# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Yong Cui' _publ_contact_author_email YONGCUI@SJTU.EDU.CN _publ_section_title ; Multiple Topological Isomerism of Three-Connected Networks In Silver-Based Metal-Organoboron Frameworks ; # Attachment 'CIF-1.txt' _publ_section_exptl_refinement ; All aromatic groups were input as idealized planar rings with C-C bond lengths of 1.39 angstrom. Some C-C bonds from the aromatic rings to the methyl groups are somewhat short and so were constrained to be ca. 1.50 angstrom. The N-O bond lengths of the nitrate anion were constrained to be reasonably. All hydrogen atoms except the H atoms of solvents were generated geometrically (C-H = 0.93 or 0.96\%A for phenyl or methyl H atoms respectively) and were included in the refinement in the riding model approximation. The displacement parameters of methyl H atoms were set to 1.5 times U~eq~ of the equivalent isotropic displacement parameters of their parent atoms, while those of other H atoms were set to 1.2 times. All non-H atoms except for the disordered ones were refined anisotropically. ; _publ_contact_author 'Yong Cui' _publ_contact_author_fax +86-21-54741297 _publ_contact_author_phone +86-21-54747687 loop_ _publ_author_name 'Yong Cui' 'Qizhuang He' 'Yan Liu' 'Qingchun Xia' 'Xin Xu' 'Guozan Yuan' #====================================================================== data_1_[AgL(NO3)].2H2O _database_code_depnum_ccdc_archive 'CCDC 747394' #TrackingRef 'CIF-1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H52 Ag B N4 O5' _chemical_formula_weight 847.59 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 22.3511(4) _cell_length_b 22.3511(4) _cell_length_c 25.3776(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12677.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 11116 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 0.351 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99180 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max ? _reflns_number_total ? _reflns_number_gt 9873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.1272P)^2^+0.1467P] 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 -0.01(3) _refine_ls_number_reflns 11116 _refine_ls_number_parameters 483 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1565 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.171 _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 -0.133402(16) -0.241981(14) 0.081593(16) 0.07774(15) Uani 1 1 d . . . B1 B -0.27422(18) 0.0678(2) 0.39245(18) 0.0567(9) Uani 1 1 d . . . N1 N -0.16200(17) -0.17246(16) 0.14172(16) 0.0745(10) Uani 1 1 d D . . C1 C -0.2093(2) -0.13769(18) 0.13417(18) 0.0694(10) Uani 1 1 d D . . H1A H -0.2290 -0.1399 0.1019 0.083 Uiso 1 1 calc R . . C2 C -0.2309(2) -0.09859(18) 0.17141(18) 0.0711(10) Uani 1 1 d D . . H2A H -0.2643 -0.0752 0.1643 0.085 Uiso 1 1 calc R . . C3 C -0.20215(19) -0.09446(19) 0.22005(17) 0.0692(10) Uani 1 1 d D . . C4 C -0.1541(3) -0.1312(3) 0.2275(3) 0.109(2) Uani 1 1 d D . . H4A H -0.1341 -0.1307 0.2596 0.130 Uiso 1 1 calc R . . C5 C -0.1352(3) -0.1684(3) 0.1888(3) 0.107(2) Uani 1 1 d D . . H5A H -0.1020 -0.1924 0.1952 0.129 Uiso 1 1 calc R . . C6 C -0.22365(18) -0.05233(18) 0.26168(17) 0.0656(9) Uani 1 1 d D . . C7 C -0.26557(19) -0.07206(18) 0.29922(17) 0.0659(9) Uani 1 1 d D . . C8 C -0.28307(17) -0.03309(18) 0.34005(16) 0.0627(9) Uani 1 1 d D . . C9 C -0.25683(16) 0.02379(17) 0.34481(15) 0.0592(8) Uani 1 1 d D . . C10 C -0.21437(17) 0.04252(17) 0.30733(17) 0.0637(9) Uani 1 1 d D . . C11 C -0.19925(19) 0.00516(18) 0.26507(18) 0.0688(10) Uani 1 1 d D . . C12 C -0.1559(3) 0.0244(2) 0.2214(2) 0.0991(18) Uani 1 1 d D . . H12A H -0.1425 0.0646 0.2279 0.149 Uiso 1 1 calc R . . H12B H -0.1759 0.0228 0.1879 0.149 Uiso 1 1 calc R . . H12C H -0.1220 -0.0020 0.2209 0.149 Uiso 1 1 calc R . . C13 C -0.1860(2) 0.1041(2) 0.3095(2) 0.0851(14) Uani 1 1 d D . . H13A H -0.1585 0.1085 0.2807 0.128 Uiso 1 1 calc R . . H13B H -0.1650 0.1088 0.3422 0.128 Uiso 1 1 calc R . . H13C H -0.2166 0.1341 0.3068 0.128 Uiso 1 1 calc R . . C14 C -0.3287(2) -0.0557(2) 0.3796(2) 0.0811(13) Uani 1 1 d . . . H14A H -0.3417 -0.0950 0.3697 0.122 Uiso 1 1 calc R . . H14B H -0.3625 -0.0291 0.3803 0.122 Uiso 1 1 calc R . . H14C H -0.3108 -0.0572 0.4140 0.122 Uiso 1 1 calc R . . C15 C -0.2904(3) -0.1343(2) 0.2955(2) 0.0883(14) Uani 1 1 d . . . H15A H -0.2737 -0.1541 0.2654 0.132 Uiso 1 1 calc R . . H15B H -0.3331 -0.1324 0.2920 0.132 Uiso 1 1 calc R . . H15C H -0.2803 -0.1561 0.3269 0.132 Uiso 1 1 calc R . . C16 C 0.0463(2) 0.1781(3) 0.4935(2) 0.0968(16) Uani 1 1 d D . . H16A H 0.0820 0.1742 0.4750 0.116 Uiso 1 1 calc R . . C17 C -0.0059(2) 0.1570(3) 0.4707(2) 0.0962(16) Uani 1 1 d D . . H17A H -0.0052 0.1413 0.4368 0.115 Uiso 1 1 calc R . . C18 C -0.05848(19) 0.1593(2) 0.49829(19) 0.0756(11) Uani 1 1 d D . . C19 C -0.0576(2) 0.1864(3) 0.5470(3) 0.1046(19) Uani 1 1 d D . . H19A H -0.0929 0.1903 0.5662 0.126 Uiso 1 1 calc R . . C20 C -0.0038(3) 0.2081(4) 0.5676(3) 0.115(2) Uani 1 1 d D . . H20A H -0.0039 0.2258 0.6007 0.138 Uiso 1 1 calc R . . N2 N 0.04738(18) 0.2041(2) 0.54133(18) 0.0872(12) Uani 1 1 d D . . C21 C -0.11631(18) 0.1360(2) 0.47548(18) 0.0724(10) Uani 1 1 d D . . C22 C -0.15897(19) 0.17582(19) 0.45777(19) 0.0688(10) Uani 1 1 d D . . C23 C -0.21278(17) 0.15456(18) 0.43587(16) 0.0625(9) Uani 1 1 d D . . C24 C -0.22156(15) 0.09246(16) 0.42832(15) 0.0582(8) Uani 1 1 d D . . C25 C -0.17767(17) 0.05217(18) 0.44853(19) 0.0670(10) Uani 1 1 d D . . C26 C -0.12551(19) 0.0740(2) 0.4724(2) 0.0759(11) Uani 1 1 d D . . C27 C -0.0788(3) 0.0315(3) 0.4956(3) 0.111(2) Uani 1 1 d D . . H27A H -0.0915 -0.0091 0.4903 0.166 Uiso 1 1 calc R . . H27B H -0.0746 0.0391 0.5326 0.166 Uiso 1 1 calc R . . H27C H -0.0411 0.0378 0.4784 0.166 Uiso 1 1 calc R . . C28 C -0.1894(3) -0.0147(2) 0.4469(3) 0.0948(16) Uani 1 1 d D . . H28A H -0.1559 -0.0356 0.4619 0.142 Uiso 1 1 calc R . . H28B H -0.1949 -0.0271 0.4110 0.142 Uiso 1 1 calc R . . H28C H -0.2248 -0.0236 0.4668 0.142 Uiso 1 1 calc R . . C29 C -0.25827(19) 0.19891(19) 0.4172(2) 0.0734(10) Uani 1 1 d . . . H29A H -0.2450 0.2387 0.4256 0.110 Uiso 1 1 calc R . . H29B H -0.2958 0.1913 0.4343 0.110 Uiso 1 1 calc R . . H29C H -0.2631 0.1952 0.3797 0.110 Uiso 1 1 calc R . . C30 C -0.1488(3) 0.2431(2) 0.4610(3) 0.0939(15) Uani 1 1 d . . . H30A H -0.1104 0.2508 0.4765 0.141 Uiso 1 1 calc R . . H30B H -0.1795 0.2609 0.4822 0.141 Uiso 1 1 calc R . . H30C H -0.1500 0.2599 0.4262 0.141 Uiso 1 1 calc R . . C31 C -0.62011(17) 0.1719(2) 0.4217(2) 0.0708(10) Uani 1 1 d D . . H31A H -0.6366 0.2089 0.4301 0.085 Uiso 1 1 calc R . . C32 C -0.55950(17) 0.16684(19) 0.42176(19) 0.0686(10) Uani 1 1 d D . . H32A H -0.5360 0.1996 0.4308 0.082 Uiso 1 1 calc R . . C33 C -0.53252(17) 0.1130(2) 0.40841(18) 0.0696(10) Uani 1 1 d D . . C34 C -0.5712(2) 0.0664(3) 0.3965(4) 0.115(2) Uani 1 1 d D . . H34A H -0.5560 0.0292 0.3872 0.138 Uiso 1 1 calc R . . C35 C -0.6315(2) 0.0752(3) 0.3982(4) 0.120(3) Uani 1 1 d D . . H35A H -0.6562 0.0429 0.3906 0.144 Uiso 1 1 calc R . . N3 N -0.65728(15) 0.12739(19) 0.41030(16) 0.0769(10) Uani 1 1 d D . . C36 C -0.46645(17) 0.1052(2) 0.40600(17) 0.0661(9) Uani 1 1 d . . . C37 C -0.43655(17) 0.1194(2) 0.35956(16) 0.0650(9) Uani 1 1 d . . . C38 C -0.37428(18) 0.10959(19) 0.35629(16) 0.0618(8) Uani 1 1 d . . . C39 C -0.34281(16) 0.08518(18) 0.39916(15) 0.0584(9) Uani 1 1 d . . . C40 C -0.37346(18) 0.07333(18) 0.44628(16) 0.0628(9) Uani 1 1 d . . . C41 C -0.43567(18) 0.0833(2) 0.45032(17) 0.0650(9) Uani 1 1 d . . . C42 C -0.4687(2) 0.0704(3) 0.5013(2) 0.0905(15) Uani 1 1 d . . . H42A H -0.5104 0.0797 0.4970 0.136 Uiso 1 1 calc R . . H42B H -0.4523 0.0944 0.5291 0.136 Uiso 1 1 calc R . . H42C H -0.4644 0.0288 0.5100 0.136 Uiso 1 1 calc R . . C43 C -0.3418(2) 0.0469(3) 0.49295(18) 0.0778(12) Uani 1 1 d . . . H43A H -0.3001 0.0424 0.4850 0.117 Uiso 1 1 calc R . . H43B H -0.3587 0.0084 0.5009 0.117 Uiso 1 1 calc R . . H43C H -0.3465 0.0728 0.5228 0.117 Uiso 1 1 calc R . . C44 C -0.3422(2) 0.1275(2) 0.30670(18) 0.0750(11) Uani 1 1 d . . . H44A H -0.3004 0.1185 0.3101 0.112 Uiso 1 1 calc R . . H44B H -0.3472 0.1697 0.3010 0.112 Uiso 1 1 calc R . . H44C H -0.3585 0.1059 0.2774 0.112 Uiso 1 1 calc R . . C45 C -0.4703(2) 0.1450(3) 0.3125(2) 0.0883(14) Uani 1 1 d . . . H45A H -0.5120 0.1487 0.3211 0.133 Uiso 1 1 calc R . . H45B H -0.4658 0.1188 0.2828 0.133 Uiso 1 1 calc R . . H45C H -0.4544 0.1837 0.3039 0.133 Uiso 1 1 calc R . . N4 N -0.23634(16) 0.76366(16) 0.0000 0.0662(11) Uiso 1 2 d S . . O1 O -0.2414(2) 0.7316(2) 0.03850(19) 0.1160(13) Uiso 1 1 d . . . O2 O -0.1970(2) 0.8030(2) 0.0000 0.120(2) Uiso 1 2 d S . . N5 N -0.9862(15) 0.9736(13) 0.1488(12) 0.37(2) Uiso 0.50 1 d PD . . O3 O -1.0271(16) 0.9499(14) 0.1246(14) 0.361(19) Uiso 0.50 1 d PD . . O4 O -0.9975(15) 1.0169(15) 0.1773(13) 0.345(16) Uiso 0.50 1 d PD . . O5 O -0.9349(14) 0.9560(17) 0.1428(15) 0.39(2) Uiso 0.50 1 d PD . . O6 O -0.3763(11) 0.7455(15) 0.3782(11) 0.456(16) Uiso 1 1 d . . . O7 O -0.5427(14) 0.9014(13) 0.4711(14) 0.524(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0755(2) 0.04989(18) 0.1078(3) -0.01370(15) 0.02196(18) -0.00443(14) B1 0.045(2) 0.055(2) 0.071(2) -0.0045(18) 0.0007(17) -0.0003(16) N1 0.073(2) 0.0563(19) 0.094(3) -0.0247(17) 0.0128(19) -0.0022(17) C1 0.074(2) 0.059(2) 0.076(2) -0.0092(18) 0.0084(19) 0.000(2) C2 0.069(2) 0.054(2) 0.090(3) -0.0071(19) 0.008(2) 0.0059(17) C3 0.063(2) 0.058(2) 0.086(3) -0.0188(19) 0.013(2) -0.0058(18) C4 0.091(4) 0.119(5) 0.116(4) -0.048(4) -0.027(3) 0.035(3) C5 0.085(3) 0.109(4) 0.128(4) -0.048(4) -0.018(3) 0.038(3) C6 0.058(2) 0.057(2) 0.081(2) -0.0190(18) 0.0079(18) -0.0037(17) C7 0.063(2) 0.056(2) 0.079(2) -0.0115(18) 0.0034(18) -0.0101(18) C8 0.0511(18) 0.067(2) 0.070(2) -0.0098(18) 0.0054(16) -0.0094(16) C9 0.0460(17) 0.0568(19) 0.075(2) -0.0104(16) 0.0058(16) -0.0027(15) C10 0.0539(19) 0.0524(19) 0.085(3) -0.0114(17) 0.0154(18) -0.0075(16) C11 0.059(2) 0.062(2) 0.086(3) -0.017(2) 0.0208(19) -0.0084(18) C12 0.098(4) 0.079(3) 0.119(4) -0.028(3) 0.056(3) -0.029(3) C13 0.075(3) 0.065(2) 0.116(4) -0.024(2) 0.032(3) -0.020(2) C14 0.081(3) 0.073(3) 0.090(3) -0.016(2) 0.022(2) -0.024(2) C15 0.094(3) 0.072(3) 0.099(3) -0.017(3) 0.014(3) -0.025(3) C16 0.058(3) 0.124(5) 0.108(4) -0.006(3) -0.014(2) -0.015(3) C17 0.067(3) 0.119(4) 0.103(3) -0.027(3) -0.013(3) -0.012(3) C18 0.056(2) 0.078(3) 0.093(3) -0.002(2) -0.018(2) -0.0058(19) C19 0.067(3) 0.137(5) 0.110(4) -0.031(4) -0.003(3) -0.019(3) C20 0.079(4) 0.164(7) 0.103(4) -0.030(4) -0.014(3) -0.024(4) N2 0.064(2) 0.095(3) 0.102(3) 0.000(2) -0.027(2) -0.018(2) C21 0.056(2) 0.075(3) 0.086(3) -0.009(2) -0.0140(18) -0.005(2) C22 0.057(2) 0.060(2) 0.089(3) -0.0068(19) -0.0108(19) -0.0009(18) C23 0.0499(19) 0.061(2) 0.077(2) -0.0085(17) -0.0064(16) 0.0035(16) C24 0.0449(17) 0.0569(19) 0.073(2) -0.0085(16) -0.0057(15) 0.0060(15) C25 0.0494(19) 0.058(2) 0.094(3) -0.0005(19) -0.0100(18) 0.0072(17) C26 0.057(2) 0.068(2) 0.103(3) 0.003(2) -0.017(2) 0.010(2) C27 0.074(3) 0.089(4) 0.170(6) 0.015(4) -0.048(4) 0.010(3) C28 0.085(3) 0.057(2) 0.143(5) 0.002(3) -0.021(3) 0.007(2) C29 0.065(2) 0.060(2) 0.095(3) -0.011(2) -0.013(2) 0.0131(19) C30 0.085(3) 0.066(3) 0.131(4) -0.011(3) -0.025(3) -0.006(2) C31 0.0481(19) 0.071(2) 0.093(3) 0.001(2) 0.0029(19) 0.0006(18) C32 0.0482(19) 0.069(2) 0.089(3) -0.005(2) 0.0012(18) -0.0048(17) C33 0.0474(19) 0.079(3) 0.082(3) -0.005(2) -0.0014(17) -0.0039(18) C34 0.055(2) 0.079(3) 0.210(7) -0.044(4) -0.005(3) -0.004(2) C35 0.052(2) 0.097(4) 0.212(8) -0.040(4) -0.006(4) -0.011(3) N3 0.0448(16) 0.091(3) 0.095(2) 0.008(2) -0.0080(15) -0.0006(17) C36 0.0456(18) 0.075(2) 0.078(2) -0.0073(19) -0.0017(16) 0.0013(17) C37 0.0510(19) 0.079(3) 0.065(2) -0.0058(18) -0.0043(16) 0.0010(18) C38 0.0539(19) 0.070(2) 0.062(2) -0.0048(17) -0.0024(16) -0.0020(17) C39 0.0452(17) 0.067(2) 0.063(2) -0.0109(16) 0.0011(15) 0.0025(16) C40 0.052(2) 0.069(2) 0.067(2) -0.0054(17) -0.0002(16) 0.0029(18) C41 0.0485(19) 0.076(2) 0.071(2) -0.0047(18) 0.0068(17) -0.0009(18) C42 0.061(2) 0.126(4) 0.085(3) 0.013(3) 0.014(2) -0.002(3) C43 0.067(2) 0.095(3) 0.071(2) 0.008(2) -0.0026(19) 0.011(2) C44 0.066(2) 0.088(3) 0.071(2) 0.006(2) 0.0068(19) 0.001(2) C45 0.061(2) 0.120(4) 0.084(3) 0.007(3) -0.011(2) 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 N3 2.265(3) 8_545 ? Ag1 N1 2.270(3) . ? Ag1 N2 2.336(4) 2_554 ? B1 C24 1.587(5) . ? B1 C39 1.591(5) . ? B1 C9 1.606(6) . ? N1 C1 1.327(6) . ? N1 C5 1.339(7) . ? C1 C2 1.375(6) . ? C2 C3 1.395(6) . ? C3 C4 1.365(7) . ? C3 C6 1.495(5) . ? C4 C5 1.354(7) . ? C6 C11 1.398(5) . ? C6 C7 1.407(6) . ? C7 C8 1.409(5) . ? C7 C15 1.500(6) . ? C8 C9 1.405(5) . ? C8 C14 1.518(6) . ? C9 C10 1.407(5) . ? C10 C11 1.401(5) . ? C10 C13 1.517(6) . ? C11 C12 1.535(6) . ? C16 N2 1.346(7) . ? C16 C17 1.385(6) . ? C17 C18 1.369(7) . ? C18 C19 1.376(7) . ? C18 C21 1.509(5) . ? C19 C20 1.399(7) . ? C20 N2 1.326(7) . ? N2 Ag1 2.336(4) 2 ? C21 C22 1.379(6) . ? C21 C26 1.404(6) . ? C22 C23 1.408(5) . ? C22 C30 1.523(6) . ? C23 C24 1.415(5) . ? C23 C29 1.497(6) . ? C24 C25 1.427(5) . ? C25 C26 1.402(6) . ? C25 C28 1.518(6) . ? C26 C27 1.528(6) . ? C31 N3 1.328(6) . ? C31 C32 1.359(5) . ? C32 C33 1.388(6) . ? C33 C34 1.387(6) . ? C33 C36 1.488(5) . ? C34 C35 1.362(7) . ? C35 N3 1.337(7) . ? N3 Ag1 2.265(3) 8_455 ? C36 C37 1.392(6) . ? C36 C41 1.406(6) . ? C37 C38 1.411(6) . ? C37 C45 1.525(6) . ? C38 C39 1.406(6) . ? C38 C44 1.503(6) . ? C39 C40 1.403(6) . ? C40 C41 1.412(6) . ? C40 C43 1.501(6) . ? C41 C42 1.517(6) . ? N4 O1 1.217(5) . ? N4 O1 1.217(5) 7_465 ? N4 O2 1.245(8) . ? N5 O3 1.221(19) . ? N5 O5 1.222(19) . ? N5 O4 1.235(19) . ? 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 N3 Ag1 N1 129.51(15) 8_545 . ? N3 Ag1 N2 110.58(16) 8_545 2_554 ? N1 Ag1 N2 106.11(15) . 2_554 ? C24 B1 C39 124.6(3) . . ? C24 B1 C9 117.7(3) . . ? C39 B1 C9 117.6(3) . . ? C1 N1 C5 116.5(4) . . ? C1 N1 Ag1 121.9(3) . . ? C5 N1 Ag1 121.3(3) . . ? N1 C1 C2 123.6(4) . . ? C1 C2 C3 119.2(4) . . ? C4 C3 C2 116.4(4) . . ? C4 C3 C6 122.3(4) . . ? C2 C3 C6 121.3(4) . . ? C5 C4 C3 121.0(5) . . ? N1 C5 C4 123.3(5) . . ? C11 C6 C7 120.4(3) . . ? C11 C6 C3 119.8(4) . . ? C7 C6 C3 119.7(3) . . ? C6 C7 C8 119.3(4) . . ? C6 C7 C15 119.7(4) . . ? C8 C7 C15 121.1(4) . . ? C9 C8 C7 120.4(4) . . ? C9 C8 C14 121.6(3) . . ? C7 C8 C14 117.9(4) . . ? C8 C9 C10 119.5(3) . . ? C8 C9 B1 121.2(3) . . ? C10 C9 B1 119.3(3) . . ? C11 C10 C9 120.2(3) . . ? C11 C10 C13 117.9(4) . . ? C9 C10 C13 121.8(3) . . ? C6 C11 C10 120.1(4) . . ? C6 C11 C12 117.4(4) . . ? C10 C11 C12 122.6(4) . . ? N2 C16 C17 122.6(5) . . ? C18 C17 C16 119.8(5) . . ? C17 C18 C19 117.7(4) . . ? C17 C18 C21 121.7(4) . . ? C19 C18 C21 120.5(4) . . ? C18 C19 C20 120.0(5) . . ? N2 C20 C19 122.1(6) . . ? C20 N2 C16 117.8(4) . . ? C20 N2 Ag1 117.7(4) . 2 ? C16 N2 Ag1 124.4(3) . 2 ? C22 C21 C26 121.2(4) . . ? C22 C21 C18 119.7(4) . . ? C26 C21 C18 119.2(4) . . ? C21 C22 C23 120.1(4) . . ? C21 C22 C30 121.0(4) . . ? C23 C22 C30 118.8(4) . . ? C22 C23 C24 120.2(4) . . ? C22 C23 C29 118.8(4) . . ? C24 C23 C29 120.8(3) . . ? C23 C24 C25 118.4(3) . . ? C23 C24 B1 121.4(3) . . ? C25 C24 B1 119.8(3) . . ? C26 C25 C24 120.5(4) . . ? C26 C25 C28 119.9(4) . . ? C24 C25 C28 119.5(4) . . ? C25 C26 C21 119.3(4) . . ? C25 C26 C27 121.1(4) . . ? C21 C26 C27 119.6(4) . . ? N3 C31 C32 124.2(4) . . ? C31 C32 C33 120.3(4) . . ? C34 C33 C32 115.6(4) . . ? C34 C33 C36 121.5(4) . . ? C32 C33 C36 122.9(4) . . ? C35 C34 C33 120.2(5) . . ? N3 C35 C34 124.0(5) . . ? C31 N3 C35 115.7(4) . . ? C31 N3 Ag1 123.9(3) . 8_455 ? C35 N3 Ag1 120.1(3) . 8_455 ? C37 C36 C41 121.5(3) . . ? C37 C36 C33 119.0(4) . . ? C41 C36 C33 119.6(4) . . ? C36 C37 C38 119.2(4) . . ? C36 C37 C45 120.8(4) . . ? C38 C37 C45 120.0(4) . . ? C39 C38 C37 120.5(4) . . ? C39 C38 C44 120.9(4) . . ? C37 C38 C44 118.6(4) . . ? C40 C39 C38 119.2(3) . . ? C40 C39 B1 121.0(4) . . ? C38 C39 B1 119.6(3) . . ? C39 C40 C41 120.8(4) . . ? C39 C40 C43 121.1(4) . . ? C41 C40 C43 118.0(4) . . ? C36 C41 C40 118.6(4) . . ? C36 C41 C42 120.7(4) . . ? C40 C41 C42 120.7(4) . . ? O1 N4 O1 122.4(6) . 7_465 ? O1 N4 O2 118.8(3) . . ? O1 N4 O2 118.8(3) 7_465 . ? O3 N5 O5 120(2) . . ? O3 N5 O4 119(2) . . ? O5 N5 O4 121(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.590 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.089 # Attachment 'CIF-2.txt' _publ_section_exptl_refinement ; All aromatic groups were input as idealized planar rings with C-C bond lengths of 1.39 angstrom. Some C-C bonds from the aromatic rings to the methyl groups are somewhat short and so were constrained to be ca. 1.50 angstrom. These C-C and C-N bonds of the CH3CN guest molecules were constrained to be reasonably. All hydrogen atoms except the H atoms of solvents were generated geometrically (C-H = 0.93 or 0.96\%A for phenyl or methyl H atoms respectively) and were included in the refinement in the riding model approximation. The displacement parameters of methyl H atoms were set to 1.5 times U~eq~ of the equivalent isotropic displacement parameters of their parent atoms, while those of other H atoms were set to 1.2 times. All non-H atoms except for the disordered ones were refined anisotropically. ; #====================================================================== data_2_[(AgL)OTf].2CH3CN.13/6H2O _database_code_depnum_ccdc_archive 'CCDC 747395' #TrackingRef 'CIF-2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H61.33 Ag B F3 N6 O5.17 S' _chemical_formula_weight 1060.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.6581(2) _cell_length_b 32.4156(5) _cell_length_c 40.5791(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17965.8(5) _cell_formula_units_Z 12 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 15204 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 50.32 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6620 _exptl_absorpt_coefficient_mu 3.475 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.620 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35420 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 50.32 _reflns_number_total 15204 _reflns_number_gt 12187 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.1700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.057(12) _refine_ls_number_reflns 15204 _refine_ls_number_parameters 1464 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0968 _refine_ls_wR_factor_ref 0.2562 _refine_ls_wR_factor_gt 0.2381 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.191 _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 -0.31588(8) 0.30431(4) 0.86983(3) 0.0860(4) Uani 1 1 d . . . Ag2 Ag 0.23574(12) 0.24452(4) 0.49934(4) 0.1134(6) Uani 1 1 d . . . Ag3 Ag 1.05127(8) -0.21307(4) 0.37639(3) 0.0840(4) Uani 1 1 d . . . B1 B 0.3134(12) 0.4195(5) 1.0022(4) 0.065(4) Uani 1 1 d . . . B2 B -0.2823(14) 0.0914(5) 0.6627(4) 0.072(5) Uani 1 1 d . . . B3 B 0.7199(11) 0.0861(5) 0.3249(3) 0.053(4) Uani 1 1 d . . . N1 N -0.1738(8) 0.3142(4) 0.8979(3) 0.112(5) Uani 1 1 d G . . C1 C -0.1562(8) 0.2954(4) 0.9281(3) 0.108(6) Uani 1 1 d G . . H1A H -0.1969 0.2743 0.9354 0.129 Uiso 1 1 calc R . . C2 C -0.0778(9) 0.3081(4) 0.9474(3) 0.107(6) Uani 1 1 d G . . H2A H -0.0660 0.2956 0.9676 0.128 Uiso 1 1 calc R . . C3 C -0.0170(7) 0.3397(4) 0.9365(3) 0.087(5) Uani 1 1 d G . . C4 C -0.0346(10) 0.3585(4) 0.9063(3) 0.141(9) Uani 1 1 d G . . H4A H 0.0061 0.3796 0.8990 0.169 Uiso 1 1 calc R . . C5 C -0.1130(11) 0.3457(5) 0.8870(3) 0.153(10) Uani 1 1 d G . . H5A H -0.1248 0.3583 0.8668 0.184 Uiso 1 1 calc R . . C6 C 0.0652(13) 0.3544(5) 0.9578(4) 0.082(5) Uani 1 1 d . . . C7 C 0.0460(11) 0.3816(5) 0.9839(4) 0.075(4) Uani 1 1 d . . . C8 C 0.1246(11) 0.4015(4) 0.9988(3) 0.068(4) Uani 1 1 d . . . C9 C 0.2245(10) 0.3924(4) 0.9882(3) 0.055(3) Uani 1 1 d . . . C10 C 0.2396(10) 0.3640(4) 0.9639(3) 0.065(4) Uani 1 1 d . . . C11 C 0.1621(11) 0.3446(5) 0.9486(4) 0.074(4) Uani 1 1 d . . . C12 C 0.1759(11) 0.3097(6) 0.9222(5) 0.107(6) Uani 1 1 d D . . H12A H 0.2445 0.3057 0.9181 0.160 Uiso 1 1 calc R . . H12B H 0.1440 0.3177 0.9021 0.160 Uiso 1 1 calc R . . H12C H 0.1477 0.2846 0.9302 0.160 Uiso 1 1 calc R . . C13 C 0.3447(10) 0.3552(5) 0.9519(4) 0.086(5) Uani 1 1 d D . . H13A H 0.3431 0.3350 0.9347 0.129 Uiso 1 1 calc R . . H13B H 0.3831 0.3449 0.9700 0.129 Uiso 1 1 calc R . . H13C H 0.3734 0.3802 0.9438 0.129 Uiso 1 1 calc R . . C14 C 0.1070(9) 0.4319(5) 1.0281(3) 0.074(4) Uani 1 1 d D . . H14A H 0.0380 0.4341 1.0323 0.111 Uiso 1 1 calc R . . H14B H 0.1328 0.4586 1.0226 0.111 Uiso 1 1 calc R . . H14C H 0.1393 0.4217 1.0474 0.111 Uiso 1 1 calc R . . C15 C -0.0598(9) 0.3912(5) 0.9943(4) 0.091(5) Uani 1 1 d D . . H15A H -0.0593 0.4101 1.0125 0.137 Uiso 1 1 calc R . . H15B H -0.0918 0.3661 1.0008 0.137 Uiso 1 1 calc R . . H15C H -0.0944 0.4032 0.9761 0.137 Uiso 1 1 calc R . . N2 N 0.8189(8) 0.3087(4) 1.0918(3) 0.122(3) Uani 1 1 d G . . C16 C 0.7560(10) 0.3362(4) 1.1074(2) 0.122(3) Uani 1 1 d G . . H16A H 0.7673 0.3439 1.1291 0.146 Uiso 1 1 calc R . . C17 C 0.6761(9) 0.3522(4) 1.0904(3) 0.122(3) Uani 1 1 d G . . H17A H 0.6339 0.3706 1.1008 0.146 Uiso 1 1 calc R . . C18 C 0.6591(9) 0.3407(4) 1.0579(3) 0.122(3) Uani 1 1 d G . . C19 C 0.7221(10) 0.3132(5) 1.0424(2) 0.122(3) Uani 1 1 d G . . H19A H 0.7108 0.3055 1.0206 0.146 Uiso 1 1 calc R . . C20 C 0.8020(9) 0.2972(4) 1.0593(3) 0.122(3) Uani 1 1 d G . . H20A H 0.8441 0.2788 1.0489 0.146 Uiso 1 1 calc R . . C21 C 0.5711(11) 0.3590(5) 1.0420(4) 0.073(4) Uani 1 1 d . . . C22 C 0.4817(11) 0.3450(4) 1.0504(3) 0.064(4) Uani 1 1 d . . . C23 C 0.3970(10) 0.3640(4) 1.0391(3) 0.058(4) Uani 1 1 d D . . C24 C 0.4028(11) 0.3963(4) 1.0155(3) 0.064(4) Uani 1 1 d . . . C25 C 0.4967(9) 0.4088(4) 1.0047(3) 0.063(4) Uani 1 1 d . . . C26 C 0.5827(11) 0.3898(6) 1.0188(4) 0.079(5) Uani 1 1 d . . . C27 C 0.6888(12) 0.4022(6) 1.0093(5) 0.113(6) Uani 1 1 d D . . H27A H 0.6870 0.4233 0.9927 0.170 Uiso 1 1 calc R . . H27B H 0.7229 0.3785 1.0009 0.170 Uiso 1 1 calc R . . H27C H 0.7222 0.4125 1.0284 0.170 Uiso 1 1 calc R . . C28 C 0.5055(11) 0.4406(5) 0.9787(4) 0.084(5) Uani 1 1 d D . . H28A H 0.5735 0.4459 0.9744 0.127 Uiso 1 1 calc R . . H28B H 0.4745 0.4656 0.9860 0.127 Uiso 1 1 calc R . . H28C H 0.4743 0.4310 0.9590 0.127 Uiso 1 1 calc R . . C29 C 0.2936(10) 0.3498(5) 1.0496(4) 0.090(5) Uani 1 1 d D . . H29A H 0.2990 0.3281 1.0656 0.135 Uiso 1 1 calc R . . H29B H 0.2589 0.3397 1.0306 0.135 Uiso 1 1 calc R . . H29C H 0.2586 0.3726 1.0589 0.135 Uiso 1 1 calc R . . C30 C 0.4785(12) 0.3066(5) 1.0748(4) 0.101(5) Uani 1 1 d D . . H30A H 0.4116 0.2992 1.0791 0.152 Uiso 1 1 calc R . . H30B H 0.5100 0.3138 1.0952 0.152 Uiso 1 1 calc R . . H30C H 0.5119 0.2837 1.0650 0.152 Uiso 1 1 calc R . . N3 N 0.2785(8) 0.6865(2) 1.0018(3) 0.079(4) Uani 1 1 d G . . C31 C 0.2223(7) 0.6649(3) 1.0245(2) 0.080(4) Uani 1 1 d G . . H31A H 0.1810 0.6790 1.0388 0.096 Uiso 1 1 calc R . . C32 C 0.2279(7) 0.6221(3) 1.0259(2) 0.073(4) Uani 1 1 d G . . H32A H 0.1902 0.6076 1.0411 0.088 Uiso 1 1 calc R . . C33 C 0.2896(8) 0.6010(2) 1.0045(3) 0.066(4) Uani 1 1 d G . . C34 C 0.3459(7) 0.6226(3) 0.9818(2) 0.085(5) Uani 1 1 d G . . H34A H 0.3872 0.6085 0.9675 0.102 Uiso 1 1 calc R . . C35 C 0.3403(7) 0.6654(3) 0.9804(2) 0.081(5) Uani 1 1 d G . . H35A H 0.3779 0.6799 0.9652 0.097 Uiso 1 1 calc R . . C36 C 0.2961(9) 0.5547(4) 1.0042(3) 0.062(4) Uani 1 1 d . . . C37 C 0.3316(9) 0.5331(5) 1.0314(3) 0.058(3) Uani 1 1 d . . . C38 C 0.3317(9) 0.4909(5) 1.0312(3) 0.055(3) Uani 1 1 d . . . C39 C 0.3015(9) 0.4678(4) 1.0043(3) 0.054(3) Uani 1 1 d . . . C40 C 0.2689(9) 0.4903(4) 0.9754(3) 0.054(3) Uani 1 1 d . . . C41 C 0.2608(9) 0.5326(5) 0.9763(3) 0.064(4) Uani 1 1 d . . . C42 C 0.2077(13) 0.5560(5) 0.9484(3) 0.081(5) Uani 1 1 d . . . H42A H 0.2072 0.5850 0.9533 0.122 Uiso 1 1 calc R . . H42B H 0.1417 0.5462 0.9466 0.122 Uiso 1 1 calc R . . H42C H 0.2414 0.5515 0.9279 0.122 Uiso 1 1 calc R . . C43 C 0.2413(11) 0.4684(5) 0.9435(3) 0.074(4) Uani 1 1 d . . . H43A H 0.2215 0.4884 0.9274 0.111 Uiso 1 1 calc R . . H43B H 0.1882 0.4497 0.9476 0.111 Uiso 1 1 calc R . . H43C H 0.2967 0.4533 0.9353 0.111 Uiso 1 1 calc R . . C44 C 0.3643(11) 0.4661(4) 1.0629(3) 0.077(4) Uani 1 1 d D . . H44A H 0.3821 0.4851 1.0800 0.115 Uiso 1 1 calc R . . H44B H 0.4196 0.4490 1.0577 0.115 Uiso 1 1 calc R . . H44C H 0.3111 0.4491 1.0703 0.115 Uiso 1 1 calc R . . C45 C 0.3804(12) 0.5595(4) 1.0593(3) 0.073(4) Uani 1 1 d D . . H45A H 0.4040 0.5415 1.0764 0.109 Uiso 1 1 calc R . . H45B H 0.3330 0.5782 1.0684 0.109 Uiso 1 1 calc R . . H45C H 0.4341 0.5749 1.0503 0.109 Uiso 1 1 calc R . . N4 N -0.3298(6) 0.2591(3) 0.8297(2) 0.079(4) Uani 1 1 d G . . C46 C -0.3525(9) 0.2710(3) 0.7977(2) 0.109(6) Uani 1 1 d G . . H46A H -0.3708 0.2981 0.7933 0.131 Uiso 1 1 calc R . . C47 C -0.3479(10) 0.2424(4) 0.77215(17) 0.105(6) Uani 1 1 d G . . H47A H -0.3631 0.2504 0.7507 0.126 Uiso 1 1 calc R . . C48 C -0.3206(8) 0.2019(3) 0.7786(2) 0.078(5) Uani 1 1 d G . . C49 C -0.2979(8) 0.1900(2) 0.8106(2) 0.094(5) Uani 1 1 d G . . H49A H -0.2796 0.1629 0.8150 0.113 Uiso 1 1 calc R . . C50 C -0.3025(7) 0.2186(3) 0.83615(17) 0.069(4) Uani 1 1 d G . . H50A H -0.2873 0.2106 0.8576 0.083 Uiso 1 1 calc R . . C51 C -0.3125(12) 0.1703(5) 0.7500(4) 0.077(4) Uani 1 1 d . . . C52 C -0.3945(14) 0.1569(6) 0.7356(4) 0.093(5) Uani 1 1 d . . . C53 C -0.3873(11) 0.1301(5) 0.7073(4) 0.075(4) Uani 1 1 d . . . C54 C -0.2933(12) 0.1167(5) 0.6970(3) 0.070(4) Uani 1 1 d . . . C55 C -0.2108(13) 0.1300(5) 0.7135(3) 0.079(5) Uani 1 1 d . . . C56 C -0.2147(10) 0.1570(4) 0.7410(3) 0.068(4) Uani 1 1 d . . . C57 C -0.1287(11) 0.1726(5) 0.7587(3) 0.081(5) Uani 1 1 d . . . H57A H -0.1495 0.1906 0.7761 0.122 Uiso 1 1 calc R . . H57B H -0.0873 0.1874 0.7437 0.122 Uiso 1 1 calc R . . H57C H -0.0930 0.1498 0.7679 0.122 Uiso 1 1 calc R . . C58 C -0.1065(12) 0.1128(5) 0.7071(4) 0.086(5) Uani 1 1 d . . . H58A H -0.1081 0.0945 0.6884 0.128 Uiso 1 1 calc R . . H58B H -0.0846 0.0979 0.7262 0.128 Uiso 1 1 calc R . . H58C H -0.0625 0.1352 0.7027 0.128 Uiso 1 1 calc R . . C59 C -0.4819(11) 0.1177(6) 0.6905(5) 0.100(6) Uani 1 1 d . . . H59A H -0.4675 0.1001 0.6721 0.149 Uiso 1 1 calc R . . H59B H -0.5154 0.1419 0.6829 0.149 Uiso 1 1 calc R . . H59C H -0.5228 0.1032 0.7058 0.149 Uiso 1 1 calc R . . C60 C -0.4940(12) 0.1679(7) 0.7478(6) 0.129(8) Uani 1 1 d . . . H60A H -0.4883 0.1855 0.7667 0.193 Uiso 1 1 calc R . . H60B H -0.5286 0.1432 0.7537 0.193 Uiso 1 1 calc R . . H60C H -0.5293 0.1822 0.7307 0.193 Uiso 1 1 calc R . . N5 N 0.1336(9) 0.2043(3) 0.5296(3) 0.112(5) Uani 1 1 d GU . . C61 C 0.1598(7) 0.1974(3) 0.5623(3) 0.097(5) Uani 1 1 d G . . H61A H 0.2198 0.2068 0.5701 0.116 Uiso 1 1 calc R . . C62 C 0.0962(8) 0.1767(3) 0.5832(2) 0.070(4) Uani 1 1 d G . . H62A H 0.1137 0.1721 0.6051 0.084 Uiso 1 1 calc R . . C63 C 0.0064(7) 0.1627(3) 0.5716(2) 0.078(4) Uani 1 1 d G . . C64 C -0.0198(8) 0.1696(4) 0.5389(3) 0.118(7) Uani 1 1 d G . . H64A H -0.0799 0.1603 0.5311 0.142 Uiso 1 1 calc R . . C65 C 0.0438(11) 0.1904(4) 0.5179(2) 0.123(7) Uani 1 1 d GU . . H65A H 0.0263 0.1950 0.4961 0.148 Uiso 1 1 calc R . . C66 C -0.0669(11) 0.1433(6) 0.5943(4) 0.075(4) Uani 1 1 d . . . C67 C -0.0572(14) 0.1026(5) 0.6060(4) 0.078(5) Uani 1 1 d . . . C68 C -0.1275(11) 0.0856(4) 0.6257(3) 0.059(3) Uani 1 1 d . . . C69 C -0.2069(11) 0.1099(5) 0.6372(3) 0.066(4) Uani 1 1 d . . . C70 C -0.2164(9) 0.1502(4) 0.6262(4) 0.066(4) Uani 1 1 d . . . C71 C -0.1477(14) 0.1672(5) 0.6051(4) 0.082(5) Uani 1 1 d . . . C72 C -0.1622(12) 0.2122(5) 0.5942(5) 0.092(5) Uani 1 1 d . . . H72A H -0.2213 0.2228 0.6038 0.138 Uiso 1 1 calc R . . H72B H -0.1667 0.2134 0.5707 0.138 Uiso 1 1 calc R . . H72C H -0.1075 0.2284 0.6015 0.138 Uiso 1 1 calc R . . C73 C -0.3071(13) 0.1768(5) 0.6349(5) 0.102(5) Uani 1 1 d . . . H73A H -0.3482 0.1620 0.6500 0.153 Uiso 1 1 calc R . . H73B H -0.3432 0.1827 0.6151 0.153 Uiso 1 1 calc R . . H73C H -0.2861 0.2022 0.6448 0.153 Uiso 1 1 calc R . . C74 C -0.1127(12) 0.0419(5) 0.6366(3) 0.075(4) Uani 1 1 d . . . H74A H -0.1665 0.0336 0.6503 0.113 Uiso 1 1 calc R . . H74B H -0.0528 0.0399 0.6488 0.113 Uiso 1 1 calc R . . H74C H -0.1094 0.0243 0.6176 0.113 Uiso 1 1 calc R . . C75 C 0.0288(11) 0.0784(5) 0.5927(4) 0.075(4) Uani 1 1 d . . . H75A H 0.0279 0.0510 0.6018 0.112 Uiso 1 1 calc R . . H75B H 0.0887 0.0919 0.5987 0.112 Uiso 1 1 calc R . . H75C H 0.0242 0.0768 0.5691 0.112 Uiso 1 1 calc R . . N6 N -0.6084(7) -0.1341(2) 0.6324(2) 0.0868(18) Uani 1 1 d GU . . C76 C -0.6357(6) -0.1066(3) 0.6570(2) 0.0868(18) Uani 1 1 d GU . . H76A H -0.6874 -0.1131 0.6710 0.104 Uiso 1 1 calc R . . C77 C -0.5857(8) -0.0696(3) 0.6607(2) 0.0868(18) Uani 1 1 d G . . H77A H -0.6040 -0.0512 0.6772 0.104 Uiso 1 1 calc R . . C78 C -0.5084(7) -0.0600(3) 0.6398(3) 0.0868(18) Uani 1 1 d G . . C79 C -0.4811(7) -0.0875(3) 0.6152(2) 0.0868(18) Uani 1 1 d G . . H79A H -0.4294 -0.0810 0.6012 0.104 Uiso 1 1 calc R . . C80 C -0.5311(7) -0.1245(3) 0.6115(2) 0.0868(18) Uani 1 1 d G . . H80A H -0.5128 -0.1429 0.5950 0.104 Uiso 1 1 calc R . . C81 C -0.4535(10) -0.0202(4) 0.6444(3) 0.060(4) Uani 1 1 d . . . C82 C -0.3875(13) -0.0172(5) 0.6731(3) 0.076(4) Uani 1 1 d D . . C83 C -0.3374(11) 0.0183(5) 0.6783(3) 0.069(4) Uani 1 1 d D . . C84 C -0.3453(11) 0.0517(5) 0.6569(3) 0.068(4) Uani 1 1 d . . . C85 C -0.4072(11) 0.0468(4) 0.6281(3) 0.068(4) Uani 1 1 d D . . C86 C -0.4612(11) 0.0118(5) 0.6233(3) 0.065(4) Uani 1 1 d . . . C87 C -0.5316(14) 0.0084(5) 0.5942(4) 0.104(6) Uani 1 1 d D . . H87A H -0.5643 0.0343 0.5910 0.157 Uiso 1 1 calc R . . H87B H -0.5791 -0.0127 0.5986 0.157 Uiso 1 1 calc R . . H87C H -0.4955 0.0015 0.5746 0.157 Uiso 1 1 calc R . . C88 C -0.4210(14) 0.0850(4) 0.6051(3) 0.088(5) Uani 1 1 d D . . H88A H -0.4624 0.0776 0.5869 0.133 Uiso 1 1 calc R . . H88B H -0.3584 0.0937 0.5969 0.133 Uiso 1 1 calc R . . H88C H -0.4507 0.1070 0.6173 0.133 Uiso 1 1 calc R . . C89 C -0.2685(12) 0.0211(5) 0.7088(3) 0.087(5) Uani 1 1 d D . . H89A H -0.2713 -0.0043 0.7209 0.131 Uiso 1 1 calc R . . H89B H -0.2892 0.0434 0.7227 0.131 Uiso 1 1 calc R . . H89C H -0.2026 0.0259 0.7015 0.131 Uiso 1 1 calc R . . C90 C -0.3796(16) -0.0553(4) 0.6960(4) 0.105(6) Uani 1 1 d D . . H90A H -0.3356 -0.0493 0.7138 0.157 Uiso 1 1 calc R . . H90B H -0.3552 -0.0784 0.6837 0.157 Uiso 1 1 calc R . . H90C H -0.4431 -0.0619 0.7047 0.157 Uiso 1 1 calc R . . N7 N 0.3329(8) 0.2082(3) 0.4640(3) 0.098(4) Uani 1 1 d GU . . C91 C 0.2958(6) 0.1975(3) 0.4333(3) 0.090(5) Uani 1 1 d G . . H91A H 0.2307 0.2029 0.4282 0.108 Uiso 1 1 calc R . . C92 C 0.3562(8) 0.1788(3) 0.4101(2) 0.071(4) Uani 1 1 d G . . H92A H 0.3314 0.1716 0.3896 0.085 Uiso 1 1 calc R . . C93 C 0.4536(7) 0.1707(3) 0.4177(2) 0.067(4) Uani 1 1 d G . . C94 C 0.4906(6) 0.1814(3) 0.4485(3) 0.078(4) Uani 1 1 d G . . H94A H 0.5558 0.1760 0.4535 0.094 Uiso 1 1 calc R . . C95 C 0.4302(9) 0.2001(3) 0.4716(2) 0.125(7) Uani 1 1 d GU . . H95A H 0.4550 0.2073 0.4922 0.150 Uiso 1 1 calc R . . C96 C 0.5174(10) 0.1493(4) 0.3945(3) 0.061(4) Uani 1 1 d . . . C97 C 0.5996(13) 0.1692(4) 0.3817(4) 0.074(4) Uani 1 1 d . . . C98 C 0.6652(10) 0.1490(5) 0.3604(4) 0.076(4) Uani 1 1 d D . . C99 C 0.6436(11) 0.1092(4) 0.3493(3) 0.067(4) Uani 1 1 d . . . C100 C 0.5542(10) 0.0900(4) 0.3607(3) 0.052(3) Uani 1 1 d . . . C101 C 0.4920(9) 0.1095(4) 0.3826(3) 0.058(3) Uani 1 1 d . . . C102 C 0.4049(11) 0.0881(5) 0.3961(4) 0.081(5) Uani 1 1 d . . . H10A H 0.3982 0.0617 0.3857 0.121 Uiso 1 1 calc R . . H10B H 0.3475 0.1044 0.3919 0.121 Uiso 1 1 calc R . . H10C H 0.4126 0.0845 0.4194 0.121 Uiso 1 1 calc R . . C103 C 0.5321(10) 0.0483(5) 0.3492(3) 0.078(5) Uani 1 1 d . . . H10D H 0.5827 0.0393 0.3344 0.117 Uiso 1 1 calc R . . H10E H 0.4704 0.0484 0.3378 0.117 Uiso 1 1 calc R . . H10F H 0.5285 0.0299 0.3677 0.117 Uiso 1 1 calc R . . C104 C 0.7613(11) 0.1698(4) 0.3491(4) 0.085(5) Uani 1 1 d D . . H10G H 0.7643 0.1973 0.3577 0.127 Uiso 1 1 calc R . . H10H H 0.7631 0.1708 0.3255 0.127 Uiso 1 1 calc R . . H10I H 0.8161 0.1542 0.3571 0.127 Uiso 1 1 calc R . . C105 C 0.6176(12) 0.2141(4) 0.3939(4) 0.091(5) Uani 1 1 d D . . H10J H 0.6754 0.2249 0.3836 0.137 Uiso 1 1 calc R . . H10K H 0.6260 0.2141 0.4174 0.137 Uiso 1 1 calc R . . H10L H 0.5623 0.2310 0.3882 0.137 Uiso 1 1 calc R . . N8 N 0.9701(6) -0.1530(2) 0.3674(2) 0.066(3) Uani 1 1 d G . . C106 C 0.8890(6) -0.1407(3) 0.3856(2) 0.076(4) Uani 1 1 d G . . H10M H 0.8639 -0.1578 0.4020 0.091 Uiso 1 1 calc R . . C107 C 0.8453(6) -0.1028(3) 0.3794(2) 0.067(4) Uani 1 1 d G . . H10N H 0.7910 -0.0945 0.3915 0.081 Uiso 1 1 calc R . . C108 C 0.8827(7) -0.0772(2) 0.3549(2) 0.079(5) Uani 1 1 d G . . C109 C 0.9639(8) -0.0895(3) 0.3368(2) 0.079(4) Uani 1 1 d G . . H10O H 0.9890 -0.0724 0.3204 0.094 Uiso 1 1 calc R . . C110 C 1.0076(6) -0.1274(3) 0.3430(2) 0.089(5) Uani 1 1 d G . . H11A H 1.0619 -0.1357 0.3309 0.107 Uiso 1 1 calc R . . C111 C 0.8347(14) -0.0357(6) 0.3467(4) 0.093(5) Uani 1 1 d . . . C112 C 0.8532(10) -0.0029(5) 0.3694(3) 0.064(4) Uani 1 1 d D . . C113 C 0.8117(10) 0.0363(4) 0.3625(3) 0.059(4) Uani 1 1 d . . . C114 C 0.7575(11) 0.0417(5) 0.3342(3) 0.068(4) Uani 1 1 d . . . C115 C 0.7404(12) 0.0076(5) 0.3134(3) 0.070(4) Uani 1 1 d . . . C116 C 0.7771(11) -0.0300(5) 0.3198(3) 0.072(4) Uani 1 1 d D . . C117 C 0.6756(12) 0.0152(4) 0.2827(3) 0.074(4) Uani 1 1 d D . . H11B H 0.6670 -0.0102 0.2709 0.112 Uiso 1 1 calc R . . H11C H 0.7068 0.0351 0.2686 0.112 Uiso 1 1 calc R . . H11D H 0.6129 0.0255 0.2895 0.112 Uiso 1 1 calc R . . C118 C 0.7528(14) -0.0675(4) 0.2976(4) 0.096(5) Uani 1 1 d D . . H11E H 0.7118 -0.0588 0.2797 0.144 Uiso 1 1 calc R . . H11F H 0.7192 -0.0880 0.3104 0.144 Uiso 1 1 calc R . . H11G H 0.8124 -0.0790 0.2890 0.144 Uiso 1 1 calc R . . C119 C 0.9205(11) -0.0110(4) 0.3993(3) 0.079(4) Uani 1 1 d D . . H11H H 0.9264 0.0137 0.4121 0.119 Uiso 1 1 calc R . . H11I H 0.9840 -0.0194 0.3917 0.119 Uiso 1 1 calc R . . H11J H 0.8927 -0.0325 0.4127 0.119 Uiso 1 1 calc R . . C120 C 0.8337(12) 0.0740(4) 0.3844(4) 0.084(4) Uani 1 1 d D . . H12D H 0.8710 0.0655 0.4033 0.126 Uiso 1 1 calc R . . H12E H 0.7733 0.0862 0.3916 0.126 Uiso 1 1 calc R . . H12F H 0.8706 0.0939 0.3720 0.126 Uiso 1 1 calc R . . N9 N 0.9017(7) 0.2417(3) 0.1624(2) 0.088(4) Uani 1 1 d G . . C121 C 0.8829(10) 0.2551(3) 0.1944(3) 0.128(8) Uani 1 1 d G . . H12G H 0.8909 0.2827 0.1998 0.153 Uiso 1 1 calc R . . C122 C 0.8521(10) 0.2271(4) 0.21816(19) 0.096(5) Uani 1 1 d G . . H12H H 0.8395 0.2360 0.2395 0.115 Uiso 1 1 calc R . . C123 C 0.8402(9) 0.1857(3) 0.2100(2) 0.086(5) Uani 1 1 d G . . C124 C 0.8590(10) 0.1723(2) 0.1781(3) 0.102(6) Uani 1 1 d G . . H12I H 0.8510 0.1447 0.1727 0.123 Uiso 1 1 calc R . . C125 C 0.8898(9) 0.2003(3) 0.1543(2) 0.089(5) Uani 1 1 d G . . H12J H 0.9023 0.1914 0.1329 0.107 Uiso 1 1 calc R . . C126 C 0.8107(11) 0.1571(4) 0.2372(3) 0.069(4) Uani 1 1 d . . . C127 C 0.7092(11) 0.1517(5) 0.2442(4) 0.083(5) Uani 1 1 d . . . C128 C 0.6805(12) 0.1277(5) 0.2711(3) 0.081(4) Uani 1 1 d . . . C129 C 0.7527(12) 0.1077(4) 0.2914(3) 0.070(4) Uani 1 1 d . . . C130 C 0.8471(10) 0.1121(5) 0.2833(3) 0.071(4) Uani 1 1 d D . . C131 C 0.8791(9) 0.1355(5) 0.2565(4) 0.069(4) Uani 1 1 d D . . C132 C 0.9868(9) 0.1407(5) 0.2457(3) 0.074(4) Uani 1 1 d D . . H13D H 1.0284 0.1253 0.2602 0.112 Uiso 1 1 calc R . . H13E H 1.0043 0.1693 0.2465 0.112 Uiso 1 1 calc R . . H13F H 0.9945 0.1306 0.2236 0.112 Uiso 1 1 calc R . . C133 C 0.9262(9) 0.0897(5) 0.3045(4) 0.090(5) Uani 1 1 d D . . H13G H 0.9901 0.0961 0.2960 0.136 Uiso 1 1 calc R . . H13H H 0.9157 0.0605 0.3035 0.136 Uiso 1 1 calc R . . H13I H 0.9214 0.0988 0.3269 0.136 Uiso 1 1 calc R . . C134 C 0.5683(12) 0.1234(7) 0.2781(5) 0.116(7) Uani 1 1 d . . . H13J H 0.5584 0.1046 0.2962 0.175 Uiso 1 1 calc R . . H13K H 0.5361 0.1129 0.2588 0.175 Uiso 1 1 calc R . . H13L H 0.5416 0.1499 0.2837 0.175 Uiso 1 1 calc R . . C135 C 0.6325(13) 0.1722(7) 0.2236(5) 0.120(7) Uani 1 1 d . . . H13M H 0.5688 0.1657 0.2321 0.180 Uiso 1 1 calc R . . H13N H 0.6374 0.1626 0.2013 0.180 Uiso 1 1 calc R . . H13O H 0.6420 0.2016 0.2241 0.180 Uiso 1 1 calc R . . S1 S 0.9286(4) -0.26669(17) 0.43374(12) 0.1046(15) Uani 1 1 d DU . . O1 O 0.8594(10) -0.2419(4) 0.4147(3) 0.114(4) Uani 1 1 d D . . O2 O 0.8894(10) -0.3081(3) 0.4440(4) 0.128(4) Uani 1 1 d DU . . O3 O 1.0269(9) -0.2684(5) 0.4220(3) 0.127(4) Uani 1 1 d D . . C136 C 0.935(2) -0.2407(7) 0.4720(4) 0.123(7) Uani 1 1 d DU . . F1 F 0.9634(11) -0.2012(4) 0.4666(4) 0.160(5) Uani 1 1 d U . . F2 F 0.8431(13) -0.2394(4) 0.4856(3) 0.160(5) Uani 1 1 d . . . F3 F 0.9921(15) -0.2574(5) 0.4931(3) 0.193(7) Uani 1 1 d U . . S3 S 0.0364(4) 0.74800(17) 0.06714(11) 0.1084(15) Uani 1 1 d D . . O7 O 0.0640(19) 0.7073(6) 0.0809(6) 0.216(9) Uiso 1 1 d D . . O8 O 0.1120(11) 0.7570(5) 0.0442(4) 0.147(5) Uiso 1 1 d D . . O9 O -0.0639(10) 0.7516(5) 0.0563(4) 0.148(5) Uiso 1 1 d D . . C138 C 0.0557(19) 0.7789(8) 0.1008(5) 0.187(11) Uiso 1 1 d D . . F7 F 0.0053(17) 0.7700(7) 0.1291(6) 0.236(8) Uiso 1 1 d D . . F8 F 0.0294(19) 0.8179(7) 0.0912(6) 0.238(8) Uiso 1 1 d D . . F9 F 0.1536(17) 0.7820(7) 0.1105(5) 0.231(8) Uiso 1 1 d D . . S2 S 0.7577(8) 0.3887(3) 0.2146(2) 0.210(4) Uiso 1 1 d D . . O4 O 0.773(2) 0.3952(8) 0.2515(4) 0.264(12) Uiso 1 1 d D . . O5 O 0.8150(19) 0.4225(8) 0.1971(7) 0.301 Uiso 1 1 d D . . O6 O 0.7970(18) 0.3480(6) 0.2039(6) 0.255(11) Uiso 1 1 d D . . C137 C 0.6317(12) 0.3926(8) 0.2060(6) 0.350 Uiso 1 1 d D . . F4 F 0.5712(16) 0.3696(8) 0.2246(7) 0.307 Uiso 1 1 d D . . F5 F 0.5863(19) 0.4287(8) 0.2092(7) 0.350 Uiso 1 1 d D . . F6 F 0.5944(18) 0.3817(9) 0.1763(6) 0.320 Uiso 1 1 d D . . N10 N 0.644(2) 0.4809(11) 0.0670(8) 0.122(10) Uiso 0.50 1 d PD . . N10A N 0.8644(19) 0.4266(8) 0.0848(6) 0.082(7) Uiso 0.50 1 d PD . . C139 C 0.705(3) 0.4754(16) 0.0908(10) 0.291(17) Uiso 1 1 d D . . C140 C 0.812(3) 0.4561(14) 0.0964(11) 0.291(17) Uiso 1 1 d D . . N11 N 0.3042(17) 0.1012(7) 0.5581(5) 0.164(5) Uiso 1 1 d D . . C141 C 0.364(2) 0.1103(9) 0.5340(6) 0.164(5) Uiso 1 1 d D . . C142 C 0.412(2) 0.0828(9) 0.5046(6) 0.164(5) Uiso 1 1 d D . . N12 N 0.723(3) 0.5278(10) 0.8401(9) 0.259(15) Uiso 1 1 d D . . C143 C 0.692(2) 0.5631(9) 0.8453(7) 0.166(10) Uiso 1 1 d D . . C144 C 0.708(2) 0.6038(8) 0.8645(6) 0.158(9) Uiso 1 1 d D . . N13 N 0.3938(16) 0.3577(7) 0.1473(5) 0.150(7) Uiso 1 1 d D . . C145 C 0.4259(19) 0.3921(7) 0.1419(6) 0.142(8) Uiso 1 1 d D . . C146 C 0.475(3) 0.4352(9) 0.1407(9) 0.211(14) Uiso 1 1 d D . . N14 N 1.020(2) 0.5497(9) 0.0146(6) 0.183(9) Uiso 1 1 d D . . C147 C 0.995(3) 0.5811(11) 0.0305(9) 0.214(14) Uiso 1 1 d D . . C148 C 0.952(4) 0.6161(13) 0.0523(11) 0.254(18) Uiso 1 1 d D . . N15 N 0.2194(16) 0.3978(6) 0.8684(5) 0.153(7) Uiso 1 1 d D . . C149 C 0.1622(16) 0.4263(7) 0.8616(5) 0.128(7) Uiso 1 1 d D . . C150 C 0.078(2) 0.4300(11) 0.8344(7) 0.193(12) Uiso 1 1 d D . . N16 N 0.921(3) 0.2934(10) 0.6771(10) 0.265(15) Uiso 1 1 d D . . C151 C 0.900(7) 0.2557(12) 0.683(3) 0.56(8) Uiso 1 1 d D . . C152 C 0.962(3) 0.2193(9) 0.6702(8) 0.196(12) Uiso 1 1 d D . . N17 N -0.0762(11) 0.2733(5) 0.8105(4) 0.032(4) Uiso 0.50 1 d PD . . N17A N 0.1461(12) 0.2437(6) 0.8514(4) 0.049(5) Uiso 0.50 1 d PD . . C153 C -0.035(2) 0.2496(9) 0.8311(8) 0.215(14) Uiso 1 1 d D . . C154 C 0.0567(14) 0.2572(7) 0.8514(5) 0.129(7) Uiso 1 1 d D . . N18 N 0.5135(11) 0.0139(4) 0.7669(3) 0.097(4) Uiso 1 1 d D . . C155 C 0.441(3) 0.0097(12) 0.7468(10) 0.28(2) Uiso 1 1 d D . . C156 C 0.3584(11) -0.0258(5) 0.7413(4) 0.078(4) Uiso 1 1 d D . . O12 O 0.7551(15) 0.4348(6) 0.9182(5) 0.085(6) Uiso 0.50 1 d P . . O13 O 0.9567(18) 0.4615(7) 0.9171(7) 0.100(7) Uiso 0.50 1 d P . . O13A O 0.950(3) 0.4701(11) 0.9387(10) 0.151(11) Uiso 0.50 1 d P . . O14 O 0.866(3) 0.5341(11) 0.1555(9) 0.292(14) Uiso 1 1 d . . . O15 O 0.269(3) 0.2124(12) 0.6952(10) 0.321(16) Uiso 1 1 d . . . O16 O 0.028(3) 0.0141(12) 0.7170(10) 0.320(17) Uiso 1 1 d . . . O17 O 0.029(3) 0.7214(11) 0.1924(9) 0.293(14) Uiso 1 1 d . . . O18 O 0.213(3) 0.8698(11) 0.7412(9) 0.288(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0805(7) 0.0807(8) 0.0968(8) -0.0272(7) -0.0099(6) 0.0088(6) Ag2 0.1466(12) 0.0624(8) 0.1314(11) -0.0098(7) 0.0698(10) 0.0036(8) Ag3 0.0779(7) 0.0763(8) 0.0977(8) -0.0282(6) -0.0156(6) 0.0169(6) B1 0.055(9) 0.066(11) 0.073(10) -0.002(9) 0.000(9) 0.002(9) B2 0.088(12) 0.048(11) 0.081(11) -0.020(9) -0.011(11) 0.033(10) B3 0.063(9) 0.051(10) 0.044(8) 0.002(7) 0.006(7) 0.008(8) N1 0.085(9) 0.122(13) 0.129(13) -0.038(11) 0.013(9) -0.027(10) C1 0.092(13) 0.116(16) 0.115(14) 0.017(12) -0.019(12) -0.016(11) C2 0.070(10) 0.114(15) 0.137(15) 0.009(13) -0.017(11) -0.006(11) C3 0.071(10) 0.059(10) 0.130(15) -0.012(10) 0.004(11) -0.014(9) C4 0.116(16) 0.20(2) 0.108(14) 0.055(16) -0.038(13) -0.059(17) C5 0.20(2) 0.129(18) 0.132(16) 0.030(15) -0.073(19) -0.078(19) C6 0.101(14) 0.076(11) 0.068(9) -0.001(9) 0.000(10) -0.012(10) C7 0.062(9) 0.067(10) 0.098(11) 0.008(9) -0.001(9) -0.001(8) C8 0.075(11) 0.067(9) 0.060(8) 0.004(8) -0.014(8) -0.020(8) C9 0.068(9) 0.055(9) 0.042(7) 0.002(7) 0.011(7) 0.014(7) C10 0.066(9) 0.058(9) 0.071(9) -0.003(8) -0.018(8) -0.012(8) C11 0.054(9) 0.090(11) 0.077(9) -0.014(9) 0.020(8) -0.005(9) C12 0.070(10) 0.123(15) 0.128(13) -0.054(12) -0.013(10) -0.011(10) C13 0.076(10) 0.076(11) 0.105(11) -0.035(9) -0.006(9) 0.004(8) C14 0.055(8) 0.086(11) 0.081(9) -0.003(8) 0.015(8) -0.002(8) C15 0.046(8) 0.116(13) 0.112(12) -0.041(11) 0.000(8) -0.013(8) N2 0.131(7) 0.117(6) 0.118(5) -0.014(5) -0.045(5) 0.037(5) C16 0.131(7) 0.117(6) 0.118(5) -0.014(5) -0.045(5) 0.037(5) C17 0.131(7) 0.117(6) 0.118(5) -0.014(5) -0.045(5) 0.037(5) C18 0.131(7) 0.117(6) 0.118(5) -0.014(5) -0.045(5) 0.037(5) C19 0.131(7) 0.117(6) 0.118(5) -0.014(5) -0.045(5) 0.037(5) C20 0.131(7) 0.117(6) 0.118(5) -0.014(5) -0.045(5) 0.037(5) C21 0.053(10) 0.067(10) 0.099(11) 0.011(9) -0.016(8) 0.015(8) C22 0.065(10) 0.044(8) 0.082(9) -0.002(7) -0.020(8) 0.014(8) C23 0.078(10) 0.041(8) 0.055(8) -0.002(7) 0.011(8) -0.009(8) C24 0.074(10) 0.048(9) 0.071(9) -0.006(8) -0.003(8) 0.014(8) C25 0.041(8) 0.070(10) 0.078(9) -0.009(8) 0.001(8) 0.013(7) C26 0.059(10) 0.096(13) 0.080(10) -0.009(10) -0.003(8) -0.022(9) C27 0.088(12) 0.114(15) 0.138(15) 0.015(12) -0.011(12) 0.004(11) C28 0.078(10) 0.077(11) 0.099(11) 0.039(9) 0.012(9) 0.013(9) C29 0.106(13) 0.071(11) 0.092(10) 0.015(9) -0.001(10) 0.012(10) C30 0.111(13) 0.074(11) 0.119(12) 0.049(10) -0.002(11) -0.011(10) N3 0.087(8) 0.058(7) 0.092(9) 0.021(8) -0.048(8) -0.012(7) C31 0.087(11) 0.086(13) 0.066(9) 0.007(9) -0.026(9) -0.004(10) C32 0.100(11) 0.059(11) 0.061(9) 0.014(8) -0.010(9) -0.001(9) C33 0.075(9) 0.077(11) 0.046(7) 0.015(8) -0.007(7) -0.001(9) C34 0.109(13) 0.070(12) 0.075(10) -0.008(9) 0.004(10) 0.018(10) C35 0.112(13) 0.077(13) 0.055(8) -0.013(8) -0.004(9) -0.001(10) C36 0.050(7) 0.057(9) 0.080(10) -0.013(8) 0.014(8) 0.004(7) C37 0.052(8) 0.068(11) 0.053(8) 0.011(7) -0.009(7) 0.002(7) C38 0.053(8) 0.063(11) 0.048(8) 0.018(7) 0.000(6) 0.021(7) C39 0.050(7) 0.065(9) 0.047(8) -0.009(7) -0.003(6) -0.001(7) C40 0.062(8) 0.038(9) 0.062(9) 0.007(7) 0.004(7) 0.004(7) C41 0.042(7) 0.095(13) 0.056(8) 0.002(8) -0.015(6) 0.003(8) C42 0.113(12) 0.078(10) 0.052(8) 0.025(7) -0.024(8) -0.011(9) C43 0.076(9) 0.081(10) 0.065(9) 0.011(8) -0.007(8) 0.006(8) C44 0.071(9) 0.097(12) 0.062(8) 0.009(8) 0.012(8) 0.023(8) C45 0.097(11) 0.076(10) 0.045(7) -0.020(7) -0.020(8) 0.004(9) N4 0.048(6) 0.072(9) 0.117(11) -0.007(7) 0.010(7) -0.008(6) C46 0.130(15) 0.143(18) 0.054(9) 0.004(11) -0.026(10) 0.011(13) C47 0.165(18) 0.080(13) 0.069(10) -0.020(10) -0.038(11) 0.039(12) C48 0.082(10) 0.106(14) 0.047(9) -0.014(9) 0.013(8) -0.027(10) C49 0.098(12) 0.074(11) 0.110(13) -0.013(11) 0.004(10) -0.029(10) C50 0.089(10) 0.059(10) 0.059(8) -0.026(8) 0.005(7) -0.018(9) C51 0.077(11) 0.081(11) 0.072(9) -0.003(8) 0.021(9) -0.012(9) C52 0.091(13) 0.099(13) 0.091(11) -0.039(11) -0.002(10) -0.026(11) C53 0.067(10) 0.074(11) 0.084(10) -0.032(9) -0.001(8) 0.001(8) C54 0.076(11) 0.069(10) 0.065(8) -0.022(8) -0.001(9) 0.006(8) C55 0.097(13) 0.089(12) 0.052(8) -0.001(8) 0.021(9) -0.014(10) C56 0.063(10) 0.069(10) 0.070(9) -0.011(8) 0.023(8) -0.016(8) C57 0.080(10) 0.100(13) 0.065(8) -0.030(8) 0.003(8) -0.004(9) C58 0.077(10) 0.095(12) 0.085(10) -0.036(9) -0.006(9) 0.013(9) C59 0.068(10) 0.110(14) 0.121(13) -0.052(11) -0.004(10) 0.014(10) C60 0.066(10) 0.150(18) 0.169(17) -0.105(16) 0.010(12) -0.004(11) N5 0.163(13) 0.076(10) 0.097(11) -0.020(8) 0.030(10) -0.005(10) C61 0.071(10) 0.092(13) 0.126(15) -0.040(12) 0.004(11) -0.023(10) C62 0.068(9) 0.064(10) 0.076(9) -0.008(8) -0.004(9) -0.017(8) C63 0.093(12) 0.055(9) 0.087(11) -0.007(8) 0.025(10) -0.009(9) C64 0.165(19) 0.135(17) 0.054(10) 0.007(10) 0.011(12) -0.003(15) C65 0.157(16) 0.151(19) 0.062(10) 0.005(12) 0.010(12) -0.003(15) C66 0.057(9) 0.095(14) 0.071(9) -0.007(9) 0.004(8) 0.009(10) C67 0.106(13) 0.068(12) 0.061(9) -0.021(9) -0.026(10) 0.011(11) C68 0.073(9) 0.059(10) 0.044(7) 0.009(7) 0.005(8) -0.002(8) C69 0.082(10) 0.063(11) 0.051(8) 0.003(7) -0.008(8) 0.015(9) C70 0.059(8) 0.051(9) 0.087(9) -0.009(8) 0.047(8) -0.003(7) C71 0.102(13) 0.079(12) 0.066(9) 0.004(8) -0.022(10) 0.003(11) C72 0.081(10) 0.059(10) 0.135(13) 0.007(10) 0.001(10) 0.002(9) C73 0.100(12) 0.082(12) 0.125(13) 0.000(10) -0.014(12) -0.005(10) C74 0.094(10) 0.079(12) 0.052(8) 0.001(8) 0.003(8) 0.005(9) C75 0.067(9) 0.061(10) 0.096(10) 0.000(8) 0.013(8) 0.010(8) N6 0.087(4) 0.096(5) 0.078(4) 0.006(3) 0.003(3) -0.013(4) C76 0.087(4) 0.096(5) 0.078(4) 0.006(3) 0.003(3) -0.013(4) C77 0.087(4) 0.096(5) 0.078(4) 0.006(3) 0.003(3) -0.013(4) C78 0.087(4) 0.096(5) 0.078(4) 0.006(3) 0.003(3) -0.013(4) C79 0.087(4) 0.096(5) 0.078(4) 0.006(3) 0.003(3) -0.013(4) C80 0.087(4) 0.096(5) 0.078(4) 0.006(3) 0.003(3) -0.013(4) C81 0.079(9) 0.065(10) 0.037(7) -0.010(7) -0.002(7) -0.001(8) C82 0.101(11) 0.063(11) 0.062(10) 0.005(8) 0.032(9) 0.003(10) C83 0.082(10) 0.074(11) 0.049(8) 0.012(8) -0.012(8) 0.000(9) C84 0.087(10) 0.076(11) 0.040(8) -0.002(8) 0.014(8) 0.021(9) C85 0.088(9) 0.079(11) 0.038(8) -0.011(8) 0.020(8) 0.014(9) C86 0.080(9) 0.068(10) 0.047(8) -0.002(8) 0.009(8) -0.009(8) C87 0.115(13) 0.102(14) 0.096(11) -0.027(10) -0.039(11) 0.000(11) C88 0.145(15) 0.064(10) 0.056(8) 0.011(8) -0.010(9) -0.010(10) C89 0.116(13) 0.090(11) 0.057(8) -0.009(8) 0.008(9) -0.019(10) C90 0.173(18) 0.077(11) 0.064(9) 0.006(9) -0.010(11) 0.018(12) N7 0.111(9) 0.063(9) 0.120(11) -0.001(8) 0.044(10) -0.031(8) C91 0.078(10) 0.064(10) 0.128(14) -0.002(10) -0.010(12) -0.005(9) C92 0.063(10) 0.071(10) 0.078(9) -0.030(8) 0.008(9) -0.005(8) C93 0.092(12) 0.042(8) 0.068(10) 0.006(7) 0.007(9) -0.020(8) C94 0.076(10) 0.059(10) 0.100(11) -0.027(8) 0.019(10) 0.017(8) C95 0.141(12) 0.109(16) 0.125(15) -0.043(13) 0.005(14) -0.010(14) C96 0.066(9) 0.047(9) 0.070(8) -0.007(8) 0.013(8) 0.001(8) C97 0.105(12) 0.032(8) 0.083(10) 0.007(8) 0.008(10) 0.013(9) C98 0.081(10) 0.064(11) 0.083(10) 0.001(9) 0.014(9) -0.006(9) C99 0.080(10) 0.051(10) 0.071(9) 0.011(8) 0.001(8) 0.005(8) C100 0.063(8) 0.037(8) 0.056(7) 0.003(7) 0.006(7) -0.011(7) C101 0.053(8) 0.065(10) 0.056(8) -0.004(7) 0.002(7) -0.002(7) C102 0.084(10) 0.067(10) 0.091(10) 0.013(8) 0.046(9) 0.015(9) C103 0.059(8) 0.111(14) 0.064(8) -0.007(9) 0.023(7) 0.015(9) C104 0.101(11) 0.049(9) 0.104(11) -0.001(8) 0.056(10) 0.000(9) C105 0.099(11) 0.050(10) 0.125(12) -0.009(9) 0.003(10) -0.004(9) N8 0.059(7) 0.062(7) 0.076(7) -0.003(6) 0.025(6) 0.010(6) C106 0.082(11) 0.069(11) 0.078(9) 0.008(8) -0.017(9) 0.017(9) C107 0.076(9) 0.080(11) 0.047(7) 0.006(7) 0.023(7) 0.004(9) C108 0.109(13) 0.047(10) 0.081(10) -0.018(8) 0.010(10) 0.021(9) C109 0.075(10) 0.080(12) 0.080(10) 0.006(8) 0.025(9) 0.027(9) C110 0.089(11) 0.076(12) 0.103(11) -0.017(10) 0.034(10) 0.005(11) C111 0.111(13) 0.093(14) 0.077(11) 0.005(11) 0.048(11) 0.001(11) C112 0.074(9) 0.074(11) 0.045(8) 0.015(8) -0.009(7) -0.008(8) C113 0.058(8) 0.064(10) 0.055(9) 0.003(7) 0.016(8) 0.004(8) C114 0.068(9) 0.086(12) 0.051(9) 0.014(8) 0.019(8) 0.018(8) C115 0.091(10) 0.068(11) 0.052(8) -0.010(8) 0.032(8) 0.006(9) C116 0.089(10) 0.089(12) 0.037(7) 0.000(7) -0.016(8) 0.056(9) C117 0.102(11) 0.074(10) 0.047(8) -0.004(7) -0.007(8) -0.011(9) C118 0.126(14) 0.082(12) 0.080(10) -0.010(9) 0.011(10) 0.023(11) C119 0.089(10) 0.065(10) 0.084(10) -0.006(8) 0.009(9) -0.002(8) C120 0.093(11) 0.087(12) 0.072(9) -0.001(9) 0.003(8) -0.016(9) N9 0.069(7) 0.061(9) 0.134(13) 0.024(8) -0.004(8) 0.006(7) C121 0.22(2) 0.107(15) 0.051(10) -0.012(11) -0.048(13) -0.046(16) C122 0.143(15) 0.090(14) 0.055(9) 0.012(9) 0.000(9) -0.028(11) C123 0.091(11) 0.066(12) 0.100(13) 0.020(10) -0.005(10) -0.016(9) C124 0.167(18) 0.054(10) 0.085(11) 0.020(10) 0.011(12) 0.012(11) C125 0.101(12) 0.085(13) 0.082(10) 0.000(10) 0.026(9) 0.004(10) C126 0.071(10) 0.053(9) 0.082(9) 0.010(8) 0.009(9) -0.006(8) C127 0.074(11) 0.073(11) 0.101(11) 0.031(10) 0.004(9) 0.007(9) C128 0.085(11) 0.101(12) 0.057(8) 0.023(9) -0.011(9) -0.018(10) C129 0.087(12) 0.056(9) 0.068(9) 0.011(7) 0.016(9) 0.022(8) C130 0.064(10) 0.083(11) 0.065(9) 0.012(8) 0.024(8) 0.008(8) C131 0.071(10) 0.062(10) 0.074(9) -0.006(8) 0.010(9) 0.011(8) C132 0.057(8) 0.080(11) 0.086(9) 0.031(8) -0.005(8) -0.007(7) C133 0.054(9) 0.117(13) 0.100(11) 0.050(10) 0.011(8) 0.021(9) C134 0.077(12) 0.154(18) 0.119(14) 0.033(13) 0.018(10) 0.049(12) C135 0.092(12) 0.165(19) 0.102(12) 0.070(13) 0.002(10) 0.047(13) S1 0.095(3) 0.128(4) 0.091(3) -0.012(3) -0.004(3) -0.001(3) O1 0.138(10) 0.082(8) 0.124(9) 0.030(7) -0.021(8) -0.002(8) O2 0.120(9) 0.071(7) 0.194(13) -0.016(8) 0.004(9) -0.005(7) O3 0.122(11) 0.133(11) 0.125(9) -0.018(8) 0.001(8) 0.005(8) C136 0.17(2) 0.120(13) 0.079(12) 0.005(12) 0.011(12) 0.051(14) F1 0.165(11) 0.126(9) 0.188(11) -0.062(9) -0.005(10) -0.011(9) F2 0.205(14) 0.157(11) 0.118(8) 0.006(8) 0.056(9) 0.043(10) F3 0.29(2) 0.203(15) 0.087(7) 0.018(8) -0.069(10) 0.015(13) S3 0.128(4) 0.115(4) 0.083(3) 0.020(3) -0.003(3) 0.012(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 N4 2.201(7) . ? Ag1 N6 2.250(7) 3_456 ? Ag1 N1 2.272(9) . ? Ag2 N3 2.246(7) 2_564 ? Ag2 N5 2.271(8) . ? Ag2 N7 2.280(7) . ? Ag3 N9 2.246(7) 3_745 ? Ag3 N8 2.269(6) . ? Ag3 N2 2.303(7) 3_746 ? Ag3 O3 2.598(15) . ? B1 C24 1.53(2) . ? B1 C39 1.58(2) . ? B1 C9 1.60(2) . ? B2 C84 1.57(2) . ? B2 C69 1.58(2) . ? B2 C54 1.62(2) . ? B3 C114 1.57(2) . ? B3 C129 1.59(2) . ? B3 C99 1.62(2) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C6 1.494(19) . ? C4 C5 1.3900 . ? C6 C7 1.40(2) . ? C6 C11 1.41(2) . ? C7 C8 1.39(2) . ? C7 C15 1.54(2) . ? C8 C9 1.46(2) . ? C8 C14 1.56(2) . ? C9 C10 1.365(18) . ? C10 C11 1.38(2) . ? C10 C13 1.54(2) . ? C11 C12 1.57(2) . ? N2 C16 1.3900 . ? N2 C20 1.3900 . ? N2 Ag3 2.303(7) 3_756 ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C18 C21 1.489(15) . ? C19 C20 1.3900 . ? C21 C22 1.35(2) . ? C21 C26 1.38(2) . ? C22 C23 1.388(19) . ? C22 C30 1.59(2) . ? C23 C24 1.421(19) . ? C23 C29 1.545(15) . ? C24 C25 1.42(2) . ? C25 C26 1.44(2) . ? C25 C28 1.480(19) . ? C26 C27 1.55(2) . ? N3 C31 1.3900 . ? N3 C35 1.3900 . ? N3 Ag2 2.246(7) 2_565 ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C33 C36 1.501(15) . ? C34 C35 1.3900 . ? C36 C37 1.394(18) . ? C36 C41 1.426(19) . ? C37 C38 1.368(18) . ? C37 C45 1.570(19) . ? C38 C39 1.386(18) . ? C38 C44 1.583(18) . ? C39 C40 1.449(17) . ? C40 C41 1.376(18) . ? C40 C43 1.524(19) . ? C41 C42 1.545(19) . ? N4 C46 1.3900 . ? N4 C50 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C48 C51 1.554(17) . ? C49 C50 1.3900 . ? C51 C52 1.34(2) . ? C51 C56 1.45(2) . ? C52 C53 1.44(2) . ? C52 C60 1.49(2) . ? C53 C54 1.42(2) . ? C53 C59 1.52(2) . ? C54 C55 1.38(2) . ? C55 C56 1.42(2) . ? C55 C58 1.55(2) . ? C56 C57 1.47(2) . ? N5 C61 1.3900 . ? N5 C65 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C63 C66 1.499(18) . ? C64 C65 1.3900 . ? C66 C67 1.41(2) . ? C66 C71 1.42(2) . ? C67 C68 1.37(2) . ? C67 C75 1.51(2) . ? C68 C69 1.418(19) . ? C68 C74 1.50(2) . ? C69 C70 1.387(19) . ? C70 C71 1.39(2) . ? C70 C73 1.55(2) . ? C71 C72 1.54(2) . ? N6 C76 1.3900 . ? N6 C80 1.3900 . ? N6 Ag1 2.250(7) 3_446 ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C78 C79 1.3900 . ? C78 C81 1.503(15) . ? C79 C80 1.3900 . ? C81 C86 1.350(19) . ? C81 C82 1.48(2) . ? C82 C83 1.36(2) . ? C82 C90 1.549(15) . ? C83 C84 1.39(2) . ? C83 C89 1.555(15) . ? C84 C85 1.45(2) . ? C85 C86 1.365(19) . ? C85 C88 1.563(15) . ? C86 C87 1.53(2) . ? N7 C91 1.3900 . ? N7 C95 1.3900 . ? C91 C92 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C93 C96 1.459(15) . ? C94 C95 1.3900 . ? C96 C97 1.39(2) . ? C96 C101 1.420(18) . ? C97 C98 1.41(2) . ? C97 C105 1.56(2) . ? C98 C99 1.40(2) . ? C98 C104 1.544(15) . ? C99 C100 1.45(2) . ? C100 C101 1.383(18) . ? C100 C103 1.461(19) . ? C101 C102 1.48(2) . ? N8 C106 1.3900 . ? N8 C110 1.3900 . ? C106 C107 1.3900 . ? C107 C108 1.3900 . ? C108 C109 1.3900 . ? C108 C111 1.531(19) . ? C109 C110 1.3900 . ? C111 C116 1.36(2) . ? C111 C112 1.43(2) . ? C112 C113 1.418(19) . ? C112 C119 1.547(15) . ? C113 C114 1.376(19) . ? C113 C120 1.54(2) . ? C114 C115 1.41(2) . ? C115 C116 1.344(18) . ? C115 C117 1.55(2) . ? C116 C118 1.547(15) . ? N9 C121 1.3900 . ? N9 C125 1.3900 . ? N9 Ag3 2.246(7) 3_755 ? C121 C122 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C123 C126 1.496(15) . ? C124 C125 1.3900 . ? C126 C131 1.41(2) . ? C126 C127 1.43(2) . ? C127 C128 1.40(2) . ? C127 C135 1.50(2) . ? C128 C129 1.44(2) . ? C128 C134 1.56(2) . ? C129 C130 1.34(2) . ? C130 C131 1.397(19) . ? C130 C133 1.557(15) . ? C131 C132 1.544(15) . ? S1 O3 1.426(13) . ? S1 O1 1.461(11) . ? S1 O2 1.503(12) . ? S1 C136 1.766(16) . ? C136 F3 1.28(2) . ? C136 F1 1.35(3) . ? C136 F2 1.37(3) . ? S3 O8 1.420(14) . ? S3 O9 1.443(14) . ? S3 O7 1.483(17) . ? S3 C138 1.714(18) . ? C138 F7 1.367(18) . ? C138 F8 1.372(18) . ? C138 F9 1.396(18) . ? S2 O6 1.490(16) . ? S2 O4 1.524(16) . ? S2 O5 1.525(16) . ? S2 C137 1.760(15) . ? C137 F5 1.331(19) . ? C137 F4 1.345(19) . ? C137 F6 1.357(19) . ? N10 C139 1.290(19) . ? N10A C140 1.28(2) . ? C139 C140 1.60(2) . ? N11 C141 1.305(18) . ? C141 C142 1.629(19) . ? N12 C143 1.238(19) . ? C143 C144 1.549(19) . ? N13 C145 1.218(17) . ? C145 C146 1.548(19) . ? N14 C147 1.250(19) . ? C147 C148 1.56(2) . ? N15 C149 1.243(17) . ? C149 C150 1.593(19) . ? N16 C151 1.27(2) . ? C151 C152 1.54(2) . ? N17 C153 1.266(18) . ? N17A C154 1.298(17) . ? C153 C154 1.522(19) . ? N18 C155 1.293(19) . ? C155 C156 1.626(19) . ? O13 O13A 0.92(3) . ? 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 N4 Ag1 N6 121.5(4) . 3_456 ? N4 Ag1 N1 122.6(4) . . ? N6 Ag1 N1 106.7(4) 3_456 . ? N3 Ag2 N5 119.6(4) 2_564 . ? N3 Ag2 N7 126.3(3) 2_564 . ? N5 Ag2 N7 113.6(4) . . ? N9 Ag3 N8 126.0(4) 3_745 . ? N9 Ag3 N2 111.9(4) 3_745 3_746 ? N8 Ag3 N2 101.7(4) . 3_746 ? N9 Ag3 O3 94.9(4) 3_745 . ? N8 Ag3 O3 130.1(4) . . ? N2 Ag3 O3 84.9(4) 3_746 . ? C24 B1 C39 123.5(13) . . ? C24 B1 C9 117.3(13) . . ? C39 B1 C9 119.0(12) . . ? C84 B2 C69 124.9(12) . . ? C84 B2 C54 119.6(14) . . ? C69 B2 C54 115.4(14) . . ? C114 B3 C129 121.0(11) . . ? C114 B3 C99 119.1(11) . . ? C129 B3 C99 119.9(11) . . ? C1 N1 C5 120.0 . . ? C1 N1 Ag1 121.9(7) . . ? C5 N1 Ag1 117.0(7) . . ? N1 C1 C2 120.0 . . ? C3 C2 C1 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 C6 120.0(10) . . ? C2 C3 C6 120.0(10) . . ? C3 C4 C5 120.0 . . ? C4 C5 N1 120.0 . . ? C7 C6 C11 121.1(15) . . ? C7 C6 C3 119.7(15) . . ? C11 C6 C3 118.7(13) . . ? C8 C7 C6 118.4(14) . . ? C8 C7 C15 120.8(14) . . ? C6 C7 C15 120.7(14) . . ? C7 C8 C9 119.9(13) . . ? C7 C8 C14 120.3(13) . . ? C9 C8 C14 119.8(11) . . ? C10 C9 C8 119.4(12) . . ? C10 C9 B1 120.8(12) . . ? C8 C9 B1 119.4(11) . . ? C9 C10 C11 121.1(13) . . ? C9 C10 C13 119.4(12) . . ? C11 C10 C13 119.4(12) . . ? C10 C11 C6 119.9(13) . . ? C10 C11 C12 122.9(13) . . ? C6 C11 C12 117.1(13) . . ? C16 N2 C20 120.0 . . ? C16 N2 Ag3 114.7(5) . 3_756 ? C20 N2 Ag3 125.2(5) . 3_756 ? C17 C16 N2 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 C21 116.0(9) . . ? C19 C18 C21 124.0(9) . . ? C18 C19 C20 120.0 . . ? C19 C20 N2 120.0 . . ? C22 C21 C26 121.3(13) . . ? C22 C21 C18 119.2(14) . . ? C26 C21 C18 119.5(15) . . ? C21 C22 C23 121.5(12) . . ? C21 C22 C30 116.5(13) . . ? C23 C22 C30 122.0(13) . . ? C22 C23 C24 120.2(12) . . ? C22 C23 C29 122.6(12) . . ? C24 C23 C29 117.1(12) . . ? C25 C24 C23 118.1(12) . . ? C25 C24 B1 118.1(12) . . ? C23 C24 B1 123.7(13) . . ? C24 C25 C26 119.5(13) . . ? C24 C25 C28 119.6(12) . . ? C26 C25 C28 120.8(12) . . ? C21 C26 C25 119.0(13) . . ? C21 C26 C27 117.5(15) . . ? C25 C26 C27 123.5(15) . . ? C31 N3 C35 120.0 . . ? C31 N3 Ag2 118.9(7) . 2_565 ? C35 N3 Ag2 121.0(7) . 2_565 ? C32 C31 N3 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 C36 117.8(9) . . ? C32 C33 C36 122.2(9) . . ? C33 C34 C35 120.0 . . ? C34 C35 N3 120.0 . . ? C37 C36 C41 119.5(13) . . ? C37 C36 C33 121.1(12) . . ? C41 C36 C33 119.3(12) . . ? C38 C37 C36 119.9(12) . . ? C38 C37 C45 123.3(12) . . ? C36 C37 C45 116.4(12) . . ? C37 C38 C39 122.9(11) . . ? C37 C38 C44 120.2(12) . . ? C39 C38 C44 116.9(12) . . ? C38 C39 C40 117.3(11) . . ? C38 C39 B1 123.1(12) . . ? C40 C39 B1 119.2(11) . . ? C41 C40 C39 120.3(11) . . ? C41 C40 C43 117.8(11) . . ? C39 C40 C43 122.0(11) . . ? C40 C41 C36 119.7(12) . . ? C40 C41 C42 120.6(12) . . ? C36 C41 C42 119.6(14) . . ? C46 N4 C50 120.0 . . ? C46 N4 Ag1 121.7(5) . . ? C50 N4 Ag1 117.8(5) . . ? C47 C46 N4 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C49 C48 C51 119.9(9) . . ? C47 C48 C51 120.1(9) . . ? C50 C49 C48 120.0 . . ? C49 C50 N4 120.0 . . ? C52 C51 C56 124.4(14) . . ? C52 C51 C48 118.8(14) . . ? C56 C51 C48 116.7(13) . . ? C51 C52 C53 119.1(15) . . ? C51 C52 C60 122.8(14) . . ? C53 C52 C60 118.1(15) . . ? C54 C53 C52 118.8(14) . . ? C54 C53 C59 123.9(12) . . ? C52 C53 C59 117.4(14) . . ? C55 C54 C53 120.0(12) . . ? C55 C54 B2 119.9(13) . . ? C53 C54 B2 119.4(13) . . ? C54 C55 C56 122.9(14) . . ? C54 C55 C58 123.7(13) . . ? C56 C55 C58 112.8(14) . . ? C55 C56 C51 114.6(14) . . ? C55 C56 C57 124.6(13) . . ? C51 C56 C57 120.8(13) . . ? C61 N5 C65 120.0 . . ? C61 N5 Ag2 116.7(7) . . ? C65 N5 Ag2 123.0(8) . . ? C62 C61 N5 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 C66 118.7(10) . . ? C62 C63 C66 121.1(9) . . ? C63 C64 C65 120.0 . . ? C64 C65 N5 120.0 . . ? C67 C66 C71 118.7(15) . . ? C67 C66 C63 122.6(14) . . ? C71 C66 C63 118.7(15) . . ? C68 C67 C66 120.7(15) . . ? C68 C67 C75 123.1(15) . . ? C66 C67 C75 116.0(16) . . ? C67 C68 C69 120.3(13) . . ? C67 C68 C74 117.3(14) . . ? C69 C68 C74 122.2(13) . . ? C70 C69 C68 119.4(13) . . ? C70 C69 B2 120.5(12) . . ? C68 C69 B2 120.1(12) . . ? C71 C70 C69 120.6(13) . . ? C71 C70 C73 117.5(14) . . ? C69 C70 C73 121.8(12) . . ? C70 C71 C66 120.2(14) . . ? C70 C71 C72 117.8(15) . . ? C66 C71 C72 122.0(16) . . ? C76 N6 C80 120.0 . . ? C76 N6 Ag1 118.3(5) . 3_446 ? C80 N6 Ag1 121.6(5) . 3_446 ? N6 C76 C77 120.0 . . ? C78 C77 C76 120.0 . . ? C77 C78 C79 120.0 . . ? C77 C78 C81 119.7(8) . . ? C79 C78 C81 120.3(8) . . ? C80 C79 C78 120.0 . . ? C79 C80 N6 120.0 . . ? C86 C81 C82 119.8(12) . . ? C86 C81 C78 122.9(12) . . ? C82 C81 C78 117.3(12) . . ? C83 C82 C81 119.2(11) . . ? C83 C82 C90 123.2(14) . . ? C81 C82 C90 117.6(14) . . ? C82 C83 C84 121.6(12) . . ? C82 C83 C89 118.6(13) . . ? C84 C83 C89 119.8(14) . . ? C83 C84 C85 117.5(13) . . ? C83 C84 B2 120.2(13) . . ? C85 C84 B2 122.1(13) . . ? C86 C85 C84 121.4(12) . . ? C86 C85 C88 120.4(13) . . ? C84 C85 C88 117.7(13) . . ? C81 C86 C85 120.3(13) . . ? C81 C86 C87 118.9(13) . . ? C85 C86 C87 120.7(14) . . ? C91 N7 C95 120.0 . . ? C91 N7 Ag2 118.7(7) . . ? C95 N7 Ag2 121.0(7) . . ? C92 C91 N7 120.0 . . ? C91 C92 C93 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 C96 118.7(9) . . ? C92 C93 C96 121.2(9) . . ? C93 C94 C95 120.0 . . ? C94 C95 N7 120.0 . . ? C97 C96 C101 119.4(12) . . ? C97 C96 C93 120.1(12) . . ? C101 C96 C93 120.3(12) . . ? C96 C97 C98 121.8(13) . . ? C96 C97 C105 116.2(13) . . ? C98 C97 C105 121.9(15) . . ? C99 C98 C97 119.5(13) . . ? C99 C98 C104 119.1(13) . . ? C97 C98 C104 121.4(13) . . ? C98 C99 C100 118.2(12) . . ? C98 C99 B3 119.2(13) . . ? C100 C99 B3 122.6(12) . . ? C101 C100 C99 121.8(12) . . ? C101 C100 C103 120.2(12) . . ? C99 C100 C103 118.0(12) . . ? C100 C101 C96 118.9(12) . . ? C100 C101 C102 121.0(13) . . ? C96 C101 C102 119.8(12) . . ? C106 N8 C110 120.0 . . ? C106 N8 Ag3 123.5(5) . . ? C110 N8 Ag3 116.5(5) . . ? N8 C106 C107 120.0 . . ? C106 C107 C108 120.0 . . ? C109 C108 C107 120.0 . . ? C109 C108 C111 118.6(8) . . ? C107 C108 C111 121.4(8) . . ? C110 C109 C108 120.0 . . ? C109 C110 N8 120.0 . . ? C116 C111 C112 121.2(15) . . ? C116 C111 C108 122.8(15) . . ? C112 C111 C108 116.0(15) . . ? C113 C112 C111 118.1(12) . . ? C113 C112 C119 123.0(13) . . ? C111 C112 C119 118.9(14) . . ? C114 C113 C112 119.6(13) . . ? C114 C113 C120 118.9(13) . . ? C112 C113 C120 121.3(12) . . ? C113 C114 C115 119.2(13) . . ? C113 C114 B3 119.5(14) . . ? C115 C114 B3 121.2(13) . . ? C116 C115 C114 122.2(14) . . ? C116 C115 C117 120.9(12) . . ? C114 C115 C117 116.8(13) . . ? C115 C116 C111 119.7(14) . . ? C115 C116 C118 121.4(12) . . ? C111 C116 C118 119.0(14) . . ? C121 N9 C125 120.0 . . ? C121 N9 Ag3 120.2(6) . 3_755 ? C125 N9 Ag3 119.8(6) . 3_755 ? N9 C121 C122 120.0 . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? C124 C123 C126 123.0(10) . . ? C122 C123 C126 117.0(10) . . ? C123 C124 C125 120.0 . . ? C124 C125 N9 120.0 . . ? C131 C126 C127 118.3(12) . . ? C131 C126 C123 122.7(13) . . ? C127 C126 C123 119.0(13) . . ? C128 C127 C126 119.8(14) . . ? C128 C127 C135 119.2(15) . . ? C126 C127 C135 120.9(14) . . ? C127 C128 C129 120.3(14) . . ? C127 C128 C134 117.8(14) . . ? C129 C128 C134 121.8(13) . . ? C130 C129 C128 118.3(12) . . ? C130 C129 B3 121.7(13) . . ? C128 C129 B3 119.5(13) . . ? C129 C130 C131 123.3(12) . . ? C129 C130 C133 119.0(12) . . ? C131 C130 C133 117.7(12) . . ? C130 C131 C126 119.8(11) . . ? C130 C131 C132 125.3(13) . . ? C126 C131 C132 114.8(12) . . ? O3 S1 O1 116.9(9) . . ? O3 S1 O2 113.2(9) . . ? O1 S1 O2 113.9(8) . . ? O3 S1 C136 105.3(11) . . ? O1 S1 C136 103.7(9) . . ? O2 S1 C136 101.6(11) . . ? S1 O3 Ag3 109.4(8) . . ? F3 C136 F1 109(2) . . ? F3 C136 F2 107.4(18) . . ? F1 C136 F2 107.1(17) . . ? F3 C136 S1 114.9(15) . . ? F1 C136 S1 108.9(14) . . ? F2 C136 S1 108.8(17) . . ? O8 S3 O9 118.3(10) . . ? O8 S3 O7 104.1(13) . . ? O9 S3 O7 115.3(13) . . ? O8 S3 C138 106.9(12) . . ? O9 S3 C138 109.9(12) . . ? O7 S3 C138 100.4(14) . . ? F7 C138 F8 107(2) . . ? F7 C138 F9 105(2) . . ? F8 C138 F9 105(2) . . ? F7 C138 S3 117.9(19) . . ? F8 C138 S3 105.8(17) . . ? F9 C138 S3 114.5(18) . . ? O6 S2 O4 111.2(12) . . ? O6 S2 O5 108.4(12) . . ? O4 S2 O5 106.7(12) . . ? O6 S2 C137 111.0(12) . . ? O4 S2 C137 108.6(12) . . ? O5 S2 C137 110.9(12) . . ? F5 C137 F4 98.5(17) . . ? F5 C137 F6 98.1(16) . . ? F4 C137 F6 97.0(17) . . ? F5 C137 S2 120.0(18) . . ? F4 C137 S2 116.7(17) . . ? F6 C137 S2 121.7(18) . . ? N10 C139 C140 139(3) . . ? N10A C140 C139 138(4) . . ? N11 C141 C142 133(3) . . ? N12 C143 C144 146(3) . . ? N13 C145 C146 171(3) . . ? N14 C147 C148 171(4) . . ? N15 C149 C150 131(2) . . ? N16 C151 C152 123(3) . . ? N17 C153 C154 128(3) . . ? N17A C154 C153 136(2) . . ? N18 C155 C156 134(3) . . ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 50.32 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 0.901 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.122 # Attachment 'CIF-3.txt' _publ_section_exptl_refinement ; All aromatic groups were input as idealized planar rings with C-C bond lengths of 1.39 angstrom. Some C-C bonds from the aromatic rings to the methyl groups are somewhat short and so were constrained to be ca. 1.50 angstrom. The C-C and C-N bonds of the CH3CN guest molecules were constrained to be reasonably. One perchlorate anion was disordered around a 3-fold. All hydrogen atoms were generated geometrically (C-H = 0.93 or 0.96\%A for phenyl or methyl H atoms respectively) and were included in the refinement in the riding model approximation. The displacement parameters of methyl H atoms were set to 1.5 times U~eq~ of the equivalent isotropic displacement parameters of their parent atoms, while those of other H atoms were set to 1.2 times. All non-H atoms except for the disordered ones were refined anisotropically. ; #====================================================================== data_3_[AgL(ClO4)].3/2CH3CN _database_code_depnum_ccdc_archive 'CCDC 747396' #TrackingRef 'CIF-3.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52.50 Ag B Cl N4.50 O4' _chemical_formula_weight 910.58 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' Cl Cl 0.1484 0.1585 '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 Trigonal _symmetry_space_group_name_H-M R32 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 18.2533(14) _cell_length_b 18.2533(14) _cell_length_c 47.517(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13711(3) _cell_formula_units_Z 12 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7002 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5676 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28389 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_limit_l_max 61 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7002 _reflns_number_gt 4054 _reflns_threshold_expression >2sigma(I) __computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^)+(0.1275P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 7002 _refine_ls_number_parameters 312 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2194 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.060 _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 0.06574(4) -0.26759(4) -0.1667 0.1081(4) Uani 1 2 d S . . Ag2 Ag -1.0000 -1.0000 0.0000 0.0959(6) Uani 1 6 d S . . B1 B -0.3993(5) -0.3993(5) 0.0000 0.058(2) Uani 1 2 d S . . B2 B 0.6667 0.3333 -0.1667 0.041(3) Uani 1 6 d S . . N1 N -0.03276(19) -0.2863(2) -0.13390(7) 0.0729(14) Uani 1 1 d G . . C1 C -0.1144(2) -0.3546(2) -0.13649(7) 0.0727(16) Uani 1 1 d G . . H1A H -0.1296 -0.3887 -0.1524 0.087 Uiso 1 1 calc R . . C2 C -0.17323(16) -0.3721(2) -0.11526(8) 0.0645(15) Uani 1 1 d G . . H2A H -0.2278 -0.4178 -0.1170 0.077 Uiso 1 1 calc R . . C3 C -0.1505(2) -0.3212(2) -0.09142(7) 0.0556(13) Uani 1 1 d G . . C4 C -0.0689(2) -0.2528(2) -0.08883(7) 0.080(2) Uani 1 1 d G . . H4A H -0.0537 -0.2188 -0.0729 0.096 Uiso 1 1 calc R . . C5 C -0.01002(19) -0.2354(2) -0.11007(9) 0.091(2) Uani 1 1 d G . . H5A H 0.0446 -0.1897 -0.1083 0.110 Uiso 1 1 calc R . . C12 C -0.2205(5) -0.2098(5) -0.08191(17) 0.090(2) Uani 1 1 d . . . H12A H -0.2470 -0.1790 -0.0753 0.136 Uiso 1 1 calc R . . H12B H -0.2379 -0.2280 -0.1009 0.136 Uiso 1 1 calc R . . H12C H -0.1601 -0.1739 -0.0813 0.136 Uiso 1 1 calc R . . C6 C -0.2166(2) -0.3436(2) -0.06811(7) 0.0568(13) Uani 1 1 d G . . C7 C -0.2443(2) -0.4163(2) -0.05200(8) 0.0580(13) Uani 1 1 d G . . C8 C -0.3025(2) -0.43419(18) -0.03049(7) 0.0573(13) Uani 1 1 d G . . C9 C -0.3330(2) -0.3794(2) -0.02508(7) 0.0554(13) Uani 1 1 d G . . C10 C -0.3053(2) -0.3067(2) -0.04119(8) 0.0608(14) Uani 1 1 d G . . C11 C -0.2471(2) -0.28878(19) -0.06271(7) 0.0630(14) Uani 1 1 d G . . C13 C -0.3373(5) -0.2479(4) -0.03709(17) 0.084(2) Uani 1 1 d . . . H13A H -0.3766 -0.2669 -0.0217 0.125 Uiso 1 1 calc R . . H13B H -0.3653 -0.2457 -0.0539 0.125 Uiso 1 1 calc R . . H13C H -0.2909 -0.1924 -0.0330 0.125 Uiso 1 1 calc R . . C14 C -0.3302(5) -0.5151(4) -0.01399(15) 0.0789(19) Uani 1 1 d . . . H14A H -0.3701 -0.5207 0.0002 0.118 Uiso 1 1 calc R . . H14B H -0.2818 -0.5130 -0.0052 0.118 Uiso 1 1 calc R . . H14C H -0.3562 -0.5627 -0.0265 0.118 Uiso 1 1 calc R . . C15 C -0.2032(5) -0.4720(4) -0.05655(14) 0.0711(17) Uani 1 1 d . . . H15A H -0.1650 -0.4506 -0.0722 0.107 Uiso 1 1 calc R . . H15B H -0.2465 -0.5292 -0.0603 0.107 Uiso 1 1 calc R . . H15C H -0.1727 -0.4706 -0.0399 0.107 Uiso 1 1 calc R . . C16 C -0.8063(4) -0.8707(4) -0.01102(17) 0.0804(19) Uani 1 1 d D . . H16A H -0.8089 -0.9181 -0.0193 0.096 Uiso 1 1 calc R . . C17 C -0.7302(4) -0.7971(4) -0.01061(16) 0.080(2) Uani 1 1 d D . . H17A H -0.6824 -0.7968 -0.0176 0.096 Uiso 1 1 calc R . . C18 C -0.7230(4) -0.7230(4) 0.0000 0.059(2) Uani 1 2 d SD . . C19 C -0.6419(4) -0.6419(4) 0.0000 0.062(2) Uani 1 2 d SD . . C20 C -0.6186(4) -0.5883(4) -0.02348(12) 0.0634(14) Uani 1 1 d D . . C21 C -0.5418(4) -0.5127(4) -0.02406(11) 0.0626(14) Uani 1 1 d D . . C22 C -0.4882(4) -0.4882(4) 0.0000 0.064(2) Uani 1 2 d SD . . C23 C -0.5164(5) -0.4574(5) -0.04968(14) 0.085(2) Uani 1 1 d D . . H23A H -0.5590 -0.4839 -0.0639 0.128 Uiso 1 1 calc R . . H23B H -0.4635 -0.4494 -0.0567 0.128 Uiso 1 1 calc R . . H23C H -0.5103 -0.4036 -0.0448 0.128 Uiso 1 1 calc R . . C24 C -0.6797(5) -0.6157(5) -0.04843(15) 0.088(2) Uani 1 1 d D . . H24A H -0.6560 -0.5738 -0.0630 0.132 Uiso 1 1 calc R . . H24B H -0.7327 -0.6218 -0.0424 0.132 Uiso 1 1 calc R . . H24C H -0.6888 -0.6689 -0.0555 0.132 Uiso 1 1 calc R . . C25 C 0.1912(4) -0.0701(4) -0.16101(18) 0.089(2) Uani 1 1 d D . . H25A H 0.1406 -0.0709 -0.1576 0.106 Uiso 1 1 calc R . . C26 C 0.2658(4) 0.0060(4) -0.16019(17) 0.080(2) Uani 1 1 d D . . H26A H 0.2655 0.0553 -0.1554 0.096 Uiso 1 1 calc R . . C27 C 0.3423(4) 0.0090(4) -0.1667 0.061(2) Uani 1 2 d SD . . C28 C 0.4246(4) 0.0912(4) -0.1667 0.0523(18) Uani 1 2 d SD . . C29 C 0.4822(3) 0.1083(3) -0.14510(10) 0.0499(11) Uani 1 1 d D . . C30 C 0.5602(3) 0.1847(3) -0.14513(10) 0.0432(10) Uani 1 1 d D . . C31 C 0.5784(3) 0.2451(3) -0.1667 0.0449(16) Uani 1 2 d SD . . C32 C 0.6191(4) 0.2007(4) -0.12106(12) 0.0621(15) Uani 1 1 d . . . H32A H 0.5956 0.1522 -0.1089 0.093 Uiso 1 1 calc R . . H32B H 0.6267 0.2492 -0.1107 0.093 Uiso 1 1 calc R . . H32C H 0.6727 0.2112 -0.1281 0.093 Uiso 1 1 calc R . . C33 C 0.4606(4) 0.0476(4) -0.12104(15) 0.0715(17) Uani 1 1 d . . . H33A H 0.4058 -0.0009 -0.1241 0.107 Uiso 1 1 calc R . . H33B H 0.4602 0.0749 -0.1038 0.107 Uiso 1 1 calc R . . H33C H 0.5021 0.0301 -0.1198 0.107 Uiso 1 1 calc R . . N2 N -0.8784(4) -0.8784(4) 0.0000 0.074(2) Uani 1 2 d SD . . N3 N 0.1891(4) -0.1442(4) -0.1667 0.080(2) Uani 1 2 d SD . . Cl1 Cl -1.0000 -1.0000 -0.07641(18) 0.110(2) Uiso 0.50 3 d SPD . . O1 O -1.0000 -1.0000 -0.1068(3) 0.312 Uiso 1 3 d SD . . O2 O -0.970(4) -1.054(4) -0.0620(10) 0.388 Uiso 0.50 1 d PD . . Cl2 Cl -1.0000 -1.0000 -0.1368(3) 0.175(5) Uiso 0.50 3 d SPD . . O3 O -0.9159(19) -0.938(3) -0.1484(7) 0.404 Uiso 0.50 1 d PD . . N4 N -1.0208(11) -0.1930(10) -0.2075(3) 0.187(5) Uiso 1 1 d D . . C34 C -0.9543(17) -0.1315(17) -0.2148(6) 0.271(12) Uiso 1 1 d D . . C35 C -0.8733(17) -0.0775(18) -0.2304(6) 0.305(14) Uiso 1 1 d D . . H35A H -0.8453 -0.0215 -0.2225 0.458 Uiso 1 1 calc R . . H35B H -0.8854 -0.0746 -0.2499 0.458 Uiso 1 1 calc R . . H35C H -0.8373 -0.1016 -0.2287 0.458 Uiso 1 1 calc R . . Cl3 Cl -0.3333 -0.6667 -0.9551(3) 0.292(6) Uiso 1 3 d SD . . O4 O -0.294(2) -0.5864(15) -0.9401(4) 0.441 Uiso 1 1 d D . . O5 O -0.3333 -0.6667 -0.9855(4) 0.220 Uiso 1 3 d SD . . 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 0.0713(3) 0.0713(3) 0.1238(7) -0.0375(3) 0.0375(3) -0.0077(4) Ag2 0.0598(5) 0.0598(5) 0.1682(16) 0.000 0.000 0.0299(2) B1 0.049(3) 0.049(3) 0.068(6) -0.006(2) 0.006(2) 0.018(4) B2 0.038(4) 0.038(4) 0.047(7) 0.000 0.000 0.0192(19) N1 0.059(3) 0.060(3) 0.078(3) -0.002(3) 0.017(3) 0.013(2) C1 0.055(3) 0.079(4) 0.075(4) -0.014(3) 0.006(3) 0.026(3) C2 0.044(3) 0.065(4) 0.067(3) -0.005(3) 0.002(2) 0.014(3) C3 0.045(3) 0.056(3) 0.068(3) 0.001(3) 0.007(2) 0.027(2) C4 0.061(4) 0.068(4) 0.079(4) -0.017(3) 0.009(3) 0.007(3) C5 0.061(4) 0.075(5) 0.100(5) -0.015(4) 0.017(4) 0.005(3) C12 0.101(6) 0.082(5) 0.102(5) 0.026(4) 0.034(4) 0.056(5) C6 0.051(3) 0.052(3) 0.064(3) -0.006(3) -0.004(2) 0.023(3) C7 0.051(3) 0.050(3) 0.069(3) -0.010(3) 0.005(2) 0.023(2) C8 0.059(3) 0.043(3) 0.058(3) -0.006(2) 0.004(3) 0.017(2) C9 0.049(3) 0.044(3) 0.062(3) -0.004(2) 0.007(2) 0.016(2) C10 0.047(3) 0.052(3) 0.076(4) -0.006(3) 0.010(3) 0.019(3) C11 0.058(3) 0.052(3) 0.075(4) -0.002(3) 0.011(3) 0.025(3) C13 0.097(5) 0.061(4) 0.099(5) 0.013(4) 0.031(4) 0.044(4) C14 0.092(5) 0.064(4) 0.082(4) 0.000(3) 0.021(4) 0.040(4) C15 0.083(4) 0.062(4) 0.077(4) 0.001(3) 0.013(3) 0.042(4) C16 0.066(4) 0.059(4) 0.120(5) -0.016(4) 0.009(4) 0.034(3) C17 0.058(4) 0.064(4) 0.114(5) -0.010(4) 0.031(4) 0.028(3) C18 0.050(3) 0.050(3) 0.076(5) -0.0065(19) 0.0065(19) 0.025(4) C19 0.054(3) 0.054(3) 0.070(5) -0.009(2) 0.009(2) 0.021(4) C20 0.052(3) 0.060(3) 0.069(3) -0.013(3) -0.003(3) 0.021(3) C21 0.061(4) 0.067(4) 0.054(3) -0.002(3) 0.002(3) 0.028(3) C22 0.055(3) 0.055(3) 0.061(5) -0.010(2) 0.010(2) 0.013(4) C23 0.079(5) 0.074(4) 0.079(4) 0.004(3) 0.002(4) 0.021(4) C24 0.081(5) 0.078(5) 0.082(4) -0.001(4) -0.015(4) 0.023(4) C25 0.050(4) 0.064(4) 0.125(6) -0.021(4) 0.006(4) 0.008(3) C26 0.054(4) 0.057(4) 0.101(5) -0.016(3) 0.014(3) 0.008(3) C27 0.045(3) 0.045(3) 0.077(5) -0.003(2) 0.003(2) 0.010(3) C28 0.039(2) 0.039(2) 0.069(5) -0.0076(18) 0.0076(18) 0.011(3) C29 0.049(3) 0.039(2) 0.062(3) 0.007(2) 0.003(2) 0.022(2) C30 0.038(2) 0.034(2) 0.060(3) 0.003(2) 0.000(2) 0.0198(19) C31 0.035(3) 0.035(3) 0.068(4) 0.0019(15) -0.0019(15) 0.019(3) C32 0.054(3) 0.056(3) 0.067(3) 0.012(3) -0.011(3) 0.021(3) C33 0.063(4) 0.048(3) 0.085(4) 0.021(3) 0.014(3) 0.015(3) N2 0.049(3) 0.049(3) 0.111(6) -0.006(2) 0.006(2) 0.016(3) N3 0.054(3) 0.054(3) 0.094(5) -0.018(2) 0.018(2) -0.002(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 N3 2.252(7) . ? Ag1 N1 2.272(2) . ? Ag1 N1 2.272(2) 16_544 ? Ag2 N2 2.219(7) . ? Ag2 N2 2.219(7) 2_345 ? Ag2 N2 2.219(7) 3_435 ? B1 C9 1.605(6) 4 ? B1 C9 1.605(5) . ? B1 C22 1.624(12) . ? B2 C31 1.611(6) 2_655 ? B2 C31 1.611(6) . ? B2 C31 1.611(6) 3_665 ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C6 1.536(3) . ? C4 C5 1.3900 . ? C12 C11 1.564(7) . ? C6 C7 1.3900 . ? C6 C11 1.3900 . ? C7 C8 1.3900 . ? C7 C15 1.552(7) . ? C8 C9 1.3900 . ? C8 C14 1.518(7) . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C10 C13 1.470(7) . ? C16 N2 1.356(7) . ? C16 C17 1.368(8) . ? C17 C18 1.387(7) . ? C18 C17 1.387(7) 4 ? C18 C19 1.480(11) . ? C19 C20 1.403(7) 4 ? C19 C20 1.403(7) . ? C20 C21 1.391(7) . ? C20 C24 1.530(9) . ? C21 C22 1.423(6) . ? C21 C23 1.499(9) . ? C22 C21 1.423(6) 4 ? C25 N3 1.361(7) . ? C25 C26 1.376(7) . ? C26 C27 1.405(7) . ? C27 C26 1.405(7) 16_544 ? C27 C28 1.501(10) . ? C28 C29 1.387(6) 16_544 ? C28 C29 1.387(6) . ? C29 C30 1.410(6) . ? C29 C33 1.501(8) . ? C30 C31 1.416(5) . ? C30 C32 1.494(7) . ? C31 C30 1.416(5) 16_544 ? N2 C16 1.356(7) 4 ? N3 C25 1.361(7) 16_544 ? Cl1 O1 1.443(15) . ? Cl1 O2 1.51(2) 2_345 ? Cl1 O2 1.51(2) 3_435 ? Cl1 O2 1.51(2) . ? O1 Cl2 1.425(15) . ? Cl2 O3 1.485(19) . ? Cl2 O3 1.485(18) 3_435 ? Cl2 O3 1.485(18) 2_345 ? N4 C34 1.222(17) . ? C34 C35 1.499(18) . ? Cl3 O5 1.445(15) . ? Cl3 O4 1.456(15) 3_545 ? Cl3 O4 1.456(16) . ? Cl3 O4 1.456(16) 2_445 ? 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 N3 Ag1 N1 118.09(9) . . ? N3 Ag1 N1 118.09(9) . 16_544 ? N1 Ag1 N1 123.82(18) . 16_544 ? N2 Ag2 N2 120.0 . 2_345 ? N2 Ag2 N2 120.000(1) . 3_435 ? N2 Ag2 N2 120.000(1) 2_345 3_435 ? C9 B1 C9 121.4(7) 4 . ? C9 B1 C22 119.3(4) 4 . ? C9 B1 C22 119.3(3) . . ? C31 B2 C31 120.0 2_655 . ? C31 B2 C31 120.000(1) 2_655 3_665 ? C31 B2 C31 120.0 . 3_665 ? C1 N1 C5 120.0 . . ? C1 N1 Ag1 119.12(17) . . ? C5 N1 Ag1 120.57(17) . . ? C2 C1 N1 120.0 . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 C6 118.5(3) . . ? C4 C3 C6 121.5(3) . . ? C5 C4 C3 120.0 . . ? C4 C5 N1 120.0 . . ? C7 C6 C11 120.0 . . ? C7 C6 C3 120.9(3) . . ? C11 C6 C3 119.1(3) . . ? C6 C7 C8 120.0 . . ? C6 C7 C15 119.0(3) . . ? C8 C7 C15 120.7(3) . . ? C7 C8 C9 120.0 . . ? C7 C8 C14 116.9(3) . . ? C9 C8 C14 123.1(3) . . ? C10 C9 C8 120.0 . . ? C10 C9 B1 119.8(2) . . ? C8 C9 B1 120.2(2) . . ? C9 C10 C11 120.0 . . ? C9 C10 C13 122.5(3) . . ? C11 C10 C13 117.5(3) . . ? C10 C11 C6 120.0 . . ? C10 C11 C12 119.7(3) . . ? C6 C11 C12 120.2(3) . . ? N2 C16 C17 123.6(6) . . ? C16 C17 C18 121.1(6) . . ? C17 C18 C17 115.4(7) . 4 ? C17 C18 C19 122.3(4) . . ? C17 C18 C19 122.3(4) 4 . ? C20 C19 C20 119.9(7) 4 . ? C20 C19 C18 120.0(4) 4 . ? C20 C19 C18 120.0(4) . . ? C21 C20 C19 120.7(5) . . ? C21 C20 C24 121.2(5) . . ? C19 C20 C24 118.1(5) . . ? C20 C21 C22 119.3(5) . . ? C20 C21 C23 120.2(5) . . ? C22 C21 C23 120.5(5) . . ? C21 C22 C21 119.9(7) . 4 ? C21 C22 B1 120.0(4) . . ? C21 C22 B1 120.0(4) 4 . ? N3 C25 C26 122.1(7) . . ? C25 C26 C27 119.7(7) . . ? C26 C27 C26 117.8(7) 16_544 . ? C26 C27 C28 121.1(4) 16_544 . ? C26 C27 C28 121.1(4) . . ? C29 C28 C29 121.1(6) 16_544 . ? C29 C28 C27 119.4(3) 16_544 . ? C29 C28 C27 119.4(3) . . ? C28 C29 C30 120.0(5) . . ? C28 C29 C33 120.5(5) . . ? C30 C29 C33 119.5(5) . . ? C29 C30 C31 119.8(4) . . ? C29 C30 C32 117.7(4) . . ? C31 C30 C32 122.3(4) . . ? C30 C31 C30 119.2(6) 16_544 . ? C30 C31 B2 120.4(3) 16_544 . ? C30 C31 B2 120.4(3) . . ? C16 N2 C16 115.0(7) 4 . ? C16 N2 Ag2 122.5(4) 4 . ? C16 N2 Ag2 122.5(4) . . ? C25 N3 C25 118.6(7) . 16_544 ? C25 N3 Ag1 120.7(4) . . ? C25 N3 Ag1 120.7(4) 16_544 . ? O1 Cl1 O2 117(2) . 2_345 ? O1 Cl1 O2 117(2) . 3_435 ? O2 Cl1 O2 101(2) 2_345 3_435 ? O1 Cl1 O2 117(2) . . ? O2 Cl1 O2 101(2) 2_345 . ? O2 Cl1 O2 101(2) 3_435 . ? Cl2 O1 Cl1 180.000(2) . . ? O1 Cl2 O3 111.8(16) . . ? O1 Cl2 O3 111.8(16) . 3_435 ? O3 Cl2 O3 107.0(17) . 3_435 ? O1 Cl2 O3 111.8(16) . 2_345 ? O3 Cl2 O3 107.0(17) . 2_345 ? O3 Cl2 O3 107.0(17) 3_435 2_345 ? N4 C34 C35 161(3) . . ? O5 Cl3 O4 119.4(13) . 3_545 ? O5 Cl3 O4 119.4(13) . . ? O4 Cl3 O4 98.0(16) 3_545 . ? O5 Cl3 O4 119.4(13) . 2_445 ? O4 Cl3 O4 98.0(16) 3_545 2_445 ? O4 Cl3 O4 98.0(16) . 2_445 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.566 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.086