Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Junk, Peter Courtney' 'Baldamus, Jens' 'Berghof, Christiane' 'Cole, Marcus L.' 'Evans, David J.' 'Hey-Hawkins, Evamarie' _publ_contact_author_name 'Dr Peter Courtney Junk' _publ_contact_author_address ; School of Chemistry Monash University P.O. Box 23 Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email 'PETER.JUNK@SCI.MONASH.EDU.AU' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; N,N'-Di(tolyl)formamidinate complexes of potassium:Studies of ancillary donor imposed molecular and supramolecular structure ; data_Compound_1 _database_code_CSD 188555 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[{K2(FTolP)2(THF)3/2}n]' _chemical_melting_point ? _chemical_formula_moiety 'C42 H54 K2 N4 O3' _chemical_formula_sum 'C42 H54 K2 N4 O3' _chemical_formula_weight 741.09 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.613(2) _cell_length_b 14.042(3) _cell_length_c 14.724(3) _cell_angle_alpha 114.64(3) _cell_angle_beta 105.23(3) _cell_angle_gamma 99.57(3) _cell_volume 1998.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needles' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.279 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.9462 _exptl_absorpt_correction_T_max 0.9593 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Kappa CCD' _diffrn_measurement_method 'single crystal' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33627 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9721 _reflns_number_gt 6159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9721 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1693 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.078 _refine_ls_shift/su_mean 0.002 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 C41 C 0.0376(3) 0.8651(3) 0.3931(3) 0.0653(10) Uani 1 1 d . . . H41A H 0.0061 0.9117 0.3638 0.078 Uiso 1 1 calc R . . H41B H 0.0470 0.8974 0.4696 0.078 Uiso 1 1 calc R . . C29 C 0.4742(3) 0.1420(3) 0.4957(3) 0.0625(9) Uani 1 1 d . . . H29A H 0.4403 0.0649 0.4775 0.094 Uiso 1 1 calc R . . H29B H 0.5362 0.1835 0.5695 0.094 Uiso 1 1 calc R . . H29C H 0.5148 0.1453 0.4460 0.094 Uiso 1 1 calc R . . C40 C 0.1591(3) 0.8550(3) 0.3810(3) 0.0654(10) Uani 1 1 d . . . H40A H 0.2314 0.9164 0.4429 0.078 Uiso 1 1 calc R . . H40B H 0.1617 0.8536 0.3138 0.078 Uiso 1 1 calc R . . C22 C -0.6490(3) 0.0493(3) 0.1689(3) 0.0661(10) Uani 1 1 d . . . H22A H -0.6901 0.0479 0.2188 0.099 Uiso 1 1 calc R . . H22B H -0.6541 -0.0260 0.1204 0.099 Uiso 1 1 calc R . . H22C H -0.6913 0.0807 0.1268 0.099 Uiso 1 1 calc R . . C42 C -0.0503(3) 0.7468(2) 0.3285(2) 0.0433(7) Uani 1 1 d . . . H42A H -0.1092 0.7349 0.3634 0.052 Uiso 1 1 calc R . . H42B H -0.0996 0.7302 0.2548 0.052 Uiso 1 1 calc R . . C7 C 0.6953(3) 0.8926(2) 0.3164(3) 0.0514(8) Uani 1 1 d . . . H7A H 0.7355 0.8828 0.3780 0.077 Uiso 1 1 calc R . . H7B H 0.6815 0.9647 0.3423 0.077 Uiso 1 1 calc R . . H7C H 0.7497 0.8886 0.2750 0.077 Uiso 1 1 calc R . . C20 C -0.4765(3) 0.2298(3) 0.3082(3) 0.0530(8) Uani 1 1 d . . . H20 H -0.5394 0.2622 0.3234 0.064 Uiso 1 1 calc R . . C37 C -0.3844(3) 0.2704(2) 0.0742(3) 0.0497(8) Uani 1 1 d . . . H37A H -0.4209 0.2521 -0.0021 0.060 Uiso 1 1 calc R . . H37B H -0.4235 0.2080 0.0826 0.060 Uiso 1 1 calc R . . C36 C -0.4021(3) 0.3766(3) 0.1477(3) 0.0499(8) Uani 1 1 d . . . H36A H -0.4810 0.3860 0.1118 0.060 Uiso 1 1 calc R . . H36B H -0.4029 0.3782 0.2154 0.060 Uiso 1 1 calc R . . C17 C -0.2931(3) 0.1393(2) 0.2712(2) 0.0483(7) Uani 1 1 d . . . H17 H -0.2303 0.1059 0.2581 0.058 Uiso 1 1 calc R . . C14 C 0.0922(3) -0.0780(2) -0.1169(2) 0.0511(8) Uani 1 1 d . . . H14A H 0.0613 -0.1291 -0.1943 0.077 Uiso 1 1 calc R . . H14B H 0.0356 -0.1015 -0.0858 0.077 Uiso 1 1 calc R . . H14C H 0.1768 -0.0781 -0.0824 0.077 Uiso 1 1 calc R . . C25 C 0.2511(3) 0.1326(2) 0.4065(2) 0.0459(7) Uani 1 1 d . . . H25 H 0.2354 0.0575 0.3569 0.055 Uiso 1 1 calc R . . C33 C 0.2433(3) 0.3229(2) 0.2371(3) 0.0469(7) Uani 1 1 d . . . H33A H 0.2414 0.2594 0.2507 0.056 Uiso 1 1 calc R . . H33B H 0.2646 0.3075 0.1726 0.056 Uiso 1 1 calc R . . C32 C 0.3358(3) 0.4293(2) 0.3344(3) 0.0500(8) Uani 1 1 d . . . H32A H 0.3372 0.4304 0.4024 0.060 Uiso 1 1 calc R . . H32B H 0.4218 0.4397 0.3335 0.060 Uiso 1 1 calc R . . C35 C -0.2889(3) 0.4636(2) 0.1684(2) 0.0405(6) Uani 1 1 d . . . H35A H -0.3036 0.4815 0.1089 0.049 Uiso 1 1 calc R . . H35B H -0.2689 0.5318 0.2365 0.049 Uiso 1 1 calc R . . C31 C 0.2838(3) 0.5160(2) 0.3208(2) 0.0396(6) Uani 1 1 d . . . H31A H 0.3066 0.5819 0.3915 0.048 Uiso 1 1 calc R . . H31B H 0.3173 0.5387 0.2751 0.048 Uiso 1 1 calc R . . C26 C 0.3682(3) 0.1919(3) 0.4864(2) 0.0457(7) Uani 1 1 d . . . C21 C -0.3515(3) 0.2935(2) 0.3626(2) 0.0471(8) Uani 1 1 d . . . H21 H -0.3304 0.3693 0.4129 0.057 Uiso 1 1 calc R . . C18 C -0.4158(3) 0.0767(2) 0.2163(2) 0.0495(7) Uani 1 1 d . . . H18 H -0.4361 0.0012 0.1654 0.059 Uiso 1 1 calc R . . C38 C -0.2424(3) 0.2971(2) 0.1121(2) 0.0478(7) Uani 1 1 d . . . H38A H -0.2140 0.2622 0.1564 0.057 Uiso 1 1 calc R . . H38B H -0.2161 0.2689 0.0496 0.057 Uiso 1 1 calc R . . C39 C 0.1591(3) 0.7463(2) 0.3774(2) 0.0457(7) Uani 1 1 d . . . H39A H 0.2094 0.7121 0.3359 0.055 Uiso 1 1 calc R . . H39B H 0.1953 0.7569 0.4510 0.055 Uiso 1 1 calc R . . C27 C 0.3873(3) 0.2999(3) 0.5567(2) 0.0483(8) Uani 1 1 d . . . H27 H 0.4668 0.3428 0.6133 0.058 Uiso 1 1 calc R . . C28 C 0.2929(3) 0.3475(2) 0.5469(2) 0.0456(7) Uani 1 1 d . . . H28 H 0.3100 0.4229 0.5963 0.055 Uiso 1 1 calc R . . C19 C -0.5122(3) 0.1195(3) 0.2320(2) 0.0479(7) Uani 1 1 d . . . C10 C 0.2061(3) 0.1131(2) -0.0772(2) 0.0399(6) Uani 1 1 d . . . H10 H 0.2797 0.0918 -0.0761 0.048 Uiso 1 1 calc R . . C24 C 0.1554(3) 0.1791(2) 0.3962(2) 0.0431(7) Uani 1 1 d . . . H24 H 0.0759 0.1354 0.3397 0.052 Uiso 1 1 calc R . . C4 C 0.5711(3) 0.8029(2) 0.2458(2) 0.0392(6) Uani 1 1 d . . . C5 C 0.4565(3) 0.8235(2) 0.2417(2) 0.0421(7) Uani 1 1 d . . . H5 H 0.4567 0.8970 0.2815 0.051 Uiso 1 1 calc R . . C3 C 0.5641(3) 0.6941(2) 0.1831(2) 0.0385(6) Uani 1 1 d . . . H3 H 0.6399 0.6772 0.1825 0.046 Uiso 1 1 calc R . . C23 C 0.1735(3) 0.2885(2) 0.4668(2) 0.0384(6) Uani 1 1 d . . . C9 C 0.2117(3) 0.2200(2) -0.0572(2) 0.0368(6) Uani 1 1 d . . . H9 H 0.2878 0.2693 -0.0450 0.044 Uiso 1 1 calc R . . C12 C -0.0094(3) 0.0697(2) -0.1035(2) 0.0436(7) Uani 1 1 d . . . H12 H -0.0869 0.0179 -0.1219 0.052 Uiso 1 1 calc R . . C16 C -0.2565(3) 0.2495(2) 0.3453(2) 0.0392(6) Uani 1 1 d . . . C34 C 0.1186(3) 0.3468(2) 0.2239(2) 0.0370(6) Uani 1 1 d . . . H34A H 0.0639 0.3095 0.1468 0.044 Uiso 1 1 calc R . . H34B H 0.0744 0.3203 0.2621 0.044 Uiso 1 1 calc R . . C13 C -0.0057(3) 0.1759(2) -0.0825(2) 0.0399(6) Uani 1 1 d . . . H13 H -0.0808 0.1952 -0.0869 0.048 Uiso 1 1 calc R . . C11 C 0.0968(3) 0.0368(2) -0.0985(2) 0.0383(6) Uani 1 1 d . . . C2 C 0.4515(3) 0.6100(2) 0.1218(2) 0.0356(6) Uani 1 1 d . . . H2 H 0.4516 0.5373 0.0792 0.043 Uiso 1 1 calc R . . C6 C 0.3422(3) 0.7388(2) 0.1807(2) 0.0382(6) Uani 1 1 d . . . H6 H 0.2663 0.7559 0.1796 0.046 Uiso 1 1 calc R . . C15 C 0.2105(3) 0.4449(2) 0.0338(2) 0.0336(6) Uani 1 1 d . . . H15 H 0.2842 0.4283 0.0600 0.040 Uiso 1 1 calc R . . C30 C -0.0388(3) 0.2795(2) 0.4152(2) 0.0380(6) Uani 1 1 d . . . H30 H -0.0587 0.2029 0.3930 0.046 Uiso 1 1 calc R . . C1 C 0.3365(2) 0.6294(2) 0.12107(19) 0.0314(6) Uani 1 1 d . . . N3 N -0.1313(2) 0.32294(18) 0.40121(18) 0.0403(5) Uani 1 1 d . . . C8 C 0.1053(3) 0.2558(2) -0.05503(19) 0.0329(6) Uani 1 1 d . . . N4 N 0.0807(2) 0.34170(18) 0.45972(18) 0.0407(5) Uani 1 1 d . . . N2 N 0.1030(2) 0.36313(18) -0.02909(17) 0.0352(5) Uani 1 1 d . . . N1 N 0.2177(2) 0.54916(18) 0.06115(17) 0.0341(5) Uani 1 1 d . . . O3 O 0.02937(18) 0.67718(14) 0.32563(14) 0.0397(4) Uani 1 1 d . . . O2 O -0.18833(17) 0.41560(15) 0.17507(14) 0.0381(4) Uani 1 1 d . . . O1 O 0.14838(16) 0.46537(14) 0.26970(14) 0.0343(4) Uani 1 1 d . . . K2 K -0.01052(5) 0.50391(4) 0.38290(4) 0.03203(16) Uani 1 1 d . . . K1 K -0.00059(5) 0.51229(4) 0.12125(4) 0.03160(15) 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 C41 0.068(2) 0.0429(19) 0.091(3) 0.0302(18) 0.039(2) 0.0232(17) C29 0.065(2) 0.082(2) 0.065(2) 0.049(2) 0.0295(19) 0.038(2) C40 0.065(2) 0.0407(18) 0.082(3) 0.0247(17) 0.024(2) 0.0134(16) C22 0.044(2) 0.082(3) 0.072(2) 0.045(2) 0.0123(18) 0.0124(18) C42 0.0472(18) 0.0440(16) 0.0463(16) 0.0245(13) 0.0217(14) 0.0182(14) C7 0.0483(19) 0.0501(18) 0.0496(18) 0.0268(15) 0.0106(15) 0.0056(14) C20 0.051(2) 0.073(2) 0.062(2) 0.0446(19) 0.0277(17) 0.0387(18) C37 0.0485(19) 0.0502(18) 0.0487(18) 0.0318(15) 0.0091(15) 0.0048(14) C36 0.0407(18) 0.070(2) 0.0567(19) 0.0429(17) 0.0220(15) 0.0189(15) C17 0.0445(19) 0.0493(18) 0.0553(19) 0.0242(15) 0.0251(16) 0.0172(15) C14 0.071(2) 0.0406(16) 0.0385(16) 0.0187(13) 0.0194(16) 0.0112(15) C25 0.059(2) 0.0348(15) 0.0431(16) 0.0181(13) 0.0204(16) 0.0129(14) C33 0.053(2) 0.0435(17) 0.0564(18) 0.0296(14) 0.0249(16) 0.0232(14) C32 0.0399(18) 0.0569(19) 0.063(2) 0.0393(16) 0.0137(15) 0.0178(15) C35 0.0491(18) 0.0445(16) 0.0396(15) 0.0265(13) 0.0205(14) 0.0188(13) C31 0.0344(16) 0.0443(16) 0.0410(15) 0.0246(13) 0.0101(13) 0.0100(12) C26 0.0481(19) 0.062(2) 0.0463(17) 0.0379(16) 0.0220(15) 0.0235(15) C21 0.069(2) 0.0368(15) 0.0337(15) 0.0191(12) 0.0095(15) 0.0227(15) C18 0.055(2) 0.0407(16) 0.0458(17) 0.0165(14) 0.0171(16) 0.0130(15) C38 0.0505(19) 0.0455(17) 0.0502(18) 0.0258(14) 0.0177(15) 0.0162(14) C39 0.0468(19) 0.0466(17) 0.0444(16) 0.0245(14) 0.0139(14) 0.0142(14) C27 0.0340(17) 0.069(2) 0.0317(15) 0.0235(15) 0.0092(13) -0.0001(15) C28 0.056(2) 0.0353(15) 0.0388(16) 0.0108(12) 0.0267(15) 0.0023(14) C19 0.0350(17) 0.060(2) 0.0510(18) 0.0388(16) 0.0062(14) 0.0057(14) C10 0.0383(16) 0.0426(16) 0.0413(15) 0.0209(13) 0.0142(13) 0.0174(13) C24 0.0377(17) 0.0495(17) 0.0328(14) 0.0197(13) 0.0060(13) 0.0037(13) C4 0.0410(17) 0.0446(16) 0.0350(14) 0.0251(13) 0.0115(13) 0.0090(13) C5 0.057(2) 0.0378(15) 0.0354(15) 0.0187(12) 0.0191(14) 0.0184(14) C3 0.0352(16) 0.0488(17) 0.0416(15) 0.0289(13) 0.0150(13) 0.0170(13) C23 0.0466(18) 0.0482(16) 0.0358(15) 0.0282(13) 0.0221(14) 0.0188(13) C9 0.0339(16) 0.0394(15) 0.0384(15) 0.0193(12) 0.0158(13) 0.0093(12) C12 0.0450(18) 0.0393(16) 0.0342(15) 0.0127(12) 0.0139(13) -0.0010(13) C16 0.0372(16) 0.0469(16) 0.0392(15) 0.0291(13) 0.0120(13) 0.0076(13) C34 0.0423(17) 0.0333(14) 0.0352(14) 0.0176(12) 0.0132(13) 0.0104(12) C13 0.0299(15) 0.0522(17) 0.0330(14) 0.0187(13) 0.0103(12) 0.0095(13) C11 0.0461(17) 0.0392(15) 0.0258(13) 0.0152(11) 0.0117(12) 0.0085(13) C2 0.0399(16) 0.0392(15) 0.0355(14) 0.0236(12) 0.0140(12) 0.0157(12) C6 0.0412(17) 0.0477(16) 0.0368(15) 0.0251(13) 0.0191(13) 0.0205(13) C15 0.0351(15) 0.0469(16) 0.0316(13) 0.0263(12) 0.0158(12) 0.0185(13) C30 0.0445(18) 0.0368(15) 0.0319(14) 0.0173(12) 0.0145(13) 0.0084(13) C1 0.0339(15) 0.0405(15) 0.0273(13) 0.0215(11) 0.0130(11) 0.0130(12) N3 0.0451(15) 0.0384(13) 0.0391(13) 0.0213(11) 0.0143(11) 0.0124(11) C8 0.0392(16) 0.0401(15) 0.0247(12) 0.0197(11) 0.0122(11) 0.0132(12) N4 0.0465(15) 0.0394(13) 0.0377(13) 0.0188(10) 0.0181(11) 0.0130(11) N2 0.0325(13) 0.0440(13) 0.0340(12) 0.0231(10) 0.0121(10) 0.0127(10) N1 0.0336(13) 0.0423(13) 0.0337(12) 0.0219(10) 0.0147(10) 0.0162(10) O3 0.0455(12) 0.0365(10) 0.0394(10) 0.0201(8) 0.0159(9) 0.0137(9) O2 0.0347(11) 0.0426(11) 0.0390(10) 0.0237(9) 0.0118(9) 0.0095(8) O1 0.0325(10) 0.0343(10) 0.0380(10) 0.0206(8) 0.0110(8) 0.0102(8) K2 0.0383(3) 0.0332(3) 0.0259(3) 0.0160(2) 0.0122(2) 0.0093(2) K1 0.0331(3) 0.0399(3) 0.0285(3) 0.0209(2) 0.0128(2) 0.0133(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C41 C40 1.491(5) . ? C41 C42 1.522(4) . ? C29 C26 1.518(4) . ? C40 C39 1.506(4) . ? C22 C19 1.516(4) . ? C42 O3 1.449(3) . ? C7 C4 1.504(4) . ? C20 C21 1.382(5) . ? C20 C19 1.387(4) . ? C37 C36 1.519(4) . ? C37 C38 1.519(4) . ? C36 C35 1.503(4) . ? C17 C18 1.357(4) . ? C17 C16 1.377(4) . ? C14 C11 1.509(4) . ? C25 C26 1.376(4) . ? C25 C24 1.386(4) . ? C33 C32 1.521(4) . ? C33 C34 1.522(4) . ? C32 C31 1.508(4) . ? C35 O2 1.444(3) . ? C31 O1 1.451(3) . ? C26 C27 1.371(4) . ? C21 C16 1.381(4) . ? C18 C19 1.382(4) . ? C38 O2 1.443(3) . ? C39 O3 1.444(3) . ? C27 C28 1.381(4) . ? C28 C23 1.394(4) . ? C10 C11 1.384(4) . ? C10 C9 1.390(4) . ? C24 C23 1.390(4) . ? C4 C3 1.391(4) . ? C4 C5 1.399(4) . ? C5 C6 1.394(4) . ? C3 C2 1.378(4) . ? C23 N4 1.415(4) . ? C9 C8 1.412(4) . ? C12 C11 1.381(4) . ? C12 C13 1.382(4) . ? C16 N3 1.421(4) . ? C34 O1 1.448(3) . ? C13 C8 1.396(4) . ? C2 C1 1.405(4) . ? C6 C1 1.394(4) . ? C15 N1 1.328(3) . ? C15 N2 1.328(3) . ? C15 K1 3.198(3) 2_565 ? C30 N4 1.327(4) . ? C30 N3 1.332(4) . ? C30 K2 3.066(3) 2_566 ? C1 N1 1.402(3) . ? N3 K2 2.843(2) . ? N3 K2 2.864(3) 2_566 ? C8 N2 1.400(3) . ? N4 K2 2.851(2) 2_566 ? N4 K2 3.148(2) . ? N2 K1 2.853(2) 2_565 ? N2 K1 3.017(2) . ? N1 K1 2.846(3) 2_565 ? N1 K1 2.933(2) . ? O3 K1 2.813(2) . ? O3 K2 2.8958(19) . ? O2 K2 2.798(2) . ? O2 K1 2.836(2) . ? O1 K2 2.770(2) . ? O1 K1 2.7923(19) . ? K2 N4 2.851(2) 2_566 ? K2 N3 2.864(3) 2_566 ? K2 C30 3.066(3) 2_566 ? K2 K2 3.4418(12) 2_566 ? K1 N1 2.846(3) 2_565 ? K1 N2 2.853(2) 2_565 ? K1 C15 3.198(3) 2_565 ? K1 K1 3.4450(12) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C40 C41 C42 103.9(3) . . ? C41 C40 C39 102.5(3) . . ? O3 C42 C41 106.1(2) . . ? C21 C20 C19 121.5(3) . . ? C36 C37 C38 103.2(2) . . ? C35 C36 C37 102.6(2) . . ? C18 C17 C16 122.3(3) . . ? C26 C25 C24 122.0(3) . . ? C32 C33 C34 102.8(2) . . ? C31 C32 C33 102.5(2) . . ? O2 C35 C36 105.0(2) . . ? O1 C31 C32 106.0(2) . . ? C27 C26 C25 117.4(3) . . ? C27 C26 C29 120.6(3) . . ? C25 C26 C29 122.0(3) . . ? C16 C21 C20 121.4(3) . . ? C17 C18 C19 122.0(3) . . ? O2 C38 C37 107.4(2) . . ? O3 C39 C40 106.4(2) . . ? C26 C27 C28 121.2(3) . . ? C27 C28 C23 122.2(3) . . ? C18 C19 C20 116.2(3) . . ? C18 C19 C22 121.6(3) . . ? C20 C19 C22 122.2(3) . . ? C11 C10 C9 122.1(3) . . ? C25 C24 C23 121.2(3) . . ? C3 C4 C5 116.3(3) . . ? C3 C4 C7 121.7(3) . . ? C5 C4 C7 122.0(3) . . ? C6 C5 C4 121.5(3) . . ? C2 C3 C4 122.5(3) . . ? C24 C23 C28 116.0(3) . . ? C24 C23 N4 124.2(3) . . ? C28 C23 N4 119.8(2) . . ? C10 C9 C8 120.6(3) . . ? C11 C12 C13 121.7(3) . . ? C17 C16 C21 116.5(3) . . ? C17 C16 N3 126.2(3) . . ? C21 C16 N3 117.2(3) . . ? O1 C34 C33 106.4(2) . . ? C12 C13 C8 121.9(3) . . ? C12 C11 C10 117.1(3) . . ? C12 C11 C14 121.0(3) . . ? C10 C11 C14 121.9(3) . . ? C3 C2 C1 121.4(3) . . ? C1 C6 C5 121.7(3) . . ? N1 C15 N2 121.8(2) . . ? N1 C15 K1 62.77(14) . 2_565 ? N2 C15 K1 63.05(13) . 2_565 ? N4 C30 N3 121.0(2) . . ? N4 C30 K2 68.10(15) . 2_566 ? N3 C30 K2 68.66(15) . 2_566 ? C6 C1 N1 118.1(2) . . ? C6 C1 C2 116.5(2) . . ? N1 C1 C2 125.3(2) . . ? C30 N3 C16 117.5(2) . . ? C30 N3 K2 100.58(17) . . ? C16 N3 K2 130.55(16) . . ? C30 N3 K2 85.67(16) . 2_566 ? C16 N3 K2 135.00(18) . 2_566 ? K2 N3 K2 74.18(7) . 2_566 ? C13 C8 N2 118.5(2) . . ? C13 C8 C9 116.3(2) . . ? N2 C8 C9 125.2(2) . . ? C30 N4 C23 117.6(2) . . ? C30 N4 K2 86.31(16) . 2_566 ? C23 N4 K2 133.01(17) . 2_566 ? C30 N4 K2 87.08(16) . . ? C23 N4 K2 143.94(17) . . ? K2 N4 K2 69.82(5) 2_566 . ? C15 N2 C8 117.5(2) . . ? C15 N2 K1 92.43(15) . 2_565 ? C8 N2 K1 141.89(16) . 2_565 ? C15 N2 K1 83.58(15) . . ? C8 N2 K1 130.79(16) . . ? K1 N2 K1 71.81(5) 2_565 . ? C15 N1 C1 118.1(2) . . ? C15 N1 K1 92.73(16) . 2_565 ? C1 N1 K1 139.02(16) . 2_565 ? C15 N1 K1 87.11(15) . . ? C1 N1 K1 130.36(15) . . ? K1 N1 K1 73.16(6) 2_565 . ? C39 O3 C42 108.6(2) . . ? C39 O3 K1 107.39(16) . . ? C42 O3 K1 116.67(15) . . ? C39 O3 K2 111.63(15) . . ? C42 O3 K2 123.30(15) . . ? K1 O3 K2 87.11(6) . . ? C38 O2 C35 108.4(2) . . ? C38 O2 K2 117.85(16) . . ? C35 O2 K2 114.64(15) . . ? C38 O2 K1 115.67(16) . . ? C35 O2 K1 110.63(14) . . ? K2 O2 K1 88.56(6) . . ? C34 O1 C31 109.19(19) . . ? C34 O1 K2 100.52(14) . . ? C31 O1 K2 122.76(15) . . ? C34 O1 K1 108.79(14) . . ? C31 O1 K1 122.51(14) . . ? K2 O1 K1 90.03(5) . . ? O1 K2 O2 81.22(6) . . ? O1 K2 N3 116.06(6) . . ? O2 K2 N3 90.16(7) . . ? O1 K2 N4 148.47(6) . 2_566 ? O2 K2 N4 111.74(7) . 2_566 ? N3 K2 N4 93.22(7) . 2_566 ? O1 K2 N3 109.02(7) . 2_566 ? O2 K2 N3 153.56(6) . 2_566 ? N3 K2 N3 105.82(7) . 2_566 ? N4 K2 N3 47.78(7) 2_566 2_566 ? O1 K2 O3 72.96(6) . . ? O2 K2 O3 74.83(6) . . ? N3 K2 O3 161.48(7) . . ? N4 K2 O3 82.66(6) 2_566 . ? N3 K2 O3 84.79(6) 2_566 . ? O1 K2 C30 124.68(7) . 2_566 ? O2 K2 C30 129.00(7) . 2_566 ? N3 K2 C30 109.54(7) . 2_566 ? N4 K2 C30 25.59(7) 2_566 2_566 ? N3 K2 C30 25.67(7) 2_566 2_566 ? O3 K2 C30 73.58(6) . 2_566 ? O1 K2 N4 85.49(6) . . ? O2 K2 N4 118.80(6) . . ? N3 K2 N4 45.09(7) . . ? N4 K2 N4 110.18(5) 2_566 . ? N3 K2 N4 86.84(7) 2_566 . ? O3 K2 N4 152.80(6) . . ? C30 K2 N4 107.38(7) 2_566 . ? O1 K2 K2 129.35(5) . 2_566 ? O2 K2 K2 138.37(5) . 2_566 ? N3 K2 K2 53.19(6) . 2_566 ? N4 K2 K2 59.16(5) 2_566 2_566 ? N3 K2 K2 52.63(5) 2_566 2_566 ? O3 K2 K2 135.05(5) . 2_566 ? C30 K2 K2 61.72(6) 2_566 2_566 ? N4 K2 K2 51.03(5) . 2_566 ? O1 K1 O3 73.92(6) . . ? O1 K1 O2 80.16(6) . . ? O3 K1 O2 75.55(7) . . ? O1 K1 N1 151.35(6) . 2_565 ? O3 K1 N1 120.16(7) . 2_565 ? O2 K1 N1 79.94(6) . 2_565 ? O1 K1 N2 159.80(6) . 2_565 ? O3 K1 N2 89.36(6) . 2_565 ? O2 K1 N2 107.01(6) . 2_565 ? N1 K1 N2 48.04(7) 2_565 2_565 ? O1 K1 N1 86.70(6) . . ? O3 K1 N1 113.64(7) . . ? O2 K1 N1 161.25(6) . . ? N1 K1 N1 106.84(6) 2_565 . ? N2 K1 N1 89.85(6) 2_565 . ? O1 K1 N2 83.37(6) . . ? O3 K1 N2 150.95(6) . . ? O2 K1 N2 118.62(6) . . ? N1 K1 N2 88.30(7) 2_565 . ? N2 K1 N2 108.19(5) 2_565 . ? N1 K1 N2 45.87(6) . . ? O1 K1 C15 169.58(6) . 2_565 ? O3 K1 C15 101.80(7) . 2_565 ? O2 K1 C15 89.59(6) . 2_565 ? N1 K1 C15 24.50(6) 2_565 2_565 ? N2 K1 C15 24.52(6) 2_565 2_565 ? N1 K1 C15 103.71(6) . 2_565 ? N2 K1 C15 103.42(7) . 2_565 ? O1 K1 K1 132.54(5) . 2_565 ? O3 K1 K1 139.15(5) . 2_565 ? O2 K1 K1 131.44(6) . 2_565 ? N1 K1 K1 54.58(5) 2_565 2_565 ? N2 K1 K1 56.32(5) 2_565 2_565 ? N1 K1 K1 52.26(5) . 2_565 ? N2 K1 K1 51.88(5) . 2_565 ? C15 K1 K1 56.63(5) 2_565 2_565 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.974 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.067 #===END data_Compound_3 _database_code_CSD 188557 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[{K(FTolP)(DME)}n]' _chemical_melting_point ? _chemical_formula_moiety 'C19 H25 K N2 O2' _chemical_formula_sum 'C19 H25 K N2 O2' _chemical_formula_weight 352.51 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7331(11) _cell_length_b 10.4662(14) _cell_length_c 13.3689(19) _cell_angle_alpha 107.764(3) _cell_angle_beta 90.529(3) _cell_angle_gamma 108.107(3) _cell_volume 972.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.9193 _exptl_absorpt_correction_T_max 0.9451 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Kappa CCD' _diffrn_measurement_method 'Single Crystal' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6518 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.98 _reflns_number_total 4496 _reflns_number_gt 2677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4496 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1744 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.29724(8) 0.02898(6) 0.52961(5) 0.0381(2) Uani 1 1 d . . . O1 O 0.1873(3) 0.1713(2) 0.71466(19) 0.0509(6) Uani 1 1 d . . . N1 N 0.3338(3) -0.2524(2) 0.40793(19) 0.0354(5) Uani 1 1 d . . . C1 C 0.2273(4) -0.3697(3) 0.3244(2) 0.0346(6) Uani 1 1 d . . . O2 O -0.0525(3) -0.0962(2) 0.58753(16) 0.0402(5) Uani 1 1 d . . . N2 N 0.4400(3) -0.1613(2) 0.58396(19) 0.0341(5) Uani 1 1 d . . . C2 C 0.0844(4) -0.4841(3) 0.3363(3) 0.0373(7) Uani 1 1 d . . . C3 C -0.0188(4) -0.5957(3) 0.2498(3) 0.0422(7) Uani 1 1 d . . . C4 C 0.0120(4) -0.5987(3) 0.1473(3) 0.0434(7) Uani 1 1 d . . . C5 C 0.1503(4) -0.4853(3) 0.1348(3) 0.0433(7) Uani 1 1 d . . . C6 C 0.2538(4) -0.3728(3) 0.2204(3) 0.0397(7) Uani 1 1 d . . . C7 C -0.1029(6) -0.7218(5) 0.0551(4) 0.0634(11) Uani 1 1 d . . . C8 C 0.4862(4) -0.1822(3) 0.6776(2) 0.0330(6) Uani 1 1 d . . . C9 C 0.5092(4) -0.3062(3) 0.6876(3) 0.0364(7) Uani 1 1 d . . . C10 C 0.5616(4) -0.3117(3) 0.7847(3) 0.0425(7) Uani 1 1 d . . . C11 C 0.5969(4) -0.1968(4) 0.8771(3) 0.0445(7) Uani 1 1 d . . . C12 C 0.5768(4) -0.0731(3) 0.8668(3) 0.0443(7) Uani 1 1 d . . . C13 C 0.5224(4) -0.0667(3) 0.7708(2) 0.0399(7) Uani 1 1 d . . . C14 C 0.6513(8) -0.2055(7) 0.9824(4) 0.0681(12) Uani 1 1 d . . . C15 C 0.3616(4) -0.2698(3) 0.4993(2) 0.0336(6) Uani 1 1 d . . . C16 C 0.0235(5) 0.0982(4) 0.7479(3) 0.0488(8) Uani 1 1 d . . . C17 C -0.0145(5) -0.0587(3) 0.6993(3) 0.0436(7) Uani 1 1 d . . . C18 C 0.2416(6) 0.3212(4) 0.7649(4) 0.0616(10) Uani 1 1 d . . . C19 C -0.0923(6) -0.2447(4) 0.5359(3) 0.0525(9) Uani 1 1 d . . . H19B H -0.099(6) -0.269(4) 0.454(4) 0.087(14) Uiso 1 1 d . . . H19C H -0.211(5) -0.299(4) 0.553(3) 0.071(12) Uiso 1 1 d . . . H19A H 0.004(6) -0.278(4) 0.551(3) 0.077(13) Uiso 1 1 d . . . H12 H 0.601(4) 0.012(3) 0.930(3) 0.042(8) Uiso 1 1 d . . . H5 H 0.169(4) -0.485(3) 0.063(2) 0.032(7) Uiso 1 1 d . . . H6 H 0.342(4) -0.298(3) 0.208(2) 0.029(7) Uiso 1 1 d . . . H15 H 0.324(4) -0.364(3) 0.500(2) 0.032(7) Uiso 1 1 d . . . H18B H 0.291(5) 0.344(4) 0.837(4) 0.078(13) Uiso 1 1 d . . . H17A H -0.122(5) -0.110(3) 0.730(3) 0.053(9) Uiso 1 1 d . . . H7A H -0.239(7) -0.732(5) 0.054(4) 0.104(16) Uiso 1 1 d . . . H7B H -0.112(8) -0.821(7) 0.050(5) 0.15(2) Uiso 1 1 d . . . H16B H -0.075(4) 0.121(3) 0.727(2) 0.041(9) Uiso 1 1 d . . . H9 H 0.484(4) -0.394(3) 0.621(3) 0.043(8) Uiso 1 1 d . . . H7C H -0.069(7) -0.710(5) -0.008(4) 0.105(19) Uiso 1 1 d . . . H10 H 0.580(5) -0.388(4) 0.788(3) 0.066(11) Uiso 1 1 d . . . H16A H 0.038(5) 0.132(4) 0.830(3) 0.065(11) Uiso 1 1 d . . . H13 H 0.511(4) 0.016(4) 0.767(3) 0.050(9) Uiso 1 1 d . . . H17B H 0.101(4) -0.082(3) 0.709(2) 0.036(8) Uiso 1 1 d . . . H2 H 0.048(4) -0.488(3) 0.404(3) 0.039(8) Uiso 1 1 d . . . H14B H 0.742(11) -0.134(8) 1.023(6) 0.18(3) Uiso 1 1 d . . . H14C H 0.725(8) -0.257(6) 0.978(4) 0.12(2) Uiso 1 1 d . . . H14A H 0.567(7) -0.220(5) 1.025(4) 0.094(17) Uiso 1 1 d . . . H3 H -0.127(5) -0.674(4) 0.261(3) 0.058(10) Uiso 1 1 d . . . H18A H 0.147(6) 0.358(5) 0.753(3) 0.088(14) Uiso 1 1 d . . . H18C H 0.356(5) 0.357(4) 0.735(3) 0.056(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0354(4) 0.0358(3) 0.0499(4) 0.0188(3) 0.0089(3) 0.0163(3) O1 0.0453(12) 0.0362(11) 0.0649(16) 0.0075(11) 0.0088(11) 0.0137(10) N1 0.0410(13) 0.0270(11) 0.0389(15) 0.0115(10) 0.0031(11) 0.0111(10) C1 0.0360(15) 0.0284(13) 0.0408(17) 0.0102(12) 0.0009(12) 0.0137(11) O2 0.0412(11) 0.0361(11) 0.0451(13) 0.0145(9) 0.0025(9) 0.0141(9) N2 0.0409(13) 0.0286(12) 0.0356(14) 0.0128(11) 0.0045(10) 0.0126(10) C2 0.0396(16) 0.0339(15) 0.0410(18) 0.0134(13) 0.0055(13) 0.0142(12) C3 0.0362(16) 0.0296(14) 0.058(2) 0.0102(14) 0.0024(14) 0.0103(12) C4 0.0408(17) 0.0384(16) 0.047(2) 0.0039(14) -0.0031(14) 0.0182(13) C5 0.0497(19) 0.0453(17) 0.0376(19) 0.0120(15) 0.0030(14) 0.0206(15) C6 0.0418(17) 0.0338(15) 0.0457(19) 0.0157(14) 0.0033(14) 0.0129(13) C7 0.056(2) 0.055(2) 0.058(3) -0.003(2) -0.009(2) 0.0114(19) C8 0.0267(13) 0.0295(13) 0.0420(17) 0.0124(12) 0.0041(11) 0.0074(11) C9 0.0371(15) 0.0292(14) 0.0434(18) 0.0109(13) 0.0015(13) 0.0126(12) C10 0.0405(17) 0.0392(17) 0.054(2) 0.0198(16) 0.0038(14) 0.0166(14) C11 0.0398(16) 0.0552(19) 0.0446(19) 0.0190(16) 0.0035(14) 0.0212(14) C12 0.0460(18) 0.0432(17) 0.0427(19) 0.0070(15) 0.0016(14) 0.0201(14) C13 0.0457(17) 0.0315(15) 0.0430(19) 0.0096(13) 0.0060(14) 0.0157(13) C14 0.079(3) 0.097(4) 0.045(2) 0.026(2) 0.003(2) 0.051(3) C15 0.0314(14) 0.0247(13) 0.0467(18) 0.0121(13) 0.0032(12) 0.0116(11) C16 0.0427(19) 0.057(2) 0.043(2) 0.0099(16) 0.0049(15) 0.0183(16) C17 0.0415(17) 0.0491(18) 0.046(2) 0.0227(16) 0.0070(14) 0.0155(15) C18 0.064(3) 0.043(2) 0.067(3) 0.0058(19) -0.010(2) 0.0167(18) C19 0.053(2) 0.0384(17) 0.065(3) 0.0113(17) 0.0115(18) 0.0183(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.764(2) . ? K1 N2 2.818(2) 2_656 ? K1 N2 2.819(2) . ? K1 O2 2.824(2) 2_556 ? K1 O2 2.843(2) . ? K1 N1 2.987(2) 2_656 ? K1 N1 3.000(2) . ? K1 C15 3.153(3) 2_656 ? K1 C15 3.223(3) . ? K1 K1 3.4299(13) 2_656 ? K1 C19 3.433(4) 2_556 ? K1 C17 3.435(3) . ? O1 C16 1.415(4) . ? O1 C18 1.426(4) . ? N1 C15 1.314(4) . ? N1 C1 1.397(4) . ? N1 K1 2.987(2) 2_656 ? C1 C6 1.399(4) . ? C1 C2 1.407(4) . ? O2 C19 1.425(4) . ? O2 C17 1.427(4) . ? O2 K1 2.824(2) 2_556 ? N2 C15 1.309(4) . ? N2 C8 1.396(4) . ? N2 K1 2.818(2) 2_656 ? C2 C3 1.385(4) . ? C3 C4 1.385(5) . ? C4 C5 1.385(4) . ? C4 C7 1.506(5) . ? C5 C6 1.382(4) . ? C8 C13 1.399(4) . ? C8 C9 1.409(4) . ? C9 C10 1.379(4) . ? C10 C11 1.390(5) . ? C11 C12 1.397(4) . ? C11 C14 1.503(5) . ? C12 C13 1.374(4) . ? C15 K1 3.153(3) 2_656 ? C16 C17 1.500(5) . ? C19 K1 3.433(4) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K1 N2 124.48(7) . 2_656 ? O1 K1 N2 104.80(7) . . ? N2 K1 N2 105.05(6) 2_656 . ? O1 K1 O2 89.58(7) . 2_556 ? N2 K1 O2 83.76(7) 2_656 2_556 ? N2 K1 O2 153.42(7) . 2_556 ? O1 K1 O2 60.46(6) . . ? N2 K1 O2 158.99(7) 2_656 . ? N2 K1 O2 91.90(6) . . ? O2 K1 O2 75.67(6) 2_556 . ? O1 K1 N1 88.50(7) . 2_656 ? N2 K1 N1 46.28(7) 2_656 2_656 ? N2 K1 N1 89.83(7) . 2_656 ? O2 K1 N1 113.16(6) 2_556 2_656 ? O2 K1 N1 148.27(7) . 2_656 ? O1 K1 N1 142.94(7) . . ? N2 K1 N1 89.57(7) 2_656 . ? N2 K1 N1 46.15(7) . . ? O2 K1 N1 110.27(7) 2_556 . ? O2 K1 N1 93.52(6) . . ? N1 K1 N1 110.10(5) 2_656 . ? O1 K1 C15 101.86(7) . 2_656 ? N2 K1 C15 24.51(7) 2_656 2_656 ? N2 K1 C15 105.85(7) . 2_656 ? O2 K1 C15 92.52(7) 2_556 2_656 ? O2 K1 C15 158.15(7) . 2_656 ? N1 K1 C15 24.52(7) 2_656 2_656 ? N1 K1 C15 107.92(7) . 2_656 ? O1 K1 C15 121.16(7) . . ? N2 K1 C15 104.05(7) 2_656 . ? N2 K1 C15 23.84(7) . . ? O2 K1 C15 130.10(7) 2_556 . ? O2 K1 C15 86.40(6) . . ? N1 K1 C15 106.45(7) 2_656 . ? N1 K1 C15 24.04(7) . . ? C15 K1 C15 114.93(6) 2_656 . ? O1 K1 K1 132.47(6) . 2_656 ? N2 K1 K1 52.53(5) 2_656 2_656 ? N2 K1 K1 52.52(5) . 2_656 ? O2 K1 K1 130.21(5) 2_556 2_656 ? O2 K1 K1 142.59(5) . 2_656 ? N1 K1 K1 55.23(5) 2_656 2_656 ? N1 K1 K1 54.87(5) . 2_656 ? C15 K1 K1 58.45(5) 2_656 2_656 ? C15 K1 K1 56.48(5) . 2_656 ? O1 K1 C19 74.11(9) . 2_556 ? N2 K1 C19 78.67(8) 2_656 2_556 ? N2 K1 C19 175.84(8) . 2_556 ? O2 K1 C19 23.89(8) 2_556 2_556 ? O2 K1 C19 84.07(8) . 2_556 ? N1 K1 C19 94.14(8) 2_656 2_556 ? N1 K1 C19 132.89(8) . 2_556 ? C15 K1 C19 78.31(8) 2_656 2_556 ? C15 K1 C19 153.98(9) . 2_556 ? K1 K1 C19 131.16(7) 2_656 2_556 ? O1 K1 C17 43.35(7) . . ? N2 K1 C17 167.68(7) 2_656 . ? N2 K1 C17 82.80(7) . . ? O2 K1 C17 93.36(7) 2_556 . ? O2 K1 C17 23.98(7) . . ? N1 K1 C17 125.72(7) 2_656 . ? N1 K1 C17 102.64(7) . . ? C15 K1 C17 144.58(8) 2_656 . ? C15 K1 C17 86.99(8) . . ? K1 K1 C17 134.41(6) 2_656 . ? C19 K1 C17 93.86(9) 2_556 . ? C16 O1 C18 112.3(3) . . ? C16 O1 K1 117.88(18) . . ? C18 O1 K1 126.9(2) . . ? C15 N1 C1 118.5(2) . . ? C15 N1 K1 84.84(16) . 2_656 ? C1 N1 K1 142.74(18) . 2_656 ? C15 N1 K1 87.54(16) . . ? C1 N1 K1 134.40(17) . . ? K1 N1 K1 69.90(5) 2_656 . ? N1 C1 C6 119.2(2) . . ? N1 C1 C2 124.6(3) . . ? C6 C1 C2 116.1(3) . . ? C19 O2 C17 111.8(3) . . ? C19 O2 K1 102.8(2) . 2_556 ? C17 O2 K1 129.38(18) . 2_556 ? C19 O2 K1 103.98(19) . . ? C17 O2 K1 101.93(17) . . ? K1 O2 K1 104.33(6) 2_556 . ? C15 N2 C8 120.6(2) . . ? C15 N2 K1 92.21(17) . 2_656 ? C8 N2 K1 122.96(16) . 2_656 ? C15 N2 K1 95.68(17) . . ? C8 N2 K1 135.95(17) . . ? K1 N2 K1 74.95(6) 2_656 . ? C3 C2 C1 121.6(3) . . ? C4 C3 C2 121.5(3) . . ? C5 C4 C3 117.2(3) . . ? C5 C4 C7 122.6(3) . . ? C3 C4 C7 120.1(3) . . ? C6 C5 C4 121.9(3) . . ? C5 C6 C1 121.6(3) . . ? N2 C8 C13 117.3(3) . . ? N2 C8 C9 126.6(3) . . ? C13 C8 C9 116.0(3) . . ? C10 C9 C8 121.0(3) . . ? C9 C10 C11 122.7(3) . . ? C10 C11 C12 116.2(3) . . ? C10 C11 C14 121.9(3) . . ? C12 C11 C14 121.9(3) . . ? C13 C12 C11 121.6(3) . . ? C12 C13 C8 122.4(3) . . ? N2 C15 N1 121.3(2) . . ? N2 C15 K1 63.28(14) . 2_656 ? N1 C15 K1 70.64(15) . 2_656 ? N2 C15 K1 60.49(14) . . ? N1 C15 K1 68.42(15) . . ? K1 C15 K1 65.07(6) 2_656 . ? O1 C16 C17 108.9(3) . . ? O2 C17 C16 108.6(3) . . ? O2 C17 K1 54.09(14) . . ? C16 C17 K1 85.83(18) . . ? O2 C19 K1 53.35(16) . 2_556 ? O2 C19 K1 52.56(15) . . ? K1 C19 K1 80.77(8) 2_556 . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.420 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.072 #===END data_Compound_4 _database_code_CSD 188558 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[K(FTolP)(18-crown-6)]' _chemical_melting_point ? _chemical_formula_moiety 'C27 H39 K N2 O6' _chemical_formula_sum 'C27 H39 K N2 O6' _chemical_formula_weight 526.70 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3213(19) _cell_length_b 23.917(5) _cell_length_c 13.559(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.56(3) _cell_angle_gamma 90.00 _cell_volume 2848.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.227 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8756 _exptl_absorpt_correction_T_max 0.9349 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14959 _diffrn_reflns_av_R_equivalents 0.0952 _diffrn_reflns_av_sigmaI/netI 0.2991 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6990 _reflns_number_gt 2383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6990 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2265 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.26347(7) 0.17398(2) 0.99126(5) 0.02825(19) Uani 1 1 d . . . O1A O -0.0723(2) 0.16448(7) 0.92779(13) 0.0302(5) Uani 1 1 d . . . O2A O 0.1115(2) 0.06517(7) 0.98342(14) 0.0317(5) Uani 1 1 d . . . O3A O 0.4339(2) 0.07087(7) 1.06948(15) 0.0360(5) Uani 1 1 d . . . O4A O 0.5376(2) 0.17175(8) 1.17178(14) 0.0374(5) Uani 1 1 d . . . O5A O 0.3640(2) 0.27058(7) 1.11274(15) 0.0330(5) Uani 1 1 d . . . O6A O 0.0540(2) 0.26197(7) 1.03154(15) 0.0323(5) Uani 1 1 d . . . N1 N 0.4109(2) 0.22451(8) 0.86252(16) 0.0242(6) Uani 1 1 d . . . N2 N 0.3086(2) 0.13809(8) 0.79764(16) 0.0246(6) Uani 1 1 d . . . C1 C 0.4843(3) 0.27319(11) 0.8461(2) 0.0230(7) Uani 1 1 d . . . C1A C -0.1291(3) 0.10968(11) 0.9304(2) 0.0392(8) Uani 1 1 d . . . H1A1 H -0.2345 0.1068 0.8807 0.047 Uiso 1 1 calc R . . H1A2 H -0.1306 0.1012 1.0015 0.047 Uiso 1 1 calc R . . C2 C 0.5066(3) 0.31613(10) 0.9204(2) 0.0286(8) Uani 1 1 d . . . H2 H 0.4733 0.3106 0.9786 0.034 Uiso 1 1 calc R . . C2A C -0.0291(3) 0.06886(11) 0.9011(2) 0.0361(8) Uani 1 1 d . . . H2A1 H -0.0787 0.0317 0.8880 0.043 Uiso 1 1 calc R . . H2A2 H -0.0122 0.0813 0.8362 0.043 Uiso 1 1 calc R . . C3 C 0.5755(3) 0.36607(11) 0.9114(2) 0.0327(8) Uani 1 1 d . . . H3 H 0.5899 0.3937 0.9641 0.039 Uiso 1 1 calc R . . C3A C 0.2115(3) 0.02568(11) 0.9618(2) 0.0346(8) Uani 1 1 d . . . H3A1 H 0.2408 0.0385 0.9018 0.042 Uiso 1 1 calc R . . H3A2 H 0.1602 -0.0110 0.9438 0.042 Uiso 1 1 calc R . . C4 C 0.6244(3) 0.37694(11) 0.8272(2) 0.0308(8) Uani 1 1 d . . . C4A C 0.3500(3) 0.02032(11) 1.0574(2) 0.0377(9) Uani 1 1 d . . . H4A1 H 0.3198 0.0136 1.1198 0.045 Uiso 1 1 calc R . . H4A2 H 0.4131 -0.0115 1.0495 0.045 Uiso 1 1 calc R . . C5 C 0.6001(3) 0.33489(11) 0.7526(2) 0.0336(8) Uani 1 1 d . . . H5 H 0.6320 0.3408 0.6938 0.040 Uiso 1 1 calc R . . C5A C 0.5571(3) 0.07361(12) 1.1658(2) 0.0431(9) Uani 1 1 d . . . H5A1 H 0.6274 0.0418 1.1714 0.052 Uiso 1 1 calc R . . H5A2 H 0.5183 0.0717 1.2254 0.052 Uiso 1 1 calc R . . C6 C 0.5313(3) 0.28492(11) 0.7607(2) 0.0288(8) Uani 1 1 d . . . H6 H 0.5156 0.2578 0.7069 0.035 Uiso 1 1 calc R . . C6A C 0.6381(3) 0.12747(12) 1.1680(2) 0.0452(9) Uani 1 1 d . . . H6A1 H 0.7316 0.1290 1.2302 0.054 Uiso 1 1 calc R . . H6A2 H 0.6675 0.1310 1.1046 0.054 Uiso 1 1 calc R . . C7 C 0.7011(3) 0.43153(11) 0.8172(2) 0.0517(10) Uani 1 1 d . . . H7A H 0.7356 0.4297 0.7565 0.078 Uiso 1 1 calc R . . H7B H 0.7888 0.4378 0.8807 0.078 Uiso 1 1 calc R . . H7C H 0.6286 0.4624 0.8080 0.078 Uiso 1 1 calc R . . C7A C 0.6044(3) 0.22493(12) 1.1652(3) 0.0518(10) Uani 1 1 d . . . H7A1 H 0.6084 0.2305 1.0938 0.062 Uiso 1 1 calc R . . H7A2 H 0.7096 0.2264 1.2154 0.062 Uiso 1 1 calc R . . C8 C 0.3084(3) 0.09377(10) 0.7294(2) 0.0253(7) Uani 1 1 d . . . C8A C 0.5105(4) 0.26983(12) 1.1900(2) 0.0498(9) Uani 1 1 d . . . H8A1 H 0.5014 0.2629 1.2596 0.060 Uiso 1 1 calc R . . H8A2 H 0.5605 0.3065 1.1920 0.060 Uiso 1 1 calc R . . C9 C 0.1748(3) 0.06220(11) 0.6891(2) 0.0289(8) Uani 1 1 d . . . H9 H 0.0873 0.0729 0.7055 0.035 Uiso 1 1 calc R . . C9A C 0.2702(4) 0.31396(11) 1.1277(2) 0.0393(9) Uani 1 1 d . . . H9A1 H 0.3228 0.3504 1.1331 0.047 Uiso 1 1 calc R . . H9A2 H 0.2481 0.3076 1.1933 0.047 Uiso 1 1 calc R . . C10 C 0.1664(3) 0.01605(10) 0.6262(2) 0.0301(8) Uani 1 1 d . . . H10 H 0.0744 -0.0048 0.6023 0.036 Uiso 1 1 calc R . . C10A C 0.1257(4) 0.31459(10) 1.0370(2) 0.0378(8) Uani 1 1 d . . . H10A H 0.0580 0.3446 1.0461 0.045 Uiso 1 1 calc R . . H10B H 0.1474 0.3218 0.9715 0.045 Uiso 1 1 calc R . . C11 C 0.2892(4) -0.00043(10) 0.5975(2) 0.0271(7) Uani 1 1 d . . . C11A C -0.0973(3) 0.26133(11) 0.9582(2) 0.0378(8) Uani 1 1 d . . . H11A H -0.0960 0.2700 0.8871 0.045 Uiso 1 1 calc R . . H11B H -0.1605 0.2897 0.9775 0.045 Uiso 1 1 calc R . . C12 C 0.4207(3) 0.03103(11) 0.6352(2) 0.0329(8) Uani 1 1 d . . . H12 H 0.5062 0.0210 0.6158 0.039 Uiso 1 1 calc R . . C12A C -0.1610(3) 0.20450(11) 0.9603(2) 0.0376(8) Uani 1 1 d . . . H12A H -0.1592 0.1956 1.0321 0.045 Uiso 1 1 calc R . . H12B H -0.2680 0.2032 0.9129 0.045 Uiso 1 1 calc R . . C13 C 0.4321(3) 0.07690(10) 0.7005(2) 0.0303(8) Uani 1 1 d . . . H13 H 0.5252 0.0970 0.7257 0.036 Uiso 1 1 calc R . . C14 C 0.2796(3) -0.05197(10) 0.5298(2) 0.0437(9) Uani 1 1 d . . . H14A H 0.3824 -0.0636 0.5343 0.066 Uiso 1 1 calc R . . H14B H 0.2202 -0.0432 0.4570 0.066 Uiso 1 1 calc R . . H14C H 0.2300 -0.0824 0.5547 0.066 Uiso 1 1 calc R . . C15 C 0.3950(3) 0.18194(10) 0.7974(2) 0.0253(7) Uani 1 1 d . . . H15 H 0.4478 0.1829 0.7484 0.030 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 K1 0.0259(4) 0.0279(3) 0.0293(4) 0.0001(3) 0.0071(3) -0.0014(3) O1A 0.0232(13) 0.0302(12) 0.0371(13) 0.0040(9) 0.0099(11) 0.0021(10) O2A 0.0284(14) 0.0261(11) 0.0395(15) -0.0032(9) 0.0098(12) 0.0020(10) O3A 0.0308(15) 0.0348(12) 0.0383(15) 0.0100(10) 0.0062(12) -0.0012(11) O4A 0.0258(13) 0.0405(13) 0.0432(14) 0.0041(10) 0.0078(11) -0.0006(11) O5A 0.0261(14) 0.0348(12) 0.0360(14) -0.0107(10) 0.0077(12) -0.0057(11) O6A 0.0273(14) 0.0255(12) 0.0424(15) 0.0062(9) 0.0095(12) -0.0006(10) N1 0.0250(16) 0.0215(13) 0.0227(15) -0.0020(11) 0.0033(13) 0.0005(12) N2 0.0232(16) 0.0217(13) 0.0267(16) 0.0011(11) 0.0051(13) -0.0014(12) C1 0.0165(19) 0.0260(17) 0.0235(19) 0.0012(14) 0.0026(16) 0.0053(14) C1A 0.025(2) 0.042(2) 0.048(2) -0.0038(16) 0.0085(18) -0.0056(17) C2 0.028(2) 0.0341(18) 0.0253(19) 0.0006(15) 0.0114(16) 0.0028(15) C2A 0.028(2) 0.0404(19) 0.039(2) -0.0075(16) 0.0095(19) -0.0072(16) C3 0.038(2) 0.0261(17) 0.035(2) -0.0062(14) 0.0137(19) -0.0018(15) C3A 0.046(2) 0.0228(16) 0.038(2) 0.0057(14) 0.018(2) 0.0036(16) C4 0.027(2) 0.0284(18) 0.038(2) 0.0034(15) 0.0118(18) -0.0019(15) C4A 0.041(2) 0.0302(19) 0.047(2) 0.0059(16) 0.022(2) 0.0069(17) C5 0.039(2) 0.0373(19) 0.029(2) 0.0052(15) 0.0173(18) -0.0022(17) C5A 0.033(2) 0.047(2) 0.044(2) 0.0176(17) 0.006(2) 0.0101(18) C6 0.028(2) 0.0319(18) 0.029(2) -0.0076(14) 0.0121(17) -0.0018(15) C6A 0.024(2) 0.059(2) 0.046(2) 0.0089(18) 0.0030(19) 0.0069(19) C7 0.066(3) 0.044(2) 0.050(2) -0.0059(17) 0.026(2) -0.0129(19) C7A 0.030(2) 0.053(2) 0.063(3) -0.0056(19) 0.003(2) -0.0087(19) C8 0.029(2) 0.0244(17) 0.025(2) 0.0039(14) 0.0115(17) 0.0020(15) C8A 0.041(3) 0.052(2) 0.044(2) -0.0176(18) -0.001(2) -0.0115(19) C9 0.029(2) 0.0323(17) 0.025(2) 0.0064(14) 0.0082(17) 0.0016(15) C9A 0.044(2) 0.0301(19) 0.049(2) -0.0055(16) 0.023(2) -0.0059(17) C10 0.028(2) 0.0274(17) 0.029(2) 0.0016(14) 0.0027(17) -0.0047(15) C10A 0.038(2) 0.0266(18) 0.053(2) 0.0022(16) 0.021(2) 0.0004(16) C11 0.036(2) 0.0195(16) 0.0244(19) 0.0022(13) 0.0086(18) 0.0029(16) C11A 0.028(2) 0.036(2) 0.048(2) 0.0043(16) 0.0104(19) 0.0096(17) C12 0.033(2) 0.0275(18) 0.043(2) 0.0007(15) 0.0189(19) 0.0061(16) C12A 0.019(2) 0.042(2) 0.048(2) -0.0007(16) 0.0059(18) 0.0036(16) C13 0.029(2) 0.0235(17) 0.036(2) 0.0031(14) 0.0085(18) -0.0020(15) C14 0.054(3) 0.0275(17) 0.051(2) -0.0088(15) 0.019(2) 0.0012(16) C15 0.0194(19) 0.0316(17) 0.0223(18) 0.0088(14) 0.0036(15) 0.0084(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O5A 2.8100(19) . ? K1 N1 2.829(2) . ? K1 O4A 2.887(2) . ? K1 N2 2.923(2) . ? K1 O3A 2.9329(19) . ? K1 O2A 2.9477(18) . ? K1 O1A 2.964(2) . ? K1 O6A 3.0419(18) . ? O1A C1A 1.418(3) . ? O1A C12A 1.428(3) . ? O2A C2A 1.412(3) . ? O2A C3A 1.425(3) . ? O3A C4A 1.419(3) . ? O3A C5A 1.423(3) . ? O4A C6A 1.426(3) . ? O4A C7A 1.432(3) . ? O5A C9A 1.415(3) . ? O5A C8A 1.416(3) . ? O6A C10A 1.415(3) . ? O6A C11A 1.428(3) . ? N1 C15 1.323(3) . ? N1 C1 1.405(3) . ? N2 C15 1.323(3) . ? N2 C8 1.406(3) . ? C1 C6 1.396(3) . ? C1 C2 1.405(3) . ? C1A C2A 1.493(3) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C2 C3 1.381(3) . ? C2 H2 0.9500 . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C3A C4A 1.498(4) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4 C5 1.390(3) . ? C4 C7 1.516(3) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5 C6 1.378(3) . ? C5 H5 0.9500 . ? C5A C6A 1.489(3) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6 H6 0.9500 . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C7A C8A 1.493(3) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8 C13 1.396(3) . ? C8 C9 1.401(3) . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C9 C10 1.380(3) . ? C9 H9 0.9500 . ? C9A C10A 1.489(4) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10 C11 1.384(3) . ? C10 H10 0.9500 . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11 C12 1.382(3) . ? C11 C14 1.521(3) . ? C11A C12A 1.488(3) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15 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 O5A K1 N1 82.81(6) . . ? O5A K1 O4A 59.43(6) . . ? N1 K1 O4A 93.21(6) . . ? O5A K1 N2 130.38(6) . . ? N1 K1 N2 47.59(6) . . ? O4A K1 N2 113.78(6) . . ? O5A K1 O3A 116.45(7) . . ? N1 K1 O3A 105.43(6) . . ? O4A K1 O3A 57.27(6) . . ? N2 K1 O3A 81.63(6) . . ? O5A K1 O2A 144.00(5) . . ? N1 K1 O2A 132.98(6) . . ? O4A K1 O2A 107.01(6) . . ? N2 K1 O2A 85.42(6) . . ? O3A K1 O2A 57.74(6) . . ? O5A K1 O1A 110.23(6) . . ? N1 K1 O1A 122.52(6) . . ? O4A K1 O1A 142.52(5) . . ? N2 K1 O1A 99.92(6) . . ? O3A K1 O1A 115.60(5) . . ? O2A K1 O1A 58.26(5) . . ? O5A K1 O6A 55.53(6) . . ? N1 K1 O6A 106.79(6) . . ? O4A K1 O6A 107.44(6) . . ? N2 K1 O6A 131.18(6) . . ? O3A K1 O6A 145.01(5) . . ? O2A K1 O6A 106.72(5) . . ? O1A K1 O6A 54.99(5) . . ? C1A O1A C12A 110.6(2) . . ? C1A O1A K1 115.48(15) . . ? C12A O1A K1 121.56(15) . . ? C2A O2A C3A 112.1(2) . . ? C2A O2A K1 106.32(14) . . ? C3A O2A K1 104.67(14) . . ? C4A O3A C5A 112.9(2) . . ? C4A O3A K1 117.64(16) . . ? C5A O3A K1 117.78(15) . . ? C6A O4A C7A 110.7(2) . . ? C6A O4A K1 112.88(16) . . ? C7A O4A K1 102.16(16) . . ? C9A O5A C8A 113.1(2) . . ? C9A O5A K1 125.89(17) . . ? C8A O5A K1 118.23(16) . . ? C10A O6A C11A 112.6(2) . . ? C10A O6A K1 107.73(15) . . ? C11A O6A K1 114.28(15) . . ? C15 N1 C1 118.9(2) . . ? C15 N1 K1 96.55(16) . . ? C1 N1 K1 144.55(16) . . ? C15 N2 C8 117.6(2) . . ? C15 N2 K1 92.31(16) . . ? C8 N2 K1 147.46(16) . . ? C6 C1 C2 115.8(2) . . ? C6 C1 N1 127.0(2) . . ? C2 C1 N1 117.1(2) . . ? O1A C1A C2A 109.1(2) . . ? O1A C1A H1A1 109.9 . . ? C2A C1A H1A1 109.9 . . ? O1A C1A H1A2 109.9 . . ? C2A C1A H1A2 109.9 . . ? H1A1 C1A H1A2 108.3 . . ? C3 C2 C1 122.0(3) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? O2A C2A C1A 109.1(2) . . ? O2A C2A H2A1 109.9 . . ? C1A C2A H2A1 109.9 . . ? O2A C2A H2A2 109.9 . . ? C1A C2A H2A2 109.9 . . ? H2A1 C2A H2A2 108.3 . . ? C2 C3 C4 121.7(3) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? O2A C3A C4A 108.2(2) . . ? O2A C3A H3A1 110.1 . . ? C4A C3A H3A1 110.1 . . ? O2A C3A H3A2 110.1 . . ? C4A C3A H3A2 110.1 . . ? H3A1 C3A H3A2 108.4 . . ? C3 C4 C5 116.4(3) . . ? C3 C4 C7 122.0(3) . . ? C5 C4 C7 121.7(3) . . ? O3A C4A C3A 108.0(2) . . ? O3A C4A H4A1 110.1 . . ? C3A C4A H4A1 110.1 . . ? O3A C4A H4A2 110.1 . . ? C3A C4A H4A2 110.1 . . ? H4A1 C4A H4A2 108.4 . . ? C6 C5 C4 122.4(3) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? O3A C5A C6A 107.8(2) . . ? O3A C5A H5A1 110.1 . . ? C6A C5A H5A1 110.1 . . ? O3A C5A H5A2 110.1 . . ? C6A C5A H5A2 110.1 . . ? H5A1 C5A H5A2 108.5 . . ? C5 C6 C1 121.6(3) . . ? C5 C6 H6 119.2 . . ? C1 C6 H6 119.2 . . ? O4A C6A C5A 108.0(2) . . ? O4A C6A H6A1 110.1 . . ? C5A C6A H6A1 110.1 . . ? O4A C6A H6A2 110.1 . . ? C5A C6A H6A2 110.1 . . ? H6A1 C6A H6A2 108.4 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O4A C7A C8A 109.0(2) . . ? 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 . . ? C13 C8 C9 116.4(3) . . ? C13 C8 N2 125.7(3) . . ? C9 C8 N2 117.9(3) . . ? O5A C8A C7A 109.6(2) . . ? O5A C8A H8A1 109.7 . . ? C7A C8A H8A1 109.7 . . ? O5A C8A H8A2 109.7 . . ? C7A C8A H8A2 109.7 . . ? H8A1 C8A H8A2 108.2 . . ? C10 C9 C8 122.1(3) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? O5A C9A C10A 108.7(2) . . ? O5A C9A H9A1 109.9 . . ? C10A C9A H9A1 109.9 . . ? O5A C9A H9A2 109.9 . . ? C10A C9A H9A2 109.9 . . ? H9A1 C9A H9A2 108.3 . . ? C9 C10 C11 121.3(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? O6A C10A C9A 108.4(2) . . ? O6A C10A H10A 110.0 . . ? C9A C10A H10A 110.0 . . ? O6A C10A H10B 110.0 . . ? C9A C10A H10B 110.0 . . ? H10A C10A H10B 108.4 . . ? C12 C11 C10 117.1(3) . . ? C12 C11 C14 122.0(3) . . ? C10 C11 C14 120.9(3) . . ? O6A C11A C12A 107.7(2) . . ? O6A C11A H11A 110.2 . . ? C12A C11A H11A 110.2 . . ? O6A C11A H11B 110.2 . . ? C12A C11A H11B 110.2 . . ? H11A C11A H11B 108.5 . . ? C11 C12 C13 122.3(3) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? O1A C12A C11A 109.3(2) . . ? O1A C12A H12A 109.8 . . ? C11A C12A H12A 109.8 . . ? O1A C12A H12B 109.8 . . ? C11A C12A H12B 109.8 . . ? H12A C12A H12B 108.3 . . ? C12 C13 C8 120.8(3) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 N1 122.7(3) . . ? N2 C15 H15 118.6 . . ? N1 C15 H15 118.6 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.234 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.057 #===END data_d:\Compound2 _database_code_CSD 191452 _audit_creation_method 'SHELXL-97' _chemical_name_systematic ; ? ; _chemical_name_common '[{K2(FTolM)2(THF)3}n].nTHF' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H62 K2 N4 O4' _chemical_formula_weight 813.20 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.325(5) _cell_length_b 13.843(5) _cell_length_c 14.742(5) _cell_angle_alpha 66.345(5) _cell_angle_beta 73.400(5) _cell_angle_gamma 63.731(5) _cell_volume 2214.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless/yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.260 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.9499 _exptl_absorpt_correction_T_max 0.9499 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40214 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10799 _reflns_number_gt 7288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10799 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1516 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.47547(3) 0.00084(3) 0.12443(3) 0.02828(12) Uani 1 1 d . . . K2 K 0.48481(3) -0.00743(3) 0.39049(3) 0.02684(12) Uani 1 1 d . . . O1 O 0.33892(11) 0.14100(11) 0.23940(10) 0.0345(3) Uani 1 1 d . . . O2 O 0.62983(11) 0.00788(11) 0.21174(10) 0.0335(3) Uani 1 1 d . . . O3 O 0.45903(11) -0.16035(11) 0.32783(10) 0.0348(3) Uani 1 1 d . . . O4 O 1.02747(13) 0.44377(14) 0.40590(14) 0.0571(4) Uani 1 1 d . . . N1 N 0.38340(13) 0.17577(12) -0.04662(11) 0.0274(3) Uani 1 1 d . . . N2 N 0.56929(13) 0.15558(13) -0.07178(12) 0.0301(3) Uani 1 1 d . . . N3 N 0.39728(13) 0.18671(12) 0.45560(11) 0.0266(3) Uani 1 1 d . . . N4 N 0.29485(13) 0.07212(12) 0.52931(11) 0.0269(3) Uani 1 1 d . . . C1 C 0.26960(15) 0.24701(15) -0.04795(13) 0.0268(4) Uani 1 1 d . . . C2 C 0.19049(16) 0.19735(16) 0.01052(14) 0.0306(4) Uani 1 1 d . . . H2 H 0.2172 0.1183 0.0466 0.037 Uiso 1 1 calc R . . C3 C 0.07516(17) 0.25887(18) 0.01777(15) 0.0359(5) Uani 1 1 d . . . C4 C 0.03638(17) 0.37460(18) -0.03587(16) 0.0399(5) Uani 1 1 d . . . H4 H -0.0422 0.4190 -0.0312 0.048 Uiso 1 1 calc R . . C5 C 0.11219(18) 0.42436(17) -0.09561(16) 0.0385(5) Uani 1 1 d . . . H5 H 0.0848 0.5031 -0.1326 0.046 Uiso 1 1 calc R . . C6 C 0.22752(16) 0.36253(15) -0.10321(14) 0.0314(4) Uani 1 1 d . . . H6 H 0.2780 0.3986 -0.1460 0.038 Uiso 1 1 calc R . . C7 C -0.0054(2) 0.2006(2) 0.08402(18) 0.0543(6) Uani 1 1 d . . . H7A H -0.0183 0.1617 0.0482 0.081 Uiso 1 1 calc R . . H7B H -0.0773 0.2574 0.1018 0.081 Uiso 1 1 calc R . . H7C H 0.0273 0.1450 0.1449 0.081 Uiso 1 1 calc R . . C8 C 0.64538(16) 0.20469(16) -0.08081(14) 0.0315(4) Uani 1 1 d . . . C9 C 0.61953(17) 0.29445(16) -0.04586(14) 0.0336(4) Uani 1 1 d . . . H9 H 0.5455 0.3256 -0.0138 0.040 Uiso 1 1 calc R . . C10 C 0.69917(19) 0.33994(19) -0.05652(16) 0.0418(5) Uani 1 1 d . . . C11 C 0.8071(2) 0.2939(2) -0.10121(16) 0.0491(6) Uani 1 1 d . . . H11 H 0.8619 0.3242 -0.1094 0.059 Uiso 1 1 calc R . . C12 C 0.83570(19) 0.2027(2) -0.13433(17) 0.0502(6) Uani 1 1 d . . . H12 H 0.9106 0.1705 -0.1642 0.060 Uiso 1 1 calc R . . C13 C 0.75686(17) 0.1581(2) -0.12447(16) 0.0415(5) Uani 1 1 d . . . H13 H 0.7783 0.0957 -0.1474 0.050 Uiso 1 1 calc R . . C14 C 0.6642(2) 0.4389(2) -0.0198(2) 0.0598(7) Uani 1 1 d . . . H14A H 0.7311 0.4420 -0.0078 0.090 Uiso 1 1 calc R . . H14B H 0.6123 0.4293 0.0425 0.090 Uiso 1 1 calc R . . H14C H 0.6263 0.5097 -0.0703 0.090 Uiso 1 1 calc R . . C15 C 0.46026(15) 0.22041(15) -0.06812(13) 0.0263(4) Uani 1 1 d . . . H15 H 0.4371 0.2997 -0.0811 0.032 Uiso 1 1 calc R . . C16 C 0.40392(16) 0.29354(15) 0.40106(13) 0.0276(4) Uani 1 1 d . . . C17 C 0.51268(17) 0.29390(16) 0.36149(14) 0.0321(4) Uani 1 1 d . . . H17 H 0.5751 0.2235 0.3748 0.039 Uiso 1 1 calc R . . C18 C 0.53375(19) 0.39226(18) 0.30377(15) 0.0397(5) Uani 1 1 d . . . C19 C 0.4416(2) 0.49568(19) 0.28546(17) 0.0487(6) Uani 1 1 d . . . H19 H 0.4533 0.5644 0.2463 0.058 Uiso 1 1 calc R . . C20 C 0.3343(2) 0.49780(17) 0.32405(18) 0.0479(6) Uani 1 1 d . . . H20 H 0.2725 0.5688 0.3110 0.058 Uiso 1 1 calc R . . C21 C 0.31311(19) 0.39961(16) 0.38150(16) 0.0374(5) Uani 1 1 d . . . H21 H 0.2379 0.4038 0.4075 0.045 Uiso 1 1 calc R . . C22 C 0.6534(2) 0.3863(2) 0.26453(19) 0.0604(7) Uani 1 1 d . . . H22A H 0.6807 0.4030 0.3095 0.091 Uiso 1 1 calc R . . H22B H 0.6554 0.4421 0.1977 0.091 Uiso 1 1 calc R . . H22C H 0.7018 0.3098 0.2609 0.091 Uiso 1 1 calc R . . C23 C 0.18974(15) 0.06172(15) 0.56417(13) 0.0278(4) Uani 1 1 d . . . C24 C 0.18141(16) -0.03770(16) 0.56958(14) 0.0304(4) Uani 1 1 d . . . H24 H 0.2466 -0.0932 0.5471 0.036 Uiso 1 1 calc R . . C25 C 0.08276(17) -0.05934(17) 0.60611(15) 0.0348(4) Uani 1 1 d . . . C26 C -0.01279(18) 0.02200(18) 0.63907(16) 0.0408(5) Uani 1 1 d . . . H26 H -0.0813 0.0090 0.6646 0.049 Uiso 1 1 calc R . . C27 C -0.00802(17) 0.12180(18) 0.63461(16) 0.0399(5) Uani 1 1 d . . . H27 H -0.0738 0.1772 0.6565 0.048 Uiso 1 1 calc R . . C28 C 0.09184(16) 0.14195(16) 0.59856(14) 0.0318(4) Uani 1 1 d . . . H28 H 0.0940 0.2102 0.5971 0.038 Uiso 1 1 calc R . . C29 C 0.0773(2) -0.16710(19) 0.61044(18) 0.0474(6) Uani 1 1 d . . . H29A H 0.1427 -0.2041 0.5682 0.071 Uiso 1 1 calc R . . H29B H 0.0078 -0.1493 0.5864 0.071 Uiso 1 1 calc R . . H29C H 0.0778 -0.2183 0.6796 0.071 Uiso 1 1 calc R . . C30 C 0.29875(16) 0.17473(15) 0.48463(13) 0.0267(4) Uani 1 1 d . . . H30 H 0.2308 0.2398 0.4734 0.032 Uiso 1 1 calc R . . C31 C 0.22354(17) 0.14965(17) 0.27110(15) 0.0363(5) Uani 1 1 d . . . H31A H 0.2134 0.1043 0.3423 0.044 Uiso 1 1 calc R . . H31B H 0.2016 0.1212 0.2309 0.044 Uiso 1 1 calc R . . C32 C 0.15257(19) 0.27381(18) 0.25598(19) 0.0493(6) Uani 1 1 d . . . H32A H 0.0800 0.2952 0.2337 0.059 Uiso 1 1 calc R . . H32B H 0.1368 0.2918 0.3184 0.059 Uiso 1 1 calc R . . C33 C 0.2231(2) 0.33374(18) 0.17714(19) 0.0491(6) Uani 1 1 d . . . H33A H 0.2079 0.4068 0.1852 0.059 Uiso 1 1 calc R . . H33B H 0.2082 0.3487 0.1098 0.059 Uiso 1 1 calc R . . C34 C 0.34242(17) 0.25340(16) 0.19245(15) 0.0357(5) Uani 1 1 d . . . H34A H 0.3919 0.2586 0.1276 0.043 Uiso 1 1 calc R . . H34B H 0.3716 0.2716 0.2358 0.043 Uiso 1 1 calc R . . C35 C 0.7300(2) -0.0895(2) 0.2077(2) 0.0533(6) Uani 1 1 d . . . H35A H 0.7180 -0.1373 0.1798 0.064 Uiso 1 1 calc R . . H35B H 0.7518 -0.1358 0.2755 0.064 Uiso 1 1 calc R . . C36 C 0.8177(2) -0.0476(2) 0.1435(2) 0.0574(7) Uani 1 1 d . . . H36A H 0.8170 -0.0348 0.0726 0.069 Uiso 1 1 calc R . . H36B H 0.8932 -0.1022 0.1625 0.069 Uiso 1 1 calc R . . C37 C 0.78836(19) 0.0627(2) 0.16050(16) 0.0464(6) Uani 1 1 d . . . H37A H 0.7987 0.1218 0.0967 0.056 Uiso 1 1 calc R . . H37B H 0.8359 0.0524 0.2070 0.056 Uiso 1 1 calc R . . C38 C 0.66598(19) 0.09464(18) 0.20527(17) 0.0442(5) Uani 1 1 d . . . H38A H 0.6571 0.0994 0.2726 0.053 Uiso 1 1 calc R . . H38B H 0.6200 0.1695 0.1627 0.053 Uiso 1 1 calc R . . C39 C 0.36356(18) -0.19017(19) 0.34426(17) 0.0427(5) Uani 1 1 d . . . H39A H 0.3577 -0.2016 0.2841 0.051 Uiso 1 1 calc R . . H39B H 0.2928 -0.1298 0.3607 0.051 Uiso 1 1 calc R . . C40 C 0.38499(18) -0.29974(17) 0.43126(17) 0.0425(5) Uani 1 1 d . . . H40A H 0.3454 -0.3449 0.4297 0.051 Uiso 1 1 calc R . . H40B H 0.3604 -0.2845 0.4958 0.051 Uiso 1 1 calc R . . C41 C 0.51210(18) -0.36030(17) 0.41473(16) 0.0392(5) Uani 1 1 d . . . H41A H 0.5325 -0.4180 0.3823 0.047 Uiso 1 1 calc R . . H41B H 0.5437 -0.3981 0.4788 0.047 Uiso 1 1 calc R . . C42 C 0.55546(17) -0.26584(16) 0.34655(16) 0.0366(5) Uani 1 1 d . . . H42A H 0.6084 -0.2620 0.3792 0.044 Uiso 1 1 calc R . . H42B H 0.5957 -0.2808 0.2829 0.044 Uiso 1 1 calc R . . C43 C 0.9983(2) 0.5501(2) 0.3275(2) 0.0562(6) Uani 1 1 d . . . H43A H 1.0289 0.5383 0.2615 0.067 Uiso 1 1 calc R . . H43B H 1.0295 0.6001 0.3333 0.067 Uiso 1 1 calc R . . C44 C 0.8706(2) 0.60300(19) 0.33864(19) 0.0513(6) Uani 1 1 d . . . H44A H 0.8403 0.6490 0.3842 0.062 Uiso 1 1 calc R . . H44B H 0.8429 0.6511 0.2732 0.062 Uiso 1 1 calc R . . C45 C 0.8399(2) 0.49958(19) 0.3827(2) 0.0522(6) Uani 1 1 d . . . H45A H 0.8430 0.4705 0.3302 0.063 Uiso 1 1 calc R . . H45B H 0.7636 0.5159 0.4216 0.063 Uiso 1 1 calc R . . C46 C 0.9299(2) 0.41712(19) 0.44924(19) 0.0516(6) Uani 1 1 d . . . H46A H 0.9045 0.4242 0.5171 0.062 Uiso 1 1 calc R . . H46B H 0.9461 0.3381 0.4545 0.062 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 K1 0.0308(2) 0.0281(2) 0.0251(2) -0.00976(16) -0.00673(16) -0.00734(17) K2 0.0295(2) 0.0275(2) 0.0235(2) -0.00839(16) -0.00428(16) -0.00989(16) O1 0.0300(7) 0.0338(7) 0.0348(8) -0.0113(6) -0.0031(6) -0.0081(6) O2 0.0288(7) 0.0424(8) 0.0351(8) -0.0172(6) -0.0010(6) -0.0160(6) O3 0.0380(8) 0.0287(7) 0.0379(8) -0.0062(6) -0.0105(6) -0.0133(6) O4 0.0388(10) 0.0555(10) 0.0726(12) -0.0264(9) -0.0206(9) -0.0005(8) N1 0.0290(8) 0.0269(8) 0.0274(8) -0.0085(6) -0.0056(6) -0.0103(6) N2 0.0289(9) 0.0321(8) 0.0298(9) -0.0095(7) -0.0067(7) -0.0105(7) N3 0.0288(9) 0.0250(8) 0.0275(8) -0.0064(6) -0.0060(6) -0.0117(6) N4 0.0255(8) 0.0283(8) 0.0270(8) -0.0088(6) -0.0020(6) -0.0110(6) C1 0.0298(10) 0.0291(9) 0.0244(9) -0.0109(7) -0.0056(8) -0.0102(8) C2 0.0316(11) 0.0351(10) 0.0269(10) -0.0065(8) -0.0075(8) -0.0147(8) C3 0.0342(11) 0.0500(12) 0.0285(11) -0.0147(9) -0.0028(9) -0.0189(9) C4 0.0294(11) 0.0480(12) 0.0428(13) -0.0215(10) -0.0069(9) -0.0074(9) C5 0.0400(12) 0.0287(10) 0.0430(12) -0.0101(9) -0.0130(10) -0.0061(9) C6 0.0336(11) 0.0289(9) 0.0316(10) -0.0084(8) -0.0053(8) -0.0121(8) C7 0.0380(13) 0.0774(17) 0.0475(14) -0.0114(12) -0.0041(11) -0.0300(12) C8 0.0319(11) 0.0378(10) 0.0233(10) -0.0032(8) -0.0087(8) -0.0146(8) C9 0.0359(11) 0.0376(10) 0.0287(10) -0.0041(8) -0.0085(8) -0.0181(9) C10 0.0485(14) 0.0493(12) 0.0336(12) 0.0004(9) -0.0141(10) -0.0303(11) C11 0.0471(14) 0.0756(16) 0.0320(12) -0.0026(11) -0.0086(10) -0.0401(13) C12 0.0301(12) 0.0834(17) 0.0352(13) -0.0146(12) -0.0031(9) -0.0242(12) C13 0.0307(11) 0.0575(13) 0.0354(12) -0.0155(10) -0.0074(9) -0.0135(10) C14 0.0655(17) 0.0625(16) 0.0729(18) -0.0196(14) -0.0158(14) -0.0401(14) C15 0.0303(10) 0.0273(9) 0.0212(9) -0.0068(7) -0.0053(7) -0.0104(8) C16 0.0384(11) 0.0260(9) 0.0233(9) -0.0068(7) -0.0108(8) -0.0131(8) C17 0.0415(12) 0.0336(10) 0.0283(10) -0.0099(8) -0.0064(8) -0.0188(9) C18 0.0571(14) 0.0464(12) 0.0289(11) -0.0075(9) -0.0082(10) -0.0332(11) C19 0.0794(18) 0.0404(12) 0.0353(12) 0.0059(9) -0.0230(12) -0.0367(12) C20 0.0629(16) 0.0278(10) 0.0525(14) 0.0006(10) -0.0311(12) -0.0141(10) C21 0.0417(12) 0.0298(10) 0.0414(12) -0.0066(9) -0.0167(9) -0.0114(9) C22 0.0754(19) 0.0735(17) 0.0479(15) -0.0114(13) 0.0026(13) -0.0547(16) C23 0.0290(10) 0.0346(10) 0.0207(9) -0.0060(7) -0.0065(7) -0.0131(8) C24 0.0307(10) 0.0329(10) 0.0287(10) -0.0096(8) -0.0031(8) -0.0136(8) C25 0.0355(11) 0.0413(11) 0.0291(10) -0.0051(8) -0.0059(9) -0.0201(9) C26 0.0320(12) 0.0524(13) 0.0366(12) -0.0084(10) -0.0032(9) -0.0207(10) C27 0.0288(11) 0.0479(12) 0.0365(12) -0.0127(10) -0.0029(9) -0.0103(9) C28 0.0307(11) 0.0355(10) 0.0287(10) -0.0106(8) -0.0042(8) -0.0115(8) C29 0.0479(14) 0.0507(13) 0.0500(14) -0.0126(11) -0.0024(11) -0.0294(11) C30 0.0301(10) 0.0278(9) 0.0226(9) -0.0095(7) -0.0083(8) -0.0070(8) C31 0.0359(11) 0.0429(11) 0.0322(11) -0.0111(9) -0.0031(9) -0.0180(9) C32 0.0342(12) 0.0447(12) 0.0623(16) -0.0198(11) -0.0045(11) -0.0079(10) C33 0.0484(14) 0.0336(11) 0.0545(15) -0.0086(10) -0.0076(11) -0.0104(10) C34 0.0410(12) 0.0390(11) 0.0325(11) -0.0139(9) -0.0008(9) -0.0196(9) C35 0.0449(14) 0.0469(13) 0.0722(18) -0.0257(13) -0.0062(12) -0.0157(11) C36 0.0338(13) 0.0774(18) 0.0679(18) -0.0385(15) 0.0078(12) -0.0220(12) C37 0.0511(14) 0.0610(14) 0.0340(12) -0.0011(10) -0.0104(10) -0.0364(12) C38 0.0557(15) 0.0402(11) 0.0394(12) -0.0124(10) 0.0032(10) -0.0262(11) C39 0.0382(12) 0.0514(13) 0.0419(13) -0.0115(10) -0.0111(10) -0.0191(10) C40 0.0443(13) 0.0423(12) 0.0438(13) -0.0119(10) -0.0045(10) -0.0211(10) C41 0.0461(13) 0.0320(10) 0.0413(12) -0.0115(9) -0.0078(10) -0.0151(9) C42 0.0365(12) 0.0331(10) 0.0373(11) -0.0111(9) -0.0049(9) -0.0107(9) C43 0.0518(15) 0.0595(15) 0.0663(18) -0.0274(14) -0.0110(13) -0.0202(12) C44 0.0563(15) 0.0384(12) 0.0570(15) -0.0194(11) -0.0208(12) -0.0040(11) C45 0.0428(14) 0.0504(13) 0.0621(16) -0.0162(12) -0.0181(12) -0.0113(11) C46 0.0497(15) 0.0445(13) 0.0538(15) -0.0181(11) -0.0171(12) -0.0034(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O2 2.7726(15) . ? K1 O1 2.7748(15) . ? K1 N1 2.7888(16) 2_655 ? K1 N1 2.8223(17) . ? K1 N2 2.8988(17) 2_655 ? K1 O3 2.9507(16) . ? K1 N2 3.1385(18) . ? K1 C15 3.180(2) 2_655 ? K1 C15 3.193(2) . ? K1 C35 3.459(3) . ? K1 K1 3.5457(14) 2_655 ? K1 K2 3.9139(14) . ? K2 O2 2.7799(15) . ? K2 N3 2.8005(16) 2_656 ? K2 O3 2.8012(15) . ? K2 N3 2.8566(17) . ? K2 N4 2.8617(17) . ? K2 O1 2.8684(16) . ? K2 N4 3.1027(19) 2_656 ? K2 C30 3.1209(19) . ? K2 C30 3.282(2) 2_656 ? K2 C38 3.382(2) . ? K2 K2 3.4619(13) 2_656 ? O1 C31 1.438(2) . ? O1 C34 1.444(2) . ? O2 C35 1.424(3) . ? O2 C38 1.441(2) . ? O3 C39 1.434(2) . ? O3 C42 1.442(2) . ? O4 C46 1.413(3) . ? O4 C43 1.428(3) . ? N1 C15 1.322(2) . ? N1 C1 1.396(2) . ? N1 K1 2.7888(16) 2_655 ? N2 C15 1.326(2) . ? N2 C8 1.403(2) . ? N2 K1 2.8988(17) 2_655 ? N3 C30 1.323(2) . ? N3 C16 1.401(2) . ? N3 K2 2.8005(16) 2_656 ? N4 C30 1.323(2) . ? N4 C23 1.398(2) . ? N4 K2 3.1027(19) 2_656 ? C1 C6 1.399(3) . ? C1 C2 1.405(3) . ? C2 C3 1.385(3) . ? C3 C4 1.394(3) . ? C3 C7 1.513(3) . ? C4 C5 1.375(3) . ? C5 C6 1.386(3) . ? C8 C9 1.401(3) . ? C8 C13 1.405(3) . ? C9 C10 1.402(3) . ? C10 C11 1.376(3) . ? C10 C14 1.507(3) . ? C11 C12 1.393(3) . ? C12 C13 1.386(3) . ? C15 K1 3.180(2) 2_655 ? C16 C17 1.401(3) . ? C16 C21 1.411(3) . ? C17 C18 1.389(3) . ? C18 C19 1.398(3) . ? C18 C22 1.509(3) . ? C19 C20 1.371(3) . ? C20 C21 1.387(3) . ? C23 C24 1.398(3) . ? C23 C28 1.408(3) . ? C24 C25 1.386(3) . ? C25 C26 1.393(3) . ? C25 C29 1.501(3) . ? C26 C27 1.385(3) . ? C27 C28 1.392(3) . ? C30 K2 3.282(2) 2_656 ? C31 C32 1.507(3) . ? C32 C33 1.488(3) . ? C33 C34 1.501(3) . ? C35 C36 1.458(3) . ? C36 C37 1.507(3) . ? C37 C38 1.507(3) . ? C39 C40 1.514(3) . ? C40 C41 1.517(3) . ? C41 C42 1.528(3) . ? C43 C44 1.514(3) . ? C44 C45 1.503(3) . ? C45 C46 1.505(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 O2 K1 O1 77.15(5) . . ? O2 K1 N1 99.54(5) . 2_655 ? O1 K1 N1 168.18(4) . 2_655 ? O2 K1 N1 122.14(5) . . ? O1 K1 N1 89.61(5) . . ? N1 K1 N1 101.62(5) 2_655 . ? O2 K1 N2 141.13(4) . 2_655 ? O1 K1 N2 129.92(5) . 2_655 ? N1 K1 N2 47.69(5) 2_655 2_655 ? N1 K1 N2 89.16(5) . 2_655 ? O2 K1 O3 77.31(4) . . ? O1 K1 O3 76.49(5) . . ? N1 K1 O3 91.73(5) 2_655 . ? N1 K1 O3 153.32(5) . . ? N2 K1 O3 82.87(5) 2_655 . ? O2 K1 N2 84.63(5) . . ? O1 K1 N2 105.71(5) . . ? N1 K1 N2 85.08(5) 2_655 . ? N1 K1 N2 45.04(5) . . ? N2 K1 N2 108.19(4) 2_655 . ? O3 K1 N2 160.89(4) . . ? O2 K1 C15 118.03(4) . 2_655 ? O1 K1 C15 149.30(5) . 2_655 ? N1 K1 C15 24.49(5) 2_655 2_655 ? N1 K1 C15 101.74(5) . 2_655 ? N2 K1 C15 24.65(5) 2_655 2_655 ? O3 K1 C15 81.10(5) . 2_655 ? N2 K1 C15 102.35(5) . 2_655 ? O2 K1 C15 98.44(5) . . ? O1 K1 C15 89.56(5) . . ? N1 K1 C15 102.19(5) 2_655 . ? N1 K1 C15 24.41(4) . . ? N2 K1 C15 107.72(5) 2_655 . ? O3 K1 C15 165.98(4) . . ? N2 K1 C15 24.16(4) . . ? C15 K1 C15 112.40(5) 2_655 . ? O2 K1 C35 23.25(5) . . ? O1 K1 C35 98.92(5) . . ? N1 K1 C35 76.60(5) 2_655 . ? N1 K1 C35 130.87(5) . . ? N2 K1 C35 118.76(5) 2_655 . ? O3 K1 C35 74.50(5) . . ? N2 K1 C35 86.44(6) . . ? C15 K1 C35 94.96(5) 2_655 . ? C15 K1 C35 106.84(6) . . ? O2 K1 K1 123.62(4) . 2_655 ? O1 K1 K1 139.85(3) . 2_655 ? N1 K1 K1 51.23(3) 2_655 2_655 ? N1 K1 K1 50.39(4) . 2_655 ? N2 K1 K1 57.24(3) 2_655 2_655 ? O3 K1 K1 137.30(4) . 2_655 ? N2 K1 K1 50.96(3) . 2_655 ? C15 K1 K1 56.37(3) 2_655 2_655 ? C15 K1 K1 56.03(4) . 2_655 ? C35 K1 K1 109.78(5) . 2_655 ? O2 K1 K2 45.26(3) . . ? O1 K1 K2 47.08(3) . . ? N1 K1 K2 122.99(3) 2_655 . ? N1 K1 K2 133.92(4) . . ? N2 K1 K2 128.27(3) 2_655 . ? O3 K1 K2 45.54(3) . . ? N2 K1 K2 122.38(4) . . ? C15 K1 K2 123.46(3) 2_655 . ? C15 K1 K2 122.65(4) . . ? C35 K1 K2 59.06(4) . . ? K1 K1 K2 168.65(2) 2_655 . ? O2 K2 N3 109.18(5) . 2_656 ? O2 K2 O3 79.74(4) . . ? N3 K2 O3 90.89(5) 2_656 . ? O2 K2 N3 115.16(4) . . ? N3 K2 N3 104.54(4) 2_656 . ? O3 K2 N3 152.36(5) . . ? O2 K2 N4 156.61(4) . . ? N3 K2 N4 91.99(5) 2_656 . ? O3 K2 N4 110.65(5) . . ? N3 K2 N4 47.22(4) . . ? O2 K2 O1 75.51(5) . . ? N3 K2 O1 166.62(4) 2_656 . ? O3 K2 O1 77.45(5) . . ? N3 K2 O1 83.85(4) . . ? N4 K2 O1 86.14(5) . . ? O2 K2 N4 80.88(5) . 2_656 ? N3 K2 N4 45.30(4) 2_656 2_656 ? O3 K2 N4 120.28(4) . 2_656 ? N3 K2 N4 86.12(4) . 2_656 ? N4 K2 N4 109.17(4) . 2_656 ? O1 K2 N4 147.31(4) . 2_656 ? O2 K2 C30 132.89(5) . . ? N3 K2 C30 107.30(5) 2_656 . ? O3 K2 C30 128.35(5) . . ? N3 K2 C30 25.07(4) . . ? N4 K2 C30 25.06(4) . . ? O1 K2 C30 75.89(5) . . ? N4 K2 C30 105.65(5) 2_656 . ? O2 K2 C30 90.18(5) . 2_656 ? N3 K2 C30 23.44(4) 2_656 2_656 ? O3 K2 C30 101.20(5) . 2_656 ? N3 K2 C30 101.84(5) . 2_656 ? N4 K2 C30 107.45(5) . 2_656 ? O1 K2 C30 165.66(4) . 2_656 ? N4 K2 C30 23.70(4) 2_656 2_656 ? C30 K2 C30 114.59(4) . 2_656 ? O2 K2 C38 24.66(4) . . ? N3 K2 C38 109.97(6) 2_656 . ? O3 K2 C38 104.35(5) . . ? N3 K2 C38 91.93(5) . . ? N4 K2 C38 138.15(5) . . ? O1 K2 C38 79.68(6) . . ? N4 K2 C38 69.64(6) 2_656 . ? C30 K2 C38 113.17(6) . . ? C30 K2 C38 86.94(6) 2_656 . ? O2 K2 K2 128.07(4) . 2_656 ? N3 K2 K2 53.01(4) 2_656 2_656 ? O3 K2 K2 138.03(3) . 2_656 ? N3 K2 K2 51.54(3) . 2_656 ? N4 K2 K2 57.84(4) . 2_656 ? O1 K2 K2 134.32(4) . 2_656 ? N4 K2 K2 51.33(3) 2_656 2_656 ? C30 K2 K2 59.54(4) . 2_656 ? C30 K2 K2 55.05(3) 2_656 2_656 ? C38 K2 K2 107.70(5) . 2_656 ? O2 K2 K1 45.10(3) . . ? N3 K2 K1 129.65(4) 2_656 . ? O3 K2 K1 48.75(3) . . ? N3 K2 K1 125.12(3) . . ? N4 K2 K1 126.42(4) . . ? O1 K2 K1 45.11(3) . . ? N4 K2 K1 123.91(3) 2_656 . ? C30 K2 K1 120.97(4) . . ? C30 K2 K1 123.77(3) 2_656 . ? C38 K2 K1 64.69(4) . . ? K2 K2 K1 172.244(19) 2_656 . ? C31 O1 C34 109.60(14) . . ? C31 O1 K1 117.83(10) . . ? C34 O1 K1 111.22(11) . . ? C31 O1 K2 114.18(11) . . ? C34 O1 K2 114.93(11) . . ? K1 O1 K2 87.81(4) . . ? C35 O2 C38 106.15(16) . . ? C35 O2 K1 106.54(12) . . ? C38 O2 K1 135.22(12) . . ? C35 O2 K2 117.10(13) . . ? C38 O2 K2 101.75(10) . . ? K1 O2 K2 89.64(5) . . ? C39 O3 C42 106.20(15) . . ? C39 O3 K2 130.36(12) . . ? C42 O3 K2 109.59(11) . . ? C39 O3 K1 109.38(11) . . ? C42 O3 K1 114.39(11) . . ? K2 O3 K1 85.72(4) . . ? C46 O4 C43 108.89(18) . . ? C15 N1 C1 119.30(15) . . ? C15 N1 K1 94.58(11) . 2_655 ? C1 N1 K1 134.44(11) . 2_655 ? C15 N1 K1 93.71(11) . . ? C1 N1 K1 124.28(11) . . ? K1 N1 K1 78.38(5) 2_655 . ? C15 N2 C8 117.77(16) . . ? C15 N2 K1 89.65(11) . 2_655 ? C8 N2 K1 147.31(12) . 2_655 ? C15 N2 K1 80.23(10) . . ? C8 N2 K1 127.12(11) . . ? K1 N2 K1 71.81(4) 2_655 . ? C30 N3 C16 120.90(16) . . ? C30 N3 K2 99.16(11) . 2_656 ? C16 N3 K2 131.14(11) . 2_656 ? C30 N3 K2 88.72(10) . . ? C16 N3 K2 127.50(11) . . ? K2 N3 K2 75.46(4) 2_656 . ? C30 N4 C23 119.04(16) . . ? C30 N4 K2 88.50(11) . . ? C23 N4 K2 135.13(11) . . ? C30 N4 K2 85.77(10) . 2_656 ? C23 N4 K2 139.59(11) . 2_656 ? K2 N4 K2 70.83(4) . 2_656 ? N1 C1 C6 125.93(17) . . ? N1 C1 C2 116.78(16) . . ? C6 C1 C2 117.28(17) . . ? C3 C2 C1 122.70(18) . . ? C2 C3 C4 118.43(19) . . ? C2 C3 C7 120.0(2) . . ? C4 C3 C7 121.6(2) . . ? C5 C4 C3 119.84(19) . . ? C4 C5 C6 121.64(19) . . ? C5 C6 C1 120.05(18) . . ? C9 C8 N2 124.66(18) . . ? C9 C8 C13 117.24(18) . . ? N2 C8 C13 118.05(18) . . ? C8 C9 C10 122.2(2) . . ? C11 C10 C9 119.2(2) . . ? C11 C10 C14 121.6(2) . . ? C9 C10 C14 119.2(2) . . ? C10 C11 C12 119.7(2) . . ? C13 C12 C11 121.2(2) . . ? C12 C13 C8 120.4(2) . . ? N1 C15 N2 120.66(16) . . ? N1 C15 K1 60.93(9) . 2_655 ? N2 C15 K1 65.70(9) . 2_655 ? N1 C15 K1 61.88(9) . . ? N2 C15 K1 75.60(10) . . ? K1 C15 K1 67.60(5) 2_655 . ? C17 C16 N3 115.93(16) . . ? C17 C16 C21 117.13(17) . . ? N3 C16 C21 126.94(18) . . ? C18 C17 C16 123.18(19) . . ? C17 C18 C19 118.0(2) . . ? C17 C18 C22 120.2(2) . . ? C19 C18 C22 121.7(2) . . ? C20 C19 C18 119.94(19) . . ? C19 C20 C21 122.1(2) . . ? C20 C21 C16 119.6(2) . . ? N4 C23 C24 118.02(16) . . ? N4 C23 C28 124.94(16) . . ? C24 C23 C28 116.98(17) . . ? C25 C24 C23 123.24(18) . . ? C24 C25 C26 118.38(19) . . ? C24 C25 C29 121.57(19) . . ? C26 C25 C29 120.05(19) . . ? C27 C26 C25 120.10(19) . . ? C26 C27 C28 120.89(19) . . ? C27 C28 C23 120.40(18) . . ? N3 C30 N4 119.97(17) . . ? N3 C30 K2 66.22(9) . . ? N4 C30 K2 66.44(10) . . ? N3 C30 K2 57.40(10) . 2_656 ? N4 C30 K2 70.53(10) . 2_656 ? K2 C30 K2 65.41(4) . 2_656 ? O1 C31 C32 106.60(16) . . ? C33 C32 C31 103.99(18) . . ? C32 C33 C34 104.43(18) . . ? O1 C34 C33 106.13(16) . . ? O2 C35 C36 106.7(2) . . ? O2 C35 K1 50.21(10) . . ? C36 C35 K1 120.41(18) . . ? C35 C36 C37 104.52(19) . . ? C36 C37 C38 104.18(17) . . ? O2 C38 C37 107.53(16) . . ? O2 C38 K2 53.59(9) . . ? C37 C38 K2 142.53(15) . . ? O3 C39 C40 105.20(16) . . ? C39 C40 C41 103.02(17) . . ? C40 C41 C42 104.40(16) . . ? O3 C42 C41 107.54(16) . . ? O4 C43 C44 106.5(2) . . ? C45 C44 C43 101.71(19) . . ? C44 C45 C46 102.11(19) . . ? O4 C46 C45 107.3(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.882 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.054