# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_(S)-1AgBF4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H34 Ag B F4 N4 O4' _chemical_formula_weight 877.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' _cell_length_a 8.2318(3) _cell_length_b 13.8544(5) _cell_length_c 41.7301(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4759.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used 9683 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 25.21 _exptl_crystal_description 'rod' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8616 _exptl_absorpt_correction_T_max 0.9536 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(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 APEXII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8406 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8406 _reflns_number_gt 6470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was dealt using SQUEEZE method with solvent removed. The methoxy group is disordered over two sites, with occupancy factors of 0.70 and 0.30. These atoms were refined isotropically. The tetrafluoroborate was restrained to a ideal tetrahedron, with isotropic refinements. ; _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^)+(0.1750P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(6) _refine_ls_number_reflns 8406 _refine_ls_number_parameters 498 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2390 _refine_ls_wR_factor_gt 0.2262 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.72223(5) 0.7500 0.0592(3) Uani 1 2 d S . . Ag2 Ag 0.5000 -0.27762(6) 0.7500 0.0779(3) Uani 1 2 d S . . O1 O 0.0661(5) 0.2823(3) 0.84217(10) 0.0457(10) Uani 1 1 d . B . O3 O 0.3323(5) 0.1414(3) 0.84423(10) 0.0417(9) Uani 1 1 d . . . O4 O 0.6005(6) 0.1067(4) 0.85684(14) 0.0727(15) Uani 1 1 d . . . N1 N -0.0785(7) 0.7811(3) 0.79755(11) 0.0443(12) Uani 1 1 d . . . N2 N 0.0663(7) 0.6079(3) 0.78997(12) 0.0450(12) Uani 1 1 d . . . N3 N 0.5275(7) -0.3474(4) 0.79923(17) 0.0633(16) Uani 1 1 d . . . N4 N 0.3780(7) -0.1786(4) 0.78852(14) 0.0559(15) Uani 1 1 d . . . C1 C -0.1535(9) 0.8694(4) 0.80134(16) 0.0534(17) Uani 1 1 d . . . H1 H -0.1532 0.9115 0.7840 0.064 Uiso 1 1 calc R . . C2 C -0.2250(9) 0.8980(5) 0.82763(16) 0.0538(17) Uani 1 1 d . . . H2 H -0.2798 0.9567 0.8281 0.065 Uiso 1 1 calc R . . C3 C -0.2190(8) 0.8407(4) 0.85477(15) 0.0458(14) Uani 1 1 d . . . H3 H -0.2659 0.8611 0.8739 0.055 Uiso 1 1 calc R . . C4 C -0.1410(7) 0.7519(4) 0.85278(14) 0.0433(13) Uani 1 1 d . . . H4 H -0.1381 0.7111 0.8705 0.052 Uiso 1 1 calc R . . C5 C -0.0672(7) 0.7241(4) 0.82417(12) 0.0326(11) Uani 1 1 d . . . C6 C 0.0166(7) 0.6306(4) 0.82013(12) 0.0354(11) Uani 1 1 d . . . C7 C 0.0469(7) 0.5707(4) 0.84665(14) 0.0390(13) Uani 1 1 d . . . H7 H 0.0139 0.5895 0.8670 0.047 Uiso 1 1 calc R . . C8 C 0.1272(7) 0.4824(4) 0.84226(14) 0.0371(12) Uani 1 1 d . . . C9 C 0.1736(8) 0.4589(5) 0.81151(15) 0.0488(15) Uani 1 1 d . . . H9 H 0.2247 0.4003 0.8075 0.059 Uiso 1 1 calc R . . C10 C 0.1446(9) 0.5222(4) 0.78664(16) 0.0529(16) Uani 1 1 d . . . H10 H 0.1809 0.5050 0.7663 0.063 Uiso 1 1 calc R . . C11 C 0.1675(7) 0.4222(4) 0.87014(13) 0.0365(12) Uani 1 1 d . . . C12 C 0.2373(7) 0.4601(4) 0.89648(12) 0.0371(12) Uani 1 1 d . . . H12 H 0.2458 0.5269 0.8980 0.045 Uiso 1 1 calc R . . C13 C 0.2987(7) 0.4026(4) 0.92216(14) 0.0409(13) Uani 1 1 d . . . C14 C 0.3836(9) 0.4452(5) 0.94947(15) 0.0566(17) Uani 1 1 d . . . H14 H 0.3955 0.5117 0.9511 0.068 Uiso 1 1 calc R . . C15 C 0.4435(9) 0.3871(5) 0.97187(16) 0.0599(18) Uani 1 1 d . . . H15 H 0.4919 0.4142 0.9899 0.072 Uiso 1 1 calc R . . C16 C 0.4362(8) 0.2866(5) 0.96925(15) 0.0537(16) Uani 1 1 d . . . H16 H 0.4862 0.2479 0.9846 0.064 Uiso 1 1 calc R . . C17 C 0.3560(7) 0.2455(5) 0.94428(13) 0.0404(13) Uani 1 1 d . . . H17 H 0.3502 0.1786 0.9432 0.048 Uiso 1 1 calc R . . C18 C 0.2797(7) 0.3017(4) 0.91958(14) 0.0385(13) Uani 1 1 d . . . C19 C 0.1936(6) 0.2605(4) 0.89360(14) 0.0343(12) Uani 1 1 d . . . C20 C 0.1410(7) 0.3193(4) 0.86940(13) 0.0355(12) Uani 1 1 d . . . C21 C -0.0956(9) 0.2505(5) 0.8464(2) 0.073(2) Uani 1 1 d D . . H21A H -0.1105 0.1868 0.8372 0.088 Uiso 0.70 1 calc PR A 1 H21B H -0.1230 0.2479 0.8690 0.088 Uiso 0.70 1 calc PR A 1 H21C H -0.0938 0.1990 0.8622 0.088 Uiso 0.30 1 calc PR A 2 H21D H -0.1310 0.2221 0.8264 0.088 Uiso 0.30 1 calc PR A 2 C23 C 0.1664(6) 0.1533(4) 0.89232(13) 0.0359(12) Uani 1 1 d . . . C24 C 0.0616(7) 0.1078(4) 0.91496(13) 0.0387(13) Uani 1 1 d . . . C25 C -0.0206(8) 0.1592(5) 0.93877(14) 0.0565(17) Uani 1 1 d . . . H25 H -0.0072 0.2257 0.9405 0.068 Uiso 1 1 calc R . . C26 C -0.1237(10) 0.1103(8) 0.96017(17) 0.080(3) Uani 1 1 d . . . H26 H -0.1750 0.1447 0.9764 0.096 Uiso 1 1 calc R . . C27 C -0.1499(11) 0.0140(7) 0.95754(17) 0.074(2) Uani 1 1 d . . . H27 H -0.2241 -0.0158 0.9711 0.089 Uiso 1 1 calc R . . C28 C -0.0682(10) -0.0405(6) 0.93510(18) 0.067(2) Uani 1 1 d . . . H28 H -0.0830 -0.1070 0.9342 0.081 Uiso 1 1 calc R . . C29 C 0.0412(7) 0.0071(4) 0.91281(14) 0.0468(15) Uani 1 1 d . . . C30 C 0.1122(7) -0.0446(4) 0.88813(15) 0.0457(15) Uani 1 1 d . . . H30 H 0.0955 -0.1109 0.8871 0.055 Uiso 1 1 calc R . . C31 C 0.2051(7) -0.0018(4) 0.86552(14) 0.0406(13) Uani 1 1 d . . . C32 C 0.2318(6) 0.0991(3) 0.86856(13) 0.0344(11) Uani 1 1 d . . . C33 C 0.4827(8) 0.1793(4) 0.85325(18) 0.0557(16) Uani 1 1 d . . . H33A H 0.5188 0.2250 0.8371 0.067 Uiso 1 1 calc R . . H33B H 0.4709 0.2139 0.8733 0.067 Uiso 1 1 calc R . . C34 C 0.6115(10) 0.0661(8) 0.8875(3) 0.090(3) Uani 1 1 d . . . H34A H 0.6458 0.1146 0.9025 0.108 Uiso 1 1 calc R . . H34B H 0.6891 0.0144 0.8873 0.108 Uiso 1 1 calc R . . H34C H 0.5072 0.0415 0.8938 0.108 Uiso 1 1 calc R . . C35 C 0.3196(10) -0.0866(5) 0.78345(17) 0.0622(19) Uani 1 1 d . . . H35 H 0.3153 -0.0643 0.7625 0.075 Uiso 1 1 calc R . . C36 C 0.2689(10) -0.0276(4) 0.80655(15) 0.0548(18) Uani 1 1 d . . . H36 H 0.2311 0.0340 0.8017 0.066 Uiso 1 1 calc R . . C37 C 0.2737(7) -0.0600(4) 0.83852(15) 0.0417(13) Uani 1 1 d . . . C38 C 0.3363(7) -0.1513(4) 0.84455(16) 0.0440(14) Uani 1 1 d . . . H38 H 0.3419 -0.1749 0.8654 0.053 Uiso 1 1 calc R . . C39 C 0.3902(8) -0.2064(4) 0.81909(17) 0.0482(15) Uani 1 1 d . . . C40 C 0.4662(7) -0.3045(4) 0.82480(18) 0.0462(15) Uani 1 1 d . . . C41 C 0.4729(9) -0.3465(4) 0.85470(19) 0.0589(17) Uani 1 1 d . . . H41 H 0.4250 -0.3154 0.8721 0.071 Uiso 1 1 calc R . . C42 C 0.5515(8) -0.4361(5) 0.8594(3) 0.083(3) Uani 1 1 d . . . H42 H 0.5579 -0.4646 0.8795 0.099 Uiso 1 1 calc R . . C43 C 0.6182(9) -0.4793(5) 0.8327(2) 0.068(2) Uani 1 1 d . . . H43 H 0.6718 -0.5382 0.8343 0.082 Uiso 1 1 calc R . . C44 C 0.6033(10) -0.4324(5) 0.8031(2) 0.074(2) Uani 1 1 d . . . H44 H 0.6485 -0.4618 0.7852 0.088 Uiso 1 1 calc R . . B1 B -0.3586(14) 0.7408(8) 0.9418(3) 0.151(6) Uiso 1 1 d D . . F1 F -0.4374(13) 0.8086(7) 0.9230(2) 0.202(4) Uiso 1 1 d D . . F2 F -0.4667(12) 0.6663(7) 0.9476(2) 0.203(4) Uiso 1 1 d D . . F3 F -0.3132(11) 0.7806(6) 0.97055(18) 0.173(3) Uiso 1 1 d D . . F4 F -0.2240(11) 0.7075(8) 0.9264(2) 0.214(5) Uiso 1 1 d D . . O2 O -0.1918(12) 0.3182(7) 0.8306(2) 0.101(2) Uiso 0.70 1 d PD B 1 C22 C -0.1769(19) 0.3157(11) 0.7955(2) 0.101(2) Uiso 0.70 1 d PD B 1 H22A H -0.0674 0.3311 0.7894 0.121 Uiso 0.70 1 calc PR B 1 H22B H -0.2499 0.3620 0.7862 0.121 Uiso 0.70 1 calc PR B 1 H22C H -0.2038 0.2523 0.7878 0.121 Uiso 0.70 1 calc PR B 1 O2' O -0.217(2) 0.3179(13) 0.8561(4) 0.086(5) Uiso 0.30 1 d PD B 2 C22' C -0.228(4) 0.327(2) 0.8913(4) 0.086(5) Uiso 0.30 1 d PD B 2 H22D H -0.3084 0.2834 0.8994 0.103 Uiso 0.30 1 calc PR B 2 H22E H -0.2586 0.3924 0.8967 0.103 Uiso 0.30 1 calc PR B 2 H22F H -0.1247 0.3128 0.9008 0.103 Uiso 0.30 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0964(6) 0.0481(4) 0.0331(3) 0.000 -0.0027(4) 0.000 Ag2 0.1006(7) 0.0518(5) 0.0814(6) 0.000 -0.0036(6) 0.000 O1 0.056(2) 0.034(2) 0.047(2) 0.0016(17) -0.0214(19) -0.0038(18) O3 0.040(2) 0.033(2) 0.052(2) 0.0061(17) 0.0049(19) -0.0079(16) O4 0.054(3) 0.082(4) 0.082(4) -0.016(3) 0.003(3) 0.019(3) N1 0.072(3) 0.030(2) 0.031(2) 0.006(2) -0.006(2) 0.005(2) N2 0.057(3) 0.031(2) 0.047(3) 0.001(2) 0.007(2) 0.006(2) N3 0.048(3) 0.043(3) 0.099(5) 0.018(3) 0.006(3) 0.003(3) N4 0.061(3) 0.037(3) 0.069(4) -0.008(3) -0.032(3) 0.010(3) C1 0.076(4) 0.033(3) 0.052(4) 0.003(3) -0.019(4) 0.018(3) C2 0.065(4) 0.041(3) 0.055(4) -0.012(3) -0.029(3) 0.012(3) C3 0.052(4) 0.032(3) 0.053(3) -0.004(3) 0.002(3) 0.001(3) C4 0.045(3) 0.040(3) 0.044(3) 0.006(2) 0.005(3) -0.001(3) C5 0.037(3) 0.029(3) 0.031(2) 0.006(2) -0.009(2) 0.000(2) C6 0.041(3) 0.035(3) 0.030(2) 0.003(2) -0.004(3) 0.001(3) C7 0.054(4) 0.022(2) 0.040(3) -0.002(2) -0.003(3) 0.006(2) C8 0.037(3) 0.027(3) 0.047(3) 0.001(2) -0.011(2) -0.004(2) C9 0.055(4) 0.039(3) 0.052(4) 0.003(3) 0.013(3) 0.009(3) C10 0.076(5) 0.035(3) 0.047(3) 0.001(3) 0.014(3) 0.008(3) C11 0.040(3) 0.029(3) 0.040(3) 0.001(2) -0.008(2) -0.001(2) C12 0.044(3) 0.029(2) 0.038(3) 0.003(2) -0.004(3) 0.000(2) C13 0.051(3) 0.028(3) 0.043(3) -0.007(2) -0.007(3) 0.000(2) C14 0.075(5) 0.048(4) 0.047(4) -0.014(3) -0.014(3) 0.000(3) C15 0.079(5) 0.055(4) 0.046(3) -0.009(3) -0.023(3) -0.001(3) C16 0.056(4) 0.063(4) 0.042(3) 0.016(3) -0.011(3) -0.009(3) C17 0.040(3) 0.049(3) 0.033(3) 0.005(2) -0.001(2) 0.001(3) C18 0.042(3) 0.031(3) 0.042(3) 0.002(2) -0.004(2) -0.007(2) C19 0.032(3) 0.025(3) 0.046(3) -0.003(2) -0.006(2) 0.0011(19) C20 0.037(3) 0.024(2) 0.045(3) -0.006(2) -0.008(2) 0.000(2) C21 0.060(4) 0.049(4) 0.110(7) -0.006(4) -0.049(5) -0.004(3) C23 0.032(3) 0.034(3) 0.041(3) 0.014(2) -0.012(2) -0.003(2) C24 0.035(3) 0.044(3) 0.037(3) 0.011(3) -0.009(2) -0.009(2) C25 0.051(4) 0.077(4) 0.042(3) 0.009(3) -0.006(3) -0.024(4) C26 0.066(5) 0.131(8) 0.044(4) 0.014(4) 0.005(4) -0.029(5) C27 0.075(5) 0.104(7) 0.044(4) 0.015(4) -0.001(4) -0.046(5) C28 0.082(5) 0.060(4) 0.060(4) 0.025(4) -0.021(4) -0.036(4) C29 0.049(4) 0.048(3) 0.043(3) 0.020(3) -0.013(3) -0.015(3) C30 0.045(3) 0.041(3) 0.050(3) 0.012(3) -0.015(3) -0.012(3) C31 0.041(3) 0.032(3) 0.049(3) 0.011(2) -0.015(3) -0.008(2) C32 0.025(2) 0.028(2) 0.051(3) 0.004(2) -0.011(2) -0.004(2) C33 0.039(3) 0.042(3) 0.086(5) 0.001(3) 0.015(3) -0.009(3) C34 0.054(5) 0.097(7) 0.119(8) -0.018(6) -0.030(5) 0.026(5) C35 0.081(5) 0.054(4) 0.051(4) 0.000(3) -0.023(4) 0.017(4) C36 0.084(5) 0.029(3) 0.052(3) -0.003(3) -0.033(4) 0.011(3) C37 0.042(3) 0.030(3) 0.053(3) 0.001(2) -0.009(3) -0.006(2) C38 0.041(3) 0.027(3) 0.064(4) 0.006(3) -0.021(3) -0.007(2) C39 0.047(3) 0.023(3) 0.074(4) 0.005(3) -0.014(3) -0.005(2) C40 0.035(3) 0.022(2) 0.082(4) 0.003(3) -0.009(3) -0.004(2) C41 0.060(4) 0.032(3) 0.084(4) 0.009(3) -0.016(4) 0.007(3) C42 0.040(4) 0.039(4) 0.169(9) 0.027(5) -0.019(5) -0.005(3) C43 0.053(4) 0.040(4) 0.113(7) 0.015(4) 0.000(4) 0.013(3) C44 0.064(5) 0.037(4) 0.119(7) 0.005(4) 0.002(5) 0.013(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 N1 2.240(5) 3_556 ? Ag1 N1 2.240(5) . ? Ag1 N2 2.364(5) . ? Ag1 N2 2.364(5) 3_556 ? Ag2 N3 2.282(7) . ? Ag2 N3 2.282(7) 3_656 ? Ag2 N4 2.340(6) . ? Ag2 N4 2.340(6) 3_656 ? O1 C20 1.391(7) . ? O1 C21 1.414(9) . ? O3 C32 1.435(7) . ? O3 C33 1.396(8) . ? O4 C34 1.402(11) . ? O4 C33 1.406(8) . ? N1 C5 1.367(7) . ? N1 C1 1.380(8) . ? N2 C6 1.360(7) . ? N2 C10 1.359(8) . ? N3 C40 1.322(9) . ? N3 C44 1.343(9) . ? N4 C39 1.337(9) . ? N4 C35 1.378(9) . ? C1 C2 1.306(10) . ? C1 H1 0.9300 . ? C2 C3 1.383(9) . ? C2 H2 0.9300 . ? C3 C4 1.391(8) . ? C3 H3 0.9300 . ? C4 C5 1.394(8) . ? C4 H4 0.9300 . ? C5 C6 1.476(8) . ? C6 C7 1.406(7) . ? C7 C8 1.403(8) . ? C7 H7 0.9300 . ? C8 C9 1.378(8) . ? C8 C11 1.470(8) . ? C9 C10 1.379(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.347(8) . ? C11 C20 1.441(7) . ? C12 C13 1.428(8) . ? C12 H12 0.9300 . ? C13 C18 1.411(8) . ? C13 C14 1.461(8) . ? C14 C15 1.328(10) . ? C14 H14 0.9300 . ? C15 C16 1.399(10) . ? C15 H15 0.9300 . ? C16 C17 1.358(9) . ? C16 H16 0.9300 . ? C17 C18 1.436(8) . ? C17 H17 0.9300 . ? C18 C19 1.415(8) . ? C19 C20 1.368(8) . ? C19 C23 1.503(8) . ? C21 O2 1.394(8) . ? C21 O2' 1.425(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21 H21D 0.9700 . ? C23 C32 1.355(8) . ? C23 C24 1.426(8) . ? C24 C25 1.397(9) . ? C24 C29 1.408(8) . ? C25 C26 1.406(10) . ? C25 H25 0.9300 . ? C26 C27 1.356(13) . ? C26 H26 0.9300 . ? C27 C28 1.378(12) . ? C27 H27 0.9300 . ? C28 C29 1.454(9) . ? C28 H28 0.9300 . ? C29 C30 1.384(9) . ? C30 C31 1.352(8) . ? C30 H30 0.9300 . ? C31 C32 1.420(7) . ? C31 C37 1.497(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.332(9) . ? C35 H35 0.9300 . ? C36 C37 1.408(9) . ? C36 H36 0.9300 . ? C37 C38 1.389(8) . ? C38 C39 1.382(10) . ? C38 H38 0.9300 . ? C39 C40 1.515(8) . ? C40 C41 1.378(10) . ? C41 C42 1.414(9) . ? C41 H41 0.9300 . ? C42 C43 1.377(13) . ? C42 H42 0.9300 . ? C43 C44 1.401(12) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? B1 F3 1.373(9) . ? B1 F2 1.385(9) . ? B1 F1 1.386(9) . ? B1 F4 1.361(9) . ? O2 C22 1.472(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? O2' C22' 1.478(10) . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? 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 137.3(2) 3_556 . ? N1 Ag1 N2 143.3(2) 3_556 . ? N1 Ag1 N2 71.68(16) . . ? N1 Ag1 N2 71.67(16) 3_556 3_556 ? N1 Ag1 N2 143.3(2) . 3_556 ? N2 Ag1 N2 95.9(3) . 3_556 ? N3 Ag2 N3 129.9(3) . 3_656 ? N3 Ag2 N4 70.9(2) . . ? N3 Ag2 N4 145.53(19) 3_656 . ? N3 Ag2 N4 145.53(19) . 3_656 ? N3 Ag2 N4 70.9(2) 3_656 3_656 ? N4 Ag2 N4 108.2(3) . 3_656 ? C20 O1 C21 115.4(5) . . ? C32 O3 C33 118.3(5) . . ? C34 O4 C33 115.4(6) . . ? C5 N1 C1 116.8(5) . . ? C5 N1 Ag1 119.3(4) . . ? C1 N1 Ag1 123.6(4) . . ? C6 N2 C10 116.1(5) . . ? C6 N2 Ag1 115.4(4) . . ? C10 N2 Ag1 128.6(4) . . ? C40 N3 C44 118.3(7) . . ? C40 N3 Ag2 119.9(4) . . ? C44 N3 Ag2 121.8(6) . . ? C39 N4 C35 116.1(6) . . ? C39 N4 Ag2 117.0(4) . . ? C35 N4 Ag2 125.9(5) . . ? C2 C1 N1 124.5(6) . . ? C2 C1 H1 117.8 . . ? N1 C1 H1 117.8 . . ? C1 C2 C3 119.9(6) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 118.4(6) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 119.8(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 N1 120.4(5) . . ? C4 C5 C6 123.0(5) . . ? N1 C5 C6 116.5(5) . . ? N2 C6 C7 122.6(5) . . ? N2 C6 C5 116.7(5) . . ? C7 C6 C5 120.7(5) . . ? C6 C7 C8 119.7(5) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 117.2(5) . . ? C9 C8 C11 122.7(5) . . ? C7 C8 C11 119.9(5) . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? N2 C10 C9 124.1(6) . . ? N2 C10 H10 117.9 . . ? C9 C10 H10 117.9 . . ? C12 C11 C20 117.9(5) . . ? C12 C11 C8 121.4(5) . . ? C20 C11 C8 120.7(5) . . ? C11 C12 C13 123.1(5) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C18 C13 C12 117.1(5) . . ? C18 C13 C14 120.8(5) . . ? C12 C13 C14 122.0(5) . . ? C15 C14 C13 118.8(6) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 122.1(6) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C17 C16 C15 119.8(6) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 122.5(6) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C13 C18 C19 120.9(5) . . ? C13 C18 C17 115.7(5) . . ? C19 C18 C17 123.4(5) . . ? C20 C19 C18 118.9(5) . . ? C20 C19 C23 121.0(5) . . ? C18 C19 C23 120.0(5) . . ? C19 C20 O1 121.6(5) . . ? C19 C20 C11 121.7(5) . . ? O1 C20 C11 116.7(5) . . ? O2 C21 O1 105.3(7) . . ? O2 C21 O2' 45.3(7) . . ? O1 C21 O2' 119.3(11) . . ? O2 C21 H21A 110.7 . . ? O1 C21 H21A 110.7 . . ? O2' C21 H21A 128.3 . . ? O2 C21 H21B 110.7 . . ? O1 C21 H21B 110.7 . . ? O2' C21 H21B 65.5 . . ? H21A C21 H21B 108.8 . . ? O2 C21 H21C 145.6 . . ? O1 C21 H21C 107.5 . . ? O2' C21 H21C 107.5 . . ? H21A C21 H21C 66.5 . . ? H21B C21 H21C 47.0 . . ? O2 C21 H21D 72.1 . . ? O1 C21 H21D 107.5 . . ? O2' C21 H21D 107.5 . . ? H21A C21 H21D 41.6 . . ? H21B C21 H21D 139.0 . . ? H21C C21 H21D 107.0 . . ? C32 C23 C24 118.7(5) . . ? C32 C23 C19 120.9(5) . . ? C24 C23 C19 120.2(5) . . ? C25 C24 C29 119.5(5) . . ? C25 C24 C23 122.6(5) . . ? C29 C24 C23 117.9(6) . . ? C24 C25 C26 119.9(7) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 121.2(9) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 121.1(7) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C29 119.2(7) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C24 120.7(5) . . ? C30 C29 C28 120.2(6) . . ? C24 C29 C28 118.9(6) . . ? C31 C30 C29 122.1(6) . . ? C31 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 117.2(6) . . ? C30 C31 C37 120.2(5) . . ? C32 C31 C37 122.6(5) . . ? C23 C32 O3 121.3(4) . . ? C23 C32 C31 123.3(5) . . ? O3 C32 C31 115.4(5) . . ? O4 C33 O3 111.8(5) . . ? O4 C33 H33A 109.3 . . ? O3 C33 H33A 109.3 . . ? O4 C33 H33B 109.3 . . ? O3 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? O4 C34 H34A 109.5 . . ? O4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N4 124.5(6) . . ? C36 C35 H35 117.8 . . ? N4 C35 H35 117.8 . . ? C35 C36 C37 118.8(5) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C38 C37 C36 118.2(6) . . ? C38 C37 C31 119.6(6) . . ? C36 C37 C31 122.1(5) . . ? C37 C38 C39 118.9(6) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? N4 C39 C38 123.4(5) . . ? N4 C39 C40 116.1(6) . . ? C38 C39 C40 120.5(6) . . ? N3 C40 C41 121.7(5) . . ? N3 C40 C39 115.7(6) . . ? C41 C40 C39 122.5(6) . . ? C40 C41 C42 120.9(8) . . ? C40 C41 H41 119.5 . . ? C42 C41 H41 119.5 . . ? C43 C42 C41 117.0(9) . . ? C43 C42 H42 121.5 . . ? C41 C42 H42 121.5 . . ? C44 C43 C42 118.4(7) . . ? C44 C43 H43 120.8 . . ? C42 C43 H43 120.8 . . ? N3 C44 C43 123.7(9) . . ? N3 C44 H44 118.2 . . ? C43 C44 H44 118.2 . . ? F3 B1 F2 108.8(8) . . ? F3 B1 F1 110.6(8) . . ? F2 B1 F1 107.7(8) . . ? F3 B1 F4 109.0(8) . . ? F2 B1 F4 110.6(8) . . ? F1 B1 F4 110.1(8) . . ? C21 O2 C22 114.2(8) . . ? C21 O2' C22' 112.7(10) . . ? O2' C22' H22D 109.5 . . ? O2' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? O2' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.246 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.142 data_(R)-1AgBF4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H34 Ag B F4 N4 O4' _chemical_formula_weight 877.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' _cell_length_a 8.2140(5) _cell_length_b 13.8169(7) _cell_length_c 41.563(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4717.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 186(2) _cell_measurement_reflns_used 9386 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 24.95 _exptl_crystal_description 'rod' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8337 _exptl_absorpt_correction_T_max 0.9222 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 186(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 APEXII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24328 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.11 _reflns_number_total 8397 _reflns_number_gt 5984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was dealt using SQUEEZE method to remove solvent molecules. One of the methoxy groups is disordered over two sites, with occupancy factors of 0.75 and 0.25. The disordered methyl C atoms were refined isotropically. The tetrafluoroborate was restrained to a ideal tetrahedron, with isotropic refinements. ; _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^)+(0.1393P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(6) _refine_ls_number_reflns 8397 _refine_ls_number_parameters 502 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.2215 _refine_ls_wR_factor_gt 0.2089 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.086 _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 0.5000 -0.22357(5) 0.7500 0.0554(3) Uani 1 2 d S . . Ag2 Ag 1.0000 0.77744(6) 0.7500 0.0744(3) Uani 1 2 d S . . N1 N 0.4221(8) -0.2818(4) 0.79801(11) 0.0430(13) Uani 1 1 d . . . N2 N 0.5636(7) -0.1080(4) 0.79016(12) 0.0395(13) Uani 1 1 d . . . N3 N 0.8784(8) 0.6787(4) 0.78843(15) 0.0527(16) Uani 1 1 d . . . N4 N 1.0293(7) 0.8473(4) 0.79948(17) 0.0596(17) Uani 1 1 d . . . O1 O 0.5638(6) 0.2173(3) 0.84243(11) 0.0474(11) Uani 1 1 d . B . O3 O 0.8295(5) 0.3581(3) 0.84473(10) 0.0407(10) Uani 1 1 d . . . O4 O 1.0960(7) 0.3914(4) 0.85733(14) 0.0663(15) Uani 1 1 d D . . C1 C 0.3447(10) -0.3692(4) 0.80090(16) 0.0481(18) Uani 1 1 d . . . H1 H 0.3437 -0.4109 0.7833 0.058 Uiso 1 1 calc R . . C2 C 0.2706(11) -0.3969(5) 0.82803(17) 0.055(2) Uani 1 1 d . . . H2 H 0.2124 -0.4546 0.8285 0.066 Uiso 1 1 calc R . . C3 C 0.2798(7) -0.3414(4) 0.85468(15) 0.0402(15) Uani 1 1 d . . . H3 H 0.2358 -0.3626 0.8740 0.048 Uiso 1 1 calc R . . C4 C 0.3562(8) -0.2521(4) 0.85263(15) 0.0402(15) Uani 1 1 d . . . H4 H 0.3577 -0.2108 0.8703 0.048 Uiso 1 1 calc R . . C5 C 0.4292(7) -0.2253(4) 0.82461(13) 0.0294(12) Uani 1 1 d . . . C6 C 0.5155(8) -0.1300(4) 0.82059(12) 0.0320(12) Uani 1 1 d . . . C7 C 0.5440(8) -0.0711(4) 0.84680(14) 0.0355(14) Uani 1 1 d . . . H7 H 0.5094 -0.0895 0.8672 0.043 Uiso 1 1 calc R . . C8 C 0.6252(8) 0.0164(4) 0.84231(15) 0.0381(15) Uani 1 1 d . . . C9 C 0.6717(9) 0.0406(5) 0.81117(15) 0.0440(16) Uani 1 1 d . . . H9 H 0.7232 0.0992 0.8070 0.053 Uiso 1 1 calc R . . C10 C 0.6409(10) -0.0224(5) 0.78713(16) 0.0503(18) Uani 1 1 d . . . H10 H 0.6762 -0.0053 0.7666 0.060 Uiso 1 1 calc R . . C11 C 0.6673(7) 0.0780(4) 0.87053(13) 0.0329(13) Uani 1 1 d . . . C12 C 0.7361(9) 0.0401(4) 0.89650(14) 0.0389(14) Uani 1 1 d . . . H12 H 0.7464 -0.0268 0.8978 0.047 Uiso 1 1 calc R . . C13 C 0.7952(8) 0.0977(4) 0.92263(14) 0.0409(16) Uani 1 1 d . . . C14 C 0.8809(10) 0.0541(6) 0.94961(15) 0.0552(19) Uani 1 1 d . . . H14 H 0.8932 -0.0127 0.9513 0.066 Uiso 1 1 calc R . . C15 C 0.9405(9) 0.1131(5) 0.97159(16) 0.0534(19) Uani 1 1 d . . . H15 H 0.9886 0.0857 0.9897 0.064 Uiso 1 1 calc R . . C16 C 0.9360(9) 0.2133(5) 0.96950(15) 0.0488(17) Uani 1 1 d . . . H16 H 0.9893 0.2516 0.9846 0.059 Uiso 1 1 calc R . . C17 C 0.8513(8) 0.2541(5) 0.94472(14) 0.0393(14) Uani 1 1 d . . . H17 H 0.8400 0.3210 0.9440 0.047 Uiso 1 1 calc R . . C18 C 0.7808(7) 0.1981(4) 0.92035(13) 0.0324(13) Uani 1 1 d . . . C19 C 0.6898(7) 0.2391(4) 0.89334(14) 0.0328(13) Uani 1 1 d . . . C20 C 0.6392(7) 0.1793(4) 0.86960(13) 0.0308(13) Uani 1 1 d . . . C23 C 0.6644(8) 0.3472(5) 0.89229(13) 0.0362(14) Uani 1 1 d . . . C24 C 0.5585(8) 0.3919(5) 0.91519(14) 0.0417(16) Uani 1 1 d . . . C25 C 0.4769(9) 0.3408(6) 0.93903(14) 0.0517(17) Uani 1 1 d . . . H25 H 0.4914 0.2742 0.9409 0.062 Uiso 1 1 calc R . . C26 C 0.3744(10) 0.3885(9) 0.95987(17) 0.076(3) Uani 1 1 d . . . H26 H 0.3214 0.3541 0.9760 0.091 Uiso 1 1 calc R . . C27 C 0.3495(11) 0.4870(7) 0.95714(18) 0.063(2) Uani 1 1 d . . . H27 H 0.2768 0.5172 0.9710 0.076 Uiso 1 1 calc R . . C28 C 0.4268(10) 0.5398(6) 0.93511(18) 0.062(2) Uani 1 1 d . . . H28 H 0.4108 0.6063 0.9340 0.075 Uiso 1 1 calc R . . C29 C 0.5359(8) 0.4919(5) 0.91297(15) 0.0464(17) Uani 1 1 d . . . C30 C 0.6075(9) 0.5439(5) 0.88793(16) 0.0476(17) Uani 1 1 d . . . H30 H 0.5888 0.6102 0.8867 0.057 Uiso 1 1 calc R . . C31 C 0.7034(8) 0.5019(4) 0.86523(15) 0.0402(16) Uani 1 1 d . . . C32 C 0.7328(8) 0.4004(4) 0.86840(14) 0.0339(13) Uani 1 1 d . . . C33 C 0.9779(9) 0.3202(5) 0.85334(19) 0.0542(18) Uani 1 1 d . . . H33A H 1.0135 0.2751 0.8369 0.065 Uiso 1 1 calc R . . H33B H 0.9661 0.2845 0.8733 0.065 Uiso 1 1 calc R . . C34 C 1.1088(11) 0.4304(8) 0.8879(2) 0.082(3) Uani 1 1 d D . . H34A H 1.0052 0.4557 0.8944 0.122 Uiso 1 1 calc R . . H34B H 1.1880 0.4815 0.8878 0.122 Uiso 1 1 calc R . . H34C H 1.1423 0.3809 0.9027 0.122 Uiso 1 1 calc R . . C35 C 0.8184(11) 0.5881(5) 0.78311(18) 0.061(2) Uani 1 1 d . . . H35 H 0.8106 0.5666 0.7620 0.073 Uiso 1 1 calc R . . C36 C 0.7699(11) 0.5279(5) 0.80668(17) 0.059(2) Uani 1 1 d . . . H36 H 0.7356 0.4655 0.8017 0.070 Uiso 1 1 calc R . . C37 C 0.7711(8) 0.5595(4) 0.83855(15) 0.0383(14) Uani 1 1 d . . . C38 C 0.8356(8) 0.6516(4) 0.84440(17) 0.0405(15) Uani 1 1 d . . . H38 H 0.8430 0.6751 0.8653 0.049 Uiso 1 1 calc R . . C39 C 0.8881(9) 0.7071(4) 0.81886(19) 0.0484(18) Uani 1 1 d . . . C40 C 0.9635(8) 0.8046(4) 0.82492(18) 0.0427(16) Uani 1 1 d . . . C41 C 0.9690(10) 0.8467(4) 0.8549(2) 0.058(2) Uani 1 1 d . . . H41 H 0.9207 0.8153 0.8722 0.070 Uiso 1 1 calc R . . C42 C 1.0463(9) 0.9361(6) 0.8599(3) 0.080(3) Uani 1 1 d . . . H42 H 1.0521 0.9645 0.8801 0.096 Uiso 1 1 calc R . . C43 C 1.1160(10) 0.9814(6) 0.8318(2) 0.066(2) Uani 1 1 d . . . H43 H 1.1672 1.0413 0.8331 0.080 Uiso 1 1 calc R . . C44 C 1.1044(10) 0.9339(5) 0.8036(3) 0.072(3) Uani 1 1 d . . . H44 H 1.1513 0.9626 0.7856 0.086 Uiso 1 1 calc R . . B1 B 0.1371(14) 0.7626(8) 0.9409(2) 0.146(7) Uiso 1 1 d D . . F1 F 0.0620(12) 0.6934(6) 0.9225(2) 0.192(4) Uiso 1 1 d D . . F2 F 0.0267(11) 0.8347(6) 0.9472(2) 0.184(4) Uiso 1 1 d D . . F3 F 0.2689(11) 0.7965(7) 0.9251(2) 0.191(4) Uiso 1 1 d D . . F4 F 0.1845(11) 0.7236(6) 0.96963(18) 0.165(3) Uiso 1 1 d D . . C21 C 0.4021(10) 0.2492(5) 0.8462(2) 0.069(3) Uani 1 1 d D . . H21A H 0.3739 0.2537 0.8688 0.083 Uiso 0.75 1 calc PR A 1 H21B H 0.3875 0.3123 0.8363 0.083 Uiso 0.75 1 calc PR A 1 H21C H 0.3683 0.2781 0.8268 0.083 Uiso 0.25 1 d PR A 2 H21D H 0.4037 0.2999 0.8629 0.083 Uiso 0.25 1 d PR A 2 O2 O 0.3075(11) 0.1814(6) 0.8311(2) 0.089(3) Uani 0.75 1 d PD B 1 C22 C 0.322(2) 0.1814(13) 0.7978(2) 0.128(6) Uiso 0.75 1 d PD B 1 H22A H 0.2643 0.2421 0.7907 0.154 Uiso 0.75 1 d P C 1 H22B H 0.2507 0.1290 0.7893 0.154 Uiso 0.75 1 d P D 1 H22C H 0.4223 0.1785 0.7905 0.154 Uiso 0.75 1 d P E 1 O2' O 0.285(3) 0.1818(17) 0.8569(5) 0.089(3) Uani 0.25 1 d PD B 2 C22' C 0.280(5) 0.174(3) 0.8901(6) 0.099(13) Uiso 0.25 1 d PD B 2 H22D H 0.3259 0.1216 0.8978 0.118 Uiso 0.25 1 d P F 2 H22E H 0.1736 0.1897 0.8959 0.118 Uiso 0.25 1 d P G 2 H22F H 0.3491 0.2342 0.8973 0.118 Uiso 0.25 1 d P H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0886(6) 0.0443(4) 0.0334(3) 0.000 -0.0036(4) 0.000 Ag2 0.0960(8) 0.0477(5) 0.0796(5) 0.000 -0.0069(6) 0.000 N1 0.068(4) 0.033(3) 0.028(2) -0.004(2) -0.007(2) -0.014(3) N2 0.041(3) 0.028(3) 0.050(3) -0.006(2) 0.001(2) -0.008(2) N3 0.056(4) 0.030(3) 0.071(4) 0.007(3) -0.038(3) 0.000(3) N4 0.041(4) 0.043(3) 0.095(5) -0.017(3) 0.009(3) -0.002(3) O1 0.056(3) 0.032(2) 0.055(2) -0.003(2) -0.019(2) 0.004(2) O3 0.042(3) 0.030(2) 0.049(2) -0.0057(18) 0.006(2) 0.010(2) O4 0.046(3) 0.074(4) 0.079(4) 0.013(3) 0.001(3) -0.013(3) C1 0.074(5) 0.026(3) 0.045(4) -0.008(3) -0.020(3) -0.015(3) C2 0.062(5) 0.043(4) 0.060(4) 0.014(3) -0.034(4) -0.011(4) C3 0.030(4) 0.036(3) 0.054(4) 0.002(3) 0.006(3) -0.001(3) C4 0.045(4) 0.030(3) 0.045(3) -0.005(3) 0.002(3) 0.003(3) C5 0.026(3) 0.028(3) 0.035(3) -0.003(2) -0.007(2) 0.001(3) C6 0.030(3) 0.033(3) 0.032(2) -0.005(2) -0.003(3) 0.000(3) C7 0.044(4) 0.019(3) 0.044(3) 0.004(2) -0.003(3) -0.005(3) C8 0.046(4) 0.022(3) 0.047(3) -0.002(3) -0.010(3) 0.011(3) C9 0.052(4) 0.033(3) 0.047(4) -0.001(3) 0.005(3) -0.003(3) C10 0.071(5) 0.027(3) 0.052(4) 0.001(3) 0.022(4) -0.005(3) C11 0.037(3) 0.024(3) 0.037(3) -0.001(2) -0.003(3) -0.005(3) C12 0.047(4) 0.024(3) 0.046(3) -0.002(2) -0.006(3) -0.010(3) C13 0.063(5) 0.025(3) 0.035(3) 0.007(2) -0.007(3) 0.000(3) C14 0.077(6) 0.047(4) 0.041(4) 0.009(3) -0.008(4) -0.003(4) C15 0.062(5) 0.050(4) 0.048(4) 0.009(3) -0.019(3) -0.002(4) C16 0.046(4) 0.056(4) 0.044(3) -0.014(3) -0.011(3) 0.005(3) C17 0.046(4) 0.033(3) 0.039(3) -0.001(2) 0.001(3) -0.001(3) C18 0.031(4) 0.028(3) 0.038(3) 0.001(2) -0.005(2) 0.002(2) C19 0.029(3) 0.023(3) 0.046(3) 0.004(2) -0.003(2) 0.002(2) C20 0.029(3) 0.027(3) 0.036(3) 0.007(2) -0.005(2) 0.003(3) C23 0.034(3) 0.039(4) 0.036(3) -0.012(3) -0.010(3) 0.000(3) C24 0.035(4) 0.050(4) 0.040(3) -0.013(3) -0.012(3) 0.010(3) C25 0.048(4) 0.065(4) 0.042(3) -0.002(3) 0.001(3) 0.018(4) C26 0.046(5) 0.139(9) 0.042(4) -0.007(5) 0.006(3) 0.020(5) C27 0.063(5) 0.082(6) 0.045(4) -0.016(4) -0.006(4) 0.034(5) C28 0.070(5) 0.060(5) 0.056(4) -0.023(4) -0.023(4) 0.033(4) C29 0.046(4) 0.048(4) 0.046(3) -0.023(3) -0.018(3) 0.010(3) C30 0.054(4) 0.038(4) 0.051(4) -0.017(3) -0.022(3) 0.011(3) C31 0.048(4) 0.028(3) 0.045(3) -0.011(3) -0.017(3) 0.006(3) C32 0.027(3) 0.027(3) 0.048(3) -0.001(2) -0.010(3) 0.001(3) C33 0.039(4) 0.032(3) 0.092(5) -0.008(3) 0.015(4) 0.005(3) C34 0.051(5) 0.100(7) 0.093(7) 0.025(6) -0.019(5) -0.019(5) C35 0.087(6) 0.041(4) 0.056(4) -0.001(3) -0.030(4) -0.021(4) C36 0.082(6) 0.030(3) 0.064(4) -0.005(3) -0.047(4) -0.004(4) C37 0.037(4) 0.025(3) 0.053(3) 0.002(3) -0.013(3) -0.002(3) C38 0.033(3) 0.016(3) 0.072(4) -0.002(3) -0.017(3) 0.002(3) C39 0.048(4) 0.015(3) 0.082(5) -0.005(3) -0.019(4) -0.001(3) C40 0.034(4) 0.018(3) 0.076(4) -0.002(3) -0.013(3) 0.002(3) C41 0.059(5) 0.024(3) 0.093(5) -0.002(3) -0.026(4) 0.001(3) C42 0.034(5) 0.045(4) 0.162(9) -0.034(5) -0.012(5) 0.004(4) C43 0.044(5) 0.037(4) 0.117(7) -0.017(5) 0.005(5) -0.008(4) C44 0.052(5) 0.034(4) 0.128(8) -0.019(5) 0.015(5) -0.016(4) C21 0.050(5) 0.050(5) 0.106(6) 0.004(4) -0.045(5) 0.003(4) O2 0.088(6) 0.089(5) 0.089(6) 0.012(6) -0.001(5) -0.001(5) O2' 0.088(6) 0.089(5) 0.089(6) 0.012(6) -0.001(5) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.244(5) . ? Ag1 N1 2.244(5) 3_656 ? Ag1 N2 2.368(5) . ? Ag1 N2 2.368(5) 3_656 ? Ag2 N4 2.284(7) 3_756 ? Ag2 N4 2.284(7) . ? Ag2 N3 2.326(6) 3_756 ? Ag2 N3 2.326(6) . ? N1 C5 1.355(7) . ? N1 C1 1.371(8) . ? N2 C10 1.349(9) . ? N2 C6 1.359(8) . ? N3 C39 1.327(9) . ? N3 C35 1.363(9) . ? N4 C40 1.326(9) . ? N4 C44 1.357(9) . ? O1 C20 1.391(7) . ? O1 C21 1.408(10) . ? O3 C33 1.374(8) . ? O3 C32 1.394(7) . ? O4 C34 1.383(8) . ? O4 C33 1.391(9) . ? C1 C2 1.337(10) . ? C1 H1 0.9300 . ? C2 C3 1.349(9) . ? C2 H2 0.9300 . ? C3 C4 1.387(9) . ? C3 H3 0.9300 . ? C4 C5 1.361(9) . ? C4 H4 0.9300 . ? C5 C6 1.505(8) . ? C6 C7 1.380(8) . ? C7 C8 1.392(9) . ? C7 H7 0.9300 . ? C8 C9 1.391(9) . ? C8 C11 1.490(8) . ? C9 C10 1.350(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.326(8) . ? C11 C20 1.419(8) . ? C12 C13 1.431(8) . ? C12 H12 0.9300 . ? C13 C18 1.395(8) . ? C13 C14 1.455(9) . ? C14 C15 1.318(10) . ? C14 H14 0.9300 . ? C15 C16 1.388(10) . ? C15 H15 0.9300 . ? C16 C17 1.365(9) . ? C16 H16 0.9300 . ? C17 C18 1.400(8) . ? C17 H17 0.9300 . ? C18 C19 1.463(8) . ? C19 C20 1.352(8) . ? C19 C23 1.509(9) . ? C23 C32 1.357(9) . ? C23 C24 1.430(9) . ? C24 C25 1.389(10) . ? C24 C29 1.398(9) . ? C25 C26 1.376(10) . ? C25 H25 0.9300 . ? C26 C27 1.380(13) . ? C26 H26 0.9300 . ? C27 C28 1.332(12) . ? C27 H27 0.9300 . ? C28 C29 1.445(10) . ? C28 H28 0.9300 . ? C29 C30 1.395(10) . ? C30 C31 1.359(9) . ? C30 H30 0.9300 . ? C31 C32 1.429(8) . ? C31 C37 1.474(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.345(10) . ? C35 H35 0.9300 . ? C36 C37 1.395(9) . ? C36 H36 0.9300 . ? C37 C38 1.400(8) . ? C38 C39 1.379(10) . ? C38 H38 0.9300 . ? C39 C40 1.503(9) . ? C40 C41 1.375(10) . ? C41 C42 1.404(10) . ? C41 H41 0.9300 . ? C42 C43 1.444(14) . ? C42 H42 0.9300 . ? C43 C44 1.345(12) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? B1 F4 1.368(9) . ? B1 F3 1.349(9) . ? B1 F2 1.373(9) . ? B1 F1 1.369(9) . ? C21 O2 1.369(8) . ? C21 O2' 1.411(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9415 . ? C21 H21D 0.9875 . ? O2 C22 1.387(8) . ? O2 H21C 1.4377 . ? C22 H22A 1.0086 . ? C22 H22B 0.9949 . ? C22 H22C 0.8808 . ? O2' C22' 1.384(10) . ? C22' H22D 0.8821 . ? C22' H22E 0.9325 . ? C22' H22F 1.0440 . ? 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 138.0(3) . 3_656 ? N1 Ag1 N2 71.19(17) . . ? N1 Ag1 N2 143.6(2) 3_656 . ? N1 Ag1 N2 143.6(2) . 3_656 ? N1 Ag1 N2 71.19(17) 3_656 3_656 ? N2 Ag1 N2 95.2(3) . 3_656 ? N4 Ag2 N4 130.0(3) 3_756 . ? N4 Ag2 N3 71.0(2) 3_756 3_756 ? N4 Ag2 N3 145.2(2) . 3_756 ? N4 Ag2 N3 145.2(2) 3_756 . ? N4 Ag2 N3 71.0(2) . . ? N3 Ag2 N3 108.2(3) 3_756 . ? C5 N1 C1 117.1(5) . . ? C5 N1 Ag1 120.5(4) . . ? C1 N1 Ag1 121.7(4) . . ? C10 N2 C6 114.8(5) . . ? C10 N2 Ag1 129.0(4) . . ? C6 N2 Ag1 116.2(4) . . ? C39 N3 C35 116.6(6) . . ? C39 N3 Ag2 117.0(5) . . ? C35 N3 Ag2 125.6(5) . . ? C40 N4 C44 118.5(7) . . ? C40 N4 Ag2 119.1(4) . . ? C44 N4 Ag2 122.3(6) . . ? C20 O1 C21 116.7(6) . . ? C33 O3 C32 118.8(5) . . ? C34 O4 C33 116.0(6) . . ? C2 C1 N1 122.5(6) . . ? C2 C1 H1 118.8 . . ? N1 C1 H1 118.8 . . ? C3 C2 C1 120.3(7) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 118.7(6) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.6(6) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 121.5(6) . . ? N1 C5 C6 115.7(5) . . ? C4 C5 C6 122.8(5) . . ? N2 C6 C7 123.7(5) . . ? N2 C6 C5 115.8(5) . . ? C7 C6 C5 120.5(5) . . ? C6 C7 C8 119.1(6) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C9 C8 C7 117.7(6) . . ? C9 C8 C11 122.0(6) . . ? C7 C8 C11 120.1(6) . . ? C10 C9 C8 118.8(6) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N2 C10 C9 125.8(6) . . ? N2 C10 H10 117.1 . . ? C9 C10 H10 117.1 . . ? C12 C11 C20 118.7(5) . . ? C12 C11 C8 120.9(5) . . ? C20 C11 C8 120.3(5) . . ? C11 C12 C13 122.9(5) . . ? C11 C12 H12 118.6 . . ? C13 C12 H12 118.6 . . ? C18 C13 C12 118.2(5) . . ? C18 C13 C14 120.4(6) . . ? C12 C13 C14 121.2(6) . . ? C15 C14 C13 117.2(7) . . ? C15 C14 H14 121.4 . . ? C13 C14 H14 121.4 . . ? C14 C15 C16 124.3(7) . . ? C14 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C17 C16 C15 118.2(6) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C16 C17 C18 121.9(6) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C13 C18 C17 117.7(5) . . ? C13 C18 C19 118.7(5) . . ? C17 C18 C19 123.6(5) . . ? C20 C19 C18 118.8(5) . . ? C20 C19 C23 122.7(5) . . ? C18 C19 C23 118.4(5) . . ? C19 C20 O1 119.9(5) . . ? C19 C20 C11 122.2(5) . . ? O1 C20 C11 117.8(5) . . ? C32 C23 C24 120.3(6) . . ? C32 C23 C19 120.0(5) . . ? C24 C23 C19 119.5(6) . . ? C25 C24 C29 119.0(6) . . ? C25 C24 C23 123.3(6) . . ? C29 C24 C23 117.6(6) . . ? C26 C25 C24 120.0(8) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 120.8(8) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 121.7(7) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 118.9(7) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C30 C29 C24 120.2(6) . . ? C30 C29 C28 120.1(7) . . ? C24 C29 C28 119.5(7) . . ? C31 C30 C29 122.9(6) . . ? C31 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? C30 C31 C32 116.9(6) . . ? C30 C31 C37 120.7(6) . . ? C32 C31 C37 122.4(6) . . ? C23 C32 O3 121.7(5) . . ? C23 C32 C31 122.0(6) . . ? O3 C32 C31 116.3(5) . . ? O3 C33 O4 112.3(5) . . ? O3 C33 H33A 109.1 . . ? O4 C33 H33A 109.1 . . ? O3 C33 H33B 109.1 . . ? O4 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? O4 C34 H34A 109.5 . . ? O4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N3 123.8(7) . . ? C36 C35 H35 118.1 . . ? N3 C35 H35 118.1 . . ? C35 C36 C37 119.7(6) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 116.9(6) . . ? C38 C37 C31 120.2(6) . . ? C36 C37 C31 122.9(6) . . ? C39 C38 C37 119.4(6) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? N3 C39 C38 123.4(6) . . ? N3 C39 C40 116.8(7) . . ? C38 C39 C40 119.9(6) . . ? N4 C40 C41 121.4(6) . . ? N4 C40 C39 115.6(6) . . ? C41 C40 C39 123.0(7) . . ? C40 C41 C42 121.4(9) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C41 C42 C43 116.2(9) . . ? C41 C42 H42 121.9 . . ? C43 C42 H42 121.9 . . ? C44 C43 C42 117.7(8) . . ? C44 C43 H43 121.2 . . ? C42 C43 H43 121.2 . . ? C43 C44 N4 124.9(9) . . ? C43 C44 H44 117.5 . . ? N4 C44 H44 117.5 . . ? F4 B1 F3 109.4(8) . . ? F4 B1 F2 107.8(8) . . ? F3 B1 F2 111.8(8) . . ? F4 B1 F1 109.9(8) . . ? F3 B1 F1 109.5(8) . . ? F2 B1 F1 108.4(8) . . ? O2 C21 O1 105.7(7) . . ? O2 C21 O2' 46.0(10) . . ? O1 C21 O2' 118.1(13) . . ? O2 C21 H21A 110.6 . . ? O1 C21 H21A 110.6 . . ? O2' C21 H21A 64.8 . . ? O2 C21 H21B 110.6 . . ? O1 C21 H21B 110.6 . . ? O2' C21 H21B 129.9 . . ? H21A C21 H21B 108.7 . . ? O2 C21 H21C 74.4 . . ? O1 C21 H21C 108.5 . . ? O2' C21 H21C 110.4 . . ? H21A C21 H21C 137.1 . . ? H21B C21 H21C 38.9 . . ? O2 C21 H21D 144.6 . . ? O1 C21 H21D 106.7 . . ? O2' C21 H21D 104.8 . . ? H21A C21 H21D 43.5 . . ? H21B C21 H21D 70.2 . . ? H21C C21 H21D 107.9 . . ? C21 O2 C22 114.1(8) . . ? C21 O2 H21C 39.1 . . ? C22 O2 H21C 81.2 . . ? O2 C22 H22A 104.7 . . ? O2 C22 H22B 107.9 . . ? H22A C22 H22B 103.0 . . ? O2 C22 H22C 115.0 . . ? H22A C22 H22C 112.0 . . ? H22B C22 H22C 113.3 . . ? C22' O2' C21 112.4(11) . . ? O2' C22' H22D 114.3 . . ? O2' C22' H22E 105.5 . . ? H22D C22' H22E 119.5 . . ? O2' C22' H22F 102.3 . . ? H22D C22' H22F 108.7 . . ? H22E C22' H22F 104.8 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.224 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.099 _vrf_PLAT772_(R)-1AgBF4 ; PROBLEM: Suspect O-H Bond in CIF: O2 -- H21C .. 1.44 Ang. RESPONSE: O2 and H21C belong to two CH3OCH2 chains with occupancy factors of 0.75 and 0.25, respectively. They can't exist at the same time. ;