# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Radu Custelcean' _publ_contact_author_address ; Chemical Sciences Division Oak Ridge National Laboratory PO Box 2008 MS-6119 Oak Ridge Tennessee 37831-6119 UNITED STATES OF AMERICA ; _publ_contact_author_email CUSTELCEANR@ORNL.GOV _publ_section_title ; A coordinatively saturated sulfate encapsulated in a metal-organic framework functionalized with urea hydrogen-bonding groups ; loop_ _publ_author_name 'Radu Custelcean' 'Benjamin Hay' 'B.A. Moyer' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 281962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H34 Ag N10 O7 S0.50' _chemical_formula_weight 770.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3995(12) _cell_length_b 13.5437(15) _cell_length_c 14.6455(17) _cell_angle_alpha 66.289(2) _cell_angle_beta 76.241(2) _cell_angle_gamma 87.576(2) _cell_volume 1831.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 790 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9107 _exptl_absorpt_correction_T_max 0.9689 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22524 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.33 _reflns_number_total 9083 _reflns_number_gt 8139 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+3.3953P] 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 9083 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 1.252 _refine_ls_restrained_S_all 1.252 _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 Ag1 Ag 0.91450(3) 0.52447(2) 0.74333(3) 0.03736(11) Uani 1 1 d . . . S1 S 0.5000 0.0000 1.0000 0.0215(2) Uani 1 2 d S . . O1 O 0.4564(5) 0.1070(4) 0.9842(4) 0.0289(11) Uani 0.50 1 d P . . N1 N 0.6229(3) 0.3075(3) 0.8569(3) 0.0323(7) Uani 1 1 d . . . H1 H 0.5975 0.2452 0.8593 0.039 Uiso 1 1 calc R . . C1 C 0.4671(4) 0.4455(3) 0.8696(3) 0.0353(9) Uani 1 1 d . . . H1C H 0.5123 0.4577 0.9169 0.042 Uiso 1 1 calc R . . H1C1 H 0.4354 0.5153 0.8281 0.042 Uiso 1 1 calc R . . O2 O 0.6524(5) 0.0085(4) 0.9661(4) 0.0312(12) Uani 0.50 1 d P . . N2 N 0.7508(3) 0.2107(2) 0.9659(3) 0.0305(7) Uani 1 1 d . . . H2 H 0.7230 0.1552 0.9575 0.037 Uiso 1 1 calc R . . C2 C 0.5648(4) 0.4054(3) 0.7992(3) 0.0360(9) Uani 1 1 d . . . H2C H 0.5188 0.3910 0.7535 0.043 Uiso 1 1 calc R . . H2C1 H 0.6362 0.4623 0.7555 0.043 Uiso 1 1 calc R . . O3 O 0.4621(6) -0.0748(4) 1.1073(4) 0.0321(12) Uani 0.50 1 d P . . N3 N 0.2532(4) 0.1995(3) 0.8708(3) 0.0369(8) Uani 1 1 d . . . H3 H 0.3025 0.1584 0.9110 0.044 Uiso 1 1 calc R . . C3 C 0.2518(5) 0.3816(3) 0.8714(4) 0.0405(10) Uani 1 1 d . . . H3C H 0.2955 0.4105 0.7971 0.049 Uiso 1 1 calc R . . H3C1 H 0.1904 0.4354 0.8835 0.049 Uiso 1 1 calc R . . O4 O 0.4539(5) -0.0421(4) 0.9347(4) 0.0296(11) Uani 0.50 1 d P . . N4 N 0.3395(4) 0.1143(3) 0.7655(3) 0.0381(8) Uani 1 1 d . . . H4 H 0.4002 0.0942 0.8013 0.046 Uiso 1 1 calc R . . C4 C 0.1729(4) 0.2767(3) 0.9010(4) 0.0388(9) Uani 1 1 d . . . H4C1 H 0.1361 0.2442 0.9764 0.047 Uiso 1 1 calc R . . H4C H 0.0975 0.2927 0.8678 0.047 Uiso 1 1 calc R . . O5 O 0.2198(3) 0.1605(2) 1.2896(2) 0.0314(6) Uani 1 1 d . . . N5 N 0.3713(3) 0.1970(3) 1.1372(2) 0.0318(7) Uani 1 1 d . . . H5 H 0.4231 0.1686 1.0983 0.038 Uiso 1 1 calc R . . C5 C 0.2984(4) 0.3720(3) 1.0295(3) 0.0362(9) Uani 1 1 d . . . H5C1 H 0.2066 0.3392 1.0572 0.043 Uiso 1 1 calc R . . H5C H 0.2950 0.4486 1.0202 0.043 Uiso 1 1 calc R . . O6 O 0.1855(4) 0.2397(3) 0.7252(3) 0.0617(11) Uani 1 1 d . . . N6 N 0.2766(3) 0.0261(2) 1.2325(2) 0.0289(7) Uani 1 1 d . . . H6 H 0.3298 0.0119 1.1834 0.035 Uiso 1 1 calc R . . C6 C 0.3812(5) 0.3131(3) 1.1064(3) 0.0359(9) Uani 1 1 d . . . H6C1 H 0.4752 0.3399 1.0753 0.043 Uiso 1 1 calc R . . H6C H 0.3507 0.3293 1.1680 0.043 Uiso 1 1 calc R . . O7 O 0.7665(3) 0.3960(2) 0.8986(2) 0.0348(6) Uani 1 1 d . . . N7 N 0.3530(3) 0.3670(2) 0.9300(3) 0.0301(7) Uani 1 1 d . . . C7 C 0.7149(4) 0.3106(3) 0.9067(3) 0.0270(7) Uani 1 1 d . . . O8 O 0.7797(4) 0.6616(3) 0.6591(3) 0.0497(8) Uani 1 1 d . . . N8 N 0.9731(4) 0.3668(3) 1.2229(3) 0.0429(9) Uani 1 1 d . . . C8 C 0.2544(4) 0.1891(3) 0.7827(3) 0.0363(9) Uani 1 1 d . . . O9 O 0.7279(10) 0.6185(7) 0.5033(6) 0.174(3) Uani 1 1 d . . . N9 N 0.4780(6) -0.2761(4) 0.6922(4) 0.0665(14) Uani 1 1 d . . . C9 C 0.2847(4) 0.1312(3) 1.2240(3) 0.0262(7) Uani 1 1 d . . . N10 N 0.0688(4) -0.4047(3) 1.3231(3) 0.0430(9) Uani 1 1 d . . . C10 C 0.8265(4) 0.1883(3) 1.0380(3) 0.0265(7) Uani 1 1 d . . . C11 C 0.8487(4) 0.2610(3) 1.0793(3) 0.0293(8) Uani 1 1 d . . . H11C H 0.8163 0.3312 1.0561 0.035 Uiso 1 1 calc R . . C12 C 0.9194(4) 0.2280(3) 1.1555(3) 0.0302(8) Uani 1 1 d . . . C13 C 0.9664(4) 0.1251(3) 1.1925(3) 0.0356(9) Uani 1 1 d . . . H13C H 1.0113 0.1036 1.2463 0.043 Uiso 1 1 calc R . . C14 C 0.9462(4) 0.0546(3) 1.1495(4) 0.0393(10) Uani 1 1 d . . . H14C H 0.9790 -0.0155 1.1727 0.047 Uiso 1 1 calc R . . C15 C 0.8780(4) 0.0865(3) 1.0721(3) 0.0338(9) Uani 1 1 d . . . H15C H 0.8662 0.0381 1.0421 0.041 Uiso 1 1 calc R . . C16 C 0.9471(4) 0.3041(3) 1.1948(3) 0.0332(8) Uani 1 1 d . . . C18 C 0.3903(4) -0.0341(3) 0.7165(3) 0.0327(8) Uani 1 1 d . . . H18C H 0.4271 -0.0678 0.7745 0.039 Uiso 1 1 calc R . . C19 C 0.3885(4) -0.0858(3) 0.6516(3) 0.0355(9) Uani 1 1 d . . . C20 C 0.3373(5) -0.0384(4) 0.5655(4) 0.0432(10) Uani 1 1 d . . . H20C H 0.3359 -0.0746 0.5220 0.052 Uiso 1 1 calc R . . C21 C 0.2885(5) 0.0629(4) 0.5446(4) 0.0495(12) Uani 1 1 d . . . H21C H 0.2556 0.0974 0.4848 0.059 Uiso 1 1 calc R . . C22 C 0.2867(5) 0.1151(4) 0.6091(4) 0.0492(12) Uani 1 1 d . . . H22C H 0.2503 0.1838 0.5941 0.059 Uiso 1 1 calc R . . C23 C 0.3380(4) 0.0675(4) 0.6963(3) 0.0354(9) Uani 1 1 d . . . C24 C 0.4392(5) -0.1924(4) 0.6757(4) 0.0459(11) Uani 1 1 d . . . C25 C 0.1933(4) -0.0604(3) 1.3105(3) 0.0245(7) Uani 1 1 d . . . C26 C 0.1761(4) -0.1499(3) 1.2888(3) 0.0261(7) Uani 1 1 d . . . H26C H 0.2189 -0.1497 1.2237 0.031 Uiso 1 1 calc R . . C27 C 0.0961(4) -0.2389(3) 1.3629(3) 0.0296(8) Uani 1 1 d . . . C28 C 0.0322(4) -0.2415(3) 1.4588(3) 0.0345(9) Uani 1 1 d . . . H28C H -0.0226 -0.3028 1.5089 0.041 Uiso 1 1 calc R . . C29 C 0.0504(4) -0.1526(3) 1.4793(3) 0.0331(8) Uani 1 1 d . . . H29C H 0.0076 -0.1533 1.5446 0.040 Uiso 1 1 calc R . . C30 C 0.1295(4) -0.0627(3) 1.4069(3) 0.0293(8) Uani 1 1 d . . . H30C H 0.1404 -0.0025 1.4227 0.035 Uiso 1 1 calc R . . C31 C 0.0799(4) -0.3309(3) 1.3395(3) 0.0323(8) Uani 1 1 d . . . H6O H 0.756(3) 0.640(3) 0.616(3) 0.003(7) Uiso 1 1 d . . . H6O1 H 0.770(9) 0.727(8) 0.674(8) 0.16(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0508(2) 0.02524(16) 0.03941(18) -0.01634(13) -0.00921(14) -0.00824(13) S1 0.0260(6) 0.0176(5) 0.0223(5) -0.0079(4) -0.0080(5) -0.0011(4) O1 0.034(3) 0.020(2) 0.037(3) -0.014(2) -0.012(2) 0.004(2) N1 0.0384(18) 0.0281(16) 0.0325(17) -0.0127(14) -0.0105(14) -0.0054(14) C1 0.050(2) 0.0203(17) 0.033(2) -0.0041(15) -0.0167(18) -0.0049(16) O2 0.020(2) 0.033(3) 0.044(3) -0.019(2) -0.005(2) -0.003(2) N2 0.0370(17) 0.0227(15) 0.0371(18) -0.0147(14) -0.0126(14) -0.0060(13) C2 0.043(2) 0.032(2) 0.0267(19) -0.0033(16) -0.0107(17) -0.0080(17) O3 0.043(3) 0.027(3) 0.021(2) -0.006(2) -0.005(2) -0.003(2) N3 0.042(2) 0.0349(18) 0.043(2) -0.0180(16) -0.0254(16) 0.0123(15) C3 0.046(2) 0.029(2) 0.054(3) -0.0154(19) -0.028(2) 0.0104(18) O4 0.039(3) 0.025(3) 0.034(3) -0.016(2) -0.016(2) 0.000(2) N4 0.045(2) 0.043(2) 0.0403(19) -0.0225(17) -0.0273(17) 0.0123(16) C4 0.035(2) 0.036(2) 0.053(3) -0.023(2) -0.0183(19) 0.0075(17) O5 0.0409(15) 0.0251(13) 0.0322(14) -0.0178(11) -0.0049(12) 0.0009(11) N5 0.0419(19) 0.0228(15) 0.0311(16) -0.0138(13) -0.0040(14) -0.0012(13) C5 0.041(2) 0.0222(18) 0.046(2) -0.0187(17) -0.0042(18) 0.0021(16) O6 0.086(3) 0.059(2) 0.069(2) -0.037(2) -0.058(2) 0.039(2) N6 0.0352(17) 0.0224(15) 0.0307(16) -0.0157(13) -0.0017(13) 0.0006(13) C6 0.051(2) 0.0255(19) 0.032(2) -0.0126(16) -0.0073(18) -0.0078(17) O7 0.0479(17) 0.0257(13) 0.0290(14) -0.0087(11) -0.0071(12) -0.0147(12) N7 0.0378(18) 0.0208(15) 0.0334(17) -0.0097(13) -0.0134(14) -0.0007(13) C7 0.0295(18) 0.0265(18) 0.0240(17) -0.0112(14) -0.0017(14) -0.0061(14) O8 0.069(2) 0.0388(18) 0.0467(19) -0.0231(16) -0.0139(17) 0.0068(16) N8 0.051(2) 0.037(2) 0.052(2) -0.0245(18) -0.0188(18) -0.0010(17) C8 0.040(2) 0.031(2) 0.045(2) -0.0154(18) -0.0223(19) 0.0015(17) O9 0.258(10) 0.159(7) 0.141(7) -0.073(6) -0.093(7) 0.025(7) N9 0.105(4) 0.047(3) 0.062(3) -0.026(2) -0.041(3) 0.017(3) C9 0.0304(18) 0.0223(17) 0.0294(18) -0.0114(14) -0.0117(15) 0.0017(14) N10 0.047(2) 0.0314(19) 0.053(2) -0.0235(17) -0.0018(18) -0.0074(16) C10 0.0241(17) 0.0240(17) 0.0329(19) -0.0122(15) -0.0069(14) -0.0059(13) C11 0.0284(18) 0.0228(17) 0.038(2) -0.0137(16) -0.0078(16) -0.0025(14) C12 0.0268(18) 0.0302(19) 0.039(2) -0.0191(17) -0.0080(16) -0.0034(15) C13 0.033(2) 0.034(2) 0.047(2) -0.0172(18) -0.0203(18) 0.0005(16) C14 0.037(2) 0.0257(19) 0.059(3) -0.0179(19) -0.017(2) 0.0042(16) C15 0.032(2) 0.0262(19) 0.050(2) -0.0217(18) -0.0099(18) -0.0030(15) C16 0.034(2) 0.031(2) 0.036(2) -0.0129(17) -0.0125(17) -0.0009(16) C18 0.034(2) 0.035(2) 0.0287(19) -0.0097(16) -0.0118(16) 0.0004(16) C19 0.039(2) 0.036(2) 0.032(2) -0.0140(17) -0.0082(17) -0.0019(17) C20 0.049(3) 0.050(3) 0.041(2) -0.023(2) -0.022(2) 0.004(2) C21 0.062(3) 0.056(3) 0.040(2) -0.019(2) -0.033(2) 0.009(2) C22 0.065(3) 0.049(3) 0.046(3) -0.022(2) -0.035(2) 0.018(2) C23 0.036(2) 0.039(2) 0.037(2) -0.0173(18) -0.0179(17) 0.0063(17) C24 0.061(3) 0.043(3) 0.039(2) -0.016(2) -0.022(2) 0.003(2) C25 0.0272(17) 0.0205(16) 0.0281(17) -0.0112(14) -0.0081(14) 0.0015(13) C26 0.0320(19) 0.0241(17) 0.0259(17) -0.0130(14) -0.0088(14) 0.0040(14) C27 0.033(2) 0.0216(17) 0.037(2) -0.0153(15) -0.0094(16) 0.0024(14) C28 0.040(2) 0.0254(19) 0.036(2) -0.0130(16) -0.0026(17) -0.0041(16) C29 0.042(2) 0.033(2) 0.0273(18) -0.0162(16) -0.0054(16) 0.0020(17) C30 0.038(2) 0.0245(18) 0.0301(18) -0.0140(15) -0.0112(16) 0.0031(15) C31 0.034(2) 0.0272(19) 0.035(2) -0.0133(16) -0.0042(16) -0.0054(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N10 2.184(4) 2_657 ? Ag1 N8 2.187(4) 2_767 ? Ag1 O8 2.386(4) . ? Ag1 O7 2.438(3) . ? S1 O1 1.443(5) . ? S1 O1 1.443(5) 2_657 ? S1 O3 1.453(5) . ? S1 O3 1.453(5) 2_657 ? S1 O4 1.465(5) 2_657 ? S1 O4 1.465(5) . ? S1 O2 1.538(5) 2_657 ? S1 O2 1.538(5) . ? O1 O3 1.614(7) 2_657 ? O1 O4 1.634(7) 2_657 ? O1 O2 1.760(7) 2_657 ? N1 C7 1.344(5) . ? N1 C2 1.453(5) . ? C1 N7 1.474(5) . ? C1 C2 1.515(6) . ? O2 O1 1.760(7) 2_657 ? O2 O3 1.767(8) 2_657 ? O2 O4 1.807(8) 2_657 ? N2 C7 1.374(5) . ? N2 C10 1.395(5) . ? O3 O1 1.614(7) 2_657 ? O3 O4 1.650(7) 2_657 ? O3 O2 1.767(8) 2_657 ? N3 C8 1.352(5) . ? N3 C4 1.453(5) . ? C3 N7 1.468(5) . ? C3 C4 1.521(6) . ? O4 O1 1.634(7) 2_657 ? O4 O3 1.650(7) 2_657 ? O4 O2 1.807(8) 2_657 ? N4 C8 1.377(5) . ? N4 C23 1.398(5) . ? O5 C9 1.229(4) . ? N5 C9 1.354(5) . ? N5 C6 1.451(5) . ? C5 N7 1.461(5) . ? C5 C6 1.526(6) . ? O6 C8 1.213(5) . ? N6 C9 1.383(4) . ? N6 C25 1.402(5) . ? O7 C7 1.246(4) . ? N8 C16 1.148(5) . ? N8 Ag1 2.187(4) 2_767 ? N9 C24 1.138(6) . ? N10 C31 1.134(5) . ? N10 Ag1 2.184(4) 2_657 ? C10 C15 1.395(5) . ? C10 C11 1.397(5) . ? C11 C12 1.395(5) . ? C12 C13 1.392(6) . ? C12 C16 1.435(5) . ? C13 C14 1.384(6) . ? C14 C15 1.391(6) . ? C18 C19 1.392(6) . ? C18 C23 1.401(6) . ? C19 C20 1.388(6) . ? C19 C24 1.449(6) . ? C20 C21 1.382(7) . ? C21 C22 1.386(7) . ? C22 C23 1.402(6) . ? C25 C30 1.398(5) . ? C25 C26 1.400(5) . ? C26 C27 1.389(5) . ? C27 C28 1.390(6) . ? C27 C31 1.445(5) . ? C28 C29 1.384(5) . ? C29 C30 1.384(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N10 Ag1 N8 144.36(15) 2_657 2_767 ? N10 Ag1 O8 107.85(14) 2_657 . ? N8 Ag1 O8 94.13(14) 2_767 . ? N10 Ag1 O7 89.10(12) 2_657 . ? N8 Ag1 O7 111.66(13) 2_767 . ? O8 Ag1 O7 106.38(12) . . ? O1 S1 O1 179.996(1) . 2_657 ? O1 S1 O3 112.3(3) . . ? O1 S1 O3 67.7(3) 2_657 . ? O1 S1 O3 67.7(3) . 2_657 ? O1 S1 O3 112.3(3) 2_657 2_657 ? O3 S1 O3 180.0(4) . 2_657 ? O1 S1 O4 68.3(3) . 2_657 ? O1 S1 O4 111.7(3) 2_657 2_657 ? O3 S1 O4 68.9(3) . 2_657 ? O3 S1 O4 111.1(3) 2_657 2_657 ? O1 S1 O4 111.7(3) . . ? O1 S1 O4 68.3(3) 2_657 . ? O3 S1 O4 111.1(3) . . ? O3 S1 O4 68.9(3) 2_657 . ? O4 S1 O4 179.999(1) 2_657 . ? O1 S1 O2 72.3(3) . 2_657 ? O1 S1 O2 107.7(3) 2_657 2_657 ? O3 S1 O2 72.4(3) . 2_657 ? O3 S1 O2 107.6(3) 2_657 2_657 ? O4 S1 O2 106.1(3) 2_657 2_657 ? O4 S1 O2 73.9(3) . 2_657 ? O1 S1 O2 107.7(3) . . ? O1 S1 O2 72.3(3) 2_657 . ? O3 S1 O2 107.6(3) . . ? O3 S1 O2 72.4(3) 2_657 . ? O4 S1 O2 73.9(3) 2_657 . ? O4 S1 O2 106.1(3) . . ? O2 S1 O2 180.0 2_657 . ? S1 O1 O3 56.4(3) . 2_657 ? S1 O1 O4 56.5(3) . 2_657 ? O3 O1 O4 95.7(4) 2_657 2_657 ? S1 O1 O2 56.4(2) . 2_657 ? O3 O1 O2 91.3(4) 2_657 2_657 ? O4 O1 O2 89.9(4) 2_657 2_657 ? C7 N1 C2 121.1(3) . . ? N7 C1 C2 111.2(3) . . ? S1 O2 O1 51.4(2) . 2_657 ? S1 O2 O3 51.6(2) . 2_657 ? O1 O2 O3 86.0(3) 2_657 2_657 ? S1 O2 O4 51.2(2) . 2_657 ? O1 O2 O4 84.8(3) 2_657 2_657 ? O3 O2 O4 84.7(3) 2_657 2_657 ? C7 N2 C10 126.8(3) . . ? N1 C2 C1 111.6(3) . . ? S1 O3 O1 55.9(3) . 2_657 ? S1 O3 O4 55.9(3) . 2_657 ? O1 O3 O4 95.0(4) 2_657 2_657 ? S1 O3 O2 56.0(3) . 2_657 ? O1 O3 O2 90.7(4) 2_657 2_657 ? O4 O3 O2 89.2(3) 2_657 2_657 ? C8 N3 C4 121.8(4) . . ? N7 C3 C4 112.4(3) . . ? S1 O4 O1 55.2(2) . 2_657 ? S1 O4 O3 55.2(2) . 2_657 ? O1 O4 O3 94.2(4) 2_657 2_657 ? S1 O4 O2 54.9(2) . 2_657 ? O1 O4 O2 88.7(4) 2_657 2_657 ? O3 O4 O2 88.5(3) 2_657 2_657 ? C8 N4 C23 125.7(3) . . ? N3 C4 C3 112.2(4) . . ? C9 N5 C6 121.8(3) . . ? N7 C5 C6 111.9(3) . . ? C9 N6 C25 127.4(3) . . ? N5 C6 C5 112.0(3) . . ? C7 O7 Ag1 125.2(2) . . ? C5 N7 C3 112.0(3) . . ? C5 N7 C1 111.3(3) . . ? C3 N7 C1 111.0(3) . . ? O7 C7 N1 123.5(4) . . ? O7 C7 N2 122.2(3) . . ? N1 C7 N2 114.3(3) . . ? C16 N8 Ag1 162.0(4) . 2_767 ? O6 C8 N3 123.1(4) . . ? O6 C8 N4 123.5(4) . . ? N3 C8 N4 113.4(3) . . ? O5 C9 N5 124.1(3) . . ? O5 C9 N6 122.7(3) . . ? N5 C9 N6 113.1(3) . . ? C31 N10 Ag1 165.6(4) . 2_657 ? N2 C10 C15 117.5(3) . . ? N2 C10 C11 123.2(3) . . ? C15 C10 C11 119.4(3) . . ? C12 C11 C10 118.5(3) . . ? C13 C12 C11 122.2(4) . . ? C13 C12 C16 119.2(4) . . ? C11 C12 C16 118.6(4) . . ? C14 C13 C12 118.7(4) . . ? C13 C14 C15 120.0(4) . . ? C14 C15 C10 121.1(4) . . ? N8 C16 C12 177.4(5) . . ? C19 C18 C23 120.0(4) . . ? C20 C19 C18 121.5(4) . . ? C20 C19 C24 119.3(4) . . ? C18 C19 C24 119.1(4) . . ? C21 C20 C19 118.3(4) . . ? C20 C21 C22 121.3(4) . . ? C21 C22 C23 120.6(4) . . ? N4 C23 C18 117.5(4) . . ? N4 C23 C22 124.3(4) . . ? C18 C23 C22 118.2(4) . . ? N9 C24 C19 178.1(5) . . ? C30 C25 C26 119.1(3) . . ? C30 C25 N6 124.5(3) . . ? C26 C25 N6 116.4(3) . . ? C27 C26 C25 119.5(3) . . ? C26 C27 C28 121.6(3) . . ? C26 C27 C31 118.9(3) . . ? C28 C27 C31 119.6(4) . . ? C29 C28 C27 118.3(4) . . ? C28 C29 C30 121.5(4) . . ? C29 C30 C25 120.1(3) . . ? N10 C31 C27 178.2(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.137 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.093 #===END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 281963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1b _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 N10 O3' _chemical_formula_weight 578.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.0827(18) _cell_length_b 13.993(2) _cell_length_c 18.274(3) _cell_angle_alpha 73.362(3) _cell_angle_beta 85.694(3) _cell_angle_gamma 63.147(2) _cell_volume 2853.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9809 _exptl_absorpt_correction_T_max 0.9936 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20199 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.1119 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10021 _reflns_number_gt 5694 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1088P)^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 10021 _refine_ls_number_parameters 794 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1380 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2133 _refine_ls_wR_factor_gt 0.1920 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.8862(2) 0.8515(2) 0.49914(15) 0.0340(7) Uani 1 1 d . . . N1 N 0.7515(3) 0.9872(3) 0.40565(18) 0.0321(8) Uani 1 1 d . . . H14 H 0.7397 1.0364 0.3605 0.039 Uiso 1 1 calc R . . C1 C 0.6029(3) 0.9263(3) 0.4019(2) 0.0276(9) Uani 1 1 d . . . H35A H 0.5299 0.9316 0.4242 0.033 Uiso 1 1 calc R . . H35B H 0.5857 0.9696 0.3472 0.033 Uiso 1 1 calc R . . O2 O 0.9697(2) 0.4756(2) 0.60081(15) 0.0340(7) Uani 1 1 d . . . N2 N 0.9381(3) 0.9525(3) 0.39412(18) 0.0301(8) Uani 1 1 d . . . H12 H 0.9146 0.9932 0.3465 0.036 Uiso 1 1 calc R . . C2 C 0.6533(3) 0.9768(3) 0.4427(2) 0.0312(10) Uani 1 1 d . . . H42A H 0.5936 1.0516 0.4440 0.037 Uiso 1 1 calc R . . H42B H 0.6773 0.9294 0.4961 0.037 Uiso 1 1 calc R . . O3 O 0.9456(3) 0.8755(2) 0.23713(16) 0.0488(8) Uani 1 1 d . . . N3 N 0.8500(3) 0.6515(2) 0.53112(18) 0.0309(8) Uani 1 1 d . . . H13 H 0.8348 0.7223 0.5194 0.037 Uiso 1 1 calc R . . C3 C 0.6590(3) 0.7321(3) 0.4727(2) 0.0305(9) Uani 1 1 d . . . H38A H 0.6012 0.7141 0.4560 0.037 Uiso 1 1 calc R . . H38B H 0.6269 0.7690 0.5137 0.037 Uiso 1 1 calc R . . O4 O 0.4293(2) 1.5191(2) -0.09873(15) 0.0360(7) Uani 1 1 d . . . N4 N 1.0213(3) 0.6165(2) 0.58212(18) 0.0315(8) Uani 1 1 d . . . H16 H 1.0034 0.6855 0.5546 0.038 Uiso 1 1 calc R . . C4 C 0.7684(3) 0.6239(3) 0.5047(2) 0.0299(9) Uani 1 1 d . . . H66A H 0.7507 0.5728 0.5475 0.036 Uiso 1 1 calc R . . H66B H 0.8009 0.5860 0.4643 0.036 Uiso 1 1 calc R . . O5 O 0.7937(2) 1.1423(2) 0.27260(15) 0.0377(7) Uani 1 1 d . . . N5 N 0.8831(3) 0.7548(3) 0.31374(18) 0.0345(8) Uani 1 1 d . . . H15 H 0.9018 0.6944 0.3526 0.041 Uiso 1 1 calc R . . C5 C 0.6880(3) 0.7812(3) 0.3360(2) 0.0317(10) Uani 1 1 d . . . H33A H 0.6101 0.8179 0.3106 0.038 Uiso 1 1 calc R . . H33B H 0.7172 0.6995 0.3469 0.038 Uiso 1 1 calc R . . O6 O 0.7420(2) 1.1613(2) 0.00534(16) 0.0419(8) Uani 1 1 d . . . N6 N 1.0734(3) 0.7086(3) 0.31745(19) 0.0388(9) Uani 1 1 d . . . H27 H 1.0785 0.6463 0.3500 0.047 Uiso 1 1 calc R . . C6 C 0.7653(3) 0.8177(3) 0.2828(2) 0.0351(10) Uani 1 1 d . . . H37A H 0.7597 0.8064 0.2325 0.042 Uiso 1 1 calc R . . H37B H 0.7400 0.8983 0.2751 0.042 Uiso 1 1 calc R . . N7 N 0.6813(3) 0.8091(2) 0.40802(16) 0.0249(7) Uani 1 1 d . . . C7 C 1.0514(3) 0.9239(3) 0.4162(2) 0.0276(9) Uani 1 1 d . . . N8 N 1.3473(4) 1.0017(3) 0.2771(2) 0.0537(11) Uani 1 1 d . . . C8 C 1.1162(3) 0.9550(3) 0.3606(2) 0.0286(9) Uani 1 1 d . . . H20 H 1.0847 0.9917 0.3093 0.034 Uiso 1 1 calc R . . N9 N 1.2780(4) 0.3034(4) 0.8815(3) 0.0723(14) Uani 1 1 d . . . C9 C 1.2288(3) 0.9328(3) 0.3790(2) 0.0309(10) Uani 1 1 d . . . N10 N 1.3958(9) 0.8659(9) 0.1261(6) 0.067(3) Uani 0.441(6) 1 d P . . C10 C 1.2762(3) 0.8768(3) 0.4539(2) 0.0327(10) Uani 1 1 d . . . H50 H 1.3527 0.8597 0.4668 0.039 Uiso 1 1 calc R . . N11 N 0.4986(3) 1.3465(3) -0.01479(18) 0.0324(8) Uani 1 1 d . . . H11 H 0.5597 1.2821 0.0024 0.039 Uiso 1 1 calc R . . C11 C 1.2095(3) 0.8469(3) 0.5088(2) 0.0332(10) Uani 1 1 d . . . H57 H 1.2411 0.8091 0.5600 0.040 Uiso 1 1 calc R . . N12 N 0.6190(3) 1.3955(3) -0.09547(18) 0.0331(8) Uani 1 1 d . . . H10 H 0.6741 1.3319 -0.0687 0.040 Uiso 1 1 calc R . . C12 C 1.0987(3) 0.8700(3) 0.4915(2) 0.0287(9) Uani 1 1 d . . . H25 H 1.0544 0.8495 0.5307 0.034 Uiso 1 1 calc R . . N13 N 0.6365(3) 1.2453(2) 0.19143(17) 0.0297(8) Uani 1 1 d . . . H7 H 0.6006 1.3026 0.1514 0.036 Uiso 1 1 calc R . . C13 C 1.2932(4) 0.9707(3) 0.3219(3) 0.0362(10) Uani 1 1 d . . . N14 N 0.7770(3) 1.3031(2) 0.18308(18) 0.0298(8) Uani 1 1 d . . . H5 H 0.7305 1.3607 0.1466 0.036 Uiso 1 1 calc R . . C14 C 1.1223(3) 0.5617(3) 0.6308(2) 0.0278(9) Uani 1 1 d . . . N15 N 0.7430(3) 1.0121(3) 0.0976(2) 0.0425(10) Uani 1 1 d . . . H48 H 0.7800 0.9599 0.1397 0.051 Uiso 1 1 calc R . . C15 C 1.1345(3) 0.4885(3) 0.7028(2) 0.0265(9) Uani 1 1 d . . . H28 H 1.0754 0.4676 0.7209 0.032 Uiso 1 1 calc R . . N16 N 0.8884(3) 1.0587(3) 0.09990(19) 0.0426(10) Uani 1 1 d . . . H22 H 0.9059 1.0098 0.1455 0.051 Uiso 1 1 calc R . . C16 C 1.2348(4) 0.4460(3) 0.7480(2) 0.0334(10) Uani 1 1 d . . . N17 N 0.4969(3) 1.1757(2) 0.11141(17) 0.0258(7) Uani 1 1 d . . . C17 C 1.3211(4) 0.4771(3) 0.7230(3) 0.0412(11) Uani 1 1 d . . . H67 H 1.3883 0.4485 0.7552 0.049 Uiso 1 1 calc R . . N18 N 0.4671(3) 1.7185(3) -0.4010(2) 0.0530(11) Uani 1 1 d . . . C18 C 1.3086(4) 0.5498(4) 0.6513(3) 0.0505(13) Uani 1 1 d . . . H83 H 1.3670 0.5719 0.6336 0.061 Uiso 1 1 calc R . . N19 N 1.1101(3) 1.4737(4) 0.0518(2) 0.0540(11) Uani 1 1 d . . . C19 C 1.2105(4) 0.5902(3) 0.6055(3) 0.0406(11) Uani 1 1 d . . . H49 H 1.2030 0.6386 0.5555 0.049 Uiso 1 1 calc R . . N20 N 1.0460(3) 1.3131(3) -0.1599(2) 0.0498(10) Uani 1 1 d . . . C20 C 1.2542(4) 0.3669(4) 0.8227(3) 0.0436(12) Uani 1 1 d . . . C21 C 1.1766(4) 0.7171(3) 0.3049(3) 0.0437(12) Uani 1 1 d . . . C22 C 1.2600(4) 0.6612(4) 0.3640(3) 0.0490(13) Uani 1 1 d . . . H79 H 1.2457 0.6194 0.4110 0.059 Uiso 1 1 calc R . . C23 C 1.3641(5) 0.6648(5) 0.3565(5) 0.080(2) Uani 1 1 d . . . C24 C 1.3883(7) 0.7232(7) 0.2869(7) 0.119(4) Uani 1 1 d . . . H1 H 1.4604 0.7246 0.2804 0.142 Uiso 1 1 calc R . . C25 C 1.4435(9) 0.6202(8) 0.4054(6) 0.054(3) Uani 0.559(6) 1 d P . . C26 C 0.3975(3) 1.2463(3) 0.0559(2) 0.0307(9) Uani 1 1 d . . . H53A H 0.3263 1.2543 0.0820 0.037 Uiso 1 1 calc R . . H53B H 0.4035 1.2098 0.0155 0.037 Uiso 1 1 calc R . . C27 C 0.3912(3) 1.3611(3) 0.0194(2) 0.0307(9) Uani 1 1 d . . . H46A H 0.3268 1.4058 -0.0202 0.037 Uiso 1 1 calc R . . H46B H 0.3780 1.4011 0.0586 0.037 Uiso 1 1 calc R . . C28 C 0.4742(3) 1.2029(3) 0.1847(2) 0.0287(9) Uani 1 1 d . . . H19A H 0.4344 1.1615 0.2166 0.034 Uiso 1 1 calc R . . H19B H 0.4229 1.2837 0.1751 0.034 Uiso 1 1 calc R . . C29 C 0.5848(3) 1.1728(3) 0.2276(2) 0.0293(9) Uani 1 1 d . . . H34A H 0.5682 1.1777 0.2805 0.035 Uiso 1 1 calc R . . H34B H 0.6401 1.0947 0.2306 0.035 Uiso 1 1 calc R . . C30 C 0.5399(4) 1.0562(3) 0.1193(2) 0.0345(10) Uani 1 1 d . . . H60A H 0.4773 1.0433 0.1039 0.041 Uiso 1 1 calc R . . H60B H 0.5639 1.0133 0.1736 0.041 Uiso 1 1 calc R . . C31 C 0.6404(4) 1.0143(3) 0.0708(2) 0.0416(11) Uani 1 1 d . . . H70A H 0.6573 0.9380 0.0705 0.050 Uiso 1 1 calc R . . H70B H 0.6188 1.0630 0.0175 0.050 Uiso 1 1 calc R . . C32 C 0.6500(3) 1.4575(3) -0.1595(2) 0.0266(9) Uani 1 1 d . . . C33 C 0.5759(3) 1.5261(3) -0.2233(2) 0.0270(9) Uani 1 1 d . . . H32 H 0.5000 1.5338 -0.2244 0.032 Uiso 1 1 calc R . . C34 C 0.6127(3) 1.5839(3) -0.2863(2) 0.0284(9) Uani 1 1 d . . . C35 C 0.7229(3) 1.5749(3) -0.2868(2) 0.0325(10) Uani 1 1 d . . . H61 H 0.7471 1.6153 -0.3295 0.039 Uiso 1 1 calc R . . C36 C 0.7962(3) 1.5047(3) -0.2227(2) 0.0339(10) Uani 1 1 d . . . H51 H 0.8727 1.4956 -0.2219 0.041 Uiso 1 1 calc R . . C37 C 0.7606(3) 1.4484(3) -0.1605(2) 0.0317(10) Uani 1 1 d . . . H21 H 0.8124 1.4020 -0.1169 0.038 Uiso 1 1 calc R . . C38 C 0.5318(4) 1.6579(4) -0.3507(2) 0.0358(10) Uani 1 1 d . . . C39 C 0.8822(3) 1.3007(3) 0.1986(2) 0.0290(9) Uani 1 1 d . . . C40 C 0.9225(3) 1.3624(3) 0.1416(2) 0.0281(9) Uani 1 1 d . . . H26 H 0.8793 1.4055 0.0941 0.034 Uiso 1 1 calc R . . C41 C 1.0269(3) 1.3606(3) 0.1548(2) 0.0321(10) Uani 1 1 d . . . C42 C 1.0918(3) 1.2978(3) 0.2241(2) 0.0331(10) Uani 1 1 d . . . H63 H 1.1637 1.2960 0.2321 0.040 Uiso 1 1 calc R . . C43 C 1.0499(3) 1.2387(3) 0.2804(2) 0.0345(10) Uani 1 1 d . . . H40 H 1.0930 1.1962 0.3280 0.041 Uiso 1 1 calc R . . C44 C 0.9453(3) 1.2399(3) 0.2688(2) 0.0312(10) Uani 1 1 d . . . H43 H 0.9169 1.1994 0.3087 0.037 Uiso 1 1 calc R . . C45 C 1.0697(4) 1.4250(4) 0.0961(3) 0.0416(11) Uani 1 1 d . . . C46 C 0.9658(4) 1.1009(3) 0.0740(2) 0.0360(11) Uani 1 1 d . . . C47 C 0.9634(4) 1.1641(3) -0.0003(2) 0.0358(10) Uani 1 1 d . . . H41 H 0.9047 1.1831 -0.0371 0.043 Uiso 1 1 calc R . . C48 C 1.0484(4) 1.1995(3) -0.0204(2) 0.0348(10) Uani 1 1 d . . . C49 C 1.1360(4) 1.1737(3) 0.0314(2) 0.0389(11) Uani 1 1 d . . . H71 H 1.1923 1.1996 0.0165 0.047 Uiso 1 1 calc R . . C50 C 1.1387(4) 1.1101(4) 0.1041(3) 0.0453(12) Uani 1 1 d . . . H78 H 1.1988 1.0897 0.1402 0.054 Uiso 1 1 calc R . . C51 C 1.0553(4) 1.0752(3) 0.1258(2) 0.0444(12) Uani 1 1 d . . . H76 H 1.0581 1.0326 0.1772 0.053 Uiso 1 1 calc R . . C52 C 1.0469(3) 1.2633(4) -0.0978(2) 0.0358(10) Uani 1 1 d . . . C53 C 0.8598(3) 0.9254(3) 0.4370(2) 0.0278(9) Uani 1 1 d . . . C54 C 0.9482(3) 0.5747(3) 0.5729(2) 0.0277(9) Uani 1 1 d . . . C55 C 0.9655(4) 0.7852(3) 0.2854(2) 0.0347(10) Uani 1 1 d . . . C56 C 0.5099(3) 1.4252(3) -0.0706(2) 0.0260(9) Uani 1 1 d . . . C57 C 0.7393(3) 1.2258(3) 0.2184(2) 0.0266(9) Uani 1 1 d . . . C58 C 0.7863(4) 1.0834(3) 0.0634(2) 0.0349(10) Uani 1 1 d . . . C82 C 1.2001(5) 0.7755(4) 0.2352(3) 0.0640(16) Uani 1 1 d . . . H82 H 1.1446 0.8126 0.1932 0.077 Uiso 1 1 calc R . . N10A N 1.5097(7) 0.5793(7) 0.4553(5) 0.077(3) Uani 0.559(6) 1 d P . . C23A C 1.3031(8) 0.7791(6) 0.2277(6) 0.102(3) Uani 1 1 d . . . C25A C 1.3587(9) 0.8229(9) 0.1771(6) 0.044(3) Uani 0.441(6) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0342(16) 0.0229(14) 0.0313(16) 0.0122(13) -0.0141(13) -0.0107(13) N1 0.029(2) 0.0241(17) 0.0300(18) 0.0079(15) -0.0109(15) -0.0077(15) C1 0.020(2) 0.022(2) 0.032(2) -0.0010(17) -0.0031(17) -0.0058(17) O2 0.0346(16) 0.0175(14) 0.0377(16) 0.0079(12) -0.0085(13) -0.0092(13) N2 0.0274(19) 0.0285(18) 0.0255(17) 0.0085(15) -0.0116(15) -0.0128(16) C2 0.024(2) 0.023(2) 0.036(2) -0.0027(18) -0.0004(18) -0.0055(18) O3 0.060(2) 0.0210(15) 0.0424(18) 0.0113(14) 0.0041(15) -0.0114(15) N3 0.034(2) 0.0150(16) 0.0362(19) 0.0038(15) -0.0104(16) -0.0095(15) C3 0.031(2) 0.028(2) 0.027(2) 0.0034(18) -0.0035(18) -0.0151(19) O4 0.0247(15) 0.0218(14) 0.0383(16) 0.0127(13) -0.0058(13) -0.0025(13) N4 0.036(2) 0.0161(16) 0.0348(19) 0.0080(14) -0.0128(16) -0.0123(15) C4 0.036(2) 0.021(2) 0.025(2) 0.0064(17) -0.0065(18) -0.0122(19) O5 0.0348(17) 0.0248(15) 0.0398(17) 0.0118(13) -0.0151(14) -0.0116(13) N5 0.032(2) 0.0207(17) 0.0315(19) 0.0092(15) 0.0023(16) -0.0056(16) C5 0.034(2) 0.024(2) 0.028(2) 0.0001(18) -0.0101(19) -0.0080(19) O6 0.0362(17) 0.0279(16) 0.0401(17) 0.0115(14) -0.0036(14) -0.0079(14) N6 0.035(2) 0.0230(18) 0.045(2) 0.0059(16) 0.0050(17) -0.0110(17) C6 0.036(3) 0.028(2) 0.022(2) 0.0010(18) -0.0017(19) -0.003(2) N7 0.0223(17) 0.0215(16) 0.0237(17) 0.0021(14) -0.0022(14) -0.0082(14) C7 0.025(2) 0.0182(19) 0.031(2) -0.0016(17) -0.0072(18) -0.0046(17) N8 0.046(3) 0.055(3) 0.055(3) -0.001(2) -0.001(2) -0.026(2) C8 0.031(2) 0.019(2) 0.028(2) -0.0005(17) -0.0058(18) -0.0076(18) N9 0.089(4) 0.081(3) 0.048(3) 0.019(3) -0.039(3) -0.054(3) C9 0.028(2) 0.022(2) 0.038(2) -0.0043(19) -0.0036(19) -0.0088(18) N10 0.064(7) 0.083(8) 0.057(7) -0.017(6) 0.006(5) -0.039(6) C10 0.027(2) 0.027(2) 0.035(2) 0.0029(19) -0.0111(19) -0.0095(19) N11 0.0231(18) 0.0208(17) 0.0340(19) 0.0091(15) -0.0021(15) -0.0029(15) C11 0.034(2) 0.024(2) 0.034(2) 0.0025(18) -0.013(2) -0.0099(19) N12 0.0230(19) 0.0255(18) 0.0296(18) 0.0099(15) -0.0041(15) -0.0028(15) C12 0.029(2) 0.020(2) 0.032(2) 0.0000(17) -0.0068(18) -0.0086(18) N13 0.0290(19) 0.0215(17) 0.0284(18) 0.0103(14) -0.0112(15) -0.0112(15) C13 0.028(2) 0.028(2) 0.043(3) -0.002(2) -0.005(2) -0.008(2) N14 0.0250(18) 0.0197(16) 0.0330(19) 0.0091(14) -0.0112(15) -0.0080(15) C14 0.024(2) 0.019(2) 0.034(2) -0.0022(18) -0.0040(18) -0.0075(18) N15 0.039(2) 0.0237(19) 0.040(2) 0.0083(16) 0.0038(18) -0.0041(17) C15 0.031(2) 0.022(2) 0.025(2) -0.0042(17) -0.0015(17) -0.0127(18) N16 0.039(2) 0.035(2) 0.0279(19) 0.0124(16) -0.0022(17) -0.0062(18) C16 0.034(3) 0.026(2) 0.032(2) -0.0061(19) -0.0105(19) -0.0055(19) N17 0.0251(18) 0.0190(16) 0.0266(17) 0.0041(14) -0.0060(14) -0.0094(14) C17 0.025(2) 0.031(2) 0.059(3) -0.004(2) -0.014(2) -0.008(2) N18 0.042(2) 0.067(3) 0.035(2) 0.010(2) -0.0084(19) -0.025(2) C18 0.037(3) 0.043(3) 0.066(3) 0.002(3) -0.007(2) -0.023(2) N19 0.046(3) 0.070(3) 0.044(2) -0.002(2) -0.002(2) -0.032(2) C19 0.040(3) 0.034(2) 0.042(3) -0.001(2) 0.003(2) -0.017(2) N20 0.033(2) 0.065(3) 0.037(2) -0.003(2) -0.0014(18) -0.016(2) C20 0.043(3) 0.048(3) 0.037(3) -0.001(2) -0.019(2) -0.021(2) C21 0.046(3) 0.026(2) 0.065(3) -0.019(2) 0.026(3) -0.021(2) C22 0.040(3) 0.034(3) 0.079(4) -0.027(3) 0.017(3) -0.017(2) C23 0.046(4) 0.058(4) 0.162(7) -0.070(5) 0.029(5) -0.027(3) C24 0.077(6) 0.066(5) 0.259(12) -0.102(7) 0.102(7) -0.053(5) C25 0.038(6) 0.052(6) 0.069(7) -0.027(5) -0.002(5) -0.012(5) C26 0.030(2) 0.032(2) 0.025(2) 0.0043(18) -0.0065(18) -0.0158(19) C27 0.023(2) 0.030(2) 0.029(2) 0.0045(18) -0.0035(18) -0.0096(18) C28 0.028(2) 0.026(2) 0.026(2) 0.0036(17) -0.0011(17) -0.0132(18) C29 0.029(2) 0.024(2) 0.027(2) 0.0021(17) -0.0031(18) -0.0099(18) C30 0.042(3) 0.026(2) 0.030(2) 0.0018(18) -0.004(2) -0.016(2) C31 0.057(3) 0.024(2) 0.036(2) -0.003(2) 0.007(2) -0.016(2) C32 0.027(2) 0.0179(19) 0.026(2) -0.0011(17) 0.0003(17) -0.0057(17) C33 0.024(2) 0.025(2) 0.027(2) -0.0024(17) -0.0031(17) -0.0089(18) C34 0.031(2) 0.026(2) 0.021(2) -0.0012(17) -0.0008(17) -0.0101(19) C35 0.033(2) 0.034(2) 0.028(2) -0.0023(19) 0.0026(19) -0.017(2) C36 0.025(2) 0.035(2) 0.037(2) -0.002(2) -0.0012(19) -0.014(2) C37 0.026(2) 0.028(2) 0.030(2) 0.0057(18) -0.0086(18) -0.0093(19) C38 0.033(2) 0.046(3) 0.025(2) 0.002(2) -0.001(2) -0.021(2) C39 0.026(2) 0.020(2) 0.032(2) -0.0016(18) -0.0057(18) -0.0056(18) C40 0.022(2) 0.023(2) 0.030(2) -0.0032(18) -0.0016(17) -0.0045(18) C41 0.031(2) 0.028(2) 0.033(2) -0.0049(19) 0.0015(19) -0.0113(19) C42 0.024(2) 0.028(2) 0.041(3) -0.009(2) -0.0054(19) -0.0064(19) C43 0.031(2) 0.024(2) 0.039(2) -0.0031(19) -0.013(2) -0.0053(19) C44 0.036(2) 0.018(2) 0.031(2) 0.0004(18) -0.0021(19) -0.0089(18) C45 0.030(3) 0.049(3) 0.040(3) -0.006(2) -0.003(2) -0.016(2) C46 0.038(3) 0.019(2) 0.032(2) -0.0013(19) 0.003(2) -0.0006(19) C47 0.031(2) 0.030(2) 0.026(2) -0.0004(19) -0.0034(19) -0.001(2) C48 0.032(2) 0.028(2) 0.028(2) -0.0053(19) 0.0001(19) -0.001(2) C49 0.035(3) 0.035(2) 0.037(3) -0.010(2) -0.004(2) -0.007(2) C50 0.043(3) 0.037(3) 0.045(3) -0.010(2) -0.012(2) -0.008(2) C51 0.049(3) 0.031(2) 0.027(2) 0.001(2) -0.008(2) 0.000(2) C52 0.026(2) 0.041(3) 0.029(3) -0.004(2) 0.0004(19) -0.009(2) C53 0.029(2) 0.025(2) 0.028(2) -0.0032(19) -0.0054(19) -0.0136(19) C54 0.029(2) 0.019(2) 0.026(2) 0.0007(17) -0.0030(18) -0.0073(18) C55 0.043(3) 0.020(2) 0.030(2) -0.0002(19) 0.008(2) -0.010(2) C56 0.022(2) 0.024(2) 0.019(2) 0.0064(17) -0.0046(17) -0.0062(18) C57 0.027(2) 0.020(2) 0.025(2) 0.0033(17) -0.0088(18) -0.0072(18) C58 0.034(3) 0.021(2) 0.033(2) 0.005(2) 0.007(2) -0.0062(19) C82 0.071(4) 0.032(3) 0.089(4) -0.024(3) 0.051(3) -0.025(3) N10A 0.049(5) 0.081(6) 0.091(7) -0.030(5) -0.016(5) -0.014(5) C23A 0.098(6) 0.051(4) 0.181(8) -0.065(5) 0.105(6) -0.050(4) C25A 0.045(7) 0.042(6) 0.047(7) -0.013(5) 0.012(6) -0.024(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C53 1.243(4) . ? N1 C53 1.347(5) . ? N1 C2 1.453(5) . ? C1 N7 1.466(4) . ? C1 C2 1.511(5) . ? O2 C54 1.236(4) . ? N2 C53 1.366(5) . ? N2 C7 1.408(5) . ? O3 C55 1.241(5) . ? N3 C54 1.348(5) . ? N3 C4 1.441(5) . ? C3 N7 1.464(5) . ? C3 C4 1.531(5) . ? O4 C56 1.243(4) . ? N4 C54 1.369(5) . ? N4 C14 1.413(5) . ? O5 C57 1.243(4) . ? N5 C55 1.348(5) . ? N5 C6 1.446(5) . ? C5 N7 1.462(5) . ? C5 C6 1.504(6) . ? O6 C58 1.229(4) . ? N6 C55 1.371(5) . ? N6 C21 1.405(6) . ? C7 C8 1.375(5) . ? C7 C12 1.400(5) . ? N8 C13 1.161(5) . ? C8 C9 1.407(5) . ? N9 C20 1.138(5) . ? C9 C10 1.396(5) . ? C9 C13 1.426(6) . ? N10 C25A 1.158(13) . ? C10 C11 1.378(6) . ? N11 C56 1.325(5) . ? N11 C27 1.446(5) . ? C11 C12 1.375(5) . ? N12 C56 1.375(5) . ? N12 C32 1.397(5) . ? N13 C57 1.348(5) . ? N13 C29 1.446(5) . ? N14 C57 1.365(5) . ? N14 C39 1.410(5) . ? C14 C15 1.384(5) . ? C14 C19 1.390(6) . ? N15 C58 1.344(5) . ? N15 C31 1.448(6) . ? C15 C16 1.391(5) . ? N16 C46 1.381(6) . ? N16 C58 1.390(5) . ? C16 C17 1.388(6) . ? C16 C20 1.445(6) . ? N17 C28 1.468(5) . ? N17 C30 1.469(5) . ? N17 C26 1.470(5) . ? C17 C18 1.378(6) . ? N18 C38 1.141(5) . ? C18 C19 1.379(6) . ? N19 C45 1.160(5) . ? N20 C52 1.146(5) . ? C21 C22 1.376(7) . ? C21 C82 1.398(6) . ? C22 C23 1.380(7) . ? C23 C25 1.225(11) . ? C23 C24 1.402(11) . ? C24 C23A 1.391(12) . ? C24 C25A 2.036(16) . ? C25 N10A 1.132(12) . ? C26 C27 1.520(5) . ? C28 C29 1.523(5) . ? C30 C31 1.511(6) . ? C32 C33 1.381(5) . ? C32 C37 1.394(5) . ? C33 C34 1.395(5) . ? C34 C35 1.388(6) . ? C34 C38 1.441(5) . ? C35 C36 1.384(5) . ? C36 C37 1.367(5) . ? C39 C40 1.387(5) . ? C39 C44 1.397(5) . ? C40 C41 1.393(6) . ? C41 C42 1.394(5) . ? C41 C45 1.445(6) . ? C42 C43 1.371(6) . ? C43 C44 1.392(6) . ? C46 C47 1.386(5) . ? C46 C51 1.410(6) . ? C47 C48 1.395(6) . ? C48 C49 1.389(6) . ? C48 C52 1.437(6) . ? C49 C50 1.364(6) . ? C50 C51 1.374(6) . ? C82 C23A 1.367(9) . ? C23A C25A 1.317(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C53 N1 C2 123.3(3) . . ? N7 C1 C2 111.9(3) . . ? C53 N2 C7 128.5(3) . . ? N1 C2 C1 112.3(3) . . ? C54 N3 C4 123.6(3) . . ? N7 C3 C4 111.7(3) . . ? C54 N4 C14 127.5(3) . . ? N3 C4 C3 108.4(3) . . ? C55 N5 C6 122.6(3) . . ? N7 C5 C6 111.9(3) . . ? C55 N6 C21 128.2(4) . . ? N5 C6 C5 110.8(3) . . ? C5 N7 C3 113.2(3) . . ? C5 N7 C1 113.1(3) . . ? C3 N7 C1 112.4(3) . . ? C8 C7 C12 119.2(4) . . ? C8 C7 N2 117.4(3) . . ? C12 C7 N2 123.4(4) . . ? C7 C8 C9 120.6(4) . . ? C10 C9 C8 119.9(4) . . ? C10 C9 C13 119.9(4) . . ? C8 C9 C13 120.2(4) . . ? C11 C10 C9 118.6(4) . . ? C56 N11 C27 123.4(3) . . ? C12 C11 C10 121.9(4) . . ? C56 N12 C32 125.6(3) . . ? C11 C12 C7 119.9(4) . . ? C57 N13 C29 120.6(3) . . ? N8 C13 C9 178.0(5) . . ? C57 N14 C39 127.1(3) . . ? C15 C14 C19 119.4(4) . . ? C15 C14 N4 123.9(4) . . ? C19 C14 N4 116.6(3) . . ? C58 N15 C31 125.3(4) . . ? C14 C15 C16 118.8(4) . . ? C46 N16 C58 128.5(3) . . ? C17 C16 C15 121.5(4) . . ? C17 C16 C20 117.0(4) . . ? C15 C16 C20 121.5(4) . . ? C28 N17 C30 113.5(3) . . ? C28 N17 C26 111.6(3) . . ? C30 N17 C26 112.5(3) . . ? C18 C17 C16 119.5(4) . . ? C17 C18 C19 119.3(4) . . ? C18 C19 C14 121.5(4) . . ? N9 C20 C16 174.7(5) . . ? C22 C21 C82 118.7(5) . . ? C22 C21 N6 117.6(4) . . ? C82 C21 N6 123.7(5) . . ? C21 C22 C23 121.4(6) . . ? C25 C23 C22 127.0(9) . . ? C25 C23 C24 112.8(8) . . ? C22 C23 C24 120.2(7) . . ? C23A C24 C23 117.7(7) . . ? C23A C24 C25A 39.9(6) . . ? C23 C24 C25A 157.5(8) . . ? N10A C25 C23 173.9(11) . . ? N17 C26 C27 111.2(3) . . ? N11 C27 C26 108.1(3) . . ? N17 C28 C29 111.5(3) . . ? N13 C29 C28 112.5(3) . . ? N17 C30 C31 111.9(3) . . ? N15 C31 C30 113.1(3) . . ? C33 C32 C37 118.2(4) . . ? C33 C32 N12 122.6(4) . . ? C37 C32 N12 119.2(3) . . ? C32 C33 C34 119.9(4) . . ? C35 C34 C33 121.6(4) . . ? C35 C34 C38 119.9(4) . . ? C33 C34 C38 118.4(4) . . ? C36 C35 C34 117.6(4) . . ? C37 C36 C35 121.2(4) . . ? C36 C37 C32 121.5(4) . . ? N18 C38 C34 178.4(5) . . ? C40 C39 C44 119.7(4) . . ? C40 C39 N14 117.9(3) . . ? C44 C39 N14 122.5(4) . . ? C39 C40 C41 119.2(4) . . ? C40 C41 C42 121.4(4) . . ? C40 C41 C45 119.9(4) . . ? C42 C41 C45 118.8(4) . . ? C43 C42 C41 118.7(4) . . ? C42 C43 C44 121.1(4) . . ? C43 C44 C39 119.9(4) . . ? N19 C45 C41 175.9(5) . . ? N16 C46 C47 124.3(4) . . ? N16 C46 C51 118.0(4) . . ? C47 C46 C51 117.7(4) . . ? C46 C47 C48 119.1(4) . . ? C49 C48 C47 122.5(4) . . ? C49 C48 C52 118.5(4) . . ? C47 C48 C52 119.0(4) . . ? C50 C49 C48 118.0(4) . . ? C49 C50 C51 120.8(4) . . ? C50 C51 C46 121.9(4) . . ? N20 C52 C48 179.1(5) . . ? O1 C53 N1 123.4(4) . . ? O1 C53 N2 123.1(3) . . ? N1 C53 N2 113.5(3) . . ? O2 C54 N3 122.9(4) . . ? O2 C54 N4 123.1(3) . . ? N3 C54 N4 114.1(3) . . ? O3 C55 N5 123.4(4) . . ? O3 C55 N6 123.1(4) . . ? N5 C55 N6 113.4(3) . . ? O4 C56 N11 123.4(3) . . ? O4 C56 N12 121.8(3) . . ? N11 C56 N12 114.8(3) . . ? O5 C57 N13 120.5(3) . . ? O5 C57 N14 123.7(3) . . ? N13 C57 N14 115.8(3) . . ? O6 C58 N15 124.1(4) . . ? O6 C58 N16 123.0(4) . . ? N15 C58 N16 112.9(4) . . ? C23A C82 C21 119.9(7) . . ? C25A C23A C82 140.5(11) . . ? C25A C23A C24 97.5(9) . . ? C82 C23A C24 122.0(7) . . ? N10 C25A C23A 171.2(12) . . ? N10 C25A C24 146.1(10) . . ? C23A C25A C24 42.6(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.315 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.070 #===END