# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address 'James Crowley' ; Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; 'Martin L. Gower' '' _publ_contact_author_name 'James Crowley' _publ_contact_author_email JCROWLEY@CHEMISTRY.OTAGO.AC.NZ _publ_section_title ; Self-assembly of silver (I) metallomacrocycles using unsupported 1,4-substituted-1,2,3-triazole "Click" ligands. ; #------------------ AUTHOR DETAILS -------------------------------------------# #Name and address of author for correspondence _publ_contact_author_address ; Department of Chemistry University of Otago P.O. Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_fax +64-3-04797731 _publ_contact_author_phone +64-3-04797906 # END of CIF # Attachment 'mlg134.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-08-18 at 12:54:57 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\program files\wingx\files\archive.reqdat # CIF files read : pcf mlg134 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_mlg134 _database_code_depnum_ccdc_archive 'CCDC 751438' #TrackingRef 'mlg134.cif' _audit_creation_date 2009-08-18T12:54:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C56 H40 Ag2 F20 N12 O2, 2(F6 Sb)' _chemical_formula_sum 'C56 H40 Ag2 F32 N12 O2 Sb2' _chemical_formula_weight 1980.24 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2003(15) _cell_length_b 13.2718(19) _cell_length_c 13.3767(21) _cell_angle_alpha 66.065(6) _cell_angle_beta 89.354(7) _cell_angle_gamma 89.478(7) _cell_volume 1655.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8238 _cell_measurement_theta_min 2.605 _cell_measurement_theta_max 26.384 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.85 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_number 29356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 6147 _reflns_number_gt 5664 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0316P)^2^+1.4140P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6147 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.071 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.675 _refine_diff_density_min -0.72 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.6634(3) 1.1281(2) 0.2536(3) 0.0234(7) Uani 1 1 d . . . C2 C 0.5863(3) 1.2103(3) 0.2617(3) 0.0284(7) Uani 1 1 d . . . C3 C 0.5239(3) 1.2832(2) 0.1706(3) 0.0280(7) Uani 1 1 d . . . C4 C 0.5383(3) 1.2749(2) 0.0725(3) 0.0240(7) Uani 1 1 d . . . C5 C 0.6154(3) 1.1914(2) 0.0662(2) 0.0202(6) Uani 1 1 d . . . C6 C 0.6806(3) 1.1161(2) 0.1562(2) 0.0172(6) Uani 1 1 d . . . C7 C 0.7724(3) 1.0305(2) 0.1465(2) 0.0180(6) Uani 1 1 d . . . H7A H 0.7756 1.0395 0.0708 0.022 Uiso 1 1 calc R . . H7B H 0.86 1.0429 0.1666 0.022 Uiso 1 1 calc R . . C8 C 0.6291(3) 0.8595(2) 0.2080(2) 0.0169(6) Uani 1 1 d . . . H8 H 0.5612 0.8843 0.158 0.02 Uiso 1 1 calc R . . C9 C 0.6447(3) 0.7559(2) 0.2904(2) 0.0151(6) Uani 1 1 d . . . C10 C 0.5650(3) 0.6559(2) 0.3200(2) 0.0145(6) Uani 1 1 d . . . C11 C 0.6233(3) 0.5515(2) 0.3634(2) 0.0162(6) Uani 1 1 d . . . H11 H 0.7131 0.5448 0.376 0.019 Uiso 1 1 calc R . . C12 C 0.5480(3) 0.4576(2) 0.3878(2) 0.0183(6) Uani 1 1 d . . . H12 H 0.5873 0.3883 0.417 0.022 Uiso 1 1 calc R . . C13 C 0.4297(3) 0.6650(2) 0.3022(2) 0.0156(6) Uani 1 1 d . . . H13 H 0.3899 0.7341 0.2741 0.019 Uiso 1 1 calc R . . C14 C 0.4146(3) 0.4673(2) 0.3685(2) 0.0172(6) Uani 1 1 d . . . H14 H 0.3645 0.4044 0.3836 0.021 Uiso 1 1 calc R . . C15 C 0.3547(3) 0.5709(2) 0.3265(2) 0.0155(6) Uani 1 1 d . . . C16 C 0.2131(3) 0.5826(2) 0.3048(2) 0.0156(6) Uani 1 1 d . . . C17 C 0.1488(3) 0.6605(2) 0.2181(2) 0.0157(6) Uani 1 1 d . . . H17 H 0.1854 0.7194 0.1597 0.019 Uiso 1 1 calc R . . C18 C -0.0890(3) 0.6840(2) 0.1622(2) 0.0172(6) Uani 1 1 d . . . H18A H -0.0818 0.7636 0.1336 0.021 Uiso 1 1 calc R . . H18B H -0.1705 0.6631 0.2033 0.021 Uiso 1 1 calc R . . C19 C -0.0924(3) 0.6489(2) 0.0681(2) 0.0153(6) Uani 1 1 d . . . C20 C -0.0120(3) 0.6980(2) -0.0225(2) 0.0169(6) Uani 1 1 d . . . C21 C -0.0178(3) 0.6727(2) -0.1121(2) 0.0218(7) Uani 1 1 d . . . C22 C -0.1070(3) 0.5958(2) -0.1126(2) 0.0243(7) Uani 1 1 d . . . C23 C -0.1870(3) 0.5431(2) -0.0232(3) 0.0235(7) Uani 1 1 d . . . C24 C -0.1793(3) 0.5704(2) 0.0657(2) 0.0201(6) Uani 1 1 d . . . C100 C 0.7483(3) 0.8285(3) 0.5938(3) 0.0358(8) Uani 1 1 d . . . H10A H 0.7056 0.8123 0.5384 0.054 Uiso 1 1 calc R . . H10B H 0.701 0.8858 0.6053 0.054 Uiso 1 1 calc R . . H10C H 0.7503 0.7634 0.6608 0.054 Uiso 1 1 calc R . . C101 C 0.8863(3) 0.8659(2) 0.5574(3) 0.0278(7) Uani 1 1 d . . . H10D H 0.8848 0.9324 0.4904 0.033 Uiso 1 1 calc R . . H10E H 0.9298 0.8826 0.613 0.033 Uiso 1 1 calc R . . C102 C 1.0857(3) 0.8145(3) 0.4989(3) 0.0306(7) Uani 1 1 d . . . H10F H 1.1367 0.8273 0.5534 0.037 Uiso 1 1 calc R . . H10G H 1.082 0.8827 0.4337 0.037 Uiso 1 1 calc R . . C103 C 1.1488(3) 0.7263(3) 0.4727(3) 0.0396(9) Uani 1 1 d . . . H10H H 1.1515 0.659 0.5374 0.059 Uiso 1 1 calc R . . H10I H 1.2365 0.7479 0.4463 0.059 Uiso 1 1 calc R . . H10J H 1.0991 0.7153 0.4175 0.059 Uiso 1 1 calc R . . N1 N 0.7334(2) 0.91675(18) 0.21580(18) 0.0157(5) Uani 1 1 d . . . N2 N 0.8131(2) 0.85612(18) 0.29693(19) 0.0166(5) Uani 1 1 d . . . N3 N 0.7584(2) 0.75806(18) 0.34271(18) 0.0154(5) Uani 1 1 d . . . N4 N 0.1198(2) 0.51304(18) 0.37028(18) 0.0145(5) Uani 1 1 d . . . N5 N 0.0023(2) 0.54353(18) 0.32807(18) 0.0160(5) Uani 1 1 d . . . N6 N 0.0215(2) 0.63357(18) 0.23570(18) 0.0144(5) Uani 1 1 d . . . F12 F -0.25830(17) 0.51817(15) 0.15187(14) 0.0304(4) Uani 1 1 d . . . F13 F -0.2699(2) 0.46572(15) -0.02308(17) 0.0389(5) Uani 1 1 d . . . F14 F -0.1143(2) 0.57022(16) -0.19939(16) 0.0377(5) Uani 1 1 d . . . F15 F 0.06241(19) 0.72168(16) -0.19800(14) 0.0326(4) Uani 1 1 d . . . F16 F 0.07536(16) 0.77343(13) -0.02322(13) 0.0222(4) Uani 1 1 d . . . Ag1 Ag 0.85067(2) 0.639575(16) 0.488886(16) 0.01723(7) Uani 1 1 d . . . O1 O 0.9565(2) 0.78067(16) 0.53970(17) 0.0224(5) Uani 1 1 d . . . F1 F 0.3339(3) 0.9855(2) 0.28222(19) 0.0584(7) Uani 1 1 d . . . F2 F 0.1515(2) 1.08659(17) 0.01895(15) 0.0378(5) Uani 1 1 d . . . F3 F 0.39374(19) 1.02748(17) 0.07643(18) 0.0419(5) Uani 1 1 d . . . F4 F 0.27996(19) 1.18243(15) 0.1273(2) 0.0420(5) Uani 1 1 d . . . F5 F 0.2000(2) 0.89230(15) 0.17546(19) 0.0480(6) Uani 1 1 d . . . F6 F 0.08597(19) 1.04927(16) 0.22239(16) 0.0359(5) Uani 1 1 d . . . Sb1 Sb 0.240742(19) 1.036575(15) 0.151815(15) 0.01975(7) Uani 1 1 d . . . F7 F 0.7259(2) 1.05843(15) 0.34328(15) 0.0347(5) Uani 1 1 d . . . F8 F 0.5728(2) 1.21843(18) 0.35821(17) 0.0440(5) Uani 1 1 d . . . F9 F 0.4472(2) 1.36288(16) 0.17796(19) 0.0420(5) Uani 1 1 d . . . F10 F 0.47649(19) 1.34559(15) -0.01668(16) 0.0379(5) Uani 1 1 d . . . F11 F 0.62807(18) 1.18592(15) -0.03168(14) 0.0293(4) 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 C1 0.0243(17) 0.0181(14) 0.0266(16) -0.0075(13) -0.0074(13) -0.0003(12) C2 0.0282(18) 0.0281(17) 0.0368(19) -0.0212(15) -0.0008(14) -0.0006(14) C3 0.0223(17) 0.0169(15) 0.046(2) -0.0138(14) 0.0012(14) -0.0002(12) C4 0.0161(15) 0.0158(14) 0.0310(17) 0.0000(13) -0.0028(13) 0.0010(12) C5 0.0182(15) 0.0180(14) 0.0204(15) -0.0035(12) 0.0040(12) -0.0050(12) C6 0.0134(14) 0.0124(13) 0.0232(15) -0.0046(11) 0.0001(11) -0.0049(11) C7 0.0190(15) 0.0101(13) 0.0200(14) -0.0011(11) 0.0023(11) -0.0029(11) C8 0.0140(14) 0.0173(13) 0.0183(14) -0.0062(11) -0.0029(11) -0.0011(11) C9 0.0130(14) 0.0170(13) 0.0150(13) -0.0063(11) -0.0004(11) 0.0010(11) C10 0.0171(15) 0.0150(13) 0.0109(12) -0.0046(11) 0.0008(11) -0.0018(11) C11 0.0140(14) 0.0173(13) 0.0158(13) -0.0051(11) -0.0004(11) 0.0023(11) C12 0.0193(15) 0.0131(13) 0.0214(14) -0.0060(11) 0.0003(12) 0.0001(11) C13 0.0175(15) 0.0135(13) 0.0130(13) -0.0027(11) -0.0015(11) -0.0002(11) C14 0.0184(15) 0.0155(13) 0.0190(14) -0.0084(11) 0.0020(11) -0.0028(11) C15 0.0169(15) 0.0182(13) 0.0115(13) -0.0061(11) 0.0003(11) 0.0002(11) C16 0.0186(15) 0.0132(13) 0.0155(13) -0.0064(11) -0.0008(11) -0.0023(11) C17 0.0160(15) 0.0122(12) 0.0167(13) -0.0034(11) -0.0001(11) -0.0030(11) C18 0.0121(14) 0.0190(13) 0.0167(14) -0.0033(11) -0.0006(11) 0.0049(11) C19 0.0139(14) 0.0144(13) 0.0145(13) -0.0028(11) -0.0034(11) 0.0045(11) C20 0.0139(14) 0.0147(13) 0.0210(14) -0.0060(11) -0.0031(11) 0.0025(11) C21 0.0230(16) 0.0220(15) 0.0184(14) -0.0061(12) 0.0000(12) 0.0059(12) C22 0.0301(18) 0.0234(15) 0.0239(16) -0.0143(13) -0.0113(13) 0.0101(13) C23 0.0226(17) 0.0157(14) 0.0328(17) -0.0100(13) -0.0122(13) 0.0022(12) C24 0.0142(15) 0.0169(14) 0.0226(15) -0.0013(12) -0.0019(12) 0.0002(11) C100 0.037(2) 0.0351(19) 0.041(2) -0.0214(16) 0.0073(16) 0.0032(16) C101 0.0361(19) 0.0211(15) 0.0298(17) -0.0141(14) -0.0013(14) 0.0038(13) C102 0.0241(18) 0.0323(17) 0.0392(19) -0.0182(16) 0.0008(14) -0.0076(14) C103 0.0245(19) 0.041(2) 0.058(2) -0.0241(19) 0.0070(17) -0.0028(15) N1 0.0146(12) 0.0117(11) 0.0169(12) -0.0017(9) -0.0014(9) -0.0001(9) N2 0.0177(13) 0.0123(11) 0.0167(12) -0.0027(9) -0.0019(10) -0.0020(9) N3 0.0158(12) 0.0126(11) 0.0154(11) -0.0032(9) -0.0018(9) -0.0019(9) N4 0.0154(12) 0.0135(11) 0.0133(11) -0.0041(9) -0.0012(9) -0.0013(9) N5 0.0144(12) 0.0165(11) 0.0144(11) -0.0033(9) -0.0012(9) -0.0004(9) N6 0.0152(12) 0.0139(11) 0.0120(11) -0.0032(9) -0.0016(9) 0.0014(9) F12 0.0224(10) 0.0299(9) 0.0280(10) -0.0005(8) 0.0030(8) -0.0107(8) F13 0.0414(12) 0.0243(10) 0.0514(13) -0.0151(9) -0.0178(10) -0.0085(9) F14 0.0558(14) 0.0361(11) 0.0312(10) -0.0239(9) -0.0134(9) 0.0122(9) F15 0.0339(11) 0.0422(11) 0.0197(9) -0.0108(8) 0.0082(8) 0.0009(9) F16 0.0198(9) 0.0214(8) 0.0229(9) -0.0063(7) 0.0011(7) -0.0073(7) Ag1 0.01673(13) 0.01435(11) 0.01548(11) -0.00068(9) -0.00304(8) -0.00054(8) O1 0.0228(11) 0.0200(10) 0.0277(11) -0.0131(9) 0.0003(9) -0.0022(8) F1 0.0690(17) 0.0691(16) 0.0424(13) -0.0282(12) -0.0316(12) 0.0361(13) F2 0.0419(12) 0.0442(12) 0.0294(10) -0.0170(9) -0.0139(9) 0.0198(9) F3 0.0264(11) 0.0452(12) 0.0533(13) -0.0195(11) 0.0066(9) 0.0105(9) F4 0.0277(11) 0.0259(10) 0.0762(16) -0.0246(11) -0.0004(10) -0.0032(8) F5 0.0638(15) 0.0178(9) 0.0609(15) -0.0146(10) 0.0106(12) -0.0049(9) F6 0.0286(11) 0.0444(11) 0.0403(11) -0.0233(10) 0.0132(9) -0.0048(9) Sb1 0.01939(12) 0.01687(11) 0.02153(11) -0.00630(8) -0.00317(8) 0.00408(8) F7 0.0456(12) 0.0345(10) 0.0261(10) -0.0144(8) -0.0155(9) 0.0136(9) F8 0.0554(14) 0.0471(12) 0.0442(12) -0.0337(11) -0.0052(10) 0.0104(10) F9 0.0380(12) 0.0283(10) 0.0626(14) -0.0217(10) 0.0014(10) 0.0123(9) F10 0.0292(11) 0.0294(10) 0.0384(11) 0.0033(9) -0.0033(9) 0.0110(8) F11 0.0308(10) 0.0315(10) 0.0185(9) -0.0028(8) -0.0004(7) 0.0044(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 F7 1.344(3) . ? C1 C2 1.378(4) . ? C1 C6 1.385(4) . ? C2 F8 1.344(4) . ? C2 C3 1.369(5) . ? C3 F9 1.345(4) . ? C3 C4 1.367(5) . ? C4 F10 1.341(3) . ? C4 C5 1.382(4) . ? C5 F11 1.346(3) . ? C5 C6 1.385(4) . ? C6 C7 1.511(4) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 N1 1.342(4) . ? C8 C9 1.378(4) . ? C8 H8 0.93 . ? C9 N3 1.368(4) . ? C9 C10 1.472(4) . ? C10 C11 1.396(4) . ? C10 C13 1.399(4) . ? C11 C12 1.389(4) . ? C11 H11 0.93 . ? C12 C14 1.384(4) . ? C12 H12 0.93 . ? C13 C15 1.390(4) . ? C13 H13 0.93 . ? C14 C15 1.395(4) . ? C14 H14 0.93 . ? C15 C16 1.472(4) . ? C16 N4 1.366(4) . ? C16 C17 1.370(4) . ? C17 N6 1.343(4) . ? C17 H17 0.93 . ? C18 N6 1.470(3) . ? C18 C19 1.509(4) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 C20 1.383(4) . ? C19 C24 1.385(4) . ? C20 F16 1.343(3) . ? C20 C21 1.373(4) . ? C21 F15 1.339(3) . ? C21 C22 1.376(5) . ? C22 F14 1.338(3) . ? C22 C23 1.377(5) . ? C23 F13 1.336(3) . ? C23 C24 1.379(4) . ? C24 F12 1.342(3) . ? C100 C101 1.506(5) . ? C100 H10A 0.96 . ? C100 H10B 0.96 . ? C100 H10C 0.96 . ? C101 O1 1.431(4) . ? C101 H10D 0.97 . ? C101 H10E 0.97 . ? C102 O1 1.425(4) . ? C102 C103 1.490(5) . ? C102 H10F 0.97 . ? C102 H10G 0.97 . ? C103 H10H 0.96 . ? C103 H10I 0.96 . ? C103 H10J 0.96 . ? N1 N2 1.336(3) . ? N1 C7 1.471(3) . ? N2 N3 1.319(3) . ? N3 Ag1 2.168(2) . ? N4 N5 1.319(3) . ? N4 Ag1 2.156(2) 2_666 ? N5 N6 1.339(3) . ? Ag1 N4 2.156(2) 2_666 ? Ag1 O1 2.494(2) . ? F1 Sb1 1.863(2) . ? F2 Sb1 1.8697(18) . ? F3 Sb1 1.878(2) . ? F4 Sb1 1.8735(19) . ? F5 Sb1 1.8598(19) . ? F6 Sb1 1.8715(18) . ? 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 C8 C9 105.0(2) . . ? N1 C8 H8 127.5 . . ? C9 C8 H8 127.5 . . ? N3 C9 C8 106.6(2) . . ? N3 C9 C10 122.8(2) . . ? C8 C9 C10 130.5(3) . . ? C11 C10 C13 119.3(3) . . ? C11 C10 C9 120.8(2) . . ? C13 C10 C9 119.9(2) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C14 C12 C11 120.0(3) . . ? C14 C12 H12 120 . . ? C11 C12 H12 120 . . ? C15 C13 C10 120.1(2) . . ? C15 C13 H13 120 . . ? C10 C13 H13 120 . . ? C12 C14 C15 120.2(3) . . ? C12 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C13 C15 C14 120.0(3) . . ? C13 C15 C16 119.2(2) . . ? C14 C15 C16 120.8(3) . . ? N4 C16 C17 106.8(2) . . ? N4 C16 C15 124.6(2) . . ? C17 C16 C15 128.5(3) . . ? N6 C17 C16 105.2(2) . . ? N6 C17 H17 127.4 . . ? C16 C17 H17 127.4 . . ? N6 C18 C19 112.0(2) . . ? N6 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N6 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C24 116.8(3) . . ? C20 C19 C18 120.9(3) . . ? C24 C19 C18 122.2(3) . . ? F16 C20 C21 118.5(3) . . ? F16 C20 C19 119.0(3) . . ? C21 C20 C19 122.5(3) . . ? F15 C21 C20 120.6(3) . . ? F15 C21 C22 120.3(3) . . ? C20 C21 C22 119.1(3) . . ? F14 C22 C21 119.9(3) . . ? F14 C22 C23 119.7(3) . . ? C21 C22 C23 120.3(3) . . ? F13 C23 C22 119.7(3) . . ? F13 C23 C24 120.9(3) . . ? C22 C23 C24 119.3(3) . . ? F12 C24 C23 118.3(3) . . ? F12 C24 C19 119.8(3) . . ? C23 C24 C19 121.9(3) . . ? C101 C100 H10A 109.5 . . ? C101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? O1 C101 C100 109.4(3) . . ? O1 C101 H10D 109.8 . . ? C100 C101 H10D 109.8 . . ? O1 C101 H10E 109.8 . . ? C100 C101 H10E 109.8 . . ? H10D C101 H10E 108.2 . . ? O1 C102 C103 108.9(3) . . ? O1 C102 H10F 109.9 . . ? C103 C102 H10F 109.9 . . ? O1 C102 H10G 109.9 . . ? C103 C102 H10G 109.9 . . ? H10F C102 H10G 108.3 . . ? C102 C103 H10H 109.5 . . ? C102 C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? C102 C103 H10J 109.5 . . ? H10H C103 H10J 109.5 . . ? H10I C103 H10J 109.5 . . ? N2 N1 C8 112.2(2) . . ? N2 N1 C7 118.1(2) . . ? C8 N1 C7 129.6(2) . . ? N3 N2 N1 105.7(2) . . ? N2 N3 C9 110.4(2) . . ? N2 N3 Ag1 116.75(17) . . ? C9 N3 Ag1 132.60(18) . . ? N5 N4 C16 110.4(2) . . ? N5 N4 Ag1 121.25(17) . 2_666 ? C16 N4 Ag1 127.80(18) . 2_666 ? N4 N5 N6 105.5(2) . . ? N5 N6 C17 112.1(2) . . ? N5 N6 C18 120.0(2) . . ? C17 N6 C18 127.6(2) . . ? N4 Ag1 N3 158.48(9) 2_666 . ? N4 Ag1 O1 104.03(8) 2_666 . ? N3 Ag1 O1 95.14(8) . . ? C102 O1 C101 111.7(2) . . ? C102 O1 Ag1 117.34(18) . . ? C101 O1 Ag1 123.99(18) . . ? F5 Sb1 F1 90.09(11) . . ? F5 Sb1 F2 89.52(10) . . ? F1 Sb1 F2 178.26(10) . . ? F5 Sb1 F6 91.04(9) . . ? F1 Sb1 F6 91.94(10) . . ? F2 Sb1 F6 89.76(9) . . ? F5 Sb1 F4 179.37(10) . . ? F1 Sb1 F4 90.44(11) . . ? F2 Sb1 F4 89.97(9) . . ? F6 Sb1 F4 88.59(9) . . ? F5 Sb1 F3 89.75(10) . . ? F1 Sb1 F3 89.88(11) . . ? F2 Sb1 F3 88.42(9) . . ? F6 Sb1 F3 178.01(9) . . ? F4 Sb1 F3 90.61(9) . . ? F7 C1 C2 118.6(3) . . ? F7 C1 C6 119.0(3) . . ? C2 C1 C6 122.4(3) . . ? F8 C2 C3 120.6(3) . . ? F8 C2 C1 120.1(3) . . ? C3 C2 C1 119.3(3) . . ? F9 C3 C4 119.8(3) . . ? F9 C3 C2 119.8(3) . . ? C4 C3 C2 120.4(3) . . ? F10 C4 C3 120.6(3) . . ? F10 C4 C5 120.0(3) . . ? C3 C4 C5 119.4(3) . . ? F11 C5 C4 117.9(3) . . ? F11 C5 C6 119.9(3) . . ? C4 C5 C6 122.2(3) . . ? C1 C6 C5 116.3(3) . . ? C1 C6 C7 121.9(3) . . ? C5 C6 C7 121.6(3) . . ? N1 C7 C6 113.2(2) . . ? N1 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? # Attachment 'mlg137new22122009.cif' data_pcf _database_code_depnum_ccdc_archive 'CCDC 751439' #------------------ AUDIT DETAILS -------------------------------------------# _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_creation_date 2009-12-22T15:04:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ? _publ_section_references ; Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. ; # Insert blank lines between references #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_moiety "C27 'H16 Ag F10 N6 O, 2(C3 H6 O), F6 Sb" _chemical_formula_sum 'C33 H28 Ag F16 N6 O3 Sb' _chemical_formula_weight 1090.23 _chemical_name_systematic ? #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_angle_alpha 90.000(0) _cell_angle_beta 113.594(9) _cell_angle_gamma 90.000(0) _cell_formula_units_Z 4 _cell_length_a 19.902(4) _cell_length_b 9.080(2) _cell_length_c 23.168(5) _cell_measurement_reflns_used 6816 _cell_measurement_temperature 89(2) _cell_measurement_theta_max 24.33 _cell_measurement_theta_min 2.29 _cell_volume 3836.7(14) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.336 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_correction_T_min 0.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_crystal_F_000 2136 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.07 _exptl_special_details ? #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 89(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_av_unetI/netI 0.0295 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 72868 _diffrn_reflns_theta_full 24.59 _diffrn_reflns_theta_max 24.59 _diffrn_reflns_theta_min 2.44 _reflns_number_gt 5735 _reflns_number_total 6446 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_diff_density_max 3.089 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.185 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0801 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 503 _refine_ls_number_reflns 6446 _refine_ls_number_restraints 127 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.206 _refine_ls_wR_factor_ref 0.2119 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+54.5334P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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^ > 2\s(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. ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.2050(8) 0.2181(16) 0.4015(5) 0.065(4) Uani 1 1 d . . . C2 C 0.2150(8) 0.297(2) 0.4522(6) 0.077(4) Uani 1 1 d . . . C3 C 0.2597(8) 0.4124(16) 0.4641(5) 0.060(3) Uani 1 1 d . . . C4 C 0.2985(9) 0.4545(15) 0.4281(7) 0.090(6) Uani 1 1 d . . . C5 C 0.2872(7) 0.3637(13) 0.3740(5) 0.059(3) Uani 1 1 d . . . C6 C 0.2416(5) 0.2483(12) 0.3605(4) 0.042(2) Uani 1 1 d . . . C7 C 0.2263(5) 0.1553(11) 0.3033(4) 0.038(2) Uani 1 1 d . . . H7A H 0.2719 0.1345 0.2989 0.046 Uiso 1 1 calc R . . H7B H 0.2049 0.0624 0.3079 0.046 Uiso 1 1 calc R . . C8 C 0.1913(5) 0.2993(10) 0.2021(4) 0.0315(19) Uani 1 1 d . . . H8 H 0.2362 0.302 0.1986 0.038 Uiso 1 1 calc R . . C9 C 0.1268(4) 0.3630(9) 0.1631(4) 0.0254(17) Uani 1 1 d . . . C10 C 0.1116(4) 0.4568(9) 0.1068(4) 0.0261(17) Uani 1 1 d . . . C11 C 0.0641(4) 0.5767(10) 0.0954(4) 0.0299(18) Uani 1 1 d . . . H11 H 0.0417 0.598 0.1227 0.036 Uiso 1 1 calc R . . C12 C 0.0508(5) 0.6638(10) 0.0426(4) 0.0304(19) Uani 1 1 d . . . H12 H 0.0176 0.7413 0.0337 0.037 Uiso 1 1 calc R . . C13 C 0.0862(5) 0.6369(10) 0.0035(4) 0.033(2) Uani 1 1 d . . . H13 H 0.078 0.6983 -0.0308 0.04 Uiso 1 1 calc R . . C14 C 0.1340(4) 0.5189(11) 0.0148(4) 0.0321(19) Uani 1 1 d . . . C15 C 0.1458(5) 0.4290(10) 0.0670(4) 0.0306(19) Uani 1 1 d . . . H15 H 0.1773 0.3489 0.0748 0.037 Uiso 1 1 calc R . . C16 C 0.1724(5) 0.4886(12) -0.0259(4) 0.039(2) Uani 1 1 d . . . C17 C 0.2407(6) 0.4318(18) -0.0113(5) 0.069(4) Uani 1 1 d . . . H17 H 0.2732 0.3967 0.0276 0.083 Uiso 1 1 calc R . . C18 C 0.3181(8) 0.418(3) -0.0778(7) 0.121(5) Uani 1 1 d U . . H18A H 0.3053 0.3688 -0.118 0.145 Uiso 1 1 calc R . . H18B H 0.338 0.5138 -0.0806 0.145 Uiso 1 1 calc R . . C19 C 0.3727(8) 0.334(3) -0.0301(6) 0.089(4) Uani 1 1 d U . . C20 C 0.0657(9) -0.115(3) 0.4816(8) 0.098(4) Uani 1 1 d U . . C21 C 0.0108(8) -0.189(3) 0.4410(7) 0.093(4) Uani 1 1 d U . . C22 C 0.0175(11) -0.335(3) 0.4452(9) 0.105(4) Uani 1 1 d U . . C23 C 0.0798(13) -0.407(3) 0.4934(10) 0.107(5) Uani 1 1 d U . . C24 C 0.3724(9) 0.172(3) -0.0310(8) 0.098(4) Uani 1 1 d U . . C100 C 0.7438(13) 0.180(3) 0.2336(9) 0.153(12) Uani 1 1 d . . . C101 C 0.6734(14) 0.225(4) 0.2442(13) 0.197(15) Uani 1 1 d . . . H10A H 0.6874 0.2593 0.2866 0.296 Uiso 1 1 calc R . . H10B H 0.6418 0.1412 0.2371 0.296 Uiso 1 1 calc R . . H10C H 0.6481 0.3022 0.2153 0.296 Uiso 1 1 calc R . . C102 C 0.7392(14) 0.195(4) 0.1708(10) 0.175(13) Uani 1 1 d . . . H10D H 0.7459 0.296 0.1625 0.263 Uiso 1 1 calc R . . H10E H 0.692 0.1617 0.1417 0.263 Uiso 1 1 calc R . . H10F H 0.7767 0.1358 0.1659 0.263 Uiso 1 1 calc R . . C200 C 0.0645(10) 1.005(2) -0.1239(8) 0.091(5) Uiso 1 1 d . . . C201 C 0.100(2) 1.119(4) -0.1438(18) 0.225(16) Uiso 1 1 d . . . H20A H 0.1501 1.0919 -0.1338 0.337 Uiso 1 1 calc R . . H20B H 0.0989 1.2091 -0.1224 0.337 Uiso 1 1 calc R . . H20C H 0.0751 1.1333 -0.1884 0.337 Uiso 1 1 calc R . . C202 C -0.0102(14) 1.022(3) -0.1345(13) 0.164(10) Uiso 1 1 d . . . H20D H -0.0273 0.9347 -0.1213 0.246 Uiso 1 1 calc R . . H20E H -0.0387 1.0381 -0.1786 0.246 Uiso 1 1 calc R . . H20F H -0.0154 1.105 -0.111 0.246 Uiso 1 1 calc R . . C300 C 0.035(3) 0.797(5) -0.3450(13) 0.34(3) Uiso 1 1 d D . . H30A H 0.0109 0.8903 -0.3476 0.504 Uiso 1 1 calc R . . H30B H 0.0013 0.7302 -0.375 0.504 Uiso 1 1 calc R . . H30C H 0.0773 0.81 -0.354 0.504 Uiso 1 1 calc R . . C301 C 0.0563(9) 0.7367(19) -0.2814(8) 0.084(4) Uiso 1 1 d D . . C302 C 0.0919(17) 0.595(3) -0.2638(15) 0.201(14) Uiso 1 1 d D . . H30D H 0.1004 0.5743 -0.2208 0.301 Uiso 1 1 calc R . . H30E H 0.1379 0.5975 -0.2682 0.301 Uiso 1 1 calc R . . H30F H 0.0611 0.5205 -0.2907 0.301 Uiso 1 1 calc R . . N1 N 0.2512(5) 0.4376(18) -0.0657(4) 0.084(4) Uani 1 1 d . . . N2 N 0.1917(5) 0.4907(14) -0.1131(4) 0.065(3) Uani 1 1 d . . . N3 N 0.1453(4) 0.5228(11) -0.0890(4) 0.042(2) Uani 1 1 d . . . N4 N 0.0753(4) 0.3300(8) 0.1865(3) 0.0291(16) Uani 1 1 d . . . N5 N 0.1053(4) 0.2500(8) 0.2376(3) 0.0324(16) Uani 1 1 d . . . N6 N 0.1753(4) 0.2327(9) 0.2463(3) 0.0318(16) Uani 1 1 d . . . F1 F 0.0328(3) 0.6351(7) 0.2336(3) 0.0475(14) Uani 1 1 d . . . F2 F 0.1324(4) 0.8484(7) 0.2755(4) 0.0603(17) Uani 1 1 d . . . F3 F 0.0426(4) 0.7918(8) 0.3319(3) 0.0603(17) Uani 1 1 d . . . F4 F 0.1856(4) 0.7290(9) 0.3877(3) 0.073(2) Uani 1 1 d . . . F5 F 0.0892(4) 0.5143(7) 0.3481(3) 0.0595(17) Uani 1 1 d . . . F6 F 0.1745(3) 0.5740(6) 0.2877(3) 0.0419(13) Uani 1 1 d . . . F7 F 0.1597(4) 0.1017(11) 0.3894(4) 0.082(2) Uani 1 1 d U . . F8 F 0.1830(6) 0.2715(17) 0.4907(4) 0.133(5) Uani 1 1 d U . . F9 F 0.2698(7) 0.5089(14) 0.5126(4) 0.139(5) Uani 1 1 d U . . F10 F 0.3449(6) 0.5667(10) 0.4379(5) 0.125(4) Uani 1 1 d U . . F11 F 0.3219(4) 0.3944(8) 0.3358(4) 0.069(2) Uani 1 1 d U . . F12 F 0.0583(7) 0.0376(17) 0.4753(6) 0.133(4) Uani 1 1 d U . . F13 F -0.0503(6) -0.1219(17) 0.3953(5) 0.131(5) Uani 1 1 d . . . F14 F -0.0352(7) -0.416(2) 0.4064(6) 0.167(7) Uani 1 1 d . . . F15 F 0.0772(12) -0.551(2) 0.4918(10) 0.207(9) Uani 1 1 d . . . F16 F 0.3151(7) 0.118(2) -0.0783(7) 0.186(8) Uani 1 1 d . . . Ag1 Ag 0.04114(4) 0.62148(9) -0.15114(3) 0.0394(2) Uani 1 1 d . . . Sb1 Sb 0.10834(3) 0.68080(7) 0.31054(3) 0.0327(2) Uani 1 1 d . . . O1 O 0.7904(7) 0.117(2) 0.2768(6) 0.144(6) Uani 1 1 d . . . O2 O 0.0963(7) 0.8874(14) -0.1014(6) 0.097(3) Uiso 1 1 d . . . O3 O 0.0584(15) 0.795(3) -0.2270(13) 0.229(11) 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 C1 0.083(9) 0.072(9) 0.027(5) 0.006(5) 0.006(6) 0.039(8) C2 0.068(9) 0.117(13) 0.045(7) -0.004(8) 0.020(7) 0.014(9) C3 0.062(8) 0.076(9) 0.029(5) -0.003(6) 0.005(5) 0.029(7) C4 0.081(10) 0.050(8) 0.074(9) 0.004(7) -0.036(8) 0.013(7) C5 0.064(8) 0.040(6) 0.042(6) 0.007(5) -0.012(6) 0.018(6) C6 0.043(5) 0.046(6) 0.026(4) 0.004(4) 0.002(4) 0.017(5) C7 0.028(5) 0.042(5) 0.036(5) 0.007(4) 0.004(4) 0.015(4) C8 0.024(4) 0.040(5) 0.028(4) 0.000(4) 0.007(4) 0.002(4) C9 0.023(4) 0.030(4) 0.020(4) 0.000(3) 0.006(3) -0.005(3) C10 0.020(4) 0.030(4) 0.020(4) 0.005(3) 0.001(3) -0.006(3) C11 0.023(4) 0.034(5) 0.028(4) -0.006(4) 0.006(3) -0.004(4) C12 0.029(4) 0.031(5) 0.028(4) 0.000(4) 0.008(4) -0.004(4) C13 0.029(5) 0.042(5) 0.019(4) 0.003(4) 0.001(3) -0.011(4) C14 0.017(4) 0.048(5) 0.024(4) 0.000(4) 0.001(3) -0.004(4) C15 0.030(4) 0.036(5) 0.021(4) 0.002(4) 0.005(3) -0.001(4) C16 0.026(5) 0.061(6) 0.025(4) 0.009(4) 0.005(4) 0.006(4) C17 0.045(6) 0.138(13) 0.023(5) 0.018(6) 0.011(5) 0.031(7) C18 0.059(8) 0.247(14) 0.063(8) 0.039(10) 0.032(6) 0.054(10) C19 0.046(6) 0.183(11) 0.048(6) 0.024(8) 0.030(5) 0.020(8) C20 0.061(7) 0.162(8) 0.083(9) -0.030(8) 0.042(6) -0.028(8) C21 0.050(6) 0.174(8) 0.061(7) -0.026(8) 0.028(5) -0.012(7) C22 0.080(8) 0.169(8) 0.084(8) -0.041(9) 0.052(6) -0.035(9) C23 0.113(11) 0.141(11) 0.096(10) -0.022(9) 0.072(8) -0.013(10) C24 0.057(8) 0.183(11) 0.066(8) 0.001(10) 0.037(7) -0.007(9) C100 0.108(16) 0.19(3) 0.079(13) 0.056(15) -0.044(12) -0.046(16) C101 0.12(2) 0.26(4) 0.14(2) -0.01(2) -0.026(17) 0.07(2) C102 0.14(2) 0.26(4) 0.088(15) 0.051(19) -0.002(14) -0.06(2) N1 0.038(5) 0.177(14) 0.038(5) 0.021(7) 0.017(4) 0.044(7) N2 0.037(5) 0.133(10) 0.023(4) 0.028(5) 0.009(4) 0.030(6) N3 0.024(4) 0.070(6) 0.030(4) 0.004(4) 0.008(3) 0.006(4) N4 0.024(4) 0.033(4) 0.022(3) -0.001(3) 0.001(3) -0.001(3) N5 0.028(4) 0.037(4) 0.027(4) 0.004(3) 0.005(3) 0.006(3) N6 0.024(4) 0.040(4) 0.028(4) 0.008(3) 0.007(3) 0.007(3) F1 0.032(3) 0.061(4) 0.036(3) -0.007(3) 0.000(2) 0.006(3) F2 0.060(4) 0.042(3) 0.087(5) 0.012(3) 0.039(4) 0.000(3) F3 0.061(4) 0.066(4) 0.062(4) -0.006(3) 0.033(3) 0.011(3) F4 0.053(4) 0.075(5) 0.057(4) -0.027(4) -0.012(3) 0.001(4) F5 0.067(4) 0.059(4) 0.057(4) 0.021(3) 0.030(3) 0.005(3) F6 0.030(3) 0.041(3) 0.052(3) -0.003(3) 0.014(2) 0.006(2) F7 0.062(5) 0.117(7) 0.068(5) 0.011(5) 0.028(4) -0.009(5) F8 0.131(9) 0.219(13) 0.064(5) 0.016(7) 0.055(6) 0.069(9) F9 0.170(10) 0.152(10) 0.053(5) -0.032(6) 0.001(6) 0.079(9) F10 0.127(8) 0.057(5) 0.102(7) -0.018(5) -0.048(6) -0.004(5) F11 0.057(4) 0.053(4) 0.071(5) 0.015(3) -0.003(4) -0.012(3) F12 0.136(9) 0.162(8) 0.132(9) -0.021(8) 0.088(8) -0.030(8) F13 0.078(6) 0.242(15) 0.086(7) -0.006(8) 0.046(6) 0.020(8) F14 0.108(9) 0.289(19) 0.136(10) -0.097(12) 0.083(8) -0.074(11) F15 0.29(2) 0.150(14) 0.30(2) -0.002(14) 0.24(2) 0.003(14) F16 0.120(10) 0.33(2) 0.147(11) -0.096(13) 0.095(10) -0.090(12) Ag1 0.0235(4) 0.0532(5) 0.0318(4) 0.0060(3) 0.0008(3) -0.0007(3) Sb1 0.0259(3) 0.0366(4) 0.0310(3) -0.0037(2) 0.0066(3) -0.0014(2) O1 0.085(9) 0.26(2) 0.085(8) 0.057(11) 0.027(7) 0.016(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u. s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u. s are taken into account individually in the estimation of s.u. s in distances, angles and torsion angles correlations between s.u. s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u. s is used for estimating s.u. s 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 C1 C2 1.321(18) . ? C1 F7 1.344(17) . ? C1 C6 1.436(17) . ? C2 F8 1.306(17) . ? C2 C3 1.33(2) . ? C3 F9 1.376(14) . ? C3 C4 1.40(2) . ? C4 F10 1.331(19) . ? C4 C5 1.44(2) . ? C5 C6 1.339(17) . ? C5 F11 1.353(16) . ? C6 C7 1.497(14) . ? C7 N6 1.482(11) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 N6 1.333(11) . ? C8 C9 1.368(12) . ? C8 H8 0.93 . ? C9 N4 1.371(11) . ? C9 C10 1.484(11) . ? C10 C15 1.371(12) . ? C10 C11 1.396(12) . ? C11 C12 1.389(12) . ? C11 H11 0.93 . ? C12 C13 1.373(13) . ? C12 H12 0.93 . ? C13 C14 1.388(13) . ? C13 H13 0.93 . ? C14 C15 1.399(12) . ? C14 C16 1.457(13) . ? C15 H15 0.93 . ? C16 C17 1.364(14) . ? C16 N3 1.375(12) . ? C17 N1 1.358(14) . ? C17 H17 0.93 . ? C18 C19 1.42(2) . ? C18 N1 1.479(16) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 C20 1.37(2) 2 ? C19 C24 1.47(3) . ? C20 C21 1.31(2) . ? C20 C19 1.37(3) 2_545 ? C20 F12 1.39(2) . ? C21 C22 1.34(3) . ? C21 F13 1.39(2) . ? C22 F14 1.30(2) . ? C22 C23 1.45(3) . ? C23 C24 1.23(3) 2_545 ? C23 F15 1.31(3) . ? C24 C23 1.23(3) 2 ? C24 F16 1.32(2) . ? C100 O1 1.20(2) . ? C100 C102 1.43(3) . ? C100 C101 1.57(4) . ? C101 H10A 0.96 . ? C101 H10B 0.96 . ? C101 H10C 0.96 . ? C102 H10D 0.96 . ? C102 H10E 0.96 . ? C102 H10F 0.96 . ? C200 O2 1.24(2) . ? C200 C202 1.42(3) . ? C200 C201 1.43(4) . ? C201 H20A 0.96 . ? C201 H20B 0.96 . ? C201 H20C 0.96 . ? C202 H20D 0.96 . ? C202 H20E 0.96 . ? C202 H20F 0.96 . ? C300 C301 1.465(10) . ? C300 H30A 0.96 . ? C300 H30B 0.96 . ? C300 H30C 0.96 . ? C301 O3 1.35(3) . ? C301 C302 1.442(10) . ? C302 H30D 0.96 . ? C302 H30E 0.96 . ? C302 H30F 0.96 . ? N1 N2 1.341(12) . ? N2 N3 1.291(12) . ? N3 Ag1 2.187(8) . ? N4 N5 1.311(10) . ? N4 Ag1 2.171(7) 3_565 ? N5 N6 1.335(10) . ? F1 Sb1 1.860(5) . ? F2 Sb1 1.874(6) . ? F3 Sb1 1.868(6) . ? F4 Sb1 1.884(6) . ? F5 Sb1 1.859(6) . ? F6 Sb1 1.874(5) . ? Ag1 N4 2.171(7) 3_565 ? Ag1 O3 2.48(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 F7 117.5(14) . . ? C2 C1 C6 123.2(15) . . ? F7 C1 C6 119.2(10) . . ? F8 C2 C1 124.7(18) . . ? F8 C2 C3 117.8(14) . . ? C1 C2 C3 117.5(14) . . ? C2 C3 F9 122.5(14) . . ? C2 C3 C4 125.2(12) . . ? F9 C3 C4 112.3(15) . . ? F10 C4 C3 128.2(16) . . ? F10 C4 C5 116.2(18) . . ? C3 C4 C5 115.5(14) . . ? C6 C5 F11 118.9(10) . . ? C6 C5 C4 120.5(15) . . ? F11 C5 C4 120.6(13) . . ? C5 C6 C1 118.1(11) . . ? C5 C6 C7 121.8(11) . . ? C1 C6 C7 120.1(11) . . ? N6 C7 C6 110.3(8) . . ? N6 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? N6 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N6 C8 C9 104.4(7) . . ? N6 C8 H8 127.8 . . ? C9 C8 H8 127.8 . . ? C8 C9 N4 107.5(7) . . ? C8 C9 C10 129.0(8) . . ? N4 C9 C10 123.5(7) . . ? C15 C10 C11 119.8(8) . . ? C15 C10 C9 120.3(8) . . ? C11 C10 C9 119.9(8) . . ? C12 C11 C10 119.2(8) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C13 C12 C11 120.8(9) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 120.5(8) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 118.6(8) . . ? C13 C14 C16 121.5(8) . . ? C15 C14 C16 120.0(8) . . ? C10 C15 C14 121.2(8) . . ? C10 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C17 C16 N3 106.1(8) . . ? C17 C16 C14 129.7(8) . . ? N3 C16 C14 124.1(8) . . ? N1 C17 C16 105.2(9) . . ? N1 C17 H17 127.4 . . ? C16 C17 H17 127.4 . . ? C19 C18 N1 112.6(13) . . ? C19 C18 H18A 109.1 . . ? N1 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? N1 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 C19 C18 128(2) 2 . ? C20 C19 C24 110.4(16) 2 . ? C18 C19 C24 121.7(19) . . ? C21 C20 C19 129(2) . 2_545 ? C21 C20 F12 114(2) . . ? C19 C20 F12 116.4(17) 2_545 . ? C22 C21 C20 115(2) . . ? C22 C21 F13 121.5(18) . . ? C20 C21 F13 123(2) . . ? F14 C22 C21 119(2) . . ? F14 C22 C23 119(2) . . ? C21 C22 C23 122(2) . . ? C24 C23 F15 128(3) 2_545 . ? C24 C23 C22 118(2) 2_545 . ? F15 C23 C22 115(2) . . ? C23 C24 F16 123(3) 2 . ? C23 C24 C19 125(2) 2 . ? F16 C24 C19 112(2) . . ? O1 C100 C102 127(3) . . ? O1 C100 C101 116(2) . . ? C102 C100 C101 116(2) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C100 C102 H10D 109.5 . . ? C100 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C100 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? O2 C200 C202 119(2) . . ? O2 C200 C201 121(2) . . ? C202 C200 C201 119(2) . . ? C200 C201 H20A 109.5 . . ? C200 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C200 C202 H20D 109.5 . . ? C200 C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? C200 C202 H20F 109.5 . . ? H20D C202 H20F 109.5 . . ? H20E C202 H20F 109.5 . . ? C301 C300 H30A 109.5 . . ? C301 C300 H30B 109.5 . . ? H30A C300 H30B 109.5 . . ? C301 C300 H30C 109.5 . . ? H30A C300 H30C 109.5 . . ? H30B C300 H30C 109.5 . . ? O3 C301 C302 105(2) . . ? O3 C301 C300 133(3) . . ? C302 C301 C300 122(2) . . ? C301 C302 H30D 109.5 . . ? C301 C302 H30E 109.5 . . ? H30D C302 H30E 109.5 . . ? C301 C302 H30F 109.5 . . ? H30D C302 H30F 109.5 . . ? H30E C302 H30F 109.5 . . ? N2 N1 C17 111.2(9) . . ? N2 N1 C18 117.0(10) . . ? C17 N1 C18 131.0(10) . . ? N3 N2 N1 106.0(7) . . ? N2 N3 C16 111.4(8) . . ? N2 N3 Ag1 117.4(6) . . ? C16 N3 Ag1 131.1(6) . . ? N5 N4 C9 109.6(7) . . ? N5 N4 Ag1 119.0(5) . 3_565 ? C9 N4 Ag1 131.3(5) . 3_565 ? N4 N5 N6 105.8(7) . . ? C8 N6 N5 112.8(7) . . ? C8 N6 C7 127.6(8) . . ? N5 N6 C7 119.5(7) . . ? N4 Ag1 N3 156.7(3) 3_565 . ? N4 Ag1 O3 91.9(6) 3_565 . ? N3 Ag1 O3 111.3(7) . . ? F5 Sb1 F1 91.7(3) . . ? F5 Sb1 F3 91.0(3) . . ? F1 Sb1 F3 89.5(3) . . ? F5 Sb1 F2 177.2(3) . . ? F1 Sb1 F2 90.9(3) . . ? F3 Sb1 F2 90.2(3) . . ? F5 Sb1 F6 90.6(3) . . ? F1 Sb1 F6 90.2(2) . . ? F3 Sb1 F6 178.3(3) . . ? F2 Sb1 F6 88.1(3) . . ? F5 Sb1 F4 89.2(3) . . ? F1 Sb1 F4 179.0(3) . . ? F3 Sb1 F4 90.9(3) . . ? F2 Sb1 F4 88.2(4) . . ? F6 Sb1 F4 89.4(3) . . ? C301 O3 Ag1 116.8(18) . . ? # END of CIF # Attachment 'mg147a.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-09-02 at 09:45:07 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\program files\wingx\files\archive.reqdat # CIF files read : pcf mg147a #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_mg147a _database_code_depnum_ccdc_archive 'CCDC 751440' #TrackingRef 'mg147a.cif' _audit_creation_date 2009-09-02T09:45:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H26 Ag2 N6, 2(F6 Sb)' _chemical_formula_sum 'C30 H26 Ag2 F12 N6 Sb2' _chemical_formula_weight 1157.83 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 9.434(2) _cell_length_b 9.945(2) _cell_length_c 10.654(2) _cell_angle_alpha 68.999(8) _cell_angle_beta 66.979(8) _cell_angle_gamma 88.489(9) _cell_volume 851.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 6595 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 33.4 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.802 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5426 _exptl_absorpt_correction_T_max 1.000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0243 _diffrn_reflns_number 15120 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 3117 _reflns_number_gt 3025 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0169P)^2^+0.7054P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3117 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0183 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.049 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.444 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.13 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C -0.2142(3) 0.5865(3) 0.9279(3) 0.0160(6) Uani 1 1 d . . . H1 H -0.1178 0.5642 0.8762 0.019 Uiso 1 1 calc R . . C2 C -0.2638(3) 0.5569(3) 1.0774(3) 0.0193(6) Uani 1 1 d . . . H2 H -0.2018 0.5121 1.1258 0.023 Uiso 1 1 calc R . . C3 C -0.4053(3) 0.5936(3) 1.1549(3) 0.0195(6) Uani 1 1 d . . . H3 H -0.438 0.5739 1.2549 0.023 Uiso 1 1 calc R . . C4 C -0.4978(3) 0.6604(3) 1.0818(3) 0.0175(6) Uani 1 1 d . . . H4 H -0.5914 0.6876 1.1327 0.021 Uiso 1 1 calc R . . C5 C -0.4512(3) 0.6863(3) 0.9337(3) 0.0146(6) Uani 1 1 d . . . H5 H -0.5151 0.7284 0.8864 0.018 Uiso 1 1 calc R . . C6 C -0.3083(3) 0.6495(3) 0.8548(3) 0.0120(5) Uani 1 1 d . . . C7 C -0.2608(3) 0.6763(3) 0.6988(3) 0.0107(5) Uani 1 1 d . . . C8 C -0.2934(3) 0.7834(3) 0.5926(3) 0.0128(5) Uani 1 1 d . . . H8 H -0.3551 0.8561 0.605 0.015 Uiso 1 1 calc R . . C9 C -0.2078(3) 0.8435(3) 0.3176(3) 0.0164(6) Uani 1 1 d . . . H9A H -0.251 0.9337 0.3143 0.02 Uiso 1 1 calc R . . H9B H -0.2682 0.7875 0.2931 0.02 Uiso 1 1 calc R . . C10 C -0.0405(3) 0.8763(3) 0.2067(3) 0.0127(5) Uani 1 1 d . . . C11 C 0.0636(3) 0.9758(3) 0.2025(3) 0.0157(6) Uani 1 1 d . . . H11 H 0.031 1.022 0.2691 0.019 Uiso 1 1 calc R . . C12 C 0.2170(3) 1.0062(3) 0.0984(3) 0.0183(6) Uani 1 1 d . . . H12 H 0.2862 1.0737 0.0952 0.022 Uiso 1 1 calc R . . C13 C 0.2670(3) 0.9368(3) -0.0001(3) 0.0187(6) Uani 1 1 d . . . H13 H 0.3695 0.958 -0.0693 0.022 Uiso 1 1 calc R . . C14 C 0.1647(3) 0.8357(3) 0.0042(3) 0.0170(6) Uani 1 1 d . . . H14 H 0.1988 0.7884 -0.0613 0.02 Uiso 1 1 calc R . . C15 C 0.0107(3) 0.8054(3) 0.1072(3) 0.0133(5) Uani 1 1 d . . . H15 H -0.0583 0.7382 0.1099 0.016 Uiso 1 1 calc R . . N1 N -0.2174(2) 0.7608(2) 0.4674(2) 0.0121(5) Uani 1 1 d . . . N2 N -0.1417(3) 0.6455(2) 0.4909(2) 0.0128(5) Uani 1 1 d . . . N3 N -0.1681(2) 0.5930(2) 0.6317(2) 0.0113(5) Uani 1 1 d . . . F1 F 0.45622(19) 0.66246(18) 0.49333(19) 0.0239(4) Uani 1 1 d . . . F2 F 0.15425(19) 0.60813(18) 0.66412(18) 0.0227(4) Uani 1 1 d . . . F3 F 0.2508(2) 0.71419(18) 0.37362(18) 0.0218(4) Uani 1 1 d . . . F4 F 0.3274(2) 0.8292(2) 0.6433(2) 0.0324(5) Uani 1 1 d . . . F5 F 0.4270(2) 0.93386(17) 0.3513(2) 0.0267(4) Uani 1 1 d . . . F6 F 0.1239(2) 0.8808(2) 0.5242(2) 0.0298(4) Uani 1 1 d . . . Ag1 Ag -0.05721(2) 0.39672(2) 0.70366(2) 0.01245(7) Uani 1 1 d . . . Sb1 Sb 0.29002(2) 0.771615(18) 0.508064(19) 0.01309(7) 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 C1 0.0180(14) 0.0132(13) 0.0172(15) -0.0063(11) -0.0071(12) -0.0002(11) C2 0.0254(16) 0.0163(13) 0.0187(15) -0.0043(12) -0.0135(13) 0.0001(12) C3 0.0274(16) 0.0174(14) 0.0102(14) -0.0048(11) -0.0039(12) -0.0061(12) C4 0.0158(14) 0.0168(13) 0.0155(15) -0.0083(12) 0.0001(12) -0.0030(12) C5 0.0151(14) 0.0120(12) 0.0148(14) -0.0045(11) -0.0047(11) -0.0005(11) C6 0.0141(13) 0.0072(11) 0.0123(13) -0.0029(10) -0.0036(11) -0.0018(10) C7 0.0067(12) 0.0100(12) 0.0122(13) -0.0037(10) -0.0010(10) -0.0012(10) C8 0.0112(13) 0.0116(12) 0.0119(14) -0.0036(10) -0.0018(11) 0.0014(10) C9 0.0145(14) 0.0189(14) 0.0115(14) -0.0016(11) -0.0051(11) 0.0041(11) C10 0.0121(13) 0.0130(12) 0.0087(13) 0.0013(10) -0.0051(11) 0.0037(11) C11 0.0208(15) 0.0127(13) 0.0144(14) -0.0047(11) -0.0087(12) 0.0034(11) C12 0.0182(15) 0.0128(13) 0.0219(15) -0.0020(11) -0.0099(12) -0.0010(11) C13 0.0118(13) 0.0196(14) 0.0153(14) 0.0010(12) -0.0031(11) 0.0029(11) C14 0.0217(15) 0.0178(13) 0.0114(14) -0.0053(11) -0.0073(12) 0.0084(12) C15 0.0171(14) 0.0103(12) 0.0125(14) -0.0013(10) -0.0089(11) 0.0019(11) N1 0.0099(11) 0.0114(10) 0.0103(11) -0.0010(9) -0.0024(9) 0.0018(9) N2 0.0127(11) 0.0115(10) 0.0103(11) -0.0023(9) -0.0025(9) 0.0023(9) N3 0.0107(11) 0.0117(10) 0.0099(11) -0.0038(9) -0.0031(9) 0.0020(9) F1 0.0157(8) 0.0260(9) 0.0286(10) -0.0088(8) -0.0093(7) 0.0057(7) F2 0.0184(9) 0.0259(9) 0.0165(9) 0.0000(7) -0.0064(7) -0.0074(7) F3 0.0261(9) 0.0268(9) 0.0175(9) -0.0109(7) -0.0114(7) 0.0023(7) F4 0.0308(10) 0.0469(12) 0.0301(10) -0.0270(9) -0.0111(9) -0.0026(9) F5 0.0236(9) 0.0166(8) 0.0261(9) -0.0067(7) 0.0027(8) -0.0049(7) F6 0.0229(9) 0.0318(10) 0.0307(10) -0.0143(8) -0.0052(8) 0.0131(8) Ag1 0.01415(12) 0.01057(11) 0.01254(12) -0.00420(8) -0.00569(9) 0.00400(8) Sb1 0.01129(10) 0.01500(10) 0.01208(11) -0.00659(8) -0.00241(8) -0.00048(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.389(4) . ? C1 C6 1.395(4) . ? C1 H1 0.93 . ? C2 C3 1.388(4) . ? C2 H2 0.93 . ? C3 C4 1.392(4) . ? C3 H3 0.93 . ? C4 C5 1.386(4) . ? C4 H4 0.93 . ? C5 C6 1.403(4) . ? C5 H5 0.93 . ? C6 C7 1.464(4) . ? C7 N3 1.364(3) . ? C7 C8 1.379(4) . ? C8 N1 1.342(3) . ? C8 H8 0.93 . ? C9 N1 1.477(3) . ? C9 C10 1.512(4) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 C11 1.390(4) . ? C10 C15 1.404(4) . ? C11 C12 1.394(4) . ? C11 H11 0.93 . ? C12 C13 1.384(4) . ? C12 H12 0.93 . ? C13 C14 1.389(4) . ? C13 H13 0.93 . ? C14 C15 1.395(4) . ? C14 H14 0.93 . ? C15 Ag1 2.457(3) 2_566 ? C15 H15 0.93 . ? N1 N2 1.334(3) . ? N2 N3 1.319(3) . ? N2 Ag1 2.353(2) 2_566 ? N3 Ag1 2.222(2) . ? F1 Sb1 1.8713(18) . ? F2 Sb1 1.8855(17) . ? F3 Sb1 1.8779(17) . ? F4 Sb1 1.8778(18) . ? F5 Sb1 1.8851(18) . ? F6 Sb1 1.8702(18) . ? Ag1 N2 2.353(2) 2_566 ? Ag1 C15 2.457(3) 2_566 ? 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 C2 C1 C6 120.4(3) . . ? C2 C1 H1 119.8 . . ? C6 C1 H1 119.8 . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 118.9(3) . . ? C1 C6 C7 121.2(2) . . ? C5 C6 C7 119.9(2) . . ? N3 C7 C8 107.0(2) . . ? N3 C7 C6 123.0(2) . . ? C8 C7 C6 130.0(2) . . ? N1 C8 C7 105.5(2) . . ? N1 C8 H8 127.2 . . ? C7 C8 H8 127.2 . . ? N1 C9 C10 110.2(2) . . ? N1 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N1 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C15 119.5(2) . . ? C11 C10 C9 120.6(2) . . ? C15 C10 C9 119.9(2) . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.2(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 119.8(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C10 120.1(3) . . ? C14 C15 Ag1 94.80(17) . 2_566 ? C10 C15 Ag1 88.54(16) . 2_566 ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? Ag1 C15 H15 86.7 2_566 . ? N2 N1 C8 110.8(2) . . ? N2 N1 C9 119.6(2) . . ? C8 N1 C9 129.6(2) . . ? N3 N2 N1 107.4(2) . . ? N3 N2 Ag1 128.14(16) . 2_566 ? N1 N2 Ag1 121.86(16) . 2_566 ? N2 N3 C7 109.2(2) . . ? N2 N3 Ag1 115.32(15) . . ? C7 N3 Ag1 135.45(18) . . ? N3 Ag1 N2 114.10(8) . 2_566 ? N3 Ag1 C15 152.51(8) . 2_566 ? N2 Ag1 C15 92.98(9) 2_566 2_566 ? F6 Sb1 F1 179.53(8) . . ? F6 Sb1 F4 89.35(9) . . ? F1 Sb1 F4 90.20(8) . . ? F6 Sb1 F3 90.22(8) . . ? F1 Sb1 F3 90.23(8) . . ? F4 Sb1 F3 179.50(8) . . ? F6 Sb1 F5 90.48(9) . . ? F1 Sb1 F5 89.64(8) . . ? F4 Sb1 F5 90.07(9) . . ? F3 Sb1 F5 90.18(8) . . ? F6 Sb1 F2 90.01(9) . . ? F1 Sb1 F2 89.87(8) . . ? F4 Sb1 F2 90.20(9) . . ? F3 Sb1 F2 89.56(8) . . ? F5 Sb1 F2 179.44(8) . . ? # END of CIF # Attachment 'mlg151a.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2009-09-16 at 10:48:20 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\program files\wingx\files\archive.reqdat # CIF files read : pcf mg151 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_mlg151a _database_code_depnum_ccdc_archive 'CCDC 751441' #TrackingRef 'mlg151a.cif' _audit_creation_date 2009-09-16T10:48:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C60 H32 Ag2 F20 N12, 2(F6 Sb)' _chemical_formula_sum 'C60 H32 Ag2 F32 N12 Sb2' _chemical_formula_weight 1988.24 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.205(2) _cell_length_b 9.169(1) _cell_length_c 28.623(4) _cell_angle_alpha 90.000(0) _cell_angle_beta 91.499(6) _cell_angle_gamma 90.000(0) _cell_volume 3202.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9416 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 36.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.584 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.580 _exptl_absorpt_correction_T_max 0.752 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_unetI/netI 0.014 _diffrn_reflns_number 109980 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5957 _reflns_number_gt 5796 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997) & Mercury (Macrae et al., 2006)' _computing_publication_material 'SHELXTL-97 (Sheldrick, 2008) & enCIFer (Allen et al., 2004)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0153P)^2^+4.4125P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5957 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0487 _refine_ls_wR_factor_gt 0.0483 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.733 _refine_diff_density_min -0.41 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C -0.1703(2) 0.0411(3) 0.72160(8) 0.0237(5) Uani 1 1 d . . . C2 C -0.2561(2) 0.1273(3) 0.70683(10) 0.0327(6) Uani 1 1 d . . . C3 C -0.3598(2) 0.0975(3) 0.72154(11) 0.0376(7) Uani 1 1 d . . . C4 C -0.3769(2) -0.0181(3) 0.75116(10) 0.0321(6) Uani 1 1 d . . . C5 C -0.2891(2) -0.1028(3) 0.76595(9) 0.0236(5) Uani 1 1 d . . . C6 C -0.18376(18) -0.0755(2) 0.75191(8) 0.0180(5) Uani 1 1 d . . . C7 C -0.08804(18) -0.1670(2) 0.76849(8) 0.0184(5) Uani 1 1 d . . . H7A H -0.1148 -0.2523 0.7847 0.022 Uiso 1 1 calc R . . H7B H -0.0477 -0.2002 0.7418 0.022 Uiso 1 1 calc R . . C8 C 0.08127(18) -0.0181(2) 0.79044(8) 0.0171(4) Uani 1 1 d . . . H8 H 0.1177 -0.02 0.7623 0.021 Uiso 1 1 calc R . . C9 C 0.11344(17) 0.0519(2) 0.83080(7) 0.0149(4) Uani 1 1 d . . . C10 C 0.21090(18) 0.1428(2) 0.84054(7) 0.0163(4) Uani 1 1 d . . . C11 C 0.31251(19) 0.1054(3) 0.82236(8) 0.0200(5) Uani 1 1 d . . . H11 H 0.3195 0.0223 0.8041 0.024 Uiso 1 1 calc R . . C12 C 0.40290(19) 0.1937(3) 0.83187(9) 0.0245(5) Uani 1 1 d . . . H12 H 0.4705 0.1695 0.8197 0.029 Uiso 1 1 calc R . . C13 C 0.3934(2) 0.3178(3) 0.85935(8) 0.0252(5) Uani 1 1 d . . . H13 H 0.4546 0.3755 0.8659 0.03 Uiso 1 1 calc R . . C14 C 0.2930(2) 0.3555(3) 0.87695(9) 0.0255(5) Uani 1 1 d . . . H14 H 0.2865 0.4386 0.8953 0.031 Uiso 1 1 calc R . . C15 C 0.2015(2) 0.2692(3) 0.86720(8) 0.0208(5) Uani 1 1 d . . . H15 H 0.1337 0.2959 0.8785 0.025 Uiso 1 1 calc R . . C16 C 0.4579(2) 0.1315(3) 1.09647(8) 0.0227(5) Uani 1 1 d . . . C17 C 0.5656(2) 0.1128(3) 1.08489(9) 0.0275(6) Uani 1 1 d . . . C18 C 0.5959(2) -0.0097(3) 1.06056(9) 0.0286(6) Uani 1 1 d . . . C19 C 0.5188(2) -0.1137(3) 1.04855(8) 0.0266(5) Uani 1 1 d . . . C20 C 0.4111(2) -0.0930(3) 1.06094(8) 0.0226(5) Uani 1 1 d . . . C21 C 0.37764(18) 0.0296(3) 1.08502(8) 0.0188(5) Uani 1 1 d . . . C22 C 0.25992(18) 0.0527(3) 1.09795(8) 0.0197(5) Uani 1 1 d . . . H22A H 0.2243 -0.0411 1.1016 0.024 Uiso 1 1 calc R . . H22B H 0.2574 0.1039 1.1276 0.024 Uiso 1 1 calc R . . C23 C 0.21371(18) 0.2789(2) 1.05037(8) 0.0172(4) Uani 1 1 d . . . H23 H 0.257 0.3475 1.0661 0.021 Uiso 1 1 calc R . . C24 C 0.14931(17) 0.3007(2) 1.01073(7) 0.0157(4) Uani 1 1 d . . . C25 C 0.13333(18) 0.4355(2) 0.98366(8) 0.0165(4) Uani 1 1 d . . . C26 C 0.1970(2) 0.5576(3) 0.99467(8) 0.0234(5) Uani 1 1 d . . . H26 H 0.2487 0.553 1.019 0.028 Uiso 1 1 calc R . . C27 C 0.1835(2) 0.6860(3) 0.96941(9) 0.0283(6) Uani 1 1 d . . . H27 H 0.2245 0.768 0.9775 0.034 Uiso 1 1 calc R . . C28 C 0.1089(2) 0.6919(3) 0.93213(9) 0.0268(5) Uani 1 1 d . . . H28 H 0.1023 0.7767 0.9144 0.032 Uiso 1 1 calc R . . C29 C 0.0444(2) 0.5725(3) 0.92118(8) 0.0233(5) Uani 1 1 d . . . H29 H -0.0059 0.5769 0.8962 0.028 Uiso 1 1 calc R . . C30 C 0.05467(18) 0.4456(3) 0.94762(8) 0.0188(5) Uani 1 1 d . . . H30 H 0.0087 0.3669 0.9412 0.023 Uiso 1 1 calc R . . N1 N -0.01435(15) -0.0837(2) 0.80008(6) 0.0154(4) Uani 1 1 d . . . N2 N -0.04347(15) -0.0587(2) 0.84407(6) 0.0159(4) Uani 1 1 d . . . N3 N 0.03457(14) 0.0243(2) 0.86278(6) 0.0146(4) Uani 1 1 d . . . N4 N 0.20094(15) 0.1379(2) 1.06162(6) 0.0163(4) Uani 1 1 d . . . N5 N 0.13220(15) 0.0703(2) 1.03141(6) 0.0166(4) Uani 1 1 d . . . N6 N 0.10091(15) 0.1705(2) 1.00034(6) 0.0155(4) Uani 1 1 d . . . F1 F -0.32658(12) 0.45142(17) 0.87526(5) 0.0331(3) Uani 1 1 d . . . F2 F -0.31027(11) 0.18674(15) 0.83773(5) 0.0242(3) Uani 1 1 d . . . F3 F -0.30100(13) 0.41699(17) 0.78211(5) 0.0346(4) Uani 1 1 d . . . F4 F -0.12138(12) 0.26602(17) 0.79982(5) 0.0314(3) Uani 1 1 d . . . F5 F -0.14348(13) 0.53075(16) 0.83522(6) 0.0346(4) Uani 1 1 d . . . F6 F -0.14712(11) 0.29394(15) 0.89011(5) 0.0236(3) Uani 1 1 d . . . F7 F -0.06933(12) 0.07125(17) 0.70645(5) 0.0329(4) Uani 1 1 d . . . F8 F -0.23853(16) 0.23905(19) 0.67763(7) 0.0518(5) Uani 1 1 d . . . F9 F -0.44411(16) 0.1791(2) 0.70661(8) 0.0606(6) Uani 1 1 d . . . F10 F -0.47760(13) -0.0481(2) 0.76562(7) 0.0531(5) Uani 1 1 d . . . F11 F -0.30792(12) -0.21485(18) 0.79502(5) 0.0329(3) Uani 1 1 d . . . F12 F 0.43007(12) 0.25383(17) 1.11892(5) 0.0320(3) Uani 1 1 d . . . F13 F 0.64044(13) 0.2142(2) 1.09662(6) 0.0442(4) Uani 1 1 d . . . F14 F 0.70031(12) -0.0281(2) 1.04828(6) 0.0417(4) Uani 1 1 d . . . F15 F 0.54789(14) -0.23239(18) 1.02461(6) 0.0410(4) Uani 1 1 d . . . F16 F 0.33772(13) -0.19579(17) 1.04912(5) 0.0329(3) Uani 1 1 d . . . Ag1 Ag 0.025141(14) 0.086006(18) 0.935863(6) 0.01824(5) Uani 1 1 d . . . Sb1 Sb -0.226659(12) 0.358518(16) 0.836751(5) 0.01649(5) 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 C1 0.0257(12) 0.0214(12) 0.0236(12) -0.0049(10) -0.0068(10) -0.0050(10) C2 0.0468(17) 0.0178(13) 0.0323(14) -0.0018(11) -0.0198(12) -0.0012(11) C3 0.0351(15) 0.0289(15) 0.0475(18) -0.0156(13) -0.0239(13) 0.0119(12) C4 0.0171(12) 0.0393(16) 0.0397(16) -0.0173(13) -0.0054(11) 0.0003(11) C5 0.0232(12) 0.0256(13) 0.0221(12) -0.0078(10) -0.0015(10) -0.0041(10) C6 0.0198(11) 0.0178(11) 0.0161(11) -0.0069(9) -0.0035(9) -0.0009(9) C7 0.0199(11) 0.0163(11) 0.0189(11) -0.0054(9) -0.0006(9) -0.0016(9) C8 0.0177(11) 0.0171(11) 0.0167(11) 0.0006(9) 0.0039(9) 0.0023(9) C9 0.0162(10) 0.0139(10) 0.0147(10) 0.0023(8) 0.0009(8) 0.0036(8) C10 0.0176(11) 0.0184(11) 0.0130(10) 0.0042(8) -0.0001(8) -0.0002(9) C11 0.0197(11) 0.0222(12) 0.0180(11) 0.0010(9) -0.0006(9) 0.0010(9) C12 0.0171(11) 0.0312(14) 0.0252(12) 0.0056(11) 0.0013(9) -0.0017(10) C13 0.0250(12) 0.0286(13) 0.0218(12) 0.0066(10) -0.0056(10) -0.0119(10) C14 0.0346(14) 0.0210(12) 0.0209(12) -0.0012(10) 0.0016(10) -0.0078(10) C15 0.0233(12) 0.0201(12) 0.0193(11) 0.0003(9) 0.0051(9) -0.0029(9) C16 0.0228(12) 0.0284(13) 0.0167(11) 0.0022(10) -0.0015(9) -0.0028(10) C17 0.0183(12) 0.0411(15) 0.0231(13) 0.0072(11) -0.0033(10) -0.0079(11) C18 0.0182(12) 0.0432(16) 0.0245(13) 0.0145(11) 0.0038(10) 0.0063(11) C19 0.0327(14) 0.0309(14) 0.0164(12) 0.0073(10) 0.0052(10) 0.0095(11) C20 0.0264(12) 0.0242(12) 0.0170(11) 0.0052(9) -0.0027(9) -0.0024(10) C21 0.0169(11) 0.0256(12) 0.0137(11) 0.0062(9) -0.0016(9) -0.0009(9) C22 0.0177(11) 0.0254(12) 0.0158(11) 0.0060(9) -0.0012(9) -0.0025(9) C23 0.0162(10) 0.0190(11) 0.0164(11) -0.0004(9) 0.0001(8) -0.0026(9) C24 0.0127(10) 0.0197(11) 0.0149(10) -0.0023(9) 0.0018(8) -0.0017(8) C25 0.0167(10) 0.0178(11) 0.0153(11) -0.0010(9) 0.0028(8) 0.0009(8) C26 0.0249(12) 0.0240(13) 0.0209(12) 0.0011(10) -0.0047(10) -0.0052(10) C27 0.0358(14) 0.0203(12) 0.0289(13) 0.0020(10) 0.0001(11) -0.0074(11) C28 0.0349(14) 0.0208(12) 0.0250(13) 0.0052(10) 0.0038(11) 0.0058(10) C29 0.0245(12) 0.0268(13) 0.0184(12) -0.0025(10) -0.0002(9) 0.0090(10) C30 0.0169(11) 0.0210(12) 0.0188(11) -0.0046(9) 0.0019(9) 0.0025(9) N1 0.0162(9) 0.0159(9) 0.0140(9) -0.0020(7) -0.0003(7) 0.0011(7) N2 0.0182(9) 0.0168(9) 0.0125(9) -0.0003(7) 0.0001(7) 0.0003(7) N3 0.0145(9) 0.0152(9) 0.0140(9) 0.0009(7) -0.0002(7) -0.0012(7) N4 0.0127(9) 0.0212(10) 0.0150(9) 0.0009(8) -0.0008(7) -0.0027(7) N5 0.0160(9) 0.0203(10) 0.0134(9) 0.0008(7) 0.0003(7) -0.0038(7) N6 0.0150(9) 0.0180(9) 0.0137(9) -0.0001(7) 0.0016(7) -0.0030(7) F1 0.0298(8) 0.0333(8) 0.0367(9) -0.0044(7) 0.0077(7) 0.0079(7) F2 0.0261(7) 0.0237(7) 0.0226(7) 0.0033(6) -0.0050(6) -0.0091(6) F3 0.0383(9) 0.0380(9) 0.0267(8) 0.0127(7) -0.0122(7) -0.0013(7) F4 0.0318(8) 0.0394(9) 0.0236(7) -0.0003(6) 0.0105(6) 0.0022(7) F5 0.0362(8) 0.0249(8) 0.0425(9) 0.0106(7) -0.0062(7) -0.0142(7) F6 0.0229(7) 0.0276(7) 0.0198(7) 0.0038(6) -0.0061(5) -0.0039(6) F7 0.0333(8) 0.0357(9) 0.0295(8) 0.0087(7) -0.0017(7) -0.0116(7) F8 0.0705(13) 0.0276(9) 0.0556(11) 0.0142(8) -0.0326(10) -0.0068(8) F9 0.0471(11) 0.0479(11) 0.0848(15) -0.0138(11) -0.0372(11) 0.0224(9) F10 0.0167(8) 0.0676(13) 0.0750(14) -0.0173(11) 0.0016(8) 0.0011(8) F11 0.0262(8) 0.0415(9) 0.0311(8) 0.0015(7) 0.0044(6) -0.0115(7) F12 0.0288(8) 0.0332(8) 0.0339(8) -0.0094(7) 0.0013(6) -0.0080(6) F13 0.0244(8) 0.0619(12) 0.0461(10) -0.0037(9) -0.0019(7) -0.0196(8) F14 0.0209(8) 0.0611(11) 0.0437(10) 0.0166(8) 0.0104(7) 0.0106(7) F15 0.0506(10) 0.0376(9) 0.0355(9) 0.0002(7) 0.0103(8) 0.0163(8) F16 0.0381(9) 0.0282(8) 0.0322(8) -0.0030(7) -0.0009(7) -0.0086(7) Ag1 0.02457(10) 0.01790(9) 0.01208(9) -0.00064(6) -0.00254(6) -0.00393(7) Sb1 0.01682(8) 0.01773(8) 0.01486(8) 0.00316(6) -0.00070(6) -0.00259(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 F7 1.346(3) . ? C1 C2 1.370(4) . ? C1 C6 1.389(3) . ? C2 F8 1.343(3) . ? C2 C3 1.372(4) . ? C3 F9 1.334(3) . ? C3 C4 1.376(4) . ? C4 F10 1.336(3) . ? C4 C5 1.380(4) . ? C5 F11 1.345(3) . ? C5 C6 1.380(3) . ? C6 C7 1.505(3) . ? C7 N1 1.472(3) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 N1 1.348(3) . ? C8 C9 1.370(3) . ? C8 H8 0.93 . ? C9 N3 1.369(3) . ? C9 C10 1.473(3) . ? C10 C15 1.394(3) . ? C10 C11 1.400(3) . ? C11 C12 1.389(3) . ? C11 H11 0.93 . ? C12 C13 1.390(4) . ? C12 H12 0.93 . ? C13 C14 1.381(4) . ? C13 H13 0.93 . ? C14 C15 1.391(3) . ? C14 H14 0.93 . ? C15 H15 0.93 . ? C16 F12 1.341(3) . ? C16 C17 1.375(4) . ? C16 C21 1.387(3) . ? C17 F13 1.339(3) . ? C17 C18 1.377(4) . ? C18 F14 1.342(3) . ? C18 C19 1.376(4) . ? C19 F15 1.339(3) . ? C19 C20 1.384(4) . ? C20 F16 1.337(3) . ? C20 C21 1.386(4) . ? C21 C22 1.508(3) . ? C22 N4 1.473(3) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 N4 1.342(3) . ? C23 C24 1.378(3) . ? C23 H23 0.93 . ? C24 N6 1.362(3) . ? C24 C25 1.469(3) . ? C25 C30 1.394(3) . ? C25 C26 1.394(3) . ? C26 C27 1.389(4) . ? C26 H26 0.93 . ? C27 C28 1.385(4) . ? C27 H27 0.93 . ? C28 C29 1.380(4) . ? C28 H28 0.93 . ? C29 C30 1.392(3) . ? C29 H29 0.93 . ? C30 H30 0.93 . ? N1 N2 1.337(3) . ? N2 N3 1.321(3) . ? N3 Ag1 2.1731(18) . ? N4 N5 1.341(3) . ? N5 N6 1.328(3) . ? N5 Ag1 2.5908(19) 3_557 ? N6 Ag1 2.1845(18) . ? F1 Sb1 1.8704(15) . ? F2 Sb1 1.8774(15) . ? F3 Sb1 1.8661(14) . ? F4 Sb1 1.8865(15) . ? F5 Sb1 1.8785(16) . ? F6 Sb1 1.8835(13) . ? Ag1 N5 2.591(2) 3_557 ? 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 F7 C1 C2 118.7(2) . . ? F7 C1 C6 118.9(2) . . ? C2 C1 C6 122.4(2) . . ? F8 C2 C1 120.0(3) . . ? F8 C2 C3 120.4(3) . . ? C1 C2 C3 119.6(3) . . ? F9 C3 C2 120.0(3) . . ? F9 C3 C4 120.1(3) . . ? C2 C3 C4 119.9(2) . . ? F10 C4 C3 120.3(3) . . ? F10 C4 C5 120.1(3) . . ? C3 C4 C5 119.6(3) . . ? F11 C5 C6 119.6(2) . . ? F11 C5 C4 118.4(2) . . ? C6 C5 C4 122.0(2) . . ? C5 C6 C1 116.6(2) . . ? C5 C6 C7 121.9(2) . . ? C1 C6 C7 121.5(2) . . ? N1 C7 C6 111.15(18) . . ? N1 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? N1 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108 . . ? N1 C8 C9 105.49(19) . . ? N1 C8 H8 127.3 . . ? C9 C8 H8 127.3 . . ? N3 C9 C8 106.62(19) . . ? N3 C9 C10 123.81(19) . . ? C8 C9 C10 129.6(2) . . ? C15 C10 C11 119.6(2) . . ? C15 C10 C9 119.8(2) . . ? C11 C10 C9 120.7(2) . . ? C12 C11 C10 119.4(2) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.7(2) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 120.0(2) . . ? C14 C13 H13 120 . . ? C12 C13 H13 120 . . ? C13 C14 C15 120.0(2) . . ? C13 C14 H14 120 . . ? C15 C14 H14 120 . . ? C14 C15 C10 120.4(2) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? F12 C16 C17 118.4(2) . . ? F12 C16 C21 119.4(2) . . ? C17 C16 C21 122.2(2) . . ? F13 C17 C16 120.2(3) . . ? F13 C17 C18 120.2(2) . . ? C16 C17 C18 119.6(2) . . ? F14 C18 C19 119.7(3) . . ? F14 C18 C17 120.3(2) . . ? C19 C18 C17 120.1(2) . . ? F15 C19 C18 120.2(2) . . ? F15 C19 C20 120.6(2) . . ? C18 C19 C20 119.3(2) . . ? F16 C20 C19 118.3(2) . . ? F16 C20 C21 119.6(2) . . ? C19 C20 C21 122.2(2) . . ? C20 C21 C16 116.7(2) . . ? C20 C21 C22 122.1(2) . . ? C16 C21 C22 121.2(2) . . ? N4 C22 C21 110.64(18) . . ? N4 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? N4 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? N4 C23 C24 105.7(2) . . ? N4 C23 H23 127.2 . . ? C24 C23 H23 127.2 . . ? N6 C24 C23 106.7(2) . . ? N6 C24 C25 124.86(19) . . ? C23 C24 C25 128.5(2) . . ? C30 C25 C26 118.9(2) . . ? C30 C25 C24 121.7(2) . . ? C26 C25 C24 119.4(2) . . ? C27 C26 C25 120.3(2) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 120 . . ? C26 C27 H27 120 . . ? C29 C28 C27 120.2(2) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.8(2) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C25 120.6(2) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? N2 N1 C8 111.67(18) . . ? N2 N1 C7 119.61(18) . . ? C8 N1 C7 128.63(19) . . ? N3 N2 N1 105.89(17) . . ? N2 N3 C9 110.33(18) . . ? N2 N3 Ag1 118.97(13) . . ? C9 N3 Ag1 130.64(15) . . ? N5 N4 C23 111.42(18) . . ? N5 N4 C22 119.73(19) . . ? C23 N4 C22 128.49(19) . . ? N6 N5 N4 106.02(17) . . ? N6 N5 Ag1 114.96(13) . 3_557 ? N4 N5 Ag1 118.67(13) . 3_557 ? N5 N6 C24 110.18(18) . . ? N5 N6 Ag1 115.37(14) . . ? C24 N6 Ag1 131.85(15) . . ? N3 Ag1 N6 150.89(7) . . ? N3 Ag1 N5 105.21(6) . 3_557 ? N6 Ag1 N5 101.07(6) . 3_557 ? F3 Sb1 F1 93.03(7) . . ? F3 Sb1 F2 90.05(7) . . ? F1 Sb1 F2 90.59(7) . . ? F3 Sb1 F5 89.44(7) . . ? F1 Sb1 F5 89.54(8) . . ? F2 Sb1 F5 179.48(7) . . ? F3 Sb1 F6 177.21(7) . . ? F1 Sb1 F6 89.74(7) . . ? F2 Sb1 F6 89.60(6) . . ? F5 Sb1 F6 90.90(7) . . ? F3 Sb1 F4 89.02(7) . . ? F1 Sb1 F4 177.65(7) . . ? F2 Sb1 F4 90.55(7) . . ? F5 Sb1 F4 89.34(8) . . ? F6 Sb1 F4 88.22(7) . . ? # END of CIF