Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Patrick Holland' _publ_contact_author_address ; Department of Chemistry University of Rochester Rochester New York 14627 UNITED STATES OF AMERICA ; _publ_contact_author_email HOLLAND@CHEM.ROCHESTER.EDU _publ_section_title ; A Dinucleating Ligand Related to the Beta-Diketiminates ; loop_ _publ_author_name 'Patrick Holland' 'William W. Brennessel' 'Christine J. Flaschenriem' 'Travis J. Hebden' # Attachment 'Travis.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 608908' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HolTH02 _chemical_melting_point ? _chemical_formula_moiety 'C44 H60 N4' _chemical_formula_sum 'C44 H60 N4' _chemical_formula_weight 644.96 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.384(3) _cell_length_b 17.457(3) _cell_length_c 13.119(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.347(3) _cell_angle_gamma 90.00 _cell_volume 3916.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 6457 _cell_measurement_theta_min 2.3335 _cell_measurement_theta_max 27.7935 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.986 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25674 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.40 _reflns_number_total 4921 _reflns_number_gt 3847 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0836P)^2^+1.8746P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4921 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N11 N 0.03894(6) 0.44071(6) 0.77212(7) 0.0217(2) Uani 1 1 d . . . N3 N 0.22244(6) 0.36872(6) 0.85072(7) 0.0224(2) Uani 1 1 d . . . C31 C 0.04024(7) 0.57870(6) 0.77205(8) 0.0199(2) Uani 1 1 d . . . C41 C 0.07653(7) 0.50526(7) 0.79289(8) 0.0196(2) Uani 1 1 d . . . C61 C 0.18206(7) 0.41863(7) 0.88807(8) 0.0204(2) Uani 1 1 d . . . C12 C 0.25346(7) 0.37951(7) 0.75899(9) 0.0237(3) Uani 1 1 d . . . C21 C 0.07991(8) 0.64933(7) 0.79220(9) 0.0253(3) Uani 1 1 d . . . H21 H 0.1342 0.6499 0.8206 0.030 Uiso 1 1 calc R . . C51 C 0.16213(7) 0.49732(7) 0.84090(9) 0.0219(2) Uani 1 1 d . . . H51A H 0.1757 0.5367 0.8954 0.026 Uiso 1 1 calc R . . H51B H 0.1943 0.5069 0.7871 0.026 Uiso 1 1 calc R . . C62 C 0.21602(8) 0.34333(7) 0.66721(9) 0.0269(3) Uani 1 1 d . . . C71 C 0.15896(7) 0.39968(7) 0.99284(9) 0.0247(3) Uani 1 1 d . . . C22 C 0.32533(8) 0.41760(7) 0.76412(11) 0.0289(3) Uani 1 1 d . . . C32 C 0.35889(9) 0.41984(8) 0.67524(12) 0.0373(3) Uani 1 1 d . . . H32 H 0.4074 0.4454 0.6773 0.045 Uiso 1 1 calc R . . C72 C 0.36642(8) 0.45135(8) 0.86612(12) 0.0340(3) Uani 1 1 d . . . H72 H 0.3249 0.4708 0.9033 0.041 Uiso 1 1 calc R . . C52 C 0.25231(10) 0.34777(8) 0.58050(10) 0.0360(3) Uani 1 1 d . . . H52 H 0.2280 0.3243 0.5176 0.043 Uiso 1 1 calc R . . C102 C 0.14219(8) 0.29803(8) 0.66774(10) 0.0309(3) Uani 1 1 d . . . H102 H 0.1101 0.3267 0.7111 0.037 Uiso 1 1 calc R . . C81 C 0.23085(9) 0.41636(10) 1.07601(10) 0.0409(4) Uani 1 1 d . . . H81A H 0.2194 0.4032 1.1444 0.061 Uiso 1 1 calc R . . H81B H 0.2440 0.4709 1.0744 0.061 Uiso 1 1 calc R . . H81C H 0.2751 0.3856 1.0625 0.061 Uiso 1 1 calc R . . C42 C 0.32267(10) 0.38538(9) 0.58409(12) 0.0410(4) Uani 1 1 d . . . H42 H 0.3462 0.3876 0.5241 0.049 Uiso 1 1 calc R . . C112 C 0.16299(10) 0.22042(8) 0.71949(13) 0.0418(4) Uani 1 1 d . . . H11A H 0.1917 0.1896 0.6763 0.063 Uiso 1 1 calc R . . H11B H 0.1149 0.1936 0.7276 0.063 Uiso 1 1 calc R . . H11C H 0.1957 0.2283 0.7877 0.063 Uiso 1 1 calc R . . C91 C 0.09063(10) 0.44721(10) 1.01640(11) 0.0422(4) Uani 1 1 d . . . H91A H 0.0441 0.4371 0.9638 0.063 Uiso 1 1 calc R . . H91B H 0.1039 0.5017 1.0157 0.063 Uiso 1 1 calc R . . H91C H 0.0800 0.4333 1.0849 0.063 Uiso 1 1 calc R . . C122 C 0.09206(10) 0.28716(10) 0.56049(12) 0.0459(4) Uani 1 1 d . . . H12A H 0.0788 0.3373 0.5286 0.069 Uiso 1 1 calc R . . H12B H 0.0439 0.2599 0.5671 0.069 Uiso 1 1 calc R . . H12C H 0.1213 0.2573 0.5169 0.069 Uiso 1 1 calc R . . C101 C 0.13868(11) 0.31494(9) 0.99669(12) 0.0422(4) Uani 1 1 d . . . H10A H 0.1235 0.3032 1.0634 0.063 Uiso 1 1 calc R . . H10B H 0.1843 0.2841 0.9888 0.063 Uiso 1 1 calc R . . H10C H 0.0952 0.3030 0.9404 0.063 Uiso 1 1 calc R . . C82 C 0.41073(10) 0.38825(10) 0.93364(14) 0.0512(4) Uani 1 1 d . . . H82A H 0.3749 0.3461 0.9408 0.077 Uiso 1 1 calc R . . H82B H 0.4322 0.4091 1.0022 0.077 Uiso 1 1 calc R . . H82C H 0.4535 0.3692 0.9010 0.077 Uiso 1 1 calc R . . C92 C 0.41977(10) 0.51848(10) 0.85435(16) 0.0504(4) Uani 1 1 d . . . H92A H 0.4655 0.5001 0.8273 0.076 Uiso 1 1 calc R . . H92B H 0.4370 0.5427 0.9220 0.076 Uiso 1 1 calc R . . H92C H 0.3913 0.5559 0.8061 0.076 Uiso 1 1 calc R . . C11 C 0.04007(8) 0.71699(7) 0.77068(10) 0.0312(3) Uani 1 1 d . . . H11 H 0.0671 0.7643 0.7840 0.037 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 N11 0.0245(5) 0.0241(5) 0.0158(4) -0.0005(4) 0.0019(4) 0.0005(4) N3 0.0240(5) 0.0266(5) 0.0160(5) -0.0007(4) 0.0026(4) 0.0002(4) C31 0.0286(6) 0.0224(6) 0.0090(5) -0.0003(4) 0.0044(4) -0.0005(4) C41 0.0252(5) 0.0245(6) 0.0096(4) -0.0005(4) 0.0047(4) 0.0001(4) C61 0.0208(5) 0.0257(6) 0.0138(5) -0.0007(4) 0.0005(4) -0.0013(4) C12 0.0297(6) 0.0230(6) 0.0194(5) 0.0005(4) 0.0076(5) 0.0053(5) C21 0.0328(6) 0.0264(6) 0.0159(5) -0.0008(4) 0.0019(4) -0.0034(5) C51 0.0249(6) 0.0235(6) 0.0175(5) -0.0017(4) 0.0039(4) -0.0010(4) C62 0.0372(7) 0.0253(6) 0.0186(6) -0.0001(4) 0.0062(5) 0.0088(5) C71 0.0307(6) 0.0295(6) 0.0140(5) 0.0003(4) 0.0048(4) 0.0023(5) C22 0.0307(6) 0.0256(6) 0.0329(7) 0.0003(5) 0.0122(5) 0.0052(5) C32 0.0394(7) 0.0323(7) 0.0468(9) 0.0054(6) 0.0254(7) 0.0053(6) C72 0.0262(6) 0.0327(7) 0.0435(8) -0.0059(6) 0.0075(6) -0.0001(5) C52 0.0571(9) 0.0321(7) 0.0215(6) -0.0005(5) 0.0144(6) 0.0122(6) C102 0.0366(7) 0.0318(7) 0.0232(6) -0.0079(5) 0.0025(5) 0.0039(5) C81 0.0456(8) 0.0584(10) 0.0154(6) 0.0033(6) -0.0032(5) -0.0044(7) C42 0.0597(10) 0.0348(7) 0.0365(8) 0.0055(6) 0.0302(7) 0.0119(7) C112 0.0493(9) 0.0310(7) 0.0430(8) -0.0033(6) 0.0029(7) -0.0051(7) C91 0.0524(9) 0.0589(10) 0.0192(6) 0.0083(6) 0.0170(6) 0.0213(8) C122 0.0460(9) 0.0547(10) 0.0325(8) -0.0176(7) -0.0052(6) 0.0115(7) C101 0.0621(10) 0.0376(8) 0.0332(7) -0.0016(6) 0.0254(7) -0.0121(7) C82 0.0460(9) 0.0456(9) 0.0541(10) -0.0039(8) -0.0123(8) -0.0004(7) C92 0.0373(8) 0.0382(9) 0.0796(13) -0.0138(8) 0.0205(8) -0.0054(7) C11 0.0461(8) 0.0224(6) 0.0228(6) -0.0009(5) 0.0003(5) -0.0050(5) _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 N11 C41 1.3066(15) . ? N11 N11 1.374(2) 2_556 ? N3 C61 1.2710(15) . ? N3 C12 1.4169(15) . ? C31 C21 1.4142(17) . ? C31 C31 1.415(2) 2_556 ? C31 C41 1.4332(16) . ? C41 C51 1.5144(16) . ? C61 C51 1.5208(16) . ? C61 C71 1.5356(16) . ? C12 C22 1.4063(18) . ? C12 C62 1.4109(17) . ? C21 C11 1.3726(18) . ? C62 C52 1.3985(18) . ? C62 C102 1.509(2) . ? C71 C101 1.524(2) . ? C71 C91 1.5253(19) . ? C71 C81 1.5321(19) . ? C22 C32 1.3949(19) . ? C22 C72 1.518(2) . ? C32 C42 1.385(2) . ? C72 C92 1.519(2) . ? C72 C82 1.532(2) . ? C52 C42 1.381(2) . ? C102 C122 1.5279(19) . ? C102 C112 1.529(2) . ? C11 C11 1.401(3) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 N11 N11 120.40(7) . 2_556 ? C61 N3 C12 123.86(10) . . ? C21 C31 C31 119.32(7) . 2_556 ? C21 C31 C41 124.12(11) . . ? C31 C31 C41 116.56(7) 2_556 . ? N11 C41 C31 123.04(11) . . ? N11 C41 C51 115.14(10) . . ? C31 C41 C51 121.82(10) . . ? N3 C61 C51 124.30(10) . . ? N3 C61 C71 116.66(10) . . ? C51 C61 C71 118.79(10) . . ? C22 C12 C62 121.48(11) . . ? C22 C12 N3 119.51(11) . . ? C62 C12 N3 118.54(11) . . ? C11 C21 C31 120.04(12) . . ? C41 C51 C61 112.77(10) . . ? C52 C62 C12 117.58(13) . . ? C52 C62 C102 122.77(12) . . ? C12 C62 C102 119.55(11) . . ? C101 C71 C91 109.16(12) . . ? C101 C71 C81 108.96(12) . . ? C91 C71 C81 108.52(12) . . ? C101 C71 C61 109.76(10) . . ? C91 C71 C61 113.73(10) . . ? C81 C71 C61 106.59(11) . . ? C32 C22 C12 118.33(13) . . ? C32 C22 C72 121.65(13) . . ? C12 C22 C72 119.93(11) . . ? C42 C32 C22 121.06(14) . . ? C22 C72 C92 114.13(14) . . ? C22 C72 C82 109.80(12) . . ? C92 C72 C82 111.14(13) . . ? C42 C52 C62 121.64(14) . . ? C62 C102 C122 113.94(12) . . ? C62 C102 C112 109.44(12) . . ? C122 C102 C112 110.43(12) . . ? C52 C42 C32 119.90(13) . . ? C21 C11 C11 120.62(8) . 2_556 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.476 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.056 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 608909' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common holph18 _chemical_melting_point ? _chemical_formula_moiety 'C88 H116 K4 N8, C4 H10 O' _chemical_formula_sum 'C92 H126 K4 N8 O' _chemical_formula_weight 1516.41 _chemical_absolute_configuration ad 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 trigonal _symmetry_space_group_name_H-M 'P 32 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 14.1939(7) _cell_length_b 14.1939(7) _cell_length_c 37.812(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6597.2(8) _cell_formula_units_Z 3 _cell_measurement_temperature 223.0(5) _cell_measurement_reflns_used 3946 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 24.04 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2454 _exptl_absorpt_coefficient_mu 0.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9239 _exptl_absorpt_correction_T_max 0.9851 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223.0(5) _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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64605 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 30.49 _reflns_number_total 13293 _reflns_number_gt 8093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SIR97, CNR-IC' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0709P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), 5870 Friedel pairs, Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_number_reflns 13293 _refine_ls_number_parameters 518 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1370 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.35450(4) 0.46999(4) -0.053193(13) 0.04401(12) Uani 1 1 d . A . K2 K 0.21844(5) 0.21844(5) 0.0000 0.05010(19) Uani 1 2 d S . . K3 K 0.60689(5) 0.60689(5) 0.0000 0.04530(17) Uani 1 2 d S A . N1 N 0.25274(14) 0.20047(14) 0.07030(4) 0.0383(4) Uani 1 1 d . A . N2 N 0.31670(14) 0.41907(14) 0.03360(5) 0.0411(4) Uani 1 1 d . A . N3 N 0.39355(15) 0.52163(14) 0.02156(5) 0.0414(4) Uani 1 1 d . . . N4 N 0.50372(15) 0.69003(14) -0.04123(5) 0.0406(4) Uani 1 1 d . . . C1 C 0.16487(16) 0.20824(19) 0.07740(5) 0.0428(5) Uani 1 1 d . A . C2 C 0.15759(19) 0.2985(2) 0.06808(6) 0.0507(6) Uani 1 1 d . A . H2A H 0.0871 0.2885 0.0701 0.061 Uiso 1 1 calc R . . C3 C 0.23798(17) 0.40573(19) 0.05575(6) 0.0420(5) Uani 1 1 d . A . C4 C 0.22859(19) 0.4987(2) 0.06687(6) 0.0468(5) Uani 1 1 d . . . C5 C 0.1477(2) 0.4909(3) 0.09016(7) 0.0661(7) Uani 1 1 d . A . H5A H 0.0980 0.4231 0.1000 0.079 Uiso 1 1 calc R . . C6 C 0.1403(3) 0.5798(3) 0.09865(9) 0.0861(10) Uani 1 1 d . . . H6A H 0.0855 0.5729 0.1142 0.103 Uiso 1 1 calc R A . C7 C 0.2125(3) 0.6801(3) 0.08470(9) 0.0900(11) Uani 1 1 d . A . H7A H 0.2054 0.7406 0.0904 0.108 Uiso 1 1 calc R . . C8 C 0.2949(3) 0.6931(3) 0.06255(8) 0.0727(8) Uani 1 1 d . . . H8A H 0.3442 0.7621 0.0534 0.087 Uiso 1 1 calc R A . C9 C 0.3047(2) 0.6017(2) 0.05364(6) 0.0473(5) Uani 1 1 d . A . C10 C 0.39140(19) 0.61054(18) 0.03071(5) 0.0422(5) Uani 1 1 d . A . C11 C 0.4760(2) 0.71803(18) 0.01912(6) 0.0473(5) Uani 1 1 d . . . H11A H 0.5046 0.7704 0.0372 0.057 Uiso 1 1 calc R A . C12 C 0.52173(18) 0.75649(17) -0.01388(6) 0.0436(5) Uani 1 1 d . A . C13 C 0.05635(19) 0.1112(2) 0.09271(7) 0.0635(7) Uani 1 1 d . . . C14 C 0.0680(2) 0.0219(3) 0.10951(9) 0.0804(10) Uani 1 1 d . A . H14A H -0.0026 -0.0353 0.1174 0.121 Uiso 1 1 calc R . . H14B H 0.1169 0.0507 0.1296 0.121 Uiso 1 1 calc R . . H14C H 0.0974 -0.0075 0.0924 0.121 Uiso 1 1 calc R . . C15 C 0.0056(3) 0.1497(3) 0.12127(10) 0.1056(14) Uani 1 1 d . A . H15A H -0.0480 0.0875 0.1346 0.158 Uiso 1 1 calc R . . H15B H -0.0293 0.1858 0.1101 0.158 Uiso 1 1 calc R . . H15C H 0.0621 0.2001 0.1371 0.158 Uiso 1 1 calc R . . C16 C -0.0225(3) 0.0641(3) 0.06173(10) 0.1163(17) Uani 1 1 d . A . H16A H -0.0928 0.0076 0.0702 0.174 Uiso 1 1 calc R . . H16B H 0.0055 0.0335 0.0446 0.174 Uiso 1 1 calc R . . H16C H -0.0306 0.1213 0.0506 0.174 Uiso 1 1 calc R . . C17 C 0.6089(2) 0.88091(18) -0.01539(8) 0.0582(7) Uani 1 1 d . . . C18 C 0.6398(3) 0.9281(2) -0.05217(10) 0.0926(12) Uani 1 1 d . A . H18A H 0.6942 1.0046 -0.0506 0.139 Uiso 1 1 calc R . . H18B H 0.5759 0.9200 -0.0642 0.139 Uiso 1 1 calc R . . H18C H 0.6692 0.8898 -0.0653 0.139 Uiso 1 1 calc R . . C19 C 0.5719(4) 0.9504(3) 0.00454(14) 0.1386(19) Uani 1 1 d . A . H19A H 0.6238 1.0268 0.0007 0.208 Uiso 1 1 calc R . . H19B H 0.5676 0.9345 0.0296 0.208 Uiso 1 1 calc R . . H19C H 0.5009 0.9342 -0.0040 0.208 Uiso 1 1 calc R . . C20 C 0.7117(3) 0.8908(3) 0.00134(12) 0.1096(15) Uani 1 1 d . A . H20A H 0.7688 0.9665 0.0015 0.164 Uiso 1 1 calc R . . H20B H 0.7355 0.8485 -0.0123 0.164 Uiso 1 1 calc R . . H20C H 0.6961 0.8636 0.0254 0.164 Uiso 1 1 calc R . . C21 C 0.29624(17) 0.14724(18) 0.09005(6) 0.0409(5) Uani 1 1 d . . . C22 C 0.32321(19) 0.07620(19) 0.07326(6) 0.0489(5) Uani 1 1 d . A . C23 C 0.3842(2) 0.0390(3) 0.09117(8) 0.0668(8) Uani 1 1 d . . . H23A H 0.4030 -0.0078 0.0795 0.080 Uiso 1 1 calc R A . C24 C 0.4172(3) 0.0693(3) 0.12527(8) 0.0863(11) Uani 1 1 d . A . H24A H 0.4588 0.0442 0.1370 0.104 Uiso 1 1 calc R . . C25 C 0.3887(3) 0.1362(3) 0.14196(7) 0.0825(10) Uani 1 1 d . . . H25A H 0.4107 0.1555 0.1656 0.099 Uiso 1 1 calc R A . C26 C 0.3290(2) 0.1773(2) 0.12605(6) 0.0545(6) Uani 1 1 d . A . C27 C 0.3030(2) 0.2550(3) 0.14554(6) 0.0641(8) Uani 1 1 d . . . H27A H 0.2340 0.2445 0.1355 0.077 Uiso 1 1 calc R A . C28 C 0.2841(3) 0.2333(3) 0.18505(7) 0.0873(11) Uani 1 1 d . A . H28A H 0.2312 0.1573 0.1889 0.131 Uiso 1 1 calc R . . H28B H 0.2571 0.2784 0.1949 0.131 Uiso 1 1 calc R . . H28C H 0.3521 0.2506 0.1965 0.131 Uiso 1 1 calc R . . C29 C 0.3873(4) 0.3718(3) 0.13917(10) 0.1050(13) Uani 1 1 d . A . H29A H 0.3871 0.3891 0.1144 0.158 Uiso 1 1 calc R . . H29B H 0.4584 0.3833 0.1456 0.158 Uiso 1 1 calc R . . H29C H 0.3707 0.4184 0.1534 0.158 Uiso 1 1 calc R . . C30 C 0.2883(3) 0.0381(2) 0.03553(8) 0.0655(7) Uani 0.625(5) 1 d PD A 1 H30A H 0.2397 0.0655 0.0278 0.079 Uiso 0.625(5) 1 calc PR A 1 C31 C 0.3740(5) 0.0733(5) 0.01021(15) 0.0730(14) Uani 0.625(5) 1 d PD A 1 H31A H 0.3440 0.0401 -0.0125 0.109 Uiso 0.625(5) 1 calc PR A 1 H31B H 0.4258 0.0519 0.0180 0.109 Uiso 0.625(5) 1 calc PR A 1 H31C H 0.4105 0.1519 0.0080 0.109 Uiso 0.625(5) 1 calc PR A 1 C32 C 0.2175(5) -0.0933(4) 0.03608(16) 0.0909(14) Uani 0.625(5) 1 d PD A 1 H32A H 0.1613 -0.1166 0.0540 0.136 Uiso 0.625(5) 1 calc PR A 1 H32B H 0.2646 -0.1226 0.0415 0.136 Uiso 0.625(5) 1 calc PR A 1 H32C H 0.1841 -0.1195 0.0131 0.136 Uiso 0.625(5) 1 calc PR A 1 C30' C 0.2883(3) 0.0381(2) 0.03553(8) 0.0655(7) Uani 0.375(5) 1 d PD A 5 H30B H 0.2999 0.1072 0.0252 0.079 Uiso 0.375(5) 1 calc PR A 5 C31' C 0.3722(9) 0.0250(9) 0.0140(3) 0.0730(14) Uani 0.375(5) 1 d PD A 5 H31D H 0.4444 0.0855 0.0188 0.109 Uiso 0.375(5) 1 calc PR A 5 H31E H 0.3563 0.0237 -0.0110 0.109 Uiso 0.375(5) 1 calc PR A 5 H31F H 0.3692 -0.0426 0.0205 0.109 Uiso 0.375(5) 1 calc PR A 5 C32' C 0.1795(7) -0.0303(7) 0.0252(3) 0.0909(14) Uani 0.375(5) 1 d PD A 5 H32D H 0.1769 -0.0460 0.0001 0.136 Uiso 0.375(5) 1 calc PR A 5 H32E H 0.1379 0.0056 0.0298 0.136 Uiso 0.375(5) 1 calc PR A 5 H32F H 0.1488 -0.0977 0.0385 0.136 Uiso 0.375(5) 1 calc PR A 5 C33 C 0.49412(18) 0.71157(17) -0.07694(6) 0.0434(5) Uani 1 1 d . A . C34 C 0.4127(2) 0.73522(19) -0.08830(7) 0.0531(6) Uani 1 1 d . . . C35 C 0.3966(3) 0.7404(3) -0.12452(9) 0.0750(8) Uani 1 1 d . A . H35A H 0.3435 0.7569 -0.1321 0.090 Uiso 1 1 calc R . . C36 C 0.4560(3) 0.7221(3) -0.14916(8) 0.0835(10) Uani 1 1 d . . . H36A H 0.4418 0.7241 -0.1733 0.100 Uiso 1 1 calc R A . C37 C 0.5367(3) 0.7009(3) -0.13878(7) 0.0696(8) Uani 1 1 d . A . H37A H 0.5783 0.6899 -0.1559 0.083 Uiso 1 1 calc R . . C38 C 0.5566(2) 0.6956(2) -0.10283(7) 0.0518(6) Uani 1 1 d . . . C39 C 0.6497(2) 0.6776(3) -0.09242(7) 0.0678(8) Uani 1 1 d . A . H39A H 0.6589 0.6878 -0.0665 0.081 Uiso 1 1 calc R . . C40 C 0.6300(3) 0.5669(3) -0.10031(11) 0.0922(11) Uani 1 1 d . . . H40A H 0.5636 0.5134 -0.0887 0.138 Uiso 1 1 calc R A . H40B H 0.6906 0.5599 -0.0917 0.138 Uiso 1 1 calc R . . H40C H 0.6230 0.5549 -0.1257 0.138 Uiso 1 1 calc R . . C41 C 0.7574(3) 0.7617(3) -0.10941(16) 0.1291(17) Uani 1 1 d . . . H41A H 0.8171 0.7587 -0.0981 0.194 Uiso 1 1 calc R A . H41B H 0.7669 0.8338 -0.1065 0.194 Uiso 1 1 calc R . . H41C H 0.7563 0.7457 -0.1344 0.194 Uiso 1 1 calc R . . C42 C 0.3425(2) 0.7535(2) -0.06201(8) 0.0627(7) Uani 1 1 d . A . H42A H 0.3902 0.7926 -0.0417 0.075 Uiso 1 1 calc R . . C43 C 0.2519(3) 0.6493(3) -0.04753(11) 0.0933(11) Uani 1 1 d . . . H43A H 0.2820 0.6110 -0.0348 0.140 Uiso 1 1 calc R A . H43B H 0.2069 0.6043 -0.0668 0.140 Uiso 1 1 calc R . . H43C H 0.2081 0.6651 -0.0316 0.140 Uiso 1 1 calc R . . C44 C 0.2984(4) 0.8252(3) -0.07556(11) 0.1001(12) Uani 1 1 d . . . H44A H 0.3568 0.8897 -0.0866 0.150 Uiso 1 1 calc R A . H44B H 0.2691 0.8464 -0.0559 0.150 Uiso 1 1 calc R . . H44C H 0.2414 0.7851 -0.0928 0.150 Uiso 1 1 calc R . . C45 C 0.580(2) -0.0815(19) 0.1108(5) 0.129(4) Uani 0.272(7) 1 d PD B -1 H45A H 0.6162 -0.0978 0.0919 0.194 Uiso 0.272(7) 1 calc PR B -1 H45B H 0.5461 -0.0426 0.1012 0.194 Uiso 0.272(7) 1 calc PR B -1 H45C H 0.5255 -0.1488 0.1216 0.194 Uiso 0.272(7) 1 calc PR B -1 C46 C 0.6528(17) -0.021(3) 0.1349(6) 0.173(5) Uani 0.272(7) 1 d PD B -1 H46A H 0.6948 0.0534 0.1256 0.207 Uiso 0.272(7) 1 calc PR B -1 H46B H 0.7034 -0.0481 0.1381 0.207 Uiso 0.272(7) 1 calc PR B -1 O1 O 0.6123(19) -0.015(3) 0.1690(8) 0.173(5) Uani 0.272(7) 1 d PD B -1 C47 C 0.6912(19) 0.095(2) 0.1789(7) 0.173(5) Uani 0.272(7) 1 d PD B -1 H47A H 0.7558 0.0956 0.1883 0.207 Uiso 0.272(7) 1 calc PR B -1 H47B H 0.7134 0.1406 0.1576 0.207 Uiso 0.272(7) 1 calc PR B -1 C48 C 0.656(2) 0.140(2) 0.2031(7) 0.129(4) Uani 0.272(7) 1 d PD B -1 H48A H 0.7178 0.2014 0.2142 0.194 Uiso 0.272(7) 1 calc PR B -1 H48B H 0.6134 0.0863 0.2210 0.194 Uiso 0.272(7) 1 calc PR B -1 H48C H 0.6109 0.1646 0.1916 0.194 Uiso 0.272(7) 1 calc PR B -1 C45' C 0.643(2) -0.026(2) 0.1143(6) 0.129(4) Uani 0.228(7) 1 d PD B -5 H45D H 0.6953 -0.0336 0.0998 0.194 Uiso 0.228(7) 1 calc PR B -5 H45E H 0.6220 0.0213 0.1025 0.194 Uiso 0.228(7) 1 calc PR B -5 H45F H 0.5794 -0.0969 0.1180 0.194 Uiso 0.228(7) 1 calc PR B -5 C46' C 0.690(2) 0.019(3) 0.1466(7) 0.173(5) Uani 0.228(7) 1 d PD B -5 H46C H 0.7484 0.0937 0.1432 0.207 Uiso 0.228(7) 1 calc PR B -5 H46D H 0.7210 -0.0230 0.1569 0.207 Uiso 0.228(7) 1 calc PR B -5 O1' O 0.610(3) 0.017(4) 0.1701(11) 0.173(5) Uani 0.228(7) 1 d PD B -5 C47' C 0.676(3) 0.105(3) 0.1931(9) 0.173(5) Uani 0.228(7) 1 d PD B -5 H47C H 0.6857 0.0747 0.2153 0.207 Uiso 0.228(7) 1 calc PR B -5 H47D H 0.7481 0.1478 0.1823 0.207 Uiso 0.228(7) 1 calc PR B -5 C48' C 0.638(3) 0.173(2) 0.2011(8) 0.129(4) Uani 0.228(7) 1 d PD B -5 H48D H 0.6462 0.1881 0.2262 0.194 Uiso 0.228(7) 1 calc PR B -5 H48E H 0.5616 0.1383 0.1947 0.194 Uiso 0.228(7) 1 calc PR B -5 H48F H 0.6786 0.2398 0.1879 0.194 Uiso 0.228(7) 1 calc PR B -5 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 0.0431(3) 0.0315(2) 0.0532(3) -0.0038(2) -0.0031(2) 0.0154(2) K2 0.0493(3) 0.0493(3) 0.0409(3) 0.00719(16) -0.00719(16) 0.0165(3) K3 0.0364(3) 0.0364(3) 0.0638(4) 0.00322(15) -0.00322(15) 0.0187(3) N1 0.0335(9) 0.0402(10) 0.0367(8) 0.0071(7) -0.0015(7) 0.0151(8) N2 0.0396(10) 0.0396(9) 0.0487(10) 0.0067(8) 0.0103(8) 0.0232(8) N3 0.0405(10) 0.0367(9) 0.0497(10) -0.0016(8) 0.0064(8) 0.0215(8) N4 0.0412(10) 0.0292(9) 0.0492(10) 0.0012(8) 0.0010(8) 0.0160(8) C1 0.0317(10) 0.0524(13) 0.0381(11) 0.0101(10) 0.0011(8) 0.0164(10) C2 0.0405(13) 0.0641(16) 0.0524(13) 0.0159(11) 0.0096(10) 0.0299(12) C3 0.0411(12) 0.0536(13) 0.0413(11) 0.0057(10) 0.0025(9) 0.0312(11) C4 0.0492(13) 0.0673(16) 0.0395(12) 0.0016(11) 0.0022(10) 0.0409(13) C5 0.0706(18) 0.088(2) 0.0563(15) 0.0037(14) 0.0164(13) 0.0525(17) C6 0.097(3) 0.116(3) 0.075(2) -0.002(2) 0.0295(19) 0.075(2) C7 0.117(3) 0.107(3) 0.090(2) -0.011(2) 0.023(2) 0.089(3) C8 0.095(2) 0.0736(19) 0.0760(19) -0.0014(15) 0.0204(17) 0.0615(19) C9 0.0607(15) 0.0571(14) 0.0412(12) -0.0015(11) 0.0037(11) 0.0423(13) C10 0.0491(13) 0.0473(12) 0.0404(11) -0.0037(9) -0.0013(10) 0.0318(11) C11 0.0556(14) 0.0381(11) 0.0537(13) -0.0086(10) -0.0054(11) 0.0276(11) C12 0.0413(12) 0.0293(10) 0.0630(14) -0.0007(10) -0.0020(10) 0.0197(9) C13 0.0339(12) 0.0702(18) 0.0716(16) 0.0280(14) 0.0051(11) 0.0148(13) C14 0.0433(15) 0.0721(19) 0.096(2) 0.0452(17) 0.0036(15) 0.0068(14) C15 0.072(2) 0.112(3) 0.128(3) 0.049(3) 0.054(2) 0.042(2) C16 0.0552(19) 0.107(3) 0.125(3) 0.047(2) -0.0379(19) -0.0059(19) C17 0.0574(15) 0.0270(11) 0.0840(18) -0.0025(12) -0.0091(13) 0.0166(11) C18 0.086(2) 0.0331(14) 0.112(3) 0.0152(16) -0.0197(19) -0.0056(14) C19 0.165(5) 0.0419(18) 0.200(5) -0.015(2) 0.046(4) 0.045(2) C20 0.071(2) 0.0539(18) 0.159(4) 0.018(2) -0.047(2) -0.0026(16) C21 0.0295(10) 0.0418(12) 0.0424(11) 0.0146(9) 0.0019(9) 0.0111(9) C22 0.0431(13) 0.0445(13) 0.0563(13) 0.0162(11) -0.0024(11) 0.0197(11) C23 0.0719(18) 0.0768(19) 0.0685(17) 0.0249(15) 0.0060(15) 0.0498(16) C24 0.102(3) 0.131(3) 0.0662(19) 0.025(2) -0.0058(18) 0.088(3) C25 0.089(2) 0.131(3) 0.0459(15) 0.0115(17) -0.0123(15) 0.069(2) C26 0.0443(13) 0.0720(18) 0.0432(13) 0.0119(12) -0.0004(11) 0.0261(13) C27 0.0488(14) 0.092(2) 0.0417(12) 0.0000(13) -0.0038(10) 0.0275(15) C28 0.075(2) 0.121(3) 0.0469(15) -0.0010(17) 0.0057(14) 0.035(2) C29 0.123(3) 0.089(3) 0.085(2) 0.003(2) 0.044(2) 0.039(2) C30 0.078(2) 0.0631(17) 0.0727(18) -0.0124(14) -0.0211(16) 0.0483(16) C31 0.087(3) 0.061(4) 0.058(2) 0.012(3) -0.005(2) 0.027(3) C32 0.088(3) 0.054(3) 0.105(3) 0.002(2) -0.006(3) 0.016(2) C30' 0.078(2) 0.0631(17) 0.0727(18) -0.0124(14) -0.0211(16) 0.0483(16) C31' 0.087(3) 0.061(4) 0.058(2) 0.012(3) -0.005(2) 0.027(3) C32' 0.088(3) 0.054(3) 0.105(3) 0.002(2) -0.006(3) 0.016(2) C33 0.0415(12) 0.0284(10) 0.0517(13) 0.0087(9) 0.0032(10) 0.0111(9) C34 0.0519(14) 0.0363(12) 0.0660(16) 0.0037(11) -0.0069(12) 0.0181(11) C35 0.083(2) 0.073(2) 0.078(2) 0.0094(16) -0.0151(17) 0.0458(18) C36 0.105(3) 0.092(2) 0.0604(17) 0.0140(16) -0.0119(18) 0.054(2) C37 0.081(2) 0.0711(19) 0.0545(16) 0.0088(14) 0.0074(14) 0.0370(17) C38 0.0494(14) 0.0456(14) 0.0546(14) 0.0052(11) 0.0023(11) 0.0193(11) C39 0.0646(18) 0.090(2) 0.0545(16) 0.0097(14) 0.0142(13) 0.0425(16) C40 0.073(2) 0.071(2) 0.135(3) 0.020(2) 0.005(2) 0.0387(18) C41 0.060(2) 0.090(3) 0.223(5) 0.038(3) 0.034(3) 0.027(2) C42 0.0555(15) 0.0519(15) 0.0878(19) 0.0037(14) -0.0077(13) 0.0321(13) C43 0.073(2) 0.067(2) 0.140(3) 0.007(2) 0.027(2) 0.0355(18) C44 0.115(3) 0.097(3) 0.127(3) 0.003(2) -0.014(2) 0.082(3) C45 0.113(9) 0.123(13) 0.166(9) -0.076(8) -0.037(7) 0.069(7) C46 0.099(6) 0.263(14) 0.145(8) -0.076(7) -0.025(6) 0.082(7) O1 0.099(6) 0.263(14) 0.145(8) -0.076(7) -0.025(6) 0.082(7) C47 0.099(6) 0.263(14) 0.145(8) -0.076(7) -0.025(6) 0.082(7) C48 0.113(9) 0.123(13) 0.166(9) -0.076(8) -0.037(7) 0.069(7) C45' 0.113(9) 0.123(13) 0.166(9) -0.076(8) -0.037(7) 0.069(7) C46' 0.099(6) 0.263(14) 0.145(8) -0.076(7) -0.025(6) 0.082(7) O1' 0.099(6) 0.263(14) 0.145(8) -0.076(7) -0.025(6) 0.082(7) C47' 0.099(6) 0.263(14) 0.145(8) -0.076(7) -0.025(6) 0.082(7) C48' 0.113(9) 0.123(13) 0.166(9) -0.076(8) -0.037(7) 0.069(7) _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 N4 2.7982(18) . ? K1 N1 2.8223(17) 4 ? K1 N2 2.8490(18) 4 ? K1 N3 2.9031(19) . ? K1 C21 3.070(2) 4 ? K1 C33 3.114(2) . ? K1 N3 3.2876(19) 4 ? K1 N2 3.3456(18) . ? K1 C22 3.506(2) 4 ? K1 C29 3.506(3) 4 ? K1 K2 3.6915(7) . ? K1 K3 3.7005(7) . ? K2 N1 2.7373(16) . ? K2 N1 2.7375(16) 4 ? K2 N2 2.7744(19) . ? K2 N2 2.7744(19) 4 ? K2 C1 3.009(2) 4 ? K2 C1 3.009(2) . ? K2 C2 3.106(2) . ? K2 C2 3.106(2) 4 ? K2 C3 3.294(2) . ? K2 C3 3.294(2) 4 ? K2 C32' 3.425(10) 4 ? K3 N3 2.7630(18) . ? K3 N3 2.7630(18) 4 ? K3 N4 2.7741(18) 4 ? K3 N4 2.7742(18) . ? K3 C12 2.968(2) 4 ? K3 C12 2.968(2) . ? K3 C11 3.064(2) . ? K3 C11 3.064(2) 4 ? K3 C10 3.296(2) . ? K3 C10 3.296(2) 4 ? K3 C20 3.530(3) 4 ? N1 C1 1.333(3) . ? N1 C21 1.406(3) . ? N1 K1 2.8222(17) 4 ? N2 C3 1.332(3) . ? N2 N3 1.389(2) . ? N2 K1 2.8490(18) 4 ? N3 C10 1.324(3) . ? N3 K1 3.2876(19) 4 ? N4 C12 1.336(3) . ? N4 C33 1.406(3) . ? C1 C2 1.382(3) . ? C1 C13 1.576(3) . ? C2 C3 1.449(3) . ? C2 H2A 0.9400 . ? C3 C4 1.454(3) . ? C4 C9 1.405(4) . ? C4 C5 1.407(3) . ? C5 C6 1.356(4) . ? C5 H5A 0.9400 . ? C6 C7 1.377(5) . ? C6 H6A 0.9400 . ? C7 C8 1.373(4) . ? C7 H7A 0.9400 . ? C8 C9 1.413(3) . ? C8 H8A 0.9400 . ? C9 C10 1.459(3) . ? C10 C11 1.460(3) . ? C11 C12 1.386(3) . ? C11 H11A 0.9400 . ? C12 C17 1.571(3) . ? C13 C14 1.499(4) . ? C13 C16 1.524(4) . ? C13 C15 1.542(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.510(4) . ? C17 C19 1.528(4) . ? C17 C20 1.531(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 C22 1.397(3) . ? C21 C26 1.433(3) . ? C21 K1 3.070(2) 4 ? C22 C23 1.394(3) . ? C22 C30 1.518(4) . ? C22 K1 3.506(2) 4 ? C23 C24 1.365(4) . ? C23 H23A 0.9400 . ? C24 C25 1.359(5) . ? C24 H24A 0.9400 . ? C25 C26 1.384(4) . ? C25 H25A 0.9400 . ? C26 C27 1.517(4) . ? C27 C29 1.501(5) . ? C27 C28 1.522(4) . ? C27 H27A 0.9900 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 C31 1.428(6) . ? C30 C32 1.617(6) . ? C30 H30A 0.9900 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C31' H31D 0.9700 . ? C31' H31E 0.9700 . ? C31' H31F 0.9700 . ? C32' H32D 0.9700 . ? C32' H32E 0.9700 . ? C32' H32F 0.9700 . ? C33 C38 1.414(3) . ? C33 C34 1.421(3) . ? C34 C35 1.396(4) . ? C34 C42 1.519(4) . ? C35 C36 1.365(5) . ? C35 H35A 0.9400 . ? C36 C37 1.380(4) . ? C36 H36A 0.9400 . ? C37 C38 1.398(4) . ? C37 H37A 0.9400 . ? C38 C39 1.518(4) . ? C39 C40 1.483(5) . ? C39 C41 1.532(4) . ? C39 H39A 0.9900 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? C42 C43 1.496(4) . ? C42 C44 1.525(4) . ? C42 H42A 0.9900 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 H43C 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C44 H44C 0.9700 . ? C45 C46 1.321(18) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C45 H45C 0.9700 . ? C46 O1 1.43(2) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? O1 C47 1.44(2) . ? C47 C48 1.347(16) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? C45' C46' 1.379(19) . ? C45' H45D 0.9700 . ? C45' H45E 0.9700 . ? C45' H45F 0.9700 . ? C46' O1' 1.43(2) . ? C46' H46C 0.9800 . ? C46' H46D 0.9800 . ? O1' C47' 1.43(2) . ? C47' C48' 1.35(2) . ? C47' H47C 0.9800 . ? C47' H47D 0.9800 . ? C48' H48D 0.9700 . ? C48' H48E 0.9700 . ? C48' H48F 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 N4 K1 N1 175.61(5) . 4 ? N4 K1 N2 117.22(5) . 4 ? N1 K1 N2 66.08(5) 4 4 ? N4 K1 N3 67.57(5) . . ? N1 K1 N3 116.42(5) 4 . ? N2 K1 N3 81.14(5) 4 . ? N4 K1 C21 148.93(6) . 4 ? N1 K1 C21 27.19(5) 4 4 ? N2 K1 C21 92.84(5) 4 4 ? N3 K1 C21 129.06(6) . 4 ? N4 K1 C33 26.84(5) . . ? N1 K1 C33 148.85(6) 4 . ? N2 K1 C33 130.19(6) 4 . ? N3 K1 C33 93.82(6) . . ? C21 K1 C33 125.48(6) 4 . ? N4 K1 N3 92.36(5) . 4 ? N1 K1 N3 90.89(5) 4 4 ? N2 K1 N3 24.86(5) 4 4 ? N3 K1 N3 69.57(5) . 4 ? C21 K1 N3 117.38(5) 4 4 ? C33 K1 N3 107.54(5) . 4 ? N4 K1 N2 91.87(5) . . ? N1 K1 N2 92.06(5) 4 . ? N2 K1 N2 70.01(5) 4 . ? N3 K1 N2 24.38(5) . . ? C21 K1 N2 106.62(5) 4 . ? C33 K1 N2 117.76(5) . . ? N3 K1 N2 68.66(4) 4 . ? N4 K1 C22 134.22(5) . 4 ? N1 K1 C22 43.44(5) 4 4 ? N2 K1 C22 107.43(5) 4 4 ? N3 K1 C22 112.15(6) . 4 ? C21 K1 C22 23.34(6) 4 4 ? C33 K1 C22 119.97(6) . 4 ? N3 K1 C22 131.85(5) 4 4 ? N2 K1 C22 94.17(5) . 4 ? N4 K1 C29 112.52(8) . 4 ? N1 K1 C29 64.36(8) 4 4 ? N2 K1 C29 83.24(9) 4 4 ? N3 K1 C29 161.95(8) . 4 ? C21 K1 C29 60.62(8) 4 4 ? C33 K1 C29 89.37(9) . 4 ? N3 K1 C29 92.52(8) 4 4 ? N2 K1 C29 150.19(9) . 4 ? C22 K1 C29 81.19(8) 4 4 ? N4 K1 K2 136.84(4) . . ? N1 K1 K2 47.42(3) 4 . ? N2 K1 K2 48.10(4) 4 . ? N3 K1 K2 69.83(4) . . ? C21 K1 K2 69.06(4) 4 . ? C33 K1 K2 163.59(5) . . ? N3 K1 K2 66.26(3) 4 . ? N2 K1 K2 46.11(3) . . ? C22 K1 K2 69.76(4) 4 . ? C29 K1 K2 105.76(8) 4 . ? N4 K1 K3 48.11(4) . . ? N1 K1 K3 135.73(4) 4 . ? N2 K1 K3 70.31(4) 4 . ? N3 K1 K3 47.60(4) . . ? C21 K1 K3 162.92(4) 4 . ? C33 K1 K3 70.27(4) . . ? N3 K1 K3 46.11(3) 4 . ? N2 K1 K3 65.72(3) . . ? C22 K1 K3 159.56(4) 4 . ? C29 K1 K3 117.93(6) 4 . ? K2 K1 K3 96.470(16) . . ? N1 K2 N1 175.15(8) . 4 ? N1 K2 N2 68.25(5) . . ? N1 K2 N2 107.81(5) 4 . ? N1 K2 N2 107.81(5) . 4 ? N1 K2 N2 68.25(5) 4 4 ? N2 K2 N2 80.27(7) . 4 ? N1 K2 C1 155.41(6) . 4 ? N1 K2 C1 26.29(5) 4 4 ? N2 K2 C1 129.85(5) . 4 ? N2 K2 C1 65.75(6) 4 4 ? N1 K2 C1 26.29(5) . . ? N1 K2 C1 155.41(6) 4 . ? N2 K2 C1 65.75(6) . . ? N2 K2 C1 129.85(5) 4 . ? C1 K2 C1 162.70(9) 4 . ? N1 K2 C2 47.48(6) . . ? N1 K2 C2 132.23(6) 4 . ? N2 K2 C2 48.23(6) . . ? N2 K2 C2 126.80(6) 4 . ? C1 K2 C2 155.72(6) 4 . ? C1 K2 C2 26.06(6) . . ? N1 K2 C2 132.23(6) . 4 ? N1 K2 C2 47.48(6) 4 4 ? N2 K2 C2 126.80(6) . 4 ? N2 K2 C2 48.23(6) 4 4 ? C1 K2 C2 26.06(6) 4 4 ? C1 K2 C2 155.72(6) . 4 ? C2 K2 C2 174.97(10) . 4 ? N1 K2 C3 60.44(5) . . ? N1 K2 C3 117.11(5) 4 . ? N2 K2 C3 23.41(5) . . ? N2 K2 C3 103.67(6) 4 . ? C1 K2 C3 143.17(5) 4 . ? C1 K2 C3 48.22(6) . . ? C2 K2 C3 25.95(6) . . ? C2 K2 C3 149.32(6) 4 . ? N1 K2 C3 117.11(5) . 4 ? N1 K2 C3 60.44(5) 4 4 ? N2 K2 C3 103.67(6) . 4 ? N2 K2 C3 23.41(5) 4 4 ? C1 K2 C3 48.21(6) 4 4 ? C1 K2 C3 143.17(5) . 4 ? C2 K2 C3 149.32(6) . 4 ? C2 K2 C3 25.95(6) 4 4 ? C3 K2 C3 127.08(8) . 4 ? N1 K2 C32' 118.16(18) . 4 ? N1 K2 C32' 65.07(17) 4 4 ? N2 K2 C32' 103.97(17) . 4 ? N2 K2 C32' 132.08(16) 4 4 ? C1 K2 C32' 76.90(19) 4 4 ? C1 K2 C32' 92.71(18) . 4 ? C2 K2 C32' 80.59(19) . 4 ? C2 K2 C32' 102.47(19) 4 4 ? C3 K2 C32' 88.40(18) . 4 ? C3 K2 C32' 124.00(18) 4 4 ? N3 K3 N3 79.83(7) . 4 ? N3 K3 N4 105.38(5) . 4 ? N3 K3 N4 69.88(5) 4 4 ? N3 K3 N4 69.89(5) . . ? N3 K3 N4 105.38(5) 4 . ? N4 K3 N4 174.12(8) 4 . ? N3 K3 C12 128.31(6) . 4 ? N3 K3 C12 67.44(6) 4 4 ? N4 K3 C12 26.62(6) 4 4 ? N4 K3 C12 155.47(6) . 4 ? N3 K3 C12 67.44(6) . . ? N3 K3 C12 128.31(6) 4 . ? N4 K3 C12 155.48(6) 4 . ? N4 K3 C12 26.62(6) . . ? C12 K3 C12 162.28(9) 4 . ? N3 K3 C11 48.87(6) . . ? N3 K3 C11 125.99(6) 4 . ? N4 K3 C11 131.80(6) 4 . ? N4 K3 C11 47.84(6) . . ? C12 K3 C11 155.37(6) 4 . ? C12 K3 C11 26.50(6) . . ? N3 K3 C11 125.99(6) . 4 ? N3 K3 C11 48.87(6) 4 4 ? N4 K3 C11 47.84(6) 4 4 ? N4 K3 C11 131.79(6) . 4 ? C12 K3 C11 26.50(6) 4 4 ? C12 K3 C11 155.36(6) . 4 ? C11 K3 C11 174.76(9) . 4 ? N3 K3 C10 23.16(5) . . ? N3 K3 C10 102.69(6) 4 . ? N4 K3 C10 116.96(5) 4 . ? N4 K3 C10 59.99(5) . . ? C12 K3 C10 143.37(6) 4 . ? C12 K3 C10 48.55(6) . . ? C11 K3 C10 26.21(6) . . ? C11 K3 C10 148.82(6) 4 . ? N3 K3 C10 102.69(6) . 4 ? N3 K3 C10 23.16(5) 4 4 ? N4 K3 C10 59.99(5) 4 4 ? N4 K3 C10 116.95(5) . 4 ? C12 K3 C10 48.56(6) 4 4 ? C12 K3 C10 143.36(6) . 4 ? C11 K3 C10 148.82(6) . 4 ? C11 K3 C10 26.20(6) 4 4 ? C10 K3 C10 125.73(8) . 4 ? N3 K3 C20 163.54(8) . 4 ? N3 K3 C20 103.88(8) 4 4 ? N4 K3 C20 62.18(7) 4 4 ? N4 K3 C20 123.15(7) . 4 ? C12 K3 C20 43.61(7) 4 4 ? C12 K3 C20 118.90(7) . 4 ? C11 K3 C20 130.12(8) . 4 ? C11 K3 C20 55.04(8) 4 4 ? C10 K3 C20 150.60(9) . 4 ? C10 K3 C20 80.90(8) 4 4 ? N3 K3 K1 50.89(4) . . ? N3 K3 K1 59.04(4) 4 . ? N4 K3 K1 125.72(4) 4 . ? N4 K3 K1 48.67(4) . . ? C12 K3 K1 125.73(5) 4 . ? C12 K3 K1 69.27(4) . . ? C11 K3 K1 73.84(4) . . ? C11 K3 K1 102.12(5) 4 . ? C10 K3 K1 62.45(4) . . ? C10 K3 K1 77.38(4) 4 . ? C20 K3 K1 144.59(8) 4 . ? C1 N1 C21 128.17(18) . . ? C1 N1 K2 88.30(11) . . ? C21 N1 K2 135.43(14) . . ? C1 N1 K1 133.40(15) . 4 ? C21 N1 K1 86.26(11) . 4 ? K2 N1 K1 83.20(5) . 4 ? C3 N2 N3 121.24(18) . . ? C3 N2 K2 100.75(14) . . ? N3 N2 K2 130.85(12) . . ? C3 N2 K1 120.80(13) . 4 ? N3 N2 K1 95.54(11) . 4 ? K2 N2 K1 82.05(5) . 4 ? C3 N2 K1 132.84(13) . . ? N3 N2 K1 59.66(10) . . ? K2 N2 K1 73.53(4) . . ? K1 N2 K1 105.00(5) 4 . ? C10 N3 N2 122.23(18) . . ? C10 N3 K3 101.66(14) . . ? N2 N3 K3 132.10(12) . . ? C10 N3 K1 113.74(14) . . ? N2 N3 K1 95.96(11) . . ? K3 N3 K1 81.51(5) . . ? C10 N3 K1 140.02(14) . 4 ? N2 N3 K1 59.60(10) . 4 ? K3 N3 K1 74.85(4) . 4 ? K1 N3 K1 105.21(5) . 4 ? C12 N4 C33 126.53(18) . . ? C12 N4 K3 84.83(13) . . ? C33 N4 K3 139.59(14) . . ? C12 N4 K1 133.18(14) . . ? C33 N4 K1 89.20(12) . . ? K3 N4 K1 83.22(5) . . ? N1 C1 C2 122.2(2) . . ? N1 C1 C13 123.2(2) . . ? C2 C1 C13 114.2(2) . . ? N1 C1 K2 65.41(11) . . ? C2 C1 K2 80.89(13) . . ? C13 C1 K2 120.83(15) . . ? C1 C2 C3 132.2(2) . . ? C1 C2 K2 73.05(13) . . ? C3 C2 K2 84.29(13) . . ? C1 C2 H2A 113.9 . . ? C3 C2 H2A 113.9 . . ? K2 C2 H2A 118.8 . . ? N2 C3 C2 121.1(2) . . ? N2 C3 C4 120.3(2) . . ? C2 C3 C4 118.6(2) . . ? N2 C3 K2 55.84(12) . . ? C2 C3 K2 69.76(13) . . ? C4 C3 K2 155.38(14) . . ? C9 C4 C5 118.5(2) . . ? C9 C4 C3 118.00(19) . . ? C5 C4 C3 123.5(2) . . ? C6 C5 C4 121.0(3) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 C7 120.4(3) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C8 C7 C6 121.1(3) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C7 C8 C9 119.3(3) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? C4 C9 C8 119.5(2) . . ? C4 C9 C10 118.6(2) . . ? C8 C9 C10 121.9(2) . . ? N3 C10 C9 119.6(2) . . ? N3 C10 C11 121.3(2) . . ? C9 C10 C11 119.1(2) . . ? N3 C10 K3 55.18(11) . . ? C9 C10 K3 163.26(15) . . ? C11 C10 K3 68.00(12) . . ? C12 C11 C10 131.3(2) . . ? C12 C11 K3 72.89(13) . . ? C10 C11 K3 85.79(13) . . ? C12 C11 H11A 114.3 . . ? C10 C11 H11A 114.3 . . ? K3 C11 H11A 116.5 . . ? N4 C12 C11 122.2(2) . . ? N4 C12 C17 122.1(2) . . ? C11 C12 C17 115.2(2) . . ? N4 C12 K3 68.55(12) . . ? C11 C12 K3 80.61(13) . . ? C17 C12 K3 115.89(15) . . ? C14 C13 C16 108.8(3) . . ? C14 C13 C15 105.8(3) . . ? C16 C13 C15 108.8(3) . . ? C14 C13 C1 114.9(2) . . ? C16 C13 C1 106.5(2) . . ? C15 C13 C1 111.9(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 106.6(3) . . ? C18 C17 C20 106.7(3) . . ? C19 C17 C20 110.9(3) . . ? C18 C17 C12 115.0(2) . . ? C19 C17 C12 112.1(2) . . ? C20 C17 C12 105.5(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N1 119.93(19) . . ? C22 C21 C26 118.8(2) . . ? N1 C21 C26 120.6(2) . . ? C22 C21 K1 96.12(13) . 4 ? N1 C21 K1 66.55(10) . 4 ? C26 C21 K1 99.21(14) . 4 ? C23 C22 C21 119.9(2) . . ? C23 C22 C30 118.4(2) . . ? C21 C22 C30 121.7(2) . . ? C23 C22 K1 113.58(18) . 4 ? C21 C22 K1 60.53(11) . 4 ? C30 C22 K1 95.87(15) . 4 ? C24 C23 C22 121.3(3) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C25 C24 C23 118.9(3) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? C24 C25 C26 123.5(3) . . ? C24 C25 H25A 118.3 . . ? C26 C25 H25A 118.3 . . ? C25 C26 C21 117.6(3) . . ? C25 C26 C27 121.2(2) . . ? C21 C26 C27 121.2(2) . . ? C29 C27 C26 112.0(2) . . ? C29 C27 C28 110.1(3) . . ? C26 C27 C28 114.4(3) . . ? C29 C27 H27A 106.6 . . ? C26 C27 H27A 106.6 . . ? C28 C27 H27A 106.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C22 115.9(3) . . ? C31 C30 C32 110.0(4) . . ? C22 C30 C32 107.6(3) . . ? C31 C30 H30A 107.7 . . ? C22 C30 H30A 107.7 . . ? C32 C30 H30A 107.7 . . ? N4 C33 C38 119.6(2) . . ? N4 C33 C34 121.4(2) . . ? C38 C33 C34 118.5(2) . . ? N4 C33 K1 63.97(10) . . ? C38 C33 K1 97.37(14) . . ? C34 C33 K1 101.68(14) . . ? C35 C34 C33 118.9(3) . . ? C35 C34 C42 119.6(3) . . ? C33 C34 C42 121.5(2) . . ? C36 C35 C34 121.8(3) . . ? C36 C35 H35A 119.1 . . ? C34 C35 H35A 119.1 . . ? C35 C36 C37 120.4(3) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C36 C37 C38 120.1(3) . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? C37 C38 C33 120.3(2) . . ? C37 C38 C39 118.5(2) . . ? C33 C38 C39 121.1(2) . . ? C40 C39 C38 114.1(3) . . ? C40 C39 C41 109.1(3) . . ? C38 C39 C41 111.9(3) . . ? C40 C39 H39A 107.1 . . ? C38 C39 H39A 107.1 . . ? C41 C39 H39A 107.1 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C34 112.6(2) . . ? C43 C42 C44 110.2(3) . . ? C34 C42 C44 114.7(3) . . ? C43 C42 H42A 106.2 . . ? C34 C42 H42A 106.2 . . ? C44 C42 H42A 106.2 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C45 C46 O1 117.0(19) . . ? C45 C46 H46A 108.0 . . ? O1 C46 H46A 108.0 . . ? C45 C46 H46B 108.0 . . ? O1 C46 H46B 108.0 . . ? H46A C46 H46B 107.3 . . ? C46 O1 C47 100(2) . . ? C48 C47 O1 114.6(17) . . ? C48 C47 H47A 108.6 . . ? O1 C47 H47A 108.6 . . ? C48 C47 H47B 108.6 . . ? O1 C47 H47B 108.6 . . ? H47A C47 H47B 107.6 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46' C45' H45D 109.5 . . ? C46' C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? C46' C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? C45' C46' O1' 110(2) . . ? C45' C46' H46C 109.6 . . ? O1' C46' H46C 109.6 . . ? C45' C46' H46D 109.6 . . ? O1' C46' H46D 109.6 . . ? H46C C46' H46D 108.1 . . ? C47' O1' C46' 101(2) . . ? C48' C47' O1' 116(2) . . ? C48' C47' H47C 108.3 . . ? O1' C47' H47C 108.3 . . ? C48' C47' H47D 108.3 . . ? O1' C47' H47D 108.3 . . ? H47C C47' H47D 107.4 . . ? C47' C48' H48D 109.5 . . ? C47' C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? C47' C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 K1 K3 N3 97.17(7) . . . . ? N1 K1 K3 N3 -85.78(7) 4 . . . ? N2 K1 K3 N3 -96.04(6) 4 . . . ? C21 K1 K3 N3 -86.20(17) 4 . . . ? C33 K1 K3 N3 115.04(7) . . . . ? N3 K1 K3 N3 -102.85(7) 4 . . . ? N2 K1 K3 N3 -19.75(6) . . . . ? C22 K1 K3 N3 -8.84(12) 4 . . . ? C29 K1 K3 N3 -166.69(10) 4 . . . ? K2 K1 K3 N3 -55.01(5) . . . . ? N4 K1 K3 N3 -159.98(7) . . . 4 ? N1 K1 K3 N3 17.07(7) 4 . . 4 ? N2 K1 K3 N3 6.81(6) 4 . . 4 ? N3 K1 K3 N3 102.85(7) . . . 4 ? C21 K1 K3 N3 16.65(17) 4 . . 4 ? C33 K1 K3 N3 -142.11(6) . . . 4 ? N2 K1 K3 N3 83.10(5) . . . 4 ? C22 K1 K3 N3 94.01(13) 4 . . 4 ? C29 K1 K3 N3 -63.84(10) 4 . . 4 ? K2 K1 K3 N3 47.84(4) . . . 4 ? N4 K1 K3 N4 177.76(3) . . . 4 ? N1 K1 K3 N4 -5.20(7) 4 . . 4 ? N2 K1 K3 N4 -15.45(6) 4 . . 4 ? N3 K1 K3 N4 80.58(7) . . . 4 ? C21 K1 K3 N4 -5.62(17) 4 . . 4 ? C33 K1 K3 N4 -164.37(6) . . . 4 ? N3 K1 K3 N4 -22.27(6) 4 . . 4 ? N2 K1 K3 N4 60.84(6) . . . 4 ? C22 K1 K3 N4 71.74(12) 4 . . 4 ? C29 K1 K3 N4 -86.11(10) 4 . . 4 ? K2 K1 K3 N4 25.58(5) . . . 4 ? N1 K1 K3 N4 177.05(8) 4 . . . ? N2 K1 K3 N4 166.79(6) 4 . . . ? N3 K1 K3 N4 -97.17(7) . . . . ? C21 K1 K3 N4 176.63(17) 4 . . . ? C33 K1 K3 N4 17.87(7) . . . . ? N3 K1 K3 N4 159.98(7) 4 . . . ? N2 K1 K3 N4 -116.92(6) . . . . ? C22 K1 K3 N4 -106.01(13) 4 . . . ? C29 K1 K3 N4 96.13(10) 4 . . . ? K2 K1 K3 N4 -152.18(5) . . . . ? N4 K1 K3 C12 -149.29(7) . . . 4 ? N1 K1 K3 C12 27.75(8) 4 . . 4 ? N2 K1 K3 C12 17.50(7) 4 . . 4 ? N3 K1 K3 C12 113.53(7) . . . 4 ? C21 K1 K3 C12 27.33(17) 4 . . 4 ? C33 K1 K3 C12 -131.42(7) . . . 4 ? N3 K1 K3 C12 10.68(7) 4 . . 4 ? N2 K1 K3 C12 93.79(7) . . . 4 ? C22 K1 K3 C12 104.69(13) 4 . . 4 ? C29 K1 K3 C12 -53.16(11) 4 . . 4 ? K2 K1 K3 C12 58.52(6) . . . 4 ? N4 K1 K3 C12 19.93(7) . . . . ? N1 K1 K3 C12 -163.02(7) 4 . . . ? N2 K1 K3 C12 -173.28(6) 4 . . . ? N3 K1 K3 C12 -77.24(7) . . . . ? C21 K1 K3 C12 -163.44(17) 4 . . . ? C33 K1 K3 C12 37.80(7) . . . . ? N3 K1 K3 C12 179.91(7) 4 . . . ? N2 K1 K3 C12 -96.99(6) . . . . ? C22 K1 K3 C12 -86.08(13) 4 . . . ? C29 K1 K3 C12 116.06(10) 4 . . . ? K2 K1 K3 C12 -132.25(5) . . . . ? N4 K1 K3 C11 47.49(7) . . . . ? N1 K1 K3 C11 -135.47(7) 4 . . . ? N2 K1 K3 C11 -145.72(6) 4 . . . ? N3 K1 K3 C11 -49.68(7) . . . . ? C21 K1 K3 C11 -135.89(17) 4 . . . ? C33 K1 K3 C11 65.36(7) . . . . ? N3 K1 K3 C11 -152.54(7) 4 . . . ? N2 K1 K3 C11 -69.43(6) . . . . ? C22 K1 K3 C11 -58.53(13) 4 . . . ? C29 K1 K3 C11 143.62(10) 4 . . . ? K2 K1 K3 C11 -104.69(5) . . . . ? N4 K1 K3 C11 -135.96(7) . . . 4 ? N1 K1 K3 C11 41.09(7) 4 . . 4 ? N2 K1 K3 C11 30.84(6) 4 . . 4 ? N3 K1 K3 C11 126.87(7) . . . 4 ? C21 K1 K3 C11 40.67(17) 4 . . 4 ? C33 K1 K3 C11 -118.09(6) . . . 4 ? N3 K1 K3 C11 24.02(6) 4 . . 4 ? N2 K1 K3 C11 107.13(6) . . . 4 ? C22 K1 K3 C11 118.03(13) 4 . . 4 ? C29 K1 K3 C11 -39.82(10) 4 . . 4 ? K2 K1 K3 C11 71.86(5) . . . 4 ? N4 K1 K3 C10 73.00(7) . . . . ? N1 K1 K3 C10 -109.95(7) 4 . . . ? N2 K1 K3 C10 -120.20(6) 4 . . . ? N3 K1 K3 C10 -24.17(6) . . . . ? C21 K1 K3 C10 -110.37(16) 4 . . . ? C33 K1 K3 C10 90.87(6) . . . . ? N3 K1 K3 C10 -127.02(6) 4 . . . ? N2 K1 K3 C10 -43.91(5) . . . . ? C22 K1 K3 C10 -33.01(13) 4 . . . ? C29 K1 K3 C10 169.14(10) 4 . . . ? K2 K1 K3 C10 -79.18(4) . . . . ? N4 K1 K3 C10 -144.64(6) . . . 4 ? N1 K1 K3 C10 32.40(7) 4 . . 4 ? N2 K1 K3 C10 22.15(5) 4 . . 4 ? N3 K1 K3 C10 118.18(6) . . . 4 ? C21 K1 K3 C10 31.98(16) 4 . . 4 ? C33 K1 K3 C10 -126.77(6) . . . 4 ? N3 K1 K3 C10 15.33(6) 4 . . 4 ? N2 K1 K3 C10 98.44(5) . . . 4 ? C22 K1 K3 C10 109.34(12) 4 . . 4 ? C29 K1 K3 C10 -48.51(10) 4 . . 4 ? K2 K1 K3 C10 63.17(4) . . . 4 ? N4 K1 K3 C20 -91.13(11) . . . 4 ? N1 K1 K3 C20 85.92(11) 4 . . 4 ? N2 K1 K3 C20 75.66(10) 4 . . 4 ? N3 K1 K3 C20 171.70(11) . . . 4 ? C21 K1 K3 C20 85.50(19) 4 . . 4 ? C33 K1 K3 C20 -73.26(11) . . . 4 ? N3 K1 K3 C20 68.85(11) 4 . . 4 ? N2 K1 K3 C20 151.95(10) . . . 4 ? C22 K1 K3 C20 162.85(15) 4 . . 4 ? C29 K1 K3 C20 5.00(14) 4 . . 4 ? K2 K1 K3 C20 116.69(10) . . . 4 ? N1 K2 N1 C1 115.20(13) 4 . . . ? N2 K2 N1 C1 79.00(13) . . . . ? N2 K2 N1 C1 150.38(13) 4 . . . ? C1 K2 N1 C1 -139.2(2) 4 . . . ? C2 K2 N1 C1 26.39(13) . . . . ? C2 K2 N1 C1 -160.42(13) 4 . . . ? C3 K2 N1 C1 54.45(13) . . . . ? C3 K2 N1 C1 173.68(13) 4 . . . ? C32' K2 N1 C1 -15.7(2) 4 . . . ? N1 K2 N1 C21 -96.50(18) 4 . . . ? N2 K2 N1 C21 -132.69(19) . . . . ? N2 K2 N1 C21 -61.32(19) 4 . . . ? C1 K2 N1 C21 9.1(3) 4 . . . ? C1 K2 N1 C21 148.3(3) . . . . ? C2 K2 N1 C21 174.7(2) . . . . ? C2 K2 N1 C21 -12.1(2) 4 . . . ? C3 K2 N1 C21 -157.2(2) . . . . ? C3 K2 N1 C21 -38.0(2) 4 . . . ? C32' K2 N1 C21 132.7(2) 4 . . . ? N1 K2 N1 K1 -18.89(3) 4 . . 4 ? N2 K2 N1 K1 -55.09(5) . . . 4 ? N2 K2 N1 K1 16.29(6) 4 . . 4 ? C1 K2 N1 K1 86.73(14) 4 . . 4 ? C1 K2 N1 K1 -134.09(15) . . . 4 ? C2 K2 N1 K1 -107.70(8) . . . 4 ? C2 K2 N1 K1 65.50(9) 4 . . 4 ? C3 K2 N1 K1 -79.63(6) . . . 4 ? C3 K2 N1 K1 39.60(7) 4 . . 4 ? C32' K2 N1 K1 -149.74(18) 4 . . 4 ? N1 K2 N2 C3 -65.46(12) . . . . ? N1 K2 N2 C3 117.55(13) 4 . . . ? N2 K2 N2 C3 -179.20(15) 4 . . . ? C1 K2 N2 C3 134.12(12) 4 . . . ? C1 K2 N2 C3 -36.98(12) . . . . ? C2 K2 N2 C3 -13.72(12) . . . . ? C2 K2 N2 C3 167.30(12) 4 . . . ? C3 K2 N2 C3 -179.53(9) 4 . . . ? C32' K2 N2 C3 49.7(2) 4 . . . ? N1 K2 N2 N3 144.99(17) . . . . ? N1 K2 N2 N3 -32.01(17) 4 . . . ? N2 K2 N2 N3 31.25(13) 4 . . . ? C1 K2 N2 N3 -15.43(19) 4 . . . ? C1 K2 N2 N3 173.47(17) . . . . ? C2 K2 N2 N3 -163.27(19) . . . . ? C2 K2 N2 N3 17.74(18) 4 . . . ? C3 K2 N2 N3 -149.6(2) . . . . ? C3 K2 N2 N3 30.92(17) 4 . . . ? C32' K2 N2 N3 -99.9(2) 4 . . . ? N1 K2 N2 K1 54.53(5) . . . 4 ? N1 K2 N2 K1 -122.46(5) 4 . . 4 ? N2 K2 N2 K1 -59.21(4) 4 . . 4 ? C1 K2 N2 K1 -105.89(7) 4 . . 4 ? C1 K2 N2 K1 83.01(6) . . . 4 ? C2 K2 N2 K1 106.27(8) . . . 4 ? C2 K2 N2 K1 -72.72(7) 4 . . 4 ? C3 K2 N2 K1 119.99(13) . . . 4 ? C3 K2 N2 K1 -59.54(5) 4 . . 4 ? C32' K2 N2 K1 169.64(17) 4 . . 4 ? N1 K2 N2 K1 162.81(5) . . . . ? N1 K2 N2 K1 -14.18(5) 4 . . . ? N2 K2 N2 K1 49.07(3) 4 . . . ? C1 K2 N2 K1 2.39(8) 4 . . . ? C1 K2 N2 K1 -168.71(6) . . . . ? C2 K2 N2 K1 -145.45(8) . . . . ? C2 K2 N2 K1 35.57(7) 4 . . . ? C3 K2 N2 K1 -131.73(13) . . . . ? C3 K2 N2 K1 48.74(5) 4 . . . ? C32' K2 N2 K1 -82.07(17) 4 . . . ? N4 K1 N2 C3 101.6(2) . . . . ? N1 K1 N2 C3 -76.4(2) 4 . . . ? N2 K1 N2 C3 -139.99(18) 4 . . . ? N3 K1 N2 C3 106.1(2) . . . . ? C21 K1 N2 C3 -53.1(2) 4 . . . ? C33 K1 N2 C3 94.2(2) . . . . ? N3 K1 N2 C3 -166.6(2) 4 . . . ? C22 K1 N2 C3 -32.9(2) 4 . . . ? C29 K1 N2 C3 -112.5(2) 4 . . . ? K2 K1 N2 C3 -89.5(2) . . . . ? K3 K1 N2 C3 143.3(2) . . . . ? N4 K1 N2 N3 -4.43(11) . . . . ? N1 K1 N2 N3 177.52(11) 4 . . . ? N2 K1 N2 N3 113.93(11) 4 . . . ? C21 K1 N2 N3 -159.14(11) 4 . . . ? C33 K1 N2 N3 -11.84(13) . . . . ? N3 K1 N2 N3 87.37(12) 4 . . . ? C22 K1 N2 N3 -139.02(11) 4 . . . ? C29 K1 N2 N3 141.44(16) 4 . . . ? K2 K1 N2 N3 164.44(12) . . . . ? K3 K1 N2 N3 37.18(10) . . . . ? N4 K1 N2 K2 -168.87(5) . . . . ? N1 K1 N2 K2 13.08(5) 4 . . . ? N2 K1 N2 K2 -50.50(4) 4 . . . ? N3 K1 N2 K2 -164.44(12) . . . . ? C21 K1 N2 K2 36.42(6) 4 . . . ? C33 K1 N2 K2 -176.27(5) . . . . ? N3 K1 N2 K2 -77.07(5) 4 . . . ? C22 K1 N2 K2 56.54(5) 4 . . . ? C29 K1 N2 K2 -22.99(15) 4 . . . ? K3 K1 N2 K2 -127.25(4) . . . . ? N4 K1 N2 K1 -92.08(6) . . . 4 ? N1 K1 N2 K1 89.87(6) 4 . . 4 ? N2 K1 N2 K1 26.29(7) 4 . . 4 ? N3 K1 N2 K1 -87.64(12) . . . 4 ? C21 K1 N2 K1 113.22(7) 4 . . 4 ? C33 K1 N2 K1 -99.48(7) . . . 4 ? N3 K1 N2 K1 -0.27(5) 4 . . 4 ? C22 K1 N2 K1 133.34(6) 4 . . 4 ? C29 K1 N2 K1 53.80(16) 4 . . 4 ? K2 K1 N2 K1 76.79(5) . . . 4 ? K3 K1 N2 K1 -50.46(4) . . . 4 ? C3 N2 N3 C10 -1.5(3) . . . . ? K2 N2 N3 C10 142.86(17) . . . . ? K1 N2 N3 C10 -132.87(18) 4 . . . ? K1 N2 N3 C10 123.0(2) . . . . ? C3 N2 N3 K3 151.56(16) . . . . ? K2 N2 N3 K3 -64.0(2) . . . . ? K1 N2 N3 K3 20.22(17) 4 . . . ? K1 N2 N3 K3 -83.93(14) . . . . ? C3 N2 N3 K1 -124.50(17) . . . . ? K2 N2 N3 K1 19.89(15) . . . . ? K1 N2 N3 K1 104.15(6) 4 . . . ? C3 N2 N3 K1 131.3(2) . . . 4 ? K2 N2 N3 K1 -84.27(13) . . . 4 ? K1 N2 N3 K1 -104.15(6) . . . 4 ? N3 K3 N3 C10 -170.78(17) 4 . . . ? N4 K3 N3 C10 123.54(13) 4 . . . ? N4 K3 N3 C10 -60.13(13) . . . . ? C12 K3 N3 C10 138.89(13) 4 . . . ? C12 K3 N3 C10 -31.63(13) . . . . ? C11 K3 N3 C10 -9.11(12) . . . . ? C11 K3 N3 C10 172.20(12) 4 . . . ? C10 K3 N3 C10 -174.48(10) 4 . . . ? C20 K3 N3 C10 84.5(3) 4 . . . ? K1 K3 N3 C10 -112.63(14) . . . . ? N3 K3 N3 N2 32.23(14) 4 . . . ? N4 K3 N3 N2 -33.45(18) 4 . . . ? N4 K3 N3 N2 142.88(18) . . . . ? C12 K3 N3 N2 -18.1(2) 4 . . . ? C12 K3 N3 N2 171.39(19) . . . . ? C11 K3 N3 N2 -166.1(2) . . . . ? C11 K3 N3 N2 15.2(2) 4 . . . ? C10 K3 N3 N2 -157.0(3) . . . . ? C10 K3 N3 N2 28.53(18) 4 . . . ? C20 K3 N3 N2 -72.4(3) 4 . . . ? K1 K3 N3 N2 90.38(17) . . . . ? N3 K3 N3 K1 -58.14(4) 4 . . . ? N4 K3 N3 K1 -123.83(5) 4 . . . ? N4 K3 N3 K1 52.50(5) . . . . ? C12 K3 N3 K1 -108.48(7) 4 . . . ? C12 K3 N3 K1 81.01(6) . . . . ? C11 K3 N3 K1 103.52(8) . . . . ? C11 K3 N3 K1 -75.17(7) 4 . . . ? C10 K3 N3 K1 112.63(14) . . . . ? C10 K3 N3 K1 -61.85(5) 4 . . . ? C20 K3 N3 K1 -162.8(3) 4 . . . ? N3 K3 N3 K1 50.23(4) 4 . . 4 ? N4 K3 N3 K1 -15.46(5) 4 . . 4 ? N4 K3 N3 K1 160.88(5) . . . 4 ? C12 K3 N3 K1 -0.11(8) 4 . . 4 ? C12 K3 N3 K1 -170.62(6) . . . 4 ? C11 K3 N3 K1 -148.11(8) . . . 4 ? C11 K3 N3 K1 33.20(7) 4 . . 4 ? C10 K3 N3 K1 -139.00(14) . . . 4 ? C10 K3 N3 K1 46.52(5) 4 . . 4 ? C20 K3 N3 K1 -54.5(3) 4 . . 4 ? K1 K3 N3 K1 108.37(4) . . . 4 ? N4 K1 N3 C10 46.03(15) . . . . ? N1 K1 N3 C10 -131.94(15) 4 . . . ? N2 K1 N3 C10 170.45(16) 4 . . . ? C21 K1 N3 C10 -103.11(16) 4 . . . ? C33 K1 N3 C10 40.34(16) . . . . ? N3 K1 N3 C10 147.65(14) 4 . . . ? N2 K1 N3 C10 -129.2(2) . . . . ? C22 K1 N3 C10 -84.25(16) 4 . . . ? C29 K1 N3 C10 140.1(3) 4 . . . ? K2 K1 N3 C10 -141.06(16) . . . . ? K3 K1 N3 C10 99.07(16) . . . . ? N4 K1 N3 N2 175.21(12) . . . . ? N1 K1 N3 N2 -2.77(12) 4 . . . ? N2 K1 N3 N2 -60.38(11) 4 . . . ? C21 K1 N3 N2 26.07(13) 4 . . . ? C33 K1 N3 N2 169.52(11) . . . . ? N3 K1 N3 N2 -83.18(11) 4 . . . ? C22 K1 N3 N2 44.92(12) 4 . . . ? C29 K1 N3 N2 -90.8(3) 4 . . . ? K2 K1 N3 N2 -11.89(9) . . . . ? K3 K1 N3 N2 -131.75(12) . . . . ? N4 K1 N3 K3 -53.04(5) . . . . ? N1 K1 N3 K3 128.98(5) 4 . . . ? N2 K1 N3 K3 71.38(5) 4 . . . ? C21 K1 N3 K3 157.82(6) 4 . . . ? C33 K1 N3 K3 -58.73(5) . . . . ? N3 K1 N3 K3 48.57(4) 4 . . . ? N2 K1 N3 K3 131.75(12) . . . . ? C22 K1 N3 K3 176.68(5) 4 . . . ? C29 K1 N3 K3 41.0(3) 4 . . . ? K2 K1 N3 K3 119.86(4) . . . . ? N4 K1 N3 K1 -124.72(7) . . . 4 ? N1 K1 N3 K1 57.31(7) 4 . . 4 ? N2 K1 N3 K1 -0.30(6) 4 . . 4 ? C21 K1 N3 K1 86.15(8) 4 . . 4 ? C33 K1 N3 K1 -130.40(6) . . . 4 ? N3 K1 N3 K1 -23.10(6) 4 . . 4 ? N2 K1 N3 K1 60.08(10) . . . 4 ? C22 K1 N3 K1 105.00(6) 4 . . 4 ? C29 K1 N3 K1 -30.7(3) 4 . . 4 ? K2 K1 N3 K1 48.19(4) . . . 4 ? K3 K1 N3 K1 -71.67(5) . . . 4 ? N3 K3 N4 C12 79.57(13) . . . . ? N3 K3 N4 C12 152.37(12) 4 . . . ? N4 K3 N4 C12 116.56(12) 4 . . . ? C12 K3 N4 C12 -138.5(2) 4 . . . ? C11 K3 N4 C12 27.40(12) . . . . ? C11 K3 N4 C12 -159.62(12) 4 . . . ? C10 K3 N4 C12 56.38(12) . . . . ? C10 K3 N4 C12 173.95(12) 4 . . . ? C20 K3 N4 C12 -89.14(15) 4 . . . ? K1 K3 N4 C12 134.64(14) . . . . ? N3 K3 N4 C33 -135.8(2) . . . . ? N3 K3 N4 C33 -63.0(2) 4 . . . ? N4 K3 N4 C33 -98.8(2) 4 . . . ? C12 K3 N4 C33 6.2(3) 4 . . . ? C12 K3 N4 C33 144.6(3) . . . . ? C11 K3 N4 C33 172.0(2) . . . . ? C11 K3 N4 C33 -15.0(2) 4 . . . ? C10 K3 N4 C33 -159.0(2) . . . . ? C10 K3 N4 C33 -41.4(2) 4 . . . ? C20 K3 N4 C33 55.5(2) 4 . . . ? K1 K3 N4 C33 -80.7(2) . . . . ? N3 K3 N4 K1 -55.07(5) . . . . ? N3 K3 N4 K1 17.73(6) 4 . . . ? N4 K3 N4 K1 -18.08(3) 4 . . . ? C12 K3 N4 K1 86.90(14) 4 . . . ? C12 K3 N4 K1 -134.64(14) . . . . ? C11 K3 N4 K1 -107.24(8) . . . . ? C11 K3 N4 K1 65.73(8) 4 . . . ? C10 K3 N4 K1 -78.26(6) . . . . ? C10 K3 N4 K1 39.31(7) 4 . . . ? C20 K3 N4 K1 136.21(9) 4 . . . ? N1 K1 N4 C12 131.7(7) 4 . . . ? N2 K1 N4 C12 -90.3(2) 4 . . . ? N3 K1 N4 C12 -23.91(19) . . . . ? C21 K1 N4 C12 105.6(2) 4 . . . ? C33 K1 N4 C12 143.4(3) . . . . ? N3 K1 N4 C12 -90.6(2) 4 . . . ? N2 K1 N4 C12 -21.9(2) . . . . ? C22 K1 N4 C12 75.7(2) 4 . . . ? C29 K1 N4 C12 175.6(2) 4 . . . ? K2 K1 N4 C12 -33.7(2) . . . . ? K3 K1 N4 C12 -76.35(19) . . . . ? N1 K1 N4 C33 -11.8(8) 4 . . . ? N2 K1 N4 C33 126.22(12) 4 . . . ? N3 K1 N4 C33 -167.35(14) . . . . ? C21 K1 N4 C33 -37.86(18) 4 . . . ? N3 K1 N4 C33 125.92(12) 4 . . . ? N2 K1 N4 C33 -165.37(12) . . . . ? C22 K1 N4 C33 -67.71(14) 4 . . . ? C29 K1 N4 C33 32.21(15) 4 . . . ? K2 K1 N4 C33 -177.10(10) . . . . ? K3 K1 N4 C33 140.22(14) . . . . ? N1 K1 N4 K3 -152.0(7) 4 . . . ? N2 K1 N4 K3 -14.00(7) 4 . . . ? N3 K1 N4 K3 52.44(5) . . . . ? C21 K1 N4 K3 -178.08(10) 4 . . . ? C33 K1 N4 K3 -140.22(14) . . . . ? N3 K1 N4 K3 -14.30(5) 4 . . . ? N2 K1 N4 K3 54.41(5) . . . . ? C22 K1 N4 K3 152.07(6) 4 . . . ? C29 K1 N4 K3 -108.01(9) 4 . . . ? K2 K1 N4 K3 42.68(7) . . . . ? C21 N1 C1 C2 147.5(2) . . . . ? K2 N1 C1 C2 -60.4(2) . . . . ? K1 N1 C1 C2 18.5(3) 4 . . . ? C21 N1 C1 C13 -40.1(3) . . . . ? K2 N1 C1 C13 112.0(2) . . . . ? K1 N1 C1 C13 -169.05(16) 4 . . . ? C21 N1 C1 K2 -152.0(2) . . . . ? K1 N1 C1 K2 78.98(14) 4 . . . ? N1 K2 C1 N1 -169.40(17) 4 . . . ? N2 K2 C1 N1 -89.67(13) . . . . ? N2 K2 C1 N1 -37.81(16) 4 . . . ? C1 K2 C1 N1 113.87(13) 4 . . . ? C2 K2 C1 N1 -131.8(2) . . . . ? C2 K2 C1 N1 37.1(2) 4 . . . ? C3 K2 C1 N1 -108.36(14) . . . . ? C3 K2 C1 N1 -9.40(19) 4 . . . ? C32' K2 C1 N1 166.2(2) 4 . . . ? N1 K2 C1 C2 131.8(2) . . . . ? N1 K2 C1 C2 -37.6(2) 4 . . . ? N2 K2 C1 C2 42.11(13) . . . . ? N2 K2 C1 C2 93.97(14) 4 . . . ? C1 K2 C1 C2 -114.35(13) 4 . . . ? C2 K2 C1 C2 168.9(2) 4 . . . ? C3 K2 C1 C2 23.42(12) . . . . ? C3 K2 C1 C2 122.38(14) 4 . . . ? C32' K2 C1 C2 -62.0(2) 4 . . . ? N1 K2 C1 C13 -115.4(2) . . . . ? N1 K2 C1 C13 75.2(2) 4 . . . ? N2 K2 C1 C13 154.97(19) . . . . ? N2 K2 C1 C13 -153.17(16) 4 . . . ? C1 K2 C1 C13 -1.50(17) 4 . . . ? C2 K2 C1 C13 112.9(2) . . . . ? C2 K2 C1 C13 -78.2(2) 4 . . . ? C3 K2 C1 C13 136.3(2) . . . . ? C3 K2 C1 C13 -124.77(17) 4 . . . ? C32' K2 C1 C13 50.9(2) 4 . . . ? N1 C1 C2 C3 -12.2(4) . . . . ? C13 C1 C2 C3 174.8(2) . . . . ? K2 C1 C2 C3 -65.4(3) . . . . ? N1 C1 C2 K2 53.23(19) . . . . ? C13 C1 C2 K2 -119.80(19) . . . . ? N1 K2 C2 C1 -26.62(12) . . . . ? N1 K2 C2 C1 159.94(12) 4 . . . ? N2 K2 C2 C1 -124.94(15) . . . . ? N2 K2 C2 C1 -106.97(13) 4 . . . ? C1 K2 C2 C1 138.8(2) 4 . . . ? C2 K2 C2 C1 -115.65(13) 4 . . . ? C3 K2 C2 C1 -137.4(2) . . . . ? C3 K2 C2 C1 -97.12(16) 4 . . . ? C32' K2 C2 C1 116.6(2) 4 . . . ? N1 K2 C2 C3 110.75(15) . . . . ? N1 K2 C2 C3 -62.69(15) 4 . . . ? N2 K2 C2 C3 12.43(11) . . . . ? N2 K2 C2 C3 30.40(15) 4 . . . ? C1 K2 C2 C3 -83.9(2) 4 . . . ? C1 K2 C2 C3 137.4(2) . . . . ? C2 K2 C2 C3 21.72(12) 4 . . . ? C3 K2 C2 C3 40.3(2) 4 . . . ? C32' K2 C2 C3 -106.01(19) 4 . . . ? N3 N2 C3 C2 179.63(19) . . . . ? K2 N2 C3 C2 26.3(2) . . . . ? K1 N2 C3 C2 -60.8(2) 4 . . . ? K1 N2 C3 C2 103.7(2) . . . . ? N3 N2 C3 C4 2.2(3) . . . . ? K2 N2 C3 C4 -151.17(17) . . . . ? K1 N2 C3 C4 121.74(18) 4 . . . ? K1 N2 C3 C4 -73.7(3) . . . . ? N3 N2 C3 K2 153.4(2) . . . . ? K1 N2 C3 K2 -87.09(12) 4 . . . ? K1 N2 C3 K2 77.44(15) . . . . ? C1 C2 C3 N2 38.0(4) . . . . ? K2 C2 C3 N2 -22.98(19) . . . . ? C1 C2 C3 C4 -144.6(3) . . . . ? K2 C2 C3 C4 154.50(18) . . . . ? C1 C2 C3 K2 60.9(3) . . . . ? N1 K2 C3 N2 103.75(13) . . . . ? N1 K2 C3 N2 -71.49(13) 4 . . . ? N2 K2 C3 N2 0.81(15) 4 . . . ? C1 K2 C3 N2 -66.83(16) 4 . . . ? C1 K2 C3 N2 132.65(15) . . . . ? C2 K2 C3 N2 156.2(2) . . . . ? C2 K2 C3 N2 -20.19(19) 4 . . . ? C3 K2 C3 N2 0.57(11) 4 . . . ? C32' K2 C3 N2 -132.28(19) 4 . . . ? N1 K2 C3 C2 -52.41(12) . . . . ? N1 K2 C3 C2 132.34(13) 4 . . . ? N2 K2 C3 C2 -156.2(2) . . . . ? N2 K2 C3 C2 -155.35(12) 4 . . . ? C1 K2 C3 C2 137.01(14) 4 . . . ? C1 K2 C3 C2 -23.51(12) . . . . ? C2 K2 C3 C2 -176.35(7) 4 . . . ? C3 K2 C3 C2 -155.59(13) 4 . . . ? C32' K2 C3 C2 71.6(2) 4 . . . ? N1 K2 C3 C4 -167.3(4) . . . . ? N1 K2 C3 C4 17.5(4) 4 . . . ? N2 K2 C3 C4 88.9(4) . . . . ? N2 K2 C3 C4 89.8(4) 4 . . . ? C1 K2 C3 C4 22.1(4) 4 . . . ? C1 K2 C3 C4 -138.4(4) . . . . ? C2 K2 C3 C4 -114.9(4) . . . . ? C2 K2 C3 C4 68.8(4) 4 . . . ? C3 K2 C3 C4 89.5(4) 4 . . . ? C32' K2 C3 C4 -43.3(4) 4 . . . ? N2 C3 C4 C9 -0.1(3) . . . . ? C2 C3 C4 C9 -177.6(2) . . . . ? K2 C3 C4 C9 -73.5(4) . . . . ? N2 C3 C4 C5 180.0(2) . . . . ? C2 C3 C4 C5 2.5(3) . . . . ? K2 C3 C4 C5 106.7(4) . . . . ? C9 C4 C5 C6 2.6(4) . . . . ? C3 C4 C5 C6 -177.6(3) . . . . ? C4 C5 C6 C7 -0.3(5) . . . . ? C5 C6 C7 C8 -1.4(6) . . . . ? C6 C7 C8 C9 0.8(5) . . . . ? C5 C4 C9 C8 -3.1(4) . . . . ? C3 C4 C9 C8 177.0(2) . . . . ? C5 C4 C9 C10 177.4(2) . . . . ? C3 C4 C9 C10 -2.5(3) . . . . ? C7 C8 C9 C4 1.5(4) . . . . ? C7 C8 C9 C10 -179.0(3) . . . . ? N2 N3 C10 C9 -1.2(3) . . . . ? K3 N3 C10 C9 -161.17(17) . . . . ? K1 N3 C10 C9 113.06(18) . . . . ? K1 N3 C10 C9 -80.9(3) 4 . . . ? N2 N3 C10 C11 176.98(19) . . . . ? K3 N3 C10 C11 17.0(2) . . . . ? K1 N3 C10 C11 -68.7(2) . . . . ? K1 N3 C10 C11 97.3(2) 4 . . . ? N2 N3 C10 K3 159.9(2) . . . . ? K1 N3 C10 K3 -85.76(10) . . . . ? K1 N3 C10 K3 80.26(19) 4 . . . ? C4 C9 C10 N3 3.2(3) . . . . ? C8 C9 C10 N3 -176.3(2) . . . . ? C4 C9 C10 C11 -175.0(2) . . . . ? C8 C9 C10 C11 5.5(4) . . . . ? C4 C9 C10 K3 -63.7(6) . . . . ? C8 C9 C10 K3 116.8(5) . . . . ? N3 K3 C10 N3 9.31(17) 4 . . . ? N4 K3 C10 N3 -64.38(14) 4 . . . ? N4 K3 C10 N3 109.90(14) . . . . ? C12 K3 C10 N3 -59.84(17) 4 . . . ? C12 K3 C10 N3 139.76(16) . . . . ? C11 K3 C10 N3 164.3(2) . . . . ? C11 K3 C10 N3 -12.25(19) 4 . . . ? C10 K3 C10 N3 6.64(12) 4 . . . ? C20 K3 C10 N3 -144.94(16) 4 . . . ? K1 K3 C10 N3 53.88(13) . . . . ? N3 K3 C10 C9 77.0(6) . . . . ? N3 K3 C10 C9 86.3(6) 4 . . . ? N4 K3 C10 C9 12.6(6) 4 . . . ? N4 K3 C10 C9 -173.1(6) . . . . ? C12 K3 C10 C9 17.2(6) 4 . . . ? C12 K3 C10 C9 -143.2(6) . . . . ? C11 K3 C10 C9 -118.6(6) . . . . ? C11 K3 C10 C9 64.8(6) 4 . . . ? C10 K3 C10 C9 83.7(6) 4 . . . ? C20 K3 C10 C9 -67.9(6) 4 . . . ? K1 K3 C10 C9 130.9(6) . . . . ? N3 K3 C10 C11 -164.3(2) . . . . ? N3 K3 C10 C11 -155.02(12) 4 . . . ? N4 K3 C10 C11 131.29(12) 4 . . . ? N4 K3 C10 C11 -54.43(12) . . . . ? C12 K3 C10 C11 135.83(13) 4 . . . ? C12 K3 C10 C11 -24.57(12) . . . . ? C11 K3 C10 C11 -176.58(6) 4 . . . ? C10 K3 C10 C11 -157.69(13) 4 . . . ? C20 K3 C10 C11 50.73(19) 4 . . . ? K1 K3 C10 C11 -110.45(13) . . . . ? N3 C10 C11 C12 47.7(4) . . . . ? C9 C10 C11 C12 -134.1(3) . . . . ? K3 C10 C11 C12 62.8(2) . . . . ? N3 C10 C11 K3 -15.0(2) . . . . ? C9 C10 C11 K3 163.18(18) . . . . ? N3 K3 C11 C12 -127.59(16) . . . . ? N3 K3 C11 C12 -105.09(14) 4 . . . ? N4 K3 C11 C12 160.37(12) 4 . . . ? N4 K3 C11 C12 -27.53(12) . . . . ? C12 K3 C11 C12 138.4(2) 4 . . . ? C11 K3 C11 C12 -115.89(13) 4 . . . ? C10 K3 C11 C12 -135.7(2) . . . . ? C10 K3 C11 C12 -99.16(16) 4 . . . ? C20 K3 C11 C12 74.11(17) 4 . . . ? K1 K3 C11 C12 -75.83(13) . . . . ? N3 K3 C11 C10 8.11(11) . . . . ? N3 K3 C11 C10 30.60(15) 4 . . . ? N4 K3 C11 C10 -63.94(15) 4 . . . ? N4 K3 C11 C10 108.17(14) . . . . ? C12 K3 C11 C10 -85.92(19) 4 . . . ? C12 K3 C11 C10 135.7(2) . . . . ? C11 K3 C11 C10 19.80(12) 4 . . . ? C10 K3 C11 C10 36.5(2) 4 . . . ? C20 K3 C11 C10 -150.20(13) 4 . . . ? K1 K3 C11 C10 59.87(12) . . . . ? C33 N4 C12 C11 144.8(2) . . . . ? K3 N4 C12 C11 -63.0(2) . . . . ? K1 N4 C12 C11 12.7(3) . . . . ? C33 N4 C12 C17 -44.3(3) . . . . ? K3 N4 C12 C17 107.9(2) . . . . ? K1 N4 C12 C17 -176.42(15) . . . . ? C33 N4 C12 K3 -152.2(2) . . . . ? K1 N4 C12 K3 75.67(15) . . . . ? C10 C11 C12 N4 -10.9(4) . . . . ? K3 C11 C12 N4 57.2(2) . . . . ? C10 C11 C12 C17 177.6(2) . . . . ? K3 C11 C12 C17 -114.29(19) . . . . ? C10 C11 C12 K3 -68.1(3) . . . . ? N3 K3 C12 N4 -89.86(13) . . . . ? N3 K3 C12 N4 -34.74(15) 4 . . . ? N4 K3 C12 N4 -167.25(17) 4 . . . ? C12 K3 C12 N4 115.26(12) 4 . . . ? C11 K3 C12 N4 -130.1(2) . . . . ? C11 K3 C12 N4 38.5(2) 4 . . . ? C10 K3 C12 N4 -105.83(14) . . . . ? C10 K3 C12 N4 -9.06(18) 4 . . . ? C20 K3 C12 N4 107.02(14) 4 . . . ? K1 K3 C12 N4 -34.84(11) . . . . ? N3 K3 C12 C11 40.27(13) . . . . ? N3 K3 C12 C11 95.40(14) 4 . . . ? N4 K3 C12 C11 -37.1(2) 4 . . . ? N4 K3 C12 C11 130.1(2) . . . . ? C12 K3 C12 C11 -114.61(13) 4 . . . ? C11 K3 C12 C11 168.6(2) 4 . . . ? C10 K3 C12 C11 24.30(12) . . . . ? C10 K3 C12 C11 121.08(14) 4 . . . ? C20 K3 C12 C11 -122.85(15) 4 . . . ? K1 K3 C12 C11 95.30(13) . . . . ? N3 K3 C12 C17 153.82(19) . . . . ? N3 K3 C12 C17 -151.05(16) 4 . . . ? N4 K3 C12 C17 76.4(2) 4 . . . ? N4 K3 C12 C17 -116.3(2) . . . . ? C12 K3 C12 C17 -1.05(17) 4 . . . ? C11 K3 C12 C17 113.6(2) . . . . ? C11 K3 C12 C17 -77.8(2) 4 . . . ? C10 K3 C12 C17 137.9(2) . . . . ? C10 K3 C12 C17 -125.37(17) 4 . . . ? C20 K3 C12 C17 -9.3(2) 4 . . . ? K1 K3 C12 C17 -151.15(18) . . . . ? N1 C1 C13 C14 18.6(4) . . . . ? C2 C1 C13 C14 -168.5(3) . . . . ? K2 C1 C13 C14 97.7(2) . . . . ? N1 C1 C13 C16 -102.0(3) . . . . ? C2 C1 C13 C16 71.0(3) . . . . ? K2 C1 C13 C16 -22.8(3) . . . . ? N1 C1 C13 C15 139.3(3) . . . . ? C2 C1 C13 C15 -47.8(3) . . . . ? K2 C1 C13 C15 -141.6(2) . . . . ? N4 C12 C17 C18 21.7(4) . . . . ? C11 C12 C17 C18 -166.8(3) . . . . ? K3 C12 C17 C18 101.6(3) . . . . ? N4 C12 C17 C19 143.6(3) . . . . ? C11 C12 C17 C19 -44.9(4) . . . . ? K3 C12 C17 C19 -136.5(3) . . . . ? N4 C12 C17 C20 -95.6(3) . . . . ? C11 C12 C17 C20 75.9(3) . . . . ? K3 C12 C17 C20 -15.7(3) . . . . ? C1 N1 C21 C22 131.1(2) . . . . ? K2 N1 C21 C22 -7.0(3) . . . . ? K1 N1 C21 C22 -83.36(19) 4 . . . ? C1 N1 C21 C26 -58.6(3) . . . . ? K2 N1 C21 C26 163.30(16) . . . . ? K1 N1 C21 C26 86.92(19) 4 . . . ? C1 N1 C21 K1 -145.5(2) . . . 4 ? K2 N1 C21 K1 76.38(15) . . . 4 ? N1 C21 C22 C23 168.2(2) . . . . ? C26 C21 C22 C23 -2.2(3) . . . . ? K1 C21 C22 C23 101.8(2) 4 . . . ? N1 C21 C22 C30 -11.4(3) . . . . ? C26 C21 C22 C30 178.1(2) . . . . ? K1 C21 C22 C30 -77.8(2) 4 . . . ? N1 C21 C22 K1 66.41(16) . . . 4 ? C26 C21 C22 K1 -104.0(2) . . . 4 ? C21 C22 C23 C24 1.0(4) . . . . ? C30 C22 C23 C24 -179.3(3) . . . . ? K1 C22 C23 C24 69.4(3) 4 . . . ? C22 C23 C24 C25 0.6(5) . . . . ? C23 C24 C25 C26 -1.1(6) . . . . ? C24 C25 C26 C21 -0.1(5) . . . . ? C24 C25 C26 C27 -177.8(3) . . . . ? C22 C21 C26 C25 1.7(4) . . . . ? N1 C21 C26 C25 -168.7(2) . . . . ? K1 C21 C26 C25 -100.5(3) 4 . . . ? C22 C21 C26 C27 179.4(2) . . . . ? N1 C21 C26 C27 9.0(3) . . . . ? K1 C21 C26 C27 77.2(2) 4 . . . ? C25 C26 C27 C29 91.7(3) . . . . ? C21 C26 C27 C29 -85.9(3) . . . . ? C25 C26 C27 C28 -34.4(4) . . . . ? C21 C26 C27 C28 148.0(2) . . . . ? C23 C22 C30 C31 -65.3(4) . . . . ? C21 C22 C30 C31 114.3(4) . . . . ? K1 C22 C30 C31 55.5(3) 4 . . . ? C23 C22 C30 C32 58.3(4) . . . . ? C21 C22 C30 C32 -122.1(3) . . . . ? K1 C22 C30 C32 179.1(3) 4 . . . ? C12 N4 C33 C38 129.2(2) . . . . ? K3 N4 C33 C38 -5.0(3) . . . . ? K1 N4 C33 C38 -83.5(2) . . . . ? C12 N4 C33 C34 -59.2(3) . . . . ? K3 N4 C33 C34 166.61(16) . . . . ? K1 N4 C33 C34 88.1(2) . . . . ? C12 N4 C33 K1 -147.3(2) . . . . ? K3 N4 C33 K1 78.55(17) . . . . ? N1 K1 C33 N4 178.27(12) 4 . . . ? N2 K1 C33 N4 -69.91(14) 4 . . . ? N3 K1 C33 N4 11.71(13) . . . . ? C21 K1 C33 N4 157.11(12) 4 . . . ? N3 K1 C33 N4 -58.06(13) 4 . . . ? N2 K1 C33 N4 16.58(14) . . . . ? C22 K1 C33 N4 130.05(12) 4 . . . ? C29 K1 C33 N4 -150.50(14) 4 . . . ? K2 K1 C33 N4 7.0(3) . . . . ? K3 K1 C33 N4 -30.40(11) . . . . ? N4 K1 C33 C38 119.4(2) . . . . ? N1 K1 C33 C38 -62.34(19) 4 . . . ? N2 K1 C33 C38 49.48(17) 4 . . . ? N3 K1 C33 C38 131.10(15) . . . . ? C21 K1 C33 C38 -83.50(16) 4 . . . ? N3 K1 C33 C38 61.33(15) 4 . . . ? N2 K1 C33 C38 135.97(14) . . . . ? C22 K1 C33 C38 -110.56(15) 4 . . . ? C29 K1 C33 C38 -31.11(16) 4 . . . ? K2 K1 C33 C38 126.42(17) . . . . ? K3 K1 C33 C38 88.99(14) . . . . ? N4 K1 C33 C34 -119.4(2) . . . . ? N1 K1 C33 C34 58.9(2) 4 . . . ? N2 K1 C33 C34 170.72(14) 4 . . . ? N3 K1 C33 C34 -107.66(16) . . . . ? C21 K1 C33 C34 37.74(18) 4 . . . ? N3 K1 C33 C34 -177.43(15) 4 . . . ? N2 K1 C33 C34 -102.79(16) . . . . ? C22 K1 C33 C34 10.68(18) 4 . . . ? C29 K1 C33 C34 90.12(17) 4 . . . ? K2 K1 C33 C34 -112.34(19) . . . . ? K3 K1 C33 C34 -149.77(16) . . . . ? N4 C33 C34 C35 -170.8(2) . . . . ? C38 C33 C34 C35 0.8(3) . . . . ? K1 C33 C34 C35 -104.3(2) . . . . ? N4 C33 C34 C42 8.4(3) . . . . ? C38 C33 C34 C42 -179.9(2) . . . . ? K1 C33 C34 C42 74.9(2) . . . . ? C33 C34 C35 C36 0.8(4) . . . . ? C42 C34 C35 C36 -178.5(3) . . . . ? C34 C35 C36 C37 -1.9(5) . . . . ? C35 C36 C37 C38 1.3(5) . . . . ? C36 C37 C38 C33 0.3(4) . . . . ? C36 C37 C38 C39 -177.0(3) . . . . ? N4 C33 C38 C37 170.4(2) . . . . ? C34 C33 C38 C37 -1.4(4) . . . . ? K1 C33 C38 C37 106.3(2) . . . . ? N4 C33 C38 C39 -12.3(3) . . . . ? C34 C33 C38 C39 175.9(2) . . . . ? K1 C33 C38 C39 -76.5(2) . . . . ? C37 C38 C39 C40 -70.3(4) . . . . ? C33 C38 C39 C40 112.4(3) . . . . ? C37 C38 C39 C41 54.1(4) . . . . ? C33 C38 C39 C41 -123.2(3) . . . . ? C35 C34 C42 C43 100.0(3) . . . . ? C33 C34 C42 C43 -79.3(3) . . . . ? C35 C34 C42 C44 -27.1(4) . . . . ? C33 C34 C42 C44 153.6(3) . . . . ? C45 C46 O1 C47 -147(4) . . . . ? C46 O1 C47 C48 157(3) . . . . ? C45' C46' O1' C47' -154(3) . . . . ? C46' O1' C47' C48' 136(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.315 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.041 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 608910' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common holph19 _chemical_melting_point ? _chemical_formula_moiety 'C48 H69 K N4 O, 0.5(C7 H8)' _chemical_formula_sum 'C51.50 H73 K N4 O' _chemical_formula_weight 803.24 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 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4799(11) _cell_length_b 32.013(4) _cell_length_c 15.8987(18) _cell_angle_alpha 90.00 _cell_angle_beta 99.512(2) _cell_angle_gamma 90.00 _cell_volume 4758.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 3458 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 29.09 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 0.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9532 _exptl_absorpt_correction_T_max 0.9762 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(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 SMART APEX II CCD Platform' _diffrn_measurement_method 'area detector, \w scans per \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55151 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 30.03 _reflns_number_total 13796 _reflns_number_gt 9393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SIR97, CNR-IC' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0828P)^2^+2.1380P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13796 _refine_ls_number_parameters 581 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.95981(4) 0.228630(12) 0.13881(3) 0.02997(11) Uani 1 1 d D . . N2 N 0.77963(16) 0.16332(5) 0.12932(9) 0.0247(3) Uani 1 1 d . A . N3 N 0.73138(15) 0.18331(4) 0.05407(9) 0.0238(3) Uani 1 1 d . A . N4 N 0.55978(15) 0.22398(4) -0.21505(9) 0.0231(3) Uani 1 1 d . . . C1 C 0.7276(2) 0.09986(6) 0.30533(11) 0.0285(4) Uani 1 1 d D . . C2 C 0.8067(2) 0.10703(6) 0.23018(11) 0.0291(4) Uani 1 1 d . A . H2A H 0.8912 0.1245 0.2513 0.035 Uiso 1 1 calc R . . H2B H 0.8433 0.0796 0.2151 0.035 Uiso 1 1 calc R . . C3 C 0.73200(19) 0.12670(5) 0.14821(10) 0.0252(3) Uani 1 1 d . . . C4 C 0.6226(2) 0.10541(5) 0.09091(11) 0.0264(4) Uani 1 1 d . A . C5 C 0.5662(2) 0.06654(6) 0.11172(12) 0.0349(4) Uani 1 1 d . . . H5A H 0.6024 0.0536 0.1647 0.042 Uiso 1 1 calc R A . C6 C 0.4598(2) 0.04726(6) 0.05617(13) 0.0378(5) Uani 1 1 d . A . H6A H 0.4208 0.0215 0.0712 0.045 Uiso 1 1 calc R . . C7 C 0.4092(2) 0.06570(6) -0.02245(12) 0.0354(4) Uani 1 1 d . . . H7A H 0.3359 0.0523 -0.0611 0.042 Uiso 1 1 calc R A . C8 C 0.4647(2) 0.10322(5) -0.04462(11) 0.0292(4) Uani 1 1 d . A . H8A H 0.4303 0.1150 -0.0990 0.035 Uiso 1 1 calc R . . C9 C 0.57138(18) 0.12445(5) 0.01177(10) 0.0229(3) Uani 1 1 d . . . C10 C 0.63234(17) 0.16538(5) -0.00688(10) 0.0216(3) Uani 1 1 d . A . C11 C 0.58551(19) 0.18326(5) -0.08734(11) 0.0239(3) Uani 1 1 d . . . H11A H 0.5185 0.1656 -0.1213 0.029 Uiso 1 1 calc R A . C12 C 0.60959(17) 0.22047(5) -0.13293(10) 0.0215(3) Uani 1 1 d . A . C13 C 0.6459(2) 0.13598(6) 0.33860(12) 0.0337(4) Uani 1 1 d . A . C14 C 0.5192(2) 0.14954(7) 0.27204(14) 0.0392(5) Uani 1 1 d . . . H14A H 0.4567 0.1255 0.2556 0.059 Uiso 1 1 calc R A . H14B H 0.5542 0.1604 0.2217 0.059 Uiso 1 1 calc R . . H14C H 0.4654 0.1714 0.2961 0.059 Uiso 1 1 calc R . . C15 C 0.5876(3) 0.12271(8) 0.41903(14) 0.0459(5) Uani 1 1 d . . . H15A H 0.5190 0.0999 0.4050 0.069 Uiso 1 1 calc R A . H15B H 0.5397 0.1465 0.4410 0.069 Uiso 1 1 calc R . . H15C H 0.6667 0.1133 0.4625 0.069 Uiso 1 1 calc R . . C16 C 0.7496(3) 0.17282(7) 0.36092(14) 0.0434(5) Uani 1 1 d . . . H16A H 0.8316 0.1637 0.4027 0.065 Uiso 1 1 calc R A . H16B H 0.7002 0.1956 0.3851 0.065 Uiso 1 1 calc R . . H16C H 0.7830 0.1826 0.3092 0.065 Uiso 1 1 calc R . . C17 C 0.69134(18) 0.25911(5) -0.09360(11) 0.0237(3) Uani 1 1 d . . . C18 C 0.6339(2) 0.27290(6) -0.01361(12) 0.0299(4) Uani 1 1 d . A . H18A H 0.6410 0.2497 0.0270 0.045 Uiso 1 1 calc R . . H18B H 0.5336 0.2813 -0.0292 0.045 Uiso 1 1 calc R . . H18C H 0.6903 0.2966 0.0126 0.045 Uiso 1 1 calc R . . C19 C 0.85110(19) 0.24765(6) -0.07370(13) 0.0330(4) Uani 1 1 d . A . H19A H 0.8872 0.2427 -0.1271 0.049 Uiso 1 1 calc R . . H19B H 0.8632 0.2223 -0.0387 0.049 Uiso 1 1 calc R . . H19C H 0.9045 0.2707 -0.0426 0.049 Uiso 1 1 calc R . . C20 C 0.6755(2) 0.29610(6) -0.15594(13) 0.0321(4) Uani 1 1 d . A . H20A H 0.7163 0.2886 -0.2067 0.048 Uiso 1 1 calc R . . H20B H 0.7261 0.3204 -0.1282 0.048 Uiso 1 1 calc R . . H20C H 0.5739 0.3029 -0.1728 0.048 Uiso 1 1 calc R . . N1 N 0.7296(9) 0.06708(15) 0.3518(5) 0.0239(9) Uani 0.651(2) 1 d PD A 1 C21 C 0.8079(7) 0.0320(2) 0.3318(5) 0.0280(10) Uani 0.651(2) 1 d PD A 1 C22 C 0.9587(4) 0.03125(12) 0.3501(3) 0.0345(8) Uani 0.651(2) 1 d PD A 1 C23 C 1.0243(5) -0.00594(14) 0.3322(4) 0.0517(12) Uani 0.651(2) 1 d PD A 1 H23A H 1.1258 -0.0076 0.3427 0.062 Uiso 0.651(2) 1 calc PR A 1 C24 C 0.9460(7) -0.04055(16) 0.2995(5) 0.0599(17) Uani 0.651(2) 1 d PD A 1 H24A H 0.9942 -0.0654 0.2878 0.072 Uiso 0.651(2) 1 calc PR A 1 C25 C 0.7985(7) -0.0392(2) 0.2838(8) 0.0482(15) Uani 0.651(2) 1 d PD A 1 H25A H 0.7464 -0.0630 0.2604 0.058 Uiso 0.651(2) 1 calc PR A 1 C26 C 0.7250(10) -0.0035(4) 0.3016(17) 0.0323(12) Uani 0.651(2) 1 d PD A 1 C27 C 1.0408(3) 0.06812(11) 0.3940(2) 0.0384(7) Uani 0.651(2) 1 d PD A 1 H27A H 0.9965 0.0941 0.3662 0.046 Uiso 0.651(2) 1 calc PR A 1 C28 C 1.0238(4) 0.06986(14) 0.4879(2) 0.0525(8) Uani 0.651(2) 1 d PD A 1 H28A H 0.9221 0.0683 0.4925 0.079 Uiso 0.651(2) 1 calc PR A 1 H28B H 1.0637 0.0961 0.5130 0.079 Uiso 0.651(2) 1 calc PR A 1 H28C H 1.0747 0.0463 0.5185 0.079 Uiso 0.651(2) 1 calc PR A 1 C29 C 1.2003(4) 0.06902(14) 0.3865(3) 0.0552(9) Uani 0.651(2) 1 d PD A 1 H29A H 1.2111 0.0644 0.3270 0.083 Uiso 0.651(2) 1 calc PR A 1 H29B H 1.2507 0.0470 0.4223 0.083 Uiso 0.651(2) 1 calc PR A 1 H29C H 1.2408 0.0963 0.4055 0.083 Uiso 0.651(2) 1 calc PR A 1 C30 C 0.5637(12) -0.0021(6) 0.2966(15) 0.0287(16) Uani 0.651(2) 1 d PD A 1 H30A H 0.5299 0.0268 0.2796 0.034 Uiso 0.651(2) 1 calc PR A 1 C31 C 0.534(5) -0.0106(15) 0.3870(15) 0.0340(13) Uani 0.651(2) 1 d PD A 1 H31A H 0.5822 0.0107 0.4260 0.051 Uiso 0.651(2) 1 calc PR A 1 H31B H 0.5712 -0.0383 0.4056 0.051 Uiso 0.651(2) 1 calc PR A 1 H31C H 0.4312 -0.0096 0.3872 0.051 Uiso 0.651(2) 1 calc PR A 1 C32 C 0.480(3) -0.0331(9) 0.2346(15) 0.048(2) Uani 0.651(2) 1 d PD A 1 H32A H 0.5123 -0.0312 0.1793 0.073 Uiso 0.651(2) 1 calc PR A 1 H32B H 0.3778 -0.0265 0.2276 0.073 Uiso 0.651(2) 1 calc PR A 1 H32C H 0.4964 -0.0615 0.2572 0.073 Uiso 0.651(2) 1 calc PR A 1 N1' N 0.7495(19) 0.0632(3) 0.3403(10) 0.0239(9) Uani 0.349(2) 1 d PD A 5 C21' C 0.8081(13) 0.0245(5) 0.3165(12) 0.0280(10) Uani 0.349(2) 1 d PD A 5 C22' C 0.9580(8) 0.0180(2) 0.3241(5) 0.0345(8) Uani 0.349(2) 1 d PD A 5 C23' C 1.0050(11) -0.0211(3) 0.2995(7) 0.0517(12) Uani 0.349(2) 1 d PD A 5 H23B H 1.1047 -0.0258 0.3028 0.062 Uiso 0.349(2) 1 calc PR A 5 C24' C 0.9128(14) -0.0525(4) 0.2712(10) 0.0599(17) Uani 0.349(2) 1 d PD A 5 H24B H 0.9482 -0.0779 0.2519 0.072 Uiso 0.349(2) 1 calc PR A 5 C25' C 0.7682(16) -0.0477(5) 0.2704(17) 0.0482(15) Uani 0.349(2) 1 d PD A 5 H25B H 0.7048 -0.0703 0.2542 0.058 Uiso 0.349(2) 1 calc PR A 5 C26' C 0.7151(19) -0.0094(7) 0.293(3) 0.0323(12) Uani 0.349(2) 1 d PD A 5 C27' C 1.0635(6) 0.0517(2) 0.3605(4) 0.0384(7) Uani 0.349(2) 1 d PD A 5 H27B H 1.0093 0.0781 0.3661 0.046 Uiso 0.349(2) 1 calc PR A 5 C28' C 1.1384(7) 0.0385(3) 0.4490(4) 0.0525(8) Uani 0.349(2) 1 d PD A 5 H28D H 1.0689 0.0380 0.4883 0.079 Uiso 0.349(2) 1 calc PR A 5 H28E H 1.2145 0.0585 0.4696 0.079 Uiso 0.349(2) 1 calc PR A 5 H28F H 1.1798 0.0106 0.4458 0.079 Uiso 0.349(2) 1 calc PR A 5 C29' C 1.1756(7) 0.0603(3) 0.3025(5) 0.0552(9) Uani 0.349(2) 1 d PD A 5 H29D H 1.2393 0.0829 0.3271 0.083 Uiso 0.349(2) 1 calc PR A 5 H29E H 1.1270 0.0686 0.2457 0.083 Uiso 0.349(2) 1 calc PR A 5 H29F H 1.2318 0.0349 0.2979 0.083 Uiso 0.349(2) 1 calc PR A 5 C30' C 0.559(2) -0.0067(13) 0.303(3) 0.0287(16) Uani 0.349(2) 1 d PD A 5 H30B H 0.5276 0.0222 0.2847 0.034 Uiso 0.349(2) 1 calc PR A 5 C31' C 0.530(9) -0.011(3) 0.393(3) 0.0340(13) Uani 0.349(2) 1 d PD A 5 H31D H 0.5859 0.0093 0.4300 0.051 Uiso 0.349(2) 1 calc PR A 5 H31E H 0.5569 -0.0396 0.4141 0.051 Uiso 0.349(2) 1 calc PR A 5 H31F H 0.4277 -0.0070 0.3942 0.051 Uiso 0.349(2) 1 calc PR A 5 C32' C 0.465(6) -0.0357(18) 0.241(3) 0.048(2) Uani 0.349(2) 1 d PD A 5 H32D H 0.4754 -0.0286 0.1824 0.073 Uiso 0.349(2) 1 calc PR A 5 H32E H 0.3653 -0.0326 0.2482 0.073 Uiso 0.349(2) 1 calc PR A 5 H32F H 0.4957 -0.0647 0.2529 0.073 Uiso 0.349(2) 1 calc PR A 5 C33 C 0.49008(18) 0.19022(5) -0.26238(10) 0.0233(3) Uani 1 1 d . . . C34 C 0.56982(19) 0.16354(6) -0.30766(11) 0.0273(4) Uani 1 1 d . . . C35 C 0.4969(2) 0.13470(6) -0.36468(12) 0.0315(4) Uani 1 1 d . . . H35A H 0.5497 0.1169 -0.3960 0.038 Uiso 1 1 calc R . . C36 C 0.3495(2) 0.13138(6) -0.37669(12) 0.0325(4) Uani 1 1 d . . . H36A H 0.3017 0.1118 -0.4164 0.039 Uiso 1 1 calc R . . C37 C 0.2726(2) 0.15660(6) -0.33076(12) 0.0320(4) Uani 1 1 d . . . H37A H 0.1716 0.1537 -0.3381 0.038 Uiso 1 1 calc R . . C38 C 0.33964(19) 0.18651(6) -0.27342(11) 0.0266(4) Uani 1 1 d . . . C39 C 0.7321(2) 0.16435(7) -0.29139(14) 0.0406(5) Uani 1 1 d . . . H39A H 0.7634 0.1928 -0.2698 0.049 Uiso 1 1 calc R . . C40 C 0.7900(3) 0.13206(9) -0.22130(17) 0.0574(7) Uani 1 1 d . . . H40A H 0.7501 0.1380 -0.1695 0.086 Uiso 1 1 calc R . . H40B H 0.8946 0.1339 -0.2086 0.086 Uiso 1 1 calc R . . H40C H 0.7620 0.1039 -0.2415 0.086 Uiso 1 1 calc R . . C41 C 0.7995(3) 0.15560(10) -0.36973(18) 0.0627(8) Uani 1 1 d . . . H41A H 0.7577 0.1742 -0.4161 0.094 Uiso 1 1 calc R . . H41B H 0.7814 0.1265 -0.3874 0.094 Uiso 1 1 calc R . . H41C H 0.9028 0.1604 -0.3563 0.094 Uiso 1 1 calc R . . C42 C 0.2513(2) 0.21284(7) -0.22242(13) 0.0354(4) Uani 1 1 d . . . H42A H 0.3164 0.2331 -0.1874 0.042 Uiso 1 1 calc R . . C43 C 0.1331(2) 0.23743(6) -0.27830(14) 0.0378(4) Uani 1 1 d . . . H43A H 0.1760 0.2572 -0.3137 0.057 Uiso 1 1 calc R . . H43B H 0.0768 0.2527 -0.2420 0.057 Uiso 1 1 calc R . . H43C H 0.0707 0.2181 -0.3150 0.057 Uiso 1 1 calc R . . C44 C 0.1821(3) 0.18505(10) -0.16176(18) 0.0632(8) Uani 1 1 d . . . H44A H 0.2564 0.1687 -0.1259 0.095 Uiso 1 1 calc R . . H44B H 0.1135 0.1661 -0.1951 0.095 Uiso 1 1 calc R . . H44C H 0.1324 0.2026 -0.1255 0.095 Uiso 1 1 calc R . . C45 C 1.1357(5) 0.10490(14) 0.1227(3) 0.0780(10) Uani 0.742(4) 1 d PD B 1 H45A H 1.1056 0.0764 0.1058 0.117 Uiso 0.742(4) 1 calc PR B 1 H45B H 1.0939 0.1132 0.1725 0.117 Uiso 0.742(4) 1 calc PR B 1 H45C H 1.2403 0.1059 0.1369 0.117 Uiso 0.742(4) 1 calc PR B 1 C46 C 1.0871(5) 0.13359(14) 0.0519(4) 0.0780(10) Uani 0.742(4) 1 d PD B 1 H46A H 1.1283 0.1247 0.0015 0.094 Uiso 0.742(4) 1 calc PR B 1 H46B H 0.9817 0.1318 0.0369 0.094 Uiso 0.742(4) 1 calc PR B 1 O1 O 1.1266(3) 0.17575(8) 0.07166(19) 0.0504(6) Uani 0.742(4) 1 d PD B 1 C47 C 1.2720(7) 0.1829(2) 0.0740(7) 0.0643(16) Uani 0.742(4) 1 d PD B 1 H47A H 1.3020 0.1721 0.0213 0.077 Uiso 0.742(4) 1 calc PR B 1 H47B H 1.3280 0.1682 0.1234 0.077 Uiso 0.742(4) 1 calc PR B 1 C48 C 1.2990(12) 0.2295(2) 0.0816(5) 0.085(3) Uani 0.742(4) 1 d PD B 1 H48A H 1.4016 0.2350 0.0856 0.128 Uiso 0.742(4) 1 calc PR B 1 H48B H 1.2662 0.2401 0.1329 0.128 Uiso 0.742(4) 1 calc PR B 1 H48C H 1.2467 0.2437 0.0313 0.128 Uiso 0.742(4) 1 calc PR B 1 C45' C 1.0740(15) 0.1205(5) 0.0251(10) 0.0780(10) Uani 0.258(4) 1 d PD B 5 H45D H 1.0717 0.0899 0.0277 0.117 Uiso 0.258(4) 1 calc PR B 5 H45E H 1.1123 0.1292 -0.0258 0.117 Uiso 0.258(4) 1 calc PR B 5 H45F H 0.9769 0.1315 0.0223 0.117 Uiso 0.258(4) 1 calc PR B 5 C46' C 1.1701(14) 0.1375(3) 0.1051(9) 0.0780(10) Uani 0.258(4) 1 d PD B 5 H46C H 1.1326 0.1281 0.1565 0.094 Uiso 0.258(4) 1 calc PR B 5 H46D H 1.2679 0.1261 0.1081 0.094 Uiso 0.258(4) 1 calc PR B 5 O1' O 1.1755(7) 0.1813(2) 0.1041(6) 0.0504(6) Uani 0.258(4) 1 d PD B 5 C47' C 1.294(2) 0.1944(8) 0.072(2) 0.0643(16) Uani 0.258(4) 1 d PD B 5 H47C H 1.2983 0.1803 0.0173 0.077 Uiso 0.258(4) 1 calc PR B 5 H47D H 1.3816 0.1875 0.1127 0.077 Uiso 0.258(4) 1 calc PR B 5 C48' C 1.282(4) 0.2412(8) 0.0594(19) 0.085(3) Uani 0.258(4) 1 d PD B 5 H48D H 1.3636 0.2514 0.0351 0.128 Uiso 0.258(4) 1 calc PR B 5 H48E H 1.2803 0.2549 0.1145 0.128 Uiso 0.258(4) 1 calc PR B 5 H48F H 1.1930 0.2477 0.0205 0.128 Uiso 0.258(4) 1 calc PR B 5 C49 C 1.1795(12) -0.0453(4) 0.0391(9) 0.124(2) Uani 0.50 1 d P C -1 H49A H 1.1893 -0.0489 0.1010 0.186 Uiso 0.50 1 calc PR C -1 H49B H 1.2689 -0.0342 0.0249 0.186 Uiso 0.50 1 calc PR C -1 H49C H 1.1586 -0.0724 0.0110 0.186 Uiso 0.50 1 calc PR C -1 C50 C 1.0642(8) -0.0166(3) 0.0104(5) 0.124(2) Uani 0.50 1 d PG C -1 C51 C 0.9765(9) -0.0096(2) 0.0710(4) 0.1109(17) Uani 0.50 1 d PG C -1 H51A H 0.9947 -0.0238 0.1242 0.133 Uiso 0.50 1 calc PR C -1 C52 C 0.8623(8) 0.0180(2) 0.0537(4) 0.111(3) Uani 0.50 1 d PG C -1 H52A H 0.8023 0.0227 0.0951 0.134 Uiso 0.50 1 calc PR C -1 C53 C 0.8357(6) 0.0386(2) -0.0243(5) 0.124(2) Uani 0.50 1 d PG C -1 H53A H 0.7576 0.0575 -0.0361 0.149 Uiso 0.50 1 calc PR C -1 C54 C 0.9233(7) 0.0317(2) -0.0848(4) 0.102(3) Uani 0.50 1 d PG C -1 H54A H 0.9052 0.0458 -0.1381 0.122 Uiso 0.50 1 calc PR C -1 C55 C 1.0376(7) 0.0041(3) -0.0675(5) 0.1109(17) Uani 0.50 1 d PG C -1 H55A H 1.0975 -0.0007 -0.1089 0.133 Uiso 0.50 1 calc PR C -1 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 0.0307(2) 0.0284(2) 0.0312(2) -0.00857(15) 0.00641(15) -0.00570(15) N2 0.0294(7) 0.0242(7) 0.0203(6) -0.0008(5) 0.0037(5) -0.0008(6) N3 0.0283(7) 0.0218(7) 0.0210(6) 0.0003(5) 0.0032(5) -0.0014(6) N4 0.0251(7) 0.0219(7) 0.0220(6) 0.0020(5) 0.0033(5) -0.0020(5) C1 0.0306(9) 0.0326(9) 0.0203(8) -0.0007(7) -0.0012(6) -0.0076(7) C2 0.0335(9) 0.0299(9) 0.0231(8) 0.0031(7) 0.0024(7) -0.0023(7) C3 0.0317(9) 0.0244(8) 0.0198(7) -0.0013(6) 0.0051(6) -0.0013(7) C4 0.0365(9) 0.0223(8) 0.0210(8) -0.0010(6) 0.0063(7) -0.0019(7) C5 0.0522(12) 0.0250(9) 0.0261(9) 0.0032(7) 0.0021(8) -0.0090(8) C6 0.0546(13) 0.0237(9) 0.0334(10) 0.0020(7) 0.0025(9) -0.0128(9) C7 0.0441(11) 0.0274(9) 0.0320(9) -0.0019(7) -0.0013(8) -0.0113(8) C8 0.0375(10) 0.0220(8) 0.0259(8) 0.0006(6) -0.0008(7) -0.0035(7) C9 0.0290(8) 0.0178(8) 0.0217(7) -0.0020(6) 0.0040(6) -0.0001(6) C10 0.0247(8) 0.0184(7) 0.0225(7) -0.0026(6) 0.0062(6) 0.0004(6) C11 0.0286(8) 0.0196(8) 0.0232(8) -0.0007(6) 0.0031(6) -0.0027(6) C12 0.0198(7) 0.0215(8) 0.0238(7) -0.0013(6) 0.0055(6) -0.0003(6) C13 0.0433(11) 0.0326(10) 0.0261(9) -0.0054(7) 0.0078(8) -0.0081(8) C14 0.0388(11) 0.0404(11) 0.0392(11) -0.0075(9) 0.0093(9) 0.0011(9) C15 0.0639(15) 0.0457(13) 0.0323(10) -0.0050(9) 0.0205(10) -0.0102(11) C16 0.0543(13) 0.0366(11) 0.0392(11) -0.0090(9) 0.0074(10) -0.0125(10) C17 0.0244(8) 0.0213(8) 0.0254(8) -0.0003(6) 0.0041(6) -0.0031(6) C18 0.0387(10) 0.0220(8) 0.0296(9) -0.0051(7) 0.0070(7) -0.0015(7) C19 0.0250(9) 0.0367(11) 0.0367(10) 0.0036(8) 0.0037(7) -0.0057(8) C20 0.0353(10) 0.0246(9) 0.0359(10) 0.0020(7) 0.0047(8) -0.0072(7) N1 0.022(3) 0.0333(12) 0.018(2) 0.0004(14) 0.0088(12) -0.0011(10) C21 0.0320(10) 0.030(3) 0.023(3) 0.0054(17) 0.0094(13) 0.0048(14) C22 0.0332(11) 0.032(2) 0.041(2) 0.0124(14) 0.0140(15) 0.0113(16) C23 0.0441(19) 0.038(3) 0.079(4) 0.019(2) 0.028(2) 0.018(2) C24 0.071(4) 0.029(3) 0.092(6) 0.015(2) 0.048(4) 0.023(3) C25 0.069(3) 0.021(3) 0.063(4) 0.008(3) 0.037(3) 0.006(2) C26 0.0447(16) 0.025(3) 0.030(5) 0.006(3) 0.016(2) 0.0069(16) C27 0.0270(13) 0.043(2) 0.044(2) 0.0137(14) 0.0020(12) 0.0054(13) C28 0.0418(17) 0.070(2) 0.0415(16) 0.0101(16) -0.0065(13) -0.0097(15) C29 0.0326(15) 0.067(2) 0.067(2) 0.0208(19) 0.0090(15) 0.0026(15) C30 0.0407(13) 0.019(5) 0.027(3) 0.005(3) 0.0062(11) -0.0019(15) C31 0.038(3) 0.034(2) 0.032(3) 0.003(3) 0.012(3) -0.0013(15) C32 0.076(6) 0.030(4) 0.035(4) 0.003(3) -0.003(3) -0.011(3) N1' 0.022(3) 0.0333(12) 0.018(2) 0.0004(14) 0.0088(12) -0.0011(10) C21' 0.0320(10) 0.030(3) 0.023(3) 0.0054(17) 0.0094(13) 0.0048(14) C22' 0.0332(11) 0.032(2) 0.041(2) 0.0124(14) 0.0140(15) 0.0113(16) C23' 0.0441(19) 0.038(3) 0.079(4) 0.019(2) 0.028(2) 0.018(2) C24' 0.071(4) 0.029(3) 0.092(6) 0.015(2) 0.048(4) 0.023(3) C25' 0.069(3) 0.021(3) 0.063(4) 0.008(3) 0.037(3) 0.006(2) C26' 0.0447(16) 0.025(3) 0.030(5) 0.006(3) 0.016(2) 0.0069(16) C27' 0.0270(13) 0.043(2) 0.044(2) 0.0137(14) 0.0020(12) 0.0054(13) C28' 0.0418(17) 0.070(2) 0.0415(16) 0.0101(16) -0.0065(13) -0.0097(15) C29' 0.0326(15) 0.067(2) 0.067(2) 0.0208(19) 0.0090(15) 0.0026(15) C30' 0.0407(13) 0.019(5) 0.027(3) 0.005(3) 0.0062(11) -0.0019(15) C31' 0.038(3) 0.034(2) 0.032(3) 0.003(3) 0.012(3) -0.0013(15) C32' 0.076(6) 0.030(4) 0.035(4) 0.003(3) -0.003(3) -0.011(3) C33 0.0269(8) 0.0215(8) 0.0202(7) 0.0043(6) 0.0002(6) -0.0018(6) C34 0.0284(9) 0.0265(9) 0.0262(8) -0.0005(7) 0.0023(7) -0.0041(7) C35 0.0380(10) 0.0259(9) 0.0295(9) -0.0040(7) 0.0027(7) -0.0030(8) C36 0.0382(10) 0.0243(9) 0.0314(9) 0.0011(7) -0.0050(8) -0.0054(8) C37 0.0250(8) 0.0304(10) 0.0369(10) 0.0073(8) -0.0058(7) -0.0047(7) C38 0.0252(8) 0.0252(9) 0.0284(8) 0.0056(7) 0.0015(7) -0.0004(7) C39 0.0281(9) 0.0474(13) 0.0470(12) -0.0216(10) 0.0079(8) -0.0045(9) C40 0.0360(12) 0.0743(18) 0.0584(15) -0.0159(13) -0.0025(11) 0.0182(12) C41 0.0419(13) 0.086(2) 0.0640(16) -0.0306(15) 0.0196(12) -0.0124(13) C42 0.0265(9) 0.0412(11) 0.0385(10) -0.0003(8) 0.0053(8) 0.0023(8) C43 0.0339(10) 0.0311(10) 0.0484(12) 0.0054(9) 0.0071(9) 0.0042(8) C44 0.0581(16) 0.0771(19) 0.0618(16) 0.0315(14) 0.0315(13) 0.0317(14) C45 0.0618(17) 0.0597(19) 0.120(3) -0.0259(17) 0.0354(18) -0.0085(15) C46 0.0618(17) 0.0597(19) 0.120(3) -0.0259(17) 0.0354(18) -0.0085(15) O1 0.0326(13) 0.0496(12) 0.0717(19) -0.0286(12) 0.0164(12) -0.0060(10) C47 0.030(3) 0.102(5) 0.0573(17) -0.021(4) -0.001(2) 0.007(2) C48 0.059(3) 0.132(7) 0.069(5) -0.026(4) 0.026(4) -0.047(4) C45' 0.0618(17) 0.0597(19) 0.120(3) -0.0259(17) 0.0354(18) -0.0085(15) C46' 0.0618(17) 0.0597(19) 0.120(3) -0.0259(17) 0.0354(18) -0.0085(15) O1' 0.0326(13) 0.0496(12) 0.0717(19) -0.0286(12) 0.0164(12) -0.0060(10) C47' 0.030(3) 0.102(5) 0.0573(17) -0.021(4) -0.001(2) 0.007(2) C48' 0.059(3) 0.132(7) 0.069(5) -0.026(4) 0.026(4) -0.047(4) C49 0.100(4) 0.122(5) 0.140(5) -0.035(4) -0.008(4) -0.023(3) C50 0.100(4) 0.122(5) 0.140(5) -0.035(4) -0.008(4) -0.023(3) C51 0.107(4) 0.091(4) 0.136(4) -0.019(3) 0.024(3) -0.038(4) C52 0.091(6) 0.073(5) 0.155(9) -0.015(5) -0.024(6) 0.005(4) C53 0.100(4) 0.122(5) 0.140(5) -0.035(4) -0.008(4) -0.023(3) C54 0.059(4) 0.141(8) 0.104(6) -0.028(6) 0.009(4) 0.035(5) C55 0.107(4) 0.091(4) 0.136(4) -0.019(3) 0.024(3) -0.038(4) _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 2.658(2) . ? K1 O1' 2.675(6) . ? K1 N2 2.6881(15) . ? K1 N3 2.7650(15) . ? K1 N4 2.8054(14) 4_666 ? K1 C33 3.0250(17) 4_666 ? K1 C38 3.3393(18) 4_666 ? N2 C3 1.309(2) . ? N2 N3 1.3672(19) . ? N3 C10 1.360(2) . ? N4 C12 1.318(2) . ? N4 C33 1.417(2) . ? N4 K1 2.8054(14) 4_565 ? C1 N1 1.282(4) . ? C1 N1' 1.299(7) . ? C1 C2 1.529(3) . ? C1 C13 1.533(3) . ? C2 C3 1.514(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.435(2) . ? C4 C9 1.410(2) . ? C4 C5 1.415(3) . ? C5 C6 1.373(3) . ? C5 H5A 0.9500 . ? C6 C7 1.394(3) . ? C6 H6A 0.9500 . ? C7 C8 1.380(3) . ? C7 H7A 0.9500 . ? C8 C9 1.410(2) . ? C8 H8A 0.9500 . ? C9 C10 1.481(2) . ? C10 C11 1.405(2) . ? C11 C12 1.432(2) . ? C11 H11A 0.9500 . ? C12 C17 1.537(2) . ? C13 C14 1.527(3) . ? C13 C15 1.535(3) . ? C13 C16 1.539(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.529(2) . ? C17 C20 1.536(2) . ? C17 C19 1.540(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? N1 C21 1.411(5) . ? C21 C22 1.410(6) . ? C21 C26 1.420(6) . ? C22 C23 1.394(5) . ? C22 C27 1.519(5) . ? C23 C24 1.386(7) . ? C23 H23A 0.9500 . ? C24 C25 1.380(7) . ? C24 H24A 0.9500 . ? C25 C26 1.392(7) . ? C25 H25A 0.9500 . ? C26 C30 1.519(6) . ? C27 C28 1.530(5) . ? C27 C29 1.536(5) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.525(8) . ? C30 C31 1.533(8) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N1' C21' 1.436(11) . ? C21' C26' 1.407(13) . ? C21' C22' 1.421(11) . ? C22' C23' 1.407(10) . ? C22' C27' 1.518(8) . ? C23' C24' 1.358(12) . ? C23' H23B 0.9500 . ? C24' C25' 1.377(13) . ? C24' H24B 0.9500 . ? C25' C26' 1.396(12) . ? C25' H25B 0.9500 . ? C26' C30' 1.518(8) . ? C27' C28' 1.527(8) . ? C27' C29' 1.542(9) . ? C27' H27B 1.0000 . ? C28' H28D 0.9800 . ? C28' H28E 0.9800 . ? C28' H28F 0.9800 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? C30' C31' 1.518(14) . ? C30' C32' 1.521(14) . ? C30' H30B 1.0000 . ? C31' H31D 0.9800 . ? C31' H31E 0.9800 . ? C31' H31F 0.9800 . ? C32' H32D 0.9800 . ? C32' H32E 0.9800 . ? C32' H32F 0.9800 . ? C33 C38 1.413(2) . ? C33 C34 1.414(3) . ? C33 K1 3.0250(17) 4_565 ? C34 C35 1.395(2) . ? C34 C39 1.517(3) . ? C35 C36 1.383(3) . ? C35 H35A 0.9500 . ? C36 C37 1.376(3) . ? C36 H36A 0.9500 . ? C37 C38 1.400(3) . ? C37 H37A 0.9500 . ? C38 C42 1.515(3) . ? C38 K1 3.3393(18) 4_565 ? C39 C41 1.517(3) . ? C39 C40 1.552(4) . ? C39 H39A 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.528(3) . ? C42 C44 1.536(3) . ? C42 H42A 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.466(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 O1 1.422(5) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? O1 C47 1.392(5) . ? C47 C48 1.517(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C45' C46' 1.536(14) . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? C46' O1' 1.403(12) . ? C46' H46C 0.9900 . ? C46' H46D 0.9900 . ? O1' C47' 1.369(15) . ? C47' C48' 1.515(17) . ? C47' H47C 0.9900 . ? C47' H47D 0.9900 . ? C48' H48D 0.9800 . ? C48' H48E 0.9800 . ? C48' H48F 0.9800 . ? C49 C50 1.444(11) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.3900 . ? C50 C55 1.3900 . ? C51 C52 1.3900 . ? C51 H51A 0.9500 . ? C52 C53 1.3900 . ? C52 H52A 0.9500 . ? C53 C54 1.3900 . ? C53 H53A 0.9500 . ? C54 C55 1.3900 . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag #O1 K1 O1' 14.17(15) . . ? #N1 C1 N1' 13.7(7) . . ? O1 K1 N2 84.07(7) . . ? O1' K1 N2 92.74(17) . . ? O1 K1 N3 86.56(7) . . ? O1' K1 N3 99.54(17) . . ? N2 K1 N3 29.00(4) . . ? O1 K1 N4 122.36(7) . 4_666 ? O1' K1 N4 108.20(18) . 4_666 ? N2 K1 N4 126.28(5) . 4_666 ? N3 K1 N4 144.84(4) . 4_666 ? O1 K1 C33 138.07(7) . 4_666 ? O1' K1 C33 125.71(17) . 4_666 ? N2 K1 C33 134.59(5) . 4_666 ? N3 K1 C33 134.68(5) . 4_666 ? N4 K1 C33 27.79(4) 4_666 4_666 ? O1 K1 C38 162.32(7) . 4_666 ? O1' K1 C38 150.74(17) . 4_666 ? N2 K1 C38 113.50(5) . 4_666 ? N3 K1 C38 109.68(4) . 4_666 ? N4 K1 C38 46.04(4) 4_666 4_666 ? C33 K1 C38 25.03(4) 4_666 4_666 ? C3 N2 N3 122.81(14) . . ? C3 N2 K1 157.49(12) . . ? N3 N2 K1 78.62(9) . . ? C10 N3 N2 121.17(14) . . ? C10 N3 K1 164.08(11) . . ? N2 N3 K1 72.38(8) . . ? C12 N4 C33 121.37(14) . . ? C12 N4 K1 152.04(11) . 4_565 ? C33 N4 K1 84.76(9) . 4_565 ? N1 C1 C2 127.6(3) . . ? N1' C1 C2 113.9(5) . . ? N1 C1 C13 112.3(2) . . ? N1' C1 C13 125.9(5) . . ? C2 C1 C13 119.80(16) . . ? C3 C2 C1 121.02(16) . . ? C3 C2 H2A 107.1 . . ? C1 C2 H2A 107.1 . . ? C3 C2 H2B 107.1 . . ? C1 C2 H2B 107.1 . . ? H2A C2 H2B 106.8 . . ? N2 C3 C4 121.37(15) . . ? N2 C3 C2 116.12(15) . . ? C4 C3 C2 122.35(15) . . ? C9 C4 C5 120.10(16) . . ? C9 C4 C3 117.85(15) . . ? C5 C4 C3 122.06(16) . . ? C6 C5 C4 120.71(17) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C7 119.61(18) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C8 C7 C6 120.54(17) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C9 121.39(16) . . ? C7 C8 H8A 119.3 . . ? C9 C8 H8A 119.3 . . ? C4 C9 C8 117.62(15) . . ? C4 C9 C10 118.22(15) . . ? C8 C9 C10 124.16(15) . . ? N3 C10 C11 123.63(15) . . ? N3 C10 C9 118.48(14) . . ? C11 C10 C9 117.88(14) . . ? C10 C11 C12 138.33(16) . . ? C10 C11 H11A 110.8 . . ? C12 C11 H11A 110.8 . . ? N4 C12 C11 120.75(15) . . ? N4 C12 C17 114.11(14) . . ? C11 C12 C17 125.13(14) . . ? C14 C13 C1 111.07(15) . . ? C14 C13 C15 107.80(18) . . ? C1 C13 C15 110.53(17) . . ? C14 C13 C16 109.96(18) . . ? C1 C13 C16 108.53(17) . . ? C15 C13 C16 108.93(16) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C20 107.69(15) . . ? C18 C17 C12 110.23(14) . . ? C20 C17 C12 111.66(14) . . ? C18 C17 C19 111.81(15) . . ? C20 C17 C19 107.73(15) . . ? C12 C17 C19 107.73(14) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C1 N1 C21 118.7(6) . . ? C22 C21 N1 121.4(5) . . ? C22 C21 C26 122.8(6) . . ? N1 C21 C26 115.5(6) . . ? C23 C22 C21 116.4(4) . . ? C23 C22 C27 123.0(3) . . ? C21 C22 C27 120.4(3) . . ? C24 C23 C22 122.0(4) . . ? C24 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 121.0(5) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C21 117.3(6) . . ? C25 C26 C30 123.2(10) . . ? C21 C26 C30 119.4(10) . . ? C22 C27 C28 110.4(3) . . ? C22 C27 C29 114.5(3) . . ? C28 C27 C29 109.8(3) . . ? C22 C27 H27A 107.3 . . ? C28 C27 H27A 107.3 . . ? C29 C27 H27A 107.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 C32 115.2(19) . . ? C26 C30 C31 106(2) . . ? C32 C30 C31 109.6(10) . . ? C26 C30 H30A 108.5 . . ? C32 C30 H30A 108.5 . . ? C31 C30 H30A 108.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 N1' C21' 135.1(13) . . ? C26' C21' C22' 119.0(11) . . ? C26' C21' N1' 118.8(12) . . ? C22' C21' N1' 121.9(12) . . ? C23' C22' C21' 117.6(8) . . ? C23' C22' C27' 121.3(7) . . ? C21' C22' C27' 121.0(7) . . ? C24' C23' C22' 122.3(9) . . ? C24' C23' H23B 118.8 . . ? C22' C23' H23B 118.8 . . ? C23' C24' C25' 120.3(10) . . ? C23' C24' H24B 119.8 . . ? C25' C24' H24B 119.8 . . ? C24' C25' C26' 119.8(12) . . ? C24' C25' H25B 120.1 . . ? C26' C25' H25B 120.1 . . ? C25' C26' C21' 120.5(13) . . ? C25' C26' C30' 118(2) . . ? C21' C26' C30' 121(2) . . ? C22' C27' C28' 109.4(6) . . ? C22' C27' C29' 112.0(6) . . ? C28' C27' C29' 109.8(5) . . ? C22' C27' H27B 108.5 . . ? C28' C27' H27B 108.5 . . ? C29' C27' H27B 108.5 . . ? C27' C28' H28D 109.5 . . ? C27' C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C27' C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C27' C29' H29D 109.5 . . ? C27' C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C27' C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C31' C30' C26' 115(5) . . ? C31' C30' C32' 112.0(19) . . ? C26' C30' C32' 112(4) . . ? C31' C30' H30B 105.7 . . ? C26' C30' H30B 105.7 . . ? C32' C30' H30B 105.7 . . ? C30' C31' H31D 109.5 . . ? C30' C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C30' C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? C30' C32' H32D 109.5 . . ? C30' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C30' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C38 C33 C34 119.98(15) . . ? C38 C33 N4 120.18(16) . . ? C34 C33 N4 119.31(15) . . ? C38 C33 K1 90.02(10) . 4_565 ? C34 C33 K1 105.49(11) . 4_565 ? N4 C33 K1 67.45(8) . 4_565 ? C35 C34 C33 118.80(17) . . ? C35 C34 C39 120.10(17) . . ? C33 C34 C39 121.02(15) . . ? C36 C35 C34 121.43(18) . . ? C36 C35 H35A 119.3 . . ? C34 C35 H35A 119.3 . . ? C37 C36 C35 119.60(17) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C36 C37 C38 121.55(17) . . ? C36 C37 H37A 119.2 . . ? C38 C37 H37A 119.2 . . ? C37 C38 C33 118.61(17) . . ? C37 C38 C42 119.82(17) . . ? C33 C38 C42 121.53(16) . . ? C37 C38 K1 115.71(12) . 4_565 ? C33 C38 K1 64.95(9) . 4_565 ? C42 C38 K1 91.60(11) . 4_565 ? C41 C39 C34 114.18(18) . . ? C41 C39 C40 108.6(2) . . ? C34 C39 C40 109.86(19) . . ? C41 C39 H39A 108.0 . . ? C34 C39 H39A 108.0 . . ? C40 C39 H39A 108.0 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 C43 113.12(17) . . ? C38 C42 C44 110.17(18) . . ? C43 C42 C44 108.38(17) . . ? C38 C42 H42A 108.4 . . ? C43 C42 H42A 108.4 . . ? C44 C42 H42A 108.4 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O1 C46 C45 112.8(4) . . ? O1 C46 H46A 109.0 . . ? C45 C46 H46A 109.0 . . ? O1 C46 H46B 109.0 . . ? C45 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C47 O1 C46 112.7(4) . . ? C47 O1 K1 122.5(3) . . ? C46 O1 K1 122.8(2) . . ? O1 C47 C48 108.5(6) . . ? O1 C47 H47A 110.0 . . ? C48 C47 H47A 110.0 . . ? O1 C47 H47B 110.0 . . ? C48 C47 H47B 110.0 . . ? H47A C47 H47B 108.4 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46' C45' H45D 109.5 . . ? C46' C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? C46' C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? O1' C46' C45' 111.2(11) . . ? O1' C46' H46C 109.4 . . ? C45' C46' H46C 109.4 . . ? O1' C46' H46D 109.4 . . ? C45' C46' H46D 109.4 . . ? H46C C46' H46D 108.0 . . ? C47' O1' C46' 110.2(12) . . ? C47' O1' K1 127.0(12) . . ? C46' O1' K1 122.2(7) . . ? O1' C47' C48' 107.8(18) . . ? O1' C47' H47C 110.2 . . ? C48' C47' H47C 110.2 . . ? O1' C47' H47D 110.2 . . ? C48' C47' H47D 110.2 . . ? H47C C47' H47D 108.5 . . ? C47' C48' H48D 109.5 . . ? C47' C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? C47' C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? C51 C50 C55 120.0 . . ? C51 C50 C49 113.0(8) . . ? C55 C50 C49 127.0(8) . . ? C50 C51 C52 120.0 . . ? C50 C51 H51A 120.0 . . ? C52 C51 H51A 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52A 120.0 . . ? C51 C52 H52A 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C54 C55 C50 120.0 . . ? C54 C55 H55A 120.0 . . ? C50 C55 H55A 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag #N1' C1 N1 C21 -2(5) . . . . ? O1 K1 N2 C3 69.7(3) . . . . ? O1' K1 N2 C3 58.5(4) . . . . ? N3 K1 N2 C3 163.3(4) . . . . ? N4 K1 N2 C3 -56.5(3) 4_666 . . . ? C33 K1 N2 C3 -91.7(3) 4_666 . . . ? C38 K1 N2 C3 -108.2(3) 4_666 . . . ? O1 K1 N2 N3 -93.61(11) . . . . ? O1' K1 N2 N3 -104.8(2) . . . . ? N4 K1 N2 N3 140.15(8) 4_666 . . . ? C33 K1 N2 N3 104.96(10) 4_666 . . . ? C38 K1 N2 N3 88.45(9) 4_666 . . . ? C3 N2 N3 C10 -1.7(2) . . . . ? K1 N2 N3 C10 170.79(15) . . . . ? C3 N2 N3 K1 -172.48(17) . . . . ? O1 K1 N3 C10 -66.1(4) . . . . ? O1' K1 N3 C10 -71.8(5) . . . . ? N2 K1 N3 C10 -150.1(5) . . . . ? N4 K1 N3 C10 146.2(4) 4_666 . . . ? C33 K1 N3 C10 105.3(4) 4_666 . . . ? C38 K1 N3 C10 106.7(4) 4_666 . . . ? O1 K1 N3 N2 83.97(11) . . . . ? O1' K1 N3 N2 78.3(2) . . . . ? N4 K1 N3 N2 -63.78(12) 4_666 . . . ? C33 K1 N3 N2 -104.62(10) 4_666 . . . ? C38 K1 N3 N2 -103.20(9) 4_666 . . . ? N1 C1 C2 C3 135.3(6) . . . . ? N1' C1 C2 C3 135.0(10) . . . . ? C13 C1 C2 C3 -51.4(2) . . . . ? N3 N2 C3 C4 -1.3(3) . . . . ? K1 N2 C3 C4 -161.7(2) . . . . ? N3 N2 C3 C2 174.24(15) . . . . ? K1 N2 C3 C2 13.8(4) . . . . ? C1 C2 C3 N2 114.51(19) . . . . ? C1 C2 C3 C4 -70.0(2) . . . . ? N2 C3 C4 C9 2.4(3) . . . . ? C2 C3 C4 C9 -172.86(16) . . . . ? N2 C3 C4 C5 -177.62(18) . . . . ? C2 C3 C4 C5 7.1(3) . . . . ? C9 C4 C5 C6 -1.2(3) . . . . ? C3 C4 C5 C6 178.9(2) . . . . ? C4 C5 C6 C7 1.6(3) . . . . ? C5 C6 C7 C8 -0.3(3) . . . . ? C6 C7 C8 C9 -1.4(3) . . . . ? C5 C4 C9 C8 -0.5(3) . . . . ? C3 C4 C9 C8 179.48(17) . . . . ? C5 C4 C9 C10 179.32(17) . . . . ? C3 C4 C9 C10 -0.7(2) . . . . ? C7 C8 C9 C4 1.8(3) . . . . ? C7 C8 C9 C10 -178.06(18) . . . . ? N2 N3 C10 C11 -175.90(16) . . . . ? K1 N3 C10 C11 -29.7(5) . . . . ? N2 N3 C10 C9 3.3(2) . . . . ? K1 N3 C10 C9 149.5(3) . . . . ? C4 C9 C10 N3 -2.0(2) . . . . ? C8 C9 C10 N3 177.78(17) . . . . ? C4 C9 C10 C11 177.18(16) . . . . ? C8 C9 C10 C11 -3.0(3) . . . . ? N3 C10 C11 C12 -1.9(3) . . . . ? C9 C10 C11 C12 178.96(19) . . . . ? C33 N4 C12 C11 -4.6(2) . . . . ? K1 N4 C12 C11 152.40(18) 4_565 . . . ? C33 N4 C12 C17 175.80(14) . . . . ? K1 N4 C12 C17 -27.2(3) 4_565 . . . ? C10 C11 C12 N4 169.9(2) . . . . ? C10 C11 C12 C17 -10.6(3) . . . . ? N1 C1 C13 C14 -119.9(5) . . . . ? N1' C1 C13 C14 -121.4(11) . . . . ? C2 C1 C13 C14 65.8(2) . . . . ? N1 C1 C13 C15 -0.3(5) . . . . ? N1' C1 C13 C15 -1.8(11) . . . . ? C2 C1 C13 C15 -174.58(17) . . . . ? N1 C1 C13 C16 119.1(5) . . . . ? N1' C1 C13 C16 117.6(11) . . . . ? C2 C1 C13 C16 -55.2(2) . . . . ? N4 C12 C17 C18 129.06(16) . . . . ? C11 C12 C17 C18 -50.5(2) . . . . ? N4 C12 C17 C20 9.4(2) . . . . ? C11 C12 C17 C20 -170.14(16) . . . . ? N4 C12 C17 C19 -108.70(17) . . . . ? C11 C12 C17 C19 71.8(2) . . . . ? C2 C1 N1 C21 -2.7(11) . . . . ? C13 C1 N1 C21 -176.4(6) . . . . ? C1 N1 C21 C22 74.7(12) . . . . ? C1 N1 C21 C26 -112.3(16) . . . . ? N1 C21 C22 C23 176.3(6) . . . . ? C26 C21 C22 C23 3.7(17) . . . . ? N1 C21 C22 C27 1.3(11) . . . . ? C26 C21 C22 C27 -171.2(15) . . . . ? C21 C22 C23 C24 -1.0(8) . . . . ? C27 C22 C23 C24 173.8(5) . . . . ? C22 C23 C24 C25 -0.3(11) . . . . ? C23 C24 C25 C26 -1(2) . . . . ? C24 C25 C26 C21 4(3) . . . . ? C24 C25 C26 C30 -171.8(18) . . . . ? C22 C21 C26 C25 -5(3) . . . . ? N1 C21 C26 C25 -178.0(16) . . . . ? C22 C21 C26 C30 170.5(16) . . . . ? N1 C21 C26 C30 -2(3) . . . . ? C23 C22 C27 C28 -102.0(5) . . . . ? C21 C22 C27 C28 72.6(6) . . . . ? C23 C22 C27 C29 22.5(5) . . . . ? C21 C22 C27 C29 -162.9(6) . . . . ? C25 C26 C30 C32 -27(3) . . . . ? C21 C26 C30 C32 158(2) . . . . ? C25 C26 C30 C31 95(3) . . . . ? C21 C26 C30 C31 -81(3) . . . . ? N1 C1 N1' C21' 167(8) . . . . ? C2 C1 N1' C21' -15(2) . . . . ? C13 C1 N1' C21' 172.3(15) . . . . ? C1 N1' C21' C26' -108(3) . . . . ? C1 N1' C21' C22' 78(3) . . . . ? C26' C21' C22' C23' 6(3) . . . . ? N1' C21' C22' C23' 179.7(14) . . . . ? C26' C21' C22' C27' -171(3) . . . . ? N1' C21' C22' C27' 2(2) . . . . ? C21' C22' C23' C24' -1.6(18) . . . . ? C27' C22' C23' C24' 176.3(11) . . . . ? C22' C23' C24' C25' -4(2) . . . . ? C23' C24' C25' C26' 4(4) . . . . ? C24' C25' C26' C21' 1(6) . . . . ? C24' C25' C26' C30' -172(3) . . . . ? C22' C21' C26' C25' -6(6) . . . . ? N1' C21' C26' C25' -180(3) . . . . ? C22' C21' C26' C30' 167(3) . . . . ? N1' C21' C26' C30' -6(6) . . . . ? C23' C22' C27' C28' -69.5(10) . . . . ? C21' C22' C27' C28' 108.3(13) . . . . ? C23' C22' C27' C29' 52.5(10) . . . . ? C21' C22' C27' C29' -129.7(12) . . . . ? C25' C26' C30' C31' 97(6) . . . . ? C21' C26' C30' C31' -77(6) . . . . ? C25' C26' C30' C32' -32(6) . . . . ? C21' C26' C30' C32' 154(4) . . . . ? C12 N4 C33 C38 93.4(2) . . . . ? K1 N4 C33 C38 -76.05(14) 4_565 . . . ? C12 N4 C33 C34 -94.9(2) . . . . ? K1 N4 C33 C34 95.66(14) 4_565 . . . ? C12 N4 C33 K1 169.41(16) . . . 4_565 ? C38 C33 C34 C35 1.9(3) . . . . ? N4 C33 C34 C35 -169.84(16) . . . . ? K1 C33 C34 C35 -97.35(16) 4_565 . . . ? C38 C33 C34 C39 -174.74(17) . . . . ? N4 C33 C34 C39 13.5(3) . . . . ? K1 C33 C34 C39 86.03(18) 4_565 . . . ? C33 C34 C35 C36 -0.9(3) . . . . ? C39 C34 C35 C36 175.74(19) . . . . ? C34 C35 C36 C37 -0.9(3) . . . . ? C35 C36 C37 C38 1.7(3) . . . . ? C36 C37 C38 C33 -0.7(3) . . . . ? C36 C37 C38 C42 -178.39(17) . . . . ? C36 C37 C38 K1 73.44(19) . . . 4_565 ? C34 C33 C38 C37 -1.1(2) . . . . ? N4 C33 C38 C37 170.57(15) . . . . ? K1 C33 C38 C37 106.89(15) 4_565 . . . ? C34 C33 C38 C42 176.53(17) . . . . ? N4 C33 C38 C42 -11.8(2) . . . . ? K1 C33 C38 C42 -75.49(16) 4_565 . . . ? C34 C33 C38 K1 -107.98(16) . . . 4_565 ? N4 C33 C38 K1 63.68(13) . . . 4_565 ? C35 C34 C39 C41 37.0(3) . . . . ? C33 C34 C39 C41 -146.5(2) . . . . ? C35 C34 C39 C40 -85.4(2) . . . . ? C33 C34 C39 C40 91.2(2) . . . . ? C37 C38 C42 C43 -57.2(2) . . . . ? C33 C38 C42 C43 125.19(18) . . . . ? K1 C38 C42 C43 63.86(16) 4_565 . . . ? C37 C38 C42 C44 64.3(2) . . . . ? C33 C38 C42 C44 -113.3(2) . . . . ? K1 C38 C42 C44 -174.67(17) 4_565 . . . ? C45 C46 O1 C47 72.8(7) . . . . ? C45 C46 O1 K1 -91.0(4) . . . . ? O1' K1 O1 C47 -35.5(10) . . . . ? N2 K1 O1 C47 -162.9(6) . . . . ? N3 K1 O1 C47 168.1(6) . . . . ? N4 K1 O1 C47 -33.2(6) 4_666 . . . ? C33 K1 O1 C47 -2.8(6) 4_666 . . . ? C38 K1 O1 C47 10.9(7) 4_666 . . . ? O1' K1 O1 C46 126.8(10) . . . . ? N2 K1 O1 C46 -0.7(4) . . . . ? N3 K1 O1 C46 -29.7(4) . . . . ? N4 K1 O1 C46 129.0(4) 4_666 . . . ? C33 K1 O1 C46 159.5(3) 4_666 . . . ? C38 K1 O1 C46 173.1(3) 4_666 . . . ? C46 O1 C47 C48 171.3(6) . . . . ? K1 O1 C47 C48 -24.9(9) . . . . ? C45' C46' O1' C47' -96(2) . . . . ? C45' C46' O1' K1 76.1(12) . . . . ? O1 K1 O1' C47' 106(2) . . . . ? N2 K1 O1' C47' 158(2) . . . . ? N3 K1 O1' C47' 130(2) . . . . ? N4 K1 O1' C47' -72(2) 4_666 . . . ? C33 K1 O1' C47' -48(2) 4_666 . . . ? C38 K1 O1' C47' -47(2) 4_666 . . . ? O1 K1 O1' C46' -64.4(10) . . . . ? N2 K1 O1' C46' -12.2(9) . . . . ? N3 K1 O1' C46' -40.5(9) . . . . ? N4 K1 O1' C46' 117.6(9) 4_666 . . . ? C33 K1 O1' C46' 142.0(8) 4_666 . . . ? C38 K1 O1' C46' 142.3(8) 4_666 . . . ? C46' O1' C47' C48' 171(2) . . . . ? K1 O1' C47' C48' 0(3) . . . . ? C55 C50 C51 C52 0.0 . . . . ? C49 C50 C51 C52 178.7(10) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C50 0.0 . . . . ? C51 C50 C55 C54 0.0 . . . . ? C49 C50 C55 C54 -178.5(12) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.037 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.059