Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Wenbin Lin' 'Helen L. Ngo' 'Chuan-De Wu' _publ_contact_author_name 'Prof Wenbin Lin' _publ_contact_author_address ; Dept of Chemistry Univ of North Carolina #3290 Chapel Hill NC 27599 UNITED STATES OF AMERICA ; _publ_contact_author_email WLIN@UNC.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Luminescent homochiral silver(I) lamellar coordination networks built from helical chains ; data_data1 _database_code_depnum_ccdc_archive 'CCDC 233672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H56 Ag N5 O7' _chemical_formula_weight 1211.09 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 33.739(16) _cell_length_b 9.704(3) _cell_length_c 8.672(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.92(4) _cell_angle_gamma 90.00 _cell_volume 2824.1(17) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 25.09 _exptl_crystal_description Bloc _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1252 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.8493 _exptl_absorpt_correction_T_max 1.0000 _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 none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11493 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.09 _reflns_number_total 4853 _reflns_number_gt 4670 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0315P)^2^+0.4619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(14) _refine_ls_number_reflns 4853 _refine_ls_number_parameters 385 _refine_ls_number_restraints 1 _refine_ls_R_factor_ref 0.0287 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.89042(2) 0.5000 0.02792(8) Uani 1 2 d S . . O1 O 0.84474(5) 0.54053(17) 0.59605(17) 0.0272(4) Uani 1 1 d . . . O2 O 0.77231(5) 0.76889(19) 0.42707(18) 0.0315(4) Uani 1 1 d . . . O3 O 0.98610(5) 0.8980(3) 0.88127(18) 0.0413(4) Uani 1 1 d . . . O4 O 1.0000 1.0888(3) 1.0000 0.0520(8) Uani 1 2 d S . . N1 N 0.97605(6) 0.4525(2) 1.2599(2) 0.0246(4) Uani 1 1 d . . . N2 N 0.55597(6) 0.7450(2) 0.4605(2) 0.0279(5) Uani 1 1 d . . . N3 N 1.0000 0.9616(3) 1.0000 0.0268(6) Uani 1 2 d S . . C1 C 0.96486(7) 0.3518(2) 1.1590(3) 0.0270(6) Uani 1 1 d . . . H1A H 0.9695 0.2610 1.1903 0.032 Uiso 1 1 calc R . . C2 C 0.94683(7) 0.3754(3) 1.0113(2) 0.0257(5) Uani 1 1 d . . . H2A H 0.9394 0.3017 0.9462 0.031 Uiso 1 1 calc R . . C3 C 0.93984(7) 0.5103(3) 0.9601(3) 0.0235(5) Uani 1 1 d . . . C4 C 0.95255(8) 0.6145(3) 1.0634(3) 0.0281(6) Uani 1 1 d . . . H4A H 0.9491 0.7064 1.0344 0.034 Uiso 1 1 calc R . . C5 C 0.97030(7) 0.5815(3) 1.2091(3) 0.0260(5) Uani 1 1 d . . . H5A H 0.9787 0.6532 1.2758 0.031 Uiso 1 1 calc R . . C6 C 0.91918(7) 0.5367(3) 0.8053(3) 0.0260(5) Uani 1 1 d . . . H6A H 0.9038 0.4663 0.7571 0.031 Uiso 1 1 calc R . . C7 C 0.92119(8) 0.6556(3) 0.7303(3) 0.0261(6) Uani 1 1 d . . . H7A H 0.9370 0.7235 0.7811 0.031 Uiso 1 1 calc R . . C8 C 0.90142(7) 0.6928(3) 0.5765(3) 0.0239(5) Uani 1 1 d . . . C9 C 0.91908(7) 0.7896(3) 0.4911(3) 0.0267(5) Uani 1 1 d . . . H9A H 0.9425 0.8310 0.5341 0.032 Uiso 1 1 calc R . . C10 C 0.90321(7) 0.8294(3) 0.3400(3) 0.0255(5) Uani 1 1 d . . . C11 C 0.92183(8) 0.9297(2) 0.2543(3) 0.0299(6) Uani 1 1 d . . . H11A H 0.9449 0.9727 0.2982 0.036 Uiso 1 1 calc R . . C12 C 0.90639(9) 0.9643(3) 0.1076(3) 0.0357(6) Uani 1 1 d . . . H12A H 0.9188 1.0310 0.0523 0.043 Uiso 1 1 calc R . . C13 C 0.87191(7) 0.8991(5) 0.0412(2) 0.0387(6) Uani 1 1 d . . . H13A H 0.8617 0.9220 -0.0592 0.046 Uiso 1 1 calc R . . C14 C 0.85285(8) 0.8019(3) 0.1209(3) 0.0314(6) Uani 1 1 d . . . H14A H 0.8300 0.7596 0.0740 0.038 Uiso 1 1 calc R . . C15 C 0.86761(7) 0.7652(3) 0.2742(3) 0.0252(5) Uani 1 1 d . . . C16 C 0.84791(7) 0.6681(2) 0.3642(2) 0.0217(5) Uani 1 1 d . . . C17 C 0.86446(7) 0.6358(2) 0.5123(3) 0.0223(5) Uani 1 1 d . . . C18 C 0.82500(9) 0.6001(3) 0.7187(3) 0.0370(6) Uani 1 1 d . . . H18A H 0.8123 0.5288 0.7723 0.056 Uiso 1 1 calc R . . H18B H 0.8053 0.6649 0.6760 0.056 Uiso 1 1 calc R . . H18C H 0.8442 0.6466 0.7900 0.056 Uiso 1 1 calc R . . C19 C 0.76890(8) 0.8909(5) 0.3343(3) 0.0435(6) Uani 1 1 d . . . H19A H 0.7679 0.9700 0.4002 0.065 Uiso 1 1 calc R . . H19B H 0.7450 0.8866 0.2643 0.065 Uiso 1 1 calc R . . H19C H 0.7915 0.8980 0.2761 0.065 Uiso 1 1 calc R . . C20 C 0.80959(7) 0.6003(2) 0.3029(2) 0.0226(5) Uani 1 1 d . . . C21 C 0.81046(7) 0.4756(3) 0.2136(2) 0.0229(5) Uani 1 1 d . . . C22 C 0.84580(7) 0.4242(3) 0.1599(3) 0.0281(6) Uani 1 1 d . . . H22A H 0.8694 0.4737 0.1791 0.034 Uiso 1 1 calc R . . C23 C 0.84563(8) 0.3028(3) 0.0802(3) 0.0352(6) Uani 1 1 d . . . H23A H 0.8691 0.2704 0.0457 0.042 Uiso 1 1 calc R . . C24 C 0.81029(9) 0.2262(3) 0.0498(3) 0.0376(7) Uani 1 1 d . . . H24A H 0.8107 0.1422 -0.0016 0.045 Uiso 1 1 calc R . . C25 C 0.77536(8) 0.2748(3) 0.0955(3) 0.0336(6) Uani 1 1 d . . . H25A H 0.7520 0.2247 0.0728 0.040 Uiso 1 1 calc R . . C26 C 0.77440(6) 0.4015(4) 0.1775(2) 0.0271(5) Uani 1 1 d . . . C27 C 0.73864(8) 0.4539(3) 0.2247(3) 0.0286(5) Uani 1 1 d . . . H27A H 0.7152 0.4044 0.2012 0.034 Uiso 1 1 calc R . . C28 C 0.73726(7) 0.5757(3) 0.3043(3) 0.0265(5) Uani 1 1 d . . . C29 C 0.77365(7) 0.6482(2) 0.3415(2) 0.0242(5) Uani 1 1 d . . . C30 C 0.70004(7) 0.6321(3) 0.3523(3) 0.0280(5) Uani 1 1 d . . . H30A H 0.7007 0.7227 0.3875 0.034 Uiso 1 1 calc R . . C31 C 0.66542(8) 0.5658(3) 0.3501(3) 0.0311(6) Uani 1 1 d . . . H31A H 0.6649 0.4736 0.3207 0.037 Uiso 1 1 calc R . . C32 C 0.59156(8) 0.7891(3) 0.5272(3) 0.0306(6) Uani 1 1 d . . . H32A H 0.5919 0.8608 0.5985 0.037 Uiso 1 1 calc R . . C33 C 0.62727(8) 0.7347(3) 0.4960(3) 0.0307(6) Uani 1 1 d . . . H33A H 0.6510 0.7696 0.5452 0.037 Uiso 1 1 calc R . . C34 C 0.62803(8) 0.6267(3) 0.3905(3) 0.0266(5) Uani 1 1 d . . . C35 C 0.59155(8) 0.5810(3) 0.3234(3) 0.0274(6) Uani 1 1 d . . . H35A H 0.5904 0.5085 0.2530 0.033 Uiso 1 1 calc R . . C36 C 0.55666(8) 0.6415(3) 0.3595(3) 0.0275(5) Uani 1 1 d . . . H36A H 0.5326 0.6087 0.3114 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02195(13) 0.04206(16) 0.01871(11) 0.000 -0.00290(8) 0.000 O1 0.0303(10) 0.0270(9) 0.0230(8) 0.0023(7) -0.0029(7) -0.0054(8) O2 0.0313(10) 0.0348(10) 0.0279(9) -0.0096(8) 0.0000(7) 0.0054(8) O3 0.0490(10) 0.0338(9) 0.0384(8) -0.0055(12) -0.0089(7) -0.0050(14) O4 0.075(2) 0.0180(14) 0.0599(19) 0.000 -0.0080(16) 0.000 N1 0.0236(11) 0.0305(10) 0.0197(10) 0.0019(9) 0.0021(8) 0.0057(9) N2 0.0224(11) 0.0318(11) 0.0293(10) -0.0008(9) 0.0016(8) 0.0014(10) N3 0.0215(16) 0.0217(15) 0.0367(16) 0.000 0.0001(12) 0.000 C1 0.0325(13) 0.0235(14) 0.0243(11) 0.0008(9) 0.0000(10) 0.0034(10) C2 0.0298(11) 0.0242(14) 0.0227(9) -0.0024(12) 0.0013(8) 0.0006(14) C3 0.0185(12) 0.0311(14) 0.0206(11) -0.0002(10) 0.0002(9) 0.0015(11) C4 0.0333(15) 0.0236(12) 0.0263(12) 0.0030(10) -0.0026(10) 0.0018(11) C5 0.0274(13) 0.0276(13) 0.0220(11) -0.0037(10) -0.0016(10) 0.0004(11) C6 0.0239(13) 0.0285(13) 0.0241(11) -0.0038(10) -0.0045(10) 0.0000(11) C7 0.0240(14) 0.0310(15) 0.0216(12) -0.0020(10) -0.0059(10) -0.0029(11) C8 0.0253(14) 0.0241(12) 0.0214(12) -0.0016(10) -0.0028(10) 0.0014(11) C9 0.0244(13) 0.0282(13) 0.0262(12) -0.0040(10) -0.0044(10) -0.0022(11) C10 0.0226(13) 0.0275(12) 0.0266(12) -0.0014(10) 0.0027(10) 0.0035(10) C11 0.0277(13) 0.0289(15) 0.0326(12) 0.0010(10) 0.0009(10) -0.0013(10) C12 0.0382(17) 0.0342(15) 0.0358(14) 0.0107(12) 0.0089(12) 0.0011(13) C13 0.0381(13) 0.0518(16) 0.0257(10) 0.0148(18) 0.0000(9) 0.010(2) C14 0.0253(14) 0.0455(16) 0.0226(11) 0.0026(11) -0.0018(10) 0.0033(12) C15 0.0230(13) 0.0283(13) 0.0242(11) -0.0011(10) 0.0027(10) 0.0069(11) C16 0.0181(12) 0.0255(12) 0.0210(10) -0.0036(9) -0.0010(9) 0.0037(10) C17 0.0248(13) 0.0193(12) 0.0226(12) -0.0009(10) 0.0011(10) 0.0022(10) C18 0.0293(15) 0.0510(17) 0.0310(13) 0.0025(12) 0.0040(11) -0.0042(13) C19 0.0515(15) 0.0336(12) 0.0445(12) -0.0086(19) 0.0009(11) 0.012(2) C20 0.0216(13) 0.0289(13) 0.0169(10) 0.0002(9) -0.0011(9) 0.0025(10) C21 0.0219(13) 0.0288(13) 0.0175(10) 0.0017(9) -0.0011(9) 0.0043(10) C22 0.0216(12) 0.0380(19) 0.0238(11) -0.0005(10) -0.0015(9) 0.0033(11) C23 0.0261(15) 0.0450(16) 0.0343(14) -0.0089(13) 0.0031(11) 0.0076(13) C24 0.0377(16) 0.0380(15) 0.0363(14) -0.0149(12) -0.0007(12) 0.0076(13) C25 0.0274(14) 0.0358(15) 0.0366(13) -0.0106(12) -0.0018(11) -0.0011(12) C26 0.0261(11) 0.0315(14) 0.0231(9) -0.0008(14) -0.0011(8) 0.0005(16) C27 0.0204(13) 0.0333(13) 0.0313(12) -0.0017(10) -0.0013(10) -0.0006(10) C28 0.0247(13) 0.0324(13) 0.0222(11) 0.0018(10) 0.0018(10) 0.0054(11) C29 0.0258(13) 0.0262(13) 0.0199(11) -0.0036(9) -0.0016(9) 0.0036(11) C30 0.0213(13) 0.0325(14) 0.0303(12) -0.0031(11) 0.0029(10) 0.0038(11) C31 0.0289(15) 0.0355(15) 0.0283(12) -0.0075(11) 0.0001(10) 0.0040(12) C32 0.0256(14) 0.0340(14) 0.0322(13) -0.0079(11) 0.0023(10) -0.0016(12) C33 0.0201(13) 0.0406(16) 0.0310(13) -0.0051(12) 0.0005(10) -0.0033(12) C34 0.0253(14) 0.0346(14) 0.0202(11) -0.0014(10) 0.0033(10) -0.0005(11) C35 0.0274(15) 0.0313(15) 0.0236(13) -0.0042(11) 0.0030(11) -0.0025(12) C36 0.0231(13) 0.0323(14) 0.0263(12) -0.0026(10) -0.0014(10) -0.0040(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.237(2) 4_657 ? Ag1 N1 2.237(2) 3_454 ? Ag1 N2 2.410(2) 2_656 ? Ag1 N2 2.410(2) . ? O1 C17 1.387(3) . ? O1 C18 1.434(3) . ? O2 C29 1.389(3) . ? O2 C19 1.429(4) . ? O3 N3 1.250(2) . ? O4 N3 1.235(4) . ? N1 C5 1.334(3) . ? N1 C1 1.339(3) . ? N1 Ag1 2.237(2) 3_546 ? N2 C36 1.334(3) . ? N2 C32 1.348(3) . ? N3 O3 1.250(2) 2_757 ? C1 C2 1.379(3) . ? C2 C3 1.395(4) . ? C3 C4 1.389(3) . ? C3 C6 1.470(3) . ? C4 C5 1.379(3) . ? C6 C7 1.329(4) . ? C7 C8 1.473(3) . ? C8 C9 1.370(4) . ? C8 C17 1.424(3) . ? C9 C10 1.417(3) . ? C10 C11 1.411(3) . ? C10 C15 1.420(4) . ? C11 C12 1.366(4) . ? C12 C13 1.396(4) . ? C13 C14 1.368(4) . ? C14 C15 1.416(3) . ? C15 C16 1.431(3) . ? C16 C17 1.383(3) . ? C16 C20 1.498(3) . ? C20 C29 1.372(3) . ? C20 C21 1.438(3) . ? C21 C22 1.415(3) . ? C21 C26 1.420(4) . ? C22 C23 1.366(4) . ? C23 C24 1.406(4) . ? C24 C25 1.366(4) . ? C25 C26 1.421(4) . ? C26 C27 1.409(4) . ? C27 C28 1.372(4) . ? C28 C29 1.423(4) . ? C28 C30 1.469(3) . ? C30 C31 1.332(4) . ? C31 C34 1.468(4) . ? C32 C33 1.368(4) . ? C33 C34 1.393(4) . ? C34 C35 1.379(4) . ? C35 C36 1.380(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 148.77(11) 4_657 3_454 ? N1 Ag1 N2 103.79(7) 4_657 2_656 ? N1 Ag1 N2 94.40(8) 3_454 2_656 ? N1 Ag1 N2 94.40(8) 4_657 . ? N1 Ag1 N2 103.79(7) 3_454 . ? N2 Ag1 N2 108.32(10) 2_656 . ? C17 O1 C18 113.8(2) . . ? C29 O2 C19 113.75(18) . . ? C5 N1 C1 116.58(19) . . ? C5 N1 Ag1 125.86(16) . 3_546 ? C1 N1 Ag1 117.50(15) . 3_546 ? C36 N2 C32 116.5(2) . . ? C36 N2 Ag1 126.93(16) . . ? C32 N2 Ag1 115.42(17) . . ? O4 N3 O3 119.61(16) . . ? O4 N3 O3 119.61(16) . 2_757 ? O3 N3 O3 120.8(3) . 2_757 ? N1 C1 C2 123.5(2) . . ? C1 C2 C3 119.7(2) . . ? C4 C3 C2 116.5(2) . . ? C4 C3 C6 123.2(2) . . ? C2 C3 C6 120.2(2) . . ? C5 C4 C3 119.8(2) . . ? N1 C5 C4 123.7(2) . . ? C7 C6 C3 123.7(2) . . ? C6 C7 C8 127.9(2) . . ? C9 C8 C17 117.8(2) . . ? C9 C8 C7 118.4(2) . . ? C17 C8 C7 123.7(2) . . ? C8 C9 C10 122.9(2) . . ? C11 C10 C9 121.9(2) . . ? C11 C10 C15 119.7(2) . . ? C9 C10 C15 118.4(2) . . ? C12 C11 C10 120.9(2) . . ? C11 C12 C13 119.6(3) . . ? C14 C13 C12 121.3(2) . . ? C13 C14 C15 120.7(2) . . ? C14 C15 C10 117.9(2) . . ? C14 C15 C16 122.7(2) . . ? C10 C15 C16 119.4(2) . . ? C17 C16 C15 119.4(2) . . ? C17 C16 C20 118.8(2) . . ? C15 C16 C20 121.88(19) . . ? C16 C17 O1 117.9(2) . . ? C16 C17 C8 121.9(2) . . ? O1 C17 C8 120.1(2) . . ? C29 C20 C21 119.0(2) . . ? C29 C20 C16 121.1(2) . . ? C21 C20 C16 119.7(2) . . ? C22 C21 C26 118.7(2) . . ? C22 C21 C20 122.6(2) . . ? C26 C21 C20 118.7(2) . . ? C23 C22 C21 120.7(2) . . ? C22 C23 C24 120.6(2) . . ? C25 C24 C23 120.2(2) . . ? C24 C25 C26 120.6(2) . . ? C27 C26 C21 119.5(3) . . ? C27 C26 C25 121.5(2) . . ? C21 C26 C25 119.0(2) . . ? C28 C27 C26 122.2(3) . . ? C27 C28 C29 117.8(2) . . ? C27 C28 C30 122.5(2) . . ? C29 C28 C30 119.6(2) . . ? C20 C29 O2 119.6(2) . . ? C20 C29 C28 122.7(2) . . ? O2 C29 C28 117.6(2) . . ? C31 C30 C28 126.2(2) . . ? C30 C31 C34 125.2(2) . . ? N2 C32 C33 123.8(2) . . ? C32 C33 C34 119.8(2) . . ? C35 C34 C33 116.3(2) . . ? C35 C34 C31 121.4(2) . . ? C33 C34 C31 122.3(2) . . ? C34 C35 C36 120.9(2) . . ? N2 C36 C35 122.8(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.310 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.040 #===END data_data2 _database_code_depnum_ccdc_archive 'CCDC 233673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H56 Ag Cl N4 O8' _chemical_formula_weight 1248.53 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 34.6314(9) _cell_length_b 10.2182(2) _cell_length_c 8.3801(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.780(2) _cell_angle_gamma 90.00 _cell_volume 2964.04(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.99 _cell_measurement_theta_max 23.29 _exptl_crystal_description Bloc _exptl_crystal_colour Colorless _exptl_crystal_size_max .70 _exptl_crystal_size_mid .50 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.448 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7060 _exptl_absorpt_correction_T_max 1.0000 _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 none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7711 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 23.29 _reflns_number_total 4024 _reflns_number_gt 3620 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0479P)^2^+6.8762P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(4) _refine_ls_number_reflns 4024 _refine_ls_number_parameters 389 _refine_ls_number_restraints 4 _refine_ls_R_factor_ref 0.0543 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.117 _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 0.0000 0.86326(7) -1.0000 0.0533(3) Uani 1 2 d S . . Cl1 Cl 0.0000 1.4758(3) -1.5000 0.0806(10) Uani 1 2 d S . . O1 O 0.26464(12) 0.7124(4) -1.0464(5) 0.0499(11) Uani 1 1 d . . . O2 O 0.33695(13) 0.4937(5) -0.8802(5) 0.0532(12) Uani 1 1 d . . . O3 O 0.0272(2) 1.5586(8) -1.5745(10) 0.116(3) Uani 1 1 d . . . O4 O -0.0195(2) 1.3961(5) -1.6149(8) 0.129(3) Uani 1 1 d . . . N1 N 0.05529(13) 0.7310(5) -1.0496(6) 0.0441(13) Uani 1 1 d . . . N2 N 0.47609(14) 0.4489(6) -0.2327(6) 0.0457(13) Uani 1 1 d . . . C1 C 0.08912(18) 0.7736(7) -0.9898(8) 0.0510(17) Uani 1 1 d . . . H1A H 0.0893 0.8497 -0.9246 0.061 Uiso 1 1 calc R . . C2 C 0.12376(18) 0.7130(7) -1.0174(7) 0.0479(16) Uani 1 1 d . . . H2A H 0.1470 0.7460 -0.9698 0.057 Uiso 1 1 calc R . . C4 C 0.0887(2) 0.5632(8) -1.1827(11) 0.065(2) Uani 1 1 d . . . H4A H 0.0875 0.4912 -1.2545 0.078 Uiso 1 1 calc R . . C5 C 0.05558(19) 0.6292(7) -1.1433(8) 0.0529(18) Uani 1 1 d . . . H5A H 0.0316 0.5987 -1.1871 0.063 Uiso 1 1 calc R . . C3 C 0.1246(2) 0.6049(7) -1.1138(9) 0.0436(18) Uani 1 1 d . . . C6 C 0.1611(2) 0.5385(7) -1.1560(7) 0.0540(18) Uani 1 1 d . . . H6A H 0.1592 0.4519 -1.1966 0.065 Uiso 1 1 calc R . . C7 C 0.19588(19) 0.5903(7) -1.1415(7) 0.0484(16) Uani 1 1 d . . . H7A H 0.1970 0.6749 -1.0945 0.058 Uiso 1 1 calc R . . C8 C 0.23291(18) 0.5358(6) -1.1878(7) 0.0420(15) Uani 1 1 d . . . C9 C 0.23585(19) 0.4217(6) -1.2733(7) 0.0468(16) Uani 1 1 d . . . H9A H 0.2129 0.3758 -1.3031 0.056 Uiso 1 1 calc R . . C10 C 0.27176(15) 0.3697(10) -1.3187(5) 0.0456(14) Uani 1 1 d . . . C11 C 0.2750(2) 0.2542(7) -1.4070(7) 0.0527(17) Uani 1 1 d . . . H11A H 0.2522 0.2073 -1.4378 0.063 Uiso 1 1 calc R . . C12 C 0.3098(2) 0.2081(7) -1.4495(8) 0.061(2) Uani 1 1 d . . . H12A H 0.3113 0.1284 -1.5073 0.073 Uiso 1 1 calc R . . C13 C 0.3438(2) 0.2780(8) -1.4081(8) 0.064(2) Uani 1 1 d . . . H13A H 0.3680 0.2459 -1.4412 0.077 Uiso 1 1 calc R . . C14 C 0.34251(19) 0.3903(8) -1.3219(6) 0.052(2) Uani 1 1 d . . . H14A H 0.3657 0.4359 -1.2952 0.062 Uiso 1 1 calc R . . C15 C 0.30616(18) 0.4402(6) -1.2711(6) 0.0439(15) Uani 1 1 d . . . C16 C 0.30341(17) 0.5556(6) -1.1768(6) 0.0416(15) Uani 1 1 d . . . C17 C 0.26754(18) 0.6009(6) -1.1406(6) 0.0436(16) Uani 1 1 d . . . C18 C 0.2590(2) 0.8299(6) -1.1368(8) 0.064(2) Uani 1 1 d . . . H18A H 0.2569 0.9044 -1.0639 0.095 Uiso 1 1 calc R . . H18B H 0.2353 0.8226 -1.2029 0.095 Uiso 1 1 calc R . . H18C H 0.2811 0.8433 -1.2056 0.095 Uiso 1 1 calc R . . C19 C 0.3168(2) 0.5443(7) -0.7482(8) 0.0576(18) Uani 1 1 d . . . H19A H 0.3049 0.4721 -0.6905 0.086 Uiso 1 1 calc R . . H19B H 0.2967 0.6049 -0.7869 0.086 Uiso 1 1 calc R . . H19C H 0.3349 0.5908 -0.6762 0.086 Uiso 1 1 calc R . . C20 C 0.33879(17) 0.6234(6) -1.1137(7) 0.0420(15) Uani 1 1 d . . . C21 C 0.35677(18) 0.7227(7) -1.2042(7) 0.0469(16) Uani 1 1 d . . . C22 C 0.34260(19) 0.7618(8) -1.3578(7) 0.0562(18) Uani 1 1 d . . . H22A H 0.3211 0.7177 -1.4057 0.067 Uiso 1 1 calc R . . C23 C 0.35949(19) 0.8617(14) -1.4372(8) 0.074(2) Uani 1 1 d . . . H23A H 0.3493 0.8864 -1.5394 0.089 Uiso 1 1 calc R . . C24 C 0.3912(2) 0.9284(9) -1.3726(10) 0.077(2) Uani 1 1 d . . . H24A H 0.4022 0.9997 -1.4280 0.093 Uiso 1 1 calc R . . C25 C 0.4063(2) 0.8895(11) -1.2281(8) 0.074(3) Uani 1 1 d . . . H25A H 0.4288 0.9321 -1.1863 0.089 Uiso 1 1 calc R . . C26 C 0.38983(19) 0.7891(7) -1.1390(8) 0.0530(17) Uani 1 1 d . . . C27 C 0.40543(19) 0.7435(9) -0.9900(8) 0.065(2) Uani 1 1 d . . . H27A H 0.4286 0.7832 -0.9500 0.078 Uiso 1 1 calc R . . C29 C 0.35497(19) 0.5887(7) -0.9674(7) 0.0483(17) Uani 1 1 d . . . C28 C 0.3896(2) 0.6466(9) -0.8997(9) 0.057(2) Uani 1 1 d D . . C30 C 0.4073(2) 0.5918(15) -0.7594(11) 0.119(5) Uani 1 1 d D . . H30A H 0.3995 0.5031 -0.7499 0.142 Uiso 1 1 calc R . . C31 C 0.4290(4) 0.619(2) -0.6474(13) 0.33(2) Uani 1 1 d D . . H31A H 0.4389 0.7062 -0.6463 0.393 Uiso 1 1 calc R . . C32 C 0.4413(3) 0.5401(18) -0.5209(11) 0.146(7) Uani 1 1 d D . . C33 C 0.4538(4) 0.6190(14) -0.4033(15) 0.128(6) Uani 1 1 d . . . H33A H 0.4505 0.7108 -0.4156 0.154 Uiso 1 1 calc R . . C34 C 0.4713(2) 0.5732(8) -0.2663(9) 0.069(2) Uani 1 1 d . . . H34A H 0.4805 0.6355 -0.1902 0.082 Uiso 1 1 calc R . . C35 C 0.4459(2) 0.4060(13) -0.4863(8) 0.093(4) Uani 1 1 d . . . H35A H 0.4367 0.3428 -0.5614 0.112 Uiso 1 1 calc R . . C36 C 0.46357(15) 0.3647(12) -0.3442(6) 0.0578(15) Uani 1 1 d . . . H36A H 0.4669 0.2736 -0.3259 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0362(3) 0.0860(6) 0.0367(3) 0.000 -0.0137(3) 0.000 Cl1 0.095(2) 0.0440(17) 0.100(2) 0.000 -0.0462(19) 0.000 O1 0.048(3) 0.060(3) 0.041(2) -0.013(2) -0.0096(19) 0.019(2) O2 0.060(3) 0.063(3) 0.036(2) 0.001(2) -0.008(2) 0.017(2) O3 0.088(5) 0.109(6) 0.149(7) 0.020(5) -0.013(5) -0.003(4) O4 0.206(7) 0.056(4) 0.117(4) 0.004(3) -0.105(5) -0.011(4) N1 0.036(3) 0.055(3) 0.040(3) -0.003(3) -0.004(2) -0.002(2) N2 0.041(3) 0.058(4) 0.038(3) 0.003(3) -0.008(2) 0.011(3) C1 0.037(4) 0.066(4) 0.050(4) -0.015(3) -0.001(3) -0.006(3) C2 0.036(4) 0.063(5) 0.044(4) -0.003(3) -0.003(3) -0.009(3) C4 0.051(5) 0.063(5) 0.081(6) -0.027(4) 0.002(4) -0.010(4) C5 0.041(4) 0.065(5) 0.052(4) -0.015(3) -0.009(3) -0.004(3) C3 0.042(4) 0.049(4) 0.040(4) -0.008(3) -0.007(3) 0.002(3) C6 0.052(4) 0.065(5) 0.045(4) -0.013(3) -0.004(3) 0.004(4) C7 0.045(4) 0.057(4) 0.043(3) -0.004(3) -0.002(3) 0.015(3) C8 0.044(4) 0.051(4) 0.031(3) -0.001(3) -0.006(3) 0.007(3) C9 0.047(4) 0.059(4) 0.035(3) 0.002(3) -0.002(3) 0.004(3) C10 0.051(3) 0.058(4) 0.028(2) -0.003(4) -0.007(2) 0.007(5) C11 0.062(4) 0.055(4) 0.041(4) -0.007(3) -0.003(3) 0.013(4) C12 0.079(6) 0.056(5) 0.048(4) -0.022(3) -0.007(4) 0.017(4) C13 0.067(5) 0.084(6) 0.041(4) -0.009(4) 0.004(4) 0.035(4) C14 0.051(4) 0.075(6) 0.029(3) -0.010(3) -0.001(2) 0.017(4) C15 0.050(4) 0.053(4) 0.028(3) -0.002(3) -0.007(3) 0.019(3) C16 0.044(4) 0.052(4) 0.028(3) 0.002(3) -0.004(3) 0.017(3) C17 0.047(4) 0.055(4) 0.029(3) -0.005(3) -0.005(3) 0.015(3) C18 0.085(5) 0.050(6) 0.054(4) -0.014(3) -0.013(3) 0.019(4) C19 0.054(4) 0.070(5) 0.049(4) -0.008(4) -0.003(3) 0.005(4) C20 0.038(3) 0.055(4) 0.032(3) -0.009(3) -0.009(3) 0.021(3) C21 0.040(4) 0.065(4) 0.035(3) -0.011(3) -0.012(3) 0.014(3) C22 0.048(4) 0.080(5) 0.039(4) 0.010(4) -0.011(3) 0.007(4) C23 0.062(4) 0.102(6) 0.059(4) 0.026(6) -0.012(3) 0.015(7) C24 0.062(5) 0.096(6) 0.074(5) 0.008(4) 0.001(4) -0.005(4) C25 0.049(4) 0.112(9) 0.060(4) -0.012(5) -0.009(3) -0.010(5) C26 0.042(4) 0.069(5) 0.048(4) -0.006(3) -0.002(3) 0.012(3) C27 0.036(4) 0.122(7) 0.038(4) -0.017(4) -0.011(3) 0.012(4) C29 0.043(4) 0.068(5) 0.034(3) -0.007(3) -0.003(3) 0.022(4) C28 0.046(5) 0.091(6) 0.035(4) 0.000(4) -0.015(4) 0.020(4) C30 0.036(5) 0.255(15) 0.065(6) -0.078(9) -0.007(4) 0.028(7) C31 0.200(17) 0.70(5) 0.084(9) 0.126(18) 0.075(10) 0.32(3) C32 0.095(8) 0.299(19) 0.045(5) 0.075(9) 0.032(5) 0.141(11) C33 0.146(12) 0.154(12) 0.089(8) 0.085(9) 0.056(8) 0.101(10) C34 0.064(5) 0.073(6) 0.070(5) 0.020(4) 0.022(4) 0.015(4) C35 0.039(4) 0.207(14) 0.032(3) -0.016(5) -0.008(3) 0.033(6) C36 0.045(3) 0.084(4) 0.044(3) 0.001(6) -0.004(3) 0.002(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 Ag1 N2 2.270(5) 4_554 ? Ag1 N2 2.270(5) 3_454 ? Ag1 N1 2.390(5) 2_553 ? Ag1 N1 2.390(5) . ? Cl1 O4 1.417(5) 2_552 ? Cl1 O4 1.417(5) . ? Cl1 O3 1.426(8) . ? Cl1 O3 1.426(8) 2_552 ? O1 C17 1.391(7) . ? O1 C18 1.430(8) . ? O2 C29 1.376(8) . ? O2 C19 1.424(8) . ? N1 C5 1.304(8) . ? N1 C1 1.333(8) . ? N2 C34 1.311(9) . ? N2 C36 1.333(10) . ? N2 Ag1 2.270(5) 3_546 ? C1 C2 1.376(9) . ? C2 C3 1.368(10) . ? C4 C5 1.379(10) . ? C4 C3 1.421(10) . ? C3 C6 1.488(10) . ? C6 C7 1.317(9) . ? C7 C8 1.462(9) . ? C8 C9 1.374(8) . ? C8 C17 1.417(9) . ? C9 C10 1.415(9) . ? C10 C11 1.400(11) . ? C10 C15 1.438(9) . ? C11 C12 1.352(10) . ? C12 C13 1.413(11) . ? C13 C14 1.357(10) . ? C14 C15 1.435(9) . ? C15 C16 1.424(8) . ? C16 C17 1.369(8) . ? C16 C20 1.490(8) . ? C20 C29 1.379(8) . ? C20 C21 1.421(9) . ? C21 C22 1.421(8) . ? C21 C26 1.425(9) . ? C22 C23 1.361(13) . ? C23 C24 1.389(12) . ? C24 C25 1.362(10) . ? C25 C26 1.401(11) . ? C26 C27 1.424(9) . ? C27 C28 1.371(11) . ? C29 C28 1.438(11) . ? C28 C30 1.425(12) . ? C30 C31 1.217(16) . ? C31 C32 1.390(14) . ? C32 C33 1.34(2) . ? C32 C35 1.409(18) . ? C33 C34 1.363(13) . ? C35 C36 1.388(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N2 134.6(3) 4_554 3_454 ? N2 Ag1 N1 109.96(17) 4_554 2_553 ? N2 Ag1 N1 95.43(18) 3_454 2_553 ? N2 Ag1 N1 95.43(18) 4_554 . ? N2 Ag1 N1 109.96(17) 3_454 . ? N1 Ag1 N1 111.2(3) 2_553 . ? O4 Cl1 O4 109.8(5) 2_552 . ? O4 Cl1 O3 109.3(4) 2_552 . ? O4 Cl1 O3 110.6(5) . . ? O4 Cl1 O3 110.6(5) 2_552 2_552 ? O4 Cl1 O3 109.3(4) . 2_552 ? O3 Cl1 O3 107.2(7) . 2_552 ? C17 O1 C18 113.4(4) . . ? C29 O2 C19 113.4(5) . . ? C5 N1 C1 117.6(6) . . ? C5 N1 Ag1 125.2(4) . . ? C1 N1 Ag1 116.7(4) . . ? C34 N2 C36 116.0(7) . . ? C34 N2 Ag1 126.8(5) . 3_546 ? C36 N2 Ag1 117.1(5) . 3_546 ? N1 C1 C2 123.4(6) . . ? C3 C2 C1 119.8(6) . . ? C5 C4 C3 118.7(7) . . ? N1 C5 C4 123.8(6) . . ? C2 C3 C4 116.6(7) . . ? C2 C3 C6 122.9(6) . . ? C4 C3 C6 120.4(7) . . ? C7 C6 C3 125.2(7) . . ? C6 C7 C8 129.0(7) . . ? C9 C8 C17 117.9(6) . . ? C9 C8 C7 122.8(6) . . ? C17 C8 C7 119.3(6) . . ? C8 C9 C10 122.6(6) . . ? C11 C10 C9 122.9(6) . . ? C11 C10 C15 119.4(6) . . ? C9 C10 C15 117.7(7) . . ? C12 C11 C10 121.2(7) . . ? C11 C12 C13 120.2(6) . . ? C14 C13 C12 121.1(7) . . ? C13 C14 C15 120.1(7) . . ? C16 C15 C14 122.2(6) . . ? C16 C15 C10 120.0(6) . . ? C14 C15 C10 117.8(6) . . ? C17 C16 C15 118.7(6) . . ? C17 C16 C20 120.4(5) . . ? C15 C16 C20 120.9(5) . . ? C16 C17 O1 119.0(5) . . ? C16 C17 C8 123.0(6) . . ? O1 C17 C8 117.9(5) . . ? C29 C20 C21 119.0(6) . . ? C29 C20 C16 120.2(6) . . ? C21 C20 C16 120.8(5) . . ? C22 C21 C20 122.6(6) . . ? C22 C21 C26 117.6(7) . . ? C20 C21 C26 119.7(5) . . ? C23 C22 C21 120.8(7) . . ? C22 C23 C24 121.6(6) . . ? C25 C24 C23 118.7(8) . . ? C24 C25 C26 122.4(7) . . ? C25 C26 C27 123.9(7) . . ? C25 C26 C21 118.7(6) . . ? C27 C26 C21 117.3(7) . . ? C28 C27 C26 124.9(7) . . ? O2 C29 C20 118.4(6) . . ? O2 C29 C28 117.8(6) . . ? C20 C29 C28 123.8(7) . . ? C27 C28 C30 124.7(9) . . ? C27 C28 C29 115.0(6) . . ? C30 C28 C29 119.8(9) . . ? C31 C30 C28 141.8(18) . . ? C30 C31 C32 128(2) . . ? C33 C32 C31 107.2(16) . . ? C33 C32 C35 113.8(7) . . ? C31 C32 C35 139.0(17) . . ? C32 C33 C34 122.7(11) . . ? N2 C34 C33 124.3(10) . . ? C36 C35 C32 121.1(10) . . ? N2 C36 C35 122.0(10) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.840 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.056 #===END