Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Jonathan Steed' ; ? # Address for author 1 ; ; ? #footnote for author 1 ; 'J. Howard' ; ? # Address 2 ; ; ? # footnote 2 ; 'Andrew D.M. Parker' '' '' 'Ivana Radosavlijevic-Evans' '' '' 'Jennifer M. Russell' '' '' _publ_contact_author_name 'Jonathan Steed' _publ_contact_author_address ; Department of Chemistry University of Durham University Science Laboratories South Road Durham DH1 3LE UNITED KINGDOM ; _publ_contact_author_email JON.STEED@DUR.AC.UK _publ_requested_journal 'Cryst Eng. Comm.' _publ_section_title ; Anion-binding mode: solid state symmetry breaking and solution chelation ; _journal_coden_ASTM ? _journal_coeditor_code ? _journal_coeditor_name ? _journal_coeditor_notes ; ? ; _journal_date_accepted ? _journal_date_from_coeditor ? _journal_date_printers_final ? _journal_date_printers_first ? _journal_date_proofs_in ? _journal_date_proofs_out ? #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_issue ? _journal_name_full ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_volume ? _journal_year ? _publ_contact_author_fax '01865 272 699' _publ_contact_author_phone '01865 270 826' # E:\Andrew\05ADP004\4Jen in Pbca # Check this file using the IUCr facility at: # http://www/iucr.ac.uk/iucr-top/journals/acta/c/services/checkcif.html #**************************************************************************** # The contents of this file between this point and the next ***** line # are held in the file REFCIF.DAT # This is a character file which you may edit to reflect local conditions # # Items which need looking at are represented by a '?' # Items for which there are choices are prefixed with 'choose from' # # 1. SUBMISSION DETAILS _publ_contact_letter ; ; _publ_requested_category CO # choose from: FI FM FO CI CM CO AD# _publ_requested_coeditor_name 'Prof William Clegg' # Attachment 'AGBF4REV2.CIF' data_AGBF4REV2.CIF _database_code_depnum_ccdc_archive 'CCDC 291485' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AgBF4rev2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 Ag B F4 N4 O2 S2' _chemical_formula_weight 711.34 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.309(3) _cell_length_b 16.716(3) _cell_length_c 18.722(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.812(3) _cell_angle_gamma 90.00 _cell_volume 5727.1(17) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7718 _exptl_absorpt_correction_T_max 0.9645 _exptl_absorpt_process_details ? _exptl_special_details ; The crystals were multiply twinned and gave a very poor diffraction pattern. The refinement gives chemical connectivity but precision is poor. Large residual peaks near the Ag ions are a result of overlap of reflections with those of twin components. Isotropic model adpoted except for Ag and S because of poor data quality. ; _diffrn_ambient_temperature 120(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 SMART' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32555 _diffrn_reflns_av_R_equivalents 0.1762 _diffrn_reflns_av_sigmaI/netI 0.1467 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 24.99 _reflns_number_total 9849 _reflns_number_gt 6288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed interface to POVRay' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.0903P)^2^+402.8168P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9849 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2219 _refine_ls_R_factor_gt 0.1685 _refine_ls_wR_factor_ref 0.3801 _refine_ls_wR_factor_gt 0.3604 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 0.18110(8) 0.16939(9) 0.25200(8) 0.0213(4) Uani 1 1 d . . . Ag2 Ag -0.31859(8) 0.17927(10) 0.23462(7) 0.0214(4) Uani 1 1 d . . . S1 S 0.1458(2) 0.1618(3) 0.3793(2) 0.0166(10) Uani 1 1 d . . . S2 S 0.1338(3) 0.1654(3) 0.1248(2) 0.0200(10) Uani 1 1 d . . . S3 S -0.3492(3) 0.1772(3) 0.3637(2) 0.0214(10) Uani 1 1 d . . . S4 S -0.3653(3) 0.1688(3) 0.1086(2) 0.0223(11) Uani 1 1 d . . . F1 F -0.0624(6) -0.0621(7) 0.3965(6) 0.024(2) Uiso 1 1 d . . . F2 F -0.0243(7) -0.1467(7) 0.3107(6) 0.030(3) Uiso 1 1 d . . . F3 F 0.0126(7) -0.0167(7) 0.3104(6) 0.030(3) Uiso 1 1 d . . . F4 F 0.0559(6) -0.1022(7) 0.3958(6) 0.023(2) Uiso 1 1 d . . . F5 F -0.5549(6) 0.3960(6) 0.3916(5) 0.021(2) Uiso 1 1 d . . . F6 F -0.5155(6) 0.4883(7) 0.3117(6) 0.026(3) Uiso 1 1 d . . . F7 F -0.4814(7) 0.3574(7) 0.3025(6) 0.030(3) Uiso 1 1 d . . . F8 F -0.4350(6) 0.4352(7) 0.3936(6) 0.022(2) Uiso 1 1 d . . . O1 O -0.2123(8) 0.2494(8) 0.2804(7) 0.024(3) Uiso 1 1 d . . . O2 O -0.2261(8) 0.0782(9) 0.2045(7) 0.025(3) Uiso 1 1 d . . . O3 O -0.7136(7) 0.0845(8) 0.2938(7) 0.020(3) Uiso 1 1 d . . . O4 O -0.7203(7) 0.2497(8) 0.2077(7) 0.021(3) Uiso 1 1 d . . . N1 N -0.0925(9) 0.2702(10) 0.2670(8) 0.021(4) Uiso 1 1 d . . . H1N H -0.0609 0.2953 0.2405 0.025 Uiso 1 1 calc R . . N2 N -0.1727(8) 0.3218(10) 0.1851(8) 0.018(3) Uiso 1 1 d . . . H2N H -0.1340 0.3356 0.1613 0.022 Uiso 1 1 calc R . . N3 N -0.1035(8) 0.0663(9) 0.2284(8) 0.016(3) Uiso 1 1 d . . . H3N H -0.0721 0.0433 0.2585 0.019 Uiso 1 1 calc R . . N4 N -0.1849(9) 0.0141(10) 0.3054(8) 0.018(3) Uiso 1 1 d . . . H4N H -0.1450 0.0018 0.3306 0.021 Uiso 1 1 calc R . . N5 N -0.5927(8) 0.0681(9) 0.2716(7) 0.011(3) Uiso 1 1 d . . . H5N H -0.5633 0.0443 0.2420 0.014 Uiso 1 1 calc R . . N6 N -0.6776(8) 0.0156(9) 0.1945(7) 0.013(3) Uiso 1 1 d . . . H6N H -0.6396 0.0023 0.1695 0.016 Uiso 1 1 calc R . . N7 N -0.5957(8) 0.2655(9) 0.2232(8) 0.015(3) Uiso 1 1 d . . . H7N H -0.5642 0.2909 0.2515 0.018 Uiso 1 1 calc R . . N8 N -0.6736(8) 0.3155(9) 0.3040(7) 0.011(3) Uiso 1 1 d . . . H8N H -0.6328 0.3288 0.3272 0.014 Uiso 1 1 calc R . . C1 C 0.1608(11) 0.0596(11) 0.4038(10) 0.019(4) Uiso 1 1 d . . . H1A H 0.1267 0.0253 0.3763 0.028 Uiso 1 1 calc R . . H1B H 0.1528 0.0529 0.4549 0.028 Uiso 1 1 calc R . . H1C H 0.2111 0.0445 0.3935 0.028 Uiso 1 1 calc R . . C2 C 0.0504(11) 0.1722(12) 0.3775(10) 0.022(4) Uiso 1 1 d . . . C3 C 0.0087(10) 0.1382(12) 0.4341(10) 0.018(4) Uiso 1 1 d . . . H3 H 0.0330 0.1111 0.4726 0.022 Uiso 1 1 calc R . . C4 C -0.0679(10) 0.1452(12) 0.4324(10) 0.020(4) Uiso 1 1 d . . . H4 H -0.0956 0.1192 0.4676 0.024 Uiso 1 1 calc R . . C5 C -0.1030(9) 0.1900(10) 0.3793(8) 0.010(3) Uiso 1 1 d . . . H5 H -0.1545 0.1969 0.3789 0.012 Uiso 1 1 calc R . . C6 C -0.0612(9) 0.2250(10) 0.3260(8) 0.010(3) Uiso 1 1 d . . . C7 C 0.0141(10) 0.2150(11) 0.3276(9) 0.014(4) Uiso 1 1 d . . . H7 H 0.0412 0.2399 0.2914 0.016 Uiso 1 1 calc R . . C8 C -0.1600(10) 0.2792(11) 0.2476(9) 0.014(4) Uiso 1 1 d . . . C9 C -0.2418(10) 0.3456(11) 0.1553(9) 0.017(4) Uiso 1 1 d . . . C10 C -0.3030(11) 0.3573(12) 0.1939(10) 0.021(4) Uiso 1 1 d . . . H10 H -0.3013 0.3490 0.2441 0.025 Uiso 1 1 calc R . . C11 C -0.3667(11) 0.3812(12) 0.1600(10) 0.021(4) Uiso 1 1 d . . . H11 H -0.4094 0.3876 0.1869 0.025 Uiso 1 1 calc R . . C12 C -0.3697(12) 0.3963(13) 0.0867(11) 0.027(5) Uiso 1 1 d . . . H12 H -0.4133 0.4149 0.0633 0.032 Uiso 1 1 calc R . . C13 C -0.3073(11) 0.3831(13) 0.0496(11) 0.025(5) Uiso 1 1 d . . . H13 H -0.3083 0.3937 -0.0002 0.030 Uiso 1 1 calc R . . C14 C -0.2429(12) 0.3551(14) 0.0814(11) 0.031(5) Uiso 1 1 d . . . H14 H -0.2014 0.3430 0.0541 0.037 Uiso 1 1 calc R . . C15 C 0.1540(13) 0.2613(14) 0.0875(12) 0.032(5) Uiso 1 1 d . . . H15A H 0.1508 0.2580 0.0352 0.048 Uiso 1 1 calc R . . H15B H 0.2035 0.2775 0.1028 0.048 Uiso 1 1 calc R . . H15C H 0.1187 0.3008 0.1040 0.048 Uiso 1 1 calc R . . C16 C 0.0379(10) 0.1612(11) 0.1167(9) 0.014(4) Uiso 1 1 d . . . C17 C -0.0042(11) 0.1931(13) 0.0640(11) 0.027(5) Uiso 1 1 d . . . H17 H 0.0183 0.2215 0.0267 0.033 Uiso 1 1 calc R . . C18 C -0.0797(10) 0.1857(12) 0.0627(10) 0.019(4) Uiso 1 1 d . . . H18 H -0.1077 0.2108 0.0255 0.023 Uiso 1 1 calc R . . C19 C -0.1158(11) 0.1418(11) 0.1154(9) 0.018(4) Uiso 1 1 d . . . H19 H -0.1673 0.1346 0.1133 0.022 Uiso 1 1 calc R . . C20 C -0.0720(9) 0.1091(10) 0.1710(9) 0.011(4) Uiso 1 1 d . . . C21 C 0.0014(9) 0.1203(10) 0.1739(8) 0.008(3) Uiso 1 1 d . . . H21 H 0.0294 0.1010 0.2139 0.010 Uiso 1 1 calc R . . C22 C -0.1740(10) 0.0562(11) 0.2429(9) 0.012(4) Uiso 1 1 d . . . C23 C -0.2500(11) -0.0115(12) 0.3339(10) 0.020(4) Uiso 1 1 d . . . C24 C -0.3126(9) -0.0193(11) 0.2983(9) 0.013(4) Uiso 1 1 d . . . H24 H -0.3155 -0.0070 0.2488 0.015 Uiso 1 1 calc R . . C25 C -0.3754(11) -0.0459(12) 0.3330(10) 0.020(4) Uiso 1 1 d . . . H25 H -0.4207 -0.0470 0.3069 0.024 Uiso 1 1 calc R . . C26 C -0.3735(12) -0.0700(13) 0.4031(11) 0.028(5) Uiso 1 1 d . . . H26 H -0.4155 -0.0913 0.4248 0.034 Uiso 1 1 calc R . . C27 C -0.3070(13) -0.0618(15) 0.4408(13) 0.036(5) Uiso 1 1 d . . . H27 H -0.3041 -0.0747 0.4902 0.043 Uiso 1 1 calc R . . C28 C -0.2445(13) -0.0350(14) 0.4072(12) 0.032(5) Uiso 1 1 d . . . H28 H -0.1989 -0.0324 0.4327 0.038 Uiso 1 1 calc R . . C29 C -0.3274(11) 0.2736(12) 0.4045(10) 0.019(4) Uiso 1 1 d . . . H29A H -0.3596 0.3148 0.3837 0.028 Uiso 1 1 calc R . . H29B H -0.2764 0.2873 0.3956 0.028 Uiso 1 1 calc R . . H29C H -0.3343 0.2706 0.4561 0.028 Uiso 1 1 calc R . . C30 C -0.4446(8) 0.1679(10) 0.3727(8) 0.007(3) Uiso 1 1 d . . . C31 C -0.4800(10) 0.2004(11) 0.4341(9) 0.015(4) Uiso 1 1 d . . . H31 H -0.4530 0.2276 0.4709 0.018 Uiso 1 1 calc R . . C32 C -0.5529(11) 0.1907(12) 0.4370(10) 0.023(4) Uiso 1 1 d . . . H32 H -0.5774 0.2163 0.4748 0.028 Uiso 1 1 calc R . . C33 C -0.5945(11) 0.1459(12) 0.3888(10) 0.019(4) Uiso 1 1 d . . . H33 H -0.6452 0.1372 0.3950 0.023 Uiso 1 1 calc R . . C34 C -0.5576(10) 0.1131(11) 0.3286(10) 0.018(4) Uiso 1 1 d . . . C35 C -0.4838(10) 0.1243(12) 0.3241(10) 0.019(4) Uiso 1 1 d . . . H35 H -0.4592 0.1007 0.2854 0.023 Uiso 1 1 calc R . . C36 C -0.6634(9) 0.0581(10) 0.2583(8) 0.009(3) Uiso 1 1 d . . . C37 C -0.7471(10) -0.0080(11) 0.1667(9) 0.017(4) Uiso 1 1 d . . . C38 C -0.8090(11) -0.0179(13) 0.2046(11) 0.025(4) Uiso 1 1 d . . . H38 H -0.8076 -0.0068 0.2544 0.030 Uiso 1 1 calc R . . C39 C -0.8747(10) -0.0440(11) 0.1717(9) 0.017(4) Uiso 1 1 d . . . H39 H -0.9175 -0.0495 0.1987 0.021 Uiso 1 1 calc R . . C40 C -0.8765(12) -0.0620(13) 0.0984(11) 0.029(5) Uiso 1 1 d . . . H40 H -0.9199 -0.0813 0.0752 0.035 Uiso 1 1 calc R . . C41 C -0.8151(11) -0.0510(12) 0.0619(11) 0.022(4) Uiso 1 1 d . . . H41 H -0.8161 -0.0624 0.0121 0.027 Uiso 1 1 calc R . . C42 C -0.7506(12) -0.0238(13) 0.0938(11) 0.029(5) Uiso 1 1 d . . . H42 H -0.7088 -0.0158 0.0659 0.035 Uiso 1 1 calc R . . C43 C -0.3489(12) 0.0653(14) 0.0828(12) 0.032(5) Uiso 1 1 d . . . H43A H -0.3690 0.0293 0.1185 0.048 Uiso 1 1 calc R . . H43B H -0.2962 0.0562 0.0799 0.048 Uiso 1 1 calc R . . H43C H -0.3727 0.0549 0.0361 0.048 Uiso 1 1 calc R . . C44 C -0.4623(9) 0.1714(10) 0.1121(8) 0.009(3) Uiso 1 1 d . . . C45 C -0.5049(10) 0.1312(11) 0.0597(9) 0.014(4) Uiso 1 1 d . . . H45 H -0.4827 0.1015 0.0230 0.017 Uiso 1 1 calc R . . C46 C -0.5795(10) 0.1361(11) 0.0629(9) 0.014(4) Uiso 1 1 d . . . H46 H -0.6099 0.1094 0.0285 0.017 Uiso 1 1 calc R . . C47 C -0.6106(10) 0.1810(11) 0.1178(9) 0.017(4) Uiso 1 1 d . . . H47 H -0.6622 0.1836 0.1212 0.021 Uiso 1 1 calc R . . C48 C -0.5659(10) 0.2218(11) 0.1671(9) 0.014(4) Uiso 1 1 d . . . C49 C -0.4935(10) 0.2157(11) 0.1634(9) 0.016(4) Uiso 1 1 d . . . H49 H -0.4632 0.2431 0.1974 0.019 Uiso 1 1 calc R . . C50 C -0.6657(11) 0.2730(12) 0.2387(10) 0.023(4) Uiso 1 1 d . . . C51 C -0.7377(11) 0.3384(13) 0.3352(10) 0.025(4) Uiso 1 1 d . . . C52 C -0.8016(10) 0.3525(11) 0.3016(10) 0.016(4) Uiso 1 1 d . . . H52 H -0.8055 0.3430 0.2516 0.020 Uiso 1 1 calc R . . C53 C -0.8625(12) 0.3803(13) 0.3359(11) 0.030(5) Uiso 1 1 d . . . H53 H -0.9059 0.3920 0.3088 0.036 Uiso 1 1 calc R . . C54 C -0.8608(13) 0.3912(14) 0.4105(12) 0.033(5) Uiso 1 1 d . . . H54 H -0.9030 0.4065 0.4353 0.040 Uiso 1 1 calc R . . C55 C -0.7952(12) 0.3786(13) 0.4450(11) 0.027(5) Uiso 1 1 d . . . H55 H -0.7910 0.3897 0.4948 0.033 Uiso 1 1 calc R . . C56 C -0.7334(11) 0.3501(12) 0.4105(10) 0.024(4) Uiso 1 1 d . . . H56 H -0.6895 0.3387 0.4370 0.028 Uiso 1 1 calc R . . B1 B -0.0063(12) -0.0815(14) 0.3544(11) 0.020(5) Uiso 1 1 d . . . B2 B -0.4974(13) 0.4169(15) 0.3509(12) 0.023(5) 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 0.0156(8) 0.0247(8) 0.0237(8) 0.0102(6) 0.0029(5) 0.0014(6) Ag2 0.0196(8) 0.0277(8) 0.0169(7) -0.0100(6) -0.0002(5) 0.0009(7) S1 0.017(2) 0.013(2) 0.020(2) -0.0001(18) 0.0007(17) -0.0051(19) S2 0.026(3) 0.014(2) 0.021(2) 0.0061(19) 0.0072(19) 0.007(2) S3 0.031(3) 0.018(2) 0.015(2) -0.0042(19) -0.0004(18) 0.001(2) S4 0.024(3) 0.026(3) 0.016(2) -0.004(2) 0.0011(18) 0.000(2) _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 O4 2.418(13) 1_655 ? Ag1 S1 2.492(5) . ? Ag1 O3 2.500(13) 1_655 ? Ag1 S2 2.510(5) . ? Ag2 O1 2.407(14) . ? Ag2 O2 2.470(14) . ? Ag2 S4 2.491(5) . ? Ag2 S3 2.498(5) . ? S1 C2 1.75(2) . ? S1 C1 1.788(19) . ? S2 C16 1.759(18) . ? S2 C15 1.79(2) . ? S3 C30 1.766(16) . ? S3 C29 1.822(19) . ? S4 C44 1.780(17) . ? S4 C43 1.82(2) . ? F1 B1 1.35(2) . ? F2 B1 1.40(3) . ? F3 B1 1.41(3) . ? F4 B1 1.40(2) . ? F5 B2 1.36(3) . ? F6 B2 1.44(3) . ? F7 B2 1.38(3) . ? F8 B2 1.41(3) . ? O1 C8 1.26(2) . ? O2 C22 1.23(2) . ? O3 C36 1.23(2) . ? O3 Ag1 2.500(13) 1_455 ? O4 C50 1.20(2) . ? O4 Ag1 2.418(13) 1_455 ? N1 C8 1.29(2) . ? N1 C6 1.44(2) . ? N2 C8 1.38(2) . ? N2 C9 1.42(2) . ? N3 C22 1.34(2) . ? N3 C20 1.43(2) . ? N4 C22 1.39(2) . ? N4 C23 1.39(2) . ? N5 C36 1.32(2) . ? N5 C34 1.44(2) . ? N6 C36 1.41(2) . ? N6 C37 1.41(2) . ? N7 C50 1.33(2) . ? N7 C48 1.40(2) . ? N8 C51 1.38(2) . ? N8 C50 1.43(2) . ? C2 C7 1.34(3) . ? C2 C3 1.44(3) . ? C3 C4 1.41(3) . ? C4 C5 1.39(3) . ? C5 C6 1.40(2) . ? C6 C7 1.39(2) . ? C9 C10 1.37(3) . ? C9 C14 1.39(3) . ? C10 C11 1.37(3) . ? C11 C12 1.40(3) . ? C12 C13 1.37(3) . ? C13 C14 1.39(3) . ? C16 C17 1.34(3) . ? C16 C21 1.45(2) . ? C17 C18 1.39(3) . ? C18 C19 1.41(3) . ? C19 C20 1.40(3) . ? C20 C21 1.36(2) . ? C23 C24 1.31(3) . ? C23 C28 1.43(3) . ? C24 C25 1.41(3) . ? C25 C26 1.37(3) . ? C26 C27 1.40(3) . ? C27 C28 1.40(3) . ? C30 C35 1.35(2) . ? C30 C31 1.44(2) . ? C31 C32 1.35(3) . ? C32 C33 1.38(3) . ? C33 C34 1.44(3) . ? C34 C35 1.37(3) . ? C37 C38 1.37(3) . ? C37 C42 1.39(3) . ? C38 C39 1.40(3) . ? C39 C40 1.40(3) . ? C40 C41 1.35(3) . ? C41 C42 1.38(3) . ? C44 C49 1.35(2) . ? C44 C45 1.40(2) . ? C45 C46 1.37(2) . ? C46 C47 1.41(2) . ? C47 C48 1.39(3) . ? C48 C49 1.33(2) . ? C51 C52 1.33(3) . ? C51 C56 1.42(3) . ? C52 C53 1.39(3) . ? C53 C54 1.41(3) . ? C54 C55 1.36(3) . ? C55 C56 1.40(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 O4 Ag1 S1 125.1(3) 1_655 . ? O4 Ag1 O3 81.1(4) 1_655 1_655 ? S1 Ag1 O3 83.8(3) . 1_655 ? O4 Ag1 S2 85.9(3) 1_655 . ? S1 Ag1 S2 144.50(17) . . ? O3 Ag1 S2 121.5(3) 1_655 . ? O1 Ag2 O2 82.1(5) . . ? O1 Ag2 S4 128.4(3) . . ? O2 Ag2 S4 87.3(3) . . ? O1 Ag2 S3 82.3(3) . . ? O2 Ag2 S3 112.8(3) . . ? S4 Ag2 S3 146.57(18) . . ? C2 S1 C1 104.2(9) . . ? C2 S1 Ag1 105.4(6) . . ? C1 S1 Ag1 104.6(6) . . ? C16 S2 C15 102.7(10) . . ? C16 S2 Ag1 113.3(6) . . ? C15 S2 Ag1 106.1(8) . . ? C30 S3 C29 104.0(8) . . ? C30 S3 Ag2 110.3(5) . . ? C29 S3 Ag2 109.9(6) . . ? C44 S4 C43 101.9(9) . . ? C44 S4 Ag2 106.0(5) . . ? C43 S4 Ag2 105.3(7) . . ? C8 O1 Ag2 129.7(12) . . ? C22 O2 Ag2 126.4(12) . . ? C36 O3 Ag1 127.9(11) . 1_455 ? C50 O4 Ag1 129.2(13) . 1_455 ? C8 N1 C6 129.3(16) . . ? C8 N2 C9 126.7(15) . . ? C22 N3 C20 129.1(15) . . ? C22 N4 C23 128.9(16) . . ? C36 N5 C34 128.1(15) . . ? C36 N6 C37 126.4(15) . . ? C50 N7 C48 127.8(16) . . ? C51 N8 C50 127.7(16) . . ? C7 C2 C3 117.4(18) . . ? C7 C2 S1 122.7(15) . . ? C3 C2 S1 119.8(14) . . ? C4 C3 C2 120.1(17) . . ? C5 C4 C3 120.0(17) . . ? C4 C5 C6 118.9(16) . . ? C7 C6 C5 119.8(15) . . ? C7 C6 N1 116.8(15) . . ? C5 C6 N1 123.3(15) . . ? C2 C7 C6 123.5(17) . . ? O1 C8 N1 123.7(17) . . ? O1 C8 N2 120.6(16) . . ? N1 C8 N2 115.6(16) . . ? C10 C9 C14 121.5(18) . . ? C10 C9 N2 124.6(17) . . ? C14 C9 N2 113.9(17) . . ? C9 C10 C11 119.9(18) . . ? C10 C11 C12 121.0(19) . . ? C13 C12 C11 117(2) . . ? C12 C13 C14 123(2) . . ? C13 C14 C9 116.7(19) . . ? C17 C16 C21 117.6(17) . . ? C17 C16 S2 126.5(15) . . ? C21 C16 S2 115.9(13) . . ? C16 C17 C18 121.8(19) . . ? C17 C18 C19 121.5(18) . . ? C20 C19 C18 116.8(17) . . ? C21 C20 C19 121.2(16) . . ? C21 C20 N3 117.6(15) . . ? C19 C20 N3 121.2(16) . . ? C20 C21 C16 120.9(15) . . ? O2 C22 N3 125.2(16) . . ? O2 C22 N4 121.1(16) . . ? N3 C22 N4 113.6(15) . . ? C24 C23 N4 125.7(18) . . ? C24 C23 C28 119.5(18) . . ? N4 C23 C28 114.7(17) . . ? C23 C24 C25 120.7(17) . . ? C26 C25 C24 122.4(19) . . ? C25 C26 C27 117(2) . . ? C26 C27 C28 121(2) . . ? C27 C28 C23 119(2) . . ? C35 C30 C31 119.7(16) . . ? C35 C30 S3 119.2(13) . . ? C31 C30 S3 120.9(12) . . ? C32 C31 C30 117.2(16) . . ? C31 C32 C33 124.3(19) . . ? C32 C33 C34 117.0(18) . . ? C35 C34 N5 116.3(16) . . ? C35 C34 C33 119.0(17) . . ? N5 C34 C33 124.7(17) . . ? C30 C35 C34 122.3(17) . . ? O3 C36 N5 126.6(16) . . ? O3 C36 N6 121.1(15) . . ? N5 C36 N6 112.2(14) . . ? C38 C37 C42 118.2(18) . . ? C38 C37 N6 126.4(17) . . ? C42 C37 N6 115.4(16) . . ? C37 C38 C39 121.5(19) . . ? C38 C39 C40 119.3(18) . . ? C41 C40 C39 118(2) . . ? C40 C41 C42 123(2) . . ? C41 C42 C37 120.0(19) . . ? C49 C44 C45 121.3(16) . . ? C49 C44 S4 119.0(13) . . ? C45 C44 S4 119.6(12) . . ? C46 C45 C44 118.2(16) . . ? C45 C46 C47 119.3(17) . . ? C48 C47 C46 120.2(17) . . ? C49 C48 C47 119.5(17) . . ? C49 C48 N7 119.3(16) . . ? C47 C48 N7 121.1(16) . . ? C48 C49 C44 121.4(17) . . ? O4 C50 N7 131.0(19) . . ? O4 C50 N8 117.9(17) . . ? N7 C50 N8 111.0(16) . . ? C52 C51 N8 126.5(18) . . ? C52 C51 C56 117.7(18) . . ? N8 C51 C56 115.8(17) . . ? C51 C52 C53 123.3(19) . . ? C52 C53 C54 121(2) . . ? C55 C54 C53 116(2) . . ? C54 C55 C56 123(2) . . ? C55 C56 C51 118.9(19) . . ? F1 B1 F2 111.0(17) . . ? F1 B1 F4 110.9(16) . . ? F2 B1 F4 107.8(17) . . ? F1 B1 F3 111.1(17) . . ? F2 B1 F3 108.4(16) . . ? F4 B1 F3 107.7(17) . . ? F5 B2 F7 111.5(18) . . ? F5 B2 F8 111.4(17) . . ? F7 B2 F8 110.1(17) . . ? F5 B2 F6 109.2(17) . . ? F7 B2 F6 108.3(16) . . ? F8 B2 F6 106.2(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N F2 0.88 2.10 2.97(2) 172.2 2 N2 H2N F4 0.88 2.09 2.947(19) 164.8 2 N3 H3N F3 0.88 2.06 2.93(2) 168.3 . N4 H4N F1 0.88 2.20 3.051(19) 163.2 . N5 H5N F6 0.88 2.02 2.887(18) 170.4 2_445 N6 H6N F8 0.88 2.15 3.000(18) 162.1 2_445 N7 H7N F7 0.88 2.09 2.96(2) 170.2 . N8 H8N F5 0.88 2.16 3.000(18) 160.6 . _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 4.778 _refine_diff_density_min -3.652 _refine_diff_density_rms 0.288 # Attachment 'AgNO3.CIF' data_agno3 _database_code_depnum_ccdc_archive 'CCDC 291486' _audit_creation_date 05-15-02 _audit_creation_method CRYSTALS_ver_12-03-99 #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? # choose from 'full, fullcycle, atomblock, userblock, diagonal, sparse' _refine_ls_matrix_type full # choose from 'heavy, direct, difmap, geom' _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # choose from 'none, undef, noref, refall, refxyz, refU, constr, mixed' _refine_ls_hydrogen_treatment mixed #**************************************************************************** # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al 2003) ; _computing_publication_material ; CRYSTALS (Watkin et al 2003) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; #============================================================= _cell_length_a 18.2449(9) _cell_angle_alpha 90 _cell_length_b 16.2679(8) _cell_angle_beta 90 _cell_length_c 18.9904(10) _cell_angle_gamma 90 _cell_volume 5636.5(5) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'Ag ' -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 8 _chemical_formula_sum ' C28 H28 Ag1 N5 O5 S2 ' _chemical_formula_moiety ' C28 H28 Ag1 N5 O5 S2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 686.56 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 120 _exptl_crystal_description ' cuboid ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 0.912 _diffrn_measurement_device_type ; Bruker SMART ; _diffrn_radiation_monochromator graphite _computing_data_collection ; SMART (Siemens, 1993) ; _computing_data_reduction ; SAINT (Siemens ,1995) ; _computing_cell_refinement ; SAINT (Siemens ,1995) ; _computing_structure_solution ; SIR92 (Altomare et al, 1994) ; _diffrn_measurement_method \w _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 1.000 # Sheldrick geometric definitions 0.95 0.95 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 120 _diffrn_reflns_number 79432 _reflns_number_total 9324 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 9324 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9766 _diffrn_reflns_theta_min 1.991 _diffrn_reflns_theta_max 31.976 _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 30.697 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min 0 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _refine_diff_density_min -0.82 _refine_diff_density_max 0.95 _refine_ls_number_reflns 5834 _refine_ls_number_restraints 0 _refine_ls_number_parameters 370 #_refine_ls_R_factor_ref 0.0338 _refine_ls_wR_factor_ref 0.0752 _refine_ls_goodness_of_fit_ref 0.9004 #_reflns_number_all 9305 _refine_ls_R_factor_all 0.0621 _refine_ls_wR_factor_all 0.0779 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 5834 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_gt 0.0752 _refine_ls_shift/su_max 0.000519 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.26 4.21 1.66 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 ## -------------------REFERENCES ----------------------## ## Insert your own references - in alphabetic order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993) SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group _atom_site_attached_hydrogens Ag1 Ag 0.812745(9) 0.175405(12) 0.239595(11) 0.0244 1.0000 Uani . . . . . . S1 S 0.85539(3) 0.15271(4) 0.11653(3) 0.0201 1.0000 Uani . . . . . . C14 C 0.95191(13) 0.16948(14) 0.11525(12) 0.0182 1.0000 Uani . . . . . . C27 C 0.98445(12) 0.21461(14) 0.16863(12) 0.0177 1.0000 Uani . . . . . . C18 C 1.05978(12) 0.22948(14) 0.16845(12) 0.0183 1.0000 Uani . . . . . . N3 N 1.08751(11) 0.27533(13) 0.22526(11) 0.0204 1.0000 Uani . . . . . . C20 C 1.15915(13) 0.28055(13) 0.24615(12) 0.0186 1.0000 Uani . . . . . . O2 O 1.21018(9) 0.25032(11) 0.21258(10) 0.0225 1.0000 Uani . . . . . . N4 N 1.16739(11) 0.32188(14) 0.30791(11) 0.0204 1.0000 Uani . . . . . . C21 C 1.23481(13) 0.33868(13) 0.34131(13) 0.0198 1.0000 Uani . . . . . . C26 C 1.29923(13) 0.35514(14) 0.30430(14) 0.0212 1.0000 Uani . . . . . . C25 C 1.36287(14) 0.37558(16) 0.34094(17) 0.0278 1.0000 Uani . . . . . . C24 C 1.36249(17) 0.38013(18) 0.41364(19) 0.0356 1.0000 Uani . . . . . . C23 C 1.29849(18) 0.36423(19) 0.45030(17) 0.0364 1.0000 Uani . . . . . . C22 C 1.23472(16) 0.34289(17) 0.41475(14) 0.0272 1.0000 Uani . . . . . . C17 C 1.10260(14) 0.19746(16) 0.11360(13) 0.0226 1.0000 Uani . . . . . . C16 C 1.06875(14) 0.15220(17) 0.06107(13) 0.0241 1.0000 Uani . . . . . . C15 C 0.99402(14) 0.13806(15) 0.06028(13) 0.0215 1.0000 Uani . . . . . . C19 C 0.85086(15) 0.04172(16) 0.10863(16) 0.0288 1.0000 Uani . . . . . . S2 S 0.85661(3) 0.17545(4) 0.36479(3) 0.0217 1.0000 Uani . . . . . . O1 O 0.71610(10) 0.07473(11) 0.21576(10) 0.0229 1.0000 Uani . . . . . . C1 C 0.66575(13) 0.04854(13) 0.25234(13) 0.0194 1.0000 Uani . . . . . . N1 N 0.59324(11) 0.05637(12) 0.23480(11) 0.0204 1.0000 Uani . . . . . . C8 C 0.56318(13) 0.10152(14) 0.17881(12) 0.0189 1.0000 Uani . . . . . . C13 C 0.48781(13) 0.11628(14) 0.18163(13) 0.0189 1.0000 Uani . . . . . . C12 C 0.45319(14) 0.16144(13) 0.12922(13) 0.0202 1.0000 Uani . . . . . . C11 C 0.49313(16) 0.19177(16) 0.07280(14) 0.0261 1.0000 Uani . . . . . . C10 C 0.56793(15) 0.17746(17) 0.07040(14) 0.0259 1.0000 Uani . . . . . . C9 C 0.60375(14) 0.13296(15) 0.12218(13) 0.0239 1.0000 Uani . . . . . . N2 N 0.67513(11) 0.00808(13) 0.31451(11) 0.0206 1.0000 Uani . . . . . . C2 C 0.74200(13) -0.01253(14) 0.34670(13) 0.0199 1.0000 Uani . . . . . . C7 C 0.80743(14) -0.02295(14) 0.30944(14) 0.0234 1.0000 Uani . . . . . . C6 C 0.87068(14) -0.04512(15) 0.34577(16) 0.0264 1.0000 Uani . . . . . . C5 C 0.86983(16) -0.05793(18) 0.41730(18) 0.0338 1.0000 Uani . . . . . . C4 C 0.80484(17) -0.0487(2) 0.45401(16) 0.0349 1.0000 Uani . . . . . . C3 C 0.74102(15) -0.02608(18) 0.41910(15) 0.0277 1.0000 Uani . . . . . . C28 C 0.34392(16) 0.27925(17) 0.10345(17) 0.0325 1.0000 Uani . . . . . . N5 N 0.50150(11) -0.08446(13) 0.36073(12) 0.0215 1.0000 Uani . . . . . . O3 O 0.54777(11) -0.04389(13) 0.39446(11) 0.0309 1.0000 Uani . . . . . . O4 O 0.50245(12) -0.08390(17) 0.29475(11) 0.0402 1.0000 Uani . . . . . . O5 O 0.45426(11) -0.12521(13) 0.39247(11) 0.0302 1.0000 Uani . . . . . . H15 H 0.95353(12) 0.23707(14) 0.20761(12) 0.0222 1.0000 Uiso R . . . . . H22 H 1.29956(13) 0.35244(14) 0.25158(14) 0.0268 1.0000 Uiso R . . . . . H21 H 1.40954(14) 0.38700(16) 0.31448(17) 0.0361 1.0000 Uiso R . . . . . H20 H 1.40852(17) 0.39487(18) 0.43971(19) 0.0439 1.0000 Uiso R . . . . . H19 H 1.29790(18) 0.36828(19) 0.50306(17) 0.0445 1.0000 Uiso R . . . . . H18 H 1.18877(16) 0.33047(17) 0.44161(14) 0.0343 1.0000 Uiso R . . . . . H14 H 1.15687(14) 0.20709(16) 0.11281(13) 0.0279 1.0000 Uiso R . . . . . H13 H 1.09941(14) 0.12915(17) 0.02223(13) 0.0295 1.0000 Uiso R . . . . . H12 H 0.97065(14) 0.10624(15) 0.02116(13) 0.0271 1.0000 Uiso R . . . . . H4 H 0.45849(13) 0.09397(14) 0.22180(13) 0.0238 1.0000 Uiso R . . . . . H3 H 0.46832(16) 0.22344(16) 0.03444(14) 0.0318 1.0000 Uiso R . . . . . H2 H 0.59698(15) 0.19976(17) 0.02999(14) 0.0328 1.0000 Uiso R . . . . . H1 H 0.65806(14) 0.12357(15) 0.11942(13) 0.0294 1.0000 Uiso R . . . . . H11 H 0.80854(14) -0.01484(14) 0.25718(14) 0.0296 1.0000 Uiso R . . . . . H10 H 0.91783(14) -0.05204(15) 0.31950(16) 0.0336 1.0000 Uiso R . . . . . H9 H 0.91595(16) -0.07332(18) 0.44287(18) 0.0417 1.0000 Uiso R . . . . . H8 H 0.80377(17) -0.0590(2) 0.50606(16) 0.0427 1.0000 Uiso R . . . . . H7 H 0.69428(15) -0.01926(18) 0.44605(15) 0.0350 1.0000 Uiso R . . . . . H6 H 0.62959(11) -0.00913(13) 0.33978(11) 0.0251 1.0000 Uiso R . . . . . H5 H 0.55755(11) 0.02662(12) 0.26548(11) 0.0255 1.0000 Uiso R . . . . . H16 H 1.05115(11) 0.30747(13) 0.25329(11) 0.0258 1.0000 Uiso R . . . . . H17 H 1.12189(11) 0.34189(14) 0.33172(11) 0.0254 1.0000 Uiso R . . . . . H25 H 0.79850(15) 0.02377(16) 0.10882(16) 0.0364 1.0000 Uiso R . . . . . H23 H 0.87710(15) 0.01586(16) 0.14939(16) 0.0364 1.0000 Uiso R . . . . . H24 H 0.87471(15) 0.02430(16) 0.06373(16) 0.0364 1.0000 Uiso R . . . . . H27 H 0.29046(16) 0.29365(17) 0.10468(17) 0.0401 1.0000 Uiso R . . . . . H28 H 0.37166(16) 0.31813(17) 0.13416(17) 0.0401 1.0000 Uiso R . . . . . H26 H 0.36219(16) 0.28330(17) 0.05402(17) 0.0401 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01435(7) 0.02826(8) 0.03048(9) -0.01226(7) 0.00314(7) -0.00164(7) S1 0.0169(2) 0.0191(2) 0.0243(3) -0.0013(2) -0.00228(19) 0.00138(19) C14 0.0178(9) 0.0171(10) 0.0196(10) 0.0030(8) 0.0017(7) 0.0015(7) C27 0.0177(10) 0.0158(9) 0.0195(10) 0.0013(8) 0.0008(8) 0.0028(7) C18 0.0192(10) 0.0171(9) 0.0185(10) 0.0028(8) -0.0011(8) 0.0004(8) N3 0.0158(8) 0.0214(9) 0.0239(11) -0.0013(7) 0.0008(7) 0.0002(7) C20 0.0182(9) 0.0168(9) 0.0209(11) 0.0054(8) -0.0019(8) 0.0000(7) O2 0.0175(7) 0.0246(8) 0.0254(8) -0.0009(7) -0.0021(6) 0.0057(6) N4 0.0166(8) 0.0234(9) 0.0213(9) -0.0010(8) -0.0005(7) 0.0006(7) C21 0.0218(10) 0.0136(10) 0.0241(11) 0.0025(7) -0.0039(8) 0.0038(7) C26 0.0216(11) 0.0155(9) 0.0266(12) 0.0008(8) -0.0024(8) 0.0014(8) C25 0.0217(11) 0.0170(10) 0.0449(16) 0.0021(10) -0.0063(10) 0.0017(9) C24 0.0337(14) 0.0270(13) 0.0461(18) -0.0032(12) -0.0183(13) 0.0057(11) C23 0.0450(18) 0.0342(15) 0.0302(14) -0.0035(11) -0.0143(12) 0.0088(12) C22 0.0324(13) 0.0262(12) 0.0231(12) 0.0003(9) -0.0011(10) 0.0069(10) C17 0.0196(10) 0.0271(12) 0.0211(11) 0.0043(9) 0.0036(9) -0.0012(8) C16 0.0237(11) 0.0300(12) 0.0185(11) -0.0005(9) 0.0045(8) -0.0008(9) C15 0.0245(11) 0.0209(11) 0.0191(11) 0.0013(8) 0.0022(8) -0.0019(9) C19 0.0278(12) 0.0227(11) 0.0359(15) -0.0091(10) 0.0068(10) -0.0054(9) S2 0.0221(3) 0.0185(2) 0.0244(3) -0.0056(2) 0.0051(2) -0.0027(2) O1 0.0202(8) 0.0215(8) 0.0271(8) -0.0008(7) 0.0018(7) -0.0055(6) C1 0.0192(9) 0.0141(8) 0.0250(12) -0.0033(8) 0.0001(8) -0.0007(7) N1 0.0181(9) 0.0205(9) 0.0224(9) 0.0031(7) 0.0028(8) -0.0003(7) C8 0.0225(10) 0.0165(9) 0.0176(10) -0.0021(8) 0.0005(8) -0.0013(8) C13 0.0212(10) 0.0161(9) 0.0194(11) -0.0007(8) -0.0002(8) -0.0030(8) C12 0.0232(10) 0.0144(10) 0.0231(11) -0.0007(8) -0.0014(8) -0.0022(7) C11 0.0327(13) 0.0232(12) 0.0223(12) 0.0026(9) 0.0021(10) -0.0012(9) C10 0.0308(12) 0.0254(11) 0.0215(11) 0.0036(10) 0.0077(9) -0.0033(10) C9 0.0258(11) 0.0224(11) 0.0234(12) 0.0011(8) 0.0050(9) -0.0011(9) N2 0.0172(9) 0.0235(9) 0.0210(10) 0.0004(7) 0.0006(7) -0.0006(7) C2 0.0198(10) 0.0155(10) 0.0243(11) -0.0023(8) -0.0001(8) -0.0007(8) C7 0.0232(11) 0.0169(9) 0.0301(12) -0.0039(8) 0.0006(9) -0.0011(9) C6 0.0209(11) 0.0164(10) 0.0420(15) -0.0024(9) 0.0006(10) -0.0007(8) C5 0.0272(13) 0.0294(13) 0.0447(17) -0.0016(12) -0.0113(12) 0.0011(11) C4 0.0356(15) 0.0394(15) 0.0296(14) 0.0013(11) -0.0091(11) 0.0041(12) C3 0.0262(12) 0.0310(12) 0.0260(12) -0.0010(10) -0.0014(10) 0.0008(10) C28 0.0315(14) 0.0249(12) 0.0412(16) 0.0130(11) 0.0028(12) 0.0040(10) N5 0.0183(9) 0.0195(9) 0.0266(11) 0.0020(8) 0.0014(8) 0.0023(7) O3 0.0294(9) 0.0295(10) 0.0337(10) -0.0091(8) 0.0060(8) -0.0120(8) O4 0.0345(11) 0.0628(16) 0.0233(10) 0.0038(10) 0.0016(8) -0.0162(11) O5 0.0266(9) 0.0344(10) 0.0296(10) 0.0109(8) -0.0026(8) -0.0115(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 . O1 . 2.4486(17) yes Ag1 . S2 . 2.5087(7) yes Ag1 . S1 . 2.4906(7) yes Ag1 . O2 8_455 2.4108(17) yes S1 . C19 . 1.814(3) yes S1 . C14 . 1.782(2) yes C14 . C15 . 1.393(3) yes C14 . C27 . 1.385(3) yes C27 . H15 . 1.000 no C27 . C18 . 1.395(3) yes C18 . C17 . 1.402(3) yes C18 . N3 . 1.406(3) yes N3 . H16 . 0.999 no N3 . C20 . 1.368(3) yes C20 . N4 . 1.360(3) yes C20 . O2 . 1.231(3) yes N4 . H17 . 1.000 no N4 . C21 . 1.411(3) yes C21 . C22 . 1.396(4) yes C21 . C26 . 1.395(3) yes C26 . H22 . 1.002 no C26 . C25 . 1.394(3) yes C25 . H21 . 1.006 no C25 . C24 . 1.383(5) yes C24 . H20 . 1.004 no C24 . C23 . 1.384(5) yes C23 . H19 . 1.004 no C23 . C22 . 1.389(4) yes C22 . H18 . 1.002 no C17 . H14 . 1.003 no C17 . C16 . 1.385(4) yes C16 . H13 . 0.999 no C16 . C15 . 1.383(3) yes C15 . H12 . 1.001 no C19 . H24 . 0.998 no C19 . H23 . 1.003 no C19 . H25 . 0.999 no S2 . C12 8_555 1.780(3) yes S2 . C28 8_555 1.808(3) yes O1 . C1 . 1.228(3) yes C1 . N2 . 1.363(3) yes C1 . N1 . 1.370(3) yes N1 . H5 . 0.999 no N1 . C8 . 1.404(3) yes C8 . C9 . 1.402(3) yes C8 . C13 . 1.397(3) yes C13 . H4 . 1.000 no C13 . C12 . 1.389(3) yes C12 . C11 . 1.386(4) yes C11 . H3 . 1.001 no C11 . C10 . 1.385(4) yes C10 . H2 . 1.001 no C10 . C9 . 1.385(4) yes C9 . H1 . 1.004 no N2 . H6 . 1.000 no N2 . C2 . 1.405(3) yes C2 . C3 . 1.393(4) yes C2 . C7 . 1.398(3) yes C7 . H11 . 1.001 no C7 . C6 . 1.392(4) yes C6 . H10 . 1.001 no C6 . C5 . 1.374(4) yes C5 . H9 . 1.003 no C5 . C4 . 1.384(4) yes C4 . H8 . 1.003 no C4 . C3 . 1.390(4) yes C3 . H7 . 1.001 no C28 . H26 . 0.998 no C28 . H28 . 0.998 no C28 . H27 . 1.003 no N5 . O5 . 1.243(3) yes N5 . O4 . 1.253(3) yes N5 . O3 . 1.248(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Ag1 . S2 . 113.90(5) yes O1 . Ag1 . S1 . 87.27(5) yes S2 . Ag1 . S1 . 142.15(2) yes O1 . Ag1 . O2 8_455 81.31(6) yes S2 . Ag1 . O2 8_455 83.71(5) yes S1 . Ag1 . O2 8_455 132.14(5) yes C19 . S1 . C14 . 101.32(12) yes C19 . S1 . Ag1 . 102.18(10) yes C14 . S1 . Ag1 . 107.39(8) yes C15 . C14 . C27 . 120.4(2) yes C15 . C14 . S1 . 119.94(18) yes C27 . C14 . S1 . 119.64(17) yes H15 . C27 . C18 . 119.613 no H15 . C27 . C14 . 119.584 no C18 . C27 . C14 . 120.8(2) yes C17 . C18 . N3 . 124.5(2) yes C17 . C18 . C27 . 119.1(2) yes N3 . C18 . C27 . 116.4(2) yes H16 . N3 . C20 . 116.585 no H16 . N3 . C18 . 116.604 no C20 . N3 . C18 . 126.8(2) yes N4 . C20 . O2 . 124.1(2) yes N4 . C20 . N3 . 112.7(2) yes O2 . C20 . N3 . 123.2(2) yes C20 . O2 . Ag1 8_555 126.43(16) yes H17 . N4 . C21 . 117.228 no H17 . N4 . C20 . 117.328 no C21 . N4 . C20 . 125.4(2) yes C22 . C21 . C26 . 119.7(2) yes C22 . C21 . N4 . 117.2(2) yes C26 . C21 . N4 . 123.0(2) yes H22 . C26 . C25 . 120.269 no H22 . C26 . C21 . 119.999 no C25 . C26 . C21 . 119.7(2) yes H21 . C25 . C24 . 119.541 no H21 . C25 . C26 . 119.992 no C24 . C25 . C26 . 120.5(3) yes H20 . C24 . C23 . 120.147 no H20 . C24 . C25 . 120.075 no C23 . C24 . C25 . 119.8(3) yes H19 . C23 . C22 . 119.489 no H19 . C23 . C24 . 119.923 no C22 . C23 . C24 . 120.6(3) yes H18 . C22 . C23 . 120.249 no H18 . C22 . C21 . 119.976 no C23 . C22 . C21 . 119.8(3) yes H14 . C17 . C16 . 120.847 no H14 . C17 . C18 . 120.210 no C16 . C17 . C18 . 118.9(2) yes H13 . C16 . C15 . 118.796 no H13 . C16 . C17 . 118.797 no C15 . C16 . C17 . 122.4(2) yes H12 . C15 . C16 . 120.945 no H12 . C15 . C14 . 120.725 no C16 . C15 . C14 . 118.3(2) yes H24 . C19 . H23 . 109.394 no H24 . C19 . H25 . 109.705 no H23 . C19 . H25 . 109.351 no H24 . C19 . S1 . 109.465 no H23 . C19 . S1 . 109.383 no H25 . C19 . S1 . 109.528 no Ag1 . S2 . C12 8_555 112.10(8) yes Ag1 . S2 . C28 8_555 105.99(11) yes C12 8_555 S2 . C28 8_555 103.01(12) yes C1 . O1 . Ag1 . 131.78(16) yes N2 . C1 . N1 . 112.1(2) yes N2 . C1 . O1 . 124.3(2) yes N1 . C1 . O1 . 123.5(2) yes H5 . N1 . C8 . 116.133 no H5 . N1 . C1 . 116.270 no C8 . N1 . C1 . 127.6(2) yes C9 . C8 . C13 . 119.1(2) yes C9 . C8 . N1 . 124.4(2) yes C13 . C8 . N1 . 116.5(2) yes H4 . C13 . C12 . 119.700 no H4 . C13 . C8 . 119.566 no C12 . C13 . C8 . 120.7(2) yes C11 . C12 . C13 . 120.2(2) yes C11 . C12 . S2 8_455 121.6(2) yes C13 . C12 . S2 8_455 118.16(19) yes H3 . C11 . C10 . 120.550 no H3 . C11 . C12 . 120.537 no C10 . C11 . C12 . 118.9(2) yes H2 . C10 . C9 . 118.960 no H2 . C10 . C11 . 119.080 no C9 . C10 . C11 . 122.0(2) yes H1 . C9 . C10 . 120.538 no H1 . C9 . C8 . 120.372 no C10 . C9 . C8 . 119.1(2) yes H6 . N2 . C2 . 116.501 no H6 . N2 . C1 . 116.536 no C2 . N2 . C1 . 127.0(2) yes C3 . C2 . C7 . 119.4(2) yes C3 . C2 . N2 . 117.1(2) yes C7 . C2 . N2 . 123.4(2) yes H11 . C7 . C6 . 120.577 no H11 . C7 . C2 . 120.185 no C6 . C7 . C2 . 119.2(2) yes H10 . C6 . C5 . 119.029 no H10 . C6 . C7 . 119.651 no C5 . C6 . C7 . 121.3(3) yes H9 . C5 . C4 . 120.130 no H9 . C5 . C6 . 120.443 no C4 . C5 . C6 . 119.4(3) yes H8 . C4 . C3 . 119.875 no H8 . C4 . C5 . 119.694 no C3 . C4 . C5 . 120.4(3) yes H7 . C3 . C4 . 119.974 no H7 . C3 . C2 . 119.885 no C4 . C3 . C2 . 120.1(3) yes H26 . C28 . H28 . 109.762 no H26 . C28 . H27 . 109.347 no H28 . C28 . H27 . 109.346 no H26 . C28 . S2 8_455 109.425 no H28 . C28 . S2 8_455 109.382 no H27 . C28 . S2 8_455 109.566 no O5 . N5 . O4 . 119.9(2) yes O5 . N5 . O3 . 120.1(2) yes O4 . N5 . O3 . 120.0(2) yes