# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- complete_cif.cif' # 1. Submission Details _publ_contact_author_name 'Ullrich Englert' _publ_contact_author_address ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; _publ_contact_author_email ullrich.englert@ac.rwth-aachen.de _publ_contact_author_fax 0049-241-8092288 _publ_contact_author_phone 0049-241-8094666 _publ_requested_category FP _publ_requested_coeditor_name ? _publ_contact_letter ; ?? ; # 2. Processing Summary (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. Titl and Author List _publ_section_title ; Bimetallic Coordination Networks based on Al(acacCN)3: A building block between Inertness and Lability ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' C.Merkens ; Institut f\"ur Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; N.Becker ; Institut f\"ur Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; K.Lamberts ; Institut f\"ur Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; U.Englert ; Institut f\"ur Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; # 4. Text _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Bruker (1999). SAINT+. Version 6.02. Program for Reduction of Data Collected on Bruker CCD Area Detector Diffractometer, Bruker AXS Inc., Madison, Wisconson, USA. Bruker (2001). SMART. Version 5.624. Program for Bruker CCD X-ray Diffractometer Control. Bruker AXS Inc., Madison, Wisconson, USA. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ; _publ_section_acknowledgements ; ; data_2a _database_code_depnum_ccdc_archive 'CCDC 872084' #TrackingRef '- complete_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2a _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 N3 O6 Al Ag, P F6, 4(C6 H6)' _chemical_formula_sum 'C42 H42 Ag Al F6 N3 O6 P' _chemical_formula_weight 964.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8241(9) _cell_length_b 19.9619(15) _cell_length_c 18.6120(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.8740(10) _cell_angle_gamma 90.00 _cell_volume 4314.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 21.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8694 _exptl_absorpt_correction_T_max 0.9649 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50747 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.61 _reflns_number_total 9003 _reflns_number_gt 7161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER smart' _computing_cell_refinement 'BRUKER saint' _computing_data_reduction 'BRUKER saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+2.4722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9003 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL c11_36 in P2(1)/c CELL 0.71073 11.8241 19.9619 18.6120 90.000 100.874 90.000 ZERR 8.00 0.0009 0.0015 0.0014 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O F AL P AG UNIT 168 168 12 24 24 4 4 4 TEMP 173.160 L.S. 8 BOND BOND$H SIZE 0.24 0.11 0.06 ACTA FMAP 2 PLAN 20 WGHT 0.0277 2.4722 FVAR 0.23714 MOLE 1 AG1 8 0.191766 0.196667 0.055869 11.00000 0.02565 0.02257 = 0.03363 0.00171 -0.00686 0.00406 AL1 6 0.678250 0.081611 0.389220 11.00000 0.01833 0.01584 = 0.01889 0.00110 0.00151 0.00029 P1 7 0.400923 -0.140902 0.205516 11.00000 0.03836 0.02410 = 0.03247 -0.00084 0.01588 -0.00338 O1 4 0.720401 0.106313 0.487956 11.00000 0.01894 0.01842 = 0.02028 0.00005 0.00237 -0.00208 O2 4 0.768634 0.150732 0.361461 11.00000 0.02488 0.01767 = 0.02046 0.00001 0.00392 -0.00286 O3 4 0.550480 0.137634 0.382299 11.00000 0.02354 0.02056 = 0.01971 -0.00088 0.00048 0.00287 O4 4 0.637383 0.057232 0.291100 11.00000 0.02135 0.01909 = 0.02075 -0.00061 0.00016 0.00092 O5 4 0.587058 0.012069 0.414967 11.00000 0.01854 0.01781 = 0.02525 0.00044 0.00354 0.00032 O6 4 0.806705 0.024348 0.401439 11.00000 0.01868 0.01773 = 0.02302 0.00257 0.00348 0.00103 N1 3 0.002118 0.224739 0.044297 11.00000 0.02688 0.03564 = 0.03575 0.00505 0.00290 0.00960 N2 3 0.319471 0.165370 0.149803 11.00000 0.02854 0.03886 = 0.02774 0.00325 -0.00073 0.00541 N3 3 0.240482 0.303279 0.021608 11.00000 0.04964 0.02335 = 0.04479 -0.00433 0.01550 -0.00444 C1 1 0.807023 0.155571 0.599140 11.00000 0.02194 0.02983 = 0.02090 -0.00232 0.00286 -0.00106 AFIX 137 H1A 2 0.733684 0.160883 0.613469 11.00000 -1.50000 H1B 2 0.854746 0.193598 0.615376 11.00000 -1.50000 H1C 2 0.843595 0.115594 0.620886 11.00000 -1.50000 AFIX 0 C2 1 0.790071 0.150370 0.518186 11.00000 0.01275 0.01633 = 0.02379 0.00052 0.00095 0.00557 C3 1 0.850292 0.193017 0.477556 11.00000 0.01512 0.01935 = 0.02378 -0.00061 0.00136 -0.00012 C4 1 0.833241 0.192663 0.400050 11.00000 0.01765 0.01674 = 0.02557 0.00342 0.00498 0.00357 C5 1 0.892991 0.242847 0.360888 11.00000 0.03182 0.02553 = 0.03053 0.00187 0.00928 -0.00575 AFIX 137 H5A 2 0.974354 0.234327 0.371103 11.00000 -1.50000 H5B 2 0.878417 0.287092 0.377195 11.00000 -1.50000 H5C 2 0.864628 0.239396 0.309181 11.00000 -1.50000 AFIX 0 C6 1 0.933019 0.239043 0.515688 11.00000 0.02256 0.02459 = 0.02773 0.00108 0.00462 0.00228 C7 1 0.382605 0.200262 0.339523 11.00000 0.02577 0.02907 = 0.02921 0.00456 0.00271 0.00680 AFIX 137 H7A 2 0.380142 0.201754 0.390760 11.00000 -1.50000 H7B 2 0.309473 0.185461 0.312681 11.00000 -1.50000 H7C 2 0.399165 0.244158 0.323145 11.00000 -1.50000 AFIX 0 C8 1 0.474386 0.152707 0.327058 11.00000 0.02037 0.01463 = 0.02766 0.00423 0.00382 -0.00266 C9 1 0.474603 0.125635 0.256705 11.00000 0.01902 0.02469 = 0.02073 0.00437 -0.00190 0.00048 C10 1 0.555080 0.077153 0.242402 11.00000 0.02173 0.02006 = 0.02028 0.00248 0.00106 -0.00509 C11 1 0.542557 0.046223 0.167939 11.00000 0.03038 0.02294 = 0.02356 -0.00165 -0.00111 -0.00050 AFIX 137 H11A 2 0.611441 0.021996 0.164431 11.00000 -1.50000 H11B 2 0.530057 0.080793 0.131442 11.00000 -1.50000 H11C 2 0.478152 0.016069 0.160251 11.00000 -1.50000 AFIX 0 C12 1 0.388036 0.147377 0.197765 11.00000 0.02437 0.02647 = 0.02786 0.00087 0.00416 0.00125 C13 1 0.513538 -0.092877 0.441513 11.00000 0.02916 0.02266 = 0.03382 0.00024 0.01193 -0.00362 AFIX 137 H13A 2 0.446551 -0.066225 0.443323 11.00000 -1.50000 H13B 2 0.535094 -0.117102 0.486577 11.00000 -1.50000 H13C 2 0.496695 -0.123954 0.401559 11.00000 -1.50000 AFIX 0 C14 1 0.610250 -0.048384 0.430767 11.00000 0.02581 0.02059 = 0.01449 -0.00141 0.00464 -0.00174 C15 1 0.723854 -0.073963 0.437640 11.00000 0.02797 0.01618 = 0.01980 0.00062 0.00533 0.00106 C16 1 0.817232 -0.036053 0.421841 11.00000 0.02124 0.02298 = 0.01380 -0.00302 0.00094 0.00224 C17 1 0.934637 -0.066669 0.429799 11.00000 0.02268 0.02574 = 0.02762 0.00022 0.00299 0.00616 AFIX 137 H17A 2 0.982926 -0.038316 0.406809 11.00000 -1.50000 H17B 2 0.928605 -0.109948 0.406903 11.00000 -1.50000 H17C 2 0.967603 -0.071358 0.480783 11.00000 -1.50000 AFIX 0 C18 1 0.743748 -0.142028 0.459795 11.00000 0.03119 0.02697 = 0.02559 -0.00289 0.00855 0.00067 MOLE 2 C19 1 0.302813 0.022971 0.014755 11.00000 0.05981 0.02735 = 0.04550 -0.01311 -0.01180 0.00793 AFIX 43 H19 2 0.347465 -0.011700 0.038490 11.00000 -1.20000 AFIX 0 C20 1 0.189627 0.026649 0.018590 11.00000 0.07628 0.04476 = 0.04867 -0.01000 0.01642 -0.02600 AFIX 43 H20 2 0.157145 -0.004881 0.045398 11.00000 -1.20000 AFIX 0 C21 1 0.122188 0.078051 -0.017947 11.00000 0.03118 0.09128 = 0.07521 -0.05747 0.00051 -0.00538 AFIX 43 H21 2 0.044516 0.081466 -0.015634 11.00000 -1.20000 AFIX 0 C22 1 0.173504 0.124151 -0.057957 11.00000 0.08355 0.04128 = 0.03134 -0.01548 -0.02649 0.02542 AFIX 43 H22 2 0.130081 0.158270 -0.083745 11.00000 -1.20000 AFIX 0 C23 1 0.288389 0.118644 -0.058863 11.00000 0.09084 0.04302 = 0.02895 -0.00885 0.01651 -0.00877 AFIX 43 H23 2 0.323622 0.149744 -0.084657 11.00000 -1.20000 AFIX 0 C24 1 0.351135 0.068461 -0.022647 11.00000 0.04628 0.05156 = 0.05181 -0.02672 0.01129 0.00183 AFIX 43 H24 2 0.429288 0.065473 -0.023727 11.00000 -1.20000 AFIX 0 MOLE 3 C25 1 0.159571 0.056151 0.759709 11.00000 0.05081 0.04232 = 0.02885 -0.00526 0.00106 0.00211 AFIX 43 H25 2 0.179498 0.011386 0.768181 11.00000 -1.20000 AFIX 0 C26 1 0.238278 0.099468 0.742955 11.00000 0.03371 0.05385 = 0.02791 -0.00859 -0.00152 0.00428 AFIX 43 H26 2 0.311812 0.084213 0.740616 11.00000 -1.20000 AFIX 0 C27 1 0.211670 0.165065 0.729446 11.00000 0.06929 0.04809 = 0.02820 -0.00826 -0.00527 -0.02474 AFIX 43 H27 2 0.265705 0.194561 0.716961 11.00000 -1.20000 AFIX 0 C28 1 0.099961 0.187586 0.734771 11.00000 0.12694 0.03725 = 0.02677 -0.01867 -0.02437 0.03335 AFIX 43 H28 2 0.079472 0.232281 0.726366 11.00000 -1.20000 AFIX 0 C29 1 0.020876 0.141223 0.752950 11.00000 0.04004 0.10093 = 0.02783 -0.03140 -0.00946 0.02190 AFIX 43 H29 2 -0.052854 0.154796 0.757112 11.00000 -1.20000 AFIX 0 C30 1 0.053130 0.076515 0.764360 11.00000 0.04859 0.06753 = 0.02864 -0.01598 0.00520 -0.01361 AFIX 43 H30 2 0.000431 0.045515 0.775659 11.00000 -1.20000 AFIX 0 MOLE 4 C31 1 0.391643 -0.197992 -0.033956 11.00000 0.07989 0.04772 = 0.06828 0.02944 -0.02416 -0.03534 AFIX 43 H31 2 0.442323 -0.210762 0.008304 11.00000 -1.20000 AFIX 0 C32 1 0.406782 -0.220307 -0.104961 11.00000 0.05413 0.01848 = 0.12740 0.00710 0.03988 -0.00289 AFIX 43 H32 2 0.467934 -0.248193 -0.109744 11.00000 -1.20000 AFIX 0 C33 1 0.329855 -0.199904 -0.165433 11.00000 0.08025 0.02995 = 0.05156 -0.00985 0.02833 -0.02139 AFIX 43 H33 2 0.337750 -0.214972 -0.211512 11.00000 -1.20000 AFIX 0 C34 1 0.244422 -0.158972 -0.158952 11.00000 0.05854 0.04580 = 0.05972 -0.00580 0.00353 -0.02174 AFIX 43 H34 2 0.194581 -0.144536 -0.200844 11.00000 -1.20000 AFIX 0 C35 1 0.228077 -0.137806 -0.093216 11.00000 0.05081 0.05062 = 0.07164 -0.00472 0.02853 -0.01406 AFIX 43 H35 2 0.166548 -0.109412 -0.090801 11.00000 -1.20000 AFIX 0 C36 1 0.297570 -0.156286 -0.031027 11.00000 0.08853 0.04297 = 0.04131 -0.01397 0.02567 -0.02527 AFIX 43 H36 2 0.283391 -0.141493 0.013822 11.00000 -1.20000 AFIX 0 MOLE 5 C37 1 0.109236 0.083908 0.222573 11.00000 0.05514 0.05018 = 0.04601 0.00773 0.00214 0.00022 AFIX 43 H37 2 0.082127 0.099135 0.175234 11.00000 -1.20000 AFIX 0 C38 1 0.198095 0.038758 0.235759 11.00000 0.04617 0.04139 = 0.04623 -0.00398 0.01991 -0.00206 AFIX 43 H38 2 0.229846 0.022441 0.197161 11.00000 -1.20000 AFIX 0 C39 1 0.240026 0.017724 0.305482 11.00000 0.03586 0.03439 = 0.05330 0.00101 0.00850 0.00028 AFIX 43 H39 2 0.301834 -0.011860 0.314648 11.00000 -1.20000 AFIX 0 C40 1 0.190614 0.040404 0.362079 11.00000 0.07033 0.04866 = 0.03658 -0.00122 0.00953 -0.00040 AFIX 43 H40 2 0.218300 0.025545 0.409493 11.00000 -1.20000 AFIX 0 C41 1 0.101392 0.084489 0.349053 11.00000 0.07213 0.05529 = 0.05655 -0.01181 0.03543 0.00290 AFIX 43 H41 2 0.068280 0.099601 0.387596 11.00000 -1.20000 AFIX 0 C42 1 0.060092 0.106724 0.279458 11.00000 0.04865 0.05174 = 0.07855 -0.00360 0.01626 0.01459 AFIX 43 H42 2 -0.000708 0.137016 0.270647 11.00000 -1.20000 AFIX 0 MOLE 6 F1 5 0.359919 -0.207861 0.161691 11.00000 0.04425 0.03399 = 0.06178 -0.01719 0.02073 -0.01141 F2 5 0.493512 -0.183037 0.261187 11.00000 0.04104 0.05743 = 0.05754 0.01064 0.00768 0.00783 F3 5 0.307991 -0.152291 0.256171 11.00000 0.04397 0.04161 = 0.04375 0.00382 0.02443 0.00069 F4 5 0.309212 -0.098589 0.150108 11.00000 0.07473 0.05342 = 0.04017 0.01262 0.01357 0.02404 F5 5 0.494041 -0.129331 0.154726 11.00000 0.06170 0.04587 = 0.05267 -0.00976 0.03664 -0.01840 F6 5 0.444185 -0.074433 0.250478 11.00000 0.07920 0.03656 = 0.04930 -0.01502 0.02970 -0.01910 HKLF 4 ; 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 0.191766(19) 0.196667(11) 0.055869(13) 0.02891(7) Uani 1 1 d . . . Al1 Al 0.67825(7) 0.08161(4) 0.38922(4) 0.01795(17) Uani 1 1 d . . . P1 P 0.40092(7) -0.14090(4) 0.20552(4) 0.03045(19) Uani 1 1 d . . . O1 O 0.72040(15) 0.10631(9) 0.48796(9) 0.0194(4) Uani 1 1 d . . . O2 O 0.76863(16) 0.15073(9) 0.36146(10) 0.0210(4) Uani 1 1 d . . . O3 O 0.55048(16) 0.13763(9) 0.38230(10) 0.0217(4) Uani 1 1 d . . . O4 O 0.63738(15) 0.05723(9) 0.29110(10) 0.0209(4) Uani 1 1 d . . . O5 O 0.58706(15) 0.01207(9) 0.41497(10) 0.0206(4) Uani 1 1 d . . . O6 O 0.80670(15) 0.02435(9) 0.40144(10) 0.0199(4) Uani 1 1 d . . . N1 N 0.0021(2) 0.22474(13) 0.04430(14) 0.0331(6) Uani 1 1 d . . . N2 N 0.3195(2) 0.16537(13) 0.14980(14) 0.0325(6) Uani 1 1 d . . . N3 N 0.2405(2) 0.30328(13) 0.02161(15) 0.0384(7) Uani 1 1 d . . . C1 C 0.8070(2) 0.15557(14) 0.59914(14) 0.0244(6) Uani 1 1 d . . . H1A H 0.7337 0.1609 0.6135 0.037 Uiso 1 1 calc R . . H1B H 0.8547 0.1936 0.6154 0.037 Uiso 1 1 calc R . . H1C H 0.8436 0.1156 0.6209 0.037 Uiso 1 1 calc R . . C2 C 0.7901(2) 0.15037(12) 0.51819(14) 0.0179(5) Uani 1 1 d . . . C3 C 0.8503(2) 0.19302(13) 0.47756(15) 0.0197(5) Uani 1 1 d . . . C4 C 0.8332(2) 0.19266(13) 0.40005(15) 0.0199(6) Uani 1 1 d . . . C5 C 0.8930(3) 0.24285(14) 0.36089(16) 0.0289(7) Uani 1 1 d . . . H5A H 0.9744 0.2343 0.3711 0.043 Uiso 1 1 calc R . . H5B H 0.8784 0.2871 0.3772 0.043 Uiso 1 1 calc R . . H5C H 0.8646 0.2394 0.3092 0.043 Uiso 1 1 calc R . . C6 C 0.9330(2) 0.23904(14) 0.51569(15) 0.0250(6) Uani 1 1 d . . . C7 C 0.3826(2) 0.20026(14) 0.33952(16) 0.0283(6) Uani 1 1 d . . . H7A H 0.3801 0.2018 0.3908 0.043 Uiso 1 1 calc R . . H7B H 0.3095 0.1855 0.3127 0.043 Uiso 1 1 calc R . . H7C H 0.3992 0.2442 0.3231 0.043 Uiso 1 1 calc R . . C8 C 0.4744(2) 0.15271(13) 0.32706(15) 0.0210(6) Uani 1 1 d . . . C9 C 0.4746(2) 0.12563(14) 0.25670(14) 0.0222(6) Uani 1 1 d . . . C10 C 0.5551(2) 0.07715(13) 0.24240(14) 0.0211(6) Uani 1 1 d . . . C11 C 0.5426(2) 0.04622(14) 0.16794(15) 0.0264(6) Uani 1 1 d . . . H11A H 0.6114 0.0220 0.1644 0.040 Uiso 1 1 calc R . . H11B H 0.5301 0.0808 0.1314 0.040 Uiso 1 1 calc R . . H11C H 0.4782 0.0161 0.1603 0.040 Uiso 1 1 calc R . . C12 C 0.3880(2) 0.14738(14) 0.19776(16) 0.0263(6) Uani 1 1 d . . . C13 C 0.5135(2) -0.09288(14) 0.44151(16) 0.0278(6) Uani 1 1 d . . . H13A H 0.4466 -0.0662 0.4433 0.042 Uiso 1 1 calc R . . H13B H 0.5351 -0.1171 0.4866 0.042 Uiso 1 1 calc R . . H13C H 0.4967 -0.1240 0.4016 0.042 Uiso 1 1 calc R . . C14 C 0.6102(2) -0.04838(13) 0.43077(14) 0.0202(6) Uani 1 1 d . . . C15 C 0.7239(2) -0.07396(13) 0.43764(14) 0.0212(6) Uani 1 1 d . . . C16 C 0.8172(2) -0.03605(13) 0.42184(14) 0.0196(6) Uani 1 1 d . . . C17 C 0.9346(2) -0.06667(14) 0.42980(15) 0.0256(6) Uani 1 1 d . . . H17A H 0.9829 -0.0383 0.4068 0.038 Uiso 1 1 calc R . . H17B H 0.9286 -0.1099 0.4069 0.038 Uiso 1 1 calc R . . H17C H 0.9676 -0.0714 0.4808 0.038 Uiso 1 1 calc R . . C18 C 0.7437(3) -0.14203(15) 0.45980(16) 0.0275(6) Uani 1 1 d . . . C19 C 0.3028(3) 0.02297(17) 0.0148(2) 0.0471(9) Uani 1 1 d . . . H19 H 0.3475 -0.0117 0.0385 0.056 Uiso 1 1 calc R . . C20 C 0.1896(4) 0.0266(2) 0.0186(2) 0.0560(11) Uani 1 1 d . . . H20 H 0.1571 -0.0049 0.0454 0.067 Uiso 1 1 calc R . . C21 C 0.1222(3) 0.0781(3) -0.0179(3) 0.0671(14) Uani 1 1 d . . . H21 H 0.0445 0.0815 -0.0156 0.081 Uiso 1 1 calc R . . C22 C 0.1735(4) 0.12415(19) -0.05796(19) 0.0569(12) Uani 1 1 d . . . H22 H 0.1301 0.1583 -0.0837 0.068 Uiso 1 1 calc R . . C23 C 0.2884(4) 0.11864(19) -0.05886(19) 0.0536(11) Uani 1 1 d . . . H23 H 0.3236 0.1497 -0.0847 0.064 Uiso 1 1 calc R . . C24 C 0.3511(3) 0.06846(19) -0.0226(2) 0.0496(10) Uani 1 1 d . . . H24 H 0.4293 0.0655 -0.0237 0.060 Uiso 1 1 calc R . . C25 C 0.1596(3) 0.05615(18) 0.75971(17) 0.0415(8) Uani 1 1 d . . . H25 H 0.1795 0.0114 0.7682 0.050 Uiso 1 1 calc R . . C26 C 0.2383(3) 0.09947(18) 0.74295(17) 0.0394(8) Uani 1 1 d . . . H26 H 0.3118 0.0842 0.7406 0.047 Uiso 1 1 calc R . . C27 C 0.2117(4) 0.16506(19) 0.72945(18) 0.0504(10) Uani 1 1 d . . . H27 H 0.2657 0.1946 0.7170 0.060 Uiso 1 1 calc R . . C28 C 0.1000(5) 0.1876(2) 0.73477(19) 0.0687(15) Uani 1 1 d . . . H28 H 0.0795 0.2323 0.7264 0.082 Uiso 1 1 calc R . . C29 C 0.0209(3) 0.1412(3) 0.75295(19) 0.0583(12) Uani 1 1 d . . . H29 H -0.0529 0.1548 0.7571 0.070 Uiso 1 1 calc R . . C30 C 0.0531(3) 0.0765(2) 0.76436(18) 0.0485(10) Uani 1 1 d . . . H30 H 0.0004 0.0455 0.7757 0.058 Uiso 1 1 calc R . . C31 C 0.3916(4) -0.1980(2) -0.0340(3) 0.0703(15) Uani 1 1 d . . . H31 H 0.4423 -0.2108 0.0083 0.084 Uiso 1 1 calc R . . C32 C 0.4068(4) -0.22031(17) -0.1050(3) 0.0637(13) Uani 1 1 d . . . H32 H 0.4679 -0.2482 -0.1097 0.076 Uiso 1 1 calc R . . C33 C 0.3299(4) -0.19990(18) -0.1654(2) 0.0519(10) Uani 1 1 d . . . H33 H 0.3378 -0.2150 -0.2115 0.062 Uiso 1 1 calc R . . C34 C 0.2444(4) -0.15897(19) -0.1590(2) 0.0557(10) Uani 1 1 d . . . H34 H 0.1946 -0.1445 -0.2008 0.067 Uiso 1 1 calc R . . C35 C 0.2281(4) -0.1378(2) -0.0932(2) 0.0555(10) Uani 1 1 d . . . H35 H 0.1665 -0.1094 -0.0908 0.067 Uiso 1 1 calc R . . C36 C 0.2976(4) -0.15629(19) -0.0310(2) 0.0559(11) Uani 1 1 d . . . H36 H 0.2834 -0.1415 0.0138 0.067 Uiso 1 1 calc R . . C37 C 0.1092(3) 0.08391(19) 0.2226(2) 0.0514(10) Uani 1 1 d . . . H37 H 0.0821 0.0991 0.1752 0.062 Uiso 1 1 calc R . . C38 C 0.1981(3) 0.03876(17) 0.2358(2) 0.0431(8) Uani 1 1 d . . . H38 H 0.2298 0.0224 0.1972 0.052 Uiso 1 1 calc R . . C39 C 0.2400(3) 0.01772(17) 0.3055(2) 0.0412(8) Uani 1 1 d . . . H39 H 0.3018 -0.0119 0.3146 0.049 Uiso 1 1 calc R . . C40 C 0.1906(4) 0.04040(19) 0.3621(2) 0.0519(10) Uani 1 1 d . . . H40 H 0.2183 0.0255 0.4095 0.062 Uiso 1 1 calc R . . C41 C 0.1014(4) 0.0845(2) 0.3491(2) 0.0583(11) Uani 1 1 d . . . H41 H 0.0683 0.0996 0.3876 0.070 Uiso 1 1 calc R . . C42 C 0.0601(3) 0.1067(2) 0.2795(2) 0.0591(11) Uani 1 1 d . . . H42 H -0.0007 0.1370 0.2706 0.071 Uiso 1 1 calc R . . F1 F 0.35992(16) -0.20786(9) 0.16169(11) 0.0453(5) Uani 1 1 d . . . F2 F 0.49351(17) -0.18304(10) 0.26119(12) 0.0522(5) Uani 1 1 d . . . F3 F 0.30799(16) -0.15229(9) 0.25617(10) 0.0410(5) Uani 1 1 d . . . F4 F 0.30921(19) -0.09859(10) 0.15011(11) 0.0558(6) Uani 1 1 d . . . F5 F 0.49404(18) -0.12933(10) 0.15473(11) 0.0500(5) Uani 1 1 d . . . F6 F 0.44418(19) -0.07443(9) 0.25048(11) 0.0527(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02565(13) 0.02257(12) 0.03363(13) 0.00171(9) -0.00686(9) 0.00406(9) Al1 0.0183(4) 0.0158(4) 0.0189(4) 0.0011(3) 0.0015(3) 0.0003(3) P1 0.0384(5) 0.0241(4) 0.0325(4) -0.0008(3) 0.0159(4) -0.0034(3) O1 0.0189(10) 0.0184(9) 0.0203(10) 0.0000(7) 0.0024(8) -0.0021(7) O2 0.0249(10) 0.0177(9) 0.0205(10) 0.0000(8) 0.0039(8) -0.0029(8) O3 0.0235(10) 0.0206(10) 0.0197(10) -0.0009(8) 0.0005(8) 0.0029(8) O4 0.0213(10) 0.0191(9) 0.0208(10) -0.0006(8) 0.0002(8) 0.0009(8) O5 0.0185(10) 0.0178(10) 0.0252(10) 0.0004(8) 0.0035(8) 0.0003(7) O6 0.0187(10) 0.0177(9) 0.0230(10) 0.0026(8) 0.0035(8) 0.0010(7) N1 0.0269(14) 0.0356(15) 0.0357(15) 0.0051(12) 0.0029(12) 0.0096(12) N2 0.0285(14) 0.0389(15) 0.0277(14) 0.0032(12) -0.0007(12) 0.0054(12) N3 0.0496(18) 0.0234(14) 0.0448(17) -0.0043(12) 0.0155(14) -0.0044(12) C1 0.0219(15) 0.0298(15) 0.0209(14) -0.0023(12) 0.0029(12) -0.0011(12) C2 0.0127(13) 0.0163(13) 0.0238(14) 0.0005(10) 0.0010(11) 0.0056(10) C3 0.0151(13) 0.0194(13) 0.0238(14) -0.0006(11) 0.0014(11) -0.0001(11) C4 0.0176(13) 0.0167(13) 0.0256(14) 0.0034(11) 0.0050(11) 0.0036(11) C5 0.0318(17) 0.0255(15) 0.0305(16) 0.0019(12) 0.0093(13) -0.0058(13) C6 0.0226(15) 0.0246(15) 0.0277(15) 0.0011(12) 0.0046(12) 0.0023(12) C7 0.0258(15) 0.0291(16) 0.0292(16) 0.0046(13) 0.0027(12) 0.0068(13) C8 0.0204(14) 0.0146(13) 0.0277(15) 0.0042(11) 0.0038(12) -0.0027(11) C9 0.0190(14) 0.0247(14) 0.0207(14) 0.0044(11) -0.0019(11) 0.0005(11) C10 0.0217(14) 0.0201(14) 0.0203(14) 0.0025(11) 0.0011(11) -0.0051(11) C11 0.0304(16) 0.0229(15) 0.0236(15) -0.0016(12) -0.0011(12) -0.0005(12) C12 0.0244(15) 0.0265(15) 0.0279(16) 0.0009(12) 0.0042(13) 0.0012(12) C13 0.0292(16) 0.0227(15) 0.0338(17) 0.0002(12) 0.0119(13) -0.0036(12) C14 0.0258(15) 0.0206(14) 0.0145(13) -0.0014(10) 0.0046(11) -0.0017(11) C15 0.0280(15) 0.0162(13) 0.0198(14) 0.0006(10) 0.0053(12) 0.0011(11) C16 0.0212(14) 0.0230(14) 0.0138(13) -0.0030(10) 0.0009(11) 0.0022(11) C17 0.0227(15) 0.0257(15) 0.0276(15) 0.0002(12) 0.0030(12) 0.0062(12) C18 0.0312(17) 0.0270(16) 0.0256(15) -0.0029(12) 0.0086(13) 0.0007(13) C19 0.060(3) 0.0274(18) 0.045(2) -0.0131(16) -0.0118(19) 0.0079(17) C20 0.076(3) 0.045(2) 0.049(2) -0.0100(19) 0.016(2) -0.026(2) C21 0.031(2) 0.091(4) 0.075(3) -0.057(3) 0.001(2) -0.005(2) C22 0.084(3) 0.041(2) 0.031(2) -0.0155(16) -0.026(2) 0.025(2) C23 0.091(3) 0.043(2) 0.0290(19) -0.0089(16) 0.017(2) -0.009(2) C24 0.046(2) 0.052(2) 0.052(2) -0.0267(19) 0.0113(19) 0.0018(18) C25 0.051(2) 0.042(2) 0.0289(18) -0.0053(15) 0.0011(16) 0.0021(17) C26 0.0337(18) 0.054(2) 0.0279(17) -0.0086(15) -0.0015(14) 0.0043(16) C27 0.069(3) 0.048(2) 0.0282(18) -0.0083(16) -0.0053(18) -0.025(2) C28 0.127(4) 0.037(2) 0.027(2) -0.0187(16) -0.024(2) 0.033(3) C29 0.040(2) 0.101(4) 0.0278(19) -0.031(2) -0.0095(16) 0.022(2) C30 0.049(2) 0.068(3) 0.0286(19) -0.0160(17) 0.0052(16) -0.014(2) C31 0.080(3) 0.048(3) 0.068(3) 0.029(2) -0.024(3) -0.035(2) C32 0.054(3) 0.0185(17) 0.127(4) 0.007(2) 0.040(3) -0.0029(17) C33 0.080(3) 0.0300(19) 0.052(2) -0.0098(17) 0.028(2) -0.021(2) C34 0.059(3) 0.046(2) 0.060(3) -0.0058(19) 0.004(2) -0.022(2) C35 0.051(2) 0.051(2) 0.072(3) -0.005(2) 0.029(2) -0.0141(19) C36 0.089(3) 0.043(2) 0.041(2) -0.0140(18) 0.026(2) -0.025(2) C37 0.055(2) 0.050(2) 0.046(2) 0.0077(18) 0.0021(19) 0.0002(19) C38 0.046(2) 0.041(2) 0.046(2) -0.0040(16) 0.0199(17) -0.0021(17) C39 0.0359(19) 0.0344(19) 0.053(2) 0.0010(16) 0.0085(17) 0.0003(15) C40 0.070(3) 0.049(2) 0.037(2) -0.0012(17) 0.0095(19) 0.000(2) C41 0.072(3) 0.055(3) 0.057(3) -0.012(2) 0.035(2) 0.003(2) C42 0.049(2) 0.052(2) 0.079(3) -0.004(2) 0.016(2) 0.0146(19) F1 0.0443(12) 0.0340(11) 0.0618(13) -0.0172(9) 0.0207(10) -0.0114(9) F2 0.0410(12) 0.0574(13) 0.0575(13) 0.0106(10) 0.0077(10) 0.0078(10) F3 0.0440(11) 0.0416(11) 0.0438(11) 0.0038(9) 0.0244(9) 0.0007(9) F4 0.0747(15) 0.0534(13) 0.0402(12) 0.0126(10) 0.0136(11) 0.0240(11) F5 0.0617(14) 0.0459(12) 0.0527(12) -0.0098(10) 0.0366(11) -0.0184(10) F6 0.0792(16) 0.0366(11) 0.0493(12) -0.0150(9) 0.0297(11) -0.0191(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.175(2) . ? Ag1 N1 2.282(2) . ? Ag1 N3 2.325(3) . ? Ag1 C22 2.541(3) . ? Al1 O4 1.8634(19) . ? Al1 O3 1.8645(19) . ? Al1 O5 1.8747(19) . ? Al1 O2 1.8765(19) . ? Al1 O1 1.8770(19) . ? Al1 O6 1.8801(19) . ? P1 F4 1.591(2) . ? P1 F1 1.5930(19) . ? P1 F3 1.5934(18) . ? P1 F2 1.597(2) . ? P1 F5 1.5975(19) . ? P1 F6 1.600(2) . ? O1 C2 1.262(3) . ? O2 C4 1.262(3) . ? O3 C8 1.268(3) . ? O4 C10 1.262(3) . ? O5 C14 1.260(3) . ? O6 C16 1.263(3) . ? N1 C6 1.144(4) 4_465 ? N2 C12 1.145(4) . ? N3 C18 1.150(4) 2_655 ? C1 C2 1.486(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.417(4) . ? C3 C4 1.418(4) . ? C3 C6 1.429(4) . ? C4 C5 1.493(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N1 1.144(4) 4_666 ? C7 C8 1.493(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.417(4) . ? C9 C10 1.417(4) . ? C9 C12 1.420(4) . ? C10 C11 1.499(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C13 C14 1.491(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.420(4) . ? C15 C16 1.414(4) . ? C15 C18 1.426(4) . ? C16 C17 1.498(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N3 1.150(4) 2_645 ? C19 C24 1.336(5) . ? C19 C20 1.356(5) . ? C19 H19 0.9300 . ? C20 C21 1.395(6) . ? C20 H20 0.9300 . ? C21 C22 1.393(6) . ? C21 H21 0.9300 . ? C22 C23 1.366(6) . ? C22 H22 0.9300 . ? C23 C24 1.349(5) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.341(5) . ? C25 C26 1.349(5) . ? C25 H25 0.9300 . ? C26 C27 1.359(5) . ? C26 H26 0.9300 . ? C27 C28 1.416(6) . ? C27 H27 0.9300 . ? C28 C29 1.402(6) . ? C28 H28 0.9300 . ? C29 C30 1.352(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.399(6) . ? C31 C32 1.437(7) . ? C31 H31 0.9300 . ? C32 C33 1.369(6) . ? C32 H32 0.9300 . ? C33 C34 1.322(6) . ? C33 H33 0.9300 . ? C34 C35 1.342(5) . ? C34 H34 0.9300 . ? C35 C36 1.339(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.371(5) . ? C37 C42 1.378(5) . ? C37 H37 0.9300 . ? C38 C39 1.365(5) . ? C38 H38 0.9300 . ? C39 C40 1.374(5) . ? C39 H39 0.9300 . ? C40 C41 1.360(5) . ? C40 H40 0.9300 . ? C41 C42 1.369(6) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 131.86(9) . . ? N2 Ag1 N3 108.24(10) . . ? N1 Ag1 N3 92.25(10) . . ? N2 Ag1 C22 116.32(11) . . ? N1 Ag1 C22 97.69(12) . . ? N3 Ag1 C22 106.21(13) . . ? O4 Al1 O3 91.83(8) . . ? O4 Al1 O5 90.10(8) . . ? O3 Al1 O5 87.95(8) . . ? O4 Al1 O2 88.74(8) . . ? O3 Al1 O2 92.07(8) . . ? O5 Al1 O2 178.85(9) . . ? O4 Al1 O1 179.62(10) . . ? O3 Al1 O1 88.40(8) . . ? O5 Al1 O1 90.20(8) . . ? O2 Al1 O1 90.95(8) . . ? O4 Al1 O6 90.80(8) . . ? O3 Al1 O6 176.96(9) . . ? O5 Al1 O6 90.54(8) . . ? O2 Al1 O6 89.50(8) . . ? O1 Al1 O6 88.97(8) . . ? F4 P1 F1 90.53(12) . . ? F4 P1 F3 89.86(11) . . ? F1 P1 F3 90.34(10) . . ? F4 P1 F2 179.67(13) . . ? F1 P1 F2 89.74(12) . . ? F3 P1 F2 90.33(11) . . ? F4 P1 F5 90.07(12) . . ? F1 P1 F5 89.74(10) . . ? F3 P1 F5 179.89(12) . . ? F2 P1 F5 89.74(12) . . ? F4 P1 F6 90.59(12) . . ? F1 P1 F6 178.87(13) . . ? F3 P1 F6 89.83(10) . . ? F2 P1 F6 89.14(12) . . ? F5 P1 F6 90.09(10) . . ? C2 O1 Al1 130.52(17) . . ? C4 O2 Al1 130.24(17) . . ? C8 O3 Al1 129.80(17) . . ? C10 O4 Al1 130.06(18) . . ? C14 O5 Al1 131.19(17) . . ? C16 O6 Al1 130.41(17) . . ? C6 N1 Ag1 143.3(2) 4_465 . ? C12 N2 Ag1 177.7(3) . . ? C18 N3 Ag1 145.2(2) 2_655 . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.2(2) . . ? O1 C2 C1 116.9(2) . . ? C3 C2 C1 120.9(2) . . ? C2 C3 C4 123.4(2) . . ? C2 C3 C6 119.1(2) . . ? C4 C3 C6 117.4(2) . . ? O2 C4 C3 122.5(2) . . ? O2 C4 C5 117.3(2) . . ? C3 C4 C5 120.2(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 177.2(3) 4_666 . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 122.3(2) . . ? O3 C8 C7 116.8(2) . . ? C9 C8 C7 121.0(2) . . ? C8 C9 C10 123.5(2) . . ? C8 C9 C12 118.1(2) . . ? C10 C9 C12 118.4(2) . . ? O4 C10 C9 122.3(2) . . ? O4 C10 C11 117.5(2) . . ? C9 C10 C11 120.2(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 179.0(3) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 121.7(2) . . ? O5 C14 C13 117.6(2) . . ? C15 C14 C13 120.7(2) . . ? C16 C15 C14 123.4(2) . . ? C16 C15 C18 118.5(2) . . ? C14 C15 C18 118.0(2) . . ? O6 C16 C15 122.5(2) . . ? O6 C16 C17 117.1(2) . . ? C15 C16 C17 120.4(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 179.3(3) 2_645 . ? C24 C19 C20 120.9(4) . . ? C24 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 119.6(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 118.7(4) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C23 C22 C21 119.2(4) . . ? C23 C22 Ag1 97.3(2) . . ? C21 C22 Ag1 84.7(2) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? Ag1 C22 H22 88.0 . . ? C24 C23 C22 120.5(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C19 C24 C23 121.1(4) . . ? C19 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C30 C25 C26 121.2(4) . . ? C30 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C27 121.0(4) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C28 118.6(4) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C29 C28 C27 118.7(3) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C30 C29 C28 119.2(4) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C25 C30 C29 121.3(4) . . ? C25 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C36 C31 C32 117.3(4) . . ? C36 C31 H31 121.4 . . ? C32 C31 H31 121.4 . . ? C33 C32 C31 119.0(4) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C34 C33 C32 120.6(4) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 121.4(4) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C36 C35 C34 122.1(4) . . ? C36 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C35 C36 C31 119.6(4) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? C38 C37 C42 120.0(4) . . ? C38 C37 H37 120.0 . . ? C42 C37 H37 120.0 . . ? C39 C38 C37 120.1(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 119.8(3) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 120.3(4) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.3(4) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 119.5(4) . . ? C41 C42 H42 120.2 . . ? C37 C42 H42 120.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.61 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.504 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.071 data_2b _database_code_depnum_ccdc_archive 'CCDC 872085' #TrackingRef '- complete_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2b _chemical_melting_point ? _chemical_formula_moiety 'C19 H22 Ag Al N3 O7, F6 P, 2(C H4 O)' _chemical_formula_sum 'C21 H30 Ag Al F6 N3 O9 P' _chemical_formula_weight 748.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3849(9) _cell_length_b 12.2052(10) _cell_length_c 13.1682(11) _cell_angle_alpha 109.1660(18) _cell_angle_beta 106.1805(18) _cell_angle_gamma 105.8493(19) _cell_volume 1519.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3662 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 23.16 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8447 _exptl_absorpt_correction_T_max 0.8925 _exptl_absorpt_process_details MULABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17889 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6129 _reflns_number_gt 4372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER smart' _computing_cell_refinement 'BRUKER saint' _computing_data_reduction 'BRUKER saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+1.0558P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6129 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1876 _refine_ls_wR_factor_gt 0.1714 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL 2b in P-1 CELL 0.71073 11.3849 12.2052 13.1682 109.166 106.180 105.849 ZERR 4.00 0.0009 0.0010 0.0011 0.002 0.002 0.002 LATT 1 SFAC C H N O AL AG P F UNIT 42 60 6 18 2 2 2 12 TEMP -173.160 L.S. 8 SIZE 0.14 0.21 0.15 BOND BOND$H ACTA FMAP 2 PLAN -40 WGHT 0.0955 1.0558 FVAR 0.86387 MOLE 1 AG1 6 0.568693 0.402765 0.484047 11.00000 0.05429 0.05309 = 0.02547 0.00611 0.01422 -0.01621 AL1 5 0.938077 0.755252 0.183127 11.00000 0.02301 0.01728 = 0.02162 0.00815 0.00836 0.00864 O1 4 0.900817 0.600556 0.062978 11.00000 0.02197 0.01735 = 0.02931 0.00579 0.00710 0.00889 O2 4 0.883967 0.817027 0.073747 11.00000 0.03028 0.01908 = 0.02193 0.00817 0.01047 0.01290 O3 4 0.971086 0.908592 0.304593 11.00000 0.02842 0.01998 = 0.02128 0.00882 0.00852 0.00899 O4 4 1.112703 0.818440 0.195067 11.00000 0.02292 0.01718 = 0.02638 0.00847 0.00803 0.00764 O5 4 0.993589 0.693206 0.291632 11.00000 0.02719 0.02358 = 0.02832 0.01455 0.00746 0.00900 O6 4 0.761257 0.692643 0.170448 11.00000 0.02628 0.02453 = 0.03533 0.01698 0.01416 0.01171 N1 3 0.659880 0.517269 -0.323496 11.00000 0.03582 0.04024 = 0.02671 0.00590 0.00717 0.00466 N2 3 1.364312 1.256052 0.417976 11.00000 0.04247 0.03060 = 0.04049 0.00784 0.00421 0.00063 N3 3 0.662777 0.456960 0.374482 11.00000 0.05113 0.05008 = 0.04174 0.02541 0.02570 0.01679 C1 1 0.804401 0.419642 -0.117447 11.00000 0.02944 0.02223 = 0.03897 0.00092 0.01086 0.00841 AFIX 137 H1A 2 0.832551 0.381791 -0.064985 11.00000 -1.50000 H1B 2 0.852457 0.414211 -0.168932 11.00000 -1.50000 H1C 2 0.708121 0.373859 -0.165373 11.00000 -1.50000 AFIX 0 C2 1 0.835122 0.555949 -0.045593 11.00000 0.01707 0.01952 = 0.03046 0.00403 0.01123 0.00676 C3 1 0.792171 0.629067 -0.099696 11.00000 0.02116 0.02234 = 0.02295 0.00427 0.00514 0.00484 C4 1 0.825106 0.760142 -0.036404 11.00000 0.02508 0.02608 = 0.02374 0.01094 0.01165 0.01118 C5 1 0.791787 0.836460 -0.099749 11.00000 0.03983 0.02957 = 0.02728 0.01252 0.01103 0.01336 AFIX 137 H5A 2 0.793815 0.914575 -0.044649 11.00000 -1.50000 H5B 2 0.702365 0.787132 -0.163467 11.00000 -1.50000 H5C 2 0.857338 0.857709 -0.132663 11.00000 -1.50000 AFIX 0 C6 1 0.720440 0.569076 -0.224087 11.00000 0.02959 0.02404 = 0.03098 0.00722 0.01453 0.00676 C7 1 1.061090 1.124308 0.439328 11.00000 0.05385 0.02568 = 0.02367 0.00482 0.01493 0.01557 AFIX 137 H7A 2 0.970059 1.101718 0.435738 11.00000 -1.50000 H7B 2 1.086078 1.198191 0.423076 11.00000 -1.50000 H7C 2 1.123118 1.144523 0.517916 11.00000 -1.50000 AFIX 0 C8 1 1.067236 1.014877 0.349423 11.00000 0.03638 0.02568 = 0.01749 0.01250 0.00706 0.01377 C9 1 1.180605 1.032608 0.320267 11.00000 0.03027 0.02013 = 0.02045 0.00821 0.00430 0.00512 C10 1 1.197991 0.930195 0.244074 11.00000 0.02265 0.02710 = 0.02092 0.01248 0.00345 0.00874 C11 1 1.319674 0.952733 0.218727 11.00000 0.02604 0.03291 = 0.03904 0.01821 0.00912 0.00986 AFIX 137 H11A 2 1.343840 0.879897 0.208806 11.00000 -1.50000 H11B 2 1.393520 1.029143 0.284281 11.00000 -1.50000 H11C 2 1.301769 0.963994 0.146408 11.00000 -1.50000 AFIX 0 C12 1 1.282619 1.157198 0.375961 11.00000 0.03828 0.02957 = 0.02471 0.00911 0.00650 0.00736 C13 1 1.001738 0.586865 0.412167 11.00000 0.03997 0.03406 = 0.02518 0.01528 0.00416 0.01313 AFIX 137 H13A 2 1.097072 0.623227 0.429331 11.00000 -1.50000 H13B 2 0.968782 0.494284 0.377749 11.00000 -1.50000 H13C 2 0.988635 0.617881 0.485123 11.00000 -1.50000 AFIX 0 C14 1 0.926538 0.625326 0.327164 11.00000 0.03485 0.01554 = 0.01873 0.00414 0.00828 0.01170 C15 1 0.786806 0.587463 0.290253 11.00000 0.03219 0.02063 = 0.02120 0.00594 0.01303 0.00919 C16 1 0.710885 0.623583 0.212585 11.00000 0.03176 0.02307 = 0.03374 0.01220 0.01765 0.01616 C17 1 0.562073 0.580329 0.177258 11.00000 0.02978 0.05476 = 0.05807 0.03425 0.02347 0.01771 AFIX 137 H17A 2 0.529277 0.629367 0.139400 11.00000 -1.50000 H17B 2 0.542734 0.593347 0.247298 11.00000 -1.50000 H17C 2 0.517551 0.490179 0.122132 11.00000 -1.50000 AFIX 0 C18 1 0.718119 0.513418 0.336526 11.00000 0.04032 0.02913 = 0.02693 0.01149 0.01331 0.01386 MOLE 2 P1 7 0.874337 0.215125 0.166305 11.00000 0.03788 0.03211 = 0.03225 0.01010 0.01276 0.01724 F1 8 0.916036 0.170431 0.059813 11.00000 0.04671 0.06927 = 0.04253 0.00769 0.02274 0.01569 F2 8 0.721114 0.130831 0.076891 11.00000 0.03790 0.05943 = 0.05212 0.00970 0.01231 0.01119 F3 8 0.830621 0.260055 0.272601 11.00000 0.08016 0.05975 = 0.05594 0.01093 0.04365 0.02698 F4 8 1.025225 0.298447 0.255154 11.00000 0.04108 0.07438 = 0.04618 0.00378 0.00250 0.01469 F5 8 0.863495 0.332774 0.143233 11.00000 0.09359 0.04176 = 0.06926 0.02608 0.01481 0.03063 F6 8 0.879192 0.096202 0.189012 11.00000 0.11740 0.04915 = 0.05217 0.02195 0.01794 0.04533 MOLE 3 O7 4 0.413134 0.698553 -0.002748 11.00000 0.04510 0.09195 = 0.09059 0.05876 0.02532 0.03897 H7D 2 0.343737 0.707352 -0.032060 11.00000 0.09171 C19 1 0.512128 0.779198 -0.021041 11.00000 0.05472 0.11247 = 0.10667 0.06673 0.03149 0.04514 AFIX 137 H19A 2 0.523768 0.867061 0.019704 11.00000 -1.50000 H19B 2 0.484478 0.755029 -0.105443 11.00000 -1.50000 H19C 2 0.596771 0.771414 0.009934 11.00000 -1.50000 AFIX 0 MOLE 4 O8 4 0.722021 0.074926 0.349600 11.00000 0.16713 0.10971 = 0.14922 0.07747 0.10500 0.08233 AFIX 3 H8 2 0.754690 0.121311 0.326153 11.00000 -1.50000 AFIX 0 C20 1 0.664718 -0.062671 0.304114 11.00000 0.09785 0.07363 = 0.16036 0.01280 0.04218 0.06017 AFIX 137 H20A 2 0.730119 -0.095683 0.287626 11.00000 -1.50000 H20B 2 0.584325 -0.099114 0.231507 11.00000 -1.50000 H20C 2 0.641216 -0.085652 0.362653 11.00000 -1.50000 AFIX 0 MOLE 5 O9 4 0.622712 0.207839 0.473464 11.00000 0.12316 0.10860 = 0.08763 0.04538 0.04692 0.06349 AFIX 3 H9 2 0.653672 0.167863 0.434872 11.00000 -1.50000 AFIX 0 C21 1 0.639022 0.175087 0.562315 11.00000 0.14542 0.11907 = 0.05498 0.04855 0.03168 0.09031 AFIX 137 H21A 2 0.734475 0.209179 0.612040 11.00000 -1.50000 H21B 2 0.601390 0.082540 0.530770 11.00000 -1.50000 H21C 2 0.593148 0.209551 0.609222 11.00000 -1.50000 HKLF 4 ; 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 0.56869(5) 0.40276(5) 0.48405(4) 0.0571(2) Uani 1 1 d . . . Al1 Al 0.93808(14) 0.75525(12) 0.18313(12) 0.0208(3) Uani 1 1 d . . . O1 O 0.9008(3) 0.6006(3) 0.0630(3) 0.0247(7) Uani 1 1 d . . . O2 O 0.8840(3) 0.8170(3) 0.0737(3) 0.0233(7) Uani 1 1 d . . . O3 O 0.9711(3) 0.9086(3) 0.3046(3) 0.0238(7) Uani 1 1 d . . . O4 O 1.1127(3) 0.8184(3) 0.1951(3) 0.0231(7) Uani 1 1 d . . . O5 O 0.9936(3) 0.6932(3) 0.2916(3) 0.0266(7) Uani 1 1 d . . . O6 O 0.7613(3) 0.6926(3) 0.1704(3) 0.0268(8) Uani 1 1 d . . . N1 N 0.6599(5) 0.5173(4) -0.3235(4) 0.0407(11) Uani 1 1 d . . . N2 N 1.3643(5) 1.2561(4) 0.4180(4) 0.0466(12) Uani 1 1 d . . . N3 N 0.6628(5) 0.4570(5) 0.3745(4) 0.0453(12) Uani 1 1 d . . . C1 C 0.8044(5) 0.4196(5) -0.1174(5) 0.0351(13) Uani 1 1 d . . . H1A H 0.8326 0.3818 -0.0650 0.053 Uiso 1 1 calc R . . H1B H 0.8525 0.4142 -0.1689 0.053 Uiso 1 1 calc R . . H1C H 0.7081 0.3739 -0.1654 0.053 Uiso 1 1 calc R . . C2 C 0.8351(4) 0.5560(4) -0.0456(4) 0.0241(10) Uani 1 1 d . . . C3 C 0.7922(5) 0.6291(4) -0.0997(4) 0.0257(10) Uani 1 1 d . . . C4 C 0.8251(5) 0.7601(4) -0.0364(4) 0.0243(10) Uani 1 1 d . . . C5 C 0.7918(5) 0.8365(5) -0.0997(4) 0.0330(12) Uani 1 1 d . . . H5A H 0.7938 0.9146 -0.0446 0.049 Uiso 1 1 calc R . . H5B H 0.7024 0.7871 -0.1635 0.049 Uiso 1 1 calc R . . H5C H 0.8573 0.8577 -0.1327 0.049 Uiso 1 1 calc R . . C6 C 0.7204(5) 0.5691(5) -0.2241(5) 0.0300(11) Uani 1 1 d . . . C7 C 1.0611(6) 1.1243(5) 0.4393(4) 0.0364(13) Uani 1 1 d . . . H7A H 0.9701 1.1017 0.4357 0.055 Uiso 1 1 calc R . . H7B H 1.0861 1.1982 0.4231 0.055 Uiso 1 1 calc R . . H7C H 1.1231 1.1445 0.5179 0.055 Uiso 1 1 calc R . . C8 C 1.0672(5) 1.0149(5) 0.3494(4) 0.0263(11) Uani 1 1 d . . . C9 C 1.1806(5) 1.0326(4) 0.3203(4) 0.0265(11) Uani 1 1 d . . . C10 C 1.1980(5) 0.9302(4) 0.2441(4) 0.0246(10) Uani 1 1 d . . . C11 C 1.3197(5) 0.9527(5) 0.2187(5) 0.0334(12) Uani 1 1 d . . . H11A H 1.3439 0.8799 0.2088 0.050 Uiso 1 1 calc R . . H11B H 1.3935 1.0292 0.2843 0.050 Uiso 1 1 calc R . . H11C H 1.3018 0.9640 0.1464 0.050 Uiso 1 1 calc R . . C12 C 1.2826(6) 1.1572(5) 0.3760(4) 0.0347(12) Uani 1 1 d . . . C13 C 1.0017(6) 0.5869(5) 0.4122(4) 0.0350(12) Uani 1 1 d . . . H13A H 1.0971 0.6232 0.4293 0.053 Uiso 1 1 calc R . . H13B H 0.9688 0.4943 0.3777 0.053 Uiso 1 1 calc R . . H13C H 0.9886 0.6179 0.4851 0.053 Uiso 1 1 calc R . . C14 C 0.9265(5) 0.6253(4) 0.3272(4) 0.0243(10) Uani 1 1 d . . . C15 C 0.7868(5) 0.5875(4) 0.2903(4) 0.0254(10) Uani 1 1 d . . . C16 C 0.7109(5) 0.6236(4) 0.2126(4) 0.0273(11) Uani 1 1 d . . . C17 C 0.5621(5) 0.5803(6) 0.1773(6) 0.0432(14) Uani 1 1 d . . . H17A H 0.5293 0.6294 0.1394 0.065 Uiso 1 1 calc R . . H17B H 0.5427 0.5934 0.2473 0.065 Uiso 1 1 calc R . . H17C H 0.5176 0.4902 0.1221 0.065 Uiso 1 1 calc R . . C18 C 0.7181(6) 0.5134(5) 0.3365(4) 0.0325(12) Uani 1 1 d . . . P1 P 0.87434(15) 0.21513(13) 0.16630(12) 0.0348(4) Uani 1 1 d . . . F1 F 0.9160(3) 0.1704(4) 0.0598(3) 0.0584(10) Uani 1 1 d . . . F2 F 0.7211(3) 0.1308(4) 0.0769(3) 0.0576(10) Uani 1 1 d . . . F3 F 0.8306(4) 0.2601(4) 0.2726(3) 0.0658(11) Uani 1 1 d . . . F4 F 1.0252(4) 0.2984(4) 0.2552(3) 0.0663(11) Uani 1 1 d . . . F5 F 0.8635(5) 0.3328(3) 0.1432(4) 0.0713(12) Uani 1 1 d . . . F6 F 0.8792(5) 0.0962(4) 0.1890(3) 0.0742(13) Uani 1 1 d . . . O7 O 0.4131(5) 0.6985(5) -0.0027(5) 0.0682(15) Uani 1 1 d . . . H7D H 0.344(9) 0.707(8) -0.032(8) 0.09(3) Uiso 1 1 d . . . C19 C 0.5121(8) 0.7792(9) -0.0210(8) 0.083(3) Uani 1 1 d . . . H19A H 0.5238 0.8671 0.0197 0.125 Uiso 1 1 calc R . . H19B H 0.4845 0.7550 -0.1054 0.125 Uiso 1 1 calc R . . H19C H 0.5968 0.7714 0.0099 0.125 Uiso 1 1 calc R . . O8 O 0.7220(8) 0.0749(7) 0.3496(7) 0.120(3) Uani 1 1 d . . . H8 H 0.7547 0.1213 0.3262 0.179 Uiso 1 1 d R . . C20 C 0.6647(10) -0.0627(9) 0.3041(11) 0.118(4) Uani 1 1 d . . . H20A H 0.7301 -0.0957 0.2876 0.177 Uiso 1 1 calc R . . H20B H 0.5843 -0.0991 0.2315 0.177 Uiso 1 1 calc R . . H20C H 0.6412 -0.0856 0.3626 0.177 Uiso 1 1 calc R . . O9 O 0.6227(7) 0.2078(6) 0.4735(6) 0.101(2) Uani 1 1 d . . . H9 H 0.6537 0.1679 0.4349 0.151 Uiso 1 1 d R . . C21 C 0.6390(11) 0.1751(10) 0.5623(7) 0.097(3) Uani 1 1 d . . . H21A H 0.7345 0.2092 0.6120 0.145 Uiso 1 1 calc R . . H21B H 0.6014 0.0825 0.5308 0.145 Uiso 1 1 calc R . . H21C H 0.5932 0.2096 0.6092 0.145 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0543(4) 0.0531(3) 0.0255(3) 0.0061(2) 0.0142(2) -0.0162(2) Al1 0.0230(7) 0.0173(7) 0.0216(7) 0.0082(6) 0.0084(6) 0.0086(6) O1 0.0220(17) 0.0173(16) 0.0293(18) 0.0058(14) 0.0071(15) 0.0089(14) O2 0.0303(18) 0.0191(16) 0.0219(17) 0.0082(14) 0.0105(15) 0.0129(14) O3 0.0284(18) 0.0200(17) 0.0213(16) 0.0088(14) 0.0085(14) 0.0090(15) O4 0.0229(17) 0.0172(16) 0.0264(17) 0.0085(14) 0.0080(14) 0.0076(14) O5 0.0272(18) 0.0236(17) 0.0283(18) 0.0146(15) 0.0075(15) 0.0090(15) O6 0.0263(18) 0.0245(18) 0.0353(19) 0.0170(16) 0.0142(16) 0.0117(15) N1 0.036(3) 0.040(3) 0.027(3) 0.006(2) 0.007(2) 0.005(2) N2 0.042(3) 0.031(3) 0.040(3) 0.008(2) 0.004(2) 0.001(2) N3 0.051(3) 0.050(3) 0.042(3) 0.025(3) 0.026(3) 0.017(3) C1 0.029(3) 0.022(3) 0.039(3) 0.001(2) 0.011(2) 0.008(2) C2 0.017(2) 0.020(2) 0.030(3) 0.004(2) 0.011(2) 0.0068(19) C3 0.021(2) 0.022(2) 0.023(2) 0.004(2) 0.005(2) 0.005(2) C4 0.025(3) 0.026(2) 0.024(2) 0.011(2) 0.012(2) 0.011(2) C5 0.040(3) 0.030(3) 0.027(3) 0.013(2) 0.011(2) 0.013(2) C6 0.030(3) 0.024(3) 0.031(3) 0.007(2) 0.015(2) 0.007(2) C7 0.054(4) 0.026(3) 0.024(3) 0.005(2) 0.015(3) 0.016(3) C8 0.036(3) 0.026(3) 0.017(2) 0.013(2) 0.007(2) 0.014(2) C9 0.030(3) 0.020(2) 0.020(2) 0.008(2) 0.004(2) 0.005(2) C10 0.023(2) 0.027(3) 0.021(2) 0.012(2) 0.003(2) 0.009(2) C11 0.026(3) 0.033(3) 0.039(3) 0.018(2) 0.009(2) 0.010(2) C12 0.038(3) 0.030(3) 0.025(3) 0.009(2) 0.006(2) 0.007(3) C13 0.040(3) 0.034(3) 0.025(3) 0.015(2) 0.004(2) 0.013(3) C14 0.035(3) 0.016(2) 0.019(2) 0.0041(19) 0.008(2) 0.012(2) C15 0.032(3) 0.021(2) 0.021(2) 0.006(2) 0.013(2) 0.009(2) C16 0.032(3) 0.023(2) 0.034(3) 0.012(2) 0.018(2) 0.016(2) C17 0.030(3) 0.055(4) 0.058(4) 0.034(3) 0.023(3) 0.018(3) C18 0.040(3) 0.029(3) 0.027(3) 0.011(2) 0.013(2) 0.014(2) P1 0.0379(8) 0.0321(8) 0.0323(7) 0.0101(6) 0.0128(6) 0.0172(7) F1 0.047(2) 0.069(2) 0.043(2) 0.0077(19) 0.0227(17) 0.0157(19) F2 0.038(2) 0.059(2) 0.052(2) 0.0097(19) 0.0123(17) 0.0112(18) F3 0.080(3) 0.060(2) 0.056(2) 0.011(2) 0.044(2) 0.027(2) F4 0.041(2) 0.074(3) 0.046(2) 0.004(2) 0.0025(18) 0.015(2) F5 0.094(3) 0.042(2) 0.069(3) 0.026(2) 0.015(2) 0.031(2) F6 0.117(4) 0.049(2) 0.052(2) 0.022(2) 0.018(2) 0.045(3) O7 0.045(3) 0.092(4) 0.091(4) 0.059(3) 0.025(3) 0.039(3) C19 0.055(5) 0.112(7) 0.107(7) 0.067(6) 0.031(5) 0.045(5) O8 0.167(7) 0.110(6) 0.149(7) 0.077(5) 0.105(6) 0.082(5) C20 0.098(8) 0.074(6) 0.160(11) 0.013(7) 0.042(7) 0.060(6) O9 0.123(6) 0.109(5) 0.088(5) 0.045(4) 0.047(4) 0.063(5) C21 0.145(9) 0.119(8) 0.055(5) 0.049(5) 0.032(5) 0.090(7) _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 2.183(5) . ? Ag1 N1 2.207(4) 1_556 ? Ag1 N2 2.225(5) 1_445 ? Ag1 O9 2.586(6) . ? Ag1 Ag1 3.1616(12) 2_666 ? Al1 O1 1.864(3) . ? Al1 O4 1.866(3) . ? Al1 O5 1.866(3) . ? Al1 O2 1.869(3) . ? Al1 O3 1.876(3) . ? Al1 O6 1.885(3) . ? O1 C2 1.253(6) . ? O2 C4 1.256(5) . ? O3 C8 1.261(6) . ? O4 C10 1.253(6) . ? O5 C14 1.263(6) . ? O6 C16 1.252(6) . ? N1 C6 1.142(7) . ? N1 Ag1 2.207(4) 1_554 ? N2 C12 1.135(7) . ? N2 Ag1 2.225(5) 1_665 ? N3 C18 1.134(7) . ? C1 C2 1.500(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.416(7) . ? C3 C4 1.420(6) . ? C3 C6 1.424(7) . ? C4 C5 1.495(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.500(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.428(7) . ? C9 C12 1.424(7) . ? C9 C10 1.425(7) . ? C10 C11 1.489(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C13 C14 1.496(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.414(7) . ? C15 C16 1.414(7) . ? C15 C18 1.429(7) . ? C16 C17 1.509(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? P1 F4 1.581(4) . ? P1 F1 1.581(4) . ? P1 F6 1.587(4) . ? P1 F5 1.591(4) . ? P1 F3 1.594(4) . ? P1 F2 1.602(4) . ? O7 C19 1.414(10) . ? O7 H7D 0.83(9) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O8 C20 1.459(11) . ? O8 H8 0.7861 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O9 C21 1.338(9) . ? O9 H9 0.8072 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N1 120.48(19) . 1_556 ? N3 Ag1 N2 125.37(19) . 1_445 ? N1 Ag1 N2 113.32(18) 1_556 1_445 ? N3 Ag1 O9 99.6(2) . . ? N1 Ag1 O9 99.6(2) 1_556 . ? N2 Ag1 O9 79.6(2) 1_445 . ? N3 Ag1 Ag1 97.03(14) . 2_666 ? N1 Ag1 Ag1 77.61(13) 1_556 2_666 ? N2 Ag1 Ag1 85.23(14) 1_445 2_666 ? O9 Ag1 Ag1 162.06(16) . 2_666 ? O1 Al1 O4 90.67(15) . . ? O1 Al1 O5 88.70(15) . . ? O4 Al1 O5 89.45(15) . . ? O1 Al1 O2 90.93(15) . . ? O4 Al1 O2 89.98(15) . . ? O5 Al1 O2 179.32(16) . . ? O1 Al1 O3 178.32(16) . . ? O4 Al1 O3 90.94(15) . . ? O5 Al1 O3 90.84(15) . . ? O2 Al1 O3 89.55(14) . . ? O1 Al1 O6 89.57(15) . . ? O4 Al1 O6 179.39(16) . . ? O5 Al1 O6 91.12(15) . . ? O2 Al1 O6 89.45(15) . . ? O3 Al1 O6 88.83(15) . . ? C2 O1 Al1 129.7(3) . . ? C4 O2 Al1 130.1(3) . . ? C8 O3 Al1 129.3(3) . . ? C10 O4 Al1 130.1(3) . . ? C14 O5 Al1 130.3(3) . . ? C16 O6 Al1 129.5(3) . . ? C6 N1 Ag1 170.1(5) . 1_554 ? C12 N2 Ag1 157.3(5) . 1_665 ? C18 N3 Ag1 163.5(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.6(4) . . ? O1 C2 C1 116.6(4) . . ? C3 C2 C1 120.8(4) . . ? C2 C3 C4 122.8(4) . . ? C2 C3 C6 117.7(4) . . ? C4 C3 C6 119.3(4) . . ? O2 C4 C3 122.1(4) . . ? O2 C4 C5 117.3(4) . . ? C3 C4 C5 120.6(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 177.4(6) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 122.6(4) . . ? O3 C8 C7 117.3(5) . . ? C9 C8 C7 120.0(5) . . ? C12 C9 C10 119.7(5) . . ? C12 C9 C8 117.6(4) . . ? C10 C9 C8 122.6(4) . . ? O4 C10 C9 122.2(4) . . ? O4 C10 C11 117.1(4) . . ? C9 C10 C11 120.7(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 178.4(6) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 122.4(4) . . ? O5 C14 C13 117.0(4) . . ? C15 C14 C13 120.6(4) . . ? C16 C15 C14 123.2(4) . . ? C16 C15 C18 117.5(5) . . ? C14 C15 C18 119.2(4) . . ? O6 C16 C15 123.1(5) . . ? O6 C16 C17 116.4(4) . . ? C15 C16 C17 120.5(5) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 178.3(6) . . ? F4 P1 F1 91.4(2) . . ? F4 P1 F6 91.6(2) . . ? F1 P1 F6 90.9(2) . . ? F4 P1 F5 90.3(2) . . ? F1 P1 F5 90.5(2) . . ? F6 P1 F5 177.7(3) . . ? F4 P1 F3 89.2(2) . . ? F1 P1 F3 179.3(2) . . ? F6 P1 F3 89.5(2) . . ? F5 P1 F3 89.1(2) . . ? F4 P1 F2 179.7(2) . . ? F1 P1 F2 88.9(2) . . ? F6 P1 F2 88.4(2) . . ? F5 P1 F2 89.8(2) . . ? F3 P1 F2 90.5(2) . . ? C19 O7 H7D 105(6) . . ? O7 C19 H19A 109.5 . . ? O7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 O8 H8 133.5 . . ? O8 C20 H20A 109.5 . . ? O8 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O8 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O9 Ag1 121.2(5) . . ? C21 O9 H9 102.8 . . ? Ag1 O9 H9 133.7 . . ? O9 C21 H21A 109.5 . . ? O9 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O9 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.039 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.125 data_2c _database_code_depnum_ccdc_archive 'CCDC 872086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2c _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 Ag Al N3 O6, F6 P, C H Cl3' _chemical_formula_sum 'C19 H19 Ag Al Cl3 F6 N3 O6 P' _chemical_formula_weight 771.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P 21 3' _symmetry_space_group_name_Hall 'P 2ac 2ab 3' 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 14.0563(4) _cell_length_b 14.0563(4) _cell_length_c 14.0563(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2777.24(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6138 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 25.97 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7561 _exptl_absorpt_correction_T_max 0.9112 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28783 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.36 _reflns_number_total 2332 _reflns_number_gt 2237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART' _computing_cell_refinement 'BRUKER SMART' _computing_data_reduction 'BRUKER SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+2.5658P] 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 -0.04(3) _refine_ls_number_reflns 2332 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL c10_17 in P2(1)3 CELL 0.71073 14.0563 14.0563 14.0563 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0004 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SYMM Z, X, Y SYMM 0.5+Z, 0.5-X, -Y SYMM 0.5-Z, -X, 0.5+Y SYMM -Z, 0.5+X, 0.5-Y SYMM Y, Z, X SYMM -Y, 0.5+Z, 0.5-X SYMM 0.5+Y, 0.5-Z, -X SYMM 0.5-Y, -Z, 0.5+X SFAC C H N O F AL P AG CL UNIT 76 76 12 24 24 4 4 4 12 TEMP -173.00 L.S. 15 ACTA BOND BOND $H SIZE 0.25 0.20 0.08 FMAP 2 PLAN -20 WGHT 0.0414 2.5658 FVAR 0.35090 MOLE 1 AG1 8 1.125903 0.374097 0.625903 10.33333 0.02025 0.02025 = 0.02025 0.00186 -0.00186 0.00186 AL1 6 0.770644 0.270644 0.229356 10.33333 0.01367 0.01367 = 0.01367 -0.00002 -0.00002 0.00002 O1 4 0.764051 0.272059 0.362470 11.00000 0.01489 0.01790 = 0.01466 -0.00088 -0.00127 0.00008 O2 4 0.902844 0.277239 0.234523 11.00000 0.01421 0.01856 = 0.01832 -0.00063 0.00007 0.00004 C1 1 0.799355 0.266064 0.526270 11.00000 0.02509 0.03316 = 0.01477 -0.00071 0.00056 -0.00255 AFIX 137 H1A 2 0.837336 0.311926 0.562532 11.00000 -1.50000 H1B 2 0.808785 0.202167 0.552522 11.00000 -1.50000 H1C 2 0.731913 0.283219 0.530532 11.00000 -1.50000 AFIX 0 C2 1 0.829924 0.267407 0.424358 11.00000 0.02310 0.01193 = 0.01558 -0.00209 -0.00180 -0.00187 C3 1 0.926935 0.263561 0.399314 11.00000 0.01740 0.01672 = 0.01899 -0.00096 -0.00515 0.00045 C4 1 0.959288 0.269729 0.304262 11.00000 0.01417 0.01264 = 0.02297 -0.00276 -0.00054 -0.00091 C5 1 1.063211 0.267799 0.281265 11.00000 0.01581 0.03302 = 0.02888 -0.00487 0.00195 -0.00091 AFIX 137 H5A 2 1.100117 0.268450 0.340411 11.00000 -1.50000 H5B 2 1.079596 0.323750 0.243031 11.00000 -1.50000 H5C 2 1.077981 0.209932 0.245291 11.00000 -1.50000 AFIX 0 C6 1 0.994922 0.262631 0.474462 11.00000 0.01769 0.02060 = 0.02463 -0.00254 -0.00038 0.00145 N1 3 1.047338 0.263377 0.536836 11.00000 0.02119 0.03241 = 0.02576 -0.00050 -0.00544 0.00353 MOLE 2 C7 1 0.561350 0.561350 0.561350 10.33333 0.02857 0.02857 = 0.02857 -0.00352 -0.00352 -0.00352 AFIX 13 H7 2 0.602424 0.602424 0.602424 10.33333 -1.20000 AFIX 0 CL1 9 0.636606 0.493541 0.489900 11.00000 0.10812 0.08199 = 0.04716 -0.00091 0.02400 0.04416 MOLE 3 P1 7 0.956062 0.543938 0.456062 10.33333 0.03209 0.03209 = 0.03209 0.00593 -0.00593 0.00593 F1 5 0.918827 0.468250 0.531740 11.00000 0.05982 0.04197 = 0.04614 -0.00997 0.02394 -0.02228 F2 5 0.881861 0.501215 0.382687 11.00000 0.07094 0.14283 = 0.07274 -0.00975 -0.04939 -0.00158 HKLF 4 ; 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 1.125904(14) 0.374096(14) 0.625904(14) 0.02026(10) Uani 1 3 d S . . Al1 Al 0.77064(6) 0.27064(6) 0.22936(6) 0.0137(3) Uani 1 3 d S . . O1 O 0.76405(13) 0.27206(13) 0.36247(13) 0.0158(3) Uani 1 1 d . . . O2 O 0.90284(13) 0.27724(14) 0.23452(14) 0.0170(4) Uani 1 1 d . . . C1 C 0.7994(2) 0.2661(2) 0.5263(2) 0.0243(6) Uani 1 1 d . . . H1A H 0.8373 0.3119 0.5625 0.037 Uiso 1 1 calc R . . H1B H 0.8088 0.2022 0.5525 0.037 Uiso 1 1 calc R . . H1C H 0.7319 0.2832 0.5305 0.037 Uiso 1 1 calc R . . C2 C 0.8299(2) 0.26741(19) 0.42436(19) 0.0169(5) Uani 1 1 d . . . C3 C 0.9269(2) 0.2636(2) 0.39931(19) 0.0177(5) Uani 1 1 d . . . C4 C 0.95929(19) 0.26973(19) 0.3043(2) 0.0166(5) Uani 1 1 d . . . C5 C 1.0632(2) 0.2678(2) 0.2813(2) 0.0259(6) Uani 1 1 d . . . H5A H 1.1001 0.2685 0.3404 0.039 Uiso 1 1 calc R . . H5B H 1.0796 0.3237 0.2430 0.039 Uiso 1 1 calc R . . H5C H 1.0780 0.2099 0.2453 0.039 Uiso 1 1 calc R . . C6 C 0.9949(2) 0.2626(2) 0.4745(2) 0.0210(5) Uani 1 1 d . . . N1 N 1.04734(18) 0.2634(2) 0.53684(19) 0.0265(5) Uani 1 1 d . . . C7 C 0.5614(2) 0.5614(2) 0.5614(2) 0.0286(11) Uani 1 3 d S . . H7 H 0.6024 0.6024 0.6024 0.034 Uiso 1 3 calc SR . . Cl1 Cl 0.63661(13) 0.49354(11) 0.48990(9) 0.0791(5) Uani 1 1 d . . . P1 P 0.95606(6) 0.54394(6) 0.45606(6) 0.0321(3) Uani 1 3 d S . . F1 F 0.91883(18) 0.46825(17) 0.53174(18) 0.0493(6) Uani 1 1 d . . . F2 F 0.8819(2) 0.5012(3) 0.3827(2) 0.0955(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02026(10) 0.02026(10) 0.02026(10) 0.00186(8) -0.00186(8) 0.00186(8) Al1 0.0137(3) 0.0137(3) 0.0137(3) 0.0000(3) 0.0000(3) 0.0000(3) O1 0.0149(8) 0.0179(8) 0.0147(8) -0.0009(7) -0.0013(7) 0.0001(7) O2 0.0142(8) 0.0186(9) 0.0183(9) -0.0006(7) 0.0001(7) 0.0000(7) C1 0.0251(14) 0.0332(16) 0.0148(13) -0.0007(12) 0.0006(11) -0.0025(13) C2 0.0231(13) 0.0119(11) 0.0156(12) -0.0021(10) -0.0018(10) -0.0019(10) C3 0.0174(12) 0.0167(12) 0.0190(13) -0.0010(10) -0.0052(10) 0.0005(10) C4 0.0142(12) 0.0126(11) 0.0230(13) -0.0028(10) -0.0005(10) -0.0009(9) C5 0.0158(12) 0.0330(16) 0.0289(15) -0.0049(13) 0.0019(11) -0.0009(12) C6 0.0177(13) 0.0206(13) 0.0246(14) -0.0025(11) -0.0004(11) 0.0015(11) N1 0.0212(12) 0.0324(13) 0.0258(13) -0.0005(11) -0.0054(10) 0.0035(10) C7 0.0286(11) 0.0286(11) 0.0286(11) -0.0035(12) -0.0035(12) -0.0035(12) Cl1 0.1081(12) 0.0820(9) 0.0472(6) -0.0009(6) 0.0240(7) 0.0442(9) P1 0.0321(3) 0.0321(3) 0.0321(3) 0.0059(3) -0.0059(3) 0.0059(3) F1 0.0598(15) 0.0420(12) 0.0461(13) -0.0100(11) 0.0239(11) -0.0223(12) F2 0.071(2) 0.143(3) 0.073(2) -0.010(2) -0.049(2) -0.002(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 N1 2.282(3) 12_664 ? Ag1 N1 2.282(3) 6_566 ? Ag1 N1 2.282(3) . ? Al1 O2 1.862(2) 8_645 ? Al1 O2 1.862(2) . ? Al1 O2 1.862(2) 11_556 ? Al1 O1 1.873(2) 11_556 ? Al1 O1 1.873(2) . ? Al1 O1 1.874(2) 8_645 ? O1 C2 1.272(3) . ? O2 C4 1.266(3) . ? C1 C2 1.496(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.409(4) . ? C3 C4 1.414(4) . ? C3 C6 1.425(4) . ? C4 C5 1.496(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.145(4) . ? C7 Cl1 1.742(2) 9 ? C7 Cl1 1.742(2) . ? C7 Cl1 1.742(2) 5 ? C7 H7 1.0000 . ? P1 F2 1.585(3) . ? P1 F2 1.585(3) 6_566 ? P1 F2 1.585(3) 12_664 ? P1 F1 1.593(2) 6_566 ? P1 F1 1.593(2) 12_664 ? P1 F1 1.593(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 116.01(4) 12_664 6_566 ? N1 Ag1 N1 116.01(4) 12_664 . ? N1 Ag1 N1 116.01(5) 6_566 . ? O2 Al1 O2 89.50(10) 8_645 . ? O2 Al1 O2 89.50(10) 8_645 11_556 ? O2 Al1 O2 89.50(10) . 11_556 ? O2 Al1 O1 178.37(9) 8_645 11_556 ? O2 Al1 O1 92.13(8) . 11_556 ? O2 Al1 O1 90.57(8) 11_556 11_556 ? O2 Al1 O1 92.13(8) 8_645 . ? O2 Al1 O1 90.57(8) . . ? O2 Al1 O1 178.37(9) 11_556 . ? O1 Al1 O1 87.81(10) 11_556 . ? O2 Al1 O1 90.57(8) 8_645 8_645 ? O2 Al1 O1 178.37(9) . 8_645 ? O2 Al1 O1 92.13(8) 11_556 8_645 ? O1 Al1 O1 87.81(10) 11_556 8_645 ? O1 Al1 O1 87.81(10) . 8_645 ? C2 O1 Al1 130.27(18) . . ? C4 O2 Al1 130.67(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.4(2) . . ? O1 C2 C1 116.5(3) . . ? C3 C2 C1 121.1(2) . . ? C2 C3 C4 123.0(2) . . ? C2 C3 C6 117.7(2) . . ? C4 C3 C6 119.0(3) . . ? O2 C4 C3 122.4(2) . . ? O2 C4 C5 116.5(3) . . ? C3 C4 C5 121.1(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 177.7(3) . . ? C6 N1 Ag1 137.5(2) . . ? Cl1 C7 Cl1 111.51(17) 9 . ? Cl1 C7 Cl1 111.51(17) 9 5 ? Cl1 C7 Cl1 111.51(17) . 5 ? Cl1 C7 H7 107.3 9 . ? Cl1 C7 H7 107.3 . . ? Cl1 C7 H7 107.3 5 . ? F2 P1 F2 93.9(2) . 6_566 ? F2 P1 F2 93.9(2) . 12_664 ? F2 P1 F2 93.9(2) 6_566 12_664 ? F2 P1 F1 176.9(2) . 6_566 ? F2 P1 F1 88.01(18) 6_566 6_566 ? F2 P1 F1 88.43(18) 12_664 6_566 ? F2 P1 F1 88.43(18) . 12_664 ? F2 P1 F1 176.9(2) 6_566 12_664 ? F2 P1 F1 88.01(18) 12_664 12_664 ? F1 P1 F1 89.59(16) 6_566 12_664 ? F2 P1 F1 88.01(18) . . ? F2 P1 F1 88.43(18) 6_566 . ? F2 P1 F1 176.9(2) 12_664 . ? F1 P1 F1 89.59(16) 6_566 . ? F1 P1 F1 89.59(16) 12_664 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.858 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.079 data_3a _database_code_depnum_ccdc_archive 'CCDC 872087' #TrackingRef '- complete_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3a _chemical_melting_point ? _chemical_formula_moiety 'C19 H18 Ag Al F3 N3 O9 S, 0.5(C6 H6), C H4 O' _chemical_formula_sum 'C23 H25 Ag Al F3 N3 O10 S' _chemical_formula_weight 727.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.560(3) _cell_length_b 12.324(4) _cell_length_c 13.523(4) _cell_angle_alpha 115.784(4) _cell_angle_beta 107.908(5) _cell_angle_gamma 92.183(5) _cell_volume 1477.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3142 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 23.53 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 734 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8893 _exptl_absorpt_correction_T_max 0.9424 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator multilayer-optics _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17651 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.73 _reflns_number_total 6218 _reflns_number_gt 4947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER smart' _computing_cell_refinement 'BRUKER saint' _computing_data_reduction 'BRUKER saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.1076P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6218 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL c11_41 in P-1 CELL 0.71073 10.5600 12.3240 13.5230 115.784 107.908 92.183 ZERR 2 0.0030 0.0040 0.0040 0.004 0.005 0.005 LATT 1 SFAC C H AG AL F N O S UNIT 46 50 2 2 6 6 20 2 L.S. 10 TEMP -173.15 ACTA SIZE 0.14 0.14 0.07 FMAP 2 PLAN -20 BOND $H BOND WGHT 0.037500 0.107600 FVAR 0.50145 AL1 4 0.439920 0.659945 0.763732 11.00000 0.01642 0.01751 = 0.01279 0.00536 0.00119 0.00146 AG1 3 0.068654 0.955205 0.370046 11.00000 0.02700 0.02245 = 0.01756 0.00886 -0.00419 -0.00099 O1 7 0.254438 0.665609 0.715332 11.00000 0.01773 0.02408 = 0.01747 0.01085 0.00259 0.00251 O2 7 0.479492 0.776482 0.718037 11.00000 0.01887 0.01586 = 0.01738 0.00573 0.00262 0.00150 O3 7 0.403956 0.538844 0.805445 11.00000 0.02193 0.01574 = 0.01523 0.00534 0.00398 0.00291 O4 7 0.411077 0.539266 0.611279 11.00000 0.02127 0.01703 = 0.01511 0.00539 0.00247 -0.00137 O5 7 0.624864 0.656417 0.812353 11.00000 0.02021 0.01975 = 0.01556 0.00518 0.00314 0.00276 O6 7 0.460720 0.782292 0.913359 11.00000 0.01935 0.01971 = 0.01468 0.00543 0.00280 0.00270 O7 7 0.290833 0.694404 0.318065 11.00000 0.04342 0.04359 = 0.03124 0.01956 0.01081 -0.00421 O8 7 0.450790 0.810115 0.286929 11.00000 0.03437 0.03297 = 0.03508 0.00955 0.01058 -0.00450 O9 7 0.223897 0.852886 0.262901 11.00000 0.06256 0.04806 = 0.04399 0.01926 0.02592 0.03265 C1 1 0.039422 0.683032 0.609276 11.00000 0.02075 0.03691 = 0.02663 0.01836 0.00313 0.00218 AFIX 137 H1A 2 0.002374 0.625145 0.524878 11.00000 -1.50000 H1B 2 0.005495 0.759313 0.623311 11.00000 -1.50000 H1C 2 0.010990 0.646489 0.652463 11.00000 -1.50000 AFIX 0 C2 1 0.191174 0.710738 0.650761 11.00000 0.02024 0.01899 = 0.01522 0.00438 0.00513 0.00357 C3 1 0.258375 0.783185 0.617589 11.00000 0.01968 0.02073 = 0.01248 0.00671 0.00232 0.00409 C4 1 0.400201 0.812724 0.651436 11.00000 0.02411 0.01338 = 0.01167 0.00106 0.00416 0.00345 C5 1 0.464249 0.887284 0.610804 11.00000 0.02739 0.02677 = 0.02288 0.01361 0.00702 0.00095 AFIX 137 H5A 2 0.557880 0.926167 0.665541 11.00000 -1.50000 H5B 2 0.412523 0.950953 0.608155 11.00000 -1.50000 H5C 2 0.464430 0.833727 0.532016 11.00000 -1.50000 AFIX 0 C6 1 0.176581 0.830525 0.546270 11.00000 0.02576 0.02333 = 0.01919 0.01009 0.00735 0.00330 C7 1 0.333943 0.352931 0.801402 11.00000 0.03153 0.02503 = 0.02752 0.01528 0.01090 0.00791 AFIX 137 H7A 2 0.333866 0.408966 0.879600 11.00000 -1.50000 H7B 2 0.406907 0.307036 0.809384 11.00000 -1.50000 H7C 2 0.246344 0.295246 0.754333 11.00000 -1.50000 AFIX 0 C8 1 0.356315 0.425224 0.741936 11.00000 0.01373 0.02454 = 0.02294 0.01288 0.00320 0.00297 C9 1 0.323283 0.365982 0.617663 11.00000 0.01758 0.01781 = 0.02040 0.00792 0.00414 0.00016 C10 1 0.352656 0.426830 0.557333 11.00000 0.01127 0.01748 = 0.01894 0.00410 0.00028 0.00419 C11 1 0.317184 0.364772 0.428156 11.00000 0.02356 0.02480 = 0.01741 0.00441 0.00467 -0.00092 AFIX 137 H11A 2 0.245523 0.399100 0.392602 11.00000 -1.50000 H11B 2 0.284848 0.276449 0.396332 11.00000 -1.50000 H11C 2 0.397690 0.377671 0.409996 11.00000 -1.50000 AFIX 0 C12 1 0.259744 0.238711 0.549648 11.00000 0.02083 0.02602 = 0.02244 0.01054 0.00674 0.00390 C13 1 0.854507 0.681966 0.924659 11.00000 0.01927 0.02965 = 0.02730 0.01144 0.00213 0.00434 AFIX 137 H13A 2 0.855291 0.626274 0.846626 11.00000 -1.50000 H13B 2 0.879004 0.642914 0.975554 11.00000 -1.50000 H13C 2 0.920269 0.758660 0.959157 11.00000 -1.50000 AFIX 0 C14 1 0.715962 0.709437 0.913461 11.00000 0.01978 0.01746 = 0.01773 0.00877 0.00242 -0.00135 C15 1 0.689321 0.791646 1.013228 11.00000 0.02059 0.01879 = 0.01674 0.00739 0.00061 -0.00237 C16 1 0.563414 0.827125 1.007964 11.00000 0.02939 0.01194 = 0.01498 0.00400 0.00607 -0.00043 C17 1 0.543952 0.922043 1.115199 11.00000 0.03189 0.02349 = 0.01751 0.00221 0.00461 0.00158 AFIX 137 H17A 2 0.467320 0.958948 1.091415 11.00000 -1.50000 H17B 2 0.626581 0.986099 1.164115 11.00000 -1.50000 H17C 2 0.525208 0.883243 1.160294 11.00000 -1.50000 AFIX 0 C18 1 0.798098 0.846740 1.125141 11.00000 0.02721 0.02734 = 0.02362 0.01410 0.00713 -0.00079 C19 1 0.251760 0.652632 0.107524 11.00000 0.02924 0.03175 = 0.03108 0.01264 0.00913 0.00416 N1 6 0.109031 0.869104 0.490845 11.00000 0.03123 0.03693 = 0.03189 0.02274 0.00874 0.00875 N2 6 0.205615 0.138968 0.490865 11.00000 0.03301 0.02163 = 0.02853 0.00796 0.00553 -0.00108 N3 6 0.885005 0.890361 1.213744 11.00000 0.02773 0.03975 = 0.01955 0.01225 -0.00084 -0.00283 F1 5 0.264025 0.702283 0.040533 11.00000 0.08222 0.05611 = 0.03146 0.02120 0.01887 -0.00272 F2 5 0.322499 0.563110 0.089329 11.00000 0.04011 0.03629 = 0.04528 0.00393 0.01510 0.00867 F3 5 0.121637 0.599238 0.067550 11.00000 0.02944 0.05092 = 0.03838 0.01443 -0.00251 -0.00164 S1 8 0.311070 0.765451 0.261761 11.00000 0.03067 0.02770 = 0.02457 0.01084 0.01027 0.00627 MOLE 2 C20 1 -0.082895 0.064331 0.055505 11.00000 0.08713 0.06008 = 0.07717 0.03419 0.03190 -0.01044 AFIX 43 H20 2 -0.139102 0.108520 0.095141 11.00000 -1.20000 AFIX 0 C21 1 0.040381 0.048193 0.119147 11.00000 0.09636 0.06385 = 0.04523 0.03001 0.00864 -0.02600 AFIX 43 H21 2 0.067437 0.082799 0.202239 11.00000 -1.20000 AFIX 0 C22 1 0.122660 -0.015886 0.065028 11.00000 0.06217 0.07463 = 0.06934 0.04188 0.00598 -0.01239 AFIX 43 H22 2 0.205619 -0.026980 0.109312 11.00000 -1.20000 AFIX 0 MOLE 3 C23 1 -0.019033 0.552604 0.266765 11.00000 0.02906 0.03612 = 0.03281 0.01558 0.00470 0.00107 AFIX 137 H23A 2 -0.029555 0.638410 0.301692 11.00000 -1.50000 H23B 2 -0.095454 0.499907 0.261321 11.00000 -1.50000 H23C 2 -0.017294 0.527486 0.187838 11.00000 -1.50000 AFIX 0 O10 7 0.104454 0.541022 0.338423 11.00000 0.03023 0.03674 = 0.03883 0.02018 0.01116 0.00347 H10 2 0.159947 0.581756 0.338652 11.00000 0.03326 HKLF 4 ; 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 Al1 Al 0.43992(10) 0.65995(9) 0.76373(8) 0.0174(2) Uani 1 1 d . . . Ag1 Ag 0.06865(3) 0.95520(3) 0.37005(2) 0.02592(10) Uani 1 1 d . . . O1 O 0.2544(2) 0.6656(2) 0.71533(19) 0.0204(5) Uani 1 1 d . . . O2 O 0.4795(2) 0.7765(2) 0.71804(19) 0.0193(5) Uani 1 1 d . . . O3 O 0.4040(2) 0.5388(2) 0.80545(19) 0.0191(5) Uani 1 1 d . . . O4 O 0.4111(2) 0.5393(2) 0.61128(19) 0.0199(5) Uani 1 1 d . . . O5 O 0.6249(2) 0.6564(2) 0.81235(19) 0.0206(5) Uani 1 1 d . . . O6 O 0.4607(2) 0.7823(2) 0.91336(19) 0.0199(5) Uani 1 1 d . . . O7 O 0.2908(3) 0.6944(3) 0.3181(2) 0.0397(7) Uani 1 1 d . . . O8 O 0.4508(3) 0.8101(2) 0.2869(2) 0.0375(7) Uani 1 1 d . . . O9 O 0.2239(3) 0.8529(3) 0.2629(3) 0.0500(8) Uani 1 1 d . . . C1 C 0.0394(4) 0.6830(4) 0.6093(3) 0.0283(9) Uani 1 1 d . . . H1A H 0.0024 0.6251 0.5249 0.042 Uiso 1 1 calc R . . H1B H 0.0055 0.7593 0.6233 0.042 Uiso 1 1 calc R . . H1C H 0.0110 0.6465 0.6525 0.042 Uiso 1 1 calc R . . C2 C 0.1912(3) 0.7107(3) 0.6508(3) 0.0199(7) Uani 1 1 d . . . C3 C 0.2584(3) 0.7832(3) 0.6176(3) 0.0190(7) Uani 1 1 d . . . C4 C 0.4002(4) 0.8127(3) 0.6514(3) 0.0189(7) Uani 1 1 d . . . C5 C 0.4642(4) 0.8873(3) 0.6108(3) 0.0256(8) Uani 1 1 d . . . H5A H 0.5579 0.9262 0.6655 0.038 Uiso 1 1 calc R . . H5B H 0.4125 0.9510 0.6082 0.038 Uiso 1 1 calc R . . H5C H 0.4644 0.8337 0.5320 0.038 Uiso 1 1 calc R . . C6 C 0.1766(4) 0.8305(3) 0.5463(3) 0.0230(8) Uani 1 1 d . . . C7 C 0.3339(4) 0.3529(3) 0.8014(3) 0.0267(8) Uani 1 1 d . . . H7A H 0.3338 0.4090 0.8796 0.040 Uiso 1 1 calc R . . H7B H 0.4069 0.3070 0.8094 0.040 Uiso 1 1 calc R . . H7C H 0.2464 0.2952 0.7543 0.040 Uiso 1 1 calc R . . C8 C 0.3563(3) 0.4252(3) 0.7419(3) 0.0206(8) Uani 1 1 d . . . C9 C 0.3233(3) 0.3660(3) 0.6177(3) 0.0198(7) Uani 1 1 d . . . C10 C 0.3527(3) 0.4268(3) 0.5573(3) 0.0189(7) Uani 1 1 d . . . C11 C 0.3172(4) 0.3648(3) 0.4282(3) 0.0250(8) Uani 1 1 d . . . H11A H 0.2455 0.3991 0.3926 0.037 Uiso 1 1 calc R . . H11B H 0.2849 0.2764 0.3963 0.037 Uiso 1 1 calc R . . H11C H 0.3977 0.3777 0.4100 0.037 Uiso 1 1 calc R . . C12 C 0.2597(4) 0.2387(3) 0.5496(3) 0.0237(8) Uani 1 1 d . . . C13 C 0.8545(4) 0.6820(3) 0.9247(3) 0.0278(8) Uani 1 1 d . . . H13A H 0.8553 0.6263 0.8466 0.042 Uiso 1 1 calc R . . H13B H 0.8790 0.6429 0.9756 0.042 Uiso 1 1 calc R . . H13C H 0.9203 0.7587 0.9592 0.042 Uiso 1 1 calc R . . C14 C 0.7160(3) 0.7094(3) 0.9135(3) 0.0194(7) Uani 1 1 d . . . C15 C 0.6893(4) 0.7916(3) 1.0132(3) 0.0209(8) Uani 1 1 d . . . C16 C 0.5634(4) 0.8271(3) 1.0080(3) 0.0203(7) Uani 1 1 d . . . C17 C 0.5440(4) 0.9220(3) 1.1152(3) 0.0284(9) Uani 1 1 d . . . H17A H 0.4673 0.9589 1.0914 0.043 Uiso 1 1 calc R . . H17B H 0.6265 0.9861 1.1641 0.043 Uiso 1 1 calc R . . H17C H 0.5253 0.8833 1.1603 0.043 Uiso 1 1 calc R . . C18 C 0.7981(4) 0.8467(3) 1.1251(3) 0.0259(8) Uani 1 1 d . . . C19 C 0.2518(4) 0.6526(4) 0.1075(3) 0.0320(9) Uani 1 1 d . . . N1 N 0.1090(3) 0.8691(3) 0.4908(3) 0.0314(8) Uani 1 1 d . . . N2 N 0.2056(3) 0.1390(3) 0.4909(3) 0.0309(8) Uani 1 1 d . . . N3 N 0.8850(3) 0.8904(3) 1.2137(3) 0.0324(8) Uani 1 1 d . . . F1 F 0.2640(3) 0.7023(2) 0.0405(2) 0.0573(8) Uani 1 1 d . . . F2 F 0.3225(2) 0.5631(2) 0.0893(2) 0.0466(6) Uani 1 1 d . . . F3 F 0.1216(2) 0.5992(2) 0.0676(2) 0.0463(6) Uani 1 1 d . . . S1 S 0.31107(10) 0.76545(9) 0.26176(8) 0.0281(2) Uani 1 1 d . . . C20 C -0.0829(7) 0.0643(5) 0.0555(6) 0.0742(18) Uani 1 1 d . . . H20 H -0.1391 0.1085 0.0951 0.089 Uiso 1 1 calc R . . C21 C 0.0404(7) 0.0482(5) 0.1191(5) 0.0725(19) Uani 1 1 d . . . H21 H 0.0674 0.0828 0.2022 0.087 Uiso 1 1 calc R . . C22 C 0.1227(6) -0.0159(6) 0.0650(6) 0.0710(17) Uani 1 1 d . . . H22 H 0.2056 -0.0270 0.1093 0.085 Uiso 1 1 calc R . . C23 C -0.0190(4) 0.5526(4) 0.2668(3) 0.0348(10) Uani 1 1 d . . . H23A H -0.0296 0.6384 0.3017 0.052 Uiso 1 1 calc R . . H23B H -0.0955 0.4999 0.2613 0.052 Uiso 1 1 calc R . . H23C H -0.0173 0.5275 0.1878 0.052 Uiso 1 1 calc R . . O10 O 0.1045(3) 0.5410(3) 0.3384(3) 0.0347(7) Uani 1 1 d . . . H10 H 0.160(4) 0.582(4) 0.339(4) 0.033(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 Al1 0.0164(5) 0.0175(5) 0.0128(5) 0.0054(4) 0.0012(4) 0.0015(4) Ag1 0.02700(17) 0.02245(16) 0.01756(15) 0.00886(12) -0.00419(12) -0.00099(11) O1 0.0177(13) 0.0241(13) 0.0175(12) 0.0109(11) 0.0026(10) 0.0025(10) O2 0.0189(13) 0.0159(12) 0.0174(12) 0.0057(10) 0.0026(10) 0.0015(10) O3 0.0219(13) 0.0157(12) 0.0152(12) 0.0053(10) 0.0040(10) 0.0029(10) O4 0.0213(13) 0.0170(12) 0.0151(12) 0.0054(10) 0.0025(10) -0.0014(10) O5 0.0202(13) 0.0198(12) 0.0156(12) 0.0052(10) 0.0031(10) 0.0028(10) O6 0.0194(13) 0.0197(13) 0.0147(12) 0.0054(10) 0.0028(10) 0.0027(10) O7 0.0434(18) 0.0436(18) 0.0312(16) 0.0196(14) 0.0108(14) -0.0042(14) O8 0.0344(17) 0.0330(16) 0.0351(16) 0.0096(13) 0.0106(13) -0.0045(13) O9 0.063(2) 0.048(2) 0.0440(19) 0.0193(16) 0.0259(17) 0.0327(17) C1 0.021(2) 0.037(2) 0.027(2) 0.0184(18) 0.0031(16) 0.0022(16) C2 0.0202(18) 0.0190(18) 0.0152(17) 0.0044(15) 0.0051(15) 0.0036(14) C3 0.0197(18) 0.0207(18) 0.0125(16) 0.0067(14) 0.0023(14) 0.0041(14) C4 0.0241(19) 0.0134(16) 0.0117(16) 0.0011(14) 0.0042(14) 0.0035(14) C5 0.027(2) 0.027(2) 0.0229(19) 0.0136(17) 0.0070(16) 0.0009(16) C6 0.026(2) 0.0233(19) 0.0192(18) 0.0101(16) 0.0073(16) 0.0033(16) C7 0.032(2) 0.025(2) 0.028(2) 0.0153(17) 0.0109(17) 0.0079(16) C8 0.0137(17) 0.0245(19) 0.0229(19) 0.0129(16) 0.0032(15) 0.0030(14) C9 0.0176(18) 0.0178(17) 0.0204(18) 0.0079(15) 0.0041(15) 0.0002(14) C10 0.0113(16) 0.0175(17) 0.0189(17) 0.0041(14) 0.0003(14) 0.0042(13) C11 0.024(2) 0.0248(19) 0.0174(18) 0.0044(16) 0.0047(16) -0.0009(15) C12 0.0208(19) 0.026(2) 0.0224(19) 0.0105(17) 0.0067(16) 0.0039(16) C13 0.0193(19) 0.030(2) 0.027(2) 0.0114(17) 0.0021(16) 0.0043(16) C14 0.0198(18) 0.0175(17) 0.0177(18) 0.0088(15) 0.0024(15) -0.0014(14) C15 0.0206(19) 0.0188(18) 0.0167(17) 0.0074(15) 0.0006(15) -0.0024(14) C16 0.029(2) 0.0119(16) 0.0150(17) 0.0040(14) 0.0061(15) -0.0004(14) C17 0.032(2) 0.023(2) 0.0175(18) 0.0022(16) 0.0046(17) 0.0016(16) C18 0.027(2) 0.027(2) 0.024(2) 0.0141(17) 0.0071(17) -0.0008(16) C19 0.029(2) 0.032(2) 0.031(2) 0.0126(19) 0.0091(18) 0.0042(18) N1 0.0312(19) 0.0369(19) 0.0319(19) 0.0227(17) 0.0087(16) 0.0088(15) N2 0.0330(19) 0.0216(18) 0.0285(18) 0.0080(15) 0.0055(15) -0.0011(14) N3 0.0277(18) 0.040(2) 0.0196(17) 0.0122(15) -0.0008(15) -0.0028(15) F1 0.082(2) 0.0561(17) 0.0315(14) 0.0212(13) 0.0189(14) -0.0027(15) F2 0.0401(15) 0.0363(14) 0.0453(15) 0.0039(12) 0.0151(13) 0.0087(12) F3 0.0294(14) 0.0509(16) 0.0384(14) 0.0144(12) -0.0025(11) -0.0016(12) S1 0.0307(5) 0.0277(5) 0.0246(5) 0.0108(4) 0.0103(4) 0.0063(4) C20 0.087(5) 0.060(4) 0.077(4) 0.034(4) 0.032(4) -0.010(3) C21 0.096(5) 0.064(4) 0.045(3) 0.030(3) 0.009(4) -0.026(4) C22 0.062(4) 0.075(4) 0.069(4) 0.042(4) 0.006(3) -0.012(3) C23 0.029(2) 0.036(2) 0.033(2) 0.0156(19) 0.0047(18) 0.0011(18) O10 0.0302(17) 0.0367(17) 0.0388(17) 0.0202(15) 0.0112(14) 0.0035(14) _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 Al1 O6 1.861(2) . ? Al1 O4 1.862(2) . ? Al1 O5 1.868(3) . ? Al1 O2 1.872(2) . ? Al1 O3 1.874(2) . ? Al1 O1 1.879(3) . ? Ag1 N3 2.181(3) 1_454 ? Ag1 N2 2.229(3) 1_565 ? Ag1 N1 2.256(3) . ? Ag1 O9 2.531(3) . ? O1 C2 1.269(4) . ? O2 C4 1.275(4) . ? O3 C8 1.259(4) . ? O4 C10 1.269(4) . ? O5 C14 1.260(4) . ? O6 C16 1.267(4) . ? O7 S1 1.435(3) . ? O8 S1 1.436(3) . ? O9 S1 1.442(3) . ? C1 C2 1.496(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.413(5) . ? C3 C4 1.406(5) . ? C3 C6 1.426(5) . ? C4 C5 1.491(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.142(4) . ? C7 C8 1.490(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.425(5) . ? C9 C10 1.412(5) . ? C9 C12 1.429(5) . ? C10 C11 1.480(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.134(4) . ? C13 C14 1.491(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.411(5) . ? C15 C16 1.406(5) . ? C15 C18 1.431(5) . ? C16 C17 1.496(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.137(4) . ? C19 F1 1.327(4) . ? C19 F2 1.332(4) . ? C19 F3 1.333(4) . ? C19 S1 1.812(4) . ? N2 Ag1 2.229(3) 1_545 ? N3 Ag1 2.181(3) 1_656 ? C20 C22 1.379(8) 2 ? C20 C21 1.398(8) . ? C20 H20 0.9500 . ? C21 C22 1.362(9) . ? C21 H21 0.9500 . ? C22 C20 1.379(8) 2 ? C22 H22 0.9500 . ? C23 O10 1.420(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O10 H10 0.76(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Al1 O4 177.26(12) . . ? O6 Al1 O5 91.16(11) . . ? O4 Al1 O5 91.48(11) . . ? O6 Al1 O2 91.75(11) . . ? O4 Al1 O2 87.60(11) . . ? O5 Al1 O2 88.27(11) . . ? O6 Al1 O3 90.27(11) . . ? O4 Al1 O3 90.46(11) . . ? O5 Al1 O3 90.33(11) . . ? O2 Al1 O3 177.57(12) . . ? O6 Al1 O1 88.47(11) . . ? O4 Al1 O1 88.88(11) . . ? O5 Al1 O1 179.27(11) . . ? O2 Al1 O1 91.11(11) . . ? O3 Al1 O1 90.30(11) . . ? N3 Ag1 N2 132.62(12) 1_454 1_565 ? N3 Ag1 N1 122.63(12) 1_454 . ? N2 Ag1 N1 100.21(12) 1_565 . ? N3 Ag1 O9 96.38(12) 1_454 . ? N2 Ag1 O9 97.94(12) 1_565 . ? N1 Ag1 O9 96.53(11) . . ? C2 O1 Al1 128.6(2) . . ? C4 O2 Al1 129.7(2) . . ? C8 O3 Al1 130.1(2) . . ? C10 O4 Al1 130.3(2) . . ? C14 O5 Al1 130.4(2) . . ? C16 O6 Al1 129.7(2) . . ? S1 O9 Ag1 138.48(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.7(3) . . ? O1 C2 C1 116.8(3) . . ? C3 C2 C1 120.5(3) . . ? C4 C3 C2 124.4(3) . . ? C4 C3 C6 118.0(3) . . ? C2 C3 C6 117.6(3) . . ? O2 C4 C3 121.3(3) . . ? O2 C4 C5 117.2(3) . . ? C3 C4 C5 121.5(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 178.3(4) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 122.3(3) . . ? O3 C8 C7 117.5(3) . . ? C9 C8 C7 120.2(3) . . ? C10 C9 C8 123.0(3) . . ? C10 C9 C12 117.6(3) . . ? C8 C9 C12 119.5(3) . . ? O4 C10 C9 121.6(3) . . ? O4 C10 C11 115.8(3) . . ? C9 C10 C11 122.6(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 176.3(4) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 121.9(3) . . ? O5 C14 C13 117.5(3) . . ? C15 C14 C13 120.6(3) . . ? C16 C15 C14 123.6(3) . . ? C16 C15 C18 118.0(3) . . ? C14 C15 C18 118.3(3) . . ? O6 C16 C15 122.7(3) . . ? O6 C16 C17 116.1(3) . . ? C15 C16 C17 121.3(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 179.6(5) . . ? F1 C19 F2 107.1(3) . . ? F1 C19 F3 107.5(3) . . ? F2 C19 F3 106.9(3) . . ? F1 C19 S1 111.9(3) . . ? F2 C19 S1 111.2(3) . . ? F3 C19 S1 112.0(3) . . ? C6 N1 Ag1 153.1(3) . . ? C12 N2 Ag1 170.7(3) . 1_545 ? C18 N3 Ag1 171.4(3) . 1_656 ? O7 S1 O8 114.68(18) . . ? O7 S1 O9 115.53(19) . . ? O8 S1 O9 115.00(19) . . ? O7 S1 C19 103.20(18) . . ? O8 S1 C19 103.13(18) . . ? O9 S1 C19 102.77(19) . . ? C22 C20 C21 119.8(6) 2 . ? C22 C20 H20 120.1 2 . ? C21 C20 H20 120.1 . . ? C22 C21 C20 121.7(6) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C20 118.5(6) . 2 ? C21 C22 H22 120.7 . . ? C20 C22 H22 120.7 2 . ? O10 C23 H23A 109.5 . . ? O10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C23 O10 H10 105(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.576 _refine_diff_density_min -0.783 _refine_diff_density_rms 0.093 data_3b _database_code_depnum_ccdc_archive 'CCDC 872088' #TrackingRef '- complete_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3b _chemical_melting_point ? _chemical_formula_moiety '2(C19 H18 Ag Al F3 N3 O9 S), 2(C3.50 H4), 2(C H4 O)' _chemical_formula_sum 'C47 H52 Ag2 Al2 F6 N6 O20 S2' _chemical_formula_weight 1468.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5796(14) _cell_length_b 12.4622(16) _cell_length_c 13.5444(18) _cell_angle_alpha 115.7537(18) _cell_angle_beta 107.7236(20) _cell_angle_gamma 93.4840(21) _cell_volume 1492.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5929 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8220 _exptl_absorpt_correction_T_max 0.8975 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18975 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.62 _reflns_number_total 6946 _reflns_number_gt 6085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.1972P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6946 _refine_ls_number_parameters 387 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL c11_51 in P-1 CELL 0.71073 10.5796 12.4622 13.5444 115.754 107.724 93.484 ZERR 2.00 0.0014 0.0016 0.0018 0.002 0.002 0.002 LATT 1 SFAC C H N O AL S AG F UNIT 47 52 6 20 2 2 2 6 TEMP -173 L.S. 6 BOND BOND$H ACTA 50 SIZE 0.19 0.24 0.13 FMAP 2 PLAN -10 WGHT 0.042400 1.197200 FVAR 0.45842 0.05831 MOLE 1 AG1 7 0.077971 0.951956 0.373399 11.00000 0.02805 0.02148 = 0.02090 0.01056 -0.00049 0.00007 AL1 5 -0.555792 0.662009 -0.235497 11.00000 0.01696 0.01594 = 0.01510 0.00678 0.00561 0.00289 O1 4 -0.513758 0.779027 -0.279948 11.00000 0.01892 0.01822 = 0.01991 0.00883 0.00663 0.00209 O2 4 -0.740954 0.667313 -0.282835 11.00000 0.01808 0.02453 = 0.02162 0.01422 0.00665 0.00465 O3 4 -0.593894 0.541675 -0.194403 11.00000 0.02412 0.01809 = 0.01777 0.00875 0.00843 0.00453 O4 4 -0.589183 0.541620 -0.388993 11.00000 0.02097 0.01769 = 0.01582 0.00628 0.00650 0.00001 O5 4 -0.528820 0.783350 -0.084139 11.00000 0.02088 0.01917 = 0.01783 0.00730 0.00691 0.00488 O6 4 -0.370814 0.657876 -0.189669 11.00000 0.01872 0.01964 = 0.01592 0.00683 0.00549 0.00404 C1 1 -0.526676 0.890586 -0.384448 11.00000 0.02556 0.02452 = 0.02514 0.01364 0.00995 0.00210 AFIX 137 H1A 2 -0.431658 0.928248 -0.330794 11.00000 -1.50000 H1B 2 -0.576073 0.954678 -0.384173 11.00000 -1.50000 H1C 2 -0.529833 0.838425 -0.464421 11.00000 -1.50000 AFIX 0 C2 1 -0.591623 0.814741 -0.344620 11.00000 0.02320 0.01392 = 0.01712 0.00485 0.00959 0.00350 C3 1 -0.734915 0.784808 -0.379454 11.00000 0.02271 0.01979 = 0.01878 0.01035 0.00834 0.00624 C4 1 -0.802965 0.710721 -0.347491 11.00000 0.02019 0.02153 = 0.01765 0.00928 0.00677 0.00544 C5 1 -0.955251 0.679694 -0.392296 11.00000 0.02148 0.04480 = 0.04035 0.03063 0.01116 0.00838 AFIX 137 H5A 2 -0.990979 0.622778 -0.477102 11.00000 -1.50000 H5B 2 -0.989083 0.754490 -0.378015 11.00000 -1.50000 H5C 2 -0.985437 0.641492 -0.351120 11.00000 -1.50000 AFIX 0 C6 1 -0.816104 0.831587 -0.449853 11.00000 0.02594 0.02502 = 0.02476 0.01453 0.01130 0.00536 C7 1 -0.666091 0.357130 -0.197930 11.00000 0.03037 0.02475 = 0.02995 0.01716 0.01382 0.00678 AFIX 137 H7A 2 -0.603514 0.301873 -0.201826 11.00000 -1.50000 H7B 2 -0.760249 0.309294 -0.237053 11.00000 -1.50000 H7C 2 -0.649386 0.413698 -0.115258 11.00000 -1.50000 AFIX 0 C8 1 -0.643459 0.427920 -0.258261 11.00000 0.01556 0.02159 = 0.02660 0.01387 0.00994 0.00656 C9 1 -0.677687 0.368879 -0.382171 11.00000 0.01456 0.01827 = 0.02164 0.00829 0.00739 0.00349 C10 1 -0.648845 0.429375 -0.442985 11.00000 0.01271 0.01907 = 0.01876 0.00590 0.00627 0.00371 C11 1 -0.686333 0.365850 -0.572852 11.00000 0.02145 0.02475 = 0.01956 0.00616 0.00897 -0.00033 AFIX 137 H11A 2 -0.750892 0.404242 -0.607898 11.00000 -1.50000 H11B 2 -0.728510 0.279598 -0.605083 11.00000 -1.50000 H11C 2 -0.604339 0.371786 -0.591284 11.00000 -1.50000 AFIX 0 C12 1 -0.741444 0.241954 -0.450111 11.00000 0.01977 0.02450 = 0.02632 0.01344 0.00954 0.00625 C13 1 -0.440528 0.916633 0.120275 11.00000 0.03249 0.02504 = 0.02020 0.00485 0.01249 0.00445 AFIX 137 H13A 2 -0.491508 0.973486 0.103088 11.00000 -1.50000 H13B 2 -0.350167 0.962115 0.180801 11.00000 -1.50000 H13C 2 -0.489734 0.874667 0.148878 11.00000 -1.50000 AFIX 0 C14 1 -0.425558 0.824645 0.010648 11.00000 0.02826 0.01461 = 0.01700 0.00690 0.00832 0.00044 C15 1 -0.301683 0.787733 0.013559 11.00000 0.01948 0.01997 = 0.01465 0.00769 0.00270 0.00018 C16 1 -0.278760 0.707489 -0.089129 11.00000 0.01978 0.01599 = 0.02060 0.01098 0.00744 0.00166 C17 1 -0.141042 0.680677 -0.080330 11.00000 0.01854 0.02997 = 0.02935 0.01390 0.00756 0.00658 AFIX 137 H17A 2 -0.144409 0.621424 -0.158421 11.00000 -1.50000 H17B 2 -0.113546 0.646665 -0.026048 11.00000 -1.50000 H17C 2 -0.074930 0.756373 -0.050754 11.00000 -1.50000 AFIX 0 C18 1 -0.191081 0.838782 0.124210 11.00000 0.02394 0.02587 = 0.02034 0.01171 0.00718 0.00095 N1 3 -0.881492 0.871382 -0.503233 11.00000 0.03266 0.03763 = 0.03607 0.02526 0.01534 0.01130 N2 3 -0.796140 0.141165 -0.509286 11.00000 0.03068 0.02198 = 0.03102 0.00958 0.00700 0.00000 N3 3 -0.103368 0.878576 0.213288 11.00000 0.02914 0.03862 = 0.02310 0.01417 0.00450 -0.00255 MOLE 2 S1 6 0.317455 0.762750 0.266423 11.00000 0.02800 0.02588 = 0.02776 0.01134 0.01378 0.00616 C19 1 0.254690 0.648203 0.111144 11.00000 0.03224 0.02967 = 0.03100 0.01338 0.01252 0.00425 F1 8 0.321861 0.558418 0.093512 11.00000 0.04212 0.02995 = 0.04738 0.00602 0.01914 0.00897 F2 8 0.123343 0.596666 0.071406 11.00000 0.02908 0.04954 = 0.04386 0.01808 0.00089 -0.00234 F3 8 0.270210 0.696859 0.044193 11.00000 0.07855 0.05157 = 0.03412 0.02324 0.02064 0.00222 O7 4 0.233053 0.849132 0.268015 11.00000 0.05084 0.04585 = 0.05050 0.01871 0.02739 0.02759 O8 4 0.457083 0.807183 0.290838 11.00000 0.03141 0.02954 = 0.03969 0.01148 0.01418 0.00009 O9 4 0.296298 0.692968 0.323178 11.00000 0.04040 0.04731 = 0.03664 0.02281 0.01446 -0.00124 MOLE 3 PART -1 SADI .02 C20 C21 C21 C22 C22 C23 C23 C24 C24 C25 C25 C20 SADI .02 C20 C22 C21 C23 C22 C24 C23 C25 C24 C20 C25 C21 DFIX 1.5 C20 C26 SADI 0.04 C21 C26 C25 C26 FLAT C20 > C26 C20 1 0.057080 -0.031302 -0.022280 10.50000 21.00000 C21 1 -0.051785 -0.027488 -0.099732 10.50000 21.00000 AFIX 43 H21 2 -0.060584 -0.064794 -0.180079 10.50000 -1.20000 AFIX 0 C22 1 -0.160024 0.031363 -0.068288 10.50000 21.00000 AFIX 43 H22 2 -0.239325 0.032420 -0.124328 10.50000 -1.20000 AFIX 0 C23 1 -0.134086 0.086343 0.054064 10.50000 21.00000 AFIX 43 H23 2 -0.194880 0.130290 0.085565 10.50000 -1.20000 AFIX 0 C24 1 -0.021370 0.074687 0.124259 10.50000 21.00000 AFIX 43 H24 2 -0.010271 0.110472 0.205097 10.50000 -1.20000 AFIX 0 C25 1 0.079815 0.019405 0.097561 10.50000 21.00000 AFIX 43 H25 2 0.156708 0.015864 0.153957 10.50000 -1.20000 AFIX 0 C26 1 0.160612 -0.095735 -0.059122 10.50000 0.10901 AFIX 137 H26A 2 0.120648 -0.183706 -0.107254 10.50000 -1.50000 H26B 2 0.238109 -0.080813 0.010863 10.50000 -1.50000 H26C 2 0.191717 -0.065405 -0.105399 10.50000 -1.50000 AFIX 0 PART 0 MOLE 4 O10 4 0.102856 0.541293 0.339565 11.00000 0.02635 0.03897 = 0.03737 0.02213 0.01168 0.00569 H10A 2 0.167165 0.584568 0.344203 11.00000 0.05617 C27 1 -0.019484 0.552522 0.267956 11.00000 0.02667 0.04183 = 0.03884 0.01965 0.01185 0.00800 AFIX 137 H27A 2 -0.027479 0.637868 0.303056 11.00000 -1.50000 H27B 2 -0.097386 0.500454 0.262368 11.00000 -1.50000 H27C 2 -0.018128 0.527006 0.188958 11.00000 -1.50000 HKLF 4 ; 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 0.07797(2) 0.951956(19) 0.373399(18) 0.02605(8) Uani 1 1 d . . . Al1 Al -0.55579(8) 0.66201(7) -0.23550(6) 0.01636(16) Uani 1 1 d . . . O1 O -0.51376(18) 0.77903(16) -0.27995(16) 0.0194(4) Uani 1 1 d . . . O2 O -0.74095(18) 0.66731(17) -0.28284(16) 0.0203(4) Uani 1 1 d . . . O3 O -0.59389(19) 0.54167(16) -0.19440(16) 0.0197(4) Uani 1 1 d . . . O4 O -0.58918(18) 0.54162(16) -0.38899(15) 0.0191(4) Uani 1 1 d . . . O5 O -0.52882(18) 0.78335(16) -0.08414(15) 0.0199(4) Uani 1 1 d . . . O6 O -0.37081(18) 0.65788(16) -0.18967(15) 0.0190(4) Uani 1 1 d . . . C1 C -0.5267(3) 0.8906(3) -0.3844(2) 0.0244(6) Uani 1 1 d . . . H1A H -0.4317 0.9282 -0.3308 0.037 Uiso 1 1 calc R . . H1B H -0.5761 0.9547 -0.3842 0.037 Uiso 1 1 calc R . . H1C H -0.5298 0.8384 -0.4644 0.037 Uiso 1 1 calc R . . C2 C -0.5916(3) 0.8147(2) -0.3446(2) 0.0185(5) Uani 1 1 d . . . C3 C -0.7349(3) 0.7848(2) -0.3795(2) 0.0197(5) Uani 1 1 d . . . C4 C -0.8030(3) 0.7107(2) -0.3475(2) 0.0198(5) Uani 1 1 d . . . C5 C -0.9553(3) 0.6797(3) -0.3923(3) 0.0315(7) Uani 1 1 d . . . H5A H -0.9910 0.6228 -0.4771 0.047 Uiso 1 1 calc R . . H5B H -0.9891 0.7545 -0.3780 0.047 Uiso 1 1 calc R . . H5C H -0.9854 0.6415 -0.3511 0.047 Uiso 1 1 calc R . . C6 C -0.8161(3) 0.8316(3) -0.4499(2) 0.0237(6) Uani 1 1 d . . . C7 C -0.6661(3) 0.3571(3) -0.1979(3) 0.0260(6) Uani 1 1 d . . . H7A H -0.6035 0.3019 -0.2018 0.039 Uiso 1 1 calc R . . H7B H -0.7602 0.3093 -0.2371 0.039 Uiso 1 1 calc R . . H7C H -0.6494 0.4137 -0.1153 0.039 Uiso 1 1 calc R . . C8 C -0.6435(3) 0.4279(2) -0.2583(2) 0.0196(5) Uani 1 1 d . . . C9 C -0.6777(3) 0.3689(2) -0.3822(2) 0.0185(5) Uani 1 1 d . . . C10 C -0.6488(2) 0.4294(2) -0.4430(2) 0.0179(5) Uani 1 1 d . . . C11 C -0.6863(3) 0.3659(3) -0.5729(2) 0.0236(6) Uani 1 1 d . . . H11A H -0.7509 0.4042 -0.6079 0.035 Uiso 1 1 calc R . . H11B H -0.7285 0.2796 -0.6051 0.035 Uiso 1 1 calc R . . H11C H -0.6043 0.3718 -0.5913 0.035 Uiso 1 1 calc R . . C12 C -0.7414(3) 0.2420(3) -0.4501(2) 0.0227(5) Uani 1 1 d . . . C13 C -0.4405(3) 0.9166(3) 0.1203(2) 0.0276(6) Uani 1 1 d . . . H13A H -0.4915 0.9735 0.1031 0.041 Uiso 1 1 calc R . . H13B H -0.3502 0.9621 0.1808 0.041 Uiso 1 1 calc R . . H13C H -0.4897 0.8747 0.1489 0.041 Uiso 1 1 calc R . . C14 C -0.4256(3) 0.8246(2) 0.0106(2) 0.0204(5) Uani 1 1 d . . . C15 C -0.3017(3) 0.7877(2) 0.0136(2) 0.0194(5) Uani 1 1 d . . . C16 C -0.2788(3) 0.7075(2) -0.0891(2) 0.0180(5) Uani 1 1 d . . . C17 C -0.1410(3) 0.6807(3) -0.0803(3) 0.0263(6) Uani 1 1 d . . . H17A H -0.1444 0.6214 -0.1584 0.039 Uiso 1 1 calc R . . H17B H -0.1135 0.6467 -0.0260 0.039 Uiso 1 1 calc R . . H17C H -0.0749 0.7564 -0.0508 0.039 Uiso 1 1 calc R . . C18 C -0.1911(3) 0.8388(3) 0.1242(2) 0.0236(6) Uani 1 1 d . . . N1 N -0.8815(3) 0.8714(2) -0.5032(2) 0.0316(6) Uani 1 1 d . . . N2 N -0.7961(3) 0.1412(2) -0.5093(2) 0.0305(6) Uani 1 1 d . . . N3 N -0.1034(3) 0.8786(2) 0.2133(2) 0.0323(6) Uani 1 1 d . . . S1 S 0.31746(8) 0.76275(7) 0.26642(6) 0.02686(16) Uani 1 1 d . . . C19 C 0.2547(3) 0.6482(3) 0.1111(3) 0.0313(7) Uani 1 1 d . . . F1 F 0.3219(2) 0.55842(17) 0.09351(18) 0.0440(5) Uani 1 1 d . . . F2 F 0.1233(2) 0.59667(19) 0.07141(18) 0.0463(5) Uani 1 1 d . . . F3 F 0.2702(3) 0.6969(2) 0.04419(18) 0.0543(6) Uani 1 1 d . . . O7 O 0.2331(3) 0.8491(2) 0.2680(2) 0.0476(6) Uani 1 1 d . . . O8 O 0.4571(2) 0.8072(2) 0.2908(2) 0.0356(5) Uani 1 1 d . . . O9 O 0.2963(2) 0.6930(2) 0.3232(2) 0.0408(6) Uani 1 1 d . . . C20 C 0.0571(8) -0.0313(8) -0.0223(7) 0.0583(9) Uiso 0.50 1 d PD A -1 C21 C -0.0518(9) -0.0275(9) -0.0997(9) 0.0583(9) Uiso 0.50 1 d PD A -1 H21 H -0.0606 -0.0648 -0.1801 0.070 Uiso 0.50 1 calc PR A -1 C22 C -0.1600(8) 0.0314(8) -0.0683(7) 0.0583(9) Uiso 0.50 1 d PD A -1 H22 H -0.2393 0.0324 -0.1243 0.070 Uiso 0.50 1 calc PR A -1 C23 C -0.1341(11) 0.0863(11) 0.0541(8) 0.0583(9) Uiso 0.50 1 d PD A -1 H23 H -0.1949 0.1303 0.0856 0.070 Uiso 0.50 1 calc PR A -1 C24 C -0.0214(8) 0.0747(8) 0.1243(7) 0.0583(9) Uiso 0.50 1 d PD A -1 H24 H -0.0103 0.1105 0.2051 0.070 Uiso 0.50 1 calc PR A -1 C25 C 0.0798(10) 0.0194(10) 0.0976(9) 0.0583(9) Uiso 0.50 1 d PD A -1 H25 H 0.1567 0.0159 0.1540 0.070 Uiso 0.50 1 calc PR A -1 C26 C 0.1606(17) -0.0957(18) -0.0591(15) 0.109(5) Uiso 0.50 1 d PD A -1 H26A H 0.1206 -0.1837 -0.1073 0.164 Uiso 0.50 1 calc PR A -1 H26B H 0.2381 -0.0808 0.0109 0.164 Uiso 0.50 1 calc PR A -1 H26C H 0.1917 -0.0654 -0.1054 0.164 Uiso 0.50 1 calc PR A -1 O10 O 0.1029(2) 0.5413(2) 0.3396(2) 0.0328(5) Uani 1 1 d . . . H10A H 0.167(4) 0.585(4) 0.344(4) 0.056(13) Uiso 1 1 d . . . C27 C -0.0195(3) 0.5525(3) 0.2680(3) 0.0356(7) Uani 1 1 d . . . H27A H -0.0275 0.6379 0.3031 0.053 Uiso 1 1 calc R . . H27B H -0.0974 0.5005 0.2624 0.053 Uiso 1 1 calc R . . H27C H -0.0181 0.5270 0.1890 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02805(13) 0.02148(12) 0.02090(12) 0.01056(9) -0.00049(9) 0.00007(8) Al1 0.0170(4) 0.0159(4) 0.0151(4) 0.0068(3) 0.0056(3) 0.0029(3) O1 0.0189(9) 0.0182(9) 0.0199(9) 0.0088(7) 0.0066(7) 0.0021(7) O2 0.0181(9) 0.0245(9) 0.0216(9) 0.0142(8) 0.0067(8) 0.0047(7) O3 0.0241(10) 0.0181(9) 0.0178(9) 0.0088(7) 0.0084(8) 0.0045(7) O4 0.0210(9) 0.0177(9) 0.0158(8) 0.0063(7) 0.0065(7) 0.0000(7) O5 0.0209(9) 0.0192(9) 0.0178(9) 0.0073(7) 0.0069(7) 0.0049(7) O6 0.0187(9) 0.0196(9) 0.0159(9) 0.0068(7) 0.0055(7) 0.0040(7) C1 0.0256(14) 0.0245(14) 0.0251(14) 0.0136(12) 0.0099(12) 0.0021(11) C2 0.0232(13) 0.0139(11) 0.0171(12) 0.0049(10) 0.0096(10) 0.0035(10) C3 0.0227(13) 0.0198(12) 0.0188(12) 0.0103(10) 0.0083(10) 0.0062(10) C4 0.0202(13) 0.0215(13) 0.0176(12) 0.0093(10) 0.0068(10) 0.0054(10) C5 0.0215(14) 0.0448(18) 0.0403(17) 0.0306(15) 0.0112(13) 0.0084(13) C6 0.0259(14) 0.0250(14) 0.0248(14) 0.0145(12) 0.0113(12) 0.0054(11) C7 0.0304(15) 0.0247(14) 0.0299(15) 0.0172(12) 0.0138(12) 0.0068(12) C8 0.0156(12) 0.0216(13) 0.0266(13) 0.0139(11) 0.0099(11) 0.0066(10) C9 0.0146(12) 0.0183(12) 0.0216(12) 0.0083(10) 0.0074(10) 0.0035(10) C10 0.0127(11) 0.0191(12) 0.0188(12) 0.0059(10) 0.0063(10) 0.0037(9) C11 0.0214(13) 0.0247(14) 0.0196(13) 0.0062(11) 0.0090(11) -0.0003(11) C12 0.0198(13) 0.0245(14) 0.0263(14) 0.0134(12) 0.0095(11) 0.0063(11) C13 0.0325(16) 0.0250(14) 0.0202(13) 0.0049(12) 0.0125(12) 0.0044(12) C14 0.0283(14) 0.0146(12) 0.0170(12) 0.0069(10) 0.0083(11) 0.0004(10) C15 0.0195(12) 0.0200(12) 0.0146(12) 0.0077(10) 0.0027(10) 0.0002(10) C16 0.0198(12) 0.0160(12) 0.0206(12) 0.0110(10) 0.0074(10) 0.0017(10) C17 0.0185(13) 0.0300(15) 0.0294(15) 0.0139(12) 0.0076(11) 0.0066(11) C18 0.0239(14) 0.0259(14) 0.0203(13) 0.0117(11) 0.0072(11) 0.0010(11) N1 0.0327(14) 0.0376(15) 0.0361(14) 0.0253(13) 0.0153(12) 0.0113(12) N2 0.0307(14) 0.0220(13) 0.0310(13) 0.0096(11) 0.0070(11) 0.0000(10) N3 0.0291(14) 0.0386(15) 0.0231(12) 0.0142(11) 0.0045(11) -0.0026(11) S1 0.0280(4) 0.0259(3) 0.0278(4) 0.0113(3) 0.0138(3) 0.0062(3) C19 0.0322(16) 0.0297(16) 0.0310(16) 0.0134(13) 0.0125(13) 0.0042(13) F1 0.0421(11) 0.0299(10) 0.0474(12) 0.0060(9) 0.0191(10) 0.0090(9) F2 0.0291(10) 0.0495(12) 0.0439(12) 0.0181(10) 0.0009(9) -0.0023(9) F3 0.0786(16) 0.0516(13) 0.0341(11) 0.0232(10) 0.0206(11) 0.0022(12) O7 0.0508(15) 0.0458(15) 0.0505(15) 0.0187(12) 0.0274(13) 0.0276(13) O8 0.0314(12) 0.0295(11) 0.0397(13) 0.0115(10) 0.0142(10) 0.0001(9) O9 0.0404(13) 0.0473(14) 0.0366(13) 0.0228(11) 0.0145(11) -0.0012(11) O10 0.0263(11) 0.0390(13) 0.0374(12) 0.0221(11) 0.0117(10) 0.0057(10) C27 0.0267(16) 0.0418(18) 0.0388(18) 0.0197(15) 0.0118(14) 0.0080(14) _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 2.179(3) . ? Ag1 N2 2.221(2) 1_666 ? Ag1 N1 2.249(2) 1_656 ? Ag1 O7 2.542(2) . ? Al1 O5 1.8623(19) . ? Al1 O4 1.8644(18) . ? Al1 O3 1.8734(19) . ? Al1 O6 1.8757(19) . ? Al1 O1 1.8799(19) . ? Al1 O2 1.882(2) . ? O1 C2 1.260(3) . ? O2 C4 1.263(3) . ? O3 C8 1.265(3) . ? O4 C10 1.270(3) . ? O5 C14 1.269(3) . ? O6 C16 1.254(3) . ? C1 C2 1.499(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.415(4) . ? C3 C4 1.419(4) . ? C3 C6 1.426(4) . ? C4 C5 1.496(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.138(4) . ? C7 C8 1.491(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.419(4) . ? C9 C10 1.416(4) . ? C9 C12 1.425(4) . ? C10 C11 1.485(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N2 1.144(4) . ? C13 C14 1.493(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.410(4) . ? C15 C16 1.421(4) . ? C15 C18 1.426(4) . ? C16 C17 1.496(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.142(4) . ? N1 Ag1 2.249(2) 1_454 ? N2 Ag1 2.221(2) 1_444 ? S1 O8 1.429(2) . ? S1 O9 1.435(2) . ? S1 O7 1.437(2) . ? S1 C19 1.824(3) . ? C19 F2 1.330(4) . ? C19 F3 1.332(4) . ? C19 F1 1.335(4) . ? C20 C21 1.320(10) . ? C20 C25 1.394(10) . ? C20 C26 1.478(14) . ? C21 C22 1.469(10) . ? C21 H21 0.9500 . ? C22 C23 1.416(10) . ? C22 H22 0.9500 . ? C23 C24 1.341(10) . ? C23 H23 0.9500 . ? C24 C25 1.364(10) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O10 C27 1.418(4) . ? O10 H10A 0.81(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N2 130.57(10) . 1_666 ? N3 Ag1 N1 122.65(10) . 1_656 ? N2 Ag1 N1 101.84(10) 1_666 1_656 ? N3 Ag1 O7 94.80(9) . . ? N2 Ag1 O7 101.27(9) 1_666 . ? N1 Ag1 O7 96.04(9) 1_656 . ? O5 Al1 O4 177.87(9) . . ? O5 Al1 O3 90.09(8) . . ? O4 Al1 O3 90.34(8) . . ? O5 Al1 O6 91.04(8) . . ? O4 Al1 O6 91.04(8) . . ? O3 Al1 O6 90.45(9) . . ? O5 Al1 O1 91.59(8) . . ? O4 Al1 O1 88.04(8) . . ? O3 Al1 O1 177.80(9) . . ? O6 Al1 O1 88.09(8) . . ? O5 Al1 O2 89.25(8) . . ? O4 Al1 O2 88.67(9) . . ? O3 Al1 O2 90.39(8) . . ? O6 Al1 O2 179.12(9) . . ? O1 Al1 O2 91.06(8) . . ? C2 O1 Al1 129.60(17) . . ? C4 O2 Al1 128.37(17) . . ? C8 O3 Al1 130.37(17) . . ? C10 O4 Al1 130.45(16) . . ? C14 O5 Al1 129.95(17) . . ? C16 O6 Al1 130.17(17) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.0(2) . . ? O1 C2 C1 117.4(2) . . ? C3 C2 C1 120.6(2) . . ? C2 C3 C4 123.5(2) . . ? C2 C3 C6 118.8(2) . . ? C4 C3 C6 117.8(2) . . ? O2 C4 C3 123.1(2) . . ? O2 C4 C5 117.1(2) . . ? C3 C4 C5 119.8(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 178.0(3) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C9 122.2(2) . . ? O3 C8 C7 117.1(2) . . ? C9 C8 C7 120.7(2) . . ? C10 C9 C8 123.2(2) . . ? C10 C9 C12 117.4(2) . . ? C8 C9 C12 119.4(2) . . ? O4 C10 C9 121.6(2) . . ? O4 C10 C11 116.2(2) . . ? C9 C10 C11 122.2(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C9 176.5(3) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 C15 122.4(2) . . ? O5 C14 C13 116.6(2) . . ? C15 C14 C13 121.0(2) . . ? C14 C15 C16 123.3(2) . . ? C14 C15 C18 118.5(2) . . ? C16 C15 C18 118.1(2) . . ? O6 C16 C15 122.2(2) . . ? O6 C16 C17 117.5(2) . . ? C15 C16 C17 120.3(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C15 179.0(3) . . ? C6 N1 Ag1 153.3(2) . 1_454 ? C12 N2 Ag1 174.2(2) . 1_444 ? C18 N3 Ag1 174.1(2) . . ? O8 S1 O9 114.66(15) . . ? O8 S1 O7 114.82(15) . . ? O9 S1 O7 115.67(16) . . ? O8 S1 C19 103.14(14) . . ? O9 S1 C19 102.96(14) . . ? O7 S1 C19 103.08(15) . . ? F2 C19 F3 107.7(3) . . ? F2 C19 F1 107.0(2) . . ? F3 C19 F1 107.3(3) . . ? F2 C19 S1 111.9(2) . . ? F3 C19 S1 111.4(2) . . ? F1 C19 S1 111.2(2) . . ? S1 O7 Ag1 139.34(16) . . ? C21 C20 C25 123.1(7) . . ? C21 C20 C26 121.4(9) . . ? C25 C20 C26 115.4(9) . . ? C20 C21 C22 123.5(8) . . ? C20 C21 H21 118.2 . . ? C22 C21 H21 118.2 . . ? C23 C22 C21 113.1(7) . . ? C23 C22 H22 123.4 . . ? C21 C22 H22 123.4 . . ? C24 C23 C22 118.2(8) . . ? C24 C23 H23 120.9 . . ? C22 C23 H23 120.9 . . ? C23 C24 C25 130.0(8) . . ? C23 C24 H24 115.0 . . ? C25 C24 H24 115.0 . . ? C24 C25 C20 112.0(7) . . ? C24 C25 H25 124.0 . . ? C20 C25 H25 124.0 . . ? C27 O10 H10A 109(3) . . ? O10 C27 H27A 109.5 . . ? O10 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O10 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.074 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.087 data_3c_100K _database_code_depnum_ccdc_archive 'CCDC 872089' #TrackingRef '- complete_cif.cif' _vrf_CHEMW03_3c_100K ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 467.78 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 13.00 156.14 N 14.01 2.00 28.01 O 16.00 5.00 79.99 Al 26.98 1.00 26.98 Ag 107.87 0.50 53.93 H 1.01 15.00 15.12 Calculated formula weight 360.19 RESPONSE: After assignment of the well-ordered electron density maxima, two large voids at Wyckoff positions 2c and 2e remained. The BYPASS procedure as implemented in PLATON indicated the presence of 61 and 63 electrons in the voids. Difference Fourier syntheses did not allow to construct a chemically meaningful disorder model. Electron count, void volume and results from thermal analysis are in reasonable agreement with the assignment of eleven water molecules and one hydroxide conteranion. Further information to the BYPASS calculation on this data set are implemented in the CIF. ; _vrf_PLAT043_3c_100K ; PROBLEM: Check Reported Molecular Weight ................ 467.78 RESPONSE: After assignment of the well-ordered electron density maxima, two large voids at Wyckoff positions 2c and 2e remained. The BYPASS procedure as implemented in PLATON indicated the presence of 61 and 63 electrons in the voids. Difference Fourier syntheses did not allow to construct a chemically meaningful disorder model. Electron count, void volume and results from thermal analysis are in reasonable agreement with the assignment of eleven water molecules and one hydroxide conteranion. Further information to the BYPASS calculation on this data set are implemented in the CIF. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3c_100K _chemical_melting_point ? _chemical_formula_moiety 'C13 H15 Ag0.5 Al N2 O5, 5(H2 O), 0.5(O H)' _chemical_formula_sum 'C13 H26.50 Ag0.50 Al N2 O11' _chemical_formula_weight 467.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c m' _symmetry_space_group_name_Hall '-P 2 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z-1/2' '-x, y, z-1/2' _cell_length_a 7.5718(10) _cell_length_b 10.8468(15) _cell_length_c 23.771(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1952.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2170 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 18.70 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8920 _exptl_absorpt_correction_T_max 0.9379 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source microsource _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21738 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.67 _reflns_number_total 2114 _reflns_number_gt 1636 _reflns_threshold_expression >2sigma(I) # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.024 0.000 0.250 122 63 '5 H2O, OH- ' 2 -0.024 0.000 0.750 122 63 '5 H2O, OH- ' 3 -0.041 0.500 0.000 155 61 '6 H2O' 4 -0.024 0.500 0.500 155 61 '6 H2O' _platon_squeeze_details ; refinement of the expected constituents resulted in unsatisfactory agreement, in particular with respect to low resoltion reflection. Difference Fourier syntheses did not allow to construct a chemically meaningful disorder model. Most likely, the voids contain one hydroxide counteranion and 11 water molecules per formula unit; this assignment is in reasonable agreement with electron count, void volume and results from thermal analyses. ; _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+7.0946P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2114 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1547 _refine_ls_wR_factor_gt 0.1444 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL c11_49 in Pccm CELL 0.71073 7.5718 10.8468 23.7714 90.000 90.000 90.000 ZERR 4.00 0.0010 0.0015 0.0032 0.000 0.000 0.000 LATT 1 SYMM -X, -Y, Z SYMM -X, Y, 0.5-Z SYMM X, -Y, 0.5-Z SFAC C N O AL AG H UNIT 52 8 44 4 2 106 TEMP -173.16 L.S. 10 ACTA SIZE 0.10 0.11 0.18 BOND BOND$H FMAP 2 PLAN -20 WGHT 0.051500 7.094600 FVAR 13.05943 MOLE 1 AG1 5 0.000000 0.500000 0.250000 10.25000 0.03215 0.03619 = 0.05952 0.00000 0.00000 0.00000 AL1 4 0.500000 0.000000 0.439975 10.50000 0.02219 0.04271 = 0.04075 0.00000 0.00000 0.00613 O1 3 0.269257 0.067489 0.434217 11.00000 0.01977 0.04276 = 0.04556 0.00597 0.00042 0.00385 O2 3 0.576122 0.115667 0.385826 11.00000 0.02303 0.07582 = 0.05162 0.02783 0.00774 0.01078 O3 3 0.562371 0.097904 0.500000 10.50000 0.02205 0.02495 = 0.04968 0.00000 0.00000 0.00056 C1 1 0.018064 0.182034 0.412399 11.00000 0.02605 0.06605 = 0.07966 0.01596 0.00252 0.01285 AFIX 137 H1A 6 -0.043447 0.161268 0.377385 11.00000 -1.50000 H1B 6 0.001914 0.269851 0.420613 11.00000 -1.50000 H1C 6 -0.030499 0.132807 0.443314 11.00000 -1.50000 AFIX 0 C2 1 0.209349 0.155024 0.406159 11.00000 0.02384 0.03750 = 0.04526 -0.00773 -0.00473 0.00680 C3 1 0.316223 0.224897 0.369089 11.00000 0.03008 0.04442 = 0.04447 0.00341 -0.00514 0.00720 C4 1 0.495246 0.205360 0.362240 11.00000 0.03393 0.06299 = 0.04405 0.01002 -0.00416 0.00306 C5 1 0.608515 0.288619 0.326487 11.00000 0.04215 0.09745 = 0.08825 0.05142 0.00195 0.00112 AFIX 137 H5A 6 0.667785 0.349218 0.350541 11.00000 -1.50000 H5B 6 0.534144 0.331541 0.299013 11.00000 -1.50000 H5C 6 0.697237 0.239212 0.306670 11.00000 -1.50000 AFIX 0 C6 1 0.237257 0.319967 0.336956 11.00000 0.03346 0.05969 = 0.07510 0.01346 0.00697 0.00834 C7 1 0.616738 0.239378 0.500000 10.50000 0.18004 0.28156 = 0.15001 0.00000 0.00000 0.17624 AFIX 3 H7A 6 0.694437 0.256744 0.532005 11.00000 -1.50000 H7B 6 0.509364 0.289366 0.500000 10.50000 -1.50000 AFIX 0 N1 2 0.169519 0.393434 0.309756 11.00000 0.05227 0.07974 = 0.10929 0.04905 0.01013 0.02446 HKLF 4 ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.5000 0.2500 0.0426(3) Uani 1 4 d S . . Al1 Al 0.5000 0.0000 0.43998(8) 0.0352(4) Uani 1 2 d S . . O1 O 0.2693(4) 0.0675(3) 0.43422(14) 0.0360(7) Uani 1 1 d . . . O2 O 0.5761(4) 0.1157(4) 0.38583(15) 0.0502(10) Uani 1 1 d . . . O3 O 0.5624(5) 0.0979(4) 0.5000 0.0322(10) Uani 1 2 d S . . C1 C 0.0181(7) 0.1820(6) 0.4124(3) 0.0573(15) Uani 1 1 d . . . H1A H -0.0434 0.1613 0.3774 0.086 Uiso 1 1 calc R . . H1B H 0.0019 0.2699 0.4206 0.086 Uiso 1 1 calc R . . H1C H -0.0305 0.1328 0.4433 0.086 Uiso 1 1 calc R . . C2 C 0.2093(6) 0.1550(4) 0.4062(2) 0.0355(10) Uani 1 1 d . . . C3 C 0.3162(6) 0.2249(5) 0.3691(2) 0.0397(11) Uani 1 1 d . . . C4 C 0.4952(7) 0.2054(5) 0.3622(2) 0.0470(12) Uani 1 1 d . . . C5 C 0.6085(8) 0.2886(7) 0.3265(3) 0.076(2) Uani 1 1 d . . . H5A H 0.6678 0.3492 0.3505 0.114 Uiso 1 1 calc R . . H5B H 0.5341 0.3315 0.2990 0.114 Uiso 1 1 calc R . . H5C H 0.6972 0.2392 0.3067 0.114 Uiso 1 1 calc R . . C6 C 0.2373(7) 0.3200(6) 0.3370(3) 0.0561(15) Uani 1 1 d . . . C7 C 0.617(3) 0.239(2) 0.5000 0.204(12) Uani 1 2 d S . . H7A H 0.6944 0.2567 0.5320 0.306 Uiso 1 1 d R . . H7B H 0.5094 0.2894 0.5000 0.306 Uiso 1 2 d SR . . N1 N 0.1695(7) 0.3934(5) 0.3098(3) 0.0804(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0321(4) 0.0362(4) 0.0595(5) 0.000 0.000 0.000 Al1 0.0222(8) 0.0427(10) 0.0408(10) 0.000 0.000 0.0061(9) O1 0.0198(14) 0.0428(18) 0.0456(18) 0.0060(15) 0.0004(14) 0.0038(14) O2 0.0230(15) 0.076(3) 0.052(2) 0.028(2) 0.0077(16) 0.0108(17) O3 0.0221(19) 0.025(2) 0.050(3) 0.000 0.000 0.0006(17) C1 0.026(2) 0.066(4) 0.080(4) 0.016(3) 0.003(3) 0.013(3) C2 0.024(2) 0.038(2) 0.045(3) -0.008(2) -0.005(2) 0.0068(19) C3 0.030(2) 0.044(3) 0.044(3) 0.003(2) -0.005(2) 0.007(2) C4 0.034(2) 0.063(3) 0.044(3) 0.010(2) -0.004(3) 0.003(3) C5 0.042(3) 0.097(5) 0.088(5) 0.051(4) 0.002(3) 0.001(3) C6 0.033(3) 0.060(4) 0.075(4) 0.013(3) 0.007(3) 0.008(3) C7 0.180(19) 0.28(3) 0.150(15) 0.000 0.000 0.18(2) N1 0.052(3) 0.080(4) 0.109(5) 0.049(4) 0.010(3) 0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.236(5) 3 ? Ag1 N1 2.236(5) 2_565 ? Ag1 N1 2.236(5) 4_565 ? Ag1 N1 2.236(5) . ? Al1 O3 1.840(3) 5_656 ? Al1 O3 1.840(3) . ? Al1 O2 1.888(4) . ? Al1 O2 1.888(4) 2_655 ? Al1 O1 1.899(3) . ? Al1 O1 1.899(3) 2_655 ? Al1 Al1 2.854(4) 5_656 ? O1 C2 1.246(5) . ? O2 C4 1.279(6) . ? O3 C7 1.59(2) . ? O3 Al1 1.840(3) 5_656 ? C1 C2 1.485(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.416(7) . ? C3 C4 1.382(7) . ? C3 C6 1.416(7) . ? C4 C5 1.508(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.147(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9772 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 109.9(3) 3 2_565 ? N1 Ag1 N1 101.1(3) 3 4_565 ? N1 Ag1 N1 117.8(4) 2_565 4_565 ? N1 Ag1 N1 117.8(4) 3 . ? N1 Ag1 N1 101.1(3) 2_565 . ? N1 Ag1 N1 109.9(3) 4_565 . ? O3 Al1 O3 78.3(2) 5_656 . ? O3 Al1 O2 172.14(18) 5_656 . ? O3 Al1 O2 93.83(16) . . ? O3 Al1 O2 93.83(16) 5_656 2_655 ? O3 Al1 O2 172.14(18) . 2_655 ? O2 Al1 O2 94.0(3) . 2_655 ? O3 Al1 O1 92.42(17) 5_656 . ? O3 Al1 O1 93.99(17) . . ? O2 Al1 O1 88.60(14) . . ? O2 Al1 O1 85.76(15) 2_655 . ? O3 Al1 O1 93.99(17) 5_656 2_655 ? O3 Al1 O1 92.42(17) . 2_655 ? O2 Al1 O1 85.77(15) . 2_655 ? O2 Al1 O1 88.60(14) 2_655 2_655 ? O1 Al1 O1 171.7(2) . 2_655 ? O3 Al1 Al1 39.16(11) 5_656 5_656 ? O3 Al1 Al1 39.16(11) . 5_656 ? O2 Al1 Al1 132.99(13) . 5_656 ? O2 Al1 Al1 132.99(13) 2_655 5_656 ? O1 Al1 Al1 94.13(11) . 5_656 ? O1 Al1 Al1 94.13(11) 2_655 5_656 ? C2 O1 Al1 131.9(3) . . ? C4 O2 Al1 131.2(3) . . ? C7 O3 Al1 128.60(14) . . ? C7 O3 Al1 128.60(14) . 5_656 ? Al1 O3 Al1 101.7(2) . 5_656 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 122.2(4) . . ? O1 C2 C1 116.9(5) . . ? C3 C2 C1 120.9(4) . . ? C4 C3 C6 117.5(5) . . ? C4 C3 C2 123.5(5) . . ? C6 C3 C2 119.0(4) . . ? O2 C4 C3 122.3(5) . . ? O2 C4 C5 115.5(5) . . ? C3 C4 C5 122.2(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 C3 177.2(7) . . ? O3 C7 H7A 109.9 . . ? O3 C7 H7B 108.7 . . ? H7A C7 H7B 113.1 . . ? C6 N1 Ag1 166.8(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.67 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.913 _refine_diff_density_min -1.024 _refine_diff_density_rms 0.089