# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'J M Shreeve' _publ_contact_author_email JSHREEVE@UIDAHO.EDU _publ_section_title ; Energetic polyazole polynitrobenzenes and their coordination complexes ; loop_ _publ_author_name 'J M Shreeve' 'Yong Guo.' 'Brendan Twamley' 'Zhuo Zeng.' # Attachment 'Zhuo_-_Chem_Commun__combined_CIF_-_revised_-_08-26-09.txt' data_cmpd3e ######bt1260 _database_code_depnum_ccdc_archive 'CCDC 732611' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common 'C10H6N10O6 + MeCN' _chemical_melting_point ? _chemical_formula_moiety 'C10 H6 N10 O6, C2 H3 N' _chemical_formula_sum 'C12 H9 N11 O6' _chemical_formula_weight 403.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6692(4) _cell_length_b 9.4624(4) _cell_length_c 19.0356(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.696(1) _cell_angle_gamma 90.00 _cell_volume 1725.95(13) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9971 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details 'SADABS-2007/4 (Bruker, 2007)' _exptl_special_details ; ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25293 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3967 _reflns_number_gt 3409 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v. 5.632 (Bruker, 2006)' _computing_cell_refinement 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_data_reduction 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_structure_solution 'XS, SHELXTL v. 6.14 (Bruker, 2003)' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)' _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^)+(0.0459P)^2^+0.5591P] 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 3967 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.16324(12) 0.78246(12) 0.91185(6) 0.0173(2) Uani 1 1 d . . . C2 C 0.20111(12) 0.73142(12) 0.98181(6) 0.0175(2) Uani 1 1 d . . . C3 C 0.10736(12) 0.71516(13) 1.02987(6) 0.0184(2) Uani 1 1 d . . . C4 C -0.03195(12) 0.75108(13) 1.01042(6) 0.0201(3) Uani 1 1 d . . . C5 C -0.07662(12) 0.80099(13) 0.94222(6) 0.0186(2) Uani 1 1 d . . . C6 C 0.01944(12) 0.81494(13) 0.89529(6) 0.0180(2) Uani 1 1 d . . . C12 C 0.23444(14) 0.52115(14) 1.17759(7) 0.0245(3) Uani 1 1 d . . . H12 H 0.2739 0.4392 1.2012 0.029 Uiso 1 1 calc R . . C14 C 0.15152(13) 0.72521(14) 1.16215(6) 0.0214(3) Uani 1 1 d . . . H14 H 0.1190 0.8183 1.1690 0.026 Uiso 1 1 calc R . . C17 C -0.33537(12) 0.76209(14) 0.92811(7) 0.0208(3) Uani 1 1 d . . . H17 H -0.3375 0.6705 0.9483 0.025 Uiso 1 1 calc R . . C19 C -0.39059(13) 0.95800(14) 0.88053(7) 0.0242(3) Uani 1 1 d . . . H19 H -0.4471 1.0330 0.8596 0.029 Uiso 1 1 calc R . . C23 C 0.41246(14) 0.32383(16) 0.78815(7) 0.0276(3) Uani 1 1 d . . . C24 C 0.37059(17) 0.46201(16) 0.81014(8) 0.0340(3) Uani 1 1 d . . . H24A H 0.4207 0.5350 0.7871 0.051 Uiso 1 1 calc R . . H24B H 0.3928 0.4707 0.8617 0.051 Uiso 1 1 calc R . . H24C H 0.2699 0.4739 0.7964 0.051 Uiso 1 1 calc R . . N8 N 0.25307(10) 0.79741(12) 0.86510(5) 0.0210(2) Uani 1 1 d . . . H8A H 0.2238 0.8285 0.8221 0.025 Uiso 1 1 calc R . . H8B H 0.3417 0.7762 0.8772 0.025 Uiso 1 1 calc R . . N9 N 0.34768(10) 0.69098(11) 1.00376(5) 0.0193(2) Uani 1 1 d . . . N10 N 0.15250(10) 0.66245(11) 1.09893(5) 0.0190(2) Uani 1 1 d . . . N11 N 0.20679(12) 0.52920(12) 1.10788(6) 0.0255(2) Uani 1 1 d . . . N13 N 0.20220(11) 0.63885(12) 1.21311(5) 0.0225(2) Uani 1 1 d . . . N15 N -0.13171(11) 0.73435(14) 1.06137(6) 0.0278(3) Uani 1 1 d . . . N16 N -0.21851(10) 0.83578(11) 0.92107(5) 0.0194(2) Uani 1 1 d . . . N18 N -0.44571(11) 0.83609(12) 0.90279(6) 0.0229(2) Uani 1 1 d . . . N20 N -0.25304(11) 0.96445(12) 0.89013(6) 0.0240(2) Uani 1 1 d . . . N21 N -0.02861(10) 0.86313(11) 0.82242(5) 0.0196(2) Uani 1 1 d . . . N22 N 0.44586(14) 0.21530(15) 0.77063(7) 0.0384(3) Uani 1 1 d . . . O1 O 0.39678(9) 0.60337(10) 0.96713(5) 0.0263(2) Uani 1 1 d . . . O2 O 0.40991(10) 0.74633(11) 1.05663(5) 0.0300(2) Uani 1 1 d . . . O3 O -0.14065(11) 0.61639(14) 1.08698(6) 0.0425(3) Uani 1 1 d . . . O4 O -0.19829(11) 0.83862(13) 1.07440(5) 0.0392(3) Uani 1 1 d . . . O5 O 0.00516(9) 0.98197(10) 0.80634(5) 0.0252(2) Uani 1 1 d . . . O6 O -0.09733(10) 0.78017(11) 0.78289(5) 0.0311(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0153(5) 0.0186(6) 0.0174(5) -0.0008(4) 0.0001(4) -0.0005(4) C2 0.0139(5) 0.0191(6) 0.0188(6) -0.0004(4) -0.0011(4) 0.0013(4) C3 0.0191(6) 0.0194(6) 0.0158(5) 0.0003(4) -0.0007(4) -0.0001(4) C4 0.0167(6) 0.0244(6) 0.0194(6) 0.0005(5) 0.0033(4) -0.0011(5) C5 0.0131(5) 0.0207(6) 0.0210(6) -0.0003(5) -0.0008(4) 0.0000(4) C6 0.0158(5) 0.0200(6) 0.0172(5) 0.0010(4) -0.0012(4) 0.0007(4) C12 0.0269(6) 0.0262(7) 0.0196(6) 0.0037(5) 0.0004(5) 0.0014(5) C14 0.0211(6) 0.0240(6) 0.0191(6) -0.0011(5) 0.0026(5) -0.0012(5) C17 0.0155(5) 0.0247(6) 0.0222(6) -0.0006(5) 0.0019(4) -0.0007(5) C19 0.0177(6) 0.0272(7) 0.0271(6) 0.0018(5) 0.0000(5) 0.0033(5) C23 0.0257(7) 0.0336(8) 0.0225(6) -0.0012(5) -0.0011(5) -0.0042(6) C24 0.0389(8) 0.0323(8) 0.0332(7) -0.0083(6) 0.0127(6) -0.0077(6) N8 0.0137(5) 0.0313(6) 0.0174(5) 0.0042(4) -0.0004(4) 0.0023(4) N9 0.0162(5) 0.0232(5) 0.0176(5) 0.0019(4) -0.0007(4) 0.0012(4) N10 0.0188(5) 0.0212(5) 0.0167(5) 0.0014(4) 0.0006(4) 0.0008(4) N11 0.0318(6) 0.0227(6) 0.0211(5) 0.0026(4) 0.0006(4) 0.0052(4) N13 0.0213(5) 0.0269(6) 0.0187(5) 0.0009(4) 0.0008(4) -0.0029(4) N15 0.0164(5) 0.0471(7) 0.0195(5) 0.0015(5) 0.0010(4) -0.0037(5) N16 0.0138(5) 0.0224(5) 0.0215(5) 0.0022(4) 0.0003(4) 0.0009(4) N18 0.0165(5) 0.0270(6) 0.0244(5) -0.0012(4) 0.0003(4) 0.0018(4) N20 0.0184(5) 0.0241(5) 0.0287(6) 0.0045(4) 0.0005(4) 0.0024(4) N21 0.0134(5) 0.0259(5) 0.0190(5) 0.0026(4) 0.0002(4) 0.0026(4) N22 0.0382(7) 0.0367(7) 0.0372(7) -0.0061(6) -0.0064(5) 0.0054(6) O1 0.0226(5) 0.0305(5) 0.0252(5) -0.0022(4) 0.0009(4) 0.0086(4) O2 0.0215(5) 0.0413(6) 0.0242(5) -0.0080(4) -0.0071(4) 0.0022(4) O3 0.0318(6) 0.0603(8) 0.0358(6) 0.0188(5) 0.0063(4) -0.0119(5) O4 0.0253(5) 0.0647(8) 0.0286(5) -0.0090(5) 0.0069(4) 0.0085(5) O5 0.0242(5) 0.0256(5) 0.0262(5) 0.0065(4) 0.0051(4) 0.0029(4) O6 0.0274(5) 0.0394(6) 0.0233(5) 0.0002(4) -0.0080(4) -0.0078(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N8 1.3317(16) . ? C1 C6 1.4176(16) . ? C1 C2 1.4179(16) . ? C2 C3 1.3799(17) . ? C2 N9 1.4734(15) . ? C3 C4 1.3905(17) . ? C3 N10 1.4191(15) . ? C4 C5 1.3946(17) . ? C4 N15 1.4651(16) . ? C5 C6 1.3786(17) . ? C5 N16 1.4159(15) . ? C6 N21 1.4748(15) . ? C12 N11 1.3202(16) . ? C12 N13 1.3605(17) . ? C12 H12 0.9500 . ? C14 N13 1.3120(16) . ? C14 N10 1.3431(16) . ? C14 H14 0.9500 . ? C17 N18 1.3127(16) . ? C17 N16 1.3496(16) . ? C17 H17 0.9500 . ? C19 N20 1.3195(16) . ? C19 N18 1.3619(17) . ? C19 H19 0.9500 . ? C23 N22 1.1397(19) . ? C23 C24 1.447(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N8 H8A 0.8800 . ? N8 H8B 0.8800 . ? N9 O2 1.2194(13) . ? N9 O1 1.2197(14) . ? N10 N11 1.3677(15) . ? N15 O4 1.2216(16) . ? N15 O3 1.2257(17) . ? N16 N20 1.3741(15) . ? N21 O6 1.2207(14) . ? N21 O5 1.2213(14) . ? 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 C1 C6 122.44(11) . . ? N8 C1 C2 123.66(11) . . ? C6 C1 C2 113.89(10) . . ? C3 C2 C1 123.41(11) . . ? C3 C2 N9 118.38(10) . . ? C1 C2 N9 118.19(10) . . ? C2 C3 C4 119.68(11) . . ? C2 C3 N10 120.36(10) . . ? C4 C3 N10 119.95(11) . . ? C3 C4 C5 119.92(11) . . ? C3 C4 N15 119.84(11) . . ? C5 C4 N15 120.23(11) . . ? C6 C5 C4 118.96(11) . . ? C6 C5 N16 120.32(10) . . ? C4 C5 N16 120.72(11) . . ? C5 C6 C1 124.13(11) . . ? C5 C6 N21 118.97(10) . . ? C1 C6 N21 116.89(10) . . ? N11 C12 N13 115.04(11) . . ? N11 C12 H12 122.5 . . ? N13 C12 H12 122.5 . . ? N13 C14 N10 109.90(11) . . ? N13 C14 H14 125.1 . . ? N10 C14 H14 125.1 . . ? N18 C17 N16 109.76(11) . . ? N18 C17 H17 125.1 . . ? N16 C17 H17 125.1 . . ? N20 C19 N18 115.17(11) . . ? N20 C19 H19 122.4 . . ? N18 C19 H19 122.4 . . ? N22 C23 C24 179.67(18) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C1 N8 H8A 120.0 . . ? C1 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? O2 N9 O1 125.23(10) . . ? O2 N9 C2 118.17(10) . . ? O1 N9 C2 116.59(10) . . ? C14 N10 N11 110.16(10) . . ? C14 N10 C3 129.53(11) . . ? N11 N10 C3 120.31(10) . . ? C12 N11 N10 101.60(10) . . ? C14 N13 C12 103.31(10) . . ? O4 N15 O3 125.99(12) . . ? O4 N15 C4 117.31(12) . . ? O3 N15 C4 116.70(12) . . ? C17 N16 N20 109.98(10) . . ? C17 N16 C5 130.08(11) . . ? N20 N16 C5 119.89(10) . . ? C17 N18 C19 103.50(10) . . ? C19 N20 N16 101.59(10) . . ? O6 N21 O5 125.40(11) . . ? O6 N21 C6 117.25(10) . . ? O5 N21 C6 117.34(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8A N13 0.88 2.08 2.9318(14) 163 4_575 N8 H8A O5 0.88 2.55 3.0543(14) 117 . N8 H8B N18 0.88 2.13 2.9278(14) 151 1_655 N8 H8B O1 0.88 2.38 2.8899(14) 118 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.337 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.051 data_cmpd3f #######bt1270t _database_code_depnum_ccdc_archive 'CCDC 732612' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common C12H6N12O6 _chemical_melting_point ? _chemical_formula_moiety 'C12 H6 N12 O6' _chemical_formula_sum 'C12 H6 N12 O6' _chemical_formula_weight 414.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2582(17) _cell_length_b 10.7107(15) _cell_length_c 24.007(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.253(2) _cell_angle_gamma 90.00 _cell_volume 3149.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9812 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.04 _exptl_crystal_description blade _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.877 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details 'Twinabs v. 2007/5 (Bruker, 2007)' _exptl_special_details ; ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72957 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7224 _reflns_number_gt 6481 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v. 5.632 (Bruker, 2006)' _computing_cell_refinement 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_data_reduction 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_structure_solution 'XS, SHELXTL v. 6.14 (Bruker, 2003)' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)' _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^)+(0.0298P)^2^+2.3532P] 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 7224 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.88586(14) 0.10787(17) 0.11499(7) 0.0148(3) Uani 1 1 d . . . C2 C 0.98085(15) 0.11506(17) 0.08580(7) 0.0144(3) Uani 1 1 d . . . C3 C 1.07641(14) 0.05481(17) 0.10357(7) 0.0146(3) Uani 1 1 d . . . C4 C 1.07451(14) -0.01870(17) 0.15097(7) 0.0152(3) Uani 1 1 d . . . C5 C 0.98154(14) -0.02777(17) 0.18223(7) 0.0146(3) Uani 1 1 d . . . C6 C 0.88879(14) 0.03637(17) 0.16348(7) 0.0151(3) Uani 1 1 d . . . C11 C 0.62169(15) 0.19906(18) 0.08403(7) 0.0189(4) Uani 1 1 d . . . H11 H 0.5454 0.1853 0.0791 0.023 Uiso 1 1 calc R . . C13 C 0.77101(16) 0.29408(18) 0.09084(8) 0.0186(4) Uani 1 1 d . . . H13 H 0.8260 0.3566 0.0928 0.022 Uiso 1 1 calc R . . C17 C 1.32016(16) 0.02696(19) 0.03883(8) 0.0211(4) Uani 1 1 d . . . H17 H 1.3766 -0.0185 0.0219 0.025 Uiso 1 1 calc R . . C19 C 1.23505(16) 0.17680(18) 0.07121(8) 0.0224(4) Uani 1 1 d . . . H19 H 1.2139 0.2570 0.0838 0.027 Uiso 1 1 calc R . . C23 C 0.97196(15) -0.08792(19) 0.32168(8) 0.0199(4) Uani 1 1 d . . . H23 H 0.9661 -0.0628 0.3594 0.024 Uiso 1 1 calc R . . C25 C 0.98642(16) -0.20477(19) 0.25229(8) 0.0201(4) Uani 1 1 d . . . H25 H 0.9924 -0.2748 0.2283 0.024 Uiso 1 1 calc R . . C26 C 0.43686(15) 0.55842(17) 0.10583(7) 0.0150(3) Uani 1 1 d . . . C27 C 0.53114(15) 0.61584(17) 0.08837(7) 0.0147(3) Uani 1 1 d . . . C28 C 0.62945(14) 0.60802(17) 0.11839(7) 0.0150(3) Uani 1 1 d . . . C29 C 0.63198(15) 0.53896(17) 0.16753(7) 0.0154(3) Uani 1 1 d . . . C30 C 0.54045(15) 0.47872(17) 0.18620(7) 0.0154(3) Uani 1 1 d . . . C31 C 0.44361(15) 0.48850(17) 0.15446(7) 0.0159(4) Uani 1 1 d . . . C34 C 0.18633(16) 0.52687(19) 0.03807(8) 0.0219(4) Uani 1 1 d . . . H34 H 0.1278 0.4805 0.0212 0.026 Uiso 1 1 calc R . . C36 C 0.27665(16) 0.67923(18) 0.06824(8) 0.0213(4) Uani 1 1 d . . . H36 H 0.3000 0.7605 0.0791 0.026 Uiso 1 1 calc R . . C40 C 0.88987(15) 0.69274(18) 0.08558(8) 0.0193(4) Uani 1 1 d . . . H40 H 0.9652 0.6772 0.0807 0.023 Uiso 1 1 calc R . . C42 C 0.74259(16) 0.79016(18) 0.08987(8) 0.0193(4) Uani 1 1 d . . . H42 H 0.6882 0.8534 0.0898 0.023 Uiso 1 1 calc R . . C46 C 0.50425(15) 0.41674(19) 0.32421(8) 0.0202(4) Uani 1 1 d . . . H46 H 0.4843 0.4397 0.3607 0.024 Uiso 1 1 calc R . . C48 C 0.55547(17) 0.30623(19) 0.25838(8) 0.0223(4) Uani 1 1 d . . . H48 H 0.5788 0.2389 0.2360 0.027 Uiso 1 1 calc R . . N9 N 0.78947(12) 0.17015(15) 0.09698(6) 0.0155(3) Uani 1 1 d . . . N10 N 0.69141(13) 0.10701(15) 0.09345(6) 0.0180(3) Uani 1 1 d . . . N12 N 0.66670(13) 0.31569(16) 0.08185(7) 0.0213(3) Uani 1 1 d . . . N14 N 0.98435(12) 0.19039(15) 0.03457(6) 0.0153(3) Uani 1 1 d . . . N15 N 1.17395(12) 0.07234(14) 0.07471(6) 0.0155(3) Uani 1 1 d . . . N16 N 1.23041(14) -0.02720(15) 0.05473(7) 0.0204(3) Uani 1 1 d . . . N18 N 1.32742(14) 0.15198(17) 0.04808(8) 0.0266(4) Uani 1 1 d . . . N20 N 1.17494(13) -0.08319(15) 0.17013(6) 0.0182(3) Uani 1 1 d . . . N21 N 0.98385(12) -0.08424(15) 0.23566(6) 0.0157(3) Uani 1 1 d . . . N22 N 0.97346(12) -0.00699(16) 0.28083(6) 0.0184(3) Uani 1 1 d . . . N24 N 0.97929(14) -0.21032(16) 0.30680(7) 0.0221(4) Uani 1 1 d . . . N26 N 0.79049(12) 0.03149(15) 0.19713(6) 0.0161(3) Uani 1 1 d . . . N32 N 0.33637(12) 0.57405(14) 0.07550(6) 0.0156(3) Uani 1 1 d . . . N33 N 0.27670(13) 0.47307(15) 0.05707(7) 0.0196(3) Uani 1 1 d . . . N35 N 0.18168(14) 0.65278(17) 0.04402(7) 0.0262(4) Uani 1 1 d . . . N37 N 0.52248(12) 0.68835(14) 0.03619(6) 0.0151(3) Uani 1 1 d . . . N38 N 0.72451(12) 0.66791(15) 0.09995(6) 0.0157(3) Uani 1 1 d . . . N39 N 0.82140(12) 0.60316(15) 0.09799(6) 0.0183(3) Uani 1 1 d . . . N41 N 0.84579(14) 0.80916(16) 0.08016(7) 0.0219(3) Uani 1 1 d . . . N43 N 0.73470(13) 0.53153(15) 0.20144(6) 0.0178(3) Uani 1 1 d . . . N44 N 0.53958(13) 0.42450(15) 0.24033(6) 0.0165(3) Uani 1 1 d . . . N45 N 0.50481(13) 0.49797(16) 0.28310(6) 0.0190(3) Uani 1 1 d . . . N47 N 0.53393(14) 0.29806(16) 0.31148(7) 0.0228(4) Uani 1 1 d . . . N49 N 0.34372(13) 0.42914(16) 0.17416(6) 0.0198(3) Uani 1 1 d . . . O1 O 1.00480(12) 0.30217(13) 0.04130(6) 0.0225(3) Uani 1 1 d . . . O2 O 0.97043(11) 0.13696(13) -0.00935(5) 0.0211(3) Uani 1 1 d . . . O3 O 1.25647(11) -0.01843(14) 0.17726(6) 0.0239(3) Uani 1 1 d . . . O4 O 1.16919(12) -0.19601(13) 0.17652(6) 0.0251(3) Uani 1 1 d . . . O5 O 0.75651(11) 0.13123(13) 0.21375(6) 0.0222(3) Uani 1 1 d . . . O6 O 0.75287(11) -0.07214(13) 0.20552(5) 0.0204(3) Uani 1 1 d . . . O7 O 0.50347(12) 0.80056(12) 0.04130(6) 0.0218(3) Uani 1 1 d . . . O8 O 0.53137(11) 0.63240(13) -0.00715(5) 0.0214(3) Uani 1 1 d . . . O9 O 0.77198(12) 0.62996(13) 0.21954(6) 0.0238(3) Uani 1 1 d . . . O10 O 0.77283(11) 0.42735(13) 0.20877(5) 0.0208(3) Uani 1 1 d . . . O11 O 0.26524(11) 0.49756(15) 0.17921(6) 0.0283(3) Uani 1 1 d . . . O12 O 0.34838(12) 0.31702(14) 0.18304(6) 0.0286(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0151(8) 0.0134(9) 0.0156(8) -0.0006(7) -0.0020(6) -0.0014(7) C2 0.0180(9) 0.0126(8) 0.0125(8) -0.0011(6) -0.0007(6) -0.0017(6) C3 0.0160(8) 0.0142(9) 0.0136(8) -0.0024(6) 0.0009(6) -0.0012(7) C4 0.0157(8) 0.0128(9) 0.0168(8) -0.0020(7) -0.0024(6) -0.0001(7) C5 0.0174(9) 0.0118(8) 0.0143(8) 0.0012(7) -0.0011(6) -0.0014(7) C6 0.0162(8) 0.0144(9) 0.0147(8) -0.0011(7) 0.0020(6) -0.0018(7) C11 0.0177(9) 0.0221(10) 0.0166(9) 0.0008(7) -0.0010(7) 0.0009(7) C13 0.0214(9) 0.0158(9) 0.0187(9) 0.0017(7) 0.0002(7) 0.0007(7) C17 0.0175(9) 0.0243(10) 0.0220(9) 0.0005(8) 0.0057(7) 0.0036(8) C19 0.0224(9) 0.0154(9) 0.0296(11) -0.0002(8) 0.0048(8) -0.0025(7) C23 0.0185(9) 0.0261(10) 0.0152(9) 0.0033(7) 0.0011(7) 0.0033(7) C25 0.0209(9) 0.0176(9) 0.0218(9) 0.0029(7) 0.0001(7) 0.0004(7) C26 0.0163(8) 0.0132(8) 0.0155(8) -0.0015(7) 0.0001(6) 0.0021(7) C27 0.0183(9) 0.0127(8) 0.0132(8) -0.0001(6) 0.0008(6) 0.0024(7) C28 0.0153(8) 0.0139(9) 0.0160(8) -0.0004(6) 0.0026(6) 0.0004(7) C29 0.0171(8) 0.0146(9) 0.0144(8) -0.0007(7) -0.0015(6) 0.0014(7) C30 0.0185(9) 0.0138(9) 0.0140(8) 0.0007(6) 0.0011(7) 0.0028(7) C31 0.0164(9) 0.0141(9) 0.0173(9) -0.0005(7) 0.0026(7) -0.0003(7) C34 0.0189(9) 0.0240(10) 0.0226(9) 0.0000(8) -0.0031(7) -0.0035(8) C36 0.0213(9) 0.0165(10) 0.0260(10) -0.0006(7) -0.0015(7) 0.0022(7) C40 0.0171(9) 0.0219(10) 0.0191(9) 0.0000(7) 0.0018(7) -0.0021(7) C42 0.0227(9) 0.0152(9) 0.0202(9) 0.0011(7) 0.0018(7) -0.0008(7) C46 0.0180(9) 0.0278(10) 0.0149(9) 0.0016(8) 0.0018(7) -0.0005(8) C48 0.0277(10) 0.0170(10) 0.0222(9) 0.0035(7) 0.0017(8) 0.0025(8) N9 0.0149(7) 0.0164(8) 0.0152(7) 0.0010(6) -0.0001(6) -0.0005(6) N10 0.0153(7) 0.0190(8) 0.0194(8) 0.0005(6) -0.0012(6) -0.0017(6) N12 0.0198(8) 0.0195(9) 0.0243(8) 0.0011(7) -0.0012(6) 0.0032(6) N14 0.0132(7) 0.0170(8) 0.0155(7) 0.0019(6) -0.0001(5) -0.0004(6) N15 0.0151(7) 0.0150(8) 0.0165(7) -0.0009(6) 0.0000(6) 0.0007(6) N16 0.0217(8) 0.0164(8) 0.0232(8) -0.0029(6) 0.0038(6) 0.0027(6) N18 0.0214(9) 0.0226(9) 0.0363(10) 0.0007(7) 0.0074(7) -0.0016(7) N20 0.0178(8) 0.0217(8) 0.0150(7) 0.0024(6) 0.0019(6) 0.0045(6) N21 0.0166(7) 0.0149(8) 0.0155(7) 0.0010(6) -0.0003(6) -0.0005(6) N22 0.0172(8) 0.0219(8) 0.0160(8) -0.0011(6) 0.0010(6) 0.0009(6) N24 0.0233(8) 0.0212(9) 0.0219(8) 0.0067(7) 0.0010(6) 0.0015(6) N26 0.0154(7) 0.0174(8) 0.0156(7) 0.0016(6) -0.0010(6) 0.0008(6) N32 0.0167(7) 0.0148(7) 0.0152(7) -0.0005(6) 0.0003(6) -0.0008(6) N33 0.0193(8) 0.0170(8) 0.0224(8) -0.0016(6) -0.0011(6) -0.0041(6) N35 0.0199(8) 0.0239(9) 0.0343(10) 0.0005(7) -0.0048(7) 0.0019(7) N37 0.0144(7) 0.0154(8) 0.0154(7) 0.0017(6) 0.0010(5) -0.0006(6) N38 0.0150(7) 0.0170(8) 0.0151(7) 0.0011(6) 0.0009(6) 0.0011(6) N39 0.0140(7) 0.0196(8) 0.0213(8) 0.0012(6) 0.0005(6) 0.0020(6) N41 0.0204(8) 0.0198(8) 0.0258(9) 0.0006(7) 0.0041(6) -0.0021(6) N43 0.0175(7) 0.0211(8) 0.0148(7) 0.0025(6) 0.0011(6) -0.0010(6) N44 0.0177(8) 0.0168(8) 0.0150(7) 0.0014(6) 0.0019(6) -0.0007(6) N45 0.0199(8) 0.0209(8) 0.0163(7) -0.0001(6) 0.0029(6) 0.0023(6) N47 0.0239(9) 0.0237(9) 0.0209(8) 0.0057(7) 0.0022(6) -0.0009(7) N49 0.0178(8) 0.0258(9) 0.0156(7) 0.0035(6) 0.0001(6) -0.0041(7) O1 0.0278(7) 0.0161(7) 0.0233(7) 0.0033(5) -0.0022(5) -0.0052(6) O2 0.0262(7) 0.0223(8) 0.0147(6) -0.0021(5) -0.0002(5) 0.0023(6) O3 0.0163(7) 0.0342(8) 0.0212(7) 0.0037(6) -0.0007(5) -0.0013(6) O4 0.0289(8) 0.0195(7) 0.0271(8) 0.0055(6) 0.0036(6) 0.0077(6) O5 0.0236(7) 0.0202(7) 0.0230(7) 0.0004(5) 0.0046(5) 0.0053(6) O6 0.0204(7) 0.0195(7) 0.0215(7) 0.0042(5) 0.0011(5) -0.0039(5) O7 0.0276(7) 0.0148(7) 0.0231(7) 0.0034(5) 0.0039(5) 0.0052(6) O8 0.0276(7) 0.0216(7) 0.0151(6) -0.0020(5) 0.0016(5) -0.0026(6) O9 0.0248(7) 0.0225(7) 0.0238(7) 0.0003(6) -0.0036(6) -0.0065(6) O10 0.0206(7) 0.0207(7) 0.0210(7) 0.0048(5) 0.0004(5) 0.0038(5) O11 0.0169(7) 0.0443(10) 0.0241(7) 0.0063(6) 0.0043(5) 0.0052(6) O12 0.0304(8) 0.0242(8) 0.0309(8) 0.0076(6) -0.0006(6) -0.0098(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 C1 C2 1.385(2) . ? C1 C6 1.393(2) . ? C1 N9 1.410(2) . ? C2 C3 1.390(3) . ? C2 N14 1.473(2) . ? C3 C4 1.385(2) . ? C3 N15 1.418(2) . ? C4 C5 1.392(2) . ? C4 N20 1.470(2) . ? C5 C6 1.388(3) . ? C5 N21 1.418(2) . ? C6 N26 1.478(2) . ? C11 N10 1.318(2) . ? C11 N12 1.367(2) . ? C11 H11 0.9500 . ? C13 N12 1.309(2) . ? C13 N9 1.354(2) . ? C13 H13 0.9500 . ? C17 N16 1.314(2) . ? C17 N18 1.360(3) . ? C17 H17 0.9500 . ? C19 N18 1.308(3) . ? C19 N15 1.351(2) . ? C19 H19 0.9500 . ? C23 N22 1.310(2) . ? C23 N24 1.363(3) . ? C23 H23 0.9500 . ? C25 N24 1.316(2) . ? C25 N21 1.351(3) . ? C25 H25 0.9500 . ? C26 C31 1.387(2) . ? C26 C27 1.388(2) . ? C26 N32 1.416(2) . ? C27 C28 1.382(3) . ? C27 N37 1.474(2) . ? C28 C29 1.392(2) . ? C28 N38 1.416(2) . ? C29 C30 1.384(3) . ? C29 N43 1.475(2) . ? C30 C31 1.389(3) . ? C30 N44 1.424(2) . ? C31 N49 1.474(2) . ? C34 N33 1.314(3) . ? C34 N35 1.358(3) . ? C34 H34 0.9500 . ? C36 N35 1.312(3) . ? C36 N32 1.351(2) . ? C36 H36 0.9500 . ? C40 N39 1.317(2) . ? C40 N41 1.363(2) . ? C40 H40 0.9500 . ? C42 N41 1.311(3) . ? C42 N38 1.351(2) . ? C42 H42 0.9500 . ? C46 N45 1.316(2) . ? C46 N47 1.360(3) . ? C46 H46 0.9500 . ? C48 N47 1.315(2) . ? C48 N44 1.351(3) . ? C48 H48 0.9500 . ? N9 N10 1.379(2) . ? N14 O2 1.206(2) . ? N14 O1 1.232(2) . ? N15 N16 1.368(2) . ? N20 O4 1.220(2) . ? N20 O3 1.223(2) . ? N21 N22 1.374(2) . ? N26 O5 1.219(2) . ? N26 O6 1.222(2) . ? N32 N33 1.369(2) . ? N37 O8 1.209(2) . ? N37 O7 1.231(2) . ? N38 N39 1.378(2) . ? N43 O10 1.220(2) . ? N43 O9 1.222(2) . ? N44 N45 1.375(2) . ? N49 O11 1.219(2) . ? N49 O12 1.221(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.32(16) . . ? C2 C1 N9 122.00(16) . . ? C6 C1 N9 120.68(16) . . ? C1 C2 C3 122.30(16) . . ? C1 C2 N14 120.38(16) . . ? C3 C2 N14 117.31(15) . . ? C4 C3 C2 118.37(16) . . ? C4 C3 N15 121.24(16) . . ? C2 C3 N15 120.36(16) . . ? C3 C4 C5 121.54(16) . . ? C3 C4 N20 118.92(15) . . ? C5 C4 N20 119.46(15) . . ? C6 C5 C4 117.91(16) . . ? C6 C5 N21 119.44(15) . . ? C4 C5 N21 121.99(16) . . ? C5 C6 C1 122.48(16) . . ? C5 C6 N26 118.71(15) . . ? C1 C6 N26 118.78(16) . . ? N10 C11 N12 115.46(17) . . ? N10 C11 H11 122.3 . . ? N12 C11 H11 122.3 . . ? N12 C13 N9 110.45(17) . . ? N12 C13 H13 124.8 . . ? N9 C13 H13 124.8 . . ? N16 C17 N18 115.96(17) . . ? N16 C17 H17 122.0 . . ? N18 C17 H17 122.0 . . ? N18 C19 N15 110.45(17) . . ? N18 C19 H19 124.8 . . ? N15 C19 H19 124.8 . . ? N22 C23 N24 115.94(17) . . ? N22 C23 H23 122.0 . . ? N24 C23 H23 122.0 . . ? N24 C25 N21 109.58(17) . . ? N24 C25 H25 125.2 . . ? N21 C25 H25 125.2 . . ? C31 C26 C27 118.07(17) . . ? C31 C26 N32 121.25(16) . . ? C27 C26 N32 120.67(16) . . ? C28 C27 C26 122.33(17) . . ? C28 C27 N37 120.47(16) . . ? C26 C27 N37 117.19(15) . . ? C27 C28 C29 117.65(16) . . ? C27 C28 N38 121.38(16) . . ? C29 C28 N38 120.97(16) . . ? C30 C29 C28 122.07(17) . . ? C30 C29 N43 118.79(15) . . ? C28 C29 N43 119.13(16) . . ? C29 C30 C31 118.26(16) . . ? C29 C30 N44 121.40(16) . . ? C31 C30 N44 119.63(16) . . ? C26 C31 C30 121.59(17) . . ? C26 C31 N49 118.69(16) . . ? C30 C31 N49 119.63(16) . . ? N33 C34 N35 115.93(18) . . ? N33 C34 H34 122.0 . . ? N35 C34 H34 122.0 . . ? N35 C36 N32 110.13(18) . . ? N35 C36 H36 124.9 . . ? N32 C36 H36 124.9 . . ? N39 C40 N41 115.75(17) . . ? N39 C40 H40 122.1 . . ? N41 C40 H40 122.1 . . ? N41 C42 N38 110.39(17) . . ? N41 C42 H42 124.8 . . ? N38 C42 H42 124.8 . . ? N45 C46 N47 116.10(16) . . ? N45 C46 H46 122.0 . . ? N47 C46 H46 122.0 . . ? N47 C48 N44 109.98(18) . . ? N47 C48 H48 125.0 . . ? N44 C48 H48 125.0 . . ? C13 N9 N10 109.43(15) . . ? C13 N9 C1 129.18(16) . . ? N10 N9 C1 120.32(15) . . ? C11 N10 N9 101.62(15) . . ? C13 N12 C11 103.01(16) . . ? O2 N14 O1 126.65(15) . . ? O2 N14 C2 117.53(15) . . ? O1 N14 C2 115.78(14) . . ? C19 N15 N16 109.53(15) . . ? C19 N15 C3 128.34(16) . . ? N16 N15 C3 121.07(15) . . ? C17 N16 N15 101.46(15) . . ? C19 N18 C17 102.55(17) . . ? O4 N20 O3 126.50(17) . . ? O4 N20 C4 116.93(16) . . ? O3 N20 C4 116.56(15) . . ? C25 N21 N22 110.13(15) . . ? C25 N21 C5 132.40(16) . . ? N22 N21 C5 117.26(15) . . ? C23 N22 N21 101.36(15) . . ? C25 N24 C23 102.99(16) . . ? O5 N26 O6 127.30(15) . . ? O5 N26 C6 116.37(15) . . ? O6 N26 C6 116.33(15) . . ? C36 N32 N33 109.70(15) . . ? C36 N32 C26 128.38(16) . . ? N33 N32 C26 121.04(15) . . ? C34 N33 N32 101.42(15) . . ? C36 N35 C34 102.77(17) . . ? O8 N37 O7 126.39(15) . . ? O8 N37 C27 117.65(15) . . ? O7 N37 C27 115.92(14) . . ? C42 N38 N39 109.51(15) . . ? C42 N38 C28 129.61(16) . . ? N39 N38 C28 120.24(15) . . ? C40 N39 N38 101.48(15) . . ? C42 N41 C40 102.86(16) . . ? O10 N43 O9 127.03(16) . . ? O10 N43 C29 116.30(16) . . ? O9 N43 C29 116.68(16) . . ? C48 N44 N45 110.01(15) . . ? C48 N44 C30 132.02(16) . . ? N45 N44 C30 117.51(15) . . ? C46 N45 N44 101.11(15) . . ? C48 N47 C46 102.79(16) . . ? O11 N49 O12 127.28(17) . . ? O11 N49 C31 116.19(16) . . ? O12 N49 C31 116.53(16) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.313 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.052 data_cmpd6 ##########bt1309 _database_code_depnum_ccdc_archive 'CCDC 732613' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(C12H6AgN11O5) + 3H2O' _chemical_melting_point ? _chemical_formula_moiety 'C12 H6 Ag N11 O5, 3(H2 O)' _chemical_formula_sum 'C12 H12 Ag N11 O8' _chemical_formula_weight 546.20 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 _symmetry_space_group_name_Hall '-C 2yc' 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 20.041(3) _cell_length_b 8.2412(8) _cell_length_c 24.046(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.131(9) _cell_angle_gamma 90.00 _cell_volume 3704.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9898 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 29.98 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.645 _exptl_absorpt_correction_T_max 0.711 _exptl_absorpt_process_details 'SADABS-2007/4 (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27473 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.24 _reflns_number_total 3333 _reflns_number_gt 3057 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v. 5.632 (Bruker, 2006)' _computing_cell_refinement 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_data_reduction 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_structure_solution 'XS, SHELXTL v. 6.14 (Bruker, 2003)' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)' _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^)+(0.0396P)^2^+23.5430P] 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 3333 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0886 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.365201(14) 0.77537(4) -0.152972(11) 0.02040(11) Uani 1 1 d . . . O1 O 0.18381(13) 0.4209(3) -0.07598(11) 0.0211(6) Uani 1 1 d . . . C1 C 0.19786(19) 0.4255(4) -0.02051(15) 0.0162(7) Uani 1 1 d . . . O2 O 0.39566(13) 0.4935(3) 0.13970(12) 0.0242(6) Uani 1 1 d . . . C2 C 0.26036(18) 0.5064(4) 0.02090(16) 0.0161(7) Uani 1 1 d . . . O3 O 0.33231(14) 0.7009(3) 0.14874(12) 0.0257(6) Uani 1 1 d . . . C3 C 0.27555(18) 0.4986(4) 0.08176(15) 0.0162(7) Uani 1 1 d . . . O4 O 0.05794(14) 0.3358(4) 0.07647(12) 0.0260(6) Uani 1 1 d . . . C4 C 0.23065(18) 0.4192(4) 0.10593(15) 0.0161(7) Uani 1 1 d . . . C5 C 0.16828(18) 0.3507(4) 0.06672(15) 0.0158(7) Uani 1 1 d . . . O5 O 0.14004(14) 0.1639(3) 0.12662(11) 0.0237(6) Uani 1 1 d . . . C6 C 0.15152(18) 0.3539(4) 0.00573(15) 0.0167(7) Uani 1 1 d . . . N7 N 0.30372(15) 0.5959(4) -0.00361(13) 0.0155(6) Uani 1 1 d . . . N8 N 0.35874(15) 0.6921(4) 0.03167(13) 0.0174(6) Uani 1 1 d . . . C9 C 0.38442(19) 0.7522(4) -0.00670(16) 0.0183(8) Uani 1 1 d . . . H9A H 0.4243 0.8237 0.0047 0.022 Uiso 1 1 calc R . . N10 N 0.34991(16) 0.7048(4) -0.06456(13) 0.0185(6) Uani 1 1 d . . . C11 C 0.30000(19) 0.6067(5) -0.06080(16) 0.0192(8) Uani 1 1 d . . . H11A H 0.2662 0.5514 -0.0935 0.023 Uiso 1 1 calc R . . N12 N 0.34025(16) 0.5716(4) 0.12641(13) 0.0182(6) Uani 1 1 d . . . N13 N 0.24665(16) 0.4142(4) 0.16844(13) 0.0172(6) Uani 1 1 d . . . N14 N 0.20035(17) 0.4792(4) 0.19283(13) 0.0221(7) Uani 1 1 d . . . C15 C 0.2292(2) 0.4349(5) 0.24906(16) 0.0239(8) Uani 1 1 d . . . H15A H 0.2087 0.4614 0.2779 0.029 Uiso 1 1 calc R . . N16 N 0.29045(17) 0.3485(4) 0.26239(14) 0.0246(7) Uani 1 1 d . . . C17 C 0.2994(2) 0.3360(5) 0.21082(16) 0.0218(8) Uani 1 1 d . . . H17A H 0.3376 0.2799 0.2047 0.026 Uiso 1 1 calc R . . N18 N 0.11822(15) 0.2770(4) 0.09188(13) 0.0183(7) Uani 1 1 d . . . N19 N 0.08772(16) 0.2806(4) -0.03300(13) 0.0160(6) Uani 1 1 d . . . N20 N 0.06732(16) 0.1289(4) -0.02146(13) 0.0186(6) Uani 1 1 d . . . C21 C 0.00613(18) 0.1094(4) -0.06551(16) 0.0183(7) Uani 1 1 d . . . H21A H -0.0217 0.0135 -0.0702 0.022 Uiso 1 1 calc R . . N22 N -0.01482(16) 0.2373(4) -0.10425(14) 0.0188(7) Uani 1 1 d . . . C23 C 0.03782(18) 0.3418(5) -0.08240(15) 0.0185(7) Uani 1 1 d . . . H23A H 0.0402 0.4451 -0.0991 0.022 Uiso 1 1 calc R . . O1S O 0.40050(18) 0.0629(5) 0.19360(15) 0.0481(9) Uani 1 1 d . . . O2S O 0.5000 0.3032(8) 0.2500 0.0675(16) Uani 1 2 d S . . O3S O 0.5000 -0.1785(9) 0.2500 0.086(2) Uani 1 2 d S . . O4S O 0.5697(3) -0.4304(7) 0.2167(2) 0.0868(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01547(16) 0.02756(18) 0.01375(16) 0.00023(11) -0.00009(11) 0.00169(11) O1 0.0193(13) 0.0237(14) 0.0176(13) -0.0004(10) 0.0033(10) -0.0041(11) C1 0.0171(17) 0.0118(17) 0.0153(17) -0.0002(13) 0.0006(14) 0.0027(13) O2 0.0148(13) 0.0286(15) 0.0251(14) 0.0053(11) 0.0022(11) 0.0013(11) C2 0.0130(16) 0.0143(17) 0.0197(17) 0.0017(14) 0.0044(14) 0.0024(14) O3 0.0249(14) 0.0266(15) 0.0235(14) -0.0066(12) 0.0061(12) -0.0051(11) C3 0.0132(17) 0.0146(17) 0.0164(17) 0.0001(13) 0.0001(14) 0.0022(13) O4 0.0164(13) 0.0338(16) 0.0269(14) -0.0047(12) 0.0069(11) 0.0000(12) C4 0.0152(17) 0.0169(18) 0.0131(16) 0.0009(14) 0.0015(14) 0.0016(14) C5 0.0151(17) 0.0122(17) 0.0189(18) 0.0016(14) 0.0047(14) 0.0019(13) O5 0.0280(14) 0.0195(13) 0.0220(13) 0.0027(11) 0.0072(11) -0.0036(11) C6 0.0134(17) 0.0140(17) 0.0191(18) -0.0010(14) 0.0015(14) 0.0005(14) N7 0.0122(14) 0.0159(15) 0.0161(14) -0.0014(12) 0.0024(12) -0.0007(12) N8 0.0151(15) 0.0152(15) 0.0203(16) -0.0006(12) 0.0042(12) -0.0018(12) C9 0.0141(17) 0.0156(18) 0.0225(19) 0.0001(14) 0.0032(15) 0.0015(14) N10 0.0137(15) 0.0220(16) 0.0184(15) 0.0016(12) 0.0041(12) 0.0008(12) C11 0.0161(18) 0.0224(19) 0.0181(18) -0.0010(15) 0.0050(14) 0.0004(15) N12 0.0171(16) 0.0198(16) 0.0156(15) 0.0021(12) 0.0032(12) -0.0021(13) N13 0.0163(15) 0.0178(15) 0.0149(14) 0.0006(12) 0.0026(12) -0.0014(12) N14 0.0279(17) 0.0204(16) 0.0170(15) 0.0000(13) 0.0070(13) 0.0043(13) C15 0.033(2) 0.021(2) 0.0149(18) 0.0006(15) 0.0055(16) 0.0046(16) N16 0.0278(17) 0.0236(17) 0.0167(16) 0.0048(13) 0.0011(13) -0.0002(14) C17 0.0184(18) 0.0211(19) 0.0219(19) 0.0062(15) 0.0022(15) -0.0007(15) N18 0.0169(16) 0.0198(16) 0.0174(16) -0.0044(13) 0.0051(13) -0.0025(12) N19 0.0145(15) 0.0160(15) 0.0151(15) 0.0003(12) 0.0026(12) -0.0011(12) N20 0.0170(15) 0.0142(15) 0.0224(16) -0.0016(12) 0.0042(13) -0.0016(12) C21 0.0143(17) 0.0176(18) 0.0212(18) -0.0042(14) 0.0042(14) -0.0013(14) N22 0.0132(15) 0.0228(17) 0.0187(15) 0.0018(12) 0.0038(12) -0.0001(12) C23 0.0165(17) 0.0198(18) 0.0179(18) 0.0032(14) 0.0048(14) 0.0010(14) O1S 0.043(2) 0.059(2) 0.0372(18) -0.0043(16) 0.0078(15) 0.0079(17) O2S 0.074(4) 0.065(4) 0.059(4) 0.000 0.019(3) 0.000 O3S 0.057(4) 0.067(4) 0.121(6) 0.000 0.018(4) 0.000 O4S 0.082(3) 0.092(4) 0.086(4) 0.002(3) 0.030(3) 0.001(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 Ag1 N22 2.285(3) 3 ? Ag1 N16 2.287(3) 6_565 ? Ag1 N10 2.328(3) . ? Ag1 N14 2.414(3) 7_565 ? O1 C1 1.260(4) . ? C1 C6 1.425(5) . ? C1 C2 1.451(5) . ? O2 N12 1.222(4) . ? C2 C3 1.385(5) . ? C2 N7 1.420(4) . ? O3 N12 1.229(4) . ? C3 C4 1.398(5) . ? C3 N12 1.481(4) . ? O4 N18 1.228(4) . ? C4 C5 1.386(5) . ? C4 N13 1.420(4) . ? C5 C6 1.382(5) . ? C5 N18 1.476(4) . ? O5 N18 1.222(4) . ? C6 N19 1.418(4) . ? N7 C11 1.353(5) . ? N7 N8 1.375(4) . ? N8 C9 1.305(5) . ? C9 N10 1.368(5) . ? C9 H9A 0.9500 . ? N10 C11 1.314(5) . ? C11 H11A 0.9500 . ? N13 C17 1.340(5) . ? N13 N14 1.373(4) . ? N14 C15 1.316(5) . ? N14 Ag1 2.414(3) 7_565 ? C15 N16 1.354(5) . ? C15 H15A 0.9500 . ? N16 C17 1.320(5) . ? N16 Ag1 2.287(3) 6_566 ? C17 H17A 0.9500 . ? N19 C23 1.345(5) . ? N19 N20 1.374(4) . ? N20 C21 1.310(5) . ? C21 N22 1.369(5) . ? C21 H21A 0.9500 . ? N22 C23 1.316(5) . ? N22 Ag1 2.285(3) 3_445 ? C23 H23A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N22 Ag1 N16 128.73(11) 3 6_565 ? N22 Ag1 N10 87.60(11) 3 . ? N16 Ag1 N10 116.20(11) 6_565 . ? N22 Ag1 N14 129.79(11) 3 7_565 ? N16 Ag1 N14 86.14(11) 6_565 7_565 ? N10 Ag1 N14 109.86(10) . 7_565 ? O1 C1 C6 121.6(3) . . ? O1 C1 C2 123.2(3) . . ? C6 C1 C2 115.2(3) . . ? C3 C2 N7 121.9(3) . . ? C3 C2 C1 120.7(3) . . ? N7 C2 C1 117.4(3) . . ? C2 C3 C4 122.1(3) . . ? C2 C3 N12 123.3(3) . . ? C4 C3 N12 114.6(3) . . ? C5 C4 C3 117.8(3) . . ? C5 C4 N13 120.8(3) . . ? C3 C4 N13 121.3(3) . . ? C6 C5 C4 121.9(3) . . ? C6 C5 N18 120.1(3) . . ? C4 C5 N18 117.9(3) . . ? C5 C6 N19 120.4(3) . . ? C5 C6 C1 122.0(3) . . ? N19 C6 C1 117.6(3) . . ? C11 N7 N8 109.1(3) . . ? C11 N7 C2 129.7(3) . . ? N8 N7 C2 121.2(3) . . ? C9 N8 N7 102.4(3) . . ? N8 C9 N10 115.3(3) . . ? N8 C9 H9A 122.4 . . ? N10 C9 H9A 122.4 . . ? C11 N10 C9 102.9(3) . . ? C11 N10 Ag1 124.8(2) . . ? C9 N10 Ag1 132.3(2) . . ? N10 C11 N7 110.3(3) . . ? N10 C11 H11A 124.9 . . ? N7 C11 H11A 124.9 . . ? O2 N12 O3 126.2(3) . . ? O2 N12 C3 116.8(3) . . ? O3 N12 C3 116.8(3) . . ? C17 N13 N14 109.4(3) . . ? C17 N13 C4 129.4(3) . . ? N14 N13 C4 120.8(3) . . ? C15 N14 N13 102.5(3) . . ? C15 N14 Ag1 127.9(3) . 7_565 ? N13 N14 Ag1 120.8(2) . 7_565 ? N14 C15 N16 114.4(3) . . ? N14 C15 H15A 122.8 . . ? N16 C15 H15A 122.8 . . ? C17 N16 C15 103.8(3) . . ? C17 N16 Ag1 122.3(3) . 6_566 ? C15 N16 Ag1 133.8(3) . 6_566 ? N16 C17 N13 109.9(3) . . ? N16 C17 H17A 125.1 . . ? N13 C17 H17A 125.1 . . ? O5 N18 O4 125.3(3) . . ? O5 N18 C5 117.7(3) . . ? O4 N18 C5 117.0(3) . . ? C23 N19 N20 109.8(3) . . ? C23 N19 C6 128.9(3) . . ? N20 N19 C6 121.3(3) . . ? C21 N20 N19 102.0(3) . . ? N20 C21 N22 115.1(3) . . ? N20 C21 H21A 122.5 . . ? N22 C21 H21A 122.5 . . ? C23 N22 C21 103.1(3) . . ? C23 N22 Ag1 131.2(3) . 3_445 ? C21 N22 Ag1 117.6(2) . 3_445 ? N22 C23 N19 110.0(3) . . ? N22 C23 H23A 125.0 . . ? N19 C23 H23A 125.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11A O1 0.95 2.14 2.699(4) 117 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.954 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.101 data_cmpd7 ############pb3 _database_code_depnum_ccdc_archive 'CCDC 732614' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common C16H11AgN18O8 _chemical_melting_point ? _chemical_formula_moiety 'C14 H8 Ag N14 O4, N3 O4, C2 H3 N' _chemical_formula_sum 'C16 H11 Ag N18 O8' _chemical_formula_weight 691.30 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' Ag Ag -0.8971 1.1015 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8611(4) _cell_length_b 11.1986(5) _cell_length_c 13.3871(6) _cell_angle_alpha 78.4787(6) _cell_angle_beta 74.2808(6) _cell_angle_gamma 84.8365(7) _cell_volume 1252.07(10) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8667 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 29.98 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8423 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_process_details 'SADABS-2007/4 (Bruker, 2007)' _exptl_special_details ; ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18562 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5758 _reflns_number_gt 5012 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v. 5.632 (Bruker, 2006)' _computing_cell_refinement 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_data_reduction 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_structure_solution 'XS, SHELXTL v. 6.14 (Bruker, 2003)' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)' _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^)+(0.0370P)^2^+0.4270P] 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 5758 _refine_ls_number_parameters 398 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.073 _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 -0.65744(2) 0.746937(17) 0.566304(15) 0.01932(7) Uani 1 1 d . . . C1 C -1.0612(3) 0.3205(2) 0.88579(19) 0.0132(5) Uani 1 1 d . . . C2 C -1.1658(3) 0.2255(2) 0.92049(19) 0.0147(5) Uani 1 1 d . . . C3 C -1.1137(3) 0.1159(2) 0.88707(19) 0.0145(5) Uani 1 1 d . . . C4 C -0.9643(3) 0.0980(2) 0.82441(19) 0.0149(5) Uani 1 1 d . . . C5 C -0.8621(3) 0.1941(2) 0.79202(19) 0.0150(5) Uani 1 1 d . . . C6 C -0.9115(3) 0.3067(2) 0.82090(19) 0.0139(5) Uani 1 1 d . . . C9 C -0.5971(3) 0.4923(2) 0.7506(2) 0.0190(5) Uani 1 1 d . . . H9A H -0.4963 0.5131 0.7521 0.023 Uiso 1 1 calc R B . C11 C -0.8099(3) 0.5020(2) 0.70638(19) 0.0161(5) Uani 1 1 d . . . H11A H -0.8929 0.5249 0.6731 0.019 Uiso 1 1 calc R B . C14 C -0.4816(3) 0.1099(2) 0.6757(2) 0.0223(6) Uani 1 1 d . . . H14A H -0.3864 0.0627 0.6731 0.027 Uiso 1 1 calc R . . C16 C -0.6447(3) 0.2430(2) 0.6287(2) 0.0181(5) Uani 1 1 d . . . H16A H -0.6953 0.3078 0.5907 0.022 Uiso 1 1 calc R . . C19 C -0.8700(3) -0.1998(2) 0.7970(2) 0.0210(6) Uani 1 1 d . . . H19A H -0.8608 -0.2846 0.8233 0.025 Uiso 1 1 calc R . . C21 C -0.8537(3) -0.0345(2) 0.6897(2) 0.0224(6) Uani 1 1 d . . . H21A H -0.8340 0.0263 0.6276 0.027 Uiso 1 1 calc R . . C25 C -1.5314(3) 0.3448(2) 1.0205(2) 0.0236(6) Uani 1 1 d . . . H25A H -1.6132 0.4056 1.0197 0.028 Uiso 1 1 calc R . . C27 C -1.4102(3) 0.1848(2) 1.0712(2) 0.0213(6) Uani 1 1 d . . . H27A H -1.3799 0.1098 1.1095 0.026 Uiso 1 1 calc R . . N7 N -0.8073(2) 0.40395(18) 0.78333(16) 0.0141(4) Uani 1 1 d . B . N8 N -0.6683(2) 0.39542(19) 0.81165(17) 0.0187(5) Uani 1 1 d . B . N10 N -0.6792(2) 0.56093(19) 0.68459(17) 0.0185(5) Uani 1 1 d . B . N12 N -0.7104(2) 0.17940(18) 0.72514(16) 0.0152(4) Uani 1 1 d . . . N13 N -0.6047(3) 0.0917(2) 0.75658(17) 0.0204(5) Uani 1 1 d . . . N15 N -0.5005(2) 0.2018(2) 0.59532(17) 0.0195(5) Uani 1 1 d . . . N17 N -0.9184(2) -0.01371(18) 0.78840(16) 0.0153(4) Uani 1 1 d . . . N18 N -0.9299(3) -0.12103(19) 0.85898(17) 0.0208(5) Uani 1 1 d . . . N20 N -0.8221(3) -0.15180(19) 0.69251(17) 0.0207(5) Uani 1 1 d . . . N22 N -1.2264(2) 0.01812(19) 0.90991(17) 0.0187(5) Uani 1 1 d . . . N23 N -1.3213(2) 0.24556(18) 0.97854(17) 0.0161(4) Uani 1 1 d . . . N24 N -1.4004(2) 0.35142(19) 0.94595(17) 0.0198(5) Uani 1 1 d . . . N26 N -1.5437(3) 0.2451(2) 1.09976(18) 0.0246(5) Uani 1 1 d . . . N28 N -1.1068(2) 0.43645(18) 0.92444(16) 0.0149(4) Uani 1 1 d . . . N29 N -0.8470(3) 0.6630(2) 0.47375(18) 0.0249(5) Uani 1 1 d . B . N30 N -0.8338(3) 0.5663(2) 0.42204(19) 0.0286(5) Uani 1 1 d . . . N31 N -0.9230(3) 0.7646(2) 0.43102(18) 0.0251(5) Uani 1 1 d . . . O1 O -1.0999(2) 0.53040(15) 0.85929(14) 0.0191(4) Uani 1 1 d . . . O2 O -1.1472(2) 0.42992(16) 1.02030(14) 0.0201(4) Uani 1 1 d . . . O3 O -1.2738(3) 0.0054(2) 0.83529(18) 0.0397(6) Uani 1 1 d . . . O4 O -1.2594(3) -0.04221(18) 0.99777(15) 0.0321(5) Uani 1 1 d . . . O5 O -0.8438(3) 0.5771(2) 0.33047(17) 0.0411(6) Uani 1 1 d . B . O6 O -0.8001(3) 0.4685(2) 0.47410(18) 0.0401(6) Uani 1 1 d . B . O7 O -1.0227(3) 0.7606(2) 0.38381(18) 0.0372(5) Uani 1 1 d . B . O8 O -0.8932(2) 0.8600(2) 0.45331(17) 0.0329(5) Uani 1 1 d . B . N32A N -0.3290(10) 0.8855(7) 0.5572(6) 0.0471(13) Uiso 0.41 1 d PD A 1 C33A C -0.2618(12) 0.8214(9) 0.6087(8) 0.038(3) Uiso 0.41 1 d PD A 1 C34A C -0.1729(14) 0.7708(11) 0.6809(10) 0.042(4) Uiso 0.41 1 d PD A 1 H34A H -0.1971 0.6848 0.7077 0.063 Uiso 0.41 1 calc PR A 1 H34B H -0.1990 0.8152 0.7398 0.063 Uiso 0.41 1 calc PR A 1 H34C H -0.0609 0.7773 0.6453 0.063 Uiso 0.41 1 calc PR A 1 N32B N -0.4291(9) 0.8132(8) 0.6281(7) 0.0471(13) Uiso 0.39 1 d PD B 2 C33B C -0.3150(11) 0.7869(10) 0.6511(8) 0.029(3) Uiso 0.39 1 d PD B 2 C34B C -0.1730(13) 0.7438(15) 0.6798(12) 0.017(3) Uiso 0.39 1 d PD B 2 H34D H -0.0920 0.8037 0.6461 0.026 Uiso 0.39 1 calc PR B 2 H34E H -0.1380 0.6660 0.6564 0.026 Uiso 0.39 1 calc PR B 2 H34F H -0.1918 0.7320 0.7567 0.026 Uiso 0.39 1 calc PR B 2 N32C N -0.407(2) 0.8524(16) 0.5966(14) 0.0471(13) Uiso 0.20 1 d PD C 3 C33C C -0.306(2) 0.8125(19) 0.6306(18) 0.016(5) Uiso 0.20 1 d PD C 3 C34C C -0.188(3) 0.736(2) 0.670(2) 0.030(8) Uiso 0.20 1 d PD C 3 H34G H -0.0847 0.7699 0.6359 0.044 Uiso 0.20 1 calc PR C 3 H34H H -0.1886 0.6537 0.6550 0.044 Uiso 0.20 1 calc PR C 3 H34I H -0.2103 0.7311 0.7466 0.044 Uiso 0.20 1 calc PR C 3 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 0.02064(11) 0.01839(11) 0.01484(11) -0.00098(7) 0.00155(8) -0.00310(8) C1 0.0162(12) 0.0117(11) 0.0120(11) -0.0025(9) -0.0048(9) 0.0023(9) C2 0.0142(12) 0.0155(12) 0.0122(12) 0.0003(9) -0.0018(9) 0.0000(9) C3 0.0178(12) 0.0114(11) 0.0130(12) 0.0002(9) -0.0027(10) -0.0030(9) C4 0.0198(13) 0.0119(11) 0.0124(12) -0.0021(9) -0.0043(10) 0.0026(10) C5 0.0145(12) 0.0156(12) 0.0121(12) 0.0003(9) -0.0016(9) 0.0017(9) C6 0.0157(12) 0.0130(11) 0.0115(11) 0.0004(9) -0.0028(9) -0.0012(9) C9 0.0181(13) 0.0177(13) 0.0208(13) -0.0031(10) -0.0033(10) -0.0047(10) C11 0.0177(12) 0.0119(12) 0.0163(12) -0.0013(10) -0.0020(10) 0.0008(10) C14 0.0193(13) 0.0230(14) 0.0202(14) -0.0027(11) -0.0011(11) 0.0062(11) C16 0.0197(13) 0.0178(13) 0.0150(12) -0.0019(10) -0.0024(10) -0.0004(10) C19 0.0324(15) 0.0133(12) 0.0163(13) -0.0022(10) -0.0053(11) 0.0000(11) C21 0.0355(16) 0.0149(12) 0.0142(13) -0.0029(10) -0.0028(11) 0.0013(11) C25 0.0166(13) 0.0201(14) 0.0319(16) -0.0054(12) -0.0021(11) 0.0001(11) C27 0.0197(13) 0.0188(13) 0.0203(14) 0.0018(11) 0.0003(11) -0.0023(11) N7 0.0128(10) 0.0134(10) 0.0146(10) -0.0004(8) -0.0023(8) -0.0009(8) N8 0.0172(11) 0.0187(11) 0.0196(11) -0.0022(9) -0.0046(9) -0.0008(9) N10 0.0183(11) 0.0149(11) 0.0191(11) -0.0028(9) -0.0003(9) 0.0004(9) N12 0.0154(10) 0.0123(10) 0.0149(10) -0.0005(8) -0.0012(8) 0.0018(8) N13 0.0186(11) 0.0176(11) 0.0201(11) 0.0007(9) -0.0021(9) 0.0060(9) N15 0.0179(11) 0.0197(11) 0.0170(11) -0.0002(9) -0.0011(9) 0.0026(9) N17 0.0188(11) 0.0117(10) 0.0139(10) -0.0008(8) -0.0030(8) -0.0004(8) N18 0.0322(13) 0.0107(10) 0.0156(11) 0.0025(8) -0.0029(9) -0.0027(9) N20 0.0311(13) 0.0129(10) 0.0166(11) -0.0012(9) -0.0050(10) 0.0003(9) N22 0.0187(11) 0.0138(11) 0.0216(12) -0.0020(9) -0.0025(9) -0.0018(9) N23 0.0152(10) 0.0130(10) 0.0181(11) -0.0023(8) -0.0015(9) 0.0001(8) N24 0.0173(11) 0.0161(11) 0.0231(12) 0.0000(9) -0.0038(9) 0.0013(9) N26 0.0210(12) 0.0211(12) 0.0257(13) -0.0032(10) 0.0039(10) -0.0022(9) N28 0.0118(10) 0.0141(10) 0.0172(11) -0.0029(8) -0.0009(8) -0.0010(8) N29 0.0250(12) 0.0300(13) 0.0221(12) -0.0036(10) -0.0114(10) 0.0015(10) N30 0.0306(14) 0.0327(14) 0.0218(13) -0.0035(11) -0.0063(10) -0.0033(11) N31 0.0206(12) 0.0362(14) 0.0155(11) -0.0004(10) -0.0025(9) -0.0023(10) O1 0.0207(9) 0.0129(9) 0.0191(9) 0.0017(7) -0.0010(7) -0.0003(7) O2 0.0248(10) 0.0201(9) 0.0133(9) -0.0047(7) -0.0003(7) -0.0002(8) O3 0.0490(14) 0.0343(12) 0.0425(14) 0.0042(10) -0.0262(12) -0.0183(11) O4 0.0431(13) 0.0263(11) 0.0201(11) 0.0017(9) 0.0039(9) -0.0164(10) O5 0.0610(16) 0.0429(14) 0.0213(11) -0.0055(10) -0.0129(11) -0.0055(12) O6 0.0552(15) 0.0325(12) 0.0334(13) -0.0015(10) -0.0179(11) 0.0036(11) O7 0.0367(13) 0.0419(13) 0.0374(13) 0.0055(10) -0.0248(11) -0.0048(10) O8 0.0330(12) 0.0336(12) 0.0333(12) -0.0093(10) -0.0093(10) 0.0017(9) _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 N15 2.231(2) 2_466 ? Ag1 N20 2.324(2) 1_565 ? Ag1 N10 2.339(2) . ? Ag1 N32B 2.599(8) . ? Ag1 N29 2.668(2) . ? C1 C6 1.389(3) . ? C1 C2 1.398(3) . ? C1 N28 1.475(3) . ? C2 C3 1.388(3) . ? C2 N23 1.409(3) . ? C3 C4 1.383(3) . ? C3 N22 1.478(3) . ? C4 C5 1.393(3) . ? C4 N17 1.417(3) . ? C5 C6 1.390(3) . ? C5 N12 1.415(3) . ? C6 N7 1.415(3) . ? C9 N8 1.316(3) . ? C9 N10 1.369(3) . ? C9 H9A 0.9500 . ? C11 N10 1.319(3) . ? C11 N7 1.350(3) . ? C11 H11A 0.9500 . ? C14 N13 1.310(3) . ? C14 N15 1.367(3) . ? C14 H14A 0.9500 . ? C16 N15 1.309(3) . ? C16 N12 1.347(3) . ? C16 H16A 0.9500 . ? C19 N18 1.310(3) . ? C19 N20 1.358(3) . ? C19 H19A 0.9500 . ? C21 N20 1.313(3) . ? C21 N17 1.348(3) . ? C21 H21A 0.9500 . ? C25 N24 1.307(3) . ? C25 N26 1.367(4) . ? C25 H25A 0.9500 . ? C27 N26 1.310(3) . ? C27 N23 1.361(3) . ? C27 H27A 0.9500 . ? N7 N8 1.374(3) . ? N12 N13 1.379(3) . ? N15 Ag1 2.231(2) 2_466 ? N17 N18 1.365(3) . ? N20 Ag1 2.324(2) 1_545 ? N22 O4 1.207(3) . ? N22 O3 1.221(3) . ? N23 N24 1.377(3) . ? N28 O1 1.220(3) . ? N28 O2 1.224(3) . ? N29 N31 1.373(3) . ? N29 N30 1.377(3) . ? N30 O5 1.234(3) . ? N30 O6 1.235(3) . ? N31 O7 1.226(3) . ? N31 O8 1.233(3) . ? N32A C33A 1.136(8) . ? C33A C34A 1.410(9) . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? N32B C33B 1.132(8) . ? C33B C34B 1.430(8) . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? N32C C33C 1.128(9) . ? C33C C34C 1.439(10) . ? C34C H34G 0.9800 . ? C34C H34H 0.9800 . ? C34C H34I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N15 Ag1 N20 136.79(8) 2_466 1_565 ? N15 Ag1 N10 130.21(8) 2_466 . ? N20 Ag1 N10 92.21(7) 1_565 . ? N15 Ag1 N32B 84.4(2) 2_466 . ? N20 Ag1 N32B 85.9(2) 1_565 . ? N10 Ag1 N32B 92.9(2) . . ? N15 Ag1 N29 86.51(8) 2_466 . ? N20 Ag1 N29 105.29(8) 1_565 . ? N10 Ag1 N29 88.03(7) . . ? N32B Ag1 N29 168.8(2) . . ? C6 C1 C2 121.9(2) . . ? C6 C1 N28 118.8(2) . . ? C2 C1 N28 119.2(2) . . ? C3 C2 C1 117.0(2) . . ? C3 C2 N23 122.3(2) . . ? C1 C2 N23 120.5(2) . . ? C4 C3 C2 122.6(2) . . ? C4 C3 N22 118.1(2) . . ? C2 C3 N22 118.9(2) . . ? C3 C4 C5 119.0(2) . . ? C3 C4 N17 120.7(2) . . ? C5 C4 N17 120.2(2) . . ? C6 C5 C4 120.1(2) . . ? C6 C5 N12 119.7(2) . . ? C4 C5 N12 120.1(2) . . ? C1 C6 C5 119.2(2) . . ? C1 C6 N7 121.9(2) . . ? C5 C6 N7 118.9(2) . . ? N8 C9 N10 115.0(2) . . ? N8 C9 H9A 122.5 . . ? N10 C9 H9A 122.5 . . ? N10 C11 N7 109.3(2) . . ? N10 C11 H11A 125.3 . . ? N7 C11 H11A 125.3 . . ? N13 C14 N15 114.9(2) . . ? N13 C14 H14A 122.5 . . ? N15 C14 H14A 122.5 . . ? N15 C16 N12 109.5(2) . . ? N15 C16 H16A 125.3 . . ? N12 C16 H16A 125.3 . . ? N18 C19 N20 115.5(2) . . ? N18 C19 H19A 122.3 . . ? N20 C19 H19A 122.3 . . ? N20 C21 N17 109.6(2) . . ? N20 C21 H21A 125.2 . . ? N17 C21 H21A 125.2 . . ? N24 C25 N26 116.0(2) . . ? N24 C25 H25A 122.0 . . ? N26 C25 H25A 122.0 . . ? N26 C27 N23 109.9(2) . . ? N26 C27 H27A 125.0 . . ? N23 C27 H27A 125.0 . . ? C11 N7 N8 110.4(2) . . ? C11 N7 C6 128.6(2) . . ? N8 N7 C6 120.08(19) . . ? C9 N8 N7 101.7(2) . . ? C11 N10 C9 103.5(2) . . ? C11 N10 Ag1 117.95(17) . . ? C9 N10 Ag1 138.27(17) . . ? C16 N12 N13 110.1(2) . . ? C16 N12 C5 129.1(2) . . ? N13 N12 C5 120.8(2) . . ? C14 N13 N12 101.7(2) . . ? C16 N15 C14 103.9(2) . . ? C16 N15 Ag1 126.28(18) . 2_466 ? C14 N15 Ag1 129.19(17) . 2_466 ? C21 N17 N18 110.0(2) . . ? C21 N17 C4 129.7(2) . . ? N18 N17 C4 120.2(2) . . ? C19 N18 N17 101.7(2) . . ? C21 N20 C19 103.2(2) . . ? C21 N20 Ag1 129.84(18) . 1_545 ? C19 N20 Ag1 124.54(17) . 1_545 ? O4 N22 O3 126.7(2) . . ? O4 N22 C3 118.1(2) . . ? O3 N22 C3 115.2(2) . . ? C27 N23 N24 109.5(2) . . ? C27 N23 C2 132.1(2) . . ? N24 N23 C2 118.0(2) . . ? C25 N24 N23 101.6(2) . . ? C27 N26 C25 102.9(2) . . ? O1 N28 O2 125.4(2) . . ? O1 N28 C1 118.0(2) . . ? O2 N28 C1 116.61(19) . . ? N31 N29 N30 113.8(2) . . ? N31 N29 Ag1 105.28(16) . . ? N30 N29 Ag1 133.02(17) . . ? O5 N30 O6 123.1(3) . . ? O5 N30 N29 123.7(2) . . ? O6 N30 N29 113.0(2) . . ? O7 N31 O8 122.4(3) . . ? O7 N31 N29 123.6(2) . . ? O8 N31 N29 113.7(2) . . ? N32A C33A C34A 164.7(12) . . ? C33B N32B Ag1 147.7(9) . . ? N32B C33B C34B 175.4(14) . . ? C33B C34B H34D 109.5 . . ? C33B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? N32C C33C C34C 167(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.897 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.091