# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ck18ck _database_code_depnum_ccdc_archive 'CCDC 893777' #TrackingRef 'CCDC_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(K(18-C-6)SiPh3) ((triphenylsilyl)(18-crown-6)potassium)' _chemical_melting_point '126\% - 130 \%C' _chemical_formula_moiety 'C30 H39 K O6 Si' _chemical_formula_sum 'C30 H39 K O6 Si' _chemical_formula_weight 562.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_int_tables_number 14 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 10.0038(4) _cell_length_b 17.7282(6) _cell_length_c 17.1680(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.224(4) _cell_angle_gamma 90.00 _cell_volume 3039.92(19) _cell_formula_units_Z 4 _cell_measurement_temperature 102(2) _cell_measurement_reflns_used 9350 _cell_measurement_theta_min 2.2930 _cell_measurement_theta_max 30.8606 _exptl_crystal_description cuboid _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_T_min 0.99218 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; The collected data cover nominally a full sphere of the reciprocal space. A combination of 12 sets of \w scans were used; each set at different \j, 2\q or \k angles and each scan 1.0 deg in \w. Each frame was exposured for 13s. Nominal crystal to detector distance 45 mm. ; _diffrn_ambient_temperature 102(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction, Xcalibur, EOS' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66552 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 29.99 _reflns_number_total 8687 _reflns_number_gt 6359 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution ; SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350.) ; _computing_structure_refinement ; SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122) ; _computing_molecular_graphics ; ORTEP3 for Windows (L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.) ; _computing_publication_material ; WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.) ; _refine_special_details ; All H atoms were refined using a riding model, with a common U restrained to be 1.2 times the equivalent isotropic displacement parameter of the parent atom. 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^)+(0.0307P)^2^+0.9030P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8687 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 C1 C 0.63567(17) 0.04531(9) 0.92221(9) 0.0318(4) Uani 1 1 d . . . H1A H 0.6100 0.0683 0.9717 0.038 Uiso 1 1 calc R . . H1B H 0.6795 0.0845 0.8914 0.038 Uiso 1 1 calc R . . C2 C 0.73026(17) -0.01841(10) 0.93892(9) 0.0322(4) Uani 1 1 d . . . H2A H 0.8095 -0.0003 0.9706 0.039 Uiso 1 1 calc R . . H2B H 0.6859 -0.0581 0.9688 0.039 Uiso 1 1 calc R . . C3 C 0.87288(17) -0.10364(10) 0.87726(10) 0.0340(4) Uani 1 1 d . . . H3A H 0.8380 -0.1486 0.9036 0.041 Uiso 1 1 calc R . . H3B H 0.9488 -0.0831 0.9102 0.041 Uiso 1 1 calc R . . C4 C 0.91907(16) -0.12505(10) 0.79912(10) 0.0331(4) Uani 1 1 d . . . H4A H 0.9489 -0.0795 0.7716 0.040 Uiso 1 1 calc R . . H4B H 0.9957 -0.1603 0.8054 0.040 Uiso 1 1 calc R . . C5 C 0.85226(15) -0.18561(9) 0.68117(9) 0.0288(4) Uani 1 1 d . . . H5A H 0.9256 -0.2228 0.6887 0.035 Uiso 1 1 calc R . . H5B H 0.8853 -0.1426 0.6509 0.035 Uiso 1 1 calc R . . C6 C 0.73443(16) -0.22123(9) 0.63791(9) 0.0291(4) Uani 1 1 d . . . H6A H 0.7632 -0.2460 0.5900 0.035 Uiso 1 1 calc R . . H6B H 0.6942 -0.2599 0.6710 0.035 Uiso 1 1 calc R . . C7 C 0.52503(16) -0.19166(9) 0.57347(9) 0.0281(3) Uani 1 1 d . . . H7A H 0.4806 -0.2318 0.6027 0.034 Uiso 1 1 calc R . . H7B H 0.5529 -0.2133 0.5237 0.034 Uiso 1 1 calc R . . C8 C 0.43097(16) -0.12765(9) 0.55763(9) 0.0273(3) Uani 1 1 d . . . H8A H 0.4773 -0.0858 0.5321 0.033 Uiso 1 1 calc R . . H8B H 0.3545 -0.1441 0.5226 0.033 Uiso 1 1 calc R . . C9 C 0.28430(16) -0.04637(10) 0.62151(9) 0.0309(4) Uani 1 1 d . . . H9A H 0.2071 -0.0656 0.5888 0.037 Uiso 1 1 calc R . . H9B H 0.3207 -0.0017 0.5954 0.037 Uiso 1 1 calc R . . C10 C 0.23998(15) -0.02478(10) 0.70033(10) 0.0314(4) Uani 1 1 d . . . H10A H 0.1619 0.0095 0.6947 0.038 Uiso 1 1 calc R . . H10B H 0.2131 -0.0704 0.7289 0.038 Uiso 1 1 calc R . . C11 C 0.30873(17) 0.04267(10) 0.81420(9) 0.0315(4) Uani 1 1 d . . . H11A H 0.2703 0.0025 0.8462 0.038 Uiso 1 1 calc R . . H11B H 0.2395 0.0819 0.8039 0.038 Uiso 1 1 calc R . . C12 C 0.42891(18) 0.07640(9) 0.85705(9) 0.0311(4) Uani 1 1 d . . . H12A H 0.4729 0.1128 0.8230 0.037 Uiso 1 1 calc R . . H12B H 0.4013 0.1037 0.9038 0.037 Uiso 1 1 calc R . . C13 C 0.85155(13) 0.15184(8) 0.79765(8) 0.0173(3) Uani 1 1 d . . . C14 C 0.95064(14) 0.10995(8) 0.84009(8) 0.0204(3) Uani 1 1 d . . . H14 H 0.9824 0.0646 0.8181 0.025 Uiso 1 1 calc R . . C15 C 1.00371(15) 0.13237(9) 0.91290(8) 0.0239(3) Uani 1 1 d . . . H15 H 1.0719 0.1031 0.9391 0.029 Uiso 1 1 calc R . . C16 C 0.95750(15) 0.19730(9) 0.94743(8) 0.0257(3) Uani 1 1 d . . . H16 H 0.9931 0.2128 0.9974 0.031 Uiso 1 1 calc R . . C17 C 0.85838(15) 0.23935(9) 0.90788(9) 0.0244(3) Uani 1 1 d . . . H17 H 0.8248 0.2835 0.9313 0.029 Uiso 1 1 calc R . . C18 C 0.80757(14) 0.21733(8) 0.83412(8) 0.0198(3) Uani 1 1 d . . . H18 H 0.7411 0.2476 0.8077 0.024 Uiso 1 1 calc R . . C19 C 0.94277(13) 0.12054(8) 0.64103(8) 0.0174(3) Uani 1 1 d . . . C20 C 1.06038(15) 0.15866(8) 0.66504(9) 0.0231(3) Uani 1 1 d . . . H20 H 1.0662 0.1818 0.7150 0.028 Uiso 1 1 calc R . . C21 C 1.16948(15) 0.16384(9) 0.61814(9) 0.0277(3) Uani 1 1 d . . . H21 H 1.2483 0.1896 0.6367 0.033 Uiso 1 1 calc R . . C22 C 1.16320(16) 0.13163(9) 0.54473(9) 0.0266(3) Uani 1 1 d . . . H22 H 1.2370 0.1353 0.5125 0.032 Uiso 1 1 calc R . . C23 C 1.04861(16) 0.09411(9) 0.51894(9) 0.0277(3) Uani 1 1 d . . . H23 H 1.0428 0.0722 0.4683 0.033 Uiso 1 1 calc R . . C24 C 0.94148(15) 0.08812(9) 0.56664(8) 0.0231(3) Uani 1 1 d . . . H24 H 0.8643 0.0610 0.5481 0.028 Uiso 1 1 calc R . . C25 C 0.69159(13) 0.20216(8) 0.65911(8) 0.0172(3) Uani 1 1 d . . . C26 C 0.55757(14) 0.21498(9) 0.67492(9) 0.0229(3) Uani 1 1 d . . . H26 H 0.5101 0.1768 0.7006 0.028 Uiso 1 1 calc R . . C27 C 0.49155(15) 0.28171(9) 0.65432(9) 0.0256(3) Uani 1 1 d . . . H27 H 0.4015 0.2891 0.6674 0.031 Uiso 1 1 calc R . . C28 C 0.55680(16) 0.33707(9) 0.61496(9) 0.0288(4) Uani 1 1 d . . . H28 H 0.5122 0.3828 0.6008 0.035 Uiso 1 1 calc R . . C29 C 0.68816(16) 0.32543(9) 0.59627(10) 0.0309(4) Uani 1 1 d . . . H29 H 0.7334 0.3630 0.5683 0.037 Uiso 1 1 calc R . . C30 C 0.75387(15) 0.25918(8) 0.61819(9) 0.0236(3) Uani 1 1 d . . . H30 H 0.8440 0.2524 0.6050 0.028 Uiso 1 1 calc R . . O1 O 0.51931(11) 0.01774(6) 0.87950(6) 0.0262(2) Uani 1 1 d . . . O2 O 0.77077(11) -0.04859(6) 0.86727(6) 0.0264(2) Uani 1 1 d . . . O3 O 0.81192(10) -0.15998(6) 0.75496(6) 0.0237(2) Uani 1 1 d . . . O4 O 0.63889(10) -0.16394(6) 0.61818(6) 0.0227(2) Uani 1 1 d . . . O5 O 0.38450(10) -0.10310(6) 0.63058(6) 0.0230(2) Uani 1 1 d . . . O6 O 0.34817(10) 0.01197(6) 0.74256(6) 0.0259(2) Uani 1 1 d . . . Si1 Si 0.78286(4) 0.11294(2) 0.69840(2) 0.01670(9) Uani 1 1 d . . . K1 K 0.59908(3) -0.053023(17) 0.733903(17) 0.01842(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 0.0385(9) 0.0336(9) 0.0241(8) -0.0097(7) 0.0075(7) -0.0184(8) C2 0.0338(9) 0.0441(10) 0.0183(7) 0.0008(7) -0.0022(6) -0.0186(8) C3 0.0293(9) 0.0383(10) 0.0328(9) 0.0098(7) -0.0138(7) -0.0031(7) C4 0.0174(8) 0.0381(10) 0.0431(10) 0.0092(8) -0.0045(7) 0.0000(7) C5 0.0232(8) 0.0332(9) 0.0309(8) 0.0092(7) 0.0101(6) 0.0120(7) C6 0.0355(9) 0.0226(8) 0.0299(8) 0.0010(7) 0.0092(7) 0.0112(7) C7 0.0292(8) 0.0273(8) 0.0283(8) -0.0106(7) 0.0048(6) -0.0068(7) C8 0.0266(8) 0.0343(9) 0.0207(7) -0.0042(6) -0.0009(6) -0.0061(7) C9 0.0257(8) 0.0327(9) 0.0330(9) -0.0001(7) -0.0105(7) 0.0075(7) C10 0.0171(8) 0.0326(9) 0.0442(10) -0.0023(8) -0.0013(7) 0.0058(6) C11 0.0321(9) 0.0318(9) 0.0317(8) -0.0011(7) 0.0123(7) 0.0102(7) C12 0.0466(10) 0.0217(8) 0.0260(8) -0.0029(6) 0.0120(7) 0.0033(7) C13 0.0148(7) 0.0174(7) 0.0200(7) 0.0042(5) 0.0031(5) -0.0018(5) C14 0.0188(7) 0.0203(7) 0.0223(7) 0.0030(6) 0.0023(5) 0.0024(6) C15 0.0196(7) 0.0304(8) 0.0215(7) 0.0070(6) 0.0000(6) 0.0015(6) C16 0.0256(8) 0.0345(9) 0.0171(7) 0.0000(6) 0.0018(6) -0.0041(7) C17 0.0246(8) 0.0251(8) 0.0244(8) -0.0032(6) 0.0073(6) -0.0006(6) C18 0.0165(7) 0.0203(7) 0.0228(7) 0.0032(6) 0.0027(5) 0.0008(5) C19 0.0165(7) 0.0140(6) 0.0215(7) 0.0036(5) 0.0000(5) 0.0029(5) C20 0.0215(7) 0.0227(8) 0.0253(7) -0.0024(6) 0.0024(6) -0.0018(6) C21 0.0198(8) 0.0268(8) 0.0366(9) 0.0019(7) 0.0032(6) -0.0045(6) C22 0.0245(8) 0.0250(8) 0.0314(8) 0.0091(6) 0.0120(6) 0.0060(6) C23 0.0321(9) 0.0303(9) 0.0210(7) 0.0002(6) 0.0053(6) 0.0061(7) C24 0.0222(7) 0.0251(8) 0.0216(7) 0.0009(6) -0.0019(6) 0.0018(6) C25 0.0165(7) 0.0175(7) 0.0173(6) 0.0000(5) -0.0014(5) -0.0002(5) C26 0.0190(7) 0.0236(8) 0.0264(8) 0.0032(6) 0.0028(6) -0.0006(6) C27 0.0169(7) 0.0290(8) 0.0305(8) -0.0038(7) -0.0013(6) 0.0063(6) C28 0.0283(8) 0.0217(8) 0.0356(9) 0.0017(7) -0.0050(7) 0.0073(6) C29 0.0295(9) 0.0248(8) 0.0386(9) 0.0140(7) 0.0032(7) 0.0025(7) C30 0.0183(7) 0.0248(8) 0.0281(8) 0.0061(6) 0.0032(6) 0.0018(6) O1 0.0334(6) 0.0204(5) 0.0247(5) -0.0013(4) 0.0006(4) -0.0061(5) O2 0.0300(6) 0.0298(6) 0.0188(5) 0.0038(4) -0.0042(4) -0.0032(5) O3 0.0172(5) 0.0282(6) 0.0258(5) 0.0049(4) 0.0027(4) 0.0019(4) O4 0.0210(5) 0.0204(5) 0.0270(5) -0.0032(4) 0.0027(4) 0.0020(4) O5 0.0206(5) 0.0256(6) 0.0223(5) -0.0002(4) -0.0023(4) 0.0040(4) O6 0.0202(5) 0.0301(6) 0.0278(6) -0.0042(5) 0.0038(4) 0.0047(4) Si1 0.01465(18) 0.01542(19) 0.01995(19) 0.00257(15) 0.00039(14) -0.00012(14) K1 0.01706(14) 0.01857(15) 0.01945(14) -0.00098(12) -0.00050(11) 0.00076(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 C1 O1 1.4268(18) . ? C1 C2 1.491(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.4210(19) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O2 1.4162(19) . ? C3 C4 1.492(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.4198(18) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O3 1.4254(18) . ? C5 C6 1.497(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.4224(17) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O4 1.4248(17) . ? C7 C8 1.489(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O5 1.4282(17) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O5 1.4223(17) . ? C9 C10 1.497(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O6 1.4259(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O6 1.4209(18) . ? C11 C12 1.498(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O1 1.4173(19) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.4017(19) . ? C13 C14 1.4085(19) . ? C13 Si1 1.9285(14) . ? C14 C15 1.388(2) . ? C14 H14 0.9500 . ? C15 C16 1.386(2) . ? C15 H15 0.9500 . ? C16 C17 1.387(2) . ? C16 H16 0.9500 . ? C17 C18 1.394(2) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.3986(19) . ? C19 C24 1.400(2) . ? C19 Si1 1.9298(14) . ? C20 C21 1.395(2) . ? C20 H20 0.9500 . ? C21 C22 1.382(2) . ? C21 H21 0.9500 . ? C22 C23 1.377(2) . ? C22 H22 0.9500 . ? C23 C24 1.389(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.398(2) . ? C25 C26 1.4014(19) . ? C25 Si1 1.9291(14) . ? C26 C27 1.391(2) . ? C26 H26 0.9500 . ? C27 C28 1.377(2) . ? C27 H27 0.9500 . ? C28 C29 1.385(2) . ? C28 H28 0.9500 . ? C29 C30 1.387(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? O1 K1 2.9466(11) . ? O2 K1 2.7851(10) . ? O3 K1 2.8589(10) . ? O4 K1 2.8392(10) . ? O5 K1 2.8485(10) . ? O6 K1 2.7735(11) . ? Si1 K1 3.5404(5) . ? 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 O1 C1 C2 109.26(13) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? O2 C2 C1 109.12(12) . . ? O2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O2 C3 C4 108.91(12) . . ? O2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? O2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? O3 C4 C3 109.17(13) . . ? O3 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O3 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? O3 C5 C6 108.72(12) . . ? O3 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? O3 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? O4 C6 C5 108.46(12) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? O4 C7 C8 108.25(12) . . ? O4 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O4 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? O5 C8 C7 107.79(12) . . ? O5 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? O5 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.5 . . ? O5 C9 C10 108.93(12) . . ? O5 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? O5 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? O6 C10 C9 108.75(13) . . ? O6 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O6 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O6 C11 C12 108.89(13) . . ? O6 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O6 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O1 C12 C11 108.83(13) . . ? O1 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? O1 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C18 C13 C14 115.79(13) . . ? C18 C13 Si1 125.85(10) . . ? C14 C13 Si1 118.29(10) . . ? C15 C14 C13 122.49(14) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C16 C15 C14 120.20(14) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 118.91(14) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 120.56(14) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 122.03(13) . . ? C17 C18 H18 119.0 . . ? C13 C18 H18 119.0 . . ? C20 C19 C24 115.57(13) . . ? C20 C19 Si1 126.23(11) . . ? C24 C19 Si1 118.13(11) . . ? C21 C20 C19 122.29(14) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C22 C21 C20 120.14(14) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.17(14) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C22 C23 C24 120.22(14) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 122.60(14) . . ? C23 C24 H24 118.7 . . ? C19 C24 H24 118.7 . . ? C30 C25 C26 116.00(13) . . ? C30 C25 Si1 123.59(11) . . ? C26 C25 Si1 120.30(11) . . ? C27 C26 C25 122.32(14) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C28 C27 C26 119.97(14) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 119.31(14) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 120.29(15) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 122.06(14) . . ? C29 C30 H30 119.0 . . ? C25 C30 H30 119.0 . . ? C12 O1 C1 112.21(12) . . ? C12 O1 K1 106.31(8) . . ? C1 O1 K1 109.25(9) . . ? C3 O2 C2 113.18(12) . . ? C3 O2 K1 119.17(9) . . ? C2 O2 K1 121.97(9) . . ? C4 O3 C5 111.75(12) . . ? C4 O3 K1 108.22(9) . . ? C5 O3 K1 110.19(8) . . ? C6 O4 C7 112.83(11) . . ? C6 O4 K1 116.53(8) . . ? C7 O4 K1 118.46(8) . . ? C9 O5 C8 112.43(11) . . ? C9 O5 K1 110.46(8) . . ? C8 O5 K1 111.71(8) . . ? C11 O6 C10 112.05(12) . . ? C11 O6 K1 120.11(9) . . ? C10 O6 K1 116.50(8) . . ? C13 Si1 C25 98.85(6) . . ? C13 Si1 C19 99.30(6) . . ? C25 Si1 C19 98.85(6) . . ? C13 Si1 K1 107.92(4) . . ? C25 Si1 K1 120.09(4) . . ? C19 Si1 K1 126.82(4) . . ? O6 K1 O2 117.54(3) . . ? O6 K1 O4 119.22(3) . . ? O2 K1 O4 119.37(3) . . ? O6 K1 O5 60.68(3) . . ? O2 K1 O5 158.28(3) . . ? O4 K1 O5 58.59(3) . . ? O6 K1 O3 159.82(3) . . ? O2 K1 O3 59.62(3) . . ? O4 K1 O3 59.76(3) . . ? O5 K1 O3 113.69(3) . . ? O6 K1 O1 59.24(3) . . ? O2 K1 O1 58.30(3) . . ? O4 K1 O1 160.69(3) . . ? O5 K1 O1 115.49(3) . . ? O3 K1 O1 114.23(3) . . ? O6 K1 Si1 98.30(2) . . ? O2 K1 Si1 79.39(2) . . ? O4 K1 Si1 111.13(2) . . ? O5 K1 Si1 122.16(2) . . ? O3 K1 Si1 100.53(2) . . ? O1 K1 Si1 87.72(2) . . ? 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 O1 C1 C2 O2 62.08(16) . . . . ? O2 C3 C4 O3 -64.25(17) . . . . ? O3 C5 C6 O4 67.93(15) . . . . ? O4 C7 C8 O5 -64.91(15) . . . . ? O5 C9 C10 O6 67.21(17) . . . . ? O6 C11 C12 O1 -66.71(16) . . . . ? C18 C13 C14 C15 -1.1(2) . . . . ? Si1 C13 C14 C15 -178.33(11) . . . . ? C13 C14 C15 C16 1.4(2) . . . . ? C14 C15 C16 C17 -0.3(2) . . . . ? C15 C16 C17 C18 -1.0(2) . . . . ? C16 C17 C18 C13 1.3(2) . . . . ? C14 C13 C18 C17 -0.3(2) . . . . ? Si1 C13 C18 C17 176.72(11) . . . . ? C24 C19 C20 C21 -0.2(2) . . . . ? Si1 C19 C20 C21 -177.26(11) . . . . ? C19 C20 C21 C22 0.9(2) . . . . ? C20 C21 C22 C23 -0.4(2) . . . . ? C21 C22 C23 C24 -0.7(2) . . . . ? C22 C23 C24 C19 1.5(2) . . . . ? C20 C19 C24 C23 -1.0(2) . . . . ? Si1 C19 C24 C23 176.33(12) . . . . ? C30 C25 C26 C27 -2.7(2) . . . . ? Si1 C25 C26 C27 173.69(11) . . . . ? C25 C26 C27 C28 2.0(2) . . . . ? C26 C27 C28 C29 0.0(2) . . . . ? C27 C28 C29 C30 -1.1(2) . . . . ? C28 C29 C30 C25 0.2(2) . . . . ? C26 C25 C30 C29 1.6(2) . . . . ? Si1 C25 C30 C29 -174.65(12) . . . . ? C11 C12 O1 C1 -178.80(12) . . . . ? C11 C12 O1 K1 61.82(13) . . . . ? C2 C1 O1 C12 -176.02(12) . . . . ? C2 C1 O1 K1 -58.37(13) . . . . ? C4 C3 O2 C2 -173.49(13) . . . . ? C4 C3 O2 K1 32.54(16) . . . . ? C1 C2 O2 C3 172.99(13) . . . . ? C1 C2 O2 K1 -33.86(15) . . . . ? C3 C4 O3 C5 -176.68(13) . . . . ? C3 C4 O3 K1 61.82(13) . . . . ? C6 C5 O3 C4 -179.67(12) . . . . ? C6 C5 O3 K1 -59.31(13) . . . . ? C5 C6 O4 C7 177.26(12) . . . . ? C5 C6 O4 K1 -40.72(14) . . . . ? C8 C7 O4 C6 178.85(12) . . . . ? C8 C7 O4 K1 37.63(15) . . . . ? C10 C9 O5 C8 179.19(13) . . . . ? C10 C9 O5 K1 -55.28(14) . . . . ? C7 C8 O5 C9 -174.64(12) . . . . ? C7 C8 O5 K1 60.51(13) . . . . ? C12 C11 O6 C10 176.90(13) . . . . ? C12 C11 O6 K1 34.58(16) . . . . ? C9 C10 O6 C11 172.56(13) . . . . ? C9 C10 O6 K1 -43.66(15) . . . . ? C18 C13 Si1 C25 16.63(13) . . . . ? C14 C13 Si1 C25 -166.44(11) . . . . ? C18 C13 Si1 C19 117.19(12) . . . . ? C14 C13 Si1 C19 -65.88(12) . . . . ? C18 C13 Si1 K1 -109.09(12) . . . . ? C14 C13 Si1 K1 67.85(11) . . . . ? C30 C25 Si1 C13 86.76(13) . . . . ? C26 C25 Si1 C13 -89.36(12) . . . . ? C30 C25 Si1 C19 -14.17(13) . . . . ? C26 C25 Si1 C19 169.70(11) . . . . ? C30 C25 Si1 K1 -156.48(10) . . . . ? C26 C25 Si1 K1 27.40(13) . . . . ? C20 C19 Si1 C13 -11.30(13) . . . . ? C24 C19 Si1 C13 171.73(11) . . . . ? C20 C19 Si1 C25 89.26(13) . . . . ? C24 C19 Si1 C25 -87.71(11) . . . . ? C20 C19 Si1 K1 -132.10(11) . . . . ? C24 C19 Si1 K1 50.93(12) . . . . ? C11 O6 K1 O2 -3.03(12) . . . . ? C10 O6 K1 O2 -143.75(10) . . . . ? C11 O6 K1 O4 154.73(10) . . . . ? C10 O6 K1 O4 14.01(11) . . . . ? C11 O6 K1 O5 152.31(11) . . . . ? C10 O6 K1 O5 11.59(10) . . . . ? C11 O6 K1 O3 73.40(14) . . . . ? C10 O6 K1 O3 -67.32(14) . . . . ? C11 O6 K1 O1 -3.02(10) . . . . ? C10 O6 K1 O1 -143.74(11) . . . . ? C11 O6 K1 Si1 -85.34(11) . . . . ? C10 O6 K1 Si1 133.94(10) . . . . ? C3 O2 K1 O6 155.28(10) . . . . ? C2 O2 K1 O6 3.67(11) . . . . ? C3 O2 K1 O4 -2.45(11) . . . . ? C2 O2 K1 O4 -154.05(10) . . . . ? C3 O2 K1 O5 75.85(14) . . . . ? C2 O2 K1 O5 -75.76(14) . . . . ? C3 O2 K1 O3 -1.85(10) . . . . ? C2 O2 K1 O3 -153.45(11) . . . . ? C3 O2 K1 O1 155.26(11) . . . . ? C2 O2 K1 O1 3.65(10) . . . . ? C3 O2 K1 Si1 -110.83(10) . . . . ? C2 O2 K1 Si1 97.56(10) . . . . ? C6 O4 K1 O6 -148.23(9) . . . . ? C7 O4 K1 O6 -8.40(11) . . . . ? C6 O4 K1 O2 9.12(11) . . . . ? C7 O4 K1 O2 148.95(9) . . . . ? C6 O4 K1 O5 -145.76(10) . . . . ? C7 O4 K1 O5 -5.93(9) . . . . ? C6 O4 K1 O3 8.52(9) . . . . ? C7 O4 K1 O3 148.35(11) . . . . ? C6 O4 K1 O1 -68.34(14) . . . . ? C7 O4 K1 O1 71.49(14) . . . . ? C6 O4 K1 Si1 98.61(9) . . . . ? C7 O4 K1 Si1 -121.57(9) . . . . ? C9 O5 K1 O6 23.16(9) . . . . ? C8 O5 K1 O6 149.09(10) . . . . ? C9 O5 K1 O2 114.47(12) . . . . ? C8 O5 K1 O2 -119.59(11) . . . . ? C9 O5 K1 O4 -154.37(10) . . . . ? C8 O5 K1 O4 -28.44(9) . . . . ? C9 O5 K1 O3 -178.54(9) . . . . ? C8 O5 K1 O3 -52.60(9) . . . . ? C9 O5 K1 O1 46.57(10) . . . . ? C8 O5 K1 O1 172.51(9) . . . . ? C9 O5 K1 Si1 -57.77(10) . . . . ? C8 O5 K1 Si1 68.17(9) . . . . ? C4 O3 K1 O6 -118.23(12) . . . . ? C5 O3 K1 O6 119.31(11) . . . . ? C4 O3 K1 O2 -30.61(9) . . . . ? C5 O3 K1 O2 -153.06(10) . . . . ? C4 O3 K1 O4 148.79(10) . . . . ? C5 O3 K1 O4 26.33(9) . . . . ? C4 O3 K1 O5 172.65(9) . . . . ? C5 O3 K1 O5 50.19(10) . . . . ? C4 O3 K1 O1 -51.89(10) . . . . ? C5 O3 K1 O1 -174.34(9) . . . . ? C4 O3 K1 Si1 40.37(9) . . . . ? C5 O3 K1 Si1 -82.09(9) . . . . ? C12 O1 K1 O6 -30.28(9) . . . . ? C1 O1 K1 O6 -151.58(10) . . . . ? C12 O1 K1 O2 149.70(10) . . . . ? C1 O1 K1 O2 28.41(9) . . . . ? C12 O1 K1 O4 -121.41(11) . . . . ? C1 O1 K1 O4 117.30(12) . . . . ? C12 O1 K1 O5 -54.06(10) . . . . ? C1 O1 K1 O5 -175.35(9) . . . . ? C12 O1 K1 O3 171.29(9) . . . . ? C1 O1 K1 O3 50.00(10) . . . . ? C12 O1 K1 Si1 70.77(9) . . . . ? C1 O1 K1 Si1 -50.52(9) . . . . ? C13 Si1 K1 O6 92.33(5) . . . . ? C25 Si1 K1 O6 -19.66(5) . . . . ? C19 Si1 K1 O6 -150.66(6) . . . . ? C13 Si1 K1 O2 -24.29(5) . . . . ? C25 Si1 K1 O2 -136.28(6) . . . . ? C19 Si1 K1 O2 92.72(6) . . . . ? C13 Si1 K1 O4 -141.85(5) . . . . ? C25 Si1 K1 O4 106.17(5) . . . . ? C19 Si1 K1 O4 -24.83(6) . . . . ? C13 Si1 K1 O5 152.80(5) . . . . ? C25 Si1 K1 O5 40.81(6) . . . . ? C19 Si1 K1 O5 -90.19(6) . . . . ? C13 Si1 K1 O3 -80.36(5) . . . . ? C25 Si1 K1 O3 167.65(5) . . . . ? C19 Si1 K1 O3 36.65(6) . . . . ? C13 Si1 K1 O1 33.86(5) . . . . ? C25 Si1 K1 O1 -78.12(5) . . . . ? C19 Si1 K1 O1 150.88(6) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.349 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.053 _exptl_crystal_recrystallization_method ; From solution in PhMe layered with n-pentane at rt. ; data_ck22ck _database_code_depnum_ccdc_archive 'CCDC 924392' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '18-Crown-6-potassium triphenyl-carbon' _chemical_melting_point ? _chemical_formula_moiety 'C31 H39 K O6' _chemical_formula_sum 'C31 H39 K O6' _chemical_formula_weight 546.72 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' K K 0.2009 0.2494 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_int_tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.8014(5) _cell_length_b 28.7693(14) _cell_length_c 19.7370(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.447(5) _cell_angle_gamma 90.00 _cell_volume 5565.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20183 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 30.84 _exptl_crystal_description fragment _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; The collected data cover nominally a full sphere of the reciprocal space. A combination of 29 sets of \w scans were used; each set at different \j, 2\q or \k angles and each scan 1.0 deg in \w. Each frame was exposured for 25s. Nominal crystal to detector distance 45 mm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction, Xcalibur, EOS' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25554 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1051 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.00 _reflns_number_total 25554 _reflns_number_gt 17536 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution ; SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350.) ; _computing_structure_refinement ; SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122) ; _computing_molecular_graphics ; Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany. ; _computing_publication_material ; WinGX v1.80.05 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.) ; _refine_special_details ; The crystal is non-meroherically twinned by a 180 deg rotation about the b-axis twinned and the twin factor refined to 0.3394(5). Both domains were indexed separately and the data were integrated to a dataset containing intensities of both domains (HKLF5). While this dataset was used in the refinement, the structure was solved with intensity data of one domain only (Rint = 13.92, wR2 = 14.79). Twin matrix: -1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 -1.00 A disordered part of two crown ether moieties was refined using a split atom model (0.504(7) and 0.468(8) SOF of main component), a common ADP was refined for each pair of disordered carbon atoms (EADP). All H atoms were refined using a riding model, with a common U restrained to be 1.2 times the equivalent isotropic displacement parameter of the parent atom. Methyl groups were treated as rigid bodies and allowed to rotate about the E-CH3 bond. 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^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(3) _refine_ls_number_reflns 25554 _refine_ls_number_parameters 1396 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.002 _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 C1 C 0.3041(4) 0.29971(12) 0.22723(17) 0.0151(8) Uani 1 1 d . . . C2 C 0.3743(4) 0.33279(12) 0.26931(18) 0.0156(9) Uani 1 1 d . . . C3 C 0.3155(4) 0.35165(12) 0.32859(18) 0.0193(9) Uani 1 1 d . B . H3 H 0.2277 0.3412 0.3418 0.023 Uiso 1 1 calc R . . C4 C 0.3809(4) 0.38459(12) 0.36780(19) 0.0222(10) Uani 1 1 d . B . H4 H 0.3361 0.3961 0.4069 0.027 Uiso 1 1 calc R . . C5 C 0.5082(4) 0.40148(14) 0.3527(2) 0.0238(11) Uani 1 1 d . . . H5 H 0.5515 0.4246 0.3796 0.029 Uiso 1 1 calc R . . C6 C 0.5701(4) 0.38270(12) 0.29563(19) 0.0201(9) Uani 1 1 d . . . H6 H 0.6595 0.3927 0.2842 0.024 Uiso 1 1 calc R . . C7 C 0.5064(4) 0.35029(13) 0.2554(2) 0.0182(9) Uani 1 1 d . . . H7 H 0.5527 0.3391 0.2165 0.022 Uiso 1 1 calc R . . C8 C 0.3761(4) 0.26998(11) 0.17931(18) 0.0139(8) Uani 1 1 d . . . C9 C 0.5085(4) 0.25300(13) 0.19338(19) 0.0167(9) Uani 1 1 d . . . H9 H 0.5522 0.2612 0.2348 0.020 Uiso 1 1 calc R . . C10 C 0.5758(4) 0.22466(12) 0.14798(19) 0.0210(9) Uani 1 1 d . . . H10 H 0.6655 0.2143 0.1585 0.025 Uiso 1 1 calc R . . C11 C 0.5155(4) 0.21111(13) 0.0875(2) 0.0219(10) Uani 1 1 d . . . H11 H 0.5621 0.1915 0.0566 0.026 Uiso 1 1 calc R . . C12 C 0.3855(4) 0.22696(12) 0.07347(19) 0.0172(9) Uani 1 1 d . . . H12 H 0.3422 0.2180 0.0323 0.021 Uiso 1 1 calc R . . C13 C 0.3171(4) 0.25539(11) 0.11750(17) 0.0170(9) Uani 1 1 d . . . H13 H 0.2276 0.2655 0.1060 0.020 Uiso 1 1 calc R . . C14 C 0.1551(4) 0.29597(13) 0.22927(18) 0.0145(9) Uani 1 1 d . . . C15 C 0.0886(4) 0.25293(13) 0.22163(19) 0.0190(9) Uani 1 1 d . . . H15 H 0.1426 0.2258 0.2159 0.023 Uiso 1 1 calc R . . C16 C -0.0486(4) 0.24851(13) 0.22210(19) 0.0205(10) Uani 1 1 d . . . H16 H -0.0880 0.2187 0.2155 0.025 Uiso 1 1 calc R . . C17 C -0.1330(4) 0.28644(13) 0.2320(2) 0.0234(10) Uani 1 1 d . . . H17 H -0.2294 0.2831 0.2325 0.028 Uiso 1 1 calc R . . C18 C -0.0717(4) 0.32963(14) 0.24109(19) 0.0204(10) Uani 1 1 d . . . H18 H -0.1267 0.3563 0.2490 0.025 Uiso 1 1 calc R . . C19 C 0.0678(4) 0.33411(14) 0.23878(19) 0.0174(10) Uani 1 1 d . . . H19 H 0.1068 0.3642 0.2438 0.021 Uiso 1 1 calc R . . C20 C 0.8156(4) 0.30169(13) 0.40499(18) 0.0252(9) Uani 1 1 d . . . H20A H 0.9162 0.3046 0.4065 0.030 Uiso 1 1 calc R . . H20B H 0.7803 0.3212 0.3674 0.030 Uiso 1 1 calc R . . C21 C 0.7764(4) 0.25238(13) 0.3939(2) 0.0264(10) Uani 1 1 d . . . H21A H 0.8288 0.2393 0.3557 0.032 Uiso 1 1 calc R . . H21B H 0.7973 0.2339 0.4350 0.032 Uiso 1 1 calc R . . C22 C 0.5884(5) 0.20399(15) 0.3680(2) 0.0361(12) Uani 1 1 d . . . H22A H 0.6074 0.1849 0.4088 0.043 Uiso 1 1 calc R . . H22B H 0.6382 0.1902 0.3294 0.043 Uiso 1 1 calc R . . C23 C 0.4406(5) 0.20415(15) 0.3533(2) 0.0375(13) Uani 1 1 d . . . H23A H 0.4209 0.2253 0.3149 0.045 Uiso 1 1 calc R . . H23B H 0.4105 0.1725 0.3404 0.045 Uiso 1 1 calc R . . C24 C 0.2253(4) 0.22084(15) 0.3986(2) 0.0362(12) Uani 1 1 d . . . H24A H 0.1915 0.1898 0.3848 0.043 Uiso 1 1 calc R . . H24B H 0.2053 0.2431 0.3615 0.043 Uiso 1 1 calc R . . C25 C 0.1574(4) 0.23582(15) 0.4612(2) 0.0445(12) Uani 1 1 d . . . H25A H 0.0574 0.2320 0.4563 0.053 Uiso 1 1 calc R . . H25B H 0.1887 0.2164 0.4996 0.053 Uiso 1 1 calc R . . C26 C 0.1312(4) 0.2998(2) 0.5346(2) 0.0559(15) Uani 1 1 d . B . H26A H 0.1666 0.2816 0.5735 0.067 Uiso 1 1 calc R . . H26B H 0.0308 0.2959 0.5328 0.067 Uiso 1 1 calc R . . C27 C 0.1646(4) 0.3494(2) 0.5444(3) 0.0572(16) Uani 1 1 d . . . H27A H 0.1549 0.3678 0.5022 0.069 Uiso 1 1 calc R A 1 H27B H 0.1117 0.3640 0.5813 0.069 Uiso 1 1 calc R A 1 O5 O 0.3058(5) 0.3413(2) 0.5631(3) 0.0187(17) Uani 0.504(6) 1 d P B 1 C28 C 0.3500(8) 0.3870(3) 0.5836(5) 0.0201(15) Uani 0.504(6) 1 d P B 1 H28A H 0.3005 0.3969 0.6247 0.024 Uiso 0.504(6) 1 calc PR B 1 H28B H 0.3314 0.4098 0.5471 0.024 Uiso 0.504(6) 1 calc PR B 1 O5D O 0.3115(5) 0.3698(2) 0.5380(3) 0.0164(16) Uani 0.496(6) 1 d P B 2 C28D C 0.3785(9) 0.3591(3) 0.5997(4) 0.0201(15) Uani 0.496(6) 1 d P B 2 H28I H 0.3953 0.3252 0.6031 0.024 Uiso 0.496(6) 1 calc PR B 2 H28J H 0.3226 0.3689 0.6387 0.024 Uiso 0.496(6) 1 calc PR B 2 C29 C 0.5072(4) 0.38443(15) 0.5987(2) 0.0294(11) Uani 1 1 d . . . H29A H 0.5398 0.4147 0.6162 0.035 Uiso 0.504(6) 1 calc PR B 1 H29B H 0.5256 0.3605 0.6336 0.035 Uiso 0.504(6) 1 calc PR B 1 H29I H 0.4898 0.4183 0.6006 0.035 Uiso 0.496(6) 1 d PR B 2 H29J H 0.5633 0.3757 0.6386 0.035 Uiso 0.496(6) 1 d PR B 2 C30 C 0.7195(4) 0.37829(13) 0.5444(2) 0.0283(10) Uani 1 1 d . . . H30A H 0.7542 0.3585 0.5818 0.034 Uiso 1 1 calc R B . H30B H 0.7419 0.4110 0.5552 0.034 Uiso 1 1 calc R . . C31 C 0.7852(4) 0.36466(12) 0.47984(19) 0.0266(10) Uani 1 1 d . B . H31A H 0.7480 0.3836 0.4422 0.032 Uiso 1 1 calc R . . H31B H 0.8847 0.3702 0.4829 0.032 Uiso 1 1 calc R . . K1 K 0.47005(9) 0.30357(3) 0.46063(5) 0.0283(2) Uani 1 1 d . . . O1 O 0.7595(3) 0.31656(8) 0.46716(12) 0.0233(7) Uani 1 1 d . B . O2 O 0.6331(3) 0.25025(8) 0.37899(13) 0.0254(7) Uani 1 1 d . B . O3 O 0.3689(3) 0.21904(9) 0.41128(13) 0.0269(7) Uani 1 1 d . B . O4 O 0.1888(3) 0.28286(10) 0.47399(13) 0.0323(8) Uani 1 1 d . B . O6 O 0.5772(3) 0.37307(10) 0.53812(13) 0.0349(8) Uani 1 1 d . B . C1A C 0.6840(4) 0.30585(11) 0.73490(18) 0.0155(8) Uani 1 1 d . . . C2A C 0.6168(4) 0.33631(12) 0.78242(18) 0.0162(9) Uani 1 1 d . . . C3A C 0.6840(4) 0.35333(12) 0.84170(18) 0.0196(9) Uani 1 1 d . . . H3A H 0.7745 0.3433 0.8513 0.024 Uiso 1 1 calc R . . C4A C 0.6222(4) 0.38383(12) 0.88557(19) 0.0217(10) Uani 1 1 d . . . H4A H 0.6709 0.3944 0.9244 0.026 Uiso 1 1 calc R . . C5A C 0.4913(4) 0.39932(13) 0.8742(2) 0.0218(10) Uani 1 1 d . . . H5A H 0.4501 0.4209 0.9043 0.026 Uiso 1 1 calc R . . C6A C 0.4211(4) 0.38292(12) 0.8185(2) 0.0214(10) Uani 1 1 d . . . H6A H 0.3292 0.3923 0.8113 0.026 Uiso 1 1 calc R . . C7A C 0.4814(4) 0.35310(12) 0.77281(19) 0.0170(9) Uani 1 1 d . . . H7A H 0.4312 0.3435 0.7339 0.020 Uiso 1 1 calc R . . C8A C 0.8326(4) 0.30458(14) 0.73277(19) 0.0185(9) Uani 1 1 d . . . C9A C 0.9153(4) 0.34442(14) 0.73937(19) 0.0179(10) Uani 1 1 d . . . H9A H 0.8729 0.3734 0.7483 0.021 Uiso 1 1 calc R . . C10A C 1.0553(5) 0.34295(15) 0.7334(2) 0.0259(11) Uani 1 1 d . . . H10A H 1.1065 0.3708 0.7379 0.031 Uiso 1 1 calc R . . C11A C 1.1219(4) 0.30196(16) 0.7212(2) 0.0275(11) Uani 1 1 d . . . H11A H 1.2184 0.3011 0.7168 0.033 Uiso 1 1 calc R . . C12A C 1.0444(4) 0.26177(15) 0.7155(2) 0.0240(10) Uani 1 1 d . . . H12A H 1.0878 0.2329 0.7069 0.029 Uiso 1 1 calc R . . C13A C 0.9046(4) 0.26360(14) 0.72232(19) 0.0199(10) Uani 1 1 d . . . H13A H 0.8548 0.2353 0.7197 0.024 Uiso 1 1 calc R . . C14A C 0.6093(4) 0.27659(11) 0.68741(18) 0.0135(8) Uani 1 1 d . B . C15A C 0.6653(4) 0.26340(11) 0.62442(18) 0.0171(9) Uani 1 1 d . . . H15A H 0.7535 0.2744 0.6128 0.021 Uiso 1 1 calc R B . C16A C 0.5961(4) 0.23505(12) 0.57918(19) 0.0209(9) Uani 1 1 d . B . H16A H 0.6382 0.2270 0.5376 0.025 Uiso 1 1 calc R . . C17A C 0.4666(4) 0.21799(13) 0.5931(2) 0.0195(10) Uani 1 1 d . . . H17A H 0.4194 0.1985 0.5619 0.023 Uiso 1 1 calc R B . C18A C 0.4096(4) 0.23056(12) 0.65392(18) 0.0191(9) Uani 1 1 d . B . H18A H 0.3207 0.2198 0.6647 0.023 Uiso 1 1 calc R . . C19A C 0.4786(4) 0.25841(12) 0.69945(19) 0.0146(9) Uani 1 1 d . . . H19A H 0.4357 0.2657 0.7411 0.018 Uiso 1 1 calc R B . C20A C 0.1637(4) 0.34908(12) 0.9623(2) 0.0294(10) Uani 1 1 d . . . H20C H 0.0627 0.3488 0.9613 0.035 Uiso 1 1 calc R . . H20D H 0.1956 0.3692 0.9250 0.035 Uiso 1 1 calc R . . C21A C 0.2127(5) 0.36818(14) 1.0287(2) 0.0333(11) Uani 1 1 d . . . H21C H 0.1745 0.3996 1.0359 0.040 Uiso 1 1 calc R . . H21D H 0.1824 0.3479 1.0662 0.040 Uiso 1 1 calc R . . C22A C 0.4117(5) 0.38570(15) 1.0904(2) 0.0309(12) Uani 1 1 d . . . H22C H 0.3877 0.3633 1.1265 0.037 Uiso 1 1 calc R . . H22D H 0.3718 0.4162 1.1023 0.037 Uiso 1 1 calc R . . C23A C 0.5625(5) 0.38993(14) 1.0862(2) 0.0324(12) Uani 1 1 d . . . H23C H 0.5860 0.4123 1.0500 0.039 Uiso 1 1 calc R . . H23D H 0.5988 0.4022 1.1296 0.039 Uiso 1 1 calc R . . C24A C 0.7675(4) 0.34936(14) 1.0727(2) 0.0312(11) Uani 1 1 d . . . H24C H 0.7997 0.3615 1.1169 0.037 Uiso 1 1 calc R . . H24D H 0.7976 0.3712 1.0370 0.037 Uiso 1 1 calc R . . C25A C 0.8279(4) 0.30315(14) 1.06061(19) 0.0295(10) Uani 1 1 d . . . H25C H 0.9284 0.3049 1.0649 0.035 Uiso 1 1 calc R . . H25D H 0.7941 0.2807 1.0947 0.035 Uiso 1 1 calc R . . C26A C 0.8426(4) 0.24303(13) 0.9814(2) 0.0302(10) Uani 1 1 d . . . H26C H 0.8117 0.2213 1.0169 0.036 Uiso 1 1 calc R . . H26D H 0.9436 0.2437 0.9820 0.036 Uiso 1 1 calc R . . C27A C 0.7917(4) 0.22740(14) 0.9135(2) 0.0319(11) Uani 1 1 d . . . H27C H 0.8152 0.2509 0.8788 0.038 Uiso 1 1 calc R . . H27D H 0.8360 0.1977 0.9011 0.038 Uiso 1 1 calc R . . C28A C 0.5928(5) 0.20723(15) 0.8514(2) 0.0294(11) Uani 1 1 d . . . H28C H 0.6355 0.1777 0.8369 0.035 Uiso 1 1 calc R . . H28D H 0.6119 0.2312 0.8167 0.035 Uiso 1 1 calc R . . C29A C 0.4444(5) 0.20085(13) 0.8578(2) 0.0300(11) Uani 1 1 d . . . H29C H 0.4065 0.1888 0.8146 0.036 Uiso 1 1 calc R . . H29D H 0.4256 0.1777 0.8937 0.036 Uiso 1 1 calc R . . C30A C 0.2371(4) 0.23941(13) 0.8776(2) 0.0264(11) Uani 1 1 d . . . H30C H 0.2117 0.2192 0.9161 0.032 Uiso 1 1 calc R . . H30D H 0.2010 0.2253 0.8354 0.032 Uiso 1 1 calc R . . C31A C 0.1774(4) 0.28641(12) 0.8869(2) 0.0280(10) Uani 1 1 d . . . H31C H 0.2127 0.3078 0.8518 0.034 Uiso 1 1 calc R . . H31D H 0.0769 0.2849 0.8821 0.034 Uiso 1 1 calc R . . K1A K 0.50616(8) 0.29949(3) 0.96607(4) 0.0200(2) Uani 1 1 d . . . O1A O 0.2133(3) 0.30332(9) 0.95276(13) 0.0233(6) Uani 1 1 d . . . O2A O 0.3566(3) 0.37028(9) 1.02757(14) 0.0238(7) Uani 1 1 d . . . O3A O 0.6236(3) 0.34684(8) 1.07242(13) 0.0238(7) Uani 1 1 d . . . O4A O 0.7905(3) 0.28788(9) 0.99376(12) 0.0264(7) Uani 1 1 d . . . O5A O 0.6489(3) 0.22135(9) 0.91523(13) 0.0264(7) Uani 1 1 d . . . O6A O 0.3805(3) 0.24325(8) 0.87411(13) 0.0239(7) Uani 1 1 d . . . C1B C 0.1836(4) 0.04185(11) 0.48269(18) 0.0162(9) Uani 1 1 d . . . C2B C 0.1181(4) 0.01093(12) 0.53061(19) 0.0165(9) Uani 1 1 d . . . C3B C 0.1855(4) -0.00808(12) 0.58726(17) 0.0165(9) Uani 1 1 d . . . H3B H 0.2772 0.0008 0.5962 0.020 Uiso 1 1 calc R . . C4B C 0.1228(4) -0.03944(12) 0.63072(19) 0.0218(10) Uani 1 1 d . . . H4B H 0.1729 -0.0518 0.6680 0.026 Uiso 1 1 calc R . . C5B C -0.0108(4) -0.05292(14) 0.6205(2) 0.0250(11) Uani 1 1 d . . . H5B H -0.0530 -0.0747 0.6498 0.030 Uiso 1 1 calc R . . C6B C -0.0812(4) -0.03391(12) 0.5667(2) 0.0227(10) Uani 1 1 d . . . H6B H -0.1739 -0.0424 0.5595 0.027 Uiso 1 1 calc R . . C7B C -0.0201(4) -0.00256(13) 0.5227(2) 0.0196(10) Uani 1 1 d . . . H7B H -0.0723 0.0101 0.4864 0.023 Uiso 1 1 calc R . . C8B C 0.1079(4) 0.07182(12) 0.43699(19) 0.0164(9) Uani 1 1 d . . . C9B C -0.0176(4) 0.09265(13) 0.4520(2) 0.0206(10) Uani 1 1 d . . . H9B H -0.0568 0.0868 0.4950 0.025 Uiso 1 1 calc R . . C10B C -0.0867(4) 0.12106(12) 0.40772(19) 0.0218(9) Uani 1 1 d . . . H10B H -0.1711 0.1344 0.4208 0.026 Uiso 1 1 calc R . . C11B C -0.0347(4) 0.13061(15) 0.3438(2) 0.0277(11) Uani 1 1 d . . . H11B H -0.0826 0.1501 0.3130 0.033 Uiso 1 1 calc R . . C12B C 0.0880(4) 0.11099(13) 0.32660(19) 0.0254(10) Uani 1 1 d . D . H12B H 0.1257 0.1172 0.2833 0.030 Uiso 1 1 calc R . . C13B C 0.1574(4) 0.08239(12) 0.37125(18) 0.0195(9) Uani 1 1 d . . . H13B H 0.2416 0.0692 0.3575 0.023 Uiso 1 1 calc R . . C14B C 0.3324(4) 0.04197(13) 0.4788(2) 0.0190(9) Uani 1 1 d . . . C15B C 0.4053(4) 0.08395(14) 0.4652(2) 0.0239(10) Uani 1 1 d . . . H15B H 0.3561 0.1123 0.4618 0.029 Uiso 1 1 calc R . . C16B C 0.5449(5) 0.08454(16) 0.4567(2) 0.0292(11) Uani 1 1 d . . . H16B H 0.5894 0.1130 0.4463 0.035 Uiso 1 1 calc R . . C17B C 0.6202(4) 0.04458(17) 0.4631(2) 0.0292(11) Uani 1 1 d . . . H17B H 0.7161 0.0453 0.4565 0.035 Uiso 1 1 calc R . . C18B C 0.5557(5) 0.00313(16) 0.4792(2) 0.0280(11) Uani 1 1 d . . . H18B H 0.6076 -0.0245 0.4851 0.034 Uiso 1 1 calc R . . C19B C 0.4150(4) 0.00229(14) 0.4865(2) 0.0225(10) Uani 1 1 d . . . H19B H 0.3725 -0.0264 0.4972 0.027 Uiso 1 1 calc R . . C20B C -0.3372(5) 0.04937(19) 0.2781(2) 0.0507(14) Uani 1 1 d . D . H20E H -0.4363 0.0556 0.2740 0.061 Uiso 1 1 calc R . . H20F H -0.3007 0.0680 0.3163 0.061 Uiso 1 1 calc R . . C21B C -0.3145(5) -0.0001(2) 0.2914(3) 0.0599(17) Uani 1 1 d . . . H21E H -0.3244 -0.0195 0.2502 0.072 Uiso 1 1 calc R C 3 H21F H -0.3731 -0.0122 0.3280 0.072 Uiso 1 1 calc R C 3 O2B O -0.1704(6) 0.0058(2) 0.3130(3) 0.023(2) Uani 0.468(8) 1 d P D 3 C22B C -0.1387(10) -0.0393(4) 0.3372(6) 0.0213(16) Uani 0.468(8) 1 d P D 3 H22E H -0.1607 -0.0629 0.3024 0.026 Uiso 0.468(8) 1 calc PR D 3 H22F H -0.1918 -0.0462 0.3785 0.026 Uiso 0.468(8) 1 calc PR D 3 O2F O -0.1774(6) -0.0237(3) 0.2904(3) 0.0269(19) Uani 0.532(8) 1 d P D 4 C22F C -0.1064(9) -0.0142(3) 0.3511(4) 0.0213(16) Uani 0.532(8) 1 d P D 4 H22L H -0.1638 -0.0228 0.3902 0.026 Uiso 0.532(8) 1 calc PR D 4 H22M H -0.0867 0.0195 0.3540 0.026 Uiso 0.532(8) 1 calc PR D 4 C23B C 0.0174(4) -0.03952(14) 0.3537(2) 0.0241(10) Uani 1 1 d . . . H23E H 0.0379 -0.0154 0.3881 0.029 Uiso 0.468(8) 1 calc PR D 3 H23F H 0.0434 -0.0701 0.3729 0.029 Uiso 0.468(8) 1 calc PR D 3 H23I H 0.0705 -0.0302 0.3943 0.029 Uiso 0.532(8) 1 d PR D 4 H23J H -0.0026 -0.0732 0.3571 0.029 Uiso 0.532(8) 1 d PR D 4 C24B C 0.2362(4) -0.03869(13) 0.3042(2) 0.0234(10) Uani 1 1 d . . . H24E H 0.2523 -0.0716 0.3168 0.028 Uiso 1 1 calc R D . H24F H 0.2713 -0.0188 0.3413 0.028 Uiso 1 1 calc R . . C25B C 0.3085(4) -0.02779(12) 0.24070(19) 0.0273(10) Uani 1 1 d . D . H25E H 0.4067 -0.0352 0.2457 0.033 Uiso 1 1 calc R . . H25F H 0.2706 -0.0466 0.2030 0.033 Uiso 1 1 calc R . . C26B C 0.3541(4) 0.03384(13) 0.16529(19) 0.0279(10) Uani 1 1 d . . . H26E H 0.3180 0.0149 0.1273 0.033 Uiso 1 1 calc R . . H26F H 0.4538 0.0288 0.1685 0.033 Uiso 1 1 calc R . . C27B C 0.3250(4) 0.08326(13) 0.1532(2) 0.0280(10) Uani 1 1 d . . . H27E H 0.3469 0.1015 0.1944 0.034 Uiso 1 1 calc R . . H27F H 0.3819 0.0949 0.1157 0.034 Uiso 1 1 calc R . . C28B C 0.1501(5) 0.13529(14) 0.1220(2) 0.0386(12) Uani 1 1 d . . . H28E H 0.2081 0.1472 0.0850 0.046 Uiso 1 1 calc R . . H28F H 0.1663 0.1547 0.1627 0.046 Uiso 1 1 calc R . . C29B C 0.0041(5) 0.13802(17) 0.1016(2) 0.0484(16) Uani 1 1 d . . . H29E H -0.0193 0.1704 0.0892 0.058 Uiso 1 1 calc R . . H29F H -0.0125 0.1180 0.0615 0.058 Uiso 1 1 calc R . . C30B C -0.2164(5) 0.11930(15) 0.1360(2) 0.0357(12) Uani 1 1 d . . . H30E H -0.2260 0.0945 0.1016 0.043 Uiso 1 1 calc R . . H30F H -0.2470 0.1490 0.1155 0.043 Uiso 1 1 calc R . . C31B C -0.3014(5) 0.10821(15) 0.1957(2) 0.0469(13) Uani 1 1 d . . . H31E H -0.2817 0.1304 0.2328 0.056 Uiso 1 1 calc R . . H31F H -0.3993 0.1107 0.1836 0.056 Uiso 1 1 calc R . . K1B K 0.00375(9) 0.03704(3) 0.21000(5) 0.0262(2) Uani 1 1 d . . . O1B O -0.2712(3) 0.06236(10) 0.21724(15) 0.0349(8) Uani 1 1 d . D . O3B O 0.0950(3) -0.03085(10) 0.29473(13) 0.0315(7) Uani 1 1 d . D . O4B O 0.2914(3) 0.02035(9) 0.22653(12) 0.0240(6) Uani 1 1 d . D . O5B O 0.1844(3) 0.08844(8) 0.13637(12) 0.0262(7) Uani 1 1 d . D . O6B O -0.0797(3) 0.12300(9) 0.15658(13) 0.0291(7) Uani 1 1 d . D . C1C C -0.1870(4) 0.04623(11) -0.02932(18) 0.0141(8) Uani 1 1 d . D . C2C C -0.1142(4) 0.01362(11) 0.01209(17) 0.0132(8) Uani 1 1 d . . . C3C C -0.1689(4) -0.00523(12) 0.07269(18) 0.0193(9) Uani 1 1 d . D . H3C H -0.2562 0.0051 0.0869 0.023 Uiso 1 1 calc R . . C4C C -0.1013(4) -0.03782(13) 0.1119(2) 0.0252(10) Uani 1 1 d . D . H4C H -0.1432 -0.0495 0.1516 0.030 Uiso 1 1 calc R . . C5C C 0.0274(4) -0.05369(13) 0.0938(2) 0.0233(10) Uani 1 1 d . D . H5C H 0.0740 -0.0762 0.1206 0.028 Uiso 1 1 calc R . . C6C C 0.0848(4) -0.03609(12) 0.03654(19) 0.0191(8) Uani 1 1 d . . . H6C H 0.1735 -0.0461 0.0240 0.023 Uiso 1 1 calc R D . C7C C 0.0169(4) -0.00408(12) -0.0038(2) 0.0189(9) Uani 1 1 d . D . H7C H 0.0600 0.0065 -0.0438 0.023 Uiso 1 1 calc R . . C8C C -0.3359(4) 0.04904(13) -0.0259(2) 0.0162(9) Uani 1 1 d . . . C9C C -0.4171(4) 0.00947(13) -0.01570(19) 0.0176(10) Uani 1 1 d . D . H9C H -0.3743 -0.0201 -0.0136 0.021 Uiso 1 1 calc R . . C10C C -0.5563(4) 0.01205(15) -0.0086(2) 0.0234(10) Uani 1 1 d . . . H10C H -0.6068 -0.0157 -0.0017 0.028 Uiso 1 1 calc R D . C11C C -0.6247(4) 0.05429(14) -0.0114(2) 0.0213(10) Uani 1 1 d . D . H11C H -0.7208 0.0561 -0.0061 0.026 Uiso 1 1 calc R . . C12C C -0.5465(4) 0.09374(14) -0.02217(19) 0.0219(10) Uani 1 1 d . . . H12C H -0.5906 0.1231 -0.0248 0.026 Uiso 1 1 calc R D . C13C C -0.4075(4) 0.09168(13) -0.02913(19) 0.0190(9) Uani 1 1 d . D . H13C H -0.3580 0.1196 -0.0363 0.023 Uiso 1 1 calc R . . C14C C -0.1190(4) 0.07653(12) -0.07773(18) 0.0163(9) Uani 1 1 d . . . C15C C -0.1832(4) 0.09175(11) -0.13812(17) 0.0185(9) Uani 1 1 d . D . H15C H -0.2747 0.0824 -0.1466 0.022 Uiso 1 1 calc R . . C16C C -0.1200(4) 0.11935(11) -0.18509(18) 0.0184(9) Uani 1 1 d . . . H16C H -0.1673 0.1281 -0.2253 0.022 Uiso 1 1 calc R D . C17C C 0.0125(4) 0.13446(13) -0.1741(2) 0.0210(10) Uani 1 1 d . . . H17C H 0.0566 0.1538 -0.2062 0.025 Uiso 1 1 calc R . . C18C C 0.0792(4) 0.12078(12) -0.1154(2) 0.0214(9) Uani 1 1 d . . . H18C H 0.1701 0.1308 -0.1070 0.026 Uiso 1 1 calc R D . C19C C 0.0150(4) 0.09291(12) -0.06921(19) 0.0182(9) Uani 1 1 d . D . H19C H 0.0638 0.0842 -0.0294 0.022 Uiso 1 1 calc R . . C20C C 0.3093(4) 0.03341(12) 0.81517(18) 0.0227(9) Uani 1 1 d . . . H20G H 0.2736 0.0567 0.8474 0.027 Uiso 1 1 calc R . . H20H H 0.4087 0.0302 0.8231 0.027 Uiso 1 1 calc R . . C21C C 0.2411(4) -0.01180(13) 0.8261(2) 0.0229(10) Uani 1 1 d . . . H21G H 0.2728 -0.0346 0.7921 0.027 Uiso 1 1 calc R . . H21H H 0.2641 -0.0238 0.8718 0.027 Uiso 1 1 calc R . . C22C C 0.0259(4) -0.04801(14) 0.8278(2) 0.0236(10) Uani 1 1 d . . . H22G H 0.0564 -0.0636 0.8700 0.028 Uiso 1 1 calc R . . H22H H 0.0462 -0.0689 0.7893 0.028 Uiso 1 1 calc R . . C23C C -0.1222(4) -0.03931(14) 0.8306(2) 0.0253(11) Uani 1 1 d . . . H23G H -0.1709 -0.0687 0.8400 0.030 Uiso 1 1 calc R . . H23H H -0.1423 -0.0172 0.8676 0.030 Uiso 1 1 calc R . . C24C C -0.3119(4) -0.01498(13) 0.7642(2) 0.0237(10) Uani 1 1 d . . . H24G H -0.3422 0.0056 0.8014 0.028 Uiso 1 1 calc R . . H24H H -0.3570 -0.0455 0.7696 0.028 Uiso 1 1 calc R . . C25C C -0.3507(4) 0.00570(12) 0.69777(19) 0.0242(9) Uani 1 1 d . . . H25G H -0.3162 -0.0140 0.6605 0.029 Uiso 1 1 calc R . . H25H H -0.4514 0.0074 0.6937 0.029 Uiso 1 1 calc R . . C26C C -0.3199(4) 0.07055(12) 0.62742(18) 0.0245(10) Uani 1 1 d . . . H26G H -0.4195 0.0743 0.6206 0.029 Uiso 1 1 calc R . . H26H H -0.2857 0.0491 0.5922 0.029 Uiso 1 1 calc R . . C27C C -0.2509(4) 0.11675(13) 0.6208(2) 0.0253(10) Uani 1 1 d . . . H27G H -0.2774 0.1316 0.5775 0.030 Uiso 1 1 calc R . . H27H H -0.2783 0.1375 0.6584 0.030 Uiso 1 1 calc R . . C28C C -0.0322(4) 0.15084(13) 0.6121(2) 0.0248(11) Uani 1 1 d . . . H28G H -0.0453 0.1724 0.6506 0.030 Uiso 1 1 calc R . . H28H H -0.0644 0.1664 0.5702 0.030 Uiso 1 1 calc R . . C29C C 0.1155(4) 0.13866(14) 0.6060(2) 0.0251(11) Uani 1 1 d . . . H29G H 0.1273 0.1149 0.5701 0.030 Uiso 1 1 calc R . . H29H H 0.1682 0.1666 0.5931 0.030 Uiso 1 1 calc R . . C30C C 0.3043(4) 0.10761(13) 0.6649(2) 0.0248(10) Uani 1 1 d . . . H30G H 0.3609 0.1344 0.6511 0.030 Uiso 1 1 calc R . . H30H H 0.3151 0.0827 0.6307 0.030 Uiso 1 1 calc R . . C31C C 0.3497(4) 0.09049(12) 0.73295(19) 0.0252(10) Uani 1 1 d . . . H31G H 0.4498 0.0859 0.7333 0.030 Uiso 1 1 calc R . . H31H H 0.3269 0.1138 0.7680 0.030 Uiso 1 1 calc R . . K1C K -0.00035(9) 0.04532(3) 0.71129(5) 0.0197(2) Uani 1 1 d . . . O1C O 0.2842(3) 0.04827(8) 0.74740(13) 0.0209(6) Uani 1 1 d . . . O2C O 0.0972(3) -0.00566(8) 0.81989(12) 0.0194(6) Uani 1 1 d . . . O3C O -0.1681(3) -0.02053(9) 0.76720(13) 0.0220(7) Uani 1 1 d . . . O4C O -0.2938(3) 0.05130(8) 0.69290(13) 0.0218(7) Uani 1 1 d . . . O5C O -0.1084(3) 0.10930(8) 0.62287(13) 0.0204(6) Uani 1 1 d . . . O6C O 0.1648(3) 0.12115(8) 0.66865(12) 0.0202(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(2) 0.0155(18) 0.013(2) -0.0020(16) -0.0003(16) -0.0023(17) C2 0.016(2) 0.0123(19) 0.019(2) 0.0008(16) -0.0034(18) 0.0070(16) C3 0.015(2) 0.022(2) 0.020(2) 0.0016(17) -0.0017(18) 0.0028(17) C4 0.028(3) 0.022(2) 0.016(2) -0.0068(18) -0.0107(19) 0.0074(19) C5 0.032(3) 0.018(2) 0.021(2) -0.0070(18) -0.017(2) 0.007(2) C6 0.019(2) 0.015(2) 0.027(2) 0.0026(18) -0.0030(19) -0.0007(16) C7 0.020(2) 0.015(2) 0.019(2) 0.0007(17) 0.0014(19) -0.0022(17) C8 0.016(2) 0.0082(18) 0.017(2) 0.0038(16) -0.0043(18) -0.0048(16) C9 0.023(2) 0.018(2) 0.009(2) -0.0043(17) 0.0009(18) -0.0035(18) C10 0.019(2) 0.0112(19) 0.033(2) 0.0015(17) -0.0037(19) 0.0042(16) C11 0.021(2) 0.019(2) 0.025(2) -0.0081(18) 0.003(2) -0.0044(18) C12 0.021(2) 0.018(2) 0.012(2) -0.0004(17) 0.0002(18) -0.0056(18) C13 0.015(2) 0.0134(19) 0.023(2) 0.0004(17) -0.0013(18) -0.0037(16) C14 0.014(2) 0.018(2) 0.012(2) 0.0016(18) -0.0029(17) -0.0020(17) C15 0.019(2) 0.024(2) 0.014(2) -0.0037(18) -0.0031(18) 0.0008(18) C16 0.024(2) 0.020(2) 0.018(2) -0.0045(18) -0.0036(19) -0.0078(18) C17 0.012(2) 0.039(3) 0.019(2) 0.003(2) 0.0013(18) -0.0063(19) C18 0.020(2) 0.023(2) 0.018(2) 0.0001(18) 0.0002(19) 0.0093(18) C19 0.019(2) 0.017(2) 0.016(2) 0.0024(18) -0.0012(18) 0.0009(17) C20 0.016(2) 0.033(2) 0.027(2) 0.0085(19) 0.0151(18) 0.0066(19) C21 0.034(3) 0.028(2) 0.017(2) 0.0034(18) 0.006(2) 0.010(2) C22 0.045(3) 0.026(2) 0.037(3) -0.006(2) 0.012(3) 0.003(2) C23 0.062(4) 0.021(2) 0.030(3) -0.005(2) -0.006(3) -0.002(2) C24 0.034(3) 0.032(2) 0.043(3) 0.001(2) -0.025(2) -0.006(2) C25 0.025(3) 0.052(3) 0.056(3) 0.026(3) -0.008(3) -0.005(2) C26 0.024(3) 0.125(5) 0.019(3) 0.011(3) 0.009(2) 0.031(3) C27 0.020(3) 0.108(5) 0.044(3) -0.040(3) -0.004(2) 0.011(3) O5 0.023(3) 0.010(3) 0.022(4) 0.002(3) 0.000(3) -0.003(2) C28 0.021(4) 0.017(4) 0.022(4) -0.002(3) 0.005(3) 0.003(3) O5D 0.012(3) 0.021(4) 0.017(4) 0.003(3) -0.004(3) -0.001(2) C28D 0.021(4) 0.017(4) 0.022(4) -0.002(3) 0.005(3) 0.003(3) C29 0.040(3) 0.031(2) 0.018(2) -0.007(2) 0.002(2) -0.004(2) C30 0.029(3) 0.023(2) 0.032(3) -0.004(2) -0.013(2) -0.0051(19) C31 0.023(2) 0.024(2) 0.033(3) 0.0038(18) -0.002(2) -0.0051(17) K1 0.0226(5) 0.0270(5) 0.0351(6) -0.0148(5) -0.0037(4) 0.0009(4) O1 0.0277(16) 0.0245(15) 0.0177(15) 0.0038(12) 0.0042(13) -0.0029(12) O2 0.0327(18) 0.0184(15) 0.0250(16) -0.0021(12) 0.0000(13) 0.0027(12) O3 0.0299(18) 0.0278(15) 0.0230(16) 0.0019(13) -0.0068(14) -0.0067(13) O4 0.0268(17) 0.047(2) 0.0235(17) 0.0068(14) 0.0044(14) 0.0023(14) O6 0.0305(18) 0.053(2) 0.0208(17) -0.0134(15) 0.0101(15) -0.0197(15) C1A 0.0101(19) 0.0152(19) 0.021(2) 0.0011(16) 0.0000(17) -0.0016(16) C2A 0.018(2) 0.0129(19) 0.018(2) 0.0029(17) 0.0033(18) -0.0052(16) C3A 0.019(2) 0.020(2) 0.020(2) 0.0048(18) -0.0010(19) -0.0025(17) C4A 0.030(3) 0.016(2) 0.019(2) 0.0052(18) 0.001(2) -0.0077(18) C5A 0.028(3) 0.015(2) 0.023(2) -0.0007(18) 0.015(2) -0.0059(18) C6A 0.020(2) 0.014(2) 0.031(3) 0.0022(19) 0.013(2) -0.0009(17) C7A 0.020(2) 0.0111(19) 0.020(2) -0.0035(16) 0.0024(18) -0.0023(16) C8A 0.015(2) 0.026(2) 0.014(2) 0.0075(18) -0.0008(18) 0.0048(18) C9A 0.013(2) 0.024(2) 0.017(2) 0.0004(18) -0.0050(18) -0.0014(17) C10A 0.025(3) 0.030(3) 0.023(3) 0.002(2) -0.003(2) -0.003(2) C11A 0.005(2) 0.053(3) 0.025(2) -0.010(2) 0.0046(18) -0.005(2) C12A 0.020(2) 0.032(2) 0.019(2) -0.005(2) 0.004(2) 0.0110(19) C13A 0.015(2) 0.028(2) 0.017(2) -0.0028(19) -0.0014(19) -0.0026(18) C14A 0.014(2) 0.0117(19) 0.015(2) 0.0054(15) 0.0009(17) 0.0040(15) C15A 0.011(2) 0.0156(19) 0.025(2) 0.0037(18) 0.0035(18) 0.0001(15) C16A 0.025(2) 0.022(2) 0.016(2) 0.0041(17) 0.0072(19) 0.0048(18) C17A 0.020(2) 0.020(2) 0.018(2) -0.0005(18) -0.0035(19) 0.0021(17) C18A 0.010(2) 0.022(2) 0.025(2) 0.0030(18) -0.0023(18) 0.0002(17) C19A 0.018(2) 0.0122(19) 0.014(2) -0.0013(15) 0.0071(18) 0.0022(16) C20A 0.022(2) 0.029(2) 0.038(3) 0.008(2) 0.008(2) 0.0099(18) C21A 0.044(3) 0.024(2) 0.032(3) 0.003(2) 0.009(2) 0.009(2) C22A 0.051(3) 0.020(2) 0.022(3) -0.0049(19) 0.012(2) -0.005(2) C23A 0.052(3) 0.020(2) 0.025(3) -0.0057(19) 0.015(2) -0.019(2) C24A 0.035(3) 0.034(3) 0.025(2) 0.006(2) -0.008(2) -0.024(2) C25A 0.021(2) 0.045(3) 0.022(2) 0.003(2) -0.0086(18) -0.014(2) C26A 0.021(2) 0.036(2) 0.034(3) 0.008(2) 0.003(2) 0.0118(19) C27A 0.027(3) 0.033(2) 0.036(3) -0.002(2) 0.001(2) 0.012(2) C28A 0.048(3) 0.021(2) 0.019(3) -0.0040(19) -0.004(2) 0.006(2) C29A 0.049(3) 0.014(2) 0.027(3) -0.0031(18) -0.001(2) 0.003(2) C30A 0.032(3) 0.023(2) 0.024(2) 0.0009(18) -0.017(2) -0.0142(19) C31A 0.021(2) 0.030(2) 0.032(3) -0.0022(19) -0.0136(19) -0.0108(18) K1A 0.0203(5) 0.0172(5) 0.0224(5) -0.0043(4) -0.0007(4) -0.0021(4) O1A 0.0239(15) 0.0220(14) 0.0241(16) 0.0059(13) -0.0056(13) 0.0035(13) O2A 0.0303(18) 0.0224(16) 0.0187(16) 0.0005(13) 0.0066(14) -0.0007(12) O3A 0.0291(18) 0.0189(15) 0.0233(16) -0.0056(12) -0.0015(13) -0.0064(12) O4A 0.0269(17) 0.0338(17) 0.0183(15) 0.0037(13) -0.0015(13) -0.0008(13) O5A 0.0318(18) 0.0258(15) 0.0217(16) 0.0011(13) 0.0022(14) 0.0063(13) O6A 0.0309(18) 0.0160(14) 0.0247(16) -0.0031(12) -0.0092(14) -0.0037(12) C1B 0.017(2) 0.013(2) 0.019(2) 0.0002(16) -0.0002(17) 0.0002(17) C2B 0.014(2) 0.015(2) 0.020(2) -0.0064(17) 0.0023(18) 0.0016(15) C3B 0.020(2) 0.017(2) 0.013(2) -0.0039(17) 0.0010(18) 0.0047(17) C4B 0.034(3) 0.016(2) 0.015(2) -0.0037(17) 0.004(2) 0.0069(18) C5B 0.035(3) 0.017(2) 0.023(3) 0.0003(19) 0.015(2) 0.004(2) C6B 0.019(2) 0.019(2) 0.031(3) -0.0065(19) 0.004(2) -0.0047(17) C7B 0.019(2) 0.018(2) 0.022(2) 0.0058(18) 0.001(2) 0.0024(18) C8B 0.016(2) 0.016(2) 0.017(2) -0.0029(17) 0.0009(18) -0.0060(17) C9B 0.021(3) 0.020(2) 0.020(2) -0.0034(18) -0.003(2) 0.0001(18) C10B 0.019(2) 0.021(2) 0.025(2) 0.0005(18) 0.0022(19) -0.0034(17) C11B 0.027(3) 0.027(3) 0.029(3) 0.006(2) -0.008(2) -0.004(2) C12B 0.034(3) 0.027(2) 0.015(2) 0.0014(19) -0.004(2) -0.010(2) C13B 0.017(2) 0.021(2) 0.020(2) -0.0066(18) 0.0028(18) -0.0038(17) C14B 0.022(2) 0.021(2) 0.014(2) 0.0052(18) -0.0016(18) -0.0005(19) C15B 0.027(3) 0.024(2) 0.021(2) 0.006(2) -0.002(2) -0.0072(19) C16B 0.034(3) 0.032(3) 0.021(3) 0.011(2) -0.001(2) -0.008(2) C17B 0.019(2) 0.058(3) 0.011(2) -0.005(2) 0.001(2) -0.008(2) C18B 0.025(3) 0.042(3) 0.017(2) -0.002(2) -0.007(2) 0.010(2) C19B 0.021(2) 0.024(2) 0.023(3) -0.0074(19) -0.002(2) 0.0001(18) C20B 0.024(3) 0.094(4) 0.034(3) -0.013(3) -0.002(2) -0.015(3) C21B 0.016(3) 0.121(5) 0.042(3) 0.037(3) 0.006(2) -0.001(3) O2B 0.020(4) 0.011(4) 0.038(4) -0.004(3) 0.008(3) 0.002(3) C22B 0.014(4) 0.027(5) 0.023(4) 0.000(4) -0.007(3) -0.003(3) O2F 0.020(3) 0.033(4) 0.028(4) 0.001(3) 0.000(3) -0.006(3) C22F 0.014(4) 0.027(5) 0.023(4) 0.000(4) -0.007(3) -0.003(3) C23B 0.035(3) 0.020(2) 0.017(2) 0.0053(18) 0.004(2) 0.0039(19) C24B 0.020(2) 0.022(2) 0.027(2) -0.0009(18) -0.0064(19) 0.0087(18) C25B 0.026(2) 0.023(2) 0.033(2) -0.0061(18) 0.002(2) 0.0046(18) C26B 0.023(2) 0.034(2) 0.026(2) -0.0086(19) 0.0071(19) -0.0083(19) C27B 0.030(3) 0.031(2) 0.022(2) 0.0025(19) 0.008(2) -0.013(2) C28B 0.046(3) 0.028(2) 0.042(3) 0.015(2) 0.017(2) 0.008(2) C29B 0.075(4) 0.036(3) 0.034(3) 0.015(2) 0.018(3) 0.014(3) C30B 0.045(3) 0.032(2) 0.030(3) -0.013(2) -0.010(2) 0.013(2) C31B 0.035(3) 0.048(3) 0.057(3) -0.027(3) -0.019(3) 0.018(2) K1B 0.0211(5) 0.0285(6) 0.0290(5) 0.0132(4) -0.0041(5) -0.0032(4) O1B 0.0282(18) 0.053(2) 0.0239(17) -0.0084(15) -0.0023(15) 0.0022(15) O3B 0.0270(18) 0.0454(18) 0.0223(17) 0.0151(14) 0.0074(14) 0.0113(14) O4B 0.0250(17) 0.0316(16) 0.0153(14) 0.0013(12) 0.0073(12) 0.0017(12) O5B 0.0349(18) 0.0193(14) 0.0246(15) 0.0032(12) 0.0053(14) -0.0019(13) O6B 0.042(2) 0.0269(16) 0.0180(16) 0.0024(13) -0.0009(14) 0.0045(14) C1C 0.015(2) 0.0138(19) 0.014(2) -0.0026(16) -0.0003(17) -0.0002(16) C2C 0.014(2) 0.0100(18) 0.015(2) -0.0043(16) 0.0042(17) -0.0052(15) C3C 0.012(2) 0.024(2) 0.022(2) -0.0024(18) -0.0021(18) -0.0040(17) C4C 0.036(3) 0.021(2) 0.018(2) 0.0029(19) 0.003(2) -0.002(2) C5C 0.022(2) 0.018(2) 0.031(3) 0.0033(19) -0.011(2) -0.0063(17) C6C 0.013(2) 0.018(2) 0.026(2) -0.0014(18) 0.0003(18) -0.0059(16) C7C 0.019(2) 0.019(2) 0.019(2) 0.0022(17) -0.0016(18) -0.0035(18) C8C 0.019(2) 0.017(2) 0.013(2) 0.0001(17) 0.0025(18) -0.0023(17) C9C 0.015(2) 0.021(2) 0.017(2) 0.0002(18) -0.0041(18) 0.0028(17) C10C 0.020(2) 0.029(2) 0.022(2) -0.0055(19) 0.0064(19) -0.0089(19) C11C 0.009(2) 0.037(3) 0.018(2) 0.0104(19) 0.0010(18) 0.0034(18) C12C 0.019(2) 0.032(2) 0.015(2) 0.0065(19) 0.0006(18) 0.0101(19) C13C 0.019(2) 0.021(2) 0.017(2) 0.0016(18) 0.0031(19) -0.0001(18) C14C 0.014(2) 0.016(2) 0.019(2) -0.0034(17) 0.0016(18) 0.0068(17) C15C 0.019(2) 0.0150(19) 0.022(2) -0.0058(17) 0.0006(18) 0.0018(16) C16C 0.033(3) 0.0131(19) 0.009(2) -0.0008(16) 0.0038(19) 0.0063(17) C17C 0.026(3) 0.016(2) 0.022(2) -0.0037(17) 0.012(2) 0.0020(18) C18C 0.012(2) 0.019(2) 0.033(3) -0.0065(19) 0.0104(19) 0.0031(16) C19C 0.016(2) 0.014(2) 0.024(2) -0.0030(17) -0.0023(18) 0.0012(17) C20C 0.021(2) 0.023(2) 0.024(2) -0.0003(18) -0.0080(18) 0.0007(17) C21C 0.029(3) 0.024(2) 0.016(2) -0.0011(17) -0.0072(19) 0.0040(18) C22C 0.032(3) 0.017(2) 0.023(2) 0.0088(17) 0.003(2) -0.0031(18) C23C 0.037(3) 0.014(2) 0.025(3) 0.0043(18) 0.002(2) -0.0005(19) C24C 0.020(2) 0.020(2) 0.031(3) 0.0013(19) 0.003(2) -0.0036(17) C25C 0.018(2) 0.022(2) 0.032(2) -0.0026(18) -0.0017(19) -0.0041(17) C26C 0.023(2) 0.026(2) 0.024(2) 0.0023(18) -0.0050(19) 0.0051(18) C27C 0.028(3) 0.026(2) 0.022(2) 0.0085(18) 0.0018(19) 0.0067(19) C28C 0.041(3) 0.0098(19) 0.024(2) 0.0096(17) -0.004(2) -0.0020(18) C29C 0.030(3) 0.019(2) 0.026(3) 0.0111(19) -0.003(2) -0.0054(18) C30C 0.024(3) 0.020(2) 0.030(3) -0.0030(18) 0.007(2) -0.0010(18) C31C 0.025(2) 0.021(2) 0.030(2) -0.0032(18) 0.0014(19) -0.0037(18) K1C 0.0191(5) 0.0172(5) 0.0229(5) 0.0037(4) 0.0009(4) -0.0009(4) O1C 0.0237(16) 0.0190(14) 0.0200(15) 0.0023(12) -0.0037(13) -0.0014(12) O2C 0.0223(16) 0.0170(14) 0.0190(15) 0.0008(11) 0.0013(12) 0.0009(12) O3C 0.0228(17) 0.0253(15) 0.0180(16) 0.0040(12) 0.0034(13) -0.0050(12) O4C 0.0252(16) 0.0224(14) 0.0179(16) 0.0026(12) 0.0004(13) -0.0035(12) O5C 0.0178(16) 0.0203(14) 0.0230(15) 0.0002(12) 0.0020(13) -0.0003(11) O6C 0.0205(16) 0.0235(14) 0.0165(15) 0.0003(12) 0.0019(12) -0.0003(12) _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 1.435(5) . ? C1 C8 1.461(5) . ? C1 C14 1.465(5) . ? C2 C3 1.416(5) . ? C2 C7 1.418(5) . ? C3 C4 1.378(5) . ? C3 K1 3.307(4) . ? C3 H3 0.9500 . ? C4 C5 1.374(5) . ? C4 K1 3.087(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(5) . ? C5 H5 0.9500 . ? C6 C7 1.373(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.410(5) . ? C8 C9 1.413(5) . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 C11 1.385(5) . ? C10 H10 0.9500 . ? C11 C12 1.379(5) . ? C11 K1A 3.494(4) 1_554 ? C11 H11 0.9500 . ? C12 C13 1.372(5) . ? C12 K1A 3.207(4) 1_554 ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.405(5) . ? C14 C15 1.407(5) . ? C15 C16 1.351(6) . ? C15 H15 0.9500 . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.392(5) . ? C17 H17 0.9500 . ? C18 C19 1.374(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 O1 1.415(4) . ? C20 C21 1.485(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O2 1.434(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O2 1.417(5) . ? C22 C23 1.475(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O3 1.413(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O3 1.428(5) . ? C24 C25 1.473(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O4 1.410(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O4 1.414(5) . ? C26 C27 1.479(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O5 1.449(7) . ? C27 O5D 1.560(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? O5 C28 1.442(11) . ? O5 K1 2.812(5) . ? C28 C29 1.568(9) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O5D C28D 1.414(12) . ? O5D K1 2.901(5) . ? C28D C29 1.457(9) . ? C28D K1 3.305(8) . ? C28D H28I 0.9900 . ? C28D H28J 0.9900 . ? C29 O6 1.422(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 H29I 0.9900 . ? C29 H29J 0.9900 . ? C30 O6 1.407(5) . ? C30 C31 1.485(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 O1 1.428(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? K1 O6 2.723(3) . ? K1 O2 2.747(3) . ? K1 O3 2.798(3) . ? K1 O4 2.835(3) . ? K1 O1 2.864(3) . ? K1 C16A 3.293(4) . ? C1A C2A 1.446(5) . ? C1A C14A 1.453(5) . ? C1A C8A 1.458(5) . ? C2A C7A 1.423(5) . ? C2A C3A 1.425(5) . ? C3A C4A 1.376(5) . ? C3A K1A 3.395(4) . ? C3A H3A 0.9500 . ? C4A C5A 1.375(5) . ? C4A K1A 3.120(4) . ? C4A H4A 0.9500 . ? C5A C6A 1.376(5) . ? C5A K1A 3.399(4) . ? C5A H5A 0.9500 . ? C6A C7A 1.381(5) . ? C6A H6A 0.9500 . ? C7A H7A 0.9500 . ? C8A C13A 1.390(5) . ? C8A C9A 1.409(5) . ? C9A C10A 1.378(6) . ? C9A H9A 0.9500 . ? C10A C11A 1.371(6) . ? C10A H10A 0.9500 . ? C11A C12A 1.388(6) . ? C11A H11A 0.9500 . ? C12A C13A 1.379(6) . ? C12A H12A 0.9500 . ? C13A H13A 0.9500 . ? C14A C19A 1.406(5) . ? C14A C15A 1.415(5) . ? C15A C16A 1.383(5) . ? C15A H15A 0.9500 . ? C16A C17A 1.391(5) . ? C16A H16A 0.9500 . ? C17A C18A 1.377(5) . ? C17A H17A 0.9500 . ? C18A C19A 1.377(5) . ? C18A H18A 0.9500 . ? C19A H19A 0.9500 . ? C20A O1A 1.417(4) . ? C20A C21A 1.497(5) . ? C20A H20C 0.9900 . ? C20A H20D 0.9900 . ? C21A O2A 1.412(5) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A O2A 1.420(5) . ? C22A C23A 1.487(6) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? C23A O3A 1.404(5) . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C24A O3A 1.412(5) . ? C24A C25A 1.475(5) . ? C24A H24C 0.9900 . ? C24A H24D 0.9900 . ? C25A O4A 1.435(4) . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C26A O4A 1.410(4) . ? C26A C27A 1.495(5) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C27A O5A 1.411(5) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C28A O5A 1.429(4) . ? C28A C29A 1.472(6) . ? C28A H28C 0.9900 . ? C28A H28D 0.9900 . ? C29A O6A 1.409(4) . ? C29A H29C 0.9900 . ? C29A H29D 0.9900 . ? C30A O6A 1.413(5) . ? C30A C31A 1.485(5) . ? C30A H30C 0.9900 . ? C30A H30D 0.9900 . ? C31A O1A 1.430(4) . ? C31A H31C 0.9900 . ? C31A H31D 0.9900 . ? K1A O6A 2.719(3) . ? K1A O3A 2.747(3) . ? K1A O2A 2.792(3) . ? K1A O5A 2.835(3) . ? K1A O4A 2.856(3) . ? K1A O1A 2.882(3) . ? K1A C12 3.207(4) 1_556 ? K1A C11 3.494(4) 1_556 ? C1B C8B 1.449(5) . ? C1B C2B 1.452(5) . ? C1B C14B 1.460(5) . ? C2B C3B 1.405(5) . ? C2B C7B 1.417(5) . ? C3B C4B 1.391(5) . ? C3B K1C 3.426(3) . ? C3B H3B 0.9500 . ? C4B C5B 1.379(6) . ? C4B K1C 3.156(4) . ? C4B H4B 0.9500 . ? C5B C6B 1.375(6) . ? C5B K1C 3.347(4) . ? C5B H5B 0.9500 . ? C6B C7B 1.392(5) . ? C6B H6B 0.9500 . ? C7B H7B 0.9500 . ? C8B C9B 1.402(5) . ? C8B C13B 1.422(5) . ? C9B C10B 1.371(5) . ? C9B H9B 0.9500 . ? C10B C11B 1.392(5) . ? C10B H10B 0.9500 . ? C11B C12B 1.373(6) . ? C11B H11B 0.9500 . ? C12B C13B 1.381(5) . ? C12B K1B 3.236(4) . ? C12B H12B 0.9500 . ? C13B H13B 0.9500 . ? C14B C19B 1.407(5) . ? C14B C15B 1.430(5) . ? C15B C16B 1.380(6) . ? C15B H15B 0.9500 . ? C16B C17B 1.372(6) . ? C16B H16B 0.9500 . ? C17B C18B 1.388(6) . ? C17B H17B 0.9500 . ? C18B C19B 1.388(6) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? C20B O1B 1.418(5) . ? C20B C21B 1.463(7) . ? C20B H20E 0.9900 . ? C20B H20F 0.9900 . ? C21B O2B 1.482(8) . ? C21B O2F 1.507(8) . ? C21B H21E 0.9900 . ? C21B H21F 0.9900 . ? O2B C22B 1.415(14) . ? O2B K1B 2.812(6) . ? C22B C23B 1.562(10) . ? C22B H22E 0.9900 . ? C22B H22F 0.9900 . ? O2F C22F 1.406(12) . ? O2F K1B 2.961(6) . ? C22F C23B 1.417(9) . ? C22F K1B 3.337(9) . ? C22F H22L 0.9900 . ? C22F H22M 0.9900 . ? C23B O3B 1.417(4) . ? C23B H23E 0.9900 . ? C23B H23F 0.9900 . ? C23B H23I 0.9900 . ? C23B H23J 0.9900 . ? C24B O3B 1.414(4) . ? C24B C25B 1.478(5) . ? C24B H24E 0.9900 . ? C24B H24F 0.9900 . ? C25B O4B 1.423(4) . ? C25B H25E 0.9900 . ? C25B H25F 0.9900 . ? C26B O4B 1.415(4) . ? C26B C27B 1.469(5) . ? C26B H26E 0.9900 . ? C26B H26F 0.9900 . ? C27B O5B 1.423(5) . ? C27B H27E 0.9900 . ? C27B H27F 0.9900 . ? C28B O5B 1.417(4) . ? C28B C29B 1.485(6) . ? C28B H28E 0.9900 . ? C28B H28F 0.9900 . ? C29B O6B 1.433(5) . ? C29B H29E 0.9900 . ? C29B H29F 0.9900 . ? C30B O6B 1.400(5) . ? C30B C31B 1.483(6) . ? C30B K1B 3.512(4) . ? C30B H30E 0.9900 . ? C30B H30F 0.9900 . ? C31B O1B 1.416(5) . ? C31B H31E 0.9900 . ? C31B H31F 0.9900 . ? K1B O3B 2.718(3) . ? K1B O5B 2.734(3) . ? K1B O1B 2.796(3) . ? K1B O6B 2.808(3) . ? K1B O4B 2.876(3) . ? K1B C4C 3.069(4) . ? K1B C3C 3.408(4) . ? K1B C5C 3.483(4) . ? C1C C2C 1.431(5) . ? C1C C14C 1.458(5) . ? C1C C8C 1.464(5) . ? C2C C7C 1.419(5) . ? C2C C3C 1.422(5) . ? C3C C4C 1.381(5) . ? C3C H3C 0.9500 . ? C4C C5C 1.390(5) . ? C4C H4C 0.9500 . ? C5C C6C 1.364(5) . ? C5C H5C 0.9500 . ? C6C C7C 1.384(5) . ? C6C H6C 0.9500 . ? C7C H7C 0.9500 . ? C8C C9C 1.404(5) . ? C8C C13C 1.414(5) . ? C9C C10C 1.374(6) . ? C9C H9C 0.9500 . ? C10C C11C 1.389(6) . ? C10C H10C 0.9500 . ? C11C C12C 1.387(5) . ? C11C H11C 0.9500 . ? C12C C13C 1.372(5) . ? C12C H12C 0.9500 . ? C13C H13C 0.9500 . ? C14C C19C 1.405(5) . ? C14C C15C 1.413(5) . ? C15C C16C 1.372(5) . ? C15C H15C 0.9500 . ? C16C C17C 1.385(5) . ? C16C K1C 3.183(3) 1_554 ? C16C H16C 0.9500 . ? C17C C18C 1.384(5) . ? C17C K1C 3.421(4) 1_554 ? C17C H17C 0.9500 . ? C18C C19C 1.370(5) . ? C18C H18C 0.9500 . ? C19C H19C 0.9500 . ? C20C O1C 1.424(4) . ? C20C C21C 1.479(5) . ? C20C H20G 0.9900 . ? C20C H20H 0.9900 . ? C21C O2C 1.426(4) . ? C21C H21G 0.9900 . ? C21C H21H 0.9900 . ? C22C O2C 1.414(4) . ? C22C C23C 1.475(6) . ? C22C H22G 0.9900 . ? C22C H22H 0.9900 . ? C23C O3C 1.432(5) . ? C23C H23G 0.9900 . ? C23C H23H 0.9900 . ? C24C O3C 1.420(5) . ? C24C C25C 1.486(5) . ? C24C H24G 0.9900 . ? C24C H24H 0.9900 . ? C25C O4C 1.429(4) . ? C25C H25G 0.9900 . ? C25C H25H 0.9900 . ? C26C O4C 1.427(4) . ? C26C C27C 1.498(5) . ? C26C H26G 0.9900 . ? C26C H26H 0.9900 . ? C27C O5C 1.413(4) . ? C27C H27G 0.9900 . ? C27C H27H 0.9900 . ? C28C O5C 1.426(4) . ? C28C C29C 1.496(6) . ? C28C H28G 0.9900 . ? C28C H28H 0.9900 . ? C29C O6C 1.417(5) . ? C29C H29G 0.9900 . ? C29C H29H 0.9900 . ? C30C O6C 1.425(5) . ? C30C C31C 1.495(5) . ? C30C H30G 0.9900 . ? C30C H30H 0.9900 . ? C31C O1C 1.404(4) . ? C31C H31G 0.9900 . ? C31C H31H 0.9900 . ? K1C O5C 2.743(3) . ? K1C O3C 2.745(3) . ? K1C O2C 2.762(3) . ? K1C O6C 2.848(3) . ? K1C O1C 2.875(3) . ? K1C O4C 2.901(3) . ? K1C C16C 3.183(3) 1_556 ? K1C C17C 3.421(4) 1_556 ? 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 C8 122.1(3) . . ? C2 C1 C14 120.4(3) . . ? C8 C1 C14 117.5(3) . . ? C3 C2 C7 113.7(3) . . ? C3 C2 C1 122.4(3) . . ? C7 C2 C1 123.9(3) . . ? C4 C3 C2 122.5(4) . . ? C4 C3 K1 68.7(2) . . ? C2 C3 K1 107.7(2) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? K1 C3 H3 93.5 . . ? C5 C4 C3 122.7(4) . . ? C5 C4 K1 98.2(2) . . ? C3 C4 K1 86.7(2) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? K1 C4 H4 84.9 . . ? C4 C5 C6 116.1(4) . . ? C4 C5 H5 121.9 . . ? C6 C5 H5 121.9 . . ? C7 C6 C5 122.2(4) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C2 122.7(4) . . ? C6 C7 H7 118.6 . . ? C2 C7 H7 118.6 . . ? C13 C8 C9 115.9(3) . . ? C13 C8 C1 122.5(3) . . ? C9 C8 C1 121.5(3) . . ? C10 C9 C8 121.2(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 121.5(4) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 117.9(4) . . ? C12 C11 K1A 66.6(2) . 1_554 ? C10 C11 K1A 113.3(2) . 1_554 ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? K1A C11 H11 90.1 1_554 . ? C13 C12 C11 121.7(4) . . ? C13 C12 K1A 102.4(2) . 1_554 ? C11 C12 K1A 90.1(2) . 1_554 ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? K1A C12 H12 77.1 1_554 . ? C12 C13 C8 121.8(4) . . ? C12 C13 H13 119.1 . . ? C8 C13 H13 119.1 . . ? C19 C14 C15 114.8(3) . . ? C19 C14 C1 123.7(3) . . ? C15 C14 C1 121.5(4) . . ? C16 C15 C14 122.8(4) . . ? C16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C15 C16 C17 121.5(4) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C18 117.6(4) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? C19 C18 C17 120.6(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C14 122.6(4) . . ? C18 C19 H19 118.7 . . ? C14 C19 H19 118.7 . . ? O1 C20 C21 108.4(3) . . ? O1 C20 H20A 110.0 . . ? C21 C20 H20A 110.0 . . ? O1 C20 H20B 110.0 . . ? C21 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? O2 C21 C20 108.8(3) . . ? O2 C21 H21A 109.9 . . ? C20 C21 H21A 109.9 . . ? O2 C21 H21B 109.9 . . ? C20 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O2 C22 C23 109.2(4) . . ? O2 C22 H22A 109.8 . . ? C23 C22 H22A 109.8 . . ? O2 C22 H22B 109.8 . . ? C23 C22 H22B 109.8 . . ? H22A C22 H22B 108.3 . . ? O3 C23 C22 109.6(4) . . ? O3 C23 H23A 109.7 . . ? C22 C23 H23A 109.7 . . ? O3 C23 H23B 109.7 . . ? C22 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? O3 C24 C25 108.3(3) . . ? O3 C24 H24A 110.0 . . ? C25 C24 H24A 110.0 . . ? O3 C24 H24B 110.0 . . ? C25 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? O4 C25 C24 109.4(3) . . ? O4 C25 H25A 109.8 . . ? C24 C25 H25A 109.8 . . ? O4 C25 H25B 109.8 . . ? C24 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? O4 C26 C27 110.7(4) . . ? O4 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? O4 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? O5 C27 C26 95.0(5) . . ? O5 C27 O5D 37.0(3) . . ? C26 C27 O5D 123.8(4) . . ? O5 C27 H27A 112.7 . . ? C26 C27 H27A 112.7 . . ? O5D C27 H27A 79.3 . . ? O5 C27 H27B 112.7 . . ? C26 C27 H27B 112.7 . . ? O5D C27 H27B 113.0 . . ? H27A C27 H27B 110.2 . . ? C28 O5 C27 102.0(6) . . ? C28 O5 K1 112.4(4) . . ? C27 O5 K1 115.5(3) . . ? O5 C28 C29 107.6(6) . . ? O5 C28 H28A 110.2 . . ? C29 C28 H28A 110.2 . . ? O5 C28 H28B 110.2 . . ? C29 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? C28D O5D C27 105.7(6) . . ? C28D O5D K1 93.5(4) . . ? C27 O5D K1 107.1(3) . . ? O5D C28D C29 106.0(7) . . ? O5D C28D K1 61.2(4) . . ? C29 C28D K1 89.5(4) . . ? O5D C28D H28I 110.5 . . ? C29 C28D H28I 110.5 . . ? K1 C28D H28I 62.4 . . ? O5D C28D H28J 110.5 . . ? C29 C28D H28J 110.5 . . ? K1 C28D H28J 160.0 . . ? H28I C28D H28J 108.7 . . ? O6 C29 C28D 108.6(4) . . ? O6 C29 C28 109.3(5) . . ? C28D C29 C28 34.6(4) . . ? O6 C29 H29A 109.8 . . ? C28D C29 H29A 135.5 . . ? C28 C29 H29A 109.8 . . ? O6 C29 H29B 109.8 . . ? C28D C29 H29B 78.2 . . ? C28 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? O6 C29 H29I 110.0 . . ? C28D C29 H29I 110.1 . . ? C28 C29 H29I 78.0 . . ? H29A C29 H29I 34.4 . . ? H29B C29 H29I 133.6 . . ? O6 C29 H29J 110.0 . . ? C28D C29 H29J 109.8 . . ? C28 C29 H29J 134.6 . . ? H29A C29 H29J 76.7 . . ? H29B C29 H29J 34.1 . . ? H29I C29 H29J 108.3 . . ? O6 C30 C31 109.4(3) . . ? O6 C30 H30A 109.8 . . ? C31 C30 H30A 109.8 . . ? O6 C30 H30B 109.8 . . ? C31 C30 H30B 109.8 . . ? H30A C30 H30B 108.2 . . ? O1 C31 C30 109.2(3) . . ? O1 C31 H31A 109.8 . . ? C30 C31 H31A 109.8 . . ? O1 C31 H31B 109.8 . . ? C30 C31 H31B 109.8 . . ? H31A C31 H31B 108.3 . . ? O6 K1 O2 121.06(9) . . ? O6 K1 O3 165.39(9) . . ? O2 K1 O3 61.10(8) . . ? O6 K1 O5 62.19(13) . . ? O2 K1 O5 167.49(15) . . ? O3 K1 O5 112.47(13) . . ? O6 K1 O4 118.25(9) . . ? O2 K1 O4 120.52(9) . . ? O3 K1 O4 60.49(8) . . ? O5 K1 O4 56.74(12) . . ? O6 K1 O1 60.08(8) . . ? O2 K1 O1 61.21(8) . . ? O3 K1 O1 118.51(8) . . ? O5 K1 O1 119.33(13) . . ? O4 K1 O1 170.81(8) . . ? O6 K1 O5D 55.11(13) . . ? O2 K1 O5D 172.85(14) . . ? O3 K1 O5D 124.35(13) . . ? O5 K1 O5D 19.29(12) . . ? O4 K1 O5D 64.13(13) . . ? O1 K1 O5D 115.17(13) . . ? O6 K1 C4 83.40(10) . . ? O2 K1 C4 103.70(9) . . ? O3 K1 C4 110.59(9) . . ? O5 K1 C4 88.54(15) . . ? O4 K1 C4 86.73(10) . . ? O1 K1 C4 101.77(10) . . ? O5D K1 C4 70.48(15) . . ? O6 K1 C16A 84.23(10) . . ? O2 K1 C16A 82.28(9) . . ? O3 K1 C16A 81.78(9) . . ? O5 K1 C16A 86.20(14) . . ? O4 K1 C16A 99.67(9) . . ? O1 K1 C16A 71.33(9) . . ? O5D K1 C16A 102.66(15) . . ? C4 K1 C16A 167.62(10) . . ? O6 K1 C28D 44.35(16) . . ? O2 K1 C28D 156.90(18) . . ? O3 K1 C28D 127.67(16) . . ? O5 K1 C28D 19.26(17) . . ? O4 K1 C28D 75.75(17) . . ? O1 K1 C28D 100.07(17) . . ? O5D K1 C28D 25.3(2) . . ? C4 K1 C28D 92.91(17) . . ? C16A K1 C28D 78.58(17) . . ? O6 K1 C3 107.92(9) . . ? O2 K1 C3 92.08(9) . . ? O3 K1 C3 86.01(9) . . ? O5 K1 C3 98.28(14) . . ? O4 K1 C3 73.83(9) . . ? O1 K1 C3 115.36(9) . . ? O5D K1 C3 84.02(14) . . ? C4 K1 C3 24.59(9) . . ? C16A K1 C3 167.79(10) . . ? C28D K1 C3 109.07(17) . . ? C20 O1 C31 112.1(3) . . ? C20 O1 K1 108.2(2) . . ? C31 O1 K1 107.9(2) . . ? C22 O2 C21 111.9(3) . . ? C22 O2 K1 115.7(2) . . ? C21 O2 K1 115.4(2) . . ? C23 O3 C24 111.4(3) . . ? C23 O3 K1 111.6(2) . . ? C24 O3 K1 112.1(2) . . ? C25 O4 C26 113.2(4) . . ? C25 O4 K1 113.3(2) . . ? C26 O4 K1 113.7(3) . . ? C30 O6 C29 112.7(3) . . ? C30 O6 K1 120.4(2) . . ? C29 O6 K1 117.0(2) . . ? C2A C1A C14A 122.6(3) . . ? C2A C1A C8A 119.6(3) . . ? C14A C1A C8A 117.7(3) . . ? C7A C2A C3A 114.7(3) . . ? C7A C2A C1A 123.3(3) . . ? C3A C2A C1A 122.0(3) . . ? C4A C3A C2A 122.2(4) . . ? C4A C3A K1A 66.75(19) . . ? C2A C3A K1A 101.5(2) . . ? C4A C3A H3A 118.9 . . ? C2A C3A H3A 118.9 . . ? K1A C3A H3A 101.6 . . ? C5A C4A C3A 121.3(4) . . ? C5A C4A K1A 89.5(2) . . ? C3A C4A K1A 89.3(2) . . ? C5A C4A H4A 119.4 . . ? C3A C4A H4A 119.4 . . ? K1A C4A H4A 91.2 . . ? C4A C5A C6A 118.6(4) . . ? C4A C5A K1A 66.6(2) . . ? C6A C5A K1A 98.9(2) . . ? C4A C5A H5A 120.7 . . ? C6A C5A H5A 120.7 . . ? K1A C5A H5A 103.7 . . ? C5A C6A C7A 121.4(4) . . ? C5A C6A H6A 119.3 . . ? C7A C6A H6A 119.3 . . ? C6A C7A C2A 121.8(4) . . ? C6A C7A H7A 119.1 . . ? C2A C7A H7A 119.1 . . ? C13A C8A C9A 114.3(3) . . ? C13A C8A C1A 122.2(4) . . ? C9A C8A C1A 123.4(4) . . ? C10A C9A C8A 122.6(4) . . ? C10A C9A H9A 118.7 . . ? C8A C9A H9A 118.7 . . ? C11A C10A C9A 121.2(4) . . ? C11A C10A H10A 119.4 . . ? C9A C10A H10A 119.4 . . ? C10A C11A C12A 118.0(4) . . ? C10A C11A H11A 121.0 . . ? C12A C11A H11A 121.0 . . ? C13A C12A C11A 120.3(4) . . ? C13A C12A H12A 119.9 . . ? C11A C12A H12A 119.9 . . ? C12A C13A C8A 123.5(4) . . ? C12A C13A H13A 118.2 . . ? C8A C13A H13A 118.2 . . ? C19A C14A C15A 114.1(3) . . ? C19A C14A C1A 124.2(3) . . ? C15A C14A C1A 121.7(3) . . ? C16A C15A C14A 122.3(3) . . ? C16A C15A H15A 118.9 . . ? C14A C15A H15A 118.9 . . ? C15A C16A C17A 121.6(3) . . ? C15A C16A K1 106.6(2) . . ? C17A C16A K1 90.8(2) . . ? C15A C16A H16A 119.2 . . ? C17A C16A H16A 119.2 . . ? K1 C16A H16A 72.2 . . ? C18A C17A C16A 117.2(4) . . ? C18A C17A H17A 121.4 . . ? C16A C17A H17A 121.4 . . ? C17A C18A C19A 121.4(4) . . ? C17A C18A H18A 119.3 . . ? C19A C18A H18A 119.3 . . ? C18A C19A C14A 123.4(3) . . ? C18A C19A H19A 118.3 . . ? C14A C19A H19A 118.3 . . ? O1A C20A C21A 110.4(3) . . ? O1A C20A H20C 109.6 . . ? C21A C20A H20C 109.6 . . ? O1A C20A H20D 109.6 . . ? C21A C20A H20D 109.6 . . ? H20C C20A H20D 108.1 . . ? O2A C21A C20A 108.4(3) . . ? O2A C21A H21C 110.0 . . ? C20A C21A H21C 110.0 . . ? O2A C21A H21D 110.0 . . ? C20A C21A H21D 110.0 . . ? H21C C21A H21D 108.4 . . ? O2A C22A C23A 110.3(4) . . ? O2A C22A H22C 109.6 . . ? C23A C22A H22C 109.6 . . ? O2A C22A H22D 109.6 . . ? C23A C22A H22D 109.6 . . ? H22C C22A H22D 108.1 . . ? O3A C23A C22A 111.4(3) . . ? O3A C23A H23C 109.4 . . ? C22A C23A H23C 109.4 . . ? O3A C23A H23D 109.4 . . ? C22A C23A H23D 109.4 . . ? H23C C23A H23D 108.0 . . ? O3A C24A C25A 110.8(3) . . ? O3A C24A H24C 109.5 . . ? C25A C24A H24C 109.5 . . ? O3A C24A H24D 109.5 . . ? C25A C24A H24D 109.5 . . ? H24C C24A H24D 108.1 . . ? O4A C25A C24A 108.9(3) . . ? O4A C25A H25C 109.9 . . ? C24A C25A H25C 109.9 . . ? O4A C25A H25D 109.9 . . ? C24A C25A H25D 109.9 . . ? H25C C25A H25D 108.3 . . ? O4A C26A C27A 108.2(3) . . ? O4A C26A H26C 110.1 . . ? C27A C26A H26C 110.1 . . ? O4A C26A H26D 110.1 . . ? C27A C26A H26D 110.1 . . ? H26C C26A H26D 108.4 . . ? O5A C27A C26A 109.8(3) . . ? O5A C27A H27C 109.7 . . ? C26A C27A H27C 109.7 . . ? O5A C27A H27D 109.7 . . ? C26A C27A H27D 109.7 . . ? H27C C27A H27D 108.2 . . ? O5A C28A C29A 109.5(4) . . ? O5A C28A H28C 109.8 . . ? C29A C28A H28C 109.8 . . ? O5A C28A H28D 109.8 . . ? C29A C28A H28D 109.8 . . ? H28C C28A H28D 108.2 . . ? O6A C29A C28A 110.6(3) . . ? O6A C29A H29C 109.5 . . ? C28A C29A H29C 109.5 . . ? O6A C29A H29D 109.5 . . ? C28A C29A H29D 109.5 . . ? H29C C29A H29D 108.1 . . ? O6A C30A C31A 109.1(3) . . ? O6A C30A H30C 109.9 . . ? C31A C30A H30C 109.9 . . ? O6A C30A H30D 109.9 . . ? C31A C30A H30D 109.9 . . ? H30C C30A H30D 108.3 . . ? O1A C31A C30A 109.1(3) . . ? O1A C31A H31C 109.9 . . ? C30A C31A H31C 109.9 . . ? O1A C31A H31D 109.9 . . ? C30A C31A H31D 109.9 . . ? H31C C31A H31D 108.3 . . ? O6A K1A O3A 171.81(9) . . ? O6A K1A O2A 119.19(9) . . ? O3A K1A O2A 61.60(9) . . ? O6A K1A O5A 60.92(8) . . ? O3A K1A O5A 117.30(8) . . ? O2A K1A O5A 173.82(8) . . ? O6A K1A O4A 119.63(8) . . ? O3A K1A O4A 60.62(8) . . ? O2A K1A O4A 121.12(9) . . ? O5A K1A O4A 59.44(8) . . ? O6A K1A O1A 61.08(8) . . ? O3A K1A O1A 117.49(8) . . ? O2A K1A O1A 59.08(8) . . ? O5A K1A O1A 119.45(8) . . ? O4A K1A O1A 172.59(8) . . ? O6A K1A C4A 106.73(9) . . ? O3A K1A C4A 81.45(9) . . ? O2A K1A C4A 81.31(9) . . ? O5A K1A C4A 104.69(9) . . ? O4A K1A C4A 80.17(10) . . ? O1A K1A C4A 106.89(10) . . ? O6A K1A C12 83.49(9) . 1_556 ? O3A K1A C12 88.40(9) . 1_556 ? O2A K1A C12 89.40(9) . 1_556 ? O5A K1A C12 84.47(9) . 1_556 ? O4A K1A C12 99.31(9) . 1_556 ? O1A K1A C12 73.32(9) . 1_556 ? C4A K1A C12 168.64(10) . 1_556 ? O6A K1A C3A 91.22(8) . . ? O3A K1A C3A 96.42(9) . . ? O2A K1A C3A 104.82(9) . . ? O5A K1A C3A 81.28(8) . . ? O4A K1A C3A 71.70(9) . . ? O1A K1A C3A 115.67(9) . . ? C4A K1A C3A 23.91(9) . . ? C12 K1A C3A 165.62(10) 1_556 . ? O6A K1A C5A 97.45(9) . . ? O3A K1A C5A 90.25(9) . . ? O2A K1A C5A 66.11(9) . . ? O5A K1A C5A 120.04(9) . . ? O4A K1A C5A 103.81(9) . . ? O1A K1A C5A 83.14(9) . . ? C4A K1A C5A 23.86(9) . . ? C12 K1A C5A 152.60(10) 1_556 . ? C3A K1A C5A 41.33(9) . . ? O6A K1A C11 91.94(9) . 1_556 ? O3A K1A C11 80.12(9) . 1_556 ? O2A K1A C11 104.10(9) . 1_556 ? O5A K1A C11 69.84(9) . 1_556 ? O4A K1A C11 76.32(9) . 1_556 ? O1A K1A C11 96.37(9) . 1_556 ? C4A K1A C11 155.15(11) . 1_556 ? C12 K1A C11 23.24(9) 1_556 1_556 ? C3A K1A C11 144.77(10) . 1_556 ? C5A K1A C11 168.91(10) . 1_556 ? C20A O1A C31A 110.8(3) . . ? C20A O1A K1A 111.5(2) . . ? C31A O1A K1A 107.9(2) . . ? C21A O2A C22A 111.8(3) . . ? C21A O2A K1A 120.2(2) . . ? C22A O2A K1A 114.3(2) . . ? C23A O3A C24A 112.4(3) . . ? C23A O3A K1A 114.1(2) . . ? C24A O3A K1A 116.1(2) . . ? C26A O4A C25A 110.4(3) . . ? C26A O4A K1A 115.4(2) . . ? C25A O4A K1A 112.4(2) . . ? C27A O5A C28A 112.9(3) . . ? C27A O5A K1A 113.8(2) . . ? C28A O5A K1A 110.5(2) . . ? C29A O6A C30A 112.8(3) . . ? C29A O6A K1A 117.9(2) . . ? C30A O6A K1A 117.4(2) . . ? C8B C1B C2B 122.9(3) . . ? C8B C1B C14B 118.3(3) . . ? C2B C1B C14B 118.8(3) . . ? C3B C2B C7B 115.1(3) . . ? C3B C2B C1B 123.3(3) . . ? C7B C2B C1B 121.5(4) . . ? C4B C3B C2B 122.4(4) . . ? C4B C3B K1C 67.07(19) . . ? C2B C3B K1C 98.3(2) . . ? C4B C3B H3B 118.8 . . ? C2B C3B H3B 118.8 . . ? K1C C3B H3B 104.7 . . ? C5B C4B C3B 121.0(4) . . ? C5B C4B K1C 85.7(2) . . ? C3B C4B K1C 88.97(19) . . ? C5B C4B H4B 119.5 . . ? C3B C4B H4B 119.5 . . ? K1C C4B H4B 95.5 . . ? C6B C5B C4B 118.1(4) . . ? C6B C5B K1C 95.2(2) . . ? C4B C5B K1C 70.1(2) . . ? C6B C5B H5B 120.9 . . ? C4B C5B H5B 120.9 . . ? K1C C5B H5B 104.1 . . ? C5B C6B C7B 121.6(4) . . ? C5B C6B H6B 119.2 . . ? C7B C6B H6B 119.2 . . ? C6B C7B C2B 121.6(4) . . ? C6B C7B H7B 119.2 . . ? C2B C7B H7B 119.2 . . ? C9B C8B C13B 114.1(4) . . ? C9B C8B C1B 124.7(3) . . ? C13B C8B C1B 121.2(3) . . ? C10B C9B C8B 123.4(4) . . ? C10B C9B H9B 118.3 . . ? C8B C9B H9B 118.3 . . ? C9B C10B C11B 120.8(4) . . ? C9B C10B H10B 119.6 . . ? C11B C10B H10B 119.6 . . ? C12B C11B C10B 118.1(4) . . ? C12B C11B H11B 121.0 . . ? C10B C11B H11B 121.0 . . ? C11B C12B C13B 121.0(4) . . ? C11B C12B K1B 103.1(3) . . ? C13B C12B K1B 100.6(2) . . ? C11B C12B H12B 119.5 . . ? C13B C12B H12B 119.5 . . ? K1B C12B H12B 65.3 . . ? C12B C13B C8B 122.7(4) . . ? C12B C13B H13B 118.7 . . ? C8B C13B H13B 118.7 . . ? C19B C14B C15B 114.7(4) . . ? C19B C14B C1B 124.5(3) . . ? C15B C14B C1B 120.8(3) . . ? C16B C15B C14B 122.1(4) . . ? C16B C15B H15B 119.0 . . ? C14B C15B H15B 119.0 . . ? C17B C16B C15B 120.8(4) . . ? C17B C16B H16B 119.6 . . ? C15B C16B H16B 119.6 . . ? C16B C17B C18B 119.7(4) . . ? C16B C17B H17B 120.2 . . ? C18B C17B H17B 120.2 . . ? C17B C18B C19B 119.6(4) . . ? C17B C18B H18B 120.2 . . ? C19B C18B H18B 120.2 . . ? C18B C19B C14B 123.1(4) . . ? C18B C19B H19B 118.4 . . ? C14B C19B H19B 118.4 . . ? O1B C20B C21B 109.8(4) . . ? O1B C20B H20E 109.7 . . ? C21B C20B H20E 109.7 . . ? O1B C20B H20F 109.7 . . ? C21B C20B H20F 109.7 . . ? H20E C20B H20F 108.2 . . ? C20B C21B O2B 94.8(5) . . ? C20B C21B O2F 124.8(5) . . ? O2B C21B O2F 37.4(3) . . ? C20B C21B H21E 112.8 . . ? O2B C21B H21E 112.8 . . ? O2F C21B H21E 79.5 . . ? C20B C21B H21F 112.8 . . ? O2B C21B H21F 112.8 . . ? O2F C21B H21F 111.8 . . ? H21E C21B H21F 110.2 . . ? C22B O2B C21B 101.5(7) . . ? C22B O2B K1B 113.8(5) . . ? C21B O2B K1B 114.3(4) . . ? O2B C22B C23B 106.7(8) . . ? O2B C22B H22E 110.4 . . ? C23B C22B H22E 110.4 . . ? O2B C22B H22F 110.4 . . ? C23B C22B H22F 110.4 . . ? H22E C22B H22F 108.6 . . ? C22F O2F C21B 109.7(7) . . ? C22F O2F K1B 92.7(5) . . ? C21B O2F K1B 106.2(4) . . ? O2F C22F C23B 110.4(7) . . ? O2F C22F K1B 62.4(4) . . ? C23B C22F K1B 88.6(4) . . ? O2F C22F H22L 109.6 . . ? C23B C22F H22L 109.6 . . ? K1B C22F H22L 161.9 . . ? O2F C22F H22M 109.6 . . ? C23B C22F H22M 109.6 . . ? K1B C22F H22M 63.4 . . ? H22L C22F H22M 108.1 . . ? C22F C23B O3B 110.2(5) . . ? C22F C23B C22B 32.0(4) . . ? O3B C23B C22B 111.1(5) . . ? C22F C23B H23E 80.4 . . ? O3B C23B H23E 109.4 . . ? C22B C23B H23E 109.4 . . ? C22F C23B H23F 133.5 . . ? O3B C23B H23F 109.4 . . ? C22B C23B H23F 109.4 . . ? H23E C23B H23F 108.0 . . ? C22F C23B H23I 109.6 . . ? O3B C23B H23I 109.6 . . ? C22B C23B H23I 132.5 . . ? H23E C23B H23I 32.0 . . ? H23F C23B H23I 78.3 . . ? C22F C23B H23J 109.6 . . ? O3B C23B H23J 109.6 . . ? C22B C23B H23J 79.9 . . ? H23E C23B H23J 132.6 . . ? H23F C23B H23J 32.4 . . ? H23I C23B H23J 108.1 . . ? O3B C24B C25B 109.2(3) . . ? O3B C24B H24E 109.8 . . ? C25B C24B H24E 109.8 . . ? O3B C24B H24F 109.8 . . ? C25B C24B H24F 109.8 . . ? H24E C24B H24F 108.3 . . ? O4B C25B C24B 108.5(3) . . ? O4B C25B H25E 110.0 . . ? C24B C25B H25E 110.0 . . ? O4B C25B H25F 110.0 . . ? C24B C25B H25F 110.0 . . ? H25E C25B H25F 108.4 . . ? O4B C26B C27B 108.6(3) . . ? O4B C26B H26E 110.0 . . ? C27B C26B H26E 110.0 . . ? O4B C26B H26F 110.0 . . ? C27B C26B H26F 110.0 . . ? H26E C26B H26F 108.4 . . ? O5B C27B C26B 109.0(3) . . ? O5B C27B H27E 109.9 . . ? C26B C27B H27E 109.9 . . ? O5B C27B H27F 109.9 . . ? C26B C27B H27F 109.9 . . ? H27E C27B H27F 108.3 . . ? O5B C28B C29B 109.4(4) . . ? O5B C28B H28E 109.8 . . ? C29B C28B H28E 109.8 . . ? O5B C28B H28F 109.8 . . ? C29B C28B H28F 109.8 . . ? H28E C28B H28F 108.3 . . ? O6B C29B C28B 109.6(4) . . ? O6B C29B H29E 109.8 . . ? C28B C29B H29E 109.8 . . ? O6B C29B H29F 109.8 . . ? C28B C29B H29F 109.8 . . ? H29E C29B H29F 108.2 . . ? O6B C30B C31B 109.2(4) . . ? O6B C30B K1B 49.31(18) . . ? C31B C30B K1B 82.7(2) . . ? O6B C30B H30E 109.8 . . ? C31B C30B H30E 109.8 . . ? K1B C30B H30E 81.6 . . ? O6B C30B H30F 109.8 . . ? C31B C30B H30F 109.8 . . ? K1B C30B H30F 159.1 . . ? H30E C30B H30F 108.3 . . ? O1B C31B C30B 108.7(3) . . ? O1B C31B H31E 109.9 . . ? C30B C31B H31E 109.9 . . ? O1B C31B H31F 109.9 . . ? C30B C31B H31F 109.9 . . ? H31E C31B H31F 108.3 . . ? O3B K1B O5B 120.29(9) . . ? O3B K1B O1B 117.92(9) . . ? O5B K1B O1B 120.98(9) . . ? O3B K1B O6B 163.23(9) . . ? O5B K1B O6B 60.79(8) . . ? O1B K1B O6B 60.77(9) . . ? O3B K1B O2B 61.59(14) . . ? O5B K1B O2B 163.04(17) . . ? O1B K1B O2B 57.02(14) . . ? O6B K1B O2B 112.10(15) . . ? O3B K1B O4B 59.52(8) . . ? O5B K1B O4B 60.80(8) . . ? O1B K1B O4B 169.10(9) . . ? O6B K1B O4B 118.17(9) . . ? O2B K1B O4B 117.69(14) . . ? O3B K1B O2F 56.07(13) . . ? O5B K1B O2F 176.05(15) . . ? O1B K1B O2F 62.88(14) . . ? O6B K1B O2F 123.15(14) . . ? O2B K1B O2F 18.90(13) . . ? O4B K1B O2F 115.59(13) . . ? O3B K1B C4C 89.50(10) . . ? O5B K1B C4C 105.05(10) . . ? O1B K1B C4C 84.05(10) . . ? O6B K1B C4C 106.61(10) . . ? O2B K1B C4C 91.67(18) . . ? O4B K1B C4C 106.16(10) . . ? O2F K1B C4C 74.02(16) . . ? O3B K1B C12B 87.36(9) . . ? O5B K1B C12B 81.93(9) . . ? O1B K1B C12B 91.89(10) . . ? O6B K1B C12B 76.11(9) . . ? O2B K1B C12B 81.33(17) . . ? O4B K1B C12B 77.56(9) . . ? O2F K1B C12B 99.05(16) . . ? C4C K1B C12B 172.99(11) . . ? O3B K1B C22F 43.65(16) . . ? O5B K1B C22F 153.83(17) . . ? O1B K1B C22F 75.76(16) . . ? O6B K1B C22F 127.37(16) . . ? O2B K1B C22F 18.84(17) . . ? O4B K1B C22F 98.91(16) . . ? O2F K1B C22F 24.9(2) . . ? C4C K1B C22F 96.17(18) . . ? C12B K1B C22F 77.26(18) . . ? O3B K1B C3C 113.07(9) . . ? O5B K1B C3C 95.16(8) . . ? O1B K1B C3C 70.17(9) . . ? O6B K1B C3C 82.78(9) . . ? O2B K1B C3C 99.21(17) . . ? O4B K1B C3C 120.73(9) . . ? O2F K1B C3C 85.40(15) . . ? C4C K1B C3C 23.90(9) . . ? C12B K1B C3C 157.27(10) . . ? C22F K1B C3C 110.12(17) . . ? O3B K1B C5C 80.98(9) . . ? O5B K1B C5C 90.51(9) . . ? O1B K1B C5C 107.33(9) . . ? O6B K1B C5C 115.70(9) . . ? O2B K1B C5C 106.25(17) . . ? O4B K1B C5C 83.08(9) . . ? O2F K1B C5C 87.36(16) . . ? C4C K1B C5C 23.42(10) . . ? C12B K1B C5C 160.53(11) . . ? C22F K1B C5C 104.00(17) . . ? C3C K1B C5C 40.92(9) . . ? C31B O1B C20B 113.8(4) . . ? C31B O1B K1B 115.2(3) . . ? C20B O1B K1B 114.9(3) . . ? C24B O3B C23B 113.2(3) . . ? C24B O3B K1B 120.9(2) . . ? C23B O3B K1B 117.1(2) . . ? C26B O4B C25B 112.6(3) . . ? C26B O4B K1B 106.8(2) . . ? C25B O4B K1B 107.4(2) . . ? C28B O5B C27B 112.0(3) . . ? C28B O5B K1B 117.8(2) . . ? C27B O5B K1B 116.7(2) . . ? C30B O6B C29B 110.9(3) . . ? C30B O6B K1B 108.5(2) . . ? C29B O6B K1B 112.5(2) . . ? C2C C1C C14C 122.5(3) . . ? C2C C1C C8C 120.2(3) . . ? C14C C1C C8C 117.3(3) . . ? C7C C2C C3C 113.4(3) . . ? C7C C2C C1C 123.9(3) . . ? C3C C2C C1C 122.7(3) . . ? C4C C3C C2C 123.2(4) . . ? C4C C3C K1B 64.1(2) . . ? C2C C3C K1B 110.1(2) . . ? C4C C3C H3C 118.4 . . ? C2C C3C H3C 118.4 . . ? K1B C3C H3C 95.5 . . ? C3C C4C C5C 120.8(4) . . ? C3C C4C K1B 92.0(2) . . ? C5C C4C K1B 95.3(2) . . ? C3C C4C H4C 119.6 . . ? C5C C4C H4C 119.6 . . ? K1B C4C H4C 82.7 . . ? C6C C5C C4C 118.1(4) . . ? C6C C5C K1B 107.3(2) . . ? C4C C5C K1B 61.3(2) . . ? C6C C5C H5C 120.9 . . ? C4C C5C H5C 120.9 . . ? K1B C5C H5C 100.2 . . ? C5C C6C C7C 121.6(4) . . ? C5C C6C H6C 119.2 . . ? C7C C6C H6C 119.2 . . ? C6C C7C C2C 123.0(3) . . ? C6C C7C H7C 118.5 . . ? C2C C7C H7C 118.5 . . ? C9C C8C C13C 115.4(4) . . ? C9C C8C C1C 121.9(4) . . ? C13C C8C C1C 122.7(3) . . ? C10C C9C C8C 122.3(4) . . ? C10C C9C H9C 118.8 . . ? C8C C9C H9C 118.8 . . ? C9C C10C C11C 121.5(4) . . ? C9C C10C H10C 119.2 . . ? C11C C10C H10C 119.2 . . ? C12C C11C C10C 117.0(4) . . ? C12C C11C H11C 121.5 . . ? C10C C11C H11C 121.5 . . ? C13C C12C C11C 122.0(4) . . ? C13C C12C H12C 119.0 . . ? C11C C12C H12C 119.0 . . ? C12C C13C C8C 121.7(4) . . ? C12C C13C H13C 119.2 . . ? C8C C13C H13C 119.2 . . ? C19C C14C C15C 114.0(3) . . ? C19C C14C C1C 123.6(3) . . ? C15C C14C C1C 122.4(3) . . ? C16C C15C C14C 123.3(4) . . ? C16C C15C H15C 118.3 . . ? C14C C15C H15C 118.3 . . ? C15C C16C C17C 120.2(4) . . ? C15C C16C K1C 102.6(2) . 1_554 ? C17C C16C K1C 87.8(2) . 1_554 ? C15C C16C H16C 119.9 . . ? C17C C16C H16C 119.9 . . ? K1C C16C H16C 79.7 1_554 . ? C18C C17C C16C 118.6(4) . . ? C18C C17C K1C 110.8(2) . 1_554 ? C16C C17C K1C 68.4(2) . 1_554 ? C18C C17C H17C 120.7 . . ? C16C C17C H17C 120.7 . . ? K1C C17C H17C 90.7 1_554 . ? C19C C18C C17C 120.5(4) . . ? C19C C18C H18C 119.8 . . ? C17C C18C H18C 119.8 . . ? C18C C19C C14C 123.4(4) . . ? C18C C19C H19C 118.3 . . ? C14C C19C H19C 118.3 . . ? O1C C20C C21C 109.0(3) . . ? O1C C20C H20G 109.9 . . ? C21C C20C H20G 109.9 . . ? O1C C20C H20H 109.9 . . ? C21C C20C H20H 109.9 . . ? H20G C20C H20H 108.3 . . ? O2C C21C C20C 109.1(3) . . ? O2C C21C H21G 109.9 . . ? C20C C21C H21G 109.9 . . ? O2C C21C H21H 109.9 . . ? C20C C21C H21H 109.9 . . ? H21G C21C H21H 108.3 . . ? O2C C22C C23C 110.2(3) . . ? O2C C22C H22G 109.6 . . ? C23C C22C H22G 109.6 . . ? O2C C22C H22H 109.6 . . ? C23C C22C H22H 109.6 . . ? H22G C22C H22H 108.1 . . ? O3C C23C C22C 109.5(3) . . ? O3C C23C H23G 109.8 . . ? C22C C23C H23G 109.8 . . ? O3C C23C H23H 109.8 . . ? C22C C23C H23H 109.8 . . ? H23G C23C H23H 108.2 . . ? O3C C24C C25C 109.3(3) . . ? O3C C24C H24G 109.8 . . ? C25C C24C H24G 109.8 . . ? O3C C24C H24H 109.8 . . ? C25C C24C H24H 109.8 . . ? H24G C24C H24H 108.3 . . ? O4C C25C C24C 109.2(3) . . ? O4C C25C H25G 109.8 . . ? C24C C25C H25G 109.8 . . ? O4C C25C H25H 109.8 . . ? C24C C25C H25H 109.8 . . ? H25G C25C H25H 108.3 . . ? O4C C26C C27C 110.2(3) . . ? O4C C26C H26G 109.6 . . ? C27C C26C H26G 109.6 . . ? O4C C26C H26H 109.6 . . ? C27C C26C H26H 109.6 . . ? H26G C26C H26H 108.1 . . ? O5C C27C C26C 108.1(3) . . ? O5C C27C H27G 110.1 . . ? C26C C27C H27G 110.1 . . ? O5C C27C H27H 110.1 . . ? C26C C27C H27H 110.1 . . ? H27G C27C H27H 108.4 . . ? O5C C28C C29C 108.9(3) . . ? O5C C28C H28G 109.9 . . ? C29C C28C H28G 109.9 . . ? O5C C28C H28H 109.9 . . ? C29C C28C H28H 109.9 . . ? H28G C28C H28H 108.3 . . ? O6C C29C C28C 109.6(3) . . ? O6C C29C H29G 109.7 . . ? C28C C29C H29G 109.7 . . ? O6C C29C H29H 109.7 . . ? C28C C29C H29H 109.7 . . ? H29G C29C H29H 108.2 . . ? O6C C30C C31C 108.8(3) . . ? O6C C30C H30G 109.9 . . ? C31C C30C H30G 109.9 . . ? O6C C30C H30H 109.9 . . ? C31C C30C H30H 109.9 . . ? H30G C30C H30H 108.3 . . ? O1C C31C C30C 109.6(3) . . ? O1C C31C H31G 109.8 . . ? C30C C31C H31G 109.8 . . ? O1C C31C H31H 109.8 . . ? C30C C31C H31H 109.8 . . ? H31G C31C H31H 108.2 . . ? O5C K1C O3C 119.29(9) . . ? O5C K1C O2C 168.40(8) . . ? O3C K1C O2C 61.73(8) . . ? O5C K1C O6C 61.02(8) . . ? O3C K1C O6C 172.29(8) . . ? O2C K1C O6C 116.24(8) . . ? O5C K1C O1C 120.46(8) . . ? O3C K1C O1C 120.23(8) . . ? O2C K1C O1C 59.60(7) . . ? O6C K1C O1C 59.87(7) . . ? O5C K1C O4C 60.21(7) . . ? O3C K1C O4C 59.67(8) . . ? O2C K1C O4C 117.74(8) . . ? O6C K1C O4C 118.87(7) . . ? O1C K1C O4C 171.22(8) . . ? O5C K1C C4B 110.19(9) . . ? O3C K1C C4B 84.37(9) . . ? O2C K1C C4B 81.33(9) . . ? O6C K1C C4B 102.86(9) . . ? O1C K1C C4B 76.91(9) . . ? O4C K1C C4B 111.43(10) . . ? O5C K1C C16C 79.48(9) . 1_556 ? O3C K1C C16C 88.77(9) . 1_556 ? O2C K1C C16C 89.07(8) . 1_556 ? O6C K1C C16C 83.71(8) . 1_556 ? O1C K1C C16C 100.53(9) . 1_556 ? O4C K1C C16C 70.78(9) . 1_556 ? C4B K1C C16C 170.04(10) . 1_556 ? O5C K1C C5B 102.48(10) . . ? O3C K1C C5B 67.45(9) . . ? O2C K1C C5B 88.62(10) . . ? O6C K1C C5B 120.25(9) . . ? O1C K1C C5B 100.55(9) . . ? O4C K1C C5B 87.53(9) . . ? C4B K1C C5B 24.26(10) . . ? C16C K1C C5B 154.01(11) 1_556 . ? O5C K1C C17C 85.97(9) . 1_556 ? O3C K1C C17C 105.69(9) . 1_556 ? O2C K1C C17C 82.77(9) . 1_556 ? O6C K1C C17C 66.62(8) . 1_556 ? O1C K1C C17C 77.49(9) . 1_556 ? O4C K1C C17C 93.99(9) . 1_556 ? C4B K1C C17C 154.16(11) . 1_556 ? C16C K1C C17C 23.86(9) 1_556 1_556 ? C5B K1C C17C 170.95(11) . 1_556 ? O5C K1C C3B 92.93(8) . . ? O3C K1C C3B 107.52(9) . . ? O2C K1C C3B 97.68(8) . . ? O6C K1C C3B 79.97(8) . . ? O1C K1C C3B 70.74(9) . . ? O4C K1C C3B 117.98(9) . . ? C4B K1C C3B 23.95(8) . . ? C16C K1C C3B 163.67(10) 1_556 . ? C5B K1C C3B 41.69(10) . . ? C17C K1C C3B 142.32(10) 1_556 . ? C31C O1C C20C 112.0(3) . . ? C31C O1C K1C 114.8(2) . . ? C20C O1C K1C 112.6(2) . . ? C22C O2C C21C 111.9(3) . . ? C22C O2C K1C 112.0(2) . . ? C21C O2C K1C 117.9(2) . . ? C24C O3C C23C 112.6(3) . . ? C24C O3C K1C 120.2(2) . . ? C23C O3C K1C 115.3(2) . . ? C26C O4C C25C 110.5(3) . . ? C26C O4C K1C 107.9(2) . . ? C25C O4C K1C 108.9(2) . . ? C27C O5C C28C 112.8(3) . . ? C27C O5C K1C 119.8(2) . . ? C28C O5C K1C 117.2(2) . . ? C29C O6C C30C 111.9(3) . . ? C29C O6C K1C 109.9(2) . . ? C30C O6C K1C 110.7(2) . . ? 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 C8 C1 C2 C3 -160.9(3) . . . . ? C14 C1 C2 C3 21.5(5) . . . . ? C8 C1 C2 C7 20.2(5) . . . . ? C14 C1 C2 C7 -157.4(4) . . . . ? C7 C2 C3 C4 1.2(5) . . . . ? C1 C2 C3 C4 -177.8(3) . . . . ? C7 C2 C3 K1 -74.4(3) . . . . ? C1 C2 C3 K1 106.6(3) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? K1 C3 C4 C5 97.6(4) . . . . ? C2 C3 C4 K1 -98.0(3) . . . . ? C3 C4 C5 C6 -1.3(6) . . . . ? K1 C4 C5 C6 90.1(3) . . . . ? C4 C5 C6 C7 2.0(6) . . . . ? C5 C6 C7 C2 -1.2(6) . . . . ? C3 C2 C7 C6 -0.4(5) . . . . ? C1 C2 C7 C6 178.5(3) . . . . ? C2 C1 C8 C13 -147.7(3) . . . . ? C14 C1 C8 C13 29.9(5) . . . . ? C2 C1 C8 C9 34.1(5) . . . . ? C14 C1 C8 C9 -148.2(4) . . . . ? C13 C8 C9 C10 1.4(5) . . . . ? C1 C8 C9 C10 179.6(3) . . . . ? C8 C9 C10 C11 -1.1(6) . . . . ? C9 C10 C11 C12 0.3(6) . . . . ? C9 C10 C11 K1A 75.1(4) . . . 1_554 ? C10 C11 C12 C13 0.2(6) . . . . ? K1A C11 C12 C13 -104.7(3) 1_554 . . . ? C10 C11 C12 K1A 105.0(3) . . . 1_554 ? C11 C12 C13 C8 0.1(5) . . . . ? K1A C12 C13 C8 -97.9(3) 1_554 . . . ? C9 C8 C13 C12 -0.9(5) . . . . ? C1 C8 C13 C12 -179.1(3) . . . . ? C2 C1 C14 C19 35.2(5) . . . . ? C8 C1 C14 C19 -142.5(4) . . . . ? C2 C1 C14 C15 -144.8(4) . . . . ? C8 C1 C14 C15 37.5(5) . . . . ? C19 C14 C15 C16 1.2(6) . . . . ? C1 C14 C15 C16 -178.8(4) . . . . ? C14 C15 C16 C17 -1.7(7) . . . . ? C15 C16 C17 C18 0.4(6) . . . . ? C16 C17 C18 C19 1.4(6) . . . . ? C17 C18 C19 C14 -1.9(6) . . . . ? C15 C14 C19 C18 0.6(6) . . . . ? C1 C14 C19 C18 -179.4(4) . . . . ? O1 C20 C21 O2 70.7(4) . . . . ? O2 C22 C23 O3 -65.8(5) . . . . ? O3 C24 C25 O4 69.5(4) . . . . ? O4 C26 C27 O5 -73.9(5) . . . . ? O4 C26 C27 O5D -48.9(7) . . . . ? C26 C27 O5 C28 -172.5(5) . . . . ? O5D C27 O5 C28 43.2(5) . . . . ? C26 C27 O5 K1 65.3(5) . . . . ? O5D C27 O5 K1 -79.0(5) . . . . ? C27 O5 C28 C29 -174.5(5) . . . . ? K1 O5 C28 C29 -50.2(7) . . . . ? O5 C27 O5D C28D -34.9(5) . . . . ? C26 C27 O5D C28D -79.3(7) . . . . ? O5 C27 O5D K1 64.0(5) . . . . ? C26 C27 O5D K1 19.6(7) . . . . ? C27 O5D C28D C29 -170.8(5) . . . . ? K1 O5D C28D C29 80.3(5) . . . . ? C27 O5D C28D K1 108.9(5) . . . . ? O5D C28D C29 O6 -53.8(7) . . . . ? K1 C28D C29 O6 5.9(4) . . . . ? O5D C28D C29 C28 43.5(8) . . . . ? K1 C28D C29 C28 103.2(9) . . . . ? O5 C28 C29 O6 63.5(7) . . . . ? O5 C28 C29 C28D -31.5(7) . . . . ? O6 C30 C31 O1 -63.2(4) . . . . ? C28 O5 K1 O6 21.0(5) . . . . ? C27 O5 K1 O6 137.5(5) . . . . ? C28 O5 K1 O2 129.3(7) . . . . ? C27 O5 K1 O2 -114.2(7) . . . . ? C28 O5 K1 O3 -174.1(5) . . . . ? C27 O5 K1 O3 -57.6(5) . . . . ? C28 O5 K1 O4 -149.4(6) . . . . ? C27 O5 K1 O4 -32.9(4) . . . . ? C28 O5 K1 O1 40.3(6) . . . . ? C27 O5 K1 O1 156.9(4) . . . . ? C28 O5 K1 O5D -42.3(6) . . . . ? C27 O5 K1 O5D 74.2(6) . . . . ? C28 O5 K1 C4 -62.3(6) . . . . ? C27 O5 K1 C4 54.2(5) . . . . ? C28 O5 K1 C16A 106.4(6) . . . . ? C27 O5 K1 C16A -137.0(5) . . . . ? C28 O5 K1 C28D 40.8(6) . . . . ? C27 O5 K1 C28D 157.3(10) . . . . ? C28 O5 K1 C3 -85.0(6) . . . . ? C27 O5 K1 C3 31.5(5) . . . . ? C28D O5D K1 O6 -55.6(4) . . . . ? C27 O5D K1 O6 -163.2(5) . . . . ? C28D O5D K1 O2 -115.2(11) . . . . ? C27 O5D K1 O2 137.2(9) . . . . ? C28D O5D K1 O3 106.6(5) . . . . ? C27 O5D K1 O3 -1.0(5) . . . . ? C28D O5D K1 O5 50.1(5) . . . . ? C27 O5D K1 O5 -57.6(5) . . . . ? C28D O5D K1 O4 112.7(5) . . . . ? C27 O5D K1 O4 5.1(3) . . . . ? C28D O5D K1 O1 -57.1(5) . . . . ? C27 O5D K1 O1 -164.8(3) . . . . ? C28D O5D K1 C4 -151.3(5) . . . . ? C27 O5D K1 C4 101.1(4) . . . . ? C28D O5D K1 C16A 18.0(5) . . . . ? C27 O5D K1 C16A -89.6(4) . . . . ? C27 O5D K1 C28D -107.6(7) . . . . ? C28D O5D K1 C3 -172.4(5) . . . . ? C27 O5D K1 C3 80.0(4) . . . . ? C5 C4 K1 O6 61.5(3) . . . . ? C3 C4 K1 O6 -175.9(3) . . . . ? C5 C4 K1 O2 -58.9(3) . . . . ? C3 C4 K1 O2 63.7(2) . . . . ? C5 C4 K1 O3 -122.8(2) . . . . ? C3 C4 K1 O3 -0.2(3) . . . . ? C5 C4 K1 O5 123.7(3) . . . . ? C3 C4 K1 O5 -113.7(3) . . . . ? C5 C4 K1 O4 -179.5(3) . . . . ? C3 C4 K1 O4 -56.9(2) . . . . ? C5 C4 K1 O1 4.0(3) . . . . ? C3 C4 K1 O1 126.6(2) . . . . ? C5 C4 K1 O5D 116.8(3) . . . . ? C3 C4 K1 O5D -120.6(3) . . . . ? C5 C4 K1 C16A 58.8(6) . . . . ? C3 C4 K1 C16A -178.6(4) . . . . ? C5 C4 K1 C28D 104.9(3) . . . . ? C3 C4 K1 C28D -132.5(3) . . . . ? C5 C4 K1 C3 -122.6(4) . . . . ? O5D C28D K1 O6 104.5(5) . . . . ? C29 C28D K1 O6 -4.2(3) . . . . ? O5D C28D K1 O2 163.3(3) . . . . ? C29 C28D K1 O2 54.7(7) . . . . ? O5D C28D K1 O3 -92.0(5) . . . . ? C29 C28D K1 O3 159.4(3) . . . . ? O5D C28D K1 O5 -50.2(5) . . . . ? C29 C28D K1 O5 -158.8(10) . . . . ? O5D C28D K1 O4 -58.9(4) . . . . ? C29 C28D K1 O4 -167.6(4) . . . . ? O5D C28D K1 O1 129.5(4) . . . . ? C29 C28D K1 O1 20.8(4) . . . . ? C29 C28D K1 O5D -108.7(7) . . . . ? O5D C28D K1 C4 27.0(5) . . . . ? C29 C28D K1 C4 -81.7(4) . . . . ? O5D C28D K1 C16A -162.1(5) . . . . ? C29 C28D K1 C16A 89.3(4) . . . . ? O5D C28D K1 C3 8.0(5) . . . . ? C29 C28D K1 C3 -100.6(4) . . . . ? C4 C3 K1 O6 4.3(3) . . . . ? C2 C3 K1 O6 123.0(2) . . . . ? C4 C3 K1 O2 -119.4(2) . . . . ? C2 C3 K1 O2 -0.6(3) . . . . ? C4 C3 K1 O3 179.8(2) . . . . ? C2 C3 K1 O3 -61.5(3) . . . . ? C4 C3 K1 O5 67.7(3) . . . . ? C2 C3 K1 O5 -173.6(3) . . . . ? C4 C3 K1 O4 119.4(3) . . . . ? C2 C3 K1 O4 -121.9(3) . . . . ? C4 C3 K1 O1 -60.4(3) . . . . ? C2 C3 K1 O1 58.3(3) . . . . ? C4 C3 K1 O5D 54.6(3) . . . . ? C2 C3 K1 O5D 173.4(3) . . . . ? C2 C3 K1 C4 118.7(4) . . . . ? C4 C3 K1 C16A 178.5(4) . . . . ? C2 C3 K1 C16A -62.7(6) . . . . ? C4 C3 K1 C28D 51.2(3) . . . . ? C2 C3 K1 C28D 169.9(3) . . . . ? C21 C20 O1 C31 -176.4(3) . . . . ? C21 C20 O1 K1 -57.5(3) . . . . ? C30 C31 O1 C20 178.0(3) . . . . ? C30 C31 O1 K1 58.9(3) . . . . ? O6 K1 O1 C20 -150.2(2) . . . . ? O2 K1 O1 C20 24.3(2) . . . . ? O3 K1 O1 C20 46.4(2) . . . . ? O5 K1 O1 C20 -170.0(2) . . . . ? O4 K1 O1 C20 127.7(5) . . . . ? O5D K1 O1 C20 -148.8(2) . . . . ? C4 K1 O1 C20 -75.0(2) . . . . ? C16A K1 O1 C20 115.6(2) . . . . ? C28D K1 O1 C20 -170.2(3) . . . . ? C3 K1 O1 C20 -53.3(2) . . . . ? O6 K1 O1 C31 -28.7(2) . . . . ? O2 K1 O1 C31 145.8(2) . . . . ? O3 K1 O1 C31 167.9(2) . . . . ? O5 K1 O1 C31 -48.5(3) . . . . ? O4 K1 O1 C31 -110.8(5) . . . . ? O5D K1 O1 C31 -27.3(3) . . . . ? C4 K1 O1 C31 46.5(2) . . . . ? C16A K1 O1 C31 -122.9(2) . . . . ? C28D K1 O1 C31 -48.7(3) . . . . ? C3 K1 O1 C31 68.2(2) . . . . ? C23 C22 O2 C21 179.7(4) . . . . ? C23 C22 O2 K1 44.7(4) . . . . ? C20 C21 O2 C22 -179.8(3) . . . . ? C20 C21 O2 K1 -44.7(4) . . . . ? O6 K1 O2 C22 150.1(3) . . . . ? O3 K1 O2 C22 -13.2(3) . . . . ? O5 K1 O2 C22 48.6(7) . . . . ? O4 K1 O2 C22 -25.1(3) . . . . ? O1 K1 O2 C22 144.5(3) . . . . ? O5D K1 O2 C22 -154.2(10) . . . . ? C4 K1 O2 C22 -119.4(3) . . . . ? C16A K1 O2 C22 71.6(3) . . . . ? C28D K1 O2 C22 105.8(5) . . . . ? C3 K1 O2 C22 -97.5(3) . . . . ? O6 K1 O2 C21 16.7(3) . . . . ? O3 K1 O2 C21 -146.6(3) . . . . ? O5 K1 O2 C21 -84.8(6) . . . . ? O4 K1 O2 C21 -158.4(2) . . . . ? O1 K1 O2 C21 11.2(2) . . . . ? O5D K1 O2 C21 72.4(11) . . . . ? C4 K1 O2 C21 107.2(2) . . . . ? C16A K1 O2 C21 -61.7(2) . . . . ? C28D K1 O2 C21 -27.6(5) . . . . ? C3 K1 O2 C21 129.2(2) . . . . ? C22 C23 O3 C24 178.5(3) . . . . ? C22 C23 O3 K1 52.4(4) . . . . ? C25 C24 O3 C23 179.1(3) . . . . ? C25 C24 O3 K1 -55.1(4) . . . . ? O6 K1 O3 C23 -123.3(4) . . . . ? O2 K1 O3 C23 -20.7(3) . . . . ? O5 K1 O3 C23 171.2(3) . . . . ? O4 K1 O3 C23 147.5(3) . . . . ? O1 K1 O3 C23 -42.9(3) . . . . ? O5D K1 O3 C23 153.8(3) . . . . ? C4 K1 O3 C23 74.0(3) . . . . ? C16A K1 O3 C23 -106.4(3) . . . . ? C28D K1 O3 C23 -175.0(3) . . . . ? C3 K1 O3 C23 73.9(3) . . . . ? O6 K1 O3 C24 111.0(4) . . . . ? O2 K1 O3 C24 -146.4(3) . . . . ? O5 K1 O3 C24 45.5(3) . . . . ? O4 K1 O3 C24 21.9(2) . . . . ? O1 K1 O3 C24 -168.6(2) . . . . ? O5D K1 O3 C24 28.2(3) . . . . ? C4 K1 O3 C24 -51.7(3) . . . . ? C16A K1 O3 C24 127.9(3) . . . . ? C28D K1 O3 C24 59.3(3) . . . . ? C3 K1 O3 C24 -51.8(3) . . . . ? C24 C25 O4 C26 -178.1(3) . . . . ? C24 C25 O4 K1 -46.7(4) . . . . ? C27 C26 O4 C25 -178.6(4) . . . . ? C27 C26 O4 K1 50.2(4) . . . . ? O6 K1 O4 C25 -150.0(3) . . . . ? O2 K1 O4 C25 25.3(3) . . . . ? O3 K1 O4 C25 13.4(2) . . . . ? O5 K1 O4 C25 -140.3(3) . . . . ? O1 K1 O4 C25 -73.0(6) . . . . ? O5D K1 O4 C25 -160.9(3) . . . . ? C4 K1 O4 C25 129.3(3) . . . . ? C16A K1 O4 C25 -61.4(3) . . . . ? C28D K1 O4 C25 -136.9(3) . . . . ? C3 K1 O4 C25 108.0(3) . . . . ? O6 K1 O4 C26 -18.9(3) . . . . ? O2 K1 O4 C26 156.4(3) . . . . ? O3 K1 O4 C26 144.5(3) . . . . ? O5 K1 O4 C26 -9.2(3) . . . . ? O1 K1 O4 C26 58.1(6) . . . . ? O5D K1 O4 C26 -29.7(3) . . . . ? C4 K1 O4 C26 -99.6(3) . . . . ? C16A K1 O4 C26 69.7(3) . . . . ? C28D K1 O4 C26 -5.8(3) . . . . ? C3 K1 O4 C26 -120.9(3) . . . . ? C31 C30 O6 C29 178.6(3) . . . . ? C31 C30 O6 K1 33.8(4) . . . . ? C28D C29 O6 C30 -154.1(5) . . . . ? C28 C29 O6 C30 169.2(5) . . . . ? C28D C29 O6 K1 -8.1(5) . . . . ? C28 C29 O6 K1 -44.8(5) . . . . ? O2 K1 O6 C30 -8.9(3) . . . . ? O3 K1 O6 C30 85.4(4) . . . . ? O5 K1 O6 C30 157.3(3) . . . . ? O4 K1 O6 C30 166.4(3) . . . . ? O1 K1 O6 C30 -3.2(3) . . . . ? O5D K1 O6 C30 178.3(3) . . . . ? C4 K1 O6 C30 -110.9(3) . . . . ? C16A K1 O6 C30 68.5(3) . . . . ? C28D K1 O6 C30 148.1(4) . . . . ? C3 K1 O6 C30 -112.7(3) . . . . ? O2 K1 O6 C29 -152.1(3) . . . . ? O3 K1 O6 C29 -57.9(5) . . . . ? O5 K1 O6 C29 14.0(3) . . . . ? O4 K1 O6 C29 23.2(3) . . . . ? O1 K1 O6 C29 -146.5(3) . . . . ? O5D K1 O6 C29 35.1(3) . . . . ? C4 K1 O6 C29 105.8(3) . . . . ? C16A K1 O6 C29 -74.7(3) . . . . ? C28D K1 O6 C29 4.8(3) . . . . ? C3 K1 O6 C29 104.0(3) . . . . ? C14A C1A C2A C7A -22.7(5) . . . . ? C8A C1A C2A C7A 156.0(4) . . . . ? C14A C1A C2A C3A 159.8(3) . . . . ? C8A C1A C2A C3A -21.5(5) . . . . ? C7A C2A C3A C4A -0.4(5) . . . . ? C1A C2A C3A C4A 177.3(3) . . . . ? C7A C2A C3A K1A 69.2(3) . . . . ? C1A C2A C3A K1A -113.1(3) . . . . ? C2A C3A C4A C5A 0.2(5) . . . . ? K1A C3A C4A C5A -89.0(3) . . . . ? C2A C3A C4A K1A 89.3(3) . . . . ? C3A C4A C5A C6A 1.4(5) . . . . ? K1A C4A C5A C6A -87.6(3) . . . . ? C3A C4A C5A K1A 88.9(3) . . . . ? C4A C5A C6A C7A -2.8(6) . . . . ? K1A C5A C6A C7A -71.0(4) . . . . ? C5A C6A C7A C2A 2.7(6) . . . . ? C3A C2A C7A C6A -1.0(5) . . . . ? C1A C2A C7A C6A -178.7(3) . . . . ? C2A C1A C8A C13A 142.2(4) . . . . ? C14A C1A C8A C13A -39.0(5) . . . . ? C2A C1A C8A C9A -39.4(6) . . . . ? C14A C1A C8A C9A 139.4(4) . . . . ? C13A C8A C9A C10A 2.3(6) . . . . ? C1A C8A C9A C10A -176.3(4) . . . . ? C8A C9A C10A C11A -0.6(7) . . . . ? C9A C10A C11A C12A -0.5(6) . . . . ? C10A C11A C12A C13A -0.2(6) . . . . ? C11A C12A C13A C8A 2.2(7) . . . . ? C9A C8A C13A C12A -3.1(6) . . . . ? C1A C8A C13A C12A 175.5(4) . . . . ? C2A C1A C14A C19A -29.3(5) . . . . ? C8A C1A C14A C19A 151.9(4) . . . . ? C2A C1A C14A C15A 151.7(3) . . . . ? C8A C1A C14A C15A -27.0(5) . . . . ? C19A C14A C15A C16A 0.0(5) . . . . ? C1A C14A C15A C16A 179.1(3) . . . . ? C14A C15A C16A C17A 0.3(5) . . . . ? C14A C15A C16A K1 101.8(3) . . . . ? O6 K1 C16A C15A -3.4(2) . . . . ? O2 K1 C16A C15A 119.1(3) . . . . ? O3 K1 C16A C15A -179.1(3) . . . . ? O5 K1 C16A C15A -65.8(3) . . . . ? O4 K1 C16A C15A -121.1(2) . . . . ? O1 K1 C16A C15A 57.0(2) . . . . ? O5D K1 C16A C15A -55.6(3) . . . . ? C4 K1 C16A C15A -0.7(6) . . . . ? C28D K1 C16A C15A -47.9(3) . . . . ? C3 K1 C16A C15A -177.9(4) . . . . ? O6 K1 C16A C17A 120.1(2) . . . . ? O2 K1 C16A C17A -117.4(2) . . . . ? O3 K1 C16A C17A -55.7(2) . . . . ? O5 K1 C16A C17A 57.7(2) . . . . ? O4 K1 C16A C17A 2.3(2) . . . . ? O1 K1 C16A C17A -179.6(2) . . . . ? O5D K1 C16A C17A 67.8(3) . . . . ? C4 K1 C16A C17A 122.8(5) . . . . ? C28D K1 C16A C17A 75.5(3) . . . . ? C3 K1 C16A C17A -54.4(6) . . . . ? C15A C16A C17A C18A 0.1(5) . . . . ? K1 C16A C17A C18A -110.0(3) . . . . ? C16A C17A C18A C19A -0.8(5) . . . . ? C17A C18A C19A C14A 1.1(6) . . . . ? C15A C14A C19A C18A -0.7(5) . . . . ? C1A C14A C19A C18A -179.7(3) . . . . ? O1A C20A C21A O2A 62.0(4) . . . . ? O2A C22A C23A O3A -61.9(5) . . . . ? O3A C24A C25A O4A 64.4(4) . . . . ? O4A C26A C27A O5A -66.4(4) . . . . ? O5A C28A C29A O6A 63.3(4) . . . . ? O6A C30A C31A O1A -68.5(4) . . . . ? C5A C4A K1A O6A 69.8(3) . . . . ? C3A C4A K1A O6A -51.5(3) . . . . ? C5A C4A K1A O3A -110.5(2) . . . . ? C3A C4A K1A O3A 128.2(3) . . . . ? C5A C4A K1A O2A -48.2(2) . . . . ? C3A C4A K1A O2A -169.4(3) . . . . ? C5A C4A K1A O5A 133.3(2) . . . . ? C3A C4A K1A O5A 12.1(3) . . . . ? C5A C4A K1A O4A -172.0(3) . . . . ? C3A C4A K1A O4A 66.7(2) . . . . ? C5A C4A K1A O1A 5.7(3) . . . . ? C3A C4A K1A O1A -115.6(2) . . . . ? C5A C4A K1A C12 -83.6(6) . . . 1_556 ? C3A C4A K1A C12 155.1(5) . . . 1_556 ? C5A C4A K1A C3A 121.3(4) . . . . ? C3A C4A K1A C5A -121.3(4) . . . . ? C5A C4A K1A C11 -153.0(3) . . . 1_556 ? C3A C4A K1A C11 85.7(3) . . . 1_556 ? C4A C3A K1A O6A 131.5(2) . . . . ? C2A C3A K1A O6A 11.2(2) . . . . ? C4A C3A K1A O3A -51.5(3) . . . . ? C2A C3A K1A O3A -171.7(2) . . . . ? C4A C3A K1A O2A 10.8(3) . . . . ? C2A C3A K1A O2A -109.5(2) . . . . ? C4A C3A K1A O5A -168.2(3) . . . . ? C2A C3A K1A O5A 71.6(2) . . . . ? C4A C3A K1A O4A -107.6(3) . . . . ? C2A C3A K1A O4A 132.1(2) . . . . ? C4A C3A K1A O1A 73.2(3) . . . . ? C2A C3A K1A O1A -47.0(3) . . . . ? C2A C3A K1A C4A -120.2(4) . . . . ? C4A C3A K1A C12 -160.5(4) . . . 1_556 ? C2A C3A K1A C12 79.3(5) . . . 1_556 ? C4A C3A K1A C5A 31.6(2) . . . . ? C2A C3A K1A C5A -88.7(3) . . . . ? C4A C3A K1A C11 -133.4(3) . . . 1_556 ? C2A C3A K1A C11 106.3(3) . . . 1_556 ? C4A C5A K1A O6A -115.0(2) . . . . ? C6A C5A K1A O6A 2.4(3) . . . . ? C4A C5A K1A O3A 67.8(2) . . . . ? C6A C5A K1A O3A -174.8(2) . . . . ? C4A C5A K1A O2A 126.3(3) . . . . ? C6A C5A K1A O2A -116.3(3) . . . . ? C4A C5A K1A O5A -54.3(3) . . . . ? C6A C5A K1A O5A 63.0(3) . . . . ? C4A C5A K1A O4A 8.1(3) . . . . ? C6A C5A K1A O4A 125.5(2) . . . . ? C4A C5A K1A O1A -174.5(3) . . . . ? C6A C5A K1A O1A -57.1(2) . . . . ? C6A C5A K1A C4A 117.4(4) . . . . ? C4A C5A K1A C12 154.8(2) . . . 1_556 ? C6A C5A K1A C12 -87.8(3) . . . 1_556 ? C4A C5A K1A C3A -31.6(2) . . . . ? C6A C5A K1A C3A 85.7(3) . . . . ? C4A C5A K1A C11 97.4(6) . . . 1_556 ? C6A C5A K1A C11 -145.3(5) . . . 1_556 ? C21A C20A O1A C31A -174.7(3) . . . . ? C21A C20A O1A K1A -54.5(3) . . . . ? C30A C31A O1A C20A 177.2(3) . . . . ? C30A C31A O1A K1A 54.9(3) . . . . ? O6A K1A O1A C20A -144.7(2) . . . . ? O3A K1A O1A C20A 44.5(2) . . . . ? O2A K1A O1A C20A 24.0(2) . . . . ? O5A K1A O1A C20A -163.0(2) . . . . ? O4A K1A O1A C20A 117.8(7) . . . . ? C4A K1A O1A C20A -44.5(2) . . . . ? C12 K1A O1A C20A 123.6(2) 1_556 . . . ? C3A K1A O1A C20A -68.5(2) . . . . ? C5A K1A O1A C20A -42.2(2) . . . . ? C11 K1A O1A C20A 126.6(2) 1_556 . . . ? O6A K1A O1A C31A -22.8(2) . . . . ? O3A K1A O1A C31A 166.3(2) . . . . ? O2A K1A O1A C31A 145.8(2) . . . . ? O5A K1A O1A C31A -41.1(2) . . . . ? O4A K1A O1A C31A -120.4(7) . . . . ? C4A K1A O1A C31A 77.3(2) . . . . ? C12 K1A O1A C31A -114.6(2) 1_556 . . . ? C3A K1A O1A C31A 53.4(2) . . . . ? C5A K1A O1A C31A 79.6(2) . . . . ? C11 K1A O1A C31A -111.5(2) 1_556 . . . ? C20A C21A O2A C22A -176.7(3) . . . . ? C20A C21A O2A K1A -38.5(4) . . . . ? C23A C22A O2A C21A -176.9(3) . . . . ? C23A C22A O2A K1A 42.2(4) . . . . ? O6A K1A O2A C21A 20.3(3) . . . . ? O3A K1A O2A C21A -150.4(3) . . . . ? O5A K1A O2A C21A -69.1(9) . . . . ? O4A K1A O2A C21A -162.5(3) . . . . ? O1A K1A O2A C21A 8.9(3) . . . . ? C4A K1A O2A C21A 124.6(3) . . . . ? C12 K1A O2A C21A -61.9(3) 1_556 . . . ? C3A K1A O2A C21A 120.2(3) . . . . ? C5A K1A O2A C21A 105.4(3) . . . . ? C11 K1A O2A C21A -80.1(3) 1_556 . . . ? O6A K1A O2A C22A 157.6(2) . . . . ? O3A K1A O2A C22A -13.1(2) . . . . ? O5A K1A O2A C22A 68.2(9) . . . . ? O4A K1A O2A C22A -25.2(3) . . . . ? O1A K1A O2A C22A 146.2(3) . . . . ? C4A K1A O2A C22A -98.1(2) . . . . ? C12 K1A O2A C22A 75.4(2) 1_556 . . . ? C3A K1A O2A C22A -102.5(2) . . . . ? C5A K1A O2A C22A -117.3(3) . . . . ? C11 K1A O2A C22A 57.2(2) 1_556 . . . ? C22A C23A O3A C24A -176.0(4) . . . . ? C22A C23A O3A K1A 49.0(4) . . . . ? C25A C24A O3A C23A 177.9(3) . . . . ? C25A C24A O3A K1A -48.1(4) . . . . ? O6A K1A O3A C23A -116.6(6) . . . . ? O2A K1A O3A C23A -18.9(2) . . . . ? O5A K1A O3A C23A 168.0(2) . . . . ? O4A K1A O3A C23A 149.3(3) . . . . ? O1A K1A O3A C23A -38.8(3) . . . . ? C4A K1A O3A C23A 65.8(2) . . . . ? C12 K1A O3A C23A -109.1(2) 1_556 . . . ? C3A K1A O3A C23A 84.5(2) . . . . ? C5A K1A O3A C23A 43.6(2) . . . . ? C11 K1A O3A C23A -130.9(2) 1_556 . . . ? O6A K1A O3A C24A 110.1(6) . . . . ? O2A K1A O3A C24A -152.1(3) . . . . ? O5A K1A O3A C24A 34.7(3) . . . . ? O4A K1A O3A C24A 16.0(2) . . . . ? O1A K1A O3A C24A -172.1(2) . . . . ? C4A K1A O3A C24A -67.4(3) . . . . ? C12 K1A O3A C24A 117.7(3) 1_556 . . . ? C3A K1A O3A C24A -48.7(3) . . . . ? C5A K1A O3A C24A -89.7(3) . . . . ? C11 K1A O3A C24A 95.8(3) 1_556 . . . ? C27A C26A O4A C25A 175.6(3) . . . . ? C27A C26A O4A K1A 46.8(4) . . . . ? C24A C25A O4A C26A -177.9(3) . . . . ? C24A C25A O4A K1A -47.5(3) . . . . ? O6A K1A O4A C26A -25.4(3) . . . . ? O3A K1A O4A C26A 145.2(3) . . . . ? O2A K1A O4A C26A 157.3(2) . . . . ? O5A K1A O4A C26A -15.5(2) . . . . ? O1A K1A O4A C26A 68.0(7) . . . . ? C4A K1A O4A C26A -129.2(2) . . . . ? C12 K1A O4A C26A 62.3(2) 1_556 . . . ? C3A K1A O4A C26A -106.1(2) . . . . ? C5A K1A O4A C26A -132.5(2) . . . . ? C11 K1A O4A C26A 58.9(2) 1_556 . . . ? O6A K1A O4A C25A -153.3(2) . . . . ? O3A K1A O4A C25A 17.3(2) . . . . ? O2A K1A O4A C25A 29.4(2) . . . . ? O5A K1A O4A C25A -143.4(2) . . . . ? O1A K1A O4A C25A -59.9(7) . . . . ? C4A K1A O4A C25A 102.9(2) . . . . ? C12 K1A O4A C25A -65.6(2) 1_556 . . . ? C3A K1A O4A C25A 126.0(2) . . . . ? C5A K1A O4A C25A 99.6(2) . . . . ? C11 K1A O4A C25A -69.0(2) 1_556 . . . ? C26A C27A O5A C28A 178.9(3) . . . . ? C26A C27A O5A K1A 52.0(4) . . . . ? C29A C28A O5A C27A 178.9(3) . . . . ? C29A C28A O5A K1A -52.4(4) . . . . ? O6A K1A O5A C27A 150.6(3) . . . . ? O3A K1A O5A C27A -38.4(3) . . . . ? O2A K1A O5A C27A -116.6(8) . . . . ? O4A K1A O5A C27A -19.5(2) . . . . ? O1A K1A O5A C27A 168.9(2) . . . . ? C4A K1A O5A C27A 49.4(3) . . . . ? C12 K1A O5A C27A -123.8(3) 1_556 . . . ? C3A K1A O5A C27A 54.3(3) . . . . ? C5A K1A O5A C27A 69.3(3) . . . . ? C11 K1A O5A C27A -105.2(3) 1_556 . . . ? O6A K1A O5A C28A 22.5(2) . . . . ? O3A K1A O5A C28A -166.6(2) . . . . ? O2A K1A O5A C28A 115.3(8) . . . . ? O4A K1A O5A C28A -147.6(3) . . . . ? O1A K1A O5A C28A 40.8(3) . . . . ? C4A K1A O5A C28A -78.7(3) . . . . ? C12 K1A O5A C28A 108.1(3) 1_556 . . . ? C3A K1A O5A C28A -73.8(3) . . . . ? C5A K1A O5A C28A -58.9(3) . . . . ? C11 K1A O5A C28A 126.7(3) 1_556 . . . ? C28A C29A O6A C30A 177.2(4) . . . . ? C28A C29A O6A K1A -41.0(4) . . . . ? C31A C30A O6A C29A -173.4(3) . . . . ? C31A C30A O6A K1A 44.6(4) . . . . ? O3A K1A O6A C29A -69.7(7) . . . . ? O2A K1A O6A C29A -163.0(2) . . . . ? O5A K1A O6A C29A 9.9(2) . . . . ? O4A K1A O6A C29A 19.7(3) . . . . ? O1A K1A O6A C29A -151.9(3) . . . . ? C4A K1A O6A C29A 107.7(3) . . . . ? C12 K1A O6A C29A -77.3(3) 1_556 . . . ? C3A K1A O6A C29A 89.3(3) . . . . ? C5A K1A O6A C29A 130.3(3) . . . . ? C11 K1A O6A C29A -55.6(3) 1_556 . . . ? O3A K1A O6A C30A 70.4(7) . . . . ? O2A K1A O6A C30A -22.9(3) . . . . ? O5A K1A O6A C30A 150.1(3) . . . . ? O4A K1A O6A C30A 159.8(2) . . . . ? O1A K1A O6A C30A -11.7(2) . . . . ? C4A K1A O6A C30A -112.1(3) . . . . ? C12 K1A O6A C30A 62.8(3) 1_556 . . . ? C3A K1A O6A C30A -130.6(3) . . . . ? C5A K1A O6A C30A -89.6(3) . . . . ? C11 K1A O6A C30A 84.5(3) 1_556 . . . ? C8B C1B C2B C3B -161.3(3) . . . . ? C14B C1B C2B C3B 20.5(5) . . . . ? C8B C1B C2B C7B 19.3(5) . . . . ? C14B C1B C2B C7B -158.9(4) . . . . ? C7B C2B C3B C4B 2.7(5) . . . . ? C1B C2B C3B C4B -176.8(3) . . . . ? C7B C2B C3B K1C -65.4(3) . . . . ? C1B C2B C3B K1C 115.1(3) . . . . ? C2B C3B C4B C5B -1.0(5) . . . . ? K1C C3B C4B C5B 84.3(3) . . . . ? C2B C3B C4B K1C -85.3(3) . . . . ? C3B C4B C5B C6B -1.0(5) . . . . ? K1C C4B C5B C6B 85.2(3) . . . . ? C3B C4B C5B K1C -86.2(3) . . . . ? C4B C5B C6B C7B 1.2(6) . . . . ? K1C C5B C6B C7B 71.3(4) . . . . ? C5B C6B C7B C2B 0.7(6) . . . . ? C3B C2B C7B C6B -2.5(5) . . . . ? C1B C2B C7B C6B 176.9(3) . . . . ? C2B C1B C8B C9B 33.1(5) . . . . ? C14B C1B C8B C9B -148.6(4) . . . . ? C2B C1B C8B C13B -146.7(3) . . . . ? C14B C1B C8B C13B 31.6(5) . . . . ? C13B C8B C9B C10B -0.5(5) . . . . ? C1B C8B C9B C10B 179.7(4) . . . . ? C8B C9B C10B C11B 0.5(6) . . . . ? C9B C10B C11B C12B -0.4(6) . . . . ? C10B C11B C12B C13B 0.4(6) . . . . ? C10B C11B C12B K1B 111.5(4) . . . . ? C11B C12B C13B C8B -0.5(6) . . . . ? K1B C12B C13B C8B -112.9(3) . . . . ? C9B C8B C13B C12B 0.5(5) . . . . ? C1B C8B C13B C12B -179.7(3) . . . . ? C8B C1B C14B C19B -142.2(4) . . . . ? C2B C1B C14B C19B 36.1(6) . . . . ? C8B C1B C14B C15B 36.5(5) . . . . ? C2B C1B C14B C15B -145.2(4) . . . . ? C19B C14B C15B C16B 3.3(6) . . . . ? C1B C14B C15B C16B -175.5(4) . . . . ? C14B C15B C16B C17B -1.9(7) . . . . ? C15B C16B C17B C18B -0.9(7) . . . . ? C16B C17B C18B C19B 2.0(6) . . . . ? C17B C18B C19B C14B -0.4(7) . . . . ? C15B C14B C19B C18B -2.1(6) . . . . ? C1B C14B C19B C18B 176.6(4) . . . . ? O1B C20B C21B O2B 74.2(5) . . . . ? O1B C20B C21B O2F 49.9(7) . . . . ? C20B C21B O2B C22B 172.0(6) . . . . ? O2F C21B O2B C22B -41.9(6) . . . . ? C20B C21B O2B K1B -65.0(5) . . . . ? O2F C21B O2B K1B 81.1(6) . . . . ? C21B O2B C22B C23B 173.3(6) . . . . ? K1B O2B C22B C23B 50.0(9) . . . . ? C20B C21B O2F C22F 78.5(8) . . . . ? O2B C21B O2F C22F 36.0(6) . . . . ? C20B C21B O2F K1B -20.5(7) . . . . ? O2B C21B O2F K1B -63.0(5) . . . . ? C21B O2F C22F C23B 174.7(5) . . . . ? K1B O2F C22F C23B -77.0(6) . . . . ? C21B O2F C22F K1B -108.3(5) . . . . ? O2F C22F C23B O3B 53.8(8) . . . . ? K1B C22F C23B O3B -6.0(4) . . . . ? O2F C22F C23B C22B -44.0(10) . . . . ? K1B C22F C23B C22B -103.7(12) . . . . ? O2B C22B C23B C22F 33.0(9) . . . . ? O2B C22B C23B O3B -61.6(9) . . . . ? O3B C24B C25B O4B 63.5(4) . . . . ? O4B C26B C27B O5B -70.3(4) . . . . ? O5B C28B C29B O6B 62.4(5) . . . . ? O6B C30B C31B O1B -69.1(4) . . . . ? K1B C30B C31B O1B -27.0(3) . . . . ? C22B O2B K1B O3B -22.3(7) . . . . ? C21B O2B K1B O3B -138.4(5) . . . . ? C22B O2B K1B O5B -123.4(7) . . . . ? C21B O2B K1B O5B 120.6(6) . . . . ? C22B O2B K1B O1B 148.0(8) . . . . ? C21B O2B K1B O1B 32.0(4) . . . . ? C22B O2B K1B O6B 174.9(7) . . . . ? C21B O2B K1B O6B 58.8(5) . . . . ? C22B O2B K1B O4B -43.0(8) . . . . ? C21B O2B K1B O4B -159.1(4) . . . . ? C22B O2B K1B O2F 45.4(7) . . . . ? C21B O2B K1B O2F -70.6(7) . . . . ? C22B O2B K1B C4C 66.2(7) . . . . ? C21B O2B K1B C4C -49.8(5) . . . . ? C22B O2B K1B C12B -114.0(7) . . . . ? C21B O2B K1B C12B 129.9(5) . . . . ? C22B O2B K1B C22F -38.2(6) . . . . ? C21B O2B K1B C22F -154.2(11) . . . . ? C22B O2B K1B C3C 89.0(7) . . . . ? C21B O2B K1B C3C -27.1(5) . . . . ? C22B O2B K1B C5C 47.6(7) . . . . ? C21B O2B K1B C5C -68.5(5) . . . . ? C22F O2F K1B O3B 51.5(5) . . . . ? C21B O2F K1B O3B 162.9(5) . . . . ? C22F O2F K1B O5B 75(2) . . . . ? C21B O2F K1B O5B -173.6(19) . . . . ? C22F O2F K1B O1B -116.6(6) . . . . ? C21B O2F K1B O1B -5.2(4) . . . . ? C22F O2F K1B O6B -108.3(5) . . . . ? C21B O2F K1B O6B 3.1(5) . . . . ? C22F O2F K1B O2B -49.7(6) . . . . ? C21B O2F K1B O2B 61.7(6) . . . . ? C22F O2F K1B O4B 51.4(6) . . . . ? C21B O2F K1B O4B 162.8(4) . . . . ? C22F O2F K1B C4C 152.0(5) . . . . ? C21B O2F K1B C4C -96.6(4) . . . . ? C22F O2F K1B C12B -29.1(5) . . . . ? C21B O2F K1B C12B 82.3(4) . . . . ? C21B O2F K1B C22F 111.4(8) . . . . ? C22F O2F K1B C3C 173.4(5) . . . . ? C21B O2F K1B C3C -75.2(4) . . . . ? C22F O2F K1B C5C 132.4(5) . . . . ? C21B O2F K1B C5C -116.2(4) . . . . ? C11B C12B K1B O3B -116.8(3) . . . . ? C13B C12B K1B O3B 8.8(2) . . . . ? C11B C12B K1B O5B 122.1(3) . . . . ? C13B C12B K1B O5B -112.3(3) . . . . ? C11B C12B K1B O1B 1.1(3) . . . . ? C13B C12B K1B O1B 126.7(3) . . . . ? C11B C12B K1B O6B 60.3(3) . . . . ? C13B C12B K1B O6B -174.1(3) . . . . ? C11B C12B K1B O2B -55.1(3) . . . . ? C13B C12B K1B O2B 70.4(3) . . . . ? C11B C12B K1B O4B -176.1(3) . . . . ? C13B C12B K1B O4B -50.6(2) . . . . ? C11B C12B K1B O2F -61.7(3) . . . . ? C13B C12B K1B O2F 63.8(3) . . . . ? C11B C12B K1B C4C -53.3(10) . . . . ? C13B C12B K1B C4C 72.2(10) . . . . ? C11B C12B K1B C22F -73.8(3) . . . . ? C13B C12B K1B C22F 51.7(3) . . . . ? C11B C12B K1B C3C 38.0(4) . . . . ? C13B C12B K1B C3C 163.6(2) . . . . ? C11B C12B K1B C5C -169.8(3) . . . . ? C13B C12B K1B C5C -44.3(4) . . . . ? O2F C22F K1B O3B -109.8(6) . . . . ? C23B C22F K1B O3B 4.2(3) . . . . ? O2F C22F K1B O5B -171.3(4) . . . . ? C23B C22F K1B O5B -57.3(7) . . . . ? O2F C22F K1B O1B 55.2(5) . . . . ? C23B C22F K1B O1B 169.2(5) . . . . ? O2F C22F K1B O6B 89.4(6) . . . . ? C23B C22F K1B O6B -156.6(3) . . . . ? O2F C22F K1B O2B 49.9(6) . . . . ? C23B C22F K1B O2B 163.9(11) . . . . ? O2F C22F K1B O4B -134.5(5) . . . . ? C23B C22F K1B O4B -20.5(4) . . . . ? C23B C22F K1B O2F 114.0(8) . . . . ? O2F C22F K1B C4C -27.0(5) . . . . ? C23B C22F K1B C4C 87.0(4) . . . . ? O2F C22F K1B C12B 150.5(5) . . . . ? C23B C22F K1B C12B -95.5(4) . . . . ? O2F C22F K1B C3C -7.0(6) . . . . ? C23B C22F K1B C3C 107.0(4) . . . . ? O2F C22F K1B C5C -49.5(5) . . . . ? C23B C22F K1B C5C 64.5(4) . . . . ? C30B C31B O1B C20B 174.4(4) . . . . ? C30B C31B O1B K1B 38.6(4) . . . . ? C21B C20B O1B C31B 172.6(4) . . . . ? C21B C20B O1B K1B -51.5(4) . . . . ? O3B K1B O1B C31B 154.4(2) . . . . ? O5B K1B O1B C31B -15.3(3) . . . . ? O6B K1B O1B C31B -6.5(2) . . . . ? O2B K1B O1B C31B 144.8(3) . . . . ? O4B K1B O1B C31B 80.9(5) . . . . ? O2F K1B O1B C31B 165.6(3) . . . . ? C4C K1B O1B C31B -119.3(3) . . . . ? C12B K1B O1B C31B 66.4(3) . . . . ? C22F K1B O1B C31B 142.8(3) . . . . ? C3C K1B O1B C31B -99.3(3) . . . . ? C5C K1B O1B C31B -116.7(3) . . . . ? O3B K1B O1B C20B 19.2(3) . . . . ? O5B K1B O1B C20B -150.6(3) . . . . ? O6B K1B O1B C20B -141.8(3) . . . . ? O2B K1B O1B C20B 9.5(3) . . . . ? O4B K1B O1B C20B -54.3(6) . . . . ? O2F K1B O1B C20B 30.4(3) . . . . ? C4C K1B O1B C20B 105.4(3) . . . . ? C12B K1B O1B C20B -68.8(3) . . . . ? C22F K1B O1B C20B 7.5(3) . . . . ? C3C K1B O1B C20B 125.4(3) . . . . ? C5C K1B O1B C20B 108.0(3) . . . . ? C25B C24B O3B C23B -178.8(3) . . . . ? C25B C24B O3B K1B -32.2(4) . . . . ? C22F C23B O3B C24B 156.2(5) . . . . ? C22B C23B O3B C24B -169.6(5) . . . . ? C22F C23B O3B K1B 8.2(6) . . . . ? C22B C23B O3B K1B 42.5(6) . . . . ? O5B K1B O3B C24B 3.2(3) . . . . ? O1B K1B O3B C24B -166.6(3) . . . . ? O6B K1B O3B C24B -85.6(4) . . . . ? O2B K1B O3B C24B -157.4(3) . . . . ? O4B K1B O3B C24B 1.3(3) . . . . ? O2F K1B O3B C24B -178.6(3) . . . . ? C4C K1B O3B C24B 110.4(3) . . . . ? C12B K1B O3B C24B -75.8(3) . . . . ? C22F K1B O3B C24B -150.1(4) . . . . ? C3C K1B O3B C24B 114.4(3) . . . . ? C5C K1B O3B C24B 88.5(3) . . . . ? O5B K1B O3B C23B 148.6(3) . . . . ? O1B K1B O3B C23B -21.3(3) . . . . ? O6B K1B O3B C23B 59.7(5) . . . . ? O2B K1B O3B C23B -12.1(3) . . . . ? O4B K1B O3B C23B 146.6(3) . . . . ? O2F K1B O3B C23B -33.3(3) . . . . ? C4C K1B O3B C23B -104.2(3) . . . . ? C12B K1B O3B C23B 69.5(3) . . . . ? C22F K1B O3B C23B -4.7(3) . . . . ? C3C K1B O3B C23B -100.2(3) . . . . ? C5C K1B O3B C23B -126.2(3) . . . . ? C27B C26B O4B C25B 177.1(3) . . . . ? C27B C26B O4B K1B 59.5(3) . . . . ? C24B C25B O4B C26B -178.3(3) . . . . ? C24B C25B O4B K1B -61.0(3) . . . . ? O3B K1B O4B C26B 151.7(2) . . . . ? O5B K1B O4B C26B -26.3(2) . . . . ? O1B K1B O4B C26B -128.8(5) . . . . ? O6B K1B O4B C26B -47.3(2) . . . . ? O2B K1B O4B C26B 172.9(3) . . . . ? O2F K1B O4B C26B 151.9(3) . . . . ? C4C K1B O4B C26B 72.2(2) . . . . ? C12B K1B O4B C26B -114.0(2) . . . . ? C22F K1B O4B C26B 171.3(3) . . . . ? C3C K1B O4B C26B 51.4(2) . . . . ? C5C K1B O4B C26B 68.2(2) . . . . ? O3B K1B O4B C25B 30.8(2) . . . . ? O5B K1B O4B C25B -147.3(2) . . . . ? O1B K1B O4B C25B 110.2(5) . . . . ? O6B K1B O4B C25B -168.3(2) . . . . ? O2B K1B O4B C25B 51.9(3) . . . . ? O2F K1B O4B C25B 30.9(3) . . . . ? C4C K1B O4B C25B -48.8(2) . . . . ? C12B K1B O4B C25B 125.1(2) . . . . ? C22F K1B O4B C25B 50.3(3) . . . . ? C3C K1B O4B C25B -69.5(2) . . . . ? C5C K1B O4B C25B -52.8(2) . . . . ? C29B C28B O5B C27B 177.2(4) . . . . ? C29B C28B O5B K1B -43.2(5) . . . . ? C26B C27B O5B C28B -178.2(3) . . . . ? C26B C27B O5B K1B 41.7(4) . . . . ? O3B K1B O5B C28B -148.0(3) . . . . ? O1B K1B O5B C28B 21.5(3) . . . . ? O6B K1B O5B C28B 12.7(3) . . . . ? O2B K1B O5B C28B -56.5(6) . . . . ? O4B K1B O5B C28B -146.0(3) . . . . ? O2F K1B O5B C28B -170(2) . . . . ? C4C K1B O5B C28B 113.6(3) . . . . ? C12B K1B O5B C28B -65.8(3) . . . . ? C22F K1B O5B C28B -103.3(5) . . . . ? C3C K1B O5B C28B 91.5(3) . . . . ? C5C K1B O5B C28B 132.2(3) . . . . ? O3B K1B O5B C27B -10.3(3) . . . . ? O1B K1B O5B C27B 159.2(2) . . . . ? O6B K1B O5B C27B 150.4(3) . . . . ? O2B K1B O5B C27B 81.2(6) . . . . ? O4B K1B O5B C27B -8.4(2) . . . . ? O2F K1B O5B C27B -33(2) . . . . ? C4C K1B O5B C27B -108.7(3) . . . . ? C12B K1B O5B C27B 71.9(3) . . . . ? C22F K1B O5B C27B 34.4(5) . . . . ? C3C K1B O5B C27B -130.8(2) . . . . ? C5C K1B O5B C27B -90.1(3) . . . . ? C31B C30B O6B C29B -174.5(3) . . . . ? K1B C30B O6B C29B 124.0(3) . . . . ? C31B C30B O6B K1B 61.5(3) . . . . ? C28B C29B O6B C30B -172.1(4) . . . . ? C28B C29B O6B K1B -50.5(4) . . . . ? O3B K1B O6B C30B -118.2(4) . . . . ? O5B K1B O6B C30B 143.3(2) . . . . ? O1B K1B O6B C30B -28.0(2) . . . . ? O2B K1B O6B C30B -53.8(3) . . . . ? O4B K1B O6B C30B 164.3(2) . . . . ? O2F K1B O6B C30B -36.4(3) . . . . ? C4C K1B O6B C30B 45.1(2) . . . . ? C12B K1B O6B C30B -128.3(2) . . . . ? C22F K1B O6B C30B -66.6(3) . . . . ? C3C K1B O6B C30B 43.2(2) . . . . ? C5C K1B O6B C30B 68.3(2) . . . . ? O3B K1B O6B C29B 118.8(4) . . . . ? O5B K1B O6B C29B 20.3(3) . . . . ? O1B K1B O6B C29B -151.1(3) . . . . ? O2B K1B O6B C29B -176.8(3) . . . . ? O4B K1B O6B C29B 41.3(3) . . . . ? O2F K1B O6B C29B -159.5(3) . . . . ? C4C K1B O6B C29B -78.0(3) . . . . ? C12B K1B O6B C29B 108.7(3) . . . . ? C22F K1B O6B C29B 170.4(3) . . . . ? C3C K1B O6B C29B -79.8(3) . . . . ? C5C K1B O6B C29B -54.8(3) . . . . ? C14C C1C C2C C7C -22.1(5) . . . . ? C8C C1C C2C C7C 155.8(4) . . . . ? C14C C1C C2C C3C 159.8(3) . . . . ? C8C C1C C2C C3C -22.4(5) . . . . ? C7C C2C C3C C4C -0.5(5) . . . . ? C1C C2C C3C C4C 177.9(3) . . . . ? C7C C2C C3C K1B 71.2(3) . . . . ? C1C C2C C3C K1B -110.5(3) . . . . ? O3B K1B C3C C4C -10.0(3) . . . . ? O5B K1B C3C C4C 116.1(3) . . . . ? O1B K1B C3C C4C -122.8(3) . . . . ? O6B K1B C3C C4C 175.7(3) . . . . ? O2B K1B C3C C4C -72.9(3) . . . . ? O4B K1B C3C C4C 57.1(3) . . . . ? O2F K1B C3C C4C -60.0(3) . . . . ? C12B K1B C3C C4C -162.5(3) . . . . ? C22F K1B C3C C4C -57.0(3) . . . . ? C5C K1B C3C C4C 31.3(2) . . . . ? O3B K1B C3C C2C -128.0(2) . . . . ? O5B K1B C3C C2C -1.9(3) . . . . ? O1B K1B C3C C2C 119.2(3) . . . . ? O6B K1B C3C C2C 57.7(2) . . . . ? O2B K1B C3C C2C 169.0(3) . . . . ? O4B K1B C3C C2C -60.9(3) . . . . ? O2F K1B C3C C2C -178.0(3) . . . . ? C4C K1B C3C C2C -118.0(4) . . . . ? C12B K1B C3C C2C 79.5(4) . . . . ? C22F K1B C3C C2C -175.1(3) . . . . ? C5C K1B C3C C2C -86.7(3) . . . . ? C2C C3C C4C C5C 0.8(6) . . . . ? K1B C3C C4C C5C -97.3(4) . . . . ? C2C C3C C4C K1B 98.1(3) . . . . ? O3B K1B C4C C3C 170.8(2) . . . . ? O5B K1B C4C C3C -67.9(3) . . . . ? O1B K1B C4C C3C 52.7(2) . . . . ? O6B K1B C4C C3C -4.4(3) . . . . ? O2B K1B C4C C3C 109.2(3) . . . . ? O4B K1B C4C C3C -131.2(2) . . . . ? O2F K1B C4C C3C 116.1(3) . . . . ? C12B K1B C4C C3C 107.5(9) . . . . ? C22F K1B C4C C3C 127.6(3) . . . . ? C5C K1B C4C C3C -121.2(4) . . . . ? O3B K1B C4C C5C -68.0(3) . . . . ? O5B K1B C4C C5C 53.3(3) . . . . ? O1B K1B C4C C5C 173.8(3) . . . . ? O6B K1B C4C C5C 116.7(2) . . . . ? O2B K1B C4C C5C -129.6(3) . . . . ? O4B K1B C4C C5C -10.1(3) . . . . ? O2F K1B C4C C5C -122.7(3) . . . . ? C12B K1B C4C C5C -131.4(9) . . . . ? C22F K1B C4C C5C -111.3(3) . . . . ? C3C K1B C4C C5C 121.2(4) . . . . ? C3C C4C C5C C6C 0.2(6) . . . . ? K1B C4C C5C C6C -95.3(3) . . . . ? C3C C4C C5C K1B 95.4(4) . . . . ? O3B K1B C5C C6C -136.8(3) . . . . ? O5B K1B C5C C6C -16.2(3) . . . . ? O1B K1B C5C C6C 106.6(3) . . . . ? O6B K1B C5C C6C 41.3(3) . . . . ? O2B K1B C5C C6C 166.4(3) . . . . ? O4B K1B C5C C6C -76.7(3) . . . . ? O2F K1B C5C C6C 167.1(3) . . . . ? C4C K1B C5C C6C 113.1(4) . . . . ? C12B K1B C5C C6C -82.9(4) . . . . ? C22F K1B C5C C6C -174.2(3) . . . . ? C3C K1B C5C C6C 81.1(3) . . . . ? O3B K1B C5C C4C 110.1(3) . . . . ? O5B K1B C5C C4C -129.3(3) . . . . ? O1B K1B C5C C4C -6.4(3) . . . . ? O6B K1B C5C C4C -71.8(3) . . . . ? O2B K1B C5C C4C 53.4(3) . . . . ? O4B K1B C5C C4C 170.2(3) . . . . ? O2F K1B C5C C4C 54.1(3) . . . . ? C12B K1B C5C C4C 164.1(3) . . . . ? C22F K1B C5C C4C 72.7(3) . . . . ? C3C K1B C5C C4C -32.0(2) . . . . ? C4C C5C C6C C7C -1.4(6) . . . . ? K1B C5C C6C C7C -67.6(4) . . . . ? C5C C6C C7C C2C 1.7(6) . . . . ? C3C C2C C7C C6C -0.8(5) . . . . ? C1C C2C C7C C6C -179.1(3) . . . . ? C2C C1C C8C C9C -35.5(6) . . . . ? C14C C1C C8C C9C 142.5(4) . . . . ? C2C C1C C8C C13C 141.3(4) . . . . ? C14C C1C C8C C13C -40.7(6) . . . . ? C13C C8C C9C C10C -0.7(6) . . . . ? C1C C8C C9C C10C 176.3(4) . . . . ? C8C C9C C10C C11C 0.2(6) . . . . ? C9C C10C C11C C12C 0.5(6) . . . . ? C10C C11C C12C C13C -0.7(6) . . . . ? C11C C12C C13C C8C 0.2(6) . . . . ? C9C C8C C13C C12C 0.5(6) . . . . ? C1C C8C C13C C12C -176.5(4) . . . . ? C2C C1C C14C C19C -30.0(5) . . . . ? C8C C1C C14C C19C 152.1(4) . . . . ? C2C C1C C14C C15C 149.5(3) . . . . ? C8C C1C C14C C15C -28.4(5) . . . . ? C19C C14C C15C C16C 1.2(5) . . . . ? C1C C14C C15C C16C -178.4(3) . . . . ? C14C C15C C16C C17C -1.2(5) . . . . ? C14C C15C C16C K1C 93.6(3) . . . 1_554 ? C15C C16C C17C C18C 0.6(5) . . . . ? K1C C16C C17C C18C -102.7(3) 1_554 . . . ? C15C C16C C17C K1C 103.3(3) . . . 1_554 ? C16C C17C C18C C19C 0.0(5) . . . . ? K1C C17C C18C C19C -76.0(4) 1_554 . . . ? C17C C18C C19C C14C 0.1(6) . . . . ? C15C C14C C19C C18C -0.6(5) . . . . ? C1C C14C C19C C18C 178.9(3) . . . . ? O1C C20C C21C O2C -64.3(4) . . . . ? O2C C22C C23C O3C 64.2(4) . . . . ? O3C C24C C25C O4C -64.0(4) . . . . ? O4C C26C C27C O5C 66.1(4) . . . . ? O5C C28C C29C O6C -66.0(4) . . . . ? O6C C30C C31C O1C 68.8(4) . . . . ? C5B C4B K1C O5C -75.2(3) . . . . ? C3B C4B K1C O5C 46.1(3) . . . . ? C5B C4B K1C O3C 44.0(3) . . . . ? C3B C4B K1C O3C 165.3(3) . . . . ? C5B C4B K1C O2C 106.2(3) . . . . ? C3B C4B K1C O2C -132.5(3) . . . . ? C5B C4B K1C O6C -138.7(2) . . . . ? C3B C4B K1C O6C -17.5(3) . . . . ? C5B C4B K1C O1C 166.9(3) . . . . ? C3B C4B K1C O1C -71.9(2) . . . . ? C5B C4B K1C O4C -10.3(3) . . . . ? C3B C4B K1C O4C 111.0(2) . . . . ? C5B C4B K1C C16C 90.7(7) . . . 1_556 ? C3B C4B K1C C16C -148.0(6) . . . 1_556 ? C3B C4B K1C C5B 121.2(4) . . . . ? C5B C4B K1C C17C 158.8(3) . . . 1_556 ? C3B C4B K1C C17C -79.9(3) . . . 1_556 ? C5B C4B K1C C3B -121.2(4) . . . . ? C6B C5B K1C O5C -6.4(3) . . . . ? C4B C5B K1C O5C 111.7(3) . . . . ? C6B C5B K1C O3C 110.4(3) . . . . ? C4B C5B K1C O3C -131.5(3) . . . . ? C6B C5B K1C O2C 170.2(3) . . . . ? C4B C5B K1C O2C -71.7(3) . . . . ? C6B C5B K1C O6C -69.9(3) . . . . ? C4B C5B K1C O6C 48.1(3) . . . . ? C6B C5B K1C O1C -131.1(2) . . . . ? C4B C5B K1C O1C -13.0(3) . . . . ? C6B C5B K1C O4C 52.4(3) . . . . ? C4B C5B K1C O4C 170.4(3) . . . . ? C6B C5B K1C C4B -118.1(4) . . . . ? C6B C5B K1C C16C 85.2(3) . . . 1_556 ? C4B C5B K1C C16C -156.8(3) . . . 1_556 ? C6B C5B K1C C17C 152.3(6) . . . 1_556 ? C4B C5B K1C C17C -89.7(7) . . . 1_556 ? C6B C5B K1C C3B -86.6(3) . . . . ? C4B C5B K1C C3B 31.5(2) . . . . ? C4B C3B K1C O5C -137.4(3) . . . . ? C2B C3B K1C O5C -15.6(2) . . . . ? C4B C3B K1C O3C -15.4(3) . . . . ? C2B C3B K1C O3C 106.4(2) . . . . ? C4B C3B K1C O2C 47.3(3) . . . . ? C2B C3B K1C O2C 169.1(2) . . . . ? C4B C3B K1C O6C 162.7(3) . . . . ? C2B C3B K1C O6C -75.5(2) . . . . ? C4B C3B K1C O1C 101.3(3) . . . . ? C2B C3B K1C O1C -137.0(2) . . . . ? C4B C3B K1C O4C -79.8(3) . . . . ? C2B C3B K1C O4C 41.9(3) . . . . ? C2B C3B K1C C4B 121.8(4) . . . . ? C4B C3B K1C C16C 161.0(3) . . . 1_556 ? C2B C3B K1C C16C -77.2(4) . . . 1_556 ? C4B C3B K1C C5B -31.9(2) . . . . ? C2B C3B K1C C5B 89.9(3) . . . . ? C4B C3B K1C C17C 135.4(3) . . . 1_556 ? C2B C3B K1C C17C -102.8(3) . . . 1_556 ? C30C C31C O1C C20C -172.2(3) . . . . ? C30C C31C O1C K1C -42.2(3) . . . . ? C21C C20C O1C C31C -178.3(3) . . . . ? C21C C20C O1C K1C 50.6(3) . . . . ? O5C K1C O1C C31C 17.2(2) . . . . ? O3C K1C O1C C31C -161.4(2) . . . . ? O2C K1C O1C C31C -149.3(2) . . . . ? O6C K1C O1C C31C 9.6(2) . . . . ? O4C K1C O1C C31C -74.6(6) . . . . ? C4B K1C O1C C31C 123.2(2) . . . . ? C16C K1C O1C C31C -66.7(2) 1_556 . . . ? C5B K1C O1C C31C 128.6(2) . . . . ? C17C K1C O1C C31C -60.4(2) 1_556 . . . ? C3B K1C O1C C31C 99.0(2) . . . . ? O5C K1C O1C C20C 147.0(2) . . . . ? O3C K1C O1C C20C -31.7(2) . . . . ? O2C K1C O1C C20C -19.6(2) . . . . ? O6C K1C O1C C20C 139.4(2) . . . . ? O4C K1C O1C C20C 55.1(6) . . . . ? C4B K1C O1C C20C -107.1(2) . . . . ? C16C K1C O1C C20C 63.1(2) 1_556 . . . ? C5B K1C O1C C20C -101.6(2) . . . . ? C17C K1C O1C C20C 69.3(2) 1_556 . . . ? C3B K1C O1C C20C -131.2(2) . . . . ? C23C C22C O2C C21C 172.1(3) . . . . ? C23C C22C O2C K1C -52.9(4) . . . . ? C20C C21C O2C C22C 178.2(3) . . . . ? C20C C21C O2C K1C 46.1(4) . . . . ? O5C K1C O2C C22C 119.7(4) . . . . ? O3C K1C O2C C22C 21.5(2) . . . . ? O6C K1C O2C C22C -166.8(2) . . . . ? O1C K1C O2C C22C -146.6(2) . . . . ? O4C K1C O2C C22C 43.0(2) . . . . ? C4B K1C O2C C22C -66.7(2) . . . . ? C16C K1C O2C C22C 110.7(2) 1_556 . . . ? C5B K1C O2C C22C -43.5(2) . . . . ? C17C K1C O2C C22C 133.7(2) 1_556 . . . ? C3B K1C O2C C22C -84.3(2) . . . . ? O5C K1C O2C C21C -108.2(4) . . . . ? O3C K1C O2C C21C 153.6(3) . . . . ? O6C K1C O2C C21C -34.7(3) . . . . ? O1C K1C O2C C21C -14.5(2) . . . . ? O4C K1C O2C C21C 175.1(2) . . . . ? C4B K1C O2C C21C 65.4(2) . . . . ? C16C K1C O2C C21C -117.3(2) 1_556 . . . ? C5B K1C O2C C21C 88.6(2) . . . . ? C17C K1C O2C C21C -94.2(2) 1_556 . . . ? C3B K1C O2C C21C 47.8(3) . . . . ? C25C C24C O3C C23C 178.6(3) . . . . ? C25C C24C O3C K1C 37.6(4) . . . . ? C22C C23C O3C C24C 174.9(3) . . . . ? C22C C23C O3C K1C -42.1(4) . . . . ? O5C K1C O3C C24C -15.4(3) . . . . ? O2C K1C O3C C24C 151.4(3) . . . . ? O6C K1C O3C C24C 74.8(7) . . . . ? O1C K1C O3C C24C 163.3(2) . . . . ? O4C K1C O3C C24C -6.5(2) . . . . ? C4B K1C O3C C24C -125.4(3) . . . . ? C16C K1C O3C C24C 61.8(3) 1_556 . . . ? C5B K1C O3C C24C -107.4(3) . . . . ? C17C K1C O3C C24C 78.8(3) 1_556 . . . ? C3B K1C O3C C24C -119.2(3) . . . . ? O5C K1C O3C C23C -155.4(2) . . . . ? O2C K1C O3C C23C 11.4(2) . . . . ? O6C K1C O3C C23C -65.2(7) . . . . ? O1C K1C O3C C23C 23.3(3) . . . . ? O4C K1C O3C C23C -146.5(3) . . . . ? C4B K1C O3C C23C 94.6(2) . . . . ? C16C K1C O3C C23C -78.2(2) 1_556 . . . ? C5B K1C O3C C23C 112.6(2) . . . . ? C17C K1C O3C C23C -61.2(2) 1_556 . . . ? C3B K1C O3C C23C 100.8(2) . . . . ? C27C C26C O4C C25C -175.6(3) . . . . ? C27C C26C O4C K1C -56.7(3) . . . . ? C24C C25C O4C C26C 175.2(3) . . . . ? C24C C25C O4C K1C 56.9(3) . . . . ? O5C K1C O4C C26C 24.86(19) . . . . ? O3C K1C O4C C26C -146.2(2) . . . . ? O2C K1C O4C C26C -168.17(19) . . . . ? O6C K1C O4C C26C 42.5(2) . . . . ? O1C K1C O4C C26C 121.8(5) . . . . ? C4B K1C O4C C26C -76.8(2) . . . . ? C16C K1C O4C C26C 113.5(2) 1_556 . . . ? C5B K1C O4C C26C -81.0(2) . . . . ? C17C K1C O4C C26C 107.9(2) 1_556 . . . ? C3B K1C O4C C26C -51.4(2) . . . . ? O5C K1C O4C C25C 144.8(2) . . . . ? O3C K1C O4C C25C -26.3(2) . . . . ? O2C K1C O4C C25C -48.2(2) . . . . ? O6C K1C O4C C25C 162.4(2) . . . . ? O1C K1C O4C C25C -118.3(5) . . . . ? C4B K1C O4C C25C 43.1(2) . . . . ? C16C K1C O4C C25C -126.5(2) 1_556 . . . ? C5B K1C O4C C25C 38.9(2) . . . . ? C17C K1C O4C C25C -132.2(2) 1_556 . . . ? C3B K1C O4C C25C 68.5(2) . . . . ? C26C C27C O5C C28C 175.8(3) . . . . ? C26C C27C O5C K1C -40.0(4) . . . . ? C29C C28C O5C C27C -172.6(3) . . . . ? C29C C28C O5C K1C 42.2(4) . . . . ? O3C K1C O5C C27C 17.6(3) . . . . ? O2C K1C O5C C27C -74.2(5) . . . . ? O6C K1C O5C C27C -153.5(3) . . . . ? O1C K1C O5C C27C -161.0(2) . . . . ? O4C K1C O5C C27C 8.8(2) . . . . ? C4B K1C O5C C27C 112.6(3) . . . . ? C16C K1C O5C C27C -64.9(3) 1_556 . . . ? C5B K1C O5C C27C 88.6(3) . . . . ? C17C K1C O5C C27C -88.1(3) 1_556 . . . ? C3B K1C O5C C27C 129.6(3) . . . . ? O3C K1C O5C C28C 160.3(2) . . . . ? O2C K1C O5C C28C 68.5(5) . . . . ? O6C K1C O5C C28C -10.8(2) . . . . ? O1C K1C O5C C28C -18.3(3) . . . . ? O4C K1C O5C C28C 151.5(3) . . . . ? C4B K1C O5C C28C -104.7(3) . . . . ? C16C K1C O5C C28C 77.8(2) 1_556 . . . ? C5B K1C O5C C28C -128.7(2) . . . . ? C17C K1C O5C C28C 54.6(2) 1_556 . . . ? C3B K1C O5C C28C -87.7(2) . . . . ? C28C C29C O6C C30C 178.1(3) . . . . ? C28C C29C O6C K1C 54.7(3) . . . . ? C31C C30C O6C C29C 178.9(3) . . . . ? C31C C30C O6C K1C -58.2(3) . . . . ? O5C K1C O6C C29C -23.2(2) . . . . ? O3C K1C O6C C29C -117.6(7) . . . . ? O2C K1C O6C C29C 169.6(2) . . . . ? O1C K1C O6C C29C 149.4(2) . . . . ? O4C K1C O6C C29C -40.6(2) . . . . ? C4B K1C O6C C29C 83.0(2) . . . . ? C16C K1C O6C C29C -104.6(2) 1_556 . . . ? C5B K1C O6C C29C 64.7(2) . . . . ? C17C K1C O6C C29C -121.9(2) 1_556 . . . ? C3B K1C O6C C29C 75.9(2) . . . . ? O5C K1C O6C C30C -147.2(2) . . . . ? O3C K1C O6C C30C 118.3(7) . . . . ? O2C K1C O6C C30C 45.5(2) . . . . ? O1C K1C O6C C30C 25.3(2) . . . . ? O4C K1C O6C C30C -164.7(2) . . . . ? C4B K1C O6C C30C -41.1(2) . . . . ? C16C K1C O6C C30C 131.3(2) 1_556 . . . ? C5B K1C O6C C30C -59.4(3) . . . . ? C17C K1C O6C C30C 114.0(2) 1_556 . . . ? C3B K1C O6C C30C -48.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.291 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.047 _exptl_crystal_recrystallization_method ; Diffusion of PhMe into a solution in THF at rt. ; _iucr_refine_instructions_details ; TITL CK22CK in P2(1) CELL 0.71073 9.8014 28.7693 19.7370 90.000 90.447 90.000 ZERR 8.00 0.0005 0.0014 0.0010 0.000 0.005 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H K O UNIT 248 312 8 48 MERG 0 OMIT -2.00 52.00 EADP C28 C28D EADP C22B C22F FMAP 2 PLAN 5 ACTA BOND BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.032800 BASF 0.33938 FVAR 1.82645 0.50357 0.46770 MOLE 1 C1 1 0.304098 0.299705 0.227234 11.00000 0.01724 0.01549 = 0.01260 -0.00201 -0.00030 -0.00233 C2 1 0.374308 0.332793 0.269313 11.00000 0.01563 0.01231 = 0.01895 0.00081 -0.00339 0.00697 C3 1 0.315531 0.351652 0.328593 11.00000 0.01534 0.02228 = 0.02014 0.00161 -0.00167 0.00284 AFIX 43 H3 2 0.227740 0.341206 0.341830 11.00000 -1.20000 AFIX 0 C4 1 0.380898 0.384588 0.367801 11.00000 0.02844 0.02168 = 0.01641 -0.00685 -0.01072 0.00744 AFIX 43 H4 2 0.336082 0.396084 0.406880 11.00000 -1.20000 AFIX 0 C5 1 0.508190 0.401482 0.352707 11.00000 0.03234 0.01818 = 0.02068 -0.00701 -0.01695 0.00731 AFIX 43 H5 2 0.551456 0.424635 0.379637 11.00000 -1.20000 AFIX 0 C6 1 0.570148 0.382701 0.295633 11.00000 0.01869 0.01492 = 0.02669 0.00257 -0.00299 -0.00066 AFIX 43 H6 2 0.659474 0.392657 0.284209 11.00000 -1.20000 AFIX 0 C7 1 0.506427 0.350287 0.255351 11.00000 0.02040 0.01480 = 0.01935 0.00075 0.00142 -0.00225 AFIX 43 H7 2 0.552733 0.339107 0.216512 11.00000 -1.20000 AFIX 0 C8 1 0.376067 0.269983 0.179311 11.00000 0.01608 0.00822 = 0.01746 0.00379 -0.00431 -0.00482 C9 1 0.508512 0.253004 0.193384 11.00000 0.02314 0.01761 = 0.00923 -0.00430 0.00091 -0.00348 AFIX 43 H9 2 0.552185 0.261210 0.234825 11.00000 -1.20000 AFIX 0 C10 1 0.575796 0.224663 0.147979 11.00000 0.01867 0.01124 = 0.03295 0.00150 -0.00373 0.00419 AFIX 43 H10 2 0.665453 0.214254 0.158541 11.00000 -1.20000 AFIX 0 C11 1 0.515455 0.211111 0.087466 11.00000 0.02145 0.01944 = 0.02496 -0.00806 0.00303 -0.00438 AFIX 43 H11 2 0.562097 0.191524 0.056579 11.00000 -1.20000 AFIX 0 C12 1 0.385468 0.226962 0.073474 11.00000 0.02132 0.01815 = 0.01228 -0.00042 0.00023 -0.00565 AFIX 43 H12 2 0.342157 0.217963 0.032292 11.00000 -1.20000 AFIX 0 C13 1 0.317093 0.255393 0.117505 11.00000 0.01498 0.01335 = 0.02262 0.00043 -0.00129 -0.00369 AFIX 43 H13 2 0.227598 0.265520 0.106033 11.00000 -1.20000 AFIX 0 C14 1 0.155132 0.295974 0.229274 11.00000 0.01357 0.01836 = 0.01155 0.00158 -0.00293 -0.00203 C15 1 0.088638 0.252926 0.221633 11.00000 0.01863 0.02399 = 0.01441 -0.00373 -0.00311 0.00075 AFIX 43 H15 2 0.142566 0.225792 0.215896 11.00000 -1.20000 AFIX 0 C16 1 -0.048561 0.248508 0.222101 11.00000 0.02394 0.01970 = 0.01771 -0.00451 -0.00361 -0.00785 AFIX 43 H16 2 -0.088015 0.218672 0.215501 11.00000 -1.20000 AFIX 0 C17 1 -0.133023 0.286436 0.231971 11.00000 0.01202 0.03925 = 0.01892 0.00296 0.00134 -0.00632 AFIX 43 H17 2 -0.229437 0.283097 0.232503 11.00000 -1.20000 AFIX 0 C18 1 -0.071654 0.329632 0.241085 11.00000 0.01963 0.02326 = 0.01837 0.00009 0.00016 0.00934 AFIX 43 H18 2 -0.126652 0.356250 0.248966 11.00000 -1.20000 AFIX 0 C19 1 0.067843 0.334112 0.238783 11.00000 0.01919 0.01731 = 0.01563 0.00236 -0.00120 0.00088 AFIX 43 H19 2 0.106751 0.364170 0.243819 11.00000 -1.20000 AFIX 0 C20 1 0.815601 0.301689 0.404987 11.00000 0.01598 0.03303 = 0.02679 0.00851 0.01508 0.00664 AFIX 23 H20A 2 0.916215 0.304636 0.406456 11.00000 -1.20000 H20B 2 0.780327 0.321189 0.367417 11.00000 -1.20000 AFIX 0 C21 1 0.776421 0.252379 0.393895 11.00000 0.03350 0.02821 = 0.01747 0.00342 0.00637 0.01031 AFIX 23 H21A 2 0.828829 0.239277 0.355705 11.00000 -1.20000 H21B 2 0.797276 0.233895 0.434997 11.00000 -1.20000 AFIX 0 C22 1 0.588414 0.203986 0.367996 11.00000 0.04532 0.02632 = 0.03697 -0.00643 0.01154 0.00334 AFIX 23 H22A 2 0.607421 0.184937 0.408763 11.00000 -1.20000 H22B 2 0.638163 0.190241 0.329404 11.00000 -1.20000 AFIX 0 C23 1 0.440599 0.204151 0.353348 11.00000 0.06202 0.02074 = 0.02963 -0.00457 -0.00627 -0.00190 AFIX 23 H23A 2 0.420866 0.225304 0.314940 11.00000 -1.20000 H23B 2 0.410494 0.172495 0.340449 11.00000 -1.20000 AFIX 0 C24 1 0.225311 0.220838 0.398566 11.00000 0.03366 0.03152 = 0.04298 0.00146 -0.02478 -0.00632 AFIX 23 H24A 2 0.191531 0.189795 0.384761 11.00000 -1.20000 H24B 2 0.205283 0.243067 0.361511 11.00000 -1.20000 AFIX 0 C25 1 0.157408 0.235816 0.461174 11.00000 0.02539 0.05164 = 0.05641 0.02633 -0.00794 -0.00499 AFIX 23 H25A 2 0.057441 0.231988 0.456261 11.00000 -1.20000 H25B 2 0.188741 0.216372 0.499643 11.00000 -1.20000 AFIX 0 C26 1 0.131158 0.299767 0.534622 11.00000 0.02384 0.12476 = 0.01916 0.01066 0.00878 0.03094 AFIX 23 H26A 2 0.166640 0.281565 0.573510 11.00000 -1.20000 H26B 2 0.030844 0.295851 0.532829 11.00000 -1.20000 AFIX 0 C27 1 0.164635 0.349444 0.544385 11.00000 0.01958 0.10765 = 0.04419 -0.04017 -0.00415 0.01130 AFIX 23 H27A 2 0.154874 0.367816 0.502212 11.00000 -1.20000 H27B 2 0.111676 0.363963 0.581280 11.00000 -1.20000 AFIX 0 PART 1 O5 4 0.305826 0.341271 0.563069 21.00000 0.02332 0.01047 = 0.02224 0.00183 0.00031 -0.00295 C28 1 0.350038 0.386995 0.583630 21.00000 0.02134 0.01722 = 0.02187 -0.00220 0.00466 0.00337 AFIX 23 H28A 2 0.300538 0.396905 0.624706 21.00000 -1.20000 H28B 2 0.331378 0.409757 0.547099 21.00000 -1.20000 AFIX 0 PART 2 O5D 4 0.311458 0.369823 0.537959 -21.00000 0.01195 0.02053 = 0.01661 0.00339 -0.00432 -0.00115 C28D 1 0.378532 0.359063 0.599673 -21.00000 0.02134 0.01722 = 0.02187 -0.00220 0.00466 0.00337 AFIX 23 H28I 2 0.395262 0.325207 0.603149 -21.00000 -1.20000 H28J 2 0.322632 0.368928 0.638682 -21.00000 -1.20000 AFIX 0 PART 0 C29 1 0.507165 0.384427 0.598710 11.00000 0.03951 0.03086 = 0.01790 -0.00669 0.00231 -0.00444 PART 1 AFIX 23 H29A 2 0.539798 0.414737 0.616198 21.00000 -1.20000 H29B 2 0.525628 0.360489 0.633631 21.00000 -1.20000 PART 2 H29I 2 0.489758 0.418296 0.600580 -21.00000 -1.20000 H29J 2 0.563334 0.375702 0.638630 -21.00000 -1.20000 AFIX 0 PART 0 C30 1 0.719473 0.378289 0.544417 11.00000 0.02920 0.02321 = 0.03226 -0.00360 -0.01271 -0.00515 AFIX 23 H30A 2 0.754156 0.358489 0.581785 11.00000 -1.20000 H30B 2 0.741887 0.411032 0.555196 11.00000 -1.20000 AFIX 0 C31 1 0.785188 0.364658 0.479844 11.00000 0.02315 0.02393 = 0.03273 0.00378 -0.00236 -0.00508 AFIX 23 H31A 2 0.747974 0.383639 0.442163 11.00000 -1.20000 H31B 2 0.884729 0.370215 0.482875 11.00000 -1.20000 AFIX 0 K1 3 0.470051 0.303571 0.460633 11.00000 0.02264 0.02696 = 0.03514 -0.01477 -0.00365 0.00090 O1 4 0.759512 0.316563 0.467156 11.00000 0.02770 0.02448 = 0.01774 0.00377 0.00417 -0.00294 O2 4 0.633117 0.250248 0.378992 11.00000 0.03269 0.01842 = 0.02499 -0.00208 0.00003 0.00270 O3 4 0.368889 0.219040 0.411281 11.00000 0.02985 0.02776 = 0.02295 0.00186 -0.00675 -0.00666 O4 4 0.188802 0.282858 0.473990 11.00000 0.02678 0.04668 = 0.02349 0.00685 0.00435 0.00227 O6 4 0.577221 0.373069 0.538123 11.00000 0.03048 0.05347 = 0.02079 -0.01338 0.01012 -0.01966 MOLE 2 C1A 1 0.684020 0.305845 0.734900 11.00000 0.01008 0.01521 = 0.02126 0.00108 -0.00001 -0.00158 C2A 1 0.616768 0.336312 0.782417 11.00000 0.01765 0.01295 = 0.01809 0.00292 0.00330 -0.00524 C3A 1 0.684005 0.353332 0.841705 11.00000 0.01941 0.01965 = 0.01984 0.00475 -0.00096 -0.00252 AFIX 43 H3A 2 0.774463 0.343294 0.851267 11.00000 -1.20000 AFIX 0 C4A 1 0.622197 0.383835 0.885566 11.00000 0.02997 0.01577 = 0.01930 0.00523 0.00141 -0.00767 AFIX 43 H4A 2 0.670933 0.394388 0.924413 11.00000 -1.20000 AFIX 0 C5A 1 0.491294 0.399324 0.874243 11.00000 0.02756 0.01525 = 0.02280 -0.00069 0.01489 -0.00590 AFIX 43 H5A 2 0.450143 0.420894 0.904259 11.00000 -1.20000 AFIX 0 C6A 1 0.421129 0.382919 0.818501 11.00000 0.02008 0.01360 = 0.03060 0.00219 0.01294 -0.00093 AFIX 43 H6A 2 0.329232 0.392312 0.811306 11.00000 -1.20000 AFIX 0 C7A 1 0.481425 0.353100 0.772809 11.00000 0.01958 0.01111 = 0.02043 -0.00349 0.00237 -0.00225 AFIX 43 H7A 2 0.431174 0.343530 0.733891 11.00000 -1.20000 AFIX 0 C8A 1 0.832648 0.304584 0.732768 11.00000 0.01526 0.02611 = 0.01408 0.00755 -0.00082 0.00485 C9A 1 0.915344 0.344415 0.739372 11.00000 0.01254 0.02404 = 0.01699 0.00039 -0.00500 -0.00141 AFIX 43 H9A 2 0.872926 0.373448 0.748275 11.00000 -1.20000 AFIX 0 C10A 1 1.055299 0.342951 0.733437 11.00000 0.02509 0.02957 = 0.02303 0.00236 -0.00291 -0.00285 AFIX 43 H10A 2 1.106459 0.370845 0.737903 11.00000 -1.20000 AFIX 0 C11A 1 1.121946 0.301959 0.721204 11.00000 0.00503 0.05266 = 0.02473 -0.00970 0.00460 -0.00526 AFIX 43 H11A 2 1.218351 0.301083 0.716751 11.00000 -1.20000 AFIX 0 C12A 1 1.044398 0.261766 0.715515 11.00000 0.02042 0.03220 = 0.01947 -0.00500 0.00413 0.01099 AFIX 43 H12A 2 1.087821 0.232866 0.706893 11.00000 -1.20000 AFIX 0 C13A 1 0.904592 0.263598 0.722324 11.00000 0.01466 0.02776 = 0.01739 -0.00276 -0.00137 -0.00260 AFIX 43 H13A 2 0.854751 0.235324 0.719738 11.00000 -1.20000 AFIX 0 C14A 1 0.609327 0.276587 0.687406 11.00000 0.01360 0.01170 = 0.01507 0.00542 0.00093 0.00396 C15A 1 0.665292 0.263399 0.624422 11.00000 0.01129 0.01559 = 0.02452 0.00370 0.00349 0.00012 AFIX 43 H15A 2 0.753451 0.274399 0.612797 11.00000 -1.20000 AFIX 0 C16A 1 0.596148 0.235053 0.579179 11.00000 0.02541 0.02156 = 0.01587 0.00406 0.00717 0.00479 AFIX 43 H16A 2 0.638189 0.227037 0.537576 11.00000 -1.20000 AFIX 0 C17A 1 0.466590 0.217990 0.593073 11.00000 0.02008 0.02043 = 0.01792 -0.00053 -0.00346 0.00210 AFIX 43 H17A 2 0.419427 0.198488 0.561903 11.00000 -1.20000 AFIX 0 C18A 1 0.409578 0.230561 0.653918 11.00000 0.01005 0.02242 = 0.02488 0.00302 -0.00229 0.00016 AFIX 43 H18A 2 0.320738 0.219801 0.664733 11.00000 -1.20000 AFIX 0 C19A 1 0.478611 0.258406 0.699445 11.00000 0.01802 0.01218 = 0.01385 -0.00126 0.00710 0.00222 AFIX 43 H19A 2 0.435693 0.265695 0.741108 11.00000 -1.20000 AFIX 0 C20A 1 0.163662 0.349080 0.962296 11.00000 0.02182 0.02877 = 0.03787 0.00834 0.00801 0.00994 AFIX 23 H20C 2 0.062664 0.348820 0.961273 11.00000 -1.20000 H20D 2 0.195566 0.369246 0.924991 11.00000 -1.20000 AFIX 0 C21A 1 0.212707 0.368179 1.028694 11.00000 0.04377 0.02413 = 0.03211 0.00292 0.00918 0.00919 AFIX 23 H21C 2 0.174501 0.399632 1.035909 11.00000 -1.20000 H21D 2 0.182425 0.347896 1.066203 11.00000 -1.20000 AFIX 0 C22A 1 0.411658 0.385696 1.090434 11.00000 0.05079 0.02024 = 0.02192 -0.00494 0.01213 -0.00516 AFIX 23 H22C 2 0.387726 0.363314 1.126541 11.00000 -1.20000 H22D 2 0.371780 0.416225 1.102263 11.00000 -1.20000 AFIX 0 C23A 1 0.562501 0.389931 1.086185 11.00000 0.05166 0.02045 = 0.02535 -0.00567 0.01509 -0.01909 AFIX 23 H23C 2 0.586041 0.412272 1.049960 11.00000 -1.20000 H23D 2 0.598816 0.402209 1.129575 11.00000 -1.20000 AFIX 0 C24A 1 0.767471 0.349360 1.072683 11.00000 0.03486 0.03375 = 0.02488 0.00552 -0.00823 -0.02448 AFIX 23 H24C 2 0.799749 0.361461 1.116944 11.00000 -1.20000 H24D 2 0.797616 0.371160 1.036992 11.00000 -1.20000 AFIX 0 C25A 1 0.827870 0.303148 1.060608 11.00000 0.02115 0.04480 = 0.02247 0.00324 -0.00858 -0.01364 AFIX 23 H25C 2 0.928445 0.304921 1.064857 11.00000 -1.20000 H25D 2 0.794091 0.280741 1.094651 11.00000 -1.20000 AFIX 0 C26A 1 0.842615 0.243030 0.981371 11.00000 0.02084 0.03584 = 0.03405 0.00835 0.00307 0.01183 AFIX 23 H26C 2 0.811725 0.221252 1.016931 11.00000 -1.20000 H26D 2 0.943602 0.243722 0.981953 11.00000 -1.20000 AFIX 0 C27A 1 0.791697 0.227396 0.913483 11.00000 0.02659 0.03306 = 0.03615 -0.00230 0.00114 0.01215 AFIX 23 H27C 2 0.815195 0.250854 0.878780 11.00000 -1.20000 H27D 2 0.836034 0.197705 0.901077 11.00000 -1.20000 AFIX 0 C28A 1 0.592770 0.207230 0.851422 11.00000 0.04841 0.02100 = 0.01877 -0.00398 -0.00364 0.00562 AFIX 23 H28C 2 0.635505 0.177727 0.836880 11.00000 -1.20000 H28D 2 0.611880 0.231160 0.816722 11.00000 -1.20000 AFIX 0 C29A 1 0.444394 0.200847 0.857813 11.00000 0.04948 0.01374 = 0.02670 -0.00307 -0.00098 0.00341 AFIX 23 H29C 2 0.406476 0.188841 0.814594 11.00000 -1.20000 H29D 2 0.425647 0.177690 0.893656 11.00000 -1.20000 AFIX 0 C30A 1 0.237060 0.239415 0.877616 11.00000 0.03202 0.02284 = 0.02398 0.00088 -0.01658 -0.01416 AFIX 23 H30C 2 0.211685 0.219184 0.916087 11.00000 -1.20000 H30D 2 0.201019 0.225265 0.835401 11.00000 -1.20000 AFIX 0 C31A 1 0.177423 0.286412 0.886860 11.00000 0.02137 0.03000 = 0.03238 -0.00218 -0.01358 -0.01080 AFIX 23 H31C 2 0.212677 0.307784 0.851797 11.00000 -1.20000 H31D 2 0.076905 0.284865 0.882074 11.00000 -1.20000 AFIX 0 K1A 3 0.506156 0.299493 0.966067 11.00000 0.02026 0.01720 = 0.02241 -0.00430 -0.00069 -0.00210 O1A 4 0.213335 0.303318 0.952758 11.00000 0.02388 0.02199 = 0.02406 0.00594 -0.00561 0.00354 O2A 4 0.356646 0.370276 1.027572 11.00000 0.03030 0.02241 = 0.01869 0.00054 0.00660 -0.00066 O3A 4 0.623558 0.346840 1.072423 11.00000 0.02909 0.01887 = 0.02333 -0.00560 -0.00149 -0.00637 O4A 4 0.790511 0.287881 0.993759 11.00000 0.02690 0.03384 = 0.01831 0.00370 -0.00146 -0.00080 O5A 4 0.648877 0.221348 0.915227 11.00000 0.03184 0.02576 = 0.02167 0.00108 0.00223 0.00634 O6A 4 0.380528 0.243247 0.874106 11.00000 0.03094 0.01601 = 0.02469 -0.00305 -0.00922 -0.00368 MOLE 3 C1B 1 0.183647 0.041852 0.482686 11.00000 0.01672 0.01262 = 0.01914 0.00016 -0.00019 0.00017 C2B 1 0.118149 0.010927 0.530614 11.00000 0.01372 0.01546 = 0.02023 -0.00642 0.00230 0.00158 C3B 1 0.185495 -0.008076 0.587256 11.00000 0.01980 0.01680 = 0.01305 -0.00390 0.00105 0.00471 AFIX 43 H3B 2 0.277222 0.000813 0.596217 11.00000 -1.20000 AFIX 0 C4B 1 0.122815 -0.039437 0.630721 11.00000 0.03366 0.01645 = 0.01531 -0.00368 0.00351 0.00687 AFIX 43 H4B 2 0.172850 -0.051760 0.668020 11.00000 -1.20000 AFIX 0 C5B 1 -0.010798 -0.052919 0.620519 11.00000 0.03481 0.01727 = 0.02328 0.00026 0.01486 0.00430 AFIX 43 H5B 2 -0.052989 -0.074721 0.649816 11.00000 -1.20000 AFIX 0 C6B 1 -0.081217 -0.033911 0.566738 11.00000 0.01877 0.01854 = 0.03091 -0.00647 0.00446 -0.00468 AFIX 43 H6B 2 -0.173864 -0.042386 0.559481 11.00000 -1.20000 AFIX 0 C7B 1 -0.020094 -0.002565 0.522678 11.00000 0.01907 0.01810 = 0.02153 0.00576 0.00076 0.00244 AFIX 43 H7B 2 -0.072341 0.010103 0.486383 11.00000 -1.20000 AFIX 0 C8B 1 0.107855 0.071822 0.436991 11.00000 0.01589 0.01642 = 0.01677 -0.00290 0.00094 -0.00599 C9B 1 -0.017624 0.092647 0.451990 11.00000 0.02131 0.02009 = 0.02038 -0.00344 -0.00298 0.00008 AFIX 43 H9B 2 -0.056815 0.086781 0.495023 11.00000 -1.20000 AFIX 0 C10B 1 -0.086701 0.121055 0.407719 11.00000 0.01884 0.02140 = 0.02511 0.00048 0.00216 -0.00345 AFIX 43 H10B 2 -0.171141 0.134385 0.420845 11.00000 -1.20000 AFIX 0 C11B 1 -0.034665 0.130607 0.343798 11.00000 0.02725 0.02669 = 0.02896 0.00600 -0.00818 -0.00374 AFIX 43 H11B 2 -0.082620 0.150135 0.312962 11.00000 -1.20000 AFIX 0 C12B 1 0.087984 0.110989 0.326599 11.00000 0.03360 0.02721 = 0.01534 0.00138 -0.00397 -0.01023 AFIX 43 H12B 2 0.125668 0.117182 0.283327 11.00000 -1.20000 AFIX 0 C13B 1 0.157379 0.082393 0.371249 11.00000 0.01696 0.02115 = 0.02050 -0.00657 0.00280 -0.00376 AFIX 43 H13B 2 0.241645 0.069248 0.357482 11.00000 -1.20000 AFIX 0 C14B 1 0.332379 0.041966 0.478835 11.00000 0.02215 0.02066 = 0.01407 0.00523 -0.00163 -0.00047 C15B 1 0.405308 0.083952 0.465159 11.00000 0.02704 0.02378 = 0.02078 0.00573 -0.00159 -0.00719 AFIX 43 H15B 2 0.356099 0.112318 0.461804 11.00000 -1.20000 AFIX 0 C16B 1 0.544880 0.084540 0.456689 11.00000 0.03431 0.03202 = 0.02136 0.01101 -0.00081 -0.00838 AFIX 43 H16B 2 0.589354 0.112974 0.446310 11.00000 -1.20000 AFIX 0 C17B 1 0.620238 0.044579 0.463068 11.00000 0.01914 0.05771 = 0.01066 -0.00504 0.00116 -0.00762 AFIX 43 H17B 2 0.716133 0.045280 0.456506 11.00000 -1.20000 AFIX 0 C18B 1 0.555745 0.003126 0.479150 11.00000 0.02517 0.04207 = 0.01655 -0.00213 -0.00728 0.00952 AFIX 43 H18B 2 0.607559 -0.024502 0.485101 11.00000 -1.20000 AFIX 0 C19B 1 0.415034 0.002292 0.486485 11.00000 0.02072 0.02368 = 0.02321 -0.00736 -0.00193 0.00012 AFIX 43 H19B 2 0.372510 -0.026431 0.497178 11.00000 -1.20000 AFIX 0 C20B 1 -0.337199 0.049367 0.278082 11.00000 0.02390 0.09417 = 0.03413 -0.01253 -0.00240 -0.01470 AFIX 23 H20E 2 -0.436276 0.055568 0.274010 11.00000 -1.20000 H20F 2 -0.300722 0.068037 0.316266 11.00000 -1.20000 AFIX 0 C21B 1 -0.314535 -0.000073 0.291403 11.00000 0.01632 0.12113 = 0.04240 0.03683 0.00567 -0.00137 AFIX 23 H21E 2 -0.324436 -0.019481 0.250237 11.00000 -1.20000 H21F 2 -0.373059 -0.012247 0.328007 11.00000 -1.20000 AFIX 0 PART 3 O2B 4 -0.170437 0.005778 0.312970 31.00000 0.01981 0.01098 = 0.03822 -0.00368 0.00756 0.00205 C22B 1 -0.138700 -0.039254 0.337225 31.00000 0.01407 0.02694 = 0.02285 0.00045 -0.00726 -0.00264 AFIX 23 H22E 2 -0.160656 -0.062908 0.302379 31.00000 -1.20000 H22F 2 -0.191775 -0.046232 0.378467 31.00000 -1.20000 AFIX 0 PART 4 O2F 4 -0.177354 -0.023677 0.290427 -31.00000 0.02017 0.03292 = 0.02772 0.00099 -0.00030 -0.00648 C22F 1 -0.106439 -0.014177 0.351064 -31.00000 0.01407 0.02694 = 0.02285 0.00045 -0.00726 -0.00264 AFIX 23 H22L 2 -0.163827 -0.022771 0.390173 -31.00000 -1.20000 H22M 2 -0.086715 0.019515 0.353992 -31.00000 -1.20000 AFIX 0 PART 0 C23B 1 0.017399 -0.039523 0.353673 11.00000 0.03504 0.02011 = 0.01726 0.00525 0.00405 0.00385 PART 3 AFIX 23 H23E 2 0.037909 -0.015426 0.388082 31.00000 -1.20000 H23F 2 0.043372 -0.070092 0.372858 31.00000 -1.20000 PART 4 H23I 2 0.070539 -0.030245 0.394336 -31.00000 -1.20000 H23J 2 -0.002579 -0.073169 0.357092 -31.00000 -1.20000 AFIX 0 PART 0 C24B 1 0.236248 -0.038686 0.304193 11.00000 0.02032 0.02245 = 0.02737 -0.00090 -0.00637 0.00866 AFIX 23 H24E 2 0.252324 -0.071552 0.316792 11.00000 -1.20000 H24F 2 0.271299 -0.018758 0.341333 11.00000 -1.20000 AFIX 0 C25B 1 0.308473 -0.027789 0.240702 11.00000 0.02596 0.02293 = 0.03295 -0.00611 0.00166 0.00465 AFIX 23 H25E 2 0.406681 -0.035192 0.245680 11.00000 -1.20000 H25F 2 0.270634 -0.046617 0.203009 11.00000 -1.20000 AFIX 0 C26B 1 0.354068 0.033838 0.165285 11.00000 0.02344 0.03419 = 0.02614 -0.00858 0.00706 -0.00826 AFIX 23 H26E 2 0.317970 0.014916 0.127278 11.00000 -1.20000 H26F 2 0.453842 0.028826 0.168458 11.00000 -1.20000 AFIX 0 C27B 1 0.324981 0.083261 0.153217 11.00000 0.03039 0.03140 = 0.02239 0.00248 0.00822 -0.01322 AFIX 23 H27E 2 0.346936 0.101532 0.194386 11.00000 -1.20000 H27F 2 0.381922 0.094944 0.115670 11.00000 -1.20000 AFIX 0 C28B 1 0.150069 0.135287 0.122019 11.00000 0.04636 0.02774 = 0.04193 0.01511 0.01712 0.00829 AFIX 23 H28E 2 0.208072 0.147162 0.085005 11.00000 -1.20000 H28F 2 0.166345 0.154732 0.162669 11.00000 -1.20000 AFIX 0 C29B 1 0.004140 0.138019 0.101594 11.00000 0.07512 0.03645 = 0.03401 0.01525 0.01826 0.01388 AFIX 23 H29E 2 -0.019276 0.170407 0.089175 11.00000 -1.20000 H29F 2 -0.012460 0.118030 0.061541 11.00000 -1.20000 AFIX 0 C30B 1 -0.216357 0.119298 0.136044 11.00000 0.04548 0.03194 = 0.02950 -0.01297 -0.00969 0.01304 AFIX 23 H30E 2 -0.225970 0.094482 0.101588 11.00000 -1.20000 H30F 2 -0.247027 0.148950 0.115532 11.00000 -1.20000 AFIX 0 C31B 1 -0.301392 0.108210 0.195725 11.00000 0.03548 0.04781 = 0.05706 -0.02734 -0.01873 0.01829 AFIX 23 H31E 2 -0.281731 0.130444 0.232820 11.00000 -1.20000 H31F 2 -0.399288 0.110745 0.183554 11.00000 -1.20000 AFIX 0 K1B 3 0.003746 0.037038 0.209998 11.00000 0.02107 0.02849 = 0.02903 0.01317 -0.00413 -0.00317 O1B 4 -0.271219 0.062356 0.217240 11.00000 0.02824 0.05257 = 0.02386 -0.00842 -0.00229 0.00219 O3B 4 0.094960 -0.030847 0.294729 11.00000 0.02700 0.04537 = 0.02234 0.01507 0.00737 0.01126 O4B 4 0.291356 0.020351 0.226534 11.00000 0.02499 0.03165 = 0.01534 0.00134 0.00732 0.00165 O5B 4 0.184413 0.088442 0.136373 11.00000 0.03490 0.01930 = 0.02462 0.00323 0.00529 -0.00190 O6B 4 -0.079724 0.123004 0.156581 11.00000 0.04247 0.02692 = 0.01797 0.00238 -0.00092 0.00449 MOLE 4 C1C 1 -0.186982 0.046227 -0.029324 11.00000 0.01493 0.01382 = 0.01355 -0.00261 -0.00033 -0.00016 C2C 1 -0.114154 0.013622 0.012093 11.00000 0.01431 0.01004 = 0.01518 -0.00426 0.00417 -0.00518 C3C 1 -0.168915 -0.005231 0.072689 11.00000 0.01248 0.02376 = 0.02173 -0.00244 -0.00208 -0.00401 AFIX 43 H3C 2 -0.256204 0.005084 0.086905 11.00000 -1.20000 AFIX 0 C4C 1 -0.101302 -0.037817 0.111872 11.00000 0.03641 0.02090 = 0.01833 0.00288 0.00315 -0.00248 AFIX 43 H4C 2 -0.143219 -0.049517 0.151618 11.00000 -1.20000 AFIX 0 C5C 1 0.027360 -0.053694 0.093832 11.00000 0.02162 0.01766 = 0.03052 0.00329 -0.01133 -0.00631 AFIX 43 H5C 2 0.073975 -0.076161 0.120630 11.00000 -1.20000 AFIX 0 C6C 1 0.084777 -0.036093 0.036542 11.00000 0.01274 0.01802 = 0.02650 -0.00144 0.00026 -0.00587 AFIX 43 H6C 2 0.173478 -0.046056 0.024014 11.00000 -1.20000 AFIX 0 C7C 1 0.016918 -0.004077 -0.003752 11.00000 0.01892 0.01858 = 0.01925 0.00221 -0.00156 -0.00346 AFIX 43 H7C 2 0.060022 0.006531 -0.043828 11.00000 -1.20000 AFIX 0 C8C 1 -0.335922 0.049037 -0.025870 11.00000 0.01851 0.01706 = 0.01292 0.00007 0.00249 -0.00230 C9C 1 -0.417118 0.009467 -0.015697 11.00000 0.01480 0.02134 = 0.01671 0.00023 -0.00414 0.00281 AFIX 43 H9C 2 -0.374331 -0.020135 -0.013645 11.00000 -1.20000 AFIX 0 C10C 1 -0.556257 0.012051 -0.008606 11.00000 0.01983 0.02905 = 0.02153 -0.00553 0.00645 -0.00886 AFIX 43 H10C 2 -0.606803 -0.015695 -0.001652 11.00000 -1.20000 AFIX 0 C11C 1 -0.624719 0.054286 -0.011371 11.00000 0.00926 0.03712 = 0.01760 0.01041 0.00100 0.00340 AFIX 43 H11C 2 -0.720835 0.056070 -0.006096 11.00000 -1.20000 AFIX 0 C12C 1 -0.546527 0.093745 -0.022174 11.00000 0.01866 0.03167 = 0.01528 0.00649 0.00058 0.01007 AFIX 43 H12C 2 -0.590609 0.123103 -0.024838 11.00000 -1.20000 AFIX 0 C13C 1 -0.407456 0.091684 -0.029135 11.00000 0.01927 0.02071 = 0.01713 0.00163 0.00308 -0.00009 AFIX 43 H13C 2 -0.357963 0.119620 -0.036331 11.00000 -1.20000 AFIX 0 C14C 1 -0.119020 0.076531 -0.077730 11.00000 0.01385 0.01647 = 0.01860 -0.00338 0.00165 0.00684 C15C 1 -0.183204 0.091753 -0.138117 11.00000 0.01864 0.01497 = 0.02185 -0.00576 0.00065 0.00178 AFIX 43 H15C 2 -0.274710 0.082408 -0.146620 11.00000 -1.20000 AFIX 0 C16C 1 -0.120042 0.119347 -0.185086 11.00000 0.03267 0.01307 = 0.00948 -0.00078 0.00382 0.00632 AFIX 43 H16C 2 -0.167338 0.128118 -0.225291 11.00000 -1.20000 AFIX 0 C17C 1 0.012469 0.134464 -0.174089 11.00000 0.02580 0.01567 = 0.02174 -0.00371 0.01190 0.00205 AFIX 43 H17C 2 0.056604 0.153811 -0.206186 11.00000 -1.20000 AFIX 0 C18C 1 0.079169 0.120783 -0.115356 11.00000 0.01237 0.01901 = 0.03285 -0.00650 0.01043 0.00309 AFIX 43 H18C 2 0.170106 0.130794 -0.106969 11.00000 -1.20000 AFIX 0 C19C 1 0.015047 0.092906 -0.069206 11.00000 0.01598 0.01440 = 0.02424 -0.00302 -0.00230 0.00120 AFIX 43 H19C 2 0.063755 0.084200 -0.029385 11.00000 -1.20000 AFIX 0 C20C 1 0.309326 0.033407 0.815167 11.00000 0.02058 0.02340 = 0.02405 -0.00030 -0.00804 0.00072 AFIX 23 H20G 2 0.273605 0.056734 0.847358 11.00000 -1.20000 H20H 2 0.408723 0.030187 0.823143 11.00000 -1.20000 AFIX 0 C21C 1 0.241108 -0.011795 0.826085 11.00000 0.02926 0.02367 = 0.01561 -0.00110 -0.00721 0.00398 AFIX 23 H21G 2 0.272842 -0.034619 0.792137 11.00000 -1.20000 H21H 2 0.264146 -0.023822 0.871757 11.00000 -1.20000 AFIX 0 C22C 1 0.025905 -0.048010 0.827772 11.00000 0.03153 0.01681 = 0.02250 0.00881 0.00261 -0.00309 AFIX 23 H22G 2 0.056398 -0.063552 0.870003 11.00000 -1.20000 H22H 2 0.046203 -0.068880 0.789264 11.00000 -1.20000 AFIX 0 C23C 1 -0.122219 -0.039312 0.830593 11.00000 0.03653 0.01381 = 0.02548 0.00432 0.00167 -0.00049 AFIX 23 H23G 2 -0.170927 -0.068727 0.840026 11.00000 -1.20000 H23H 2 -0.142284 -0.017153 0.867574 11.00000 -1.20000 AFIX 0 C24C 1 -0.311904 -0.014976 0.764166 11.00000 0.02027 0.02001 = 0.03092 0.00130 0.00346 -0.00359 AFIX 23 H24G 2 -0.342179 0.005564 0.801380 11.00000 -1.20000 H24H 2 -0.356963 -0.045534 0.769581 11.00000 -1.20000 AFIX 0 C25C 1 -0.350740 0.005698 0.697768 11.00000 0.01793 0.02224 = 0.03241 -0.00255 -0.00170 -0.00411 AFIX 23 H25G 2 -0.316196 -0.013992 0.660512 11.00000 -1.20000 H25H 2 -0.451356 0.007362 0.693685 11.00000 -1.20000 AFIX 0 C26C 1 -0.319919 0.070549 0.627422 11.00000 0.02350 0.02648 = 0.02356 0.00234 -0.00501 0.00506 AFIX 23 H26G 2 -0.419467 0.074345 0.620585 11.00000 -1.20000 H26H 2 -0.285747 0.049126 0.592157 11.00000 -1.20000 AFIX 0 C27C 1 -0.250875 0.116750 0.620817 11.00000 0.02829 0.02570 = 0.02179 0.00852 0.00180 0.00671 AFIX 23 H27G 2 -0.277423 0.131646 0.577462 11.00000 -1.20000 H27H 2 -0.278268 0.137458 0.658392 11.00000 -1.20000 AFIX 0 C28C 1 -0.032226 0.150845 0.612099 11.00000 0.04055 0.00980 = 0.02402 0.00963 -0.00368 -0.00197 AFIX 23 H28G 2 -0.045318 0.172439 0.650557 11.00000 -1.20000 H28H 2 -0.064364 0.166424 0.570194 11.00000 -1.20000 AFIX 0 C29C 1 0.115517 0.138663 0.605968 11.00000 0.03019 0.01895 = 0.02622 0.01107 -0.00302 -0.00544 AFIX 23 H29G 2 0.127310 0.114950 0.570139 11.00000 -1.20000 H29H 2 0.168213 0.166618 0.593103 11.00000 -1.20000 AFIX 0 C30C 1 0.304348 0.107607 0.664900 11.00000 0.02409 0.02000 = 0.03030 -0.00301 0.00737 -0.00098 AFIX 23 H30G 2 0.360913 0.134449 0.651114 11.00000 -1.20000 H30H 2 0.315119 0.082703 0.630742 11.00000 -1.20000 AFIX 0 C31C 1 0.349665 0.090486 0.732946 11.00000 0.02465 0.02063 = 0.03032 -0.00317 0.00144 -0.00374 AFIX 23 H31G 2 0.449783 0.085925 0.733329 11.00000 -1.20000 H31H 2 0.326944 0.113782 0.768010 11.00000 -1.20000 AFIX 0 K1C 3 -0.000348 0.045322 0.711287 11.00000 0.01906 0.01722 = 0.02289 0.00367 0.00087 -0.00093 O1C 4 0.284235 0.048266 0.747397 11.00000 0.02366 0.01904 = 0.02002 0.00226 -0.00375 -0.00136 O2C 4 0.097199 -0.005661 0.819887 11.00000 0.02233 0.01704 = 0.01897 0.00084 0.00135 0.00085 O3C 4 -0.168064 -0.020530 0.767201 11.00000 0.02282 0.02526 = 0.01800 0.00403 0.00342 -0.00498 O4C 4 -0.293816 0.051297 0.692896 11.00000 0.02520 0.02244 = 0.01790 0.00263 0.00036 -0.00346 O5C 4 -0.108412 0.109301 0.622872 11.00000 0.01781 0.02033 = 0.02298 0.00018 0.00197 -0.00034 O6C 4 0.164786 0.121154 0.668651 11.00000 0.02048 0.02351 = 0.01650 0.00031 0.00186 -0.00031 HKLF 5 REM CK22CK in P2(1) REM R1 = 0.0422 for 17536 Fo > 4sig(Fo) and 0.0743 for all 25554 data REM 1396 parameters refined using 1 restraints END WGHT 0.0328 0.0000 REM Highest difference peak 0.291, deepest hole -0.550, 1-sigma level 0.047 Q1 1 0.1233 0.0722 0.4122 11.00000 0.05 0.29 Q2 1 0.5876 0.2925 1.0021 11.00000 0.05 0.27 Q3 1 0.5648 0.2922 0.9317 11.00000 0.05 0.24 Q4 1 -0.0774 0.0573 0.6781 11.00000 0.05 0.24 Q5 1 -0.2714 0.0419 -0.0537 11.00000 0.05 0.23 ; data_ck25ck _database_code_depnum_ccdc_archive 'CCDC 924393' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '18-Crown-6-potassium triphenyl-silicon' _chemical_melting_point ? _chemical_formula_moiety 'C30 H39 K O6 Si' _chemical_formula_sum 'C30 H39 K O6 Si' _chemical_formula_weight 562.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_int_tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 18.3527(8) _cell_length_b 15.2640(8) _cell_length_c 10.4474(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2926.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12945 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 29.24 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96421 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; The collected data cover nominally a full sphere of the reciprocal space. A combination of 22 sets of \w scans were used; each set at different \j, 2\q or \k angles and each scan 1.0 deg in \w. Each frame was exposured for 25s. Nominal crystal to detector distance 45 mm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction, Xcalibur, EOS' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93602 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6396 _reflns_number_gt 5594 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution ; SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350.) ; _computing_structure_refinement ; SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122) ; _computing_molecular_graphics ; Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany. ; _computing_publication_material ; WinGX v1.80.05 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.) ; _refine_special_details ; All H atoms were refined using a riding model, with a common U restrained to be 1.2 (1.5 for methyl groups) times the equivalent isotropic displacement parameter of the parent atom. Methyl groups were treated as rigid bodies and allowed to rotate about the E-CH3 bond. 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^)+(0.0000P)^2^+4.4268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 3018 Friedel pairs' _refine_ls_abs_structure_Flack 0.03(6) _refine_ls_number_reflns 6396 _refine_ls_number_parameters 343 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1109 _refine_ls_goodness_of_fit_ref 1.313 _refine_ls_restrained_S_all 1.313 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7620(2) 0.0186(3) 0.6028(4) 0.0376(11) Uani 1 1 d . . . H1A H 0.7101 0.0296 0.6226 0.045 Uiso 1 1 calc R . . H1B H 0.7655 -0.0363 0.5527 0.045 Uiso 1 1 calc R . . C2 C 0.7928(2) 0.0932(3) 0.5281(4) 0.0395(12) Uani 1 1 d . . . H2A H 0.8456 0.0838 0.5138 0.047 Uiso 1 1 calc R . . H2B H 0.7686 0.0968 0.4436 0.047 Uiso 1 1 calc R . . C3 C 0.8071(2) 0.2465(3) 0.5264(4) 0.0411(12) Uani 1 1 d . . . H3A H 0.7810 0.2504 0.4436 0.049 Uiso 1 1 calc R . . H3B H 0.8598 0.2404 0.5087 0.049 Uiso 1 1 calc R . . C4 C 0.7933(2) 0.3278(3) 0.6043(4) 0.0424(12) Uani 1 1 d . . . H4A H 0.8038 0.3806 0.5523 0.051 Uiso 1 1 calc R . . H4B H 0.7417 0.3300 0.6313 0.051 Uiso 1 1 calc R . . C5 C 0.8319(2) 0.4039(3) 0.7881(5) 0.0425(12) Uani 1 1 d . . . H5A H 0.7804 0.4113 0.8142 0.051 Uiso 1 1 calc R . . H5B H 0.8463 0.4554 0.7364 0.051 Uiso 1 1 calc R . . C6 C 0.8792(2) 0.3970(3) 0.9036(4) 0.0349(11) Uani 1 1 d . . . H6A H 0.9303 0.3857 0.8782 0.042 Uiso 1 1 calc R . . H6B H 0.8774 0.4521 0.9535 0.042 Uiso 1 1 calc R . . C7 C 0.8912(2) 0.3134(3) 1.0942(4) 0.0355(11) Uani 1 1 d . . . H7A H 0.8902 0.3679 1.1454 0.043 Uiso 1 1 calc R . . H7B H 0.9426 0.2988 1.0750 0.043 Uiso 1 1 calc R . . C8 C 0.8568(2) 0.2410(3) 1.1671(4) 0.0337(11) Uani 1 1 d . . . H8A H 0.8777 0.2381 1.2543 0.040 Uiso 1 1 calc R . . H8B H 0.8037 0.2513 1.1747 0.040 Uiso 1 1 calc R . . C9 C 0.8453(2) 0.0859(3) 1.1715(4) 0.0304(10) Uani 1 1 d . . . H9A H 0.7922 0.0903 1.1871 0.036 Uiso 1 1 calc R . . H9B H 0.8703 0.0834 1.2554 0.036 Uiso 1 1 calc R . . C10 C 0.8616(2) 0.0052(3) 1.0964(4) 0.0301(9) Uani 1 1 d . . . H10A H 0.9132 0.0056 1.0685 0.036 Uiso 1 1 calc R . . H10B H 0.8534 -0.0474 1.1498 0.036 Uiso 1 1 calc R . . C11 C 0.8307(2) -0.0688(3) 0.9060(4) 0.0337(11) Uani 1 1 d . . . H11A H 0.8222 -0.1245 0.9523 0.040 Uiso 1 1 calc R . . H11B H 0.8825 -0.0668 0.8795 0.040 Uiso 1 1 calc R . . C12 C 0.7824(2) -0.0640(3) 0.7904(5) 0.0352(11) Uani 1 1 d . . . H12A H 0.7880 -0.1176 0.7380 0.042 Uiso 1 1 calc R . . H12B H 0.7308 -0.0592 0.8170 0.042 Uiso 1 1 calc R . . C13 C 0.5961(2) 0.1173(3) 0.9685(4) 0.0244(8) Uani 1 1 d . . . C14 C 0.6010(2) 0.0972(3) 0.8378(4) 0.0265(9) Uani 1 1 d . . . H14 H 0.6217 0.1389 0.7810 0.032 Uiso 1 1 calc R . . C15 C 0.5761(2) 0.0177(3) 0.7891(4) 0.0310(10) Uani 1 1 d . . . H15 H 0.5791 0.0068 0.6997 0.037 Uiso 1 1 calc R . . C16 C 0.5471(2) -0.0458(3) 0.8693(5) 0.0372(10) Uani 1 1 d . . . H16 H 0.5296 -0.0998 0.8361 0.045 Uiso 1 1 calc R . . C17 C 0.5445(2) -0.0280(3) 0.9988(4) 0.0329(10) Uani 1 1 d . . . H17 H 0.5271 -0.0717 1.0559 0.040 Uiso 1 1 calc R . . C18 C 0.5667(2) 0.0520(3) 1.0471(4) 0.0280(9) Uani 1 1 d . . . H18 H 0.5619 0.0629 1.1363 0.034 Uiso 1 1 calc R . . C19 C 0.5673(2) 0.3103(3) 0.9376(3) 0.0221(8) Uani 1 1 d . . . C20 C 0.5204(2) 0.2893(3) 0.8360(3) 0.0254(9) Uani 1 1 d . . . H20 H 0.5147 0.2295 0.8129 0.030 Uiso 1 1 calc R . . C21 C 0.4817(2) 0.3525(3) 0.7676(4) 0.0313(10) Uani 1 1 d . . . H21 H 0.4513 0.3353 0.6984 0.038 Uiso 1 1 calc R . . C22 C 0.4873(2) 0.4397(3) 0.7997(4) 0.0271(9) Uani 1 1 d . . . H22 H 0.4612 0.4830 0.7534 0.033 Uiso 1 1 calc R . . C23 C 0.5323(2) 0.4628(3) 0.9018(4) 0.0295(10) Uani 1 1 d . . . H23 H 0.5361 0.5226 0.9264 0.035 Uiso 1 1 calc R . . C24 C 0.5720(2) 0.3995(3) 0.9684(4) 0.0290(9) Uani 1 1 d . . . H24 H 0.6030 0.4173 1.0364 0.035 Uiso 1 1 calc R . . C25 C 0.5982(2) 0.2341(3) 1.1994(4) 0.0241(8) Uani 1 1 d . . . C26 C 0.6348(2) 0.1828(3) 1.2918(4) 0.0275(9) Uani 1 1 d . . . H26 H 0.6740 0.1465 1.2651 0.033 Uiso 1 1 calc R . . C27 C 0.6154(2) 0.1834(3) 1.4208(4) 0.0305(10) Uani 1 1 d . . . H27 H 0.6408 0.1473 1.4798 0.037 Uiso 1 1 calc R . . C28 C 0.5597(2) 0.2358(3) 1.4627(4) 0.0269(9) Uani 1 1 d . . . H28 H 0.5468 0.2367 1.5507 0.032 Uiso 1 1 calc R . . C29 C 0.5224(2) 0.2874(3) 1.3754(4) 0.0269(8) Uani 1 1 d . . . H29 H 0.4836 0.3238 1.4036 0.032 Uiso 1 1 calc R . . C30 C 0.5418(2) 0.2861(3) 1.2460(4) 0.0238(9) Uani 1 1 d . . . H30 H 0.5156 0.3220 1.1877 0.029 Uiso 1 1 calc R . . O1 O 0.80301(15) 0.0110(2) 0.7182(3) 0.0308(7) Uani 1 1 d . . . O2 O 0.78183(15) 0.1726(2) 0.5967(2) 0.0320(7) Uani 1 1 d . . . O3 O 0.83974(16) 0.3257(2) 0.7141(3) 0.0337(7) Uani 1 1 d . . . O4 O 0.85168(15) 0.32556(19) 0.9782(3) 0.0283(7) Uani 1 1 d . . . O5 O 0.86982(15) 0.16015(17) 1.1010(2) 0.0244(6) Uani 1 1 d . . . O6 O 0.81474(15) 0.0038(2) 0.9878(3) 0.0283(7) Uani 1 1 d . . . Si1 Si 0.63227(6) 0.22979(7) 1.02363(11) 0.0244(2) Uani 1 1 d . . . K1 K 0.80219(4) 0.17146(5) 0.86649(8) 0.02279(16) 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 0.031(2) 0.051(3) 0.031(2) -0.021(2) -0.0064(19) 0.007(2) C2 0.032(2) 0.072(3) 0.0142(18) -0.017(2) -0.0034(18) 0.015(2) C3 0.033(2) 0.078(4) 0.0123(18) 0.015(2) 0.0035(19) 0.008(2) C4 0.036(2) 0.058(3) 0.033(2) 0.024(3) -0.003(2) 0.005(2) C5 0.034(2) 0.030(3) 0.064(3) 0.017(2) 0.006(2) 0.005(2) C6 0.032(2) 0.025(2) 0.048(3) 0.002(2) 0.009(2) -0.0018(19) C7 0.034(2) 0.034(2) 0.038(2) -0.018(2) -0.010(2) -0.002(2) C8 0.027(2) 0.051(3) 0.023(2) -0.011(2) -0.0011(17) 0.001(2) C9 0.033(2) 0.046(3) 0.0115(18) 0.0124(18) 0.0037(16) 0.003(2) C10 0.029(2) 0.036(2) 0.026(2) 0.0133(19) -0.0014(18) 0.0035(19) C11 0.030(2) 0.022(2) 0.049(3) 0.0007(19) 0.010(2) 0.0043(18) C12 0.032(2) 0.024(2) 0.050(3) -0.007(2) 0.005(2) -0.0037(19) C13 0.0204(18) 0.030(2) 0.022(2) -0.0057(17) -0.0022(16) 0.0044(17) C14 0.025(2) 0.031(2) 0.024(2) -0.0088(17) 0.0024(15) 0.0003(17) C15 0.025(2) 0.036(2) 0.031(2) -0.015(2) 0.0025(17) 0.0016(19) C16 0.029(2) 0.032(2) 0.051(3) -0.013(2) 0.004(2) -0.0014(18) C17 0.032(2) 0.025(2) 0.041(3) -0.002(2) 0.0038(19) 0.0002(18) C18 0.028(2) 0.027(2) 0.029(2) 0.0004(17) -0.0016(17) 0.0013(17) C19 0.0238(19) 0.028(2) 0.0143(18) -0.0018(16) 0.0037(15) -0.0041(16) C20 0.026(2) 0.030(2) 0.021(2) -0.0069(16) 0.0009(15) 0.0049(17) C21 0.029(2) 0.047(3) 0.0177(19) 0.0002(19) 0.0041(17) 0.009(2) C22 0.031(2) 0.035(2) 0.0155(19) 0.0098(17) 0.0066(16) 0.0094(19) C23 0.033(2) 0.025(2) 0.030(2) 0.0049(17) 0.0108(17) -0.0019(18) C24 0.023(2) 0.031(2) 0.033(2) -0.0055(19) 0.0055(18) -0.0050(17) C25 0.0197(18) 0.025(2) 0.028(2) -0.0042(17) -0.0045(16) -0.0023(17) C26 0.0219(19) 0.031(2) 0.029(2) -0.0022(19) -0.0041(17) 0.0051(18) C27 0.028(2) 0.037(3) 0.027(2) 0.002(2) -0.0041(17) -0.0005(19) C28 0.032(2) 0.030(2) 0.0185(18) -0.0004(17) 0.0007(17) -0.0068(18) C29 0.0282(19) 0.026(2) 0.027(2) -0.0063(19) 0.0032(19) -0.0024(16) C30 0.0188(19) 0.026(2) 0.027(2) -0.0005(18) -0.0042(15) 0.0006(16) O1 0.0278(15) 0.0354(18) 0.0292(16) -0.0100(14) -0.0067(13) -0.0022(14) O2 0.0341(16) 0.0528(19) 0.0092(12) 0.0004(14) 0.0015(11) 0.0082(15) O3 0.0330(16) 0.0378(18) 0.0302(17) 0.0116(14) -0.0015(13) 0.0068(14) O4 0.0272(15) 0.0272(16) 0.0306(15) -0.0033(13) -0.0002(12) -0.0036(12) O5 0.0306(15) 0.0303(15) 0.0124(12) 0.0019(12) 0.0035(11) 0.0006(12) O6 0.0260(14) 0.0310(17) 0.0278(16) 0.0050(13) 0.0009(12) 0.0066(12) Si1 0.0202(5) 0.0285(6) 0.0244(5) -0.0040(5) 0.0010(4) 0.0004(5) K1 0.0285(4) 0.0283(4) 0.0116(3) 0.0003(4) -0.0016(4) 0.0003(4) _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 O1 1.425(5) . ? C1 C2 1.492(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.423(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O2 1.423(5) . ? C3 C4 1.505(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.429(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O3 1.429(6) . ? C5 C6 1.490(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.432(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O4 1.424(5) . ? C7 C8 1.483(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O5 1.434(5) . ? C8 K1 3.463(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 O5 1.426(5) . ? C9 C10 1.490(6) . ? C9 K1 3.534(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 O6 1.424(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O6 1.429(5) . ? C11 C12 1.500(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O1 1.423(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.400(6) . ? C13 C14 1.403(5) . ? C13 Si1 1.929(4) . ? C14 C15 1.393(5) . ? C14 H14 0.9500 . ? C15 C16 1.387(6) . ? C15 H15 0.9500 . ? C16 C17 1.381(7) . ? C16 H16 0.9500 . ? C17 C18 1.383(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.402(5) . ? C19 C20 1.403(5) . ? C19 Si1 1.934(4) . ? C20 C21 1.395(6) . ? C20 H20 0.9500 . ? C21 C22 1.375(6) . ? C21 K1 3.472(4) 4_455 ? C21 H21 0.9500 . ? C22 C23 1.395(6) . ? C22 H22 0.9500 . ? C23 C24 1.396(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.391(5) . ? C25 C26 1.413(6) . ? C25 Si1 1.941(4) . ? C26 C27 1.393(5) . ? C26 H26 0.9500 . ? C27 C28 1.369(6) . ? C27 H27 0.9500 . ? C28 C29 1.386(6) . ? C28 H28 0.9500 . ? C29 C30 1.399(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? O1 K1 2.898(3) . ? O2 K1 2.844(3) . ? O3 K1 2.925(3) . ? O4 K1 2.778(3) . ? O5 K1 2.752(3) . ? O6 K1 2.866(3) . ? Si1 K1 3.6349(13) . ? K1 C21 3.472(4) 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 O1 C1 C2 107.7(4) . . ? O1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? O1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? O2 C2 C1 109.4(3) . . ? O2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? O2 C3 C4 108.7(3) . . ? O2 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? O2 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? O3 C4 C3 108.4(4) . . ? O3 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? O3 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? O3 C5 C6 108.7(4) . . ? O3 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? O3 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.3 . . ? O4 C6 C5 106.8(4) . . ? O4 C6 H6A 110.4 . . ? C5 C6 H6A 110.4 . . ? O4 C6 H6B 110.4 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? O4 C7 C8 108.5(3) . . ? O4 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O4 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? O5 C8 C7 108.8(3) . . ? O5 C8 K1 49.31(17) . . ? C7 C8 K1 83.4(2) . . ? O5 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? K1 C8 H8A 159.0 . . ? O5 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? K1 C8 H8B 80.7 . . ? H8A C8 H8B 108.3 . . ? O5 C9 C10 108.7(3) . . ? O5 C9 K1 46.40(16) . . ? C10 C9 K1 82.8(2) . . ? O5 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? K1 C9 H9A 84.4 . . ? O5 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? K1 C9 H9B 156.3 . . ? H9A C9 H9B 108.3 . . ? O6 C10 C9 108.1(3) . . ? O6 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O6 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? O6 C11 C12 108.8(3) . . ? O6 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O6 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O1 C12 C11 108.0(3) . . ? O1 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O1 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C18 C13 C14 116.1(4) . . ? C18 C13 Si1 126.3(3) . . ? C14 C13 Si1 117.6(3) . . ? C15 C14 C13 121.7(4) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C16 C15 C14 120.9(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 117.9(4) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 C18 121.4(4) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 121.9(4) . . ? C17 C18 H18 119.1 . . ? C13 C18 H18 119.1 . . ? C24 C19 C20 115.7(4) . . ? C24 C19 Si1 118.2(3) . . ? C20 C19 Si1 125.8(3) . . ? C21 C20 C19 122.8(4) . . ? C21 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? C22 C21 C20 120.4(4) . . ? C22 C21 K1 95.8(3) . 4_455 ? C20 C21 K1 104.9(3) . 4_455 ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? K1 C21 H21 68.9 4_455 . ? C21 C22 C23 118.4(4) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? C22 C23 C24 121.0(4) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C19 121.7(4) . . ? C23 C24 H24 119.1 . . ? C19 C24 H24 119.1 . . ? C30 C25 C26 115.5(4) . . ? C30 C25 Si1 126.1(3) . . ? C26 C25 Si1 118.3(3) . . ? C27 C26 C25 122.4(4) . . ? C27 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C28 C27 C26 120.2(4) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 119.4(4) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 120.1(4) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 122.4(4) . . ? C25 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? C12 O1 C1 111.9(3) . . ? C12 O1 K1 113.3(2) . . ? C1 O1 K1 112.4(2) . . ? C2 O2 C3 111.6(3) . . ? C2 O2 K1 118.4(2) . . ? C3 O2 K1 118.3(2) . . ? C5 O3 C4 110.8(3) . . ? C5 O3 K1 110.7(3) . . ? C4 O3 K1 108.3(3) . . ? C7 O4 C6 112.5(3) . . ? C7 O4 K1 114.4(2) . . ? C6 O4 K1 122.1(2) . . ? C9 O5 C8 112.5(3) . . ? C9 O5 K1 111.6(2) . . ? C8 O5 K1 107.4(2) . . ? C10 O6 C11 111.4(3) . . ? C10 O6 K1 112.8(2) . . ? C11 O6 K1 116.4(2) . . ? C13 Si1 C19 102.36(17) . . ? C13 Si1 C25 101.65(18) . . ? C19 Si1 C25 102.69(17) . . ? C13 Si1 K1 86.71(12) . . ? C19 Si1 K1 118.35(11) . . ? C25 Si1 K1 135.38(12) . . ? O5 K1 O4 62.07(8) . . ? O5 K1 O2 160.43(8) . . ? O4 K1 O2 117.01(9) . . ? O5 K1 O6 60.92(8) . . ? O4 K1 O6 122.96(9) . . ? O2 K1 O6 117.04(9) . . ? O5 K1 O1 114.88(9) . . ? O4 K1 O1 159.76(9) . . ? O2 K1 O1 58.39(9) . . ? O6 K1 O1 58.76(8) . . ? O5 K1 O3 115.39(8) . . ? O4 K1 O3 58.00(9) . . ? O2 K1 O3 59.09(9) . . ? O6 K1 O3 160.22(9) . . ? O1 K1 O3 112.83(9) . . ? O5 K1 C8 23.26(9) . . ? O4 K1 C8 42.71(10) . . ? O2 K1 C8 159.25(11) . . ? O6 K1 C8 81.33(10) . . ? O1 K1 C8 137.93(10) . . ? O3 K1 C8 100.30(10) . . ? O5 K1 C21 80.23(9) . 4 ? O4 K1 C21 84.50(10) . 4 ? O2 K1 C21 80.24(9) . 4 ? O6 K1 C21 87.77(10) . 4 ? O1 K1 C21 75.33(9) . 4 ? O3 K1 C21 72.51(10) . 4 ? C8 K1 C21 91.58(10) . 4 ? O5 K1 C9 22.03(9) . . ? O4 K1 C9 82.01(10) . . ? O2 K1 C9 157.77(10) . . ? O6 K1 C9 41.65(10) . . ? O1 K1 C9 99.71(10) . . ? O3 K1 C9 137.38(10) . . ? C8 K1 C9 39.71(11) . . ? C21 K1 C9 90.97(10) 4 . ? O5 K1 Si1 90.01(6) . . ? O4 K1 Si1 83.30(6) . . ? O2 K1 Si1 109.48(6) . . ? O6 K1 Si1 95.05(6) . . ? O1 K1 Si1 116.94(7) . . ? O3 K1 Si1 104.52(7) . . ? C8 K1 Si1 76.32(7) . . ? C21 K1 Si1 166.97(8) 4 . ? C9 K1 Si1 82.83(7) . . ? 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 O1 C1 C2 O2 -64.7(4) . . . . ? O2 C3 C4 O3 67.8(4) . . . . ? O3 C5 C6 O4 -64.0(4) . . . . ? O4 C7 C8 O5 69.4(4) . . . . ? O4 C7 C8 K1 26.6(3) . . . . ? O5 C9 C10 O6 -70.0(4) . . . . ? K1 C9 C10 O6 -30.9(3) . . . . ? O6 C11 C12 O1 67.0(4) . . . . ? C18 C13 C14 C15 1.7(6) . . . . ? Si1 C13 C14 C15 -179.9(3) . . . . ? C13 C14 C15 C16 -1.6(6) . . . . ? C14 C15 C16 C17 -0.8(6) . . . . ? C15 C16 C17 C18 3.1(6) . . . . ? C16 C17 C18 C13 -3.1(6) . . . . ? C14 C13 C18 C17 0.6(6) . . . . ? Si1 C13 C18 C17 -177.7(3) . . . . ? C24 C19 C20 C21 1.3(5) . . . . ? Si1 C19 C20 C21 -171.7(3) . . . . ? C19 C20 C21 C22 -1.3(6) . . . . ? C19 C20 C21 K1 -107.3(4) . . . 4_455 ? C20 C21 C22 C23 -0.1(6) . . . . ? K1 C21 C22 C23 111.0(3) 4_455 . . . ? C21 C22 C23 C24 1.3(6) . . . . ? C22 C23 C24 C19 -1.3(6) . . . . ? C20 C19 C24 C23 0.0(6) . . . . ? Si1 C19 C24 C23 173.5(3) . . . . ? C30 C25 C26 C27 0.5(6) . . . . ? Si1 C25 C26 C27 178.4(3) . . . . ? C25 C26 C27 C28 -0.9(7) . . . . ? C26 C27 C28 C29 0.7(7) . . . . ? C27 C28 C29 C30 -0.3(6) . . . . ? C26 C25 C30 C29 -0.1(6) . . . . ? Si1 C25 C30 C29 -177.7(3) . . . . ? C28 C29 C30 C25 0.0(6) . . . . ? C11 C12 O1 C1 177.2(3) . . . . ? C11 C12 O1 K1 -54.4(4) . . . . ? C2 C1 O1 C12 -174.2(3) . . . . ? C2 C1 O1 K1 57.0(4) . . . . ? C1 C2 O2 C3 -177.1(3) . . . . ? C1 C2 O2 K1 40.4(4) . . . . ? C4 C3 O2 C2 179.7(3) . . . . ? C4 C3 O2 K1 -37.7(4) . . . . ? C6 C5 O3 C4 178.0(3) . . . . ? C6 C5 O3 K1 57.7(4) . . . . ? C3 C4 O3 C5 176.8(4) . . . . ? C3 C4 O3 K1 -61.5(4) . . . . ? C8 C7 O4 C6 177.5(3) . . . . ? C8 C7 O4 K1 -37.4(4) . . . . ? C5 C6 O4 C7 -178.3(3) . . . . ? C5 C6 O4 K1 39.7(4) . . . . ? C10 C9 O5 C8 -179.5(3) . . . . ? K1 C9 O5 C8 120.8(3) . . . . ? C10 C9 O5 K1 59.7(3) . . . . ? C7 C8 O5 C9 173.8(3) . . . . ? K1 C8 O5 C9 -123.2(3) . . . . ? C7 C8 O5 K1 -63.1(3) . . . . ? C9 C10 O6 C11 175.9(3) . . . . ? C9 C10 O6 K1 43.0(3) . . . . ? C12 C11 O6 C10 -177.0(3) . . . . ? C12 C11 O6 K1 -45.9(4) . . . . ? C18 C13 Si1 C19 -117.3(3) . . . . ? C14 C13 Si1 C19 64.4(3) . . . . ? C18 C13 Si1 C25 -11.3(4) . . . . ? C14 C13 Si1 C25 170.4(3) . . . . ? C18 C13 Si1 K1 124.4(3) . . . . ? C14 C13 Si1 K1 -53.9(3) . . . . ? C24 C19 Si1 C13 172.3(3) . . . . ? C20 C19 Si1 C13 -15.0(4) . . . . ? C24 C19 Si1 C25 67.1(3) . . . . ? C20 C19 Si1 C25 -120.1(3) . . . . ? C24 C19 Si1 K1 -94.8(3) . . . . ? C20 C19 Si1 K1 78.0(3) . . . . ? C30 C25 Si1 C13 -107.4(4) . . . . ? C26 C25 Si1 C13 75.0(3) . . . . ? C30 C25 Si1 C19 -1.7(4) . . . . ? C26 C25 Si1 C19 -179.3(3) . . . . ? C30 C25 Si1 K1 155.4(3) . . . . ? C26 C25 Si1 K1 -22.2(4) . . . . ? C9 O5 K1 O4 152.9(3) . . . . ? C8 O5 K1 O4 29.2(2) . . . . ? C9 O5 K1 O2 -114.6(3) . . . . ? C8 O5 K1 O2 121.7(3) . . . . ? C9 O5 K1 O6 -25.2(2) . . . . ? C8 O5 K1 O6 -149.0(2) . . . . ? C9 O5 K1 O1 -49.4(3) . . . . ? C8 O5 K1 O1 -173.2(2) . . . . ? C9 O5 K1 O3 176.7(2) . . . . ? C8 O5 K1 O3 52.9(2) . . . . ? C9 O5 K1 C8 123.7(3) . . . . ? C9 O5 K1 C21 -118.1(2) . . . 4 ? C8 O5 K1 C21 118.1(2) . . . 4 ? C8 O5 K1 C9 -123.7(3) . . . . ? C9 O5 K1 Si1 70.5(2) . . . . ? C8 O5 K1 Si1 -53.2(2) . . . . ? C7 O4 K1 O5 4.8(2) . . . . ? C6 O4 K1 O5 146.2(3) . . . . ? C7 O4 K1 O2 -153.1(2) . . . . ? C6 O4 K1 O2 -11.7(3) . . . . ? C7 O4 K1 O6 6.7(3) . . . . ? C6 O4 K1 O6 148.1(3) . . . . ? C7 O4 K1 O1 -81.7(4) . . . . ? C6 O4 K1 O1 59.7(4) . . . . ? C7 O4 K1 O3 -149.8(3) . . . . ? C6 O4 K1 O3 -8.4(2) . . . . ? C7 O4 K1 C8 21.3(2) . . . . ? C6 O4 K1 C8 162.7(3) . . . . ? C7 O4 K1 C21 -77.0(3) . . . 4 ? C6 O4 K1 C21 64.3(3) . . . 4 ? C7 O4 K1 C9 14.8(3) . . . . ? C6 O4 K1 C9 156.1(3) . . . . ? C7 O4 K1 Si1 98.4(2) . . . . ? C6 O4 K1 Si1 -120.2(3) . . . . ? C2 O2 K1 O5 66.6(4) . . . . ? C3 O2 K1 O5 -73.4(4) . . . . ? C2 O2 K1 O4 148.8(3) . . . . ? C3 O2 K1 O4 8.8(3) . . . . ? C2 O2 K1 O6 -12.2(3) . . . . ? C3 O2 K1 O6 -152.3(2) . . . . ? C2 O2 K1 O1 -8.5(3) . . . . ? C3 O2 K1 O1 -148.6(3) . . . . ? C2 O2 K1 O3 145.6(3) . . . . ? C3 O2 K1 O3 5.5(2) . . . . ? C2 O2 K1 C8 138.1(3) . . . . ? C3 O2 K1 C8 -1.9(4) . . . . ? C2 O2 K1 C21 70.2(3) . . . 4 ? C3 O2 K1 C21 -69.9(3) . . . 4 ? C2 O2 K1 C9 2.2(4) . . . . ? C3 O2 K1 C9 -137.8(3) . . . . ? C2 O2 K1 Si1 -118.8(3) . . . . ? C3 O2 K1 Si1 101.1(3) . . . . ? C10 O6 K1 O5 -10.4(2) . . . . ? C11 O6 K1 O5 -140.8(3) . . . . ? C10 O6 K1 O4 -12.3(3) . . . . ? C11 O6 K1 O4 -142.7(2) . . . . ? C10 O6 K1 O2 147.5(2) . . . . ? C11 O6 K1 O2 17.1(3) . . . . ? C10 O6 K1 O1 143.9(3) . . . . ? C11 O6 K1 O1 13.4(2) . . . . ? C10 O6 K1 O3 74.1(4) . . . . ? C11 O6 K1 O3 -56.4(4) . . . . ? C10 O6 K1 C8 -22.2(2) . . . . ? C11 O6 K1 C8 -152.7(3) . . . . ? C10 O6 K1 C21 69.7(2) . . . 4 ? C11 O6 K1 C21 -60.8(3) . . . 4 ? C10 O6 K1 C9 -24.3(2) . . . . ? C11 O6 K1 C9 -154.7(3) . . . . ? C10 O6 K1 Si1 -97.6(2) . . . . ? C11 O6 K1 Si1 132.0(2) . . . . ? C12 O1 K1 O5 46.9(3) . . . . ? C1 O1 K1 O5 175.0(3) . . . . ? C12 O1 K1 O4 123.4(3) . . . . ? C1 O1 K1 O4 -108.5(3) . . . . ? C12 O1 K1 O2 -154.0(3) . . . . ? C1 O1 K1 O2 -25.9(3) . . . . ? C12 O1 K1 O6 22.2(2) . . . . ? C1 O1 K1 O6 150.3(3) . . . . ? C12 O1 K1 O3 -178.0(2) . . . . ? C1 O1 K1 O3 -49.9(3) . . . . ? C12 O1 K1 C8 42.9(3) . . . . ? C1 O1 K1 C8 171.0(3) . . . . ? C12 O1 K1 C21 118.6(3) . . . 4 ? C1 O1 K1 C21 -113.3(3) . . . 4 ? C12 O1 K1 C9 30.1(3) . . . . ? C1 O1 K1 C9 158.2(3) . . . . ? C12 O1 K1 Si1 -56.7(3) . . . . ? C1 O1 K1 Si1 71.4(3) . . . . ? C5 O3 K1 O5 -50.7(3) . . . . ? C4 O3 K1 O5 -172.4(3) . . . . ? C5 O3 K1 O4 -25.9(2) . . . . ? C4 O3 K1 O4 -147.6(3) . . . . ? C5 O3 K1 O2 150.7(3) . . . . ? C4 O3 K1 O2 28.9(3) . . . . ? C5 O3 K1 O6 -125.0(3) . . . . ? C4 O3 K1 O6 113.3(3) . . . . ? C5 O3 K1 O1 174.5(2) . . . . ? C4 O3 K1 O1 52.7(3) . . . . ? C5 O3 K1 C8 -32.0(3) . . . . ? C4 O3 K1 C8 -153.7(3) . . . . ? C5 O3 K1 C21 -120.4(3) . . . 4 ? C4 O3 K1 C21 117.9(3) . . . 4 ? C5 O3 K1 C9 -48.8(3) . . . . ? C4 O3 K1 C9 -170.6(3) . . . . ? C5 O3 K1 Si1 46.4(3) . . . . ? C4 O3 K1 Si1 -75.3(3) . . . . ? C7 C8 K1 O5 121.8(4) . . . . ? O5 C8 K1 O4 -140.5(3) . . . . ? C7 C8 K1 O4 -18.7(2) . . . . ? O5 C8 K1 O2 -126.4(3) . . . . ? C7 C8 K1 O2 -4.6(4) . . . . ? O5 C8 K1 O6 27.1(2) . . . . ? C7 C8 K1 O6 149.0(3) . . . . ? O5 C8 K1 O1 9.3(3) . . . . ? C7 C8 K1 O1 131.1(2) . . . . ? O5 C8 K1 O3 -132.9(2) . . . . ? C7 C8 K1 O3 -11.1(3) . . . . ? O5 C8 K1 C21 -60.4(2) . . . 4 ? C7 C8 K1 C21 61.5(3) . . . 4 ? O5 C8 K1 C9 29.2(2) . . . . ? C7 C8 K1 C9 151.1(3) . . . . ? O5 C8 K1 Si1 124.5(2) . . . . ? C7 C8 K1 Si1 -113.6(3) . . . . ? C10 C9 K1 O5 -124.5(4) . . . . ? O5 C9 K1 O4 -23.9(2) . . . . ? C10 C9 K1 O4 -148.4(2) . . . . ? O5 C9 K1 O2 126.4(3) . . . . ? C10 C9 K1 O2 1.9(4) . . . . ? O5 C9 K1 O6 145.9(3) . . . . ? C10 C9 K1 O6 21.4(2) . . . . ? O5 C9 K1 O1 135.6(2) . . . . ? C10 C9 K1 O1 11.2(2) . . . . ? O5 C9 K1 O3 -4.5(3) . . . . ? C10 C9 K1 O3 -128.9(2) . . . . ? O5 C9 K1 C8 -30.9(2) . . . . ? C10 C9 K1 C8 -155.4(3) . . . . ? O5 C9 K1 C21 60.4(2) . . . 4 ? C10 C9 K1 C21 -64.1(2) . . . 4 ? O5 C9 K1 Si1 -108.1(2) . . . . ? C10 C9 K1 Si1 127.4(2) . . . . ? C13 Si1 K1 O5 -111.46(13) . . . . ? C19 Si1 K1 O5 146.26(15) . . . . ? C25 Si1 K1 O5 -8.2(2) . . . . ? C13 Si1 K1 O4 -173.32(14) . . . . ? C19 Si1 K1 O4 84.40(15) . . . . ? C25 Si1 K1 O4 -70.0(2) . . . . ? C13 Si1 K1 O2 70.36(14) . . . . ? C19 Si1 K1 O2 -31.92(16) . . . . ? C25 Si1 K1 O2 173.64(19) . . . . ? C13 Si1 K1 O6 -50.67(14) . . . . ? C19 Si1 K1 O6 -152.95(15) . . . . ? C25 Si1 K1 O6 52.6(2) . . . . ? C13 Si1 K1 O1 6.71(14) . . . . ? C19 Si1 K1 O1 -95.57(16) . . . . ? C25 Si1 K1 O1 110.0(2) . . . . ? C13 Si1 K1 O3 132.25(14) . . . . ? C19 Si1 K1 O3 29.96(15) . . . . ? C25 Si1 K1 O3 -124.5(2) . . . . ? C13 Si1 K1 C8 -130.45(15) . . . . ? C19 Si1 K1 C8 127.27(16) . . . . ? C25 Si1 K1 C8 -27.2(2) . . . . ? C13 Si1 K1 C21 -152.7(4) . . . 4 ? C19 Si1 K1 C21 105.0(4) . . . 4 ? C25 Si1 K1 C21 -49.4(4) . . . 4 ? C13 Si1 K1 C9 -90.57(15) . . . . ? C19 Si1 K1 C9 167.15(16) . . . . ? C25 Si1 K1 C9 12.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.310 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.074 _exptl_crystal_recrystallization_method ; From solution in PhMe layered with n-pentane at -20 deg C. ; data_ck23ck _database_code_depnum_ccdc_archive 'CCDC 924394' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '18-Crown-6-potassium triphenyl-germanium' _chemical_melting_point ? _chemical_formula_moiety 'C30 H39 Ge K O6' _chemical_formula_sum 'C30 H39 Ge K O6' _chemical_formula_weight 607.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_int_tables_number 14 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 9.8669(1) _cell_length_b 17.2748(2) _cell_length_c 17.9326(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.857(1) _cell_angle_gamma 90.00 _cell_volume 3011.47(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 57011 _cell_measurement_theta_min 3.58 _cell_measurement_theta_max 75.72 _exptl_crystal_description 'fragment of needle' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 2.940 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.20429 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; The collected data cover nominally a full sphere of the reciprocal space. A combination of 70 sets of \w scans were used; each set at different \j, 2\q or \k angles and each scan 1.5 deg in \w. Each frame was exposured for 5 s (low 2\q angles) or 10 s (high 2\q angles). Nominal crystal to detector distance 55 mm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction, Xcalibur, Atlas, Nova' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77176 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0099 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 75.91 _reflns_number_total 6263 _reflns_number_gt 6118 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution ; SHELXS-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122) ; _computing_structure_refinement ; SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 122-122)' ; _computing_molecular_graphics ; Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany. ; _computing_publication_material ; WinGX v1.80.05 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.) ; _refine_special_details ; All H atoms were refined using a riding model, with a common U restrained to be 1.2 times the equivalent isotropic displacement parameter of the parent atom. 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^)+(0.0342P)^2^+1.2242P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6263 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.003 _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 C1 C 0.56124(13) 0.30841(7) 0.65323(7) 0.0246(2) Uani 1 1 d . . . C2 C 0.44974(14) 0.35920(8) 0.64698(8) 0.0319(3) Uani 1 1 d . . . H2 H 0.4600 0.4063 0.6748 0.038 Uiso 1 1 calc R . . C3 C 0.32370(15) 0.34302(10) 0.60113(9) 0.0395(3) Uani 1 1 d . . . H3 H 0.2505 0.3794 0.5969 0.047 Uiso 1 1 calc R . . C4 C 0.30596(16) 0.27400(11) 0.56194(8) 0.0424(4) Uani 1 1 d . . . H4 H 0.2210 0.2630 0.5300 0.051 Uiso 1 1 calc R . . C5 C 0.41196(16) 0.22117(10) 0.56933(8) 0.0412(4) Uani 1 1 d . . . H5 H 0.3990 0.1728 0.5439 0.049 Uiso 1 1 calc R . . C6 C 0.53848(14) 0.23853(8) 0.61410(8) 0.0312(3) Uani 1 1 d . . . H6 H 0.6110 0.2018 0.6180 0.037 Uiso 1 1 calc R . . C7 C 0.68526(12) 0.38165(8) 0.80387(7) 0.0252(2) Uani 1 1 d . . . C8 C 0.59693(14) 0.33971(8) 0.84254(8) 0.0303(3) Uani 1 1 d . . . H8 H 0.5554 0.2938 0.8201 0.036 Uiso 1 1 calc R . . C9 C 0.56806(14) 0.36274(9) 0.91214(8) 0.0353(3) Uani 1 1 d . . . H9 H 0.5085 0.3324 0.9367 0.042 Uiso 1 1 calc R . . C10 C 0.62556(15) 0.42963(9) 0.94590(8) 0.0363(3) Uani 1 1 d . . . H10 H 0.6067 0.4454 0.9938 0.044 Uiso 1 1 calc R . . C11 C 0.71134(15) 0.47360(9) 0.90877(8) 0.0355(3) Uani 1 1 d . . . H11 H 0.7507 0.5200 0.9312 0.043 Uiso 1 1 calc R . . C12 C 0.74028(13) 0.44994(8) 0.83842(7) 0.0295(3) Uani 1 1 d . . . H12 H 0.7986 0.4810 0.8137 0.035 Uiso 1 1 calc R . . C13 C 0.81302(13) 0.41994(7) 0.66147(7) 0.0245(2) Uani 1 1 d . . . C14 C 0.95318(13) 0.42618(8) 0.65802(8) 0.0294(3) Uani 1 1 d . . . H14 H 1.0148 0.3882 0.6825 0.035 Uiso 1 1 calc R . . C15 C 1.00501(15) 0.48674(9) 0.61951(9) 0.0361(3) Uani 1 1 d . . . H15 H 1.1008 0.4896 0.6184 0.043 Uiso 1 1 calc R . . C16 C 0.91714(16) 0.54251(8) 0.58305(8) 0.0345(3) Uani 1 1 d . . . H16 H 0.9520 0.5835 0.5565 0.041 Uiso 1 1 calc R . . C17 C 0.77772(15) 0.53805(8) 0.58568(8) 0.0337(3) Uani 1 1 d . . . H17 H 0.7166 0.5763 0.5612 0.040 Uiso 1 1 calc R . . C18 C 0.72745(14) 0.47730(8) 0.62434(8) 0.0308(3) Uani 1 1 d . . . H18 H 0.6316 0.4749 0.6254 0.037 Uiso 1 1 calc R . . C19 C 0.87201(14) 0.23077(8) 0.99161(7) 0.0308(3) Uani 1 1 d . . . H19A H 0.9367 0.1942 1.0217 0.037 Uiso 1 1 calc R . . H19B H 0.8143 0.2547 1.0254 0.037 Uiso 1 1 calc R . . C20 C 0.94999(13) 0.29201(8) 0.95753(7) 0.0286(3) Uani 1 1 d . . . H20A H 0.8853 0.3256 0.9236 0.034 Uiso 1 1 calc R . . H20B H 1.0020 0.3247 0.9980 0.034 Uiso 1 1 calc R . . C21 C 1.12194(14) 0.30972(8) 0.88274(8) 0.0306(3) Uani 1 1 d . . . H21A H 1.1743 0.3429 0.9226 0.037 Uiso 1 1 calc R . . H21B H 1.0608 0.3433 0.8469 0.037 Uiso 1 1 calc R . . C22 C 1.21926(13) 0.26679(8) 0.84169(8) 0.0318(3) Uani 1 1 d . . . H22A H 1.2832 0.3035 0.8232 0.038 Uiso 1 1 calc R . . H22B H 1.2740 0.2292 0.8761 0.038 Uiso 1 1 calc R . . C23 C 1.21939(14) 0.18363(9) 0.73630(8) 0.0323(3) Uani 1 1 d . . . H23A H 1.2616 0.1387 0.7659 0.039 Uiso 1 1 calc R . . H23B H 1.2937 0.2160 0.7220 0.039 Uiso 1 1 calc R . . C24 C 1.12404(15) 0.15650(9) 0.66662(8) 0.0323(3) Uani 1 1 d . . . H24A H 1.0741 0.2012 0.6405 0.039 Uiso 1 1 calc R . . H24B H 1.1777 0.1316 0.6313 0.039 Uiso 1 1 calc R . . C25 C 0.93568(14) 0.07380(8) 0.62464(7) 0.0306(3) Uani 1 1 d . . . H25A H 0.9873 0.0467 0.5897 0.037 Uiso 1 1 calc R . . H25B H 0.8843 0.1172 0.5969 0.037 Uiso 1 1 calc R . . C26 C 0.83720(14) 0.01873(8) 0.65215(7) 0.0303(3) Uani 1 1 d . . . H26A H 0.7804 -0.0075 0.6086 0.036 Uiso 1 1 calc R . . H26B H 0.8888 -0.0212 0.6850 0.036 Uiso 1 1 calc R . . C27 C 0.64611(14) 0.01442(8) 0.71544(8) 0.0330(3) Uani 1 1 d . . . H27A H 0.6869 -0.0321 0.7428 0.040 Uiso 1 1 calc R . . H27B H 0.5812 -0.0028 0.6701 0.040 Uiso 1 1 calc R . . C28 C 0.57143(14) 0.06162(8) 0.76582(8) 0.0326(3) Uani 1 1 d . . . H28A H 0.5411 0.1114 0.7410 0.039 Uiso 1 1 calc R . . H28B H 0.4892 0.0333 0.7758 0.039 Uiso 1 1 calc R . . C29 C 0.59692(15) 0.11058(9) 0.89127(9) 0.0374(3) Uani 1 1 d . . . H29A H 0.5317 0.0735 0.9080 0.045 Uiso 1 1 calc R . . H29B H 0.5445 0.1566 0.8698 0.045 Uiso 1 1 calc R . . C30 C 0.70315(16) 0.13392(9) 0.95721(8) 0.0366(3) Uani 1 1 d . . . H30A H 0.6584 0.1553 0.9981 0.044 Uiso 1 1 calc R . . H30B H 0.7591 0.0886 0.9773 0.044 Uiso 1 1 calc R . . K1 K 0.89281(3) 0.162139(14) 0.800232(15) 0.02339(7) Uani 1 1 d . . . O1 O 0.78793(10) 0.19105(5) 0.93130(5) 0.02901(19) Uani 1 1 d . . . O2 O 0.66316(9) 0.07553(5) 0.83507(5) 0.0303(2) Uani 1 1 d . . . O3 O 0.75186(9) 0.06119(5) 0.69331(5) 0.02829(19) Uani 1 1 d . . . O4 O 1.02856(9) 0.10265(5) 0.68807(5) 0.02808(19) Uani 1 1 d . . . O5 O 1.13919(9) 0.22762(6) 0.77987(5) 0.02883(19) Uani 1 1 d . . . O6 O 1.04246(9) 0.25504(5) 0.91570(5) 0.02538(18) Uani 1 1 d . . . Ge1 Ge 0.749207(14) 0.327672(8) 0.716028(8) 0.02420(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 0.0238(6) 0.0265(6) 0.0233(6) 0.0021(5) 0.0034(4) -0.0020(5) C2 0.0262(6) 0.0294(7) 0.0379(7) -0.0006(6) -0.0006(5) 0.0011(5) C3 0.0258(7) 0.0485(9) 0.0416(8) 0.0107(7) -0.0020(6) 0.0014(6) C4 0.0320(7) 0.0680(11) 0.0250(6) 0.0001(7) -0.0010(5) -0.0177(7) C5 0.0432(8) 0.0525(9) 0.0308(7) -0.0159(6) 0.0148(6) -0.0203(7) C6 0.0322(7) 0.0321(7) 0.0321(7) -0.0041(5) 0.0134(5) -0.0048(5) C7 0.0204(5) 0.0305(6) 0.0233(6) 0.0050(5) -0.0001(4) 0.0015(5) C8 0.0264(6) 0.0340(7) 0.0295(7) 0.0044(5) 0.0019(5) -0.0028(5) C9 0.0297(7) 0.0463(8) 0.0303(7) 0.0082(6) 0.0062(5) -0.0021(6) C10 0.0331(7) 0.0504(9) 0.0250(6) 0.0010(6) 0.0036(5) 0.0031(6) C11 0.0361(7) 0.0366(7) 0.0319(7) -0.0040(6) 0.0003(6) -0.0029(6) C12 0.0263(6) 0.0328(7) 0.0285(6) 0.0031(5) 0.0019(5) -0.0025(5) C13 0.0262(6) 0.0246(6) 0.0235(6) -0.0022(5) 0.0061(5) -0.0006(5) C14 0.0250(6) 0.0306(7) 0.0320(6) -0.0025(5) 0.0031(5) -0.0022(5) C15 0.0299(7) 0.0380(8) 0.0419(8) -0.0073(6) 0.0104(6) -0.0106(6) C16 0.0460(8) 0.0274(7) 0.0330(7) -0.0041(5) 0.0147(6) -0.0102(6) C17 0.0424(8) 0.0265(6) 0.0339(7) 0.0030(5) 0.0110(6) 0.0036(6) C18 0.0295(6) 0.0297(7) 0.0353(7) 0.0034(5) 0.0113(5) 0.0041(5) C19 0.0320(7) 0.0352(7) 0.0249(6) -0.0045(5) 0.0038(5) 0.0015(5) C20 0.0284(6) 0.0283(6) 0.0271(6) -0.0057(5) -0.0005(5) 0.0032(5) C21 0.0319(7) 0.0273(6) 0.0305(6) 0.0010(5) -0.0005(5) -0.0072(5) C22 0.0238(6) 0.0385(7) 0.0311(7) 0.0002(6) -0.0008(5) -0.0078(5) C23 0.0235(6) 0.0420(8) 0.0323(7) 0.0022(6) 0.0071(5) 0.0011(5) C24 0.0316(7) 0.0381(7) 0.0291(7) 0.0008(5) 0.0102(5) -0.0013(6) C25 0.0333(7) 0.0342(7) 0.0239(6) -0.0006(5) 0.0034(5) 0.0024(5) C26 0.0353(7) 0.0265(6) 0.0279(6) -0.0025(5) 0.0017(5) 0.0013(5) C27 0.0327(7) 0.0300(7) 0.0352(7) -0.0010(5) 0.0025(5) -0.0112(5) C28 0.0248(6) 0.0335(7) 0.0385(7) 0.0037(6) 0.0026(5) -0.0045(5) C29 0.0322(7) 0.0341(7) 0.0505(9) -0.0079(6) 0.0201(6) -0.0076(6) C30 0.0436(8) 0.0338(7) 0.0366(7) -0.0024(6) 0.0192(6) -0.0072(6) K1 0.02164(13) 0.02275(13) 0.02547(13) -0.00031(9) 0.00314(10) -0.00113(9) O1 0.0308(5) 0.0294(5) 0.0274(4) -0.0010(4) 0.0065(4) -0.0048(4) O2 0.0265(4) 0.0303(5) 0.0344(5) -0.0031(4) 0.0062(4) -0.0019(4) O3 0.0280(4) 0.0236(4) 0.0333(5) -0.0006(4) 0.0053(4) -0.0026(3) O4 0.0280(4) 0.0309(5) 0.0253(4) 0.0011(4) 0.0044(3) 0.0005(4) O5 0.0208(4) 0.0371(5) 0.0277(4) -0.0023(4) 0.0016(3) -0.0020(4) O6 0.0256(4) 0.0245(4) 0.0252(4) 0.0002(3) 0.0021(3) 0.0003(3) Ge1 0.01970(8) 0.02386(8) 0.02818(9) 0.00352(5) 0.00171(6) 0.00251(5) _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 C6 1.3951(18) . ? C1 C2 1.3966(18) . ? C1 Ge1 2.0257(12) . ? C2 C3 1.397(2) . ? C2 H2 0.9500 . ? C3 C4 1.380(2) . ? C3 H3 0.9500 . ? C4 C5 1.377(3) . ? C4 H4 0.9500 . ? C5 C6 1.396(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.3983(19) . ? C7 C8 1.4044(18) . ? C7 Ge1 2.0222(13) . ? C8 C9 1.385(2) . ? C8 H8 0.9500 . ? C9 C10 1.381(2) . ? C9 H9 0.9500 . ? C10 C11 1.389(2) . ? C10 H10 0.9500 . ? C11 C12 1.401(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.3947(18) . ? C13 C14 1.3991(18) . ? C13 Ge1 2.0261(12) . ? C14 C15 1.398(2) . ? C14 H14 0.9500 . ? C15 C16 1.383(2) . ? C15 K1 3.4310(14) 2_756 ? C15 H15 0.9500 . ? C16 C17 1.387(2) . ? C16 K1 3.2901(14) 2_756 ? C16 H16 0.9500 . ? C17 C18 1.3950(19) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O1 1.4218(16) . ? C19 C20 1.4985(19) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O6 1.4274(15) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O6 1.4196(16) . ? C21 C22 1.502(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O5 1.4181(15) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O5 1.4234(16) . ? C23 C24 1.5045(19) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O4 1.4231(16) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O4 1.4232(16) . ? C25 C26 1.5022(19) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O3 1.4159(16) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O3 1.4285(15) . ? C27 C28 1.501(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O2 1.4263(16) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O2 1.4266(17) . ? C29 C30 1.495(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O1 1.4222(16) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? K1 O5 2.7617(9) . ? K1 O1 2.7708(9) . ? K1 O3 2.7819(9) . ? K1 O4 2.7961(9) . ? K1 O6 2.8278(9) . ? K1 O2 2.8719(10) . ? K1 C16 3.2901(14) 2_746 ? K1 Ge1 3.4252(3) . ? K1 C15 3.4310(14) 2_746 ? 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 C6 C1 C2 116.52(12) . . ? C6 C1 Ge1 118.35(10) . . ? C2 C1 Ge1 125.11(10) . . ? C1 C2 C3 122.09(14) . . ? C1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 119.69(14) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 119.70(13) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.17(14) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 121.74(14) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C12 C7 C8 116.31(12) . . ? C12 C7 Ge1 125.80(10) . . ? C8 C7 Ge1 116.71(10) . . ? C9 C8 C7 122.51(13) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C10 C9 C8 120.20(13) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.06(13) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 120.46(13) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 121.43(13) . . ? C7 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C18 C13 C14 116.51(12) . . ? C18 C13 Ge1 125.21(10) . . ? C14 C13 Ge1 118.24(9) . . ? C15 C14 C13 121.84(13) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C16 C15 C14 120.14(13) . . ? C16 C15 K1 72.46(8) . 2_756 ? C14 C15 K1 124.05(9) . 2_756 ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? K1 C15 H15 75.0 2_756 . ? C15 C16 C17 119.37(13) . . ? C15 C16 K1 83.90(9) . 2_756 ? C17 C16 K1 118.29(9) . 2_756 ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? K1 C16 H16 68.6 2_756 . ? C16 C17 C18 119.86(13) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 122.28(13) . . ? C13 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? O1 C19 C20 107.70(10) . . ? O1 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? O1 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? O6 C20 C19 108.51(10) . . ? O6 C20 H20A 110.0 . . ? C19 C20 H20A 110.0 . . ? O6 C20 H20B 110.0 . . ? C19 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? O6 C21 C22 108.70(11) . . ? O6 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? O6 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? H21A C21 H21B 108.3 . . ? O5 C22 C21 107.54(10) . . ? O5 C22 H22A 110.2 . . ? C21 C22 H22A 110.2 . . ? O5 C22 H22B 110.2 . . ? C21 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? O5 C23 C24 107.15(11) . . ? O5 C23 H23A 110.3 . . ? C24 C23 H23A 110.3 . . ? O5 C23 H23B 110.3 . . ? C24 C23 H23B 110.3 . . ? H23A C23 H23B 108.5 . . ? O4 C24 C23 109.14(11) . . ? O4 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O4 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? O4 C25 C26 108.88(10) . . ? O4 C25 H25A 109.9 . . ? C26 C25 H25A 109.9 . . ? O4 C25 H25B 109.9 . . ? C26 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? O3 C26 C25 108.61(11) . . ? O3 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O3 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.3 . . ? O3 C27 C28 108.49(11) . . ? O3 C27 H27A 110.0 . . ? C28 C27 H27A 110.0 . . ? O3 C27 H27B 110.0 . . ? C28 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? O2 C28 C27 108.17(11) . . ? O2 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? O2 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? O2 C29 C30 109.22(11) . . ? O2 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? O2 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? O1 C30 C29 107.50(12) . . ? O1 C30 H30A 110.2 . . ? C29 C30 H30A 110.2 . . ? O1 C30 H30B 110.2 . . ? C29 C30 H30B 110.2 . . ? H30A C30 H30B 108.5 . . ? O5 K1 O1 120.22(3) . . ? O5 K1 O3 120.88(3) . . ? O1 K1 O3 118.84(3) . . ? O5 K1 O4 60.95(3) . . ? O1 K1 O4 166.14(3) . . ? O3 K1 O4 61.21(3) . . ? O5 K1 O6 60.21(3) . . ? O1 K1 O6 60.04(3) . . ? O3 K1 O6 175.74(3) . . ? O4 K1 O6 118.74(3) . . ? O5 K1 O2 170.87(3) . . ? O1 K1 O2 59.08(3) . . ? O3 K1 O2 60.22(3) . . ? O4 K1 O2 117.25(3) . . ? O6 K1 O2 117.97(3) . . ? O5 K1 C16 85.56(3) . 2_746 ? O1 K1 C16 80.13(3) . 2_746 ? O3 K1 C16 102.00(3) . 2_746 ? O4 K1 C16 86.31(3) . 2_746 ? O6 K1 C16 73.82(3) . 2_746 ? O2 K1 C16 85.37(3) . 2_746 ? O5 K1 Ge1 84.65(2) . . ? O1 K1 Ge1 92.13(2) . . ? O3 K1 Ge1 95.70(2) . . ? O4 K1 Ge1 101.69(2) . . ? O6 K1 Ge1 88.494(19) . . ? O2 K1 Ge1 104.40(2) . . ? C16 K1 Ge1 162.28(3) 2_746 . ? O5 K1 C15 102.42(3) . 2_746 ? O1 K1 C15 85.92(3) . 2_746 ? O3 K1 C15 79.15(3) . 2_746 ? O4 K1 C15 80.48(3) . 2_746 ? O6 K1 C15 96.60(3) . 2_746 ? O2 K1 C15 68.58(3) . 2_746 ? C16 K1 C15 23.63(4) 2_746 2_746 ? Ge1 K1 C15 172.69(3) . 2_746 ? C19 O1 C30 112.69(10) . . ? C19 O1 K1 118.57(7) . . ? C30 O1 K1 118.56(8) . . ? C28 O2 C29 112.79(11) . . ? C28 O2 K1 107.76(7) . . ? C29 O2 K1 113.98(7) . . ? C26 O3 C27 112.32(10) . . ? C26 O3 K1 114.35(7) . . ? C27 O3 K1 117.77(8) . . ? C24 O4 C25 112.23(10) . . ? C24 O4 K1 112.02(8) . . ? C25 O4 K1 112.42(7) . . ? C22 O5 C23 113.34(10) . . ? C22 O5 K1 118.51(7) . . ? C23 O5 K1 116.01(8) . . ? C21 O6 C20 111.68(10) . . ? C21 O6 K1 109.22(7) . . ? C20 O6 K1 109.76(7) . . ? C7 Ge1 C1 97.51(5) . . ? C7 Ge1 C13 100.23(5) . . ? C1 Ge1 C13 101.04(5) . . ? C7 Ge1 K1 101.67(3) . . ? C1 Ge1 K1 112.22(4) . . ? C13 Ge1 K1 136.92(4) . . ? 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 C6 C1 C2 C3 -3.0(2) . . . . ? Ge1 C1 C2 C3 178.44(11) . . . . ? C1 C2 C3 C4 1.7(2) . . . . ? C2 C3 C4 C5 1.0(2) . . . . ? C3 C4 C5 C6 -2.3(2) . . . . ? C2 C1 C6 C5 1.72(19) . . . . ? Ge1 C1 C6 C5 -179.66(10) . . . . ? C4 C5 C6 C1 0.9(2) . . . . ? C12 C7 C8 C9 -1.83(19) . . . . ? Ge1 C7 C8 C9 166.48(11) . . . . ? C7 C8 C9 C10 0.7(2) . . . . ? C8 C9 C10 C11 0.6(2) . . . . ? C9 C10 C11 C12 -0.7(2) . . . . ? C8 C7 C12 C11 1.73(19) . . . . ? Ge1 C7 C12 C11 -165.37(10) . . . . ? C10 C11 C12 C7 -0.5(2) . . . . ? C18 C13 C14 C15 0.11(19) . . . . ? Ge1 C13 C14 C15 178.02(10) . . . . ? C13 C14 C15 C16 -0.4(2) . . . . ? C13 C14 C15 K1 88.03(15) . . . 2_756 ? C14 C15 C16 C17 0.6(2) . . . . ? K1 C15 C16 C17 -119.13(13) 2_756 . . . ? C14 C15 C16 K1 119.70(13) . . . 2_756 ? C15 C16 C17 C18 -0.5(2) . . . . ? K1 C16 C17 C18 -100.02(14) 2_756 . . . ? C14 C13 C18 C17 -0.1(2) . . . . ? Ge1 C13 C18 C17 -177.84(10) . . . . ? C16 C17 C18 C13 0.3(2) . . . . ? O1 C19 C20 O6 -65.82(13) . . . . ? O6 C21 C22 O5 66.36(13) . . . . ? O5 C23 C24 O4 -67.05(14) . . . . ? O4 C25 C26 O3 67.56(13) . . . . ? O3 C27 C28 O2 -68.03(14) . . . . ? O2 C29 C30 O1 63.52(15) . . . . ? C20 C19 O1 C30 -176.84(11) . . . . ? C20 C19 O1 K1 38.31(13) . . . . ? C29 C30 O1 C19 166.21(11) . . . . ? C29 C30 O1 K1 -48.94(14) . . . . ? O5 K1 O1 C19 -8.74(10) . . . . ? O3 K1 O1 C19 168.51(8) . . . . ? O4 K1 O1 C19 82.15(15) . . . . ? O6 K1 O1 C19 -6.76(8) . . . . ? O2 K1 O1 C19 160.68(10) . . . . ? C16 K1 O1 C19 70.17(9) 2_746 . . . ? Ge1 K1 O1 C19 -93.79(9) . . . . ? C15 K1 O1 C19 93.27(9) 2_746 . . . ? O5 K1 O1 C30 -151.52(9) . . . . ? O3 K1 O1 C30 25.73(10) . . . . ? O4 K1 O1 C30 -60.63(16) . . . . ? O6 K1 O1 C30 -149.54(10) . . . . ? O2 K1 O1 C30 17.89(9) . . . . ? C16 K1 O1 C30 -72.61(10) 2_746 . . . ? Ge1 K1 O1 C30 123.43(9) . . . . ? C15 K1 O1 C30 -49.52(10) 2_746 . . . ? C27 C28 O2 C29 -171.68(11) . . . . ? C27 C28 O2 K1 61.63(11) . . . . ? C30 C29 O2 C28 -171.53(11) . . . . ? C30 C29 O2 K1 -48.23(14) . . . . ? O5 K1 O2 C28 -128.67(17) . . . . ? O1 K1 O2 C28 142.96(9) . . . . ? O3 K1 O2 C28 -29.13(8) . . . . ? O4 K1 O2 C28 -52.35(8) . . . . ? O6 K1 O2 C28 155.28(7) . . . . ? C16 K1 O2 C28 -135.79(8) 2_746 . . . ? Ge1 K1 O2 C28 59.22(8) . . . . ? C15 K1 O2 C28 -118.65(8) 2_746 . . . ? O5 K1 O2 C29 105.33(19) . . . . ? O1 K1 O2 C29 16.97(9) . . . . ? O3 K1 O2 C29 -155.12(10) . . . . ? O4 K1 O2 C29 -178.34(9) . . . . ? O6 K1 O2 C29 29.29(10) . . . . ? C16 K1 O2 C29 98.22(9) 2_746 . . . ? Ge1 K1 O2 C29 -66.77(9) . . . . ? C15 K1 O2 C29 115.36(10) 2_746 . . . ? C25 C26 O3 C27 174.36(10) . . . . ? C25 C26 O3 K1 -48.03(11) . . . . ? C28 C27 O3 C26 173.70(11) . . . . ? C28 C27 O3 K1 37.67(13) . . . . ? O5 K1 O3 C26 28.99(9) . . . . ? O1 K1 O3 C26 -148.24(8) . . . . ? O4 K1 O3 C26 15.93(8) . . . . ? O6 K1 O3 C26 -74.6(4) . . . . ? O2 K1 O3 C26 -140.50(9) . . . . ? C16 K1 O3 C26 -63.01(8) 2_746 . . . ? Ge1 K1 O3 C26 116.16(8) . . . . ? C15 K1 O3 C26 -69.09(8) 2_746 . . . ? O5 K1 O3 C27 164.18(8) . . . . ? O1 K1 O3 C27 -13.06(9) . . . . ? O4 K1 O3 C27 151.11(9) . . . . ? O6 K1 O3 C27 60.6(4) . . . . ? O2 K1 O3 C27 -5.31(8) . . . . ? C16 K1 O3 C27 72.17(9) 2_746 . . . ? Ge1 K1 O3 C27 -108.66(8) . . . . ? C15 K1 O3 C27 66.10(9) 2_746 . . . ? C23 C24 O4 C25 -179.36(11) . . . . ? C23 C24 O4 K1 53.06(12) . . . . ? C26 C25 O4 C24 -178.96(11) . . . . ? C26 C25 O4 K1 -51.60(12) . . . . ? O5 K1 O4 C24 -20.34(8) . . . . ? O1 K1 O4 C24 -119.13(13) . . . . ? O3 K1 O4 C24 146.84(9) . . . . ? O6 K1 O4 C24 -38.03(9) . . . . ? O2 K1 O4 C24 169.82(8) . . . . ? C16 K1 O4 C24 -107.31(8) 2_746 . . . ? Ge1 K1 O4 C24 56.73(8) . . . . ? C15 K1 O4 C24 -130.37(8) 2_746 . . . ? O5 K1 O4 C25 -147.81(9) . . . . ? O1 K1 O4 C25 113.40(13) . . . . ? O3 K1 O4 C25 19.36(8) . . . . ? O6 K1 O4 C25 -165.50(7) . . . . ? O2 K1 O4 C25 42.35(9) . . . . ? C16 K1 O4 C25 125.22(8) 2_746 . . . ? Ge1 K1 O4 C25 -70.74(8) . . . . ? C15 K1 O4 C25 102.15(8) 2_746 . . . ? C21 C22 O5 C23 -179.38(11) . . . . ? C21 C22 O5 K1 -38.31(13) . . . . ? C24 C23 O5 C22 -170.98(11) . . . . ? C24 C23 O5 K1 46.92(12) . . . . ? O1 K1 O5 C22 8.78(10) . . . . ? O3 K1 O5 C22 -168.41(8) . . . . ? O4 K1 O5 C22 -155.32(10) . . . . ? O6 K1 O5 C22 6.81(8) . . . . ? O2 K1 O5 C22 -74.2(2) . . . . ? C16 K1 O5 C22 -67.08(9) 2_746 . . . ? Ge1 K1 O5 C22 98.13(9) . . . . ? C15 K1 O5 C22 -83.74(9) 2_746 . . . ? O1 K1 O5 C23 148.85(8) . . . . ? O3 K1 O5 C23 -28.35(9) . . . . ? O4 K1 O5 C23 -15.25(8) . . . . ? O6 K1 O5 C23 146.88(9) . . . . ? O2 K1 O5 C23 65.9(2) . . . . ? C16 K1 O5 C23 72.99(8) 2_746 . . . ? Ge1 K1 O5 C23 -121.80(8) . . . . ? C15 K1 O5 C23 56.33(9) 2_746 . . . ? C22 C21 O6 C20 178.39(10) . . . . ? C22 C21 O6 K1 -60.00(11) . . . . ? C19 C20 O6 C21 -178.97(10) . . . . ? C19 C20 O6 K1 59.74(10) . . . . ? O5 K1 O6 C21 27.70(7) . . . . ? O1 K1 O6 C21 -150.33(8) . . . . ? O3 K1 O6 C21 133.7(4) . . . . ? O4 K1 O6 C21 45.52(8) . . . . ? O2 K1 O6 C21 -162.52(7) . . . . ? C16 K1 O6 C21 121.90(8) 2_746 . . . ? Ge1 K1 O6 C21 -57.00(8) . . . . ? C15 K1 O6 C21 128.26(8) 2_746 . . . ? O5 K1 O6 C20 150.46(8) . . . . ? O1 K1 O6 C20 -27.57(7) . . . . ? O3 K1 O6 C20 -103.6(4) . . . . ? O4 K1 O6 C20 168.28(7) . . . . ? O2 K1 O6 C20 -39.77(8) . . . . ? C16 K1 O6 C20 -115.34(8) 2_746 . . . ? Ge1 K1 O6 C20 65.76(7) . . . . ? C15 K1 O6 C20 -108.98(8) 2_746 . . . ? C12 C7 Ge1 C1 -133.90(11) . . . . ? C8 C7 Ge1 C1 59.05(10) . . . . ? C12 C7 Ge1 C13 -31.19(12) . . . . ? C8 C7 Ge1 C13 161.76(10) . . . . ? C12 C7 Ge1 K1 111.47(10) . . . . ? C8 C7 Ge1 K1 -55.58(10) . . . . ? C6 C1 Ge1 C7 -141.62(10) . . . . ? C2 C1 Ge1 C7 36.87(12) . . . . ? C6 C1 Ge1 C13 116.36(10) . . . . ? C2 C1 Ge1 C13 -65.14(12) . . . . ? C6 C1 Ge1 K1 -35.71(11) . . . . ? C2 C1 Ge1 K1 142.78(10) . . . . ? C18 C13 Ge1 C7 -67.93(12) . . . . ? C14 C13 Ge1 C7 114.36(10) . . . . ? C18 C13 Ge1 C1 31.89(12) . . . . ? C14 C13 Ge1 C1 -145.83(10) . . . . ? C18 C13 Ge1 K1 172.48(9) . . . . ? C14 C13 Ge1 K1 -5.23(13) . . . . ? O5 K1 Ge1 C7 -109.91(4) . . . . ? O1 K1 Ge1 C7 10.25(4) . . . . ? O3 K1 Ge1 C7 129.52(4) . . . . ? O4 K1 Ge1 C7 -168.76(4) . . . . ? O6 K1 Ge1 C7 -49.69(4) . . . . ? O2 K1 Ge1 C7 68.83(4) . . . . ? C16 K1 Ge1 C7 -53.16(9) 2_746 . . . ? C15 K1 Ge1 C7 84.6(2) 2_746 . . . ? O5 K1 Ge1 C1 146.88(4) . . . . ? O1 K1 Ge1 C1 -92.96(4) . . . . ? O3 K1 Ge1 C1 26.31(4) . . . . ? O4 K1 Ge1 C1 88.03(4) . . . . ? O6 K1 Ge1 C1 -152.90(4) . . . . ? O2 K1 Ge1 C1 -34.37(4) . . . . ? C16 K1 Ge1 C1 -156.37(9) 2_746 . . . ? C15 K1 Ge1 C1 -18.6(2) 2_746 . . . ? O5 K1 Ge1 C13 9.18(5) . . . . ? O1 K1 Ge1 C13 129.34(5) . . . . ? O3 K1 Ge1 C13 -111.39(5) . . . . ? O4 K1 Ge1 C13 -49.66(5) . . . . ? O6 K1 Ge1 C13 69.40(5) . . . . ? O2 K1 Ge1 C13 -172.07(5) . . . . ? C16 K1 Ge1 C13 65.93(10) 2_746 . . . ? C15 K1 Ge1 C13 -156.3(2) 2_746 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 75.91 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.340 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.041 _exptl_crystal_recrystallization_method ; From a solution in PhMe layered with n-pentane at -20deg C. ; _iucr_refine_instructions_details ; TITL ck23ck in P2(1)/c CELL 1.54184 9.8669 17.2748 17.9326 90.000 99.857 90.000 ZERR 4.00 0.0001 0.0002 0.0002 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H K O GE UNIT 120 156 4 24 4 MERG 2 OMIT 2 5 6 OMIT 3 8 2 OMIT 1 8 3 OMIT -8 2 19 FMAP 2 PLAN 5 ACTA BOND BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.034200 1.224200 FVAR 3.79826 C1 1 0.561236 0.308411 0.653235 11.00000 0.02381 0.02646 = 0.02327 0.00214 0.00337 -0.00196 C2 1 0.449740 0.359204 0.646983 11.00000 0.02619 0.02944 = 0.03794 -0.00061 -0.00059 0.00114 AFIX 43 H2 2 0.459954 0.406258 0.674801 11.00000 -1.20000 AFIX 0 C3 1 0.323696 0.343021 0.601131 11.00000 0.02579 0.04845 = 0.04163 0.01071 -0.00202 0.00144 AFIX 43 H3 2 0.250521 0.379362 0.596943 11.00000 -1.20000 AFIX 0 C4 1 0.305959 0.273995 0.561944 11.00000 0.03200 0.06803 = 0.02500 0.00005 -0.00098 -0.01766 AFIX 43 H4 2 0.221007 0.262961 0.530012 11.00000 -1.20000 AFIX 0 C5 1 0.411963 0.221173 0.569332 11.00000 0.04321 0.05247 = 0.03082 -0.01594 0.01479 -0.02029 AFIX 43 H5 2 0.398971 0.172806 0.543902 11.00000 -1.20000 AFIX 0 C6 1 0.538484 0.238526 0.614104 11.00000 0.03216 0.03207 = 0.03213 -0.00411 0.01340 -0.00479 AFIX 43 H6 2 0.610982 0.201775 0.618022 11.00000 -1.20000 AFIX 0 C7 1 0.685260 0.381651 0.803869 11.00000 0.02043 0.03050 = 0.02334 0.00502 -0.00007 0.00151 C8 1 0.596934 0.339708 0.842540 11.00000 0.02636 0.03398 = 0.02954 0.00438 0.00187 -0.00281 AFIX 43 H8 2 0.555400 0.293789 0.820111 11.00000 -1.20000 AFIX 0 C9 1 0.568063 0.362739 0.912140 11.00000 0.02967 0.04626 = 0.03031 0.00820 0.00622 -0.00206 AFIX 43 H9 2 0.508521 0.332411 0.936716 11.00000 -1.20000 AFIX 0 C10 1 0.625557 0.429633 0.945900 11.00000 0.03308 0.05037 = 0.02499 0.00096 0.00356 0.00312 AFIX 43 H10 2 0.606713 0.445374 0.993846 11.00000 -1.20000 AFIX 0 C11 1 0.711345 0.473596 0.908772 11.00000 0.03611 0.03665 = 0.03188 -0.00399 0.00033 -0.00291 AFIX 43 H11 2 0.750668 0.520023 0.931231 11.00000 -1.20000 AFIX 0 C12 1 0.740284 0.449938 0.838422 11.00000 0.02626 0.03281 = 0.02849 0.00309 0.00189 -0.00253 AFIX 43 H12 2 0.798557 0.480971 0.813663 11.00000 -1.20000 AFIX 0 C13 1 0.813017 0.419944 0.661472 11.00000 0.02617 0.02456 = 0.02349 -0.00216 0.00611 -0.00064 C14 1 0.953181 0.426178 0.658019 11.00000 0.02499 0.03058 = 0.03197 -0.00255 0.00305 -0.00223 AFIX 43 H14 2 1.014848 0.388189 0.682528 11.00000 -1.20000 AFIX 0 C15 1 1.005014 0.486743 0.619513 11.00000 0.02995 0.03797 = 0.04189 -0.00728 0.01036 -0.01060 AFIX 43 H15 2 1.100793 0.489611 0.618385 11.00000 -1.20000 AFIX 0 C16 1 0.917139 0.542505 0.583048 11.00000 0.04598 0.02743 = 0.03297 -0.00411 0.01473 -0.01024 AFIX 43 H16 2 0.951972 0.583469 0.556451 11.00000 -1.20000 AFIX 0 C17 1 0.777719 0.538051 0.585680 11.00000 0.04238 0.02647 = 0.03389 0.00300 0.01102 0.00357 AFIX 43 H17 2 0.716563 0.576293 0.561206 11.00000 -1.20000 AFIX 0 C18 1 0.727452 0.477296 0.624342 11.00000 0.02951 0.02974 = 0.03528 0.00337 0.01132 0.00408 AFIX 43 H18 2 0.631616 0.474903 0.625419 11.00000 -1.20000 AFIX 0 C19 1 0.872006 0.230774 0.991606 11.00000 0.03205 0.03517 = 0.02491 -0.00446 0.00378 0.00152 AFIX 23 H19A 2 0.936696 0.194210 1.021727 11.00000 -1.20000 H19B 2 0.814270 0.254660 1.025395 11.00000 -1.20000 AFIX 0 C20 1 0.949992 0.292013 0.957534 11.00000 0.02841 0.02834 = 0.02713 -0.00571 -0.00046 0.00318 AFIX 23 H20A 2 0.885325 0.325570 0.923625 11.00000 -1.20000 H20B 2 1.002027 0.324674 0.997963 11.00000 -1.20000 AFIX 0 C21 1 1.121941 0.309724 0.882740 11.00000 0.03188 0.02735 = 0.03050 0.00098 -0.00053 -0.00715 AFIX 23 H21A 2 1.174327 0.342862 0.922635 11.00000 -1.20000 H21B 2 1.060802 0.343307 0.846936 11.00000 -1.20000 AFIX 0 C22 1 1.219263 0.266789 0.841688 11.00000 0.02383 0.03848 = 0.03112 0.00017 -0.00081 -0.00780 AFIX 23 H22A 2 1.283180 0.303455 0.823220 11.00000 -1.20000 H22B 2 1.274025 0.229182 0.876070 11.00000 -1.20000 AFIX 0 C23 1 1.219393 0.183625 0.736299 11.00000 0.02346 0.04197 = 0.03234 0.00219 0.00715 0.00111 AFIX 23 H23A 2 1.261607 0.138739 0.765857 11.00000 -1.20000 H23B 2 1.293739 0.215971 0.722027 11.00000 -1.20000 AFIX 0 C24 1 1.124041 0.156503 0.666618 11.00000 0.03162 0.03806 = 0.02910 0.00083 0.01022 -0.00129 AFIX 23 H24A 2 1.074138 0.201235 0.640492 11.00000 -1.20000 H24B 2 1.177659 0.131595 0.631329 11.00000 -1.20000 AFIX 0 C25 1 0.935682 0.073798 0.624638 11.00000 0.03334 0.03417 = 0.02390 -0.00058 0.00342 0.00236 AFIX 23 H25A 2 0.987315 0.046723 0.589701 11.00000 -1.20000 H25B 2 0.884345 0.117204 0.596893 11.00000 -1.20000 AFIX 0 C26 1 0.837200 0.018734 0.652146 11.00000 0.03531 0.02653 = 0.02791 -0.00254 0.00175 0.00126 AFIX 23 H26A 2 0.780375 -0.007499 0.608580 11.00000 -1.20000 H26B 2 0.888775 -0.021216 0.685023 11.00000 -1.20000 AFIX 0 C27 1 0.646111 0.014417 0.715437 11.00000 0.03272 0.03004 = 0.03515 -0.00100 0.00246 -0.01119 AFIX 23 H27A 2 0.686928 -0.032053 0.742823 11.00000 -1.20000 H27B 2 0.581236 -0.002763 0.670121 11.00000 -1.20000 AFIX 0 C28 1 0.571430 0.061621 0.765818 11.00000 0.02484 0.03346 = 0.03849 0.00371 0.00255 -0.00452 AFIX 23 H28A 2 0.541074 0.111357 0.741016 11.00000 -1.20000 H28B 2 0.489167 0.033312 0.775829 11.00000 -1.20000 AFIX 0 C29 1 0.596920 0.110580 0.891266 11.00000 0.03218 0.03409 = 0.05047 -0.00787 0.02007 -0.00757 AFIX 23 H29A 2 0.531690 0.073506 0.907966 11.00000 -1.20000 H29B 2 0.544472 0.156630 0.869847 11.00000 -1.20000 AFIX 0 C30 1 0.703146 0.133922 0.957206 11.00000 0.04365 0.03381 = 0.03663 -0.00240 0.01917 -0.00715 AFIX 23 H30A 2 0.658408 0.155269 0.998121 11.00000 -1.20000 H30B 2 0.759074 0.088554 0.977257 11.00000 -1.20000 AFIX 0 K1 3 0.892805 0.162139 0.800232 11.00000 0.02164 0.02275 = 0.02547 -0.00031 0.00314 -0.00113 O1 4 0.787930 0.191047 0.931299 11.00000 0.03081 0.02939 = 0.02736 -0.00101 0.00648 -0.00482 O2 4 0.663165 0.075526 0.835069 11.00000 0.02645 0.03031 = 0.03437 -0.00305 0.00622 -0.00187 O3 4 0.751858 0.061186 0.693313 11.00000 0.02800 0.02359 = 0.03330 -0.00058 0.00529 -0.00257 O4 4 1.028564 0.102647 0.688074 11.00000 0.02800 0.03094 = 0.02525 0.00115 0.00440 0.00053 O5 4 1.139194 0.227620 0.779873 11.00000 0.02084 0.03707 = 0.02766 -0.00226 0.00157 -0.00199 O6 4 1.042462 0.255045 0.915695 11.00000 0.02564 0.02453 = 0.02518 0.00018 0.00209 0.00033 GE1 5 0.749207 0.327672 0.716028 11.00000 0.01970 0.02386 = 0.02818 0.00352 0.00171 0.00251 HKLF 4 REM ck23ck in P2(1)/c REM R1 = 0.0236 for 6118 Fo > 4sig(Fo) and 0.0241 for all 6263 data REM 343 parameters refined using 0 restraints END WGHT 0.0342 1.2242 REM Highest difference peak 0.340, deepest hole -0.342, 1-sigma level 0.041 Q1 1 0.7066 0.3568 0.7634 11.00000 0.05 0.34 Q2 1 0.7958 0.3840 0.6828 11.00000 0.05 0.34 Q3 1 0.6338 0.3176 0.6694 11.00000 0.05 0.29 Q4 1 0.7625 0.2940 0.6697 11.00000 0.05 0.29 Q5 1 0.8304 0.2802 0.7490 11.00000 0.05 0.26 ; data_ck27ck _database_code_depnum_ccdc_archive 'CCDC 924395' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '18-Crown-6-potassium triphenyl-tin' _chemical_melting_point ? _chemical_formula_moiety 'C30 H39 K O6 Sn' _chemical_formula_sum 'C30 H39 K O6 Sn' _chemical_formula_weight 653.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.6725(2) _cell_length_b 12.6028(2) _cell_length_c 24.4563(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2981.24(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24000 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 30.78 _exptl_crystal_description 'fragment of cuboid' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; The collected data cover nominally a full sphere of the reciprocal space. A combination of 15 sets of \w scans were used; each set at different \j, 2\q or \k angles and each scan 1.0 deg in \w. Each frame was exposured for 10s. Nominal crystal to detector distance 45 mm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction, Xcalibur, EOS' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73495 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8585 _reflns_number_gt 8152 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution ; SIR-92 (A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi, J. Appl. Crystallogr. 1993, 26, 343-350.) ; _computing_structure_refinement ; SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122) ; _computing_molecular_graphics ; Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany. ; _computing_publication_material ; WinGX v1.80.05 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.) ; _refine_special_details ; All H atoms were refined using a riding model, with a common U restrained to be 1.2 (1.5 for methyl groups) times the equivalent isotropic displacement parameter of the parent atom. Methyl groups were treated as rigid bodies and allowed to rotate about the E-CH3 bond. 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^)+(0.0144P)^2^+0.7527P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881; 3662 Friedel pairs' _refine_ls_abs_structure_Flack -0.021(9) _refine_ls_number_reflns 8585 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0403 _refine_ls_wR_factor_gt 0.0393 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.004 _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 C1 C 0.79709(16) 0.95463(13) 0.44546(6) 0.0154(3) Uani 1 1 d . . . C2 C 0.92082(17) 0.96597(14) 0.47498(6) 0.0187(3) Uani 1 1 d . . . H2 H 0.9800 1.0239 0.4667 0.022 Uiso 1 1 calc R . . C3 C 0.95961(18) 0.89517(14) 0.51587(7) 0.0230(4) Uani 1 1 d . . . H3 H 1.0445 0.9051 0.5347 0.028 Uiso 1 1 calc R . . C4 C 0.87523(19) 0.81045(14) 0.52918(7) 0.0233(4) Uani 1 1 d . . . H4 H 0.9014 0.7622 0.5572 0.028 Uiso 1 1 calc R . . C5 C 0.7514(2) 0.79684(11) 0.50100(6) 0.0210(3) Uani 1 1 d . . . H5 H 0.6919 0.7394 0.5099 0.025 Uiso 1 1 calc R . . C6 C 0.71498(16) 0.86753(13) 0.45977(6) 0.0184(3) Uani 1 1 d . . . H6 H 0.6309 0.8562 0.4405 0.022 Uiso 1 1 calc R . . C7 C 0.52029(15) 1.04485(12) 0.37908(6) 0.0150(3) Uani 1 1 d . . . C8 C 0.44094(17) 1.01338(13) 0.42408(7) 0.0176(3) Uani 1 1 d . . . H8 H 0.4861 1.0011 0.4580 0.021 Uiso 1 1 calc R . . C9 C 0.29837(17) 0.99938(13) 0.42104(7) 0.0192(3) Uani 1 1 d . . . H9 H 0.2484 0.9760 0.4522 0.023 Uiso 1 1 calc R . . C10 C 0.22945(17) 1.01969(12) 0.37242(6) 0.0212(3) Uani 1 1 d . . . H10 H 0.1321 1.0108 0.3701 0.025 Uiso 1 1 calc R . . C11 C 0.30470(17) 1.05320(13) 0.32710(7) 0.0207(3) Uani 1 1 d . . . H11 H 0.2585 1.0681 0.2937 0.025 Uiso 1 1 calc R . . C12 C 0.44728(16) 1.06486(12) 0.33063(6) 0.0175(3) Uani 1 1 d . . . H12 H 0.4970 1.0871 0.2992 0.021 Uiso 1 1 calc R . . C13 C 0.80529(16) 0.99792(12) 0.30990(6) 0.0145(3) Uani 1 1 d . . . C14 C 0.73399(17) 0.91102(12) 0.28801(6) 0.0182(3) Uani 1 1 d . . . H14 H 0.6534 0.8863 0.3062 0.022 Uiso 1 1 calc R . . C15 C 0.77674(17) 0.85954(13) 0.24066(6) 0.0210(4) Uani 1 1 d . . . H15 H 0.7250 0.8015 0.2266 0.025 Uiso 1 1 calc R . . C16 C 0.89546(18) 0.89348(14) 0.21400(7) 0.0228(4) Uani 1 1 d . . . H16 H 0.9267 0.8576 0.1821 0.027 Uiso 1 1 calc R . . C17 C 0.96823(18) 0.97985(14) 0.23403(7) 0.0215(4) Uani 1 1 d . . . H17 H 1.0490 1.0039 0.2157 0.026 Uiso 1 1 calc R . . C18 C 0.92267(16) 1.03135(13) 0.28107(6) 0.0178(3) Uani 1 1 d . . . H18 H 0.9728 1.0911 0.2940 0.021 Uiso 1 1 calc R . . C19 C 0.7290(2) 1.20546(12) 0.54640(6) 0.0228(4) Uani 1 1 d . . . H19A H 0.7528 1.1675 0.5122 0.027 Uiso 1 1 calc R . . H19B H 0.7501 1.2817 0.5413 0.027 Uiso 1 1 calc R . . C20 C 0.57853(19) 1.19136(14) 0.55886(8) 0.0227(4) Uani 1 1 d . . . H20A H 0.5554 1.2275 0.5936 0.027 Uiso 1 1 calc R . . H20B H 0.5221 1.2233 0.5294 0.027 Uiso 1 1 calc R . . C21 C 0.40591(17) 1.06118(14) 0.57272(7) 0.0211(4) Uani 1 1 d . . . H21A H 0.3495 1.0946 0.5436 0.025 Uiso 1 1 calc R . . H21B H 0.3778 1.0918 0.6083 0.025 Uiso 1 1 calc R . . C22 C 0.38305(17) 0.94344(14) 0.57292(7) 0.0207(3) Uani 1 1 d . . . H22A H 0.2831 0.9278 0.5764 0.025 Uiso 1 1 calc R . . H22B H 0.4167 0.9123 0.5382 0.025 Uiso 1 1 calc R . . C23 C 0.44426(16) 0.78567(12) 0.61973(7) 0.0187(3) Uani 1 1 d . . . H23A H 0.4847 0.7542 0.5863 0.022 Uiso 1 1 calc R . . H23B H 0.3456 0.7651 0.6216 0.022 Uiso 1 1 calc R . . C24 C 0.51918(16) 0.74563(13) 0.66914(7) 0.0182(3) Uani 1 1 d . . . H24A H 0.4848 0.7823 0.7023 0.022 Uiso 1 1 calc R . . H24B H 0.5027 0.6686 0.6736 0.022 Uiso 1 1 calc R . . C25 C 0.7394(2) 0.73007(11) 0.70913(6) 0.0188(3) Uani 1 1 d . . . H25A H 0.7159 0.6553 0.7174 0.023 Uiso 1 1 calc R . . H25B H 0.7156 0.7740 0.7413 0.023 Uiso 1 1 calc R . . C26 C 0.89079(17) 0.73974(13) 0.69676(7) 0.0186(3) Uani 1 1 d . . . H26A H 0.9459 0.7102 0.7273 0.022 Uiso 1 1 calc R . . H26B H 0.9135 0.6997 0.6631 0.022 Uiso 1 1 calc R . . C27 C 1.06551(16) 0.86778(14) 0.67977(7) 0.0195(3) Uani 1 1 d . . . H27A H 1.0929 0.8367 0.6442 0.023 Uiso 1 1 calc R . . H27B H 1.1215 0.8341 0.7089 0.023 Uiso 1 1 calc R . . C28 C 1.08944(18) 0.98538(14) 0.67937(7) 0.0218(4) Uani 1 1 d . . . H28A H 1.0550 1.0171 0.7138 0.026 Uiso 1 1 calc R . . H28B H 1.1896 1.0005 0.6763 0.026 Uiso 1 1 calc R . . C29 C 1.02929(19) 1.14242(13) 0.63229(7) 0.0212(4) Uani 1 1 d . . . H29A H 1.1278 1.1632 0.6299 0.025 Uiso 1 1 calc R . . H29B H 0.9899 1.1735 0.6660 0.025 Uiso 1 1 calc R . . C30 C 0.95237(19) 1.18287(14) 0.58331(7) 0.0214(4) Uani 1 1 d . . . H30A H 0.9694 1.2598 0.5788 0.026 Uiso 1 1 calc R . . H30B H 0.9850 1.1460 0.5500 0.026 Uiso 1 1 calc R . . O1 O 0.80776(12) 1.16398(9) 0.59087(5) 0.0197(2) Uani 1 1 d . . . O2 O 0.54878(11) 1.08117(9) 0.56319(4) 0.0186(2) Uani 1 1 d . . . O3 O 0.45628(11) 0.89884(8) 0.61788(4) 0.0171(2) Uani 1 1 d . . . O4 O 0.66382(11) 0.76532(9) 0.66252(5) 0.0173(2) Uani 1 1 d . . . O5 O 0.92249(11) 0.84961(9) 0.68947(5) 0.0179(2) Uani 1 1 d . . . O6 O 1.01785(12) 1.02965(9) 0.63397(4) 0.0189(2) Uani 1 1 d . . . K1 K 0.73942(4) 0.95972(2) 0.621065(12) 0.01628(6) Uani 1 1 d . . . Sn1 Sn 0.744348(11) 1.083707(7) 0.385768(4) 0.01457(3) 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 0.0141(7) 0.0173(7) 0.0148(7) -0.0047(6) 0.0003(6) 0.0046(5) C2 0.0164(8) 0.0229(8) 0.0167(8) -0.0072(6) 0.0001(6) -0.0007(6) C3 0.0188(8) 0.0333(10) 0.0170(8) -0.0056(7) -0.0038(6) 0.0068(7) C4 0.0291(9) 0.0266(9) 0.0142(8) -0.0002(7) 0.0006(7) 0.0114(7) C5 0.0238(7) 0.0180(6) 0.0211(7) -0.0015(5) 0.0066(9) 0.0028(9) C6 0.0154(8) 0.0198(8) 0.0201(8) -0.0039(6) -0.0009(6) 0.0030(6) C7 0.0153(7) 0.0124(6) 0.0172(8) -0.0025(6) -0.0002(6) 0.0028(5) C8 0.0188(8) 0.0191(8) 0.0149(7) 0.0007(6) -0.0009(6) 0.0039(6) C9 0.0176(8) 0.0220(8) 0.0181(8) 0.0007(6) 0.0037(6) 0.0006(6) C10 0.0133(8) 0.0240(7) 0.0262(8) -0.0032(6) -0.0003(6) 0.0012(6) C11 0.0213(8) 0.0232(8) 0.0176(8) -0.0015(6) -0.0047(6) 0.0020(6) C12 0.0183(7) 0.0183(8) 0.0160(7) -0.0003(6) 0.0012(6) 0.0013(6) C13 0.0145(7) 0.0144(7) 0.0147(7) 0.0028(6) -0.0016(6) 0.0024(6) C14 0.0154(7) 0.0206(7) 0.0186(6) 0.0020(6) 0.0005(6) 0.0000(8) C15 0.0223(10) 0.0209(7) 0.0196(7) -0.0015(6) -0.0050(6) 0.0015(6) C16 0.0267(9) 0.0299(10) 0.0118(7) 0.0015(7) 0.0022(6) 0.0090(7) C17 0.0193(8) 0.0295(9) 0.0159(8) 0.0096(7) 0.0038(6) 0.0041(7) C18 0.0173(8) 0.0186(8) 0.0175(8) 0.0062(6) -0.0015(6) 0.0010(6) C19 0.0350(11) 0.0173(7) 0.0161(7) 0.0049(5) -0.0019(7) -0.0025(8) C20 0.0315(10) 0.0161(8) 0.0206(9) 0.0041(7) -0.0035(7) 0.0046(7) C21 0.0178(8) 0.0279(10) 0.0177(8) 0.0019(7) -0.0027(6) 0.0050(6) C22 0.0180(8) 0.0301(9) 0.0142(7) 0.0016(7) -0.0036(6) -0.0019(6) C23 0.0170(7) 0.0187(7) 0.0204(8) -0.0029(7) 0.0005(7) -0.0049(6) C24 0.0169(8) 0.0163(7) 0.0213(8) 0.0011(6) 0.0005(6) -0.0046(6) C25 0.0222(8) 0.0149(6) 0.0192(7) 0.0053(5) 0.0006(8) -0.0005(8) C26 0.0192(8) 0.0160(8) 0.0207(8) 0.0038(6) -0.0004(7) 0.0028(6) C27 0.0132(7) 0.0278(9) 0.0175(8) 0.0030(7) -0.0011(6) 0.0012(7) C28 0.0187(8) 0.0290(9) 0.0178(8) 0.0023(7) -0.0027(7) -0.0046(7) C29 0.0240(9) 0.0187(8) 0.0210(8) -0.0021(6) 0.0007(7) -0.0093(7) C30 0.0281(9) 0.0166(8) 0.0196(9) 0.0001(7) 0.0034(7) -0.0083(7) O1 0.0250(6) 0.0179(6) 0.0162(5) 0.0042(4) -0.0008(5) -0.0042(5) O2 0.0205(5) 0.0165(5) 0.0189(5) 0.0029(5) -0.0010(4) 0.0011(5) O3 0.0194(5) 0.0178(5) 0.0141(5) 0.0008(4) -0.0046(5) -0.0031(4) O4 0.0157(5) 0.0173(5) 0.0188(6) 0.0050(4) -0.0003(4) -0.0028(4) O5 0.0147(5) 0.0150(5) 0.0240(6) 0.0029(5) 0.0014(5) 0.0005(4) O6 0.0232(6) 0.0168(6) 0.0167(6) 0.0007(4) -0.0027(5) -0.0058(5) K1 0.01369(14) 0.01272(12) 0.02242(14) 0.00309(11) 0.00070(16) -0.00031(13) Sn1 0.01387(4) 0.01294(4) 0.01691(4) -0.00170(3) -0.00070(5) 0.00013(5) _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 C6 1.399(2) . ? C1 C2 1.405(2) . ? C1 Sn1 2.2445(16) . ? C2 C3 1.392(2) . ? C2 H2 0.9500 . ? C3 C4 1.383(3) . ? C3 K1 3.4375(17) . ? C3 H3 0.9500 . ? C4 C5 1.393(3) . ? C4 K1 3.2116(17) . ? C4 H4 0.9500 . ? C5 C6 1.391(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.399(2) . ? C7 C12 1.402(2) . ? C7 Sn1 2.2279(15) . ? C8 C9 1.392(2) . ? C8 H8 0.9500 . ? C9 C10 1.387(2) . ? C9 H9 0.9500 . ? C10 C11 1.392(2) . ? C10 H10 0.9500 . ? C11 C12 1.390(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.401(2) . ? C13 C18 1.401(2) . ? C13 Sn1 2.2269(15) . ? C14 C15 1.390(2) . ? C14 H14 0.9500 . ? C15 C16 1.388(2) . ? C15 H15 0.9500 . ? C16 C17 1.386(3) . ? C16 K1 3.2080(17) 2_674 ? C16 H16 0.9500 . ? C17 C18 1.392(2) . ? C17 K1 3.4996(17) 2_674 ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O1 1.4272(19) . ? C19 C20 1.497(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O2 1.422(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O2 1.4239(19) . ? C21 C22 1.500(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O3 1.4237(19) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O3 1.4318(18) . ? C23 C24 1.497(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O4 1.4301(18) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O4 1.4254(18) . ? C25 C26 1.500(2) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O5 1.4293(19) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O5 1.4221(19) . ? C27 C28 1.500(2) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O6 1.423(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O6 1.4262(19) . ? C29 C30 1.499(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O1 1.431(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O1 K1 2.7585(11) . ? O2 K1 2.7833(11) . ? O3 K1 2.8452(11) . ? O4 K1 2.7504(11) . ? O5 K1 2.8036(12) . ? O6 K1 2.8511(12) . ? K1 C16 3.2080(17) 2_675 ? K1 C17 3.4996(17) 2_675 ? 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 C6 C1 C2 115.77(15) . . ? C6 C1 Sn1 127.02(11) . . ? C2 C1 Sn1 117.01(12) . . ? C3 C2 C1 122.25(16) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C4 C3 C2 120.33(16) . . ? C4 C3 K1 68.95(9) . . ? C2 C3 K1 102.65(10) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? K1 C3 H3 98.1 . . ? C3 C4 C5 119.10(16) . . ? C3 C4 K1 87.36(10) . . ? C5 C4 K1 93.81(10) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? K1 C4 H4 88.8 . . ? C6 C5 C4 119.85(16) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 122.68(15) . . ? C5 C6 H6 118.7 . . ? C1 C6 H6 118.7 . . ? C8 C7 C12 116.06(14) . . ? C8 C7 Sn1 122.57(11) . . ? C12 C7 Sn1 120.82(11) . . ? C9 C8 C7 122.51(15) . . ? C9 C8 H8 118.7 . . ? C7 C8 H8 118.7 . . ? C10 C9 C8 119.90(15) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 119.17(15) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 120.12(15) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 122.22(15) . . ? C11 C12 H12 118.9 . . ? C7 C12 H12 118.9 . . ? C14 C13 C18 116.21(14) . . ? C14 C13 Sn1 124.60(11) . . ? C18 C13 Sn1 119.20(11) . . ? C15 C14 C13 122.47(15) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C16 C15 C14 119.57(16) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 119.75(15) . . ? C17 C16 K1 90.23(10) . 2_674 ? C15 C16 K1 100.03(10) . 2_674 ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? K1 C16 H16 79.8 2_674 . ? C16 C17 C18 119.82(16) . . ? C16 C17 K1 66.45(9) . 2_674 ? C18 C17 K1 111.66(11) . 2_674 ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? K1 C17 H17 91.7 2_674 . ? C17 C18 C13 122.15(16) . . ? C17 C18 H18 118.9 . . ? C13 C18 H18 118.9 . . ? O1 C19 C20 108.70(13) . . ? O1 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? O1 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.3 . . ? O2 C20 C19 109.13(14) . . ? O2 C20 H20A 109.9 . . ? C19 C20 H20A 109.9 . . ? O2 C20 H20B 109.9 . . ? C19 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? O2 C21 C22 108.58(13) . . ? O2 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? O2 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? O3 C22 C21 108.64(13) . . ? O3 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? O3 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.3 . . ? O3 C23 C24 108.79(13) . . ? O3 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? O3 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O4 C24 C23 108.89(13) . . ? O4 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O4 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? O4 C25 C26 108.31(12) . . ? O4 C25 H25A 110.0 . . ? C26 C25 H25A 110.0 . . ? O4 C25 H25B 110.0 . . ? C26 C25 H25B 110.0 . . ? H25A C25 H25B 108.4 . . ? O5 C26 C25 108.26(12) . . ? O5 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O5 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? O5 C27 C28 108.08(14) . . ? O5 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? O5 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? O6 C28 C27 108.51(14) . . ? O6 C28 H28A 110.0 . . ? C27 C28 H28A 110.0 . . ? O6 C28 H28B 110.0 . . ? C27 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? O6 C29 C30 108.86(14) . . ? O6 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? O6 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? O1 C30 C29 108.98(13) . . ? O1 C30 H30A 109.9 . . ? C29 C30 H30A 109.9 . . ? O1 C30 H30B 109.9 . . ? C29 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C19 O1 C30 111.26(13) . . ? C19 O1 K1 114.70(9) . . ? C30 O1 K1 115.09(9) . . ? C20 O2 C21 112.42(13) . . ? C20 O2 K1 116.16(9) . . ? C21 O2 K1 117.54(9) . . ? C22 O3 C23 112.16(12) . . ? C22 O3 K1 113.18(9) . . ? C23 O3 K1 110.24(8) . . ? C25 O4 C24 110.93(12) . . ? C25 O4 K1 115.85(9) . . ? C24 O4 K1 117.16(9) . . ? C27 O5 C26 112.68(12) . . ? C27 O5 K1 115.79(9) . . ? C26 O5 K1 114.73(9) . . ? C28 O6 C29 112.06(13) . . ? C28 O6 K1 115.15(9) . . ? C29 O6 K1 112.22(10) . . ? O4 K1 O1 173.54(4) . . ? O4 K1 O2 120.08(4) . . ? O1 K1 O2 60.62(3) . . ? O4 K1 O5 60.47(3) . . ? O1 K1 O5 118.05(4) . . ? O2 K1 O5 173.78(4) . . ? O4 K1 O3 60.92(3) . . ? O1 K1 O3 118.36(3) . . ? O2 K1 O3 59.78(3) . . ? O5 K1 O3 119.39(3) . . ? O4 K1 O6 119.06(3) . . ? O1 K1 O6 60.98(3) . . ? O2 K1 O6 120.80(3) . . ? O5 K1 O6 59.36(3) . . ? O3 K1 O6 174.62(3) . . ? O4 K1 C16 98.31(4) . 2_675 ? O1 K1 C16 75.46(4) . 2_675 ? O2 K1 C16 76.92(4) . 2_675 ? O5 K1 C16 96.87(4) . 2_675 ? O3 K1 C16 77.49(4) . 2_675 ? O6 K1 C16 97.32(4) . 2_675 ? O4 K1 C4 81.08(4) . . ? O1 K1 C4 105.15(4) . . ? O2 K1 C4 103.73(4) . . ? O5 K1 C4 82.49(4) . . ? O3 K1 C4 102.51(4) . . ? O6 K1 C4 82.65(4) . . ? C16 K1 C4 179.27(5) 2_675 . ? O4 K1 C3 103.29(4) . . ? O1 K1 C3 82.65(4) . . ? O2 K1 C3 99.21(4) . . ? O5 K1 C3 86.45(4) . . ? O3 K1 C3 120.81(4) . . ? O6 K1 C3 64.58(4) . . ? C16 K1 C3 156.74(5) 2_675 . ? C4 K1 C3 23.69(4) . . ? O4 K1 C17 75.54(4) . 2_675 ? O1 K1 C17 98.38(4) . 2_675 ? O2 K1 C17 84.35(4) . 2_675 ? O5 K1 C17 89.95(4) . 2_675 ? O3 K1 C17 61.82(4) . 2_675 ? O6 K1 C17 112.80(4) . 2_675 ? C16 K1 C17 23.33(4) 2_675 2_675 ? C4 K1 C17 156.15(5) . 2_675 ? C3 K1 C17 176.32(4) . 2_675 ? C13 Sn1 C7 95.14(6) . . ? C13 Sn1 C1 97.46(5) . . ? C7 Sn1 C1 96.29(6) . . ? 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 C6 C1 C2 C3 0.0(2) . . . . ? Sn1 C1 C2 C3 175.30(12) . . . . ? C1 C2 C3 C4 -0.5(2) . . . . ? C1 C2 C3 K1 -73.38(16) . . . . ? C2 C3 C4 C5 0.2(2) . . . . ? K1 C3 C4 C5 92.89(15) . . . . ? C2 C3 C4 K1 -92.68(15) . . . . ? C3 C4 C5 C6 0.6(2) . . . . ? K1 C4 C5 C6 89.71(14) . . . . ? C4 C5 C6 C1 -1.2(2) . . . . ? C2 C1 C6 C5 0.8(2) . . . . ? Sn1 C1 C6 C5 -173.90(11) . . . . ? C12 C7 C8 C9 1.9(2) . . . . ? Sn1 C7 C8 C9 173.42(12) . . . . ? C7 C8 C9 C10 -1.8(2) . . . . ? C8 C9 C10 C11 0.5(2) . . . . ? C9 C10 C11 C12 0.7(2) . . . . ? C10 C11 C12 C7 -0.6(3) . . . . ? C8 C7 C12 C11 -0.6(2) . . . . ? Sn1 C7 C12 C11 -172.36(12) . . . . ? C18 C13 C14 C15 0.5(2) . . . . ? Sn1 C13 C14 C15 -179.52(11) . . . . ? C13 C14 C15 C16 1.0(2) . . . . ? C14 C15 C16 C17 -1.6(2) . . . . ? C14 C15 C16 K1 -97.65(14) . . . 2_674 ? C15 C16 C17 C18 0.7(2) . . . . ? K1 C16 C17 C18 102.37(14) 2_674 . . . ? C15 C16 C17 K1 -101.70(15) . . . 2_674 ? C16 C17 C18 C13 0.9(2) . . . . ? K1 C17 C18 C13 75.38(16) 2_674 . . . ? C14 C13 C18 C17 -1.5(2) . . . . ? Sn1 C13 C18 C17 178.57(12) . . . . ? O1 C19 C20 O2 -62.63(17) . . . . ? O2 C21 C22 O3 64.38(17) . . . . ? O3 C23 C24 O4 -66.29(16) . . . . ? O4 C25 C26 O5 64.37(15) . . . . ? O5 C27 C28 O6 -65.16(17) . . . . ? O6 C29 C30 O1 66.94(18) . . . . ? C20 C19 O1 C30 -175.35(13) . . . . ? C20 C19 O1 K1 51.81(15) . . . . ? C29 C30 O1 C19 177.34(13) . . . . ? C29 C30 O1 K1 -50.03(15) . . . . ? C19 C20 O2 C21 -177.49(13) . . . . ? C19 C20 O2 K1 43.06(16) . . . . ? C22 C21 O2 C20 176.24(13) . . . . ? C22 C21 O2 K1 -44.91(15) . . . . ? C21 C22 O3 C23 -177.67(13) . . . . ? C21 C22 O3 K1 -52.17(14) . . . . ? C24 C23 O3 C22 -177.84(13) . . . . ? C24 C23 O3 K1 55.07(13) . . . . ? C26 C25 O4 C24 172.73(13) . . . . ? C26 C25 O4 K1 -50.52(13) . . . . ? C23 C24 O4 C25 179.00(12) . . . . ? C23 C24 O4 K1 42.87(15) . . . . ? C28 C27 O5 C26 -173.43(13) . . . . ? C28 C27 O5 K1 51.70(15) . . . . ? C25 C26 O5 C27 177.51(13) . . . . ? C25 C26 O5 K1 -47.12(14) . . . . ? C27 C28 O6 C29 176.87(14) . . . . ? C27 C28 O6 K1 47.01(16) . . . . ? C30 C29 O6 C28 179.60(13) . . . . ? C30 C29 O6 K1 -49.04(15) . . . . ? C25 O4 K1 O1 -59.6(4) . . . . ? C24 O4 K1 O1 74.4(4) . . . . ? C25 O4 K1 O2 -153.93(9) . . . . ? C24 O4 K1 O2 -19.92(11) . . . . ? C25 O4 K1 O5 18.93(9) . . . . ? C24 O4 K1 O5 152.94(11) . . . . ? C25 O4 K1 O3 -144.92(11) . . . . ? C24 O4 K1 O3 -10.91(9) . . . . ? C25 O4 K1 O6 28.92(11) . . . . ? C24 O4 K1 O6 162.93(9) . . . . ? C25 O4 K1 C16 -74.28(10) . . . 2_675 ? C24 O4 K1 C16 59.72(11) . . . 2_675 ? C25 O4 K1 C4 105.31(10) . . . . ? C24 O4 K1 C4 -120.68(11) . . . . ? C25 O4 K1 C3 97.00(10) . . . . ? C24 O4 K1 C3 -129.00(10) . . . . ? C25 O4 K1 C17 -79.41(10) . . . 2_675 ? C24 O4 K1 C17 54.60(10) . . . 2_675 ? C19 O1 K1 O4 -119.3(3) . . . . ? C30 O1 K1 O4 109.7(3) . . . . ? C19 O1 K1 O2 -21.26(10) . . . . ? C30 O1 K1 O2 -152.27(11) . . . . ? C19 O1 K1 O5 165.66(10) . . . . ? C30 O1 K1 O5 34.66(11) . . . . ? C19 O1 K1 O3 -37.46(11) . . . . ? C30 O1 K1 O3 -168.47(10) . . . . ? C19 O1 K1 O6 148.63(11) . . . . ? C30 O1 K1 O6 17.62(10) . . . . ? C19 O1 K1 C16 -104.24(11) . . . 2_675 ? C30 O1 K1 C16 124.75(11) . . . 2_675 ? C19 O1 K1 C4 76.19(11) . . . . ? C30 O1 K1 C4 -54.82(11) . . . . ? C19 O1 K1 C3 83.68(10) . . . . ? C30 O1 K1 C3 -47.33(10) . . . . ? C19 O1 K1 C17 -99.89(10) . . . 2_675 ? C30 O1 K1 C17 129.10(10) . . . 2_675 ? C20 O2 K1 O4 160.05(10) . . . . ? C21 O2 K1 O4 22.72(11) . . . . ? C20 O2 K1 O1 -12.56(10) . . . . ? C21 O2 K1 O1 -149.89(11) . . . . ? C20 O2 K1 O5 66.8(4) . . . . ? C21 O2 K1 O5 -70.5(4) . . . . ? C20 O2 K1 O3 150.94(11) . . . . ? C21 O2 K1 O3 13.60(10) . . . . ? C20 O2 K1 O6 -22.85(12) . . . . ? C21 O2 K1 O6 -160.18(10) . . . . ? C20 O2 K1 C16 67.94(11) . . . 2_675 ? C21 O2 K1 C16 -69.39(11) . . . 2_675 ? C20 O2 K1 C4 -112.41(11) . . . . ? C21 O2 K1 C4 110.25(11) . . . . ? C20 O2 K1 C3 -88.67(11) . . . . ? C21 O2 K1 C3 134.00(10) . . . . ? C20 O2 K1 C17 90.37(11) . . . 2_675 ? C21 O2 K1 C17 -46.96(11) . . . 2_675 ? C27 O5 K1 O4 149.94(11) . . . . ? C26 O5 K1 O4 16.00(9) . . . . ? C27 O5 K1 O1 -37.23(11) . . . . ? C26 O5 K1 O1 -171.18(9) . . . . ? C27 O5 K1 O2 -113.3(3) . . . . ? C26 O5 K1 O2 112.8(3) . . . . ? C27 O5 K1 O3 166.14(10) . . . . ? C26 O5 K1 O3 32.20(11) . . . . ? C27 O5 K1 O6 -19.91(10) . . . . ? C26 O5 K1 O6 -153.86(11) . . . . ? C27 O5 K1 C16 -114.38(11) . . . 2_675 ? C26 O5 K1 C16 111.68(10) . . . 2_675 ? C27 O5 K1 C4 65.97(11) . . . . ? C26 O5 K1 C4 -67.97(10) . . . . ? C27 O5 K1 C3 42.50(11) . . . . ? C26 O5 K1 C3 -91.45(10) . . . . ? C27 O5 K1 C17 -136.71(11) . . . 2_675 ? C26 O5 K1 C17 89.35(10) . . . 2_675 ? C22 O3 K1 O4 -149.94(11) . . . . ? C23 O3 K1 O4 -23.41(9) . . . . ? C22 O3 K1 O1 37.37(11) . . . . ? C23 O3 K1 O1 163.90(9) . . . . ? C22 O3 K1 O2 21.03(9) . . . . ? C23 O3 K1 O2 147.56(10) . . . . ? C22 O3 K1 O5 -166.07(9) . . . . ? C23 O3 K1 O5 -39.54(10) . . . . ? C22 O3 K1 O6 118.8(4) . . . . ? C23 O3 K1 O6 -114.7(4) . . . . ? C22 O3 K1 C16 103.04(10) . . . 2_675 ? C23 O3 K1 C16 -130.43(10) . . . 2_675 ? C22 O3 K1 C4 -77.71(10) . . . . ? C23 O3 K1 C4 48.82(10) . . . . ? C22 O3 K1 C3 -61.40(11) . . . . ? C23 O3 K1 C3 65.13(10) . . . . ? C22 O3 K1 C17 121.56(10) . . . 2_675 ? C23 O3 K1 C17 -111.91(10) . . . 2_675 ? C28 O6 K1 O4 -25.53(11) . . . . ? C29 O6 K1 O4 -155.32(10) . . . . ? C28 O6 K1 O1 147.08(11) . . . . ? C29 O6 K1 O1 17.30(10) . . . . ? C28 O6 K1 O2 157.34(10) . . . . ? C29 O6 K1 O2 27.56(11) . . . . ? C28 O6 K1 O5 -15.43(10) . . . . ? C29 O6 K1 O5 -145.21(11) . . . . ? C28 O6 K1 O3 62.7(4) . . . . ? C29 O6 K1 O3 -67.0(4) . . . . ? C28 O6 K1 C16 78.24(11) . . . 2_675 ? C29 O6 K1 C16 -51.55(11) . . . 2_675 ? C28 O6 K1 C4 -101.02(11) . . . . ? C29 O6 K1 C4 129.19(11) . . . . ? C28 O6 K1 C3 -117.08(11) . . . . ? C29 O6 K1 C3 113.14(11) . . . . ? C28 O6 K1 C17 60.09(11) . . . 2_675 ? C29 O6 K1 C17 -69.69(11) . . . 2_675 ? C3 C4 K1 O4 -159.50(11) . . . . ? C5 C4 K1 O4 81.50(10) . . . . ? C3 C4 K1 O1 18.77(11) . . . . ? C5 C4 K1 O1 -100.24(10) . . . . ? C3 C4 K1 O2 81.56(10) . . . . ? C5 C4 K1 O2 -37.44(11) . . . . ? C3 C4 K1 O5 -98.35(10) . . . . ? C5 C4 K1 O5 142.65(11) . . . . ? C3 C4 K1 O3 143.11(10) . . . . ? C5 C4 K1 O3 24.10(11) . . . . ? C3 C4 K1 O6 -38.44(10) . . . . ? C5 C4 K1 O6 -157.44(11) . . . . ? C3 C4 K1 C16 -127(4) . . . 2_675 ? C5 C4 K1 C16 114(4) . . . 2_675 ? C5 C4 K1 C3 -119.00(16) . . . . ? C3 C4 K1 C17 -170.87(10) . . . 2_675 ? C5 C4 K1 C17 70.13(15) . . . 2_675 ? C4 C3 K1 O4 20.83(11) . . . . ? C2 C3 K1 O4 138.74(11) . . . . ? C4 C3 K1 O1 -161.75(10) . . . . ? C2 C3 K1 O1 -43.84(11) . . . . ? C4 C3 K1 O2 -103.23(10) . . . . ? C2 C3 K1 O2 14.69(11) . . . . ? C4 C3 K1 O5 79.36(10) . . . . ? C2 C3 K1 O5 -162.73(11) . . . . ? C4 C3 K1 O3 -43.03(11) . . . . ? C2 C3 K1 O3 74.89(12) . . . . ? C4 C3 K1 O6 136.95(11) . . . . ? C2 C3 K1 O6 -105.13(11) . . . . ? C4 C3 K1 C16 178.51(11) . . . 2_675 ? C2 C3 K1 C16 -63.57(16) . . . 2_675 ? C2 C3 K1 C4 117.92(16) . . . . ? C4 C3 K1 C17 91.8(7) . . . 2_675 ? C2 C3 K1 C17 -150.3(7) . . . 2_675 ? C14 C13 Sn1 C7 -27.11(13) . . . . ? C18 C13 Sn1 C7 152.84(12) . . . . ? C14 C13 Sn1 C1 69.94(13) . . . . ? C18 C13 Sn1 C1 -110.11(12) . . . . ? C8 C7 Sn1 C13 137.08(13) . . . . ? C12 C7 Sn1 C13 -51.76(13) . . . . ? C8 C7 Sn1 C1 38.96(13) . . . . ? C12 C7 Sn1 C1 -149.87(12) . . . . ? C6 C1 Sn1 C13 -82.71(14) . . . . ? C2 C1 Sn1 C13 102.62(12) . . . . ? C6 C1 Sn1 C7 13.34(14) . . . . ? C2 C1 Sn1 C7 -161.33(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.355 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.053 _exptl_crystal_recrystallization_method ; From solution in PhMe layered with n-pentane at rt. ; _iucr_refine_instructions_details ; TITL ck27ck in P2(1)2(1)2(1) CELL 0.71073 9.6725 12.6028 24.4563 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0005 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O K SN UNIT 120 156 24 4 4 MERG 2 OMIT -2.00 60.00 OMIT 3 3 8 OMIT -3 3 8 FMAP 2 PLAN 5 ACTA BOND BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.014400 0.752700 FVAR 2.86929 C1 1 0.797095 0.954626 0.445460 11.00000 0.01409 0.01727 = 0.01482 -0.00473 0.00026 0.00457 C2 1 0.920821 0.965966 0.474976 11.00000 0.01638 0.02294 = 0.01669 -0.00724 0.00011 -0.00070 AFIX 43 H2 2 0.980035 1.023943 0.466739 11.00000 -1.20000 AFIX 0 C3 1 0.959614 0.895174 0.515868 11.00000 0.01880 0.03332 = 0.01700 -0.00564 -0.00378 0.00680 AFIX 43 H3 2 1.044492 0.905105 0.534732 11.00000 -1.20000 AFIX 0 C4 1 0.875230 0.810452 0.529178 11.00000 0.02909 0.02657 = 0.01421 -0.00016 0.00060 0.01138 AFIX 43 H4 2 0.901393 0.762184 0.557163 11.00000 -1.20000 AFIX 0 C5 1 0.751383 0.796845 0.501004 11.00000 0.02380 0.01804 = 0.02107 -0.00145 0.00655 0.00283 AFIX 43 H5 2 0.691895 0.739419 0.509928 11.00000 -1.20000 AFIX 0 C6 1 0.714979 0.867527 0.459766 11.00000 0.01542 0.01977 = 0.02013 -0.00386 -0.00089 0.00303 AFIX 43 H6 2 0.630939 0.856211 0.440527 11.00000 -1.20000 AFIX 0 C7 1 0.520288 1.044854 0.379084 11.00000 0.01527 0.01237 = 0.01723 -0.00248 -0.00016 0.00280 C8 1 0.440938 1.013380 0.424075 11.00000 0.01883 0.01906 = 0.01494 0.00074 -0.00090 0.00386 AFIX 43 H8 2 0.486057 1.001090 0.457992 11.00000 -1.20000 AFIX 0 C9 1 0.298374 0.999382 0.421038 11.00000 0.01756 0.02198 = 0.01806 0.00072 0.00366 0.00064 AFIX 43 H9 2 0.248375 0.975960 0.452218 11.00000 -1.20000 AFIX 0 C10 1 0.229451 1.019686 0.372417 11.00000 0.01333 0.02401 = 0.02619 -0.00323 -0.00029 0.00119 AFIX 43 H10 2 0.132093 1.010827 0.370082 11.00000 -1.20000 AFIX 0 C11 1 0.304704 1.053197 0.327102 11.00000 0.02125 0.02322 = 0.01759 -0.00150 -0.00469 0.00202 AFIX 43 H11 2 0.258520 1.068127 0.293694 11.00000 -1.20000 AFIX 0 C12 1 0.447281 1.064859 0.330628 11.00000 0.01831 0.01831 = 0.01597 -0.00029 0.00124 0.00126 AFIX 43 H12 2 0.496976 1.087137 0.299151 11.00000 -1.20000 AFIX 0 C13 1 0.805287 0.997922 0.309899 11.00000 0.01449 0.01436 = 0.01465 0.00281 -0.00161 0.00240 C14 1 0.733989 0.911022 0.288006 11.00000 0.01545 0.02060 = 0.01857 0.00203 0.00052 0.00000 AFIX 43 H14 2 0.653386 0.886331 0.306194 11.00000 -1.20000 AFIX 0 C15 1 0.776740 0.859543 0.240663 11.00000 0.02228 0.02094 = 0.01964 -0.00154 -0.00497 0.00147 AFIX 43 H15 2 0.725034 0.801512 0.226647 11.00000 -1.20000 AFIX 0 C16 1 0.895456 0.893476 0.214001 11.00000 0.02667 0.02994 = 0.01178 0.00151 0.00217 0.00903 AFIX 43 H16 2 0.926698 0.857625 0.182144 11.00000 -1.20000 AFIX 0 C17 1 0.968235 0.979846 0.234029 11.00000 0.01928 0.02948 = 0.01587 0.00965 0.00381 0.00407 AFIX 43 H17 2 1.049004 1.003857 0.215716 11.00000 -1.20000 AFIX 0 C18 1 0.922665 1.031346 0.281065 11.00000 0.01730 0.01856 = 0.01746 0.00620 -0.00147 0.00101 AFIX 43 H18 2 0.972784 1.091090 0.294032 11.00000 -1.20000 AFIX 0 C19 1 0.728954 1.205463 0.546405 11.00000 0.03497 0.01733 = 0.01609 0.00492 -0.00186 -0.00249 AFIX 23 H19A 2 0.752849 1.167498 0.512249 11.00000 -1.20000 H19B 2 0.750062 1.281690 0.541309 11.00000 -1.20000 AFIX 0 C20 1 0.578533 1.191365 0.558860 11.00000 0.03153 0.01611 = 0.02057 0.00411 -0.00350 0.00461 AFIX 23 H20A 2 0.555413 1.227509 0.593618 11.00000 -1.20000 H20B 2 0.522076 1.223304 0.529378 11.00000 -1.20000 AFIX 0 C21 1 0.405908 1.061182 0.572724 11.00000 0.01779 0.02793 = 0.01768 0.00192 -0.00266 0.00505 AFIX 23 H21A 2 0.349539 1.094579 0.543648 11.00000 -1.20000 H21B 2 0.377800 1.091753 0.608318 11.00000 -1.20000 AFIX 0 C22 1 0.383046 0.943436 0.572920 11.00000 0.01796 0.03011 = 0.01416 0.00157 -0.00362 -0.00190 AFIX 23 H22A 2 0.283128 0.927770 0.576357 11.00000 -1.20000 H22B 2 0.416721 0.912252 0.538236 11.00000 -1.20000 AFIX 0 C23 1 0.444259 0.785666 0.619734 11.00000 0.01703 0.01866 = 0.02037 -0.00286 0.00055 -0.00493 AFIX 23 H23A 2 0.484723 0.754197 0.586274 11.00000 -1.20000 H23B 2 0.345601 0.765074 0.621612 11.00000 -1.20000 AFIX 0 C24 1 0.519176 0.745629 0.669141 11.00000 0.01693 0.01630 = 0.02126 0.00115 0.00051 -0.00460 AFIX 23 H24A 2 0.484774 0.782279 0.702259 11.00000 -1.20000 H24B 2 0.502651 0.668580 0.673552 11.00000 -1.20000 AFIX 0 C25 1 0.739428 0.730068 0.709131 11.00000 0.02219 0.01486 = 0.01922 0.00527 0.00056 -0.00050 AFIX 23 H25A 2 0.715942 0.655320 0.717419 11.00000 -1.20000 H25B 2 0.715571 0.773976 0.741344 11.00000 -1.20000 AFIX 0 C26 1 0.890788 0.739742 0.696759 11.00000 0.01921 0.01602 = 0.02070 0.00377 -0.00041 0.00279 AFIX 23 H26A 2 0.945892 0.710204 0.727288 11.00000 -1.20000 H26B 2 0.913498 0.699682 0.663116 11.00000 -1.20000 AFIX 0 C27 1 1.065512 0.867778 0.679769 11.00000 0.01324 0.02783 = 0.01754 0.00299 -0.00108 0.00124 AFIX 23 H27A 2 1.092918 0.836729 0.644200 11.00000 -1.20000 H27B 2 1.121529 0.834134 0.708876 11.00000 -1.20000 AFIX 0 C28 1 1.089442 0.985382 0.679366 11.00000 0.01867 0.02897 = 0.01780 0.00228 -0.00272 -0.00461 AFIX 23 H28A 2 1.055040 1.017131 0.713802 11.00000 -1.20000 H28B 2 1.189578 1.000523 0.676316 11.00000 -1.20000 AFIX 0 C29 1 1.029288 1.142421 0.632287 11.00000 0.02403 0.01872 = 0.02099 -0.00210 0.00067 -0.00933 AFIX 23 H29A 2 1.127795 1.163249 0.629915 11.00000 -1.20000 H29B 2 0.989903 1.173514 0.666040 11.00000 -1.20000 AFIX 0 C30 1 0.952367 1.182871 0.583308 11.00000 0.02809 0.01662 = 0.01957 0.00012 0.00339 -0.00828 AFIX 23 H30A 2 0.969403 1.259826 0.578762 11.00000 -1.20000 H30B 2 0.985008 1.146022 0.549970 11.00000 -1.20000 AFIX 0 O1 3 0.807758 1.163985 0.590871 11.00000 0.02502 0.01790 = 0.01619 0.00418 -0.00077 -0.00424 O2 3 0.548777 1.081174 0.563190 11.00000 0.02051 0.01647 = 0.01886 0.00286 -0.00098 0.00112 O3 3 0.456278 0.898842 0.617884 11.00000 0.01942 0.01778 = 0.01414 0.00084 -0.00462 -0.00309 O4 3 0.663821 0.765321 0.662519 11.00000 0.01566 0.01732 = 0.01882 0.00501 -0.00028 -0.00278 O5 3 0.922495 0.849608 0.689472 11.00000 0.01465 0.01497 = 0.02401 0.00289 0.00144 0.00046 O6 3 1.017848 1.029646 0.633966 11.00000 0.02317 0.01682 = 0.01667 0.00074 -0.00269 -0.00580 K1 4 0.739423 0.959715 0.621065 11.00000 0.01369 0.01272 = 0.02242 0.00309 0.00070 -0.00031 SN1 5 0.744348 1.083707 0.385768 11.00000 0.01387 0.01294 = 0.01691 -0.00170 -0.00070 0.00013 HKLF 4 REM ck27ck in P2(1)2(1)2(1) REM R1 = 0.0208 for 8152 Fo > 4sig(Fo) and 0.0237 for all 8585 data REM 343 parameters refined using 0 restraints END WGHT 0.0144 0.7528 REM Highest difference peak 0.355, deepest hole -0.311, 1-sigma level 0.053 Q1 1 0.7507 1.0745 0.3485 11.00000 0.05 0.36 Q2 1 0.3811 1.0458 0.3333 11.00000 0.05 0.28 Q3 1 0.8025 0.7356 0.6896 11.00000 0.05 0.27 Q4 1 0.7538 0.8198 0.4736 11.00000 0.05 0.26 Q5 1 0.7594 0.9595 0.3016 11.00000 0.05 0.26 ; data_ck28ck _database_code_depnum_ccdc_archive 'CCDC 924396' #TrackingRef 'CCDC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '18-Crown-6-potassium triphenyl-lead' _chemical_melting_point ? _chemical_formula_moiety 'C30 H39 K O6 Pb' _chemical_formula_sum 'C30 H39 K O6 Pb' _chemical_formula_weight 741.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.6839(4) _cell_length_b 12.5929(4) _cell_length_c 24.5776(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2997.20(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5970 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 29.31 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 5.807 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; The collected data cover nominally a full sphere of the reciprocal space. A combination of 11 sets of \w scans were used; each set at different \j, 2\q or \k angles and each scan 1.0 deg in \w. Each frame was exposured for 35s. Nominal crystal to detector distance 45 mm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction, Xcalibur, EOS' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52235 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0742 _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 -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7157 _reflns_number_gt 5122 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution ; SHELXS-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122) ; _computing_structure_refinement ; SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 112-122) ; _computing_molecular_graphics ; Diamond 3.2i, K. Brandenburg, Crystal Impact GbR, Bonn, Germany. ; _computing_publication_material ; WinGX v1.80.05 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.) ; _refine_special_details ; All H atoms were refined using a riding model, with a common U restrained to be 1.2 (1.5 for methyl groups) times the equivalent isotropic displacement parameter of the parent atom. Methyl groups were treated as rigid bodies and allowed to rotate about the E-CH3 bond. 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^)+(0.0244P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 3116 Friedel Pairs' _refine_ls_abs_structure_Flack -0.031(7) _refine_ls_number_reflns 7157 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.002 _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 C1 C 0.3000(6) 0.4536(5) 0.4470(2) 0.0159(14) Uani 1 1 d . . . C2 C 0.4242(7) 0.4635(5) 0.4768(3) 0.0202(15) Uani 1 1 d . . . H2 H 0.4847 0.5208 0.4687 0.024 Uiso 1 1 calc R . . C3 C 0.4606(7) 0.3924(5) 0.5174(2) 0.0241(16) Uani 1 1 d . . . H3 H 0.5452 0.4013 0.5364 0.029 Uiso 1 1 calc R . . C4 C 0.3752(8) 0.3093(5) 0.5303(3) 0.0246(17) Uani 1 1 d . . . H4 H 0.3998 0.2606 0.5582 0.029 Uiso 1 1 calc R . . C5 C 0.2511(12) 0.2974(4) 0.5018(2) 0.0218(12) Uani 1 1 d . . . H5 H 0.1898 0.2413 0.5109 0.026 Uiso 1 1 calc R . . C6 C 0.2174(7) 0.3676(5) 0.4600(2) 0.0225(19) Uani 1 1 d . . . H6 H 0.1350 0.3560 0.4399 0.027 Uiso 1 1 calc R . . C7 C 0.0168(6) 0.5479(5) 0.3785(2) 0.0143(13) Uani 1 1 d . . . C8 C -0.0619(7) 0.5142(5) 0.4230(3) 0.0201(15) Uani 1 1 d . . . H8 H -0.0165 0.5015 0.4566 0.024 Uiso 1 1 calc R . . C9 C -0.2032(6) 0.4986(5) 0.4200(2) 0.0193(15) Uani 1 1 d . . . H9 H -0.2525 0.4737 0.4509 0.023 Uiso 1 1 calc R . . C10 C -0.2726(8) 0.5194(4) 0.3719(2) 0.0201(18) Uani 1 1 d . . . H10 H -0.3697 0.5097 0.3694 0.024 Uiso 1 1 calc R . . C11 C -0.1974(7) 0.5546(5) 0.3274(3) 0.0257(17) Uani 1 1 d . . . H11 H -0.2440 0.5697 0.2943 0.031 Uiso 1 1 calc R . . C12 C -0.0554(7) 0.5683(5) 0.3302(2) 0.0179(15) Uani 1 1 d . . . H12 H -0.0065 0.5919 0.2990 0.021 Uiso 1 1 calc R . . C13 C 0.3078(6) 0.4984(5) 0.3065(2) 0.0144(13) Uani 1 1 d . . . C14 C 0.2351(10) 0.4117(4) 0.2865(2) 0.0215(15) Uani 1 1 d . . . H14 H 0.1551 0.3881 0.3054 0.026 Uiso 1 1 calc R . . C15 C 0.2766(8) 0.3580(5) 0.2395(2) 0.024(2) Uani 1 1 d . . . H15 H 0.2239 0.2999 0.2262 0.028 Uiso 1 1 calc R . . C16 C 0.3953(7) 0.3900(5) 0.2122(3) 0.0261(17) Uani 1 1 d . . . H16 H 0.4249 0.3535 0.1804 0.031 Uiso 1 1 calc R . . C17 C 0.4693(7) 0.4747(5) 0.2316(2) 0.0227(16) Uani 1 1 d . . . H17 H 0.5511 0.4964 0.2134 0.027 Uiso 1 1 calc R . . C18 C 0.4257(7) 0.5292(5) 0.2778(2) 0.0184(15) Uani 1 1 d . . . H18 H 0.4774 0.5887 0.2901 0.022 Uiso 1 1 calc R . . C19 C 0.2314(10) 0.7038(5) 0.5463(2) 0.0247(19) Uani 1 1 d . . . H19A H 0.2555 0.6657 0.5123 0.030 Uiso 1 1 calc R . . H19B H 0.2526 0.7800 0.5411 0.030 Uiso 1 1 calc R . . C20 C 0.0815(8) 0.6901(6) 0.5582(3) 0.0274(19) Uani 1 1 d . . . H20A H 0.0580 0.7262 0.5928 0.033 Uiso 1 1 calc R . . H20B H 0.0258 0.7226 0.5288 0.033 Uiso 1 1 calc R . . C21 C -0.0927(7) 0.5613(5) 0.5710(3) 0.0221(16) Uani 1 1 d . . . H21A H -0.1479 0.5936 0.5415 0.027 Uiso 1 1 calc R . . H21B H -0.1221 0.5931 0.6060 0.027 Uiso 1 1 calc R . . C22 C -0.1157(7) 0.4441(5) 0.5722(2) 0.0210(15) Uani 1 1 d . . . H22A H -0.2156 0.4290 0.5759 0.025 Uiso 1 1 calc R . . H22B H -0.0831 0.4122 0.5377 0.025 Uiso 1 1 calc R . . C23 C -0.0563(6) 0.2861(5) 0.6187(3) 0.0205(14) Uani 1 1 d . . . H23A H -0.0155 0.2541 0.5856 0.025 Uiso 1 1 calc R . . H23B H -0.1551 0.2663 0.6202 0.025 Uiso 1 1 calc R . . C24 C 0.0176(7) 0.2455(5) 0.6687(3) 0.0205(15) Uani 1 1 d . . . H24A H -0.0167 0.2828 0.7014 0.025 Uiso 1 1 calc R . . H24B H 0.0000 0.1685 0.6732 0.025 Uiso 1 1 calc R . . C25 C 0.2388(11) 0.2293(4) 0.7085(2) 0.0206(14) Uani 1 1 d . . . H25A H 0.2148 0.1547 0.7170 0.025 Uiso 1 1 calc R . . H25B H 0.2149 0.2737 0.7405 0.025 Uiso 1 1 calc R . . C26 C 0.3890(7) 0.2381(5) 0.6968(3) 0.0207(15) Uani 1 1 d . . . H26A H 0.4431 0.2083 0.7274 0.025 Uiso 1 1 calc R . . H26B H 0.4119 0.1976 0.6635 0.025 Uiso 1 1 calc R . . C27 C 0.5639(7) 0.3661(5) 0.6796(3) 0.0213(16) Uani 1 1 d . . . H27A H 0.5907 0.3353 0.6441 0.026 Uiso 1 1 calc R . . H27B H 0.6202 0.3318 0.7083 0.026 Uiso 1 1 calc R . . C28 C 0.5893(7) 0.4829(5) 0.6795(3) 0.0225(16) Uani 1 1 d . . . H28A H 0.5547 0.5148 0.7137 0.027 Uiso 1 1 calc R . . H28B H 0.6895 0.4974 0.6768 0.027 Uiso 1 1 calc R . . C29 C 0.5312(7) 0.6409(5) 0.6329(3) 0.0200(15) Uani 1 1 d . . . H29A H 0.6298 0.6613 0.6309 0.024 Uiso 1 1 calc R . . H29B H 0.4913 0.6717 0.6665 0.024 Uiso 1 1 calc R . . C30 C 0.4547(8) 0.6817(6) 0.5836(3) 0.0247(18) Uani 1 1 d . . . H30A H 0.4716 0.7587 0.5791 0.030 Uiso 1 1 calc R . . H30B H 0.4882 0.6449 0.5505 0.030 Uiso 1 1 calc R . . O1 O 0.3106(5) 0.6626(3) 0.59045(17) 0.0227(11) Uani 1 1 d . . . O2 O 0.0509(5) 0.5813(3) 0.56218(16) 0.0202(10) Uani 1 1 d . . . O3 O -0.0428(4) 0.3986(3) 0.61679(17) 0.0195(9) Uani 1 1 d . . . O4 O 0.1632(4) 0.2643(3) 0.66207(18) 0.0208(10) Uani 1 1 d . . . O5 O 0.4223(5) 0.3476(3) 0.68944(18) 0.0210(11) Uani 1 1 d . . . O6 O 0.5183(5) 0.5280(3) 0.63378(17) 0.0222(11) Uani 1 1 d . . . K1 K 0.2400(3) 0.45900(9) 0.62144(5) 0.0190(3) Uani 1 1 d . . . Pb1 Pb 0.24969(5) 0.590535(14) 0.385516(8) 0.01734(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(3) 0.016(3) 0.014(3) -0.008(3) 0.005(3) 0.006(3) C2 0.015(4) 0.026(4) 0.019(3) -0.008(3) 0.002(3) 0.000(3) C3 0.023(4) 0.032(4) 0.017(3) -0.012(3) -0.014(3) 0.008(3) C4 0.031(5) 0.027(4) 0.015(4) 0.005(3) 0.002(3) 0.016(3) C5 0.021(3) 0.017(3) 0.028(3) -0.003(2) 0.011(6) 0.009(6) C6 0.024(6) 0.022(3) 0.021(3) -0.005(3) 0.002(3) 0.007(3) C7 0.012(3) 0.021(3) 0.010(3) -0.004(3) -0.001(3) 0.003(3) C8 0.023(4) 0.018(3) 0.020(4) -0.001(3) -0.002(3) 0.007(3) C9 0.016(4) 0.024(3) 0.018(3) 0.004(3) 0.006(3) 0.003(3) C10 0.009(5) 0.027(3) 0.024(4) -0.004(2) 0.000(3) 0.000(3) C11 0.022(4) 0.031(4) 0.024(4) -0.004(3) -0.004(3) -0.002(3) C12 0.017(4) 0.022(4) 0.015(3) -0.003(3) 0.003(3) 0.003(3) C13 0.017(3) 0.016(3) 0.010(3) 0.002(3) 0.000(3) 0.001(3) C14 0.019(4) 0.023(3) 0.022(3) 0.008(3) 0.002(4) 0.001(4) C15 0.028(6) 0.020(3) 0.022(3) -0.001(3) -0.004(3) -0.002(3) C16 0.030(4) 0.038(5) 0.010(3) -0.001(3) 0.001(3) 0.013(3) C17 0.019(4) 0.034(4) 0.014(3) 0.012(3) 0.006(3) 0.003(3) C18 0.013(4) 0.022(4) 0.020(4) 0.009(3) -0.008(3) 0.000(3) C19 0.036(6) 0.021(3) 0.017(3) 0.006(2) 0.000(4) 0.001(4) C20 0.037(5) 0.023(4) 0.023(4) 0.001(4) -0.004(4) 0.007(4) C21 0.025(4) 0.031(4) 0.010(3) 0.007(3) -0.007(3) 0.005(3) C22 0.020(4) 0.030(4) 0.012(3) 0.001(3) -0.002(3) -0.003(3) C23 0.016(3) 0.023(3) 0.022(3) -0.006(3) 0.003(3) -0.005(3) C24 0.020(4) 0.014(3) 0.028(4) -0.001(3) 0.000(3) -0.005(3) C25 0.025(4) 0.019(3) 0.018(3) 0.009(2) 0.004(5) 0.001(5) C26 0.014(4) 0.023(4) 0.026(4) 0.002(3) -0.003(3) 0.004(3) C27 0.011(4) 0.030(4) 0.023(4) 0.004(3) -0.004(3) 0.000(3) C28 0.017(4) 0.034(4) 0.017(4) 0.002(3) -0.001(3) -0.006(3) C29 0.020(4) 0.023(4) 0.017(3) -0.006(3) -0.001(3) -0.006(3) C30 0.029(5) 0.022(4) 0.024(4) -0.009(3) 0.008(4) -0.006(3) O1 0.029(3) 0.024(2) 0.015(2) 0.005(2) 0.001(2) -0.006(2) O2 0.024(3) 0.017(2) 0.020(2) 0.001(2) 0.001(2) 0.001(2) O3 0.021(2) 0.020(2) 0.017(2) 0.002(2) -0.003(2) -0.0024(19) O4 0.017(3) 0.022(2) 0.023(3) 0.005(2) 0.001(2) -0.004(2) O5 0.016(3) 0.021(2) 0.026(3) 0.003(2) -0.002(2) 0.000(2) O6 0.026(3) 0.019(3) 0.022(2) -0.002(2) -0.001(2) -0.005(2) K1 0.0166(8) 0.0151(5) 0.0252(6) 0.0040(5) -0.0006(11) 0.0000(9) Pb1 0.01602(9) 0.01585(9) 0.02015(10) -0.00190(10) -0.0006(3) 0.0004(3) _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 C6 1.384(8) . ? C1 C2 1.414(9) . ? C1 Pb1 2.344(6) . ? C2 C3 1.386(9) . ? C2 H2 0.9500 . ? C3 C4 1.371(9) . ? C3 K1 3.436(7) . ? C3 H3 0.9500 . ? C4 C5 1.399(12) . ? C4 K1 3.207(6) . ? C4 H4 0.9500 . ? C5 C6 1.393(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.400(8) . ? C7 C12 1.400(8) . ? C7 Pb1 2.325(6) . ? C8 C9 1.384(9) . ? C8 H8 0.9500 . ? C9 C10 1.386(8) . ? C9 H9 0.9500 . ? C10 C11 1.387(8) . ? C10 H10 0.9500 . ? C11 C12 1.387(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.389(9) . ? C13 C18 1.397(8) . ? C13 Pb1 2.331(6) . ? C14 C15 1.399(8) . ? C14 H14 0.9500 . ? C15 C16 1.390(9) . ? C15 H15 0.9500 . ? C16 C17 1.371(9) . ? C16 K1 3.211(7) 2_564 ? C16 H16 0.9500 . ? C17 C18 1.392(8) . ? C17 K1 3.485(6) 2_564 ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 O1 1.426(8) . ? C19 C20 1.491(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O2 1.406(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 O2 1.430(8) . ? C21 C22 1.493(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 O3 1.424(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O3 1.423(7) . ? C23 C24 1.511(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O4 1.440(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O4 1.426(8) . ? C25 C26 1.487(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O5 1.428(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O5 1.412(7) . ? C27 C28 1.492(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 O6 1.435(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O6 1.427(7) . ? C29 C30 1.511(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O1 1.426(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O1 K1 2.761(4) . ? O2 K1 2.802(5) . ? O3 K1 2.845(5) . ? O4 K1 2.749(4) . ? O5 K1 2.807(5) . ? O6 K1 2.848(5) . ? K1 C16 3.211(7) 2_565 ? K1 C17 3.485(6) 2_565 ? 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 C6 C1 C2 116.2(6) . . ? C6 C1 Pb1 127.2(5) . . ? C2 C1 Pb1 116.5(5) . . ? C3 C2 C1 122.1(6) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C4 C3 C2 120.4(6) . . ? C4 C3 K1 68.8(4) . . ? C2 C3 K1 102.7(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? K1 C3 H3 98.1 . . ? C3 C4 C5 118.9(6) . . ? C3 C4 K1 87.7(4) . . ? C5 C4 K1 93.6(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? K1 C4 H4 88.8 . . ? C6 C5 C4 120.2(8) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C1 C6 C5 122.1(7) . . ? C1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C8 C7 C12 116.5(6) . . ? C8 C7 Pb1 122.7(4) . . ? C12 C7 Pb1 120.4(4) . . ? C9 C8 C7 122.7(6) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C8 C9 C10 119.8(6) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 118.6(7) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C10 C11 C12 121.4(6) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 121.0(6) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? C14 C13 C18 117.0(6) . . ? C14 C13 Pb1 124.3(5) . . ? C18 C13 Pb1 118.7(4) . . ? C13 C14 C15 121.8(8) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 119.3(6) . . ? C17 C16 K1 89.7(4) . 2_564 ? C15 C16 K1 99.7(4) . 2_564 ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? K1 C16 H16 80.7 2_564 . ? C16 C17 C18 120.6(6) . . ? C16 C17 K1 67.2(4) . 2_564 ? C18 C17 K1 109.8(4) . 2_564 ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? K1 C17 H17 92.8 2_564 . ? C17 C18 C13 121.5(6) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? O1 C19 C20 109.4(5) . . ? O1 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? O1 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? O2 C20 C19 109.3(6) . . ? O2 C20 H20A 109.8 . . ? C19 C20 H20A 109.8 . . ? O2 C20 H20B 109.8 . . ? C19 C20 H20B 109.8 . . ? H20A C20 H20B 108.3 . . ? O2 C21 C22 108.8(5) . . ? O2 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? O2 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O3 C22 C21 109.8(5) . . ? O3 C22 H22A 109.7 . . ? C21 C22 H22A 109.7 . . ? O3 C22 H22B 109.7 . . ? C21 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? O3 C23 C24 108.6(5) . . ? O3 C23 H23A 110.0 . . ? C24 C23 H23A 110.0 . . ? O3 C23 H23B 110.0 . . ? C24 C23 H23B 110.0 . . ? H23A C23 H23B 108.3 . . ? O4 C24 C23 108.4(5) . . ? O4 C24 H24A 110.0 . . ? C23 C24 H24A 110.0 . . ? O4 C24 H24B 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? O4 C25 C26 108.9(5) . . ? O4 C25 H25A 109.9 . . ? C26 C25 H25A 109.9 . . ? O4 C25 H25B 109.9 . . ? C26 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? O5 C26 C25 108.5(5) . . ? O5 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? O5 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? O5 C27 C28 108.8(5) . . ? O5 C27 H27A 109.9 . . ? C28 C27 H27A 109.9 . . ? O5 C27 H27B 109.9 . . ? C28 C27 H27B 109.9 . . ? H27A C27 H27B 108.3 . . ? O6 C28 C27 108.2(5) . . ? O6 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? O6 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? O6 C29 C30 107.9(5) . . ? O6 C29 H29A 110.1 . . ? C30 C29 H29A 110.1 . . ? O6 C29 H29B 110.1 . . ? C30 C29 H29B 110.1 . . ? H29A C29 H29B 108.4 . . ? O1 C30 C29 109.1(6) . . ? O1 C30 H30A 109.9 . . ? C29 C30 H30A 109.9 . . ? O1 C30 H30B 109.9 . . ? C29 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C30 O1 C19 112.0(5) . . ? C30 O1 K1 115.5(4) . . ? C19 O1 K1 114.5(4) . . ? C20 O2 C21 112.8(5) . . ? C20 O2 K1 115.8(4) . . ? C21 O2 K1 117.3(3) . . ? C23 O3 C22 112.3(5) . . ? C23 O3 K1 110.7(3) . . ? C22 O3 K1 113.6(3) . . ? C25 O4 C24 111.2(5) . . ? C25 O4 K1 115.3(4) . . ? C24 O4 K1 116.9(3) . . ? C27 O5 C26 113.6(5) . . ? C27 O5 K1 115.3(4) . . ? C26 O5 K1 114.6(4) . . ? C29 O6 C28 111.4(5) . . ? C29 O6 K1 112.6(4) . . ? C28 O6 K1 114.6(4) . . ? O4 K1 O1 174.41(14) . . ? O4 K1 O2 120.14(15) . . ? O1 K1 O2 60.51(13) . . ? O4 K1 O5 60.54(13) . . ? O1 K1 O5 118.23(15) . . ? O2 K1 O5 174.62(13) . . ? O4 K1 O3 61.02(13) . . ? O1 K1 O3 118.41(14) . . ? O2 K1 O3 59.79(13) . . ? O5 K1 O3 119.70(13) . . ? O4 K1 O6 119.30(14) . . ? O1 K1 O6 60.77(13) . . ? O2 K1 O6 120.42(13) . . ? O5 K1 O6 59.60(13) . . ? O3 K1 O6 175.53(13) . . ? O4 K1 C4 80.79(16) . . ? O1 K1 C4 104.61(16) . . ? O2 K1 C4 103.11(15) . . ? O5 K1 C4 82.27(16) . . ? O3 K1 C4 101.98(16) . . ? O6 K1 C4 82.39(17) . . ? O4 K1 C16 99.52(16) . 2_565 ? O1 K1 C16 75.08(16) . 2_565 ? O2 K1 C16 76.62(15) . 2_565 ? O5 K1 C16 98.00(15) . 2_565 ? O3 K1 C16 78.08(16) . 2_565 ? O6 K1 C16 97.56(16) . 2_565 ? C4 K1 C16 179.66(18) . 2_565 ? O4 K1 C3 102.75(15) . . ? O1 K1 C3 82.39(15) . . ? O2 K1 C3 98.84(14) . . ? O5 K1 C3 86.00(15) . . ? O3 K1 C3 120.21(14) . . ? O6 K1 C3 64.25(14) . . ? C4 K1 C3 23.49(16) . . ? C16 K1 C3 156.26(19) 2_565 . ? O4 K1 C17 76.95(15) . 2_565 ? O1 K1 C17 97.80(15) . 2_565 ? O2 K1 C17 83.80(15) . 2_565 ? O5 K1 C17 91.31(15) . 2_565 ? O3 K1 C17 62.31(15) . 2_565 ? O6 K1 C17 113.24(15) . 2_565 ? C4 K1 C17 157.11(18) . 2_565 ? C16 K1 C17 23.17(16) 2_565 2_565 ? C3 K1 C17 177.03(16) . 2_565 ? C7 Pb1 C13 93.3(2) . . ? C7 Pb1 C1 94.6(2) . . ? C13 Pb1 C1 96.9(2) . . ? 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 C6 C1 C2 C3 -1.0(9) . . . . ? Pb1 C1 C2 C3 174.9(5) . . . . ? C1 C2 C3 C4 -0.5(10) . . . . ? C1 C2 C3 K1 -73.2(6) . . . . ? C2 C3 C4 C5 0.2(10) . . . . ? K1 C3 C4 C5 92.8(6) . . . . ? C2 C3 C4 K1 -92.7(6) . . . . ? C3 C4 C5 C6 1.6(10) . . . . ? K1 C4 C5 C6 90.9(6) . . . . ? C2 C1 C6 C5 2.8(9) . . . . ? Pb1 C1 C6 C5 -172.5(5) . . . . ? C4 C5 C6 C1 -3.2(10) . . . . ? C12 C7 C8 C9 1.7(9) . . . . ? Pb1 C7 C8 C9 173.6(4) . . . . ? C7 C8 C9 C10 -1.8(9) . . . . ? C8 C9 C10 C11 0.6(9) . . . . ? C9 C10 C11 C12 0.5(9) . . . . ? C10 C11 C12 C7 -0.6(10) . . . . ? C8 C7 C12 C11 -0.5(9) . . . . ? Pb1 C7 C12 C11 -172.6(5) . . . . ? C18 C13 C14 C15 -0.8(10) . . . . ? Pb1 C13 C14 C15 -178.6(5) . . . . ? C13 C14 C15 C16 1.5(11) . . . . ? C14 C15 C16 C17 -0.7(10) . . . . ? C14 C15 C16 K1 -95.9(6) . . . 2_564 ? C15 C16 C17 C18 -0.7(10) . . . . ? K1 C16 C17 C18 100.3(6) 2_564 . . . ? C15 C16 C17 K1 -101.0(6) . . . 2_564 ? C16 C17 C18 C13 1.4(9) . . . . ? K1 C17 C18 C13 76.0(6) 2_564 . . . ? C14 C13 C18 C17 -0.7(9) . . . . ? Pb1 C13 C18 C17 177.3(4) . . . . ? O1 C19 C20 O2 -63.0(7) . . . . ? O2 C21 C22 O3 63.1(7) . . . . ? O3 C23 C24 O4 -66.5(6) . . . . ? O4 C25 C26 O5 64.5(6) . . . . ? O5 C27 C28 O6 -65.9(7) . . . . ? O6 C29 C30 O1 66.7(7) . . . . ? C29 C30 O1 C19 177.3(5) . . . . ? C29 C30 O1 K1 -49.2(6) . . . . ? C20 C19 O1 C30 -174.9(5) . . . . ? C20 C19 O1 K1 51.0(6) . . . . ? C19 C20 O2 C21 -177.2(5) . . . . ? C19 C20 O2 K1 43.6(6) . . . . ? C22 C21 O2 C20 177.5(5) . . . . ? C22 C21 O2 K1 -44.0(6) . . . . ? C24 C23 O3 C22 -177.0(5) . . . . ? C24 C23 O3 K1 54.8(5) . . . . ? C21 C22 O3 C23 -177.6(5) . . . . ? C21 C22 O3 K1 -50.9(6) . . . . ? C26 C25 O4 C24 173.0(5) . . . . ? C26 C25 O4 K1 -50.9(5) . . . . ? C23 C24 O4 C25 179.0(5) . . . . ? C23 C24 O4 K1 43.6(6) . . . . ? C28 C27 O5 C26 -173.0(5) . . . . ? C28 C27 O5 K1 51.9(6) . . . . ? C25 C26 O5 C27 178.2(5) . . . . ? C25 C26 O5 K1 -46.4(6) . . . . ? C30 C29 O6 C28 179.7(5) . . . . ? C30 C29 O6 K1 -50.0(6) . . . . ? C27 C28 O6 C29 176.5(6) . . . . ? C27 C28 O6 K1 47.2(6) . . . . ? C25 O4 K1 O1 -59.7(18) . . . . ? C24 O4 K1 O1 73.9(18) . . . . ? C25 O4 K1 O2 -154.7(4) . . . . ? C24 O4 K1 O2 -21.2(4) . . . . ? C25 O4 K1 O5 19.1(4) . . . . ? C24 O4 K1 O5 152.6(4) . . . . ? C25 O4 K1 O3 -145.3(5) . . . . ? C24 O4 K1 O3 -11.8(4) . . . . ? C25 O4 K1 O6 29.6(5) . . . . ? C24 O4 K1 O6 163.1(4) . . . . ? C25 O4 K1 C4 105.4(5) . . . . ? C24 O4 K1 C4 -121.1(4) . . . . ? C25 O4 K1 C16 -74.8(4) . . . 2_565 ? C24 O4 K1 C16 58.8(4) . . . 2_565 ? C25 O4 K1 C3 97.0(4) . . . . ? C24 O4 K1 C3 -129.5(4) . . . . ? C25 O4 K1 C17 -80.0(5) . . . 2_565 ? C24 O4 K1 C17 53.6(4) . . . 2_565 ? C30 O1 K1 O4 109.0(17) . . . . ? C19 O1 K1 O4 -118.6(17) . . . . ? C30 O1 K1 O2 -152.7(4) . . . . ? C19 O1 K1 O2 -20.3(4) . . . . ? C30 O1 K1 O5 33.3(4) . . . . ? C19 O1 K1 O5 165.6(4) . . . . ? C30 O1 K1 O3 -168.3(4) . . . . ? C19 O1 K1 O3 -36.0(5) . . . . ? C30 O1 K1 O6 16.7(4) . . . . ? C19 O1 K1 O6 149.0(5) . . . . ? C30 O1 K1 C4 -55.7(4) . . . . ? C19 O1 K1 C4 76.7(5) . . . . ? C30 O1 K1 C16 124.5(4) . . . 2_565 ? C19 O1 K1 C16 -103.2(5) . . . 2_565 ? C30 O1 K1 C3 -48.0(4) . . . . ? C19 O1 K1 C3 84.4(4) . . . . ? C30 O1 K1 C17 129.0(4) . . . 2_565 ? C19 O1 K1 C17 -98.6(4) . . . 2_565 ? C20 O2 K1 O4 160.3(4) . . . . ? C21 O2 K1 O4 23.1(4) . . . . ? C20 O2 K1 O1 -13.3(4) . . . . ? C21 O2 K1 O1 -150.5(4) . . . . ? C20 O2 K1 O5 64.7(17) . . . . ? C21 O2 K1 O5 -72.6(17) . . . . ? C20 O2 K1 O3 150.8(5) . . . . ? C21 O2 K1 O3 13.6(4) . . . . ? C20 O2 K1 O6 -24.0(5) . . . . ? C21 O2 K1 O6 -161.2(4) . . . . ? C20 O2 K1 C4 -112.8(4) . . . . ? C21 O2 K1 C4 110.0(4) . . . . ? C20 O2 K1 C16 67.0(4) . . . 2_565 ? C21 O2 K1 C16 -70.3(4) . . . 2_565 ? C20 O2 K1 C3 -89.3(4) . . . . ? C21 O2 K1 C3 133.5(4) . . . . ? C20 O2 K1 C17 89.4(4) . . . 2_565 ? C21 O2 K1 C17 -47.9(4) . . . 2_565 ? C27 O5 K1 O4 150.0(4) . . . . ? C26 O5 K1 O4 15.3(4) . . . . ? C27 O5 K1 O1 -36.3(4) . . . . ? C26 O5 K1 O1 -170.9(4) . . . . ? C27 O5 K1 O2 -111.3(16) . . . . ? C26 O5 K1 O2 114.1(16) . . . . ? C27 O5 K1 O3 165.6(4) . . . . ? C26 O5 K1 O3 31.0(4) . . . . ? C27 O5 K1 O6 -19.5(4) . . . . ? C26 O5 K1 O6 -154.1(4) . . . . ? C27 O5 K1 C4 66.2(4) . . . . ? C26 O5 K1 C4 -68.4(4) . . . . ? C27 O5 K1 C16 -113.6(4) . . . 2_565 ? C26 O5 K1 C16 111.8(4) . . . 2_565 ? C27 O5 K1 C3 42.9(4) . . . . ? C26 O5 K1 C3 -91.8(4) . . . . ? C27 O5 K1 C17 -135.8(4) . . . 2_565 ? C26 O5 K1 C17 89.5(4) . . . 2_565 ? C23 O3 K1 O4 -23.1(3) . . . . ? C22 O3 K1 O4 -150.6(4) . . . . ? C23 O3 K1 O1 163.3(3) . . . . ? C22 O3 K1 O1 35.7(4) . . . . ? C23 O3 K1 O2 147.5(4) . . . . ? C22 O3 K1 O2 20.0(3) . . . . ? C23 O3 K1 O5 -38.7(4) . . . . ? C22 O3 K1 O5 -166.2(3) . . . . ? C23 O3 K1 O6 -118.5(16) . . . . ? C22 O3 K1 O6 114.0(16) . . . . ? C23 O3 K1 C4 49.2(4) . . . . ? C22 O3 K1 C4 -78.3(4) . . . . ? C23 O3 K1 C16 -131.2(4) . . . 2_565 ? C22 O3 K1 C16 101.3(4) . . . 2_565 ? C23 O3 K1 C3 65.2(4) . . . . ? C22 O3 K1 C3 -62.3(4) . . . . ? C23 O3 K1 C17 -113.0(4) . . . 2_565 ? C22 O3 K1 C17 119.5(4) . . . 2_565 ? C29 O6 K1 O4 -154.9(4) . . . . ? C28 O6 K1 O4 -26.2(4) . . . . ? C29 O6 K1 O1 18.7(4) . . . . ? C28 O6 K1 O1 147.4(4) . . . . ? C29 O6 K1 O2 29.4(4) . . . . ? C28 O6 K1 O2 158.1(4) . . . . ? C29 O6 K1 O5 -144.3(4) . . . . ? C28 O6 K1 O5 -15.7(4) . . . . ? C29 O6 K1 O3 -62.0(17) . . . . ? C28 O6 K1 O3 66.7(17) . . . . ? C29 O6 K1 C4 130.2(4) . . . . ? C28 O6 K1 C4 -101.2(4) . . . . ? C29 O6 K1 C16 -49.5(4) . . . 2_565 ? C28 O6 K1 C16 79.2(4) . . . 2_565 ? C29 O6 K1 C3 114.5(4) . . . . ? C28 O6 K1 C3 -116.8(4) . . . . ? C29 O6 K1 C17 -67.2(4) . . . 2_565 ? C28 O6 K1 C17 61.4(4) . . . 2_565 ? C3 C4 K1 O4 -159.1(4) . . . . ? C5 C4 K1 O4 82.1(4) . . . . ? C3 C4 K1 O1 19.4(4) . . . . ? C5 C4 K1 O1 -99.4(4) . . . . ? C3 C4 K1 O2 81.9(4) . . . . ? C5 C4 K1 O2 -36.9(4) . . . . ? C3 C4 K1 O5 -97.8(4) . . . . ? C5 C4 K1 O5 143.4(4) . . . . ? C3 C4 K1 O3 143.3(4) . . . . ? C5 C4 K1 O3 24.5(4) . . . . ? C3 C4 K1 O6 -37.6(4) . . . . ? C5 C4 K1 O6 -156.4(4) . . . . ? C3 C4 K1 C16 44(35) . . . 2_565 ? C5 C4 K1 C16 -75(35) . . . 2_565 ? C5 C4 K1 C3 -118.8(6) . . . . ? C3 C4 K1 C17 -172.6(4) . . . 2_565 ? C5 C4 K1 C17 68.6(6) . . . 2_565 ? C4 C3 K1 O4 21.2(4) . . . . ? C2 C3 K1 O4 139.2(4) . . . . ? C4 C3 K1 O1 -161.0(4) . . . . ? C2 C3 K1 O1 -43.0(4) . . . . ? C4 C3 K1 O2 -102.6(4) . . . . ? C2 C3 K1 O2 15.4(4) . . . . ? C4 C3 K1 O5 79.8(4) . . . . ? C2 C3 K1 O5 -162.2(4) . . . . ? C4 C3 K1 O3 -42.5(4) . . . . ? C2 C3 K1 O3 75.5(5) . . . . ? C4 C3 K1 O6 137.8(4) . . . . ? C2 C3 K1 O6 -104.2(4) . . . . ? C2 C3 K1 C4 118.0(6) . . . . ? C4 C3 K1 C16 -179.4(5) . . . 2_565 ? C2 C3 K1 C16 -61.4(6) . . . 2_565 ? C4 C3 K1 C17 105(3) . . . 2_565 ? C2 C3 K1 C17 -137(3) . . . 2_565 ? C8 C7 Pb1 C13 135.7(5) . . . . ? C12 C7 Pb1 C13 -52.7(5) . . . . ? C8 C7 Pb1 C1 38.5(5) . . . . ? C12 C7 Pb1 C1 -149.9(5) . . . . ? C14 C13 Pb1 C7 -27.5(6) . . . . ? C18 C13 Pb1 C7 154.7(5) . . . . ? C14 C13 Pb1 C1 67.5(6) . . . . ? C18 C13 Pb1 C1 -110.3(5) . . . . ? C6 C1 Pb1 C7 13.3(5) . . . . ? C2 C1 Pb1 C7 -162.0(4) . . . . ? C6 C1 Pb1 C13 -80.6(5) . . . . ? C2 C1 Pb1 C13 104.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.497 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.160 _exptl_crystal_recrystallization_method ; From solution in THF layered with n-pentane at -20 deg C. ; _iucr_refine_instructions_details ; TITL ck28_P212121 in P2(1)2(1)2(1) CELL 0.71073 9.6839 12.5929 24.5776 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0004 0.0008 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O K PB UNIT 120 156 24 4 4 MERG 2 OMIT -2.00 56.00 FMAP 2 PLAN 5 ACTA BOND BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.024400 FVAR 0.47290 C1 1 0.299975 0.453568 0.446971 11.00000 0.01751 0.01607 = 0.01424 -0.00764 0.00535 0.00644 C2 1 0.424188 0.463501 0.476777 11.00000 0.01542 0.02600 = 0.01916 -0.00841 0.00194 -0.00003 AFIX 43 H2 2 0.484687 0.520765 0.468717 11.00000 -1.20000 AFIX 0 C3 1 0.460560 0.392379 0.517386 11.00000 0.02299 0.03190 = 0.01728 -0.01195 -0.01359 0.00839 AFIX 43 H3 2 0.545205 0.401283 0.536384 11.00000 -1.20000 AFIX 0 C4 1 0.375168 0.309292 0.530300 11.00000 0.03088 0.02739 = 0.01539 0.00499 0.00230 0.01556 AFIX 43 H4 2 0.399816 0.260580 0.558171 11.00000 -1.20000 AFIX 0 C5 1 0.251137 0.297413 0.501762 11.00000 0.02056 0.01733 = 0.02764 -0.00251 0.01078 0.00914 AFIX 43 H5 2 0.189753 0.241323 0.510882 11.00000 -1.20000 AFIX 0 C6 1 0.217369 0.367557 0.460025 11.00000 0.02435 0.02213 = 0.02093 -0.00481 0.00181 0.00698 AFIX 43 H6 2 0.135017 0.356008 0.439871 11.00000 -1.20000 AFIX 0 C7 1 0.016813 0.547907 0.378451 11.00000 0.01248 0.02058 = 0.00989 -0.00398 -0.00076 0.00265 C8 1 -0.061915 0.514210 0.422984 11.00000 0.02278 0.01773 = 0.01987 -0.00066 -0.00174 0.00654 AFIX 43 H8 2 -0.016508 0.501537 0.456626 11.00000 -1.20000 AFIX 0 C9 1 -0.203211 0.498592 0.420023 11.00000 0.01609 0.02354 = 0.01817 0.00358 0.00587 0.00266 AFIX 43 H9 2 -0.252470 0.473695 0.450921 11.00000 -1.20000 AFIX 0 C10 1 -0.272623 0.519360 0.371888 11.00000 0.00921 0.02695 = 0.02412 -0.00430 0.00046 0.00025 AFIX 43 H10 2 -0.369707 0.509666 0.369407 11.00000 -1.20000 AFIX 0 C11 1 -0.197358 0.554597 0.327413 11.00000 0.02173 0.03122 = 0.02428 -0.00364 -0.00403 -0.00225 AFIX 43 H11 2 -0.244017 0.569663 0.294299 11.00000 -1.20000 AFIX 0 C12 1 -0.055377 0.568323 0.330231 11.00000 0.01707 0.02169 = 0.01489 -0.00289 0.00277 0.00319 AFIX 43 H12 2 -0.006453 0.591918 0.298985 11.00000 -1.20000 AFIX 0 C13 1 0.307808 0.498397 0.306499 11.00000 0.01683 0.01621 = 0.01011 0.00180 0.00010 0.00105 C14 1 0.235116 0.411655 0.286548 11.00000 0.01914 0.02308 = 0.02228 0.00767 0.00178 0.00107 AFIX 43 H14 2 0.155084 0.388138 0.305376 11.00000 -1.20000 AFIX 0 C15 1 0.276626 0.357977 0.239451 11.00000 0.02829 0.02050 = 0.02186 -0.00092 -0.00351 -0.00241 AFIX 43 H15 2 0.223875 0.299907 0.226154 11.00000 -1.20000 AFIX 0 C16 1 0.395339 0.389950 0.212198 11.00000 0.03045 0.03771 = 0.01006 -0.00122 0.00129 0.01256 AFIX 43 H16 2 0.424898 0.353474 0.180432 11.00000 -1.20000 AFIX 0 C17 1 0.469314 0.474654 0.231633 11.00000 0.01935 0.03424 = 0.01443 0.01210 0.00600 0.00327 AFIX 43 H17 2 0.551097 0.496355 0.213410 11.00000 -1.20000 AFIX 0 C18 1 0.425746 0.529167 0.277810 11.00000 0.01302 0.02193 = 0.02013 0.00860 -0.00844 0.00019 AFIX 43 H18 2 0.477387 0.588655 0.290099 11.00000 -1.20000 AFIX 0 C19 1 0.231402 0.703766 0.546281 11.00000 0.03617 0.02119 = 0.01668 0.00641 -0.00034 0.00144 AFIX 23 H19A 2 0.255452 0.665672 0.512344 11.00000 -1.20000 H19B 2 0.252595 0.780010 0.541113 11.00000 -1.20000 AFIX 0 C20 1 0.081459 0.690140 0.558186 11.00000 0.03708 0.02264 = 0.02251 0.00135 -0.00447 0.00681 AFIX 23 H20A 2 0.058030 0.726188 0.592772 11.00000 -1.20000 H20B 2 0.025844 0.722598 0.528762 11.00000 -1.20000 AFIX 0 C21 1 -0.092691 0.561262 0.571048 11.00000 0.02507 0.03080 = 0.01046 0.00665 -0.00697 0.00485 AFIX 23 H21A 2 -0.147926 0.593626 0.541486 11.00000 -1.20000 H21B 2 -0.122127 0.593127 0.605998 11.00000 -1.20000 AFIX 0 C22 1 -0.115688 0.444080 0.572238 11.00000 0.02022 0.03034 = 0.01237 0.00082 -0.00178 -0.00288 AFIX 23 H22A 2 -0.215587 0.429011 0.575923 11.00000 -1.20000 H22B 2 -0.083085 0.412157 0.537742 11.00000 -1.20000 AFIX 0 C23 1 -0.056301 0.286093 0.618679 11.00000 0.01645 0.02339 = 0.02154 -0.00564 0.00345 -0.00513 AFIX 23 H23A 2 -0.015466 0.254110 0.585587 11.00000 -1.20000 H23B 2 -0.155147 0.266252 0.620208 11.00000 -1.20000 AFIX 0 C24 1 0.017551 0.245488 0.668674 11.00000 0.01983 0.01411 = 0.02755 -0.00139 0.00032 -0.00523 AFIX 23 H24A 2 -0.016744 0.282824 0.701446 11.00000 -1.20000 H24B 2 0.000028 0.168548 0.673234 11.00000 -1.20000 AFIX 0 C25 1 0.238797 0.229346 0.708538 11.00000 0.02512 0.01862 = 0.01801 0.00913 0.00416 0.00097 AFIX 23 H25A 2 0.214792 0.154723 0.716974 11.00000 -1.20000 H25B 2 0.214927 0.273653 0.740455 11.00000 -1.20000 AFIX 0 C26 1 0.388982 0.238076 0.696796 11.00000 0.01369 0.02271 = 0.02569 0.00170 -0.00284 0.00368 AFIX 23 H26A 2 0.443060 0.208347 0.727398 11.00000 -1.20000 H26B 2 0.411922 0.197592 0.663471 11.00000 -1.20000 AFIX 0 C27 1 0.563938 0.366050 0.679633 11.00000 0.01118 0.02987 = 0.02279 0.00396 -0.00402 0.00040 AFIX 23 H27A 2 0.590715 0.335341 0.644086 11.00000 -1.20000 H27B 2 0.620155 0.331777 0.708330 11.00000 -1.20000 AFIX 0 C28 1 0.589267 0.482927 0.679533 11.00000 0.01667 0.03421 = 0.01656 0.00192 -0.00094 -0.00556 AFIX 23 H28A 2 0.554655 0.514800 0.713736 11.00000 -1.20000 H28B 2 0.689507 0.497397 0.676769 11.00000 -1.20000 AFIX 0 C29 1 0.531188 0.640876 0.632913 11.00000 0.02038 0.02276 = 0.01678 -0.00562 -0.00064 -0.00648 AFIX 23 H29A 2 0.629769 0.661320 0.630892 11.00000 -1.20000 H29B 2 0.491273 0.671702 0.666465 11.00000 -1.20000 AFIX 0 C30 1 0.454692 0.681658 0.583552 11.00000 0.02863 0.02152 = 0.02392 -0.00857 0.00834 -0.00584 AFIX 23 H30A 2 0.471605 0.758713 0.579146 11.00000 -1.20000 H30B 2 0.488204 0.644938 0.550474 11.00000 -1.20000 AFIX 0 O1 3 0.310568 0.662604 0.590448 11.00000 0.02854 0.02441 = 0.01519 0.00492 0.00104 -0.00606 O2 3 0.050873 0.581314 0.562176 11.00000 0.02366 0.01745 = 0.01951 0.00088 0.00078 0.00107 O3 3 -0.042779 0.398553 0.616795 11.00000 0.02119 0.02034 = 0.01711 0.00242 -0.00325 -0.00239 O4 3 0.163216 0.264345 0.662066 11.00000 0.01714 0.02212 = 0.02317 0.00465 0.00083 -0.00357 O5 3 0.422268 0.347585 0.689443 11.00000 0.01598 0.02134 = 0.02571 0.00306 -0.00155 -0.00045 O6 3 0.518323 0.528018 0.633783 11.00000 0.02560 0.01895 = 0.02192 -0.00161 -0.00110 -0.00458 K1 4 0.240017 0.459004 0.621441 11.00000 0.01663 0.01511 = 0.02519 0.00397 -0.00060 -0.00001 PB1 5 0.249690 0.590535 0.385516 11.00000 0.01602 0.01585 = 0.02015 -0.00190 -0.00060 0.00036 HKLF 4 REM ck28_P212121 in P2(1)2(1)2(1) REM R1 = 0.0380 for 5122 Fo > 4sig(Fo) and 0.0762 for all 7157 data REM 343 parameters refined using 0 restraints END WGHT 0.0244 0.0000 REM Highest difference peak 1.497, deepest hole -0.788, 1-sigma level 0.160 Q1 1 -0.2512 0.2722 0.6146 11.00000 0.05 1.50 Q2 1 0.2524 0.4134 0.3439 11.00000 0.05 1.35 Q3 1 0.2148 0.5164 0.3937 11.00000 0.05 1.08 Q4 1 0.2981 0.6752 0.3858 11.00000 0.05 1.02 Q5 1 0.2111 0.6726 0.3859 11.00000 0.05 0.98 ; #================================================END