# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Goicoechea, Jose' _publ_contact_author_email jose.goicoechea@chem.ox.ac.uk _publ_section_title ; A versatile salt-metathesis route to heteroatomic clusters derived from phosphorus and arsenic Zintl anions ; _publ_contact_author ; Dr. J. M. Goicoechea Chemistry Research Laboratory University of Oxford Mansfield Road Oxford OX1 3TA UK ; _publ_contact_author_fax '+44 1865 272690' _publ_contact_author_phone '+44 1865 275961' loop_ _publ_author_name C.Knapp J.Large N.Rees J.Goicoechea # Attachment '- combined_revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 786255' #TrackingRef '- combined_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]6[In(P7)2]2*7py ; _chemical_name_common (K(2,2,2-crypt))6(In(P7)2)2*7py _chemical_melting_point . _chemical_formula_moiety '6(C18 H36 K N2 O6), 2(In P14), 7(C5 H5 N)' _chemical_formula_sum 'C143 H251 In2 K6 N19 O36 P28' _chemical_formula_weight 4144.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.97760(10) _cell_length_b 25.12080(10) _cell_length_c 27.1871(2) _cell_angle_alpha 113.8600(10) _cell_angle_beta 94.3940(10) _cell_angle_gamma 94.2590(10) _cell_volume 9883.65(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 235366 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4324 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7795 _exptl_absorpt_correction_T_max 0.9374 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 82170 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 27.47 _reflns_number_total 44881 _reflns_number_gt 26797 _reflns_threshold_expression >2\s(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The 2,2,2-crypt moiety associated with K6 exhibits some disorder in one of the cryptand arms. This was modelled and the the following constraints and restraints were applied: DFIX 1.60 0.020 C601 C602 DFIX 1.50 0.020 O61 C603 DFIX 1.50 0.020 C603 C604 DFIX 1.50 0.020 C604 O62 DFIX 2.500 0.020 O61 C604 DFIX 2.500 0.020 C603 O62 DFIX 1.50 0.020 O61 C3A DFIX 1.50 0.020 C3A C4A DFIX 1.50 0.010 C4A O62 DFIX 2.500 0.020 O61 C4A DFIX 2.500 0.020 C3A O62 DFIX 2.500 0.020 C4A C605 EADP O61 C3A EADP C4A O62 EADP C601 C602 EADP C603 C604 EADP N11 C613 ISOR 0.02 C3A C4A C602 C604 C613 DFIX 2.500 0.020 C602 N61 DFIX 2.500 0.020 O61 C601 ; _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^)+(0.0417P)^2^+1.9222P] 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 44881 _refine_ls_number_parameters 2096 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.022 _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 In1 In 0.348677(13) 0.232971(9) 0.599123(8) 0.03072(6) Uani 1 1 d . . . P11 P 0.44784(5) 0.32268(3) 0.56268(3) 0.03133(18) Uani 1 1 d . . . P12 P 0.49061(5) 0.23965(4) 0.56108(3) 0.03221(18) Uani 1 1 d . . . P13 P 0.31080(5) 0.29221(3) 0.54317(3) 0.03011(18) Uani 1 1 d . . . P14 P 0.48227(5) 0.32371(4) 0.48825(3) 0.03468(19) Uani 1 1 d . . . P15 P 0.43554(5) 0.17983(3) 0.47997(3) 0.03286(19) Uani 1 1 d . . . P16 P 0.31269(5) 0.21510(3) 0.46768(3) 0.03223(18) Uani 1 1 d . . . P17 P 0.42826(5) 0.23721(4) 0.43496(3) 0.03449(19) Uani 1 1 d . . . P21 P 0.22365(5) 0.19406(4) 0.66979(3) 0.03192(18) Uani 1 1 d . . . P22 P 0.34587(5) 0.25147(3) 0.70088(3) 0.03393(19) Uani 1 1 d . . . P23 P 0.25747(5) 0.13951(3) 0.58872(3) 0.02956(17) Uani 1 1 d . . . P24 P 0.22782(5) 0.13606(4) 0.70984(4) 0.0399(2) Uani 1 1 d . . . P25 P 0.43068(5) 0.18455(4) 0.68927(3) 0.03356(19) Uani 1 1 d . . . P26 P 0.37157(5) 0.10870(3) 0.61171(3) 0.03075(18) Uani 1 1 d . . . P27 P 0.35023(5) 0.10937(4) 0.69209(3) 0.03364(19) Uani 1 1 d . . . In2 In 0.847972(13) 0.239332(9) 0.115427(9) 0.03432(6) Uani 1 1 d . . . P31 P 0.95416(5) 0.33557(3) 0.09117(3) 0.03276(18) Uani 1 1 d . . . P32 P 0.99263(5) 0.24900(4) 0.08206(3) 0.03608(19) Uani 1 1 d . . . P33 P 0.81674(5) 0.30749(3) 0.06729(3) 0.03313(19) Uani 1 1 d . . . P34 P 0.99517(5) 0.34482(3) 0.02154(3) 0.03388(19) Uani 1 1 d . . . P35 P 0.94032(5) 0.19680(3) -0.00148(4) 0.0365(2) Uani 1 1 d . . . P36 P 0.82024(5) 0.23598(3) -0.01168(3) 0.03415(19) Uani 1 1 d . . . P37 P 0.94007(5) 0.26139(3) -0.03884(3) 0.03501(19) Uani 1 1 d . . . P41 P 0.72180(5) 0.18918(4) 0.17784(3) 0.03522(19) Uani 1 1 d . . . P42 P 0.84210(6) 0.24729(4) 0.21347(3) 0.0411(2) Uani 1 1 d . . . P43 P 0.75751(5) 0.14238(3) 0.09523(3) 0.03008(18) Uani 1 1 d . . . P44 P 0.72846(5) 0.12394(4) 0.20975(4) 0.0427(2) Uani 1 1 d . . . P45 P 0.93018(5) 0.18111(4) 0.19541(3) 0.0400(2) Uani 1 1 d . . . P46 P 0.87312(5) 0.11033(3) 0.11412(3) 0.03237(18) Uani 1 1 d . . . P47 P 0.85221(5) 0.10143(4) 0.19076(4) 0.0390(2) Uani 1 1 d . . . K1 K 0.70680(4) -0.06813(3) 0.83249(2) 0.02753(14) Uani 1 1 d . . . K2 K 0.79400(4) 0.08457(3) 0.67328(2) 0.02767(14) Uani 1 1 d . . . K3 K 0.26651(4) 0.57968(3) 0.17164(3) 0.03557(16) Uani 1 1 d . . . K4 K 0.37406(4) 0.17267(3) 0.96888(2) 0.02642(14) Uani 1 1 d . . . K5 K 0.74124(4) 0.41434(3) 0.35404(3) 0.04265(18) Uani 1 1 d . . . K6 K 0.87840(4) 0.17178(3) 0.46134(2) 0.02822(14) Uani 1 1 d . A . N11 N 0.53940(16) -0.10427(12) 0.76436(12) 0.0468(5) Uani 1 1 d . . . N12 N 0.87334(15) -0.03259(12) 0.89967(10) 0.0399(6) Uani 1 1 d . . . N21 N 0.63313(14) 0.04343(11) 0.60005(10) 0.0343(6) Uani 1 1 d . . . N22 N 0.95326(16) 0.12570(11) 0.74773(10) 0.0402(6) Uani 1 1 d . . . N31 N 0.17352(16) 0.52151(11) 0.06130(10) 0.0427(7) Uani 1 1 d . . . N32 N 0.36244(17) 0.63828(13) 0.28119(11) 0.0517(8) Uani 1 1 d . . . N41 N 0.22776(15) 0.09475(11) 0.89451(10) 0.0391(6) Uani 1 1 d . . . N42 N 0.52230(15) 0.24955(10) 1.04455(9) 0.0318(6) Uani 1 1 d . . . N51 N 0.55425(18) 0.41064(13) 0.33989(14) 0.0598(9) Uani 1 1 d . . . N52 N 0.92725(17) 0.42164(13) 0.37145(12) 0.0537(8) Uani 1 1 d . . . N61 N 1.02374(18) 0.25764(15) 0.52914(15) 0.0622(9) Uani 1 1 d D A . N62 N 0.73554(18) 0.08651(11) 0.39127(10) 0.0443(7) Uani 1 1 d . A . O11 O 0.57700(11) 0.01140(8) 0.85729(7) 0.0315(5) Uani 1 1 d . . . O12 O 0.72299(12) 0.03140(8) 0.92983(8) 0.0326(5) Uani 1 1 d . . . O13 O 0.69973(12) -0.09210(9) 0.72235(8) 0.0352(5) Uani 1 1 d . . . O14 O 0.85383(12) -0.03904(9) 0.78857(8) 0.0364(5) Uani 1 1 d . . . O15 O 0.60854(13) -0.17325(8) 0.82105(8) 0.0355(5) Uani 1 1 d . . . O16 O 0.77637(13) -0.14835(10) 0.86893(9) 0.0426(5) Uani 1 1 d . . . O21 O 0.64232(12) 0.05842(9) 0.71368(8) 0.0373(5) Uani 1 1 d . . . O22 O 0.78754(14) 0.12001(9) 0.78588(8) 0.0435(5) Uani 1 1 d . . . O23 O 0.72918(12) 0.15840(9) 0.62643(8) 0.0341(5) Uani 1 1 d . . . O24 O 0.89535(12) 0.18455(8) 0.67885(8) 0.0379(5) Uani 1 1 d . . . O25 O 0.78923(12) -0.01635(8) 0.57808(8) 0.0321(5) Uani 1 1 d . . . O26 O 0.92562(12) 0.00767(8) 0.65826(8) 0.0339(5) Uani 1 1 d . . . O31 O 0.09379(14) 0.53901(10) 0.16042(9) 0.0509(6) Uani 1 1 d . . . O32 O 0.19358(15) 0.57345(11) 0.26052(9) 0.0566(7) Uani 1 1 d . . . O33 O 0.23742(14) 0.64687(9) 0.11079(9) 0.0486(6) Uani 1 1 d . . . O34 O 0.29120(15) 0.70274(9) 0.22267(10) 0.0541(6) Uani 1 1 d . . . O35 O 0.33142(14) 0.48201(9) 0.09162(9) 0.0439(5) Uani 1 1 d . . . O36 O 0.43249(13) 0.55152(9) 0.18937(9) 0.0465(6) Uani 1 1 d . . . O41 O 0.21782(14) 0.21749(11) 0.96524(10) 0.0530(6) Uani 1 1 d . . . O42 O 0.34774(14) 0.27933(9) 1.05351(9) 0.0455(6) Uani 1 1 d . . . O43 O 0.38658(13) 0.12008(9) 0.85624(8) 0.0360(5) Uani 1 1 d . . . O44 O 0.50582(11) 0.21430(8) 0.92748(8) 0.0320(5) Uani 1 1 d . . . O45 O 0.31937(11) 0.06740(8) 0.97805(8) 0.0308(5) Uani 1 1 d . . . O46 O 0.47758(12) 0.12838(8) 1.02986(8) 0.0313(5) Uani 1 1 d . . . O51 O 0.66302(16) 0.41686(11) 0.25789(10) 0.0596(7) Uani 1 1 d . . . O52 O 0.83391(16) 0.40511(10) 0.26984(9) 0.0558(6) Uani 1 1 d . . . O53 O 0.63840(16) 0.31456(10) 0.34716(9) 0.0536(6) Uani 1 1 d . . . O54 O 0.81175(16) 0.33158(10) 0.38571(9) 0.0546(6) Uani 1 1 d . . . O55 O 0.66034(16) 0.50472(10) 0.42933(11) 0.0682(8) Uani 1 1 d . . . O56 O 0.83542(15) 0.52033(10) 0.43154(10) 0.0561(6) Uani 1 1 d . . . O61 O 1.0023(2) 0.21406(10) 0.41189(11) 0.0788(9) Uani 1 1 d D . . O62 O 0.89545(14) 0.10573(11) 0.35163(9) 0.0572(7) Uani 1 1 d D . . O63 O 0.84875(15) 0.28380(10) 0.53970(9) 0.0520(6) Uani 1 1 d . . . O64 O 0.72022(12) 0.20996(10) 0.45633(9) 0.0429(6) Uani 1 1 d . . . O65 O 0.98700(13) 0.13885(11) 0.52659(10) 0.0514(6) Uani 1 1 d . . . O66 O 0.83276(13) 0.07034(9) 0.48002(8) 0.0381(5) Uani 1 1 d . . . C101 C 0.49112(19) -0.05333(13) 0.77570(13) 0.0384(8) Uani 1 1 d . . . H10A H 0.4317 -0.0678 0.7597 0.046 Uiso 1 1 calc R . . H10B H 0.5146 -0.0294 0.7576 0.046 Uiso 1 1 calc R . . C102 C 0.49238(18) -0.01485(13) 0.83503(12) 0.0363(7) Uani 1 1 d . . . H10C H 0.4548 0.0160 0.8398 0.044 Uiso 1 1 calc R . . H10D H 0.4717 -0.0385 0.8541 0.044 Uiso 1 1 calc R . . C103 C 0.58081(18) 0.04749(12) 0.91337(11) 0.0304(7) Uani 1 1 d . . . H10E H 0.5621 0.0236 0.9327 0.036 Uiso 1 1 calc R . . H10F H 0.5424 0.0781 0.9190 0.036 Uiso 1 1 calc R . . C104 C 0.66866(19) 0.07551(12) 0.93545(12) 0.0339(7) Uani 1 1 d . . . H10G H 0.6879 0.0988 0.9157 0.041 Uiso 1 1 calc R . . H10H H 0.6705 0.1023 0.9742 0.041 Uiso 1 1 calc R . . C105 C 0.80796(19) 0.05768(15) 0.95054(13) 0.0461(9) Uani 1 1 d . . . H10I H 0.8091 0.0893 0.9872 0.055 Uiso 1 1 calc R . . H10J H 0.8306 0.0751 0.9268 0.055 Uiso 1 1 calc R . . C106 C 0.8613(2) 0.01220(16) 0.95301(13) 0.0508(9) Uani 1 1 d . . . H10K H 0.9174 0.0318 0.9727 0.061 Uiso 1 1 calc R . . H10L H 0.8348 -0.0074 0.9740 0.061 Uiso 1 1 calc R . . C107 C 0.5535(2) -0.12918(13) 0.70670(11) 0.0368(7) Uani 1 1 d . . . H10M H 0.4997 -0.1328 0.6844 0.044 Uiso 1 1 calc R . . H10N H 0.5702 -0.1691 0.6968 0.044 Uiso 1 1 calc R . . C108 C 0.6202(2) -0.09325(14) 0.69338(12) 0.0388(8) Uani 1 1 d . . . H10O H 0.6241 -0.1107 0.6539 0.047 Uiso 1 1 calc R . . H10P H 0.6052 -0.0529 0.7039 0.047 Uiso 1 1 calc R . . C109 C 0.7673(2) -0.06721(14) 0.70437(12) 0.0403(8) Uani 1 1 d . . . H10Q H 0.7612 -0.0255 0.7132 0.048 Uiso 1 1 calc R . . H10R H 0.7657 -0.0880 0.6646 0.048 Uiso 1 1 calc R . . C110 C 0.8494(2) -0.07197(14) 0.73110(13) 0.0409(8) Uani 1 1 d . . . H11A H 0.8549 -0.1136 0.7229 0.049 Uiso 1 1 calc R . . H11B H 0.8965 -0.0567 0.7170 0.049 Uiso 1 1 calc R . . C111 C 0.93262(19) -0.04271(16) 0.81493(14) 0.0457(9) Uani 1 1 d . . . H11C H 0.9797 -0.0270 0.8012 0.055 Uiso 1 1 calc R . . H11D H 0.9390 -0.0842 0.8071 0.055 Uiso 1 1 calc R . . C112 C 0.93547(19) -0.00822(16) 0.87467(14) 0.0469(9) Uani 1 1 d . . . H11E H 0.9928 -0.0067 0.8921 0.056 Uiso 1 1 calc R . . H11F H 0.9250 0.0325 0.8817 0.056 Uiso 1 1 calc R . . C113 C 0.49105(18) -0.14891(13) 0.77657(12) 0.0354(7) Uani 1 1 d . . . H11G H 0.4417 -0.1670 0.7487 0.042 Uiso 1 1 calc R . . H11H H 0.4694 -0.1293 0.8119 0.042 Uiso 1 1 calc R . . C114 C 0.5410(2) -0.19665(13) 0.77855(13) 0.0396(8) Uani 1 1 d . . . H11I H 0.5034 -0.2263 0.7843 0.048 Uiso 1 1 calc R . . H11J H 0.5637 -0.2163 0.7436 0.048 Uiso 1 1 calc R . . C115 C 0.6576(2) -0.21743(14) 0.82319(15) 0.0476(9) Uani 1 1 d . . . H11K H 0.6874 -0.2328 0.7905 0.057 Uiso 1 1 calc R . . H11L H 0.6201 -0.2503 0.8239 0.057 Uiso 1 1 calc R . . C116 C 0.7200(2) -0.19291(15) 0.87216(15) 0.0477(9) Uani 1 1 d . . . H11M H 0.6905 -0.1764 0.9049 0.057 Uiso 1 1 calc R . . H11N H 0.7518 -0.2242 0.8747 0.057 Uiso 1 1 calc R . . C117 C 0.8386(2) -0.12319(17) 0.91521(14) 0.0501(9) Uani 1 1 d . . . H11O H 0.8650 -0.1547 0.9215 0.060 Uiso 1 1 calc R . . H11P H 0.8116 -0.1003 0.9477 0.060 Uiso 1 1 calc R . . C118 C 0.9051(2) -0.08375(16) 0.90576(15) 0.0501(9) Uani 1 1 d . . . H11Q H 0.9505 -0.0695 0.9365 0.060 Uiso 1 1 calc R . . H11R H 0.9304 -0.1070 0.8727 0.060 Uiso 1 1 calc R . . C201 C 0.56955(19) 0.01895(15) 0.62405(14) 0.0461(9) Uani 1 1 d . . . H20A H 0.5828 -0.0204 0.6199 0.055 Uiso 1 1 calc R . . H20B H 0.5134 0.0141 0.6036 0.055 Uiso 1 1 calc R . . C202 C 0.5646(2) 0.05563(16) 0.68262(15) 0.0494(9) Uani 1 1 d . . . H20C H 0.5534 0.0956 0.6876 0.059 Uiso 1 1 calc R . . H20D H 0.5176 0.0384 0.6952 0.059 Uiso 1 1 calc R . . C203 C 0.6384(2) 0.09355(14) 0.76929(14) 0.0492(9) Uani 1 1 d . . . H20E H 0.5898 0.0776 0.7817 0.059 Uiso 1 1 calc R . . H20F H 0.6297 0.1340 0.7743 0.059 Uiso 1 1 calc R . . C204 C 0.7178(2) 0.09462(15) 0.80209(14) 0.0534(10) Uani 1 1 d . . . H20G H 0.7135 0.1178 0.8410 0.064 Uiso 1 1 calc R . . H20H H 0.7268 0.0542 0.7969 0.064 Uiso 1 1 calc R . . C205 C 0.8642(2) 0.12533(16) 0.81909(14) 0.0576(10) Uani 1 1 d . . . H20I H 0.8786 0.0859 0.8141 0.069 Uiso 1 1 calc R . . H20J H 0.8570 0.1475 0.8577 0.069 Uiso 1 1 calc R . . C206 C 0.9343(2) 0.15675(16) 0.80364(14) 0.0557(10) Uani 1 1 d . . . H20K H 0.9186 0.1958 0.8085 0.067 Uiso 1 1 calc R . . H20L H 0.9860 0.1628 0.8286 0.067 Uiso 1 1 calc R . . C207 C 0.60146(19) 0.09233(14) 0.59057(13) 0.0405(8) Uani 1 1 d . . . H20M H 0.5749 0.1169 0.6226 0.049 Uiso 1 1 calc R . . H20N H 0.5570 0.0762 0.5592 0.049 Uiso 1 1 calc R . . C208 C 0.66835(19) 0.13057(15) 0.57987(13) 0.0406(8) Uani 1 1 d . . . H20O H 0.6965 0.1064 0.5484 0.049 Uiso 1 1 calc R . . H20P H 0.6419 0.1606 0.5712 0.049 Uiso 1 1 calc R . . C209 C 0.79075(19) 0.19746(13) 0.61885(13) 0.0373(7) Uani 1 1 d . . . H20Q H 0.7626 0.2270 0.6102 0.045 Uiso 1 1 calc R . . H20R H 0.8219 0.1754 0.5882 0.045 Uiso 1 1 calc R . . C210 C 0.8509(2) 0.22735(14) 0.66932(14) 0.0449(8) Uani 1 1 d . . . H21A H 0.8914 0.2568 0.6654 0.054 Uiso 1 1 calc R . . H21B H 0.8195 0.2478 0.7004 0.054 Uiso 1 1 calc R . . C211 C 0.9604(2) 0.21173(14) 0.72312(15) 0.0482(9) Uani 1 1 d . . . H21C H 0.9356 0.2353 0.7563 0.058 Uiso 1 1 calc R . . H21D H 1.0009 0.2383 0.7153 0.058 Uiso 1 1 calc R . . C212 C 1.0056(2) 0.16541(15) 0.73177(15) 0.0493(9) Uani 1 1 d . . . H21E H 1.0286 0.1417 0.6979 0.059 Uiso 1 1 calc R . . H21F H 1.0540 0.1849 0.7601 0.059 Uiso 1 1 calc R . . C213 C 0.6503(2) -0.00264(15) 0.54863(13) 0.0473(9) Uani 1 1 d . . . H21G H 0.6777 0.0161 0.5273 0.057 Uiso 1 1 calc R . . H21H H 0.5959 -0.0243 0.5277 0.057 Uiso 1 1 calc R . . C214 C 0.7057(2) -0.04565(13) 0.55530(13) 0.0407(8) Uani 1 1 d . . . H21I H 0.6820 -0.0621 0.5795 0.049 Uiso 1 1 calc R . . H21J H 0.7081 -0.0783 0.5197 0.049 Uiso 1 1 calc R . . C215 C 0.84726(19) -0.05808(13) 0.57460(12) 0.0355(7) Uani 1 1 d . . . H21K H 0.8519 -0.0831 0.5361 0.043 Uiso 1 1 calc R . . H21L H 0.8267 -0.0836 0.5920 0.043 Uiso 1 1 calc R . . C216 C 0.93126(18) -0.02628(13) 0.60236(12) 0.0349(7) Uani 1 1 d . . . H21M H 0.9726 -0.0547 0.5986 0.042 Uiso 1 1 calc R . . H21N H 0.9512 -0.0003 0.5853 0.042 Uiso 1 1 calc R . . C217 C 1.0075(2) 0.03411(15) 0.68677(16) 0.0539(10) Uani 1 1 d . . . H21O H 1.0359 0.0559 0.6682 0.065 Uiso 1 1 calc R . . H21P H 1.0425 0.0033 0.6870 0.065 Uiso 1 1 calc R . . C218 C 0.9988(2) 0.07507(15) 0.74363(15) 0.0562(10) Uani 1 1 d . . . H21Q H 0.9684 0.0530 0.7612 0.067 Uiso 1 1 calc R . . H21R H 1.0559 0.0899 0.7638 0.067 Uiso 1 1 calc R . . C301 C 0.0824(2) 0.51272(16) 0.06515(15) 0.0555(10) Uani 1 1 d . . . H30A H 0.0546 0.4826 0.0301 0.067 Uiso 1 1 calc R . . H30B H 0.0582 0.5498 0.0714 0.067 Uiso 1 1 calc R . . C302 C 0.0619(2) 0.49416(15) 0.10909(15) 0.0545(10) Uani 1 1 d . . . H30C H -0.0002 0.4859 0.1072 0.065 Uiso 1 1 calc R . . H30D H 0.0872 0.4578 0.1041 0.065 Uiso 1 1 calc R . . C303 C 0.0660(2) 0.52631(17) 0.20324(16) 0.0627(11) Uani 1 1 d . . . H30E H 0.0827 0.4879 0.1999 0.075 Uiso 1 1 calc R . . H30F H 0.0036 0.5240 0.2011 0.075 Uiso 1 1 calc R . . C304 C 0.1046(2) 0.57343(19) 0.25664(16) 0.0681(12) Uani 1 1 d . . . H30G H 0.0899 0.6120 0.2594 0.082 Uiso 1 1 calc R . . H30H H 0.0824 0.5661 0.2866 0.082 Uiso 1 1 calc R . . C305 C 0.2322(2) 0.6091(2) 0.31391(15) 0.0701(12) Uani 1 1 d . . . H30I H 0.2133 0.5925 0.3392 0.084 Uiso 1 1 calc R . . H30J H 0.2150 0.6490 0.3256 0.084 Uiso 1 1 calc R . . C306 C 0.3278(3) 0.6120(2) 0.31545(16) 0.0739(13) Uani 1 1 d . . . H30K H 0.3535 0.6350 0.3533 0.089 Uiso 1 1 calc R . . H30L H 0.3440 0.5718 0.3039 0.089 Uiso 1 1 calc R . . C307 C 0.1889(2) 0.55861(16) 0.03200(14) 0.0530(9) Uani 1 1 d . . . H30M H 0.1496 0.5430 -0.0019 0.064 Uiso 1 1 calc R . . H30N H 0.2472 0.5561 0.0220 0.064 Uiso 1 1 calc R . . C308 C 0.1778(2) 0.62209(16) 0.06359(15) 0.0585(10) Uani 1 1 d . . . H30O H 0.1860 0.6439 0.0407 0.070 Uiso 1 1 calc R . . H30P H 0.1198 0.6253 0.0741 0.070 Uiso 1 1 calc R . . C309 C 0.2210(3) 0.70508(16) 0.14389(18) 0.0724(12) Uani 1 1 d . . . H30Q H 0.1663 0.7037 0.1584 0.087 Uiso 1 1 calc R . . H30R H 0.2170 0.7280 0.1217 0.087 Uiso 1 1 calc R . . C310 C 0.2879(3) 0.73342(17) 0.18832(19) 0.0734(12) Uani 1 1 d . . . H31A H 0.3427 0.7341 0.1738 0.088 Uiso 1 1 calc R . . H31B H 0.2776 0.7744 0.2096 0.088 Uiso 1 1 calc R . . C311 C 0.3594(2) 0.72781(16) 0.26398(16) 0.0622(11) Uani 1 1 d . . . H31C H 0.3573 0.7706 0.2826 0.075 Uiso 1 1 calc R . . H31D H 0.4133 0.7214 0.2479 0.075 Uiso 1 1 calc R . . C312 C 0.3558(2) 0.70164(17) 0.30326(15) 0.0641(12) Uani 1 1 d . . . H31E H 0.3018 0.7088 0.3191 0.077 Uiso 1 1 calc R . . H31F H 0.4021 0.7219 0.3330 0.077 Uiso 1 1 calc R . . C313 C 0.2040(2) 0.46447(15) 0.03263(14) 0.0525(9) Uani 1 1 d . . . H31G H 0.1816 0.4490 -0.0061 0.063 Uiso 1 1 calc R . . H31H H 0.1808 0.4369 0.0472 0.063 Uiso 1 1 calc R . . C314 C 0.2986(2) 0.46589(15) 0.03695(13) 0.0499(9) Uani 1 1 d . . . H31I H 0.3141 0.4268 0.0140 0.060 Uiso 1 1 calc R . . H31J H 0.3231 0.4945 0.0239 0.060 Uiso 1 1 calc R . . C315 C 0.4208(2) 0.48394(15) 0.09698(14) 0.0468(9) Uani 1 1 d . . . H31K H 0.4460 0.5151 0.0872 0.056 Uiso 1 1 calc R . . H31L H 0.4373 0.4460 0.0720 0.056 Uiso 1 1 calc R . . C316 C 0.4530(2) 0.49598(15) 0.15374(14) 0.0496(9) Uani 1 1 d . . . H31M H 0.4273 0.4651 0.1636 0.059 Uiso 1 1 calc R . . H31N H 0.5150 0.4955 0.1570 0.059 Uiso 1 1 calc R . . C317 C 0.4677(2) 0.56737(18) 0.24359(15) 0.0623(11) Uani 1 1 d . . . H31O H 0.5290 0.5637 0.2447 0.075 Uiso 1 1 calc R . . H31P H 0.4408 0.5405 0.2578 0.075 Uiso 1 1 calc R . . C318 C 0.4539(2) 0.62939(18) 0.27836(15) 0.0621(11) Uani 1 1 d . . . H31Q H 0.4819 0.6404 0.3155 0.075 Uiso 1 1 calc R . . H31R H 0.4810 0.6558 0.2638 0.075 Uiso 1 1 calc R . . C401 C 0.1627(2) 0.13016(18) 0.88819(17) 0.0603(11) Uani 1 1 d . . . H40A H 0.1099 0.1039 0.8699 0.072 Uiso 1 1 calc R . . H40B H 0.1808 0.1489 0.8644 0.072 Uiso 1 1 calc R . . C402 C 0.1441(2) 0.17668(19) 0.94018(19) 0.0673(12) Uani 1 1 d . . . H40C H 0.0973 0.1972 0.9330 0.081 Uiso 1 1 calc R . . H40D H 0.1265 0.1587 0.9647 0.081 Uiso 1 1 calc R . . C403 C 0.2030(2) 0.26085(19) 1.01634(16) 0.0623(11) Uani 1 1 d . . . H40E H 0.1923 0.2423 1.0415 0.075 Uiso 1 1 calc R . . H40F H 0.1527 0.2799 1.0118 0.075 Uiso 1 1 calc R . . C404 C 0.2778(3) 0.30484(16) 1.03864(16) 0.0590(11) Uani 1 1 d . . . H40G H 0.2930 0.3194 1.0113 0.071 Uiso 1 1 calc R . . H40H H 0.2648 0.3385 1.0709 0.071 Uiso 1 1 calc R . . C405 C 0.4185(2) 0.32176(14) 1.07880(15) 0.0551(10) Uani 1 1 d . . . H40I H 0.4039 0.3528 1.1124 0.066 Uiso 1 1 calc R . . H40J H 0.4346 0.3402 1.0544 0.066 Uiso 1 1 calc R . . C406 C 0.4913(2) 0.29328(14) 1.09198(13) 0.0468(9) Uani 1 1 d . . . H40K H 0.5384 0.3241 1.1127 0.056 Uiso 1 1 calc R . . H40L H 0.4736 0.2742 1.1156 0.056 Uiso 1 1 calc R . . C407 C 0.2551(2) 0.05981(15) 0.84180(13) 0.0494(9) Uani 1 1 d . . . H40M H 0.2045 0.0405 0.8152 0.059 Uiso 1 1 calc R . . H40N H 0.2866 0.0287 0.8451 0.059 Uiso 1 1 calc R . . C408 C 0.3100(2) 0.09503(16) 0.82056(13) 0.0507(9) Uani 1 1 d . . . H40O H 0.3233 0.0695 0.7840 0.061 Uiso 1 1 calc R . . H40P H 0.2793 0.1266 0.8175 0.061 Uiso 1 1 calc R . . C409 C 0.4353(2) 0.15789(14) 0.83876(12) 0.0407(8) Uani 1 1 d . . . H40Q H 0.4045 0.1916 0.8417 0.049 Uiso 1 1 calc R . . H40R H 0.4442 0.1363 0.8004 0.049 Uiso 1 1 calc R . . C410 C 0.51846(19) 0.17933(14) 0.87281(12) 0.0392(8) Uani 1 1 d . . . H41A H 0.5482 0.1456 0.8713 0.047 Uiso 1 1 calc R . . H41B H 0.5539 0.2029 0.8589 0.047 Uiso 1 1 calc R . . C411 C 0.58436(18) 0.23934(14) 0.96030(12) 0.0370(7) Uani 1 1 d . . . H41C H 0.6180 0.2617 0.9443 0.044 Uiso 1 1 calc R . . H41D H 0.6168 0.2079 0.9618 0.044 Uiso 1 1 calc R . . C412 C 0.56895(19) 0.27932(13) 1.01636(12) 0.0372(7) Uani 1 1 d . . . H41E H 0.6240 0.2982 1.0381 0.045 Uiso 1 1 calc R . . H41F H 0.5367 0.3106 1.0142 0.045 Uiso 1 1 calc R . . C413 C 0.19423(19) 0.05600(15) 0.91878(14) 0.0439(8) Uani 1 1 d . . . H41G H 0.1503 0.0262 0.8922 0.053 Uiso 1 1 calc R . . H41H H 0.1667 0.0795 0.9508 0.053 Uiso 1 1 calc R . . C414 C 0.26008(19) 0.02526(13) 0.93588(13) 0.0389(8) Uani 1 1 d . . . H41I H 0.2328 -0.0025 0.9489 0.047 Uiso 1 1 calc R . . H41J H 0.2897 0.0027 0.9046 0.047 Uiso 1 1 calc R . . C415 C 0.38491(18) 0.03910(12) 0.99198(12) 0.0335(7) Uani 1 1 d . . . H41K H 0.4190 0.0231 0.9614 0.040 Uiso 1 1 calc R . . H41L H 0.3602 0.0061 0.9994 0.040 Uiso 1 1 calc R . . C416 C 0.43977(18) 0.08205(13) 1.04097(12) 0.0350(7) Uani 1 1 d . . . H41M H 0.4055 0.0981 1.0714 0.042 Uiso 1 1 calc R . . H41N H 0.4843 0.0621 1.0516 0.042 Uiso 1 1 calc R . . C417 C 0.53087(19) 0.16968(14) 1.07610(13) 0.0390(8) Uani 1 1 d . . . H41O H 0.5716 0.1492 1.0893 0.047 Uiso 1 1 calc R . . H41P H 0.4963 0.1896 1.1055 0.047 Uiso 1 1 calc R . . C418 C 0.57795(18) 0.21422(13) 1.06121(13) 0.0368(7) Uani 1 1 d . . . H41Q H 0.6182 0.2407 1.0927 0.044 Uiso 1 1 calc R . . H41R H 0.6112 0.1936 1.0312 0.044 Uiso 1 1 calc R . . C501 C 0.5332(3) 0.4309(2) 0.2972(2) 0.0827(15) Uani 1 1 d . . . H50A H 0.5493 0.4738 0.3122 0.099 Uiso 1 1 calc R . . H50B H 0.4712 0.4236 0.2873 0.099 Uiso 1 1 calc R . . C502 C 0.5749(3) 0.4026(2) 0.24661(19) 0.0796(14) Uani 1 1 d . . . H50C H 0.5609 0.3596 0.2317 0.096 Uiso 1 1 calc R . . H50D H 0.5533 0.4162 0.2191 0.096 Uiso 1 1 calc R . . C503 C 0.7058(3) 0.38670(19) 0.21274(17) 0.0726(12) Uani 1 1 d . . . H50E H 0.6793 0.3908 0.1805 0.087 Uiso 1 1 calc R . . H50F H 0.7009 0.3445 0.2051 0.087 Uiso 1 1 calc R . . C504 C 0.7960(3) 0.41036(18) 0.22333(15) 0.0649(11) Uani 1 1 d . . . H50G H 0.8253 0.3885 0.1916 0.078 Uiso 1 1 calc R . . H50H H 0.8012 0.4521 0.2292 0.078 Uiso 1 1 calc R . . C505 C 0.9235(3) 0.41723(19) 0.27725(16) 0.0665(11) Uani 1 1 d . . . H50I H 0.9400 0.4599 0.2904 0.080 Uiso 1 1 calc R . . H50J H 0.9464 0.3972 0.2424 0.080 Uiso 1 1 calc R . . C506 C 0.9590(2) 0.39571(19) 0.31822(16) 0.0679(11) Uani 1 1 d . . . H50K H 0.9453 0.3526 0.3032 0.082 Uiso 1 1 calc R . . H50L H 1.0213 0.4044 0.3235 0.082 Uiso 1 1 calc R . . C507 C 0.5157(2) 0.35052(17) 0.32393(17) 0.0649(11) Uani 1 1 d . . . H50M H 0.5212 0.3277 0.2852 0.078 Uiso 1 1 calc R . . H50N H 0.4546 0.3511 0.3278 0.078 Uiso 1 1 calc R . . C508 C 0.5530(2) 0.31993(17) 0.35571(16) 0.0617(11) Uani 1 1 d . . . H50O H 0.5488 0.3425 0.3947 0.074 Uiso 1 1 calc R . . H50P H 0.5215 0.2806 0.3442 0.074 Uiso 1 1 calc R . . C509 C 0.6744(3) 0.28080(17) 0.37201(16) 0.0623(11) Uani 1 1 d . . . H50Q H 0.6424 0.2412 0.3573 0.075 Uiso 1 1 calc R . . H50R H 0.6711 0.2995 0.4115 0.075 Uiso 1 1 calc R . . C510 C 0.7651(3) 0.27572(16) 0.36178(15) 0.0615(11) Uani 1 1 d . . . H51A H 0.7889 0.2498 0.3772 0.074 Uiso 1 1 calc R . . H51B H 0.7687 0.2582 0.3223 0.074 Uiso 1 1 calc R . . C511 C 0.8992(3) 0.32736(19) 0.38121(16) 0.0675(12) Uani 1 1 d . . . H51C H 0.9075 0.3054 0.3428 0.081 Uiso 1 1 calc R . . H51D H 0.9209 0.3058 0.4020 0.081 Uiso 1 1 calc R . . C512 C 0.9472(3) 0.3878(2) 0.40270(17) 0.0698(12) Uani 1 1 d . . . H51E H 0.9354 0.4099 0.4404 0.084 Uiso 1 1 calc R . . H51F H 1.0085 0.3839 0.4037 0.084 Uiso 1 1 calc R . . C513 C 0.5255(3) 0.44808(19) 0.3923(2) 0.0880(16) Uani 1 1 d . . . H51G H 0.5324 0.4288 0.4175 0.106 Uiso 1 1 calc R . . H51H H 0.4646 0.4515 0.3863 0.106 Uiso 1 1 calc R . . C514 C 0.5737(3) 0.50912(19) 0.4184(2) 0.0904(16) Uani 1 1 d . . . H51I H 0.5669 0.5290 0.3937 0.108 Uiso 1 1 calc R . . H51J H 0.5510 0.5326 0.4525 0.108 Uiso 1 1 calc R . . C515 C 0.7069(3) 0.56148(15) 0.45441(18) 0.0684(12) Uani 1 1 d . . . H51K H 0.6784 0.5870 0.4850 0.082 Uiso 1 1 calc R . . H51L H 0.7091 0.5793 0.4279 0.082 Uiso 1 1 calc R . . C516 C 0.7936(3) 0.55715(16) 0.47436(16) 0.0665(11) Uani 1 1 d . . . H51M H 0.8256 0.5967 0.4914 0.080 Uiso 1 1 calc R . . H51N H 0.7913 0.5413 0.5022 0.080 Uiso 1 1 calc R . . C517 C 0.9198(2) 0.51810(18) 0.44882(16) 0.0694(12) Uani 1 1 d . . . H51O H 0.9213 0.5001 0.4752 0.083 Uiso 1 1 calc R . . H51P H 0.9495 0.5583 0.4671 0.083 Uiso 1 1 calc R . . C518 C 0.9638(2) 0.48271(18) 0.40109(17) 0.0718(12) Uani 1 1 d . . . H51Q H 0.9630 0.5019 0.3757 0.086 Uiso 1 1 calc R . . H51R H 1.0237 0.4834 0.4141 0.086 Uiso 1 1 calc R . . C601 C 1.0675(3) 0.2835(2) 0.4981(2) 0.0933(13) Uani 1 1 d D . . H60A H 1.0336 0.3126 0.4929 0.112 Uiso 1 1 calc R A . H60B H 1.1223 0.3045 0.5190 0.112 Uiso 1 1 calc R . . C602 C 1.0826(3) 0.2410(2) 0.4461(2) 0.0933(13) Uani 1 1 d DU A . H60C H 1.1135 0.2103 0.4508 0.112 Uiso 1 1 calc R . . H60D H 1.1179 0.2603 0.4283 0.112 Uiso 1 1 calc R . . C605 C 0.8185(2) 0.08285(15) 0.31655(13) 0.0492(9) Uani 1 1 d D A . H60I H 0.8303 0.0566 0.2799 0.059 Uiso 1 1 calc R . . H60J H 0.7898 0.1153 0.3138 0.059 Uiso 1 1 calc R . . C606 C 0.7623(3) 0.04934(16) 0.33874(13) 0.0631(11) Uani 1 1 d . . . H60K H 0.7115 0.0300 0.3123 0.076 Uiso 1 1 calc R A . H60L H 0.7928 0.0183 0.3430 0.076 Uiso 1 1 calc R . . C607 C 0.9943(3) 0.3051(2) 0.5739(2) 0.0875(15) Uani 1 1 d . . . H60M H 1.0406 0.3376 0.5905 0.105 Uiso 1 1 calc R A . H60N H 0.9806 0.2909 0.6018 0.105 Uiso 1 1 calc R . . C608 C 0.9186(3) 0.32778(16) 0.55728(18) 0.0759(13) Uani 1 1 d . A . H60O H 0.9055 0.3627 0.5883 0.091 Uiso 1 1 calc R . . H60P H 0.9302 0.3395 0.5276 0.091 Uiso 1 1 calc R . . C609 C 0.7757(3) 0.30415(17) 0.52272(15) 0.0632(12) Uani 1 1 d . A . H60Q H 0.7872 0.3153 0.4927 0.076 Uiso 1 1 calc R . . H60R H 0.7617 0.3393 0.5531 0.076 Uiso 1 1 calc R . . C610 C 0.7036(2) 0.25778(19) 0.50463(15) 0.0594(11) Uani 1 1 d . A . H61A H 0.6953 0.2439 0.5334 0.071 Uiso 1 1 calc R . . H61B H 0.6513 0.2735 0.4972 0.071 Uiso 1 1 calc R . . C611 C 0.6481(2) 0.16807(19) 0.43391(17) 0.0606(11) Uani 1 1 d . A . H61C H 0.5999 0.1867 0.4254 0.073 Uiso 1 1 calc R . . H61D H 0.6323 0.1523 0.4604 0.073 Uiso 1 1 calc R . . C612 C 0.6674(2) 0.11917(18) 0.38319(16) 0.0618(11) Uani 1 1 d . . . H61E H 0.6155 0.0914 0.3665 0.074 Uiso 1 1 calc R A . H61F H 0.6829 0.1358 0.3573 0.074 Uiso 1 1 calc R . . C613 C 1.0818(2) 0.22602(15) 0.55044(15) 0.0468(5) Uani 1 1 d U . . H61G H 1.1155 0.2034 0.5215 0.056 Uiso 1 1 calc R A . H61H H 1.1216 0.2552 0.5807 0.056 Uiso 1 1 calc R . . C614 C 1.0372(2) 0.1853(2) 0.56990(19) 0.0736(13) Uani 1 1 d . A . H61I H 1.0792 0.1692 0.5871 0.088 Uiso 1 1 calc R . . H61J H 1.0009 0.2071 0.5975 0.088 Uiso 1 1 calc R . . C615 C 0.9570(2) 0.09403(16) 0.54224(15) 0.0507(10) Uani 1 1 d . A . H61K H 0.9246 0.1107 0.5736 0.061 Uiso 1 1 calc R . . H61L H 1.0055 0.0774 0.5533 0.061 Uiso 1 1 calc R . . C616 C 0.9017(2) 0.04682(15) 0.49596(14) 0.0482(9) Uani 1 1 d . A . H61M H 0.9347 0.0291 0.4651 0.058 Uiso 1 1 calc R . . H61N H 0.8808 0.0157 0.5070 0.058 Uiso 1 1 calc R . . C617 C 0.7761(2) 0.02461(14) 0.43886(13) 0.0527(10) Uani 1 1 d . A . H61O H 0.7522 -0.0026 0.4536 0.063 Uiso 1 1 calc R . . H61P H 0.8071 0.0022 0.4083 0.063 Uiso 1 1 calc R . . C618 C 0.7062(2) 0.05014(15) 0.41919(14) 0.0544(10) Uani 1 1 d . . . H61Q H 0.6639 0.0179 0.3940 0.065 Uiso 1 1 calc R A . H61R H 0.6778 0.0744 0.4504 0.065 Uiso 1 1 calc R . . C603 C 1.0292(3) 0.1723(2) 0.3658(2) 0.0377(13) Uani 0.594(7) 1 d PD A 1 H60E H 1.0557 0.1418 0.3738 0.045 Uiso 0.594(7) 1 calc PR A 1 H60F H 1.0694 0.1904 0.3495 0.045 Uiso 0.594(7) 1 calc PR A 1 C604 C 0.9453(3) 0.1472(3) 0.3291(2) 0.0377(13) Uani 0.594(7) 1 d PDU A 1 H60G H 0.9557 0.1244 0.2912 0.045 Uiso 0.594(7) 1 calc PR A 1 H60H H 0.9119 0.1793 0.3302 0.045 Uiso 0.594(7) 1 calc PR A 1 C3A C 0.9711(9) 0.1801(4) 0.3462(4) 0.0788(9) Uani 0.406(7) 1 d PDU A 2 H3A1 H 0.9158 0.1918 0.3379 0.095 Uiso 0.406(7) 1 calc PR A 2 H3A2 H 1.0125 0.1916 0.3259 0.095 Uiso 0.406(7) 1 calc PR A 2 C4A C 0.9639(5) 0.1181(4) 0.3296(3) 0.0572(7) Uani 0.406(7) 1 d PDU A 2 H4A1 H 0.9551 0.0974 0.2896 0.069 Uiso 0.406(7) 1 calc PR A 2 H4A2 H 1.0154 0.1063 0.3432 0.069 Uiso 0.406(7) 1 calc PR A 2 N1R N 0.1476(3) 0.3299(3) 0.3495(2) 0.1227(17) Uani 1 1 d . . . C1R C 0.1199(3) 0.2831(2) 0.3054(2) 0.0821(14) Uani 1 1 d . . . H1R H 0.0663 0.2821 0.2871 0.099 Uiso 1 1 calc R . . C2R C 0.1613(4) 0.2376(2) 0.2850(2) 0.0953(17) Uani 1 1 d . . . H2R H 0.1386 0.2057 0.2521 0.114 Uiso 1 1 calc R . . C3R C 0.2363(5) 0.2354(3) 0.3104(4) 0.137(4) Uani 1 1 d . . . H3R H 0.2658 0.2019 0.2967 0.165 Uiso 1 1 calc R . . C4R C 0.2679(4) 0.2832(6) 0.3564(5) 0.168(5) Uani 1 1 d . . . H4R H 0.3206 0.2838 0.3754 0.202 Uiso 1 1 calc R . . C5R C 0.2237(6) 0.3296(4) 0.3746(2) 0.150(3) Uani 1 1 d . . . H5R H 0.2468 0.3632 0.4062 0.180 Uiso 1 1 calc R . . N1S N 0.4356(2) 0.35945(14) 0.95841(12) 0.0558(8) Uani 1 1 d . . . C1S C 0.3829(3) 0.32800(18) 0.91418(16) 0.0639(11) Uani 1 1 d . . . H1S H 0.3278 0.3151 0.9189 0.077 Uiso 1 1 calc R . . C2S C 0.4013(3) 0.31281(17) 0.86282(16) 0.0606(11) Uani 1 1 d . . . H2S H 0.3603 0.2904 0.8329 0.073 Uiso 1 1 calc R . . C3S C 0.4787(3) 0.33003(19) 0.85504(18) 0.0695(12) Uani 1 1 d . . . H3S H 0.4933 0.3203 0.8194 0.083 Uiso 1 1 calc R . . C4S C 0.5371(3) 0.36234(19) 0.8998(2) 0.0739(13) Uani 1 1 d . . . H4S H 0.5929 0.3742 0.8955 0.089 Uiso 1 1 calc R . . C5S C 0.5121(3) 0.37699(15) 0.95154(17) 0.0563(10) Uani 1 1 d . . . H5S H 0.5510 0.4001 0.9824 0.068 Uiso 1 1 calc R . . N1T N 0.1069(3) 0.42532(17) 0.69117(16) 0.0911(12) Uani 1 1 d . . . C1T C 0.1165(4) 0.3827(2) 0.7074(2) 0.1002(17) Uani 1 1 d . . . H1T H 0.0694 0.3668 0.7183 0.120 Uiso 1 1 calc R . . C2T C 0.1926(4) 0.3610(3) 0.7088(3) 0.116(2) Uani 1 1 d . . . H2T H 0.1962 0.3293 0.7191 0.139 Uiso 1 1 calc R . . C3T C 0.2621(4) 0.3838(2) 0.6960(2) 0.1045(19) Uani 1 1 d . . . H3T H 0.3151 0.3698 0.6989 0.125 Uiso 1 1 calc R . . C4T C 0.2551(4) 0.4259(2) 0.6791(2) 0.0987(17) Uani 1 1 d . . . H4T H 0.3025 0.4424 0.6689 0.118 Uiso 1 1 calc R . . C5T C 0.1765(4) 0.4453(2) 0.6768(2) 0.1005(17) Uani 1 1 d . . . H5T H 0.1718 0.4751 0.6639 0.121 Uiso 1 1 calc R . . N1U N 0.2978(4) 0.4027(5) 0.2501(3) 0.172(3) Uani 1 1 d . . . C1U C 0.2346(6) 0.3576(4) 0.2396(3) 0.132(3) Uani 1 1 d . . . H1U H 0.2352 0.3351 0.2604 0.158 Uiso 1 1 calc R . . C2U C 0.1734(4) 0.3463(2) 0.1999(3) 0.1026(19) Uani 1 1 d . . . H2U H 0.1271 0.3175 0.1938 0.123 Uiso 1 1 calc R . . C3U C 0.1770(3) 0.3752(3) 0.16908(19) 0.0889(16) Uani 1 1 d . . . H3U H 0.1348 0.3664 0.1395 0.107 Uiso 1 1 calc R . . C4U C 0.2411(4) 0.4172(3) 0.1801(3) 0.0938(16) Uani 1 1 d . . . H4U H 0.2433 0.4391 0.1586 0.113 Uiso 1 1 calc R . . C5U C 0.3013(4) 0.4289(3) 0.2203(3) 0.113(2) Uani 1 1 d . . . H5U H 0.3477 0.4576 0.2263 0.135 Uiso 1 1 calc R . . N1V N 0.6435(2) 0.47186(15) 0.07209(15) 0.0727(10) Uani 1 1 d . . . C1V C 0.6531(2) 0.52950(18) 0.09905(17) 0.0632(11) Uani 1 1 d . . . H1V H 0.6105 0.5510 0.0924 0.076 Uiso 1 1 calc R . . C2V C 0.7202(3) 0.55912(18) 0.1354(2) 0.1007(18) Uani 1 1 d . . . H2V H 0.7237 0.6004 0.1550 0.121 Uiso 1 1 calc R . . C3V C 0.7843(3) 0.5283(2) 0.1439(2) 0.107(2) Uani 1 1 d . . . H3V H 0.8330 0.5482 0.1688 0.128 Uiso 1 1 calc R . . C4V C 0.7760(3) 0.46894(17) 0.11574(17) 0.0628(11) Uani 1 1 d . . . H4V H 0.8189 0.4464 0.1200 0.075 Uiso 1 1 calc R . . C5V C 0.7052(3) 0.44341(16) 0.08177(16) 0.0580(10) Uani 1 1 d . . . H5V H 0.6986 0.4019 0.0632 0.070 Uiso 1 1 calc R . . N1W N 0.0935(3) 0.33170(16) 0.80645(14) 0.0756(10) Uani 1 1 d . . . C1W C 0.1481(3) 0.29462(18) 0.80780(18) 0.0699(13) Uani 1 1 d . . . H1W H 0.1766 0.2766 0.7768 0.084 Uiso 1 1 calc R . . C2W C 0.1658(3) 0.28089(18) 0.8512(2) 0.0758(13) Uani 1 1 d . . . H2W H 0.2050 0.2539 0.8502 0.091 Uiso 1 1 calc R . . C3W C 0.1251(3) 0.3074(2) 0.89645(18) 0.0688(12) Uani 1 1 d . . . H3W H 0.1357 0.2997 0.9277 0.083 Uiso 1 1 calc R . . C4W C 0.0693(3) 0.34488(19) 0.89465(16) 0.0642(11) Uani 1 1 d . . . H4W H 0.0400 0.3637 0.9251 0.077 Uiso 1 1 calc R . . C5W C 0.0549(3) 0.35568(18) 0.85014(17) 0.0661(11) Uani 1 1 d . . . H5W H 0.0149 0.3819 0.8503 0.079 Uiso 1 1 calc R . . N1Q N 0.8161(3) 0.4757(2) 0.5561(2) 0.1068(15) Uani 1 1 d . . . C1Q C 0.7893(4) 0.5004(3) 0.6049(3) 0.1080(19) Uani 1 1 d . . . H1Q H 0.8272 0.5286 0.6340 0.130 Uiso 1 1 calc R . . C2Q C 0.7099(4) 0.4866(2) 0.6147(3) 0.1077(18) Uani 1 1 d . . . H2Q H 0.6938 0.5033 0.6503 0.129 Uiso 1 1 calc R . . C3Q C 0.6543(3) 0.4487(2) 0.5727(3) 0.0882(16) Uani 1 1 d . . . H3Q H 0.5983 0.4388 0.5782 0.106 Uiso 1 1 calc R . . C4Q C 0.6797(3) 0.42578(19) 0.5238(2) 0.0764(13) Uani 1 1 d . . . H4Q H 0.6415 0.3994 0.4938 0.092 Uiso 1 1 calc R . . C5Q C 0.7596(3) 0.4397(2) 0.5163(2) 0.0865(14) Uani 1 1 d . . . H5Q H 0.7759 0.4229 0.4808 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.03096(12) 0.03463(12) 0.03140(12) 0.01822(10) 0.00629(9) 0.00299(9) P11 0.0325(4) 0.0286(4) 0.0307(4) 0.0108(3) 0.0031(3) -0.0007(3) P12 0.0249(4) 0.0405(5) 0.0360(5) 0.0210(4) 0.0019(3) 0.0038(3) P13 0.0265(4) 0.0311(4) 0.0378(5) 0.0177(4) 0.0089(3) 0.0078(3) P14 0.0328(4) 0.0359(5) 0.0412(5) 0.0218(4) 0.0089(4) 0.0003(4) P15 0.0293(4) 0.0279(4) 0.0404(5) 0.0123(4) 0.0067(4) 0.0057(3) P16 0.0248(4) 0.0335(4) 0.0351(5) 0.0121(4) -0.0011(3) 0.0003(3) P17 0.0342(5) 0.0406(5) 0.0285(4) 0.0132(4) 0.0069(4) 0.0063(4) P21 0.0237(4) 0.0469(5) 0.0304(4) 0.0200(4) 0.0046(3) 0.0097(4) P22 0.0352(5) 0.0361(5) 0.0282(4) 0.0115(4) 0.0013(3) 0.0037(4) P23 0.0278(4) 0.0347(4) 0.0274(4) 0.0152(4) -0.0012(3) 0.0007(3) P24 0.0281(4) 0.0633(6) 0.0425(5) 0.0351(5) 0.0094(4) 0.0072(4) P25 0.0220(4) 0.0402(5) 0.0373(5) 0.0162(4) -0.0016(3) 0.0003(3) P26 0.0273(4) 0.0344(4) 0.0324(4) 0.0151(4) 0.0054(3) 0.0048(3) P27 0.0281(4) 0.0451(5) 0.0361(5) 0.0255(4) 0.0016(3) 0.0048(4) In2 0.03551(13) 0.03472(13) 0.03680(13) 0.01905(10) 0.00695(10) 0.00043(10) P31 0.0342(4) 0.0289(4) 0.0325(5) 0.0112(4) 0.0026(4) -0.0018(3) P32 0.0273(4) 0.0410(5) 0.0459(5) 0.0246(4) 0.0019(4) 0.0027(4) P33 0.0293(4) 0.0316(4) 0.0415(5) 0.0168(4) 0.0088(4) 0.0070(3) P34 0.0327(4) 0.0311(4) 0.0379(5) 0.0154(4) 0.0041(4) -0.0029(3) P35 0.0310(4) 0.0274(4) 0.0476(5) 0.0115(4) 0.0075(4) 0.0026(3) P36 0.0262(4) 0.0336(4) 0.0385(5) 0.0125(4) -0.0013(4) -0.0024(3) P37 0.0347(5) 0.0348(5) 0.0322(5) 0.0108(4) 0.0055(4) 0.0008(4) P41 0.0295(4) 0.0485(5) 0.0348(5) 0.0228(4) 0.0084(4) 0.0092(4) P42 0.0464(5) 0.0420(5) 0.0306(5) 0.0113(4) 0.0035(4) 0.0013(4) P43 0.0261(4) 0.0355(4) 0.0303(4) 0.0164(4) 0.0002(3) 0.0006(3) P44 0.0327(5) 0.0645(6) 0.0486(6) 0.0395(5) 0.0117(4) 0.0089(4) P45 0.0269(4) 0.0549(6) 0.0374(5) 0.0203(4) -0.0027(4) -0.0015(4) P46 0.0266(4) 0.0372(5) 0.0355(5) 0.0169(4) 0.0051(3) 0.0044(3) P47 0.0321(5) 0.0539(5) 0.0441(5) 0.0327(4) 0.0053(4) 0.0095(4) K1 0.0266(3) 0.0319(3) 0.0261(3) 0.0131(3) 0.0065(3) 0.0055(3) K2 0.0282(3) 0.0313(3) 0.0241(3) 0.0112(3) 0.0045(3) 0.0067(3) K3 0.0343(4) 0.0322(4) 0.0341(4) 0.0086(3) 0.0005(3) 0.0006(3) K4 0.0233(3) 0.0301(3) 0.0289(3) 0.0149(3) 0.0033(3) 0.0048(3) K5 0.0442(4) 0.0377(4) 0.0442(4) 0.0174(3) -0.0061(3) 0.0021(3) K6 0.0261(3) 0.0330(3) 0.0303(4) 0.0167(3) 0.0062(3) 0.0070(3) N11 0.0323(12) 0.0534(14) 0.0592(15) 0.0313(12) -0.0073(10) -0.0029(10) N12 0.0252(14) 0.0582(18) 0.0371(16) 0.0192(14) 0.0061(12) 0.0099(13) N21 0.0285(14) 0.0430(15) 0.0342(15) 0.0183(12) 0.0025(11) 0.0085(12) N22 0.0415(16) 0.0357(15) 0.0368(16) 0.0109(13) -0.0101(12) 0.0037(13) N31 0.0439(17) 0.0395(16) 0.0377(16) 0.0109(13) -0.0031(13) -0.0001(13) N32 0.0411(17) 0.069(2) 0.0331(16) 0.0090(15) 0.0009(13) 0.0084(15) N41 0.0301(14) 0.0511(17) 0.0412(17) 0.0276(14) -0.0071(12) -0.0036(12) N42 0.0328(14) 0.0319(14) 0.0283(14) 0.0114(11) -0.0002(11) -0.0008(11) N51 0.0453(18) 0.0505(19) 0.073(2) 0.0170(17) -0.0080(16) 0.0058(15) N52 0.0447(18) 0.064(2) 0.0456(19) 0.0163(16) 0.0010(14) 0.0074(15) N61 0.0353(17) 0.072(2) 0.091(3) 0.053(2) -0.0191(17) -0.0132(16) N62 0.0578(18) 0.0440(16) 0.0309(16) 0.0204(13) -0.0062(13) -0.0131(14) O11 0.0296(11) 0.0348(11) 0.0254(11) 0.0072(9) 0.0060(9) 0.0042(9) O12 0.0292(11) 0.0316(11) 0.0323(12) 0.0087(9) 0.0031(9) 0.0019(9) O13 0.0391(12) 0.0426(12) 0.0293(12) 0.0195(10) 0.0110(10) 0.0031(10) O14 0.0309(12) 0.0442(13) 0.0365(13) 0.0164(10) 0.0127(9) 0.0114(10) O15 0.0416(12) 0.0286(11) 0.0383(13) 0.0151(10) 0.0071(10) 0.0061(10) O16 0.0402(13) 0.0566(14) 0.0463(14) 0.0345(12) 0.0106(11) 0.0145(11) O21 0.0374(12) 0.0407(12) 0.0385(13) 0.0172(10) 0.0181(10) 0.0145(10) O22 0.0625(15) 0.0422(13) 0.0275(12) 0.0157(10) 0.0086(11) 0.0059(11) O23 0.0357(12) 0.0416(12) 0.0315(12) 0.0206(10) 0.0049(9) 0.0087(10) O24 0.0354(12) 0.0327(12) 0.0441(13) 0.0159(10) -0.0036(10) 0.0027(10) O25 0.0352(12) 0.0291(11) 0.0306(12) 0.0099(9) 0.0061(9) 0.0078(9) O26 0.0285(11) 0.0358(12) 0.0380(13) 0.0149(10) 0.0061(9) 0.0062(9) O31 0.0427(14) 0.0475(14) 0.0481(15) 0.0082(12) 0.0027(11) -0.0103(11) O32 0.0506(16) 0.0695(17) 0.0406(15) 0.0132(13) 0.0114(12) 0.0024(13) O33 0.0556(15) 0.0362(13) 0.0532(15) 0.0202(11) -0.0058(12) 0.0032(11) O34 0.0615(16) 0.0346(13) 0.0525(16) 0.0081(12) -0.0062(13) -0.0054(12) O35 0.0456(14) 0.0435(13) 0.0392(14) 0.0124(11) 0.0087(11) 0.0088(11) O36 0.0475(14) 0.0480(14) 0.0381(14) 0.0108(11) 0.0008(11) 0.0168(11) O41 0.0372(14) 0.0687(16) 0.0633(17) 0.0334(14) 0.0135(12) 0.0234(13) O42 0.0507(14) 0.0386(13) 0.0502(15) 0.0172(11) 0.0147(12) 0.0206(12) O43 0.0421(13) 0.0394(12) 0.0284(12) 0.0176(10) 0.0018(10) -0.0034(10) O44 0.0252(11) 0.0395(12) 0.0299(12) 0.0128(9) 0.0067(9) 0.0016(9) O45 0.0297(11) 0.0315(11) 0.0319(12) 0.0148(9) -0.0012(9) 0.0020(9) O46 0.0304(11) 0.0341(11) 0.0329(12) 0.0193(10) -0.0027(9) 0.0002(9) O51 0.0620(17) 0.0537(16) 0.0568(17) 0.0224(13) -0.0191(14) -0.0017(13) O52 0.0594(17) 0.0646(16) 0.0419(15) 0.0214(13) -0.0003(12) 0.0087(13) O53 0.0680(18) 0.0517(15) 0.0498(15) 0.0290(12) 0.0110(13) 0.0065(13) O54 0.0664(17) 0.0509(16) 0.0485(15) 0.0196(12) 0.0079(13) 0.0236(13) O55 0.0538(17) 0.0381(14) 0.091(2) 0.0055(14) -0.0067(14) 0.0105(12) O56 0.0550(16) 0.0462(14) 0.0504(16) 0.0062(12) -0.0036(12) -0.0025(12) O61 0.124(3) 0.0442(15) 0.0767(19) 0.0232(13) 0.0702(19) 0.0108(15) O62 0.0493(15) 0.0899(18) 0.0263(13) 0.0155(12) 0.0045(10) 0.0203(13) O63 0.0634(16) 0.0409(14) 0.0500(15) 0.0159(12) 0.0010(12) 0.0187(13) O64 0.0247(12) 0.0631(15) 0.0493(14) 0.0291(12) 0.0100(10) 0.0151(11) O65 0.0333(13) 0.0711(17) 0.0742(18) 0.0554(15) 0.0023(12) 0.0084(12) O66 0.0503(14) 0.0350(12) 0.0354(13) 0.0194(10) 0.0098(10) 0.0106(11) C101 0.0268(17) 0.0418(19) 0.044(2) 0.0161(16) -0.0066(14) 0.0055(14) C102 0.0246(16) 0.0375(18) 0.043(2) 0.0125(15) 0.0039(14) 0.0083(14) C103 0.0376(18) 0.0315(16) 0.0260(16) 0.0131(13) 0.0117(13) 0.0122(14) C104 0.050(2) 0.0264(16) 0.0248(17) 0.0094(13) 0.0075(14) 0.0044(15) C105 0.0353(19) 0.053(2) 0.0308(19) 0.0001(16) 0.0001(15) -0.0080(16) C106 0.0317(19) 0.074(3) 0.038(2) 0.0162(19) -0.0068(15) 0.0026(18) C107 0.0437(19) 0.0392(18) 0.0224(16) 0.0092(14) -0.0004(14) -0.0012(15) C108 0.053(2) 0.0395(19) 0.0218(17) 0.0121(14) 0.0018(15) 0.0012(16) C109 0.052(2) 0.0436(19) 0.0296(18) 0.0181(15) 0.0177(16) 0.0035(16) C110 0.046(2) 0.0404(19) 0.041(2) 0.0176(16) 0.0263(16) 0.0066(16) C111 0.0276(18) 0.064(2) 0.056(2) 0.0325(19) 0.0170(16) 0.0096(16) C112 0.0208(17) 0.066(2) 0.053(2) 0.0244(19) 0.0026(15) 0.0027(16) C113 0.0331(17) 0.0376(18) 0.0327(18) 0.0125(14) 0.0049(14) -0.0012(14) C114 0.048(2) 0.0319(17) 0.0351(19) 0.0115(15) 0.0061(16) -0.0051(15) C115 0.060(2) 0.0367(19) 0.057(2) 0.0272(18) 0.0203(19) 0.0133(17) C116 0.053(2) 0.051(2) 0.057(2) 0.0363(19) 0.0179(19) 0.0180(18) C117 0.045(2) 0.077(3) 0.047(2) 0.041(2) 0.0063(17) 0.0225(19) C118 0.0303(19) 0.078(3) 0.052(2) 0.036(2) 0.0033(16) 0.0167(18) C201 0.0240(17) 0.058(2) 0.064(2) 0.035(2) 0.0019(16) -0.0003(16) C202 0.035(2) 0.062(2) 0.071(3) 0.042(2) 0.0274(18) 0.0200(17) C203 0.063(2) 0.040(2) 0.047(2) 0.0151(17) 0.0381(19) 0.0094(17) C204 0.086(3) 0.048(2) 0.031(2) 0.0171(17) 0.026(2) 0.004(2) C205 0.085(3) 0.055(2) 0.0264(19) 0.0143(17) -0.0077(19) 0.001(2) C206 0.066(3) 0.048(2) 0.038(2) 0.0087(18) -0.0219(18) -0.0021(19) C207 0.0295(17) 0.055(2) 0.045(2) 0.0278(17) 0.0018(15) 0.0120(16) C208 0.0382(19) 0.056(2) 0.0346(19) 0.0256(17) -0.0012(15) 0.0136(16) C209 0.0435(19) 0.0394(18) 0.0386(19) 0.0237(15) 0.0104(15) 0.0130(15) C210 0.051(2) 0.0331(18) 0.056(2) 0.0225(17) 0.0052(18) 0.0076(16) C211 0.044(2) 0.040(2) 0.055(2) 0.0179(17) -0.0083(17) -0.0053(16) C212 0.0351(19) 0.048(2) 0.057(2) 0.0193(18) -0.0153(17) -0.0027(16) C213 0.042(2) 0.054(2) 0.036(2) 0.0117(17) -0.0101(15) 0.0018(17) C214 0.043(2) 0.0343(18) 0.0300(18) 0.0001(14) -0.0023(15) 0.0016(15) C215 0.051(2) 0.0308(17) 0.0282(17) 0.0124(14) 0.0166(15) 0.0138(15) C216 0.0371(18) 0.0340(17) 0.044(2) 0.0224(15) 0.0189(15) 0.0156(14) C217 0.0297(19) 0.043(2) 0.079(3) 0.016(2) -0.0082(18) 0.0110(16) C218 0.052(2) 0.044(2) 0.065(3) 0.0199(19) -0.0255(19) 0.0085(18) C301 0.047(2) 0.055(2) 0.049(2) 0.0096(19) -0.0105(18) -0.0047(18) C302 0.040(2) 0.049(2) 0.055(2) 0.0047(19) -0.0019(17) -0.0119(17) C303 0.052(2) 0.064(3) 0.060(3) 0.014(2) 0.020(2) -0.008(2) C304 0.052(3) 0.082(3) 0.055(3) 0.013(2) 0.017(2) -0.001(2) C305 0.064(3) 0.103(3) 0.036(2) 0.021(2) 0.0074(19) 0.010(2) C306 0.070(3) 0.110(4) 0.036(2) 0.024(2) 0.000(2) 0.018(3) C307 0.059(2) 0.061(2) 0.038(2) 0.0218(19) -0.0019(17) 0.0050(19) C308 0.063(3) 0.059(3) 0.060(3) 0.033(2) -0.008(2) 0.006(2) C309 0.094(3) 0.035(2) 0.086(3) 0.026(2) -0.009(3) 0.009(2) C310 0.093(3) 0.036(2) 0.084(3) 0.020(2) 0.004(3) 0.000(2) C311 0.052(2) 0.047(2) 0.059(3) -0.006(2) 0.003(2) -0.0022(19) C312 0.047(2) 0.069(3) 0.040(2) -0.014(2) -0.0114(18) 0.012(2) C313 0.062(2) 0.043(2) 0.039(2) 0.0058(17) -0.0036(18) 0.0010(18) C314 0.062(2) 0.043(2) 0.034(2) 0.0051(16) 0.0069(17) 0.0082(18) C315 0.050(2) 0.0386(19) 0.053(2) 0.0170(17) 0.0134(17) 0.0145(16) C316 0.049(2) 0.052(2) 0.051(2) 0.0212(18) 0.0119(18) 0.0180(18) C317 0.049(2) 0.087(3) 0.050(2) 0.026(2) -0.0007(18) 0.023(2) C318 0.042(2) 0.083(3) 0.040(2) 0.005(2) -0.0068(17) 0.013(2) C401 0.038(2) 0.076(3) 0.075(3) 0.044(2) -0.0173(19) 0.0014(19) C402 0.024(2) 0.085(3) 0.112(4) 0.059(3) 0.003(2) 0.017(2) C403 0.053(2) 0.095(3) 0.069(3) 0.053(3) 0.031(2) 0.049(2) C404 0.075(3) 0.054(2) 0.061(3) 0.027(2) 0.029(2) 0.045(2) C405 0.070(3) 0.0323(19) 0.052(2) 0.0024(17) 0.021(2) 0.0131(19) C406 0.054(2) 0.0396(19) 0.0328(19) 0.0029(16) -0.0004(16) -0.0043(17) C407 0.053(2) 0.059(2) 0.034(2) 0.0231(17) -0.0090(16) -0.0184(18) C408 0.059(2) 0.058(2) 0.0318(19) 0.0211(17) -0.0093(17) -0.0138(18) C409 0.054(2) 0.0425(19) 0.0287(18) 0.0183(15) 0.0092(15) 0.0002(16) C410 0.0399(19) 0.048(2) 0.0327(18) 0.0184(16) 0.0165(15) 0.0046(15) C411 0.0225(16) 0.0481(19) 0.045(2) 0.0249(16) 0.0029(14) -0.0038(14) C412 0.0332(18) 0.0334(17) 0.044(2) 0.0174(15) -0.0038(15) -0.0035(14) C413 0.0311(18) 0.057(2) 0.046(2) 0.0276(18) -0.0046(15) -0.0117(16) C414 0.0440(19) 0.0362(18) 0.0361(19) 0.0193(15) -0.0038(15) -0.0142(15) C415 0.0347(17) 0.0281(16) 0.0445(19) 0.0202(15) 0.0098(15) 0.0080(14) C416 0.0338(17) 0.0395(18) 0.0407(19) 0.0263(16) 0.0007(14) 0.0054(14) C417 0.0318(18) 0.048(2) 0.0382(19) 0.0219(16) -0.0092(14) -0.0039(15) C418 0.0305(17) 0.0381(18) 0.0400(19) 0.0175(15) -0.0076(14) -0.0031(14) C501 0.049(3) 0.069(3) 0.132(5) 0.048(3) -0.017(3) 0.008(2) C502 0.072(3) 0.083(3) 0.084(4) 0.046(3) -0.040(3) -0.006(3) C503 0.089(3) 0.073(3) 0.051(3) 0.026(2) -0.017(2) 0.001(3) C504 0.086(3) 0.064(3) 0.042(2) 0.024(2) -0.003(2) 0.003(2) C505 0.066(3) 0.081(3) 0.046(2) 0.021(2) 0.007(2) 0.004(2) C506 0.050(2) 0.087(3) 0.056(3) 0.019(2) 0.005(2) 0.008(2) C507 0.055(2) 0.062(3) 0.065(3) 0.019(2) -0.004(2) -0.012(2) C508 0.067(3) 0.058(2) 0.052(2) 0.020(2) -0.004(2) -0.016(2) C509 0.097(3) 0.047(2) 0.049(2) 0.0264(19) 0.012(2) 0.005(2) C510 0.099(3) 0.046(2) 0.046(2) 0.0223(19) 0.019(2) 0.023(2) C511 0.071(3) 0.087(3) 0.053(3) 0.033(2) 0.004(2) 0.043(3) C512 0.056(3) 0.097(4) 0.060(3) 0.035(3) -0.003(2) 0.024(2) C513 0.048(3) 0.078(3) 0.101(4) 0.000(3) 0.004(2) 0.013(2) C514 0.059(3) 0.063(3) 0.112(4) -0.002(3) -0.005(3) 0.021(2) C515 0.078(3) 0.032(2) 0.084(3) 0.014(2) 0.004(2) 0.005(2) C516 0.075(3) 0.041(2) 0.063(3) 0.003(2) 0.010(2) -0.005(2) C517 0.052(3) 0.073(3) 0.055(3) 0.003(2) -0.009(2) -0.009(2) C518 0.048(2) 0.078(3) 0.066(3) 0.010(2) -0.003(2) -0.010(2) C601 0.0394(17) 0.124(4) 0.163(4) 0.106(3) 0.022(2) 0.001(2) C602 0.0394(17) 0.124(4) 0.163(4) 0.106(3) 0.022(2) 0.001(2) C605 0.070(3) 0.052(2) 0.0256(18) 0.0172(16) 0.0017(17) 0.0031(19) C606 0.104(3) 0.051(2) 0.027(2) 0.0152(17) -0.003(2) -0.021(2) C607 0.090(4) 0.065(3) 0.085(4) 0.025(3) -0.047(3) -0.029(3) C608 0.109(4) 0.036(2) 0.064(3) 0.006(2) -0.007(3) 0.001(2) C609 0.092(3) 0.061(3) 0.045(2) 0.022(2) 0.017(2) 0.050(3) C610 0.053(2) 0.096(3) 0.054(2) 0.045(2) 0.0262(19) 0.051(2) C611 0.0242(19) 0.104(3) 0.081(3) 0.066(3) 0.0043(19) 0.008(2) C612 0.044(2) 0.088(3) 0.061(3) 0.048(2) -0.0214(19) -0.025(2) C613 0.0323(12) 0.0534(14) 0.0592(15) 0.0313(12) -0.0073(10) -0.0029(10) C614 0.032(2) 0.107(4) 0.106(4) 0.078(3) -0.025(2) -0.011(2) C615 0.044(2) 0.072(3) 0.067(3) 0.054(2) 0.0182(19) 0.0295(19) C616 0.063(2) 0.047(2) 0.058(2) 0.0370(19) 0.035(2) 0.0302(19) C617 0.092(3) 0.0322(19) 0.035(2) 0.0170(16) 0.011(2) -0.0090(19) C618 0.075(3) 0.049(2) 0.039(2) 0.0246(18) -0.0061(18) -0.0268(19) C603 0.031(2) 0.058(3) 0.042(2) 0.032(2) 0.0222(18) 0.026(2) C604 0.031(2) 0.058(3) 0.042(2) 0.032(2) 0.0222(18) 0.026(2) C3A 0.124(3) 0.0442(15) 0.0767(19) 0.0232(13) 0.0702(19) 0.0108(15) C4A 0.0493(15) 0.0899(18) 0.0263(13) 0.0155(12) 0.0045(10) 0.0203(13) N1R 0.104(4) 0.146(5) 0.100(4) 0.030(4) 0.012(3) 0.031(3) C1R 0.058(3) 0.095(4) 0.108(4) 0.057(3) -0.001(3) 0.010(3) C2R 0.090(4) 0.063(3) 0.142(5) 0.046(3) 0.046(4) 0.008(3) C3R 0.099(6) 0.094(5) 0.303(12) 0.144(6) 0.116(7) 0.058(4) C4R 0.061(4) 0.278(12) 0.303(14) 0.263(12) 0.006(6) 0.023(6) C5R 0.141(7) 0.225(9) 0.066(4) 0.062(5) -0.036(4) -0.041(6) N1S 0.053(2) 0.069(2) 0.0437(19) 0.0200(16) 0.0059(16) 0.0172(17) C1S 0.054(2) 0.086(3) 0.050(3) 0.025(2) 0.003(2) 0.014(2) C2S 0.073(3) 0.065(3) 0.045(2) 0.022(2) 0.005(2) 0.025(2) C3S 0.097(4) 0.073(3) 0.052(3) 0.031(2) 0.031(3) 0.030(3) C4S 0.061(3) 0.071(3) 0.113(4) 0.056(3) 0.034(3) 0.014(2) C5S 0.061(3) 0.045(2) 0.065(3) 0.026(2) -0.005(2) 0.0067(19) N1T 0.127(4) 0.061(3) 0.080(3) 0.027(2) -0.008(3) 0.005(2) C1T 0.140(5) 0.087(4) 0.099(4) 0.057(3) 0.037(4) 0.037(4) C2T 0.126(5) 0.112(5) 0.175(6) 0.109(5) 0.066(4) 0.065(4) C3T 0.142(5) 0.082(4) 0.127(5) 0.066(4) 0.068(4) 0.058(4) C4T 0.135(5) 0.075(4) 0.092(4) 0.036(3) 0.032(4) 0.023(3) C5T 0.133(5) 0.084(4) 0.103(4) 0.063(3) -0.004(4) -0.002(4) N1U 0.070(4) 0.310(10) 0.100(5) 0.056(5) -0.016(3) -0.016(5) C1U 0.146(7) 0.180(7) 0.127(6) 0.113(6) 0.029(5) 0.057(6) C2U 0.117(5) 0.080(4) 0.090(4) 0.021(3) 0.021(4) -0.035(3) C3U 0.049(3) 0.149(5) 0.062(3) 0.042(3) -0.014(2) -0.001(3) C4U 0.114(5) 0.090(4) 0.105(5) 0.061(4) 0.046(4) 0.030(4) C5U 0.104(5) 0.120(5) 0.078(4) 0.016(4) 0.022(4) -0.067(4) N1V 0.059(2) 0.053(2) 0.088(3) 0.0158(19) -0.0121(19) 0.0001(18) C1V 0.050(2) 0.055(3) 0.081(3) 0.025(2) 0.000(2) 0.009(2) C2V 0.090(4) 0.037(2) 0.151(5) 0.025(3) -0.038(3) -0.002(2) C3V 0.081(3) 0.060(3) 0.151(5) 0.028(3) -0.054(3) -0.006(3) C4V 0.067(3) 0.046(2) 0.076(3) 0.028(2) -0.008(2) 0.007(2) C5V 0.065(3) 0.035(2) 0.067(3) 0.0169(19) 0.001(2) 0.0022(19) N1W 0.099(3) 0.066(2) 0.050(2) 0.0153(19) 0.014(2) -0.012(2) C1W 0.074(3) 0.048(3) 0.059(3) -0.007(2) 0.025(2) -0.010(2) C2W 0.058(3) 0.052(3) 0.100(4) 0.019(3) -0.006(3) -0.015(2) C3W 0.060(3) 0.093(3) 0.060(3) 0.041(3) 0.006(2) -0.005(2) C4W 0.063(3) 0.086(3) 0.045(2) 0.028(2) 0.016(2) 0.002(2) C5W 0.071(3) 0.064(3) 0.059(3) 0.022(2) 0.016(2) 0.000(2) N1Q 0.080(3) 0.120(4) 0.111(4) 0.051(3) -0.019(3) -0.034(3) C1Q 0.093(4) 0.113(5) 0.092(4) 0.030(4) -0.014(3) -0.046(3) C2Q 0.093(4) 0.099(4) 0.116(5) 0.033(4) 0.002(4) -0.004(3) C3Q 0.046(3) 0.068(3) 0.135(5) 0.027(3) 0.007(3) 0.008(2) C4Q 0.054(3) 0.061(3) 0.116(4) 0.043(3) -0.006(3) 0.002(2) C5Q 0.078(4) 0.077(3) 0.111(4) 0.049(3) -0.001(3) -0.004(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 In1 P23 2.5705(8) . ? In1 P12 2.5854(8) . ? In1 P13 2.5922(8) . ? In1 P22 2.6178(8) . ? P11 P14 2.1467(11) . ? P11 P13 2.2149(11) . ? P11 P12 2.2276(11) . ? P12 P15 2.1727(11) . ? P13 P16 2.1834(11) . ? P14 P17 2.1326(12) . ? P15 P17 2.2403(11) . ? P15 P16 2.2686(11) . ? P16 P17 2.2378(11) . ? P21 P24 2.1446(11) . ? P21 P23 2.2085(11) . ? P21 P22 2.2249(11) . ? P22 P25 2.1763(11) . ? P23 P26 2.1770(11) . ? P24 P27 2.1412(11) . ? P25 P27 2.2353(11) . ? P25 P26 2.2685(11) . ? P26 P27 2.2311(11) . ? In2 P43 2.5682(8) . ? In2 P32 2.5767(8) . ? In2 P33 2.5947(8) . ? In2 P42 2.6008(9) . ? P31 P34 2.1423(11) . ? P31 P33 2.2183(11) . ? P31 P32 2.2261(11) . ? P32 P35 2.1712(12) . ? P33 P36 2.1800(11) . ? P34 P37 2.1409(11) . ? P35 P37 2.2356(12) . ? P35 P36 2.2685(11) . ? P36 P37 2.2438(11) . ? P41 P44 2.1475(12) . ? P41 P43 2.2161(11) . ? P41 P42 2.2175(12) . ? P42 P45 2.1858(12) . ? P43 P46 2.1759(11) . ? P44 P47 2.1405(11) . ? P45 P47 2.2306(12) . ? P45 P46 2.2691(12) . ? P46 P47 2.2306(11) . ? K1 O12 2.7871(19) . ? K1 O13 2.797(2) . ? K1 O16 2.838(2) . ? K1 O15 2.860(2) . ? K1 O14 2.891(2) . ? K1 O11 2.9133(19) . ? K1 N12 2.966(3) . ? K1 N11 2.988(3) . ? K2 O25 2.7864(19) . ? K2 O24 2.829(2) . ? K2 O22 2.834(2) . ? K2 O23 2.851(2) . ? K2 O21 2.875(2) . ? K2 O26 2.9014(19) . ? K2 N22 2.961(3) . ? K2 N21 2.966(2) . ? K3 O34 2.811(2) . ? K3 O32 2.816(2) . ? K3 O31 2.820(2) . ? K3 O33 2.839(2) . ? K3 O36 2.850(2) . ? K3 O35 2.870(2) . ? K3 N31 2.965(3) . ? K3 N32 2.967(3) . ? K4 O44 2.7894(19) . ? K4 O42 2.825(2) . ? K4 O41 2.825(2) . ? K4 O43 2.833(2) . ? K4 O45 2.8359(19) . ? K4 O46 2.8402(19) . ? K4 N41 2.963(3) . ? K4 N42 2.989(2) . ? K5 O52 2.762(2) . ? K5 O53 2.825(2) . ? K5 O54 2.825(2) . ? K5 O51 2.836(2) . ? K5 O55 2.846(2) . ? K5 O56 2.859(2) . ? K5 N52 2.954(3) . ? K5 N51 2.973(3) . ? K6 O64 2.782(2) . ? K6 O65 2.788(2) . ? K6 O62 2.813(2) . ? K6 O61 2.847(2) . ? K6 O66 2.848(2) . ? K6 O63 2.861(2) . ? K6 N62 2.955(3) . ? K6 N61 2.971(3) . ? N11 C113 1.475(4) . ? N11 C107 1.477(4) . ? N11 C101 1.480(4) . ? N12 C106 1.470(4) . ? N12 C112 1.474(4) . ? N12 C118 1.481(4) . ? N21 C207 1.470(4) . ? N21 C213 1.472(4) . ? N21 C201 1.473(4) . ? N22 C206 1.469(4) . ? N22 C212 1.471(4) . ? N22 C218 1.482(4) . ? N31 C313 1.468(4) . ? N31 C307 1.469(4) . ? N31 C301 1.475(4) . ? N32 C306 1.460(5) . ? N32 C312 1.472(5) . ? N32 C318 1.498(4) . ? N41 C401 1.462(4) . ? N41 C407 1.466(4) . ? N41 C413 1.472(4) . ? N42 C406 1.465(4) . ? N42 C418 1.471(4) . ? N42 C412 1.473(4) . ? N51 C507 1.463(5) . ? N51 C501 1.470(5) . ? N51 C513 1.486(5) . ? N52 C512 1.460(5) . ? N52 C518 1.462(5) . ? N52 C506 1.474(4) . ? N61 C601 1.444(5) . ? N61 C607 1.456(6) . ? N61 C613 1.492(4) . ? N62 C612 1.466(4) . ? N62 C606 1.473(4) . ? N62 C618 1.477(4) . ? O11 C103 1.418(3) . ? O11 C102 1.431(3) . ? O12 C104 1.425(3) . ? O12 C105 1.430(3) . ? O13 C109 1.423(3) . ? O13 C108 1.435(4) . ? O14 C111 1.428(4) . ? O14 C110 1.435(4) . ? O15 C114 1.418(4) . ? O15 C115 1.423(4) . ? O16 C116 1.419(4) . ? O16 C117 1.429(4) . ? O21 C203 1.419(4) . ? O21 C202 1.428(4) . ? O22 C204 1.428(4) . ? O22 C205 1.429(4) . ? O23 C209 1.423(3) . ? O23 C208 1.425(4) . ? O24 C211 1.426(4) . ? O24 C210 1.428(3) . ? O25 C215 1.430(3) . ? O25 C214 1.437(3) . ? O26 C216 1.424(3) . ? O26 C217 1.432(4) . ? O31 C302 1.418(4) . ? O31 C303 1.419(4) . ? O32 C304 1.417(4) . ? O32 C305 1.421(4) . ? O33 C308 1.421(4) . ? O33 C309 1.430(4) . ? O34 C311 1.409(4) . ? O34 C310 1.432(5) . ? O35 C314 1.418(4) . ? O35 C315 1.419(4) . ? O36 C317 1.419(4) . ? O36 C316 1.419(4) . ? O41 C402 1.427(4) . ? O41 C403 1.427(4) . ? O42 C405 1.412(4) . ? O42 C404 1.439(4) . ? O43 C408 1.430(4) . ? O43 C409 1.431(3) . ? O44 C411 1.423(3) . ? O44 C410 1.427(3) . ? O45 C415 1.419(3) . ? O45 C414 1.427(3) . ? O46 C416 1.421(3) . ? O46 C417 1.425(3) . ? O51 C502 1.404(5) . ? O51 C503 1.415(5) . ? O52 C504 1.419(4) . ? O52 C505 1.423(4) . ? O53 C509 1.408(4) . ? O53 C508 1.409(4) . ? O54 C510 1.407(4) . ? O54 C511 1.419(4) . ? O55 C514 1.415(4) . ? O55 C515 1.425(4) . ? O56 C517 1.406(4) . ? O56 C516 1.414(4) . ? O61 C603 1.394(5) . ? O61 C602 1.464(5) . ? O61 C3A 1.654(11) . ? O62 C4A 1.361(7) . ? O62 C605 1.423(4) . ? O62 C604 1.600(6) . ? O63 C608 1.415(5) . ? O63 C609 1.427(4) . ? O64 C611 1.415(4) . ? O64 C610 1.436(4) . ? O65 C614 1.413(5) . ? O65 C615 1.420(4) . ? O66 C616 1.408(4) . ? O66 C617 1.429(4) . ? C101 C102 1.506(4) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.486(4) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.495(5) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.504(4) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.486(4) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.495(5) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.505(4) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.478(5) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.507(5) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? C201 C202 1.495(5) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.486(5) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.504(5) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.507(4) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.492(4) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.500(4) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.503(4) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.485(4) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.495(5) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? C301 C302 1.497(5) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.501(5) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 C306 1.520(5) . ? C305 H30I 0.9900 . ? C305 H30J 0.9900 . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 C308 1.506(5) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 C310 1.449(6) . ? C309 H30Q 0.9900 . ? C309 H30R 0.9900 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C312 1.466(5) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 H31E 0.9900 . ? C312 H31F 0.9900 . ? C313 C314 1.503(5) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 C316 1.488(5) . ? C315 H31K 0.9900 . ? C315 H31L 0.9900 . ? C316 H31M 0.9900 . ? C316 H31N 0.9900 . ? C317 C318 1.504(5) . ? C317 H31O 0.9900 . ? C317 H31P 0.9900 . ? C318 H31Q 0.9900 . ? C318 H31R 0.9900 . ? C401 C402 1.493(5) . ? C401 H40A 0.9900 . ? C401 H40B 0.9900 . ? C402 H40C 0.9900 . ? C402 H40D 0.9900 . ? C403 C404 1.472(5) . ? C403 H40E 0.9900 . ? C403 H40F 0.9900 . ? C404 H40G 0.9900 . ? C404 H40H 0.9900 . ? C405 C406 1.504(5) . ? C405 H40I 0.9900 . ? C405 H40J 0.9900 . ? C406 H40K 0.9900 . ? C406 H40L 0.9900 . ? C407 C408 1.503(4) . ? C407 H40M 0.9900 . ? C407 H40N 0.9900 . ? C408 H40O 0.9900 . ? C408 H40P 0.9900 . ? C409 C410 1.488(4) . ? C409 H40Q 0.9900 . ? C409 H40R 0.9900 . ? C410 H41A 0.9900 . ? C410 H41B 0.9900 . ? C411 C412 1.499(4) . ? C411 H41C 0.9900 . ? C411 H41D 0.9900 . ? C412 H41E 0.9900 . ? C412 H41F 0.9900 . ? C413 C414 1.502(4) . ? C413 H41G 0.9900 . ? C413 H41H 0.9900 . ? C414 H41I 0.9900 . ? C414 H41J 0.9900 . ? C415 C416 1.492(4) . ? C415 H41K 0.9900 . ? C415 H41L 0.9900 . ? C416 H41M 0.9900 . ? C416 H41N 0.9900 . ? C417 C418 1.507(4) . ? C417 H41O 0.9900 . ? C417 H41P 0.9900 . ? C418 H41Q 0.9900 . ? C418 H41R 0.9900 . ? C501 C502 1.504(6) . ? C501 H50A 0.9900 . ? C501 H50B 0.9900 . ? C502 H50C 0.9900 . ? C502 H50D 0.9900 . ? C503 C504 1.477(5) . ? C503 H50E 0.9900 . ? C503 H50F 0.9900 . ? C504 H50G 0.9900 . ? C504 H50H 0.9900 . ? C505 C506 1.513(5) . ? C505 H50I 0.9900 . ? C505 H50J 0.9900 . ? C506 H50K 0.9900 . ? C506 H50L 0.9900 . ? C507 C508 1.489(5) . ? C507 H50M 0.9900 . ? C507 H50N 0.9900 . ? C508 H50O 0.9900 . ? C508 H50P 0.9900 . ? C509 C510 1.501(5) . ? C509 H50Q 0.9900 . ? C509 H50R 0.9900 . ? C510 H51A 0.9900 . ? C510 H51B 0.9900 . ? C511 C512 1.508(6) . ? C511 H51C 0.9900 . ? C511 H51D 0.9900 . ? C512 H51E 0.9900 . ? C512 H51F 0.9900 . ? C513 C514 1.519(6) . ? C513 H51G 0.9900 . ? C513 H51H 0.9900 . ? C514 H51I 0.9900 . ? C514 H51J 0.9900 . ? C515 C516 1.476(5) . ? C515 H51K 0.9900 . ? C515 H51L 0.9900 . ? C516 H51M 0.9900 . ? C516 H51N 0.9900 . ? C517 C518 1.506(5) . ? C517 H51O 0.9900 . ? C517 H51P 0.9900 . ? C518 H51Q 0.9900 . ? C518 H51R 0.9900 . ? C601 C602 1.439(6) . ? C601 H60A 0.9900 . ? C601 H60B 0.9900 . ? C602 H60C 0.9900 . ? C602 H60D 0.9900 . ? C605 C606 1.503(5) . ? C605 H60I 0.9900 . ? C605 H60J 0.9900 . ? C606 H60K 0.9900 . ? C606 H60L 0.9900 . ? C607 C608 1.491(6) . ? C607 H60M 0.9900 . ? C607 H60N 0.9900 . ? C608 H60O 0.9900 . ? C608 H60P 0.9900 . ? C609 C610 1.475(5) . ? C609 H60Q 0.9900 . ? C609 H60R 0.9900 . ? C610 H61A 0.9900 . ? C610 H61B 0.9900 . ? C611 C612 1.502(5) . ? C611 H61C 0.9900 . ? C611 H61D 0.9900 . ? C612 H61E 0.9900 . ? C612 H61F 0.9900 . ? C613 C614 1.491(5) . ? C613 H61G 0.9900 . ? C613 H61H 0.9900 . ? C614 H61I 0.9900 . ? C614 H61J 0.9900 . ? C615 C616 1.496(5) . ? C615 H61K 0.9900 . ? C615 H61L 0.9900 . ? C616 H61M 0.9900 . ? C616 H61N 0.9900 . ? C617 C618 1.496(5) . ? C617 H61O 0.9900 . ? C617 H61P 0.9900 . ? C618 H61Q 0.9900 . ? C618 H61R 0.9900 . ? C603 C604 1.533(8) . ? C603 H60E 0.9900 . ? C603 H60F 0.9900 . ? C604 H60G 0.9900 . ? C604 H60H 0.9900 . ? C3A C4A 1.429(12) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? N1R C1R 1.310(6) . ? N1R C5R 1.350(8) . ? C1R C2R 1.307(6) . ? C1R H1R 0.9500 . ? C2R C3R 1.352(9) . ? C2R H2R 0.9500 . ? C3R C4R 1.364(12) . ? C3R H3R 0.9500 . ? C4R C5R 1.345(11) . ? C4R H4R 0.9500 . ? C5R H5R 0.9500 . ? N1S C5S 1.320(4) . ? N1S C1S 1.326(5) . ? C1S C2S 1.353(5) . ? C1S H1S 0.9500 . ? C2S C3S 1.339(5) . ? C2S H2S 0.9500 . ? C3S C4S 1.388(6) . ? C3S H3S 0.9500 . ? C4S C5S 1.401(6) . ? C4S H4S 0.9500 . ? C5S H5S 0.9500 . ? N1T C1T 1.326(6) . ? N1T C5T 1.337(6) . ? C1T C2T 1.374(7) . ? C1T H1T 0.9500 . ? C2T C3T 1.345(7) . ? C2T H2T 0.9500 . ? C3T C4T 1.320(6) . ? C3T H3T 0.9500 . ? C4T C5T 1.386(7) . ? C4T H4T 0.9500 . ? C5T H5T 0.9500 . ? N1U C5U 1.235(9) . ? N1U C1U 1.381(9) . ? C1U C2U 1.323(8) . ? C1U H1U 0.9500 . ? C2U C3U 1.314(7) . ? C2U H2U 0.9500 . ? C3U C4U 1.337(7) . ? C3U H3U 0.9500 . ? C4U C5U 1.321(8) . ? C4U H4U 0.9500 . ? C5U H5U 0.9500 . ? N1V C1V 1.322(5) . ? N1V C5V 1.330(5) . ? C1V C2V 1.343(5) . ? C1V H1V 0.9500 . ? C2V C3V 1.389(6) . ? C2V H2V 0.9500 . ? C3V C4V 1.363(5) . ? C3V H3V 0.9500 . ? C4V C5V 1.340(5) . ? C4V H4V 0.9500 . ? C5V H5V 0.9500 . ? N1W C5W 1.320(5) . ? N1W C1W 1.332(5) . ? C1W C2W 1.374(6) . ? C1W H1W 0.9500 . ? C2W C3W 1.380(6) . ? C2W H2W 0.9500 . ? C3W C4W 1.356(5) . ? C3W H3W 0.9500 . ? C4W C5W 1.350(5) . ? C4W H4W 0.9500 . ? C5W H5W 0.9500 . ? N1Q C5Q 1.319(6) . ? N1Q C1Q 1.338(6) . ? C1Q C2Q 1.364(7) . ? C1Q H1Q 0.9500 . ? C2Q C3Q 1.355(7) . ? C2Q H2Q 0.9500 . ? C3Q C4Q 1.329(6) . ? C3Q H3Q 0.9500 . ? C4Q C5Q 1.350(6) . ? C4Q H4Q 0.9500 . ? C5Q H5Q 0.9500 . ? 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 P23 In1 P12 127.25(3) . . ? P23 In1 P13 122.53(3) . . ? P12 In1 P13 80.12(2) . . ? P23 In1 P22 79.53(3) . . ? P12 In1 P22 120.55(3) . . ? P13 In1 P22 134.07(3) . . ? P14 P11 P13 102.80(4) . . ? P14 P11 P12 103.36(4) . . ? P13 P11 P12 97.20(4) . . ? P15 P12 P11 99.45(4) . . ? P15 P12 In1 91.34(3) . . ? P11 P12 In1 82.22(3) . . ? P16 P13 P11 99.49(4) . . ? P16 P13 In1 90.84(3) . . ? P11 P13 In1 82.30(3) . . ? P17 P14 P11 98.23(4) . . ? P12 P15 P17 103.73(4) . . ? P12 P15 P16 104.15(4) . . ? P17 P15 P16 59.51(3) . . ? P13 P16 P17 103.33(4) . . ? P13 P16 P15 104.12(4) . . ? P17 P16 P15 59.62(3) . . ? P14 P17 P16 108.17(4) . . ? P14 P17 P15 108.42(5) . . ? P16 P17 P15 60.87(3) . . ? P24 P21 P23 102.57(5) . . ? P24 P21 P22 103.96(4) . . ? P23 P21 P22 96.94(4) . . ? P25 P22 P21 99.18(4) . . ? P25 P22 In1 88.84(3) . . ? P21 P22 In1 83.35(3) . . ? P26 P23 P21 99.86(4) . . ? P26 P23 In1 88.28(3) . . ? P21 P23 In1 84.79(3) . . ? P27 P24 P21 98.10(4) . . ? P22 P25 P27 104.40(4) . . ? P22 P25 P26 103.85(4) . . ? P27 P25 P26 59.38(3) . . ? P23 P26 P27 103.10(4) . . ? P23 P26 P25 104.06(4) . . ? P27 P26 P25 59.57(4) . . ? P24 P27 P26 108.25(4) . . ? P24 P27 P25 108.03(5) . . ? P26 P27 P25 61.05(4) . . ? P43 In2 P32 125.39(3) . . ? P43 In2 P33 123.84(3) . . ? P32 In2 P33 80.37(2) . . ? P43 In2 P42 80.07(3) . . ? P32 In2 P42 119.36(3) . . ? P33 In2 P42 134.48(3) . . ? P34 P31 P33 102.97(5) . . ? P34 P31 P32 103.08(4) . . ? P33 P31 P32 97.32(4) . . ? P35 P32 P31 99.37(4) . . ? P35 P32 In2 91.40(3) . . ? P31 P32 In2 82.06(3) . . ? P36 P33 P31 99.59(4) . . ? P36 P33 In2 90.93(3) . . ? P31 P33 In2 81.80(3) . . ? P37 P34 P31 98.34(4) . . ? P32 P35 P37 103.93(4) . . ? P32 P35 P36 104.37(4) . . ? P37 P35 P36 59.75(4) . . ? P33 P36 P37 103.41(4) . . ? P33 P36 P35 104.06(4) . . ? P37 P36 P35 59.39(4) . . ? P34 P37 P35 107.98(5) . . ? P34 P37 P36 107.98(4) . . ? P35 P37 P36 60.85(4) . . ? P44 P41 P43 101.86(5) . . ? P44 P41 P42 103.73(5) . . ? P43 P41 P42 97.18(4) . . ? P45 P42 P41 99.46(5) . . ? P45 P42 In2 87.34(4) . . ? P41 P42 In2 83.65(3) . . ? P46 P43 P41 100.16(4) . . ? P46 P43 In2 87.11(3) . . ? P41 P43 In2 84.45(3) . . ? P47 P44 P41 98.30(4) . . ? P42 P45 P47 103.96(4) . . ? P42 P45 P46 103.95(4) . . ? P47 P45 P46 59.43(4) . . ? P43 P46 P47 102.94(4) . . ? P43 P46 P45 104.06(4) . . ? P47 P46 P45 59.43(4) . . ? P44 P47 P45 108.33(5) . . ? P44 P47 P46 108.18(4) . . ? P45 P47 P46 61.14(4) . . ? O12 K1 O13 136.68(6) . . ? O12 K1 O16 100.10(6) . . ? O13 K1 O16 118.46(6) . . ? O12 K1 O15 120.32(6) . . ? O13 K1 O15 97.41(6) . . ? O16 K1 O15 58.83(6) . . ? O12 K1 O14 98.58(6) . . ? O13 K1 O14 59.49(6) . . ? O16 K1 O14 97.68(6) . . ? O15 K1 O14 136.24(6) . . ? O12 K1 O11 59.04(5) . . ? O13 K1 O11 96.69(6) . . ? O16 K1 O11 139.52(6) . . ? O15 K1 O11 99.68(6) . . ? O14 K1 O11 118.34(6) . . ? O12 K1 N12 62.13(6) . . ? O13 K1 N12 119.06(7) . . ? O16 K1 N12 61.12(7) . . ? O15 K1 N12 119.14(7) . . ? O14 K1 N12 60.46(6) . . ? O11 K1 N12 120.05(7) . . ? O12 K1 N11 118.12(7) . . ? O13 K1 N11 60.72(7) . . ? O16 K1 N11 118.83(7) . . ? O15 K1 N11 60.85(7) . . ? O14 K1 N11 119.34(7) . . ? O11 K1 N11 60.17(7) . . ? N12 K1 N11 179.74(9) . . ? O25 K2 O24 116.01(6) . . ? O25 K2 O22 140.78(6) . . ? O24 K2 O22 97.87(6) . . ? O25 K2 O23 97.87(6) . . ? O24 K2 O23 59.38(6) . . ? O22 K2 O23 116.96(6) . . ? O25 K2 O21 100.70(6) . . ? O24 K2 O21 138.17(6) . . ? O22 K2 O21 59.15(6) . . ? O23 K2 O21 97.96(6) . . ? O25 K2 O26 59.09(6) . . ? O24 K2 O26 97.76(6) . . ? O22 K2 O26 99.09(6) . . ? O23 K2 O26 138.50(6) . . ? O21 K2 O26 118.84(6) . . ? O25 K2 N22 118.16(6) . . ? O24 K2 N22 61.30(7) . . ? O22 K2 N22 60.72(7) . . ? O23 K2 N22 119.41(7) . . ? O21 K2 N22 118.58(7) . . ? O26 K2 N22 60.44(6) . . ? O25 K2 N21 62.36(6) . . ? O24 K2 N21 119.20(7) . . ? O22 K2 N21 118.44(7) . . ? O23 K2 N21 60.93(6) . . ? O21 K2 N21 60.59(6) . . ? O26 K2 N21 119.90(6) . . ? N22 K2 N21 179.16(7) . . ? O34 K3 O32 91.47(7) . . ? O34 K3 O31 110.29(7) . . ? O32 K3 O31 59.91(7) . . ? O34 K3 O33 59.77(7) . . ? O32 K3 O33 132.44(7) . . ? O31 K3 O33 93.31(7) . . ? O34 K3 O36 101.25(7) . . ? O32 K3 O36 101.29(7) . . ? O31 K3 O36 142.90(7) . . ? O33 K3 O36 119.87(7) . . ? O34 K3 O35 141.44(7) . . ? O32 K3 O35 123.05(7) . . ? O31 K3 O35 102.51(7) . . ? O33 K3 O35 99.48(7) . . ? O36 K3 O35 58.82(6) . . ? O34 K3 N31 119.16(8) . . ? O32 K3 N31 120.09(8) . . ? O31 K3 N31 61.36(7) . . ? O33 K3 N31 60.86(7) . . ? O36 K3 N31 118.65(7) . . ? O35 K3 N31 60.88(7) . . ? O34 K3 N32 60.65(8) . . ? O32 K3 N32 60.96(8) . . ? O31 K3 N32 119.70(8) . . ? O33 K3 N32 118.69(8) . . ? O36 K3 N32 60.60(7) . . ? O35 K3 N32 118.53(7) . . ? N31 K3 N32 178.93(8) . . ? O44 K4 O42 98.91(6) . . ? O44 K4 O41 117.14(7) . . ? O42 K4 O41 61.01(7) . . ? O44 K4 O43 60.57(6) . . ? O42 K4 O43 142.38(6) . . ? O41 K4 O43 98.54(7) . . ? O44 K4 O45 137.47(6) . . ? O42 K4 O45 117.51(6) . . ? O41 K4 O45 100.18(6) . . ? O43 K4 O45 96.02(6) . . ? O44 K4 O46 96.05(6) . . ? O42 K4 O46 98.78(6) . . ? O41 K4 O46 142.44(7) . . ? O43 K4 O46 113.64(6) . . ? O45 K4 O46 59.17(5) . . ? O44 K4 N41 119.87(7) . . ? O42 K4 N41 119.73(7) . . ? O41 K4 N41 60.65(7) . . ? O43 K4 N41 60.85(7) . . ? O45 K4 N41 61.00(6) . . ? O46 K4 N41 118.67(6) . . ? O44 K4 N42 60.65(6) . . ? O42 K4 N42 60.77(7) . . ? O41 K4 N42 120.07(7) . . ? O43 K4 N42 119.42(6) . . ? O45 K4 N42 117.97(6) . . ? O46 K4 N42 60.29(6) . . ? N41 K4 N42 178.96(7) . . ? O52 K5 O53 119.00(7) . . ? O52 K5 O54 99.72(7) . . ? O53 K5 O54 59.95(7) . . ? O52 K5 O51 59.45(8) . . ? O53 K5 O51 95.98(7) . . ? O54 K5 O51 137.43(7) . . ? O52 K5 O55 135.06(8) . . ? O53 K5 O55 100.22(8) . . ? O54 K5 O55 119.54(8) . . ? O51 K5 O55 97.76(8) . . ? O52 K5 O56 95.76(7) . . ? O53 K5 O56 141.39(7) . . ? O54 K5 O56 100.36(8) . . ? O51 K5 O56 117.27(7) . . ? O55 K5 O56 58.52(7) . . ? O52 K5 N52 60.74(8) . . ? O53 K5 N52 120.70(8) . . ? O54 K5 N52 62.02(8) . . ? O51 K5 N52 119.42(9) . . ? O55 K5 N52 118.00(8) . . ? O56 K5 N52 60.57(8) . . ? O52 K5 N51 120.49(9) . . ? O53 K5 N51 60.32(8) . . ? O54 K5 N51 118.58(9) . . ? O51 K5 N51 61.56(9) . . ? O55 K5 N51 60.08(8) . . ? O56 K5 N51 117.56(8) . . ? N52 K5 N51 178.08(9) . . ? O64 K6 O65 141.53(7) . . ? O64 K6 O62 102.65(7) . . ? O65 K6 O62 109.86(7) . . ? O64 K6 O61 115.45(8) . . ? O65 K6 O61 98.29(8) . . ? O62 K6 O61 61.11(8) . . ? O64 K6 O66 99.76(6) . . ? O65 K6 O66 59.27(7) . . ? O62 K6 O66 93.11(7) . . ? O61 K6 O66 139.40(7) . . ? O64 K6 O63 60.62(7) . . ? O65 K6 O63 99.29(7) . . ? O62 K6 O63 145.05(7) . . ? O61 K6 O63 96.68(7) . . ? O66 K6 O63 118.80(7) . . ? O64 K6 N62 61.18(7) . . ? O65 K6 N62 118.80(7) . . ? O62 K6 N62 60.99(7) . . ? O61 K6 N62 118.63(8) . . ? O66 K6 N62 61.11(7) . . ? O63 K6 N62 120.45(8) . . ? O64 K6 N61 119.16(8) . . ? O65 K6 N61 62.00(8) . . ? O62 K6 N61 117.59(9) . . ? O61 K6 N61 59.83(9) . . ? O66 K6 N61 119.97(7) . . ? O63 K6 N61 60.24(9) . . ? N62 K6 N61 178.46(9) . . ? C113 N11 C107 109.7(2) . . ? C113 N11 C101 109.3(2) . . ? C107 N11 C101 109.3(2) . . ? C113 N11 K1 108.99(18) . . ? C107 N11 K1 108.86(18) . . ? C101 N11 K1 110.63(18) . . ? C106 N12 C112 109.7(3) . . ? C106 N12 C118 109.9(3) . . ? C112 N12 C118 108.8(2) . . ? C106 N12 K1 107.46(17) . . ? C112 N12 K1 110.80(18) . . ? C118 N12 K1 110.13(19) . . ? C207 N21 C213 110.1(2) . . ? C207 N21 C201 109.5(2) . . ? C213 N21 C201 109.4(3) . . ? C207 N21 K2 110.04(18) . . ? C213 N21 K2 107.65(17) . . ? C201 N21 K2 110.13(18) . . ? C206 N22 C212 110.2(3) . . ? C206 N22 C218 109.4(3) . . ? C212 N22 C218 109.7(3) . . ? C206 N22 K2 109.65(19) . . ? C212 N22 K2 108.00(18) . . ? C218 N22 K2 109.90(18) . . ? C313 N31 C307 109.7(3) . . ? C313 N31 C301 109.4(3) . . ? C307 N31 C301 110.0(3) . . ? C313 N31 K3 109.13(19) . . ? C307 N31 K3 109.01(19) . . ? C301 N31 K3 109.52(19) . . ? C306 N32 C312 111.2(3) . . ? C306 N32 C318 109.1(3) . . ? C312 N32 C318 108.4(3) . . ? C306 N32 K3 108.1(2) . . ? C312 N32 K3 109.8(2) . . ? C318 N32 K3 110.25(19) . . ? C401 N41 C407 110.2(3) . . ? C401 N41 C413 109.6(3) . . ? C407 N41 C413 110.0(3) . . ? C401 N41 K4 109.4(2) . . ? C407 N41 K4 109.70(18) . . ? C413 N41 K4 107.88(17) . . ? C406 N42 C418 110.2(2) . . ? C406 N42 C412 109.5(2) . . ? C418 N42 C412 109.8(2) . . ? C406 N42 K4 108.66(17) . . ? C418 N42 K4 110.15(16) . . ? C412 N42 K4 108.43(17) . . ? C507 N51 C501 110.6(3) . . ? C507 N51 C513 108.1(3) . . ? C501 N51 C513 112.5(4) . . ? C507 N51 K5 109.3(2) . . ? C501 N51 K5 107.0(2) . . ? C513 N51 K5 109.2(2) . . ? C512 N52 C518 110.3(3) . . ? C512 N52 C506 110.0(3) . . ? C518 N52 C506 110.5(3) . . ? C512 N52 K5 107.2(2) . . ? C518 N52 K5 110.2(2) . . ? C506 N52 K5 108.5(2) . . ? C601 N61 C607 107.4(4) . . ? C601 N61 C613 110.4(3) . . ? C607 N61 C613 110.0(3) . . ? C601 N61 K6 111.1(3) . . ? C607 N61 K6 110.2(2) . . ? C613 N61 K6 107.7(2) . . ? C612 N62 C606 110.1(3) . . ? C612 N62 C618 109.7(3) . . ? C606 N62 C618 110.2(3) . . ? C612 N62 K6 108.3(2) . . ? C606 N62 K6 110.3(2) . . ? C618 N62 K6 108.29(19) . . ? C103 O11 C102 110.8(2) . . ? C103 O11 K1 112.84(15) . . ? C102 O11 K1 115.88(15) . . ? C104 O12 C105 110.1(2) . . ? C104 O12 K1 118.96(15) . . ? C105 O12 K1 114.69(16) . . ? C109 O13 C108 111.1(2) . . ? C109 O13 K1 118.53(17) . . ? C108 O13 K1 118.87(15) . . ? C111 O14 C110 110.6(2) . . ? C111 O14 K1 114.49(17) . . ? C110 O14 K1 112.37(16) . . ? C114 O15 C115 111.7(2) . . ? C114 O15 K1 117.19(16) . . ? C115 O15 K1 113.96(17) . . ? C116 O16 C117 111.4(2) . . ? C116 O16 K1 117.80(17) . . ? C117 O16 K1 115.78(18) . . ? C203 O21 C202 110.1(2) . . ? C203 O21 K2 114.42(18) . . ? C202 O21 K2 116.14(17) . . ? C204 O22 C205 111.2(3) . . ? C204 O22 K2 117.37(18) . . ? C205 O22 K2 118.07(19) . . ? C209 O23 C208 111.3(2) . . ? C209 O23 K2 115.45(16) . . ? C208 O23 K2 116.24(17) . . ? C211 O24 C210 111.0(2) . . ? C211 O24 K2 117.76(18) . . ? C210 O24 K2 115.70(17) . . ? C215 O25 C214 110.4(2) . . ? C215 O25 K2 119.95(16) . . ? C214 O25 K2 114.20(15) . . ? C216 O26 C217 110.8(2) . . ? C216 O26 K2 111.62(15) . . ? C217 O26 K2 116.68(16) . . ? C302 O31 C303 111.6(3) . . ? C302 O31 K3 115.04(19) . . ? C303 O31 K3 116.3(2) . . ? C304 O32 C305 111.4(3) . . ? C304 O32 K3 114.1(2) . . ? C305 O32 K3 119.4(2) . . ? C308 O33 C309 110.1(3) . . ? C308 O33 K3 118.20(19) . . ? C309 O33 K3 112.4(2) . . ? C311 O34 C310 110.7(3) . . ? C311 O34 K3 116.4(2) . . ? C310 O34 K3 117.0(2) . . ? C314 O35 C315 110.9(2) . . ? C314 O35 K3 116.54(17) . . ? C315 O35 K3 114.90(18) . . ? C317 O36 C316 112.1(3) . . ? C317 O36 K3 117.94(18) . . ? C316 O36 K3 117.36(18) . . ? C402 O41 C403 110.6(3) . . ? C402 O41 K4 118.00(19) . . ? C403 O41 K4 113.01(19) . . ? C405 O42 C404 111.1(3) . . ? C405 O42 K4 117.74(17) . . ? C404 O42 K4 112.03(19) . . ? C408 O43 C409 110.1(2) . . ? C408 O43 K4 117.60(18) . . ? C409 O43 K4 112.19(16) . . ? C411 O44 C410 111.0(2) . . ? C411 O44 K4 119.81(16) . . ? C410 O44 K4 116.67(16) . . ? C415 O45 C414 109.9(2) . . ? C415 O45 K4 115.01(15) . . ? C414 O45 K4 118.15(16) . . ? C416 O46 C417 110.8(2) . . ? C416 O46 K4 117.20(15) . . ? C417 O46 K4 117.74(16) . . ? C502 O51 C503 112.6(3) . . ? C502 O51 K5 117.3(2) . . ? C503 O51 K5 111.7(2) . . ? C504 O52 C505 113.0(3) . . ? C504 O52 K5 120.4(2) . . ? C505 O52 K5 122.4(2) . . ? C509 O53 C508 111.6(3) . . ? C509 O53 K5 116.5(2) . . ? C508 O53 K5 118.2(2) . . ? C510 O54 C511 110.8(3) . . ? C510 O54 K5 113.2(2) . . ? C511 O54 K5 116.1(2) . . ? C514 O55 C515 110.4(3) . . ? C514 O55 K5 120.5(2) . . ? C515 O55 K5 116.8(2) . . ? C517 O56 C516 112.1(3) . . ? C517 O56 K5 117.9(2) . . ? C516 O56 K5 117.6(2) . . ? C603 O61 C602 101.7(4) . . ? C602 O61 C3A 136.2(5) . . ? C603 O61 K6 116.0(3) . . ? C602 O61 K6 115.1(2) . . ? C3A O61 K6 104.7(4) . . ? C4A O62 C605 116.8(4) . . ? C605 O62 C604 105.4(3) . . ? C4A O62 K6 120.4(4) . . ? C605 O62 K6 115.58(18) . . ? C604 O62 K6 108.5(2) . . ? C608 O63 C609 110.8(3) . . ? C608 O63 K6 115.5(2) . . ? C609 O63 K6 112.0(2) . . ? C611 O64 C610 110.7(3) . . ? C611 O64 K6 119.20(19) . . ? C610 O64 K6 115.16(19) . . ? C614 O65 C615 111.5(3) . . ? C614 O65 K6 115.7(2) . . ? C615 O65 K6 119.18(18) . . ? C616 O66 C617 110.1(3) . . ? C616 O66 K6 114.29(18) . . ? C617 O66 K6 116.90(17) . . ? N11 C101 C102 114.1(3) . . ? N11 C101 H10A 108.7 . . ? C102 C101 H10A 108.7 . . ? N11 C101 H10B 108.7 . . ? C102 C101 H10B 108.7 . . ? H10A C101 H10B 107.6 . . ? O11 C102 C101 109.2(2) . . ? O11 C102 H10C 109.8 . . ? C101 C102 H10C 109.8 . . ? O11 C102 H10D 109.8 . . ? C101 C102 H10D 109.8 . . ? H10C C102 H10D 108.3 . . ? O11 C103 C104 110.0(2) . . ? O11 C103 H10E 109.7 . . ? C104 C103 H10E 109.7 . . ? O11 C103 H10F 109.7 . . ? C104 C103 H10F 109.7 . . ? H10E C103 H10F 108.2 . . ? O12 C104 C103 109.5(2) . . ? O12 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O12 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.2 . . ? O12 C105 C106 109.5(3) . . ? O12 C105 H10I 109.8 . . ? C106 C105 H10I 109.8 . . ? O12 C105 H10J 109.8 . . ? C106 C105 H10J 109.8 . . ? H10I C105 H10J 108.2 . . ? N12 C106 C105 114.0(3) . . ? N12 C106 H10K 108.8 . . ? C105 C106 H10K 108.8 . . ? N12 C106 H10L 108.8 . . ? C105 C106 H10L 108.8 . . ? H10K C106 H10L 107.6 . . ? N11 C107 C108 113.7(2) . . ? N11 C107 H10M 108.8 . . ? C108 C107 H10M 108.8 . . ? N11 C107 H10N 108.8 . . ? C108 C107 H10N 108.8 . . ? H10M C107 H10N 107.7 . . ? O13 C108 C107 108.8(2) . . ? O13 C108 H10O 109.9 . . ? C107 C108 H10O 109.9 . . ? O13 C108 H10P 109.9 . . ? C107 C108 H10P 109.9 . . ? H10O C108 H10P 108.3 . . ? O13 C109 C110 109.8(2) . . ? O13 C109 H10Q 109.7 . . ? C110 C109 H10Q 109.7 . . ? O13 C109 H10R 109.7 . . ? C110 C109 H10R 109.7 . . ? H10Q C109 H10R 108.2 . . ? O14 C110 C109 109.8(2) . . ? O14 C110 H11A 109.7 . . ? C109 C110 H11A 109.7 . . ? O14 C110 H11B 109.7 . . ? C109 C110 H11B 109.7 . . ? H11A C110 H11B 108.2 . . ? O14 C111 C112 109.5(2) . . ? O14 C111 H11C 109.8 . . ? C112 C111 H11C 109.8 . . ? O14 C111 H11D 109.8 . . ? C112 C111 H11D 109.8 . . ? H11C C111 H11D 108.2 . . ? N12 C112 C111 113.5(3) . . ? N12 C112 H11E 108.9 . . ? C111 C112 H11E 108.9 . . ? N12 C112 H11F 108.9 . . ? C111 C112 H11F 108.9 . . ? H11E C112 H11F 107.7 . . ? N11 C113 C114 114.3(2) . . ? N11 C113 H11G 108.7 . . ? C114 C113 H11G 108.7 . . ? N11 C113 H11H 108.7 . . ? C114 C113 H11H 108.7 . . ? H11G C113 H11H 107.6 . . ? O15 C114 C113 110.6(2) . . ? O15 C114 H11I 109.5 . . ? C113 C114 H11I 109.5 . . ? O15 C114 H11J 109.5 . . ? C113 C114 H11J 109.5 . . ? H11I C114 H11J 108.1 . . ? O15 C115 C116 110.0(3) . . ? O15 C115 H11K 109.7 . . ? C116 C115 H11K 109.7 . . ? O15 C115 H11L 109.7 . . ? C116 C115 H11L 109.7 . . ? H11K C115 H11L 108.2 . . ? O16 C116 C115 108.9(3) . . ? O16 C116 H11M 109.9 . . ? C115 C116 H11M 109.9 . . ? O16 C116 H11N 109.9 . . ? C115 C116 H11N 109.9 . . ? H11M C116 H11N 108.3 . . ? O16 C117 C118 109.4(3) . . ? O16 C117 H11O 109.8 . . ? C118 C117 H11O 109.8 . . ? O16 C117 H11P 109.8 . . ? C118 C117 H11P 109.8 . . ? H11O C117 H11P 108.2 . . ? N12 C118 C117 114.2(3) . . ? N12 C118 H11Q 108.7 . . ? C117 C118 H11Q 108.7 . . ? N12 C118 H11R 108.7 . . ? C117 C118 H11R 108.7 . . ? H11Q C118 H11R 107.6 . . ? N21 C201 C202 114.1(3) . . ? N21 C201 H20A 108.7 . . ? C202 C201 H20A 108.7 . . ? N21 C201 H20B 108.7 . . ? C202 C201 H20B 108.7 . . ? H20A C201 H20B 107.6 . . ? O21 C202 C201 109.7(2) . . ? O21 C202 H20C 109.7 . . ? C201 C202 H20C 109.7 . . ? O21 C202 H20D 109.7 . . ? C201 C202 H20D 109.7 . . ? H20C C202 H20D 108.2 . . ? O21 C203 C204 110.3(3) . . ? O21 C203 H20E 109.6 . . ? C204 C203 H20E 109.6 . . ? O21 C203 H20F 109.6 . . ? C204 C203 H20F 109.6 . . ? H20E C203 H20F 108.1 . . ? O22 C204 C203 109.8(3) . . ? O22 C204 H20G 109.7 . . ? C203 C204 H20G 109.7 . . ? O22 C204 H20H 109.7 . . ? C203 C204 H20H 109.7 . . ? H20G C204 H20H 108.2 . . ? O22 C205 C206 109.3(3) . . ? O22 C205 H20I 109.8 . . ? C206 C205 H20I 109.8 . . ? O22 C205 H20J 109.8 . . ? C206 C205 H20J 109.8 . . ? H20I C205 H20J 108.3 . . ? N22 C206 C205 114.1(3) . . ? N22 C206 H20K 108.7 . . ? C205 C206 H20K 108.7 . . ? N22 C206 H20L 108.7 . . ? C205 C206 H20L 108.7 . . ? H20K C206 H20L 107.6 . . ? N21 C207 C208 114.2(2) . . ? N21 C207 H20M 108.7 . . ? C208 C207 H20M 108.7 . . ? N21 C207 H20N 108.7 . . ? C208 C207 H20N 108.7 . . ? H20M C207 H20N 107.6 . . ? O23 C208 C207 109.8(2) . . ? O23 C208 H20O 109.7 . . ? C207 C208 H20O 109.7 . . ? O23 C208 H20P 109.7 . . ? C207 C208 H20P 109.7 . . ? H20O C208 H20P 108.2 . . ? O23 C209 C210 109.4(2) . . ? O23 C209 H20Q 109.8 . . ? C210 C209 H20Q 109.8 . . ? O23 C209 H20R 109.8 . . ? C210 C209 H20R 109.8 . . ? H20Q C209 H20R 108.2 . . ? O24 C210 C209 109.0(2) . . ? O24 C210 H21A 109.9 . . ? C209 C210 H21A 109.9 . . ? O24 C210 H21B 109.9 . . ? C209 C210 H21B 109.9 . . ? H21A C210 H21B 108.3 . . ? O24 C211 C212 109.3(3) . . ? O24 C211 H21C 109.8 . . ? C212 C211 H21C 109.8 . . ? O24 C211 H21D 109.8 . . ? C212 C211 H21D 109.8 . . ? H21C C211 H21D 108.3 . . ? N22 C212 C211 115.0(3) . . ? N22 C212 H21E 108.5 . . ? C211 C212 H21E 108.5 . . ? N22 C212 H21F 108.5 . . ? C211 C212 H21F 108.5 . . ? H21E C212 H21F 107.5 . . ? N21 C213 C214 114.1(3) . . ? N21 C213 H21G 108.7 . . ? C214 C213 H21G 108.7 . . ? N21 C213 H21H 108.7 . . ? C214 C213 H21H 108.7 . . ? H21G C213 H21H 107.6 . . ? O25 C214 C213 109.3(2) . . ? O25 C214 H21I 109.8 . . ? C213 C214 H21I 109.8 . . ? O25 C214 H21J 109.8 . . ? C213 C214 H21J 109.8 . . ? H21I C214 H21J 108.3 . . ? O25 C215 C216 109.0(2) . . ? O25 C215 H21K 109.9 . . ? C216 C215 H21K 109.9 . . ? O25 C215 H21L 109.9 . . ? C216 C215 H21L 109.9 . . ? H21K C215 H21L 108.3 . . ? O26 C216 C215 110.0(2) . . ? O26 C216 H21M 109.7 . . ? C215 C216 H21M 109.7 . . ? O26 C216 H21N 109.7 . . ? C215 C216 H21N 109.7 . . ? H21M C216 H21N 108.2 . . ? O26 C217 C218 109.7(3) . . ? O26 C217 H21O 109.7 . . ? C218 C217 H21O 109.7 . . ? O26 C217 H21P 109.7 . . ? C218 C217 H21P 109.7 . . ? H21O C217 H21P 108.2 . . ? N22 C218 C217 113.9(3) . . ? N22 C218 H21Q 108.8 . . ? C217 C218 H21Q 108.8 . . ? N22 C218 H21R 108.8 . . ? C217 C218 H21R 108.8 . . ? H21Q C218 H21R 107.7 . . ? N31 C301 C302 114.4(3) . . ? N31 C301 H30A 108.7 . . ? C302 C301 H30A 108.7 . . ? N31 C301 H30B 108.7 . . ? C302 C301 H30B 108.7 . . ? H30A C301 H30B 107.6 . . ? O31 C302 C301 110.0(3) . . ? O31 C302 H30C 109.7 . . ? C301 C302 H30C 109.7 . . ? O31 C302 H30D 109.7 . . ? C301 C302 H30D 109.7 . . ? H30C C302 H30D 108.2 . . ? O31 C303 C304 109.6(3) . . ? O31 C303 H30E 109.7 . . ? C304 C303 H30E 109.7 . . ? O31 C303 H30F 109.7 . . ? C304 C303 H30F 109.7 . . ? H30E C303 H30F 108.2 . . ? O32 C304 C303 109.0(3) . . ? O32 C304 H30G 109.9 . . ? C303 C304 H30G 109.9 . . ? O32 C304 H30H 109.9 . . ? C303 C304 H30H 109.9 . . ? H30G C304 H30H 108.3 . . ? O32 C305 C306 109.9(3) . . ? O32 C305 H30I 109.7 . . ? C306 C305 H30I 109.7 . . ? O32 C305 H30J 109.7 . . ? C306 C305 H30J 109.7 . . ? H30I C305 H30J 108.2 . . ? N32 C306 C305 114.0(3) . . ? N32 C306 H30K 108.8 . . ? C305 C306 H30K 108.8 . . ? N32 C306 H30L 108.8 . . ? C305 C306 H30L 108.8 . . ? H30K C306 H30L 107.7 . . ? N31 C307 C308 114.1(3) . . ? N31 C307 H30M 108.7 . . ? C308 C307 H30M 108.7 . . ? N31 C307 H30N 108.7 . . ? C308 C307 H30N 108.7 . . ? H30M C307 H30N 107.6 . . ? O33 C308 C307 110.0(3) . . ? O33 C308 H30O 109.7 . . ? C307 C308 H30O 109.7 . . ? O33 C308 H30P 109.7 . . ? C307 C308 H30P 109.7 . . ? H30O C308 H30P 108.2 . . ? O33 C309 C310 110.4(3) . . ? O33 C309 H30Q 109.6 . . ? C310 C309 H30Q 109.6 . . ? O33 C309 H30R 109.6 . . ? C310 C309 H30R 109.6 . . ? H30Q C309 H30R 108.1 . . ? O34 C310 C309 110.3(3) . . ? O34 C310 H31A 109.6 . . ? C309 C310 H31A 109.6 . . ? O34 C310 H31B 109.6 . . ? C309 C310 H31B 109.6 . . ? H31A C310 H31B 108.1 . . ? O34 C311 C312 110.4(3) . . ? O34 C311 H31C 109.6 . . ? C312 C311 H31C 109.6 . . ? O34 C311 H31D 109.6 . . ? C312 C311 H31D 109.6 . . ? H31C C311 H31D 108.1 . . ? C311 C312 N32 115.1(3) . . ? C311 C312 H31E 108.5 . . ? N32 C312 H31E 108.5 . . ? C311 C312 H31F 108.5 . . ? N32 C312 H31F 108.5 . . ? H31E C312 H31F 107.5 . . ? N31 C313 C314 114.6(3) . . ? N31 C313 H31G 108.6 . . ? C314 C313 H31G 108.6 . . ? N31 C313 H31H 108.6 . . ? C314 C313 H31H 108.6 . . ? H31G C313 H31H 107.6 . . ? O35 C314 C313 109.7(3) . . ? O35 C314 H31I 109.7 . . ? C313 C314 H31I 109.7 . . ? O35 C314 H31J 109.7 . . ? C313 C314 H31J 109.7 . . ? H31I C314 H31J 108.2 . . ? O35 C315 C316 109.9(3) . . ? O35 C315 H31K 109.7 . . ? C316 C315 H31K 109.7 . . ? O35 C315 H31L 109.7 . . ? C316 C315 H31L 109.7 . . ? H31K C315 H31L 108.2 . . ? O36 C316 C315 109.7(3) . . ? O36 C316 H31M 109.7 . . ? C315 C316 H31M 109.7 . . ? O36 C316 H31N 109.7 . . ? C315 C316 H31N 109.7 . . ? H31M C316 H31N 108.2 . . ? O36 C317 C318 110.2(3) . . ? O36 C317 H31O 109.6 . . ? C318 C317 H31O 109.6 . . ? O36 C317 H31P 109.6 . . ? C318 C317 H31P 109.6 . . ? H31O C317 H31P 108.1 . . ? N32 C318 C317 113.2(3) . . ? N32 C318 H31Q 108.9 . . ? C317 C318 H31Q 108.9 . . ? N32 C318 H31R 108.9 . . ? C317 C318 H31R 108.9 . . ? H31Q C318 H31R 107.7 . . ? N41 C401 C402 114.2(3) . . ? N41 C401 H40A 108.7 . . ? C402 C401 H40A 108.7 . . ? N41 C401 H40B 108.7 . . ? C402 C401 H40B 108.7 . . ? H40A C401 H40B 107.6 . . ? O41 C402 C401 109.5(3) . . ? O41 C402 H40C 109.8 . . ? C401 C402 H40C 109.8 . . ? O41 C402 H40D 109.8 . . ? C401 C402 H40D 109.8 . . ? H40C C402 H40D 108.2 . . ? O41 C403 C404 108.9(3) . . ? O41 C403 H40E 109.9 . . ? C404 C403 H40E 109.9 . . ? O41 C403 H40F 109.9 . . ? C404 C403 H40F 109.9 . . ? H40E C403 H40F 108.3 . . ? O42 C404 C403 110.0(3) . . ? O42 C404 H40G 109.7 . . ? C403 C404 H40G 109.7 . . ? O42 C404 H40H 109.7 . . ? C403 C404 H40H 109.7 . . ? H40G C404 H40H 108.2 . . ? O42 C405 C406 109.8(3) . . ? O42 C405 H40I 109.7 . . ? C406 C405 H40I 109.7 . . ? O42 C405 H40J 109.7 . . ? C406 C405 H40J 109.7 . . ? H40I C405 H40J 108.2 . . ? N42 C406 C405 114.4(3) . . ? N42 C406 H40K 108.7 . . ? C405 C406 H40K 108.7 . . ? N42 C406 H40L 108.7 . . ? C405 C406 H40L 108.7 . . ? H40K C406 H40L 107.6 . . ? N41 C407 C408 113.7(3) . . ? N41 C407 H40M 108.8 . . ? C408 C407 H40M 108.8 . . ? N41 C407 H40N 108.8 . . ? C408 C407 H40N 108.8 . . ? H40M C407 H40N 107.7 . . ? O43 C408 C407 110.0(3) . . ? O43 C408 H40O 109.7 . . ? C407 C408 H40O 109.7 . . ? O43 C408 H40P 109.7 . . ? C407 C408 H40P 109.7 . . ? H40O C408 H40P 108.2 . . ? O43 C409 C410 109.8(2) . . ? O43 C409 H40Q 109.7 . . ? C410 C409 H40Q 109.7 . . ? O43 C409 H40R 109.7 . . ? C410 C409 H40R 109.7 . . ? H40Q C409 H40R 108.2 . . ? O44 C410 C409 109.6(2) . . ? O44 C410 H41A 109.7 . . ? C409 C410 H41A 109.7 . . ? O44 C410 H41B 109.7 . . ? C409 C410 H41B 109.7 . . ? H41A C410 H41B 108.2 . . ? O44 C411 C412 109.7(2) . . ? O44 C411 H41C 109.7 . . ? C412 C411 H41C 109.7 . . ? O44 C411 H41D 109.7 . . ? C412 C411 H41D 109.7 . . ? H41C C411 H41D 108.2 . . ? N42 C412 C411 113.9(2) . . ? N42 C412 H41E 108.8 . . ? C411 C412 H41E 108.8 . . ? N42 C412 H41F 108.8 . . ? C411 C412 H41F 108.8 . . ? H41E C412 H41F 107.7 . . ? N41 C413 C414 113.9(2) . . ? N41 C413 H41G 108.8 . . ? C414 C413 H41G 108.8 . . ? N41 C413 H41H 108.8 . . ? C414 C413 H41H 108.8 . . ? H41G C413 H41H 107.7 . . ? O45 C414 C413 109.5(2) . . ? O45 C414 H41I 109.8 . . ? C413 C414 H41I 109.8 . . ? O45 C414 H41J 109.8 . . ? C413 C414 H41J 109.8 . . ? H41I C414 H41J 108.2 . . ? O45 C415 C416 109.4(2) . . ? O45 C415 H41K 109.8 . . ? C416 C415 H41K 109.8 . . ? O45 C415 H41L 109.8 . . ? C416 C415 H41L 109.8 . . ? H41K C415 H41L 108.2 . . ? O46 C416 C415 109.9(2) . . ? O46 C416 H41M 109.7 . . ? C415 C416 H41M 109.7 . . ? O46 C416 H41N 109.7 . . ? C415 C416 H41N 109.7 . . ? H41M C416 H41N 108.2 . . ? O46 C417 C418 109.5(2) . . ? O46 C417 H41O 109.8 . . ? C418 C417 H41O 109.8 . . ? O46 C417 H41P 109.8 . . ? C418 C417 H41P 109.8 . . ? H41O C417 H41P 108.2 . . ? N42 C418 C417 113.4(2) . . ? N42 C418 H41Q 108.9 . . ? C417 C418 H41Q 108.9 . . ? N42 C418 H41R 108.9 . . ? C417 C418 H41R 108.9 . . ? H41Q C418 H41R 107.7 . . ? N51 C501 C502 115.2(3) . . ? N51 C501 H50A 108.5 . . ? C502 C501 H50A 108.5 . . ? N51 C501 H50B 108.5 . . ? C502 C501 H50B 108.5 . . ? H50A C501 H50B 107.5 . . ? O51 C502 C501 110.5(3) . . ? O51 C502 H50C 109.6 . . ? C501 C502 H50C 109.6 . . ? O51 C502 H50D 109.6 . . ? C501 C502 H50D 109.6 . . ? H50C C502 H50D 108.1 . . ? O51 C503 C504 110.6(3) . . ? O51 C503 H50E 109.5 . . ? C504 C503 H50E 109.5 . . ? O51 C503 H50F 109.5 . . ? C504 C503 H50F 109.5 . . ? H50E C503 H50F 108.1 . . ? O52 C504 C503 109.6(3) . . ? O52 C504 H50G 109.7 . . ? C503 C504 H50G 109.7 . . ? O52 C504 H50H 109.7 . . ? C503 C504 H50H 109.7 . . ? H50G C504 H50H 108.2 . . ? O52 C505 C506 108.7(3) . . ? O52 C505 H50I 109.9 . . ? C506 C505 H50I 109.9 . . ? O52 C505 H50J 109.9 . . ? C506 C505 H50J 109.9 . . ? H50I C505 H50J 108.3 . . ? N52 C506 C505 114.6(3) . . ? N52 C506 H50K 108.6 . . ? C505 C506 H50K 108.6 . . ? N52 C506 H50L 108.6 . . ? C505 C506 H50L 108.6 . . ? H50K C506 H50L 107.6 . . ? N51 C507 C508 114.5(3) . . ? N51 C507 H50M 108.6 . . ? C508 C507 H50M 108.6 . . ? N51 C507 H50N 108.6 . . ? C508 C507 H50N 108.6 . . ? H50M C507 H50N 107.6 . . ? O53 C508 C507 109.3(3) . . ? O53 C508 H50O 109.8 . . ? C507 C508 H50O 109.8 . . ? O53 C508 H50P 109.8 . . ? C507 C508 H50P 109.8 . . ? H50O C508 H50P 108.3 . . ? O53 C509 C510 110.1(3) . . ? O53 C509 H50Q 109.6 . . ? C510 C509 H50Q 109.6 . . ? O53 C509 H50R 109.6 . . ? C510 C509 H50R 109.6 . . ? H50Q C509 H50R 108.2 . . ? O54 C510 C509 109.7(3) . . ? O54 C510 H51A 109.7 . . ? C509 C510 H51A 109.7 . . ? O54 C510 H51B 109.7 . . ? C509 C510 H51B 109.7 . . ? H51A C510 H51B 108.2 . . ? O54 C511 C512 110.1(3) . . ? O54 C511 H51C 109.7 . . ? C512 C511 H51C 109.7 . . ? O54 C511 H51D 109.7 . . ? C512 C511 H51D 109.7 . . ? H51C C511 H51D 108.2 . . ? N52 C512 C511 114.7(3) . . ? N52 C512 H51E 108.6 . . ? C511 C512 H51E 108.6 . . ? N52 C512 H51F 108.6 . . ? C511 C512 H51F 108.6 . . ? H51E C512 H51F 107.6 . . ? N51 C513 C514 113.1(4) . . ? N51 C513 H51G 109.0 . . ? C514 C513 H51G 109.0 . . ? N51 C513 H51H 109.0 . . ? C514 C513 H51H 109.0 . . ? H51G C513 H51H 107.8 . . ? O55 C514 C513 109.3(3) . . ? O55 C514 H51I 109.8 . . ? C513 C514 H51I 109.8 . . ? O55 C514 H51J 109.8 . . ? C513 C514 H51J 109.8 . . ? H51I C514 H51J 108.3 . . ? O55 C515 C516 110.0(3) . . ? O55 C515 H51K 109.7 . . ? C516 C515 H51K 109.7 . . ? O55 C515 H51L 109.7 . . ? C516 C515 H51L 109.7 . . ? H51K C515 H51L 108.2 . . ? O56 C516 C515 110.9(3) . . ? O56 C516 H51M 109.5 . . ? C515 C516 H51M 109.5 . . ? O56 C516 H51N 109.5 . . ? C515 C516 H51N 109.5 . . ? H51M C516 H51N 108.1 . . ? O56 C517 C518 110.1(3) . . ? O56 C517 H51O 109.6 . . ? C518 C517 H51O 109.6 . . ? O56 C517 H51P 109.6 . . ? C518 C517 H51P 109.6 . . ? H51O C517 H51P 108.2 . . ? N52 C518 C517 115.0(3) . . ? N52 C518 H51Q 108.5 . . ? C517 C518 H51Q 108.5 . . ? N52 C518 H51R 108.5 . . ? C517 C518 H51R 108.5 . . ? H51Q C518 H51R 107.5 . . ? C602 C601 N61 113.0(4) . . ? C602 C601 H60A 109.0 . . ? N61 C601 H60A 109.0 . . ? C602 C601 H60B 109.0 . . ? N61 C601 H60B 109.0 . . ? H60A C601 H60B 107.8 . . ? C601 C602 O61 110.2(4) . . ? C601 C602 H60C 109.6 . . ? O61 C602 H60C 109.6 . . ? C601 C602 H60D 109.6 . . ? O61 C602 H60D 109.6 . . ? H60C C602 H60D 108.1 . . ? O62 C605 C606 109.2(3) . . ? O62 C605 H60I 109.8 . . ? C606 C605 H60I 109.8 . . ? O62 C605 H60J 109.8 . . ? C606 C605 H60J 109.8 . . ? H60I C605 H60J 108.3 . . ? N62 C606 C605 113.2(3) . . ? N62 C606 H60K 108.9 . . ? C605 C606 H60K 108.9 . . ? N62 C606 H60L 108.9 . . ? C605 C606 H60L 108.9 . . ? H60K C606 H60L 107.8 . . ? N61 C607 C608 113.3(4) . . ? N61 C607 H60M 108.9 . . ? C608 C607 H60M 108.9 . . ? N61 C607 H60N 108.9 . . ? C608 C607 H60N 108.9 . . ? H60M C607 H60N 107.7 . . ? O63 C608 C607 109.7(3) . . ? O63 C608 H60O 109.7 . . ? C607 C608 H60O 109.7 . . ? O63 C608 H60P 109.7 . . ? C607 C608 H60P 109.7 . . ? H60O C608 H60P 108.2 . . ? O63 C609 C610 110.0(3) . . ? O63 C609 H60Q 109.7 . . ? C610 C609 H60Q 109.7 . . ? O63 C609 H60R 109.7 . . ? C610 C609 H60R 109.7 . . ? H60Q C609 H60R 108.2 . . ? O64 C610 C609 109.1(3) . . ? O64 C610 H61A 109.9 . . ? C609 C610 H61A 109.9 . . ? O64 C610 H61B 109.9 . . ? C609 C610 H61B 109.9 . . ? H61A C610 H61B 108.3 . . ? O64 C611 C612 109.2(3) . . ? O64 C611 H61C 109.8 . . ? C612 C611 H61C 109.8 . . ? O64 C611 H61D 109.8 . . ? C612 C611 H61D 109.8 . . ? H61C C611 H61D 108.3 . . ? N62 C612 C611 114.7(3) . . ? N62 C612 H61E 108.6 . . ? C611 C612 H61E 108.6 . . ? N62 C612 H61F 108.6 . . ? C611 C612 H61F 108.6 . . ? H61E C612 H61F 107.6 . . ? C614 C613 N61 113.6(3) . . ? C614 C613 H61G 108.9 . . ? N61 C613 H61G 108.9 . . ? C614 C613 H61H 108.9 . . ? N61 C613 H61H 108.9 . . ? H61G C613 H61H 107.7 . . ? O65 C614 C613 110.9(3) . . ? O65 C614 H61I 109.5 . . ? C613 C614 H61I 109.5 . . ? O65 C614 H61J 109.5 . . ? C613 C614 H61J 109.5 . . ? H61I C614 H61J 108.1 . . ? O65 C615 C616 109.8(3) . . ? O65 C615 H61K 109.7 . . ? C616 C615 H61K 109.7 . . ? O65 C615 H61L 109.7 . . ? C616 C615 H61L 109.7 . . ? H61K C615 H61L 108.2 . . ? O66 C616 C615 109.9(3) . . ? O66 C616 H61M 109.7 . . ? C615 C616 H61M 109.7 . . ? O66 C616 H61N 109.7 . . ? C615 C616 H61N 109.7 . . ? H61M C616 H61N 108.2 . . ? O66 C617 C618 110.0(3) . . ? O66 C617 H61O 109.7 . . ? C618 C617 H61O 109.7 . . ? O66 C617 H61P 109.7 . . ? C618 C617 H61P 109.7 . . ? H61O C617 H61P 108.2 . . ? N62 C618 C617 113.2(3) . . ? N62 C618 H61Q 108.9 . . ? C617 C618 H61Q 108.9 . . ? N62 C618 H61R 108.9 . . ? C617 C618 H61R 108.9 . . ? H61Q C618 H61R 107.8 . . ? O61 C603 C604 101.1(4) . . ? O61 C603 H60E 111.6 . . ? C604 C603 H60E 111.6 . . ? O61 C603 H60F 111.6 . . ? C604 C603 H60F 111.6 . . ? H60E C603 H60F 109.4 . . ? C603 C604 O62 106.8(4) . . ? C603 C604 H60G 110.4 . . ? O62 C604 H60G 110.4 . . ? C603 C604 H60H 110.4 . . ? O62 C604 H60H 110.4 . . ? H60G C604 H60H 108.6 . . ? C4A C3A O61 110.1(8) . . ? C4A C3A H3A1 109.6 . . ? O61 C3A H3A1 109.6 . . ? C4A C3A H3A2 109.6 . . ? O61 C3A H3A2 109.6 . . ? H3A1 C3A H3A2 108.1 . . ? O62 C4A C3A 104.8(8) . . ? O62 C4A H4A1 110.8 . . ? C3A C4A H4A1 110.8 . . ? O62 C4A H4A2 110.8 . . ? C3A C4A H4A2 110.8 . . ? H4A1 C4A H4A2 108.9 . . ? C1R N1R C5R 116.4(6) . . ? C2R C1R N1R 124.1(5) . . ? C2R C1R H1R 118.0 . . ? N1R C1R H1R 118.0 . . ? C1R C2R C3R 120.6(6) . . ? C1R C2R H2R 119.7 . . ? C3R C2R H2R 119.7 . . ? C2R C3R C4R 117.4(6) . . ? C2R C3R H3R 121.3 . . ? C4R C3R H3R 121.3 . . ? C5R C4R C3R 119.4(7) . . ? C5R C4R H4R 120.3 . . ? C3R C4R H4R 120.3 . . ? C4R C5R N1R 122.1(7) . . ? C4R C5R H5R 119.0 . . ? N1R C5R H5R 119.0 . . ? C5S N1S C1S 117.2(3) . . ? N1S C1S C2S 125.0(4) . . ? N1S C1S H1S 117.5 . . ? C2S C1S H1S 117.5 . . ? C3S C2S C1S 118.7(4) . . ? C3S C2S H2S 120.7 . . ? C1S C2S H2S 120.7 . . ? C2S C3S C4S 119.0(4) . . ? C2S C3S H3S 120.5 . . ? C4S C3S H3S 120.5 . . ? C3S C4S C5S 118.5(4) . . ? C3S C4S H4S 120.7 . . ? C5S C4S H4S 120.7 . . ? N1S C5S C4S 121.7(4) . . ? N1S C5S H5S 119.2 . . ? C4S C5S H5S 119.2 . . ? C1T N1T C5T 114.9(5) . . ? N1T C1T C2T 122.0(5) . . ? N1T C1T H1T 119.0 . . ? C2T C1T H1T 119.0 . . ? C3T C2T C1T 121.3(5) . . ? C3T C2T H2T 119.3 . . ? C1T C2T H2T 119.3 . . ? C4T C3T C2T 118.6(6) . . ? C4T C3T H3T 120.7 . . ? C2T C3T H3T 120.7 . . ? C3T C4T C5T 118.1(6) . . ? C3T C4T H4T 121.0 . . ? C5T C4T H4T 121.0 . . ? N1T C5T C4T 125.0(5) . . ? N1T C5T H5T 117.5 . . ? C4T C5T H5T 117.5 . . ? C5U N1U C1U 120.7(6) . . ? C2U C1U N1U 118.9(6) . . ? C2U C1U H1U 120.5 . . ? N1U C1U H1U 120.5 . . ? C3U C2U C1U 119.5(6) . . ? C3U C2U H2U 120.3 . . ? C1U C2U H2U 120.3 . . ? C2U C3U C4U 118.9(5) . . ? C2U C3U H3U 120.5 . . ? C4U C3U H3U 120.5 . . ? C5U C4U C3U 121.2(5) . . ? C5U C4U H4U 119.4 . . ? C3U C4U H4U 119.4 . . ? N1U C5U C4U 120.4(6) . . ? N1U C5U H5U 119.8 . . ? C4U C5U H5U 119.8 . . ? C1V N1V C5V 116.7(3) . . ? N1V C1V C2V 123.1(4) . . ? N1V C1V H1V 118.4 . . ? C2V C1V H1V 118.4 . . ? C1V C2V C3V 118.8(4) . . ? C1V C2V H2V 120.6 . . ? C3V C2V H2V 120.6 . . ? C4V C3V C2V 118.8(4) . . ? C4V C3V H3V 120.6 . . ? C2V C3V H3V 120.6 . . ? C5V C4V C3V 117.7(4) . . ? C5V C4V H4V 121.1 . . ? C3V C4V H4V 121.1 . . ? N1V C5V C4V 124.9(3) . . ? N1V C5V H5V 117.6 . . ? C4V C5V H5V 117.6 . . ? C5W N1W C1W 116.2(4) . . ? N1W C1W C2W 124.0(4) . . ? N1W C1W H1W 118.0 . . ? C2W C1W H1W 118.0 . . ? C1W C2W C3W 118.1(4) . . ? C1W C2W H2W 121.0 . . ? C3W C2W H2W 121.0 . . ? C4W C3W C2W 117.5(4) . . ? C4W C3W H3W 121.2 . . ? C2W C3W H3W 121.2 . . ? C5W C4W C3W 120.8(4) . . ? C5W C4W H4W 119.6 . . ? C3W C4W H4W 119.6 . . ? N1W C5W C4W 123.4(4) . . ? N1W C5W H5W 118.3 . . ? C4W C5W H5W 118.3 . . ? C5Q N1Q C1Q 116.4(5) . . ? N1Q C1Q C2Q 122.7(5) . . ? N1Q C1Q H1Q 118.7 . . ? C2Q C1Q H1Q 118.7 . . ? C3Q C2Q C1Q 118.8(6) . . ? C3Q C2Q H2Q 120.6 . . ? C1Q C2Q H2Q 120.6 . . ? C4Q C3Q C2Q 118.7(5) . . ? C4Q C3Q H3Q 120.7 . . ? C2Q C3Q H3Q 120.7 . . ? C3Q C4Q C5Q 120.4(5) . . ? C3Q C4Q H4Q 119.8 . . ? C5Q C4Q H4Q 119.8 . . ? N1Q C5Q C4Q 122.9(5) . . ? N1Q C5Q H5Q 118.5 . . ? C4Q C5Q H5Q 118.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.267 _refine_diff_density_min -1.549 _refine_diff_density_rms 0.071 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 786256' #TrackingRef '- combined_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]2[TlP7]*py ; _chemical_name_common (K(2,2,2-crypt))2(TlP7)*py _chemical_melting_point . _chemical_formula_moiety '2(C18 H36 K N2 O6), P7 Tl, C5 H5 N' _chemical_formula_sum 'C41 H77 K2 N5 O12 P7 Tl' _chemical_formula_weight 1331.44 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.18330(10) _cell_length_b 20.5010(2) _cell_length_c 25.6093(3) _cell_angle_alpha 66.9990(10) _cell_angle_beta 79.2500(10) _cell_angle_gamma 87.8950(10) _cell_volume 5779.95(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 88030 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.16 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 3.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3619 _exptl_absorpt_correction_T_max 0.6294 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 33025 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20159 _reflns_number_gt 12168 _reflns_threshold_expression >2\s(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure exhibits pseudo-symmetry. The K-crypts defined by K1 and K2 are related by a C-centering, as are the two [TlP7]2-- clusters. The symmetry is broken by the remaining two [K(2,2,2-crypt)]+ cations and the solvent. As a result, PLATON finds an 80% fit over the whole structure to a smaller cell. The absence associated with the pseudo C-centering is the hkl, h+k=2n which has a mean I/sigma(I) of 660 for h+k even and 200 for h+k odd, showing a marked weakness, but not an absense. The following constraints were applied to improve ADP values for cryptand carbon atoms: EADP O41 C403 EADP C404 O42 EADP O43 C409 EADP O32 C304 EADP O16 C115 EADP O34 C310 ; _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^)+(0.1087P)^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_number_reflns 20159 _refine_ls_number_parameters 1189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1999 _refine_ls_wR_factor_gt 0.1810 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 K1 K 0.12926(13) 0.66727(9) 0.41968(6) 0.0167(4) Uani 1 1 d . . . O11 O 0.0679(4) 0.6848(3) 0.3156(2) 0.0192(12) Uani 1 1 d . . . O12 O 0.2303(4) 0.5827(3) 0.3601(2) 0.0214(13) Uani 1 1 d . . . O13 O 0.1238(4) 0.8143(3) 0.4013(2) 0.0243(13) Uani 1 1 d . . . O14 O 0.3240(4) 0.7373(3) 0.4156(2) 0.0222(12) Uani 1 1 d . . . O15 O -0.0909(4) 0.6266(3) 0.4960(2) 0.0234(13) Uani 1 1 d . . . O16 O 0.1097(4) 0.5672(3) 0.5326(2) 0.0236(11) Uani 1 1 d . . . N11 N -0.0780(5) 0.7493(4) 0.3869(3) 0.0250(16) Uani 1 1 d . . . N12 N 0.3290(5) 0.5842(3) 0.4565(2) 0.0186(15) Uani 1 1 d . . . C101 C -0.0801(7) 0.7615(5) 0.3253(3) 0.030(2) Uani 1 1 d . . . H10G H -0.1564 0.7741 0.3176 0.036 Uiso 1 1 calc R . . H10H H -0.0284 0.8020 0.2993 0.036 Uiso 1 1 calc R . . C102 C -0.0472(7) 0.6978(5) 0.3125(4) 0.030(2) Uani 1 1 d . . . H10M H -0.0942 0.6560 0.3406 0.036 Uiso 1 1 calc R . . H10N H -0.0594 0.7055 0.2733 0.036 Uiso 1 1 calc R . . C103 C 0.1069(7) 0.6324(5) 0.2933(3) 0.027(2) Uani 1 1 d . . . H10C H 0.1017 0.6499 0.2520 0.033 Uiso 1 1 calc R . . H10D H 0.0591 0.5885 0.3143 0.033 Uiso 1 1 calc R . . C104 C 0.2246(7) 0.6163(5) 0.2999(3) 0.026(2) Uani 1 1 d . . . H10I H 0.2536 0.5846 0.2800 0.031 Uiso 1 1 calc R . . H10J H 0.2714 0.6608 0.2819 0.031 Uiso 1 1 calc R . . C105 C 0.3411(7) 0.5610(5) 0.3663(3) 0.029(2) Uani 1 1 d . . . H10E H 0.3947 0.6020 0.3454 0.035 Uiso 1 1 calc R . . H10F H 0.3613 0.5247 0.3499 0.035 Uiso 1 1 calc R . . C106 C 0.3454(7) 0.5305(5) 0.4300(3) 0.027(2) Uani 1 1 d . . . H10K H 0.2868 0.4922 0.4505 0.033 Uiso 1 1 calc R . . H10L H 0.4187 0.5091 0.4354 0.033 Uiso 1 1 calc R . . C107 C -0.0691(8) 0.8181(5) 0.3922(4) 0.038(2) Uani 1 1 d . . . H10O H -0.0876 0.8104 0.4336 0.045 Uiso 1 1 calc R . . H10P H -0.1248 0.8499 0.3725 0.045 Uiso 1 1 calc R . . C108 C 0.0473(7) 0.8546(5) 0.3665(4) 0.035(2) Uani 1 1 d . . . H10Q H 0.0709 0.8576 0.3264 0.042 Uiso 1 1 calc R . . H10R H 0.0457 0.9033 0.3657 0.042 Uiso 1 1 calc R . . C109 C 0.2338(7) 0.8461(5) 0.3764(4) 0.027(2) Uani 1 1 d . . . H10A H 0.2337 0.8963 0.3720 0.032 Uiso 1 1 calc R . . H10B H 0.2575 0.8449 0.3376 0.032 Uiso 1 1 calc R . . C110 C 0.3153(7) 0.8059(4) 0.4152(4) 0.028(2) Uani 1 1 d . . . H11A H 0.3896 0.8310 0.4006 0.033 Uiso 1 1 calc R . . H11B H 0.2882 0.8033 0.4549 0.033 Uiso 1 1 calc R . . C111 C 0.4094(7) 0.7002(5) 0.4459(3) 0.026(2) Uani 1 1 d . . . H11C H 0.3863 0.6900 0.4876 0.031 Uiso 1 1 calc R . . H11D H 0.4796 0.7298 0.4313 0.031 Uiso 1 1 calc R . . C112 C 0.4284(7) 0.6309(5) 0.4371(4) 0.027(2) Uani 1 1 d . . . H11K H 0.4559 0.6422 0.3955 0.033 Uiso 1 1 calc R . . H11L H 0.4876 0.6054 0.4581 0.033 Uiso 1 1 calc R . . C113 C -0.1796(7) 0.7090(5) 0.4240(3) 0.030(2) Uani 1 1 d . . . H11I H -0.1948 0.6708 0.4115 0.036 Uiso 1 1 calc R . . H11J H -0.2433 0.7409 0.4187 0.036 Uiso 1 1 calc R . . C114 C -0.1733(7) 0.6767(5) 0.4868(4) 0.034(2) Uani 1 1 d . . . H11Q H -0.1555 0.7141 0.4996 0.041 Uiso 1 1 calc R . . H11R H -0.2465 0.6537 0.5097 0.041 Uiso 1 1 calc R . . C115 C -0.0804(7) 0.5954(4) 0.5549(3) 0.0236(11) Uani 1 1 d . . . H11M H -0.1541 0.5756 0.5793 0.028 Uiso 1 1 calc R . . H11N H -0.0550 0.6321 0.5666 0.028 Uiso 1 1 calc R . . C116 C 0.0025(7) 0.5371(5) 0.5641(3) 0.027(2) Uani 1 1 d . . . H11O H 0.0051 0.5132 0.6058 0.032 Uiso 1 1 calc R . . H11P H -0.0207 0.5014 0.5508 0.032 Uiso 1 1 calc R . . C117 C 0.1912(7) 0.5143(5) 0.5444(3) 0.029(2) Uani 1 1 d . . . H11G H 0.1794 0.4803 0.5270 0.035 Uiso 1 1 calc R . . H11H H 0.1833 0.4878 0.5867 0.035 Uiso 1 1 calc R . . C118 C 0.3070(7) 0.5486(5) 0.5198(3) 0.026(2) Uani 1 1 d . . . H11E H 0.3168 0.5838 0.5364 0.031 Uiso 1 1 calc R . . H11F H 0.3628 0.5119 0.5316 0.031 Uiso 1 1 calc R . . K2 K 0.64289(13) 0.16494(9) 0.41635(6) 0.0161(4) Uani 1 1 d . . . O21 O 0.8378(4) 0.2402(3) 0.4075(2) 0.0231(13) Uani 1 1 d . . . O22 O 0.6332(4) 0.3124(3) 0.3970(2) 0.0217(12) Uani 1 1 d . . . O23 O 0.6291(4) 0.0653(3) 0.5292(2) 0.0225(13) Uani 1 1 d . . . O24 O 0.4254(4) 0.1190(3) 0.4941(2) 0.0229(13) Uani 1 1 d . . . O25 O 0.7424(5) 0.0796(3) 0.3575(2) 0.0249(13) Uani 1 1 d . . . O26 O 0.5762(4) 0.1777(3) 0.3144(2) 0.0211(12) Uani 1 1 d . . . N21 N 0.8484(6) 0.0870(4) 0.4498(3) 0.0244(16) Uani 1 1 d . . . N22 N 0.4335(5) 0.2429(4) 0.3862(3) 0.0227(16) Uani 1 1 d . . . C201 C 0.9446(7) 0.1350(5) 0.4288(4) 0.035(2) Uani 1 1 d . . . H20Q H 0.9700 0.1457 0.3871 0.042 Uiso 1 1 calc R . . H20R H 1.0057 0.1109 0.4489 0.042 Uiso 1 1 calc R . . C202 C 0.9253(7) 0.2042(5) 0.4367(4) 0.033(2) Uani 1 1 d . . . H20M H 0.9043 0.1947 0.4783 0.039 Uiso 1 1 calc R . . H20N H 0.9949 0.2344 0.4208 0.039 Uiso 1 1 calc R . . C203 C 0.8275(7) 0.3089(4) 0.4077(4) 0.0238(19) Uani 1 1 d . . . H20A H 0.9006 0.3353 0.3917 0.029 Uiso 1 1 calc R . . H20B H 0.8032 0.3058 0.4478 0.029 Uiso 1 1 calc R . . C204 C 0.7413(7) 0.3478(4) 0.3710(3) 0.0233(19) Uani 1 1 d . . . H20C H 0.7378 0.3974 0.3681 0.028 Uiso 1 1 calc R . . H20D H 0.7638 0.3486 0.3316 0.028 Uiso 1 1 calc R . . C205 C 0.5528(7) 0.3512(5) 0.3651(4) 0.032(2) Uani 1 1 d . . . H20O H 0.5741 0.3564 0.3244 0.038 Uiso 1 1 calc R . . H20P H 0.5482 0.3991 0.3659 0.038 Uiso 1 1 calc R . . C206 C 0.4410(8) 0.3115(5) 0.3920(4) 0.036(2) Uani 1 1 d . . . H20I H 0.4249 0.3028 0.4335 0.044 Uiso 1 1 calc R . . H20J H 0.3823 0.3420 0.3739 0.044 Uiso 1 1 calc R . . C207 C 0.8272(7) 0.0520(5) 0.5136(3) 0.031(2) Uani 1 1 d . . . H20E H 0.8353 0.0882 0.5293 0.037 Uiso 1 1 calc R . . H20F H 0.8856 0.0171 0.5251 0.037 Uiso 1 1 calc R . . C208 C 0.7160(8) 0.0150(5) 0.5405(3) 0.035(2) Uani 1 1 d . . . H20K H 0.7059 -0.0209 0.5247 0.041 Uiso 1 1 calc R . . H20L H 0.7116 -0.0097 0.5827 0.041 Uiso 1 1 calc R . . C209 C 0.5231(7) 0.0326(5) 0.5611(3) 0.029(2) Uani 1 1 d . . . H20G H 0.5268 0.0087 0.6026 0.035 Uiso 1 1 calc R . . H20H H 0.5026 -0.0036 0.5476 0.035 Uiso 1 1 calc R . . C210 C 0.4360(7) 0.0879(5) 0.5531(3) 0.026(2) Uani 1 1 d . . . H21G H 0.3633 0.0659 0.5774 0.032 Uiso 1 1 calc R . . H21H H 0.4580 0.1250 0.5653 0.032 Uiso 1 1 calc R . . C211 C 0.3417(7) 0.1689(5) 0.4867(4) 0.034(2) Uani 1 1 d . . . H21Q H 0.3599 0.2060 0.4998 0.041 Uiso 1 1 calc R . . H21R H 0.2690 0.1455 0.5099 0.041 Uiso 1 1 calc R . . C212 C 0.3343(7) 0.2023(5) 0.4228(3) 0.028(2) Uani 1 1 d . . . H21E H 0.3197 0.1643 0.4100 0.033 Uiso 1 1 calc R . . H21F H 0.2699 0.2337 0.4180 0.033 Uiso 1 1 calc R . . C213 C 0.8625(8) 0.0303(5) 0.4258(4) 0.034(2) Uani 1 1 d . . . H21C H 0.8042 -0.0079 0.4479 0.041 Uiso 1 1 calc R . . H21D H 0.9363 0.0093 0.4304 0.041 Uiso 1 1 calc R . . C214 C 0.8539(7) 0.0597(5) 0.3628(4) 0.033(2) Uani 1 1 d . . . H21I H 0.9058 0.1015 0.3411 0.040 Uiso 1 1 calc R . . H21J H 0.8747 0.0235 0.3465 0.040 Uiso 1 1 calc R . . C215 C 0.7316(7) 0.1096(5) 0.2978(3) 0.027(2) Uani 1 1 d . . . H21O H 0.7586 0.0760 0.2795 0.032 Uiso 1 1 calc R . . H21P H 0.7781 0.1541 0.2773 0.032 Uiso 1 1 calc R . . C216 C 0.6142(7) 0.1245(4) 0.2931(3) 0.0223(19) Uani 1 1 d . . . H21A H 0.6065 0.1407 0.2521 0.027 Uiso 1 1 calc R . . H21B H 0.5673 0.0805 0.3154 0.027 Uiso 1 1 calc R . . C217 C 0.4613(7) 0.1916(5) 0.3110(4) 0.030(2) Uani 1 1 d . . . H21K H 0.4135 0.1500 0.3387 0.036 Uiso 1 1 calc R . . H21L H 0.4494 0.2005 0.2717 0.036 Uiso 1 1 calc R . . C218 C 0.4300(7) 0.2556(5) 0.3249(3) 0.026(2) Uani 1 1 d . . . H21M H 0.4820 0.2959 0.2989 0.031 Uiso 1 1 calc R . . H21N H 0.3537 0.2688 0.3176 0.031 Uiso 1 1 calc R . . K3 K 0.24088(13) 0.90902(8) 0.01030(6) 0.0125(3) Uani 1 1 d . . . O31 O 0.3427(4) 0.9839(3) 0.0626(2) 0.0162(11) Uani 1 1 d . . . O32 O 0.3055(4) 1.0527(3) -0.0524(2) 0.0156(9) Uani 1 1 d . . . O33 O 0.0337(4) 0.8678(3) 0.0902(2) 0.0178(12) Uani 1 1 d . . . O34 O 0.0427(4) 0.9049(3) -0.0300(2) 0.0168(10) Uani 1 1 d . . . O35 O 0.3512(4) 0.7807(3) 0.0563(2) 0.0205(12) Uani 1 1 d . . . O36 O 0.3759(4) 0.8563(3) -0.0632(2) 0.0192(12) Uani 1 1 d . . . N31 N 0.2414(5) 0.8452(3) 0.1373(2) 0.0176(14) Uani 1 1 d . . . N32 N 0.2395(5) 0.9744(3) -0.1175(2) 0.0144(14) Uani 1 1 d . . . C301 C 0.3170(7) 0.8853(5) 0.1530(3) 0.025(2) Uani 1 1 d . . . H30I H 0.3946 0.8717 0.1434 0.030 Uiso 1 1 calc R . . H30J H 0.2987 0.8722 0.1953 0.030 Uiso 1 1 calc R . . C302 C 0.3105(7) 0.9638(5) 0.1230(3) 0.026(2) Uani 1 1 d . . . H30K H 0.2332 0.9780 0.1322 0.031 Uiso 1 1 calc R . . H30L H 0.3606 0.9881 0.1366 0.031 Uiso 1 1 calc R . . C303 C 0.3481(7) 1.0601(4) 0.0327(3) 0.0203(18) Uani 1 1 d . . . H30G H 0.4012 1.0812 0.0471 0.024 Uiso 1 1 calc R . . H30H H 0.2735 1.0790 0.0402 0.024 Uiso 1 1 calc R . . C304 C 0.3852(6) 1.0799(4) -0.0306(3) 0.0156(9) Uani 1 1 d . . . H30C H 0.3927 1.1321 -0.0507 0.019 Uiso 1 1 calc R . . H30D H 0.4591 1.0602 -0.0381 0.019 Uiso 1 1 calc R . . C305 C 0.3347(6) 1.0775(4) -0.1135(3) 0.0186(17) Uani 1 1 d . . . H30A H 0.4085 1.0598 -0.1245 0.022 Uiso 1 1 calc R . . H30B H 0.3404 1.1300 -0.1304 0.022 Uiso 1 1 calc R . . C306 C 0.2476(6) 1.0522(4) -0.1366(3) 0.0197(18) Uani 1 1 d . . . H30M H 0.1740 1.0689 -0.1242 0.024 Uiso 1 1 calc R . . H30N H 0.2653 1.0738 -0.1793 0.024 Uiso 1 1 calc R . . C307 C 0.1252(6) 0.8445(5) 0.1693(3) 0.025(2) Uani 1 1 d . . . H30Q H 0.1216 0.8131 0.2104 0.030 Uiso 1 1 calc R . . H30R H 0.1093 0.8930 0.1674 0.030 Uiso 1 1 calc R . . C308 C 0.0356(7) 0.8204(5) 0.1476(3) 0.028(2) Uani 1 1 d . . . H30O H 0.0500 0.7720 0.1488 0.033 Uiso 1 1 calc R . . H30P H -0.0378 0.8189 0.1724 0.033 Uiso 1 1 calc R . . C309 C -0.0507(6) 0.8448(4) 0.0682(3) 0.0156(17) Uani 1 1 d . . . H30E H -0.1236 0.8385 0.0946 0.019 Uiso 1 1 calc R . . H30F H -0.0314 0.7987 0.0656 0.019 Uiso 1 1 calc R . . C310 C -0.0589(6) 0.8987(4) 0.0100(3) 0.0168(10) Uani 1 1 d . . . H31A H -0.1213 0.8849 -0.0038 0.020 Uiso 1 1 calc R . . H31B H -0.0750 0.9452 0.0125 0.020 Uiso 1 1 calc R . . C311 C 0.0317(6) 0.9537(4) -0.0864(3) 0.0205(18) Uani 1 1 d . . . H31C H 0.0205 1.0018 -0.0865 0.025 Uiso 1 1 calc R . . H31D H -0.0345 0.9396 -0.0975 0.025 Uiso 1 1 calc R . . C312 C 0.1348(6) 0.9546(4) -0.1292(3) 0.0227(19) Uani 1 1 d . . . H31Q H 0.1419 0.9069 -0.1303 0.027 Uiso 1 1 calc R . . H31R H 0.1250 0.9882 -0.1680 0.027 Uiso 1 1 calc R . . C313 C 0.2776(7) 0.7709(5) 0.1526(3) 0.029(2) Uani 1 1 d . . . H31I H 0.2153 0.7413 0.1525 0.035 Uiso 1 1 calc R . . H31J H 0.2930 0.7525 0.1924 0.035 Uiso 1 1 calc R . . C314 C 0.3795(7) 0.7629(4) 0.1128(3) 0.0242(19) Uani 1 1 d . . . H31O H 0.4412 0.7950 0.1099 0.029 Uiso 1 1 calc R . . H31P H 0.4042 0.7136 0.1278 0.029 Uiso 1 1 calc R . . C315 C 0.4474(7) 0.7749(4) 0.0165(3) 0.0216(18) Uani 1 1 d . . . H31E H 0.4786 0.7274 0.0327 0.026 Uiso 1 1 calc R . . H31F H 0.5058 0.8110 0.0102 0.026 Uiso 1 1 calc R . . C316 C 0.4143(7) 0.7858(4) -0.0394(3) 0.025(2) Uani 1 1 d . . . H31M H 0.4791 0.7793 -0.0664 0.031 Uiso 1 1 calc R . . H31N H 0.3541 0.7509 -0.0331 0.031 Uiso 1 1 calc R . . C317 C 0.3536(7) 0.8727(4) -0.1205(3) 0.0220(19) Uani 1 1 d . . . H31K H 0.2860 0.8455 -0.1180 0.026 Uiso 1 1 calc R . . H31L H 0.4174 0.8593 -0.1440 0.026 Uiso 1 1 calc R . . C318 C 0.3364(6) 0.9502(4) -0.1482(3) 0.0198(18) Uani 1 1 d . . . H31G H 0.4046 0.9766 -0.1503 0.024 Uiso 1 1 calc R . . H31H H 0.3260 0.9618 -0.1883 0.024 Uiso 1 1 calc R . . K4 K 0.73792(13) 0.41083(8) 0.02568(6) 0.0138(4) Uani 1 1 d . . . O41 O 0.8192(4) 0.5470(3) -0.0534(2) 0.0233(10) Uani 1 1 d . . . O42 O 0.8390(4) 0.5027(3) 0.0631(2) 0.0259(11) Uani 1 1 d . . . O43 O 0.5564(4) 0.3948(3) -0.0203(2) 0.0190(10) Uani 1 1 d . . . O44 O 0.5100(4) 0.3984(3) 0.0910(2) 0.0182(12) Uani 1 1 d . . . O45 O 0.8922(4) 0.3340(3) -0.0205(2) 0.0195(12) Uani 1 1 d . . . O46 O 0.8149(4) 0.2827(3) 0.0987(2) 0.0215(13) Uani 1 1 d . . . N41 N 0.7721(5) 0.4437(3) -0.0993(2) 0.0197(15) Uani 1 1 d . . . N42 N 0.7031(5) 0.3778(4) 0.1494(3) 0.0234(16) Uani 1 1 d . . . C401 C 0.7766(7) 0.5202(4) -0.1303(3) 0.026(2) Uani 1 1 d . . . H40Q H 0.7002 0.5375 -0.1246 0.032 Uiso 1 1 calc R . . H40R H 0.8006 0.5312 -0.1721 0.032 Uiso 1 1 calc R . . C402 C 0.8546(7) 0.5608(4) -0.1125(3) 0.0250(19) Uani 1 1 d . . . H40I H 0.9322 0.5457 -0.1194 0.030 Uiso 1 1 calc R . . H40J H 0.8531 0.6123 -0.1357 0.030 Uiso 1 1 calc R . . C403 C 0.8947(6) 0.5823(4) -0.0356(3) 0.0233(10) Uani 1 1 d . . . H40G H 0.9027 0.6332 -0.0614 0.028 Uiso 1 1 calc R . . H40H H 0.9693 0.5617 -0.0384 0.028 Uiso 1 1 calc R . . C404 C 0.8520(7) 0.5746(5) 0.0252(4) 0.0259(11) Uani 1 1 d . . . H40C H 0.9050 0.5991 0.0371 0.031 Uiso 1 1 calc R . . H40D H 0.7791 0.5973 0.0274 0.031 Uiso 1 1 calc R . . C405 C 0.7995(7) 0.4949(5) 0.1216(4) 0.036(2) Uani 1 1 d . . . H40M H 0.7272 0.5181 0.1244 0.043 Uiso 1 1 calc R . . H40N H 0.8537 0.5186 0.1335 0.043 Uiso 1 1 calc R . . C406 C 0.7848(7) 0.4187(5) 0.1610(4) 0.035(2) Uani 1 1 d . . . H40K H 0.8580 0.3965 0.1585 0.042 Uiso 1 1 calc R . . H40L H 0.7615 0.4155 0.2011 0.042 Uiso 1 1 calc R . . C407 C 0.6789(7) 0.4104(4) -0.1093(3) 0.0233(19) Uani 1 1 d . . . H40O H 0.6883 0.3586 -0.0946 0.028 Uiso 1 1 calc R . . H40P H 0.6818 0.4276 -0.1515 0.028 Uiso 1 1 calc R . . C408 C 0.5658(7) 0.4244(4) -0.0815(3) 0.0239(19) Uani 1 1 d . . . H40E H 0.5555 0.4761 -0.0952 0.029 Uiso 1 1 calc R . . H40F H 0.5070 0.4029 -0.0924 0.029 Uiso 1 1 calc R . . C409 C 0.4451(6) 0.4011(4) 0.0085(3) 0.0190(10) Uani 1 1 d . . . H40A H 0.3896 0.3797 -0.0045 0.023 Uiso 1 1 calc R . . H40B H 0.4290 0.4518 -0.0016 0.023 Uiso 1 1 calc R . . C410 C 0.4362(6) 0.3648(4) 0.0715(3) 0.0208(18) Uani 1 1 d . . . H41A H 0.3584 0.3660 0.0910 0.025 Uiso 1 1 calc R . . H41B H 0.4552 0.3145 0.0814 0.025 Uiso 1 1 calc R . . C411 C 0.4970(7) 0.3700(5) 0.1523(3) 0.026(2) Uani 1 1 d . . . H41I H 0.4985 0.3176 0.1672 0.031 Uiso 1 1 calc R . . H41J H 0.4239 0.3830 0.1692 0.031 Uiso 1 1 calc R . . C412 C 0.5885(6) 0.3982(5) 0.1696(3) 0.027(2) Uani 1 1 d . . . H41O H 0.5746 0.3808 0.2123 0.033 Uiso 1 1 calc R . . H41P H 0.5864 0.4505 0.1541 0.033 Uiso 1 1 calc R . . C413 C 0.8779(7) 0.4150(5) -0.1168(3) 0.029(2) Uani 1 1 d . . . H41M H 0.9402 0.4449 -0.1172 0.035 Uiso 1 1 calc R . . H41N H 0.8823 0.4181 -0.1567 0.035 Uiso 1 1 calc R . . C414 C 0.8938(7) 0.3382(4) -0.0780(3) 0.028(2) Uani 1 1 d . . . H41E H 0.8331 0.3072 -0.0777 0.034 Uiso 1 1 calc R . . H41F H 0.9660 0.3221 -0.0928 0.034 Uiso 1 1 calc R . . C415 C 0.9104(7) 0.2631(4) 0.0163(3) 0.0233(19) Uani 1 1 d . . . H41C H 0.9808 0.2468 -0.0004 0.028 Uiso 1 1 calc R . . H41D H 0.8483 0.2312 0.0194 0.028 Uiso 1 1 calc R . . C416 C 0.9174(6) 0.2596(4) 0.0746(3) 0.0216(18) Uani 1 1 d . . . H41G H 0.9304 0.2104 0.1000 0.026 Uiso 1 1 calc R . . H41H H 0.9809 0.2904 0.0718 0.026 Uiso 1 1 calc R . . C417 C 0.8159(8) 0.2728(5) 0.1564(3) 0.041(3) Uani 1 1 d . . . H41K H 0.8835 0.2971 0.1578 0.049 Uiso 1 1 calc R . . H41L H 0.8192 0.2216 0.1800 0.049 Uiso 1 1 calc R . . C418 C 0.7139(8) 0.3015(5) 0.1813(3) 0.035(2) Uani 1 1 d . . . H41Q H 0.6468 0.2756 0.1814 0.042 Uiso 1 1 calc R . . H41R H 0.7166 0.2927 0.2219 0.042 Uiso 1 1 calc R . . N1S N 0.4228(6) 0.0459(4) 0.6908(3) 0.0294(17) Uani 1 1 d . . . C1S C 0.3689(7) 0.1044(5) 0.6881(4) 0.029(2) Uani 1 1 d . . . H1S H 0.3034 0.1133 0.6716 0.035 Uiso 1 1 calc R . . C2S C 0.4020(7) 0.1532(5) 0.7077(4) 0.030(2) Uani 1 1 d . . . H2S H 0.3616 0.1948 0.7041 0.036 Uiso 1 1 calc R . . C3S C 0.4966(7) 0.1393(5) 0.7329(4) 0.029(2) Uani 1 1 d . . . H3S H 0.5232 0.1714 0.7467 0.035 Uiso 1 1 calc R . . C4S C 0.5505(7) 0.0781(4) 0.7373(3) 0.0227(19) Uani 1 1 d . . . H4S H 0.6144 0.0667 0.7550 0.027 Uiso 1 1 calc R . . C5S C 0.5118(7) 0.0329(4) 0.7159(3) 0.0200(18) Uani 1 1 d . . . H5S H 0.5503 -0.0093 0.7194 0.024 Uiso 1 1 calc R . . N1T N 0.1570(9) 0.4021(7) 0.3016(4) 0.080(4) Uani 1 1 d . . . C1T C 0.1131(9) 0.3483(5) 0.2872(4) 0.041(3) Uani 1 1 d . . . H1T H 0.1482 0.3045 0.2929 0.049 Uiso 1 1 calc R . . C2T C 0.0172(9) 0.3646(5) 0.2649(4) 0.038(2) Uani 1 1 d . . . H2T H -0.0148 0.3323 0.2530 0.046 Uiso 1 1 calc R . . C3T C -0.0320(7) 0.4262(5) 0.2597(3) 0.028(2) Uani 1 1 d . . . H3T H -0.0992 0.4375 0.2449 0.033 Uiso 1 1 calc R . . C4T C 0.0171(8) 0.4727(5) 0.2763(3) 0.030(2) Uani 1 1 d . . . H4T H -0.0177 0.5162 0.2723 0.035 Uiso 1 1 calc R . . C5T C 0.1069(8) 0.4601(5) 0.2970(4) 0.028(2) Uani 1 1 d . . . H5T H 0.1366 0.4932 0.3088 0.033 Uiso 1 1 calc R . . Tl1 Tl 0.70400(3) 0.69977(2) 0.105535(15) 0.04264(15) Uani 1 1 d . . . P11 P 0.7082(2) 0.55079(12) 0.23817(9) 0.0294(6) Uani 1 1 d . . . P12 P 0.83402(17) 0.63857(13) 0.19173(9) 0.0257(5) Uani 1 1 d . . . P13 P 0.56001(19) 0.60073(13) 0.20500(10) 0.0287(5) Uani 1 1 d . . . P14 P 0.6777(2) 0.55158(12) 0.32335(9) 0.0302(6) Uani 1 1 d . . . P15 P 0.74772(18) 0.72045(11) 0.21418(9) 0.0225(5) Uani 1 1 d . . . P16 P 0.55997(18) 0.69430(12) 0.22413(9) 0.0251(5) Uani 1 1 d . . . P17 P 0.64469(18) 0.66123(11) 0.30095(8) 0.0203(5) Uani 1 1 d . . . Tl2 Tl 0.20953(3) 0.19986(2) 0.098031(16) 0.04464(15) Uani 1 1 d . . . P21 P 0.1944(2) 0.04821(13) 0.23100(10) 0.0378(7) Uani 1 1 d . . . P22 P 0.3332(2) 0.1244(2) 0.18211(11) 0.0589(10) Uani 1 1 d . . . P23 P 0.05524(19) 0.11168(14) 0.19942(10) 0.0326(6) Uani 1 1 d . . . P24 P 0.1797(2) 0.04948(12) 0.31582(9) 0.0310(6) Uani 1 1 d . . . P25 P 0.2758(3) 0.21230(16) 0.20494(10) 0.0533(8) Uani 1 1 d . . . P26 P 0.0821(2) 0.20300(13) 0.21727(10) 0.0343(6) Uani 1 1 d . . . P27 P 0.1709(2) 0.16049(12) 0.29284(9) 0.0298(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 K1 0.0175(9) 0.0152(9) 0.0151(8) -0.0043(7) -0.0006(7) -0.0040(8) O11 0.013(3) 0.023(3) 0.023(3) -0.008(2) -0.010(2) -0.003(2) O12 0.027(3) 0.023(3) 0.010(2) -0.006(2) 0.002(2) 0.001(3) O13 0.020(3) 0.015(3) 0.031(3) -0.004(3) 0.001(3) -0.003(3) O14 0.017(3) 0.023(3) 0.031(3) -0.015(3) -0.004(2) -0.002(3) O15 0.018(3) 0.031(4) 0.017(3) -0.008(3) 0.003(2) 0.002(3) O16 0.023(3) 0.027(3) 0.014(2) -0.004(2) 0.004(2) -0.006(2) N11 0.018(4) 0.028(4) 0.024(4) -0.006(3) -0.001(3) -0.001(3) N12 0.020(4) 0.022(4) 0.008(3) -0.002(3) 0.002(3) 0.001(3) C101 0.025(5) 0.038(6) 0.023(4) -0.006(4) -0.007(4) 0.001(4) C102 0.020(5) 0.051(6) 0.022(4) -0.015(4) -0.008(4) -0.007(4) C103 0.040(5) 0.033(5) 0.012(4) -0.012(4) -0.004(4) -0.007(4) C104 0.035(5) 0.028(5) 0.009(4) -0.003(3) -0.001(4) 0.005(4) C105 0.024(5) 0.039(6) 0.029(5) -0.019(4) -0.006(4) 0.008(4) C106 0.034(5) 0.030(5) 0.024(4) -0.013(4) -0.016(4) 0.011(4) C107 0.030(6) 0.029(6) 0.054(6) -0.015(5) -0.009(5) 0.006(5) C108 0.033(6) 0.022(5) 0.048(6) -0.007(4) -0.016(5) 0.006(4) C109 0.022(5) 0.020(5) 0.035(5) -0.007(4) -0.004(4) -0.012(4) C110 0.022(5) 0.020(5) 0.040(5) -0.012(4) -0.003(4) -0.008(4) C111 0.014(4) 0.032(5) 0.025(4) -0.002(4) -0.006(4) -0.010(4) C112 0.017(5) 0.035(6) 0.025(4) -0.007(4) -0.002(4) 0.002(4) C113 0.017(5) 0.032(6) 0.031(5) -0.004(4) 0.001(4) 0.001(4) C114 0.025(5) 0.035(6) 0.036(5) -0.015(4) 0.014(4) -0.014(5) C115 0.023(3) 0.027(3) 0.014(2) -0.004(2) 0.004(2) -0.006(2) C116 0.030(5) 0.027(5) 0.015(4) 0.000(4) 0.000(4) -0.010(4) C117 0.039(6) 0.029(5) 0.014(4) -0.002(4) -0.008(4) -0.002(5) C118 0.028(5) 0.027(5) 0.018(4) -0.003(4) -0.007(4) -0.001(4) K2 0.0168(9) 0.0159(9) 0.0143(8) -0.0048(7) -0.0020(7) -0.0008(7) O21 0.021(3) 0.021(3) 0.031(3) -0.011(3) -0.011(3) 0.000(3) O22 0.019(3) 0.016(3) 0.024(3) -0.004(2) 0.002(2) -0.001(3) O23 0.025(3) 0.018(3) 0.020(3) -0.002(2) -0.008(3) 0.001(3) O24 0.020(3) 0.028(3) 0.019(3) -0.009(3) 0.002(2) -0.003(3) O25 0.031(3) 0.028(4) 0.021(3) -0.014(3) -0.009(3) 0.009(3) O26 0.020(3) 0.022(3) 0.023(3) -0.010(2) -0.006(2) -0.001(3) N21 0.029(4) 0.025(4) 0.023(4) -0.014(3) -0.005(3) 0.006(4) N22 0.019(4) 0.022(4) 0.024(4) -0.007(3) -0.004(3) 0.005(3) C201 0.018(5) 0.048(7) 0.042(5) -0.022(5) -0.003(4) 0.009(5) C202 0.025(5) 0.036(6) 0.038(5) -0.012(4) -0.008(4) -0.005(4) C203 0.022(5) 0.017(5) 0.032(4) -0.009(4) -0.004(4) -0.006(4) C204 0.028(5) 0.017(5) 0.023(4) -0.006(4) -0.004(4) -0.002(4) C205 0.030(5) 0.021(5) 0.042(5) -0.010(4) -0.009(4) 0.003(4) C206 0.035(6) 0.031(6) 0.049(6) -0.020(5) -0.017(5) 0.019(5) C207 0.035(5) 0.033(6) 0.028(5) -0.010(4) -0.021(4) 0.014(5) C208 0.046(6) 0.036(6) 0.017(4) -0.006(4) -0.003(4) -0.005(5) C209 0.038(6) 0.027(5) 0.017(4) -0.006(4) 0.001(4) -0.011(5) C210 0.028(5) 0.038(6) 0.015(4) -0.015(4) 0.003(4) -0.007(4) C211 0.022(5) 0.041(6) 0.038(5) -0.019(5) 0.012(4) -0.009(5) C212 0.022(5) 0.027(5) 0.032(5) -0.009(4) -0.007(4) 0.004(4) C213 0.039(6) 0.027(5) 0.041(5) -0.017(4) -0.017(4) 0.023(5) C214 0.030(5) 0.042(6) 0.035(5) -0.023(5) -0.006(4) 0.013(5) C215 0.038(5) 0.024(5) 0.016(4) -0.008(4) -0.001(4) 0.004(4) C216 0.033(5) 0.021(5) 0.016(4) -0.010(4) -0.007(4) -0.001(4) C217 0.018(5) 0.044(6) 0.029(5) -0.014(4) -0.008(4) -0.003(4) C218 0.027(5) 0.032(5) 0.021(4) -0.011(4) -0.010(4) 0.006(4) K3 0.0110(8) 0.0115(9) 0.0134(7) -0.0040(7) -0.0003(6) -0.0017(7) O31 0.020(3) 0.012(3) 0.017(3) -0.006(2) -0.004(2) 0.000(2) O32 0.012(2) 0.013(2) 0.019(2) -0.0038(18) -0.0006(18) -0.0069(19) O33 0.015(3) 0.018(3) 0.015(3) -0.001(2) 0.000(2) -0.007(2) O34 0.007(2) 0.022(3) 0.020(2) -0.009(2) 0.0028(17) 0.0013(19) O35 0.020(3) 0.018(3) 0.020(3) -0.003(2) -0.006(2) 0.005(3) O36 0.027(3) 0.012(3) 0.018(3) -0.008(2) -0.001(2) 0.004(3) N31 0.018(4) 0.014(4) 0.014(3) 0.001(3) -0.001(3) -0.010(3) N32 0.016(3) 0.014(4) 0.014(3) -0.006(3) -0.002(3) -0.005(3) C301 0.026(5) 0.038(6) 0.017(4) -0.012(4) -0.009(4) 0.001(4) C302 0.027(5) 0.028(5) 0.023(4) -0.015(4) 0.004(4) -0.005(4) C303 0.026(5) 0.015(5) 0.025(4) -0.008(4) -0.016(4) -0.003(4) C304 0.012(2) 0.013(2) 0.019(2) -0.0038(18) -0.0006(18) -0.0069(19) C305 0.023(4) 0.018(5) 0.012(4) -0.004(3) 0.003(3) -0.008(4) C306 0.016(4) 0.023(5) 0.016(4) -0.002(3) -0.005(3) -0.006(4) C307 0.019(5) 0.031(5) 0.016(4) -0.002(4) 0.007(3) -0.015(4) C308 0.019(5) 0.031(5) 0.021(4) -0.003(4) 0.009(4) -0.007(4) C309 0.012(4) 0.016(4) 0.017(4) -0.010(3) 0.008(3) -0.005(3) C310 0.007(2) 0.022(3) 0.020(2) -0.009(2) 0.0028(17) 0.0013(19) C311 0.021(4) 0.026(5) 0.013(4) -0.005(3) -0.006(3) 0.003(4) C312 0.029(5) 0.021(5) 0.018(4) -0.009(4) 0.000(4) 0.001(4) C313 0.034(5) 0.029(5) 0.014(4) 0.005(4) -0.010(4) -0.011(4) C314 0.024(5) 0.017(5) 0.031(5) -0.004(4) -0.012(4) -0.001(4) C315 0.023(5) 0.005(4) 0.033(5) -0.003(3) -0.008(4) 0.004(4) C316 0.026(5) 0.024(5) 0.030(4) -0.018(4) -0.001(4) 0.010(4) C317 0.015(4) 0.027(5) 0.027(4) -0.016(4) 0.003(4) -0.004(4) C318 0.020(4) 0.027(5) 0.010(4) -0.006(3) 0.002(3) -0.007(4) K4 0.0111(8) 0.0117(9) 0.0179(8) -0.0055(7) -0.0016(7) 0.0006(7) O41 0.016(2) 0.018(3) 0.032(3) -0.006(2) 0.000(2) -0.008(2) O42 0.016(2) 0.026(3) 0.042(3) -0.019(2) -0.006(2) -0.002(2) O43 0.012(2) 0.018(3) 0.028(2) -0.011(2) -0.0031(19) 0.003(2) O44 0.014(3) 0.014(3) 0.021(3) -0.003(2) 0.002(2) -0.010(2) O45 0.024(3) 0.007(3) 0.022(3) -0.002(2) 0.001(2) 0.005(2) O46 0.019(3) 0.024(3) 0.023(3) -0.010(3) -0.009(2) 0.007(3) N41 0.025(4) 0.013(4) 0.016(3) -0.004(3) 0.005(3) 0.002(3) N42 0.023(4) 0.024(4) 0.021(3) -0.007(3) -0.004(3) 0.004(3) C401 0.035(5) 0.017(5) 0.024(4) -0.009(4) 0.004(4) -0.001(4) C402 0.019(5) 0.016(5) 0.030(5) -0.005(4) 0.011(4) -0.009(4) C403 0.016(2) 0.018(3) 0.032(3) -0.006(2) 0.000(2) -0.008(2) C404 0.016(2) 0.026(3) 0.042(3) -0.019(2) -0.006(2) -0.002(2) C405 0.024(5) 0.052(7) 0.046(6) -0.033(5) -0.003(4) -0.014(5) C406 0.030(5) 0.055(7) 0.027(5) -0.022(5) -0.009(4) 0.000(5) C407 0.031(5) 0.017(5) 0.022(4) -0.008(4) -0.007(4) -0.001(4) C408 0.031(5) 0.020(5) 0.025(4) -0.009(4) -0.016(4) 0.002(4) C409 0.012(2) 0.018(3) 0.028(2) -0.011(2) -0.0031(19) 0.003(2) C410 0.010(4) 0.021(5) 0.037(5) -0.020(4) 0.003(4) -0.003(4) C411 0.020(5) 0.023(5) 0.023(4) 0.001(4) -0.001(4) 0.003(4) C412 0.021(5) 0.032(5) 0.016(4) 0.000(4) 0.005(4) 0.004(4) C413 0.035(5) 0.023(5) 0.018(4) -0.002(4) 0.009(4) 0.000(4) C414 0.031(5) 0.018(5) 0.027(4) -0.005(4) 0.006(4) 0.003(4) C415 0.018(5) 0.016(5) 0.034(5) -0.012(4) 0.006(4) -0.002(4) C416 0.016(4) 0.012(4) 0.037(5) -0.009(4) -0.009(4) 0.002(4) C417 0.061(7) 0.034(6) 0.024(5) -0.005(4) -0.019(5) 0.026(5) C418 0.047(6) 0.036(6) 0.012(4) -0.001(4) -0.003(4) 0.021(5) N1S 0.034(4) 0.034(5) 0.028(4) -0.019(4) -0.011(3) 0.003(4) C1S 0.024(5) 0.041(6) 0.029(5) -0.019(4) -0.011(4) 0.008(5) C2S 0.033(5) 0.027(5) 0.030(5) -0.015(4) 0.003(4) 0.009(4) C3S 0.037(5) 0.025(5) 0.031(5) -0.015(4) -0.007(4) -0.002(4) C4S 0.022(5) 0.027(5) 0.019(4) -0.009(4) -0.003(4) -0.001(4) C5S 0.031(5) 0.010(4) 0.013(4) 0.000(3) -0.001(4) 0.003(4) N1T 0.075(8) 0.133(11) 0.047(6) -0.047(7) -0.013(5) -0.008(8) C1T 0.065(7) 0.025(6) 0.019(4) 0.000(4) 0.002(5) 0.021(5) C2T 0.055(7) 0.024(6) 0.032(5) -0.012(4) 0.008(5) -0.016(5) C3T 0.032(5) 0.032(6) 0.020(4) -0.011(4) -0.003(4) -0.001(4) C4T 0.045(6) 0.026(5) 0.019(4) -0.008(4) -0.008(4) -0.006(5) C5T 0.040(6) 0.019(5) 0.038(5) -0.022(4) -0.018(5) 0.007(4) Tl1 0.0484(3) 0.0471(3) 0.0310(2) -0.01227(19) -0.01144(18) 0.0058(2) P11 0.0409(15) 0.0213(13) 0.0285(12) -0.0133(10) -0.0063(11) 0.0092(11) P12 0.0169(12) 0.0347(14) 0.0223(11) -0.0105(10) 0.0021(9) 0.0050(11) P13 0.0282(13) 0.0330(15) 0.0294(12) -0.0138(11) -0.0107(10) -0.0079(11) P14 0.0452(15) 0.0223(13) 0.0200(11) -0.0046(10) -0.0078(11) 0.0041(12) P15 0.0250(12) 0.0191(12) 0.0201(10) -0.0043(9) -0.0031(9) -0.0056(10) P16 0.0187(12) 0.0264(13) 0.0294(12) -0.0096(10) -0.0073(10) 0.0096(10) P17 0.0248(12) 0.0203(12) 0.0166(10) -0.0095(9) 0.0005(9) -0.0028(10) Tl2 0.0459(3) 0.0516(3) 0.0333(2) -0.01219(19) -0.01085(19) 0.0085(2) P21 0.0621(18) 0.0239(14) 0.0273(12) -0.0130(11) -0.0053(12) 0.0213(13) P22 0.0186(14) 0.106(3) 0.0276(13) -0.0060(15) 0.0058(11) 0.0124(16) P23 0.0254(13) 0.0433(16) 0.0379(13) -0.0223(12) -0.0111(11) -0.0053(12) P24 0.0440(15) 0.0244(14) 0.0180(11) -0.0016(10) -0.0064(10) 0.0090(12) P25 0.068(2) 0.0523(19) 0.0252(13) 0.0082(12) -0.0170(13) -0.0447(16) P26 0.0415(15) 0.0307(15) 0.0410(14) -0.0199(12) -0.0231(12) 0.0222(12) P27 0.0409(15) 0.0255(14) 0.0269(12) -0.0108(10) -0.0132(11) -0.0054(11) _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 K1 O14 2.782(5) . ? K1 O11 2.787(5) . ? K1 O16 2.788(5) . ? K1 O12 2.840(5) . ? K1 O13 2.862(6) . ? K1 O15 2.940(5) . ? K1 N12 3.002(6) . ? K1 N11 3.047(7) . ? O11 C102 1.429(9) . ? O11 C103 1.431(9) . ? O12 C105 1.424(9) . ? O12 C104 1.436(8) . ? O13 C108 1.421(9) . ? O13 C109 1.432(10) . ? O14 C110 1.403(9) . ? O14 C111 1.431(9) . ? O15 C114 1.394(10) . ? O15 C115 1.420(9) . ? O16 C116 1.419(10) . ? O16 C117 1.424(10) . ? N11 C113 1.463(11) . ? N11 C107 1.477(11) . ? N11 C101 1.504(10) . ? N12 C112 1.457(11) . ? N12 C118 1.470(9) . ? N12 C106 1.493(10) . ? C101 C102 1.492(12) . ? C101 H10G 0.9900 . ? C101 H10H 0.9900 . ? C102 H10M 0.9900 . ? C102 H10N 0.9900 . ? C103 C104 1.484(11) . ? C103 H10C 0.9900 . ? C103 H10D 0.9900 . ? C104 H10I 0.9900 . ? C104 H10J 0.9900 . ? C105 C106 1.513(11) . ? C105 H10E 0.9900 . ? C105 H10F 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.533(13) . ? C107 H10O 0.9900 . ? C107 H10P 0.9900 . ? C108 H10Q 0.9900 . ? C108 H10R 0.9900 . ? C109 C110 1.523(11) . ? C109 H10A 0.9900 . ? C109 H10B 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.527(12) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11K 0.9900 . ? C112 H11L 0.9900 . ? C113 C114 1.498(12) . ? C113 H11I 0.9900 . ? C113 H11J 0.9900 . ? C114 H11Q 0.9900 . ? C114 H11R 0.9900 . ? C115 C116 1.511(11) . ? C115 H11M 0.9900 . ? C115 H11N 0.9900 . ? C116 H11O 0.9900 . ? C116 H11P 0.9900 . ? C117 C118 1.509(12) . ? C117 H11G 0.9900 . ? C117 H11H 0.9900 . ? C118 H11E 0.9900 . ? C118 H11F 0.9900 . ? K2 O23 2.789(5) . ? K2 O26 2.790(5) . ? K2 O21 2.804(6) . ? K2 O25 2.832(5) . ? K2 O22 2.868(5) . ? K2 O24 2.937(5) . ? K2 N21 2.999(7) . ? K2 N22 3.022(6) . ? O21 C203 1.413(9) . ? O21 C202 1.430(9) . ? O22 C205 1.411(9) . ? O22 C204 1.439(10) . ? O23 C209 1.424(10) . ? O23 C208 1.439(10) . ? O24 C211 1.402(10) . ? O24 C210 1.420(9) . ? O25 C214 1.419(9) . ? O25 C215 1.439(9) . ? O26 C216 1.428(9) . ? O26 C217 1.430(9) . ? N21 C201 1.439(11) . ? N21 C207 1.479(10) . ? N21 C213 1.504(10) . ? N22 C212 1.440(11) . ? N22 C206 1.477(11) . ? N22 C218 1.495(9) . ? C201 C202 1.515(12) . ? C201 H20Q 0.9900 . ? C201 H20R 0.9900 . ? C202 H20M 0.9900 . ? C202 H20N 0.9900 . ? C203 C204 1.530(11) . ? C203 H20A 0.9900 . ? C203 H20B 0.9900 . ? C204 H20C 0.9900 . ? C204 H20D 0.9900 . ? C205 C206 1.512(13) . ? C205 H20O 0.9900 . ? C205 H20P 0.9900 . ? C206 H20I 0.9900 . ? C206 H20J 0.9900 . ? C207 C208 1.484(13) . ? C207 H20E 0.9900 . ? C207 H20F 0.9900 . ? C208 H20K 0.9900 . ? C208 H20L 0.9900 . ? C209 C210 1.505(12) . ? C209 H20G 0.9900 . ? C209 H20H 0.9900 . ? C210 H21G 0.9900 . ? C210 H21H 0.9900 . ? C211 C212 1.527(12) . ? C211 H21Q 0.9900 . ? C211 H21R 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.509(12) . ? C213 H21C 0.9900 . ? C213 H21D 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.470(11) . ? C215 H21O 0.9900 . ? C215 H21P 0.9900 . ? C216 H21A 0.9900 . ? C216 H21B 0.9900 . ? C217 C218 1.507(12) . ? C217 H21K 0.9900 . ? C217 H21L 0.9900 . ? C218 H21M 0.9900 . ? C218 H21N 0.9900 . ? K3 O36 2.779(5) . ? K3 O32 2.806(5) . ? K3 O34 2.814(5) . ? K3 O35 2.833(5) . ? K3 O31 2.840(5) . ? K3 O33 2.855(5) . ? K3 N31 2.996(6) . ? K3 N32 3.017(6) . ? O31 C302 1.415(9) . ? O31 C303 1.443(9) . ? O32 C305 1.419(8) . ? O32 C304 1.432(8) . ? O33 C308 1.414(9) . ? O33 C309 1.436(8) . ? O34 C310 1.426(8) . ? O34 C311 1.429(8) . ? O35 C315 1.438(9) . ? O35 C314 1.452(9) . ? O36 C316 1.431(9) . ? O36 C317 1.448(9) . ? N31 C301 1.461(10) . ? N31 C313 1.490(10) . ? N31 C307 1.495(10) . ? N32 C312 1.469(9) . ? N32 C318 1.475(9) . ? N32 C306 1.475(10) . ? C301 C302 1.494(12) . ? C301 H30I 0.9900 . ? C301 H30J 0.9900 . ? C302 H30K 0.9900 . ? C302 H30L 0.9900 . ? C303 C304 1.491(10) . ? C303 H30G 0.9900 . ? C303 H30H 0.9900 . ? C304 H30C 0.9900 . ? C304 H30D 0.9900 . ? C305 C306 1.505(10) . ? C305 H30A 0.9900 . ? C305 H30B 0.9900 . ? C306 H30M 0.9900 . ? C306 H30N 0.9900 . ? C307 C308 1.492(11) . ? C307 H30Q 0.9900 . ? C307 H30R 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 C310 1.486(10) . ? C309 H30E 0.9900 . ? C309 H30F 0.9900 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C312 1.501(10) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 H31Q 0.9900 . ? C312 H31R 0.9900 . ? C313 C314 1.500(11) . ? C313 H31I 0.9900 . ? C313 H31J 0.9900 . ? C314 H31O 0.9900 . ? C314 H31P 0.9900 . ? C315 C316 1.491(10) . ? C315 H31E 0.9900 . ? C315 H31F 0.9900 . ? C316 H31M 0.9900 . ? C316 H31N 0.9900 . ? C317 C318 1.491(11) . ? C317 H31K 0.9900 . ? C317 H31L 0.9900 . ? C318 H31G 0.9900 . ? C318 H31H 0.9900 . ? K4 O43 2.777(5) . ? K4 O45 2.798(5) . ? K4 O41 2.812(6) . ? K4 O46 2.813(5) . ? K4 O42 2.829(5) . ? K4 N42 2.918(6) . ? K4 O44 2.926(5) . ? K4 N41 2.952(6) . ? O41 C402 1.409(9) . ? O41 C403 1.430(9) . ? O42 C404 1.408(10) . ? O42 C405 1.432(10) . ? O43 C408 1.427(9) . ? O43 C409 1.444(9) . ? O44 C410 1.421(8) . ? O44 C411 1.423(9) . ? O45 C415 1.427(9) . ? O45 C414 1.436(9) . ? O46 C417 1.414(9) . ? O46 C416 1.437(9) . ? N41 C401 1.452(10) . ? N41 C407 1.457(10) . ? N41 C413 1.463(10) . ? N42 C406 1.466(11) . ? N42 C418 1.470(11) . ? N42 C412 1.499(10) . ? C401 C402 1.523(11) . ? C401 H40Q 0.9900 . ? C401 H40R 0.9900 . ? C402 H40I 0.9900 . ? C402 H40J 0.9900 . ? C403 C404 1.493(11) . ? C403 H40G 0.9900 . ? C403 H40H 0.9900 . ? C404 H40C 0.9900 . ? C404 H40D 0.9900 . ? C405 C406 1.487(13) . ? C405 H40M 0.9900 . ? C405 H40N 0.9900 . ? C406 H40K 0.9900 . ? C406 H40L 0.9900 . ? C407 C408 1.500(11) . ? C407 H40O 0.9900 . ? C407 H40P 0.9900 . ? C408 H40E 0.9900 . ? C408 H40F 0.9900 . ? C409 C410 1.473(11) . ? C409 H40A 0.9900 . ? C409 H40B 0.9900 . ? C410 H41A 0.9900 . ? C410 H41B 0.9900 . ? C411 C412 1.485(11) . ? C411 H41I 0.9900 . ? C411 H41J 0.9900 . ? C412 H41O 0.9900 . ? C412 H41P 0.9900 . ? C413 C414 1.525(11) . ? C413 H41M 0.9900 . ? C413 H41N 0.9900 . ? C414 H41E 0.9900 . ? C414 H41F 0.9900 . ? C415 C416 1.485(10) . ? C415 H41C 0.9900 . ? C415 H41D 0.9900 . ? C416 H41G 0.9900 . ? C416 H41H 0.9900 . ? C417 C418 1.497(12) . ? C417 H41K 0.9900 . ? C417 H41L 0.9900 . ? C418 H41Q 0.9900 . ? C418 H41R 0.9900 . ? N1S C5S 1.328(10) . ? N1S C1S 1.330(11) . ? C1S C2S 1.383(12) . ? C1S H1S 0.9500 . ? C2S C3S 1.392(12) . ? C2S H2S 0.9500 . ? C3S C4S 1.368(11) . ? C3S H3S 0.9500 . ? C4S C5S 1.381(11) . ? C4S H4S 0.9500 . ? C5S H5S 0.9500 . ? N1T C5T 1.289(14) . ? N1T C1T 1.442(15) . ? C1T C2T 1.369(13) . ? C1T H1T 0.9500 . ? C2T C3T 1.349(12) . ? C2T H2T 0.9500 . ? C3T C4T 1.378(12) . ? C3T H3T 0.9500 . ? C4T C5T 1.278(11) . ? C4T H4T 0.9500 . ? C5T H5T 0.9500 . ? Tl1 P12 2.819(2) . ? Tl1 P13 2.871(2) . ? Tl1 P15 3.114(2) . ? Tl1 P16 3.174(2) . ? P11 P14 2.150(3) . ? P11 P13 2.187(3) . ? P11 P12 2.203(3) . ? P12 P15 2.157(3) . ? P13 P16 2.157(3) . ? P14 P17 2.134(3) . ? P15 P17 2.225(3) . ? P15 P16 2.313(3) . ? P16 P17 2.249(3) . ? Tl2 P22 2.781(3) . ? Tl2 P23 2.882(3) . ? Tl2 P25 3.098(2) . ? Tl2 P26 3.181(2) . ? P21 P24 2.156(3) . ? P21 P22 2.178(4) . ? P21 P23 2.180(3) . ? P22 P25 2.157(5) . ? P23 P26 2.143(3) . ? P24 P27 2.120(3) . ? P25 P27 2.233(4) . ? P25 P26 2.326(4) . ? P26 P27 2.252(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 K1 O11 118.17(16) . . ? O14 K1 O16 97.52(16) . . ? O11 K1 O16 140.05(17) . . ? O14 K1 O12 97.12(16) . . ? O11 K1 O12 61.44(15) . . ? O16 K1 O12 98.95(16) . . ? O14 K1 O13 60.86(15) . . ? O11 K1 O13 95.74(16) . . ? O16 K1 O13 118.32(16) . . ? O12 K1 O13 137.72(16) . . ? O14 K1 O15 136.53(15) . . ? O11 K1 O15 99.19(15) . . ? O16 K1 O15 59.44(15) . . ? O12 K1 O15 121.13(16) . . ? O13 K1 O15 96.05(16) . . ? O14 K1 N12 59.98(17) . . ? O11 K1 N12 120.93(15) . . ? O16 K1 N12 60.95(16) . . ? O12 K1 N12 60.64(15) . . ? O13 K1 N12 119.81(17) . . ? O15 K1 N12 119.64(16) . . ? O14 K1 N11 120.78(18) . . ? O11 K1 N11 60.74(16) . . ? O16 K1 N11 116.96(17) . . ? O12 K1 N11 120.68(16) . . ? O13 K1 N11 60.58(17) . . ? O15 K1 N11 58.36(17) . . ? N12 K1 N11 177.89(18) . . ? C102 O11 C103 110.9(6) . . ? C102 O11 K1 116.1(4) . . ? C103 O11 K1 115.2(4) . . ? C105 O12 C104 109.7(6) . . ? C105 O12 K1 117.9(4) . . ? C104 O12 K1 110.2(4) . . ? C108 O13 C109 109.2(6) . . ? C108 O13 K1 115.6(5) . . ? C109 O13 K1 109.1(4) . . ? C110 O14 C111 111.0(6) . . ? C110 O14 K1 117.8(4) . . ? C111 O14 K1 121.4(5) . . ? C114 O15 C115 111.7(6) . . ? C114 O15 K1 117.9(5) . . ? C115 O15 K1 111.2(4) . . ? C116 O16 C117 110.1(6) . . ? C116 O16 K1 119.2(4) . . ? C117 O16 K1 117.8(4) . . ? C113 N11 C107 110.9(7) . . ? C113 N11 C101 109.1(6) . . ? C107 N11 C101 109.8(7) . . ? C113 N11 K1 110.8(5) . . ? C107 N11 K1 108.2(5) . . ? C101 N11 K1 108.0(4) . . ? C112 N12 C118 110.0(6) . . ? C112 N12 C106 109.6(6) . . ? C118 N12 C106 110.2(6) . . ? C112 N12 K1 110.4(5) . . ? C118 N12 K1 108.6(4) . . ? C106 N12 K1 108.0(4) . . ? C102 C101 N11 112.1(7) . . ? C102 C101 H10G 109.2 . . ? N11 C101 H10G 109.2 . . ? C102 C101 H10H 109.2 . . ? N11 C101 H10H 109.2 . . ? H10G C101 H10H 107.9 . . ? O11 C102 C101 109.9(7) . . ? O11 C102 H10M 109.7 . . ? C101 C102 H10M 109.7 . . ? O11 C102 H10N 109.7 . . ? C101 C102 H10N 109.7 . . ? H10M C102 H10N 108.2 . . ? O11 C103 C104 110.5(6) . . ? O11 C103 H10C 109.6 . . ? C104 C103 H10C 109.6 . . ? O11 C103 H10D 109.6 . . ? C104 C103 H10D 109.6 . . ? H10C C103 H10D 108.1 . . ? O12 C104 C103 109.7(6) . . ? O12 C104 H10I 109.7 . . ? C103 C104 H10I 109.7 . . ? O12 C104 H10J 109.7 . . ? C103 C104 H10J 109.7 . . ? H10I C104 H10J 108.2 . . ? O12 C105 C106 108.0(6) . . ? O12 C105 H10E 110.1 . . ? C106 C105 H10E 110.1 . . ? O12 C105 H10F 110.1 . . ? C106 C105 H10F 110.1 . . ? H10E C105 H10F 108.4 . . ? N12 C106 C105 113.4(7) . . ? N12 C106 H10K 108.9 . . ? C105 C106 H10K 108.9 . . ? N12 C106 H10L 108.9 . . ? C105 C106 H10L 108.9 . . ? H10K C106 H10L 107.7 . . ? N11 C107 C108 113.3(7) . . ? N11 C107 H10O 108.9 . . ? C108 C107 H10O 108.9 . . ? N11 C107 H10P 108.9 . . ? C108 C107 H10P 108.9 . . ? H10O C107 H10P 107.7 . . ? O13 C108 C107 108.5(7) . . ? O13 C108 H10Q 110.0 . . ? C107 C108 H10Q 110.0 . . ? O13 C108 H10R 110.0 . . ? C107 C108 H10R 110.0 . . ? H10Q C108 H10R 108.4 . . ? O13 C109 C110 109.7(7) . . ? O13 C109 H10A 109.7 . . ? C110 C109 H10A 109.7 . . ? O13 C109 H10B 109.7 . . ? C110 C109 H10B 109.7 . . ? H10A C109 H10B 108.2 . . ? O14 C110 C109 108.9(6) . . ? O14 C110 H11A 109.9 . . ? C109 C110 H11A 109.9 . . ? O14 C110 H11B 109.9 . . ? C109 C110 H11B 109.9 . . ? H11A C110 H11B 108.3 . . ? O14 C111 C112 108.9(6) . . ? O14 C111 H11C 109.9 . . ? C112 C111 H11C 109.9 . . ? O14 C111 H11D 109.9 . . ? C112 C111 H11D 109.9 . . ? H11C C111 H11D 108.3 . . ? N12 C112 C111 114.0(6) . . ? N12 C112 H11K 108.8 . . ? C111 C112 H11K 108.8 . . ? N12 C112 H11L 108.8 . . ? C111 C112 H11L 108.8 . . ? H11K C112 H11L 107.6 . . ? N11 C113 C114 113.8(7) . . ? N11 C113 H11I 108.8 . . ? C114 C113 H11I 108.8 . . ? N11 C113 H11J 108.8 . . ? C114 C113 H11J 108.8 . . ? H11I C113 H11J 107.7 . . ? O15 C114 C113 109.8(7) . . ? O15 C114 H11Q 109.7 . . ? C113 C114 H11Q 109.7 . . ? O15 C114 H11R 109.7 . . ? C113 C114 H11R 109.7 . . ? H11Q C114 H11R 108.2 . . ? O15 C115 C116 110.3(6) . . ? O15 C115 H11M 109.6 . . ? C116 C115 H11M 109.6 . . ? O15 C115 H11N 109.6 . . ? C116 C115 H11N 109.6 . . ? H11M C115 H11N 108.1 . . ? O16 C116 C115 109.0(7) . . ? O16 C116 H11O 109.9 . . ? C115 C116 H11O 109.9 . . ? O16 C116 H11P 109.9 . . ? C115 C116 H11P 109.9 . . ? H11O C116 H11P 108.3 . . ? O16 C117 C118 109.8(7) . . ? O16 C117 H11G 109.7 . . ? C118 C117 H11G 109.7 . . ? O16 C117 H11H 109.7 . . ? C118 C117 H11H 109.7 . . ? H11G C117 H11H 108.2 . . ? N12 C118 C117 113.2(6) . . ? N12 C118 H11E 108.9 . . ? C117 C118 H11E 108.9 . . ? N12 C118 H11F 108.9 . . ? C117 C118 H11F 108.9 . . ? H11E C118 H11F 107.8 . . ? O23 K2 O26 138.82(17) . . ? O23 K2 O21 98.69(16) . . ? O26 K2 O21 118.04(16) . . ? O23 K2 O25 98.28(16) . . ? O26 K2 O25 61.07(15) . . ? O21 K2 O25 97.49(16) . . ? O23 K2 O22 118.66(15) . . ? O26 K2 O22 96.54(15) . . ? O21 K2 O22 60.42(15) . . ? O25 K2 O22 138.28(16) . . ? O23 K2 O24 59.27(15) . . ? O26 K2 O24 97.97(15) . . ? O21 K2 O24 138.31(15) . . ? O25 K2 O24 119.13(17) . . ? O22 K2 O24 97.33(15) . . ? O23 K2 N21 61.63(17) . . ? O26 K2 N21 120.50(16) . . ? O21 K2 N21 59.89(18) . . ? O25 K2 N21 60.72(16) . . ? O22 K2 N21 119.23(18) . . ? O24 K2 N21 120.02(18) . . ? O23 K2 N22 116.90(17) . . ? O26 K2 N22 61.03(16) . . ? O21 K2 N22 120.22(18) . . ? O25 K2 N22 120.64(16) . . ? O22 K2 N22 60.56(17) . . ? O24 K2 N22 58.67(17) . . ? N21 K2 N22 178.36(17) . . ? C203 O21 C202 110.8(6) . . ? C203 O21 K2 118.3(4) . . ? C202 O21 K2 120.3(5) . . ? C205 O22 C204 109.5(6) . . ? C205 O22 K2 116.4(5) . . ? C204 O22 K2 110.9(4) . . ? C209 O23 C208 110.9(6) . . ? C209 O23 K2 118.9(4) . . ? C208 O23 K2 117.6(4) . . ? C211 O24 C210 110.0(6) . . ? C211 O24 K2 117.1(5) . . ? C210 O24 K2 112.1(4) . . ? C214 O25 C215 110.5(6) . . ? C214 O25 K2 117.4(4) . . ? C215 O25 K2 111.3(4) . . ? C216 O26 C217 111.2(6) . . ? C216 O26 K2 115.6(4) . . ? C217 O26 K2 117.0(4) . . ? C201 N21 C207 111.1(6) . . ? C201 N21 C213 111.7(7) . . ? C207 N21 C213 108.2(7) . . ? C201 N21 K2 110.7(5) . . ? C207 N21 K2 107.2(4) . . ? C213 N21 K2 107.8(4) . . ? C212 N22 C206 110.8(7) . . ? C212 N22 C218 108.8(6) . . ? C206 N22 C218 109.7(7) . . ? C212 N22 K2 111.6(5) . . ? C206 N22 K2 107.7(5) . . ? C218 N22 K2 108.1(4) . . ? N21 C201 C202 114.7(7) . . ? N21 C201 H20Q 108.6 . . ? C202 C201 H20Q 108.6 . . ? N21 C201 H20R 108.6 . . ? C202 C201 H20R 108.6 . . ? H20Q C201 H20R 107.6 . . ? O21 C202 C201 109.4(7) . . ? O21 C202 H20M 109.8 . . ? C201 C202 H20M 109.8 . . ? O21 C202 H20N 109.8 . . ? C201 C202 H20N 109.8 . . ? H20M C202 H20N 108.2 . . ? O21 C203 C204 108.8(6) . . ? O21 C203 H20A 109.9 . . ? C204 C203 H20A 109.9 . . ? O21 C203 H20B 109.9 . . ? C204 C203 H20B 109.9 . . ? H20A C203 H20B 108.3 . . ? O22 C204 C203 109.8(6) . . ? O22 C204 H20C 109.7 . . ? C203 C204 H20C 109.7 . . ? O22 C204 H20D 109.7 . . ? C203 C204 H20D 109.7 . . ? H20C C204 H20D 108.2 . . ? O22 C205 C206 108.3(7) . . ? O22 C205 H20O 110.0 . . ? C206 C205 H20O 110.0 . . ? O22 C205 H20P 110.0 . . ? C206 C205 H20P 110.0 . . ? H20O C205 H20P 108.4 . . ? N22 C206 C205 114.8(7) . . ? N22 C206 H20I 108.6 . . ? C205 C206 H20I 108.6 . . ? N22 C206 H20J 108.6 . . ? C205 C206 H20J 108.6 . . ? H20I C206 H20J 107.5 . . ? N21 C207 C208 115.3(7) . . ? N21 C207 H20E 108.4 . . ? C208 C207 H20E 108.4 . . ? N21 C207 H20F 108.4 . . ? C208 C207 H20F 108.4 . . ? H20E C207 H20F 107.5 . . ? O23 C208 C207 110.1(7) . . ? O23 C208 H20K 109.6 . . ? C207 C208 H20K 109.6 . . ? O23 C208 H20L 109.6 . . ? C207 C208 H20L 109.6 . . ? H20K C208 H20L 108.2 . . ? O23 C209 C210 109.5(7) . . ? O23 C209 H20G 109.8 . . ? C210 C209 H20G 109.8 . . ? O23 C209 H20H 109.8 . . ? C210 C209 H20H 109.8 . . ? H20G C209 H20H 108.2 . . ? O24 C210 C209 109.8(6) . . ? O24 C210 H21G 109.7 . . ? C209 C210 H21G 109.7 . . ? O24 C210 H21H 109.7 . . ? C209 C210 H21H 109.7 . . ? H21G C210 H21H 108.2 . . ? O24 C211 C212 108.6(6) . . ? O24 C211 H21Q 110.0 . . ? C212 C211 H21Q 110.0 . . ? O24 C211 H21R 110.0 . . ? C212 C211 H21R 110.0 . . ? H21Q C211 H21R 108.3 . . ? N22 C212 C211 113.8(7) . . ? N22 C212 H21E 108.8 . . ? C211 C212 H21E 108.8 . . ? N22 C212 H21F 108.8 . . ? C211 C212 H21F 108.8 . . ? H21E C212 H21F 107.7 . . ? N21 C213 C214 111.4(7) . . ? N21 C213 H21C 109.3 . . ? C214 C213 H21C 109.3 . . ? N21 C213 H21D 109.3 . . ? C214 C213 H21D 109.3 . . ? H21C C213 H21D 108.0 . . ? O25 C214 C213 109.0(7) . . ? O25 C214 H21I 109.9 . . ? C213 C214 H21I 109.9 . . ? O25 C214 H21J 109.9 . . ? C213 C214 H21J 109.9 . . ? H21I C214 H21J 108.3 . . ? O25 C215 C216 110.1(6) . . ? O25 C215 H21O 109.6 . . ? C216 C215 H21O 109.6 . . ? O25 C215 H21P 109.6 . . ? C216 C215 H21P 109.6 . . ? H21O C215 H21P 108.2 . . ? O26 C216 C215 110.8(6) . . ? O26 C216 H21A 109.5 . . ? C215 C216 H21A 109.5 . . ? O26 C216 H21B 109.5 . . ? C215 C216 H21B 109.5 . . ? H21A C216 H21B 108.1 . . ? O26 C217 C218 109.4(7) . . ? O26 C217 H21K 109.8 . . ? C218 C217 H21K 109.8 . . ? O26 C217 H21L 109.8 . . ? C218 C217 H21L 109.8 . . ? H21K C217 H21L 108.3 . . ? N22 C218 C217 112.6(7) . . ? N22 C218 H21M 109.1 . . ? C217 C218 H21M 109.1 . . ? N22 C218 H21N 109.1 . . ? C217 C218 H21N 109.1 . . ? H21M C218 H21N 107.8 . . ? O36 K3 O32 97.17(15) . . ? O36 K3 O34 96.00(14) . . ? O32 K3 O34 99.61(15) . . ? O36 K3 O35 59.88(14) . . ? O32 K3 O35 136.18(15) . . ? O34 K3 O35 118.29(16) . . ? O36 K3 O31 118.95(15) . . ? O32 K3 O31 60.47(14) . . ? O34 K3 O31 140.40(15) . . ? O35 K3 O31 96.41(14) . . ? O36 K3 O33 136.67(16) . . ? O32 K3 O33 120.93(15) . . ? O34 K3 O33 60.35(14) . . ? O35 K3 O33 97.75(15) . . ? O31 K3 O33 98.78(14) . . ? O36 K3 N31 120.25(16) . . ? O32 K3 N31 118.96(16) . . ? O34 K3 N31 119.83(16) . . ? O35 K3 N31 61.19(16) . . ? O31 K3 N31 59.47(16) . . ? O33 K3 N31 60.45(15) . . ? O36 K3 N32 60.21(15) . . ? O32 K3 N32 60.67(15) . . ? O34 K3 N32 60.10(15) . . ? O35 K3 N32 119.29(15) . . ? O31 K3 N32 120.24(16) . . ? O33 K3 N32 119.39(15) . . ? N31 K3 N32 179.51(18) . . ? C302 O31 C303 111.2(5) . . ? C302 O31 K3 117.9(4) . . ? C303 O31 K3 114.8(4) . . ? C305 O32 C304 109.9(5) . . ? C305 O32 K3 118.4(4) . . ? C304 O32 K3 115.2(4) . . ? C308 O33 C309 110.1(6) . . ? C308 O33 K3 118.3(4) . . ? C309 O33 K3 112.9(4) . . ? C310 O34 C311 110.3(5) . . ? C310 O34 K3 115.9(4) . . ? C311 O34 K3 119.2(4) . . ? C315 O35 C314 110.0(5) . . ? C315 O35 K3 112.6(4) . . ? C314 O35 K3 116.9(4) . . ? C316 O36 C317 110.8(5) . . ? C316 O36 K3 118.7(4) . . ? C317 O36 K3 119.8(4) . . ? C301 N31 C313 109.9(6) . . ? C301 N31 C307 109.7(6) . . ? C313 N31 C307 109.0(6) . . ? C301 N31 K3 111.3(4) . . ? C313 N31 K3 108.0(4) . . ? C307 N31 K3 108.8(4) . . ? C312 N32 C318 110.5(5) . . ? C312 N32 C306 108.9(6) . . ? C318 N32 C306 109.9(6) . . ? C312 N32 K3 110.3(4) . . ? C318 N32 K3 109.1(4) . . ? C306 N32 K3 108.2(4) . . ? N31 C301 C302 113.2(6) . . ? N31 C301 H30I 108.9 . . ? C302 C301 H30I 108.9 . . ? N31 C301 H30J 108.9 . . ? C302 C301 H30J 108.9 . . ? H30I C301 H30J 107.7 . . ? O31 C302 C301 109.7(6) . . ? O31 C302 H30K 109.7 . . ? C301 C302 H30K 109.7 . . ? O31 C302 H30L 109.7 . . ? C301 C302 H30L 109.7 . . ? H30K C302 H30L 108.2 . . ? O31 C303 C304 110.1(6) . . ? O31 C303 H30G 109.6 . . ? C304 C303 H30G 109.6 . . ? O31 C303 H30H 109.6 . . ? C304 C303 H30H 109.6 . . ? H30G C303 H30H 108.2 . . ? O32 C304 C303 109.9(6) . . ? O32 C304 H30C 109.7 . . ? C303 C304 H30C 109.7 . . ? O32 C304 H30D 109.7 . . ? C303 C304 H30D 109.7 . . ? H30C C304 H30D 108.2 . . ? O32 C305 C306 109.9(6) . . ? O32 C305 H30A 109.7 . . ? C306 C305 H30A 109.7 . . ? O32 C305 H30B 109.7 . . ? C306 C305 H30B 109.7 . . ? H30A C305 H30B 108.2 . . ? N32 C306 C305 113.7(6) . . ? N32 C306 H30M 108.8 . . ? C305 C306 H30M 108.8 . . ? N32 C306 H30N 108.8 . . ? C305 C306 H30N 108.8 . . ? H30M C306 H30N 107.7 . . ? C308 C307 N31 115.2(6) . . ? C308 C307 H30Q 108.5 . . ? N31 C307 H30Q 108.5 . . ? C308 C307 H30R 108.5 . . ? N31 C307 H30R 108.5 . . ? H30Q C307 H30R 107.5 . . ? O33 C308 C307 109.3(7) . . ? O33 C308 H30O 109.8 . . ? C307 C308 H30O 109.8 . . ? O33 C308 H30P 109.8 . . ? C307 C308 H30P 109.8 . . ? H30O C308 H30P 108.3 . . ? O33 C309 C310 109.4(6) . . ? O33 C309 H30E 109.8 . . ? C310 C309 H30E 109.8 . . ? O33 C309 H30F 109.8 . . ? C310 C309 H30F 109.8 . . ? H30E C309 H30F 108.2 . . ? O34 C310 C309 110.8(6) . . ? O34 C310 H31A 109.5 . . ? C309 C310 H31A 109.5 . . ? O34 C310 H31B 109.5 . . ? C309 C310 H31B 109.5 . . ? H31A C310 H31B 108.1 . . ? O34 C311 C312 109.9(6) . . ? O34 C311 H31C 109.7 . . ? C312 C311 H31C 109.7 . . ? O34 C311 H31D 109.7 . . ? C312 C311 H31D 109.7 . . ? H31C C311 H31D 108.2 . . ? N32 C312 C311 115.2(6) . . ? N32 C312 H31Q 108.5 . . ? C311 C312 H31Q 108.5 . . ? N32 C312 H31R 108.5 . . ? C311 C312 H31R 108.5 . . ? H31Q C312 H31R 107.5 . . ? N31 C313 C314 114.1(7) . . ? N31 C313 H31I 108.7 . . ? C314 C313 H31I 108.7 . . ? N31 C313 H31J 108.7 . . ? C314 C313 H31J 108.7 . . ? H31I C313 H31J 107.6 . . ? O35 C314 C313 108.3(6) . . ? O35 C314 H31O 110.0 . . ? C313 C314 H31O 110.0 . . ? O35 C314 H31P 110.0 . . ? C313 C314 H31P 110.0 . . ? H31O C314 H31P 108.4 . . ? O35 C315 C316 109.4(6) . . ? O35 C315 H31E 109.8 . . ? C316 C315 H31E 109.8 . . ? O35 C315 H31F 109.8 . . ? C316 C315 H31F 109.8 . . ? H31E C315 H31F 108.2 . . ? O36 C316 C315 108.3(6) . . ? O36 C316 H31M 110.0 . . ? C315 C316 H31M 110.0 . . ? O36 C316 H31N 110.0 . . ? C315 C316 H31N 110.0 . . ? H31M C316 H31N 108.4 . . ? O36 C317 C318 109.0(6) . . ? O36 C317 H31K 109.9 . . ? C318 C317 H31K 109.9 . . ? O36 C317 H31L 109.9 . . ? C318 C317 H31L 109.9 . . ? H31K C317 H31L 108.3 . . ? N32 C318 C317 113.6(6) . . ? N32 C318 H31G 108.8 . . ? C317 C318 H31G 108.8 . . ? N32 C318 H31H 108.8 . . ? C317 C318 H31H 108.8 . . ? H31G C318 H31H 107.7 . . ? O43 K4 O45 98.79(15) . . ? O43 K4 O41 100.07(16) . . ? O45 K4 O41 97.12(15) . . ? O43 K4 O46 114.34(16) . . ? O45 K4 O46 59.76(14) . . ? O41 K4 O46 140.25(16) . . ? O43 K4 O42 143.24(16) . . ? O45 K4 O42 113.27(16) . . ? O41 K4 O42 59.88(16) . . ? O46 K4 O42 97.68(16) . . ? O43 K4 N42 118.10(18) . . ? O45 K4 N42 118.83(17) . . ? O41 K4 N42 119.64(18) . . ? O46 K4 N42 60.98(16) . . ? O42 K4 N42 61.73(18) . . ? O43 K4 O44 59.45(14) . . ? O45 K4 O44 141.08(16) . . ? O41 K4 O44 117.19(15) . . ? O46 K4 O44 97.85(15) . . ? O42 K4 O44 100.25(15) . . ? N42 K4 O44 60.58(16) . . ? O43 K4 N41 61.63(17) . . ? O45 K4 N41 61.20(15) . . ? O41 K4 N41 60.62(17) . . ? O46 K4 N41 118.96(16) . . ? O42 K4 N41 118.56(18) . . ? N42 K4 N41 179.7(2) . . ? O44 K4 N41 119.19(16) . . ? C402 O41 C403 109.3(6) . . ? C402 O41 K4 120.7(4) . . ? C403 O41 K4 116.4(4) . . ? C404 O42 C405 111.5(6) . . ? C404 O42 K4 116.2(4) . . ? C405 O42 K4 116.4(5) . . ? C408 O43 C409 111.5(5) . . ? C408 O43 K4 118.4(4) . . ? C409 O43 K4 118.8(4) . . ? C410 O44 C411 112.6(6) . . ? C410 O44 K4 111.0(4) . . ? C411 O44 K4 116.8(4) . . ? C415 O45 C414 110.0(5) . . ? C415 O45 K4 117.6(4) . . ? C414 O45 K4 119.7(4) . . ? C417 O46 C416 109.9(6) . . ? C417 O46 K4 118.5(4) . . ? C416 O46 K4 115.5(4) . . ? C401 N41 C407 111.5(6) . . ? C401 N41 C413 109.6(6) . . ? C407 N41 C413 110.4(6) . . ? C401 N41 K4 108.8(4) . . ? C407 N41 K4 107.5(4) . . ? C413 N41 K4 109.0(4) . . ? C406 N42 C418 110.2(7) . . ? C406 N42 C412 107.9(6) . . ? C418 N42 C412 108.9(7) . . ? C406 N42 K4 109.7(5) . . ? C418 N42 K4 110.1(4) . . ? C412 N42 K4 110.0(4) . . ? N41 C401 C402 115.1(7) . . ? N41 C401 H40Q 108.5 . . ? C402 C401 H40Q 108.5 . . ? N41 C401 H40R 108.5 . . ? C402 C401 H40R 108.5 . . ? H40Q C401 H40R 107.5 . . ? O41 C402 C401 108.8(6) . . ? O41 C402 H40I 109.9 . . ? C401 C402 H40I 109.9 . . ? O41 C402 H40J 109.9 . . ? C401 C402 H40J 109.9 . . ? H40I C402 H40J 108.3 . . ? O41 C403 C404 110.1(6) . . ? O41 C403 H40G 109.6 . . ? C404 C403 H40G 109.6 . . ? O41 C403 H40H 109.6 . . ? C404 C403 H40H 109.6 . . ? H40G C403 H40H 108.2 . . ? O42 C404 C403 111.2(6) . . ? O42 C404 H40C 109.4 . . ? C403 C404 H40C 109.4 . . ? O42 C404 H40D 109.4 . . ? C403 C404 H40D 109.4 . . ? H40C C404 H40D 108.0 . . ? O42 C405 C406 110.9(7) . . ? O42 C405 H40M 109.5 . . ? C406 C405 H40M 109.5 . . ? O42 C405 H40N 109.5 . . ? C406 C405 H40N 109.5 . . ? H40M C405 H40N 108.1 . . ? N42 C406 C405 115.0(7) . . ? N42 C406 H40K 108.5 . . ? C405 C406 H40K 108.5 . . ? N42 C406 H40L 108.5 . . ? C405 C406 H40L 108.5 . . ? H40K C406 H40L 107.5 . . ? N41 C407 C408 114.5(6) . . ? N41 C407 H40O 108.6 . . ? C408 C407 H40O 108.6 . . ? N41 C407 H40P 108.6 . . ? C408 C407 H40P 108.6 . . ? H40O C407 H40P 107.6 . . ? O43 C408 C407 109.7(6) . . ? O43 C408 H40E 109.7 . . ? C407 C408 H40E 109.7 . . ? O43 C408 H40F 109.7 . . ? C407 C408 H40F 109.7 . . ? H40E C408 H40F 108.2 . . ? O43 C409 C410 109.8(6) . . ? O43 C409 H40A 109.7 . . ? C410 C409 H40A 109.7 . . ? O43 C409 H40B 109.7 . . ? C410 C409 H40B 109.7 . . ? H40A C409 H40B 108.2 . . ? O44 C410 C409 110.1(6) . . ? O44 C410 H41A 109.6 . . ? C409 C410 H41A 109.6 . . ? O44 C410 H41B 109.6 . . ? C409 C410 H41B 109.6 . . ? H41A C410 H41B 108.2 . . ? O44 C411 C412 110.0(7) . . ? O44 C411 H41I 109.7 . . ? C412 C411 H41I 109.7 . . ? O44 C411 H41J 109.7 . . ? C412 C411 H41J 109.7 . . ? H41I C411 H41J 108.2 . . ? C411 C412 N42 114.3(7) . . ? C411 C412 H41O 108.7 . . ? N42 C412 H41O 108.7 . . ? C411 C412 H41P 108.7 . . ? N42 C412 H41P 108.7 . . ? H41O C412 H41P 107.6 . . ? N41 C413 C414 114.4(7) . . ? N41 C413 H41M 108.7 . . ? C414 C413 H41M 108.7 . . ? N41 C413 H41N 108.7 . . ? C414 C413 H41N 108.7 . . ? H41M C413 H41N 107.6 . . ? O45 C414 C413 108.9(6) . . ? O45 C414 H41E 109.9 . . ? C413 C414 H41E 109.9 . . ? O45 C414 H41F 109.9 . . ? C413 C414 H41F 109.9 . . ? H41E C414 H41F 108.3 . . ? O45 C415 C416 110.1(6) . . ? O45 C415 H41C 109.6 . . ? C416 C415 H41C 109.6 . . ? O45 C415 H41D 109.6 . . ? C416 C415 H41D 109.6 . . ? H41C C415 H41D 108.2 . . ? O46 C416 C415 109.4(6) . . ? O46 C416 H41G 109.8 . . ? C415 C416 H41G 109.8 . . ? O46 C416 H41H 109.8 . . ? C415 C416 H41H 109.8 . . ? H41G C416 H41H 108.2 . . ? O46 C417 C418 111.2(7) . . ? O46 C417 H41K 109.4 . . ? C418 C417 H41K 109.4 . . ? O46 C417 H41L 109.4 . . ? C418 C417 H41L 109.4 . . ? H41K C417 H41L 108.0 . . ? N42 C418 C417 113.1(7) . . ? N42 C418 H41Q 109.0 . . ? C417 C418 H41Q 109.0 . . ? N42 C418 H41R 109.0 . . ? C417 C418 H41R 109.0 . . ? H41Q C418 H41R 107.8 . . ? C5S N1S C1S 117.2(7) . . ? N1S C1S C2S 124.2(8) . . ? N1S C1S H1S 117.9 . . ? C2S C1S H1S 117.9 . . ? C1S C2S C3S 117.6(8) . . ? C1S C2S H2S 121.2 . . ? C3S C2S H2S 121.2 . . ? C4S C3S C2S 118.3(8) . . ? C4S C3S H3S 120.9 . . ? C2S C3S H3S 120.9 . . ? C3S C4S C5S 119.9(7) . . ? C3S C4S H4S 120.1 . . ? C5S C4S H4S 120.1 . . ? N1S C5S C4S 122.7(7) . . ? N1S C5S H5S 118.7 . . ? C4S C5S H5S 118.7 . . ? C5T N1T C1T 122.8(9) . . ? C2T C1T N1T 115.3(9) . . ? C2T C1T H1T 122.3 . . ? N1T C1T H1T 122.3 . . ? C3T C2T C1T 120.2(9) . . ? C3T C2T H2T 119.9 . . ? C1T C2T H2T 119.9 . . ? C2T C3T C4T 118.8(9) . . ? C2T C3T H3T 120.6 . . ? C4T C3T H3T 120.6 . . ? C5T C4T C3T 123.3(9) . . ? C5T C4T H4T 118.4 . . ? C3T C4T H4T 118.4 . . ? C4T C5T N1T 119.5(9) . . ? C4T C5T H5T 120.3 . . ? N1T C5T H5T 120.3 . . ? P12 Tl1 P13 72.87(6) . . ? P12 Tl1 P15 42.27(6) . . ? P13 Tl1 P15 71.87(6) . . ? P12 Tl1 P16 72.25(5) . . ? P13 Tl1 P16 41.44(6) . . ? P15 Tl1 P16 43.15(6) . . ? P14 P11 P13 102.15(12) . . ? P14 P11 P12 101.28(12) . . ? P13 P11 P12 100.67(12) . . ? P15 P12 P11 99.34(11) . . ? P15 P12 Tl1 76.18(8) . . ? P11 P12 Tl1 90.05(9) . . ? P16 P13 P11 99.95(11) . . ? P16 P13 Tl1 76.84(9) . . ? P11 P13 Tl1 89.03(10) . . ? P17 P14 P11 98.67(12) . . ? P12 P15 P17 103.78(12) . . ? P12 P15 P16 104.90(12) . . ? P17 P15 P16 59.39(9) . . ? P12 P15 Tl1 61.55(7) . . ? P17 P15 Tl1 121.05(10) . . ? P16 P15 Tl1 69.82(7) . . ? P13 P16 P17 104.00(12) . . ? P13 P16 P15 103.73(11) . . ? P17 P16 P15 58.36(9) . . ? P13 P16 Tl1 61.72(8) . . ? P17 P16 Tl1 117.79(9) . . ? P15 P16 Tl1 67.03(7) . . ? P14 P17 P15 107.07(11) . . ? P14 P17 P16 106.33(11) . . ? P15 P17 P16 62.25(9) . . ? P22 Tl2 P23 72.23(7) . . ? P22 Tl2 P25 42.63(9) . . ? P23 Tl2 P25 71.62(6) . . ? P22 Tl2 P26 72.42(7) . . ? P23 Tl2 P26 41.02(7) . . ? P25 Tl2 P26 43.47(7) . . ? P24 P21 P22 101.68(15) . . ? P24 P21 P23 102.20(12) . . ? P22 P21 P23 100.04(14) . . ? P25 P22 P21 99.74(13) . . ? P25 P22 Tl2 76.54(11) . . ? P21 P22 Tl2 91.67(11) . . ? P26 P23 P21 100.58(12) . . ? P26 P23 Tl2 77.00(11) . . ? P21 P23 Tl2 88.98(10) . . ? P27 P24 P21 98.64(12) . . ? P22 P25 P27 103.78(15) . . ? P22 P25 P26 104.09(14) . . ? P27 P25 P26 59.15(11) . . ? P22 P25 Tl2 60.83(9) . . ? P27 P25 Tl2 121.29(11) . . ? P26 P25 Tl2 70.16(8) . . ? P23 P26 P27 103.68(13) . . ? P23 P26 P25 103.14(13) . . ? P27 P26 P25 58.35(10) . . ? P23 P26 Tl2 61.98(9) . . ? P27 P26 Tl2 117.34(10) . . ? P25 P26 Tl2 66.37(9) . . ? P24 P27 P25 106.78(14) . . ? P24 P27 P26 106.81(12) . . ? P25 P27 P26 62.49(11) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.532 _refine_diff_density_min -1.925 _refine_diff_density_rms 0.162 #===END data_4b _database_code_depnum_ccdc_archive 'CCDC 786257' #TrackingRef '- combined_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(18-crown-6)]2[TlAs7] ; _chemical_name_common (K(18-crown-6))2(TlAs7) _chemical_melting_point . _chemical_formula_moiety 'C24 H48 As7 K2 O12 Tl' _chemical_formula_sum 'C24 H48 As7 K2 O12 Tl' _chemical_formula_weight 1335.63 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tl Tl -2.8358 9.6688 '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_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.8701(3) _cell_length_b 11.4835(3) _cell_length_c 20.8037(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.8300(10) _cell_angle_gamma 90.00 _cell_volume 4291.53(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 320176 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.05 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 9.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1536 _exptl_absorpt_correction_T_max 0.6518 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 14444 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7489 _reflns_number_gt 6461 _reflns_threshold_expression >2\s(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The 18-crown-6 moiety defined by K2 exhibits some 'rotational' disorder which can be modelled by two different components in a 63:37 ratio. Such a model requires the application of extensive restraints. Both of the components of the diordered 18-crown-6 unit were restrained with respect to the 18-crown-6 moiety defined by K1 using the SAME command. In addition the following constraints/restraints were also employed: EADP C10A O6A EADP O1A C1A EADP C205 C206 EADP O4A C7A ISOR O1A O4A O5A ISOR C3A C4A C6A C8A C9A C10A C11A C12A C201 ISOR 0.02 O2A O3A C2A C5A C203 C212 ; _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^)+(0.0661P)^2^+107.0257P] 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 7489 _refine_ls_number_parameters 554 _refine_ls_number_restraints 265 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1869 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.113 _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 As11 As 0.20600(7) 0.71974(11) 0.25350(7) 0.0367(3) Uani 1 1 d . . . As12 As 0.13883(7) 0.53768(12) 0.23146(7) 0.0429(3) Uani 1 1 d . . . As13 As 0.32327(8) 0.65400(12) 0.24210(7) 0.0387(3) Uani 1 1 d . . . As14 As 0.22957(8) 0.73364(13) 0.37116(7) 0.0433(3) Uani 1 1 d . . . As15 As 0.21945(9) 0.41495(12) 0.31277(8) 0.0455(4) Uani 1 1 d . . . As16 As 0.35149(8) 0.50012(14) 0.32199(7) 0.0460(4) Uani 1 1 d . . . As17 As 0.28611(9) 0.55122(15) 0.40362(7) 0.0486(4) Uani 1 1 d . . . Tl1 Tl 0.24899(4) 0.44381(5) 0.17273(3) 0.0533(2) Uani 1 1 d . . . K1 K 0.09160(16) 0.5465(2) 0.40762(15) 0.0412(7) Uani 1 1 d . . . K2 K 0.40528(17) 0.8487(3) 0.39622(15) 0.0448(7) Uani 1 1 d . . . O11 O -0.0279(5) 0.4096(8) 0.3179(4) 0.042(2) Uani 1 1 d D . . O12 O 0.0936(5) 0.2954(7) 0.4081(4) 0.041(2) Uani 1 1 d D . . O13 O 0.1696(5) 0.4135(8) 0.5296(5) 0.048(2) Uani 1 1 d D . . O14 O 0.1694(5) 0.6587(8) 0.5330(4) 0.045(2) Uani 1 1 d D . . O15 O 0.0375(6) 0.7622(8) 0.4515(5) 0.049(2) Uani 1 1 d D . . O16 O -0.0397(5) 0.6505(8) 0.3270(5) 0.045(2) Uani 1 1 d D . . C101 C 0.0044(8) 0.3064(13) 0.3004(7) 0.050(4) Uani 1 1 d D . . H10A H 0.0445 0.3273 0.2810 0.060 Uiso 1 1 calc R . . H10B H -0.0338 0.2612 0.2664 0.060 Uiso 1 1 calc R . . C102 C 0.0350(8) 0.2367(12) 0.3619(7) 0.049(3) Uani 1 1 d D . . H10C H -0.0046 0.2206 0.3827 0.058 Uiso 1 1 calc R . . H10D H 0.0531 0.1612 0.3500 0.058 Uiso 1 1 calc R . . C103 C 0.1243(8) 0.2384(12) 0.4697(7) 0.047(3) Uani 1 1 d D . . H10E H 0.1387 0.1581 0.4615 0.057 Uiso 1 1 calc R . . H10F H 0.0869 0.2336 0.4941 0.057 Uiso 1 1 calc R . . C104 C 0.1918(8) 0.3035(12) 0.5120(8) 0.051(4) Uani 1 1 d D . . H10G H 0.2165 0.2586 0.5535 0.061 Uiso 1 1 calc R . . H10H H 0.2277 0.3137 0.4864 0.061 Uiso 1 1 calc R . . C105 C 0.2304(8) 0.4790(13) 0.5690(7) 0.050(4) Uani 1 1 d D . . H10I H 0.2648 0.4960 0.5425 0.060 Uiso 1 1 calc R . . H10J H 0.2581 0.4335 0.6094 0.060 Uiso 1 1 calc R . . C106 C 0.2038(9) 0.5905(14) 0.5906(7) 0.053(4) Uani 1 1 d D . . H10K H 0.1678 0.5739 0.6154 0.064 Uiso 1 1 calc R . . H10L H 0.2463 0.6336 0.6211 0.064 Uiso 1 1 calc R . . C107 C 0.1409(9) 0.7640(14) 0.5516(7) 0.055(4) Uani 1 1 d D . . H10M H 0.1824 0.8129 0.5790 0.066 Uiso 1 1 calc R . . H10N H 0.1076 0.7464 0.5789 0.066 Uiso 1 1 calc R . . C108 C 0.0985(11) 0.8281(13) 0.4882(9) 0.067(5) Uani 1 1 d D . . H10O H 0.0812 0.9040 0.5003 0.081 Uiso 1 1 calc R . . H10P H 0.1316 0.8432 0.4603 0.081 Uiso 1 1 calc R . . C109 C -0.0062(10) 0.8201(13) 0.3937(7) 0.062(5) Uani 1 1 d D . . H10Q H 0.0248 0.8413 0.3647 0.074 Uiso 1 1 calc R . . H10R H -0.0264 0.8927 0.4069 0.074 Uiso 1 1 calc R . . C110 C -0.0691(9) 0.7427(15) 0.3551(7) 0.062(5) Uani 1 1 d D . . H11A H -0.0957 0.7119 0.3857 0.075 Uiso 1 1 calc R . . H11B H -0.1048 0.7878 0.3189 0.075 Uiso 1 1 calc R . . C111 C -0.0976(8) 0.5803(13) 0.2829(8) 0.051(4) Uani 1 1 d D . . H11C H -0.1253 0.6265 0.2430 0.061 Uiso 1 1 calc R . . H11D H -0.1330 0.5556 0.3069 0.061 Uiso 1 1 calc R . . C112 C -0.0647(9) 0.4767(13) 0.2611(7) 0.050(4) Uani 1 1 d D . . H11E H -0.1044 0.4298 0.2295 0.060 Uiso 1 1 calc R . . H11F H -0.0291 0.5012 0.2373 0.060 Uiso 1 1 calc R . . O21 O 0.5374(10) 0.7244(16) 0.4680(9) 0.070(6) Uani 0.634(17) 1 d PD A 1 O22 O 0.5223(8) 0.8177(16) 0.3396(8) 0.069(6) Uani 0.634(17) 1 d PD A 1 O23 O 0.4205(9) 1.0020(16) 0.2931(8) 0.063(6) Uani 0.634(17) 1 d PD A 1 O24 O 0.3197(11) 1.0562(14) 0.3639(8) 0.061(5) Uani 0.634(17) 1 d PD A 1 O25 O 0.3462(9) 0.9702(13) 0.4945(8) 0.055(5) Uani 0.634(17) 1 d PD A 1 O26 O 0.4302(10) 0.7650(16) 0.5312(8) 0.072(6) Uani 0.634(17) 1 d PD A 1 C201 C 0.5756(15) 0.678(3) 0.4255(14) 0.079(12) Uani 0.634(17) 1 d PDU A 1 H20A H 0.5467 0.6125 0.3992 0.094 Uiso 0.634(17) 1 calc PR A 1 H20B H 0.6245 0.6477 0.4531 0.094 Uiso 0.634(17) 1 calc PR A 1 C202 C 0.5865(14) 0.766(3) 0.3796(17) 0.098(13) Uani 0.634(17) 1 d PD A 1 H20C H 0.6192 0.8277 0.4065 0.118 Uiso 0.634(17) 1 calc PR A 1 H20D H 0.6127 0.7305 0.3501 0.118 Uiso 0.634(17) 1 calc PR A 1 C203 C 0.5286(13) 0.894(2) 0.2901(13) 0.063(7) Uani 0.634(17) 1 d PDU A 1 H20E H 0.5512 0.8539 0.2592 0.075 Uiso 0.634(17) 1 calc PR A 1 H20F H 0.5616 0.9600 0.3114 0.075 Uiso 0.634(17) 1 calc PR A 1 C204 C 0.4532(16) 0.941(3) 0.2508(13) 0.070(10) Uani 0.634(17) 1 d PD A 1 H20G H 0.4582 0.9928 0.2146 0.084 Uiso 0.634(17) 1 calc PR A 1 H20H H 0.4205 0.8748 0.2293 0.084 Uiso 0.634(17) 1 calc PR A 1 C205 C 0.3493(13) 1.045(2) 0.2600(10) 0.074(7) Uani 0.634(17) 1 d PD A 1 H20I H 0.3153 0.9790 0.2421 0.089 Uiso 0.634(17) 1 calc PR A 1 H20J H 0.3513 1.0936 0.2213 0.089 Uiso 0.634(17) 1 calc PR A 1 C206 C 0.319(2) 1.115(3) 0.3051(13) 0.074(7) Uani 0.634(17) 1 d PD A 1 H20K H 0.3494 1.1871 0.3177 0.089 Uiso 0.634(17) 1 calc PR A 1 H20L H 0.2677 1.1383 0.2804 0.089 Uiso 0.634(17) 1 calc PR A 1 C207 C 0.2965(19) 1.118(2) 0.4114(13) 0.068(10) Uani 0.634(17) 1 d PD A 1 H20M H 0.2502 1.1617 0.3886 0.082 Uiso 0.634(17) 1 calc PR A 1 H20N H 0.3353 1.1755 0.4346 0.082 Uiso 0.634(17) 1 calc PR A 1 C208 C 0.2827(13) 1.035(2) 0.4623(12) 0.062(8) Uani 0.634(17) 1 d PD A 1 H20O H 0.2671 1.0793 0.4964 0.074 Uiso 0.634(17) 1 calc PR A 1 H20P H 0.2418 0.9814 0.4391 0.074 Uiso 0.634(17) 1 calc PR A 1 C209 C 0.3343(16) 0.891(2) 0.5417(12) 0.068(8) Uani 0.634(17) 1 d PD A 1 H20Q H 0.2943 0.8363 0.5184 0.081 Uiso 0.634(17) 1 calc PR A 1 H20R H 0.3177 0.9345 0.5757 0.081 Uiso 0.634(17) 1 calc PR A 1 C210 C 0.4030(18) 0.825(3) 0.5766(12) 0.085(11) Uani 0.634(17) 1 d PD A 1 H21A H 0.4416 0.8788 0.6033 0.102 Uiso 0.634(17) 1 calc PR A 1 H21B H 0.3918 0.7683 0.6083 0.102 Uiso 0.634(17) 1 calc PR A 1 C211 C 0.4965(17) 0.701(4) 0.5625(12) 0.100(17) Uani 0.634(17) 1 d PD A 1 H21C H 0.4872 0.6431 0.5944 0.120 Uiso 0.634(17) 1 calc PR A 1 H21D H 0.5364 0.7541 0.5881 0.120 Uiso 0.634(17) 1 calc PR A 1 C212 C 0.5197(19) 0.641(2) 0.5099(14) 0.082(10) Uani 0.634(17) 1 d PDU A 1 H21E H 0.5636 0.5911 0.5310 0.099 Uiso 0.634(17) 1 calc PR A 1 H21F H 0.4789 0.5901 0.4829 0.099 Uiso 0.634(17) 1 calc PR A 1 O1A O 0.537(2) 0.730(4) 0.385(2) 0.130(19) Uani 0.366(17) 1 d PDU A 2 O2A O 0.479(2) 0.909(3) 0.2922(17) 0.102(15) Uani 0.366(17) 1 d PDU A 2 O3A O 0.359(2) 1.041(4) 0.3092(17) 0.118(17) Uani 0.366(17) 1 d PDU A 2 O4A O 0.334(2) 1.041(3) 0.4342(15) 0.120(18) Uani 0.366(17) 1 d PDU A 2 O5A O 0.398(2) 0.869(3) 0.5285(15) 0.106(16) Uani 0.366(17) 1 d PDU A 2 O6A O 0.5034(16) 0.716(3) 0.5040(16) 0.088(13) Uani 0.366(17) 1 d PD A 2 C1A C 0.562(3) 0.744(6) 0.329(3) 0.130(19) Uani 0.366(17) 1 d PD A 2 H1A1 H 0.5683 0.6666 0.3107 0.155 Uiso 0.366(17) 1 calc PR A 2 H1A2 H 0.6114 0.7825 0.3433 0.155 Uiso 0.366(17) 1 calc PR A 2 C2A C 0.513(4) 0.813(5) 0.275(2) 0.13(3) Uani 0.366(17) 1 d PDU A 2 H2A1 H 0.5412 0.8383 0.2450 0.153 Uiso 0.366(17) 1 calc PR A 2 H2A2 H 0.4728 0.7603 0.2485 0.153 Uiso 0.366(17) 1 calc PR A 2 C3A C 0.435(4) 0.980(6) 0.242(2) 0.14(4) Uani 0.366(17) 1 d PDU A 2 H3A1 H 0.3941 0.9327 0.2120 0.168 Uiso 0.366(17) 1 calc PR A 2 H3A2 H 0.4652 1.0103 0.2140 0.168 Uiso 0.366(17) 1 calc PR A 2 C4A C 0.403(3) 1.080(4) 0.270(3) 0.13(3) Uani 0.366(17) 1 d PDU A 2 H4A1 H 0.4438 1.1290 0.2982 0.155 Uiso 0.366(17) 1 calc PR A 2 H4A2 H 0.3721 1.1284 0.2325 0.155 Uiso 0.366(17) 1 calc PR A 2 C5A C 0.309(3) 1.119(5) 0.322(3) 0.079(19) Uani 0.366(17) 1 d PDU A 2 H5A1 H 0.2663 1.1284 0.2808 0.095 Uiso 0.366(17) 1 calc PR A 2 H5A2 H 0.3337 1.1959 0.3329 0.095 Uiso 0.366(17) 1 calc PR A 2 C6A C 0.280(2) 1.087(5) 0.378(2) 0.09(2) Uani 0.366(17) 1 d PDU A 2 H6A1 H 0.2575 1.1565 0.3924 0.112 Uiso 0.366(17) 1 calc PR A 2 H6A2 H 0.2397 1.0283 0.3616 0.112 Uiso 0.366(17) 1 calc PR A 2 C7A C 0.314(3) 1.029(5) 0.494(2) 0.120(18) Uani 0.366(17) 1 d PD A 2 H7A1 H 0.2704 0.9768 0.4851 0.144 Uiso 0.366(17) 1 calc PR A 2 H7A2 H 0.3008 1.1055 0.5081 0.144 Uiso 0.366(17) 1 calc PR A 2 C8A C 0.379(3) 0.978(4) 0.5480(19) 0.13(3) Uani 0.366(17) 1 d PDU A 2 H8A1 H 0.4224 1.0309 0.5569 0.156 Uiso 0.366(17) 1 calc PR A 2 H8A2 H 0.3658 0.9695 0.5902 0.156 Uiso 0.366(17) 1 calc PR A 2 C9A C 0.453(3) 0.813(5) 0.5807(19) 0.11(3) Uani 0.366(17) 1 d PDU A 2 H9A1 H 0.4334 0.7991 0.6192 0.132 Uiso 0.366(17) 1 calc PR A 2 H9A2 H 0.4973 0.8638 0.5967 0.132 Uiso 0.366(17) 1 calc PR A 2 C10A C 0.475(4) 0.700(4) 0.557(3) 0.088(13) Uani 0.366(17) 1 d PDU A 2 H10S H 0.5127 0.6610 0.5949 0.105 Uiso 0.366(17) 1 calc PR A 2 H10T H 0.4308 0.6478 0.5425 0.105 Uiso 0.366(17) 1 calc PR A 2 C11A C 0.517(5) 0.613(3) 0.472(3) 0.18(5) Uani 0.366(17) 1 d PDU A 2 H11G H 0.4698 0.5801 0.4430 0.215 Uiso 0.366(17) 1 calc PR A 2 H11H H 0.5420 0.5545 0.5061 0.215 Uiso 0.366(17) 1 calc PR A 2 C12A C 0.566(5) 0.640(6) 0.430(3) 0.15(5) Uani 0.366(17) 1 d PDU A 2 H12A H 0.6158 0.6610 0.4591 0.180 Uiso 0.366(17) 1 calc PR A 2 H12B H 0.5705 0.5692 0.4038 0.180 Uiso 0.366(17) 1 calc PR A 2 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 As11 0.0418(7) 0.0277(6) 0.0402(7) 0.0064(5) 0.0118(6) 0.0031(5) As12 0.0324(7) 0.0393(7) 0.0518(8) -0.0073(6) 0.0052(6) -0.0056(6) As13 0.0410(7) 0.0384(7) 0.0414(7) -0.0022(6) 0.0197(6) -0.0086(6) As14 0.0474(8) 0.0420(8) 0.0440(8) -0.0114(6) 0.0192(6) -0.0046(6) As15 0.0581(9) 0.0278(7) 0.0587(9) 0.0081(6) 0.0302(7) 0.0025(6) As16 0.0364(7) 0.0575(9) 0.0430(7) 0.0080(7) 0.0106(6) 0.0170(7) As17 0.0470(8) 0.0655(10) 0.0322(7) 0.0122(7) 0.0107(6) 0.0120(7) Tl1 0.0666(4) 0.0475(3) 0.0518(4) -0.0182(3) 0.0271(3) -0.0139(3) K1 0.0385(15) 0.0339(14) 0.0463(16) 0.0006(12) 0.0055(12) 0.0056(12) K2 0.0399(16) 0.0471(17) 0.0458(16) 0.0016(14) 0.0107(13) 0.0043(13) O11 0.042(5) 0.042(5) 0.039(5) 0.004(4) 0.009(4) -0.001(4) O12 0.049(5) 0.035(5) 0.039(5) 0.005(4) 0.015(4) 0.002(4) O13 0.050(6) 0.047(6) 0.038(5) -0.001(4) 0.002(4) 0.012(5) O14 0.057(6) 0.043(5) 0.036(5) -0.006(4) 0.015(4) 0.008(5) O15 0.068(7) 0.040(5) 0.044(5) 0.008(4) 0.021(5) 0.019(5) O16 0.039(5) 0.048(6) 0.048(5) 0.010(4) 0.010(4) 0.015(4) C101 0.053(9) 0.049(8) 0.053(8) -0.016(7) 0.025(7) -0.017(7) C102 0.055(9) 0.034(7) 0.056(9) -0.006(6) 0.016(7) -0.006(6) C103 0.062(9) 0.034(7) 0.052(8) 0.004(6) 0.026(7) 0.001(7) C104 0.055(9) 0.040(8) 0.059(9) 0.012(7) 0.019(7) 0.013(7) C105 0.046(8) 0.058(9) 0.042(7) 0.006(7) 0.007(6) 0.012(7) C106 0.064(10) 0.062(10) 0.030(7) -0.009(7) 0.008(7) 0.010(8) C107 0.063(10) 0.058(10) 0.044(8) -0.020(7) 0.015(7) -0.002(8) C108 0.101(14) 0.038(8) 0.072(11) -0.011(8) 0.042(11) 0.009(9) C109 0.096(13) 0.047(9) 0.038(8) 0.011(7) 0.014(8) 0.027(9) C110 0.071(11) 0.074(11) 0.041(8) 0.014(8) 0.016(8) 0.048(10) C111 0.047(8) 0.055(9) 0.051(8) 0.019(7) 0.015(7) 0.003(7) C112 0.051(8) 0.056(9) 0.042(8) 0.006(7) 0.013(7) 0.002(7) O21 0.052(12) 0.072(14) 0.092(15) -0.004(11) 0.029(11) 0.013(10) O22 0.032(9) 0.092(15) 0.085(14) -0.020(12) 0.021(9) -0.020(10) O23 0.068(12) 0.086(14) 0.043(10) 0.007(10) 0.030(9) -0.022(11) O24 0.089(15) 0.046(11) 0.056(11) 0.008(9) 0.033(10) 0.010(10) O25 0.059(11) 0.044(10) 0.062(11) -0.007(8) 0.018(9) 0.012(8) O26 0.080(14) 0.064(13) 0.061(12) 0.005(10) 0.007(10) 0.031(11) C201 0.020(13) 0.11(3) 0.09(3) -0.02(2) -0.003(15) 0.020(16) C202 0.06(2) 0.13(4) 0.12(3) -0.01(3) 0.05(2) 0.01(2) C203 0.068(14) 0.070(14) 0.072(14) 0.004(12) 0.054(12) -0.005(12) C204 0.08(3) 0.07(2) 0.052(18) 0.004(16) 0.006(17) -0.019(18) C205 0.097(18) 0.061(14) 0.055(13) -0.006(10) 0.012(13) -0.028(13) C206 0.097(18) 0.061(14) 0.055(13) -0.006(10) 0.012(13) -0.028(13) C207 0.07(2) 0.045(18) 0.07(2) -0.015(15) 0.002(17) 0.024(15) C208 0.058(16) 0.069(19) 0.065(17) -0.032(15) 0.029(14) 0.003(14) C209 0.11(2) 0.065(18) 0.042(13) -0.001(13) 0.046(16) 0.020(17) C210 0.10(3) 0.12(3) 0.041(16) 0.009(18) 0.030(17) 0.00(2) C211 0.07(3) 0.17(4) 0.048(18) 0.02(2) -0.007(17) 0.04(3) C212 0.075(16) 0.086(17) 0.073(16) 0.024(14) 0.003(13) 0.028(14) O1A 0.05(2) 0.17(4) 0.17(5) -0.04(4) 0.03(3) -0.02(3) O2A 0.11(2) 0.09(2) 0.11(2) -0.011(17) 0.043(17) -0.032(17) O3A 0.12(2) 0.11(2) 0.12(2) 0.014(18) 0.025(17) -0.001(17) O4A 0.15(4) 0.07(2) 0.11(3) -0.04(2) -0.01(3) 0.03(2) O5A 0.17(5) 0.05(2) 0.11(3) -0.01(2) 0.06(3) 0.01(3) O6A 0.037(18) 0.08(2) 0.12(4) 0.01(2) -0.020(16) 0.018(16) C1A 0.05(2) 0.17(4) 0.17(5) -0.04(4) 0.03(3) -0.02(3) C2A 0.13(3) 0.13(3) 0.13(3) -0.016(19) 0.05(2) -0.006(19) C3A 0.07(4) 0.23(10) 0.12(6) 0.05(6) 0.04(4) -0.01(6) C4A 0.18(7) 0.14(6) 0.04(3) 0.03(4) 0.00(4) -0.05(6) C5A 0.09(2) 0.06(2) 0.08(2) 0.018(18) 0.006(17) -0.002(17) C6A 0.11(5) 0.05(3) 0.12(6) 0.00(4) 0.02(5) 0.03(3) C7A 0.15(4) 0.07(2) 0.11(3) -0.04(2) -0.01(3) 0.03(2) C8A 0.12(5) 0.21(8) 0.09(4) -0.07(5) 0.06(4) -0.02(5) C9A 0.06(4) 0.15(6) 0.10(5) -0.01(5) 0.00(4) 0.01(4) C10A 0.037(18) 0.08(2) 0.12(4) 0.01(2) -0.020(16) 0.018(16) C11A 0.10(6) 0.16(7) 0.22(9) -0.07(7) -0.03(6) 0.04(6) C12A 0.14(8) 0.20(9) 0.14(8) -0.02(6) 0.10(6) 0.02(7) _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 As11 As14 2.3556(19) . ? As11 As12 2.4149(19) . ? As11 As13 2.4176(19) . ? As12 As15 2.363(2) . ? As12 Tl1 2.9209(16) . ? As13 As16 2.372(2) . ? As13 Tl1 2.9385(15) . ? As13 K2 3.825(3) . ? As14 As17 2.354(2) . ? As14 K2 3.457(3) . ? As14 K1 3.631(3) . ? As15 As17 2.479(2) . ? As15 As16 2.629(2) . ? As15 Tl1 3.1469(16) . ? As15 K1 3.861(3) . ? As16 As17 2.456(2) . ? As16 Tl1 3.1818(16) . ? As17 K1 3.697(3) . ? K1 O16 2.800(9) . ? K1 O14 2.876(9) . ? K1 O12 2.883(9) . ? K1 O11 2.909(9) . ? K1 O15 2.929(9) . ? K1 O13 2.940(9) . ? K2 O5A 2.80(3) . ? K2 O3A 2.82(3) . ? K2 O22 2.826(15) . ? K2 O4A 2.82(3) . ? K2 O24 2.841(16) . ? K2 O6A 2.87(2) . ? K2 O23 2.857(16) . ? K2 O21 2.864(16) . ? K2 O26 2.868(15) . ? K2 O1A 2.90(3) . ? K2 O25 2.961(15) . ? K2 O2A 3.00(3) . ? O11 C112 1.403(16) . ? O11 C101 1.429(16) . ? O12 C102 1.397(16) . ? O12 C103 1.398(15) . ? O13 C105 1.407(17) . ? O13 C104 1.413(16) . ? O14 C106 1.413(16) . ? O14 C107 1.424(16) . ? O15 C108 1.394(19) . ? O15 C109 1.400(15) . ? O16 C110 1.403(16) . ? O16 C111 1.439(17) . ? C101 C102 1.47(2) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.51(2) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.49(2) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.51(2) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.50(2) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.48(2) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? O21 C212 1.41(2) . ? O21 C201 1.41(2) . ? O22 C202 1.37(2) . ? O22 C203 1.39(2) . ? O23 C205 1.40(2) . ? O23 C204 1.41(2) . ? O24 C207 1.39(2) . ? O24 C206 1.40(2) . ? O25 C208 1.39(2) . ? O25 C209 1.40(2) . ? O26 C210 1.38(2) . ? O26 C211 1.43(2) . ? C201 C202 1.45(3) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.50(2) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.47(2) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.51(3) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.49(3) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.47(3) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? O1A C12A 1.39(2) . ? O1A C1A 1.40(2) . ? O2A C2A 1.37(2) . ? O2A C3A 1.39(2) . ? O3A C5A 1.39(2) . ? O3A C4A 1.40(2) . ? O4A C6A 1.40(2) . ? O4A C7A 1.40(2) . ? O5A C8A 1.39(2) . ? O5A C9A 1.41(2) . ? O6A C10A 1.38(2) . ? O6A C11A 1.43(2) . ? C1A C2A 1.44(3) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A C4A 1.50(3) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.48(3) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C8A 1.51(3) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C9A C10A 1.49(3) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A H10S 0.9900 . ? C10A H10T 0.9900 . ? C11A C12A 1.47(3) . ? C11A H11G 0.9900 . ? C11A H11H 0.9900 . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? 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 As14 As11 As12 100.20(7) . . ? As14 As11 As13 103.64(7) . . ? As12 As11 As13 98.86(7) . . ? As15 As12 As11 101.24(7) . . ? As15 As12 Tl1 72.23(5) . . ? As11 As12 Tl1 89.97(6) . . ? As16 As13 As11 100.36(7) . . ? As16 As13 Tl1 72.74(5) . . ? As11 As13 Tl1 89.50(5) . . ? As16 As13 K2 84.36(7) . . ? As11 As13 K2 83.27(7) . . ? Tl1 As13 K2 154.35(7) . . ? As17 As14 As11 99.36(7) . . ? As17 As14 K2 88.13(8) . . ? As11 As14 K2 92.85(8) . . ? As17 As14 K1 72.80(7) . . ? As11 As14 K1 104.93(7) . . ? K2 As14 K1 155.60(8) . . ? As12 As15 As17 103.56(7) . . ? As12 As15 As16 102.61(7) . . ? As17 As15 As16 57.40(6) . . ? As12 As15 Tl1 62.11(5) . . ? As17 As15 Tl1 116.55(6) . . ? As16 As15 Tl1 66.15(5) . . ? As12 As15 K1 76.50(7) . . ? As17 As15 K1 67.31(6) . . ? As16 As15 K1 122.94(7) . . ? Tl1 As15 K1 138.37(6) . . ? As13 As16 As17 104.71(7) . . ? As13 As16 As15 102.80(7) . . ? As17 As16 As15 58.25(6) . . ? As13 As16 Tl1 61.88(5) . . ? As17 As16 Tl1 116.06(6) . . ? As15 As16 Tl1 64.77(5) . . ? As14 As17 As16 107.08(7) . . ? As14 As17 As15 105.27(7) . . ? As16 As17 As15 64.36(6) . . ? As14 As17 K1 69.74(7) . . ? As16 As17 K1 136.41(8) . . ? As15 As17 K1 74.48(7) . . ? As12 Tl1 As13 77.58(4) . . ? As12 Tl1 As15 45.66(4) . . ? As13 Tl1 As15 79.91(4) . . ? As12 Tl1 As16 79.31(4) . . ? As13 Tl1 As16 45.39(4) . . ? As15 Tl1 As16 49.08(4) . . ? O16 K1 O14 117.7(3) . . ? O16 K1 O12 115.9(3) . . ? O14 K1 O12 116.3(3) . . ? O16 K1 O11 58.4(3) . . ? O14 K1 O11 154.7(3) . . ? O12 K1 O11 57.9(3) . . ? O16 K1 O15 59.8(3) . . ? O14 K1 O15 57.9(3) . . ? O12 K1 O15 148.2(3) . . ? O11 K1 O15 112.4(3) . . ? O16 K1 O13 148.9(3) . . ? O14 K1 O13 57.9(3) . . ? O12 K1 O13 58.4(3) . . ? O11 K1 O13 111.0(3) . . ? O15 K1 O13 107.5(3) . . ? O16 K1 As14 100.5(2) . . ? O14 K1 As14 74.0(2) . . ? O12 K1 As14 125.7(2) . . ? O11 K1 As14 130.6(2) . . ? O15 K1 As14 84.5(2) . . ? O13 K1 As14 106.6(2) . . ? O16 K1 As17 133.1(2) . . ? O14 K1 As17 77.3(2) . . ? O12 K1 As17 90.1(2) . . ? O11 K1 As17 125.0(2) . . ? O15 K1 As17 115.9(2) . . ? O13 K1 As17 77.8(2) . . ? As14 K1 As17 37.46(5) . . ? O16 K1 As15 116.0(2) . . ? O14 K1 As15 114.4(2) . . ? O12 K1 As15 66.48(19) . . ? O11 K1 As15 86.8(2) . . ? O15 K1 As15 145.3(2) . . ? O13 K1 As15 90.7(2) . . ? As14 K1 As15 61.61(6) . . ? As17 K1 As15 38.22(5) . . ? O5A K2 O3A 117.7(9) . . ? O5A K2 O22 134.2(9) . . ? O3A K2 O22 87.7(8) . . ? O5A K2 O4A 59.3(6) . . ? O3A K2 O4A 59.0(7) . . ? O22 K2 O4A 135.6(9) . . ? O5A K2 O24 88.1(6) . . ? O3A K2 O24 31.7(7) . . ? O22 K2 O24 117.9(5) . . ? O4A K2 O24 28.9(6) . . ? O5A K2 O6A 59.4(7) . . ? O3A K2 O6A 156.4(12) . . ? O22 K2 O6A 81.9(7) . . ? O4A K2 O6A 116.4(8) . . ? O24 K2 O6A 144.5(7) . . ? O5A K2 O23 136.9(8) . . ? O3A K2 O23 28.1(7) . . ? O22 K2 O23 59.6(4) . . ? O4A K2 O23 83.9(8) . . ? O24 K2 O23 59.1(4) . . ? O6A K2 O23 136.4(8) . . ? O5A K2 O21 79.9(7) . . ? O3A K2 O21 140.8(10) . . ? O22 K2 O21 59.2(4) . . ? O4A K2 O21 131.1(8) . . ? O24 K2 O21 151.9(6) . . ? O6A K2 O21 22.7(7) . . ? O23 K2 O21 115.3(5) . . ? O5A K2 O26 27.2(6) . . ? O3A K2 O26 144.8(8) . . ? O22 K2 O26 116.8(5) . . ? O4A K2 O26 86.4(7) . . ? O24 K2 O26 115.1(4) . . ? O6A K2 O26 35.3(6) . . ? O23 K2 O26 156.6(6) . . ? O21 K2 O26 57.8(4) . . ? O5A K2 O1A 114.7(9) . . ? O3A K2 O1A 114.8(9) . . ? O22 K2 O1A 27.1(8) . . ? O4A K2 O1A 151.8(13) . . ? O24 K2 O1A 144.3(9) . . ? O6A K2 O1A 56.7(7) . . ? O23 K2 O1A 86.7(8) . . ? O21 K2 O1A 34.9(7) . . ? O26 K2 O1A 92.0(8) . . ? O5A K2 O25 30.9(5) . . ? O3A K2 O25 88.0(8) . . ? O22 K2 O25 148.7(5) . . ? O4A K2 O25 29.0(7) . . ? O24 K2 O25 57.4(4) . . ? O6A K2 O25 90.0(7) . . ? O23 K2 O25 111.9(5) . . ? O21 K2 O25 109.0(5) . . ? O26 K2 O25 57.7(4) . . ? O1A K2 O25 142.1(9) . . ? O5A K2 O2A 149.5(12) . . ? O3A K2 O2A 58.5(7) . . ? O22 K2 O2A 29.6(7) . . ? O4A K2 O2A 112.9(9) . . ? O24 K2 O2A 89.6(8) . . ? O6A K2 O2A 110.8(8) . . ? O23 K2 O2A 30.5(7) . . ? O21 K2 O2A 88.1(8) . . ? O26 K2 O2A 144.3(9) . . ? O1A K2 O2A 56.6(7) . . ? O25 K2 O2A 138.4(8) . . ? C112 O11 C101 112.4(10) . . ? C112 O11 K1 109.3(8) . . ? C101 O11 K1 107.7(7) . . ? C102 O12 C103 115.1(10) . . ? C102 O12 K1 118.3(7) . . ? C103 O12 K1 118.2(7) . . ? C105 O13 C104 112.1(10) . . ? C105 O13 K1 109.2(8) . . ? C104 O13 K1 110.6(8) . . ? C106 O14 C107 110.7(10) . . ? C106 O14 K1 119.7(8) . . ? C107 O14 K1 119.8(8) . . ? C108 O15 C109 112.5(12) . . ? C108 O15 K1 108.8(8) . . ? C109 O15 K1 107.7(8) . . ? C110 O16 C111 111.7(11) . . ? C110 O16 K1 117.5(8) . . ? C111 O16 K1 120.2(7) . . ? O11 C101 C102 108.4(11) . . ? O11 C101 H10A 110.0 . . ? C102 C101 H10A 110.0 . . ? O11 C101 H10B 110.0 . . ? C102 C101 H10B 110.0 . . ? H10A C101 H10B 108.4 . . ? O12 C102 C101 110.7(11) . . ? O12 C102 H10C 109.5 . . ? C101 C102 H10C 109.5 . . ? O12 C102 H10D 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 108.1 . . ? O12 C103 C104 110.0(11) . . ? O12 C103 H10E 109.7 . . ? C104 C103 H10E 109.7 . . ? O12 C103 H10F 109.7 . . ? C104 C103 H10F 109.7 . . ? H10E C103 H10F 108.2 . . ? O13 C104 C103 109.3(11) . . ? O13 C104 H10G 109.8 . . ? C103 C104 H10G 109.8 . . ? O13 C104 H10H 109.8 . . ? C103 C104 H10H 109.8 . . ? H10G C104 H10H 108.3 . . ? O13 C105 C106 110.1(11) . . ? O13 C105 H10I 109.6 . . ? C106 C105 H10I 109.6 . . ? O13 C105 H10J 109.6 . . ? C106 C105 H10J 109.6 . . ? H10I C105 H10J 108.2 . . ? O14 C106 C105 109.3(11) . . ? O14 C106 H10K 109.8 . . ? C105 C106 H10K 109.8 . . ? O14 C106 H10L 109.8 . . ? C105 C106 H10L 109.8 . . ? H10K C106 H10L 108.3 . . ? O14 C107 C108 108.7(11) . . ? O14 C107 H10M 109.9 . . ? C108 C107 H10M 109.9 . . ? O14 C107 H10N 109.9 . . ? C108 C107 H10N 109.9 . . ? H10M C107 H10N 108.3 . . ? O15 C108 C107 110.0(13) . . ? O15 C108 H10O 109.7 . . ? C107 C108 H10O 109.7 . . ? O15 C108 H10P 109.7 . . ? C107 C108 H10P 109.7 . . ? H10O C108 H10P 108.2 . . ? O15 C109 C110 109.8(12) . . ? O15 C109 H10Q 109.7 . . ? C110 C109 H10Q 109.7 . . ? O15 C109 H10R 109.7 . . ? C110 C109 H10R 109.7 . . ? H10Q C109 H10R 108.2 . . ? O16 C110 C109 108.8(12) . . ? O16 C110 H11A 109.9 . . ? C109 C110 H11A 109.9 . . ? O16 C110 H11B 109.9 . . ? C109 C110 H11B 109.9 . . ? H11A C110 H11B 108.3 . . ? O16 C111 C112 109.8(11) . . ? O16 C111 H11C 109.7 . . ? C112 C111 H11C 109.7 . . ? O16 C111 H11D 109.7 . . ? C112 C111 H11D 109.7 . . ? H11C C111 H11D 108.2 . . ? O11 C112 C111 109.3(12) . . ? O11 C112 H11E 109.8 . . ? C111 C112 H11E 109.8 . . ? O11 C112 H11F 109.8 . . ? C111 C112 H11F 109.8 . . ? H11E C112 H11F 108.3 . . ? C212 O21 C201 113.3(19) . . ? C212 O21 K2 109.3(15) . . ? C201 O21 K2 113.1(13) . . ? C202 O22 C203 117.6(17) . . ? C202 O22 K2 117.2(14) . . ? C203 O22 K2 119.0(12) . . ? C205 O23 C204 114.0(16) . . ? C205 O23 K2 106.5(12) . . ? C204 O23 K2 108.9(16) . . ? C207 O24 C206 117.0(17) . . ? C207 O24 K2 122.8(12) . . ? C206 O24 K2 117.6(13) . . ? C208 O25 C209 112.6(17) . . ? C208 O25 K2 111.7(12) . . ? C209 O25 K2 110.7(12) . . ? C210 O26 C211 113.7(18) . . ? C210 O26 K2 121.2(13) . . ? C211 O26 K2 118.5(13) . . ? O21 C201 C202 111(2) . . ? O21 C201 H20A 109.5 . . ? C202 C201 H20A 109.5 . . ? O21 C201 H20B 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 108.1 . . ? O22 C202 C201 115(2) . . ? O22 C202 H20C 108.5 . . ? C201 C202 H20C 108.5 . . ? O22 C202 H20D 108.5 . . ? C201 C202 H20D 108.5 . . ? H20C C202 H20D 107.5 . . ? O22 C203 C204 110.2(19) . . ? O22 C203 H20E 109.6 . . ? C204 C203 H20E 109.6 . . ? O22 C203 H20F 109.6 . . ? C204 C203 H20F 109.6 . . ? H20E C203 H20F 108.1 . . ? O23 C204 C203 111.0(19) . . ? O23 C204 H20G 109.4 . . ? C203 C204 H20G 109.4 . . ? O23 C204 H20H 109.4 . . ? C203 C204 H20H 109.4 . . ? H20G C204 H20H 108.0 . . ? O23 C205 C206 112(2) . . ? O23 C205 K2 51.1(10) . . ? C206 C205 K2 85.2(13) . . ? O23 C205 H20I 109.2 . . ? C206 C205 H20I 109.2 . . ? K2 C205 H20I 79.2 . . ? O23 C205 H20J 109.2 . . ? C206 C205 H20J 109.2 . . ? K2 C205 H20J 159.8 . . ? H20I C205 H20J 107.9 . . ? O24 C206 C205 113(2) . . ? O24 C206 H20K 108.9 . . ? C205 C206 H20K 108.9 . . ? O24 C206 H20L 108.9 . . ? C205 C206 H20L 108.9 . . ? H20K C206 H20L 107.8 . . ? O24 C207 C208 109.2(18) . . ? O24 C207 H20M 109.8 . . ? C208 C207 H20M 109.8 . . ? O24 C207 H20N 109.8 . . ? C208 C207 H20N 109.8 . . ? H20M C207 H20N 108.3 . . ? O25 C208 C207 111.7(18) . . ? O25 C208 H20O 109.3 . . ? C207 C208 H20O 109.3 . . ? O25 C208 H20P 109.3 . . ? C207 C208 H20P 109.3 . . ? H20O C208 H20P 107.9 . . ? O25 C209 C210 112(2) . . ? O25 C209 H20Q 109.2 . . ? C210 C209 H20Q 109.2 . . ? O25 C209 H20R 109.2 . . ? C210 C209 H20R 109.2 . . ? H20Q C209 H20R 107.9 . . ? O26 C210 C209 111.8(19) . . ? O26 C210 H21A 109.3 . . ? C209 C210 H21A 109.3 . . ? O26 C210 H21B 109.3 . . ? C209 C210 H21B 109.3 . . ? H21A C210 H21B 107.9 . . ? O26 C211 C212 108.9(19) . . ? O26 C211 H21C 109.9 . . ? C212 C211 H21C 109.9 . . ? O26 C211 H21D 109.9 . . ? C212 C211 H21D 109.9 . . ? H21C C211 H21D 108.3 . . ? O21 C212 C211 109(2) . . ? O21 C212 H21E 109.9 . . ? C211 C212 H21E 109.9 . . ? O21 C212 H21F 109.9 . . ? C211 C212 H21F 109.9 . . ? H21E C212 H21F 108.3 . . ? C12A O1A C1A 119(2) . . ? C12A O1A K2 118(2) . . ? C1A O1A K2 122.0(18) . . ? C2A O2A C3A 120(3) . . ? C2A O2A K2 111(3) . . ? C3A O2A K2 112(3) . . ? C5A O3A C4A 118(3) . . ? C5A O3A K2 118.5(16) . . ? C4A O3A K2 120.1(19) . . ? C6A O4A C7A 117(2) . . ? C6A O4A K2 110(2) . . ? C7A O4A K2 116(2) . . ? C8A O5A C9A 112(2) . . ? C8A O5A K2 117(2) . . ? C9A O5A K2 118(2) . . ? C10A O6A C11A 116(3) . . ? C10A O6A K2 113(2) . . ? C11A O6A K2 104(3) . . ? O1A C1A C2A 114(3) . . ? O1A C1A H1A1 108.8 . . ? C2A C1A H1A1 108.8 . . ? O1A C1A H1A2 108.8 . . ? C2A C1A H1A2 108.8 . . ? H1A1 C1A H1A2 107.7 . . ? O2A C2A C1A 118(3) . . ? O2A C2A H2A1 107.7 . . ? C1A C2A H2A1 107.7 . . ? O2A C2A H2A2 107.7 . . ? C1A C2A H2A2 107.7 . . ? H2A1 C2A H2A2 107.1 . . ? O2A C3A C4A 112(3) . . ? O2A C3A H3A1 109.2 . . ? C4A C3A H3A1 109.2 . . ? O2A C3A H3A2 109.2 . . ? C4A C3A H3A2 109.2 . . ? H3A1 C3A H3A2 107.9 . . ? O3A C4A C3A 111(3) . . ? O3A C4A H4A1 109.4 . . ? C3A C4A H4A1 109.4 . . ? O3A C4A H4A2 109.4 . . ? C3A C4A H4A2 109.4 . . ? H4A1 C4A H4A2 108.0 . . ? O3A C5A C6A 115(3) . . ? O3A C5A H5A1 108.4 . . ? C6A C5A H5A1 108.4 . . ? O3A C5A H5A2 108.4 . . ? C6A C5A H5A2 108.4 . . ? H5A1 C5A H5A2 107.5 . . ? O4A C6A C5A 113(3) . . ? O4A C6A H6A1 108.9 . . ? C5A C6A H6A1 108.9 . . ? O4A C6A H6A2 108.9 . . ? C5A C6A H6A2 108.9 . . ? H6A1 C6A H6A2 107.7 . . ? O4A C7A C8A 109(3) . . ? O4A C7A H7A1 109.9 . . ? C8A C7A H7A1 109.9 . . ? O4A C7A H7A2 109.9 . . ? C8A C7A H7A2 109.9 . . ? H7A1 C7A H7A2 108.3 . . ? O5A C8A C7A 111(3) . . ? O5A C8A H8A1 109.5 . . ? C7A C8A H8A1 109.5 . . ? O5A C8A H8A2 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 108.1 . . ? O5A C9A C10A 111(3) . . ? O5A C9A H9A1 109.4 . . ? C10A C9A H9A1 109.4 . . ? O5A C9A H9A2 109.4 . . ? C10A C9A H9A2 109.4 . . ? H9A1 C9A H9A2 108.0 . . ? O6A C10A C9A 111(3) . . ? O6A C10A H10S 109.5 . . ? C9A C10A H10S 109.5 . . ? O6A C10A H10T 109.5 . . ? C9A C10A H10T 109.5 . . ? H10S C10A H10T 108.1 . . ? O6A C11A C12A 110(3) . . ? O6A C11A H11G 109.6 . . ? C12A C11A H11G 109.6 . . ? O6A C11A H11H 109.6 . . ? C12A C11A H11H 109.6 . . ? H11G C11A H11H 108.1 . . ? O1A C12A C11A 111(3) . . ? O1A C12A H12A 109.3 . . ? C11A C12A H12A 109.3 . . ? O1A C12A H12B 109.3 . . ? C11A C12A H12B 109.3 . . ? H12A C12A H12B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.812 _refine_diff_density_min -1.624 _refine_diff_density_rms 0.219 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 786258' #TrackingRef '- combined_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]3[SnP15]*en ; _chemical_name_common (K(2,2,2-crypt))3(SnP15)*en _chemical_melting_point ? _chemical_formula_moiety '3(C18 H36 K N2 O6), P15 Sn, C2 H8 N2' _chemical_formula_sum 'C56 H116 K3 N8 O18 P15 Sn' _chemical_formula_weight 1890.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Ibca _symmetry_space_group_name_Hall '-I 2b 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' _cell_length_a 23.8480(3) _cell_length_b 24.4219(4) _cell_length_c 30.8233(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17951.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 64705 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 23.817 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7872 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9152 _exptl_absorpt_correction_T_max 0.9634 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; This sample was poorly crystalline and weakly diffracting. Data were only collected to a maximum theta value of 23.80 Deg. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 13132 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 23.80 _reflns_number_total 6818 _reflns_number_gt 5103 _reflns_threshold_expression >2\s(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure reveals solvent accessible voids of 43 cubic angstroms, however, no solvent molecules could be located. The highest residual electron density is located in close proximity to the cluster or the cryptand moieties. This issue may arise due to highly diordered ethylenediamine molecules present in the lattice. The following constraints/restraints were employed during refinement: EADP Sn1 P8 EXYZ Sn1 P8 ISOR C116 ISOR 0.05 C118 C209 ; _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^)+(0.0510P)^2^+131.5054P] 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 6818 _refine_ls_number_parameters 456 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1420 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.029 _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 P1 P 1.06913(7) 0.21508(7) 0.42761(5) 0.0584(4) Uani 1 1 d . . . P2 P 1.03259(6) 0.15451(6) 0.38376(5) 0.0559(4) Uani 1 1 d . . . P3 P 0.89917(9) 0.22407(6) 0.38162(5) 0.0698(5) Uani 1 1 d . . . P4 P 1.14666(7) 0.17476(7) 0.44338(5) 0.0612(4) Uani 1 1 d . . . P5 P 0.89935(7) 0.35715(6) 0.33727(5) 0.0570(4) Uani 1 1 d . . . P6 P 0.85372(8) 0.27564(7) 0.33485(5) 0.0680(5) Uani 1 1 d . . . P7 P 0.82380(7) 0.34321(8) 0.37881(6) 0.0681(5) Uani 1 1 d . . . P8 P 0.97032(3) 0.20257(3) 0.32774(2) 0.0634(2) Uani 0.50 1 d P . . Sn1 Sn 0.97032(3) 0.20257(3) 0.32774(2) 0.0634(2) Uani 0.50 1 d P . . K1 K 0.59462(5) 0.13322(5) 0.39479(4) 0.0540(3) Uani 1 1 d . . . N1 N 0.5552(3) 0.1069(3) 0.4836(2) 0.099(2) Uani 1 1 d . . . N2 N 0.6327(4) 0.1607(4) 0.3043(2) 0.136(4) Uani 1 1 d . . . O1 O 0.4773(2) 0.1390(2) 0.4129(2) 0.0976(17) Uani 1 1 d . . . O2 O 0.5169(3) 0.1772(3) 0.3332(2) 0.114(2) Uani 1 1 d . . . O3 O 0.61628(18) 0.02902(16) 0.42992(13) 0.0648(11) Uani 1 1 d . . . O4 O 0.6376(2) 0.04895(19) 0.34094(13) 0.0765(13) Uani 1 1 d . . . O5 O 0.6393(3) 0.1913(3) 0.4638(3) 0.122(2) Uani 1 1 d . . . O6 O 0.6858(3) 0.2056(3) 0.3820(3) 0.138(3) Uani 1 1 d . . . C101 C 0.4924(4) 0.1044(4) 0.4841(3) 0.104(3) Uani 1 1 d . . . H10G H 0.4805 0.0679 0.4735 0.125 Uiso 1 1 calc R . . H10H H 0.4793 0.1082 0.5144 0.125 Uiso 1 1 calc R . . C102 C 0.4649(4) 0.1473(4) 0.4570(4) 0.120(3) Uani 1 1 d . . . H10M H 0.4238 0.1459 0.4613 0.144 Uiso 1 1 calc R . . H10N H 0.4783 0.1839 0.4660 0.144 Uiso 1 1 calc R . . C103 C 0.4458(4) 0.1724(4) 0.3835(4) 0.121(3) Uani 1 1 d . . . H10I H 0.4525 0.2115 0.3902 0.145 Uiso 1 1 calc R . . H10J H 0.4053 0.1649 0.3872 0.145 Uiso 1 1 calc R . . C104 C 0.4620(5) 0.1613(6) 0.3390(5) 0.148(4) Uani 1 1 d . . . H10E H 0.4580 0.1217 0.3327 0.177 Uiso 1 1 calc R . . H10F H 0.4374 0.1817 0.3188 0.177 Uiso 1 1 calc R . . C105 C 0.5326(6) 0.1751(6) 0.2879(3) 0.155(5) Uani 1 1 d . . . H10Q H 0.5066 0.1977 0.2704 0.186 Uiso 1 1 calc R . . H10R H 0.5312 0.1370 0.2772 0.186 Uiso 1 1 calc R . . C106 C 0.5922(6) 0.1975(5) 0.2848(3) 0.149(5) Uani 1 1 d . . . H10O H 0.6019 0.2032 0.2539 0.178 Uiso 1 1 calc R . . H10P H 0.5940 0.2335 0.2995 0.178 Uiso 1 1 calc R . . C107 C 0.5794(5) 0.0548(4) 0.4977(3) 0.115(3) Uani 1 1 d . . . H10C H 0.5579 0.0411 0.5229 0.138 Uiso 1 1 calc R . . H10D H 0.6184 0.0612 0.5073 0.138 Uiso 1 1 calc R . . C108 C 0.5794(4) 0.0120(3) 0.4632(3) 0.106(3) Uani 1 1 d . . . H10K H 0.5921 -0.0234 0.4754 0.127 Uiso 1 1 calc R . . H10L H 0.5411 0.0072 0.4515 0.127 Uiso 1 1 calc R . . C109 C 0.6252(3) -0.0131(3) 0.3988(2) 0.079(2) Uani 1 1 d . . . H10A H 0.5888 -0.0242 0.3861 0.095 Uiso 1 1 calc R . . H10B H 0.6419 -0.0454 0.4131 0.095 Uiso 1 1 calc R . . C110 C 0.6620(3) 0.0058(3) 0.3647(2) 0.087(2) Uani 1 1 d . . . H11A H 0.6978 0.0185 0.3776 0.105 Uiso 1 1 calc R . . H11B H 0.6705 -0.0250 0.3448 0.105 Uiso 1 1 calc R . . C111 C 0.6696(5) 0.0647(5) 0.3049(3) 0.142(5) Uani 1 1 d . . . H11I H 0.6750 0.0329 0.2854 0.171 Uiso 1 1 calc R . . H11J H 0.7070 0.0773 0.3146 0.171 Uiso 1 1 calc R . . C112 C 0.6406(5) 0.1105(5) 0.2803(3) 0.146(5) Uani 1 1 d . . . H11C H 0.6628 0.1188 0.2540 0.176 Uiso 1 1 calc R . . H11D H 0.6035 0.0972 0.2706 0.176 Uiso 1 1 calc R . . C113 C 0.5710(5) 0.1502(5) 0.5119(3) 0.134(4) Uani 1 1 d . . . H11G H 0.5645 0.1389 0.5423 0.161 Uiso 1 1 calc R . . H11H H 0.5474 0.1827 0.5059 0.161 Uiso 1 1 calc R . . C114 C 0.6342(5) 0.1656(6) 0.5057(3) 0.148(5) Uani 1 1 d . . . H11O H 0.6465 0.1911 0.5288 0.177 Uiso 1 1 calc R . . H11P H 0.6579 0.1323 0.5070 0.177 Uiso 1 1 calc R . . C115 C 0.6920(5) 0.2108(6) 0.4566(5) 0.152(5) Uani 1 1 d . . . H11E H 0.7182 0.1794 0.4548 0.183 Uiso 1 1 calc R . . H11F H 0.7034 0.2335 0.4817 0.183 Uiso 1 1 calc R . . C116 C 0.6973(4) 0.2425(4) 0.4184(7) 0.171(7) Uani 1 1 d U . . H11M H 0.7356 0.2578 0.4160 0.205 Uiso 1 1 calc R . . H11N H 0.6701 0.2731 0.4186 0.205 Uiso 1 1 calc R . . C117 C 0.6887(6) 0.2336(7) 0.3442(7) 0.195(8) Uani 1 1 d . . . H11Q H 0.7238 0.2552 0.3432 0.235 Uiso 1 1 calc R . . H11R H 0.6567 0.2592 0.3420 0.235 Uiso 1 1 calc R . . C118 C 0.6873(5) 0.1944(8) 0.3073(5) 0.180(8) Uani 1 1 d U . . H11K H 0.7194 0.1689 0.3102 0.216 Uiso 1 1 calc R . . H11L H 0.6923 0.2151 0.2800 0.216 Uiso 1 1 calc R . . K2 K 0.12801(7) 0.5000 0.2500 0.0705(6) Uani 1 2 d S . . N21 N 0.1245(4) 0.4766(3) 0.3451(2) 0.114(3) Uani 1 1 d . . . O21 O 0.1842(2) 0.40583(18) 0.28030(15) 0.0802(13) Uani 1 1 d . . . O22 O 0.16566(18) 0.42001(18) 0.19013(15) 0.0726(12) Uani 1 1 d . . . O23 O 0.0251(3) 0.4980(4) 0.2936(4) 0.157(3) Uani 1 1 d . . . C201 C 0.1673(5) 0.4349(4) 0.3541(3) 0.124(3) Uani 1 1 d . . . H20E H 0.1615 0.4205 0.3838 0.149 Uiso 1 1 calc R . . H20F H 0.2047 0.4523 0.3531 0.149 Uiso 1 1 calc R . . C202 C 0.1663(5) 0.3867(4) 0.3219(3) 0.129(4) Uani 1 1 d . . . H20G H 0.1916 0.3573 0.3321 0.155 Uiso 1 1 calc R . . H20H H 0.1279 0.3716 0.3198 0.155 Uiso 1 1 calc R . . C203 C 0.1832(3) 0.3628(3) 0.2492(3) 0.080(2) Uani 1 1 d . . . H20C H 0.1443 0.3494 0.2455 0.096 Uiso 1 1 calc R . . H20D H 0.2065 0.3318 0.2596 0.096 Uiso 1 1 calc R . . C204 C 0.2047(3) 0.3825(3) 0.2077(2) 0.0782(19) Uani 1 1 d . . . H20A H 0.2414 0.4008 0.2121 0.094 Uiso 1 1 calc R . . H20B H 0.2102 0.3514 0.1876 0.094 Uiso 1 1 calc R . . C205 C 0.1830(4) 0.4397(4) 0.1491(3) 0.112(3) Uani 1 1 d . . . H20M H 0.1921 0.4086 0.1297 0.135 Uiso 1 1 calc R . . H20N H 0.2170 0.4626 0.1523 0.135 Uiso 1 1 calc R . . C206 C 0.1362(5) 0.4732(4) 0.1298(3) 0.130(4) Uani 1 1 d . . . H20O H 0.1462 0.4834 0.0997 0.155 Uiso 1 1 calc R . . H20P H 0.1018 0.4505 0.1286 0.155 Uiso 1 1 calc R . . C207 C 0.0677(5) 0.4571(5) 0.3566(4) 0.142(4) Uani 1 1 d . . . H20K H 0.0643 0.4182 0.3480 0.170 Uiso 1 1 calc R . . H20L H 0.0631 0.4592 0.3884 0.170 Uiso 1 1 calc R . . C208 C 0.0242(5) 0.4869(5) 0.3368(5) 0.150(5) Uani 1 1 d . . . H20I H -0.0111 0.4671 0.3428 0.180 Uiso 1 1 calc R . . H20J H 0.0217 0.5225 0.3521 0.180 Uiso 1 1 calc R . . C209 C -0.0158(6) 0.4909(10) 0.2733(6) 0.286(13) Uani 1 1 d U . . H20Q H -0.0469 0.5099 0.2883 0.343 Uiso 1 1 calc R . . H20R H -0.0243 0.4512 0.2739 0.343 Uiso 1 1 calc R . . C1E C 0.2348(6) 0.0511(7) 0.5195(6) 0.211(9) Uani 1 1 d . . . H1E4 H 0.2609 0.0390 0.5426 0.253 Uiso 1 1 calc R . . H1E5 H 0.2058 0.0222 0.5169 0.253 Uiso 1 1 calc R . . N1E N 0.2060(5) 0.1011(7) 0.5359(3) 0.187(5) Uani 1 1 d . . . H1E1 H 0.1879 0.0932 0.5612 0.281 Uiso 0.67 1 calc PR . . H1E2 H 0.1807 0.1129 0.5159 0.281 Uiso 0.67 1 calc PR . . H1E3 H 0.2318 0.1279 0.5408 0.281 Uiso 0.67 1 calc PR . . 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 P1 0.0683(10) 0.0665(10) 0.0404(8) 0.0060(7) 0.0087(7) 0.0185(8) P2 0.0503(9) 0.0572(9) 0.0603(9) 0.0097(7) 0.0093(7) -0.0015(7) P3 0.1252(16) 0.0417(8) 0.0425(8) -0.0008(6) 0.0043(9) -0.0049(9) P4 0.0565(9) 0.0661(10) 0.0611(9) 0.0002(8) 0.0014(7) 0.0031(8) P5 0.0560(9) 0.0526(9) 0.0623(9) 0.0137(7) -0.0128(7) -0.0072(7) P6 0.0855(12) 0.0659(10) 0.0526(9) 0.0133(8) -0.0180(8) -0.0296(9) P7 0.0506(9) 0.0775(12) 0.0761(11) 0.0199(9) -0.0127(8) -0.0066(8) P8 0.0653(4) 0.0523(4) 0.0725(5) -0.0040(3) 0.0250(3) -0.0070(3) Sn1 0.0653(4) 0.0523(4) 0.0725(5) -0.0040(3) 0.0250(3) -0.0070(3) K1 0.0535(7) 0.0491(7) 0.0594(7) -0.0033(6) 0.0134(6) 0.0021(6) N1 0.130(6) 0.098(5) 0.071(4) -0.019(4) 0.037(4) -0.003(4) N2 0.159(8) 0.165(8) 0.085(5) 0.055(5) 0.049(5) 0.095(7) O1 0.071(3) 0.082(3) 0.140(5) 0.019(3) 0.040(3) 0.017(3) O2 0.094(4) 0.119(5) 0.129(5) 0.034(4) 0.012(4) 0.044(4) O3 0.073(3) 0.059(2) 0.063(2) 0.004(2) 0.007(2) -0.002(2) O4 0.091(3) 0.079(3) 0.059(3) -0.008(2) 0.000(2) 0.037(3) O5 0.093(4) 0.119(5) 0.154(6) -0.057(4) -0.009(4) -0.032(4) O6 0.092(4) 0.126(6) 0.196(8) 0.046(6) 0.042(5) -0.030(4) C101 0.104(7) 0.123(7) 0.086(5) 0.002(5) 0.052(5) -0.003(6) C102 0.115(7) 0.079(6) 0.165(9) -0.009(6) 0.064(7) 0.009(5) C103 0.071(5) 0.107(7) 0.185(11) 0.021(7) 0.010(6) 0.038(5) C104 0.112(9) 0.157(11) 0.174(12) 0.033(9) -0.016(9) 0.032(8) C105 0.186(13) 0.189(12) 0.091(7) 0.035(7) -0.011(8) 0.090(11) C106 0.187(12) 0.150(9) 0.109(7) 0.070(7) 0.074(8) 0.093(9) C107 0.159(9) 0.131(8) 0.056(4) 0.017(5) 0.032(5) 0.021(7) C108 0.124(7) 0.086(6) 0.108(6) 0.029(5) 0.029(6) 0.008(5) C109 0.094(5) 0.050(4) 0.094(5) -0.007(4) -0.019(4) 0.015(4) C110 0.106(6) 0.082(5) 0.074(4) -0.008(4) -0.002(4) 0.048(5) C111 0.202(11) 0.164(9) 0.060(5) 0.015(5) 0.036(6) 0.111(9) C112 0.181(10) 0.201(11) 0.057(5) 0.029(6) 0.036(6) 0.121(10) C113 0.170(11) 0.156(9) 0.076(6) -0.053(6) 0.032(6) -0.022(8) C114 0.141(10) 0.220(13) 0.082(7) -0.087(8) -0.002(6) -0.004(9) C115 0.107(9) 0.117(9) 0.234(15) -0.040(10) -0.032(9) -0.022(7) C116 0.082(7) 0.073(7) 0.36(2) 0.007(11) -0.041(10) -0.036(6) C117 0.139(11) 0.174(14) 0.27(2) 0.085(15) 0.112(13) -0.009(10) C118 0.110(9) 0.242(17) 0.189(13) 0.141(13) 0.085(9) 0.053(10) K2 0.0397(10) 0.0656(12) 0.1064(16) 0.0019(11) 0.000 0.000 N21 0.147(7) 0.092(5) 0.104(5) 0.007(4) 0.055(5) -0.027(5) O21 0.100(4) 0.058(3) 0.083(3) 0.019(2) 0.001(3) -0.011(2) O22 0.064(3) 0.070(3) 0.083(3) 0.010(2) -0.009(2) 0.009(2) O23 0.082(5) 0.187(8) 0.203(9) 0.026(7) 0.034(5) -0.019(5) C201 0.179(10) 0.109(8) 0.084(6) 0.033(6) 0.019(6) -0.001(7) C202 0.193(11) 0.078(6) 0.116(7) 0.040(6) 0.037(7) 0.005(6) C203 0.080(5) 0.052(4) 0.108(6) 0.013(4) -0.017(4) 0.002(3) C204 0.070(4) 0.071(4) 0.093(5) -0.003(4) -0.014(4) 0.015(4) C205 0.145(8) 0.103(7) 0.089(6) 0.003(5) 0.009(6) 0.018(6) C206 0.197(11) 0.097(7) 0.094(6) 0.008(5) -0.031(7) 0.020(7) C207 0.144(10) 0.131(9) 0.151(10) 0.023(8) 0.061(8) -0.056(8) C208 0.135(11) 0.139(10) 0.174(13) 0.060(9) 0.022(9) -0.054(8) C209 0.096(9) 0.42(3) 0.34(3) 0.14(2) -0.022(12) -0.104(15) C1E 0.133(15) 0.204(15) 0.30(3) 0.068(15) 0.013(13) 0.015(11) N1E 0.140(9) 0.310(17) 0.111(7) 0.067(9) 0.003(6) 0.011(10) _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 P1 P4 2.151(2) . ? P1 P2 2.185(2) . ? P1 P3 2.188(2) 6_654 ? P2 P5 2.184(2) 6_654 ? P2 P8 2.5623(17) . ? P3 P1 2.188(2) 6_654 ? P3 P6 2.200(2) . ? P3 P8 2.4317(19) . ? P4 P7 2.156(2) 6_654 ? P5 P2 2.184(2) 6_654 ? P5 P7 2.236(2) . ? P5 P6 2.270(2) . ? P6 P7 2.251(3) . ? P7 P4 2.156(2) 6_654 ? P8 Sn1 2.7148(13) 6_654 ? K1 O5 2.770(6) . ? K1 O3 2.813(4) . ? K1 O6 2.830(6) . ? K1 O4 2.835(4) . ? K1 O1 2.857(5) . ? K1 O2 2.862(6) . ? K1 N1 2.963(6) . ? K1 N2 3.010(7) . ? N1 C113 1.421(10) . ? N1 C107 1.463(10) . ? N1 C101 1.499(11) . ? N2 C112 1.445(13) . ? N2 C106 1.451(11) . ? N2 C118 1.545(18) . ? O1 C102 1.404(10) . ? O1 C103 1.432(10) . ? O2 C104 1.377(12) . ? O2 C105 1.445(12) . ? O3 C108 1.413(8) . ? O3 C109 1.423(7) . ? O4 C111 1.403(10) . ? O4 C110 1.409(8) . ? O5 C115 1.363(13) . ? O5 C114 1.441(13) . ? O6 C117 1.352(16) . ? O6 C116 1.464(15) . ? C101 C102 1.493(12) . ? C101 H10G 0.9900 . ? C101 H10H 0.9900 . ? C102 H10M 0.9900 . ? C102 H10N 0.9900 . ? C103 C104 1.453(14) . ? C103 H10I 0.9900 . ? C103 H10J 0.9900 . ? C104 H10E 0.9900 . ? C104 H10F 0.9900 . ? C105 C106 1.527(16) . ? C105 H10Q 0.9900 . ? C105 H10R 0.9900 . ? C106 H10O 0.9900 . ? C106 H10P 0.9900 . ? C107 C108 1.490(11) . ? C107 H10C 0.9900 . ? C107 H10D 0.9900 . ? C108 H10K 0.9900 . ? C108 H10L 0.9900 . ? C109 C110 1.446(10) . ? C109 H10A 0.9900 . ? C109 H10B 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.517(11) . ? C111 H11I 0.9900 . ? C111 H11J 0.9900 . ? C112 H11C 0.9900 . ? C112 H11D 0.9900 . ? C113 C114 1.567(14) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11O 0.9900 . ? C114 H11P 0.9900 . ? C115 C116 1.414(17) . ? C115 H11E 0.9900 . ? C115 H11F 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.48(2) . ? C117 H11Q 0.9900 . ? C117 H11R 0.9900 . ? C118 H11K 0.9900 . ? C118 H11L 0.9900 . ? K2 O23 2.797(7) 8_455 ? K2 O23 2.797(7) . ? K2 O21 2.821(5) . ? K2 O21 2.821(5) 8_455 ? K2 O22 2.833(5) 8_455 ? K2 O22 2.833(5) . ? K2 N21 2.988(7) . ? K2 N21 2.988(7) 8_455 ? N21 C201 1.467(12) . ? N21 C206 1.477(11) 8_455 ? N21 C207 1.479(12) . ? O21 C203 1.423(8) . ? O21 C202 1.429(9) . ? O22 C204 1.414(7) . ? O22 C205 1.416(9) . ? O23 C209 1.170(15) . ? O23 C208 1.360(13) . ? C201 C202 1.540(13) . ? C201 H20E 0.9900 . ? C201 H20F 0.9900 . ? C202 H20G 0.9900 . ? C202 H20H 0.9900 . ? C203 C204 1.460(10) . ? C203 H20C 0.9900 . ? C203 H20D 0.9900 . ? C204 H20A 0.9900 . ? C204 H20B 0.9900 . ? C205 C206 1.506(12) . ? C205 H20M 0.9900 . ? C205 H20N 0.9900 . ? C206 N21 1.477(11) 8_455 ? C206 H20O 0.9900 . ? C206 H20P 0.9900 . ? C207 C208 1.405(15) . ? C207 H20K 0.9900 . ? C207 H20L 0.9900 . ? C208 H20I 0.9900 . ? C208 H20J 0.9900 . ? C209 C209 1.51(3) 8_455 ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C1E C1E 1.41(3) 7_545 ? C1E N1E 1.491(17) . ? C1E H1E4 0.9900 . ? C1E H1E5 0.9900 . ? N1E H1E1 0.9100 . ? N1E H1E2 0.9100 . ? N1E H1E3 0.9100 . ? 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 P4 P1 P2 99.94(9) . . ? P4 P1 P3 99.22(10) . 6_654 ? P2 P1 P3 101.36(8) . 6_654 ? P5 P2 P1 101.41(8) 6_654 . ? P5 P2 P8 92.77(7) 6_654 . ? P1 P2 P8 109.74(8) . . ? P1 P3 P6 101.89(9) 6_654 . ? P1 P3 P8 110.36(10) 6_654 . ? P6 P3 P8 91.13(8) . . ? P1 P4 P7 99.52(9) . 6_654 ? P2 P5 P7 101.73(9) 6_654 . ? P2 P5 P6 105.29(8) 6_654 . ? P7 P5 P6 59.94(8) . . ? P3 P6 P7 100.44(9) . . ? P3 P6 P5 104.13(9) . . ? P7 P6 P5 59.29(8) . . ? P4 P7 P5 107.23(9) 6_654 . ? P4 P7 P6 107.63(10) 6_654 . ? P5 P7 P6 60.77(8) . . ? P3 P8 P2 92.47(6) . . ? P3 P8 Sn1 100.35(5) . 6_654 ? P2 P8 Sn1 95.09(4) . 6_654 ? O5 K1 O3 95.57(19) . . ? O5 K1 O6 59.4(3) . . ? O3 K1 O6 118.55(18) . . ? O5 K1 O4 133.02(17) . . ? O3 K1 O4 60.16(13) . . ? O6 K1 O4 95.4(2) . . ? O5 K1 O1 101.6(2) . . ? O3 K1 O1 98.57(14) . . ? O6 K1 O1 138.50(19) . . ? O4 K1 O1 120.27(16) . . ? O5 K1 O2 124.5(2) . . ? O3 K1 O2 135.50(18) . . ? O6 K1 O2 99.8(2) . . ? O4 K1 O2 96.77(16) . . ? O1 K1 O2 58.47(18) . . ? O5 K1 N1 61.6(2) . . ? O3 K1 N1 60.45(17) . . ? O6 K1 N1 120.5(3) . . ? O4 K1 N1 119.86(17) . . ? O1 K1 N1 61.3(2) . . ? O2 K1 N1 119.2(2) . . ? O5 K1 N2 118.8(3) . . ? O3 K1 N2 120.21(18) . . ? O6 K1 N2 60.0(3) . . ? O4 K1 N2 60.7(2) . . ? O1 K1 N2 117.8(2) . . ? O2 K1 N2 59.8(2) . . ? N1 K1 N2 179.0(2) . . ? C113 N1 C107 111.2(8) . . ? C113 N1 C101 106.8(7) . . ? C107 N1 C101 110.7(8) . . ? C113 N1 K1 108.8(5) . . ? C107 N1 K1 109.7(4) . . ? C101 N1 K1 109.6(5) . . ? C112 N2 C106 113.7(9) . . ? C112 N2 C118 111.9(10) . . ? C106 N2 C118 104.9(10) . . ? C112 N2 K1 109.0(6) . . ? C106 N2 K1 108.8(5) . . ? C118 N2 K1 108.5(7) . . ? C102 O1 C103 114.7(7) . . ? C102 O1 K1 113.7(5) . . ? C103 O1 K1 114.7(5) . . ? C104 O2 C105 111.2(10) . . ? C104 O2 K1 115.1(6) . . ? C105 O2 K1 117.4(5) . . ? C108 O3 C109 111.7(6) . . ? C108 O3 K1 115.6(4) . . ? C109 O3 K1 114.9(4) . . ? C111 O4 C110 113.1(6) . . ? C111 O4 K1 117.5(5) . . ? C110 O4 K1 112.8(4) . . ? C115 O5 C114 112.1(10) . . ? C115 O5 K1 114.1(7) . . ? C114 O5 K1 115.7(5) . . ? C117 O6 C116 109.9(12) . . ? C117 O6 K1 118.4(9) . . ? C116 O6 K1 114.9(7) . . ? C102 C101 N1 113.8(7) . . ? C102 C101 H10G 108.8 . . ? N1 C101 H10G 108.8 . . ? C102 C101 H10H 108.8 . . ? N1 C101 H10H 108.8 . . ? H10G C101 H10H 107.7 . . ? O1 C102 C101 110.3(7) . . ? O1 C102 H10M 109.6 . . ? C101 C102 H10M 109.6 . . ? O1 C102 H10N 109.6 . . ? C101 C102 H10N 109.6 . . ? H10M C102 H10N 108.1 . . ? O1 C103 C104 110.6(8) . . ? O1 C103 H10I 109.5 . . ? C104 C103 H10I 109.5 . . ? O1 C103 H10J 109.5 . . ? C104 C103 H10J 109.5 . . ? H10I C103 H10J 108.1 . . ? O2 C104 C103 108.8(11) . . ? O2 C104 H10E 109.9 . . ? C103 C104 H10E 109.9 . . ? O2 C104 H10F 109.9 . . ? C103 C104 H10F 109.9 . . ? H10E C104 H10F 108.3 . . ? O2 C105 C106 106.9(10) . . ? O2 C105 H10Q 110.3 . . ? C106 C105 H10Q 110.3 . . ? O2 C105 H10R 110.3 . . ? C106 C105 H10R 110.3 . . ? H10Q C105 H10R 108.6 . . ? N2 C106 C105 111.8(9) . . ? N2 C106 H10O 109.3 . . ? C105 C106 H10O 109.3 . . ? N2 C106 H10P 109.3 . . ? C105 C106 H10P 109.3 . . ? H10O C106 H10P 107.9 . . ? N1 C107 C108 113.5(7) . . ? N1 C107 H10C 108.9 . . ? C108 C107 H10C 108.9 . . ? N1 C107 H10D 108.9 . . ? C108 C107 H10D 108.9 . . ? H10C C107 H10D 107.7 . . ? O3 C108 C107 108.1(7) . . ? O3 C108 H10K 110.1 . . ? C107 C108 H10K 110.1 . . ? O3 C108 H10L 110.1 . . ? C107 C108 H10L 110.1 . . ? H10K C108 H10L 108.4 . . ? O3 C109 C110 110.5(6) . . ? O3 C109 H10A 109.5 . . ? C110 C109 H10A 109.5 . . ? O3 C109 H10B 109.5 . . ? C110 C109 H10B 109.5 . . ? H10A C109 H10B 108.1 . . ? O4 C110 C109 111.4(6) . . ? O4 C110 H11A 109.4 . . ? C109 C110 H11A 109.4 . . ? O4 C110 H11B 109.4 . . ? C109 C110 H11B 109.4 . . ? H11A C110 H11B 108.0 . . ? O4 C111 C112 110.5(7) . . ? O4 C111 H11I 109.5 . . ? C112 C111 H11I 109.5 . . ? O4 C111 H11J 109.5 . . ? C112 C111 H11J 109.5 . . ? H11I C111 H11J 108.1 . . ? N2 C112 C111 115.4(8) . . ? N2 C112 H11C 108.4 . . ? C111 C112 H11C 108.4 . . ? N2 C112 H11D 108.4 . . ? C111 C112 H11D 108.4 . . ? H11C C112 H11D 107.5 . . ? N1 C113 C114 111.0(8) . . ? N1 C113 H11G 109.4 . . ? C114 C113 H11G 109.4 . . ? N1 C113 H11H 109.4 . . ? C114 C113 H11H 109.4 . . ? H11G C113 H11H 108.0 . . ? O5 C114 C113 107.1(9) . . ? O5 C114 H11O 110.3 . . ? C113 C114 H11O 110.3 . . ? O5 C114 H11P 110.3 . . ? C113 C114 H11P 110.3 . . ? H11O C114 H11P 108.6 . . ? O5 C115 C116 114.1(11) . . ? O5 C115 H11E 108.7 . . ? C116 C115 H11E 108.7 . . ? O5 C115 H11F 108.7 . . ? C116 C115 H11F 108.7 . . ? H11E C115 H11F 107.6 . . ? C115 C116 O6 106.6(9) . . ? C115 C116 H11M 110.4 . . ? O6 C116 H11M 110.4 . . ? C115 C116 H11N 110.4 . . ? O6 C116 H11N 110.4 . . ? H11M C116 H11N 108.6 . . ? O6 C117 C118 109.5(13) . . ? O6 C117 H11Q 109.8 . . ? C118 C117 H11Q 109.8 . . ? O6 C117 H11R 109.8 . . ? C118 C117 H11R 109.8 . . ? H11Q C117 H11R 108.2 . . ? C117 C118 N2 114.1(10) . . ? C117 C118 H11K 108.7 . . ? N2 C118 H11K 108.7 . . ? C117 C118 H11L 108.7 . . ? N2 C118 H11L 108.7 . . ? H11K C118 H11L 107.6 . . ? O23 K2 O23 57.4(5) 8_455 . ? O23 K2 O21 126.1(2) 8_455 . ? O23 K2 O21 104.1(2) . . ? O23 K2 O21 104.1(2) 8_455 8_455 ? O23 K2 O21 126.1(2) . 8_455 ? O21 K2 O21 123.3(2) . 8_455 ? O23 K2 O22 125.3(2) 8_455 8_455 ? O23 K2 O22 88.7(2) . 8_455 ? O21 K2 O22 101.30(14) . 8_455 ? O21 K2 O22 60.20(13) 8_455 8_455 ? O23 K2 O22 88.7(2) 8_455 . ? O23 K2 O22 125.3(2) . . ? O21 K2 O22 60.20(13) . . ? O21 K2 O22 101.30(14) 8_455 . ? O22 K2 O22 143.06(19) 8_455 . ? O23 K2 N21 116.8(3) 8_455 . ? O23 K2 N21 60.1(3) . . ? O21 K2 N21 62.1(2) . . ? O21 K2 N21 119.60(18) 8_455 . ? O22 K2 N21 60.11(17) 8_455 . ? O22 K2 N21 121.05(19) . . ? O23 K2 N21 60.1(3) 8_455 8_455 ? O23 K2 N21 116.8(3) . 8_455 ? O21 K2 N21 119.60(18) . 8_455 ? O21 K2 N21 62.1(2) 8_455 8_455 ? O22 K2 N21 121.05(19) 8_455 8_455 ? O22 K2 N21 60.11(17) . 8_455 ? N21 K2 N21 176.8(4) . 8_455 ? O23 K2 C209 40.8(4) 8_455 . ? O23 K2 C209 17.0(4) . . ? O21 K2 C209 110.2(4) . . ? O21 K2 C209 125.7(4) 8_455 . ? O22 K2 C209 102.7(4) 8_455 . ? O22 K2 C209 113.5(4) . . ? N21 K2 C209 76.1(3) . . ? N21 K2 C209 100.7(3) 8_455 . ? O23 K2 C209 17.0(4) 8_455 8_455 ? O23 K2 C209 40.8(4) . 8_455 ? O21 K2 C209 125.7(4) . 8_455 ? O21 K2 C209 110.2(4) 8_455 8_455 ? O22 K2 C209 113.5(4) 8_455 8_455 ? O22 K2 C209 102.7(4) . 8_455 ? N21 K2 C209 100.7(3) . 8_455 ? N21 K2 C209 76.1(3) 8_455 8_455 ? C209 K2 C209 24.8(5) . 8_455 ? C201 N21 C206 110.4(9) . 8_455 ? C201 N21 C207 111.6(9) . . ? C206 N21 C207 108.3(8) 8_455 . ? C201 N21 K2 107.3(5) . . ? C206 N21 K2 110.5(5) 8_455 . ? C207 N21 K2 108.7(7) . . ? C203 O21 C202 110.9(6) . . ? C203 O21 K2 111.8(4) . . ? C202 O21 K2 114.9(5) . . ? C204 O22 C205 111.7(6) . . ? C204 O22 K2 113.9(4) . . ? C205 O22 K2 116.1(4) . . ? C209 O23 C208 118.7(11) . . ? C209 O23 K2 118.5(11) . . ? C208 O23 K2 119.2(8) . . ? N21 C201 C202 113.5(9) . . ? N21 C201 H20E 108.9 . . ? C202 C201 H20E 108.9 . . ? N21 C201 H20F 108.9 . . ? C202 C201 H20F 108.9 . . ? H20E C201 H20F 107.7 . . ? O21 C202 C201 108.8(7) . . ? O21 C202 H20G 109.9 . . ? C201 C202 H20G 109.9 . . ? O21 C202 H20H 109.9 . . ? C201 C202 H20H 109.9 . . ? H20G C202 H20H 108.3 . . ? O21 C203 C204 109.8(5) . . ? O21 C203 H20C 109.7 . . ? C204 C203 H20C 109.7 . . ? O21 C203 H20D 109.7 . . ? C204 C203 H20D 109.7 . . ? H20C C203 H20D 108.2 . . ? O22 C204 C203 108.6(6) . . ? O22 C204 H20A 110.0 . . ? C203 C204 H20A 110.0 . . ? O22 C204 H20B 110.0 . . ? C203 C204 H20B 110.0 . . ? H20A C204 H20B 108.4 . . ? O22 C205 C206 108.7(8) . . ? O22 C205 H20M 110.0 . . ? C206 C205 H20M 110.0 . . ? O22 C205 H20N 110.0 . . ? C206 C205 H20N 110.0 . . ? H20M C205 H20N 108.3 . . ? N21 C206 C205 112.5(8) 8_455 . ? N21 C206 H20O 109.1 8_455 . ? C205 C206 H20O 109.1 . . ? N21 C206 H20P 109.1 8_455 . ? C205 C206 H20P 109.1 . . ? H20O C206 H20P 107.8 . . ? C208 C207 N21 113.9(9) . . ? C208 C207 H20K 108.8 . . ? N21 C207 H20K 108.8 . . ? C208 C207 H20L 108.8 . . ? N21 C207 H20L 108.8 . . ? H20K C207 H20L 107.7 . . ? O23 C208 C207 121.0(13) . . ? O23 C208 H20I 107.1 . . ? C207 C208 H20I 107.1 . . ? O23 C208 H20J 107.1 . . ? C207 C208 H20J 107.1 . . ? H20I C208 H20J 106.8 . . ? O23 C209 C209 117.7(12) . 8_455 ? C209 C209 K2 77.6(3) 8_455 . ? O23 C209 H20Q 107.9 . . ? C209 C209 H20Q 107.9 8_455 . ? K2 C209 H20Q 143.0 . . ? O23 C209 H20R 107.9 . . ? C209 C209 H20R 107.9 8_455 . ? K2 C209 H20R 105.5 . . ? H20Q C209 H20R 107.2 . . ? C1E C1E N1E 121.9(9) 7_545 . ? C1E C1E H1E4 106.9 7_545 . ? N1E C1E H1E4 106.9 . . ? C1E C1E H1E5 106.9 7_545 . ? N1E C1E H1E5 106.9 . . ? H1E4 C1E H1E5 106.7 . . ? C1E N1E H1E1 109.5 . . ? C1E N1E H1E2 109.5 . . ? H1E1 N1E H1E2 109.5 . . ? C1E N1E H1E3 109.5 . . ? H1E1 N1E H1E3 109.5 . . ? H1E2 N1E H1E3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.80 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.150 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.073 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 786259' #TrackingRef '- combined_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]3[PbP15]*en ; _chemical_name_common (K(2,2,2-crypt))3(PbP15)*en _chemical_melting_point ? _chemical_formula_moiety '3(C18 H36 K N2 O6), P15 Pb, C2 H8 N2' _chemical_formula_sum 'C56 H116 K3 N8 O18 P15 Pb' _chemical_formula_weight 1978.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Ibca _symmetry_space_group_name_Hall '-I 2b 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' _cell_length_a 23.8547(2) _cell_length_b 24.2093(2) _cell_length_c 30.8457(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17813.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10875 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8128 _exptl_absorpt_coefficient_mu 2.365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5573 _exptl_absorpt_correction_T_max 0.7645 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 15030 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 5.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7792 _reflns_number_gt 6789 _reflns_threshold_expression >2\s(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure reveals solvent accessible voids of 46 cubic angstroms, however, no solvent molecules could be located. The highest residual electron density is located in close proximity to the cluster or the cryptand moieties. This issue may arise due to highly diordered ethylenediamine molecules present in the lattice. The following contraints/restraints were employed during refinement: EADP Pb1 P8 EADP O23 C208 EADP C117 C118 ISOR C117 ISOR 0.05 C104 C105 C111 ISOR 0.02 C106 C118 C209 ; _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^+356.9491P] 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 7792 _refine_ls_number_parameters 447 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0847 _refine_ls_wR_factor_ref 0.1779 _refine_ls_wR_factor_gt 0.1748 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.179 _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 Pb1 Pb 0.53363(3) 0.29966(3) 0.17814(2) 0.04324(19) Uani 0.50 1 d P . . P1 P 0.43055(11) 0.28508(11) 0.07365(7) 0.0590(7) Uani 1 1 d . . . P2 P 0.60168(18) 0.27562(10) 0.11959(8) 0.0827(11) Uani 1 1 d . . . P3 P 0.46669(10) 0.34583(11) 0.11732(8) 0.0551(6) Uani 1 1 d . . . P4 P 0.35336(10) 0.32516(10) 0.05743(8) 0.0537(6) Uani 1 1 d . . . P5 P 0.35410(14) 0.27665(12) 0.16554(8) 0.0748(9) Uani 1 1 d . . . P6 P 0.39875(10) 0.35694(9) 0.16336(8) 0.0524(6) Uani 1 1 d . . . P7 P 0.32393(10) 0.34328(12) 0.12190(10) 0.0664(7) Uani 1 1 d . . . P8 P 0.5182(2) 0.2969(2) 0.16211(18) 0.04324(19) Uani 0.50 1 d P . . K1 K 0.40539(8) 0.36659(7) 0.39614(6) 0.0500(5) Uani 1 1 d . . . N11 N 0.4439(5) 0.3935(5) 0.4848(3) 0.101(4) Uani 1 1 d . . . N12 N 0.3676(7) 0.3390(6) 0.3052(4) 0.136(6) Uani 1 1 d . . . O11 O 0.3601(4) 0.3093(4) 0.4656(5) 0.130(4) Uani 1 1 d . . . O12 O 0.3141(4) 0.2940(5) 0.3824(6) 0.150(5) Uani 1 1 d . . . O13 O 0.5213(3) 0.3601(3) 0.4157(3) 0.099(3) Uani 1 1 d . . . O14 O 0.4831(4) 0.3226(4) 0.3345(4) 0.120(4) Uani 1 1 d . . . O15 O 0.3840(3) 0.4709(3) 0.4307(2) 0.0594(16) Uani 1 1 d . . . O16 O 0.3636(3) 0.4510(3) 0.3421(2) 0.0688(19) Uani 1 1 d . . . C101 C 0.4292(9) 0.3492(8) 0.5124(5) 0.140(7) Uani 1 1 d . . . H10A H 0.4383 0.3589 0.5427 0.168 Uiso 1 1 calc R . . H10B H 0.4511 0.3160 0.5044 0.168 Uiso 1 1 calc R . . C102 C 0.3653(9) 0.3365(10) 0.5083(6) 0.163(9) Uani 1 1 d . . . H10C H 0.3527 0.3117 0.5319 0.195 Uiso 1 1 calc R . . H10D H 0.3430 0.3710 0.5094 0.195 Uiso 1 1 calc R . . C103 C 0.3076(9) 0.2912(9) 0.4588(9) 0.163(9) Uani 1 1 d . . . H10E H 0.2823 0.3234 0.4560 0.195 Uiso 1 1 calc R . . H10F H 0.2953 0.2696 0.4843 0.195 Uiso 1 1 calc R . . C104 C 0.3028(8) 0.2577(8) 0.4209(10) 0.169(10) Uani 1 1 d U . . H10G H 0.2646 0.2418 0.4190 0.202 Uiso 1 1 calc R . . H10H H 0.3302 0.2271 0.4220 0.202 Uiso 1 1 calc R . . C105 C 0.3096(9) 0.2671(10) 0.3467(10) 0.183(11) Uani 1 1 d U . . H10I H 0.2733 0.2473 0.3463 0.220 Uiso 1 1 calc R . . H10J H 0.3399 0.2393 0.3450 0.220 Uiso 1 1 calc R . . C106 C 0.3129(9) 0.3044(10) 0.3086(8) 0.161(8) Uani 1 1 d U . . H10K H 0.2807 0.3301 0.3096 0.193 Uiso 1 1 calc R . . H10L H 0.3092 0.2819 0.2820 0.193 Uiso 1 1 calc R . . C107 C 0.5080(6) 0.3949(7) 0.4846(4) 0.106(5) Uani 1 1 d . . . H10M H 0.5203 0.4317 0.4744 0.127 Uiso 1 1 calc R . . H10N H 0.5213 0.3907 0.5149 0.127 Uiso 1 1 calc R . . C108 C 0.5351(7) 0.3531(6) 0.4581(6) 0.121(6) Uani 1 1 d . . . H10O H 0.5762 0.3557 0.4615 0.145 Uiso 1 1 calc R . . H10P H 0.5231 0.3159 0.4678 0.145 Uiso 1 1 calc R . . C109 C 0.5546(6) 0.3258(7) 0.3850(7) 0.125(7) Uani 1 1 d . . . H10Q H 0.5950 0.3340 0.3885 0.150 Uiso 1 1 calc R . . H10R H 0.5487 0.2861 0.3913 0.150 Uiso 1 1 calc R . . C110 C 0.5378(8) 0.3374(10) 0.3417(8) 0.166(9) Uani 1 1 d . . . H11A H 0.5423 0.3774 0.3359 0.200 Uiso 1 1 calc R . . H11B H 0.5623 0.3171 0.3213 0.200 Uiso 1 1 calc R . . C111 C 0.4664(10) 0.3245(9) 0.2899(6) 0.164(9) Uani 1 1 d U . . H11C H 0.4922 0.3018 0.2721 0.197 Uiso 1 1 calc R . . H11D H 0.4680 0.3630 0.2791 0.197 Uiso 1 1 calc R . . C112 C 0.4082(9) 0.3030(8) 0.2858(6) 0.163(10) Uani 1 1 d . . . H11E H 0.3991 0.2981 0.2547 0.195 Uiso 1 1 calc R . . H11F H 0.4060 0.2663 0.2999 0.195 Uiso 1 1 calc R . . C113 C 0.4199(7) 0.4460(7) 0.4988(4) 0.121(6) Uani 1 1 d . . . H11G H 0.4417 0.4604 0.5237 0.145 Uiso 1 1 calc R . . H11H H 0.3809 0.4398 0.5087 0.145 Uiso 1 1 calc R . . C114 C 0.4198(6) 0.4877(6) 0.4637(5) 0.101(4) Uani 1 1 d . . . H11I H 0.4073 0.5238 0.4753 0.122 Uiso 1 1 calc R . . H11J H 0.4583 0.4922 0.4522 0.122 Uiso 1 1 calc R . . C115 C 0.3754(5) 0.5130(4) 0.3992(4) 0.079(3) Uani 1 1 d . . . H11K H 0.4120 0.5240 0.3867 0.095 Uiso 1 1 calc R . . H11L H 0.3588 0.5459 0.4133 0.095 Uiso 1 1 calc R . . C116 C 0.3393(6) 0.4945(5) 0.3654(4) 0.088(4) Uani 1 1 d . . . H11M H 0.3033 0.4820 0.3780 0.106 Uiso 1 1 calc R . . H11N H 0.3313 0.5256 0.3455 0.106 Uiso 1 1 calc R . . C117 C 0.3315(7) 0.4361(7) 0.3053(4) 0.132(4) Uani 1 1 d U . . H11O H 0.3287 0.4681 0.2854 0.158 Uiso 1 1 calc R . . H11P H 0.2931 0.4259 0.3145 0.158 Uiso 1 1 calc R . . C118 C 0.3583(7) 0.3875(7) 0.2815(4) 0.132(4) Uani 1 1 d U . . H11Q H 0.3342 0.3782 0.2564 0.158 Uiso 1 1 calc R . . H11R H 0.3948 0.4001 0.2698 0.158 Uiso 1 1 calc R . . K2 K 0.37076(11) 0.0000 0.2500 0.0657(8) Uani 1 2 d S . . N21 N 0.3754(7) 0.0229(5) 0.1554(4) 0.129(5) Uani 1 1 d . . . O21 O 0.3147(4) 0.0940(3) 0.2195(2) 0.079(2) Uani 1 1 d . . . O22 O 0.3338(3) 0.0804(3) 0.3097(2) 0.0716(19) Uani 1 1 d . . . O23 O 0.4729(6) 0.0027(6) 0.2063(6) 0.172(6) Uani 1 1 d . . . C201 C 0.3325(9) 0.0640(7) 0.1459(5) 0.139(7) Uani 1 1 d . . . H20A H 0.2952 0.0461 0.1470 0.167 Uiso 1 1 calc R . . H20B H 0.3382 0.0781 0.1161 0.167 Uiso 1 1 calc R . . C202 C 0.3334(9) 0.1135(6) 0.1783(5) 0.141(7) Uani 1 1 d . . . H20C H 0.3718 0.1285 0.1807 0.169 Uiso 1 1 calc R . . H20D H 0.3083 0.1433 0.1678 0.169 Uiso 1 1 calc R . . C203 C 0.3160(5) 0.1372(4) 0.2514(5) 0.080(3) Uani 1 1 d . . . H20E H 0.3550 0.1505 0.2550 0.095 Uiso 1 1 calc R . . H20F H 0.2928 0.1686 0.2413 0.095 Uiso 1 1 calc R . . C204 C 0.2953(5) 0.1182(5) 0.2924(4) 0.075(3) Uani 1 1 d . . . H20G H 0.2906 0.1499 0.3124 0.089 Uiso 1 1 calc R . . H20H H 0.2583 0.1002 0.2885 0.089 Uiso 1 1 calc R . . C205 C 0.3172(9) 0.0613(6) 0.3514(5) 0.132(7) Uani 1 1 d . . . H20I H 0.2827 0.0388 0.3489 0.158 Uiso 1 1 calc R . . H20J H 0.3091 0.0932 0.3705 0.158 Uiso 1 1 calc R . . C206 C 0.3634(10) 0.0273(7) 0.3703(5) 0.149(8) Uani 1 1 d . . . H20K H 0.3978 0.0501 0.3721 0.179 Uiso 1 1 calc R . . H20L H 0.3530 0.0163 0.4002 0.179 Uiso 1 1 calc R . . C207 C 0.4325(8) 0.0409(8) 0.1456(7) 0.164(9) Uani 1 1 d . . . H20M H 0.4369 0.0404 0.1137 0.197 Uiso 1 1 calc R . . H20N H 0.4358 0.0800 0.1549 0.197 Uiso 1 1 calc R . . C208 C 0.4780(8) 0.0121(11) 0.1634(8) 0.172(6) Uani 1 1 d . . . H20O H 0.4819 -0.0237 0.1483 0.207 Uiso 1 1 calc R . . H20P H 0.5127 0.0335 0.1582 0.207 Uiso 1 1 calc R . . C209 C 0.5142(13) 0.0138(15) 0.2277(9) 0.260(16) Uani 1 1 d U . . H20Q H 0.5162 0.0544 0.2316 0.312 Uiso 1 1 calc R . . H20R H 0.5481 0.0021 0.2116 0.312 Uiso 1 1 calc R . . N1E N 0.2955(6) 0.3965(9) -0.0358(5) 0.166(7) Uani 1 1 d . . . H1E1 H 0.3150 0.4050 -0.0602 0.250 Uiso 0.67 1 calc PR . . H1E2 H 0.2695 0.3702 -0.0420 0.250 Uiso 0.67 1 calc PR . . H1E3 H 0.3195 0.3835 -0.0152 0.250 Uiso 0.67 1 calc PR . . C1E C 0.2667(8) 0.4471(9) -0.0193(8) 0.171(11) Uani 1 1 d . . . H1E4 H 0.2962 0.4754 -0.0150 0.206 Uiso 1 1 calc R . . H1E5 H 0.2424 0.4605 -0.0430 0.206 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0426(4) 0.0479(3) 0.0392(4) -0.0071(3) 0.0054(3) -0.0079(3) P1 0.0721(16) 0.0700(16) 0.0350(11) 0.0078(11) 0.0102(11) 0.0304(13) P2 0.176(3) 0.0323(12) 0.0398(13) -0.0006(10) 0.0064(17) -0.0013(16) P3 0.0444(12) 0.0633(15) 0.0576(14) 0.0144(12) 0.0104(11) 0.0016(11) P4 0.0485(13) 0.0562(14) 0.0565(14) 0.0003(11) 0.0022(11) 0.0037(11) P5 0.103(2) 0.0710(17) 0.0499(14) -0.0142(13) 0.0304(15) -0.0471(17) P6 0.0494(13) 0.0445(12) 0.0632(14) -0.0181(11) 0.0120(11) -0.0066(10) P7 0.0425(13) 0.0809(18) 0.0756(18) -0.0282(15) 0.0118(12) -0.0061(12) P8 0.0426(4) 0.0479(3) 0.0392(4) -0.0071(3) 0.0054(3) -0.0079(3) K1 0.0485(10) 0.0427(10) 0.0589(11) 0.0036(8) -0.0134(9) 0.0004(8) N11 0.137(10) 0.094(8) 0.071(7) 0.014(6) -0.047(7) 0.004(7) N12 0.166(13) 0.133(11) 0.109(9) -0.065(8) -0.054(9) 0.090(10) O11 0.080(7) 0.118(8) 0.192(12) 0.082(8) 0.007(7) -0.021(6) O12 0.080(7) 0.125(9) 0.245(16) -0.049(11) -0.056(9) -0.017(6) O13 0.073(5) 0.073(5) 0.152(8) -0.025(5) -0.047(5) 0.027(4) O14 0.098(7) 0.129(8) 0.133(9) -0.047(7) -0.029(6) 0.064(6) O15 0.065(4) 0.054(4) 0.059(4) -0.008(3) -0.004(3) -0.003(3) O16 0.084(5) 0.069(4) 0.053(4) 0.005(3) 0.005(4) 0.035(4) C101 0.186(19) 0.164(16) 0.071(9) 0.058(10) -0.024(11) -0.012(14) C102 0.141(17) 0.25(3) 0.093(13) 0.099(15) -0.009(12) 0.001(17) C103 0.114(16) 0.114(15) 0.26(3) 0.056(17) 0.023(17) -0.001(13) C104 0.097(12) 0.086(11) 0.32(3) 0.026(17) 0.052(16) -0.039(10) C105 0.118(14) 0.157(19) 0.28(3) -0.08(2) -0.082(18) -0.010(13) C106 0.152(14) 0.173(15) 0.159(14) -0.084(12) -0.069(12) 0.001(12) C107 0.103(11) 0.123(12) 0.093(10) -0.003(9) -0.051(8) 0.000(9) C108 0.109(11) 0.071(8) 0.182(17) 0.009(10) -0.078(12) 0.002(8) C109 0.060(8) 0.110(11) 0.21(2) -0.040(13) -0.026(11) 0.040(8) C110 0.098(14) 0.19(2) 0.21(2) -0.074(19) 0.035(15) 0.033(14) C111 0.20(2) 0.197(19) 0.096(12) -0.057(12) 0.023(13) 0.103(17) C112 0.178(18) 0.177(17) 0.134(14) -0.099(13) -0.096(14) 0.110(15) C113 0.159(14) 0.154(14) 0.048(7) -0.019(9) -0.037(8) 0.024(12) C114 0.099(10) 0.088(9) 0.117(11) -0.028(8) -0.022(9) 0.023(8) C115 0.101(9) 0.042(5) 0.095(8) 0.008(5) 0.025(7) 0.008(6) C116 0.134(11) 0.068(7) 0.063(7) 0.001(6) -0.001(7) 0.052(7) C117 0.167(9) 0.168(10) 0.059(5) -0.026(6) -0.033(6) 0.106(8) C118 0.167(9) 0.168(10) 0.059(5) -0.026(6) -0.033(6) 0.106(8) K2 0.0355(14) 0.0553(16) 0.106(2) -0.0038(17) 0.000 0.000 N21 0.200(15) 0.077(8) 0.110(9) 0.010(7) 0.071(10) -0.014(9) O21 0.109(6) 0.053(4) 0.076(5) 0.015(4) 0.001(4) -0.003(4) O22 0.072(5) 0.064(4) 0.079(5) 0.006(4) -0.004(4) 0.011(4) O23 0.104(7) 0.182(10) 0.230(16) 0.006(12) 0.073(10) -0.042(7) C201 0.22(2) 0.104(12) 0.089(11) 0.043(10) 0.033(12) 0.005(13) C202 0.23(2) 0.066(8) 0.124(13) 0.043(9) 0.070(13) 0.018(11) C203 0.067(7) 0.051(6) 0.120(10) 0.017(7) -0.008(7) 0.008(5) C204 0.065(7) 0.066(7) 0.092(8) -0.010(6) 0.002(6) 0.014(5) C205 0.23(2) 0.091(10) 0.077(9) 0.000(8) 0.030(11) -0.009(12) C206 0.28(2) 0.089(10) 0.078(10) 0.000(8) -0.056(13) 0.037(13) C207 0.144(16) 0.124(14) 0.22(2) -0.001(14) 0.111(16) -0.057(12) C208 0.104(7) 0.182(10) 0.230(16) 0.006(12) 0.073(10) -0.042(7) C209 0.201(19) 0.29(2) 0.28(2) 0.039(18) -0.027(16) -0.050(17) N1E 0.129(12) 0.26(2) 0.114(11) 0.072(13) 0.005(9) 0.035(13) C1E 0.12(2) 0.134(15) 0.26(4) 0.046(17) -0.008(16) 0.004(13) _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 Pb1 P8 0.619(5) . ? Pb1 P2 2.497(3) . ? Pb1 P8 2.692(6) 6_554 ? Pb1 P3 2.705(3) . ? Pb1 Pb1 2.8905(14) 6_554 ? P1 P4 2.141(3) . ? P1 P3 2.173(4) . ? P1 P2 2.182(4) 6_554 ? P2 P5 2.173(4) 6_554 ? P2 P1 2.182(4) 6_554 ? P2 P8 2.439(7) . ? P3 P6 2.171(3) . ? P3 P8 2.196(6) . ? P4 P7 2.154(4) . ? P5 P2 2.173(4) 6_554 ? P5 P6 2.217(3) . ? P5 P7 2.221(5) . ? P6 P7 2.221(4) . ? P8 P8 2.434(12) 6_554 ? P8 Pb1 2.692(6) 6_554 ? K1 O11 2.770(10) . ? K1 O15 2.789(6) . ? K1 O16 2.820(6) . ? K1 O12 2.831(10) . ? K1 O13 2.835(8) . ? K1 O14 2.860(10) . ? K1 N11 2.957(10) . ? K1 N12 3.022(12) . ? N11 C101 1.413(17) . ? N11 C113 1.460(17) . ? N11 C107 1.530(18) . ? N12 C118 1.401(19) . ? N12 C112 1.433(18) . ? N12 C106 1.55(3) . ? O11 C103 1.34(2) . ? O11 C102 1.48(2) . ? O12 C105 1.28(2) . ? O12 C104 1.50(2) . ? O13 C108 1.358(17) . ? O13 C109 1.490(17) . ? O14 C110 1.37(2) . ? O14 C111 1.434(19) . ? O15 C114 1.390(14) . ? O15 C115 1.423(12) . ? O16 C116 1.401(11) . ? O16 C117 1.415(14) . ? C101 C102 1.56(2) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.43(3) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.48(3) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.454(19) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.42(3) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.49(3) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.479(19) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.425(16) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.527(17) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? K2 O23 2.785(12) 8_445 ? K2 O23 2.785(12) . ? K2 O21 2.802(7) 8_445 ? K2 O21 2.802(7) . ? K2 O22 2.822(7) 8_445 ? K2 O22 2.822(7) . ? K2 N21 2.972(13) 8_445 ? K2 N21 2.972(13) . ? N21 C201 1.46(2) . ? N21 C207 1.461(19) . ? N21 C206 1.480(18) 8_445 ? O21 C202 1.427(14) . ? O21 C203 1.437(14) . ? O22 C204 1.402(12) . ? O22 C205 1.422(15) . ? O23 C209 1.22(3) . ? O23 C208 1.35(2) . ? C201 C202 1.56(2) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.432(15) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.50(2) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 N21 1.480(18) 8_445 ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.40(3) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C209 1.53(5) 8_445 ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? N1E C1E 1.49(2) . ? N1E H1E1 0.9100 . ? N1E H1E2 0.9100 . ? N1E H1E3 0.9100 . ? C1E C1E 1.43(4) 7_544 ? C1E H1E4 0.9900 . ? C1E H1E5 0.9900 . ? 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 P8 Pb1 P2 77.5(5) . . ? P8 Pb1 P8 59.3(6) . 6_554 ? P2 Pb1 P8 87.91(13) . 6_554 ? P8 Pb1 P3 30.7(6) . . ? P2 Pb1 P3 88.77(9) . . ? P8 Pb1 P3 87.73(13) 6_554 . ? P8 Pb1 Pb1 65.3(6) . 6_554 ? P2 Pb1 Pb1 99.61(7) . 6_554 ? P8 Pb1 Pb1 12.07(11) 6_554 6_554 ? P3 Pb1 Pb1 90.92(6) . 6_554 ? P4 P1 P3 100.34(14) . . ? P4 P1 P2 98.86(16) . 6_554 ? P3 P1 P2 101.12(13) . 6_554 ? P5 P2 P1 101.69(14) 6_554 6_554 ? P5 P2 P8 99.71(19) 6_554 . ? P1 P2 P8 101.8(2) 6_554 . ? P5 P2 Pb1 88.83(13) 6_554 . ? P1 P2 Pb1 113.43(18) 6_554 . ? P6 P3 P1 101.14(13) . . ? P6 P3 P8 94.20(18) . . ? P1 P3 P8 104.33(19) . . ? P6 P3 Pb1 92.19(11) . . ? P1 P3 Pb1 112.61(12) . . ? P1 P4 P7 99.02(14) . . ? P2 P5 P6 104.92(15) 6_554 . ? P2 P5 P7 100.65(14) 6_554 . ? P6 P5 P7 60.04(12) . . ? P3 P6 P5 105.65(13) . . ? P3 P6 P7 101.82(14) . . ? P5 P6 P7 60.06(14) . . ? P4 P7 P6 107.47(14) . . ? P4 P7 P5 107.83(15) . . ? P6 P7 P5 59.90(12) . . ? Pb1 P8 P3 141.0(7) . . ? Pb1 P8 P8 108.1(6) . 6_554 ? P3 P8 P8 107.6(3) . 6_554 ? Pb1 P8 P2 88.1(6) . . ? P3 P8 P2 103.5(2) . . ? P8 P8 P2 95.4(3) 6_554 . ? Pb1 P8 Pb1 102.6(6) . 6_554 ? P3 P8 Pb1 109.1(2) . 6_554 ? P2 P8 Pb1 106.9(2) . 6_554 ? O11 K1 O15 95.0(3) . . ? O11 K1 O16 133.0(3) . . ? O15 K1 O16 60.3(2) . . ? O11 K1 O12 60.3(5) . . ? O15 K1 O12 118.6(3) . . ? O16 K1 O12 95.1(3) . . ? O11 K1 O13 100.8(3) . . ? O15 K1 O13 98.5(2) . . ? O16 K1 O13 120.7(3) . . ? O12 K1 O13 138.4(3) . . ? O11 K1 O14 125.5(3) . . ? O15 K1 O14 135.2(3) . . ? O16 K1 O14 96.1(3) . . ? O12 K1 O14 99.7(4) . . ? O13 K1 O14 59.3(3) . . ? O11 K1 N11 61.1(4) . . ? O15 K1 N11 60.2(3) . . ? O16 K1 N11 119.8(3) . . ? O12 K1 N11 121.0(5) . . ? O13 K1 N11 60.8(3) . . ? O14 K1 N11 119.7(3) . . ? O11 K1 N12 119.4(5) . . ? O15 K1 N12 120.0(3) . . ? O16 K1 N12 60.4(3) . . ? O12 K1 N12 59.6(5) . . ? O13 K1 N12 118.5(4) . . ? O14 K1 N12 59.6(3) . . ? N11 K1 N12 179.3(4) . . ? O11 K1 C103 20.3(4) . . ? O15 K1 C103 97.9(5) . . ? O16 K1 C103 117.6(4) . . ? O12 K1 C103 41.8(6) . . ? O13 K1 C103 119.9(4) . . ? O14 K1 C103 126.8(5) . . ? N11 K1 C103 79.2(5) . . ? N12 K1 C103 101.3(6) . . ? C101 N11 C113 112.6(14) . . ? C101 N11 C107 105.4(12) . . ? C113 N11 C107 112.0(12) . . ? C101 N11 K1 108.2(9) . . ? C113 N11 K1 110.1(7) . . ? C107 N11 K1 108.3(8) . . ? C118 N12 C112 113.6(16) . . ? C118 N12 C106 110.8(15) . . ? C112 N12 C106 105.5(15) . . ? C118 N12 K1 110.2(9) . . ? C112 N12 K1 108.6(8) . . ? C106 N12 K1 107.8(11) . . ? C103 O11 C102 111.2(18) . . ? C103 O11 K1 114.0(13) . . ? C102 O11 K1 115.7(9) . . ? C105 O12 C104 111.5(19) . . ? C105 O12 K1 120.5(15) . . ? C104 O12 K1 112.5(11) . . ? C108 O13 C109 114.5(12) . . ? C108 O13 K1 116.6(9) . . ? C109 O13 K1 114.6(7) . . ? C110 O14 C111 114.3(18) . . ? C110 O14 K1 114.3(10) . . ? C111 O14 K1 116.5(8) . . ? C114 O15 C115 112.3(9) . . ? C114 O15 K1 115.6(6) . . ? C115 O15 K1 114.4(6) . . ? C116 O16 C117 112.3(9) . . ? C116 O16 K1 112.8(6) . . ? C117 O16 K1 118.7(8) . . ? N11 C101 C102 110.1(14) . . ? N11 C101 H10A 109.6 . . ? C102 C101 H10A 109.6 . . ? N11 C101 H10B 109.6 . . ? C102 C101 H10B 109.6 . . ? H10A C101 H10B 108.2 . . ? O11 C102 C101 103.9(16) . . ? O11 C102 H10C 111.0 . . ? C101 C102 H10C 111.0 . . ? O11 C102 H10D 111.0 . . ? C101 C102 H10D 111.0 . . ? H10C C102 H10D 109.0 . . ? O11 C103 C104 113(2) . . ? O11 C103 K1 45.7(9) . . ? C104 C103 K1 84.2(12) . . ? O11 C103 H10E 109.0 . . ? C104 C103 H10E 109.0 . . ? K1 C103 H10E 87.1 . . ? O11 C103 H10F 109.0 . . ? C104 C103 H10F 109.0 . . ? K1 C103 H10F 154.6 . . ? H10E C103 H10F 107.8 . . ? C103 C104 O12 107.6(16) . . ? C103 C104 H10G 110.2 . . ? O12 C104 H10G 110.2 . . ? C103 C104 H10H 110.2 . . ? O12 C104 H10H 110.2 . . ? H10G C104 H10H 108.5 . . ? O12 C105 C106 111(2) . . ? O12 C105 H10I 109.3 . . ? C106 C105 H10I 109.3 . . ? O12 C105 H10J 109.3 . . ? C106 C105 H10J 109.3 . . ? H10I C105 H10J 108.0 . . ? C105 C106 N12 115.4(16) . . ? C105 C106 H10K 108.4 . . ? N12 C106 H10K 108.4 . . ? C105 C106 H10L 108.4 . . ? N12 C106 H10L 108.4 . . ? H10K C106 H10L 107.5 . . ? C108 C107 N11 115.4(12) . . ? C108 C107 H10M 108.4 . . ? N11 C107 H10M 108.4 . . ? C108 C107 H10N 108.4 . . ? N11 C107 H10N 108.4 . . ? H10M C107 H10N 107.5 . . ? O13 C108 C107 110.3(11) . . ? O13 C108 H10O 109.6 . . ? C107 C108 H10O 109.6 . . ? O13 C108 H10P 109.6 . . ? C107 C108 H10P 109.6 . . ? H10O C108 H10P 108.1 . . ? C110 C109 O13 109.7(12) . . ? C110 C109 H10Q 109.7 . . ? O13 C109 H10Q 109.7 . . ? C110 C109 H10R 109.7 . . ? O13 C109 H10R 109.7 . . ? H10Q C109 H10R 108.2 . . ? O14 C110 C109 111.6(19) . . ? O14 C110 H11A 109.3 . . ? C109 C110 H11A 109.3 . . ? O14 C110 H11B 109.3 . . ? C109 C110 H11B 109.3 . . ? H11A C110 H11B 108.0 . . ? O14 C111 C112 109.1(16) . . ? O14 C111 H11C 109.9 . . ? C112 C111 H11C 109.9 . . ? O14 C111 H11D 109.9 . . ? C112 C111 H11D 109.9 . . ? H11C C111 H11D 108.3 . . ? N12 C112 C111 112.5(15) . . ? N12 C112 H11E 109.1 . . ? C111 C112 H11E 109.1 . . ? N12 C112 H11F 109.1 . . ? C111 C112 H11F 109.1 . . ? H11E C112 H11F 107.8 . . ? N11 C113 C114 112.2(11) . . ? N11 C113 H11G 109.2 . . ? C114 C113 H11G 109.2 . . ? N11 C113 H11H 109.2 . . ? C114 C113 H11H 109.2 . . ? H11G C113 H11H 107.9 . . ? O15 C114 C113 109.7(11) . . ? O15 C114 H11I 109.7 . . ? C113 C114 H11I 109.7 . . ? O15 C114 H11J 109.7 . . ? C113 C114 H11J 109.7 . . ? H11I C114 H11J 108.2 . . ? O15 C115 C116 111.2(9) . . ? O15 C115 H11K 109.4 . . ? C116 C115 H11K 109.4 . . ? O15 C115 H11L 109.4 . . ? C116 C115 H11L 109.4 . . ? H11K C115 H11L 108.0 . . ? O16 C116 C115 111.2(10) . . ? O16 C116 H11M 109.4 . . ? C115 C116 H11M 109.4 . . ? O16 C116 H11N 109.4 . . ? C115 C116 H11N 109.4 . . ? H11M C116 H11N 108.0 . . ? O16 C117 C118 110.9(10) . . ? O16 C117 H11O 109.5 . . ? C118 C117 H11O 109.5 . . ? O16 C117 H11P 109.5 . . ? C118 C117 H11P 109.5 . . ? H11O C117 H11P 108.1 . . ? N12 C118 C117 117.4(12) . . ? N12 C118 H11Q 107.9 . . ? C117 C118 H11Q 107.9 . . ? N12 C118 H11R 107.9 . . ? C117 C118 H11R 107.9 . . ? H11Q C118 H11R 107.2 . . ? O23 K2 O23 57.9(8) 8_445 . ? O23 K2 O21 103.6(4) 8_445 8_445 ? O23 K2 O21 126.8(4) . 8_445 ? O23 K2 O21 126.8(4) 8_445 . ? O23 K2 O21 103.6(4) . . ? O21 K2 O21 123.0(3) 8_445 . ? O23 K2 O22 125.0(4) 8_445 8_445 ? O23 K2 O22 88.5(4) . 8_445 ? O21 K2 O22 60.6(2) 8_445 8_445 ? O21 K2 O22 101.1(2) . 8_445 ? O23 K2 O22 88.5(4) 8_445 . ? O23 K2 O22 125.0(4) . . ? O21 K2 O22 101.1(2) 8_445 . ? O21 K2 O22 60.6(2) . . ? O22 K2 O22 143.5(3) 8_445 . ? O23 K2 N21 59.2(5) 8_445 8_445 ? O23 K2 N21 116.5(5) . 8_445 ? O21 K2 N21 62.4(3) 8_445 8_445 ? O21 K2 N21 119.9(3) . 8_445 ? O22 K2 N21 121.6(3) 8_445 8_445 ? O22 K2 N21 60.0(3) . 8_445 ? O23 K2 N21 116.5(5) 8_445 . ? O23 K2 N21 59.2(5) . . ? O21 K2 N21 119.9(3) 8_445 . ? O21 K2 N21 62.4(3) . . ? O22 K2 N21 60.0(3) 8_445 . ? O22 K2 N21 121.6(3) . . ? N21 K2 N21 175.7(7) 8_445 . ? O23 K2 C209 18.0(6) 8_445 8_445 ? O23 K2 C209 40.8(6) . 8_445 ? O21 K2 C209 108.8(6) 8_445 8_445 ? O21 K2 C209 127.5(6) . 8_445 ? O22 K2 C209 111.6(6) 8_445 8_445 ? O22 K2 C209 104.1(6) . 8_445 ? N21 K2 C209 75.7(5) 8_445 8_445 ? N21 K2 C209 100.0(5) . 8_445 ? O23 K2 C209 40.8(6) 8_445 . ? O23 K2 C209 18.0(6) . . ? O21 K2 C209 127.5(6) 8_445 . ? O21 K2 C209 108.8(6) . . ? O22 K2 C209 104.1(6) 8_445 . ? O22 K2 C209 111.6(6) . . ? N21 K2 C209 100.0(5) 8_445 . ? N21 K2 C209 75.7(5) . . ? C209 K2 C209 25.2(8) 8_445 . ? C201 N21 C207 114.2(14) . . ? C201 N21 C206 108.4(17) . 8_445 ? C207 N21 C206 108.3(14) . 8_445 ? C201 N21 K2 107.4(9) . . ? C207 N21 K2 107.0(13) . . ? C206 N21 K2 111.5(8) 8_445 . ? C202 O21 C203 111.3(10) . . ? C202 O21 K2 114.8(8) . . ? C203 O21 K2 110.5(6) . . ? C204 O22 C205 112.0(11) . . ? C204 O22 K2 114.0(6) . . ? C205 O22 K2 117.0(7) . . ? C209 O23 C208 115.0(19) . . ? C209 O23 K2 117(2) . . ? C208 O23 K2 123.9(14) . . ? N21 C201 C202 112.7(16) . . ? N21 C201 H20A 109.1 . . ? C202 C201 H20A 109.1 . . ? N21 C201 H20B 109.1 . . ? C202 C201 H20B 109.1 . . ? H20A C201 H20B 107.8 . . ? O21 C202 C201 108.2(10) . . ? O21 C202 H20C 110.1 . . ? C201 C202 H20C 110.1 . . ? O21 C202 H20D 110.1 . . ? C201 C202 H20D 110.1 . . ? H20C C202 H20D 108.4 . . ? C204 C203 O21 111.4(9) . . ? C204 C203 H20E 109.4 . . ? O21 C203 H20E 109.4 . . ? C204 C203 H20F 109.4 . . ? O21 C203 H20F 109.4 . . ? H20E C203 H20F 108.0 . . ? O22 C204 C203 108.6(9) . . ? O22 C204 H20G 110.0 . . ? C203 C204 H20G 110.0 . . ? O22 C204 H20H 110.0 . . ? C203 C204 H20H 110.0 . . ? H20G C204 H20H 108.3 . . ? O22 C205 C206 109.1(15) . . ? O22 C205 H20I 109.9 . . ? C206 C205 H20I 109.9 . . ? O22 C205 H20J 109.9 . . ? C206 C205 H20J 109.9 . . ? H20I C205 H20J 108.3 . . ? N21 C206 C205 112.7(13) 8_445 . ? N21 C206 H20K 109.1 8_445 . ? C205 C206 H20K 109.1 . . ? N21 C206 H20L 109.1 8_445 . ? C205 C206 H20L 109.1 . . ? H20K C206 H20L 107.8 . . ? C208 C207 N21 119.5(17) . . ? C208 C207 H20M 107.4 . . ? N21 C207 H20M 107.4 . . ? C208 C207 H20N 107.4 . . ? N21 C207 H20N 107.4 . . ? H20M C207 H20N 107.0 . . ? O23 C208 C207 113.5(19) . . ? O23 C208 H20O 108.9 . . ? C207 C208 H20O 108.9 . . ? O23 C208 H20P 108.9 . . ? C207 C208 H20P 108.9 . . ? H20O C208 H20P 107.7 . . ? O23 C209 C209 113(2) . 8_445 ? O23 C209 K2 45.1(15) . . ? C209 C209 K2 77.4(4) 8_445 . ? O23 C209 H20Q 109.0 . . ? C209 C209 H20Q 109.0 8_445 . ? K2 C209 H20Q 96.8 . . ? O23 C209 H20R 109.0 . . ? C209 C209 H20R 109.0 8_445 . ? K2 C209 H20R 150.2 . . ? H20Q C209 H20R 107.8 . . ? C1E N1E H1E1 109.5 . . ? C1E N1E H1E2 109.5 . . ? H1E1 N1E H1E2 109.5 . . ? C1E N1E H1E3 109.5 . . ? H1E1 N1E H1E3 109.5 . . ? H1E2 N1E H1E3 109.5 . . ? C1E C1E N1E 122.7(12) 7_544 . ? C1E C1E H1E4 106.7 7_544 . ? N1E C1E H1E4 106.7 . . ? C1E C1E H1E5 106.7 7_544 . ? N1E C1E H1E5 106.7 . . ? H1E4 C1E H1E5 106.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.856 _refine_diff_density_min -1.894 _refine_diff_density_rms 0.111 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 786260' #TrackingRef '- combined_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(2,2,2-crypt)]3[SnAs15]*2en ; _chemical_name_common (K(2,2,2-crypt))3(SnAs15)*2en _chemical_melting_point ? _chemical_formula_moiety '3(C18 H36 K N2 O6), As15 Sn, 2(C2 H8 N2)' _chemical_formula_sum 'C58 H124 As15 K3 N10 O18 Sn' _chemical_formula_weight 2609.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.04090(10) _cell_length_b 18.3450(2) _cell_length_c 30.3204(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.7830(10) _cell_angle_gamma 90.00 _cell_volume 9457.97(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 90982 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.06 #_exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5152 _exptl_absorpt_coefficient_mu 5.671 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2487 _exptl_absorpt_correction_T_max 0.7272 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 32094 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16456 _reflns_number_gt 12640 _reflns_threshold_expression >2\s(I) _computing_data_collection ; KappaCCD software "Collect" (Nonius, 2000) ; _computing_cell_refinement ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_data_reduction ; KappaCCD software "DENZO" (Otwinowski & Minor, 1996) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 2005)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0893P)^2^+7.2783P] 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 16456 _refine_ls_number_parameters 946 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Sn1 Sn 0.27811(3) 0.79440(3) 0.287983(16) 0.04044(14) Uani 1 1 d . . . As1 As 0.28529(4) 0.67142(4) 0.39896(2) 0.03377(17) Uani 1 1 d . . . As2 As 0.14691(4) 0.68196(4) 0.37537(2) 0.03689(18) Uani 1 1 d . . . As3 As 0.34432(4) 0.67992(4) 0.32910(2) 0.03404(17) Uani 1 1 d . . . As4 As 0.29048(4) 0.54396(4) 0.41092(2) 0.04252(19) Uani 1 1 d . . . As5 As 0.13538(4) 0.59512(4) 0.31569(2) 0.03803(18) Uani 1 1 d . . . As6 As 0.26629(4) 0.59350(4) 0.28619(2) 0.03544(17) Uani 1 1 d . . . As7 As 0.23286(4) 0.50301(4) 0.34152(2) 0.03991(18) Uani 1 1 d . . . As8 As 0.28656(4) 0.88368(4) 0.41026(2) 0.03497(17) Uani 1 1 d . . . As9 As 0.14987(4) 0.88207(4) 0.38419(2) 0.03377(17) Uani 1 1 d . . . As10 As 0.35013(4) 0.89088(4) 0.34144(2) 0.03741(18) Uani 1 1 d . . . As11 As 0.29083(4) 1.00718(4) 0.43327(2) 0.0454(2) Uani 1 1 d . . . As12 As 0.14333(4) 0.98069(4) 0.33147(2) 0.03949(18) Uani 1 1 d . . . As13 As 0.27719(4) 0.98810(4) 0.30550(2) 0.04222(19) Uani 1 1 d . . . As14 As 0.24039(4) 1.06541(4) 0.36705(2) 0.04280(19) Uani 1 1 d . . . As15 As 0.13558(4) 0.78811(3) 0.325286(19) 0.02843(16) Uani 1 1 d . . . K1 K 0.04053(7) 0.74140(8) 0.58472(4) 0.0298(3) Uani 1 1 d . . . N11 N 0.0005(3) 0.5795(3) 0.59178(18) 0.0379(13) Uani 1 1 d . . . N12 N 0.0810(3) 0.8995(3) 0.57792(18) 0.0363(13) Uani 1 1 d . . . O11 O 0.1270(2) 0.6359(2) 0.53870(14) 0.0369(10) Uani 1 1 d . . . O12 O 0.1446(3) 0.7881(3) 0.52328(15) 0.0409(11) Uani 1 1 d . . . O13 O 0.0390(3) 0.6716(3) 0.66859(14) 0.0426(12) Uani 1 1 d . . . O14 O 0.1033(3) 0.8125(3) 0.66034(14) 0.0408(11) Uani 1 1 d . . . O15 O -0.1110(2) 0.6908(3) 0.55547(14) 0.0369(11) Uani 1 1 d . . . O16 O -0.0757(2) 0.8431(2) 0.56283(15) 0.0401(11) Uani 1 1 d . . . C101 C 0.0640(4) 0.5373(4) 0.5737(3) 0.0473(18) Uani 1 1 d . . . H10A H 0.0453 0.4867 0.5684 0.057 Uiso 1 1 calc R . . H10B H 0.1089 0.5353 0.5961 0.057 Uiso 1 1 calc R . . C102 C 0.0925(4) 0.5664(4) 0.5316(2) 0.0452(18) Uani 1 1 d . . . H10C H 0.1318 0.5325 0.5204 0.054 Uiso 1 1 calc R . . H10D H 0.0480 0.5701 0.5091 0.054 Uiso 1 1 calc R . . C103 C 0.1526(4) 0.6647(4) 0.4981(2) 0.0468(18) Uani 1 1 d . . . H10E H 0.1066 0.6733 0.4772 0.056 Uiso 1 1 calc R . . H10F H 0.1875 0.6291 0.4846 0.056 Uiso 1 1 calc R . . C104 C 0.1962(4) 0.7353(4) 0.5070(2) 0.0437(17) Uani 1 1 d . . . H10G H 0.2409 0.7271 0.5290 0.052 Uiso 1 1 calc R . . H10H H 0.2175 0.7532 0.4794 0.052 Uiso 1 1 calc R . . C105 C 0.1812(4) 0.8570(4) 0.5269(3) 0.0495(19) Uani 1 1 d . . . H10I H 0.2053 0.8690 0.4989 0.059 Uiso 1 1 calc R . . H10J H 0.2234 0.8561 0.5509 0.059 Uiso 1 1 calc R . . C106 C 0.1207(4) 0.9145(4) 0.5366(3) 0.0473(18) Uani 1 1 d . . . H10K H 0.1469 0.9626 0.5392 0.057 Uiso 1 1 calc R . . H10L H 0.0806 0.9170 0.5115 0.057 Uiso 1 1 calc R . . C107 C -0.0078(4) 0.5590(4) 0.6385(2) 0.0459(18) Uani 1 1 d . . . H10M H -0.0019 0.5055 0.6415 0.055 Uiso 1 1 calc R . . H10N H -0.0614 0.5720 0.6466 0.055 Uiso 1 1 calc R . . C108 C 0.0511(4) 0.5955(4) 0.6700(2) 0.0468(18) Uani 1 1 d . . . H10O H 0.0454 0.5773 0.7004 0.056 Uiso 1 1 calc R . . H10P H 0.1050 0.5841 0.6618 0.056 Uiso 1 1 calc R . . C109 C 0.0834(4) 0.7068(5) 0.7037(2) 0.0464(19) Uani 1 1 d . . . H10Q H 0.1397 0.6944 0.7024 0.056 Uiso 1 1 calc R . . H10R H 0.0658 0.6896 0.7323 0.056 Uiso 1 1 calc R . . C110 C 0.0733(5) 0.7869(5) 0.7004(2) 0.054(2) Uani 1 1 d . . . H11A H 0.0169 0.7994 0.7009 0.064 Uiso 1 1 calc R . . H11B H 0.1018 0.8107 0.7260 0.064 Uiso 1 1 calc R . . C111 C 0.1060(5) 0.8890(4) 0.6596(3) 0.0514(19) Uani 1 1 d . . . H11C H 0.1412 0.9066 0.6846 0.062 Uiso 1 1 calc R . . H11D H 0.0527 0.9087 0.6632 0.062 Uiso 1 1 calc R . . C112 C 0.1354(4) 0.9162(4) 0.6165(2) 0.0466(18) Uani 1 1 d . . . H11E H 0.1432 0.9696 0.6185 0.056 Uiso 1 1 calc R . . H11F H 0.1871 0.8936 0.6122 0.056 Uiso 1 1 calc R . . C113 C -0.0749(4) 0.5675(4) 0.5658(2) 0.0421(17) Uani 1 1 d . . . H11G H -0.0956 0.5189 0.5733 0.051 Uiso 1 1 calc R . . H11H H -0.0649 0.5670 0.5340 0.051 Uiso 1 1 calc R . . C114 C -0.1356(4) 0.6235(4) 0.5734(2) 0.0414(17) Uani 1 1 d . . . H11I H -0.1868 0.6086 0.5589 0.050 Uiso 1 1 calc R . . H11J H -0.1418 0.6288 0.6055 0.050 Uiso 1 1 calc R . . C115 C -0.1693(4) 0.7470(4) 0.5605(2) 0.0421(17) Uani 1 1 d . . . H11K H -0.1759 0.7552 0.5923 0.051 Uiso 1 1 calc R . . H11L H -0.2205 0.7310 0.5464 0.051 Uiso 1 1 calc R . . C116 C -0.1450(4) 0.8154(4) 0.5401(2) 0.0394(16) Uani 1 1 d . . . H11M H -0.1351 0.8065 0.5087 0.047 Uiso 1 1 calc R . . H11N H -0.1878 0.8518 0.5410 0.047 Uiso 1 1 calc R . . C117 C -0.0568(4) 0.9140(4) 0.5480(2) 0.0458(18) Uani 1 1 d . . . H11O H -0.1034 0.9461 0.5487 0.055 Uiso 1 1 calc R . . H11P H -0.0414 0.9116 0.5171 0.055 Uiso 1 1 calc R . . C118 C 0.0093(4) 0.9446(4) 0.5770(3) 0.0502(19) Uani 1 1 d . . . H11Q H 0.0218 0.9941 0.5665 0.060 Uiso 1 1 calc R . . H11R H -0.0078 0.9492 0.6075 0.060 Uiso 1 1 calc R . . K2 K 0.47041(7) 0.76555(7) 0.59827(4) 0.0283(3) Uani 1 1 d . . . N21 N 0.4688(3) 0.8748(3) 0.67353(17) 0.0361(13) Uani 1 1 d . . . N22 N 0.4706(3) 0.6532(3) 0.52291(16) 0.0297(11) Uani 1 1 d . . . O21 O 0.3507(2) 0.7587(3) 0.65617(14) 0.0362(10) Uani 1 1 d . . . O22 O 0.3454(2) 0.6641(2) 0.58340(14) 0.0340(10) Uani 1 1 d . . . O23 O 0.5975(3) 0.7736(3) 0.66145(14) 0.0412(11) Uani 1 1 d . . . O24 O 0.5927(2) 0.6628(3) 0.59603(14) 0.0355(10) Uani 1 1 d . . . O25 O 0.4478(3) 0.9155(2) 0.58046(14) 0.0361(10) Uani 1 1 d . . . O26 O 0.4709(2) 0.8123(2) 0.51011(13) 0.0304(9) Uani 1 1 d . . . C201 C 0.4107(4) 0.8488(4) 0.7040(2) 0.0445(17) Uani 1 1 d . . . H20A H 0.3984 0.8890 0.7243 0.053 Uiso 1 1 calc R . . H20B H 0.4340 0.8084 0.7221 0.053 Uiso 1 1 calc R . . C202 C 0.3356(4) 0.8228(4) 0.6803(2) 0.0456(18) Uani 1 1 d . . . H20C H 0.2961 0.8125 0.7020 0.055 Uiso 1 1 calc R . . H20D H 0.3143 0.8612 0.6599 0.055 Uiso 1 1 calc R . . C203 C 0.2792(4) 0.7259(4) 0.6388(2) 0.0444(18) Uani 1 1 d . . . H20E H 0.2535 0.7576 0.6157 0.053 Uiso 1 1 calc R . . H20F H 0.2428 0.7197 0.6627 0.053 Uiso 1 1 calc R . . C204 C 0.2971(4) 0.6540(4) 0.6197(2) 0.0423(17) Uani 1 1 d . . . H20G H 0.3249 0.6231 0.6425 0.051 Uiso 1 1 calc R . . H20H H 0.2477 0.6292 0.6095 0.051 Uiso 1 1 calc R . . C205 C 0.3591(4) 0.5975(4) 0.5610(2) 0.0392(16) Uani 1 1 d . . . H20I H 0.3090 0.5706 0.5556 0.047 Uiso 1 1 calc R . . H20J H 0.3958 0.5665 0.5795 0.047 Uiso 1 1 calc R . . C206 C 0.3938(4) 0.6143(4) 0.5176(2) 0.0384(16) Uani 1 1 d . . . H20K H 0.4012 0.5680 0.5015 0.046 Uiso 1 1 calc R . . H20L H 0.3561 0.6445 0.4993 0.046 Uiso 1 1 calc R . . C207 C 0.5476(4) 0.8782(4) 0.6969(2) 0.0476(18) Uani 1 1 d . . . H20M H 0.5432 0.9017 0.7261 0.057 Uiso 1 1 calc R . . H20N H 0.5823 0.9090 0.6797 0.057 Uiso 1 1 calc R . . C208 C 0.5847(4) 0.8037(4) 0.7037(2) 0.0476(18) Uani 1 1 d . . . H20O H 0.6353 0.8080 0.7215 0.057 Uiso 1 1 calc R . . H20P H 0.5495 0.7716 0.7197 0.057 Uiso 1 1 calc R . . C209 C 0.6470(4) 0.7117(4) 0.6645(2) 0.0443(18) Uani 1 1 d . . . H20Q H 0.6210 0.6717 0.6798 0.053 Uiso 1 1 calc R . . H20R H 0.6968 0.7238 0.6815 0.053 Uiso 1 1 calc R . . C210 C 0.6631(4) 0.6889(4) 0.6191(2) 0.0447(18) Uani 1 1 d . . . H21A H 0.6840 0.7308 0.6030 0.054 Uiso 1 1 calc R . . H21B H 0.7033 0.6499 0.6205 0.054 Uiso 1 1 calc R . . C211 C 0.6072(4) 0.6342(4) 0.5536(2) 0.0396(16) Uani 1 1 d . . . H21C H 0.6498 0.5975 0.5565 0.047 Uiso 1 1 calc R . . H21D H 0.6241 0.6739 0.5342 0.047 Uiso 1 1 calc R . . C212 C 0.5336(4) 0.5999(4) 0.5335(2) 0.0382(16) Uani 1 1 d . . . H21E H 0.5457 0.5739 0.5062 0.046 Uiso 1 1 calc R . . H21F H 0.5146 0.5633 0.5544 0.046 Uiso 1 1 calc R . . C213 C 0.4479(5) 0.9467(4) 0.6559(2) 0.0433(17) Uani 1 1 d . . . H21G H 0.4649 0.9840 0.6781 0.052 Uiso 1 1 calc R . . H21H H 0.3900 0.9499 0.6511 0.052 Uiso 1 1 calc R . . C214 C 0.4837(4) 0.9638(4) 0.6137(2) 0.0442(17) Uani 1 1 d . . . H21I H 0.4737 1.0153 0.6053 0.053 Uiso 1 1 calc R . . H21J H 0.5413 0.9558 0.6168 0.053 Uiso 1 1 calc R . . C215 C 0.4723(4) 0.9343(4) 0.5378(2) 0.0357(15) Uani 1 1 d . . . H21K H 0.5304 0.9323 0.5380 0.043 Uiso 1 1 calc R . . H21L H 0.4553 0.9846 0.5302 0.043 Uiso 1 1 calc R . . C216 C 0.4371(4) 0.8825(3) 0.5043(2) 0.0320(14) Uani 1 1 d . . . H21M H 0.3797 0.8794 0.5071 0.038 Uiso 1 1 calc R . . H21N H 0.4460 0.9006 0.4743 0.038 Uiso 1 1 calc R . . C217 C 0.4409(4) 0.7624(3) 0.4763(2) 0.0339(14) Uani 1 1 d . . . H21O H 0.4479 0.7834 0.4467 0.041 Uiso 1 1 calc R . . H21P H 0.3840 0.7541 0.4791 0.041 Uiso 1 1 calc R . . C218 C 0.4847(4) 0.6913(4) 0.4813(2) 0.0380(16) Uani 1 1 d . . . H21Q H 0.4684 0.6592 0.4560 0.046 Uiso 1 1 calc R . . H21R H 0.5417 0.7008 0.4802 0.046 Uiso 1 1 calc R . . K3 K 0.22749(7) 0.25088(8) 0.15944(5) 0.0324(3) Uani 1 1 d . . . N31 N 0.1566(3) 0.3699(3) 0.20809(17) 0.0322(12) Uani 1 1 d . . . N32 N 0.2980(3) 0.1240(3) 0.1150(2) 0.0488(16) Uani 1 1 d . . . O31 O 0.3247(2) 0.3701(3) 0.18738(14) 0.0363(10) Uani 1 1 d . . . O32 O 0.3908(3) 0.2396(3) 0.1609(2) 0.0721(18) Uani 1 1 d . . . O33 O 0.0856(2) 0.3046(3) 0.12598(15) 0.0387(11) Uani 1 1 d . . . O34 O 0.1672(3) 0.2091(2) 0.07344(15) 0.0379(11) Uani 1 1 d . . . O35 O 0.1814(3) 0.2253(3) 0.24612(18) 0.0556(14) Uani 1 1 d . . . O36 O 0.1728(3) 0.1107(3) 0.1767(2) 0.0621(15) Uani 1 1 d . . . C301 C 0.2084(4) 0.4339(4) 0.2049(2) 0.0388(16) Uani 1 1 d . . . H30A H 0.1897 0.4731 0.2241 0.047 Uiso 1 1 calc R . . H30B H 0.2042 0.4520 0.1741 0.047 Uiso 1 1 calc R . . C302 C 0.2935(4) 0.4183(4) 0.2182(2) 0.0377(15) Uani 1 1 d . . . H30C H 0.3238 0.4644 0.2192 0.045 Uiso 1 1 calc R . . H30D H 0.2981 0.3963 0.2481 0.045 Uiso 1 1 calc R . . C303 C 0.4039(4) 0.3502(4) 0.1998(2) 0.0407(16) Uani 1 1 d . . . H30E H 0.4059 0.3244 0.2286 0.049 Uiso 1 1 calc R . . H30F H 0.4365 0.3947 0.2034 0.049 Uiso 1 1 calc R . . C304 C 0.4355(4) 0.3029(5) 0.1664(3) 0.056(2) Uani 1 1 d . . . H30G H 0.4353 0.3293 0.1379 0.067 Uiso 1 1 calc R . . H30H H 0.4906 0.2899 0.1755 0.067 Uiso 1 1 calc R . . C305 C 0.4210(6) 0.1949(7) 0.1263(5) 0.108(5) Uani 1 1 d . . . H30I H 0.4112 0.2196 0.0975 0.130 Uiso 1 1 calc R . . H30J H 0.4785 0.1889 0.1319 0.130 Uiso 1 1 calc R . . C306 C 0.3853(5) 0.1265(5) 0.1247(4) 0.083(3) Uani 1 1 d . . . H30K H 0.3975 0.1021 0.1534 0.100 Uiso 1 1 calc R . . H30L H 0.4099 0.0973 0.1019 0.100 Uiso 1 1 calc R . . C307 C 0.0780(4) 0.3868(4) 0.1859(2) 0.0433(17) Uani 1 1 d . . . H30M H 0.0385 0.3535 0.1975 0.052 Uiso 1 1 calc R . . H30N H 0.0633 0.4372 0.1935 0.052 Uiso 1 1 calc R . . C308 C 0.0756(4) 0.3797(4) 0.1373(2) 0.0402(16) Uani 1 1 d . . . H30O H 0.0245 0.3976 0.1241 0.048 Uiso 1 1 calc R . . H30P H 0.1179 0.4093 0.1255 0.048 Uiso 1 1 calc R . . C309 C 0.0617(4) 0.2908(4) 0.0805(2) 0.0452(18) Uani 1 1 d . . . H30Q H 0.0876 0.3258 0.0613 0.054 Uiso 1 1 calc R . . H30R H 0.0040 0.2969 0.0755 0.054 Uiso 1 1 calc R . . C310 C 0.0840(4) 0.2162(4) 0.0696(2) 0.0484(19) Uani 1 1 d . . . H31A H 0.0603 0.1816 0.0900 0.058 Uiso 1 1 calc R . . H31B H 0.0639 0.2043 0.0391 0.058 Uiso 1 1 calc R . . C311 C 0.1926(5) 0.1414(4) 0.0555(3) 0.053(2) Uani 1 1 d . . . H31C H 0.1837 0.1419 0.0229 0.063 Uiso 1 1 calc R . . H31D H 0.1621 0.1006 0.0672 0.063 Uiso 1 1 calc R . . C312 C 0.2798(5) 0.1312(5) 0.0685(3) 0.058(2) Uani 1 1 d . . . H31E H 0.2986 0.0872 0.0535 0.069 Uiso 1 1 calc R . . H31F H 0.3090 0.1736 0.0576 0.069 Uiso 1 1 calc R . . C313 C 0.1471(4) 0.3491(4) 0.2544(2) 0.0469(18) Uani 1 1 d . . . H31G H 0.1080 0.3818 0.2669 0.056 Uiso 1 1 calc R . . H31H H 0.1978 0.3559 0.2718 0.056 Uiso 1 1 calc R . . C314 C 0.1207(5) 0.2713(4) 0.2590(3) 0.054(2) Uani 1 1 d . . . H31I H 0.1095 0.2613 0.2901 0.065 Uiso 1 1 calc R . . H31J H 0.0721 0.2626 0.2400 0.065 Uiso 1 1 calc R . . C315 C 0.1670(7) 0.1498(5) 0.2539(3) 0.079(3) Uani 1 1 d . . . H31K H 0.1336 0.1454 0.2793 0.095 Uiso 1 1 calc R . . H31L H 0.2177 0.1254 0.2622 0.095 Uiso 1 1 calc R . . C316 C 0.1286(7) 0.1120(6) 0.2162(4) 0.098(4) Uani 1 1 d . . . H31M H 0.1183 0.0611 0.2249 0.117 Uiso 1 1 calc R . . H31N H 0.0772 0.1355 0.2087 0.117 Uiso 1 1 calc R . . C317 C 0.2394(6) 0.0645(5) 0.1788(3) 0.069(3) Uani 1 1 d . . . H31O H 0.2254 0.0161 0.1904 0.083 Uiso 1 1 calc R . . H31P H 0.2816 0.0856 0.1989 0.083 Uiso 1 1 calc R . . C318 C 0.2679(5) 0.0567(4) 0.1325(3) 0.063(2) Uani 1 1 d . . . H31Q H 0.3098 0.0193 0.1330 0.076 Uiso 1 1 calc R . . H31R H 0.2237 0.0392 0.1124 0.076 Uiso 1 1 calc R . . N1E N 0.5201(4) 0.5226(4) 0.6475(2) 0.0544(17) Uani 1 1 d . . . H1E3 H 0.5616 0.4980 0.6373 0.082 Uiso 0.67 1 calc PR . . H1E4 H 0.5247 0.5709 0.6413 0.082 Uiso 0.67 1 calc PR . . H1E5 H 0.4746 0.5051 0.6342 0.082 Uiso 0.67 1 calc PR . . C1E C 0.5194(4) 0.5128(4) 0.6950(2) 0.0455(17) Uani 1 1 d . . . H1E1 H 0.5701 0.5299 0.7092 0.055 Uiso 1 1 calc R . . H1E2 H 0.5144 0.4602 0.7016 0.055 Uiso 1 1 calc R . . C2E C 0.4528(4) 0.5538(4) 0.7146(3) 0.0511(19) Uani 1 1 d . . . H2E1 H 0.4022 0.5373 0.7001 0.061 Uiso 1 1 calc R . . H2E2 H 0.4525 0.5421 0.7465 0.061 Uiso 1 1 calc R . . N2E N 0.4595(4) 0.6312(4) 0.7094(3) 0.066(2) Uani 1 1 d . . . H2E3 H 0.4183 0.6535 0.7214 0.098 Uiso 0.67 1 calc PR . . H2E4 H 0.4592 0.6423 0.6802 0.098 Uiso 0.67 1 calc PR . . H2E5 H 0.5053 0.6469 0.7234 0.098 Uiso 0.67 1 calc PR . . N1S N 0.7194(5) 0.9433(6) 0.4090(3) 0.107(3) Uani 1 1 d . . . H1S3 H 0.7680 0.9505 0.3991 0.160 Uiso 0.67 1 calc PR . . H1S4 H 0.7014 0.9858 0.4201 0.160 Uiso 0.67 1 calc PR . . H1S5 H 0.6859 0.9281 0.3862 0.160 Uiso 0.67 1 calc PR . . C1S C 0.7237(5) 0.8887(7) 0.4430(3) 0.086(3) Uani 1 1 d . . . H1S1 H 0.7606 0.9060 0.4674 0.103 Uiso 1 1 calc R . . H1S2 H 0.7464 0.8439 0.4309 0.103 Uiso 1 1 calc R . . C2S C 0.6463(5) 0.8691(6) 0.4621(3) 0.075(3) Uani 1 1 d . . . H2S1 H 0.6194 0.9146 0.4701 0.090 Uiso 1 1 calc R . . H2S2 H 0.6124 0.8442 0.4390 0.090 Uiso 1 1 calc R . . N2S N 0.6548(4) 0.8239(4) 0.4996(2) 0.0592(18) Uani 1 1 d . . . H2S3 H 0.6067 0.8153 0.5099 0.089 Uiso 0.67 1 calc PR . . H2S4 H 0.6862 0.8462 0.5210 0.089 Uiso 0.67 1 calc PR . . H2S5 H 0.6770 0.7808 0.4922 0.089 Uiso 0.67 1 calc PR . . 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 Sn1 0.0410(3) 0.0388(3) 0.0413(3) -0.0047(2) 0.0008(2) -0.0014(2) As1 0.0413(4) 0.0307(4) 0.0280(3) -0.0052(3) -0.0072(3) 0.0058(3) As2 0.0349(4) 0.0467(5) 0.0294(3) 0.0002(3) 0.0042(3) 0.0070(3) As3 0.0296(3) 0.0296(4) 0.0429(4) -0.0020(3) 0.0025(3) -0.0032(3) As4 0.0610(5) 0.0311(4) 0.0342(4) 0.0025(3) -0.0069(3) 0.0030(3) As5 0.0365(4) 0.0417(4) 0.0352(4) 0.0001(3) -0.0025(3) -0.0118(3) As6 0.0476(4) 0.0318(4) 0.0278(3) -0.0056(3) 0.0086(3) -0.0074(3) As7 0.0568(4) 0.0269(4) 0.0356(4) -0.0006(3) -0.0004(3) -0.0075(3) As8 0.0377(4) 0.0337(4) 0.0322(4) -0.0023(3) -0.0081(3) 0.0052(3) As9 0.0320(3) 0.0342(4) 0.0348(4) 0.0011(3) -0.0005(3) 0.0002(3) As10 0.0331(4) 0.0345(4) 0.0446(4) -0.0074(3) 0.0027(3) 0.0048(3) As11 0.0515(4) 0.0383(4) 0.0448(4) -0.0133(3) -0.0082(3) 0.0027(3) As12 0.0357(4) 0.0352(4) 0.0465(4) 0.0075(3) -0.0053(3) 0.0058(3) As13 0.0497(4) 0.0351(4) 0.0427(4) 0.0062(3) 0.0101(3) 0.0025(3) As14 0.0474(4) 0.0282(4) 0.0530(4) -0.0017(3) 0.0045(3) 0.0020(3) As15 0.0343(3) 0.0284(4) 0.0222(3) 0.0016(2) -0.0006(2) 0.0038(3) K1 0.0289(7) 0.0312(8) 0.0292(7) -0.0022(6) 0.0008(5) -0.0001(6) N11 0.036(3) 0.033(3) 0.044(3) 0.004(3) -0.001(2) 0.000(3) N12 0.035(3) 0.030(3) 0.044(3) -0.004(2) 0.002(2) 0.000(2) O11 0.043(3) 0.035(3) 0.033(2) -0.003(2) 0.0069(19) 0.000(2) O12 0.037(3) 0.039(3) 0.048(3) 0.001(2) 0.013(2) 0.004(2) O13 0.043(3) 0.054(3) 0.030(2) 0.006(2) -0.005(2) -0.004(2) O14 0.042(3) 0.048(3) 0.034(3) -0.010(2) 0.006(2) -0.010(2) O15 0.030(2) 0.039(3) 0.042(3) 0.003(2) 0.0018(19) 0.000(2) O16 0.031(2) 0.032(3) 0.056(3) 0.005(2) -0.006(2) 0.002(2) C101 0.045(4) 0.025(4) 0.072(5) -0.001(3) 0.009(4) 0.008(3) C102 0.043(4) 0.039(4) 0.055(4) -0.016(3) 0.011(3) 0.003(3) C103 0.050(4) 0.055(5) 0.037(4) -0.010(3) 0.013(3) 0.005(4) C104 0.042(4) 0.055(5) 0.034(4) 0.006(3) 0.009(3) -0.001(4) C105 0.042(4) 0.050(5) 0.058(5) 0.002(4) 0.010(3) -0.009(4) C106 0.050(4) 0.029(4) 0.064(5) 0.011(3) 0.006(4) -0.006(3) C107 0.051(4) 0.036(4) 0.051(4) 0.023(3) 0.005(3) -0.008(3) C108 0.046(4) 0.048(5) 0.046(4) 0.017(4) -0.001(3) -0.004(4) C109 0.040(4) 0.072(6) 0.026(3) 0.003(3) -0.003(3) -0.014(4) C110 0.055(5) 0.077(6) 0.029(4) -0.010(4) 0.005(3) -0.016(4) C111 0.060(5) 0.043(5) 0.049(5) -0.012(4) -0.009(4) -0.001(4) C112 0.047(4) 0.034(4) 0.058(5) -0.007(3) -0.005(3) -0.007(3) C113 0.043(4) 0.033(4) 0.050(4) 0.001(3) 0.000(3) -0.012(3) C114 0.032(3) 0.036(4) 0.056(4) 0.003(3) 0.001(3) -0.005(3) C115 0.028(3) 0.057(5) 0.041(4) -0.004(3) -0.005(3) 0.006(3) C116 0.028(3) 0.043(4) 0.046(4) -0.001(3) -0.009(3) 0.009(3) C117 0.037(4) 0.044(5) 0.055(5) 0.006(4) -0.001(3) 0.002(3) C118 0.050(4) 0.030(4) 0.070(5) -0.006(4) -0.001(4) 0.010(3) K2 0.0280(7) 0.0270(7) 0.0301(7) 0.0022(5) 0.0021(5) 0.0003(6) N21 0.038(3) 0.038(3) 0.033(3) -0.003(2) 0.005(2) -0.002(3) N22 0.031(3) 0.027(3) 0.031(3) 0.001(2) 0.000(2) 0.002(2) O21 0.032(2) 0.040(3) 0.036(2) -0.001(2) 0.0062(19) -0.001(2) O22 0.037(2) 0.029(3) 0.037(2) 0.0056(19) 0.0070(19) -0.005(2) O23 0.039(3) 0.049(3) 0.035(3) -0.001(2) -0.0062(19) -0.001(2) O24 0.025(2) 0.041(3) 0.040(3) 0.002(2) 0.0001(18) 0.001(2) O25 0.049(3) 0.027(2) 0.033(2) 0.0027(19) 0.0052(19) -0.006(2) O26 0.038(2) 0.021(2) 0.031(2) 0.0007(17) -0.0030(18) -0.0014(19) C201 0.045(4) 0.050(5) 0.040(4) -0.002(3) 0.010(3) -0.002(4) C202 0.052(4) 0.052(5) 0.035(4) -0.002(3) 0.017(3) 0.005(4) C203 0.033(4) 0.052(5) 0.049(4) -0.009(4) 0.004(3) -0.003(3) C204 0.032(3) 0.053(5) 0.042(4) 0.012(3) 0.002(3) -0.010(3) C205 0.041(4) 0.029(4) 0.048(4) -0.005(3) 0.004(3) -0.007(3) C206 0.037(4) 0.034(4) 0.044(4) -0.008(3) 0.000(3) -0.004(3) C207 0.048(4) 0.053(5) 0.041(4) -0.010(3) -0.003(3) -0.008(4) C208 0.048(4) 0.052(5) 0.041(4) -0.006(3) -0.007(3) 0.004(4) C209 0.032(4) 0.046(5) 0.053(4) 0.005(3) -0.012(3) 0.006(3) C210 0.023(3) 0.049(5) 0.061(5) 0.006(4) -0.002(3) 0.010(3) C211 0.037(4) 0.034(4) 0.050(4) 0.007(3) 0.012(3) 0.011(3) C212 0.046(4) 0.026(4) 0.042(4) -0.005(3) 0.001(3) 0.011(3) C213 0.068(5) 0.024(4) 0.038(4) -0.004(3) 0.002(3) 0.006(3) C214 0.060(5) 0.032(4) 0.042(4) -0.012(3) 0.011(3) -0.010(3) C215 0.049(4) 0.025(4) 0.033(3) 0.006(3) 0.007(3) -0.004(3) C216 0.038(3) 0.024(3) 0.034(3) 0.008(3) 0.000(3) -0.001(3) C217 0.044(4) 0.029(4) 0.027(3) -0.001(3) -0.005(3) -0.006(3) C218 0.045(4) 0.036(4) 0.034(4) -0.005(3) 0.004(3) 0.006(3) K3 0.0301(7) 0.0266(8) 0.0400(8) 0.0011(6) -0.0013(6) 0.0007(6) N31 0.029(3) 0.030(3) 0.037(3) -0.006(2) -0.001(2) 0.000(2) N32 0.051(4) 0.032(3) 0.061(4) -0.013(3) -0.013(3) 0.007(3) O31 0.029(2) 0.042(3) 0.037(2) 0.001(2) -0.0057(18) 0.001(2) O32 0.034(3) 0.065(4) 0.117(5) -0.039(4) 0.005(3) 0.002(3) O33 0.034(2) 0.040(3) 0.041(3) 0.002(2) -0.004(2) 0.005(2) O34 0.040(3) 0.034(3) 0.040(3) -0.006(2) 0.000(2) -0.001(2) O35 0.067(4) 0.035(3) 0.066(4) 0.018(3) 0.019(3) 0.004(3) O36 0.073(4) 0.039(3) 0.075(4) 0.014(3) 0.006(3) -0.010(3) C301 0.046(4) 0.027(4) 0.042(4) -0.008(3) -0.002(3) 0.004(3) C302 0.040(4) 0.035(4) 0.038(4) -0.005(3) -0.004(3) -0.007(3) C303 0.034(4) 0.042(4) 0.045(4) 0.004(3) -0.007(3) -0.005(3) C304 0.029(4) 0.070(6) 0.068(5) -0.007(4) -0.001(3) -0.005(4) C305 0.047(5) 0.122(10) 0.155(11) -0.092(9) -0.002(6) 0.014(6) C306 0.047(5) 0.063(6) 0.136(9) -0.052(6) -0.017(5) 0.023(5) C307 0.032(4) 0.039(4) 0.059(5) -0.005(3) 0.004(3) 0.009(3) C308 0.032(3) 0.034(4) 0.053(4) -0.003(3) -0.007(3) 0.006(3) C309 0.035(4) 0.056(5) 0.043(4) 0.000(3) -0.009(3) 0.009(3) C310 0.046(4) 0.060(5) 0.039(4) -0.011(4) -0.006(3) -0.012(4) C311 0.063(5) 0.043(5) 0.050(4) -0.010(4) -0.010(4) 0.005(4) C312 0.071(5) 0.039(5) 0.065(5) -0.007(4) 0.015(4) 0.006(4) C313 0.043(4) 0.057(5) 0.040(4) -0.008(4) 0.004(3) 0.003(4) C314 0.052(5) 0.056(5) 0.058(5) 0.009(4) 0.020(4) -0.008(4) C315 0.105(8) 0.056(6) 0.080(7) 0.013(5) 0.030(6) -0.012(6) C316 0.102(8) 0.080(8) 0.111(9) 0.028(7) 0.012(7) -0.045(7) C317 0.100(7) 0.034(5) 0.069(6) 0.008(4) -0.020(5) -0.004(5) C318 0.081(6) 0.028(4) 0.079(6) -0.013(4) -0.021(5) 0.009(4) N1E 0.053(4) 0.065(5) 0.045(4) 0.000(3) -0.003(3) -0.016(3) C1E 0.048(4) 0.044(5) 0.044(4) 0.007(3) 0.000(3) 0.004(3) C2E 0.055(5) 0.044(5) 0.052(5) 0.001(4) -0.009(4) -0.009(4) N2E 0.059(4) 0.039(4) 0.095(6) 0.001(4) -0.026(4) -0.003(3) N1S 0.082(6) 0.142(10) 0.096(7) -0.001(7) 0.011(5) -0.026(6) C1S 0.068(6) 0.137(10) 0.053(6) 0.021(6) 0.011(5) 0.013(6) C2S 0.059(5) 0.088(7) 0.077(6) 0.026(6) -0.008(5) -0.005(5) N2S 0.046(4) 0.058(5) 0.072(5) -0.001(4) -0.005(3) 0.002(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 Sn1 As10 2.6465(8) . ? Sn1 As3 2.6555(8) . ? Sn1 As15 2.7485(8) . ? As1 As4 2.3670(10) . ? As1 As3 2.4092(9) . ? As1 As2 2.4264(9) . ? As2 As5 2.4089(10) . ? As2 As15 2.4691(9) . ? As3 As6 2.3970(9) . ? As4 As7 2.3840(10) . ? As5 As6 2.4579(9) . ? As5 As7 2.4608(10) . ? As6 As7 2.4537(9) . ? As8 As11 2.3703(10) . ? As8 As9 2.4101(9) . ? As8 As10 2.4174(10) . ? As9 As12 2.4119(9) . ? As9 As15 2.4824(9) . ? As10 As13 2.3948(10) . ? As11 As14 2.3840(11) . ? As12 As13 2.4656(10) . ? As12 As14 2.4658(10) . ? As13 As14 2.4582(10) . ? K1 O16 2.769(4) . ? K1 O14 2.790(5) . ? K1 O12 2.790(5) . ? K1 O15 2.831(4) . ? K1 O13 2.849(5) . ? K1 O11 2.853(4) . ? K1 N12 2.991(6) . ? K1 N11 3.058(6) . ? N11 C101 1.466(8) . ? N11 C113 1.478(8) . ? N11 C107 1.481(8) . ? N12 C118 1.474(8) . ? N12 C112 1.477(9) . ? N12 C106 1.488(9) . ? O11 C102 1.414(8) . ? O11 C103 1.433(8) . ? O12 C105 1.411(8) . ? O12 C104 1.419(8) . ? O13 C108 1.411(9) . ? O13 C109 1.420(8) . ? O14 C111 1.403(9) . ? O14 C110 1.429(8) . ? O15 C114 1.424(8) . ? O15 C115 1.446(8) . ? O16 C117 1.421(8) . ? O16 C116 1.422(7) . ? C101 C102 1.494(10) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.509(10) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? C105 C106 1.517(10) . ? C105 H10I 0.9900 . ? C105 H10J 0.9900 . ? C106 H10K 0.9900 . ? C106 H10L 0.9900 . ? C107 C108 1.498(10) . ? C107 H10M 0.9900 . ? C107 H10N 0.9900 . ? C108 H10O 0.9900 . ? C108 H10P 0.9900 . ? C109 C110 1.481(11) . ? C109 H10Q 0.9900 . ? C109 H10R 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.515(10) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.487(9) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 C116 1.472(10) . ? C115 H11K 0.9900 . ? C115 H11L 0.9900 . ? C116 H11M 0.9900 . ? C116 H11N 0.9900 . ? C117 C118 1.493(10) . ? C117 H11O 0.9900 . ? C117 H11P 0.9900 . ? C118 H11Q 0.9900 . ? C118 H11R 0.9900 . ? K2 O21 2.781(4) . ? K2 O23 2.800(4) . ? K2 O26 2.808(4) . ? K2 O24 2.814(4) . ? K2 O25 2.826(5) . ? K2 O22 2.842(4) . ? K2 N21 3.038(5) . ? K2 N22 3.077(5) . ? N21 C213 1.460(8) . ? N21 C201 1.477(8) . ? N21 C207 1.479(8) . ? N22 C212 1.472(8) . ? N22 C218 1.477(8) . ? N22 C206 1.490(8) . ? O21 C202 1.417(8) . ? O21 C203 1.428(8) . ? O22 C205 1.424(8) . ? O22 C204 1.430(7) . ? O23 C209 1.412(8) . ? O23 C208 1.426(8) . ? O24 C211 1.427(8) . ? O24 C210 1.431(8) . ? O25 C215 1.427(7) . ? O25 C214 1.446(8) . ? O26 C216 1.416(7) . ? O26 C217 1.443(7) . ? C201 C202 1.503(10) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C203 C204 1.479(10) . ? C203 H20E 0.9900 . ? C203 H20F 0.9900 . ? C204 H20G 0.9900 . ? C204 H20H 0.9900 . ? C205 C206 1.511(9) . ? C205 H20I 0.9900 . ? C205 H20J 0.9900 . ? C206 H20K 0.9900 . ? C206 H20L 0.9900 . ? C207 C208 1.515(10) . ? C207 H20M 0.9900 . ? C207 H20N 0.9900 . ? C208 H20O 0.9900 . ? C208 H20P 0.9900 . ? C209 C210 1.480(10) . ? C209 H20Q 0.9900 . ? C209 H20R 0.9900 . ? C210 H21A 0.9900 . ? C210 H21B 0.9900 . ? C211 C212 1.497(9) . ? C211 H21C 0.9900 . ? C211 H21D 0.9900 . ? C212 H21E 0.9900 . ? C212 H21F 0.9900 . ? C213 C214 1.487(9) . ? C213 H21G 0.9900 . ? C213 H21H 0.9900 . ? C214 H21I 0.9900 . ? C214 H21J 0.9900 . ? C215 C216 1.488(9) . ? C215 H21K 0.9900 . ? C215 H21L 0.9900 . ? C216 H21M 0.9900 . ? C216 H21N 0.9900 . ? C217 C218 1.505(9) . ? C217 H21O 0.9900 . ? C217 H21P 0.9900 . ? C218 H21Q 0.9900 . ? C218 H21R 0.9900 . ? K3 O33 2.742(4) . ? K3 O32 2.788(5) . ? K3 O36 2.796(5) . ? K3 O35 2.831(5) . ? K3 O31 2.838(5) . ? K3 O34 2.844(5) . ? K3 N31 2.939(5) . ? K3 N32 2.983(6) . ? K3 C317 3.473(8) . ? N31 C313 1.475(8) . ? N31 C301 1.476(8) . ? N31 C307 1.490(8) . ? N32 C312 1.430(10) . ? N32 C318 1.450(10) . ? N32 C306 1.497(9) . ? O31 C302 1.416(8) . ? O31 C303 1.425(7) . ? O32 C304 1.393(9) . ? O32 C305 1.452(11) . ? O33 C308 1.433(8) . ? O33 C309 1.436(8) . ? O34 C310 1.421(8) . ? O34 C311 1.435(8) . ? O35 C314 1.411(9) . ? O35 C315 1.430(10) . ? O36 C317 1.415(10) . ? O36 C316 1.456(12) . ? C301 C302 1.507(9) . ? C301 H30A 0.9900 . ? C301 H30B 0.9900 . ? C302 H30C 0.9900 . ? C302 H30D 0.9900 . ? C303 C304 1.464(10) . ? C303 H30E 0.9900 . ? C303 H30F 0.9900 . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 C306 1.394(14) . ? C305 H30I 0.9900 . ? C305 H30J 0.9900 . ? C306 H30K 0.9900 . ? C306 H30L 0.9900 . ? C307 C308 1.477(10) . ? C307 H30M 0.9900 . ? C307 H30N 0.9900 . ? C308 H30O 0.9900 . ? C308 H30P 0.9900 . ? C309 C310 1.463(10) . ? C309 H30Q 0.9900 . ? C309 H30R 0.9900 . ? C310 H31A 0.9900 . ? C310 H31B 0.9900 . ? C311 C312 1.525(10) . ? C311 H31C 0.9900 . ? C311 H31D 0.9900 . ? C312 H31E 0.9900 . ? C312 H31F 0.9900 . ? C313 C314 1.504(11) . ? C313 H31G 0.9900 . ? C313 H31H 0.9900 . ? C314 H31I 0.9900 . ? C314 H31J 0.9900 . ? C315 C316 1.457(14) . ? C315 H31K 0.9900 . ? C315 H31L 0.9900 . ? C316 H31M 0.9900 . ? C316 H31N 0.9900 . ? C317 C318 1.523(12) . ? C317 H31O 0.9900 . ? C317 H31P 0.9900 . ? C318 H31Q 0.9900 . ? C318 H31R 0.9900 . ? N1E C1E 1.451(9) . ? N1E H1E3 0.9100 . ? N1E H1E4 0.9100 . ? N1E H1E5 0.9100 . ? C1E C2E 1.516(10) . ? C1E H1E1 0.9900 . ? C1E H1E2 0.9900 . ? C2E N2E 1.433(10) . ? C2E H2E1 0.9900 . ? C2E H2E2 0.9900 . ? N2E H2E3 0.9100 . ? N2E H2E4 0.9100 . ? N2E H2E5 0.9100 . ? N1S C1S 1.436(13) . ? N1S H1S3 0.9100 . ? N1S H1S4 0.9100 . ? N1S H1S5 0.9100 . ? C1S C2S 1.518(12) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S N2S 1.408(10) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? N2S H2S3 0.9100 . ? N2S H2S4 0.9100 . ? N2S H2S5 0.9100 . ? 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 As10 Sn1 As3 94.36(3) . . ? As10 Sn1 As15 99.36(2) . . ? As3 Sn1 As15 97.66(2) . . ? As4 As1 As3 100.67(3) . . ? As4 As1 As2 98.61(4) . . ? As3 As1 As2 100.93(3) . . ? As5 As2 As1 101.43(3) . . ? As5 As2 As15 93.47(3) . . ? As1 As2 As15 106.21(3) . . ? As6 As3 As1 100.70(3) . . ? As6 As3 Sn1 93.73(3) . . ? As1 As3 Sn1 105.95(3) . . ? As1 As4 As7 99.61(3) . . ? As2 As5 As6 104.50(3) . . ? As2 As5 As7 101.26(3) . . ? As6 As5 As7 59.85(3) . . ? As3 As6 As7 102.81(3) . . ? As3 As6 As5 106.18(3) . . ? As7 As6 As5 60.13(3) . . ? As4 As7 As6 106.84(3) . . ? As4 As7 As5 107.13(4) . . ? As6 As7 As5 60.02(3) . . ? As11 As8 As9 96.81(3) . . ? As11 As8 As10 101.24(4) . . ? As9 As8 As10 101.30(3) . . ? As8 As9 As12 102.10(3) . . ? As8 As9 As15 106.93(3) . . ? As12 As9 As15 92.64(3) . . ? As13 As10 As8 100.65(3) . . ? As13 As10 Sn1 90.78(3) . . ? As8 As10 Sn1 106.02(3) . . ? As8 As11 As14 100.26(3) . . ? As9 As12 As13 104.46(3) . . ? As9 As12 As14 100.51(3) . . ? As13 As12 As14 59.80(3) . . ? As10 As13 As14 103.59(4) . . ? As10 As13 As12 106.08(3) . . ? As14 As13 As12 60.11(3) . . ? As11 As14 As13 106.56(4) . . ? As11 As14 As12 106.28(4) . . ? As13 As14 As12 60.10(3) . . ? As2 As15 As9 96.04(3) . . ? As2 As15 Sn1 104.53(3) . . ? As9 As15 Sn1 102.68(3) . . ? O16 K1 O14 96.40(14) . . ? O16 K1 O12 96.25(14) . . ? O14 K1 O12 100.30(14) . . ? O16 K1 O15 61.49(14) . . ? O14 K1 O15 134.70(14) . . ? O12 K1 O15 119.89(14) . . ? O16 K1 O13 117.91(14) . . ? O14 K1 O13 60.15(14) . . ? O12 K1 O13 141.06(14) . . ? O15 K1 O13 94.03(13) . . ? O16 K1 O11 136.41(14) . . ? O14 K1 O11 122.46(14) . . ? O12 K1 O11 60.68(13) . . ? O15 K1 O11 96.57(13) . . ? O13 K1 O11 99.61(14) . . ? O16 K1 N12 59.66(14) . . ? O14 K1 N12 61.67(15) . . ? O12 K1 N12 59.77(14) . . ? O15 K1 N12 120.39(14) . . ? O13 K1 N12 120.88(15) . . ? O11 K1 N12 119.69(14) . . ? O16 K1 N11 120.78(14) . . ? O14 K1 N11 118.17(15) . . ? O12 K1 N11 119.98(15) . . ? O15 K1 N11 60.03(14) . . ? O13 K1 N11 59.04(15) . . ? O11 K1 N11 60.00(14) . . ? N12 K1 N11 179.56(15) . . ? C101 N11 C113 111.0(6) . . ? C101 N11 C107 110.1(5) . . ? C113 N11 C107 109.7(5) . . ? C101 N11 K1 108.3(4) . . ? C113 N11 K1 107.3(4) . . ? C107 N11 K1 110.4(4) . . ? C118 N12 C112 112.0(5) . . ? C118 N12 C106 107.6(6) . . ? C112 N12 C106 109.4(5) . . ? C118 N12 K1 110.6(4) . . ? C112 N12 K1 106.3(4) . . ? C106 N12 K1 110.9(4) . . ? C102 O11 C103 110.4(5) . . ? C102 O11 K1 117.6(4) . . ? C103 O11 K1 111.5(4) . . ? C105 O12 C104 110.9(5) . . ? C105 O12 K1 121.4(4) . . ? C104 O12 K1 117.3(4) . . ? C108 O13 C109 111.0(5) . . ? C108 O13 K1 117.5(4) . . ? C109 O13 K1 115.3(4) . . ? C111 O14 C110 110.8(6) . . ? C111 O14 K1 117.8(4) . . ? C110 O14 K1 113.9(4) . . ? C114 O15 C115 110.9(5) . . ? C114 O15 K1 116.7(4) . . ? C115 O15 K1 110.6(4) . . ? C117 O16 C116 111.8(5) . . ? C117 O16 K1 121.3(4) . . ? C116 O16 K1 115.7(4) . . ? N11 C101 C102 114.9(6) . . ? N11 C101 H10A 108.6 . . ? C102 C101 H10A 108.6 . . ? N11 C101 H10B 108.5 . . ? C102 C101 H10B 108.6 . . ? H10A C101 H10B 107.5 . . ? O11 C102 C101 110.4(6) . . ? O11 C102 H10C 109.6 . . ? C101 C102 H10C 109.6 . . ? O11 C102 H10D 109.6 . . ? C101 C102 H10D 109.6 . . ? H10C C102 H10D 108.1 . . ? O11 C103 C104 109.8(5) . . ? O11 C103 H10E 109.7 . . ? C104 C103 H10E 109.7 . . ? O11 C103 H10F 109.7 . . ? C104 C103 H10F 109.7 . . ? H10E C103 H10F 108.2 . . ? O12 C104 C103 109.8(6) . . ? O12 C104 H10G 109.7 . . ? C103 C104 H10G 109.7 . . ? O12 C104 H10H 109.7 . . ? C103 C104 H10H 109.7 . . ? H10G C104 H10H 108.2 . . ? O12 C105 C106 109.5(5) . . ? O12 C105 H10I 109.8 . . ? C106 C105 H10I 109.8 . . ? O12 C105 H10J 109.8 . . ? C106 C105 H10J 109.8 . . ? H10I C105 H10J 108.2 . . ? N12 C106 C105 112.8(6) . . ? N12 C106 H10K 109.0 . . ? C105 C106 H10K 109.0 . . ? N12 C106 H10L 109.0 . . ? C105 C106 H10L 109.0 . . ? H10K C106 H10L 107.8 . . ? N11 C107 C108 113.3(6) . . ? N11 C107 H10M 108.9 . . ? C108 C107 H10M 108.9 . . ? N11 C107 H10N 108.9 . . ? C108 C107 H10N 108.9 . . ? H10M C107 H10N 107.7 . . ? O13 C108 C107 109.4(6) . . ? O13 C108 H10O 109.8 . . ? C107 C108 H10O 109.8 . . ? O13 C108 H10P 109.8 . . ? C107 C108 H10P 109.8 . . ? H10O C108 H10P 108.3 . . ? O13 C109 C110 110.4(6) . . ? O13 C109 H10Q 109.6 . . ? C110 C109 H10Q 109.6 . . ? O13 C109 H10R 109.6 . . ? C110 C109 H10R 109.6 . . ? H10Q C109 H10R 108.1 . . ? O14 C110 C109 109.7(6) . . ? O14 C110 H11A 109.7 . . ? C109 C110 H11A 109.7 . . ? O14 C110 H11B 109.7 . . ? C109 C110 H11B 109.7 . . ? H11A C110 H11B 108.2 . . ? O14 C111 C112 110.8(6) . . ? O14 C111 H11C 109.5 . . ? C112 C111 H11C 109.5 . . ? O14 C111 H11D 109.5 . . ? C112 C111 H11D 109.5 . . ? H11C C111 H11D 108.1 . . ? N12 C112 C111 112.9(6) . . ? N12 C112 H11E 109.0 . . ? C111 C112 H11E 109.0 . . ? N12 C112 H11F 109.0 . . ? C111 C112 H11F 109.0 . . ? H11E C112 H11F 107.8 . . ? N11 C113 C114 113.8(6) . . ? N11 C113 H11G 108.8 . . ? C114 C113 H11G 108.8 . . ? N11 C113 H11H 108.8 . . ? C114 C113 H11H 108.8 . . ? H11G C113 H11H 107.7 . . ? O15 C114 C113 108.3(5) . . ? O15 C114 H11I 110.0 . . ? C113 C114 H11I 110.0 . . ? O15 C114 H11J 110.0 . . ? C113 C114 H11J 110.0 . . ? H11I C114 H11J 108.4 . . ? O15 C115 C116 110.4(5) . . ? O15 C115 H11K 109.6 . . ? C116 C115 H11K 109.6 . . ? O15 C115 H11L 109.6 . . ? C116 C115 H11L 109.6 . . ? H11K C115 H11L 108.1 . . ? O16 C116 C115 110.3(5) . . ? O16 C116 H11M 109.6 . . ? C115 C116 H11M 109.6 . . ? O16 C116 H11N 109.6 . . ? C115 C116 H11N 109.6 . . ? H11M C116 H11N 108.1 . . ? O16 C117 C118 109.6(6) . . ? O16 C117 H11O 109.8 . . ? C118 C117 H11O 109.8 . . ? O16 C117 H11P 109.8 . . ? C118 C117 H11P 109.8 . . ? H11O C117 H11P 108.2 . . ? N12 C118 C117 113.1(6) . . ? N12 C118 H11Q 109.0 . . ? C117 C118 H11Q 109.0 . . ? N12 C118 H11R 109.0 . . ? C117 C118 H11R 109.0 . . ? H11Q C118 H11R 107.8 . . ? O21 K2 O23 97.89(13) . . ? O21 K2 O26 131.53(13) . . ? O23 K2 O26 125.78(14) . . ? O21 K2 O24 124.09(14) . . ? O23 K2 O24 60.71(13) . . ? O26 K2 O24 97.65(13) . . ? O21 K2 O25 93.89(13) . . ? O23 K2 O25 99.75(14) . . ? O26 K2 O25 61.92(12) . . ? O24 K2 O25 137.70(13) . . ? O21 K2 O22 59.82(13) . . ? O23 K2 O22 132.92(14) . . ? O26 K2 O22 95.64(12) . . ? O24 K2 O22 96.08(13) . . ? O25 K2 O22 121.06(13) . . ? O21 K2 N21 60.79(14) . . ? O23 K2 N21 59.76(14) . . ? O26 K2 N21 120.94(14) . . ? O24 K2 N21 120.22(14) . . ? O25 K2 N21 59.57(14) . . ? O22 K2 N21 120.47(14) . . ? O21 K2 N22 118.38(14) . . ? O23 K2 N22 120.30(14) . . ? O26 K2 N22 59.85(13) . . ? O24 K2 N22 59.76(13) . . ? O25 K2 N22 121.14(13) . . ? O22 K2 N22 58.73(13) . . ? N21 K2 N22 179.08(15) . . ? C213 N21 C201 111.3(5) . . ? C213 N21 C207 109.2(6) . . ? C201 N21 C207 109.8(5) . . ? C213 N21 K2 109.6(4) . . ? C201 N21 K2 107.3(4) . . ? C207 N21 K2 109.6(4) . . ? C212 N22 C218 110.2(5) . . ? C212 N22 C206 109.1(5) . . ? C218 N22 C206 109.0(5) . . ? C212 N22 K2 108.6(3) . . ? C218 N22 K2 109.0(4) . . ? C206 N22 K2 111.0(3) . . ? C202 O21 C203 111.2(5) . . ? C202 O21 K2 117.0(4) . . ? C203 O21 K2 115.4(4) . . ? C205 O22 C204 112.1(5) . . ? C205 O22 K2 119.5(3) . . ? C204 O22 K2 115.2(4) . . ? C209 O23 C208 112.3(5) . . ? C209 O23 K2 115.7(4) . . ? C208 O23 K2 118.6(4) . . ? C211 O24 C210 112.0(5) . . ? C211 O24 K2 116.1(3) . . ? C210 O24 K2 111.2(4) . . ? C215 O25 C214 110.3(5) . . ? C215 O25 K2 111.3(4) . . ? C214 O25 K2 114.6(4) . . ? C216 O26 C217 111.5(4) . . ? C216 O26 K2 111.7(3) . . ? C217 O26 K2 117.4(3) . . ? N21 C201 C202 112.8(6) . . ? N21 C201 H20A 109.0 . . ? C202 C201 H20A 109.0 . . ? N21 C201 H20B 109.0 . . ? C202 C201 H20B 109.0 . . ? H20A C201 H20B 107.8 . . ? O21 C202 C201 109.4(6) . . ? O21 C202 H20C 109.8 . . ? C201 C202 H20C 109.8 . . ? O21 C202 H20D 109.8 . . ? C201 C202 H20D 109.8 . . ? H20C C202 H20D 108.2 . . ? O21 C203 C204 109.1(5) . . ? O21 C203 H20E 109.9 . . ? C204 C203 H20E 109.9 . . ? O21 C203 H20F 109.9 . . ? C204 C203 H20F 109.9 . . ? H20E C203 H20F 108.3 . . ? O22 C204 C203 109.3(6) . . ? O22 C204 H20G 109.8 . . ? C203 C204 H20G 109.8 . . ? O22 C204 H20H 109.8 . . ? C203 C204 H20H 109.8 . . ? H20G C204 H20H 108.3 . . ? O22 C205 C206 109.0(5) . . ? O22 C205 H20I 109.9 . . ? C206 C205 H20I 109.9 . . ? O22 C205 H20J 109.9 . . ? C206 C205 H20J 109.9 . . ? H20I C205 H20J 108.3 . . ? N22 C206 C205 113.3(5) . . ? N22 C206 H20K 108.9 . . ? C205 C206 H20K 108.9 . . ? N22 C206 H20L 108.9 . . ? C205 C206 H20L 108.9 . . ? H20K C206 H20L 107.7 . . ? N21 C207 C208 112.6(6) . . ? N21 C207 H20M 109.1 . . ? C208 C207 H20M 109.1 . . ? N21 C207 H20N 109.1 . . ? C208 C207 H20N 109.1 . . ? H20M C207 H20N 107.8 . . ? O23 C208 C207 108.4(6) . . ? O23 C208 H20O 110.0 . . ? C207 C208 H20O 110.0 . . ? O23 C208 H20P 110.0 . . ? C207 C208 H20P 110.0 . . ? H20O C208 H20P 108.4 . . ? O23 C209 C210 108.3(5) . . ? O23 C209 H20Q 110.0 . . ? C210 C209 H20Q 110.0 . . ? O23 C209 H20R 110.0 . . ? C210 C209 H20R 110.0 . . ? H20Q C209 H20R 108.4 . . ? O24 C210 C209 110.4(5) . . ? O24 C210 H21A 109.6 . . ? C209 C210 H21A 109.6 . . ? O24 C210 H21B 109.6 . . ? C209 C210 H21B 109.6 . . ? H21A C210 H21B 108.1 . . ? O24 C211 C212 109.3(5) . . ? O24 C211 H21C 109.8 . . ? C212 C211 H21C 109.8 . . ? O24 C211 H21D 109.8 . . ? C212 C211 H21D 109.8 . . ? H21C C211 H21D 108.3 . . ? N22 C212 C211 112.8(5) . . ? N22 C212 H21E 109.0 . . ? C211 C212 H21E 109.0 . . ? N22 C212 H21F 109.0 . . ? C211 C212 H21F 109.0 . . ? H21E C212 H21F 107.8 . . ? N21 C213 C214 113.7(6) . . ? N21 C213 H21G 108.8 . . ? C214 C213 H21G 108.8 . . ? N21 C213 H21H 108.8 . . ? C214 C213 H21H 108.8 . . ? H21G C213 H21H 107.7 . . ? O25 C214 C213 107.0(5) . . ? O25 C214 H21I 110.3 . . ? C213 C214 H21I 110.3 . . ? O25 C214 H21J 110.3 . . ? C213 C214 H21J 110.3 . . ? H21I C214 H21J 108.6 . . ? O25 C215 C216 109.6(5) . . ? O25 C215 H21K 109.8 . . ? C216 C215 H21K 109.8 . . ? O25 C215 H21L 109.8 . . ? C216 C215 H21L 109.8 . . ? H21K C215 H21L 108.2 . . ? O26 C216 C215 110.7(5) . . ? O26 C216 H21M 109.5 . . ? C215 C216 H21M 109.5 . . ? O26 C216 H21N 109.5 . . ? C215 C216 H21N 109.5 . . ? H21M C216 H21N 108.1 . . ? O26 C217 C218 109.2(5) . . ? O26 C217 H21O 109.8 . . ? C218 C217 H21O 109.8 . . ? O26 C217 H21P 109.8 . . ? C218 C217 H21P 109.8 . . ? H21O C217 H21P 108.3 . . ? N22 C218 C217 112.9(5) . . ? N22 C218 H21Q 109.0 . . ? C217 C218 H21Q 109.0 . . ? N22 C218 H21R 109.0 . . ? C217 C218 H21R 109.0 . . ? H21Q C218 H21R 107.8 . . ? O33 K3 O32 152.52(19) . . ? O33 K3 O36 95.90(16) . . ? O32 K3 O36 105.88(19) . . ? O33 K3 O35 96.39(15) . . ? O32 K3 O35 108.10(19) . . ? O36 K3 O35 63.77(17) . . ? O33 K3 O31 108.44(14) . . ? O32 K3 O31 59.35(15) . . ? O36 K3 O31 147.99(16) . . ? O35 K3 O31 92.45(15) . . ? O33 K3 O34 60.09(13) . . ? O32 K3 O34 107.12(17) . . ? O36 K3 O34 79.56(16) . . ? O35 K3 O34 134.51(16) . . ? O31 K3 O34 130.50(14) . . ? O33 K3 N31 62.42(14) . . ? O32 K3 N31 119.36(16) . . ? O36 K3 N31 115.86(17) . . ? O35 K3 N31 60.58(15) . . ? O31 K3 N31 61.91(13) . . ? O34 K3 N31 121.64(14) . . ? O33 K3 N32 119.01(15) . . ? O32 K3 N32 61.17(17) . . ? O36 K3 N32 61.03(18) . . ? O35 K3 N32 115.77(17) . . ? O31 K3 N32 119.46(15) . . ? O34 K3 N32 60.49(15) . . ? N31 K3 N32 176.35(18) . . ? O33 K3 C317 117.17(19) . . ? O32 K3 C317 82.9(2) . . ? O36 K3 C317 23.01(19) . . ? O35 K3 C317 72.34(19) . . ? O31 K3 C317 132.96(18) . . ? O34 K3 C317 84.46(17) . . ? N31 K3 C317 131.9(2) . . ? N32 K3 C317 44.5(2) . . ? O33 K3 C308 22.08(14) . . ? O32 K3 C308 140.36(19) . . ? O36 K3 C308 113.63(17) . . ? O35 K3 C308 92.43(16) . . ? O31 K3 C308 86.98(14) . . ? O34 K3 C308 77.90(15) . . ? N31 K3 C308 43.84(15) . . ? N32 K3 C308 138.38(16) . . ? C317 K3 C308 136.4(2) . . ? C313 N31 C301 111.8(5) . . ? C313 N31 C307 109.4(5) . . ? C301 N31 C307 109.2(5) . . ? C313 N31 K3 111.1(4) . . ? C301 N31 K3 106.9(3) . . ? C307 N31 K3 108.4(4) . . ? C312 N32 C318 112.4(6) . . ? C312 N32 C306 109.8(7) . . ? C318 N32 C306 109.0(7) . . ? C312 N32 K3 107.8(4) . . ? C318 N32 K3 109.6(5) . . ? C306 N32 K3 108.2(4) . . ? C302 O31 C303 112.0(5) . . ? C302 O31 K3 116.3(3) . . ? C303 O31 K3 113.9(4) . . ? C304 O32 C305 109.9(7) . . ? C304 O32 K3 118.5(4) . . ? C305 O32 K3 115.5(5) . . ? C308 O33 C309 111.6(5) . . ? C308 O33 K3 111.9(3) . . ? C309 O33 K3 118.7(4) . . ? C310 O34 C311 111.9(5) . . ? C310 O34 K3 110.3(4) . . ? C311 O34 K3 118.8(4) . . ? C314 O35 C315 113.4(6) . . ? C314 O35 K3 114.3(4) . . ? C315 O35 K3 112.1(5) . . ? C317 O36 C316 115.4(7) . . ? C317 O36 K3 106.4(5) . . ? C316 O36 K3 109.6(5) . . ? N31 C301 C302 113.7(5) . . ? N31 C301 H30A 108.8 . . ? C302 C301 H30A 108.8 . . ? N31 C301 H30B 108.8 . . ? C302 C301 H30B 108.8 . . ? H30A C301 H30B 107.7 . . ? O31 C302 C301 109.8(5) . . ? O31 C302 H30C 109.7 . . ? C301 C302 H30C 109.7 . . ? O31 C302 H30D 109.7 . . ? C301 C302 H30D 109.7 . . ? H30C C302 H30D 108.2 . . ? O31 C303 C304 110.7(5) . . ? O31 C303 H30E 109.5 . . ? C304 C303 H30E 109.5 . . ? O31 C303 H30F 109.5 . . ? C304 C303 H30F 109.5 . . ? H30E C303 H30F 108.1 . . ? O32 C304 C303 110.6(6) . . ? O32 C304 H30G 109.5 . . ? C303 C304 H30G 109.5 . . ? O32 C304 H30H 109.5 . . ? C303 C304 H30H 109.5 . . ? H30G C304 H30H 108.1 . . ? C306 C305 O32 111.1(10) . . ? C306 C305 H30I 109.4 . . ? O32 C305 H30I 109.4 . . ? C306 C305 H30J 109.4 . . ? O32 C305 H30J 109.4 . . ? H30I C305 H30J 108.0 . . ? C305 C306 N32 117.4(8) . . ? C305 C306 H30K 107.9 . . ? N32 C306 H30K 107.9 . . ? C305 C306 H30L 107.9 . . ? N32 C306 H30L 107.9 . . ? H30K C306 H30L 107.2 . . ? C308 C307 N31 113.4(5) . . ? C308 C307 H30M 108.9 . . ? N31 C307 H30M 108.9 . . ? C308 C307 H30N 108.9 . . ? N31 C307 H30N 108.9 . . ? H30M C307 H30N 107.7 . . ? O33 C308 C307 109.2(6) . . ? O33 C308 K3 46.0(3) . . ? C307 C308 K3 84.1(4) . . ? O33 C308 H30O 109.8 . . ? C307 C308 H30O 109.8 . . ? K3 C308 H30O 155.8 . . ? O33 C308 H30P 109.8 . . ? C307 C308 H30P 109.8 . . ? K3 C308 H30P 83.9 . . ? H30O C308 H30P 108.3 . . ? O33 C309 C310 108.6(6) . . ? O33 C309 H30Q 110.0 . . ? C310 C309 H30Q 110.0 . . ? O33 C309 H30R 110.0 . . ? C310 C309 H30R 110.0 . . ? H30Q C309 H30R 108.4 . . ? O34 C310 C309 109.9(6) . . ? O34 C310 H31A 109.7 . . ? C309 C310 H31A 109.7 . . ? O34 C310 H31B 109.7 . . ? C309 C310 H31B 109.7 . . ? H31A C310 H31B 108.2 . . ? O34 C311 C312 108.7(6) . . ? O34 C311 H31C 109.9 . . ? C312 C311 H31C 109.9 . . ? O34 C311 H31D 109.9 . . ? C312 C311 H31D 109.9 . . ? H31C C311 H31D 108.3 . . ? N32 C312 C311 114.2(7) . . ? N32 C312 H31E 108.7 . . ? C311 C312 H31E 108.7 . . ? N32 C312 H31F 108.7 . . ? C311 C312 H31F 108.7 . . ? H31E C312 H31F 107.6 . . ? N31 C313 C314 112.7(6) . . ? N31 C313 H31G 109.1 . . ? C314 C313 H31G 109.1 . . ? N31 C313 H31H 109.1 . . ? C314 C313 H31H 109.1 . . ? H31G C313 H31H 107.8 . . ? O35 C314 C313 108.2(6) . . ? O35 C314 H31I 110.1 . . ? C313 C314 H31I 110.1 . . ? O35 C314 H31J 110.1 . . ? C313 C314 H31J 110.1 . . ? H31I C314 H31J 108.4 . . ? O35 C315 C316 113.9(8) . . ? O35 C315 H31K 108.8 . . ? C316 C315 H31K 108.8 . . ? O35 C315 H31L 108.8 . . ? C316 C315 H31L 108.8 . . ? H31K C315 H31L 107.7 . . ? O36 C316 C315 115.2(8) . . ? O36 C316 H31M 108.5 . . ? C315 C316 H31M 108.5 . . ? O36 C316 H31N 108.5 . . ? C315 C316 H31N 108.5 . . ? H31M C316 H31N 107.5 . . ? O36 C317 C318 108.5(7) . . ? O36 C317 K3 50.6(3) . . ? C318 C317 K3 87.4(4) . . ? O36 C317 H31O 110.0 . . ? C318 C317 H31O 110.0 . . ? K3 C317 H31O 158.5 . . ? O36 C317 H31P 110.0 . . ? C318 C317 H31P 110.0 . . ? K3 C317 H31P 75.6 . . ? H31O C317 H31P 108.4 . . ? N32 C318 C317 113.5(6) . . ? N32 C318 H31Q 108.9 . . ? C317 C318 H31Q 108.9 . . ? N32 C318 H31R 108.9 . . ? C317 C318 H31R 108.9 . . ? H31Q C318 H31R 107.7 . . ? C1E N1E H1E3 109.5 . . ? C1E N1E H1E4 109.5 . . ? H1E3 N1E H1E4 109.5 . . ? C1E N1E H1E5 109.5 . . ? H1E3 N1E H1E5 109.5 . . ? H1E4 N1E H1E5 109.5 . . ? N1E C1E C2E 112.5(6) . . ? N1E C1E H1E1 109.1 . . ? C2E C1E H1E1 109.1 . . ? N1E C1E H1E2 109.1 . . ? C2E C1E H1E2 109.1 . . ? H1E1 C1E H1E2 107.8 . . ? N2E C2E C1E 112.4(7) . . ? N2E C2E H2E1 109.1 . . ? C1E C2E H2E1 109.1 . . ? N2E C2E H2E2 109.1 . . ? C1E C2E H2E2 109.1 . . ? H2E1 C2E H2E2 107.8 . . ? C2E N2E H2E3 109.5 . . ? C2E N2E H2E4 109.5 . . ? H2E3 N2E H2E4 109.5 . . ? C2E N2E H2E5 109.5 . . ? H2E3 N2E H2E5 109.5 . . ? H2E4 N2E H2E5 109.5 . . ? C1S N1S H1S3 109.5 . . ? C1S N1S H1S4 109.5 . . ? H1S3 N1S H1S4 109.5 . . ? C1S N1S H1S5 109.5 . . ? H1S3 N1S H1S5 109.5 . . ? H1S4 N1S H1S5 109.5 . . ? N1S C1S C2S 115.7(8) . . ? N1S C1S H1S1 108.3 . . ? C2S C1S H1S1 108.3 . . ? N1S C1S H1S2 108.3 . . ? C2S C1S H1S2 108.3 . . ? H1S1 C1S H1S2 107.4 . . ? N2S C2S C1S 113.7(7) . . ? N2S C2S H2S1 108.8 . . ? C1S C2S H2S1 108.8 . . ? N2S C2S H2S2 108.8 . . ? C1S C2S H2S2 108.8 . . ? H2S1 C2S H2S2 107.7 . . ? C2S N2S H2S3 109.5 . . ? C2S N2S H2S4 109.5 . . ? H2S3 N2S H2S4 109.5 . . ? C2S N2S H2S5 109.5 . . ? H2S3 N2S H2S5 109.5 . . ? H2S4 N2S H2S5 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.616 _refine_diff_density_min -1.757 _refine_diff_density_rms 0.162