Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'ProfD Alessia Bacchi' _publ_contact_author_address ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisic University of Parma Parco Area delle Scienze 17A Parma I-43100 ITALY ; _publ_contact_author_email ALESSIA.BACCHI@UNIPR.IT _publ_section_title ; Deconvolution of supramolecular tectons and analysis of the structural role of the anions for two 'wheel-and-axle' silver complexes ; loop_ _publ_author_name 'Alessia Bacchi' 'Elsa Bosetti' 'Mauro Carcelli' 'Paolo Pelagatti' 'Dominga Rogolino' data_[Ag(LOH)2]BF4 _database_code_depnum_ccdc_archive 'CCDC 225185' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Ag B F4 N2 O2' _chemical_formula_weight 717.30 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9013(7) _cell_length_b 11.9578(7) _cell_length_c 13.8143(8) _cell_angle_alpha 112.2450(10) _cell_angle_beta 112.2240(10) _cell_angle_gamma 91.3010(10) _cell_volume 1652.59(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4290 _cell_measurement_theta_min 4.8 _cell_measurement_theta_max 55.4 _exptl_crystal_description 'thin platelet' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type 'symmetry-related measurements' _exptl_absorpt_correction_T_min 0.8136 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'according to procedures implemented in the SADABS package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22365 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8176 _reflns_number_gt 5905 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_cell_refinement ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_data_reduction ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. SADABS: Siemens Area Detector Absorption Correction Software, Sheldrick G., 1996, University of Goettingen, Germany. ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'PARST - M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659' _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^)+(0.0486P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8176 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.5000 0.5000 0.5000 0.05931(8) Uani 1 2 d S . . N1 N 0.54787(14) 0.40530(14) 0.60900(13) 0.0503(3) Uani 1 1 d . . . O1 O 0.6143(2) 0.09619(14) 0.76368(15) 0.0931(7) Uani 1 1 d . . . C1 C 0.6326(2) 0.22304(18) 0.83762(17) 0.0625(5) Uani 1 1 d . . . C2 C 0.60335(19) 0.28769(16) 0.75658(15) 0.0525(4) Uani 1 1 d . . . C3 C 0.6336(3) 0.41353(19) 0.79692(19) 0.0808(8) Uani 1 1 d . . . C4 C 0.6036(2) 0.46811(19) 0.72171(18) 0.0707(6) Uani 1 1 d . . . C5 C 0.5210(2) 0.2838(2) 0.5699(2) 0.0678(6) Uani 1 1 d . . . C6 C 0.5467(2) 0.2230(2) 0.63996(18) 0.0662(6) Uani 1 1 d . . . C7 C 0.5460(2) 0.23969(18) 0.89757(17) 0.0610(5) Uani 1 1 d . . . C8 C 0.4505(4) 0.3012(3) 0.8785(3) 0.0936(10) Uani 1 1 d . . . C9 C 0.3756(4) 0.3142(3) 0.9370(3) 0.1122(12) Uani 1 1 d . . . C10 C 0.3973(4) 0.2667(3) 1.0163(3) 0.0986(11) Uani 1 1 d . . . C11 C 0.4894(3) 0.2007(3) 1.0338(2) 0.0936(10) Uani 1 1 d . . . C12 C 0.5637(3) 0.1881(2) 0.9762(2) 0.0770(7) Uani 1 1 d . . . C13 C 0.7666(2) 0.2741(2) 0.9241(2) 0.0746(6) Uani 1 1 d . . . C14 C 0.8011(3) 0.3708(3) 1.0302(3) 0.0886(8) Uani 1 1 d . . . C15 C 0.9235(4) 0.4217(5) 1.1033(4) 0.1238(14) Uani 1 1 d . . . C16 C 1.0145(5) 0.3744(8) 1.0663(7) 0.155(3) Uani 1 1 d . . . C17 C 0.9815(5) 0.2789(7) 0.9658(7) 0.152(2) Uani 1 1 d . . . C18 C 0.8601(4) 0.2290(5) 0.8933(4) 0.1197(13) Uani 1 1 d . . . B B 0.6907(2) -0.18264(18) 0.76877(18) 0.0492(4) Uani 1 1 d . . . F1 F 0.73145(14) -0.15375(14) 0.69911(12) 0.0884(4) Uani 1 1 d . . . F2 F 0.57573(11) -0.26155(12) 0.70179(12) 0.0770(4) Uani 1 1 d . . . F3 F 0.77168(11) -0.24092(12) 0.82569(12) 0.0753(3) Uani 1 1 d . . . F4 F 0.67701(15) -0.07818(11) 0.84853(11) 0.0778(4) Uani 1 1 d . . . H8 H 0.431(3) 0.321(3) 0.830(2) 0.084(9) Uiso 1 1 d . . . H6 H 0.526(2) 0.141(2) 0.607(2) 0.099(9) Uiso 1 1 d . . . H1O H 0.623(3) 0.063(3) 0.800(2) 0.098(10) Uiso 1 1 d . . . H10 H 0.348(3) 0.273(3) 1.051(2) 0.107(10) Uiso 1 1 d . . . H4 H 0.628(2) 0.553(3) 0.747(2) 0.107(9) Uiso 1 1 d . . . H3 H 0.681(3) 0.463(3) 0.874(3) 0.104(9) Uiso 1 1 d . . . H11 H 0.507(3) 0.167(3) 1.089(3) 0.121(11) Uiso 1 1 d . . . H14 H 0.747(3) 0.409(3) 1.061(2) 0.092(10) Uiso 1 1 d . . . H5 H 0.490(2) 0.238(2) 0.496(2) 0.086(8) Uiso 1 1 d . . . H12 H 0.630(3) 0.155(2) 0.995(2) 0.092(9) Uiso 1 1 d . . . H15 H 0.938(3) 0.499(3) 1.168(3) 0.093(10) Uiso 1 1 d . . . H9 H 0.315(3) 0.353(3) 0.922(3) 0.125(12) Uiso 1 1 d . . . H17 H 1.033(5) 0.245(5) 0.923(5) 0.23(3) Uiso 1 1 d . . . H18 H 0.840(3) 0.173(3) 0.819(3) 0.111(12) Uiso 1 1 d . . . H16 H 1.076(4) 0.423(4) 1.116(4) 0.16(2) Uiso 1 1 d . . . Ag2 Ag 0.0000 0.0000 1.0000 0.06773(8) Uani 1 2 d S . . N2 N 0.07453(14) -0.06587(14) 0.87570(12) 0.0534(4) Uani 1 1 d . . . O2 O 0.37066(14) -0.14342(16) 0.70234(15) 0.0728(4) Uani 1 1 d . . . C19 C 0.24267(16) -0.20158(18) 0.63531(15) 0.0532(4) Uani 1 1 d . . . C20 C 0.18184(15) -0.15566(17) 0.71965(14) 0.0451(4) Uani 1 1 d . . . C21 C 0.07860(18) -0.2230(2) 0.70880(17) 0.0599(5) Uani 1 1 d . . . C22 C 0.02764(19) -0.17608(19) 0.78682(18) 0.0623(5) Uani 1 1 d . . . C23 C 0.1738(2) -0.00010(19) 0.88544(16) 0.0588(5) Uani 1 1 d . . . C24 C 0.22859(19) -0.0408(2) 0.81034(16) 0.0556(5) Uani 1 1 d . . . C25 C 0.1856(2) -0.1532(2) 0.54254(18) 0.0718(6) Uani 1 1 d . . . C26 C 0.0625(3) -0.1867(4) 0.4724(3) 0.1038(10) Uani 1 1 d . . . C27 C 0.0090(5) -0.1424(6) 0.3873(3) 0.1400(17) Uani 1 1 d . . . C28 C 0.0835(6) -0.0623(5) 0.3774(4) 0.151(2) Uani 1 1 d . . . C29 C 0.2063(6) -0.0268(5) 0.4476(5) 0.1454(17) Uani 1 1 d . . . C30 C 0.2586(4) -0.0709(3) 0.5316(3) 0.1014(9) Uani 1 1 d . . . C31 C 0.23265(17) -0.34107(19) 0.58758(17) 0.0587(5) Uani 1 1 d . . . C32 C 0.2602(2) -0.3979(2) 0.6617(2) 0.0790(7) Uani 1 1 d . . . C33 C 0.2583(3) -0.5240(3) 0.6212(3) 0.0995(10) Uani 1 1 d . . . C34 C 0.2299(2) -0.5933(3) 0.5070(3) 0.0952(10) Uani 1 1 d . . . C35 C 0.2060(3) -0.5379(3) 0.4343(3) 0.0952(10) Uani 1 1 d . . . C36 C 0.2062(2) -0.4129(2) 0.4723(2) 0.0756(7) Uani 1 1 d . . . H22 H -0.046(2) -0.2202(19) 0.7864(18) 0.063(6) Uiso 1 1 d . . . H21 H 0.043(2) -0.301(2) 0.652(2) 0.070(6) Uiso 1 1 d . . . H35 H 0.177(2) -0.582(2) 0.352(2) 0.077(7) Uiso 1 1 d . . . H24 H 0.301(2) 0.008(2) 0.8249(18) 0.068(6) Uiso 1 1 d . . . H23 H 0.211(2) 0.083(2) 0.957(2) 0.074(7) Uiso 1 1 d . . . H32 H 0.279(2) -0.347(2) 0.741(2) 0.081(7) Uiso 1 1 d . . . H2O H 0.410(2) -0.189(2) 0.6903(19) 0.063(7) Uiso 1 1 d . . . H33 H 0.272(2) -0.556(2) 0.671(2) 0.081(8) Uiso 1 1 d . . . H36 H 0.189(3) -0.365(3) 0.424(2) 0.105(10) Uiso 1 1 d . . . H34 H 0.227(3) -0.678(3) 0.485(3) 0.111(10) Uiso 1 1 d . . . H27 H -0.080(4) -0.200(3) 0.344(3) 0.130(14) Uiso 1 1 d . . . H26 H 0.013(2) -0.255(2) 0.4680(19) 0.063(7) Uiso 1 1 d . . . H30 H 0.363(4) -0.044(4) 0.594(4) 0.162(15) Uiso 1 1 d . . . H28 H 0.036(4) -0.043(4) 0.303(4) 0.207(18) Uiso 1 1 d . . . H29 H 0.253(5) 0.033(5) 0.429(5) 0.22(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.07504(15) 0.06467(14) 0.05382(12) 0.04113(11) 0.02586(10) 0.02180(11) N1 0.0580(9) 0.0532(9) 0.0496(8) 0.0312(7) 0.0225(7) 0.0135(7) O1 0.183(2) 0.0534(9) 0.0761(11) 0.0421(9) 0.0707(12) 0.0493(11) C1 0.1004(16) 0.0512(11) 0.0573(11) 0.0358(9) 0.0405(11) 0.0312(11) C2 0.0763(12) 0.0481(10) 0.0501(10) 0.0305(8) 0.0331(9) 0.0226(9) C3 0.144(2) 0.0458(11) 0.0428(11) 0.0225(9) 0.0249(13) 0.0149(13) C4 0.1114(19) 0.0436(11) 0.0510(11) 0.0270(9) 0.0210(11) 0.0074(11) C5 0.0908(17) 0.0577(13) 0.0474(11) 0.0256(10) 0.0178(11) 0.0121(11) C6 0.0947(16) 0.0438(11) 0.0561(12) 0.0248(9) 0.0239(11) 0.0110(10) C7 0.0922(15) 0.0471(10) 0.0477(10) 0.0222(9) 0.0312(10) 0.0076(10) C8 0.148(3) 0.0868(18) 0.107(2) 0.0650(18) 0.088(2) 0.0556(19) C9 0.164(3) 0.094(2) 0.140(3) 0.060(2) 0.112(3) 0.055(2) C10 0.150(3) 0.0676(16) 0.0835(19) 0.0106(14) 0.077(2) -0.0137(18) C11 0.120(2) 0.097(2) 0.0508(13) 0.0299(13) 0.0270(14) -0.0319(18) C12 0.0914(18) 0.0817(16) 0.0569(13) 0.0409(12) 0.0192(12) -0.0052(14) C13 0.0945(17) 0.0859(16) 0.0830(16) 0.0658(15) 0.0452(14) 0.0408(14) C14 0.0773(18) 0.102(2) 0.090(2) 0.0603(18) 0.0184(16) 0.0138(16) C15 0.099(3) 0.139(4) 0.122(3) 0.082(3) 0.009(2) 0.008(2) C16 0.081(3) 0.207(6) 0.205(6) 0.155(6) 0.018(4) 0.031(4) C17 0.110(4) 0.227(7) 0.203(6) 0.156(5) 0.082(4) 0.087(4) C18 0.129(3) 0.164(4) 0.141(3) 0.113(3) 0.080(3) 0.092(3) B 0.0550(12) 0.0428(10) 0.0507(11) 0.0216(9) 0.0208(9) 0.0141(9) F1 0.1105(11) 0.1027(10) 0.0878(9) 0.0561(8) 0.0606(8) 0.0312(9) F2 0.0574(7) 0.0681(8) 0.0816(8) 0.0215(7) 0.0149(6) 0.0104(6) F3 0.0603(7) 0.0810(8) 0.0983(9) 0.0568(8) 0.0269(6) 0.0289(6) F4 0.1282(11) 0.0491(6) 0.0557(7) 0.0213(5) 0.0380(7) 0.0290(7) Ag2 0.07496(16) 0.07922(16) 0.05247(13) 0.01456(11) 0.04336(11) 0.01094(12) N2 0.0555(9) 0.0583(9) 0.0440(8) 0.0119(7) 0.0282(7) 0.0064(7) O2 0.0451(8) 0.0697(10) 0.0951(12) 0.0189(9) 0.0366(8) 0.0089(7) C19 0.0439(10) 0.0645(11) 0.0489(10) 0.0145(9) 0.0263(8) 0.0112(8) C20 0.0389(9) 0.0554(10) 0.0374(8) 0.0145(7) 0.0170(7) 0.0100(7) C21 0.0503(11) 0.0570(12) 0.0538(11) 0.0002(9) 0.0268(9) -0.0029(9) C22 0.0560(11) 0.0604(12) 0.0634(12) 0.0084(10) 0.0362(10) -0.0017(9) C23 0.0657(12) 0.0579(12) 0.0417(10) 0.0060(9) 0.0266(9) 0.0006(10) C24 0.0518(11) 0.0600(12) 0.0473(10) 0.0110(9) 0.0249(9) -0.0025(9) C25 0.0810(16) 0.0935(17) 0.0547(12) 0.0285(11) 0.0436(12) 0.0376(13) C26 0.090(2) 0.157(3) 0.0698(17) 0.053(2) 0.0331(16) 0.038(2) C27 0.141(4) 0.213(5) 0.084(2) 0.076(3) 0.049(3) 0.084(4) C28 0.211(5) 0.202(5) 0.104(3) 0.100(3) 0.091(4) 0.114(4) C29 0.206(5) 0.166(4) 0.147(4) 0.111(4) 0.109(4) 0.082(4) C30 0.131(3) 0.107(2) 0.107(2) 0.0608(19) 0.074(2) 0.037(2) C31 0.0410(10) 0.0667(12) 0.0554(11) 0.0087(9) 0.0238(8) 0.0098(9) C32 0.0783(16) 0.0694(15) 0.0737(16) 0.0174(13) 0.0280(13) 0.0268(12) C33 0.092(2) 0.080(2) 0.116(3) 0.037(2) 0.0359(19) 0.0349(16) C34 0.0632(15) 0.0593(16) 0.123(3) -0.0016(17) 0.0391(17) 0.0084(13) C35 0.0796(18) 0.0786(19) 0.087(2) -0.0132(16) 0.0433(16) -0.0051(14) C36 0.0649(14) 0.0744(15) 0.0670(14) 0.0003(12) 0.0372(12) -0.0011(11) _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 2.1320(13) . ? Ag1 N1 2.1320(13) 2_666 ? N1 C4 1.319(3) . ? N1 C5 1.326(3) . ? O1 C1 1.427(2) . ? C1 C13 1.519(3) . ? C1 C7 1.523(3) . ? C1 C2 1.531(2) . ? C2 C6 1.364(3) . ? C2 C3 1.376(3) . ? C3 C4 1.370(3) . ? C5 C6 1.370(3) . ? C7 C8 1.364(4) . ? C7 C12 1.394(3) . ? C8 C9 1.390(4) . ? C9 C10 1.361(5) . ? C10 C11 1.366(5) . ? C11 C12 1.374(4) . ? C13 C14 1.375(4) . ? C13 C18 1.387(4) . ? C14 C15 1.376(5) . ? C15 C16 1.408(8) . ? C16 C17 1.324(8) . ? C17 C18 1.364(7) . ? B F1 1.370(2) . ? B F3 1.380(2) . ? B F4 1.380(2) . ? B F2 1.394(2) . ? Ag2 N2 2.1249(14) . ? Ag2 N2 2.1249(14) 2_557 ? N2 C22 1.334(2) . ? N2 C23 1.338(2) . ? O2 C19 1.435(2) . ? C19 C31 1.526(3) . ? C19 C20 1.535(2) . ? C19 C25 1.536(3) . ? C20 C24 1.378(3) . ? C20 C21 1.380(3) . ? C21 C22 1.377(3) . ? C23 C24 1.372(3) . ? C25 C26 1.361(4) . ? C25 C30 1.386(4) . ? C26 C27 1.411(5) . ? C27 C28 1.370(7) . ? C28 C29 1.359(7) . ? C29 C30 1.394(5) . ? C31 C32 1.378(3) . ? C31 C36 1.395(3) . ? C32 C33 1.391(4) . ? C33 C34 1.372(5) . ? C34 C35 1.351(5) . ? C35 C36 1.383(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 N1 Ag1 N1 180.00(6) . 2_666 ? C4 N1 C5 116.59(16) . . ? C4 N1 Ag1 119.98(13) . . ? C5 N1 Ag1 123.39(13) . . ? O1 C1 C13 111.66(19) . . ? O1 C1 C7 109.80(18) . . ? C13 C1 C7 111.32(17) . . ? O1 C1 C2 104.10(15) . . ? C13 C1 C2 107.58(16) . . ? C7 C1 C2 112.17(16) . . ? C6 C2 C3 116.36(17) . . ? C6 C2 C1 121.52(17) . . ? C3 C2 C1 122.12(17) . . ? C4 C3 C2 120.4(2) . . ? N1 C4 C3 123.1(2) . . ? N1 C5 C6 123.6(2) . . ? C2 C6 C5 120.0(2) . . ? C8 C7 C12 117.4(2) . . ? C8 C7 C1 124.09(18) . . ? C12 C7 C1 118.5(2) . . ? C7 C8 C9 121.2(3) . . ? C10 C9 C8 120.3(4) . . ? C9 C10 C11 119.5(3) . . ? C10 C11 C12 120.1(3) . . ? C11 C12 C7 121.3(3) . . ? C14 C13 C18 117.5(3) . . ? C14 C13 C1 122.9(2) . . ? C18 C13 C1 119.5(3) . . ? C13 C14 C15 121.7(4) . . ? C14 C15 C16 118.5(5) . . ? C17 C16 C15 119.8(5) . . ? C16 C17 C18 121.5(5) . . ? C17 C18 C13 121.0(5) . . ? F1 B F3 111.11(17) . . ? F1 B F4 110.79(16) . . ? F3 B F4 109.17(16) . . ? F1 B F2 109.23(17) . . ? F3 B F2 108.44(15) . . ? F4 B F2 108.01(17) . . ? N2 Ag2 N2 180.00(5) . 2_557 ? C22 N2 C23 116.85(16) . . ? C22 N2 Ag2 121.83(13) . . ? C23 N2 Ag2 121.28(12) . . ? O2 C19 C31 108.99(15) . . ? O2 C19 C20 104.91(14) . . ? C31 C19 C20 112.04(16) . . ? O2 C19 C25 109.01(17) . . ? C31 C19 C25 114.05(16) . . ? C20 C19 C25 107.42(15) . . ? C24 C20 C21 116.70(16) . . ? C24 C20 C19 120.02(16) . . ? C21 C20 C19 123.27(16) . . ? C22 C21 C20 120.47(18) . . ? N2 C22 C21 122.64(18) . . ? N2 C23 C24 123.50(18) . . ? C23 C24 C20 119.83(18) . . ? C26 C25 C30 118.8(3) . . ? C26 C25 C19 121.0(3) . . ? C30 C25 C19 120.2(2) . . ? C25 C26 C27 121.5(4) . . ? C28 C27 C26 118.5(5) . . ? C29 C28 C27 120.7(4) . . ? C28 C29 C30 120.5(5) . . ? C25 C30 C29 120.0(4) . . ? C32 C31 C36 118.1(2) . . ? C32 C31 C19 119.46(18) . . ? C36 C31 C19 122.3(2) . . ? C31 C32 C33 120.5(3) . . ? C34 C33 C32 120.4(4) . . ? C35 C34 C33 119.5(3) . . ? C34 C35 C36 121.1(3) . . ? C35 C36 C31 120.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N1 N1 C5 2.3(3) . . 2_666 2_666 ? C22 N2 N2 C23 -2.4(3) . . 2_557 2_557 ? O1 C1 C2 C6 12.7(3) . . . . ? O2 C19 C20 C24 30.0(2) . . . . ? O1 C1 C1 O1 180.0 . . 2_666 2_666 ? O2 C19 C19 O2 180.0 . . 2_557 2_557 ? C6 C2 C1 O1 12.7(3) . . . . ? C12 C7 C1 O1 66.3(3) . . . . ? C18 C13 C1 O1 32.6(3) . . . . ? C24 C20 C19 O2 30.0(2) . . . . ? C32 C31 C19 O2 69.4(2) . . . . ? C30 C25 C19 O2 2.8(3) . . . . ? C1 C1 C19 C19 -109.46(3) 2_666 . . 2_557 ? O1 F4 F2 O2 -56.55(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O F4 0.73(3) 2.07(3) 2.7456(19) 154(3) . O2 H2O F2 0.74(2) 2.15(2) 2.849(2) 159(2) . C4 H4 F2 0.93(3) 2.56(3) 3.360(2) 144(2) 1_565 C5 H5 F2 0.88(3) 2.67(3) 3.383(3) 140(2) 2_656 C22 H22 F3 1.01(2) 2.45(2) 3.408(2) 157.1(17) 1_455 C23 H23 F3 1.04(2) 2.80(2) 3.728(2) 149.8(17) 2_657 C23 H23 F4 1.04(2) 2.53(2) 3.149(2) 117.9(16) 2_657 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.274 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.041 ### END data_[Ag(LOH)2]PF6 _database_code_depnum_ccdc_archive 'CCDC 225186' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H30 Ag F6 N2 O2 P' _chemical_formula_weight 775.46 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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4855(7) _cell_length_b 8.6349(5) _cell_length_c 15.6533(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.2860(10) _cell_angle_gamma 90.00 _cell_volume 1669.98(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8152 _cell_measurement_theta_min 5.3 _cell_measurement_theta_max 49.4 _exptl_crystal_description 'thin needles' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type 'symmetry-related measurements' _exptl_absorpt_correction_T_min 0.6565 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'according to procedures implemented in the SADABS package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16273 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.71 _reflns_number_total 2844 _reflns_number_gt 2323 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_cell_refinement ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. ; _computing_data_reduction ; SAINT: SAX, Area Detector Integration, Siemens Analytical instruments INC., Madison, Wisconsin, USA. SADABS: Siemens Area Detector Absorption Correction Software, Sheldrick G., 1996, University of Goettingen, Germany. ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'PARST - M. Nardelli, J. Appl. Crystallogr. 1995, 28, 659' _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^)+(0.0500P)^2^+0.6036P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2844 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0822 _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 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 Ag Ag 1.0000 0.0000 1.0000 0.07307(15) Uani 1 2 d S . . P P 1.0000 0.0000 0.5000 0.0626(3) Uani 1 2 d S . . N N 0.88470(16) 0.0388(2) 0.88752(13) 0.0538(5) Uani 1 1 d . . . O1 O 0.71831(16) 0.0975(2) 0.57895(10) 0.0552(4) Uani 1 1 d . . . F1 F 0.87868(16) -0.0246(3) 0.45908(19) 0.1150(8) Uani 1 1 d . . . F2 F 0.98270(17) -0.1101(2) 0.57756(15) 0.1040(7) Uani 1 1 d . . . F3 F 1.03932(18) -0.1440(2) 0.44875(15) 0.1057(6) Uani 1 1 d . . . C1 C 0.69483(17) 0.1935(2) 0.64865(13) 0.0425(5) Uani 1 1 d . . . C2 C 0.76089(15) 0.1369(2) 0.73347(13) 0.0398(4) Uani 1 1 d . . . C3 C 0.8294(2) 0.0122(3) 0.73595(18) 0.0575(6) Uani 1 1 d . . . C4 C 0.8886(2) -0.0336(3) 0.81305(19) 0.0656(7) Uani 1 1 d . . . C5 C 0.8158(2) 0.1553(3) 0.88515(16) 0.0661(7) Uani 1 1 d . . . C6 C 0.7541(2) 0.2067(3) 0.81137(16) 0.0630(7) Uani 1 1 d . . . C7 C 0.71951(18) 0.3622(3) 0.62681(15) 0.0482(5) Uani 1 1 d . . . C8 C 0.8076(2) 0.4442(3) 0.6661(2) 0.0633(7) Uani 1 1 d . . . C9 C 0.8277(3) 0.5937(4) 0.6382(3) 0.0793(9) Uani 1 1 d . . . C10 C 0.7603(3) 0.6619(4) 0.5726(2) 0.0799(9) Uani 1 1 d . . . C11 C 0.6747(3) 0.5812(4) 0.5327(3) 0.0925(11) Uani 1 1 d . . . C12 C 0.6538(3) 0.4317(4) 0.5585(2) 0.0780(9) Uani 1 1 d . . . C13 C 0.57379(17) 0.1732(2) 0.65348(13) 0.0441(5) Uani 1 1 d . . . C14 C 0.5193(2) 0.2782(3) 0.69818(18) 0.0622(7) Uani 1 1 d . . . C15 C 0.4099(2) 0.2603(4) 0.7027(2) 0.0769(9) Uani 1 1 d . . . C16 C 0.3529(2) 0.1405(4) 0.65994(19) 0.0698(8) Uani 1 1 d . . . C17 C 0.4048(2) 0.0397(4) 0.61382(18) 0.0656(7) Uani 1 1 d . . . C18 C 0.5158(2) 0.0526(3) 0.61137(15) 0.0537(6) Uani 1 1 d . . . H18 H 0.554(2) -0.020(3) 0.586(2) 0.062(8) Uiso 1 1 d . . . H17 H 0.371(3) -0.044(4) 0.586(2) 0.081(9) Uiso 1 1 d . . . H5 H 0.812(3) 0.201(4) 0.937(2) 0.097(10) Uiso 1 1 d . . . H3 H 0.836(2) -0.039(3) 0.686(2) 0.066(8) Uiso 1 1 d . . . H16 H 0.277(3) 0.138(4) 0.656(2) 0.091(10) Uiso 1 1 d . . . H8 H 0.848(2) 0.403(3) 0.7111(19) 0.067(8) Uiso 1 1 d . . . H6 H 0.705(3) 0.284(4) 0.814(2) 0.080(9) Uiso 1 1 d . . . H12 H 0.596(3) 0.374(4) 0.529(2) 0.094(11) Uiso 1 1 d . . . H4 H 0.938(3) -0.129(4) 0.815(2) 0.104(11) Uiso 1 1 d . . . H14 H 0.559(2) 0.367(3) 0.724(2) 0.077(8) Uiso 1 1 d . . . H10 H 0.777(3) 0.764(4) 0.556(2) 0.096(11) Uiso 1 1 d . . . H9 H 0.889(3) 0.643(4) 0.668(2) 0.106(12) Uiso 1 1 d . . . H15 H 0.374(3) 0.335(5) 0.735(3) 0.115(13) Uiso 1 1 d . . . H1O H 0.774(2) 0.117(4) 0.5708(19) 0.066(10) Uiso 1 1 d . . . H11 H 0.626(4) 0.621(6) 0.484(3) 0.139(16) 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 Ag 0.0750(2) 0.0813(2) 0.0534(2) 0.00413(13) -0.02302(15) 0.00977(15) P 0.0461(5) 0.0618(6) 0.0843(7) 0.0045(5) 0.0241(5) -0.0073(4) N 0.0508(11) 0.0624(12) 0.0446(11) 0.0014(9) -0.0059(9) 0.0041(9) O1 0.0609(11) 0.0649(11) 0.0397(8) -0.0109(7) 0.0069(8) 0.0015(9) F1 0.0586(11) 0.1364(19) 0.146(2) 0.0087(15) 0.0001(12) -0.0219(10) F2 0.1032(14) 0.1003(14) 0.1190(16) 0.0351(12) 0.0516(13) 0.0064(11) F3 0.1227(16) 0.0848(13) 0.1148(16) -0.0109(11) 0.0351(13) 0.0080(11) C1 0.0462(11) 0.0453(11) 0.0354(10) -0.0031(9) 0.0036(9) -0.0007(9) C2 0.0382(10) 0.0414(11) 0.0389(10) -0.0032(9) 0.0027(8) -0.0040(9) C3 0.0636(15) 0.0605(15) 0.0457(13) -0.0115(11) -0.0014(11) 0.0173(12) C4 0.0665(16) 0.0682(16) 0.0572(16) -0.0064(12) -0.0072(13) 0.0230(13) C5 0.0741(17) 0.0824(19) 0.0389(13) -0.0101(13) -0.0016(12) 0.0207(15) C6 0.0716(16) 0.0717(16) 0.0429(13) -0.0099(12) -0.0013(12) 0.0278(14) C7 0.0466(11) 0.0510(12) 0.0474(12) 0.0048(10) 0.0082(10) -0.0014(10) C8 0.0547(14) 0.0551(14) 0.0776(19) 0.0079(14) 0.0006(14) -0.0039(12) C9 0.0699(18) 0.0593(17) 0.108(3) 0.0022(17) 0.0105(18) -0.0182(15) C10 0.086(2) 0.0595(17) 0.098(2) 0.0214(17) 0.0239(18) -0.0049(16) C11 0.101(2) 0.080(2) 0.092(2) 0.042(2) -0.003(2) -0.003(2) C12 0.080(2) 0.0730(18) 0.0741(19) 0.0257(16) -0.0132(16) -0.0134(16) C13 0.0461(11) 0.0494(12) 0.0339(10) 0.0031(9) -0.0044(8) -0.0055(9) C14 0.0474(13) 0.0675(16) 0.0695(17) -0.0173(13) 0.0004(12) -0.0039(12) C15 0.0486(15) 0.096(2) 0.085(2) -0.0145(18) 0.0053(14) 0.0024(14) C16 0.0483(14) 0.097(2) 0.0613(16) 0.0139(16) -0.0001(12) -0.0136(15) C17 0.0712(17) 0.0759(18) 0.0450(13) 0.0080(13) -0.0073(12) -0.0355(15) C18 0.0655(15) 0.0563(14) 0.0378(11) 0.0000(10) 0.0027(11) -0.0162(12) _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 Ag N 2.1340(19) 3_757 ? Ag N 2.1340(19) . ? P F1 1.572(2) 3_756 ? P F1 1.572(2) . ? P F2 1.5809(19) 3_756 ? P F2 1.5809(19) . ? P F3 1.595(2) . ? P F3 1.595(2) 3_756 ? N C5 1.321(3) . ? N C4 1.330(4) . ? O1 C1 1.434(3) . ? C1 C13 1.534(3) . ? C1 C7 1.538(3) . ? C1 C2 1.538(3) . ? C2 C3 1.372(3) . ? C2 C6 1.374(3) . ? C3 C4 1.379(4) . ? C5 C6 1.367(4) . ? C7 C8 1.377(4) . ? C7 C12 1.386(4) . ? C8 C9 1.397(4) . ? C9 C10 1.364(5) . ? C10 C11 1.351(5) . ? C11 C12 1.389(5) . ? C13 C18 1.381(3) . ? C13 C14 1.383(3) . ? C14 C15 1.386(4) . ? C15 C16 1.373(4) . ? C16 C17 1.354(4) . ? C17 C18 1.396(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 N Ag N 180.000(1) 3_757 . ? F1 P F1 180.00(6) 3_756 . ? F1 P F2 90.08(12) 3_756 3_756 ? F1 P F2 89.92(12) . 3_756 ? F1 P F2 89.92(12) 3_756 . ? F1 P F2 90.08(12) . . ? F2 P F2 180.000(1) 3_756 . ? F1 P F3 87.82(13) 3_756 . ? F1 P F3 92.18(13) . . ? F2 P F3 89.80(12) 3_756 . ? F2 P F3 90.20(12) . . ? F1 P F3 92.18(13) 3_756 3_756 ? F1 P F3 87.82(13) . 3_756 ? F2 P F3 90.20(12) 3_756 3_756 ? F2 P F3 89.80(12) . 3_756 ? F3 P F3 180.00(14) . 3_756 ? C5 N C4 116.1(2) . . ? C5 N Ag 120.12(17) . . ? C4 N Ag 122.96(17) . . ? O1 C1 C13 106.42(17) . . ? O1 C1 C7 107.99(17) . . ? C13 C1 C7 110.45(17) . . ? O1 C1 C2 109.29(17) . . ? C13 C1 C2 109.32(16) . . ? C7 C1 C2 113.14(17) . . ? C3 C2 C6 115.9(2) . . ? C3 C2 C1 121.88(19) . . ? C6 C2 C1 122.2(2) . . ? C2 C3 C4 120.2(2) . . ? N C4 C3 123.4(2) . . ? N C5 C6 123.8(2) . . ? C5 C6 C2 120.6(2) . . ? C8 C7 C12 117.9(2) . . ? C8 C7 C1 124.1(2) . . ? C12 C7 C1 117.8(2) . . ? C7 C8 C9 120.2(3) . . ? C10 C9 C8 121.0(3) . . ? C11 C10 C9 119.2(3) . . ? C10 C11 C12 120.9(3) . . ? C7 C12 C11 120.8(3) . . ? C18 C13 C14 118.3(2) . . ? C18 C13 C1 121.0(2) . . ? C14 C13 C1 120.70(19) . . ? C13 C14 C15 120.9(3) . . ? C16 C15 C14 120.3(3) . . ? C17 C16 C15 119.3(3) . . ? C16 C17 C18 121.1(3) . . ? C13 C18 C17 120.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N N C5 -11.0(4) . . 3_757 3_757 ? O1 C1 C2 C3 -0.3(3) . . . . ? O1 C1 C1 O1 180.000(2) . . 3_757 3_757 ? C3 C2 C1 O1 -0.3(3) . . . . ? C12 C7 C1 O1 67.8(3) . . . . ? C18 C13 C1 O1 15.0(3) . . . . ? C1 C1 C1 C1 0.0 3_757 . 3_756 1_556 ? O1 F1 F1 O1 180.0 . . 3_756 3_756 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1O F1 0.75(3) 2.63(3) 3.118(3) 125(3) . O1 H1O F3 0.75(3) 2.40(3) 3.144(3) 172(3) 3_756 C17 H17 O1 0.92(3) 2.70(3) 3.396(3) 134(3) 3_656 C16 H16 F1 0.94(3) 2.65(3) 3.359(3) 133(3) 3_656 C5 H5 F3 0.91(4) 2.73(4) 3.417(4) 132(3) 2_756 C4 H4 F3 1.02(4) 3.01(4) 3.828(4) 138(2) 4_556 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.283 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.050