# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'S. Batten' 'Sze Nee Pek.' 'David Turner' _publ_contact_author_name 'Stuart Batten' _publ_contact_author_address ; School of Chemistry Monash University Clayton 3800 AUSTRALIA ; _publ_contact_author_email STUART.BATTEN@SCI.MONASH.EDU.AU _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Amide-Water Hydrogen Bond Motifs in Alkali-Metal/Crown Ether Complexes of Carbamoyldicyanomethanide, C(CONH2)(CN)2- ; data_NA12C4 _database_code_depnum_ccdc_archive 'CCDC 669556' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Na(12c4)2](cdm).H2O ; _chemical_name_common '[Na(12c4)2](cdm).H2O' _chemical_melting_point ? _chemical_formula_moiety C16H32Na1O8,2(H2O1),C4N3H2O1 _chemical_formula_sum 'C20 H38 N3 Na1 O11' _chemical_formula_weight 519.52 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' Na Na 0.0362 0.0249 '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 16.7758(3) _cell_length_b 14.1320(3) _cell_length_c 23.1203(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.1930(10) _cell_angle_gamma 90.00 _cell_volume 5336.59(17) _cell_formula_units_Z 8 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 32478 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9802 _exptl_absorpt_correction_T_max 0.9860 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'phi 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 32478 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.1091 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12218 _reflns_number_gt 6327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression ? _refine_ls_number_reflns 12218 _refine_ls_number_parameters 777 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 Na1 Na 0.62800(6) 0.74966(7) 0.02185(4) 0.0247(2) Uani 1 1 d . . . O1 O 0.51194(10) 0.67926(12) 0.05932(7) 0.0300(4) Uani 1 1 d . . . N1 N 0.56891(11) 0.33064(14) 0.25349(8) 0.0249(5) Uani 1 1 d . . . H1N H 0.5698 0.2685 0.2560 0.030 Uiso 1 1 calc R . . H2N H 0.6137 0.3617 0.2517 0.030 Uiso 1 1 calc R . . C1 C 0.46802(17) 0.7543(2) 0.08010(12) 0.0373(7) Uani 1 1 d . . . H1A H 0.4294 0.7267 0.1020 0.045 Uiso 1 1 calc R . . H1B H 0.4356 0.7891 0.0455 0.045 Uiso 1 1 calc R . . Na2 Na 0.12391(6) 0.75576(7) 0.01689(4) 0.0269(2) Uani 1 1 d . . . O2 O 0.57609(11) 0.86292(12) 0.08633(7) 0.0315(4) Uani 1 1 d . . . N2 N 0.36980(18) 0.5695(2) 0.24741(14) 0.0713(9) Uani 1 1 d . . . C2 C 0.52336(17) 0.8221(2) 0.11971(12) 0.0383(7) Uani 1 1 d . . . H2A H 0.4908 0.8721 0.1336 0.046 Uiso 1 1 calc R . . H2B H 0.5559 0.7886 0.1548 0.046 Uiso 1 1 calc R . . O3 O 0.73615(10) 0.79091(12) 0.10743(7) 0.0297(4) Uani 1 1 d . . . N3 N 0.63738(17) 0.56681(19) 0.25727(11) 0.0527(7) Uani 1 1 d . . . C3 C 0.64489(17) 0.9119(2) 0.12111(11) 0.0386(7) Uani 1 1 d . . . H3A H 0.6265 0.9504 0.1514 0.046 Uiso 1 1 calc R . . H3B H 0.6666 0.9557 0.0950 0.046 Uiso 1 1 calc R . . O4 O 0.67222(10) 0.60736(12) 0.08207(7) 0.0276(4) Uani 1 1 d . . . N4 N 1.06904(12) 0.62812(15) 0.26084(9) 0.0266(5) Uani 1 1 d . . . H3N H 1.0701 0.6902 0.2636 0.032 Uiso 1 1 calc R . . H4N H 1.1150 0.5962 0.2646 0.032 Uiso 1 1 calc R . . C4 C 0.71211(17) 0.8477(2) 0.15156(12) 0.0401(7) Uani 1 1 d . . . H4A H 0.7592 0.8853 0.1734 0.048 Uiso 1 1 calc R . . H4B H 0.6928 0.8069 0.1804 0.048 Uiso 1 1 calc R . . O5 O 0.51988(10) 0.81615(12) -0.05631(7) 0.0308(4) Uani 1 1 d . . . N5 N 0.86075(15) 0.39514(18) 0.22374(10) 0.0437(6) Uani 1 1 d . . . C5 C 0.77991(15) 0.7061(2) 0.12958(12) 0.0358(7) Uani 1 1 d . . . H5A H 0.8182 0.7202 0.1680 0.043 Uiso 1 1 calc R . . H5B H 0.8127 0.6855 0.1013 0.043 Uiso 1 1 calc R . . O6 O 0.67661(11) 0.89441(12) -0.02132(7) 0.0321(4) Uani 1 1 d . . . N6 N 1.13070(16) 0.39323(18) 0.24255(11) 0.0488(7) Uani 1 1 d . . . C6 C 0.72455(16) 0.6276(2) 0.13822(11) 0.0355(7) Uani 1 1 d . . . H6A H 0.7570 0.5708 0.1539 0.043 Uiso 1 1 calc R . . H6B H 0.6918 0.6466 0.1669 0.043 Uiso 1 1 calc R . . O7 O 0.74500(10) 0.71109(13) -0.02323(7) 0.0312(4) Uani 1 1 d . . . C7 C 0.60294(16) 0.5500(2) 0.08456(12) 0.0367(7) Uani 1 1 d . . . H7A H 0.6205 0.4987 0.1138 0.044 Uiso 1 1 calc R . . H7B H 0.5819 0.5203 0.0452 0.044 Uiso 1 1 calc R . . O8 O 0.58677(10) 0.63304(12) -0.05860(7) 0.0301(4) Uani 1 1 d . . . C8 C 0.53504(16) 0.6052(2) 0.10148(12) 0.0393(7) Uani 1 1 d . . . H8A H 0.4877 0.5633 0.1013 0.047 Uiso 1 1 calc R . . H8B H 0.5540 0.6319 0.1419 0.047 Uiso 1 1 calc R . . O9 O 0.00521(11) 0.83358(13) 0.04730(7) 0.0328(4) Uani 1 1 d . A . C9 C 0.53644(18) 0.91372(19) -0.06609(12) 0.0417(7) Uani 1 1 d . . . H9A H 0.5281 0.9517 -0.0320 0.050 Uiso 1 1 calc R . . H9B H 0.4972 0.9364 -0.1021 0.050 Uiso 1 1 calc R . . O10 O 0.05992(11) 0.64638(13) 0.07750(8) 0.0328(4) Uani 1 1 d . A . C10 C 0.62240(17) 0.92868(19) -0.07361(11) 0.0392(7) Uani 1 1 d . . . H10A H 0.6309 0.8938 -0.1089 0.047 Uiso 1 1 calc R . . H10B H 0.6324 0.9968 -0.0791 0.047 Uiso 1 1 calc R . . O11 O 0.22209(11) 0.71276(14) 0.10628(7) 0.0356(5) Uani 1 1 d . A . C11 C 0.75831(17) 0.8784(2) -0.02829(12) 0.0409(7) Uani 1 1 d . . . H11A H 0.7965 0.8786 0.0113 0.049 Uiso 1 1 calc R . . H11B H 0.7742 0.9305 -0.0519 0.049 Uiso 1 1 calc R . . O12 O 0.16674(11) 0.89880(13) 0.07768(7) 0.0350(5) Uani 1 1 d . A . C12 C 0.76574(18) 0.7851(2) -0.05884(13) 0.0414(7) Uani 1 1 d . . . H12A H 0.7283 0.7842 -0.0987 0.050 Uiso 1 1 calc R . . H12B H 0.8224 0.7765 -0.0637 0.050 Uiso 1 1 calc R . . C13 C 0.72858(17) 0.62256(19) -0.05418(12) 0.0368(7) Uani 1 1 d . . . H13A H 0.7338 0.5707 -0.0248 0.044 Uiso 1 1 calc R . . H13B H 0.7701 0.6121 -0.0778 0.044 Uiso 1 1 calc R . . O13A O 0.0096(7) 0.7103(6) -0.0668(5) 0.0369(19) Uani 0.632(6) 1 d P A 1 O13B O 0.0278(12) 0.6821(10) -0.0654(9) 0.039(3) Uani 0.368(6) 1 d P A 2 C14 C 0.64532(17) 0.6188(2) -0.09453(12) 0.0382(7) Uani 1 1 d . . . H14A H 0.6396 0.6689 -0.1252 0.046 Uiso 1 1 calc R . . H14B H 0.6363 0.5567 -0.1147 0.046 Uiso 1 1 calc R . . O14A O 0.1520(4) 0.6021(7) -0.0256(4) 0.0355(16) Uani 0.632(6) 1 d P A 1 O14B O 0.1861(6) 0.6060(11) -0.0156(6) 0.033(3) Uani 0.368(6) 1 d P A 2 O15 O 0.25084(12) 0.77318(15) -0.02105(8) 0.0448(5) Uani 1 1 d . A . C15 C 0.50668(16) 0.65888(19) -0.09169(11) 0.0324(6) Uani 1 1 d . . . H15A H 0.4665 0.6457 -0.0673 0.039 Uiso 1 1 calc R . . H15B H 0.4922 0.6192 -0.1278 0.039 Uiso 1 1 calc R . . O16 O 0.10414(11) 0.86902(13) -0.06588(7) 0.0361(5) Uani 1 1 d . A . C16 C 0.50073(17) 0.76117(19) -0.10950(11) 0.0323(6) Uani 1 1 d . . . H16A H 0.5398 0.7754 -0.1346 0.039 Uiso 1 1 calc R . . H16B H 0.4447 0.7759 -0.1324 0.039 Uiso 1 1 calc R . . O17 O 0.43454(11) 0.33249(13) 0.25510(8) 0.0392(5) Uani 1 1 d . . . C17 C -0.0435(2) 0.7611(2) 0.06677(16) 0.0559(9) Uani 1 1 d . . . H17A H -0.0827 0.7917 0.0871 0.067 Uiso 1 1 calc R A . H17B H -0.0757 0.7277 0.0315 0.067 Uiso 1 1 calc R . . O18 O 0.93139(11) 0.62851(13) 0.24545(8) 0.0395(5) Uani 1 1 d . . . C18 C 0.0040(2) 0.6925(2) 0.10646(15) 0.0543(9) Uani 1 1 d . A . H18A H 0.0347 0.7246 0.1429 0.065 Uiso 1 1 calc R B 2 H18B H -0.0328 0.6452 0.1182 0.065 Uiso 1 1 calc R B 2 O19 O 0.26737(11) 0.31803(15) 0.20184(8) 0.0465(5) Uani 1 1 d . . . C19A C 0.1275(4) 0.5975(5) 0.1179(3) 0.0367(15) Uani 0.826(6) 1 d P A 1 H19A H 0.1524 0.5516 0.0948 0.044 Uiso 0.826(6) 1 calc PR A 1 H19B H 0.1055 0.5614 0.1474 0.044 Uiso 0.826(6) 1 calc PR A 1 C19B C 0.1030(18) 0.621(2) 0.1246(17) 0.037(7) Uani 0.174(6) 1 d P A 2 H19C H 0.0813 0.5601 0.1360 0.044 Uiso 0.174(6) 1 calc PR A 2 H19D H 0.0986 0.6680 0.1553 0.044 Uiso 0.174(6) 1 calc PR A 2 O20 O 0.25626(12) 0.12068(15) 0.19179(8) 0.0510(6) Uani 1 1 d . . . C20A C 0.1919(2) 0.6631(3) 0.14951(15) 0.0368(10) Uani 0.826(6) 1 d P A 1 H20A H 0.1686 0.7078 0.1742 0.044 Uiso 0.826(6) 1 calc PR A 1 H20B H 0.2366 0.6271 0.1757 0.044 Uiso 0.826(6) 1 calc PR A 1 C20B C 0.1940(13) 0.6073(12) 0.1248(8) 0.037(5) Uani 0.174(6) 1 d P A 2 H20C H 0.2013 0.5589 0.0955 0.044 Uiso 0.174(6) 1 calc PR A 2 H20D H 0.2258 0.5885 0.1647 0.044 Uiso 0.174(6) 1 calc PR A 2 O21 O 0.69114(11) 0.33828(14) 0.18360(8) 0.0442(5) Uani 1 1 d . . . C21A C 0.2672(2) 0.7995(3) 0.1298(2) 0.0337(11) Uani 0.826(6) 1 d P A 1 H21A H 0.3034 0.8179 0.1034 0.040 Uiso 0.826(6) 1 calc PR A 1 H21B H 0.3023 0.7858 0.1695 0.040 Uiso 0.826(6) 1 calc PR A 1 C21B C 0.2515(12) 0.7601(13) 0.1494(8) 0.035(5) Uani 0.174(6) 1 d PU A 2 H21C H 0.3062 0.7367 0.1700 0.042 Uiso 0.174(6) 1 calc PR A 2 H21D H 0.2153 0.7629 0.1777 0.042 Uiso 0.174(6) 1 calc PR A 2 O22 O 0.69842(12) 0.13854(16) 0.19733(8) 0.0520(6) Uani 1 1 d . . . C22A C 0.2117(2) 0.8814(2) 0.13492(14) 0.0324(9) Uani 0.826(6) 1 d P A 1 H22A H 0.1750 0.8650 0.1614 0.039 Uiso 0.826(6) 1 calc PR A 1 H22B H 0.2442 0.9378 0.1512 0.039 Uiso 0.826(6) 1 calc PR A 1 C22B C 0.2566(11) 0.8528(14) 0.1204(8) 0.024(4) Uani 0.174(6) 1 d PU A 2 H22C H 0.2963 0.8467 0.0947 0.029 Uiso 0.174(6) 1 calc PR A 2 H22D H 0.2794 0.8995 0.1517 0.029 Uiso 0.174(6) 1 calc PR A 2 C23A C 0.0953(2) 0.9610(3) 0.07560(18) 0.0285(9) Uani 0.826(6) 1 d P A 1 H23A H 0.0786 0.9897 0.0356 0.034 Uiso 0.826(6) 1 calc PR A 1 H23B H 0.1110 1.0128 0.1048 0.034 Uiso 0.826(6) 1 calc PR A 1 C23B C 0.1281(10) 0.9273(13) 0.1122(9) 0.036(5) Uani 0.174(6) 1 d P A 2 H23C H 0.1467 0.9904 0.1285 0.043 Uiso 0.174(6) 1 calc PR A 2 H23D H 0.1287 0.8822 0.1451 0.043 Uiso 0.174(6) 1 calc PR A 2 C24A C 0.0232(2) 0.9074(3) 0.08919(17) 0.0308(10) Uani 0.826(6) 1 d P A 1 H24A H 0.0376 0.8815 0.1300 0.037 Uiso 0.826(6) 1 calc PR A 1 H24B H -0.0246 0.9499 0.0856 0.037 Uiso 0.826(6) 1 calc PR A 1 C24B C 0.0480(12) 0.9311(13) 0.0701(9) 0.025(4) Uani 0.174(6) 1 d PU A 2 H24C H 0.0545 0.9677 0.0350 0.030 Uiso 0.174(6) 1 calc PR A 2 H24D H 0.0101 0.9671 0.0890 0.030 Uiso 0.174(6) 1 calc PR A 2 C25A C 0.0238(4) 0.6265(5) -0.0983(3) 0.0449(16) Uani 0.632(6) 1 d P A 1 H25A H 0.0499 0.6436 -0.1311 0.054 Uiso 0.632(6) 1 calc PR A 1 H25B H -0.0289 0.5947 -0.1154 0.054 Uiso 0.632(6) 1 calc PR A 1 C25B C 0.0480(9) 0.5862(10) -0.0711(7) 0.043(4) Uani 0.368(6) 1 d P A 2 H25C H 0.0140 0.5612 -0.1087 0.051 Uiso 0.368(6) 1 calc PR A 2 H25D H 0.0343 0.5500 -0.0380 0.051 Uiso 0.368(6) 1 calc PR A 2 C26A C 0.0789(5) 0.5609(7) -0.0554(4) 0.043(2) Uani 0.632(6) 1 d P A 1 H26A H 0.0490 0.5382 -0.0258 0.051 Uiso 0.632(6) 1 calc PR A 1 H26B H 0.0916 0.5051 -0.0776 0.051 Uiso 0.632(6) 1 calc PR A 1 C26B C 0.1399(6) 0.5693(6) -0.0707(4) 0.043(3) Uani 0.368(6) 1 d P A 2 H26C H 0.1508 0.5008 -0.0739 0.051 Uiso 0.368(6) 1 calc PR A 2 H26D H 0.1547 0.6024 -0.1045 0.051 Uiso 0.368(6) 1 calc PR A 2 C27A C 0.2135(3) 0.6054(3) -0.0588(2) 0.0380(14) Uani 0.632(6) 1 d P A 1 H27A H 0.1897 0.6281 -0.0996 0.046 Uiso 0.632(6) 1 calc PR A 1 H27B H 0.2363 0.5414 -0.0614 0.046 Uiso 0.632(6) 1 calc PR A 1 C27B C 0.2678(8) 0.6239(8) -0.0181(6) 0.042(3) Uani 0.368(6) 1 d P A 2 H27C H 0.2872 0.5701 -0.0387 0.051 Uiso 0.368(6) 1 calc PR A 2 H27D H 0.3016 0.6253 0.0231 0.051 Uiso 0.368(6) 1 calc PR A 2 C28A C 0.2803(4) 0.6721(5) -0.0279(3) 0.0366(17) Uani 0.632(6) 1 d P A 1 H28A H 0.3236 0.6742 -0.0508 0.044 Uiso 0.632(6) 1 calc PR A 1 H28B H 0.3052 0.6465 0.0120 0.044 Uiso 0.632(6) 1 calc PR A 1 C28B C 0.2835(8) 0.7152(8) -0.0491(5) 0.051(3) Uani 0.368(6) 1 d P A 2 H28C H 0.3428 0.7277 -0.0442 0.062 Uiso 0.368(6) 1 calc PR A 2 H28D H 0.2566 0.7145 -0.0919 0.062 Uiso 0.368(6) 1 calc PR A 2 C29A C 0.2405(3) 0.8193(4) -0.0761(2) 0.0365(13) Uani 0.632(6) 1 d P A 1 H29A H 0.2151 0.7764 -0.1091 0.044 Uiso 0.632(6) 1 calc PR A 1 H29B H 0.2937 0.8417 -0.0826 0.044 Uiso 0.632(6) 1 calc PR A 1 C29B C 0.2446(7) 0.8769(7) -0.0497(4) 0.044(3) Uani 0.368(6) 1 d P A 2 H29C H 0.2454 0.9257 -0.0189 0.053 Uiso 0.368(6) 1 calc PR A 2 H29D H 0.2911 0.8885 -0.0686 0.053 Uiso 0.368(6) 1 calc PR A 2 C30A C 0.1856(6) 0.9002(6) -0.0720(3) 0.0361(18) Uani 0.632(6) 1 d P A 1 H30A H 0.2110 0.9398 -0.0374 0.043 Uiso 0.632(6) 1 calc PR A 1 H30B H 0.1794 0.9396 -0.1082 0.043 Uiso 0.632(6) 1 calc PR A 1 C30B C 0.1658(12) 0.8799(12) -0.0949(6) 0.051(4) Uani 0.368(6) 1 d P A 2 H30C H 0.1600 0.9412 -0.1162 0.061 Uiso 0.368(6) 1 calc PR A 2 H30D H 0.1638 0.8285 -0.1243 0.061 Uiso 0.368(6) 1 calc PR A 2 C31A C 0.0523(6) 0.8393(9) -0.1198(4) 0.044(2) Uani 0.632(6) 1 d P A 1 H31A H 0.0818 0.7963 -0.1416 0.052 Uiso 0.632(6) 1 calc PR A 1 H31B H 0.0321 0.8944 -0.1454 0.052 Uiso 0.632(6) 1 calc PR A 1 C31B C 0.0255(10) 0.8403(13) -0.1052(7) 0.045(4) Uani 0.368(6) 1 d P A 2 H31C H 0.0165 0.8782 -0.1422 0.054 Uiso 0.368(6) 1 calc PR A 2 H31D H -0.0194 0.8552 -0.0853 0.054 Uiso 0.368(6) 1 calc PR A 2 C32A C -0.0176(3) 0.7886(5) -0.1029(2) 0.0412(14) Uani 0.632(6) 1 d P A 1 H32A H -0.0466 0.8327 -0.0815 0.049 Uiso 0.632(6) 1 calc PR A 1 H32B H -0.0569 0.7674 -0.1393 0.049 Uiso 0.632(6) 1 calc PR A 1 C32B C 0.0211(7) 0.7354(6) -0.1215(4) 0.050(3) Uani 0.368(6) 1 d P A 2 H32C H -0.0314 0.7209 -0.1496 0.060 Uiso 0.368(6) 1 calc PR A 2 H32D H 0.0665 0.7182 -0.1403 0.060 Uiso 0.368(6) 1 calc PR A 2 C33 C 0.50204(15) 0.47864(19) 0.24984(10) 0.0314(6) Uani 1 1 d . . . C34 C 0.4295(2) 0.5291(2) 0.24837(12) 0.0441(8) Uani 1 1 d . . . C35 C 0.57563(19) 0.5281(2) 0.25353(11) 0.0359(7) Uani 1 1 d . . . C36 C 0.50078(15) 0.37695(19) 0.25244(10) 0.0270(6) Uani 1 1 d . . . C37 C 0.99856(14) 0.48114(18) 0.24574(10) 0.0262(6) Uani 1 1 d . . . C38 C 0.92296(18) 0.4334(2) 0.23366(11) 0.0313(6) Uani 1 1 d . . . C39 C 1.07016(17) 0.43150(19) 0.24476(11) 0.0316(6) Uani 1 1 d . . . C40 C 0.99918(15) 0.58325(19) 0.25112(10) 0.0252(6) Uani 1 1 d . . . H5O H 0.7447 0.3576 0.1975 0.050 Uiso 1 1 d . . . H1O H 0.2359 0.3572 0.2131 0.050 Uiso 1 1 d . . . H7O H 0.7415 0.1090 0.2153 0.050 Uiso 1 1 d . . . H3O H 0.2746 0.1634 0.2041 0.050 Uiso 1 1 d . . . H2O H 0.3182 0.3305 0.2206 0.050 Uiso 1 1 d . . . H4O H 0.2167 0.1024 0.2136 0.050 Uiso 1 1 d . . . H8O H 0.6583 0.1256 0.2154 0.050 Uiso 1 1 d . . . H6O H 0.6936 0.2869 0.1855 0.050 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 Na1 0.0284(6) 0.0240(5) 0.0222(5) 0.0011(4) 0.0066(4) -0.0006(4) O1 0.0287(10) 0.0298(11) 0.0325(9) 0.0029(9) 0.0090(8) 0.0035(8) N1 0.0183(11) 0.0188(11) 0.0391(12) 0.0030(10) 0.0093(9) -0.0024(9) C1 0.0299(16) 0.0425(18) 0.0413(16) 0.0016(14) 0.0118(13) 0.0056(14) Na2 0.0366(6) 0.0234(5) 0.0225(5) -0.0014(4) 0.0106(4) -0.0027(4) O2 0.0395(11) 0.0277(10) 0.0273(9) -0.0018(8) 0.0076(8) 0.0001(9) N2 0.057(2) 0.0518(19) 0.098(2) -0.0127(17) 0.0038(17) 0.0203(16) C2 0.0419(17) 0.0403(18) 0.0377(15) -0.0015(14) 0.0192(13) 0.0069(14) O3 0.0329(10) 0.0322(11) 0.0240(9) -0.0004(8) 0.0065(8) -0.0013(9) N3 0.074(2) 0.0438(17) 0.0500(15) -0.0063(13) 0.0351(15) -0.0190(15) C3 0.0502(19) 0.0320(17) 0.0305(14) -0.0066(13) 0.0027(13) -0.0028(14) O4 0.0258(9) 0.0292(10) 0.0290(9) 0.0036(8) 0.0088(7) -0.0002(8) N4 0.0171(11) 0.0208(12) 0.0429(12) 0.0010(10) 0.0091(9) 0.0039(9) C4 0.0403(17) 0.0452(19) 0.0324(14) -0.0105(14) 0.0033(13) -0.0047(15) O5 0.0361(11) 0.0279(11) 0.0277(9) 0.0005(8) 0.0058(8) 0.0020(8) N5 0.0456(16) 0.0458(16) 0.0428(14) -0.0040(12) 0.0164(12) -0.0137(13) C5 0.0234(15) 0.0500(19) 0.0326(14) 0.0045(14) 0.0033(12) 0.0006(14) O6 0.0391(11) 0.0275(10) 0.0292(9) 0.0004(8) 0.0067(8) -0.0059(9) N6 0.0487(17) 0.0407(16) 0.0518(15) -0.0048(13) 0.0004(13) 0.0134(14) C6 0.0312(16) 0.0387(17) 0.0352(15) 0.0069(13) 0.0046(12) 0.0037(13) O7 0.0344(11) 0.0320(11) 0.0299(9) 0.0034(9) 0.0132(8) -0.0009(8) C7 0.0379(17) 0.0290(16) 0.0458(16) 0.0081(13) 0.0148(13) -0.0043(13) O8 0.0378(11) 0.0282(10) 0.0259(9) 0.0012(8) 0.0110(8) -0.0018(8) C8 0.0309(16) 0.0398(17) 0.0486(17) 0.0155(15) 0.0119(13) -0.0023(13) O9 0.0387(11) 0.0296(11) 0.0319(9) -0.0005(9) 0.0119(8) -0.0029(9) C9 0.060(2) 0.0235(16) 0.0391(16) 0.0046(13) 0.0067(14) 0.0129(14) O10 0.0407(12) 0.0300(11) 0.0307(10) -0.0013(9) 0.0143(9) -0.0031(9) C10 0.058(2) 0.0224(15) 0.0350(15) 0.0062(13) 0.0067(14) -0.0029(14) O11 0.0353(11) 0.0449(12) 0.0271(9) -0.0017(9) 0.0078(8) -0.0007(9) C11 0.0463(19) 0.0370(18) 0.0424(16) -0.0016(14) 0.0161(14) -0.0152(14) O12 0.0411(11) 0.0361(11) 0.0303(9) -0.0060(9) 0.0131(9) -0.0100(9) C12 0.0448(18) 0.0425(18) 0.0442(16) 0.0082(15) 0.0254(14) -0.0041(15) C13 0.0483(18) 0.0267(16) 0.0404(15) 0.0007(13) 0.0202(14) 0.0095(13) O13A 0.050(4) 0.032(5) 0.030(3) -0.002(4) 0.012(3) -0.008(3) O13B 0.073(10) 0.012(6) 0.024(4) -0.001(5) -0.005(5) -0.003(5) C14 0.0486(18) 0.0348(17) 0.0366(15) -0.0069(13) 0.0208(14) -0.0046(14) O14A 0.047(4) 0.030(2) 0.030(4) -0.004(2) 0.011(3) -0.003(4) O14B 0.049(7) 0.023(4) 0.025(5) -0.009(3) 0.003(6) 0.005(6) O15 0.0438(12) 0.0580(14) 0.0391(11) 0.0093(11) 0.0228(10) 0.0080(10) C15 0.0354(16) 0.0336(16) 0.0269(13) -0.0006(12) 0.0045(12) -0.0090(13) O16 0.0521(13) 0.0306(11) 0.0278(9) 0.0011(8) 0.0135(9) 0.0022(9) C16 0.0316(15) 0.0332(16) 0.0275(13) -0.0018(12) -0.0029(11) 0.0000(13) O17 0.0315(11) 0.0373(12) 0.0496(11) 0.0015(9) 0.0106(9) -0.0023(9) C17 0.048(2) 0.061(2) 0.066(2) 0.0193(19) 0.0284(17) 0.0003(18) O18 0.0318(11) 0.0347(12) 0.0542(12) -0.0020(9) 0.0144(9) 0.0031(9) C18 0.056(2) 0.042(2) 0.078(2) 0.0053(18) 0.0426(19) -0.0045(17) O19 0.0341(11) 0.0628(15) 0.0455(11) -0.0122(11) 0.0151(9) -0.0071(10) C19A 0.047(5) 0.028(3) 0.039(2) 0.013(2) 0.017(3) 0.009(3) C19B 0.022(15) 0.021(15) 0.067(18) -0.002(12) 0.011(12) -0.010(11) O20 0.0546(13) 0.0550(15) 0.0441(11) -0.0068(10) 0.0126(10) 0.0051(11) C20A 0.045(2) 0.039(3) 0.0275(18) 0.0120(19) 0.0105(16) 0.0079(18) C20B 0.080(15) 0.003(8) 0.037(10) -0.003(7) 0.033(10) -0.011(9) O21 0.0324(11) 0.0525(13) 0.0483(11) -0.0056(10) 0.0106(9) 0.0023(10) C21A 0.029(2) 0.033(3) 0.037(3) -0.006(2) 0.0040(18) 0.003(2) C21B 0.037(8) 0.027(8) 0.033(8) 0.010(7) -0.006(6) -0.003(7) O22 0.0463(13) 0.0647(15) 0.0488(12) 0.0040(11) 0.0189(10) -0.0125(11) C22A 0.028(2) 0.035(2) 0.0327(18) -0.0090(16) 0.0034(15) 0.0000(17) C22B 0.020(8) 0.026(8) 0.024(7) 0.001(7) 0.001(6) 0.006(7) C23A 0.027(2) 0.024(2) 0.035(2) -0.0018(17) 0.0072(19) 0.0052(17) C23B 0.025(10) 0.037(11) 0.044(11) -0.025(9) 0.005(9) 0.004(8) C24A 0.028(2) 0.030(2) 0.037(2) -0.0050(18) 0.0111(17) 0.0006(17) C24B 0.016(8) 0.016(8) 0.041(8) -0.006(7) 0.003(7) 0.004(6) C25A 0.045(4) 0.051(5) 0.038(3) -0.015(3) 0.007(3) -0.012(3) C25B 0.039(10) 0.029(10) 0.052(10) -0.019(7) -0.007(7) -0.007(6) C26A 0.051(6) 0.036(5) 0.045(5) -0.017(4) 0.016(4) -0.012(4) C26B 0.064(8) 0.027(5) 0.035(5) -0.007(4) 0.007(5) 0.006(5) C27A 0.046(4) 0.032(3) 0.038(3) -0.007(2) 0.014(3) 0.010(2) C27B 0.039(7) 0.039(7) 0.055(7) -0.010(6) 0.025(5) 0.001(6) C28A 0.027(3) 0.043(5) 0.042(4) -0.001(4) 0.014(3) 0.008(4) C28B 0.083(8) 0.035(7) 0.048(7) -0.008(5) 0.040(6) -0.003(6) C29A 0.041(3) 0.036(3) 0.040(3) 0.004(3) 0.025(2) -0.008(2) C29B 0.065(7) 0.016(5) 0.058(6) 0.011(5) 0.032(6) -0.005(5) C30A 0.048(5) 0.025(4) 0.041(5) 0.004(3) 0.021(4) -0.008(3) C30B 0.082(12) 0.039(9) 0.041(8) 0.005(6) 0.032(8) -0.015(7) C31A 0.053(6) 0.049(4) 0.030(4) 0.008(3) 0.010(3) 0.003(4) C31B 0.065(13) 0.030(6) 0.030(8) -0.004(7) -0.009(7) 0.010(8) C32A 0.039(3) 0.053(4) 0.028(3) 0.000(3) 0.001(2) 0.008(3) C32B 0.073(7) 0.041(6) 0.027(4) -0.002(4) -0.009(4) 0.002(5) C33 0.0401(17) 0.0253(15) 0.0287(14) 0.0020(12) 0.0077(12) 0.0030(13) C34 0.051(2) 0.0338(18) 0.0418(17) -0.0011(14) -0.0003(15) 0.0016(16) C35 0.058(2) 0.0288(16) 0.0247(14) -0.0012(12) 0.0176(14) -0.0021(15) C36 0.0314(15) 0.0295(15) 0.0187(12) 0.0021(11) 0.0028(11) 0.0011(13) C37 0.0292(15) 0.0233(15) 0.0273(13) 0.0010(11) 0.0086(11) 0.0005(12) C38 0.0403(17) 0.0318(16) 0.0243(13) 0.0019(12) 0.0126(12) 0.0037(14) C39 0.0391(17) 0.0268(15) 0.0264(13) -0.0005(12) 0.0020(12) 0.0026(14) C40 0.0244(14) 0.0302(15) 0.0226(12) 0.0034(11) 0.0088(11) 0.0028(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O3 2.4306(18) . ? Na1 O5 2.4377(18) . ? Na1 O4 2.4620(19) . ? Na1 O8 2.4632(19) . ? Na1 O2 2.4769(19) . ? Na1 O7 2.4839(18) . ? Na1 O6 2.4935(19) . ? Na1 O1 2.5101(18) . ? O1 C8 1.423(3) . ? O1 C1 1.435(3) . ? N1 C36 1.312(3) . ? C1 C2 1.494(4) . ? Na2 O11 2.408(2) . ? Na2 O13B 2.43(2) . ? Na2 O16 2.4585(19) . ? Na2 O14A 2.473(10) . ? Na2 O12 2.473(2) . ? Na2 O13A 2.479(13) . ? Na2 O10 2.4884(19) . ? Na2 O15 2.493(2) . ? Na2 O9 2.512(2) . ? Na2 O14B 2.546(15) . ? O2 C2 1.422(3) . ? O2 C3 1.426(3) . ? N2 C34 1.148(4) . ? O3 C4 1.427(3) . ? O3 C5 1.437(3) . ? N3 C35 1.157(3) . ? C3 C4 1.493(4) . ? O4 C6 1.420(3) . ? O4 C7 1.429(3) . ? N4 C40 1.306(3) . ? O5 C16 1.428(3) . ? O5 C9 1.435(3) . ? N5 C38 1.151(3) . ? C5 C6 1.490(4) . ? O6 C10 1.422(3) . ? O6 C11 1.434(3) . ? N6 C39 1.162(3) . ? O7 C12 1.422(3) . ? O7 C13 1.436(3) . ? C7 C8 1.504(4) . ? O8 C15 1.433(3) . ? O8 C14 1.438(3) . ? O9 C24A 1.409(4) . ? O9 C17 1.445(3) . ? O9 C24B 1.587(19) . ? C9 C10 1.506(4) . ? O10 C19B 1.22(4) . ? O10 C18 1.428(3) . ? O10 C19A 1.467(7) . ? O11 C21B 1.208(18) . ? O11 C20A 1.407(3) . ? O11 C21A 1.478(5) . ? O11 C20B 1.648(15) . ? C11 C12 1.514(4) . ? O12 C23B 1.207(15) . ? O12 C22A 1.388(3) . ? O12 C23A 1.478(4) . ? O12 C22B 1.729(17) . ? C13 C14 1.493(4) . ? O13A C32A 1.398(11) . ? O13A C25A 1.437(10) . ? O13B C25B 1.410(17) . ? O13B C32B 1.48(2) . ? O14A C26A 1.391(11) . ? O14A C27A 1.419(10) . ? O14B C27B 1.409(16) . ? O14B C26B 1.430(15) . ? O15 C28B 1.247(11) . ? O15 C29A 1.405(5) . ? O15 C28A 1.532(7) . ? O15 C29B 1.602(9) . ? C15 C16 1.500(4) . ? O16 C30B 1.363(18) . ? O16 C31A 1.412(12) . ? O16 C30A 1.474(10) . ? O16 C31B 1.478(18) . ? O17 C36 1.290(3) . ? C17 C18 1.443(4) . ? O18 C40 1.285(3) . ? C18 C19B 1.91(3) . ? C19A C20A 1.483(9) . ? C19B C20B 1.54(3) . ? C21A C22A 1.506(5) . ? C21B C22B 1.48(2) . ? C23A C24A 1.519(5) . ? C23B C24B 1.47(2) . ? C25A C26A 1.510(9) . ? C25B C26B 1.557(16) . ? C27A C28A 1.514(8) . ? C27B C28B 1.528(14) . ? C29A C30A 1.484(12) . ? C29B C30B 1.49(2) . ? C31A C32A 1.500(11) . ? C31B C32B 1.53(2) . ? C33 C35 1.404(4) . ? C33 C34 1.405(4) . ? C33 C36 1.439(4) . ? C37 C39 1.396(4) . ? C37 C38 1.407(4) . ? C37 C40 1.448(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Na1 O5 143.31(7) . . ? O3 Na1 O4 70.30(6) . . ? O5 Na1 O4 144.22(7) . . ? O3 Na1 O8 143.51(7) . . ? O5 Na1 O8 70.42(6) . . ? O4 Na1 O8 82.93(6) . . ? O3 Na1 O2 69.80(6) . . ? O5 Na1 O2 83.84(6) . . ? O4 Na1 O2 106.82(6) . . ? O8 Na1 O2 144.12(7) . . ? O3 Na1 O7 83.09(6) . . ? O5 Na1 O7 107.40(6) . . ? O4 Na1 O7 83.86(6) . . ? O8 Na1 O7 69.44(6) . . ? O2 Na1 O7 144.53(7) . . ? O3 Na1 O6 82.97(6) . . ? O5 Na1 O6 69.08(6) . . ? O4 Na1 O6 144.35(7) . . ? O8 Na1 O6 107.92(6) . . ? O2 Na1 O6 84.42(6) . . ? O7 Na1 O6 69.52(6) . . ? O3 Na1 O1 107.93(6) . . ? O5 Na1 O1 84.50(6) . . ? O4 Na1 O1 68.80(6) . . ? O8 Na1 O1 83.64(6) . . ? O2 Na1 O1 68.99(6) . . ? O7 Na1 O1 143.83(7) . . ? O6 Na1 O1 144.45(7) . . ? C8 O1 C1 113.25(19) . . ? C8 O1 Na1 114.63(14) . . ? C1 O1 Na1 108.69(15) . . ? O1 C1 C2 112.6(2) . . ? O11 Na2 O13B 140.0(3) . . ? O11 Na2 O16 140.95(7) . . ? O13B Na2 O16 73.8(4) . . ? O11 Na2 O14A 87.94(18) . . ? O13B Na2 O14A 57.7(3) . . ? O16 Na2 O14A 105.5(2) . . ? O11 Na2 O12 70.46(7) . . ? O13B Na2 O12 148.2(3) . . ? O16 Na2 O12 83.12(6) . . ? O14A Na2 O12 152.43(15) . . ? O11 Na2 O13A 149.4(2) . . ? O13B Na2 O13A 11.6(4) . . ? O16 Na2 O13A 67.5(2) . . ? O14A Na2 O13A 69.3(2) . . ? O12 Na2 O13A 136.75(17) . . ? O11 Na2 O10 70.03(7) . . ? O13B Na2 O10 83.1(5) . . ? O16 Na2 O10 147.55(8) . . ? O14A Na2 O10 79.9(2) . . ? O12 Na2 O10 107.12(6) . . ? O13A Na2 O10 85.5(2) . . ? O11 Na2 O15 81.67(7) . . ? O13B Na2 O15 103.5(5) . . ? O16 Na2 O15 68.66(7) . . ? O14A Na2 O15 72.02(19) . . ? O12 Na2 O15 87.63(7) . . ? O13A Na2 O15 108.8(3) . . ? O10 Na2 O15 140.56(7) . . ? O11 Na2 O9 107.51(6) . . ? O13B Na2 O9 88.9(4) . . ? O16 Na2 O9 87.60(6) . . ? O14A Na2 O9 136.98(17) . . ? O12 Na2 O9 68.23(6) . . ? O13A Na2 O9 79.1(2) . . ? O10 Na2 O9 69.07(6) . . ? O15 Na2 O9 148.27(7) . . ? O11 Na2 O14B 78.3(3) . . ? O13B Na2 O14B 69.9(4) . . ? O16 Na2 O14B 107.6(4) . . ? O14A Na2 O14B 12.9(3) . . ? O12 Na2 O14B 139.6(2) . . ? O13A Na2 O14B 81.4(3) . . ? O10 Na2 O14B 84.7(4) . . ? O15 Na2 O14B 62.5(3) . . ? O9 Na2 O14B 148.3(3) . . ? C2 O2 C3 114.47(19) . . ? C2 O2 Na1 114.36(15) . . ? C3 O2 Na1 107.62(15) . . ? O2 C2 C1 107.7(2) . . ? C4 O3 C5 114.76(19) . . ? C4 O3 Na1 115.90(15) . . ? C5 O3 Na1 108.42(14) . . ? O2 C3 C4 113.4(2) . . ? C6 O4 C7 114.59(19) . . ? C6 O4 Na1 113.34(15) . . ? C7 O4 Na1 110.07(14) . . ? O3 C4 C3 108.1(2) . . ? C16 O5 C9 113.63(19) . . ? C16 O5 Na1 114.32(14) . . ? C9 O5 Na1 110.44(15) . . ? O3 C5 C6 112.7(2) . . ? C10 O6 C11 113.6(2) . . ? C10 O6 Na1 114.56(15) . . ? C11 O6 Na1 108.88(15) . . ? O4 C6 C5 107.5(2) . . ? C12 O7 C13 113.35(19) . . ? C12 O7 Na1 113.74(15) . . ? C13 O7 Na1 108.67(14) . . ? O4 C7 C8 112.8(2) . . ? C15 O8 C14 114.08(18) . . ? C15 O8 Na1 107.45(14) . . ? C14 O8 Na1 114.75(15) . . ? O1 C8 C7 107.9(2) . . ? C24A O9 C17 111.0(3) . . ? C24A O9 C24B 28.2(7) . . ? C17 O9 C24B 139.2(8) . . ? C24A O9 Na2 117.23(19) . . ? C17 O9 Na2 108.53(17) . . ? C24B O9 Na2 98.4(7) . . ? O5 C9 C10 112.2(2) . . ? C19B O10 C18 92.0(12) . . ? C19B O10 C19A 22.4(13) . . ? C18 O10 C19A 114.3(3) . . ? C19B O10 Na2 116.4(14) . . ? C18 O10 Na2 113.21(16) . . ? C19A O10 Na2 106.3(3) . . ? O6 C10 C9 107.3(2) . . ? C21B O11 C20A 80.6(10) . . ? C21B O11 C21A 32.7(9) . . ? C20A O11 C21A 112.9(3) . . ? C21B O11 C20B 111.9(11) . . ? C20A O11 C20B 36.3(6) . . ? C21A O11 C20B 143.8(7) . . ? C21B O11 Na2 129.7(9) . . ? C20A O11 Na2 116.66(17) . . ? C21A O11 Na2 107.4(2) . . ? C20B O11 Na2 105.8(8) . . ? O6 C11 C12 111.9(2) . . ? C23B O12 C22A 71.7(9) . . ? C23B O12 C23A 43.0(10) . . ? C22A O12 C23A 113.4(2) . . ? C23B O12 C22B 106.1(11) . . ? C22A O12 C22B 34.5(6) . . ? C23A O12 C22B 146.8(7) . . ? C23B O12 Na2 121.2(8) . . ? C22A O12 Na2 114.91(18) . . ? C23A O12 Na2 109.82(18) . . ? C22B O12 Na2 96.9(7) . . ? O7 C12 C11 108.2(2) . . ? O7 C13 C14 112.8(2) . . ? C32A O13A C25A 114.8(9) . . ? C32A O13A Na2 110.5(6) . . ? C25A O13A Na2 114.9(6) . . ? C25B O13B C32B 112.3(15) . . ? C25B O13B Na2 110.7(11) . . ? C32B O13B Na2 111.8(11) . . ? O8 C14 C13 107.4(2) . . ? C26A O14A C27A 114.4(7) . . ? C26A O14A Na2 109.8(6) . . ? C27A O14A Na2 114.4(5) . . ? C27B O14B C26B 111.2(12) . . ? C27B O14B Na2 109.4(9) . . ? C26B O14B Na2 112.9(7) . . ? C28B O15 C29A 79.1(6) . . ? C28B O15 C28A 31.0(4) . . ? C29A O15 C28A 108.3(4) . . ? C28B O15 C29B 112.4(6) . . ? C29A O15 C29B 38.6(3) . . ? C28A O15 C29B 143.3(5) . . ? C28B O15 Na2 129.1(6) . . ? C29A O15 Na2 115.2(2) . . ? C28A O15 Na2 105.5(3) . . ? C29B O15 Na2 104.8(4) . . ? O8 C15 C16 112.8(2) . . ? C30B O16 C31A 89.0(6) . . ? C30B O16 C30A 25.1(5) . . ? C31A O16 C30A 113.7(4) . . ? C30B O16 C31B 113.5(8) . . ? C31A O16 C31B 24.7(5) . . ? C30A O16 C31B 137.7(6) . . ? C30B O16 Na2 118.3(8) . . ? C31A O16 Na2 116.1(5) . . ? C30A O16 Na2 107.8(4) . . ? C31B O16 Na2 104.1(7) . . ? O5 C16 C15 107.5(2) . . ? C18 C17 O9 113.8(3) . . ? O10 C18 C17 109.6(3) . . ? O10 C18 C19B 39.6(11) . . ? C17 C18 C19B 145.4(11) . . ? O10 C19A C20A 112.9(5) . . ? O10 C19B C20B 115(3) . . ? O10 C19B C18 48.4(10) . . ? C20B C19B C18 152(2) . . ? O11 C20A C19A 107.5(4) . . ? C19B C20B O11 103.3(16) . . ? O11 C21A C22A 113.1(3) . . ? O11 C21B C22B 99.9(15) . . ? O12 C22A C21A 105.8(3) . . ? C21B C22B O12 117.2(14) . . ? O12 C23A C24A 112.0(3) . . ? O12 C23B C24B 97.0(16) . . ? O9 C24A C23A 106.4(3) . . ? C23B C24B O9 117.7(14) . . ? O13A C25A C26A 108.8(7) . . ? O13B C25B C26B 114.0(14) . . ? O14A C26A C25A 114.0(8) . . ? O14B C26B C25B 106.4(9) . . ? O14A C27A C28A 108.5(5) . . ? O14B C27B C28B 116.4(13) . . ? C27A C28A O15 114.0(4) . . ? O15 C28B C27B 99.7(9) . . ? O15 C29A C30A 104.5(5) . . ? C30B C29B O15 106.3(9) . . ? O16 C30A C29A 112.2(6) . . ? O16 C30B C29B 107.7(10) . . ? O16 C31A C32A 105.8(6) . . ? O16 C31B C32B 113.8(12) . . ? O13A C32A C31A 111.5(7) . . ? O13B C32B C31B 106.8(10) . . ? C35 C33 C34 119.6(3) . . ? C35 C33 C36 121.0(2) . . ? C34 C33 C36 119.2(2) . . ? N2 C34 C33 179.2(4) . . ? N3 C35 C33 178.2(3) . . ? O17 C36 N1 120.8(2) . . ? O17 C36 C33 120.6(2) . . ? N1 C36 C33 118.5(2) . . ? C39 C37 C38 119.7(2) . . ? C39 C37 C40 120.9(2) . . ? C38 C37 C40 118.9(2) . . ? N5 C38 C37 179.3(3) . . ? N6 C39 C37 177.1(3) . . ? O18 C40 N4 120.9(2) . . ? O18 C40 C37 119.9(2) . . ? N4 C40 C37 119.2(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O18 0.88 1.98 2.857(3) 175.3 2_645 N1 H2N O21 0.88 2.28 2.888(2) 126.0 . N4 H3N O17 0.88 2.05 2.910(3) 164.1 2_655 N4 H4N O20 0.88 2.19 2.887(3) 135.6 2_655 O21 H5O N5 0.92 1.97 2.898(3) 177.0 . O19 H1O N6 0.85 2.09 2.873(3) 152.9 1_455 O22 H7O N3 0.86 2.07 2.898(3) 161.6 2_645 O20 H3O O19 0.71 2.19 2.801(3) 145.7 . O19 H2O O17 0.88 1.93 2.801(2) 168.0 . O20 H4O N2 0.96 1.93 2.886(4) 175.5 2_545 O22 H8O O18 0.89 1.93 2.798(2) 166.9 2_645 O21 H6O O22 0.73 2.11 2.840(3) 175.7 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.633 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.070 # Attachment '2.CIF' data_K12c4 _database_code_depnum_ccdc_archive 'CCDC 669557' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(12-crown-4)potassium carbamoyldicyanomethanide hydrate ; _chemical_name_common '[K(12c4)2]cdm.H2O' _chemical_melting_point ? _chemical_formula_moiety C16H32K1O8.C4H2N3O1.H2O1 _chemical_formula_sum 'C20 H36 K1 N3 O10' _chemical_formula_weight 517.62 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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.138(3) _cell_length_b 11.009(3) _cell_length_c 25.629(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.335(12) _cell_angle_gamma 90.00 _cell_volume 2562.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 37454 _cell_measurement_theta_min 2.02 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9395 _exptl_absorpt_correction_T_max 0.9691 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37454 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5827 _reflns_number_gt 5638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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 5827 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1276 _refine_ls_R_factor_gt 0.1261 _refine_ls_wR_factor_ref 0.3257 _refine_ls_wR_factor_gt 0.3244 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 K1 K 0.27108(11) 0.76865(9) 0.05035(4) 0.0304(3) Uani 1 1 d . . . O1 O 0.2542(4) 0.5290(3) 0.28560(16) 0.0383(8) Uani 1 1 d . . . N1 N 0.0428(4) 0.6341(4) 0.27711(18) 0.0308(8) Uani 1 1 d . . . C1 C 0.2694(5) 0.7382(3) 0.29960(17) 0.0248(8) Uani 1 1 d . . . H1N H -0.001(6) 0.576(5) 0.259(2) 0.021(12) Uiso 1 1 d . . . H1O H 0.206(6) 0.379(5) 0.246(2) 0.021(12) Uiso 1 1 d . . . O2 O 0.4127(4) 0.6027(3) 0.11960(14) 0.0327(7) Uani 1 1 d . . . N2 N 0.5490(5) 0.7330(4) 0.3140(2) 0.0403(10) Uani 1 1 d . . . C2 C 0.4237(5) 0.7337(3) 0.30728(17) 0.0250(8) Uani 1 1 d . . . H2N H 0.006(6) 0.694(5) 0.276(2) 0.022(12) Uiso 1 1 d . . . H2O H 0.261(9) 0.289(7) 0.222(3) 0.052(19) Uiso 1 1 d . . . O3 O 0.1044(4) 0.6499(3) 0.11480(12) 0.0280(7) Uani 1 1 d . . . N3 N 0.1497(5) 0.9477(4) 0.2996(2) 0.0397(10) Uani 1 1 d . . . C3 C 0.2032(5) 0.8535(4) 0.29978(17) 0.0260(8) Uani 1 1 d . . . O4 O 0.1534(3) 0.9011(3) 0.12804(13) 0.0292(7) Uani 1 1 d . . . C4 C 0.1887(5) 0.6276(4) 0.28722(17) 0.0256(8) Uani 1 1 d . . . O5 O 0.4575(4) 0.8540(3) 0.13191(13) 0.0309(7) Uani 1 1 d . . . C5 C 0.3074(6) 0.5176(4) 0.1340(2) 0.0407(12) Uani 1 1 d . . . H5A H 0.3558 0.4619 0.1609 0.049 Uiso 1 1 calc R . . H5B H 0.2713 0.4685 0.1029 0.049 Uiso 1 1 calc R . . O6 O 0.4502(4) 0.6997(3) -0.02294(15) 0.0380(8) Uani 1 1 d . . . C6 C 0.1780(5) 0.5776(4) 0.1553(2) 0.0347(10) Uani 1 1 d . . . H6A H 0.1102 0.5152 0.1667 0.042 Uiso 1 1 calc R . . H6B H 0.2124 0.6290 0.1859 0.042 Uiso 1 1 calc R . . O7 O 0.1757(4) 0.5828(3) -0.01930(15) 0.0381(8) Uani 1 1 d . . . C7 C -0.0015(5) 0.7287(4) 0.13322(18) 0.0285(9) Uani 1 1 d . . . H7A H -0.0596 0.6830 0.1570 0.034 Uiso 1 1 calc R . . H7B H -0.0699 0.7568 0.1030 0.034 Uiso 1 1 calc R . . O8 O 0.0412(4) 0.8142(4) -0.02493(17) 0.0446(9) Uani 1 1 d . . . C8 C 0.0666(5) 0.8371(4) 0.16181(18) 0.0309(9) Uani 1 1 d . . . H8A H -0.0114 0.8910 0.1726 0.037 Uiso 1 1 calc R . . H8B H 0.1291 0.8106 0.1938 0.037 Uiso 1 1 calc R . . O9 O 0.3149(4) 0.9315(3) -0.02802(15) 0.0410(9) Uani 1 1 d . . . C9 C 0.2637(5) 0.9771(4) 0.1553(2) 0.0340(10) Uani 1 1 d . . . H9A H 0.2222 1.0170 0.1851 0.041 Uiso 1 1 calc R . . H9B H 0.2910 1.0415 0.1313 0.041 Uiso 1 1 calc R . . O10 O 0.1849(4) 0.3119(4) 0.2342(2) 0.0525(12) Uani 1 1 d . . . C10 C 0.3991(5) 0.9082(4) 0.17587(19) 0.0324(10) Uani 1 1 d . . . H10A H 0.4725 0.9638 0.1945 0.039 Uiso 1 1 calc R . . H10B H 0.3743 0.8447 0.2008 0.039 Uiso 1 1 calc R . . C11 C 0.5700(6) 0.7675(5) 0.1462(2) 0.0422(12) Uani 1 1 d . . . H11A H 0.6379 0.8004 0.1757 0.051 Uiso 1 1 calc R . . H11B H 0.6274 0.7544 0.1161 0.051 Uiso 1 1 calc R . . C12 C 0.5104(6) 0.6480(5) 0.1624(2) 0.0414(12) Uani 1 1 d . . . H12A H 0.5920 0.5899 0.1713 0.050 Uiso 1 1 calc R . . H12B H 0.4572 0.6589 0.1937 0.050 Uiso 1 1 calc R . . C13 C 0.3910(6) 0.6217(5) -0.0636(2) 0.0428(12) Uani 1 1 d . . . H13A H 0.4713 0.5811 -0.0799 0.051 Uiso 1 1 calc R . . H13B H 0.3306 0.6686 -0.0911 0.051 Uiso 1 1 calc R . . C14 C 0.2981(7) 0.5295(5) -0.0401(3) 0.0488(14) Uani 1 1 d . . . H14A H 0.2623 0.4694 -0.0673 0.059 Uiso 1 1 calc R . . H14B H 0.3591 0.4858 -0.0118 0.059 Uiso 1 1 calc R . . C15 C 0.0560(7) 0.6070(5) -0.0574(3) 0.0522(15) Uani 1 1 d . . . H15A H -0.0034 0.5325 -0.0647 0.063 Uiso 1 1 calc R . . H15B H 0.0925 0.6338 -0.0905 0.063 Uiso 1 1 calc R . . C16 C -0.0359(6) 0.7040(6) -0.0372(3) 0.0566(17) Uani 1 1 d . . . H16A H -0.1204 0.7209 -0.0638 0.068 Uiso 1 1 calc R . . H16B H -0.0756 0.6739 -0.0052 0.068 Uiso 1 1 calc R . . C17 C 0.0716(8) 0.8827(6) -0.0694(3) 0.0605(18) Uani 1 1 d . . . H17A H -0.0202 0.9191 -0.0868 0.073 Uiso 1 1 calc R . . H17B H 0.1146 0.8298 -0.0949 0.073 Uiso 1 1 calc R . . C18 C 0.1784(8) 0.9803(5) -0.0503(3) 0.0588(17) Uani 1 1 d . . . H18A H 0.1955 1.0341 -0.0800 0.071 Uiso 1 1 calc R . . H18B H 0.1356 1.0301 -0.0236 0.071 Uiso 1 1 calc R . . C19 C 0.4106(8) 0.8972(5) -0.0657(2) 0.0500(15) Uani 1 1 d . . . H19A H 0.4631 0.9696 -0.0771 0.060 Uiso 1 1 calc R . . H19B H 0.3529 0.8615 -0.0969 0.060 Uiso 1 1 calc R . . C20 C 0.5174(6) 0.8078(5) -0.0418(2) 0.0453(13) Uani 1 1 d . . . H20A H 0.5837 0.7839 -0.0681 0.054 Uiso 1 1 calc R . . H20B H 0.5784 0.8467 -0.0121 0.054 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 0.0388(6) 0.0315(5) 0.0216(5) 0.0004(3) 0.0062(4) -0.0029(4) O1 0.0349(18) 0.0191(14) 0.059(2) 0.0010(14) -0.0032(15) 0.0049(13) N1 0.0287(19) 0.0180(17) 0.046(2) 0.0016(16) 0.0043(16) 0.0017(15) C1 0.028(2) 0.0154(17) 0.031(2) 0.0020(15) 0.0027(16) 0.0020(15) O2 0.0336(17) 0.0252(15) 0.0402(18) -0.0015(13) 0.0072(14) 0.0053(13) N2 0.033(2) 0.0258(19) 0.062(3) 0.0047(19) 0.005(2) 0.0003(16) C2 0.027(2) 0.0161(17) 0.032(2) -0.0009(15) 0.0058(16) 0.0005(14) O3 0.0345(16) 0.0208(14) 0.0297(15) -0.0035(11) 0.0083(12) 0.0005(12) N3 0.038(2) 0.0224(18) 0.058(3) -0.0053(18) 0.0012(19) 0.0033(16) C3 0.0257(19) 0.0212(19) 0.031(2) -0.0020(16) 0.0028(16) -0.0025(15) O4 0.0316(16) 0.0235(14) 0.0324(16) 0.0037(12) 0.0035(12) -0.0025(12) C4 0.029(2) 0.0218(18) 0.0266(19) 0.0029(15) 0.0055(16) -0.0022(16) O5 0.0326(16) 0.0258(15) 0.0348(16) -0.0025(13) 0.0061(13) -0.0054(12) C5 0.046(3) 0.020(2) 0.058(3) 0.007(2) 0.019(2) 0.0068(19) O6 0.0365(18) 0.0354(18) 0.0428(19) -0.0002(15) 0.0074(15) 0.0077(14) C6 0.037(2) 0.028(2) 0.040(2) 0.0119(19) 0.014(2) 0.0079(19) O7 0.045(2) 0.0258(16) 0.044(2) -0.0041(14) 0.0067(16) -0.0016(14) C7 0.028(2) 0.026(2) 0.032(2) -0.0004(17) 0.0042(17) -0.0010(16) O8 0.039(2) 0.038(2) 0.055(2) -0.0022(17) 0.0009(17) 0.0070(16) C8 0.036(2) 0.026(2) 0.033(2) -0.0030(17) 0.0118(18) -0.0005(17) O9 0.057(2) 0.0242(16) 0.044(2) 0.0000(14) 0.0157(17) -0.0040(15) C9 0.040(2) 0.0169(18) 0.046(3) -0.0064(18) 0.009(2) -0.0060(17) O10 0.033(2) 0.0283(19) 0.099(4) -0.015(2) 0.019(2) -0.0094(15) C10 0.035(2) 0.030(2) 0.033(2) -0.0099(18) 0.0051(18) -0.0097(18) C11 0.030(2) 0.040(3) 0.056(3) -0.012(2) 0.005(2) 0.000(2) C12 0.046(3) 0.035(3) 0.042(3) 0.000(2) -0.002(2) 0.016(2) C13 0.048(3) 0.037(3) 0.046(3) -0.005(2) 0.018(2) 0.007(2) C14 0.067(4) 0.025(2) 0.056(3) -0.005(2) 0.012(3) 0.011(2) C15 0.055(3) 0.039(3) 0.059(4) -0.013(3) -0.008(3) -0.004(3) C16 0.030(3) 0.059(4) 0.078(4) -0.018(3) -0.006(3) -0.008(3) C17 0.060(4) 0.056(4) 0.062(4) 0.013(3) -0.012(3) 0.025(3) C18 0.076(4) 0.027(3) 0.075(4) 0.012(3) 0.015(3) 0.023(3) C19 0.079(4) 0.032(3) 0.045(3) 0.001(2) 0.029(3) -0.013(3) C20 0.039(3) 0.045(3) 0.054(3) 0.001(3) 0.017(2) -0.007(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 K1 O3 2.704(3) . ? K1 O5 2.715(3) . ? K1 O6 2.731(4) . ? K1 O8 2.737(4) . ? K1 O9 2.754(4) . ? K1 O2 2.767(4) . ? K1 O4 2.778(3) . ? K1 O7 2.791(4) . ? O1 C4 1.242(5) . ? N1 C4 1.332(6) . ? N1 H1N 0.86(6) . ? N1 H2N 0.74(6) . ? C1 C2 1.403(6) . ? C1 C3 1.406(5) . ? C1 C4 1.441(6) . ? O2 C5 1.420(6) . ? O2 C12 1.425(6) . ? N2 C2 1.139(6) . ? O3 C6 1.417(6) . ? O3 C7 1.419(5) . ? N3 C3 1.146(6) . ? O4 C8 1.423(5) . ? O4 C9 1.432(6) . ? O5 C11 1.419(6) . ? O5 C10 1.430(5) . ? C5 C6 1.508(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? O6 C13 1.412(7) . ? O6 C20 1.447(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C15 1.410(7) . ? O7 C14 1.418(7) . ? C7 C8 1.499(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O8 C17 1.419(8) . ? O8 C16 1.420(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? O9 C18 1.419(8) . ? O9 C19 1.423(7) . ? C9 C10 1.496(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O10 H1O 0.81(6) . ? O10 H2O 0.83(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.499(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.492(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.488(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.498(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.471(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 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 O3 K1 O5 92.57(10) . . ? O3 K1 O6 134.93(11) . . ? O5 K1 O6 104.65(11) . . ? O3 K1 O8 94.53(12) . . ? O5 K1 O8 147.90(11) . . ? O6 K1 O8 92.16(12) . . ? O3 K1 O9 153.79(12) . . ? O5 K1 O9 101.94(11) . . ? O6 K1 O9 62.16(11) . . ? O8 K1 O9 61.89(13) . . ? O3 K1 O2 62.87(10) . . ? O5 K1 O2 61.65(10) . . ? O6 K1 O2 89.11(11) . . ? O8 K1 O2 147.28(12) . . ? O9 K1 O2 143.34(12) . . ? O3 K1 O4 61.79(9) . . ? O5 K1 O4 61.72(10) . . ? O6 K1 O4 161.31(11) . . ? O8 K1 O4 94.67(11) . . ? O9 K1 O4 106.26(10) . . ? O2 K1 O4 94.43(10) . . ? O3 K1 O7 83.05(10) . . ? O5 K1 O7 150.61(11) . . ? O6 K1 O7 61.64(11) . . ? O8 K1 O7 61.47(11) . . ? O9 K1 O7 94.08(11) . . ? O2 K1 O7 90.97(11) . . ? O4 K1 O7 136.46(11) . . ? C4 N1 H1N 118(3) . . ? C4 N1 H2N 120(4) . . ? H1N N1 H2N 117(5) . . ? C2 C1 C3 117.2(4) . . ? C2 C1 C4 118.9(4) . . ? C3 C1 C4 123.6(4) . . ? C5 O2 C12 114.6(4) . . ? C5 O2 K1 108.6(3) . . ? C12 O2 K1 118.1(3) . . ? N2 C2 C1 178.2(5) . . ? C6 O3 C7 112.7(3) . . ? C6 O3 K1 117.7(3) . . ? C7 O3 K1 111.0(2) . . ? N3 C3 C1 179.5(5) . . ? C8 O4 C9 113.7(4) . . ? C8 O4 K1 117.5(2) . . ? C9 O4 K1 110.5(3) . . ? O1 C4 N1 121.1(4) . . ? O1 C4 C1 120.6(4) . . ? N1 C4 C1 118.3(4) . . ? C11 O5 C10 113.5(4) . . ? C11 O5 K1 110.0(3) . . ? C10 O5 K1 119.6(3) . . ? O2 C5 C6 112.7(4) . . ? O2 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? O2 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C13 O6 C20 113.3(4) . . ? C13 O6 K1 117.8(3) . . ? C20 O6 K1 108.0(3) . . ? O3 C6 C5 108.0(4) . . ? O3 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O3 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C15 O7 C14 113.6(5) . . ? C15 O7 K1 117.9(3) . . ? C14 O7 K1 109.9(3) . . ? O3 C7 C8 112.8(4) . . ? O3 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? O3 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C17 O8 C16 114.4(5) . . ? C17 O8 K1 117.4(4) . . ? C16 O8 K1 108.8(4) . . ? O4 C8 C7 109.0(4) . . ? O4 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? O4 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? C18 O9 C19 114.0(5) . . ? C18 O9 K1 110.3(3) . . ? C19 O9 K1 118.2(3) . . ? O4 C9 C10 112.7(4) . . ? O4 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? O4 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? H1O O10 H2O 104(6) . . ? O5 C10 C9 107.5(4) . . ? O5 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? O5 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? O5 C11 C12 112.6(4) . . ? O5 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? O5 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? O2 C12 C11 108.1(4) . . ? O2 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O2 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? O6 C13 C14 107.7(4) . . ? O6 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? O6 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? O7 C14 C13 112.2(4) . . ? O7 C14 H14A 109.2 . . ? C13 C14 H14A 109.2 . . ? O7 C14 H14B 109.2 . . ? C13 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? O7 C15 C16 108.5(5) . . ? O7 C15 H15A 110.0 . . ? C16 C15 H15A 110.0 . . ? O7 C15 H15B 110.0 . . ? C16 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? O8 C16 C15 113.9(5) . . ? O8 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? O8 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? O8 C17 C18 107.3(6) . . ? O8 C17 H17A 110.3 . . ? C18 C17 H17A 110.3 . . ? O8 C17 H17B 110.3 . . ? C18 C17 H17B 110.3 . . ? H17A C17 H17B 108.5 . . ? O9 C18 C17 111.8(4) . . ? O9 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? O9 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? O9 C19 C20 108.9(5) . . ? O9 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O9 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? O6 C20 C19 113.8(4) . . ? O6 C20 H20A 108.8 . . ? C19 C20 H20A 108.8 . . ? O6 C20 H20B 108.8 . . ? C19 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H2N O10 0.74(6) 2.17(6) 2.847(6) 154(5) 2 O10 H1O O1 0.81(6) 1.97(6) 2.768(5) 170(5) . N1 H1N N3 0.86(6) 2.38(6) 3.227(6) 169(5) 2_545 O10 H2O N2 0.83(8) 2.14(8) 2.977(6) 178(7) 2_645 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.390 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.138 # Attachment '3b.CIF' data_SNZ59 _database_code_depnum_ccdc_archive 'CCDC 669558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(15c5)2](cdm).H2O ; _chemical_name_common '[K(15c5)2](cdm).H2O' _chemical_melting_point ? _chemical_formula_moiety C20H40K1O10,O1H2,C4N3H2O1 _chemical_formula_sum 'C24 H44 K1 N3 O12' _chemical_formula_weight 605.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 16.1381(3) _cell_length_b 18.4737(4) _cell_length_c 22.6934(5) _cell_angle_alpha 113.457(1) _cell_angle_beta 96.583(1) _cell_angle_gamma 93.778(1) _cell_volume 6119.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 52606 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9456 _exptl_absorpt_correction_T_max 0.9544 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi 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 52606 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 26518 _reflns_number_gt 16950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression ? _refine_ls_number_reflns 26518 _refine_ls_number_parameters 1505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 0.73742(3) 0.35810(2) 0.955070(19) 0.018 Uani 1 1 d . . . O1 O 0.07008(8) -0.06874(8) 0.74794(7) 0.024 Uani 1 1 d . . . N1 N 0.17755(11) 0.02188(11) 0.75721(9) 0.025 Uani 1 1 d . . . C1 C 0.03922(12) 0.05993(11) 0.76696(9) 0.018 Uani 1 1 d . . . H1N H 0.2072(14) 0.4880(13) 0.7602(10) 0.038 Uiso 1 1 d . . . H1O H 0.3706(16) 1.0595(15) 0.7514(12) 0.054 Uiso 1 1 d . . . K2 K 0.73630(3) 0.86128(2) 0.961160(19) 0.019 Uani 1 1 d . . . O2 O 0.27901(8) 0.40227(8) 0.72929(7) 0.024 Uani 1 1 d . . . N2 N 0.09093(11) 0.20378(10) 0.78865(9) 0.034 Uani 1 1 d . . . C2 C 0.06641(12) 0.13925(12) 0.77906(9) 0.021 Uani 1 1 d . . . H2N H 0.1950(14) 0.5795(13) 0.7781(10) 0.037 Uiso 1 1 d . . . H2O H 0.3636(19) 0.9777(18) 0.7390(13) 0.085 Uiso 1 1 d . . . K3 K 0.76755(3) 0.14269(2) 0.536100(18) 0.017 Uani 1 1 d . . . O3 O 0.06708(8) 0.43646(7) 0.75906(6) 0.023 Uani 1 1 d . . . N3 N -0.11703(11) 0.02028(10) 0.76349(8) 0.027 Uani 1 1 d . . . C3 C -0.04677(13) 0.03813(11) 0.76556(9) 0.019 Uani 1 1 d . . . H3N H 0.1732(13) 0.2822(13) 0.7567(10) 0.033 Uiso 1 1 d . . . H3O H 0.504(2) 1.0004(19) 0.7357(15) 0.103 Uiso 1 1 d . . . K4 K 0.76399(3) 0.63793(2) 0.534790(18) 0.017 Uani 1 1 d . . . O4 O 0.28142(8) 0.89448(7) 0.72356(6) 0.022 Uani 1 1 d . . . N4 N 0.18433(11) 0.32197(10) 0.74816(8) 0.021 Uani 1 1 d . . . C4 C 0.09577(12) 0.00061(11) 0.75694(9) 0.018 Uani 1 1 d . . . H4N H 0.1471(13) 0.3573(12) 0.7524(9) 0.030 Uiso 1 1 d . . . H4O H 0.5442(17) 0.9253(16) 0.7242(12) 0.066 Uiso 1 1 d . . . O5 O 0.40188(10) 0.52538(10) 0.74834(9) 0.036 Uani 1 1 d . . . N5 N 0.30218(11) 0.16909(10) 0.76715(8) 0.025 Uani 1 1 d . . . C5 C 0.32468(12) 0.28847(11) 0.73804(9) 0.018 Uani 1 1 d . . . H5N H 0.1992(13) 0.0726(12) 0.7650(9) 0.030 Uiso 1 1 d . . . H5O H 0.3749(18) 0.5616(16) 0.7556(13) 0.065 Uiso 1 1 d . . . O6 O 0.56298(11) 0.47615(10) 0.73380(9) 0.042 Uani 1 1 d . . . N6 N 0.46659(11) 0.31616(10) 0.70614(8) 0.029 Uani 1 1 d . . . C6 C 0.31204(12) 0.22239(11) 0.75373(9) 0.018 Uani 1 1 d . . . H6N H 0.2121(13) -0.0157(11) 0.7470(9) 0.020 Uiso 1 1 d . . . H6O H 0.3662(16) 0.4808(15) 0.7404(11) 0.051 Uiso 1 1 d . . . O7 O 0.39837(10) 1.02401(9) 0.74475(8) 0.031 Uani 1 1 d . . . N7 N 0.17664(11) 0.52977(10) 0.77727(8) 0.021 Uani 1 1 d . . . C7 C 0.40307(12) 0.30394(11) 0.72045(9) 0.020 Uani 1 1 d . . . H7N H 0.1481(14) 0.8544(12) 0.7477(10) 0.032 Uiso 1 1 d . . . H7O H 0.505(2) 0.509(2) 0.7407(16) 0.126 Uiso 1 1 d . . . O8 O 0.55927(11) 0.97266(10) 0.72903(9) 0.043 Uani 1 1 d . . . N8 N 0.09017(11) 0.70707(10) 0.79446(9) 0.032 Uani 1 1 d . . . C8 C 0.26173(12) 0.34039(11) 0.73845(8) 0.017 Uani 1 1 d . . . H8N H 0.1766(12) 0.7804(12) 0.7573(9) 0.025 Uiso 1 1 d . . . H8O H 0.545(2) 0.4311(19) 0.7219(15) 0.095 Uiso 1 1 d . . . O9 O 0.63150(10) 0.38681(9) 1.04948(7) 0.034 Uani 1 1 d . . . N9 N -0.12165(11) 0.52156(10) 0.75923(8) 0.026 Uani 1 1 d . . . C9 C 0.03603(12) 0.56380(11) 0.77312(9) 0.017 Uani 1 1 d . . . O10 O 0.73311(9) 0.51675(8) 1.04364(6) 0.028 Uani 1 1 d . . . N10 N 0.18615(11) 0.82004(10) 0.74797(8) 0.022 Uani 1 1 d . . . C10 C 0.06453(12) 0.64302(11) 0.78483(9) 0.021 Uani 1 1 d . . . O11 O 0.89691(9) 0.46067(8) 1.02133(6) 0.025 Uani 1 1 d . . . N11 N 0.30002(11) 0.66562(10) 0.76814(8) 0.028 Uani 1 1 d . . . C11 C -0.05078(13) 0.54057(11) 0.76590(9) 0.018 Uani 1 1 d . . . O12 O 0.86390(9) 0.32865(8) 1.04970(7) 0.028 Uani 1 1 d . . . N12 N 0.47036(11) 0.81621(10) 0.71230(8) 0.029 Uani 1 1 d . . . C12 C 0.09330(12) 0.50592(11) 0.76881(8) 0.017 Uani 1 1 d . . . O13 O 0.70526(9) 0.24024(8) 1.00286(6) 0.029 Uani 1 1 d . . . C13 C 0.26387(12) 0.83601(11) 0.73696(8) 0.017 Uani 1 1 d . . . O14 O 0.56201(9) 0.28835(8) 0.88882(6) 0.024 Uani 1 1 d . . . C14 C 0.32660(12) 0.78497(11) 0.73965(9) 0.017 Uani 1 1 d . . . O15 O 0.62856(9) 0.44734(8) 0.90979(6) 0.024 Uani 1 1 d . . . C15 C 0.31178(12) 0.71928(11) 0.75528(9) 0.019 Uani 1 1 d . . . O16 O 0.79421(9) 0.42716(8) 0.87455(6) 0.023 Uani 1 1 d . . . C16 C 0.40607(12) 0.80163(11) 0.72467(9) 0.019 Uani 1 1 d . . . O17 O 0.86019(8) 0.28857(8) 0.87987(6) 0.023 Uani 1 1 d . . . C17 C 0.64571(16) 0.46543(14) 1.10107(11) 0.041 Uani 1 1 d . . . H17A H 0.6953 0.4697 1.1328 0.050 Uiso 1 1 calc R . . H17B H 0.5963 0.4759 1.1241 0.050 Uiso 1 1 calc R . . O18 O 0.69676(8) 0.21251(7) 0.83122(6) 0.023 Uani 1 1 d . . . C18 C 0.65983(15) 0.52383(14) 1.07330(11) 0.039 Uani 1 1 d . . . H18A H 0.6106 0.5174 1.0406 0.047 Uiso 1 1 calc R . . H18B H 0.6641 0.5780 1.1082 0.047 Uiso 1 1 calc R . . O19 O 0.63714(9) 0.91124(9) 1.06118(6) 0.030 Uani 1 1 d . . . C19 C 0.80892(14) 0.55299(12) 1.08725(9) 0.028 Uani 1 1 d . . . H19A H 0.8183 0.5283 1.1186 0.033 Uiso 1 1 calc R . . H19B H 0.8064 0.6105 1.1118 0.033 Uiso 1 1 calc R . . O20 O 0.75714(10) 1.02486(8) 1.04818(6) 0.031 Uani 1 1 d . . . C20 C 0.87855(14) 0.54067(12) 1.04709(10) 0.029 Uani 1 1 d . . . H20A H 0.8627 0.5563 1.0107 0.035 Uiso 1 1 calc R . . H20B H 0.9298 0.5758 1.0743 0.035 Uiso 1 1 calc R . . O21 O 0.90486(9) 0.94323(9) 1.02468(6) 0.034 Uani 1 1 d . . . C21 C 0.95294(13) 0.44335(13) 1.06574(10) 0.028 Uani 1 1 d . . . H21A H 0.9383 0.4686 1.1100 0.034 Uiso 1 1 calc R . . H21B H 1.0113 0.4646 1.0668 0.034 Uiso 1 1 calc R . . O22 O 0.84828(10) 0.81731(9) 1.05429(7) 0.034 Uani 1 1 d . . . C22 C 0.94622(13) 0.35534(12) 1.04433(10) 0.029 Uani 1 1 d . . . H22A H 0.9564 0.3295 0.9988 0.034 Uiso 1 1 calc R . . H22B H 0.9886 0.3416 1.0721 0.034 Uiso 1 1 calc R . . O23 O 0.68193(10) 0.75081(8) 1.01009(7) 0.033 Uani 1 1 d . . . C23 C 0.85186(14) 0.24631(12) 1.03490(10) 0.032 Uani 1 1 d . . . H23A H 0.8949 0.2330 1.0625 0.038 Uiso 1 1 calc R . . H23B H 0.8571 0.2151 0.9888 0.038 Uiso 1 1 calc R . . O24 O 0.55790(9) 0.80737(9) 0.89853(7) 0.030 Uani 1 1 d . . . C24 C 0.76620(15) 0.22695(13) 1.04728(10) 0.033 Uani 1 1 d . . . H24A H 0.7578 0.1707 1.0412 0.039 Uiso 1 1 calc R . . H24B H 0.7598 0.2610 1.0926 0.039 Uiso 1 1 calc R . . O25 O 0.64019(10) 0.95970(8) 0.91788(7) 0.031 Uani 1 1 d . . . C25 C 0.62448(14) 0.24837(13) 1.02243(10) 0.035 Uani 1 1 d . . . H25A H 0.6106 0.2072 1.0385 0.042 Uiso 1 1 calc R . . H25B H 0.5822 0.2388 0.9841 0.042 Uiso 1 1 calc R . . O26 O 0.80244(10) 0.92377(8) 0.87971(6) 0.031 Uani 1 1 d . . . C26 C 0.61850(15) 0.32850(14) 1.07446(10) 0.035 Uani 1 1 d . . . H26A H 0.5624 0.3295 1.0882 0.043 Uiso 1 1 calc R . . H26B H 0.6615 0.3397 1.1128 0.043 Uiso 1 1 calc R . . O27 O 0.84950(9) 0.77826(8) 0.88272(6) 0.028 Uani 1 1 d . . . C27 C 0.51347(13) 0.34957(13) 0.88792(11) 0.030 Uani 1 1 d . . . H27A H 0.5023 0.3811 0.9325 0.036 Uiso 1 1 calc R . . H27B H 0.4587 0.3251 0.8599 0.036 Uiso 1 1 calc R . . O28 O 0.68206(9) 0.71756(8) 0.83589(7) 0.027 Uani 1 1 d . . . C28 C 0.55679(13) 0.40412(13) 0.86331(10) 0.029 Uani 1 1 d . . . H28A H 0.5740 0.3728 0.8208 0.035 Uiso 1 1 calc R . . H28B H 0.5183 0.4412 0.8576 0.035 Uiso 1 1 calc R . . O29 O 0.64740(8) 0.21859(8) 0.61355(6) 0.021 Uani 1 1 d . . . C29 C 0.67676(14) 0.50019(12) 0.89098(10) 0.026 Uani 1 1 d . . . H29A H 0.7107 0.5422 0.9303 0.032 Uiso 1 1 calc R . . H29B H 0.6379 0.5262 0.8709 0.032 Uiso 1 1 calc R . . O30 O 0.81663(8) 0.27914(7) 0.65981(6) 0.020 Uani 1 1 d . . . C30 C 0.73413(14) 0.45898(12) 0.84398(9) 0.026 Uani 1 1 d . . . H30A H 0.7011 0.4157 0.8049 0.031 Uiso 1 1 calc R . . H30B H 0.7630 0.4972 0.8302 0.031 Uiso 1 1 calc R . . O31 O 0.94375(8) 0.18780(8) 0.60111(6) 0.021 Uani 1 1 d . . . C31 C 0.85050(13) 0.38532(12) 0.83217(9) 0.025 Uani 1 1 d . . . H31A H 0.8852 0.4226 0.8207 0.030 Uiso 1 1 calc R . . H31B H 0.8183 0.3440 0.7916 0.030 Uiso 1 1 calc R . . O32 O 0.85619(9) 0.03851(8) 0.57894(6) 0.024 Uani 1 1 d . . . C32 C 0.90560(13) 0.34774(12) 0.86653(9) 0.025 Uani 1 1 d . . . H32A H 0.9486 0.3232 0.8395 0.030 Uiso 1 1 calc R . . H32B H 0.9353 0.3895 0.9080 0.030 Uiso 1 1 calc R . . O33 O 0.69126(9) 0.07158(8) 0.61355(6) 0.024 Uani 1 1 d . . . C33 C 0.84154(14) 0.21377(11) 0.82535(10) 0.027 Uani 1 1 d . . . H33A H 0.8900 0.1829 0.8226 0.033 Uiso 1 1 calc R . . H33B H 0.8302 0.2219 0.7848 0.033 Uiso 1 1 calc R . . O34 O 0.60131(9) 0.10341(8) 0.46152(6) 0.028 Uani 1 1 d . . . C34 C 0.76596(13) 0.16952(11) 0.83361(10) 0.025 Uani 1 1 d . . . H34A H 0.7546 0.1153 0.7985 0.030 Uiso 1 1 calc R . . H34B H 0.7755 0.1650 0.8758 0.030 Uiso 1 1 calc R . . O35 O 0.69831(9) 0.25444(8) 0.48991(6) 0.026 Uani 1 1 d . . . C35 C 0.61903(13) 0.17088(12) 0.83082(10) 0.026 Uani 1 1 d . . . H35A H 0.6210 0.1608 0.8706 0.031 Uiso 1 1 calc R . . H35B H 0.6079 0.1191 0.7926 0.031 Uiso 1 1 calc R . . O36 O 0.86643(9) 0.22204(8) 0.47139(6) 0.025 Uani 1 1 d . . . C36 C 0.55147(13) 0.22165(12) 0.82797(9) 0.028 Uani 1 1 d . . . H36A H 0.5559 0.2394 0.7925 0.033 Uiso 1 1 calc R . . H36B H 0.4954 0.1911 0.8195 0.033 Uiso 1 1 calc R . . O37 O 0.82447(9) 0.05600(8) 0.41705(7) 0.028 Uani 1 1 d . . . C37 C 0.66364(15) 0.98818(13) 1.11147(10) 0.033 Uani 1 1 d . . . H37A H 0.7129 0.9864 1.1410 0.040 Uiso 1 1 calc R . . H37B H 0.6178 1.0069 1.1372 0.040 Uiso 1 1 calc R . . O38 O 0.70123(9) -0.02030(8) 0.45580(6) 0.027 Uani 1 1 d . . . C38 C 0.68638(16) 1.04364(13) 1.08052(10) 0.036 Uani 1 1 d . . . H38A H 0.6377 1.0418 1.0489 0.044 Uiso 1 1 calc R . . H38B H 0.6982 1.0986 1.1145 0.044 Uiso 1 1 calc R . . O39 O 0.64875(8) 0.72683(7) 0.61129(6) 0.022 Uani 1 1 d . . . C39 C 0.83513(15) 1.05384(13) 1.08973(10) 0.037 Uani 1 1 d . . . H39A H 0.8385 1.0329 1.1238 0.045 Uiso 1 1 calc R . . H39B H 0.8416 1.1126 1.1111 0.045 Uiso 1 1 calc R . . O40 O 0.81788(8) 0.77463(8) 0.66422(6) 0.022 Uani 1 1 d . . . C40 C 0.90276(16) 1.02645(14) 1.04873(11) 0.043 Uani 1 1 d . . . H40A H 0.8938 1.0418 1.0116 0.051 Uiso 1 1 calc R . . H40B H 0.9579 1.0538 1.0749 0.051 Uiso 1 1 calc R . . O41 O 0.93844(8) 0.67669(8) 0.60098(6) 0.024 Uani 1 1 d . . . C41 C 0.95310(14) 0.92037(16) 1.06968(11) 0.042 Uani 1 1 d . . . H41A H 0.9392 0.9491 1.1138 0.050 Uiso 1 1 calc R . . H41B H 1.0138 0.9340 1.0708 0.050 Uiso 1 1 calc R . . O42 O 0.84394(9) 0.52787(8) 0.57448(6) 0.025 Uani 1 1 d . . . C42 C 0.93337(15) 0.83304(15) 1.04880(11) 0.043 Uani 1 1 d . . . H42A H 0.9425 0.8044 1.0033 0.052 Uiso 1 1 calc R . . H42B H 0.9704 0.8149 1.0767 0.052 Uiso 1 1 calc R . . O43 O 0.68432(9) 0.57630(8) 0.61366(6) 0.022 Uani 1 1 d . . . C43 C 0.82375(17) 0.73611(13) 1.03894(11) 0.043 Uani 1 1 d . . . H43A H 0.8619 0.7175 1.0658 0.051 Uiso 1 1 calc R . . H43B H 0.8265 0.7036 0.9926 0.051 Uiso 1 1 calc R . . O44 O 0.59346(9) 0.57596(9) 0.46898(7) 0.032 Uani 1 1 d . . . C44 C 0.73636(17) 0.72805(14) 1.05214(11) 0.042 Uani 1 1 d . . . H44A H 0.7187 0.6723 1.0445 0.050 Uiso 1 1 calc R . . H44B H 0.7334 0.7624 1.0981 0.050 Uiso 1 1 calc R . . O45 O 0.67279(10) 0.69852(9) 0.44629(8) 0.039 Uani 1 1 d . . . C45 C 0.60502(15) 0.77308(14) 1.03293(11) 0.039 Uani 1 1 d . . . H45A H 0.5825 0.7342 1.0488 0.046 Uiso 1 1 calc R . . H45B H 0.5638 0.7706 0.9961 0.046 Uiso 1 1 calc R . . O46 O 0.84432(10) 0.74414(8) 0.48958(7) 0.031 Uani 1 1 d . . . C46 C 0.61370(15) 0.85425(14) 1.08606(10) 0.037 Uani 1 1 d . . . H46A H 0.5597 0.8645 1.1029 0.045 Uiso 1 1 calc R . . H46B H 0.6571 0.8586 1.1223 0.045 Uiso 1 1 calc R . . O47 O 0.86123(9) 0.57637(8) 0.43291(6) 0.027 Uani 1 1 d . . . C47 C 0.51687(15) 0.87394(15) 0.90087(12) 0.041 Uani 1 1 d . . . H47A H 0.5107 0.9067 0.9465 0.050 Uiso 1 1 calc R . . H47B H 0.4598 0.8550 0.8753 0.050 Uiso 1 1 calc R . . O48 O 0.72389(9) 0.47423(8) 0.44447(6) 0.027 Uani 1 1 d . . . C48 C 0.56388(15) 0.92445(15) 0.87478(12) 0.042 Uani 1 1 d . . . H48A H 0.5756 0.8914 0.8307 0.050 Uiso 1 1 calc R . . H48B H 0.5301 0.9661 0.8720 0.050 Uiso 1 1 calc R . . C49 C 0.69298(16) 1.00630(13) 0.89631(11) 0.037 Uani 1 1 d . . . H49A H 0.7307 1.0467 0.9344 0.045 Uiso 1 1 calc R . . H49B H 0.6575 1.0348 0.8763 0.045 Uiso 1 1 calc R . . C50 C 0.74477(16) 0.95771(13) 0.84831(10) 0.036 Uani 1 1 d . . . H50A H 0.7080 0.9150 0.8111 0.043 Uiso 1 1 calc R . . H50B H 0.7760 0.9916 0.8316 0.043 Uiso 1 1 calc R . . C51 C 0.85556(15) 0.87697(13) 0.83730(10) 0.034 Uani 1 1 d . . . H51A H 0.8953 0.9117 0.8269 0.041 Uiso 1 1 calc R . . H51B H 0.8213 0.8388 0.7962 0.041 Uiso 1 1 calc R . . C52 C 0.90299(14) 0.83309(14) 0.87040(10) 0.034 Uani 1 1 d . . . H52A H 0.9435 0.8041 0.8428 0.040 Uiso 1 1 calc R . . H52B H 0.9354 0.8719 0.9121 0.040 Uiso 1 1 calc R . . C53 C 0.82416(15) 0.70528(12) 0.82707(11) 0.036 Uani 1 1 d . . . H53A H 0.8685 0.6697 0.8226 0.043 Uiso 1 1 calc R . . H53B H 0.8152 0.7156 0.7873 0.043 Uiso 1 1 calc R . . C54 C 0.74473(15) 0.66706(12) 0.83526(10) 0.032 Uani 1 1 d . . . H54A H 0.7282 0.6141 0.7989 0.038 Uiso 1 1 calc R . . H54B H 0.7523 0.6601 0.8765 0.038 Uiso 1 1 calc R . . C55 C 0.60067(14) 0.68356(13) 0.83639(10) 0.033 Uani 1 1 d . . . H55A H 0.6004 0.6722 0.8755 0.040 Uiso 1 1 calc R . . H55B H 0.5841 0.6331 0.7974 0.040 Uiso 1 1 calc R . . C56 C 0.54105(14) 0.74181(14) 0.83684(10) 0.034 Uani 1 1 d . . . H56A H 0.5483 0.7601 0.8020 0.041 Uiso 1 1 calc R . . H56B H 0.4824 0.7167 0.8290 0.041 Uiso 1 1 calc R . . C57 C 0.67390(12) 0.29147(11) 0.66908(9) 0.023 Uani 1 1 d . . . H57A H 0.6840 0.2812 0.7088 0.028 Uiso 1 1 calc R . . H57B H 0.6299 0.3275 0.6743 0.028 Uiso 1 1 calc R . . C58 C 0.75311(12) 0.32861(11) 0.65905(9) 0.021 Uani 1 1 d . . . H58A H 0.7447 0.3333 0.6169 0.025 Uiso 1 1 calc R . . H58B H 0.7696 0.3825 0.6941 0.025 Uiso 1 1 calc R . . C59 C 0.89743(12) 0.31304(12) 0.65720(10) 0.024 Uani 1 1 d . . . H59A H 0.9131 0.3656 0.6941 0.028 Uiso 1 1 calc R . . H59B H 0.8966 0.3203 0.6162 0.028 Uiso 1 1 calc R . . C60 C 0.95922(12) 0.25781(12) 0.66063(9) 0.025 Uani 1 1 d . . . H60A H 1.0172 0.2839 0.6671 0.030 Uiso 1 1 calc R . . H60B H 0.9532 0.2435 0.6977 0.030 Uiso 1 1 calc R . . C61 C 0.98355(13) 0.12358(13) 0.60543(10) 0.027 Uani 1 1 d . . . H61A H 1.0366 0.1446 0.6364 0.032 Uiso 1 1 calc R . . H61B H 0.9977 0.0899 0.5623 0.032 Uiso 1 1 calc R . . C62 C 0.92839(13) 0.07391(12) 0.62747(10) 0.028 Uani 1 1 d . . . H62A H 0.9591 0.0321 0.6336 0.034 Uiso 1 1 calc R . . H62B H 0.9113 0.1075 0.6694 0.034 Uiso 1 1 calc R . . C63 C 0.79958(15) -0.01189(12) 0.59417(10) 0.030 Uani 1 1 d . . . H63A H 0.8325 -0.0440 0.6120 0.036 Uiso 1 1 calc R . . H63B H 0.7634 -0.0490 0.5536 0.036 Uiso 1 1 calc R . . C64 C 0.74481(14) 0.03260(12) 0.64221(10) 0.029 Uani 1 1 d . . . H64A H 0.7108 -0.0047 0.6540 0.035 Uiso 1 1 calc R . . H64B H 0.7800 0.0721 0.6822 0.035 Uiso 1 1 calc R . . C65 C 0.63970(13) 0.11845(12) 0.65727(9) 0.025 Uani 1 1 d . . . H65A H 0.6749 0.1557 0.6983 0.031 Uiso 1 1 calc R . . H65B H 0.5999 0.0838 0.6676 0.031 Uiso 1 1 calc R . . C66 C 0.59231(12) 0.16391(12) 0.62545(9) 0.025 Uani 1 1 d . . . H66A H 0.5590 0.1261 0.5837 0.030 Uiso 1 1 calc R . . H66B H 0.5527 0.1934 0.6538 0.030 Uiso 1 1 calc R . . C67 C 0.57783(14) 0.15370(13) 0.43043(10) 0.033 Uani 1 1 d . . . H67A H 0.5159 0.1472 0.4191 0.040 Uiso 1 1 calc R . . H67B H 0.6024 0.1392 0.3898 0.040 Uiso 1 1 calc R . . C68 C 0.60878(13) 0.23790(13) 0.47521(11) 0.033 Uani 1 1 d . . . H68A H 0.5871 0.2731 0.4552 0.040 Uiso 1 1 calc R . . H68B H 0.5857 0.2507 0.5163 0.040 Uiso 1 1 calc R . . C69 C 0.73624(14) 0.26572(13) 0.44050(10) 0.030 Uani 1 1 d . . . H69A H 0.7135 0.3096 0.4318 0.036 Uiso 1 1 calc R . . H69B H 0.7245 0.2167 0.3998 0.036 Uiso 1 1 calc R . . C70 C 0.82887(14) 0.28549(12) 0.46348(10) 0.031 Uani 1 1 d . . . H70A H 0.8559 0.2995 0.4317 0.038 Uiso 1 1 calc R . . H70B H 0.8392 0.3327 0.5055 0.038 Uiso 1 1 calc R . . C71 C 0.89312(14) 0.16932(12) 0.41314(10) 0.027 Uani 1 1 d . . . H71A H 0.9467 0.1931 0.4074 0.033 Uiso 1 1 calc R . . H71B H 0.8505 0.1606 0.3752 0.033 Uiso 1 1 calc R . . C72 C 0.90459(13) 0.09233(13) 0.41736(10) 0.028 Uani 1 1 d . . . H72A H 0.9299 0.0577 0.3799 0.034 Uiso 1 1 calc R . . H72B H 0.9424 0.1013 0.4578 0.034 Uiso 1 1 calc R . . C73 C 0.82149(14) -0.02580(12) 0.40571(10) 0.029 Uani 1 1 d . . . H73A H 0.8530 -0.0316 0.4433 0.035 Uiso 1 1 calc R . . H73B H 0.8467 -0.0554 0.3666 0.035 Uiso 1 1 calc R . . C74 C 0.73124(15) -0.05716(12) 0.39619(9) 0.031 Uani 1 1 d . . . H74A H 0.6986 -0.0453 0.3621 0.037 Uiso 1 1 calc R . . H74B H 0.7252 -0.1155 0.3823 0.037 Uiso 1 1 calc R . . C75 C 0.61089(14) -0.02881(13) 0.45006(10) 0.033 Uani 1 1 d . . . H75A H 0.5950 -0.0156 0.4937 0.039 Uiso 1 1 calc R . . H75B H 0.5886 -0.0850 0.4225 0.039 Uiso 1 1 calc R . . C76 C 0.57115(14) 0.02259(13) 0.42158(10) 0.034 Uani 1 1 d . . . H76A H 0.5848 0.0088 0.3772 0.040 Uiso 1 1 calc R . . H76B H 0.5093 0.0140 0.4185 0.040 Uiso 1 1 calc R . . C77 C 0.67675(13) 0.79986(11) 0.66604(10) 0.027 Uani 1 1 d . . . H77A H 0.6783 0.7915 0.7066 0.032 Uiso 1 1 calc R . . H77B H 0.6376 0.8393 0.6673 0.032 Uiso 1 1 calc R . . C78 C 0.76270(13) 0.82974(11) 0.66071(10) 0.024 Uani 1 1 d . . . H78A H 0.7620 0.8350 0.6189 0.029 Uiso 1 1 calc R . . H78B H 0.7817 0.8826 0.6965 0.029 Uiso 1 1 calc R . . C79 C 0.90363(13) 0.80274(12) 0.66686(10) 0.027 Uani 1 1 d . . . H79A H 0.9225 0.8509 0.7074 0.032 Uiso 1 1 calc R . . H79B H 0.9094 0.8165 0.6295 0.032 Uiso 1 1 calc R . . C80 C 0.95549(13) 0.73844(13) 0.66481(9) 0.028 Uani 1 1 d . . . H80A H 1.0159 0.7594 0.6757 0.034 Uiso 1 1 calc R . . H80B H 0.9414 0.7176 0.6969 0.034 Uiso 1 1 calc R . . C81 C 0.97461(14) 0.60678(13) 0.59495(11) 0.031 Uani 1 1 d . . . H81A H 1.0313 0.6217 0.6212 0.038 Uiso 1 1 calc R . . H81B H 0.9810 0.5765 0.5490 0.038 Uiso 1 1 calc R . . C82 C 0.92245(13) 0.55439(13) 0.61688(11) 0.033 Uani 1 1 d . . . H82A H 0.9517 0.5083 0.6151 0.040 Uiso 1 1 calc R . . H82B H 0.9133 0.5845 0.6622 0.040 Uiso 1 1 calc R . . C83 C 0.78520(14) 0.48487(11) 0.59496(10) 0.025 Uani 1 1 d . . . H83A H 0.8159 0.4527 0.6140 0.031 Uiso 1 1 calc R . . H83B H 0.7454 0.4479 0.5565 0.031 Uiso 1 1 calc R . . C84 C 0.73644(13) 0.53769(12) 0.64392(9) 0.025 Uani 1 1 d . . . H84A H 0.7015 0.5057 0.6602 0.030 Uiso 1 1 calc R . . H84B H 0.7755 0.5777 0.6813 0.030 Uiso 1 1 calc R . . C85 C 0.63674(13) 0.62865(12) 0.65732(9) 0.024 Uani 1 1 d . . . H85A H 0.6744 0.6659 0.6970 0.029 Uiso 1 1 calc R . . H85B H 0.5955 0.5979 0.6702 0.029 Uiso 1 1 calc R . . C86 C 0.59198(12) 0.67403(12) 0.62433(10) 0.024 Uani 1 1 d . . . H86A H 0.5583 0.6360 0.5829 0.028 Uiso 1 1 calc R . . H86B H 0.5528 0.7052 0.6522 0.028 Uiso 1 1 calc R . . C87 C 0.55578(15) 0.60510(15) 0.42485(11) 0.042 Uani 1 1 d . . . H87A H 0.4938 0.5968 0.4209 0.050 Uiso 1 1 calc R . . H87B H 0.5717 0.5766 0.3813 0.050 Uiso 1 1 calc R . . C88 C 0.58594(14) 0.69176(15) 0.45033(11) 0.040 Uani 1 1 d . . . H88A H 0.5551 0.7161 0.4240 0.048 Uiso 1 1 calc R . . H88B H 0.5767 0.7192 0.4960 0.048 Uiso 1 1 calc R . . C89 C 0.70825(16) 0.77544(13) 0.46287(12) 0.043 Uani 1 1 d . . . H89A H 0.7068 0.8080 0.5094 0.051 Uiso 1 1 calc R . . H89B H 0.6756 0.7992 0.4369 0.051 Uiso 1 1 calc R . . C90 C 0.79781(16) 0.77535(13) 0.45014(11) 0.039 Uani 1 1 d . . . H90A H 0.7995 0.7424 0.4037 0.046 Uiso 1 1 calc R . . H90B H 0.8227 0.8302 0.4604 0.046 Uiso 1 1 calc R . . C91 C 0.91600(14) 0.71120(13) 0.46427(10) 0.034 Uani 1 1 d . . . H91A H 0.9547 0.7068 0.4995 0.041 Uiso 1 1 calc R . . H91B H 0.9457 0.7478 0.4492 0.041 Uiso 1 1 calc R . . C92 C 0.89524(14) 0.63100(13) 0.40903(10) 0.031 Uani 1 1 d . . . H92A H 0.8538 0.6337 0.3745 0.037 Uiso 1 1 calc R . . H92B H 0.9466 0.6131 0.3903 0.037 Uiso 1 1 calc R . . C93 C 0.82559(14) 0.50331(12) 0.38208(9) 0.028 Uani 1 1 d . . . H93A H 0.8685 0.4793 0.3548 0.034 Uiso 1 1 calc R . . H93B H 0.7789 0.5121 0.3543 0.034 Uiso 1 1 calc R . . C94 C 0.79348(15) 0.44860(12) 0.41073(10) 0.030 Uani 1 1 d . . . H94A H 0.7761 0.3950 0.3754 0.036 Uiso 1 1 calc R . . H94B H 0.8398 0.4442 0.4413 0.036 Uiso 1 1 calc R . . C95 C 0.64575(15) 0.45350(13) 0.40331(10) 0.036 Uani 1 1 d . . . H95A H 0.6314 0.3950 0.3826 0.043 Uiso 1 1 calc R . . H95B H 0.6481 0.4731 0.3687 0.043 Uiso 1 1 calc R . . C96 C 0.58158(15) 0.49110(13) 0.44445(11) 0.038 Uani 1 1 d . . . H96A H 0.5249 0.4711 0.4184 0.046 Uiso 1 1 calc R . . H96B H 0.5844 0.4753 0.4814 0.046 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 0.020 0.017 0.017 0.007 0.004 0.003 O1 0.018 0.017 0.039 0.012 0.004 0.004 N1 0.017 0.016 0.041 0.011 0.003 0.003 C1 0.018 0.018 0.021 0.010 0.003 0.003 K2 0.021 0.018 0.017 0.007 0.004 0.002 O2 0.022 0.019 0.035 0.014 0.008 0.005 N2 0.029 0.025 0.054 0.022 0.010 0.005 C2 0.017 0.024 0.027 0.013 0.005 0.005 K3 0.018 0.016 0.015 0.005 0.003 0.002 O3 0.021 0.015 0.031 0.008 0.003 0.003 N3 0.023 0.022 0.041 0.016 0.011 0.006 C3 0.025 0.012 0.020 0.008 0.006 0.007 K4 0.019 0.017 0.016 0.007 0.004 0.002 O4 0.023 0.017 0.028 0.012 0.005 0.004 N4 0.018 0.018 0.030 0.011 0.007 0.006 C4 0.017 0.019 0.015 0.005 -0.001 0.003 O5 0.030 0.027 0.056 0.018 0.015 0.007 N5 0.027 0.022 0.030 0.012 0.004 0.007 C5 0.018 0.017 0.020 0.007 0.003 0.002 O6 0.035 0.036 0.052 0.015 0.004 0.002 N6 0.022 0.032 0.036 0.016 0.009 0.009 C6 0.016 0.018 0.016 0.003 0.000 0.003 O7 0.028 0.026 0.041 0.013 0.012 0.006 N7 0.018 0.018 0.028 0.009 0.003 0.003 C7 0.021 0.018 0.019 0.006 0.000 0.006 O8 0.032 0.029 0.062 0.015 0.007 0.000 N8 0.029 0.024 0.050 0.021 0.007 0.005 C8 0.020 0.014 0.015 0.005 0.001 0.003 O9 0.038 0.040 0.029 0.017 0.015 0.009 N9 0.022 0.023 0.038 0.015 0.009 0.006 C9 0.018 0.016 0.019 0.008 0.004 0.003 O10 0.027 0.027 0.024 0.002 0.004 0.008 N10 0.018 0.018 0.032 0.014 0.005 0.005 C10 0.019 0.023 0.026 0.014 0.006 0.007 O11 0.027 0.027 0.020 0.007 0.002 0.004 N11 0.026 0.025 0.037 0.017 0.005 0.006 C11 0.025 0.012 0.018 0.007 0.005 0.007 O12 0.027 0.025 0.034 0.012 0.006 0.008 N12 0.024 0.031 0.040 0.019 0.011 0.009 C12 0.018 0.018 0.013 0.006 0.002 0.004 O13 0.033 0.030 0.025 0.015 0.002 -0.001 C13 0.019 0.014 0.012 0.002 0.000 0.001 O14 0.024 0.029 0.021 0.011 0.003 0.003 C14 0.019 0.016 0.019 0.007 0.003 0.005 O15 0.028 0.024 0.021 0.011 0.003 0.004 C15 0.016 0.021 0.019 0.006 0.002 0.005 O16 0.030 0.021 0.019 0.008 0.007 0.005 C16 0.023 0.016 0.020 0.009 0.001 0.005 O17 0.025 0.018 0.019 0.003 0.003 0.003 C17 0.042 0.056 0.031 0.017 0.018 0.023 O18 0.025 0.016 0.026 0.008 0.003 0.000 C18 0.038 0.039 0.037 0.008 0.012 0.018 O19 0.031 0.040 0.023 0.018 0.008 0.008 C19 0.038 0.018 0.020 0.002 -0.002 0.004 O20 0.047 0.024 0.018 0.004 0.006 0.005 C20 0.033 0.021 0.029 0.008 -0.001 -0.004 O21 0.028 0.048 0.019 0.008 0.002 -0.004 C21 0.022 0.036 0.024 0.010 0.001 0.003 O22 0.034 0.033 0.036 0.014 0.007 0.015 C22 0.022 0.036 0.026 0.010 0.003 0.011 O23 0.046 0.029 0.025 0.015 0.000 -0.003 C23 0.042 0.025 0.028 0.011 0.000 0.013 O24 0.026 0.040 0.028 0.018 0.002 0.003 C24 0.048 0.025 0.029 0.017 0.000 0.005 O25 0.041 0.029 0.027 0.015 0.004 0.008 C25 0.034 0.042 0.033 0.023 0.002 -0.009 O26 0.049 0.024 0.020 0.007 0.013 0.002 C26 0.031 0.053 0.030 0.024 0.010 0.003 O27 0.028 0.026 0.022 0.003 0.005 0.005 C27 0.020 0.039 0.036 0.019 0.006 0.009 O28 0.031 0.018 0.030 0.010 0.004 -0.002 C28 0.027 0.034 0.029 0.017 -0.001 0.008 O29 0.019 0.020 0.019 0.002 0.003 -0.002 C29 0.036 0.019 0.026 0.012 0.004 0.005 O30 0.016 0.016 0.026 0.007 0.005 0.000 C30 0.035 0.022 0.023 0.014 0.003 0.002 O31 0.020 0.025 0.018 0.007 0.001 0.005 C31 0.030 0.024 0.021 0.008 0.010 0.000 O32 0.032 0.022 0.020 0.010 0.001 0.005 C32 0.020 0.026 0.022 0.002 0.007 -0.002 O33 0.034 0.021 0.017 0.008 0.005 0.003 C33 0.032 0.017 0.026 0.001 0.007 0.008 O34 0.027 0.030 0.024 0.008 -0.002 -0.001 C34 0.034 0.015 0.023 0.005 0.003 0.008 O35 0.028 0.029 0.024 0.013 0.008 0.010 C35 0.031 0.020 0.024 0.008 0.002 -0.007 O36 0.029 0.026 0.023 0.011 0.005 0.002 C36 0.025 0.031 0.022 0.009 -0.001 -0.007 O37 0.030 0.024 0.036 0.014 0.015 0.009 C37 0.040 0.039 0.020 0.008 0.010 0.017 O38 0.034 0.024 0.019 0.006 0.000 -0.004 C38 0.057 0.030 0.022 0.007 0.009 0.021 O39 0.021 0.017 0.020 0.001 0.004 0.000 C39 0.056 0.024 0.023 0.003 -0.002 -0.006 O40 0.018 0.020 0.026 0.007 0.004 -0.002 C40 0.046 0.042 0.032 0.012 -0.001 -0.025 O41 0.024 0.028 0.021 0.011 0.005 0.007 C41 0.022 0.073 0.025 0.015 0.001 0.003 O42 0.029 0.027 0.024 0.015 0.005 0.005 C42 0.031 0.067 0.029 0.017 0.002 0.021 O43 0.029 0.020 0.017 0.008 0.005 0.004 C43 0.065 0.031 0.033 0.013 0.002 0.024 O44 0.027 0.040 0.023 0.007 0.000 0.002 C44 0.072 0.027 0.031 0.018 0.001 0.007 O45 0.039 0.039 0.050 0.025 0.011 0.015 C45 0.038 0.047 0.036 0.026 0.003 -0.014 O46 0.043 0.027 0.026 0.014 0.006 -0.002 C46 0.035 0.057 0.029 0.025 0.012 0.002 O47 0.036 0.026 0.021 0.011 0.007 0.004 C47 0.026 0.061 0.046 0.028 0.006 0.014 O48 0.033 0.023 0.019 0.005 0.001 -0.002 C48 0.041 0.049 0.045 0.030 -0.002 0.014 C49 0.064 0.022 0.031 0.015 0.009 0.007 C50 0.060 0.027 0.025 0.015 0.011 0.001 C51 0.045 0.031 0.022 0.004 0.016 -0.005 C52 0.023 0.043 0.024 0.002 0.008 -0.004 C53 0.041 0.023 0.034 -0.001 0.010 0.012 C54 0.048 0.014 0.029 0.004 0.004 0.006 C55 0.041 0.026 0.028 0.011 -0.002 -0.015 C56 0.027 0.047 0.028 0.018 -0.005 -0.011 C57 0.020 0.018 0.024 0.000 0.006 0.003 C58 0.023 0.015 0.021 0.004 0.004 0.004 C59 0.018 0.021 0.027 0.006 0.004 -0.005 C60 0.016 0.029 0.022 0.005 0.001 -0.001 C61 0.022 0.035 0.025 0.012 0.004 0.013 C62 0.033 0.030 0.026 0.015 0.001 0.012 C63 0.042 0.021 0.028 0.013 0.001 0.002 C64 0.041 0.027 0.023 0.015 0.002 0.000 C65 0.029 0.025 0.018 0.005 0.007 -0.005 C66 0.016 0.029 0.021 0.003 0.005 -0.006 C67 0.028 0.043 0.029 0.018 -0.005 0.005 C68 0.027 0.042 0.038 0.021 0.007 0.013 C69 0.040 0.031 0.027 0.018 0.010 0.012 C70 0.045 0.021 0.033 0.013 0.015 0.003 C71 0.026 0.033 0.024 0.011 0.011 0.003 C72 0.024 0.035 0.026 0.011 0.007 0.010 C73 0.039 0.024 0.027 0.008 0.010 0.015 C74 0.049 0.019 0.021 0.005 0.005 0.004 C75 0.031 0.031 0.028 0.008 0.001 -0.013 C76 0.028 0.035 0.027 0.005 -0.002 -0.009 C77 0.026 0.017 0.029 0.000 0.005 0.003 C78 0.030 0.016 0.025 0.006 0.006 0.002 C79 0.021 0.026 0.026 0.003 0.005 -0.007 C80 0.018 0.042 0.019 0.008 0.000 -0.003 C81 0.025 0.038 0.041 0.022 0.011 0.013 C82 0.028 0.041 0.041 0.027 0.001 0.011 C83 0.037 0.017 0.025 0.011 0.006 0.005 C84 0.034 0.024 0.021 0.013 0.005 0.004 C85 0.025 0.027 0.018 0.005 0.008 -0.001 C86 0.017 0.024 0.024 0.004 0.005 -0.001 C87 0.033 0.058 0.029 0.012 -0.002 0.011 C88 0.028 0.068 0.039 0.033 0.009 0.024 C89 0.053 0.027 0.046 0.016 -0.002 0.005 C90 0.063 0.030 0.034 0.022 0.018 0.011 C91 0.035 0.039 0.033 0.020 0.006 -0.007 C92 0.031 0.041 0.025 0.016 0.012 0.003 C93 0.034 0.030 0.020 0.008 0.009 0.009 C94 0.045 0.023 0.020 0.006 0.007 0.008 C95 0.042 0.026 0.027 0.002 -0.002 -0.007 C96 0.031 0.036 0.033 0.003 0.001 -0.016 _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 O9 2.8014(15) . ? K1 O17 2.8023(14) . ? K1 O16 2.8093(13) . ? K1 O10 2.8291(15) . ? K1 O13 2.8366(13) . ? K1 O15 2.8595(14) . ? K1 O11 2.9458(14) . ? K1 O18 2.9817(13) . ? K1 O14 2.9892(14) . ? K1 O12 3.0241(14) . ? K1 C25 3.519(2) . ? K1 C32 3.529(2) . ? O1 C4 1.248(2) . ? N1 C4 1.351(2) . ? N1 H5N 0.92(2) . ? N1 H6N 0.89(2) . ? C1 C2 1.408(3) . ? C1 C3 1.412(3) . ? C1 C4 1.438(3) . ? K2 O27 2.7928(15) . ? K2 O26 2.8066(13) . ? K2 O19 2.8150(15) . ? K2 O23 2.8212(14) . ? K2 O20 2.8474(14) . ? K2 O25 2.8496(15) . ? K2 O21 2.9309(15) . ? K2 O24 2.9762(15) . ? K2 O28 3.0019(14) . ? K2 O22 3.0127(15) . ? K2 C45 3.499(2) . ? K2 C52 3.514(2) . ? O2 C8 1.260(2) . ? N2 C2 1.156(2) . ? K3 O29 2.8271(14) . ? K3 O37 2.8330(15) . ? K3 O32 2.8686(14) . ? K3 O38 2.8796(14) . ? K3 O34 2.8832(14) . ? K3 O35 2.8927(14) . ? K3 O33 2.9072(13) . ? K3 O30 2.9079(13) . ? K3 O31 2.9502(13) . ? K3 O36 2.9655(13) . ? K3 C58 3.502(2) . ? O3 C12 1.247(2) . ? N3 C3 1.150(2) . ? K4 O39 2.8360(14) . ? K4 O47 2.8417(15) . ? K4 O43 2.8478(13) . ? K4 O42 2.8543(14) . ? K4 O46 2.8558(13) . ? K4 O48 2.8755(14) . ? K4 O44 2.8976(15) . ? K4 O41 2.9331(14) . ? K4 O45 2.9634(16) . ? K4 O40 2.9968(13) . ? O4 C13 1.257(2) . ? N4 C8 1.338(2) . ? N4 H3N 0.85(2) . ? N4 H4N 0.90(2) . ? O5 H5O 0.79(3) . ? O5 H6O 0.92(2) . ? N5 C6 1.148(2) . ? C5 C6 1.410(2) . ? C5 C7 1.414(3) . ? C5 C8 1.441(3) . ? O6 H7O 1.14(4) . ? O6 H8O 0.79(3) . ? N6 C7 1.145(2) . ? O7 H1O 0.79(3) . ? O7 H2O 0.95(3) . ? N7 C12 1.355(2) . ? N7 H1N 0.92(2) . ? N7 H2N 0.94(2) . ? O8 H3O 1.05(4) . ? O8 H4O 0.85(3) . ? N8 C10 1.152(2) . ? O9 C26 1.418(2) . ? O9 C17 1.440(3) . ? N9 C11 1.149(2) . ? C9 C11 1.409(3) . ? C9 C10 1.413(2) . ? C9 C12 1.440(3) . ? O10 C18 1.415(3) . ? O10 C19 1.418(2) . ? N10 C13 1.343(2) . ? N10 H7N 0.91(2) . ? N10 H8N 0.85(2) . ? O11 C21 1.422(2) . ? O11 C20 1.422(2) . ? N11 C15 1.150(2) . ? O12 C23 1.416(2) . ? O12 C22 1.422(2) . ? N12 C16 1.148(2) . ? O13 C25 1.423(3) . ? O13 C24 1.430(2) . ? C13 C14 1.441(3) . ? O14 C36 1.421(2) . ? O14 C27 1.423(2) . ? C14 C15 1.407(2) . ? C14 C16 1.409(3) . ? O15 C28 1.421(2) . ? O15 C29 1.431(2) . ? O16 C30 1.419(2) . ? O16 C31 1.431(2) . ? O17 C33 1.425(2) . ? O17 C32 1.426(2) . ? C17 C18 1.468(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O18 C34 1.421(2) . ? O18 C35 1.425(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O19 C37 1.422(2) . ? O19 C46 1.428(2) . ? C19 C20 1.499(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? O20 C39 1.413(3) . ? O20 C38 1.416(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? O21 C40 1.416(3) . ? O21 C41 1.425(3) . ? C21 C22 1.492(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? O22 C42 1.415(3) . ? O22 C43 1.415(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? O23 C45 1.422(3) . ? O23 C44 1.426(3) . ? C23 C24 1.491(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O24 C47 1.420(3) . ? O24 C56 1.421(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O25 C48 1.417(3) . ? O25 C49 1.429(2) . ? C25 C26 1.499(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? O26 C51 1.426(3) . ? O26 C50 1.431(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? O27 C52 1.419(2) . ? O27 C53 1.426(2) . ? C27 C28 1.504(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? O28 C54 1.418(3) . ? O28 C55 1.421(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? O29 C57 1.426(2) . ? O29 C66 1.427(2) . ? C29 C30 1.499(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O30 C58 1.421(2) . ? O30 C59 1.427(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O31 C61 1.417(2) . ? O31 C60 1.431(2) . ? C31 C32 1.495(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? O32 C62 1.425(2) . ? O32 C63 1.427(2) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? O33 C64 1.419(2) . ? O33 C65 1.424(2) . ? C33 C34 1.495(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O34 C67 1.418(2) . ? O34 C76 1.419(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? O35 C69 1.415(2) . ? O35 C68 1.429(2) . ? C35 C36 1.496(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? O36 C70 1.418(2) . ? O36 C71 1.429(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O37 C72 1.415(2) . ? O37 C73 1.425(2) . ? C37 C38 1.503(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? O38 C74 1.410(2) . ? O38 C75 1.441(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? O39 C77 1.423(2) . ? O39 C86 1.433(2) . ? C39 C40 1.498(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? O40 C78 1.415(2) . ? O40 C79 1.432(2) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? O41 C81 1.416(2) . ? O41 C80 1.424(2) . ? C41 C42 1.489(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O42 C82 1.426(2) . ? O42 C83 1.429(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? O43 C85 1.420(2) . ? O43 C84 1.423(2) . ? C43 C44 1.485(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O44 C87 1.413(3) . ? O44 C96 1.430(3) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? O45 C89 1.381(3) . ? O45 C88 1.416(3) . ? C45 C46 1.489(3) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? O46 C91 1.416(3) . ? O46 C90 1.418(3) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? O47 C93 1.410(2) . ? O47 C92 1.430(2) . ? C47 C48 1.499(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? O48 C95 1.411(3) . ? O48 C94 1.432(3) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.490(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.497(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.489(3) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.488(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.494(3) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.490(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.498(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.500(3) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.501(3) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.491(3) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.496(3) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.485(3) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.490(3) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.485(3) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.495(3) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.486(3) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C82 1.505(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.498(3) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.497(3) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.493(3) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.506(3) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.496(3) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.498(3) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.492(3) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 H96A 0.9900 . ? C96 H96B 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 O9 K1 O17 158.48(4) . . ? O9 K1 O16 139.43(5) . . ? O17 K1 O16 61.69(4) . . ? O9 K1 O10 61.36(4) . . ? O17 K1 O10 130.73(4) . . ? O16 K1 O10 84.83(4) . . ? O9 K1 O13 61.46(4) . . ? O17 K1 O13 98.06(4) . . ? O16 K1 O13 158.55(4) . . ? O10 K1 O13 115.62(4) . . ? O9 K1 O15 83.09(4) . . ? O17 K1 O15 117.70(4) . . ? O16 K1 O15 61.12(4) . . ? O10 K1 O15 64.27(4) . . ? O13 K1 O15 132.05(4) . . ? O9 K1 O11 106.33(4) . . ? O17 K1 O11 73.91(4) . . ? O16 K1 O11 71.00(4) . . ? O10 K1 O11 60.87(4) . . ? O13 K1 O11 112.09(4) . . ? O15 K1 O11 108.04(4) . . ? O9 K1 O18 119.47(4) . . ? O17 K1 O18 57.48(4) . . ? O16 K1 O18 83.49(4) . . ? O10 K1 O18 157.84(4) . . ? O13 K1 O18 79.08(4) . . ? O15 K1 O18 93.58(4) . . ? O11 K1 O18 131.34(4) . . ? O9 K1 O14 71.15(4) . . ? O17 K1 O14 113.32(4) . . ? O16 K1 O14 102.27(4) . . ? O10 K1 O14 108.16(4) . . ? O13 K1 O14 78.37(4) . . ? O15 K1 O14 59.21(4) . . ? O11 K1 O14 166.99(4) . . ? O18 K1 O14 56.53(4) . . ? O9 K1 O12 85.80(4) . . ? O17 K1 O12 76.61(4) . . ? O16 K1 O12 119.40(4) . . ? O10 K1 O12 92.28(4) . . ? O13 K1 O12 56.79(4) . . ? O15 K1 O12 156.55(4) . . ? O11 K1 O12 55.78(4) . . ? O18 K1 O12 109.86(4) . . ? O14 K1 O12 135.15(4) . . ? O9 K1 C25 42.20(5) . . ? O17 K1 C25 119.15(5) . . ? O16 K1 C25 165.38(5) . . ? O10 K1 C25 102.34(5) . . ? O13 K1 C25 22.79(5) . . ? O15 K1 C25 110.27(5) . . ? O11 K1 C25 123.61(4) . . ? O18 K1 C25 85.42(5) . . ? O14 K1 C25 63.51(4) . . ? O12 K1 C25 73.47(5) . . ? O9 K1 C32 167.07(5) . . ? O17 K1 C32 22.49(4) . . ? O16 K1 C32 42.07(4) . . ? O10 K1 C32 110.26(5) . . ? O13 K1 C32 119.33(5) . . ? O15 K1 C32 102.48(4) . . ? O11 K1 C32 60.93(4) . . ? O18 K1 C32 72.23(4) . . ? O14 K1 C32 121.75(4) . . ? O12 K1 C32 84.72(4) . . ? C25 K1 C32 141.29(5) . . ? C4 N1 H5N 123.4(14) . . ? C4 N1 H6N 118.8(12) . . ? H5N N1 H6N 117.7(18) . . ? C2 C1 C3 118.68(18) . . ? C2 C1 C4 122.55(17) . . ? C3 C1 C4 118.76(16) . . ? O27 K2 O26 61.56(4) . . ? O27 K2 O19 160.58(4) . . ? O26 K2 O19 136.83(5) . . ? O27 K2 O23 100.77(5) . . ? O26 K2 O23 160.59(5) . . ? O19 K2 O23 61.85(4) . . ? O27 K2 O20 127.70(4) . . ? O26 K2 O20 82.05(4) . . ? O19 K2 O20 61.29(4) . . ? O23 K2 O20 116.83(4) . . ? O27 K2 O25 117.47(4) . . ? O26 K2 O25 61.39(5) . . ? O19 K2 O25 81.70(4) . . ? O23 K2 O25 128.88(5) . . ? O20 K2 O25 64.89(4) . . ? O27 K2 O21 73.09(4) . . ? O26 K2 O21 72.12(4) . . ? O19 K2 O21 104.25(4) . . ? O23 K2 O21 112.18(4) . . ? O20 K2 O21 60.06(5) . . ? O25 K2 O21 110.63(5) . . ? O27 K2 O24 112.92(4) . . ? O26 K2 O24 102.60(4) . . ? O19 K2 O24 73.05(4) . . ? O23 K2 O24 75.90(4) . . ? O20 K2 O24 110.66(5) . . ? O25 K2 O24 59.09(4) . . ? O21 K2 O24 169.45(5) . . ? O27 K2 O28 57.01(4) . . ? O26 K2 O28 83.02(4) . . ? O19 K2 O28 122.82(4) . . ? O23 K2 O28 80.15(4) . . ? O20 K2 O28 157.28(4) . . ? O25 K2 O28 92.87(4) . . ? O21 K2 O28 130.10(4) . . ? O24 K2 O28 56.48(4) . . ? O27 K2 O22 78.30(4) . . ? O26 K2 O22 121.68(5) . . ? O19 K2 O22 84.35(4) . . ? O23 K2 O22 56.64(4) . . ? O20 K2 O22 92.74(4) . . ? O25 K2 O22 157.35(4) . . ? O21 K2 O22 56.04(4) . . ? O24 K2 O22 132.54(4) . . ? O28 K2 O22 109.70(4) . . ? O27 K2 C45 122.30(5) . . ? O26 K2 C45 164.69(5) . . ? O19 K2 C45 42.49(5) . . ? O23 K2 C45 22.96(5) . . ? O20 K2 C45 102.90(5) . . ? O25 K2 C45 107.23(5) . . ? O21 K2 C45 122.98(5) . . ? O24 K2 C45 62.09(5) . . ? O28 K2 C45 87.62(5) . . ? O22 K2 C45 72.95(5) . . ? O27 K2 C52 22.50(5) . . ? O26 K2 C52 42.31(5) . . ? O19 K2 C52 164.42(5) . . ? O23 K2 C52 121.94(5) . . ? O20 K2 C52 106.86(5) . . ? O25 K2 C52 102.97(5) . . ? O21 K2 C52 60.17(4) . . ? O24 K2 C52 122.20(5) . . ? O28 K2 C52 72.18(4) . . ? O22 K2 C52 86.29(5) . . ? C45 K2 C52 144.32(6) . . ? N2 C2 C1 178.1(2) . . ? O29 K3 O37 154.38(4) . . ? O29 K3 O32 114.86(4) . . ? O37 K3 O32 83.44(4) . . ? O29 K3 O38 109.38(4) . . ? O37 K3 O38 58.26(4) . . ? O32 K3 O38 69.98(4) . . ? O29 K3 O34 68.54(4) . . ? O37 K3 O34 86.36(4) . . ? O32 K3 O34 125.45(4) . . ? O38 K3 O34 59.34(4) . . ? O29 K3 O35 70.58(4) . . ? O37 K3 O35 92.99(4) . . ? O32 K3 O35 172.80(4) . . ? O38 K3 O35 113.39(4) . . ? O34 K3 O35 60.28(4) . . ? O29 K3 O33 59.62(4) . . ? O37 K3 O33 124.67(4) . . ? O32 K3 O33 60.18(4) . . ? O38 K3 O33 70.13(4) . . ? O34 K3 O33 83.73(4) . . ? O35 K3 O33 126.68(4) . . ? O29 K3 O30 58.33(4) . . ? O37 K3 O30 142.24(4) . . ? O32 K3 O30 93.43(4) . . ? O38 K3 O30 153.83(4) . . ? O34 K3 O30 124.06(4) . . ? O35 K3 O30 85.54(4) . . ? O33 K3 O30 84.15(4) . . ? O29 K3 O31 115.27(4) . . ? O37 K3 O31 89.29(4) . . ? O32 K3 O31 58.44(4) . . ? O38 K3 O31 121.75(4) . . ? O34 K3 O31 173.65(4) . . ? O35 K3 O31 115.42(4) . . ? O33 K3 O31 102.56(4) . . ? O30 K3 O31 58.22(4) . . ? O29 K3 O36 121.93(4) . . ? O37 K3 O36 57.98(4) . . ? O32 K3 O36 114.53(4) . . ? O38 K3 O36 114.71(4) . . ? O34 K3 O36 104.24(4) . . ? O35 K3 O36 58.40(4) . . ? O33 K3 O36 171.95(4) . . ? O30 K3 O36 90.33(4) . . ? O31 K3 O36 69.49(4) . . ? O29 K3 C58 42.15(4) . . ? O37 K3 C58 147.63(4) . . ? O32 K3 C58 114.76(4) . . ? O38 K3 C58 151.38(4) . . ? O34 K3 C58 101.78(4) . . ? O35 K3 C58 65.62(4) . . ? O33 K3 C58 87.56(4) . . ? O30 K3 C58 23.34(4) . . ? O31 K3 C58 79.56(4) . . ? O36 K3 C58 89.69(4) . . ? N3 C3 C1 179.0(2) . . ? O39 K4 O47 160.94(4) . . ? O39 K4 O43 61.27(4) . . ? O47 K4 O43 135.18(4) . . ? O39 K4 O42 118.10(4) . . ? O47 K4 O42 80.93(4) . . ? O43 K4 O42 61.19(4) . . ? O39 K4 O46 104.53(4) . . ? O47 K4 O46 60.96(4) . . ? O43 K4 O46 162.44(4) . . ? O42 K4 O46 125.64(5) . . ? O39 K4 O48 123.49(4) . . ? O47 K4 O48 61.39(4) . . ? O43 K4 O48 80.45(4) . . ? O42 K4 O48 65.27(4) . . ? O46 K4 O48 117.04(4) . . ? O39 K4 O44 70.08(4) . . ? O47 K4 O44 102.93(4) . . ? O43 K4 O44 73.46(4) . . ? O42 K4 O44 112.26(4) . . ? O46 K4 O44 112.98(4) . . ? O48 K4 O44 59.59(4) . . ? O39 K4 O41 114.02(4) . . ? O47 K4 O41 75.53(4) . . ? O43 K4 O41 101.46(4) . . ? O42 K4 O41 59.16(4) . . ? O46 K4 O41 73.95(4) . . ? O48 K4 O41 113.10(4) . . ? O44 K4 O41 171.36(4) . . ? O39 K4 O45 77.71(4) . . ? O47 K4 O45 83.68(4) . . ? O43 K4 O45 123.79(4) . . ? O42 K4 O45 158.20(4) . . ? O46 K4 O45 57.12(4) . . ? O48 K4 O45 93.77(4) . . ? O44 K4 O45 56.61(4) . . ? O41 K4 O45 130.91(4) . . ? O39 K4 O40 56.97(4) . . ? O47 K4 O40 127.11(4) . . ? O43 K4 O40 81.04(4) . . ? O42 K4 O40 93.47(4) . . ? O46 K4 O40 82.32(4) . . ? O48 K4 O40 156.80(4) . . ? O44 K4 O40 127.05(4) . . ? O41 K4 O40 57.57(4) . . ? O45 K4 O40 108.14(4) . . ? C8 N4 H3N 120.6(15) . . ? C8 N4 H4N 118.5(13) . . ? H3N N4 H4N 120.0(19) . . ? O1 C4 N1 120.82(18) . . ? O1 C4 C1 121.03(17) . . ? N1 C4 C1 118.15(17) . . ? H5O O5 H6O 108(2) . . ? C6 C5 C7 118.08(18) . . ? C6 C5 C8 123.42(17) . . ? C7 C5 C8 118.49(16) . . ? H7O O6 H8O 104(3) . . ? N5 C6 C5 179.3(2) . . ? H1O O7 H2O 109(2) . . ? C12 N7 H1N 112.6(14) . . ? C12 N7 H2N 119.9(14) . . ? H1N N7 H2N 119.5(19) . . ? N6 C7 C5 179.7(2) . . ? H3O O8 H4O 105(2) . . ? O2 C8 N4 120.18(18) . . ? O2 C8 C5 120.47(17) . . ? N4 C8 C5 119.34(16) . . ? C26 O9 C17 110.81(16) . . ? C26 O9 K1 117.76(13) . . ? C17 O9 K1 115.39(12) . . ? C11 C9 C10 119.33(18) . . ? C11 C9 C12 118.78(16) . . ? C10 C9 C12 121.89(17) . . ? C18 O10 C19 114.83(16) . . ? C18 O10 K1 111.02(12) . . ? C19 O10 K1 114.58(12) . . ? C13 N10 H7N 117.9(13) . . ? C13 N10 H8N 117.7(14) . . ? H7N N10 H8N 124.2(19) . . ? N8 C10 C9 178.0(2) . . ? C21 O11 C20 113.02(15) . . ? C21 O11 K1 120.98(11) . . ? C20 O11 K1 107.45(11) . . ? N9 C11 C9 179.1(2) . . ? C23 O12 C22 113.02(17) . . ? C23 O12 K1 107.14(11) . . ? C22 O12 K1 109.24(11) . . ? O3 C12 N7 121.02(18) . . ? O3 C12 C9 121.01(17) . . ? N7 C12 C9 117.95(16) . . ? C25 O13 C24 113.71(15) . . ? C25 O13 K1 106.67(12) . . ? C24 O13 K1 122.30(11) . . ? O4 C13 N10 120.23(18) . . ? O4 C13 C14 120.23(17) . . ? N10 C13 C14 119.53(16) . . ? C36 O14 C27 113.19(15) . . ? C36 O14 K1 117.76(12) . . ? C27 O14 K1 110.08(11) . . ? C15 C14 C16 119.04(18) . . ? C15 C14 C13 123.31(17) . . ? C16 C14 C13 117.64(16) . . ? C28 O15 C29 113.26(14) . . ? C28 O15 K1 117.12(11) . . ? C29 O15 K1 109.93(11) . . ? N11 C15 C14 179.7(2) . . ? C30 O16 C31 112.46(14) . . ? C30 O16 K1 117.25(11) . . ? C31 O16 K1 116.46(10) . . ? N12 C16 C14 178.9(2) . . ? C33 O17 C32 113.28(14) . . ? C33 O17 K1 121.67(11) . . ? C32 O17 K1 108.74(11) . . ? O9 C17 C18 109.08(18) . . ? O9 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? O9 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C34 O18 C35 112.57(15) . . ? C34 O18 K1 102.93(10) . . ? C35 O18 K1 109.05(11) . . ? O10 C18 C17 113.5(2) . . ? O10 C18 H18A 108.9 . . ? C17 C18 H18A 108.9 . . ? O10 C18 H18B 108.9 . . ? C17 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C37 O19 C46 112.22(15) . . ? C37 O19 K2 115.71(12) . . ? C46 O19 K2 116.17(13) . . ? O10 C19 C20 107.01(16) . . ? O10 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O10 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? C39 O20 C38 114.10(16) . . ? C39 O20 K2 116.01(13) . . ? C38 O20 K2 110.44(12) . . ? O11 C20 C19 112.99(16) . . ? O11 C20 H20A 109.0 . . ? C19 C20 H20A 109.0 . . ? O11 C20 H20B 109.0 . . ? C19 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C40 O21 C41 112.61(17) . . ? C40 O21 K2 109.33(13) . . ? C41 O21 K2 120.63(13) . . ? O11 C21 C22 108.70(16) . . ? O11 C21 H21A 109.9 . . ? C22 C21 H21A 109.9 . . ? O11 C21 H21B 109.9 . . ? C22 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? C42 O22 C43 112.86(19) . . ? C42 O22 K2 109.60(12) . . ? C43 O22 K2 106.93(12) . . ? O12 C22 C21 107.89(17) . . ? O12 C22 H22A 110.1 . . ? C21 C22 H22A 110.1 . . ? O12 C22 H22B 110.1 . . ? C21 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C45 O23 C44 113.61(16) . . ? C45 O23 K2 106.37(12) . . ? C44 O23 K2 122.90(13) . . ? O12 C23 C24 107.96(18) . . ? O12 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? O12 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? C47 O24 C56 113.60(17) . . ? C47 O24 K2 109.66(12) . . ? C56 O24 K2 117.98(13) . . ? O13 C24 C23 108.85(16) . . ? O13 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O13 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C48 O25 C49 112.96(16) . . ? C48 O25 K2 118.20(12) . . ? C49 O25 K2 110.27(13) . . ? O13 C25 C26 113.47(17) . . ? O13 C25 K1 50.54(9) . . ? C26 C25 K1 84.13(11) . . ? O13 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? K1 C25 H25A 159.4 . . ? O13 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? K1 C25 H25B 81.8 . . ? H25A C25 H25B 107.7 . . ? C51 O26 C50 112.48(15) . . ? C51 O26 K2 116.68(12) . . ? C50 O26 K2 115.88(12) . . ? O9 C26 C25 108.79(16) . . ? O9 C26 H26A 109.9 . . ? C25 C26 H26A 109.9 . . ? O9 C26 H26B 109.9 . . ? C25 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? C52 O27 C53 112.99(16) . . ? C52 O27 K2 108.66(12) . . ? C53 O27 K2 122.58(12) . . ? O14 C27 C28 112.38(17) . . ? O14 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? O14 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C54 O28 C55 112.90(16) . . ? C54 O28 K2 103.77(11) . . ? C55 O28 K2 109.06(12) . . ? O15 C28 C27 107.87(16) . . ? O15 C28 H28A 110.1 . . ? C27 C28 H28A 110.1 . . ? O15 C28 H28B 110.1 . . ? C27 C28 H28B 110.1 . . ? H28A C28 H28B 108.4 . . ? C57 O29 C66 113.62(14) . . ? C57 O29 K3 119.00(10) . . ? C66 O29 K3 112.29(11) . . ? O15 C29 C30 112.97(16) . . ? O15 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? O15 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C58 O30 C59 112.57(14) . . ? C58 O30 K3 102.49(10) . . ? C59 O30 K3 105.97(11) . . ? O16 C30 C29 109.09(15) . . ? O16 C30 H30A 109.9 . . ? C29 C30 H30A 109.9 . . ? O16 C30 H30B 109.9 . . ? C29 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? C61 O31 C60 112.97(15) . . ? C61 O31 K3 113.89(11) . . ? C60 O31 K3 115.74(11) . . ? O16 C31 C32 108.32(15) . . ? O16 C31 H31A 110.0 . . ? C32 C31 H31A 110.0 . . ? O16 C31 H31B 110.0 . . ? C32 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? C62 O32 C63 112.99(14) . . ? C62 O32 K3 116.83(11) . . ? C63 O32 K3 110.94(12) . . ? O17 C32 C31 112.97(16) . . ? O17 C32 K1 48.76(9) . . ? C31 C32 K1 83.67(11) . . ? O17 C32 H32A 109.0 . . ? C31 C32 H32A 109.0 . . ? K1 C32 H32A 157.7 . . ? O17 C32 H32B 109.0 . . ? C31 C32 H32B 109.0 . . ? K1 C32 H32B 84.0 . . ? H32A C32 H32B 107.8 . . ? C64 O33 C65 112.16(14) . . ? C64 O33 K3 115.91(11) . . ? C65 O33 K3 116.55(10) . . ? O17 C33 C34 108.38(16) . . ? O17 C33 H33A 110.0 . . ? C34 C33 H33A 110.0 . . ? O17 C33 H33B 110.0 . . ? C34 C33 H33B 110.0 . . ? H33A C33 H33B 108.4 . . ? C67 O34 C76 111.38(15) . . ? C67 O34 K3 116.34(11) . . ? C76 O34 K3 119.19(13) . . ? O18 C34 C33 107.71(16) . . ? O18 C34 H34A 110.2 . . ? C33 C34 H34A 110.2 . . ? O18 C34 H34B 110.2 . . ? C33 C34 H34B 110.2 . . ? H34A C34 H34B 108.5 . . ? C69 O35 C68 113.70(15) . . ? C69 O35 K3 115.96(12) . . ? C68 O35 K3 110.35(11) . . ? O18 C35 C36 107.54(15) . . ? O18 C35 H35A 110.2 . . ? C36 C35 H35A 110.2 . . ? O18 C35 H35B 110.2 . . ? C36 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? C70 O36 C71 112.44(15) . . ? C70 O36 K3 113.41(11) . . ? C71 O36 K3 114.80(11) . . ? O14 C36 C35 107.77(16) . . ? O14 C36 H36A 110.2 . . ? C35 C36 H36A 110.2 . . ? O14 C36 H36B 110.2 . . ? C35 C36 H36B 110.2 . . ? H36A C36 H36B 108.5 . . ? C72 O37 C73 114.50(16) . . ? C72 O37 K3 109.16(11) . . ? C73 O37 K3 110.00(11) . . ? O19 C37 C38 108.17(16) . . ? O19 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O19 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? C74 O38 C75 113.86(15) . . ? C74 O38 K3 117.34(11) . . ? C75 O38 K3 109.42(12) . . ? O20 C38 C37 113.11(18) . . ? O20 C38 H38A 109.0 . . ? C37 C38 H38A 109.0 . . ? O20 C38 H38B 109.0 . . ? C37 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C77 O39 C86 113.51(14) . . ? C77 O39 K4 121.01(11) . . ? C86 O39 K4 108.98(11) . . ? O20 C39 C40 107.41(17) . . ? O20 C39 H39A 110.2 . . ? C40 C39 H39A 110.2 . . ? O20 C39 H39B 110.2 . . ? C40 C39 H39B 110.2 . . ? H39A C39 H39B 108.5 . . ? C78 O40 C79 112.02(14) . . ? C78 O40 K4 101.56(10) . . ? C79 O40 K4 107.52(11) . . ? O21 C40 C39 112.94(17) . . ? O21 C40 H40A 109.0 . . ? C39 C40 H40A 109.0 . . ? O21 C40 H40B 109.0 . . ? C39 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? C81 O41 C80 113.92(16) . . ? C81 O41 K4 110.88(11) . . ? C80 O41 K4 117.57(12) . . ? O21 C41 C42 108.66(18) . . ? O21 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O21 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.3 . . ? C82 O42 C83 112.97(14) . . ? C82 O42 K4 118.83(11) . . ? C83 O42 K4 110.70(11) . . ? O22 C42 C41 108.0(2) . . ? O22 C42 H42A 110.1 . . ? C41 C42 H42A 110.1 . . ? O22 C42 H42B 110.1 . . ? C41 C42 H42B 110.1 . . ? H42A C42 H42B 108.4 . . ? C85 O43 C84 112.19(14) . . ? C85 O43 K4 115.61(10) . . ? C84 O43 K4 114.97(11) . . ? O22 C43 C44 108.00(19) . . ? O22 C43 H43A 110.1 . . ? C44 C43 H43A 110.1 . . ? O22 C43 H43B 110.1 . . ? C44 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? C87 O44 C96 113.09(16) . . ? C87 O44 K4 120.03(13) . . ? C96 O44 K4 110.64(13) . . ? O23 C44 C43 109.01(18) . . ? O23 C44 H44A 109.9 . . ? C43 C44 H44A 109.9 . . ? O23 C44 H44B 109.9 . . ? C43 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? C89 O45 C88 113.77(19) . . ? C89 O45 K4 107.82(13) . . ? C88 O45 K4 109.24(12) . . ? O23 C45 C46 113.47(18) . . ? O23 C45 K2 50.67(8) . . ? C46 C45 K2 84.76(11) . . ? O23 C45 H45A 108.9 . . ? C46 C45 H45A 108.9 . . ? K2 C45 H45A 159.4 . . ? O23 C45 H45B 108.9 . . ? C46 C45 H45B 108.9 . . ? K2 C45 H45B 81.0 . . ? H45A C45 H45B 107.7 . . ? C91 O46 C90 113.32(16) . . ? C91 O46 K4 107.54(11) . . ? C90 O46 K4 121.30(13) . . ? O19 C46 C45 109.00(16) . . ? O19 C46 H46A 109.9 . . ? C45 C46 H46A 109.9 . . ? O19 C46 H46B 109.9 . . ? C45 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? C93 O47 C92 112.04(14) . . ? C93 O47 K4 114.88(11) . . ? C92 O47 K4 116.77(12) . . ? O24 C47 C48 112.5(2) . . ? O24 C47 H47A 109.1 . . ? C48 C47 H47A 109.1 . . ? O24 C47 H47B 109.1 . . ? C48 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C95 O48 C94 113.76(16) . . ? C95 O48 K4 116.63(13) . . ? C94 O48 K4 109.54(11) . . ? O25 C48 C47 107.63(18) . . ? O25 C48 H48A 110.2 . . ? C47 C48 H48A 110.2 . . ? O25 C48 H48B 110.2 . . ? C47 C48 H48B 110.2 . . ? H48A C48 H48B 108.5 . . ? O25 C49 C50 112.87(17) . . ? O25 C49 H49A 109.0 . . ? C50 C49 H49A 109.0 . . ? O25 C49 H49B 109.0 . . ? C50 C49 H49B 109.0 . . ? H49A C49 H49B 107.8 . . ? O26 C50 C49 108.73(16) . . ? O26 C50 H50A 109.9 . . ? C49 C50 H50A 109.9 . . ? O26 C50 H50B 109.9 . . ? C49 C50 H50B 109.9 . . ? H50A C50 H50B 108.3 . . ? O26 C51 C52 108.63(16) . . ? O26 C51 H51A 110.0 . . ? C52 C51 H51A 110.0 . . ? O26 C51 H51B 110.0 . . ? C52 C51 H51B 110.0 . . ? H51A C51 H51B 108.3 . . ? O27 C52 C51 112.64(18) . . ? O27 C52 K2 48.84(9) . . ? C51 C52 K2 84.06(12) . . ? O27 C52 H52A 109.1 . . ? C51 C52 H52A 109.1 . . ? K2 C52 H52A 157.9 . . ? O27 C52 H52B 109.1 . . ? C51 C52 H52B 109.1 . . ? K2 C52 H52B 83.2 . . ? H52A C52 H52B 107.8 . . ? O27 C53 C54 108.58(18) . . ? O27 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? O27 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? O28 C54 C53 107.39(17) . . ? O28 C54 H54A 110.2 . . ? C53 C54 H54A 110.2 . . ? O28 C54 H54B 110.2 . . ? C53 C54 H54B 110.2 . . ? H54A C54 H54B 108.5 . . ? O28 C55 C56 107.67(16) . . ? O28 C55 H55A 110.2 . . ? C56 C55 H55A 110.2 . . ? O28 C55 H55B 110.2 . . ? C56 C55 H55B 110.2 . . ? H55A C55 H55B 108.5 . . ? O24 C56 C55 108.27(17) . . ? O24 C56 H56A 110.0 . . ? C55 C56 H56A 110.0 . . ? O24 C56 H56B 110.0 . . ? C55 C56 H56B 110.0 . . ? H56A C56 H56B 108.4 . . ? O29 C57 C58 107.91(15) . . ? O29 C57 H57A 110.1 . . ? C58 C57 H57A 110.1 . . ? O29 C57 H57B 110.1 . . ? C58 C57 H57B 110.1 . . ? H57A C57 H57B 108.4 . . ? O30 C58 C57 107.74(15) . . ? O30 C58 K3 54.18(8) . . ? C57 C58 K3 86.94(11) . . ? O30 C58 H58A 110.2 . . ? C57 C58 H58A 110.2 . . ? K3 C58 H58A 71.9 . . ? O30 C58 H58B 110.2 . . ? C57 C58 H58B 110.2 . . ? K3 C58 H58B 160.8 . . ? H58A C58 H58B 108.5 . . ? O30 C59 C60 107.94(15) . . ? O30 C59 H59A 110.1 . . ? C60 C59 H59A 110.1 . . ? O30 C59 H59B 110.1 . . ? C60 C59 H59B 110.1 . . ? H59A C59 H59B 108.4 . . ? O31 C60 C59 108.64(16) . . ? O31 C60 H60A 110.0 . . ? C59 C60 H60A 110.0 . . ? O31 C60 H60B 110.0 . . ? C59 C60 H60B 110.0 . . ? H60A C60 H60B 108.3 . . ? O31 C61 C62 111.56(17) . . ? O31 C61 H61A 109.3 . . ? C62 C61 H61A 109.3 . . ? O31 C61 H61B 109.3 . . ? C62 C61 H61B 109.3 . . ? H61A C61 H61B 108.0 . . ? O32 C62 C61 108.01(15) . . ? O32 C62 H62A 110.1 . . ? C61 C62 H62A 110.1 . . ? O32 C62 H62B 110.1 . . ? C61 C62 H62B 110.1 . . ? H62A C62 H62B 108.4 . . ? O32 C63 C64 113.53(17) . . ? O32 C63 H63A 108.9 . . ? C64 C63 H63A 108.9 . . ? O32 C63 H63B 108.9 . . ? C64 C63 H63B 108.9 . . ? H63A C63 H63B 107.7 . . ? O33 C64 C63 108.57(15) . . ? O33 C64 H64A 110.0 . . ? C63 C64 H64A 110.0 . . ? O33 C64 H64B 110.0 . . ? C63 C64 H64B 110.0 . . ? H64A C64 H64B 108.4 . . ? O33 C65 C66 108.33(15) . . ? O33 C65 H65A 110.0 . . ? C66 C65 H65A 110.0 . . ? O33 C65 H65B 110.0 . . ? C66 C65 H65B 110.0 . . ? H65A C65 H65B 108.4 . . ? O29 C66 C65 111.80(16) . . ? O29 C66 H66A 109.3 . . ? C65 C66 H66A 109.3 . . ? O29 C66 H66B 109.3 . . ? C65 C66 H66B 109.3 . . ? H66A C66 H66B 107.9 . . ? O34 C67 C68 109.12(16) . . ? O34 C67 H67A 109.9 . . ? C68 C67 H67A 109.9 . . ? O34 C67 H67B 109.9 . . ? C68 C67 H67B 109.9 . . ? H67A C67 H67B 108.3 . . ? O35 C68 C67 113.80(19) . . ? O35 C68 H68A 108.8 . . ? C67 C68 H68A 108.8 . . ? O35 C68 H68B 108.8 . . ? C67 C68 H68B 108.8 . . ? H68A C68 H68B 107.7 . . ? O35 C69 C70 107.78(16) . . ? O35 C69 H69A 110.1 . . ? C70 C69 H69A 110.1 . . ? O35 C69 H69B 110.1 . . ? C70 C69 H69B 110.1 . . ? H69A C69 H69B 108.5 . . ? O36 C70 C69 112.83(16) . . ? O36 C70 H70A 109.0 . . ? C69 C70 H70A 109.0 . . ? O36 C70 H70B 109.0 . . ? C69 C70 H70B 109.0 . . ? H70A C70 H70B 107.8 . . ? O36 C71 C72 109.33(16) . . ? O36 C71 H71A 109.8 . . ? C72 C71 H71A 109.8 . . ? O36 C71 H71B 109.8 . . ? C72 C71 H71B 109.8 . . ? H71A C71 H71B 108.3 . . ? O37 C72 C71 107.66(17) . . ? O37 C72 H72A 110.2 . . ? C71 C72 H72A 110.2 . . ? O37 C72 H72B 110.2 . . ? C71 C72 H72B 110.2 . . ? H72A C72 H72B 108.5 . . ? O37 C73 C74 107.00(17) . . ? O37 C73 H73A 110.3 . . ? C74 C73 H73A 110.3 . . ? O37 C73 H73B 110.3 . . ? C74 C73 H73B 110.3 . . ? H73A C73 H73B 108.6 . . ? O38 C74 C73 108.02(16) . . ? O38 C74 H74A 110.1 . . ? C73 C74 H74A 110.1 . . ? O38 C74 H74B 110.1 . . ? C73 C74 H74B 110.1 . . ? H74A C74 H74B 108.4 . . ? O38 C75 C76 113.28(16) . . ? O38 C75 H75A 108.9 . . ? C76 C75 H75A 108.9 . . ? O38 C75 H75B 108.9 . . ? C76 C75 H75B 108.9 . . ? H75A C75 H75B 107.7 . . ? O34 C76 C75 109.31(16) . . ? O34 C76 H76A 109.8 . . ? C75 C76 H76A 109.8 . . ? O34 C76 H76B 109.8 . . ? C75 C76 H76B 109.8 . . ? H76A C76 H76B 108.3 . . ? O39 C77 C78 108.71(16) . . ? O39 C77 H77A 109.9 . . ? C78 C77 H77A 109.9 . . ? O39 C77 H77B 109.9 . . ? C78 C77 H77B 109.9 . . ? H77A C77 H77B 108.3 . . ? O40 C78 C77 108.10(15) . . ? O40 C78 H78A 110.1 . . ? C77 C78 H78A 110.1 . . ? O40 C78 H78B 110.1 . . ? C77 C78 H78B 110.1 . . ? H78A C78 H78B 108.4 . . ? O40 C79 C80 108.00(16) . . ? O40 C79 H79A 110.1 . . ? C80 C79 H79A 110.1 . . ? O40 C79 H79B 110.1 . . ? C80 C79 H79B 110.1 . . ? H79A C79 H79B 108.4 . . ? O41 C80 C79 108.31(16) . . ? O41 C80 H80A 110.0 . . ? C79 C80 H80A 110.0 . . ? O41 C80 H80B 110.0 . . ? C79 C80 H80B 110.0 . . ? H80A C80 H80B 108.4 . . ? O41 C81 C82 112.42(18) . . ? O41 C81 H81A 109.1 . . ? C82 C81 H81A 109.1 . . ? O41 C81 H81B 109.1 . . ? C82 C81 H81B 109.1 . . ? H81A C81 H81B 107.9 . . ? O42 C82 C81 107.90(16) . . ? O42 C82 H82A 110.1 . . ? C81 C82 H82A 110.1 . . ? O42 C82 H82B 110.1 . . ? C81 C82 H82B 110.1 . . ? H82A C82 H82B 108.4 . . ? O42 C83 C84 113.12(16) . . ? O42 C83 H83A 109.0 . . ? C84 C83 H83A 109.0 . . ? O42 C83 H83B 109.0 . . ? C84 C83 H83B 109.0 . . ? H83A C83 H83B 107.8 . . ? O43 C84 C83 108.67(15) . . ? O43 C84 H84A 110.0 . . ? C83 C84 H84A 110.0 . . ? O43 C84 H84B 110.0 . . ? C83 C84 H84B 110.0 . . ? H84A C84 H84B 108.3 . . ? O43 C85 C86 108.83(15) . . ? O43 C85 H85A 109.9 . . ? C86 C85 H85A 109.9 . . ? O43 C85 H85B 109.9 . . ? C86 C85 H85B 109.9 . . ? H85A C85 H85B 108.3 . . ? O39 C86 C85 112.39(16) . . ? O39 C86 H86A 109.1 . . ? C85 C86 H86A 109.1 . . ? O39 C86 H86B 109.1 . . ? C85 C86 H86B 109.1 . . ? H86A C86 H86B 107.9 . . ? O44 C87 C88 107.78(17) . . ? O44 C87 H87A 110.2 . . ? C88 C87 H87A 110.2 . . ? O44 C87 H87B 110.2 . . ? C88 C87 H87B 110.2 . . ? H87A C87 H87B 108.5 . . ? O45 C88 C87 107.0(2) . . ? O45 C88 H88A 110.3 . . ? C87 C88 H88A 110.3 . . ? O45 C88 H88B 110.3 . . ? C87 C88 H88B 110.3 . . ? H88A C88 H88B 108.6 . . ? O45 C89 C90 109.7(2) . . ? O45 C89 H89A 109.7 . . ? C90 C89 H89A 109.7 . . ? O45 C89 H89B 109.7 . . ? C90 C89 H89B 109.7 . . ? H89A C89 H89B 108.2 . . ? O46 C90 C89 108.94(17) . . ? O46 C90 H90A 109.9 . . ? C89 C90 H90A 109.9 . . ? O46 C90 H90B 109.9 . . ? C89 C90 H90B 109.9 . . ? H90A C90 H90B 108.3 . . ? O46 C91 C92 113.22(18) . . ? O46 C91 H91A 108.9 . . ? C92 C91 H91A 108.9 . . ? O46 C91 H91B 108.9 . . ? C92 C91 H91B 108.9 . . ? H91A C91 H91B 107.7 . . ? O47 C92 C91 108.59(16) . . ? O47 C92 H92A 110.0 . . ? C91 C92 H92A 110.0 . . ? O47 C92 H92B 110.0 . . ? C91 C92 H92B 110.0 . . ? H92A C92 H92B 108.4 . . ? O47 C93 C94 108.99(15) . . ? O47 C93 H93A 109.9 . . ? C94 C93 H93A 109.9 . . ? O47 C93 H93B 109.9 . . ? C94 C93 H93B 109.9 . . ? H93A C93 H93B 108.3 . . ? O48 C94 C93 113.56(18) . . ? O48 C94 H94A 108.9 . . ? C93 C94 H94A 108.9 . . ? O48 C94 H94B 108.9 . . ? C93 C94 H94B 108.9 . . ? H94A C94 H94B 107.7 . . ? O48 C95 C96 107.24(17) . . ? O48 C95 H95A 110.3 . . ? C96 C95 H95A 110.3 . . ? O48 C95 H95B 110.3 . . ? C96 C95 H95B 110.3 . . ? H95A C95 H95B 108.5 . . ? O44 C96 C95 112.52(17) . . ? O44 C96 H96A 109.1 . . ? C95 C96 H96A 109.1 . . ? O44 C96 H96B 109.1 . . ? C95 C96 H96B 109.1 . . ? H96A C96 H96B 107.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H5N N5 0.92(2) 2.34(2) 3.190(2) 154.5(18) . N1 H6N O4 0.89(2) 1.99(2) 2.884(2) 175.4(17) 1_545 N4 H3N N2 0.85(2) 2.28(2) 3.060(2) 154(2) . N4 H4N O3 0.90(2) 1.99(2) 2.887(2) 177.5(19) . N7 H2N N11 0.94(2) 2.34(2) 3.187(2) 149.9(19) . N7 H1N O2 0.92(2) 1.97(2) 2.889(2) 176(2) . N10 H8N N8 0.85(2) 2.33(2) 3.093(2) 150.0(19) . N10 H7N O1 0.91(2) 1.96(2) 2.870(2) 177.8(18) 1_565 O5 H5O N11 0.79(3) 2.28(3) 3.069(2) 175(3) . O5 H6O O2 0.92(2) 1.87(2) 2.778(2) 170(2) . O6 H8O N6 0.79(3) 2.27(3) 3.040(2) 164(3) . O6 H7O O5 1.14(4) 1.73(4) 2.822(2) 160(3) . O7 H1O N5 0.79(3) 2.29(3) 3.082(2) 173(2) 1_565 O7 H2O O4 0.95(3) 1.86(3) 2.7928(19) 171(3) . O8 H4O N12 0.85(3) 2.17(3) 3.002(2) 163(3) . O8 H3O O7 1.05(4) 1.81(4) 2.835(2) 166(3) . _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.036 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.053 # Attachment '4.CIF' data_KcdmH _database_code_depnum_ccdc_archive 'CCDC 669559' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [K(15c5)2](cdm)(cdmH) ; _chemical_name_common '[K(15c5)2](cdm)(cdmH)' _chemical_melting_point ? _chemical_formula_moiety 'C28 H45 K1 N6 O12' _chemical_formula_sum 'C28 H45 K1 N6 O12' _chemical_formula_weight 696.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Na Na 0.0362 0.0249 '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 10.4626(2) _cell_length_b 11.7836(3) _cell_length_c 14.8886(3) _cell_angle_alpha 106.085(2) _cell_angle_beta 90.672(1) _cell_angle_gamma 91.569(1) _cell_volume 1762.69(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 23796 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9580 _exptl_absorpt_correction_T_max 0.9621 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(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 'phi 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 23796 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7914 _reflns_number_gt 5598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.1046P)^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 7914 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1756 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.75122(5) 0.01467(4) 0.25215(3) 0.02052(15) Uani 1 1 d . . . O1 O 0.44015(15) 0.51021(14) 0.18399(10) 0.0240(4) Uani 1 1 d . . . N1 N 0.2749(2) 0.49078(18) 0.27584(13) 0.0242(4) Uani 1 1 d . . . C1 C 0.2340(2) 0.52120(17) 0.12674(13) 0.0176(4) Uani 1 1 d . . . H1N H 0.197(3) 0.510(2) 0.2908(17) 0.034(7) Uiso 1 1 d . . . H1O H 0.507(3) 0.516(3) 0.250(2) 0.077(11) Uiso 1 1 d . . . O2 O 0.57234(15) 0.52357(13) 0.32208(10) 0.0228(3) Uani 1 1 d . . . N2 N -0.00478(19) 0.47430(17) 0.13681(12) 0.0262(4) Uani 1 1 d . . . C2 C 0.1023(2) 0.49676(17) 0.13116(13) 0.0183(4) Uani 1 1 d . . . H2N H 0.320(3) 0.479(2) 0.3138(19) 0.031(7) Uiso 1 1 d . . . O3 O 0.57330(17) 0.15903(13) 0.37908(11) 0.0278(4) Uani 1 1 d . . . N3 N 0.3175(2) 0.57645(19) -0.01708(13) 0.0330(5) Uani 1 1 d . . . C3 C 0.2814(2) 0.55109(19) 0.04707(14) 0.0215(5) Uani 1 1 d . . . H3N H 0.686(3) 0.488(2) 0.1738(17) 0.025(6) Uiso 1 1 d . . . O4 O 0.55057(18) 0.13091(14) 0.18038(11) 0.0325(4) Uani 1 1 d . . . N4 N 0.7375(2) 0.50386(17) 0.22189(13) 0.0209(4) Uani 1 1 d . . . C4 C 0.3198(2) 0.50731(17) 0.19740(13) 0.0165(4) Uani 1 1 d . . . H4N H 0.811(3) 0.499(2) 0.2076(16) 0.018(6) Uiso 1 1 d . . . O5 O 0.78853(18) 0.07882(14) 0.08246(10) 0.0312(4) Uani 1 1 d . . . N5 N 0.6918(2) 0.58963(17) 0.55273(12) 0.0284(5) Uani 1 1 d . . . C5 C 0.7786(2) 0.55205(17) 0.38687(13) 0.0165(4) Uani 1 1 d . . . O6 O 0.98581(17) 0.14073(13) 0.22428(10) 0.0269(4) Uani 1 1 d . . . N6 N 1.0206(2) 0.55769(17) 0.36437(12) 0.0277(5) Uani 1 1 d . . . C6 C 0.7293(2) 0.57331(17) 0.47806(14) 0.0194(5) Uani 1 1 d . . . O7 O 0.82119(16) 0.24797(13) 0.36844(10) 0.0254(4) Uani 1 1 d . . . C7 C 0.9113(2) 0.55506(17) 0.37573(13) 0.0181(4) Uani 1 1 d . . . O8 O 0.51316(17) -0.11957(13) 0.26528(10) 0.0286(4) Uani 1 1 d . . . C8 C 0.6932(2) 0.52577(17) 0.30837(13) 0.0169(4) Uani 1 1 d . . . O9 O 0.66025(17) -0.16646(13) 0.09818(10) 0.0283(4) Uani 1 1 d . . . C9 C 0.4550(3) 0.1604(2) 0.32949(17) 0.0332(6) Uani 1 1 d . . . H9A H 0.3955 0.2090 0.3718 0.040 Uiso 1 1 calc R . . H9B H 0.4183 0.0807 0.3092 0.040 Uiso 1 1 calc R . . O10 O 0.92662(17) -0.16252(13) 0.15583(11) 0.0308(4) Uani 1 1 d . . . C10 C 0.4705(3) 0.2065(2) 0.24652(18) 0.0378(6) Uani 1 1 d . . . H10A H 0.3875 0.2101 0.2179 0.045 Uiso 1 1 calc R . . H10B H 0.5084 0.2858 0.2658 0.045 Uiso 1 1 calc R . . O11 O 0.96812(17) -0.05387(13) 0.35193(11) 0.0301(4) Uani 1 1 d . . . C11 C 0.5859(3) 0.1803(2) 0.10698(18) 0.0408(7) Uani 1 1 d . . . H11A H 0.6312 0.2555 0.1326 0.049 Uiso 1 1 calc R . . H11B H 0.5099 0.1939 0.0739 0.049 Uiso 1 1 calc R . . O12 O 0.72201(17) -0.13947(14) 0.37934(10) 0.0299(4) Uani 1 1 d . . . C12 C 0.6694(3) 0.0969(2) 0.04132(17) 0.0403(7) Uani 1 1 d . . . H12A H 0.6239 0.0214 0.0182 0.048 Uiso 1 1 calc R . . H12B H 0.6864 0.1272 -0.0118 0.048 Uiso 1 1 calc R . . C13 C 0.8846(3) 0.1675(2) 0.08390(16) 0.0366(7) Uani 1 1 d . . . H13A H 0.8561 0.2443 0.1195 0.044 Uiso 1 1 calc R . . H13B H 0.9018 0.1706 0.0207 0.044 Uiso 1 1 calc R . . C14 C 1.0028(3) 0.1364(2) 0.12831(16) 0.0347(6) Uani 1 1 d . . . H14A H 1.0269 0.0575 0.0942 0.042 Uiso 1 1 calc R . . H14B H 1.0721 0.1909 0.1239 0.042 Uiso 1 1 calc R . . C15 C 1.0097(3) 0.25638(19) 0.28534(15) 0.0287(5) Uani 1 1 d . . . H15A H 0.9695 0.3146 0.2603 0.034 Uiso 1 1 calc R . . H15B H 1.1010 0.2743 0.2914 0.034 Uiso 1 1 calc R . . C16 C 0.9558(2) 0.2599(2) 0.37914(15) 0.0257(5) Uani 1 1 d . . . H16A H 0.9886 0.1959 0.4011 0.031 Uiso 1 1 calc R . . H16B H 0.9798 0.3342 0.4244 0.031 Uiso 1 1 calc R . . C17 C 0.7564(2) 0.26768(19) 0.45488(14) 0.0271(5) Uani 1 1 d . . . H17A H 0.7874 0.3411 0.4983 0.032 Uiso 1 1 calc R . . H17B H 0.7716 0.2037 0.4826 0.032 Uiso 1 1 calc R . . C18 C 0.6169(2) 0.27363(18) 0.43507(15) 0.0277(5) Uani 1 1 d . . . H18A H 0.5706 0.2955 0.4931 0.033 Uiso 1 1 calc R . . H18B H 0.6025 0.3324 0.4018 0.033 Uiso 1 1 calc R . . C19 C 0.4683(2) -0.1842(2) 0.17471(15) 0.0297(5) Uani 1 1 d . . . H19A H 0.4327 -0.1300 0.1432 0.036 Uiso 1 1 calc R . . H19B H 0.4004 -0.2393 0.1806 0.036 Uiso 1 1 calc R . . C20 C 0.5725(3) -0.2516(2) 0.11618(16) 0.0313(6) Uani 1 1 d . . . H20A H 0.6152 -0.3003 0.1494 0.038 Uiso 1 1 calc R . . H20B H 0.5369 -0.3024 0.0580 0.038 Uiso 1 1 calc R . . C21 C 0.7625(3) -0.21662(19) 0.03875(15) 0.0300(6) Uani 1 1 d . . . H21A H 0.7980 -0.1574 0.0112 0.036 Uiso 1 1 calc R . . H21B H 0.7283 -0.2817 -0.0117 0.036 Uiso 1 1 calc R . . C22 C 0.8684(3) -0.2609(2) 0.08818(16) 0.0322(6) Uani 1 1 d . . . H22A H 0.8341 -0.3177 0.1186 0.039 Uiso 1 1 calc R . . H22B H 0.9312 -0.2996 0.0435 0.039 Uiso 1 1 calc R . . C23 C 1.0275(3) -0.1969(2) 0.20616(18) 0.0369(6) Uani 1 1 d . . . H23A H 1.0991 -0.2222 0.1654 0.044 Uiso 1 1 calc R . . H23B H 0.9987 -0.2626 0.2291 0.044 Uiso 1 1 calc R . . C24 C 1.0685(3) -0.0928(2) 0.28750(17) 0.0344(6) Uani 1 1 d . . . H24A H 1.1402 -0.1149 0.3202 0.041 Uiso 1 1 calc R . . H24B H 1.0972 -0.0279 0.2637 0.041 Uiso 1 1 calc R . . C25 C 0.9438(3) -0.1295(2) 0.40986(18) 0.0364(6) Uani 1 1 d . . . H25A H 1.0090 -0.1160 0.4588 0.044 Uiso 1 1 calc R . . H25B H 0.9461 -0.2114 0.3730 0.044 Uiso 1 1 calc R . . C26 C 0.8160(3) -0.1049(2) 0.45203(16) 0.0337(6) Uani 1 1 d . . . H26A H 0.8024 -0.1489 0.4976 0.040 Uiso 1 1 calc R . . H26B H 0.8103 -0.0213 0.4836 0.040 Uiso 1 1 calc R . . C27 C 0.5949(3) -0.1266(2) 0.41254(16) 0.0344(6) Uani 1 1 d . . . H27A H 0.5764 -0.0435 0.4364 0.041 Uiso 1 1 calc R . . H27B H 0.5842 -0.1638 0.4626 0.041 Uiso 1 1 calc R . . C28 C 0.5072(3) -0.1841(2) 0.33266(18) 0.0383(6) Uani 1 1 d . . . H28A H 0.5320 -0.2648 0.3047 0.046 Uiso 1 1 calc R . . H28B H 0.4204 -0.1861 0.3545 0.046 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 0.0229(3) 0.0183(2) 0.0200(2) 0.00513(17) -0.00204(19) -0.00199(19) O1 0.0118(9) 0.0396(9) 0.0210(8) 0.0094(6) -0.0016(6) -0.0018(7) N1 0.0129(11) 0.0429(12) 0.0214(10) 0.0163(8) -0.0027(8) 0.0023(9) C1 0.0121(12) 0.0229(10) 0.0173(10) 0.0052(8) -0.0018(8) -0.0035(8) O2 0.0107(9) 0.0368(9) 0.0239(8) 0.0136(6) -0.0005(6) -0.0023(7) N2 0.0157(12) 0.0384(11) 0.0245(10) 0.0092(8) -0.0035(8) -0.0026(9) C2 0.0194(13) 0.0194(10) 0.0151(10) 0.0034(7) -0.0027(8) 0.0003(9) O3 0.0265(10) 0.0213(8) 0.0342(9) 0.0055(6) 0.0000(7) 0.0007(7) N3 0.0235(13) 0.0558(13) 0.0217(10) 0.0155(9) -0.0061(8) -0.0115(10) C3 0.0148(12) 0.0282(11) 0.0210(11) 0.0068(8) -0.0078(8) -0.0070(9) O4 0.0362(12) 0.0273(8) 0.0365(9) 0.0134(7) -0.0075(8) 0.0006(8) N4 0.0118(11) 0.0330(10) 0.0173(9) 0.0064(7) -0.0028(8) -0.0015(8) C4 0.0106(11) 0.0192(10) 0.0195(10) 0.0049(7) -0.0008(8) 0.0001(8) O5 0.0396(12) 0.0305(9) 0.0245(8) 0.0109(6) -0.0085(7) -0.0124(8) N5 0.0288(13) 0.0368(11) 0.0206(10) 0.0092(8) 0.0008(8) 0.0077(9) C5 0.0132(12) 0.0192(10) 0.0167(9) 0.0046(7) -0.0015(8) -0.0014(8) O6 0.0317(11) 0.0241(8) 0.0236(8) 0.0049(6) 0.0017(7) -0.0048(7) N6 0.0185(12) 0.0370(11) 0.0233(10) 0.0014(8) -0.0033(8) -0.0019(9) C6 0.0176(13) 0.0199(10) 0.0209(11) 0.0058(8) -0.0049(9) 0.0025(9) O7 0.0229(10) 0.0316(8) 0.0191(7) 0.0034(6) -0.0033(6) -0.0018(7) C7 0.0202(13) 0.0178(10) 0.0144(9) 0.0017(7) -0.0032(8) -0.0008(9) O8 0.0301(11) 0.0282(8) 0.0285(8) 0.0101(6) -0.0035(7) -0.0044(7) C8 0.0147(12) 0.0179(10) 0.0197(10) 0.0082(8) -0.0013(8) -0.0016(8) O9 0.0342(11) 0.0209(8) 0.0271(8) 0.0032(6) -0.0010(7) -0.0071(7) C9 0.0236(15) 0.0274(12) 0.0447(14) 0.0032(10) -0.0005(11) 0.0018(10) O10 0.0311(11) 0.0235(8) 0.0340(9) 0.0017(6) -0.0010(7) 0.0008(7) C10 0.0327(17) 0.0283(13) 0.0508(16) 0.0081(11) -0.0113(12) 0.0069(12) O11 0.0300(11) 0.0269(8) 0.0347(9) 0.0109(7) -0.0049(7) -0.0010(7) C11 0.0436(19) 0.0411(15) 0.0446(15) 0.0247(12) -0.0165(13) -0.0039(13) O12 0.0298(11) 0.0357(9) 0.0244(8) 0.0097(7) -0.0068(7) -0.0054(8) C12 0.053(2) 0.0436(15) 0.0270(13) 0.0165(11) -0.0180(12) -0.0165(14) C13 0.053(2) 0.0359(13) 0.0225(12) 0.0121(10) -0.0025(11) -0.0175(13) C14 0.0382(18) 0.0373(13) 0.0252(12) 0.0038(10) 0.0081(11) -0.0101(12) C15 0.0286(15) 0.0273(12) 0.0284(12) 0.0059(9) -0.0029(10) -0.0085(10) C16 0.0258(15) 0.0259(11) 0.0246(11) 0.0066(9) -0.0069(9) -0.0070(10) C17 0.0358(16) 0.0238(11) 0.0206(11) 0.0046(8) -0.0010(10) 0.0006(10) C18 0.0320(16) 0.0195(11) 0.0285(12) 0.0017(9) 0.0026(10) 0.0002(10) C19 0.0246(15) 0.0316(12) 0.0315(12) 0.0074(10) -0.0087(10) -0.0052(11) C20 0.0318(16) 0.0260(12) 0.0328(12) 0.0041(9) -0.0061(10) -0.0090(11) C21 0.0403(17) 0.0230(11) 0.0233(11) 0.0010(9) 0.0039(10) -0.0030(11) C22 0.0356(17) 0.0234(11) 0.0322(12) -0.0013(9) 0.0074(11) -0.0030(11) C23 0.0324(17) 0.0311(13) 0.0447(15) 0.0059(11) 0.0011(12) 0.0086(12) C24 0.0274(16) 0.0327(13) 0.0436(14) 0.0117(11) -0.0049(11) 0.0003(11) C25 0.0412(18) 0.0304(13) 0.0422(14) 0.0192(11) -0.0173(12) -0.0037(12) C26 0.0385(17) 0.0383(13) 0.0262(12) 0.0134(10) -0.0084(11) -0.0074(12) C27 0.0328(16) 0.0461(15) 0.0285(12) 0.0182(11) 0.0017(11) -0.0060(12) C28 0.0301(17) 0.0478(15) 0.0440(15) 0.0260(12) -0.0041(12) -0.0109(13) _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 O9 2.8005(15) . ? K1 O5 2.8587(15) . ? K1 O7 2.8834(15) . ? K1 O4 2.8881(17) . ? K1 O10 2.8976(16) . ? K1 O3 2.8991(16) . ? K1 O6 2.9272(17) . ? K1 O11 2.9487(17) . ? K1 O8 2.9515(18) . ? K1 O12 2.9778(16) . ? O1 C4 1.278(3) . ? O1 H1O 1.19(3) . ? N1 C4 1.325(3) . ? N1 H1N 0.87(3) . ? N1 H2N 0.78(3) . ? C1 C2 1.406(3) . ? C1 C3 1.419(3) . ? C1 C4 1.422(3) . ? O2 C8 1.284(3) . ? O2 H1O 1.25(3) . ? N2 C2 1.153(3) . ? O3 C18 1.435(3) . ? O3 C9 1.437(3) . ? N3 C3 1.142(3) . ? O4 C11 1.421(3) . ? O4 C10 1.428(3) . ? N4 C8 1.332(3) . ? N4 H3N 0.86(3) . ? N4 H4N 0.80(3) . ? O5 C13 1.425(3) . ? O5 C12 1.429(3) . ? N5 C6 1.150(3) . ? C5 C7 1.401(3) . ? C5 C6 1.417(3) . ? C5 C8 1.421(3) . ? O6 C15 1.427(3) . ? O6 C14 1.429(3) . ? N6 C7 1.158(3) . ? O7 C16 1.414(3) . ? O7 C17 1.426(3) . ? O8 C28 1.418(3) . ? O8 C19 1.420(3) . ? O9 C20 1.424(3) . ? O9 C21 1.430(3) . ? C9 C10 1.490(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? O10 C23 1.418(3) . ? O10 C22 1.425(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O11 C25 1.421(3) . ? O11 C24 1.428(3) . ? C11 C12 1.490(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? O12 C26 1.419(3) . ? O12 C27 1.422(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.498(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.503(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.493(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.504(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.505(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.514(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.486(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.486(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? 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 O9 K1 O5 69.39(4) . . ? O9 K1 O7 160.47(5) . . ? O5 K1 O7 93.34(4) . . ? O9 K1 O4 78.54(5) . . ? O5 K1 O4 60.47(5) . . ? O7 K1 O4 85.06(4) . . ? O9 K1 O10 61.20(5) . . ? O5 K1 O10 78.54(5) . . ? O7 K1 O10 125.97(5) . . ? O4 K1 O10 130.68(5) . . ? O9 K1 O3 120.22(5) . . ? O5 K1 O3 114.71(5) . . ? O7 K1 O3 57.77(5) . . ? O4 K1 O3 59.93(5) . . ? O10 K1 O3 166.63(5) . . ? O9 K1 O6 116.16(5) . . ? O5 K1 O6 59.37(5) . . ? O7 K1 O6 57.74(4) . . ? O4 K1 O6 104.13(5) . . ? O10 K1 O6 73.11(5) . . ? O3 K1 O6 114.44(5) . . ? O9 K1 O11 113.46(5) . . ? O5 K1 O11 120.93(5) . . ? O7 K1 O11 82.87(4) . . ? O4 K1 O11 167.90(5) . . ? O10 K1 O11 58.73(4) . . ? O3 K1 O11 112.22(5) . . ? O6 K1 O11 69.81(5) . . ? O9 K1 O8 59.80(5) . . ? O5 K1 O8 116.89(5) . . ? O7 K1 O8 125.61(5) . . ? O4 K1 O8 74.44(5) . . ? O10 K1 O8 104.72(5) . . ? O3 K1 O8 68.43(5) . . ? O6 K1 O8 175.81(4) . . ? O11 K1 O8 112.34(5) . . ? O9 K1 O12 91.78(4) . . ? O5 K1 O12 158.80(5) . . ? O7 K1 O12 106.65(4) . . ? O4 K1 O12 127.00(5) . . ? O10 K1 O12 83.89(5) . . ? O3 K1 O12 82.77(4) . . ? O6 K1 O12 126.16(5) . . ? O11 K1 O12 56.72(5) . . ? O8 K1 O12 56.49(5) . . ? C4 O1 H1O 116.3(16) . . ? C4 N1 H1N 118.3(17) . . ? C4 N1 H2N 121(2) . . ? H1N N1 H2N 119(3) . . ? C2 C1 C3 118.98(18) . . ? C2 C1 C4 120.57(18) . . ? C3 C1 C4 120.3(2) . . ? C8 O2 H1O 112.9(16) . . ? N2 C2 C1 177.6(2) . . ? C18 O3 C9 113.55(17) . . ? C18 O3 K1 118.40(13) . . ? C9 O3 K1 108.85(13) . . ? N3 C3 C1 178.7(3) . . ? C11 O4 C10 112.20(19) . . ? C11 O4 K1 115.61(15) . . ? C10 O4 K1 117.64(13) . . ? C8 N4 H3N 121.5(17) . . ? C8 N4 H4N 126.1(17) . . ? H3N N4 H4N 112(2) . . ? O1 C4 N1 120.66(19) . . ? O1 C4 C1 119.23(18) . . ? N1 C4 C1 120.1(2) . . ? C13 O5 C12 114.00(18) . . ? C13 O5 K1 117.04(12) . . ? C12 O5 K1 111.38(14) . . ? C7 C5 C6 119.15(18) . . ? C7 C5 C8 121.17(18) . . ? C6 C5 C8 119.7(2) . . ? C15 O6 C14 112.36(17) . . ? C15 O6 K1 117.32(13) . . ? C14 O6 K1 112.11(14) . . ? N5 C6 C5 178.4(2) . . ? C16 O7 C17 113.48(16) . . ? C16 O7 K1 109.56(12) . . ? C17 O7 K1 108.85(12) . . ? N6 C7 C5 178.4(2) . . ? C28 O8 C19 114.12(18) . . ? C28 O8 K1 118.71(15) . . ? C19 O8 K1 110.25(13) . . ? O2 C8 N4 120.37(19) . . ? O2 C8 C5 118.89(18) . . ? N4 C8 C5 120.7(2) . . ? C20 O9 C21 113.99(17) . . ? C20 O9 K1 117.18(12) . . ? C21 O9 K1 111.06(13) . . ? O3 C9 C10 113.1(2) . . ? O3 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? O3 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C23 O10 C22 111.95(17) . . ? C23 O10 K1 120.12(13) . . ? C22 O10 K1 114.91(14) . . ? O4 C10 C9 109.70(19) . . ? O4 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? O4 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C25 O11 C24 113.33(19) . . ? C25 O11 K1 118.71(15) . . ? C24 O11 K1 108.88(13) . . ? O4 C11 C12 109.0(2) . . ? O4 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O4 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C26 O12 C27 113.05(18) . . ? C26 O12 K1 108.99(13) . . ? C27 O12 K1 106.50(12) . . ? O5 C12 C11 113.7(2) . . ? O5 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? O5 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O5 C13 C14 107.77(19) . . ? O5 C13 H13A 110.2 . . ? C14 C13 H13A 110.2 . . ? O5 C13 H13B 110.2 . . ? C14 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? O6 C14 C13 112.5(2) . . ? O6 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? O6 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? O6 C15 C16 108.19(18) . . ? O6 C15 H15A 110.1 . . ? C16 C15 H15A 110.1 . . ? O6 C15 H15B 110.1 . . ? C16 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? O7 C16 C15 107.66(18) . . ? O7 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? O7 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? O7 C17 C18 107.78(18) . . ? O7 C17 H17A 110.2 . . ? C18 C17 H17A 110.2 . . ? O7 C17 H17B 110.2 . . ? C18 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? O3 C18 C17 107.77(17) . . ? O3 C18 H18A 110.2 . . ? C17 C18 H18A 110.2 . . ? O3 C18 H18B 110.2 . . ? C17 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? O8 C19 C20 112.4(2) . . ? O8 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? O8 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? O9 C20 C19 106.96(19) . . ? O9 C20 H20A 110.3 . . ? C19 C20 H20A 110.3 . . ? O9 C20 H20B 110.3 . . ? C19 C20 H20B 110.3 . . ? H20A C20 H20B 108.6 . . ? O9 C21 C22 113.86(18) . . ? O9 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? O9 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? O10 C22 C21 108.36(18) . . ? O10 C22 H22A 110.0 . . ? C21 C22 H22A 110.0 . . ? O10 C22 H22B 110.0 . . ? C21 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? O10 C23 C24 108.89(19) . . ? O10 C23 H23A 109.9 . . ? C24 C23 H23A 109.9 . . ? O10 C23 H23B 109.9 . . ? C24 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? O11 C24 C23 112.7(2) . . ? O11 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? O11 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? O11 C25 C26 109.22(19) . . ? O11 C25 H25A 109.8 . . ? C26 C25 H25A 109.8 . . ? O11 C25 H25B 109.8 . . ? C26 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? O12 C26 C25 108.2(2) . . ? O12 C26 H26A 110.1 . . ? C25 C26 H26A 110.1 . . ? O12 C26 H26B 110.1 . . ? C25 C26 H26B 110.1 . . ? H26A C26 H26B 108.4 . . ? O12 C27 C28 107.6(2) . . ? O12 C27 H27A 110.2 . . ? C28 C27 H27A 110.2 . . ? O12 C27 H27B 110.2 . . ? C28 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? O8 C28 C27 109.2(2) . . ? O8 C28 H28A 109.8 . . ? C27 C28 H28A 109.8 . . ? O8 C28 H28B 109.8 . . ? C27 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H2N N5 0.78(3) 2.35(3) 2.978(3) 139(3) 2_666 N1 H1N N6 0.87(3) 2.17(3) 3.010(3) 165(2) 1_455 N4 H4N N2 0.80(3) 2.19(3) 2.981(3) 167(2) 1_655 N4 H3N N3 0.86(3) 2.24(2) 2.976(3) 143(2) 2_665 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.574 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.097 # Attachment '5.CIF' data_DTK18C6 _database_code_depnum_ccdc_archive 'CCDC 669560' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(aqua)(carbamoyldicyanomethanido)(18-crown-6)potassium] ; _chemical_name_common '[K(18c6)(cdm)(H2O)]' _chemical_melting_point ? _chemical_formula_moiety 'C16 H28 K1 N3 O8' _chemical_formula_sum 'C16 H28 K1 N3 O8' _chemical_formula_weight 429.51 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 13.4619(2) _cell_length_b 17.6252(3) _cell_length_c 18.4777(3) _cell_angle_alpha 90.386(1) _cell_angle_beta 90.441(1) _cell_angle_gamma 103.642(1) _cell_volume 4260.20(12) _cell_formula_units_Z 8 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 42330 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.295 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9488 _exptl_absorpt_correction_T_max 0.9854 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42330 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19367 _reflns_number_gt 14899 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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^)+(0.2000P)^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_extinction_expression ? _refine_ls_number_reflns 19367 _refine_ls_number_parameters 1236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0773 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.76471(2) -0.225368(16) 1.104369(14) 0.02078(7) Uani 1 1 d . . . O1 O 0.96119(7) -0.24924(6) 1.10773(5) 0.0248(2) Uani 1 1 d . . . N1 N 0.70840(11) -0.07837(8) 0.76444(6) 0.0315(3) Uani 1 1 d . . . C1 C 1.04436(10) -0.19959(9) 1.14466(8) 0.0282(3) Uani 1 1 d . . . H1A H 1.1087 -0.1991 1.1189 0.034 Uiso 1 1 calc R . . H1B H 1.0502 -0.2191 1.1942 0.034 Uiso 1 1 calc R . . K2 K 0.78590(2) 0.281868(16) 1.097511(14) 0.01999(7) Uani 1 1 d . . . O2 O 0.93693(7) -0.11899(5) 1.18795(5) 0.0233(2) Uani 1 1 d . . . N2 N 0.81698(11) -0.10143(7) 1.00713(6) 0.0379(3) Uani 1 1 d . . . C2 C 1.02737(11) -0.11860(9) 1.14807(8) 0.0292(3) Uani 1 1 d . . . H2A H 1.0868 -0.0830 1.1718 0.035 Uiso 1 1 calc R . . H2B H 1.0204 -0.0995 1.0985 0.035 Uiso 1 1 calc R . . K3 K 0.75790(2) 0.024674(16) 0.418683(14) 0.01833(6) Uani 1 1 d . . . O3 O 0.73722(7) -0.09266(5) 1.19087(5) 0.0227(2) Uani 1 1 d . . . N3 N 0.68479(10) 0.07027(7) 0.89103(6) 0.0277(3) Uani 1 1 d . . . C3 C 0.91735(11) -0.04336(8) 1.19011(7) 0.0255(3) Uani 1 1 d . . . H3A H 0.9104 -0.0249 1.1402 0.031 Uiso 1 1 calc R . . H3B H 0.9751 -0.0063 1.2142 0.031 Uiso 1 1 calc R . . K4 K 0.76004(2) 0.526246(16) 0.421189(14) 0.01861(6) Uani 1 1 d . . . O4 O 0.57206(7) -0.22339(6) 1.17883(5) 0.0270(2) Uani 1 1 d . . . N4 N 0.72965(10) 0.42360(8) 0.76212(6) 0.0257(3) Uani 1 1 d . . . C4 C 0.82092(11) -0.04654(8) 1.23087(7) 0.0248(3) Uani 1 1 d . . . H4A H 0.8253 -0.0697 1.2791 0.030 Uiso 1 1 calc R . . H4B H 0.8109 0.0069 1.2379 0.030 Uiso 1 1 calc R . . O5 O 0.60258(7) -0.35855(6) 1.11355(5) 0.0288(2) Uani 1 1 d . . . N5 N 0.84491(9) 0.41389(7) 1.00584(6) 0.0278(3) Uani 1 1 d . A . C5 C 0.64341(11) -0.09742(9) 1.22687(7) 0.0274(3) Uani 1 1 d . . . H5A H 0.6318 -0.0445 1.2341 0.033 Uiso 1 1 calc R . . H5B H 0.6452 -0.1216 1.2749 0.033 Uiso 1 1 calc R . . O6 O 0.80095(7) -0.38416(5) 1.10500(5) 0.0258(2) Uani 1 1 d . . . N6 N 0.67921(9) 0.56280(7) 0.88673(6) 0.0257(3) Uani 1 1 d . A . C6 C 0.55937(11) -0.14571(9) 1.18157(8) 0.0299(3) Uani 1 1 d . . . H6A H 0.4923 -0.1450 1.2028 0.036 Uiso 1 1 calc R . . H6B H 0.5616 -0.1242 1.1321 0.036 Uiso 1 1 calc R . . O7 O 0.73924(8) -0.17708(5) 0.83184(5) 0.0267(2) Uani 1 1 d . . . N7 N 0.72530(9) 0.17373(7) 0.75721(6) 0.0206(2) Uani 1 1 d . . . C7 C 0.49425(11) -0.27350(10) 1.13680(10) 0.0389(4) Uani 1 1 d . . . H7A H 0.4996 -0.2571 1.0856 0.047 Uiso 1 1 calc R . . H7B H 0.4261 -0.2705 1.1546 0.047 Uiso 1 1 calc R . . O8 O 0.71000(9) -0.27268(7) 0.96018(6) 0.0320(2) Uani 1 1 d . . . N8 N 0.84217(10) 0.15061(7) 0.51660(6) 0.0287(3) Uani 1 1 d . . . C8 C 0.50671(11) -0.35523(9) 1.14285(9) 0.0383(4) Uani 1 1 d . . . H8A H 0.5035 -0.3710 1.1943 0.046 Uiso 1 1 calc R . . H8B H 0.4510 -0.3914 1.1160 0.046 Uiso 1 1 calc R . . N9 N 0.70028(9) 0.31784(7) 0.62963(6) 0.0244(3) Uani 1 1 d . . . C9 C 0.62070(12) -0.43477(8) 1.11782(8) 0.0307(3) Uani 1 1 d . . . H9A H 0.5607 -0.4738 1.0987 0.037 Uiso 1 1 calc R . . H9B H 0.6320 -0.4476 1.1689 0.037 Uiso 1 1 calc R . . O9A O 0.9950(4) 0.2991(3) 1.1305(2) 0.0281(7) Uani 0.783(7) 1 d P A 1 N10 N 0.70957(9) 0.66994(7) 0.75642(6) 0.0217(2) Uani 1 1 d . . . C10 C 0.71267(12) -0.43667(8) 1.07440(8) 0.0306(3) Uani 1 1 d . . . H10A H 0.7233 -0.4904 1.0736 0.037 Uiso 1 1 calc R . . H10B H 0.7022 -0.4215 1.0239 0.037 Uiso 1 1 calc R . . O10A O 0.8952(3) 0.4001(3) 1.2022(3) 0.0280(7) Uani 0.783(7) 1 d P A 1 N11 N 0.84589(10) 0.65285(7) 0.52069(6) 0.0285(3) Uani 1 1 d . . . C11 C 0.88683(12) -0.37482(9) 1.05832(7) 0.0305(3) Uani 1 1 d . . . H11A H 0.8729 -0.3499 1.0127 0.037 Uiso 1 1 calc R . . H11B H 0.8995 -0.4265 1.0463 0.037 Uiso 1 1 calc R . . O11A O 0.6823(3) 0.3822(3) 1.1771(3) 0.0298(7) Uani 0.783(7) 1 d P A 1 N12 N 0.69582(9) 0.81818(7) 0.63141(6) 0.0251(3) Uani 1 1 d . . . C12 C 0.97854(11) -0.32522(9) 1.09526(8) 0.0293(3) Uani 1 1 d . . . H12A H 0.9909 -0.3490 1.1419 0.035 Uiso 1 1 calc R . . H12B H 1.0395 -0.3213 1.0646 0.035 Uiso 1 1 calc R . . O12A O 0.5717(3) 0.2314(2) 1.13845(18) 0.0297(6) Uani 0.783(7) 1 d P A 1 C13 C 0.74338(10) -0.05757(7) 0.89055(6) 0.0203(3) Uani 1 1 d . . . O13A O 0.6745(3) 0.1260(3) 1.0805(2) 0.0278(7) Uani 0.783(7) 1 d P A 1 C14 C 0.73157(10) -0.10810(7) 0.82777(7) 0.0210(3) Uani 1 1 d . . . O14A O 0.8855(3) 0.1482(3) 1.1021(3) 0.0258(6) Uani 0.783(7) 1 d P A 1 O15 O 0.77578(7) 0.33033(5) 0.82894(4) 0.0216(2) Uani 1 1 d . . . C15 C 0.78286(11) -0.08189(8) 0.95481(7) 0.0247(3) Uani 1 1 d . . . O16 O 0.73349(8) 0.24026(7) 0.95639(5) 0.0281(2) Uani 1 1 d . A . C16 C 0.71219(10) 0.01274(8) 0.89076(6) 0.0195(3) Uani 1 1 d . . . O17 O 0.55307(6) -0.06269(5) 0.40767(5) 0.0214(2) Uani 1 1 d . . . C17A C 1.0483(3) 0.3618(3) 1.1749(3) 0.0339(10) Uani 0.783(7) 1 d P A 1 H17A H 1.1193 0.3802 1.1575 0.041 Uiso 0.783(7) 1 calc PR A 1 H17B H 1.0512 0.3438 1.2253 0.041 Uiso 0.783(7) 1 calc PR A 1 O18 O 0.59670(7) 0.07664(5) 0.32989(5) 0.0229(2) Uani 1 1 d . . . C18A C 0.9954(4) 0.4274(3) 1.1728(3) 0.0348(10) Uani 0.783(7) 1 d P A 1 H18A H 1.0345 0.4723 1.2016 0.042 Uiso 0.783(7) 1 calc PR A 1 H18B H 0.9905 0.4447 1.1223 0.042 Uiso 0.783(7) 1 calc PR A 1 O19 O 0.79780(7) 0.16475(5) 0.32454(4) 0.0213(2) Uani 1 1 d . . . C19A C 0.8448(4) 0.4625(3) 1.2074(3) 0.0378(12) Uani 0.783(7) 1 d P A 1 H19A H 0.8432 0.4870 1.1595 0.045 Uiso 0.783(7) 1 calc PR A 1 H19B H 0.8821 0.5027 1.2418 0.045 Uiso 0.783(7) 1 calc PR A 1 O20 O 0.95231(6) 0.08196(5) 0.34691(5) 0.02024(19) Uani 1 1 d . . . C20A C 0.7384(4) 0.4308(3) 1.2331(2) 0.0370(9) Uani 0.783(7) 1 d P A 1 H20A H 0.7394 0.4001 1.2776 0.044 Uiso 0.783(7) 1 calc PR A 1 H20B H 0.7056 0.4742 1.2442 0.044 Uiso 0.783(7) 1 calc PR A 1 O21 O 0.90722(6) -0.06091(5) 0.41746(5) 0.01991(19) Uani 1 1 d . . . C21A C 0.5786(3) 0.3530(2) 1.1958(2) 0.0391(11) Uani 0.783(7) 1 d P A 1 H21A H 0.5443 0.3967 1.2007 0.047 Uiso 0.783(7) 1 calc PR A 1 H21B H 0.5742 0.3257 1.2428 0.047 Uiso 0.783(7) 1 calc PR A 1 O22 O 0.70205(6) -0.14965(5) 0.41518(4) 0.01823(19) Uani 1 1 d . . . C22A C 0.5270(3) 0.2976(3) 1.1379(2) 0.0409(9) Uani 0.783(7) 1 d P A 1 H22A H 0.4528 0.2810 1.1472 0.049 Uiso 0.783(7) 1 calc PR A 1 H22B H 0.5369 0.3233 1.0901 0.049 Uiso 0.783(7) 1 calc PR A 1 O23 O 0.76693(7) 0.07606(5) 0.69277(4) 0.02015(19) Uani 1 1 d . . . C23A C 0.5244(3) 0.1740(3) 1.08706(19) 0.0389(9) Uani 0.783(7) 1 d P A 1 H23A H 0.5377 0.1946 1.0374 0.047 Uiso 0.783(7) 1 calc PR A 1 H23B H 0.4496 0.1597 1.0945 0.047 Uiso 0.783(7) 1 calc PR A 1 O24 O 0.73752(7) -0.02067(6) 0.56687(5) 0.0217(2) Uani 1 1 d . . . C24A C 0.5680(3) 0.1036(2) 1.09664(19) 0.0372(8) Uani 0.783(7) 1 d P A 1 H24A H 0.5582 0.0848 1.1470 0.045 Uiso 0.783(7) 1 calc PR A 1 H24B H 0.5330 0.0610 1.0636 0.045 Uiso 0.783(7) 1 calc PR A 1 O25 O 0.55406(6) 0.43920(5) 0.41031(5) 0.0221(2) Uani 1 1 d . . . C25A C 0.7213(3) 0.0625(3) 1.0818(3) 0.0308(10) Uani 0.783(7) 1 d P A 1 H25A H 0.6826 0.0193 1.0510 0.037 Uiso 0.783(7) 1 calc PR A 1 H25B H 0.7236 0.0432 1.1319 0.037 Uiso 0.783(7) 1 calc PR A 1 O26 O 0.59778(7) 0.58264(5) 0.33718(5) 0.0231(2) Uani 1 1 d . . . C26A C 0.8279(3) 0.0916(3) 1.0536(2) 0.0299(10) Uani 0.783(7) 1 d P A 1 H26A H 0.8612 0.0474 1.0484 0.036 Uiso 0.783(7) 1 calc PR A 1 H26B H 0.8251 0.1151 1.0053 0.036 Uiso 0.783(7) 1 calc PR A 1 O27 O 0.80168(7) 0.67025(5) 0.33234(4) 0.0212(2) Uani 1 1 d . . . C27A C 0.9864(3) 0.1765(3) 1.0762(3) 0.0343(10) Uani 0.783(7) 1 d P A 1 H27A H 0.9841 0.1990 1.0275 0.041 Uiso 0.783(7) 1 calc PR A 1 H27B H 1.0211 0.1330 1.0725 0.041 Uiso 0.783(7) 1 calc PR A 1 O28 O 0.95160(7) 0.58406(5) 0.34918(5) 0.02121(19) Uani 1 1 d . . . C28A C 1.0447(4) 0.2379(3) 1.1274(3) 0.0323(11) Uani 0.783(7) 1 d P A 1 H28A H 1.0476 0.2155 1.1761 0.039 Uiso 0.783(7) 1 calc PR A 1 H28B H 1.1155 0.2574 1.1102 0.039 Uiso 0.783(7) 1 calc PR A 1 O29 O 0.90628(7) 0.43822(5) 0.41472(5) 0.0213(2) Uani 1 1 d . . . C29 C 0.76331(10) 0.44694(7) 0.88808(6) 0.0177(3) Uani 1 1 d . A . O30 O 0.70102(6) 0.35058(5) 0.41159(4) 0.01974(19) Uani 1 1 d . . . C30 C 0.75789(10) 0.39649(7) 0.82524(6) 0.0177(3) Uani 1 1 d . . . O31 O 0.76153(7) 0.57590(5) 0.69308(4) 0.01950(19) Uani 1 1 d . . . C31 C 0.80771(10) 0.42826(7) 0.95282(7) 0.0191(3) Uani 1 1 d . . . O32 O 0.73958(7) 0.47938(6) 0.56632(5) 0.0220(2) Uani 1 1 d . . . C32 C 0.71855(10) 0.51102(7) 0.88758(6) 0.0182(3) Uani 1 1 d . . . C33 C 0.47496(10) -0.03480(8) 0.37139(8) 0.0258(3) Uani 1 1 d . . . H33A H 0.4093 -0.0525 0.3969 0.031 Uiso 1 1 calc R . . H33B H 0.4661 -0.0557 0.3213 0.031 Uiso 1 1 calc R . . C34 C 0.50515(10) 0.05249(8) 0.37034(8) 0.0265(3) Uani 1 1 d . . . H34A H 0.4499 0.0730 0.3479 0.032 Uiso 1 1 calc R . . H34B H 0.5164 0.0732 0.4204 0.032 Uiso 1 1 calc R . . C35 C 0.62042(11) 0.15847(8) 0.31763(8) 0.0261(3) Uani 1 1 d . . . H35A H 0.6255 0.1870 0.3644 0.031 Uiso 1 1 calc R . . H35B H 0.5657 0.1724 0.2882 0.031 Uiso 1 1 calc R . . C36 C 0.72001(10) 0.18085(8) 0.27865(7) 0.0243(3) Uani 1 1 d . . . H36A H 0.7161 0.1506 0.2330 0.029 Uiso 1 1 calc R . . H36B H 0.7357 0.2371 0.2668 0.029 Uiso 1 1 calc R . . C37 C 0.89488(10) 0.18448(8) 0.29083(7) 0.0218(3) Uani 1 1 d . . . H37A H 0.9134 0.2409 0.2799 0.026 Uiso 1 1 calc R . . H37B H 0.8925 0.1550 0.2448 0.026 Uiso 1 1 calc R . . C38 C 0.97290(10) 0.16476(8) 0.34087(7) 0.0228(3) Uani 1 1 d . . . H38A H 1.0424 0.1852 0.3215 0.027 Uiso 1 1 calc R . . H38B H 0.9692 0.1888 0.3891 0.027 Uiso 1 1 calc R . . C39 C 1.02570(10) 0.05846(8) 0.39212(8) 0.0279(3) Uani 1 1 d . . . H39A H 1.0197 0.0762 0.4425 0.034 Uiso 1 1 calc R . . H39B H 1.0956 0.0822 0.3751 0.034 Uiso 1 1 calc R . . C40 C 1.00648(10) -0.02875(8) 0.38931(8) 0.0264(3) Uani 1 1 d . . . H40A H 1.0104 -0.0466 0.3387 0.032 Uiso 1 1 calc R . . H40B H 1.0588 -0.0463 0.4185 0.032 Uiso 1 1 calc R . . C41 C 0.88119(10) -0.14396(7) 0.41343(7) 0.0203(3) Uani 1 1 d . . . H41A H 0.9361 -0.1649 0.4359 0.024 Uiso 1 1 calc R . . H41B H 0.8734 -0.1613 0.3622 0.024 Uiso 1 1 calc R . . C42 C 0.78311(10) -0.17353(8) 0.45248(7) 0.0198(3) Uani 1 1 d . . . H42A H 0.7677 -0.2312 0.4549 0.024 Uiso 1 1 calc R . . H42B H 0.7893 -0.1525 0.5026 0.024 Uiso 1 1 calc R . . C43 C 0.60933(9) -0.16993(8) 0.45464(7) 0.0196(3) Uani 1 1 d . . . H43A H 0.6187 -0.1436 0.5026 0.024 Uiso 1 1 calc R . . H43B H 0.5901 -0.2270 0.4624 0.024 Uiso 1 1 calc R . . C44 C 0.52663(10) -0.14534(7) 0.41308(7) 0.0209(3) Uani 1 1 d . . . H44A H 0.5196 -0.1694 0.3642 0.025 Uiso 1 1 calc R . . H44B H 0.4606 -0.1626 0.4383 0.025 Uiso 1 1 calc R . . C45 C 0.76684(9) 0.19346(7) 0.63266(6) 0.0163(3) Uani 1 1 d . . . C46 C 0.75448(9) 0.14400(7) 0.69566(6) 0.0159(3) Uani 1 1 d . . . C47 C 0.80823(10) 0.16968(7) 0.56871(7) 0.0192(3) Uani 1 1 d . . . C48 C 0.73133(10) 0.26211(7) 0.63127(6) 0.0176(3) Uani 1 1 d . . . C49 C 0.47687(10) 0.46878(8) 0.37460(8) 0.0266(3) Uani 1 1 d . . . H49A H 0.4104 0.4497 0.3988 0.032 Uiso 1 1 calc R . . H49B H 0.4696 0.4504 0.3236 0.032 Uiso 1 1 calc R . . C50 C 0.50671(10) 0.55590(8) 0.37730(8) 0.0279(3) Uani 1 1 d . . . H50A H 0.4512 0.5774 0.3565 0.034 Uiso 1 1 calc R . . H50B H 0.5181 0.5741 0.4282 0.034 Uiso 1 1 calc R . . C51 C 0.62516(11) 0.66563(8) 0.33372(8) 0.0260(3) Uani 1 1 d . . . H51A H 0.6354 0.6882 0.3832 0.031 Uiso 1 1 calc R . . H51B H 0.5698 0.6848 0.3099 0.031 Uiso 1 1 calc R . . C52 C 0.72164(10) 0.69017(8) 0.29166(7) 0.0244(3) Uani 1 1 d . . . H52A H 0.7140 0.6631 0.2441 0.029 Uiso 1 1 calc R . . H52B H 0.7374 0.7472 0.2833 0.029 Uiso 1 1 calc R . . C53 C 0.89562(10) 0.68786(8) 0.29458(7) 0.0234(3) Uani 1 1 d . . . H53A H 0.9150 0.7442 0.2831 0.028 Uiso 1 1 calc R . . H53B H 0.8885 0.6579 0.2486 0.028 Uiso 1 1 calc R . . C54 C 0.97611(10) 0.66681(8) 0.34126(7) 0.0247(3) Uani 1 1 d . . . H54A H 1.0440 0.6845 0.3186 0.030 Uiso 1 1 calc R . . H54B H 0.9783 0.6925 0.3893 0.030 Uiso 1 1 calc R . . C55 C 1.02518(10) 0.55844(9) 0.39225(8) 0.0293(3) Uani 1 1 d . . . H55A H 1.0201 0.5741 0.4434 0.035 Uiso 1 1 calc R . . H55B H 1.0949 0.5825 0.3752 0.035 Uiso 1 1 calc R . . C56 C 1.00497(10) 0.47128(9) 0.38615(8) 0.0286(3) Uani 1 1 d . . . H56A H 1.0077 0.4555 0.3348 0.034 Uiso 1 1 calc R . . H56B H 1.0576 0.4523 0.4135 0.034 Uiso 1 1 calc R . . C57 C 0.87945(10) 0.35578(8) 0.40620(7) 0.0222(3) Uani 1 1 d . . . H57A H 0.9346 0.3332 0.4260 0.027 Uiso 1 1 calc R . . H57B H 0.8704 0.3418 0.3542 0.027 Uiso 1 1 calc R . . C58 C 0.78218(10) 0.32388(8) 0.44556(7) 0.0213(3) Uani 1 1 d . . . H58A H 0.7664 0.2661 0.4446 0.026 Uiso 1 1 calc R . . H58B H 0.7896 0.3416 0.4967 0.026 Uiso 1 1 calc R . . C59 C 0.60897(10) 0.32851(8) 0.45144(7) 0.0209(3) Uani 1 1 d . . . H59A H 0.6192 0.3519 0.5006 0.025 Uiso 1 1 calc R . . H59B H 0.5891 0.2710 0.4563 0.025 Uiso 1 1 calc R . . C60 C 0.52637(10) 0.35629(7) 0.41252(7) 0.0209(3) Uani 1 1 d . . . H60A H 0.5179 0.3345 0.3627 0.025 Uiso 1 1 calc R . . H60B H 0.4607 0.3385 0.4381 0.025 Uiso 1 1 calc R . . C61 C 0.76294(9) 0.69422(7) 0.63416(6) 0.0168(3) Uani 1 1 d . . . C62 C 0.74582(9) 0.64299(7) 0.69607(6) 0.0161(3) Uani 1 1 d . . . C63 C 0.80857(10) 0.67155(7) 0.57165(7) 0.0197(3) Uani 1 1 d . . . C64 C 0.72739(10) 0.76257(7) 0.63256(6) 0.0179(3) Uani 1 1 d . . . C20B C 0.7888(14) 0.4496(7) 1.2288(7) 0.034(4) Uani 0.217(7) 1 d P A 2 H20C H 0.7944 0.4252 1.2763 0.041 Uiso 0.217(7) 1 calc PR A 2 H20D H 0.7675 0.4989 1.2374 0.041 Uiso 0.217(7) 1 calc PR A 2 O10B O 0.9259(10) 0.3971(13) 1.1920(10) 0.031(3) Uani 0.217(7) 1 d P A 2 O12B O 0.5817(11) 0.2556(9) 1.1576(10) 0.055(4) Uani 0.217(7) 1 d P A 2 C22B C 0.5491(10) 0.3257(15) 1.1648(9) 0.068(10) Uani 0.217(7) 1 d P A 2 H22C H 0.4775 0.3149 1.1815 0.081 Uiso 0.217(7) 1 calc PR A 2 H22D H 0.5536 0.3531 1.1179 0.081 Uiso 0.217(7) 1 calc PR A 2 C19B C 0.8886(15) 0.4665(14) 1.1933(12) 0.050(5) Uani 0.217(7) 1 d P A 2 H19C H 0.8816 0.4845 1.1433 0.060 Uiso 0.217(7) 1 calc PR A 2 H19D H 0.9372 0.5083 1.2200 0.060 Uiso 0.217(7) 1 calc PR A 2 O11B O 0.7151(12) 0.3991(9) 1.1857(9) 0.030(3) Uani 0.217(7) 1 d P A 2 O14B O 0.8516(14) 0.1317(10) 1.1033(10) 0.052(4) Uani 0.217(7) 1 d P A 2 C21B C 0.6190(15) 0.3741(15) 1.2194(10) 0.076(7) Uani 0.217(7) 1 d P A 2 H21C H 0.5926 0.4196 1.2344 0.091 Uiso 0.217(7) 1 calc PR A 2 H21D H 0.6251 0.3428 1.2628 0.091 Uiso 0.217(7) 1 calc PR A 2 O13B O 0.6416(12) 0.1322(10) 1.0902(10) 0.051(4) Uani 0.217(7) 1 d P A 2 C26B C 0.776(2) 0.0765(8) 1.0667(9) 0.084(13) Uani 0.217(7) 1 d P A 2 H26C H 0.7978 0.0268 1.0644 0.101 Uiso 0.217(7) 1 calc PR A 2 H26D H 0.7716 0.0944 1.0163 0.101 Uiso 0.217(7) 1 calc PR A 2 C18B C 1.0193(13) 0.4054(13) 1.1594(11) 0.045(5) Uani 0.217(7) 1 d P A 2 H18C H 1.0701 0.4470 1.1849 0.054 Uiso 0.217(7) 1 calc PR A 2 H18D H 1.0142 0.4219 1.1087 0.054 Uiso 0.217(7) 1 calc PR A 2 O9B O 0.9863(16) 0.2804(12) 1.1146(9) 0.051(4) Uani 0.217(7) 1 d P A 2 C25B C 0.6697(19) 0.0594(10) 1.0974(13) 0.117(10) Uani 0.217(7) 1 d P A 2 H25C H 0.6226 0.0175 1.0695 0.140 Uiso 0.217(7) 1 calc PR A 2 H25D H 0.6699 0.0438 1.1488 0.140 Uiso 0.217(7) 1 calc PR A 2 C17B C 1.0550(17) 0.3327(15) 1.1602(13) 0.077(8) Uani 0.217(7) 1 d P A 2 H17C H 1.1256 0.3417 1.1416 0.092 Uiso 0.217(7) 1 calc PR A 2 H17D H 1.0537 0.3119 1.2099 0.092 Uiso 0.217(7) 1 calc PR A 2 C28B C 1.0217(15) 0.2077(12) 1.1115(11) 0.056(7) Uani 0.217(7) 1 d P A 2 H28C H 1.0273 0.1874 1.1608 0.067 Uiso 0.217(7) 1 calc PR A 2 H28D H 1.0895 0.2168 1.0883 0.067 Uiso 0.217(7) 1 calc PR A 2 C24B C 0.5393(14) 0.1275(11) 1.1147(13) 0.085(7) Uani 0.217(7) 1 d P A 2 H24C H 0.5322 0.1076 1.1648 0.103 Uiso 0.217(7) 1 calc PR A 2 H24D H 0.4903 0.0904 1.0835 0.103 Uiso 0.217(7) 1 calc PR A 2 C23B C 0.5148(16) 0.2040(12) 1.1127(13) 0.090(7) Uani 0.217(7) 1 d P A 2 H23C H 0.5206 0.2237 1.0625 0.108 Uiso 0.217(7) 1 calc PR A 2 H23D H 0.4437 0.1993 1.1288 0.108 Uiso 0.217(7) 1 calc PR A 2 C27B C 0.945(2) 0.1515(13) 1.0682(12) 0.091(9) Uani 0.217(7) 1 d P A 2 H27C H 0.9352 0.1748 1.0208 0.109 Uiso 0.217(7) 1 calc PR A 2 H27D H 0.9695 0.1038 1.0592 0.109 Uiso 0.217(7) 1 calc PR A 2 H7N H 0.7021(11) 0.6396(9) 0.7936(8) 0.026(4) Uiso 1 1 d . . . H5N H 0.7173(11) 0.1446(9) 0.7936(8) 0.026(4) Uiso 1 1 d . . . H6O H 0.7230(13) -0.0648(10) 0.5873(9) 0.035(5) Uiso 1 1 d . . . H2N H 0.7209(12) -0.0297(10) 0.7571(8) 0.036(5) Uiso 1 1 d . . . H4N H 0.7302(11) 0.4716(10) 0.7565(8) 0.028(4) Uiso 1 1 d . . . H1N H 0.7054(11) -0.1070(9) 0.7257(8) 0.029(4) Uiso 1 1 d . . . H3N H 0.7223(12) 0.3930(9) 0.7254(9) 0.032(4) Uiso 1 1 d . . . H7O H 0.7520(12) 0.5114(10) 0.6004(9) 0.036(5) Uiso 1 1 d . . . H6N H 0.7346(12) 0.2235(10) 0.7623(8) 0.033(4) Uiso 1 1 d . . . H5O H 0.7524(13) 0.0103(10) 0.6023(9) 0.038(5) Uiso 1 1 d . . . H8N H 0.7157(12) 0.7193(10) 0.7626(8) 0.036(5) Uiso 1 1 d . . . H8O H 0.7256(13) 0.4344(11) 0.5850(9) 0.043(5) Uiso 1 1 d . . . H3O H 0.7434(13) 0.2690(10) 0.9184(9) 0.038(5) Uiso 1 1 d . . . H1O H 0.7231(14) -0.2377(11) 0.9233(10) 0.055(6) Uiso 1 1 d . . . H4O H 0.7092(14) 0.1986(11) 0.9401(10) 0.043(6) Uiso 1 1 d . . . H2O H 0.6900(15) -0.3194(12) 0.9381(11) 0.064(6) 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 0.02063(15) 0.01865(15) 0.02364(14) 0.00206(11) 0.00048(11) 0.00578(11) O1 0.0207(5) 0.0263(5) 0.0293(5) 0.0001(4) 0.0016(4) 0.0092(4) N1 0.0632(9) 0.0149(7) 0.0180(6) -0.0007(5) -0.0063(6) 0.0130(6) C1 0.0168(7) 0.0379(9) 0.0297(7) 0.0032(6) 0.0047(6) 0.0060(6) K2 0.02140(15) 0.01944(15) 0.01889(13) 0.00052(11) -0.00074(10) 0.00436(11) O2 0.0204(5) 0.0226(5) 0.0256(5) 0.0020(4) 0.0051(4) 0.0025(4) N2 0.0680(10) 0.0247(7) 0.0249(6) -0.0011(5) -0.0062(6) 0.0191(7) C2 0.0190(7) 0.0319(9) 0.0328(8) 0.0016(6) 0.0066(6) -0.0018(6) K3 0.01622(14) 0.01745(15) 0.02151(13) 0.00062(10) 0.00101(10) 0.00427(11) O3 0.0237(5) 0.0229(5) 0.0215(4) -0.0020(4) 0.0041(4) 0.0056(4) N3 0.0406(7) 0.0224(7) 0.0212(6) 0.0018(5) 0.0005(5) 0.0099(6) C3 0.0292(8) 0.0184(7) 0.0265(7) -0.0002(5) -0.0017(6) 0.0013(6) K4 0.01665(14) 0.01775(15) 0.02155(13) 0.00094(11) 0.00125(10) 0.00422(11) O4 0.0185(5) 0.0248(6) 0.0376(5) 0.0028(4) -0.0020(4) 0.0046(4) N4 0.0491(8) 0.0143(6) 0.0158(6) -0.0011(5) -0.0021(5) 0.0115(6) C4 0.0315(8) 0.0204(7) 0.0232(7) -0.0034(5) -0.0033(6) 0.0074(6) O5 0.0264(5) 0.0223(5) 0.0354(5) 0.0018(4) -0.0020(4) 0.0014(4) N5 0.0386(7) 0.0216(6) 0.0240(6) -0.0019(5) -0.0049(5) 0.0091(5) C5 0.0296(8) 0.0273(8) 0.0284(7) 0.0015(6) 0.0091(6) 0.0126(6) O6 0.0322(6) 0.0231(5) 0.0220(5) -0.0036(4) 0.0005(4) 0.0065(4) N6 0.0388(7) 0.0213(6) 0.0190(5) 0.0023(5) 0.0028(5) 0.0112(6) C6 0.0228(7) 0.0306(9) 0.0405(8) 0.0048(6) 0.0053(6) 0.0147(6) O7 0.0462(6) 0.0138(5) 0.0214(5) 0.0013(4) 0.0001(4) 0.0092(4) N7 0.0317(7) 0.0135(6) 0.0170(5) 0.0023(5) 0.0016(5) 0.0060(5) C7 0.0182(7) 0.0412(10) 0.0560(10) -0.0036(8) -0.0094(7) 0.0047(7) O8 0.0442(7) 0.0236(6) 0.0263(5) 0.0025(5) -0.0026(5) 0.0041(5) N8 0.0443(8) 0.0211(6) 0.0231(6) 0.0033(5) 0.0047(5) 0.0123(6) C8 0.0192(7) 0.0346(9) 0.0559(10) -0.0041(7) -0.0025(7) -0.0040(6) N9 0.0397(7) 0.0182(6) 0.0176(5) 0.0006(4) -0.0014(5) 0.0115(5) C9 0.0354(8) 0.0178(8) 0.0351(8) -0.0013(6) -0.0088(6) -0.0007(6) O9A 0.0186(10) 0.0351(14) 0.0275(17) 0.0031(11) -0.0043(12) 0.0003(10) N10 0.0360(7) 0.0132(6) 0.0173(5) 0.0029(5) 0.0022(5) 0.0084(5) C10 0.0444(9) 0.0201(8) 0.0263(7) -0.0062(6) -0.0083(6) 0.0060(7) O10A 0.033(2) 0.0182(11) 0.0295(14) 0.0026(8) -0.0049(13) -0.0004(15) N11 0.0431(8) 0.0223(6) 0.0232(6) 0.0039(5) 0.0052(5) 0.0134(6) C11 0.0436(9) 0.0270(8) 0.0254(7) -0.0006(6) 0.0081(6) 0.0174(7) O11A 0.0337(18) 0.0348(17) 0.0224(11) -0.0031(10) 0.0032(13) 0.0113(12) N12 0.0413(7) 0.0191(6) 0.0174(5) 0.0014(4) 0.0004(5) 0.0120(5) C12 0.0318(8) 0.0299(8) 0.0328(8) 0.0037(6) 0.0091(6) 0.0201(7) O12A 0.0171(15) 0.0357(18) 0.0347(12) 0.0032(9) -0.0021(10) 0.0030(13) C13 0.0294(7) 0.0143(7) 0.0171(6) 0.0027(5) 0.0008(5) 0.0051(5) O13A 0.0258(16) 0.0226(11) 0.0309(8) 0.0024(7) 0.0009(10) -0.0025(11) C14 0.0283(7) 0.0142(7) 0.0197(6) 0.0020(5) 0.0007(5) 0.0032(5) O14A 0.0326(13) 0.0289(16) 0.0175(9) -0.0035(9) 0.0034(10) 0.0102(9) O15 0.0327(5) 0.0142(5) 0.0193(4) 0.0008(3) 0.0013(4) 0.0082(4) C15 0.0397(8) 0.0140(7) 0.0210(7) -0.0012(5) 0.0016(6) 0.0076(6) O16 0.0426(6) 0.0196(6) 0.0202(5) 0.0022(4) -0.0004(4) 0.0034(5) C16 0.0266(7) 0.0156(7) 0.0145(6) 0.0020(5) 0.0014(5) 0.0015(6) O17 0.0141(4) 0.0178(5) 0.0323(5) 0.0028(4) -0.0029(4) 0.0037(4) C17A 0.0190(19) 0.037(2) 0.0367(15) 0.0084(15) -0.0094(13) -0.0116(15) O18 0.0192(5) 0.0184(5) 0.0319(5) 0.0031(4) 0.0033(4) 0.0061(4) C18A 0.040(3) 0.0230(18) 0.0321(19) 0.0046(12) -0.0100(16) -0.0111(15) O19 0.0201(5) 0.0242(5) 0.0196(4) 0.0053(4) 0.0021(4) 0.0049(4) C19A 0.059(4) 0.016(2) 0.037(3) -0.003(2) -0.023(2) 0.009(3) O20 0.0164(4) 0.0189(5) 0.0245(5) 0.0021(4) -0.0035(4) 0.0024(4) C20A 0.063(3) 0.034(2) 0.0230(13) -0.0062(14) -0.0067(18) 0.0284(19) O21 0.0156(4) 0.0185(5) 0.0259(5) 0.0014(4) 0.0015(4) 0.0045(4) C21A 0.042(4) 0.049(2) 0.037(3) 0.016(2) 0.0161(18) 0.033(2) O22 0.0158(4) 0.0200(5) 0.0195(4) 0.0050(3) 0.0010(3) 0.0053(4) C22A 0.0202(18) 0.053(2) 0.053(2) 0.0147(16) 0.0020(14) 0.0160(14) O23 0.0282(5) 0.0135(5) 0.0198(4) 0.0012(3) -0.0016(4) 0.0070(4) C23A 0.0172(11) 0.053(3) 0.0391(15) 0.0036(13) -0.0060(10) -0.0065(14) O24 0.0263(5) 0.0172(5) 0.0211(5) 0.0004(4) 0.0010(4) 0.0043(4) C24A 0.0328(18) 0.034(2) 0.0354(13) 0.0035(11) 0.0002(11) -0.0120(14) O25 0.0152(4) 0.0180(5) 0.0325(5) 0.0012(4) -0.0031(4) 0.0031(4) C25A 0.051(3) 0.010(2) 0.0255(12) 0.0009(11) -0.0067(17) -0.0043(18) O26 0.0197(5) 0.0176(5) 0.0325(5) 0.0002(4) 0.0016(4) 0.0052(4) C26A 0.052(2) 0.020(2) 0.0205(11) -0.0043(12) 0.0003(14) 0.0149(17) O27 0.0205(5) 0.0235(5) 0.0200(4) 0.0050(4) 0.0009(4) 0.0058(4) C27A 0.0336(17) 0.046(3) 0.0281(18) 0.0013(16) 0.0105(13) 0.0199(15) O28 0.0169(5) 0.0190(5) 0.0271(5) 0.0021(4) -0.0024(4) 0.0029(4) C28A 0.0201(12) 0.045(3) 0.0338(14) 0.0116(17) 0.0053(10) 0.0110(16) O29 0.0173(5) 0.0202(5) 0.0267(5) 0.0013(4) 0.0030(4) 0.0053(4) C29 0.0233(7) 0.0133(6) 0.0165(6) 0.0008(5) 0.0011(5) 0.0043(5) O30 0.0176(5) 0.0218(5) 0.0207(4) 0.0057(4) 0.0020(3) 0.0063(4) C30 0.0205(6) 0.0144(7) 0.0176(6) 0.0023(5) 0.0020(5) 0.0027(5) O31 0.0275(5) 0.0128(5) 0.0192(4) 0.0009(3) -0.0019(4) 0.0069(4) C31 0.0240(7) 0.0110(6) 0.0217(6) -0.0027(5) 0.0016(5) 0.0031(5) O32 0.0267(5) 0.0176(5) 0.0213(5) 0.0002(4) 0.0008(4) 0.0045(4) C32 0.0250(7) 0.0150(7) 0.0129(6) 0.0015(5) 0.0018(5) 0.0011(5) C33 0.0130(6) 0.0268(8) 0.0380(8) 0.0053(6) -0.0016(6) 0.0055(6) C34 0.0178(7) 0.0281(8) 0.0363(8) 0.0054(6) 0.0047(6) 0.0106(6) C35 0.0253(7) 0.0202(7) 0.0354(8) 0.0047(6) -0.0018(6) 0.0106(6) C36 0.0265(7) 0.0210(7) 0.0265(7) 0.0069(5) -0.0019(6) 0.0077(6) C37 0.0231(7) 0.0182(7) 0.0224(6) 0.0042(5) 0.0048(5) 0.0015(5) C38 0.0202(7) 0.0184(7) 0.0265(7) 0.0007(5) 0.0013(5) -0.0023(5) C39 0.0151(7) 0.0324(8) 0.0340(8) 0.0078(6) -0.0063(6) 0.0011(6) C40 0.0134(6) 0.0320(8) 0.0353(8) 0.0095(6) 0.0016(6) 0.0078(6) C41 0.0209(7) 0.0188(7) 0.0241(6) 0.0002(5) -0.0024(5) 0.0104(5) C42 0.0218(7) 0.0175(7) 0.0212(6) 0.0033(5) -0.0029(5) 0.0066(5) C43 0.0199(7) 0.0180(7) 0.0200(6) 0.0031(5) 0.0035(5) 0.0023(5) C44 0.0173(6) 0.0177(7) 0.0255(7) 0.0019(5) 0.0025(5) -0.0002(5) C45 0.0186(6) 0.0128(6) 0.0173(6) 0.0004(5) -0.0005(5) 0.0032(5) C46 0.0145(6) 0.0139(7) 0.0180(6) 0.0002(5) -0.0037(5) 0.0010(5) C47 0.0242(7) 0.0127(6) 0.0207(6) 0.0029(5) -0.0017(5) 0.0047(5) C48 0.0219(7) 0.0162(7) 0.0126(6) 0.0004(5) -0.0011(5) 0.0003(5) C49 0.0137(6) 0.0275(8) 0.0388(8) 0.0037(6) -0.0019(6) 0.0053(6) C50 0.0189(7) 0.0278(8) 0.0397(8) 0.0040(6) 0.0043(6) 0.0105(6) C51 0.0259(7) 0.0172(7) 0.0365(8) -0.0006(6) -0.0045(6) 0.0084(6) C52 0.0290(8) 0.0180(7) 0.0262(7) 0.0044(5) -0.0061(6) 0.0055(6) C53 0.0269(7) 0.0178(7) 0.0249(7) 0.0041(5) 0.0075(5) 0.0035(6) C54 0.0200(7) 0.0189(7) 0.0319(7) 0.0008(6) 0.0033(6) -0.0020(5) C55 0.0157(7) 0.0330(9) 0.0373(8) 0.0101(6) -0.0055(6) 0.0019(6) C56 0.0159(7) 0.0343(9) 0.0380(8) 0.0123(6) 0.0039(6) 0.0099(6) C57 0.0254(7) 0.0203(7) 0.0241(6) -0.0007(5) -0.0012(5) 0.0117(6) C58 0.0247(7) 0.0175(7) 0.0232(6) 0.0041(5) -0.0030(5) 0.0078(5) C59 0.0229(7) 0.0180(7) 0.0204(6) 0.0026(5) 0.0039(5) 0.0020(5) C60 0.0180(6) 0.0183(7) 0.0234(6) -0.0001(5) 0.0011(5) -0.0019(5) C61 0.0196(6) 0.0127(6) 0.0179(6) 0.0012(5) -0.0002(5) 0.0035(5) C62 0.0151(6) 0.0136(7) 0.0182(6) -0.0003(5) -0.0037(5) 0.0010(5) C63 0.0246(7) 0.0128(6) 0.0216(6) 0.0040(5) -0.0030(5) 0.0045(5) C64 0.0227(7) 0.0162(7) 0.0135(6) 0.0010(5) -0.0003(5) 0.0020(5) C20B 0.073(14) 0.016(7) 0.016(5) 0.002(4) 0.001(8) 0.014(9) O10B 0.021(7) 0.036(5) 0.028(5) 0.006(4) -0.004(4) -0.009(6) O12B 0.023(4) 0.048(9) 0.083(10) 0.039(6) -0.016(6) -0.015(5) C22B 0.010(8) 0.14(3) 0.051(15) 0.071(14) 0.004(8) 0.022(12) C19B 0.072(13) 0.030(6) 0.036(7) 0.002(5) -0.015(8) -0.015(10) O11B 0.044(8) 0.029(6) 0.023(6) 0.007(5) 0.008(5) 0.018(5) O14B 0.104(13) 0.036(8) 0.030(4) 0.006(5) -0.003(8) 0.045(8) C21B 0.073(13) 0.149(19) 0.041(9) 0.047(10) 0.031(8) 0.094(14) O13B 0.048(10) 0.020(5) 0.075(9) 0.026(6) -0.037(6) -0.011(6) C26B 0.19(3) 0.004(8) 0.051(19) -0.007(10) -0.09(2) 0.02(2) C18B 0.020(7) 0.059(15) 0.041(8) 0.009(8) -0.001(5) -0.022(8) O9B 0.040(8) 0.095(13) 0.032(7) 0.009(6) -0.001(5) 0.042(8) C25B 0.15(2) 0.032(7) 0.149(18) 0.033(10) -0.111(15) -0.021(11) C17B 0.039(8) 0.12(2) 0.081(15) 0.065(14) 0.025(9) 0.029(13) C28B 0.059(18) 0.064(17) 0.068(17) 0.045(11) 0.047(13) 0.058(13) C24B 0.056(11) 0.052(11) 0.125(16) 0.020(10) -0.047(10) -0.031(8) C23B 0.053(10) 0.082(15) 0.117(18) 0.051(12) -0.028(12) -0.022(10) C27B 0.20(3) 0.061(14) 0.043(9) 0.026(10) 0.042(16) 0.100(17) _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 2.7748(9) . ? K1 N2 2.8005(13) . ? K1 O5 2.8102(10) . ? K1 O8 2.8260(11) . ? K1 O3 2.9206(9) . ? K1 O6 2.9522(10) . ? K1 O4 2.9524(10) . ? K1 O2 3.0217(10) . ? K1 C11 3.5213(14) . ? O1 C1 1.4152(17) . ? O1 C12 1.4300(16) . ? N1 C14 1.3495(17) . ? N1 H2N 0.846(17) . ? N1 H1N 0.869(16) . ? C1 C2 1.499(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? K2 O9B 2.72(2) . ? K2 O16 2.7453(10) . ? K2 O13A 2.817(5) . ? K2 O9A 2.821(5) . ? K2 N5 2.8490(12) . ? K2 O13B 2.885(16) . ? K2 O11A 2.897(5) . ? K2 O12B 2.908(16) . ? K2 O12A 2.918(4) . ? K2 O10A 2.951(5) . ? K2 O11B 2.956(17) . ? K2 O10B 2.969(19) . ? O2 C3 1.4188(16) . ? O2 C2 1.4266(16) . ? N2 C15 1.1560(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? K3 O21 2.7834(9) . ? K3 O17 2.8284(9) . ? K3 O24 2.8547(10) . ? K3 N8 2.8660(12) . ? K3 O20 2.9074(9) . ? K3 O19 2.9760(9) . ? K3 O22 2.9861(9) . ? K3 O18 3.0238(9) . ? O3 C5 1.4171(16) . ? O3 C4 1.4226(16) . ? N3 C16 1.1579(17) . ? C3 C4 1.4957(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? K4 O29 2.7819(9) . ? K4 O32 2.8077(10) . ? K4 O25 2.8397(9) . ? K4 O28 2.8792(9) . ? K4 N11 2.8967(12) . ? K4 O27 2.9750(9) . ? K4 O30 3.0132(9) . ? K4 O26 3.0269(9) . ? K4 C55 3.5250(14) . ? O4 C6 1.4199(17) . ? O4 C7 1.4219(17) . ? N4 C30 1.3490(16) . ? N4 H4N 0.850(16) . ? N4 H3N 0.854(16) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C8 1.4171(18) . ? O5 C9 1.4234(17) . ? N5 C31 1.1534(16) . ? C5 C6 1.492(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? O6 C11 1.4266(17) . ? O6 C10 1.4326(17) . ? N6 C32 1.1583(16) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C14 1.2469(15) . ? N7 C46 1.3485(16) . ? N7 H5N 0.841(16) . ? N7 H6N 0.861(17) . ? C7 C8 1.494(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O8 H1O 0.91(2) . ? O8 H2O 0.90(2) . ? N8 C47 1.1505(16) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N9 C48 1.1551(16) . ? C9 C10 1.487(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O9A C28A 1.398(8) . ? O9A C17A 1.420(4) . ? N10 C62 1.3482(16) . ? N10 H7N 0.865(16) . ? N10 H8N 0.862(17) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O10A C19A 1.425(7) . ? O10A C18A 1.433(5) . ? N11 C63 1.1528(16) . ? C11 C12 1.491(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? O11A C21A 1.416(5) . ? O11A C20A 1.429(4) . ? N12 C64 1.1569(16) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O12A C23A 1.415(4) . ? O12A C22A 1.434(6) . ? C13 C16 1.3992(18) . ? C13 C15 1.4074(18) . ? C13 C14 1.4424(17) . ? O13A C25A 1.407(6) . ? O13A C24A 1.429(4) . ? O14A C26A 1.419(6) . ? O14A C27A 1.421(5) . ? O15 C30 1.2473(15) . ? O16 H3O 0.862(18) . ? O16 H4O 0.787(19) . ? O17 C44 1.4202(15) . ? O17 C33 1.4261(15) . ? C17A C18A 1.494(5) . ? C17A H17A 0.9900 . ? C17A H17B 0.9900 . ? O18 C35 1.4219(16) . ? O18 C34 1.4247(15) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? O19 C37 1.4206(15) . ? O19 C36 1.4233(15) . ? C19A C20A 1.491(4) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? O20 C38 1.4250(15) . ? O20 C39 1.4249(15) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? O21 C41 1.4238(15) . ? O21 C40 1.4263(15) . ? C21A C22A 1.495(5) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? O22 C43 1.4229(14) . ? O22 C42 1.4323(14) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? O23 C46 1.2485(14) . ? C23A C24A 1.503(6) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? O24 H6O 0.847(18) . ? O24 H5O 0.842(18) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? O25 C60 1.4213(15) . ? O25 C49 1.4270(15) . ? C25A C26A 1.504(5) . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? O26 C50 1.4216(16) . ? O26 C51 1.4236(16) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? O27 C53 1.4190(15) . ? O27 C52 1.4208(15) . ? C27A C28A 1.501(5) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? O28 C55 1.4220(16) . ? O28 C54 1.4262(16) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? O29 C57 1.4194(15) . ? O29 C56 1.4258(15) . ? C29 C32 1.3999(18) . ? C29 C31 1.4084(18) . ? C29 C30 1.4485(16) . ? O30 C59 1.4212(15) . ? O30 C58 1.4300(15) . ? O31 C62 1.2504(14) . ? O32 H7O 0.833(17) . ? O32 H8O 0.848(19) . ? C33 C34 1.4960(19) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.4969(19) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.4968(18) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.498(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.4936(17) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.4954(18) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C48 1.4024(18) . ? C45 C47 1.4128(17) . ? C45 C46 1.4460(16) . ? C49 C50 1.493(2) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.4944(19) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.4950(19) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.499(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.4942(18) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.4975(18) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C64 1.3977(18) . ? C61 C63 1.4112(17) . ? C61 C62 1.4480(17) . ? C20B O11B 1.406(15) . ? C20B C19B 1.467(16) . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? O10B C18B 1.375(16) . ? O10B C19B 1.43(3) . ? O12B C23B 1.385(18) . ? O12B C22B 1.41(2) . ? C22B C21B 1.49(2) . ? C22B H22C 0.9900 . ? C22B H22D 0.9900 . ? C19B H19C 0.9900 . ? C19B H19D 0.9900 . ? O11B C21B 1.42(2) . ? O14B C27B 1.39(2) . ? O14B C26B 1.40(2) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? O13B C25B 1.43(2) . ? O13B C24B 1.438(19) . ? C26B C25B 1.50(2) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? C18B C17B 1.47(2) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? O9B C17B 1.41(2) . ? O9B C28B 1.47(3) . ? C25B H25C 0.9900 . ? C25B H25D 0.9900 . ? C17B H17C 0.9900 . ? C17B H17D 0.9900 . ? C28B C27B 1.48(2) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? C24B C23B 1.46(2) . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C27B H27C 0.9900 . ? C27B H27D 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 O1 K1 N2 93.19(4) . . ? O1 K1 O5 116.90(3) . . ? N2 K1 O5 134.50(4) . . ? O1 K1 O8 99.31(3) . . ? N2 K1 O8 67.74(4) . . ? O5 K1 O8 73.99(3) . . ? O1 K1 O3 114.72(3) . . ? N2 K1 O3 77.50(3) . . ? O5 K1 O3 114.19(3) . . ? O8 K1 O3 132.26(3) . . ? O1 K1 O6 58.63(3) . . ? N2 K1 O6 132.69(3) . . ? O5 K1 O6 58.46(3) . . ? O8 K1 O6 79.55(3) . . ? O3 K1 O6 146.59(3) . . ? O1 K1 O4 149.94(3) . . ? N2 K1 O4 110.93(4) . . ? O5 K1 O4 57.63(3) . . ? O8 K1 O4 106.18(3) . . ? O3 K1 O4 57.07(3) . . ? O6 K1 O4 110.42(3) . . ? O1 K1 O2 57.78(3) . . ? N2 K1 O2 80.00(3) . . ? O5 K1 O2 144.41(3) . . ? O8 K1 O2 139.62(3) . . ? O3 K1 O2 56.96(3) . . ? O6 K1 O2 108.03(3) . . ? O4 K1 O2 107.66(3) . . ? O1 K1 C11 42.31(3) . . ? N2 K1 C11 110.61(4) . . ? O5 K1 C11 78.47(3) . . ? O8 K1 C11 71.88(3) . . ? O3 K1 C11 154.05(3) . . ? O6 K1 C11 23.41(3) . . ? O4 K1 C11 133.53(3) . . ? O2 K1 C11 99.16(3) . . ? C1 O1 C12 111.88(10) . . ? C1 O1 K1 123.86(8) . . ? C12 O1 K1 120.77(8) . . ? C14 N1 H2N 122.1(11) . . ? C14 N1 H1N 118.0(10) . . ? H2N N1 H1N 114.9(15) . . ? O1 C1 C2 109.27(11) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? O9B K2 O16 107.0(3) . . ? O9B K2 O13A 107.6(4) . . ? O16 K2 O13A 66.42(9) . . ? O9B K2 O9A 8.7(4) . . ? O16 K2 O9A 114.35(9) . . ? O13A K2 O9A 114.44(12) . . ? O9B K2 N5 89.3(5) . . ? O16 K2 N5 69.70(3) . . ? O13A K2 N5 135.87(9) . . ? O9A K2 N5 87.62(10) . . ? O9B K2 O13B 116.8(5) . . ? O16 K2 O13B 69.3(3) . . ? O13A K2 O13B 10.3(4) . . ? O9A K2 O13B 123.0(3) . . ? N5 K2 O13B 136.3(3) . . ? O9B K2 O11A 124.9(3) . . ? O16 K2 O11A 120.85(9) . . ? O13A K2 O11A 115.11(8) . . ? O9A K2 O11A 116.15(10) . . ? N5 K2 O11A 83.62(10) . . ? O13B K2 O11A 105.0(4) . . ? O9B K2 O12B 149.2(5) . . ? O16 K2 O12B 98.8(3) . . ? O13A K2 O12B 67.6(3) . . ? O9A K2 O12B 144.9(3) . . ? N5 K2 O12B 115.8(3) . . ? O13B K2 O12B 57.4(4) . . ? O11A K2 O12B 47.6(3) . . ? O9B K2 O12A 151.5(4) . . ? O16 K2 O12A 89.99(7) . . ? O13A K2 O12A 57.95(8) . . ? O9A K2 O12A 150.04(12) . . ? N5 K2 O12A 118.43(9) . . ? O13B K2 O12A 47.7(3) . . ? O11A K2 O12A 57.74(8) . . ? O12B K2 O12A 10.7(3) . . ? O9B K2 O10A 66.8(3) . . ? O16 K2 O10A 148.71(11) . . ? O13A K2 O10A 144.71(13) . . ? O9A K2 O10A 58.05(10) . . ? N5 K2 O10A 79.40(11) . . ? O13B K2 O10A 141.7(4) . . ? O11A K2 O10A 58.16(8) . . ? O12B K2 O10A 98.9(3) . . ? O12A K2 O10A 109.50(8) . . ? O9B K2 O11B 115.5(4) . . ? O16 K2 O11B 126.9(3) . . ? O13A K2 O11B 123.5(3) . . ? O9A K2 O11B 106.8(3) . . ? N5 K2 O11B 80.4(3) . . ? O13B K2 O11B 113.6(4) . . ? O11A K2 O11B 9.6(3) . . ? O12B K2 O11B 56.5(3) . . ? O12A K2 O11B 66.9(3) . . ? O10A K2 O11B 48.7(3) . . ? O9B K2 O10B 58.2(4) . . ? O16 K2 O10B 144.2(3) . . ? O13A K2 O10B 146.2(4) . . ? O9A K2 O10B 49.5(3) . . ? N5 K2 O10B 77.3(4) . . ? O13B K2 O10B 145.8(5) . . ? O11A K2 O10B 66.9(3) . . ? O12B K2 O10B 107.9(3) . . ? O12A K2 O10B 118.4(2) . . ? O10A K2 O10B 9.1(3) . . ? O11B K2 O10B 57.4(3) . . ? C3 O2 C2 110.80(10) . . ? C3 O2 K1 108.01(7) . . ? C2 O2 K1 105.65(7) . . ? C15 N2 K1 136.87(12) . . ? O2 C2 C1 109.66(11) . . ? O2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O21 K3 O17 116.12(3) . . ? O21 K3 O24 83.80(3) . . ? O17 K3 O24 83.63(3) . . ? O21 K3 N8 102.79(3) . . ? O17 K3 N8 128.05(3) . . ? O24 K3 N8 67.16(3) . . ? O21 K3 O20 58.50(2) . . ? O17 K3 O20 147.44(3) . . ? O24 K3 O20 124.34(3) . . ? N8 K3 O20 82.05(3) . . ? O21 K3 O19 115.57(3) . . ? O17 K3 O19 112.19(3) . . ? O24 K3 O19 141.98(3) . . ? N8 K3 O19 76.42(3) . . ? O20 K3 O19 57.66(2) . . ? O21 K3 O22 58.73(2) . . ? O17 K3 O22 57.50(2) . . ? O24 K3 O22 74.93(3) . . ? N8 K3 O22 139.67(3) . . ? O20 K3 O22 109.81(2) . . ? O19 K3 O22 142.97(2) . . ? O21 K3 O18 145.12(3) . . ? O17 K3 O18 56.98(2) . . ? O24 K3 O18 125.09(3) . . ? N8 K3 O18 106.41(3) . . ? O20 K3 O18 107.18(2) . . ? O19 K3 O18 55.37(2) . . ? O22 K3 O18 106.28(2) . . ? C5 O3 C4 111.45(10) . . ? C5 O3 K1 119.40(8) . . ? C4 O3 K1 120.09(7) . . ? O2 C3 C4 109.19(11) . . ? O2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? O29 K4 O32 84.95(3) . . ? O29 K4 O25 115.17(3) . . ? O32 K4 O25 83.26(3) . . ? O29 K4 O28 58.92(3) . . ? O32 K4 O28 124.97(3) . . ? O25 K4 O28 147.34(3) . . ? O29 K4 N11 104.56(3) . . ? O32 K4 N11 67.68(3) . . ? O25 K4 N11 127.94(3) . . ? O28 K4 N11 82.04(3) . . ? O29 K4 O27 115.80(3) . . ? O32 K4 O27 140.54(3) . . ? O25 K4 O27 113.01(3) . . ? O28 K4 O27 57.44(2) . . ? N11 K4 O27 74.48(3) . . ? O29 K4 O30 58.29(2) . . ? O32 K4 O30 76.22(3) . . ? O25 K4 O30 56.96(2) . . ? O28 K4 O30 109.70(3) . . ? N11 K4 O30 141.57(3) . . ? O27 K4 O30 143.10(2) . . ? O29 K4 O26 145.17(3) . . ? O32 K4 O26 123.80(3) . . ? O25 K4 O26 57.23(3) . . ? O28 K4 O26 107.40(3) . . ? N11 K4 O26 104.71(3) . . ? O27 K4 O26 55.97(2) . . ? O30 K4 O26 106.03(2) . . ? O29 K4 C55 42.25(3) . . ? O32 K4 C55 103.09(3) . . ? O25 K4 C55 154.15(3) . . ? O28 K4 C55 22.94(3) . . ? N11 K4 C55 76.81(4) . . ? O27 K4 C55 78.06(3) . . ? O30 K4 C55 99.72(3) . . ? O26 K4 C55 130.32(3) . . ? C6 O4 C7 112.11(11) . . ? C6 O4 K1 109.36(7) . . ? C7 O4 K1 105.05(8) . . ? C30 N4 H4N 121.8(10) . . ? C30 N4 H3N 117.3(10) . . ? H4N N4 H3N 119.9(14) . . ? O3 C4 C3 108.94(10) . . ? O3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? O3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C8 O5 C9 112.08(11) . . ? C8 O5 K1 121.93(8) . . ? C9 O5 K1 121.36(8) . . ? C31 N5 K2 129.63(10) . . ? O3 C5 C6 108.44(11) . . ? O3 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? O3 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C11 O6 C10 111.46(10) . . ? C11 O6 K1 101.29(7) . . ? C10 O6 K1 108.16(8) . . ? O4 C6 C5 108.61(11) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.3 . . ? C46 N7 H5N 116.6(10) . . ? C46 N7 H6N 119.7(10) . . ? H5N N7 H6N 120.6(14) . . ? O4 C7 C8 108.78(12) . . ? O4 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O4 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? K1 O8 H1O 120.8(12) . . ? K1 O8 H2O 133.6(13) . . ? H1O O8 H2O 104.7(17) . . ? C47 N8 K3 129.53(10) . . ? O5 C8 C7 108.61(13) . . ? O5 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O5 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? O5 C9 C10 108.49(12) . . ? O5 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O5 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C28A O9A C17A 112.2(4) . . ? C28A O9A K2 123.8(3) . . ? C17A O9A K2 120.7(3) . . ? C62 N10 H7N 116.3(10) . . ? C62 N10 H8N 120.2(11) . . ? H7N N10 H8N 119.5(14) . . ? O6 C10 C9 110.12(11) . . ? O6 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? O6 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? C19A O10A C18A 110.4(4) . . ? C19A O10A K2 109.8(3) . . ? C18A O10A K2 105.0(3) . . ? C63 N11 K4 127.68(10) . . ? O6 C11 C12 109.29(11) . . ? O6 C11 K1 55.30(6) . . ? C12 C11 K1 85.53(8) . . ? O6 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? K1 C11 H11A 72.7 . . ? O6 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? K1 C11 H11B 162.5 . . ? H11A C11 H11B 108.3 . . ? C21A O11A C20A 111.8(4) . . ? C21A O11A K2 118.9(3) . . ? C20A O11A K2 117.8(3) . . ? O1 C12 C11 108.87(11) . . ? O1 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? O1 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C23A O12A C22A 111.8(3) . . ? C23A O12A K2 106.5(2) . . ? C22A O12A K2 108.9(3) . . ? C16 C13 C15 118.96(11) . . ? C16 C13 C14 122.27(11) . . ? C15 C13 C14 118.69(12) . . ? C25A O13A C24A 112.7(4) . . ? C25A O13A K2 122.6(2) . . ? C24A O13A K2 121.0(2) . . ? O7 C14 N1 121.07(12) . . ? O7 C14 C13 121.78(11) . . ? N1 C14 C13 117.11(12) . . ? C26A O14A C27A 110.4(4) . . ? C26A O14A K2 105.3(3) . . ? C27A O14A K2 106.5(3) . . ? N2 C15 C13 178.81(17) . . ? K2 O16 H3O 128.7(11) . . ? K2 O16 H4O 128.8(13) . . ? H3O O16 H4O 102.4(17) . . ? N3 C16 C13 178.92(14) . . ? C44 O17 C33 111.33(10) . . ? C44 O17 K3 121.99(7) . . ? C33 O17 K3 122.96(7) . . ? O9A C17A C18A 110.0(4) . . ? O9A C17A H17A 109.7 . . ? C18A C17A H17A 109.7 . . ? O9A C17A H17B 109.7 . . ? C18A C17A H17B 109.7 . . ? H17A C17A H17B 108.2 . . ? C35 O18 C34 111.35(10) . . ? C35 O18 K3 113.10(7) . . ? C34 O18 K3 104.71(7) . . ? O10A C18A C17A 108.2(4) . . ? O10A C18A H18A 110.1 . . ? C17A C18A H18A 110.1 . . ? O10A C18A H18B 110.1 . . ? C17A C18A H18B 110.1 . . ? H18A C18A H18B 108.4 . . ? C37 O19 C36 111.37(9) . . ? C37 O19 K3 116.31(7) . . ? C36 O19 K3 121.19(7) . . ? O10A C19A C20A 108.9(4) . . ? O10A C19A H19A 109.9 . . ? C20A C19A H19A 109.9 . . ? O10A C19A H19B 109.9 . . ? C20A C19A H19B 109.9 . . ? H19A C19A H19B 108.3 . . ? C38 O20 C39 111.56(10) . . ? C38 O20 K3 109.73(7) . . ? C39 O20 K3 104.88(7) . . ? O11A C20A C19A 108.3(3) . . ? O11A C20A H20A 110.0 . . ? C19A C20A H20A 110.0 . . ? O11A C20A H20B 110.0 . . ? C19A C20A H20B 110.0 . . ? H20A C20A H20B 108.4 . . ? C41 O21 C40 111.87(10) . . ? C41 O21 K3 121.57(7) . . ? C40 O21 K3 121.13(7) . . ? O11A C21A C22A 108.9(4) . . ? O11A C21A H21A 109.9 . . ? C22A C21A H21A 109.9 . . ? O11A C21A H21B 109.9 . . ? C22A C21A H21B 109.9 . . ? H21A C21A H21B 108.3 . . ? C43 O22 C42 111.19(9) . . ? C43 O22 K3 104.17(7) . . ? C42 O22 K3 105.77(7) . . ? O12A C22A C21A 107.8(3) . . ? O12A C22A H22A 110.2 . . ? C21A C22A H22A 110.2 . . ? O12A C22A H22B 110.2 . . ? C21A C22A H22B 110.2 . . ? H22A C22A H22B 108.5 . . ? O12A C23A C24A 108.2(3) . . ? O12A C23A H23A 110.1 . . ? C24A C23A H23A 110.1 . . ? O12A C23A H23B 110.1 . . ? C24A C23A H23B 110.1 . . ? H23A C23A H23B 108.4 . . ? K3 O24 H6O 132.7(11) . . ? K3 O24 H5O 124.7(12) . . ? H6O O24 H5O 102.3(15) . . ? O13A C24A C23A 107.9(3) . . ? O13A C24A H24A 110.1 . . ? C23A C24A H24A 110.1 . . ? O13A C24A H24B 110.1 . . ? C23A C24A H24B 110.1 . . ? H24A C24A H24B 108.4 . . ? C60 O25 C49 110.85(10) . . ? C60 O25 K4 122.61(7) . . ? C49 O25 K4 122.17(7) . . ? O13A C25A C26A 107.0(4) . . ? O13A C25A H25A 110.3 . . ? C26A C25A H25A 110.3 . . ? O13A C25A H25B 110.3 . . ? C26A C25A H25B 110.3 . . ? H25A C25A H25B 108.6 . . ? C50 O26 C51 111.29(10) . . ? C50 O26 K4 104.69(7) . . ? C51 O26 K4 109.44(7) . . ? O14A C26A C25A 109.6(4) . . ? O14A C26A H26A 109.7 . . ? C25A C26A H26A 109.7 . . ? O14A C26A H26B 109.7 . . ? C25A C26A H26B 109.7 . . ? H26A C26A H26B 108.2 . . ? C53 O27 C52 111.84(10) . . ? C53 O27 K4 116.42(7) . . ? C52 O27 K4 120.20(7) . . ? O14A C27A C28A 109.4(5) . . ? O14A C27A H27A 109.8 . . ? C28A C27A H27A 109.8 . . ? O14A C27A H27B 109.8 . . ? C28A C27A H27B 109.8 . . ? H27A C27A H27B 108.2 . . ? C55 O28 C54 112.10(10) . . ? C55 O28 K4 104.96(7) . . ? C54 O28 K4 112.71(7) . . ? O9A C28A C27A 108.5(5) . . ? O9A C28A H28A 110.0 . . ? C27A C28A H28A 110.0 . . ? O9A C28A H28B 110.0 . . ? C27A C28A H28B 110.0 . . ? H28A C28A H28B 108.4 . . ? C57 O29 C56 111.53(10) . . ? C57 O29 K4 122.19(7) . . ? C56 O29 K4 120.18(7) . . ? C32 C29 C31 118.89(11) . . ? C32 C29 C30 121.28(11) . . ? C31 C29 C30 119.66(11) . . ? C59 O30 C58 111.42(9) . . ? C59 O30 K4 104.86(7) . . ? C58 O30 K4 106.24(7) . . ? O15 C30 N4 121.03(11) . . ? O15 C30 C29 122.24(11) . . ? N4 C30 C29 116.71(12) . . ? N5 C31 C29 179.13(15) . . ? K4 O32 H7O 122.0(12) . . ? K4 O32 H8O 131.2(12) . . ? H7O O32 H8O 106.7(16) . . ? N6 C32 C29 178.31(14) . . ? O17 C33 C34 108.73(11) . . ? O17 C33 H33A 109.9 . . ? C34 C33 H33A 109.9 . . ? O17 C33 H33B 109.9 . . ? C34 C33 H33B 109.9 . . ? H33A C33 H33B 108.3 . . ? O18 C34 C33 108.97(11) . . ? O18 C34 H34A 109.9 . . ? C33 C34 H34A 109.9 . . ? O18 C34 H34B 109.9 . . ? C33 C34 H34B 109.9 . . ? H34A C34 H34B 108.3 . . ? O18 C35 C36 108.80(11) . . ? O18 C35 H35A 109.9 . . ? C36 C35 H35A 109.9 . . ? O18 C35 H35B 109.9 . . ? C36 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? O19 C36 C35 108.25(10) . . ? O19 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? O19 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O19 C37 C38 108.90(10) . . ? O19 C37 H37A 109.9 . . ? C38 C37 H37A 109.9 . . ? O19 C37 H37B 109.9 . . ? C38 C37 H37B 109.9 . . ? H37A C37 H37B 108.3 . . ? O20 C38 C37 108.27(10) . . ? O20 C38 H38A 110.0 . . ? C37 C38 H38A 110.0 . . ? O20 C38 H38B 110.0 . . ? C37 C38 H38B 110.0 . . ? H38A C38 H38B 108.4 . . ? O20 C39 C40 108.61(11) . . ? O20 C39 H39A 110.0 . . ? C40 C39 H39A 110.0 . . ? O20 C39 H39B 110.0 . . ? C40 C39 H39B 110.0 . . ? H39A C39 H39B 108.3 . . ? O21 C40 C39 108.47(11) . . ? O21 C40 H40A 110.0 . . ? C39 C40 H40A 110.0 . . ? O21 C40 H40B 110.0 . . ? C39 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? O21 C41 C42 108.68(10) . . ? O21 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O21 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.3 . . ? O22 C42 C41 109.55(10) . . ? O22 C42 H42A 109.8 . . ? C41 C42 H42A 109.8 . . ? O22 C42 H42B 109.8 . . ? C41 C42 H42B 109.8 . . ? H42A C42 H42B 108.2 . . ? O22 C43 C44 109.30(10) . . ? O22 C43 H43A 109.8 . . ? C44 C43 H43A 109.8 . . ? O22 C43 H43B 109.8 . . ? C44 C43 H43B 109.8 . . ? H43A C43 H43B 108.3 . . ? O17 C44 C43 108.31(10) . . ? O17 C44 H44A 110.0 . . ? C43 C44 H44A 110.0 . . ? O17 C44 H44B 110.0 . . ? C43 C44 H44B 110.0 . . ? H44A C44 H44B 108.4 . . ? C48 C45 C47 118.46(11) . . ? C48 C45 C46 121.56(11) . . ? C47 C45 C46 119.79(11) . . ? O23 C46 N7 121.43(11) . . ? O23 C46 C45 121.71(11) . . ? N7 C46 C45 116.82(11) . . ? N8 C47 C45 179.74(17) . . ? N9 C48 C45 178.68(14) . . ? O25 C49 C50 108.78(11) . . ? O25 C49 H49A 109.9 . . ? C50 C49 H49A 109.9 . . ? O25 C49 H49B 109.9 . . ? C50 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? O26 C50 C49 109.25(11) . . ? O26 C50 H50A 109.8 . . ? C49 C50 H50A 109.8 . . ? O26 C50 H50B 109.8 . . ? C49 C50 H50B 109.8 . . ? H50A C50 H50B 108.3 . . ? O26 C51 C52 108.81(11) . . ? O26 C51 H51A 109.9 . . ? C52 C51 H51A 109.9 . . ? O26 C51 H51B 109.9 . . ? C52 C51 H51B 109.9 . . ? H51A C51 H51B 108.3 . . ? O27 C52 C51 107.99(10) . . ? O27 C52 H52A 110.1 . . ? C51 C52 H52A 110.1 . . ? O27 C52 H52B 110.1 . . ? C51 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? O27 C53 C54 108.65(10) . . ? O27 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? O27 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.3 . . ? O28 C54 C53 108.13(10) . . ? O28 C54 H54A 110.1 . . ? C53 C54 H54A 110.1 . . ? O28 C54 H54B 110.1 . . ? C53 C54 H54B 110.1 . . ? H54A C54 H54B 108.4 . . ? O28 C55 C56 108.46(11) . . ? O28 C55 K4 52.10(6) . . ? C56 C55 K4 85.05(7) . . ? O28 C55 H55A 110.0 . . ? C56 C55 H55A 110.0 . . ? K4 C55 H55A 76.0 . . ? O28 C55 H55B 110.0 . . ? C56 C55 H55B 110.0 . . ? K4 C55 H55B 160.7 . . ? H55A C55 H55B 108.4 . . ? O29 C56 C55 108.65(11) . . ? O29 C56 H56A 110.0 . . ? C55 C56 H56A 110.0 . . ? O29 C56 H56B 110.0 . . ? C55 C56 H56B 110.0 . . ? H56A C56 H56B 108.3 . . ? O29 C57 C58 108.87(10) . . ? O29 C57 H57A 109.9 . . ? C58 C57 H57A 109.9 . . ? O29 C57 H57B 109.9 . . ? C58 C57 H57B 109.9 . . ? H57A C57 H57B 108.3 . . ? O30 C58 C57 109.26(10) . . ? O30 C58 H58A 109.8 . . ? C57 C58 H58A 109.8 . . ? O30 C58 H58B 109.8 . . ? C57 C58 H58B 109.8 . . ? H58A C58 H58B 108.3 . . ? O30 C59 C60 109.04(10) . . ? O30 C59 H59A 109.9 . . ? C60 C59 H59A 109.9 . . ? O30 C59 H59B 109.9 . . ? C60 C59 H59B 109.9 . . ? H59A C59 H59B 108.3 . . ? O25 C60 C59 108.62(10) . . ? O25 C60 H60A 110.0 . . ? C59 C60 H60A 110.0 . . ? O25 C60 H60B 110.0 . . ? C59 C60 H60B 110.0 . . ? H60A C60 H60B 108.3 . . ? C64 C61 C63 118.97(11) . . ? C64 C61 C62 121.35(11) . . ? C63 C61 C62 119.45(11) . . ? O31 C62 N10 121.43(11) . . ? O31 C62 C61 121.40(11) . . ? N10 C62 C61 117.14(11) . . ? N11 C63 C61 179.80(15) . . ? N12 C64 C61 178.51(14) . . ? O11B C20B C19B 110.5(14) . . ? O11B C20B H20C 109.6 . . ? C19B C20B H20C 109.6 . . ? O11B C20B H20D 109.6 . . ? C19B C20B H20D 109.6 . . ? H20C C20B H20D 108.1 . . ? C18B O10B C19B 114.4(16) . . ? C18B O10B K2 103.4(11) . . ? C19B O10B K2 107.4(12) . . ? C23B O12B C22B 110.0(15) . . ? C23B O12B K2 108.5(12) . . ? C22B O12B K2 112.0(9) . . ? O12B C22B C21B 106.1(13) . . ? O12B C22B H22C 110.5 . . ? C21B C22B H22C 110.5 . . ? O12B C22B H22D 110.5 . . ? C21B C22B H22D 110.5 . . ? H22C C22B H22D 108.7 . . ? O10B C19B C20B 108.8(17) . . ? O10B C19B H19C 109.9 . . ? C20B C19B H19C 109.9 . . ? O10B C19B H19D 109.9 . . ? C20B C19B H19D 109.9 . . ? H19C C19B H19D 108.3 . . ? C20B O11B C21B 113.8(13) . . ? C20B O11B K2 116.9(10) . . ? C21B O11B K2 116.8(11) . . ? C27B O14B C26B 114.8(19) . . ? C27B O14B K2 101.3(11) . . ? C26B O14B K2 106.1(11) . . ? O11B C21B C22B 106.6(14) . . ? O11B C21B H21C 110.4 . . ? C22B C21B H21C 110.4 . . ? O11B C21B H21D 110.4 . . ? C22B C21B H21D 110.4 . . ? H21C C21B H21D 108.6 . . ? C25B O13B C24B 111.7(14) . . ? C25B O13B K2 123.7(10) . . ? C24B O13B K2 118.1(10) . . ? O14B C26B C25B 117.4(17) . . ? O14B C26B H26C 107.9 . . ? C25B C26B H26C 107.9 . . ? O14B C26B H26D 107.9 . . ? C25B C26B H26D 107.9 . . ? H26C C26B H26D 107.2 . . ? O10B C18B C17B 112.4(17) . . ? O10B C18B H18C 109.1 . . ? C17B C18B H18C 109.1 . . ? O10B C18B H18D 109.1 . . ? C17B C18B H18D 109.1 . . ? H18C C18B H18D 107.9 . . ? C17B O9B C28B 107.1(18) . . ? C17B O9B K2 123.8(14) . . ? C28B O9B K2 122.0(11) . . ? O13B C25B C26B 102.8(15) . . ? O13B C25B H25C 111.2 . . ? C26B C25B H25C 111.2 . . ? O13B C25B H25D 111.2 . . ? C26B C25B H25D 111.2 . . ? H25C C25B H25D 109.1 . . ? O9B C17B C18B 105.2(18) . . ? O9B C17B H17C 110.7 . . ? C18B C17B H17C 110.7 . . ? O9B C17B H17D 110.7 . . ? C18B C17B H17D 110.7 . . ? H17C C17B H17D 108.8 . . ? O9B C28B C27B 106.4(15) . . ? O9B C28B H28C 110.5 . . ? C27B C28B H28C 110.5 . . ? O9B C28B H28D 110.5 . . ? C27B C28B H28D 110.5 . . ? H28C C28B H28D 108.6 . . ? O13B C24B C23B 111.0(16) . . ? O13B C24B H24C 109.4 . . ? C23B C24B H24C 109.4 . . ? O13B C24B H24D 109.4 . . ? C23B C24B H24D 109.4 . . ? H24C C24B H24D 108.0 . . ? O12B C23B C24B 109.6(16) . . ? O12B C23B H23C 109.7 . . ? C24B C23B H23C 109.7 . . ? O12B C23B H23D 109.7 . . ? C24B C23B H23D 109.7 . . ? H23C C23B H23D 108.2 . . ? O14B C27B C28B 111.5(17) . . ? O14B C27B K2 56.0(10) . . ? C28B C27B K2 85.4(10) . . ? O14B C27B H27C 109.3 . . ? C28B C27B H27C 109.3 . . ? K2 C27B H27C 73.1 . . ? O14B C27B H27D 109.3 . . ? C28B C27B H27D 109.3 . . ? K2 C27B H27D 163.2 . . ? H27C C27B H27D 108.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N10 H7N N6 0.865(16) 2.175(16) 3.0402(16) 178.5(14) . N7 H5N N3 0.841(16) 2.218(16) 3.0577(16) 175.5(14) . O24 H6O N12 0.847(18) 2.174(18) 3.0180(15) 174.1(15) 1_545 N1 H2N O23 0.846(17) 2.183(17) 2.9725(15) 155.1(14) . N4 H4N O31 0.850(16) 2.145(16) 2.9202(15) 151.3(13) . N1 H1N N12 0.869(16) 2.162(16) 3.0303(16) 178.0(14) 1_545 N4 H3N N9 0.854(16) 2.179(17) 3.0331(16) 177.7(15) . O32 H7O O31 0.833(17) 2.035(18) 2.8575(13) 169.6(16) . N7 H6N O15 0.861(17) 2.199(17) 2.9813(15) 151.0(14) . O24 H5O O23 0.842(18) 2.009(18) 2.8441(13) 171.2(16) . N10 H8N O7 0.862(17) 2.181(17) 2.9673(15) 151.5(14) 1_565 O32 H8O N9 0.848(19) 2.170(19) 3.0165(15) 175.8(17) . O16 H3O O15 0.862(18) 1.975(18) 2.8345(13) 175.0(16) . O8 H1O O7 0.91(2) 1.99(2) 2.8936(14) 169.9(17) . O16 H4O N3 0.787(19) 2.379(19) 3.1428(16) 163.8(17) . O8 H2O N6 0.90(2) 2.25(2) 3.1296(16) 166.3(18) 1_545 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.363 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.041