5095(12) 0.383(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0516(3) 0.0228(2) 0.0510(3) 0.01059(18) 0.0148(2) 0.00378(17) Pb2 0.0543(3) 0.0315(2) 0.0516(3) 0.0127(2) 0.0137(2) 0.00220(18) Pb3 0.0518(3) 0.0289(2) 0.0782(4) 0.0104(2) 0.0258(2) 0.00464(19) C1 0.084(9) 0.033(7) 0.066(9) -0.003(6) 0.037(7) 0.004(6) C2 0.063(8) 0.055(8) 0.065(10) -0.023(7) 0.023(7) -0.008(6) C3 0.070(8) 0.061(9) 0.046(8) -0.003(7) 0.013(6) 0.009(7) C4 0.066(7) 0.033(6) 0.052(8) 0.000(6) 0.012(6) 0.005(5) C5 0.036(6) 0.048(7) 0.033(7) -0.006(5) 0.015(5) 0.007(5) C6 0.033(5) 0.032(6) 0.041(7) 0.008(5) 0.011(5) 0.006(4) C7 0.051(6) 0.038(6) 0.040(7) 0.024(5) 0.015(5) 0.009(5) C8 0.039(6) 0.039(6) 0.040(7) 0.011(5) 0.005(5) 0.004(5) C9 0.029(5) 0.031(6) 0.078(9) 0.009(6) 0.008(5) -0.007(4) C10 0.033(5) 0.031(6) 0.042(7) 0.010(5) 0.014(5) -0.001(4) C11 0.037(5) 0.037(6) 0.035(6) 0.008(5) 0.011(5) 0.002(5) C12 0.051(6) 0.043(7) 0.035(7) 0.004(5) 0.002(5) -0.009(5) C13 0.054(7) 0.046(7) 0.057(8) -0.011(6) 0.015(6) 0.003(6) C14 0.090(10) 0.063(9) 0.042(8) 0.011(7) 0.003(7) -0.013(7) C15 0.091(10) 0.060(9) 0.055(9) 0.029(7) -0.007(7) -0.008(7) C16 0.042(6) 0.033(6) 0.040(6) 0.011(5) 0.014(5) 0.000(5) C17 0.041(6) 0.047(7) 0.032(6) 0.006(5) 0.009(5) -0.004(5) C18 0.033(6) 0.041(6) 0.063(8) 0.026(6) 0.007(5) -0.009(5) C19 0.046(6) 0.041(7) 0.047(7) 0.016(5) 0.010(5) -0.010(5) C20 0.069(7) 0.047(7) 0.051(7) 0.014(6) 0.036(6) -0.004(6) C21 0.068(8) 0.040(7) 0.091(10) 0.029(7) 0.039(7) 0.016(6) C22 0.086(9) 0.046(8) 0.071(10) 0.033(7) 0.017(8) 0.005(7) C23 0.107(11) 0.058(9) 0.105(12) 0.055(8) 0.056(9) 0.018(8) C24 0.133(12) 0.071(10) 0.061(9) 0.034(8) 0.056(9) 0.021(9) C25 0.107(10) 0.049(7) 0.068(9) 0.022(7) 0.046(8) 0.032(7) C26 0.043(6) 0.046(7) 0.050(7) 0.031(6) 0.007(5) 0.015(5) C27 0.023(5) 0.033(6) 0.067(8) 0.008(6) 0.010(5) 0.008(4) C28 0.046(6) 0.038(6) 0.045(7) 0.007(5) 0.009(5) 0.017(5) C29 0.038(5) 0.026(5) 0.040(6) 0.002(5) 0.015(5) 0.009(4) C30 0.038(5) 0.034(6) 0.034(6) 0.008(5) 0.010(5) 0.003(4) C31 0.043(6) 0.020(5) 0.036(6) 0.005(4) 0.014(5) 0.001(4) C32 0.038(5) 0.029(6) 0.036(6) 0.000(5) 0.011(5) 0.006(4) C33 0.062(7) 0.035(6) 0.055(8) 0.003(6) 0.026(6) 0.014(5) C34 0.068(8) 0.049(8) 0.057(8) 0.009(6) 0.026(6) 0.005(6) C35 0.058(7) 0.056(8) 0.053(8) -0.009(6) 0.026(6) 0.014(6) C36 0.078(8) 0.044(7) 0.091(11) -0.014(7) 0.052(8) -0.003(6) C37 0.030(5) 0.030(6) 0.040(7) -0.007(5) 0.016(5) 0.005(4) C38 0.032(5) 0.034(6) 0.030(6) 0.009(5) 0.013(4) 0.007(4) C39 0.041(6) 0.032(6) 0.047(7) 0.018(5) 0.009(5) 0.002(5) C40 0.036(5) 0.032(6) 0.030(6) 0.002(5) 0.006(4) 0.000(4) C41 0.045(6) 0.037(6) 0.029(6) -0.003(5) 0.004(5) -0.004(5) C42 0.046(6) 0.032(6) 0.032(6) 0.006(5) 0.012(5) 0.015(5) C43 0.042(6) 0.057(8) 0.066(9) -0.024(7) 0.012(6) -0.002(6) C44 0.048(7) 0.061(9) 0.042(8) -0.014(6) 0.000(6) 0.008(6) C45 0.043(6) 0.071(9) 0.052(8) 0.006(7) 0.014(6) 0.016(6) C46 0.065(7) 0.040(7) 0.050(8) 0.011(6) 0.017(6) 0.010(6) C47 0.031(5) 0.033(6) 0.036(6) 0.011(5) 0.010(4) 0.010(4) C48 0.033(5) 0.025(5) 0.032(6) 0.013(4) 0.012(4) 0.006(4) C49 0.033(5) 0.029(6) 0.037(6) 0.013(5) 0.000(4) 0.000(4) C50 0.032(5) 0.020(5) 0.062(8) 0.008(5) 0.018(5) 0.008(4) C51 0.051(6) 0.027(6) 0.040(7) 0.003(5) 0.012(5) 0.003(5) C52 0.035(5) 0.035(6) 0.040(7) 0.009(5) 0.017(5) 0.005(4) C53 0.039(6) 0.037(6) 0.037(7) 0.004(5) 0.005(5) -0.002(5) C54 0.072(8) 0.041(7) 0.046(8) 0.011(6) 0.001(6) -0.002(6) C55 0.104(10) 0.059(9) 0.040(8) 0.015(6) -0.005(7) -0.007(7) C56 0.132(12) 0.046(8) 0.053(9) 0.022(7) 0.005(8) 0.021(8) C57 0.085(9) 0.035(7) 0.058(9) 0.007(6) 0.019(7) 0.012(6) C58 0.030(5) 0.021(5) 0.045(7) 0.011(5) 0.003(4) 0.005(4) C59 0.043(6) 0.024(6) 0.045(7) 0.005(5) 0.009(5) 0.003(4) C60 0.036(5) 0.030(6) 0.034(6) -0.003(5) 0.009(5) 0.005(4) C61 0.041(6) 0.021(5) 0.062(8) 0.011(5) 0.012(5) -0.001(4) C62 0.077(8) 0.027(6) 0.052(7) 0.012(5) 0.031(6) 0.000(5) C63 0.075(7) 0.027(6) 0.042(7) 0.003(5) 0.036(6) 0.009(5) N1 0.064(6) 0.026(5) 0.048(6) 0.003(4) 0.024(5) 0.001(4) N2 0.045(5) 0.037(5) 0.029(5) 0.004(4) 0.012(4) 0.006(4) N3 0.071(6) 0.038(5) 0.033(5) 0.011(4) 0.008(4) 0.001(4) N4 0.036(5) 0.026(5) 0.060(6) 0.011(4) 0.012(4) 0.010(4) N04 0.056(6) 0.030(5) 0.068(7) 0.019(5) 0.013(5) 0.000(4) N6 0.064(6) 0.029(5) 0.080(8) -0.002(5) 0.034(5) -0.004(4) N7 0.056(5) 0.026(5) 0.048(6) 0.008(4) 0.016(4) -0.001(4) N8 0.040(4) 0.019(4) 0.032(5) 0.001(4) 0.014(4) 0.004(3) N9 0.070(6) 0.034(5) 0.040(6) 0.019(4) 0.010(5) 0.010(4) O1 0.073(5) 0.067(6) 0.050(5) 0.006(4) 0.006(4) 0.005(4) O2 0.078(5) 0.047(5) 0.098(7) 0.023(5) 0.045(5) 0.020(4) O3 0.056(5) 0.048(5) 0.064(5) 0.019(4) 0.022(4) 0.004(4) O4 0.127(8) 0.087(7) 0.053(6) 0.023(5) 0.028(5) -0.027(6) O5 0.069(6) 0.108(8) 0.171(11) 0.100(7) 0.037(6) 0.034(5) O6 0.067(5) 0.048(5) 0.083(6) 0.014(4) 0.026(5) -0.009(4) O7 0.050(4) 0.034(4) 0.057(5) -0.006(4) 0.011(4) -0.005(3) O8 0.092(6) 0.047(5) 0.034(5) 0.011(4) -0.005(4) 0.004(4) O9 0.072(5) 0.062(5) 0.032(4) 0.002(4) 0.028(4) 0.006(4) O10 0.049(5) 0.048(5) 0.083(6) -0.010(4) 0.008(4) -0.004(4) O11 0.173(9) 0.034(5) 0.062(6) 0.010(4) 0.004(6) 0.008(5) O12 0.091(6) 0.049(5) 0.130(9) -0.019(5) 0.071(6) 0.004(5) O13 0.071(5) 0.053(5) 0.035(4) 0.008(4) 0.010(4) 0.009(4) O14 0.058(5) 0.064(5) 0.055(5) 0.006(4) 0.014(4) -0.024(4) O15 0.101(6) 0.049(5) 0.063(6) 0.002(4) 0.047(5) 0.018(4) O16 0.041(8) 0.032(8) 0.095(12) 0.017(9) -0.006(8) 0.008(7) O17 0.049(7) 0.012(6) 0.056(8) -0.003(6) -0.013(6) 0.001(5) O18 0.088(10) 0.055(8) 0.052(9) 0.021(7) 0.019(8) -0.019(8) O18' 0.144(12) 0.062(9) 0.090(11) 0.032(9) -0.001(11) 0.012(10) O17' 0.069(9) 0.065(8) 0.102(11) 0.029(9) 0.010(9) -0.009(8) O16' 0.106(11) 0.045(8) 0.094(11) -0.012(9) 0.037(9) 0.002(9) S1 0.0568(17) 0.0411(17) 0.058(2) 0.0105(14) 0.0237(15) 0.0055(14) S2 0.0558(18) 0.056(2) 0.073(2) 0.0359(17) 0.0166(16) -0.0021(15) S3 0.0548(16) 0.0378(16) 0.0315(16) 0.0058(12) 0.0078(13) 0.0019(13) S4 0.0503(16) 0.0289(15) 0.0523(19) 0.0009(13) 0.0150(14) 0.0058(12) S5 0.0554(17) 0.0368(16) 0.0435(17) 0.0055(13) 0.0196(14) -0.0004(13) S6 0.0618(19) 0.0210(14) 0.073(2) 0.0125(14) 0.0194(17) 0.0003(13) O1W 0.089(6) 0.065(6) 0.115(8) 0.040(5) 0.051(6) 0.017(5) O2W 0.121(9) 0.129(10) 0.234(16) 0.073(10) 0.013(10) 0.023(8) O3W 0.289(16) 0.070(7) 0.087(8) -0.006(6) 0.084(9) -0.020(8) O4W 0.203(12) 0.094(8) 0.116(10) 0.016(7) 0.043(9) 0.038(8) O5W 0.096(6) 0.091(6) 0.057(6) 0.018(5) 0.036(5) 0.025(5) O6W 0.65(4) 0.065(9) 0.153(15) -0.011(9) 0.091(19) -0.030(15) O7W 0.28(2) 0.169(14) 0.224(19) -0.002(13) 0.115(15) 0.020(14) O8W 0.149(10) 0.223(14) 0.097(9) -0.043(9) 0.067(8) -0.073(10) O9W 0.67(5) 0.35(3) 0.22(2) 0.16(2) 0.21(3) 0.38(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N8 2.497(7) 1_445 ? Pb1 O10 2.507(7) 1_445 ? Pb1 N7 2.514(8) 1_445 ? Pb1 N9 2.523(8) 1_445 ? Pb1 O6 2.574(7) . ? Pb2 O1W 2.478(8) . ? Pb2 N2 2.502(8) . ? Pb2 N3 2.516(8) . ? Pb2 N1 2.519(9) . ? Pb2 O7 2.656(6) . ? Pb3 N4 2.507(7) . ? Pb3 O17 2.514(12) . ? Pb3 N04 2.510(9) . ? Pb3 N6 2.515(9) . ? Pb3 O17' 2.757(19) . ? Pb3 O3 2.631(7) . ? C1 N1 1.333(12) . ? C1 C2 1.414(16) . ? C2 C3 1.362(16) . ? C3 C4 1.373(14) . ? C4 C5 1.385(14) . ? C5 N1 1.350(12) . ? C5 C6 1.470(13) . ? C6 N2 1.347(12) . ? C6 C7 1.366(12) . ? C7 C8 1.376(13) . ? C8 C9 1.379(14) . ? C8 C16 1.503(13) . ? C9 C10 1.377(13) . ? C10 N2 1.367(11) . ? C10 C11 1.472(13) . ? C11 N3 1.335(11) . ? C11 C12 1.378(13) . ? C12 C13 1.382(14) . ? C13 C14 1.366(15) . ? C14 C15 1.348(15) . ? C15 N3 1.370(14) . ? C16 C21 1.383(14) . ? C16 C17 1.407(13) . ? C17 C18 1.396(13) . ? C17 S1 1.768(10) . ? C18 C19 1.368(14) . ? C19 C20 1.364(13) . ? C19 S2 1.785(10) . ? C20 C21 1.398(14) . ? C22 N04 1.310(13) . ? C22 C23 1.383(17) . ? C23 C24 1.379(16) . ? C24 C25 1.373(16) . ? C25 C26 1.405(15) . ? C26 N04 1.326(12) . ? C26 C27 1.481(14) . ? C27 N4 1.364(12) . ? C27 C28 1.408(13) . ? C28 C29 1.359(13) . ? C29 C30 1.404(12) . ? C29 C37 1.515(12) . ? C30 C31 1.379(12) . ? C31 N4 1.346(11) . ? C31 C32 1.489(12) . ? C32 N6 1.344(11) . ? C32 C33 1.383(13) . ? C33 C34 1.377(14) . ? C34 C35 1.380(14) . ? C35 C36 1.337(15) . ? C36 N6 1.360(13) . ? C37 C38 1.380(12) . ? C37 C42 1.385(12) . ? C38 C39 1.408(12) . ? C38 S3 1.791(9) . ? C39 C40 1.377(13) . ? C40 C41 1.389(13) . ? C40 S4 1.780(9) . ? C41 C42 1.392(12) . ? C43 C44 1.370(16) . ? C43 N7 1.372(13) . ? C44 C45 1.334(15) . ? C45 C46 1.374(14) . ? C46 C47 1.391(13) . ? C47 N7 1.324(11) . ? C47 C48 1.503(12) . ? C48 N8 1.348(11) . ? C48 C49 1.378(11) . ? C49 C50 1.404(13) . ? C50 C51 1.382(13) . ? C50 C58 1.502(12) . ? C51 C52 1.387(12) . ? C52 N8 1.348(11) . ? C52 C53 1.486(13) . ? C53 N9 1.362(11) . ? C53 C54 1.370(13) . ? C54 C55 1.386(14) . ? C55 C56 1.358(15) . ? C56 C57 1.375(15) . ? C57 N9 1.315(13) . ? C58 C63 1.377(13) . ? C58 C59 1.407(13) . ? C59 C60 1.384(12) . ? C59 S5 1.804(10) . ? C60 C61 1.374(13) . ? C61 C62 1.368(13) . ? C61 S6 1.782(9) . ? C62 C63 1.398(12) . ? N7 Pb1 2.514(8) 1_665 ? N8 Pb1 2.497(7) 1_665 ? N9 Pb1 2.523(8) 1_665 ? O1 S1 1.455(8) . ? O2 S1 1.465(7) . ? O3 S1 1.461(7) . ? O4 S2 1.450(9) . ? O5 S2 1.435(8) . ? O6 S2 1.473(8) . ? O7 S3 1.466(7) . ? O8 S3 1.454(7) . ? O9 S3 1.439(7) . ? O10 S4 1.466(7) . ? O10 Pb1 2.507(7) 1_665 ? O11 S4 1.409(8) . ? O12 S4 1.428(8) . ? O13 S5 1.470(7) . ? O14 S5 1.447(7) . ? O15 S5 1.436(7) . ? O16 S6 1.421(16) . ? O17 S6 1.516(12) . ? O18 S6 1.425(16) . ? O18' S6 1.565(19) . ? O17' S6 1.358(17) . ? O16' S6 1.37(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 N8 Pb1 O10 75.8(2) 1_445 1_445 ? N8 Pb1 N7 64.9(3) 1_445 1_445 ? O10 Pb1 N7 79.0(3) 1_445 1_445 ? N8 Pb1 N9 65.3(3) 1_445 1_445 ? O10 Pb1 N9 90.3(3) 1_445 1_445 ? N7 Pb1 N9 130.2(3) 1_445 1_445 ? N8 Pb1 O6 84.9(2) 1_445 . ? O10 Pb1 O6 160.6(2) 1_445 . ? N7 Pb1 O6 94.3(3) 1_445 . ? N9 Pb1 O6 80.1(3) 1_445 . ? O1W Pb2 N2 77.6(2) . . ? O1W Pb2 N3 85.1(3) . . ? N2 Pb2 N3 64.9(3) . . ? O1W Pb2 N1 82.2(3) . . ? N2 Pb2 N1 65.4(3) . . ? N3 Pb2 N1 130.2(3) . . ? O1W Pb2 O7 147.8(2) . . ? N2 Pb2 O7 70.7(2) . . ? N3 Pb2 O7 87.1(2) . . ? N1 Pb2 O7 79.3(2) . . ? N4 Pb3 O17 75.3(3) . . ? N4 Pb3 N04 64.8(3) . . ? O17 Pb3 N04 101.2(4) . . ? N4 Pb3 N6 64.8(3) . . ? O17 Pb3 N6 66.9(4) . . ? N04 Pb3 N6 129.6(3) . . ? N4 Pb3 O17' 72.5(4) . . ? O17 Pb3 O17' 34.4(5) . . ? N04 Pb3 O17' 69.0(5) . . ? N6 Pb3 O17' 97.0(5) . . ? N4 Pb3 O3 69.8(2) . . ? O17 Pb3 O3 143.9(3) . . ? N04 Pb3 O3 71.9(2) . . ? N6 Pb3 O3 89.8(3) . . ? O17' Pb3 O3 134.1(4) . . ? N1 C1 C2 122.0(11) . . ? C3 C2 C1 117.5(11) . . ? C4 C3 C2 120.4(12) . . ? C3 C4 C5 120.0(11) . . ? N1 C5 C4 120.3(9) . . ? N1 C5 C6 117.5(9) . . ? C4 C5 C6 122.2(10) . . ? N2 C6 C7 120.6(9) . . ? N2 C6 C5 117.3(8) . . ? C7 C6 C5 122.1(10) . . ? C6 C7 C8 121.5(10) . . ? C9 C8 C7 117.0(9) . . ? C9 C8 C16 123.0(9) . . ? C7 C8 C16 119.8(9) . . ? C8 C9 C10 121.5(10) . . ? C9 C10 N2 119.5(9) . . ? C9 C10 C11 123.2(9) . . ? N2 C10 C11 117.3(8) . . ? N3 C11 C12 121.9(9) . . ? N3 C11 C10 116.2(8) . . ? C12 C11 C10 121.9(9) . . ? C13 C12 C11 118.3(10) . . ? C12 C13 C14 120.2(10) . . ? C15 C14 C13 119.2(11) . . ? C14 C15 N3 121.9(11) . . ? C21 C16 C17 118.5(9) . . ? C21 C16 C8 115.8(9) . . ? C17 C16 C8 125.6(9) . . ? C18 C17 C16 118.5(9) . . ? C18 C17 S1 117.3(8) . . ? C16 C17 S1 124.2(8) . . ? C19 C18 C17 121.0(10) . . ? C20 C19 C18 121.7(9) . . ? C20 C19 S2 121.0(8) . . ? C18 C19 S2 117.2(8) . . ? C19 C20 C21 117.7(10) . . ? C16 C21 C20 122.4(10) . . ? N04 C22 C23 122.8(11) . . ? C22 C23 C24 117.9(11) . . ? C25 C24 C23 120.2(12) . . ? C24 C25 C26 117.6(11) . . ? N04 C26 C25 121.8(10) . . ? N04 C26 C27 116.9(10) . . ? C25 C26 C27 121.3(10) . . ? N4 C27 C28 119.8(10) . . ? N4 C27 C26 116.5(9) . . ? C28 C27 C26 123.7(10) . . ? C29 C28 C27 121.6(10) . . ? C28 C29 C30 117.2(9) . . ? C28 C29 C37 120.4(9) . . ? C30 C29 C37 122.3(9) . . ? C31 C30 C29 120.1(9) . . ? N4 C31 C30 122.2(9) . . ? N4 C31 C32 116.7(8) . . ? C30 C31 C32 121.2(9) . . ? N6 C32 C33 121.0(9) . . ? N6 C32 C31 116.0(9) . . ? C33 C32 C31 123.0(9) . . ? C32 C33 C34 119.4(10) . . ? C35 C34 C33 119.5(11) . . ? C36 C35 C34 118.2(10) . . ? C35 C36 N6 124.1(11) . . ? C38 C37 C42 118.6(8) . . ? C38 C37 C29 128.0(9) . . ? C42 C37 C29 113.3(9) . . ? C37 C38 C39 119.1(9) . . ? C37 C38 S3 125.0(7) . . ? C39 C38 S3 115.7(7) . . ? C40 C39 C38 121.7(9) . . ? C39 C40 C41 119.4(9) . . ? C39 C40 S4 120.9(7) . . ? C41 C40 S4 119.6(7) . . ? C42 C41 C40 118.6(9) . . ? C41 C42 C37 122.6(9) . . ? C44 C43 N7 122.8(11) . . ? C45 C44 C43 118.6(11) . . ? C44 C45 C46 120.6(11) . . ? C45 C46 C47 118.7(10) . . ? N7 C47 C46 121.8(9) . . ? N7 C47 C48 116.8(8) . . ? C46 C47 C48 121.4(9) . . ? N8 C48 C49 122.9(9) . . ? N8 C48 C47 115.6(8) . . ? C49 C48 C47 121.5(8) . . ? C48 C49 C50 119.3(9) . . ? C51 C50 C49 117.2(8) . . ? C51 C50 C58 123.0(9) . . ? C49 C50 C58 119.6(9) . . ? C50 C51 C52 120.8(9) . . ? N8 C52 C51 121.5(9) . . ? N8 C52 C53 118.0(8) . . ? C51 C52 C53 120.4(9) . . ? N9 C53 C54 120.9(9) . . ? N9 C53 C52 115.6(9) . . ? C54 C53 C52 123.3(9) . . ? C55 C54 C53 120.3(10) . . ? C56 C55 C54 117.6(11) . . ? C55 C56 C57 120.2(11) . . ? N9 C57 C56 122.7(10) . . ? C63 C58 C59 118.3(8) . . ? C63 C58 C50 116.2(9) . . ? C59 C58 C50 125.5(9) . . ? C58 C59 C60 119.0(9) . . ? C58 C59 S5 125.3(7) . . ? C60 C59 S5 115.7(7) . . ? C61 C60 C59 121.2(9) . . ? C60 C61 C62 121.1(9) . . ? C60 C61 S6 120.2(8) . . ? C62 C61 S6 118.7(8) . . ? C61 C62 C63 117.8(10) . . ? C58 C63 C62 122.6(9) . . ? C5 N1 C1 119.8(10) . . ? C5 N1 Pb2 119.3(6) . . ? C1 N1 Pb2 120.7(7) . . ? C6 N2 C10 119.9(8) . . ? C6 N2 Pb2 120.2(6) . . ? C10 N2 Pb2 119.9(6) . . ? C11 N3 C15 118.5(9) . . ? C11 N3 Pb2 120.9(6) . . ? C15 N3 Pb2 119.6(7) . . ? C31 N4 C27 119.0(8) . . ? C31 N4 Pb3 120.7(6) . . ? C27 N4 Pb3 120.2(6) . . ? C22 N04 C26 119.7(11) . . ? C22 N04 Pb3 118.8(8) . . ? C26 N04 Pb3 121.3(7) . . ? C32 N6 C36 117.8(10) . . ? C32 N6 Pb3 120.4(7) . . ? C36 N6 Pb3 120.7(7) . . ? C47 N7 C43 117.4(9) . . ? C47 N7 Pb1 120.4(6) . 1_665 ? C43 N7 Pb1 121.2(7) . 1_665 ? C48 N8 C52 118.2(8) . . ? C48 N8 Pb1 121.2(6) . 1_665 ? C52 N8 Pb1 120.5(6) . 1_665 ? C57 N9 C53 118.4(9) . . ? C57 N9 Pb1 121.1(7) . 1_665 ? C53 N9 Pb1 120.5(6) . 1_665 ? S1 O3 Pb3 108.1(4) . . ? S2 O6 Pb1 116.0(4) . . ? S3 O7 Pb2 107.9(3) . . ? S4 O10 Pb1 131.7(5) . 1_665 ? S6 O17 Pb3 133.2(9) . . ? S6 O17' Pb3 125.9(13) . . ? O1 S1 O3 113.1(5) . . ? O1 S1 O2 114.2(5) . . ? O3 S1 O2 109.9(4) . . ? O1 S1 C17 105.7(5) . . ? O3 S1 C17 108.4(4) . . ? O2 S1 C17 105.0(5) . . ? O5 S2 O4 116.3(6) . . ? O5 S2 O6 111.4(6) . . ? O4 S2 O6 110.3(5) . . ? O5 S2 C19 105.0(5) . . ? O4 S2 C19 106.4(5) . . ? O6 S2 C19 106.7(5) . . ? O9 S3 O8 114.4(5) . . ? O9 S3 O7 112.8(4) . . ? O8 S3 O7 110.9(4) . . ? O9 S3 C38 107.3(4) . . ? O8 S3 C38 105.9(4) . . ? O7 S3 C38 104.8(4) . . ? O11 S4 O12 116.3(6) . . ? O11 S4 O10 112.3(5) . . ? O12 S4 O10 109.0(5) . . ? O11 S4 C40 108.8(5) . . ? O12 S4 C40 105.6(5) . . ? O10 S4 C40 103.9(4) . . ? O15 S5 O14 113.3(5) . . ? O15 S5 O13 112.7(5) . . ? O14 S5 O13 112.0(4) . . ? O15 S5 C59 106.5(4) . . ? O14 S5 C59 106.0(4) . . ? O13 S5 C59 105.5(4) . . ? O18 S6 O16 117.8(11) . . ? O18 S6 O17' 44.1(9) . . ? O16 S6 O17' 143.2(10) . . ? O18 S6 O16' 139.5(11) . . ? O16 S6 O16' 37.7(9) . . ? O17' S6 O16' 127.8(12) . . ? O18 S6 O17 109.6(9) . . ? O16 S6 O17 110.7(10) . . ? O17' S6 O17 66.3(10) . . ? O16' S6 O17 73.5(11) . . ? O18 S6 O18' 55.0(10) . . ? O16 S6 O18' 68.6(11) . . ? O17' S6 O18' 98.5(12) . . ? O16' S6 O18' 104.5(12) . . ? O17 S6 O18' 154.5(9) . . ? O18 S6 C61 107.6(7) . . ? O16 S6 C61 106.3(7) . . ? O17' S6 C61 110.0(8) . . ? O16' S6 C61 110.8(9) . . ? O17 S6 C61 103.8(6) . . ? O18' S6 C61 100.6(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.78 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.543 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.146 ######################################################################## _database_code_depnum_ccdc_archive 'CCDC 958309'